Stability of extemporaneously prepared rifaximin oral suspensions.
Cober, Mary Petrea; Johnson, Cary E; Lee, Jordan; Currie, Kenne
2010-02-15
The stability of extemporaneously prepared rifaximin oral suspensions was studied. An oral suspension of rifaximin 20 mg/mL was prepared by thoroughly grinding six 200-mg tablets of rifaximin in a glass mortar. Thirty milliliters of Ora-Plus and 30 mL of either Ora-Sweet or Ora-Sweet SF were mixed and added to the powder to make a final volume of 60 mL. Three identical samples of each formulation were prepared and placed in 2-oz amber plastic bottles with child-resistant caps and were stored at room temperature (23-25 degrees C). A 1-mL sample was withdrawn from each of the six bottles with a micropipette immediately after preparation and at 7, 15, 30, and 60 days. After further dilution to an expected concentration of 20 microg/mL with mobile phase, the samples were assayed in duplicate using stability-indicating high-performance liquid chromatography. The samples were visually examined for any color change and pH was tested on each day of analysis. Stability was determined by evaluating the percentage of the initial concentration remaining at each time point and defined as retention of at least 90% of the initial concentration of rifaximin. At least 99% of the initial rifaximin remained throughout the 60-day study period in both preparations. There were no detectable changes in color, odor, taste, or pH and no visible microbial growth in any sample. Extemporaneously prepared suspensions of rifaximin 20 mg/mL in 1:1 mixtures of Ora-Plus with either Ora-Sweet or Ora-Sweet SF were stable for at least 60 days when stored in 2-oz amber plastic bottles at room temperature.
Stability of an extemporaneously prepared alcohol-free phenobarbital suspension.
Cober, Mary Petrea; Johnson, Cary E
2007-03-15
The physical and chemical short-term stability of alcohol-free, oral suspensions of phenobarbital 10 mg/mL prepared from commercially available tablets in both a sugar and a sugar-free vehicle was assessed at room temperature. Phenobarbital oral suspension 10 mg/mL was prepared by crushing 10 60-mg tablets of phenobarbital with a mortar and pestle. A small amount of Ora-Plus was added to the phenobarbital powder to sufficiently wet the particles. A 1:1 mixture of Ora-Plus and either Ora-Sweet or Ora-Sweet SF was combined with the phenobarbital powder to produce a final volume of 60 mL. Three identical samples of each of the two different formulations were prepared and stored at room temperature in 2-oz amber plastic bottles. Immediately after preparation and at 15, 30, 60, and 115 days, the samples were assayed in duplicate by stability-indicating high-performance liquid chromatography. The samples were tasted and inspected for color and odor changes. The percent of the initial concentration remaining at each study time for each phenobarbital suspension was determined. Stability was defined as the retention of at least 90% of the initial concentration. There were no detectable changes in color, odor, and taste and no visible microbial growth in any sample. At least 98% of the initial phenobarbital concentration remained throughout the 115-day study period in both preparations. An extemporaneously prepared alcohol-free suspension of phenobarbital 10 mg/mL in a 1:1 mixture of Ora-Plus and Ora-Sweet or Ora-Sweet SF was stable for at least 115 days when stored in 2-oz amber plastic bottles at room temperature.
Stability of an extemporaneously prepared thalidomide suspension.
Kraft, Shawna; Johnson, Cary E; Tyler, Ryan P
2012-01-01
The short-term physical and chemical stability of an oral suspension of thalidomide 20 mg/mL was studied. An oral suspension of thalidomide 20 mg/mL was prepared by emptying the contents of 12 100-mg thalidomide capsules into a glass mortar; 30 mL of Ora-Plus and 30 mL of Ora-Sweet were mixed and added to the thalidomide powder to make a final volume of 60 mL. Three identical samples of the formulation were prepared and placed in 2-oz amber plastic bottles with child-resistant caps and stored under refrigeration (3-5 °C). A 1-mL sample was withdrawn from each of the three samples with a micropipette immediately after preparation and at 7, 14, 21, 28, and 35 days. After further dilution to an expected concentration of 20 μg/mL with acetonitrile-methanol and then dilution with mobile phase, the samples were assayed in duplicate using stability-indicating high-performance liquid chromatography. Stability was determined by evaluating the percentage of the initial concentration remaining at each time point; stability was defined as the retention of at least 90% of the initial concentration of thalidomide. At least 92% of the initial thalidomide concentration remained throughout the 35-day study period. There were no detectable changes in color, odor, or pH and no visible microbial growth in any sample. An extemporaneously prepared suspension of thalidomide 20 mg/mL in a 1:1 mixture of Ora-Plus and Ora-Sweet was stable for at least 35 days when stored in 2-oz amber plastic bottles under refrigeration.
Stability of extemporaneously prepared moxifloxacin oral suspensions.
Hutchinson, David J; Johnson, Cary E; Klein, Kristin C
2009-04-01
The stability of extemporaneously prepared moxifloxacin oral suspensions was studied. An oral suspension of moxifloxacin 20 mg/mL was prepared by thoroughly grinding three 400-mg tablets of moxifloxacin in a glass mortar. Thirty milliliters of Ora-Plus and 30 mL of either Ora-Sweet or Ora-Sweet SF were mixed and added to the powder to make a final volume of 60 mL. Three identical samples of each formulation were prepared and placed in 2-oz amber plastic bottles with child-resistant caps and were stored at room temperature (23-25 degrees C). A 1-mL sample was withdrawn from each of the six bottles with a micropipette immediately after preparation and at 7, 14, 28, 60, and 90 days. After further dilution to an expected concentration of 8 microg/ mL with sample diluent, the samples were assayed in duplicate by stability-indicating high-performance liquid chromatography. Stability was defined as the retention of at least 90% of the initial concentration. At least 99% of the initial moxifloxacin remained throughout the 90-day study period in both preparations. There were no detectable changes in color, odor, taste, and pH and no visible microbial growth in any sample. Extemporaneously compounded suspensions of moxifloxacin 20 mg/mL in a 1:1 mixture of Ora-Plus and Ora-Sweet or Ora-Sweet SF were stable for at least 90 days when stored in 2-oz amber plastic bottles at room temperature.
Preparation and recrystallization behavior of spray-dried co-amorphous naproxen-indomethacin.
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.
Stability of extemporaneously prepared glycopyrrolate oral suspensions.
Cober, Mary Petrea; Johnson, Cary E; Sudekum, David; Penprase, Kimberly
2011-05-01
The stability of extemporaneously prepared glycopyrrolate 0.5-mg/mL suspensions was evaluated. An oral suspension of glycopyrrolate 0.5 mg/mL was prepared by thoroughly grinding 30 1-mg tablets of glycopyrrolate in a glass mortar. Thirty milliliters of Ora-Plus and 30 mL of either Ora-Sweet or Ora-Sweet SF were mixed and added to the powder to make a final volume of 60 mL. Three identical samples of the formulation were prepared and placed in 2-oz amber plastic bottles with child-resistant caps and stored at room temperature (23-25 °C). A 1-mL sample was withdrawn from each of the three bottles with a micropipette immediately after preparation and 7, 15, 30, 60, and 90 days afterward. After further dilution to an expected concentration of 50 μg/mL with sample diluent, the samples were assayed in duplicate by stability-indicating high-performance liquid chromatography. The samples were visually examined for any color change and evaluated for pH on each day of analysis. Taste evaluations were performed at the beginning and end of the study. Stability was defined as the retention of at least 90% of the initial concentration. At least 95% of the initial glycopyrrolate remained throughout the 90-day study period in both preparations. There were no detectable changes in color, odor, taste, and pH, and no visible microbial growth was observed in any sample. Extemporaneously compounded suspensions of glycopyrrolate 0.5 mg/mL in a 1:1 mixture of Ora-Plus/Ora-Sweet or Ora-Plus/Ora-Sweet SF were stable for at least 90 days when stored in amber plastic bottles at room temperature.
Microstructural and mechanical characteristics of porous iron prepared by powder metallurgy.
Capek, Jaroslav; Vojtěch, Dalibor
2014-10-01
The demand for porous biodegradable load-bearing implants has been increasing recently. Based on investigations of biodegradable stents, porous iron may be a suitable material for such applications. In this study, we prepared porous iron samples with porosities of 34-51 vol.% by powder metallurgy using ammonium bicarbonate as a space-holder material. We studied sample microstructure (SEM-EDX and XRD), flexural and compressive behaviors (universal loading machine) and hardness HV5 (hardness tester) of the prepared samples. Sample porosity increased with the amount of spacer in the initial mixtures. Only the pore surfaces had insignificant oxidation and no other contamination was observed. Increasing porosity decreased the mechanical properties of the samples; although, the properties were still comparable with human bone and higher than those of porous non-metallic biomaterials and porous magnesium prepared in a similar way. Based on these results, powder metallurgy appears to be a suitable method for the preparation of porous iron for orthopedic applications. Copyright © 2014 Elsevier B.V. All rights reserved.
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.
Stability of an extemporaneously prepared tadalafil suspension.
Pettit, Rebecca S; Johnson, Cary E; Caruthers, Regine L
2012-04-01
The stability of an extemporaneously prepared tadalafil oral suspension was studied. An oral suspension of tadalafil 5 mg/mL was prepared by thoroughly grinding 15 20-mg tadalafil tablets in a glass mortar. Thirty milliliters of Ora-Plus and 30 mL of Ora-Sweet were mixed and added to the powder to make a final volume of 60 mL. Three identical samples of the formulation were prepared and placed in 2-oz amber plastic bottles with child-resistant caps and stored at room temperature (23-25 °C). A 1-mL sample was withdrawn from each of the three bottles with a micropipette immediately after preparation and at 7, 14, 28, 57, and 91 days. After double dilution (1:10 and 0.1:5 v/v) to an expected concentration of 10 μg/mL with methanol and mobile phase, respectively, the samples were assayed in duplicate using stability-indicating high-performance liquid chromatography. The samples were visually examined for any color change and evaluated for pH changes on each day of analysis. Taste evaluation was performed at the beginning and end of the study. Stability was defined as the retention of at least 90% of the initial concentration. At least 99% of the initial tadalafil concentration remained throughout the 91-day study period. There were no detectable changes in color, odor, taste, and pH, and no visible microbial growth was observed in any sample. An extemporaneously prepared suspension of tadalafil 5 mg/mL in a 1:1 mixture of Ora-Plus and Ora-Sweet was stable for at least 91 days when stored in amber plastic bottles at room temperature.
Preparation and Characterization of Niobium Doped Lead-Telluride Glass Ceramics
DOE Office of Scientific and Technical Information (OSTI.GOV)
Sathish, M.; Eraiah, B.; Anavekar, R. V.
2011-07-15
Niobium-lead-telluride glass ceramics of composition xNb{sub 2}O{sub 5}-(20-x) pbO-80TeO{sub 2}(where x = 0.1 mol% to 0.5 mol%) were prepared by using conventional melt quenching method. The prepared glass samples were initially amorphous in nature after annealed at 400 deg. c all samples were crystallized. This was confined by X-ray diffraction and scanning electron microscopy. The particle size of these glass ceramics have been calculated by using Debye-Scherer formula and the particle size is in the order of 15 nm to 60 nm. The scanning electron microscopy (SEM) photograph shows the presence of needle-like crystals in these samples.
Novel strategies for sample preparation in forensic toxicology.
Samanidou, Victoria; Kovatsi, Leda; Fragou, Domniki; Rentifis, Konstantinos
2011-09-01
This paper provides a review of novel strategies for sample preparation in forensic toxicology. The review initially outlines the principle of each technique, followed by sections addressing each class of abused drugs separately. The novel strategies currently reviewed focus on the preparation of various biological samples for the subsequent determination of opiates, benzodiazepines, amphetamines, cocaine, hallucinogens, tricyclic antidepressants, antipsychotics and cannabinoids. According to our experience, these analytes are the most frequently responsible for intoxications in Greece. The applications of techniques such as disposable pipette extraction, microextraction by packed sorbent, matrix solid-phase dispersion, solid-phase microextraction, polymer monolith microextraction, stir bar sorptive extraction and others, which are rapidly gaining acceptance in the field of toxicology, are currently reviewed.
Emwas, Abdul-Hamid M; Al-Talla, Zeyad A; Kharbatia, Najeh M
2015-01-01
To maximize the utility of gas chromatography-mass spectrometry (GC-MS) in metabonomics research, all stages of the experimental design should be standardized, including sample collection, storage, preparation, and sample separation. Moreover, the prerequisite for any GC-MS analysis is that a compound must be volatile and thermally stable if it is to be analyzed using this technique. Since many metabolites are nonvolatile and polar in nature, they are not readily amenable to analysis by GC-MS and require initial chemical derivatization of the polar functional groups in order to reduce the polarity and to increase the thermal stability and volatility of the analytes. In this chapter, an overview is presented of the optimum approach to sample collection, storage, and preparation for gas chromatography-mass spectrometry-based metabonomics with particular focus on urine samples as example of biofluids.
The Preparation and Simple Analysis of a Clay Nanoparticle Composite Hydrogel
ERIC Educational Resources Information Center
Warren, David S.; Sutherland, Sam P. H.; Kao, Jacqueline Y.; Weal, Geoffrey R.; Mackay, Sean M.
2017-01-01
Samples of a composite hydrogel incorporating clay (Laponite XLG and S-482) nanoparticles were prepared using N-isopropylacrylamide. The hydrogels were formed via a radical-initiated addition polymerization using potassium persulfate and N,N,N',N'-tetramethylethylenediamine. Students then measured the force required to stretch the gels and…
NEW COLUMN SEPARATION METHOD FOR EMERGENCY URINE SAMPLES
DOE Office of Scientific and Technical Information (OSTI.GOV)
Maxwell, S; Brian Culligan, B
2007-08-28
The Savannah River Site Environmental Bioassay Lab participated in the 2007 NRIP Emergency Response program administered by the National Institute for Standards and Technology (NIST) in May, 2007. A new rapid column separation method was applied directly to the NRIP 2007 emergency urine samples, with only minimal sample preparation to reduce preparation time. Calcium phosphate precipitation, previously used to pre-concentrate actinides and Sr-90 in NRIP 2006 urine and water samples, was not used for the NRIP 2007 urine samples. Instead, the raw urine was acidified and passed directly through the stacked resin columns (TEVA+TRU+SR Resins) to separate the actinides andmore » strontium from the NRIP urine samples more quickly. This improvement reduced sample preparation time for the NRIP 2007 emergency urine analyses significantly. This approach works well for small volume urine samples expected during an emergency response event. Based on initial feedback from NIST, the SRS Environmental Bioassay Lab had the most rapid analysis times for actinides and strontium-90 analyses for NRIP 2007 urine samples.« less
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 ...
Stability of Hydrocortisone Preservative-Free Oral Solutions.
Chappe, Julie; Osman, Névine; Cisternino, Salvatore; Fontan, Jean-Eudes; Schlatter, Joël
2015-01-01
The physical and chemical stability of a preservative-free oral solution of hydrocortisone succinate was studied at different pH values and storage temperatures. Oral solutions of hydrocortisone 1 mg/mL were prepared by dissolving hydrocortisone succinate powder in citrate buffers at pH 4.0, 5.5, and 6.5, or with sterile water (pH 7.4) stored in amber glass vials. Three identical samples of the formulations were prepared and stored under refrigeration (3-7°C), ambient temperature (20-22°C) and high temperature (29-31°C). A 200-μL sample was withdrawn from each of the 3 samples immediately after preparation and at 1, 7, 14, 21, and 35 days. Samples were assayed in duplicate using stability-indicating liquid chromatography. Stability was determined by evaluating the percentage of the initial concentration remaining at each time point; stability was defined as the retention of at least 90% of the initial concentration of hydrocortisone succinate. At least 92% of the initial hydrocortisone succinate concentration in solutions pH 5.5, 6.5, and 7.4 remained throughout the 14-day study period under refrigeration. There were no detectable changes in color, odor, or pH and no visible microbial growth in these samples. In other storage conditions, hydrocortisone succinate was rapidly degraded. The hydrocortisone succinate preservative-free oral solutions at pH 5.5, 6.5, or 7.4 are chemically stable when stored under refrigeration for at least 14 days. They provide flexible and convenient dosage forms without any preservatives for pediatric patients.
Aerosol preparation of intact lipoproteins
Benner, W Henry [Danville, CA; Krauss, Ronald M [Berkeley, CA; Blanche, Patricia J [Berkeley, CA
2012-01-17
A medical diagnostic method and instrumentation system for analyzing noncovalently bonded agglomerated biological particles is described. The method and system comprises: a method of preparation for the biological particles; an electrospray generator; an alpha particle radiation source; a differential mobility analyzer; a particle counter; and data acquisition and analysis means. The medical device is useful for the assessment of human diseases, such as cardiac disease risk and hyperlipidemia, by rapid quantitative analysis of lipoprotein fraction densities. Initially, purification procedures are described to reduce an initial blood sample to an analytical input to the instrument. The measured sizes from the analytical sample are correlated with densities, resulting in a spectrum of lipoprotein densities. The lipoprotein density distribution can then be used to characterize cardiac and other lipid-related health risks.
Process dependency of radiation hardness of rapid thermal reoxidized nitrided gate oxides
DOE Office of Scientific and Technical Information (OSTI.GOV)
Weishin Lu; Kuanchin Lin; Jenngwo Hwu
The radiation hardness of MOS capacitors with various reoxidized nitrided oxide (RNO) structures is studied by changing the durations of rapid thermal processes during sample preparation and by applying irradiation-then-anneal (ITA) treatments on samples after preparation. It is found that the initial flatband voltage and midgap interface trap density of MOS capacitors exhibit turnaround'' dependency on the total time of nitridation and reoxidation processes. For samples with nitrided oxide (NO) structures, the radiation-induced variations of above parameters are also turnaround''-dependent on nitridation time. However, when the reoxidation process is performed, the radiation hardness for all samples will be gradually improvedmore » with increasing reoxidation time no matter what the nitridation time is. The most radiation-hard process for RNO structures is suggested. Finally, it is found that when ITA treatments are applied on samples after preparation, their radiation hardness is much improved.« less
DOE Office of Scientific and Technical Information (OSTI.GOV)
Maharrey, Sean P.; Highley, Aaron M.; Behrens, Richard, Jr.
2007-12-01
The objective of this short-term LDRD project was to acquire the tools needed to use our chemical imaging precision mass analyzer (ChIPMA) instrument to analyze tissue samples. This effort was an outgrowth of discussions with oncologists on the need to find the cellular origin of signals in mass spectra of serum samples, which provide biomarkers for ovarian cancer. The ultimate goal would be to collect chemical images of biopsy samples allowing the chemical images of diseased and nondiseased sections of a sample to be compared. The equipment needed to prepare tissue samples have been acquired and built. This equipment includesmore » an cyro-ultramicrotome for preparing thin sections of samples and a coating unit. The coating unit uses an electrospray system to deposit small droplets of a UV-photo absorbing compound on the surface of the tissue samples. Both units are operational. The tissue sample must be coated with the organic compound to enable matrix assisted laser desorption/ionization (MALDI) and matrix enhanced secondary ion mass spectrometry (ME-SIMS) measurements with the ChIPMA instrument Initial plans to test the sample preparation using human tissue samples required development of administrative procedures beyond the scope of this LDRD. Hence, it was decided to make two types of measurements: (1) Testing the spatial resolution of ME-SIMS by preparing a substrate coated with a mixture of an organic matrix and a bio standard and etching a defined pattern in the coating using a liquid metal ion beam, and (2) preparing and imaging C. elegans worms. Difficulties arose in sectioning the C. elegans for analysis and funds and time to overcome these difficulties were not available in this project. The facilities are now available for preparing biological samples for analysis with the ChIPMA instrument. Some further investment of time and resources in sample preparation should make this a useful tool for chemical imaging applications.« less
NASA Astrophysics Data System (ADS)
Giovambattista, Nicolas; Starr, Francis W.; Poole, Peter H.
2017-07-01
Experiments and computer simulations of the transformations of amorphous ices display different behaviors depending on sample preparation methods and on the rates of change of temperature and pressure to which samples are subjected. In addition to these factors, simulation results also depend strongly on the chosen water model. Using computer simulations of the ST2 water model, we study how the sharpness of the compression-induced transition from low-density amorphous ice (LDA) to high-density amorphous ice (HDA) is influenced by the preparation of LDA. By studying LDA samples prepared using widely different procedures, we find that the sharpness of the LDA-to-HDA transformation is correlated with the depth of the initial LDA sample in the potential energy landscape (PEL), as characterized by the inherent structure energy. Our results show that the complex phenomenology of the amorphous ices reported in experiments and computer simulations can be understood and predicted in a unified way from knowledge of the PEL of the system.
NASA Astrophysics Data System (ADS)
Liao, Li; Wang, Xianyou; Luo, Xufang; Wang, Ximing; Gamboa, Sergio; Sebastian, P. J.
The cathode-active materials, layered Li[Ni 0.333Co 0.333Mn 0.293Al 0.04]O 2- zF z (0 ≤ z ≤ 0.1), were synthesized from a sol-gel precursor at 900 °C in air. The influence of Al-F co-substitution on the structural and electrochemical properties of the as-prepared samples was characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and electrochemical experiments. The results showed that Li[Ni 0.333Co 0.333Mn 0.293Al 0.04]O 2- zF z has a typical hexagonal structure with a single phase, the particle sizes of the samples tended to increase with increasing fluorine content. It has been found that Li[Ni 0.333Co 0.333Mn 0.293Al 0.04]O 1.95F 0.05 showed an improved cathodic behavior and discharge capacity retention compared to the undoped samples in the voltage range of 3.0-4.3 V. The electrodes prepared from Li[Ni 0.333Co 0.333Mn 0.293Al 0.04]O 1.95F 0.05 delivered an initial discharge capacity of 158 mAh -1 g and an initial coulombic efficiency is 91.3%, and the capacity retention at the 20th cycle was 94.9%. Though the F-doped samples had lower initial capacities, they showed better cycle performances compared with F-free samples. Therefore, this is a promising material for a lithium-ion battery.
Outcomes of using wet pooling to detect STEC and Salmonella
USDA-ARS?s Scientific Manuscript database
Objective: The objective of this work was to examine the reliability of wet pooling sample broths. Experimental Design & Analysis: Fresh sample enrichment broths (n=737) were used to prepare 148 wet pools of 5 broths each. The initial broths and the pools were screened for STEC and Salmonella. ...
Stability of extemporaneously prepared sodium phenylbutyrate oral suspensions.
Caruthers, Regine L; Johnson, Cary E
2007-07-15
In an effort to minimize barriers to compliance and adherence and to improve the accuracy of dosage measurement, sugar-containing and sugar-free sodium phenylbutyrate suspensions were formulated, and the stability of these products over a 90-day period was determined. An oral suspension of sodium phenylbutyrate 200 mg/mL was prepared by thoroughly grinding 12 g of Sodium Phenylbutyrate Powder, USP, in a glass mortar. Thirty milliliters of Ora-Plus and 30 mL of either Ora-Sweet or Ora-Sweet SF were mixed and added to the powder to make a final volume of 60 mL. Three identical samples of each formulation were prepared and placed in 2-oz amber plastic bottles with child-resistant caps and were stored at room temperature. A 500-microL sample was withdrawn from each of the six bottles with a micropipette immediately after preparation and at 7, 14, 28, 60, and 90 days. After further dilution to an expected concentration of 100 microg/mL with the mobile phase, the samples were assayed by high-performance liquid chromatography. Stability was defined as the retention of at least 90% of the initial concentration. At least 95% of the initial sodium phenylbutyrate concentration remained throughout the 90-day study period in both preparations. There were no detectable changes in color, odor, taste, and pH and no visible microbial growth in any sample. Extemporaneously compounded suspensions of sodium phenylbutyrate, 200 mg/mL, in a 1:1 mixture of Ora-Plus and Ora-Sweet or Ora-Sweet SF were stable for at least 90 days when stored in 2-oz amber plastic bottles at room temperature.
Stark, Peter C [Los Alamos, NM; Zurek, Eduardo [Barranquilla, CO; Wheat, Jeffrey V [Fort Walton Beach, FL; Dunbar, John M [Santa Fe, NM; Olivares, Jose A [Los Alamos, NM; Garcia-Rubio, Luis H [Temple Terrace, FL; Ward, Michael D [Los Alamos, NM
2011-07-26
There is provided a method and device for remote sampling, preparation and optical interrogation of a sample using light scattering and light absorption methods. The portable device is a filtration-based device that removes interfering background particle material from the sample matrix by segregating or filtering the chosen analyte from the sample solution or matrix while allowing the interfering background particles to be pumped out of the device. The segregated analyte is then suspended in a diluent for analysis. The device is capable of calculating an initial concentration of the analyte, as well as diluting the analyte such that reliable optical measurements can be made. Suitable analytes include cells, microorganisms, bioparticles, pathogens and diseases. Sample matrixes include biological fluids such as blood and urine, as well as environmental samples including waste water.
NASA Astrophysics Data System (ADS)
Bharathi, S.; Nataraj, D.; Mangalaraj, D.; Masuda, Y.; Senthil, K.; Yong, K.
2010-01-01
Single-crystalline porous hematite nanorods and spindle-like nanostructures were successfully synthesized by a low temperature reflux condensation method. Two different iron sources, namely, FeCl3·6H2O and Fe(NO3)3·9H2O, were hydrolyzed in the presence of urea to selectively prepare nanorods and spindle-like nanostructures. Initially, the akagenite phase was obtained by refluxing the precursor for 12 h and then the as-prepared akagenite nanostructures were transformed to porous hematite nanostructures upon calcination at 300 °C for 1 h. The shape and the aspect ratio of the 12 h refluxed sample was retained even after calcination and this shows the topotactic transformation of the nanostructure. TEM and HRTEM investigations have shown the porous nature of the prepared sample. Brunauer-Emmett-Teller and Barret-Joyner-Halenda measurements have shown a large surface area and distribution of mesopores in the nanorods sample. The photocatalytic activity of the prepared nanostructures towards RhB has reflected this variation in the pore size distribution and specific surface area, by showing a higher activity for the nanorods sample. Magnetic studies by VSM have shown a weak ferromagnetic behaviour in both the samples due to shape anisotropy.
Stability of extemporaneously prepared oxandrolone oral suspensions.
Johnson, Cary E; Cober, Mary Petrea; Hawkins, Katherine A; Julian, Justin D
2011-03-15
The stability of extemporaneously prepared oxandrolone oral suspensions was studied. Oxandrolone oral suspension (1 mg/mL) was prepared using oxandrolone tablets, Ora-Plus, and either Ora-Sweet or Ora-Sweet SF. Three identical samples of each formulation were prepared and stored in 2-oz amber plastic bottles with child-resistant caps at room temperature (23-25 °C). After thorough but gentle shaking by hand to prevent foaming, a 1-mL sample was withdrawn from each of the six bottles, diluted with mobile phase to an expected concentration of 200 μg/mL, and assayed in duplicate by injecting 5 μL into the high-performance liquid chromatography system immediately after preparation and at 7, 14, 35, 60, and 90 days. The samples were examined for any change in color or pH on each day of analysis. The stability of the suspensions was determined by calculating the percentage of the initial oxandrolone concentration remaining on each test day. Stability was defined as the retention of at least 90% of the initial oxandrolone concentration. At least 98% of the original oxandrolone concentration remained in both formulations at the end of the 90-day study period. There was no appreciable change in odor, taste, color, or pH. Both suspensions remained white in color and sweet with no aftertaste throughout the study period. The oxandrolone was easily resuspended with gentle shaking. Extemporaneously prepared suspensions of oxandrolone 1 mg/mL in 1:1 mixtures of Ora-Plus and either Ora-Sweet or Ora-Sweet SF were stable for at least 90 days when stored in 2-oz amber plastic bottles at room temperature.
Marine sediment sample preparation for analysis for low concentrations of fine detrital gold
Clifton, H. Edward; Hubert, Arthur; Phillips, R. Lawrence
1967-01-01
Analyses by atomic absorption for detrital gold in more than 2,000 beach, offshore, marine-terrace, and alluvial sands from southern Oregon have shown that the values determined from raw or unconcentrated sediment containing small amounts of gold are neither reproducible nor representative of the initial sample. This difficulty results from a 'particle sparsity effect', whereby the analysis for gold in a given sample depends more upon the occurrence of random flakes of gold in the analyzed portion than upon the actual gold content of the sample. The particle sparsity effect can largely be eliminated by preparing a gold concentrate prior to analysis. A combination of sieve, gravimetric, and magnetic separation produces a satisfactory concentrate that yields accurate and reproducible analyses. In concentrates of nearly every marine and beach sand studied, the gold occurs in the nonmagnetic fraction smaller than 0.124 mm and with a specific gravity greater than 3.3. The grain size of gold in stream sediments is somewhat more variable. Analysis of concentrates provides a means of greatly increasing the sensitivity of the analytical technique in relation to the initial sample. Gold rarely exceeds 1 part per million in even the richest black sand analyzed; to establish the distribution of gold (and platinum) in marine sediments and its relationship to source and environmental factors, one commonly needs to know their content to the part per billion range. Analysis of a concentrate and recalculation to the value in the initial sample permits this degree of sensitivity.
NASA Astrophysics Data System (ADS)
Smirnov, Michael A.; Sokolova, Maria P.; Bobrova, Natalya V.; Kasatkin, Igor A.; Lahderanta, Erkki; Elyashevich, Galina K.
2016-02-01
Electroconducting hydrogels (EH) based on copoly(aniline - p-phenylenediamine) grafted to the polyacrylamide for the application as pseudo-supercapacitor's electrodes have been prepared. The influence of preparation conditions on the structure and capacitance properties of the systems were investigated: we determined the optimal amount of p-phenylenediamine to obtain the network of swollen interconnected nanofibrils inside the hydrogel which provides the formation of continuous conducting phase. Structure and morphology of the prepared samples were investigated with UV-VIS spectroscopy, scanning electron microscopy (SEM) and wide-angle X-ray diffraction (WAXD). The maximal value of capacitance was 364 F g-1 at 0.2 A g-1. It was shown that the EH samples demonstrate the retention of 50% of their capacity at high current density 16 A g-1. Cycle-life measurements show evidence that capacitance of EH electrodes after 1000 cycles is higher than its initial value for all prepared samples. Changes of the copolymer structure during swelling in water have been studied with WAXD.
Nguyen, Van Cuong; Pho, Quoc Hue
2014-01-01
An adsorbent called chitosan coated magnetic hydroxyapatite nanoparticles (CS-MHAP) was prepared with the purpose of improvement for the removal of Ni2+ ions and textile dye by coprecipitation. Structure and properties of CS-MHAP were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and vibrating sample magnetometer (VSM). Weight percent of chitosan was investigated by thermal gravimetric analysis (TGA). The prepared CS-MHAP presents a significant improvement on the removal efficiency of Ni2+ ions and reactive blue 19 dye (RB19) in comparison with chitosan and magnetic hydroxyapatite nanoparticles. Moreover, the adsorption capacities were affected by several parameters such as contact time, initial concentration, adsorbent dosage, and initial pH. Interestingly, the prepared adsorbent could be easily recycled from an aqueous solution by an external magnet and reused for adsorption with high removal efficiency. PMID:24592158
Quantitation of heat-shock proteins in clinical samples using mass spectrometry.
Kaur, Punit; Asea, Alexzander
2011-01-01
Mass spectrometry (MS) is a powerful analytical tool for proteomics research and drug and biomarker discovery. MS enables identification and quantification of known and unknown compounds by revealing their structural and chemical properties. Proper sample preparation for MS-based analysis is a critical step in the proteomics workflow because the quality and reproducibility of sample extraction and preparation for downstream analysis significantly impact the separation and identification capabilities of mass spectrometers. The highly expressed proteins represent potential biomarkers that could aid in diagnosis, therapy, or drug development. Because the proteome is so complex, there is no one standard method for preparing protein samples for MS analysis. Protocols differ depending on the type of sample, source, experiment, and method of analysis. Molecular chaperones play significant roles in almost all biological functions due to their capacity for detecting intracellular denatured/unfolded proteins, initiating refolding or denaturation of such malfolded protein sequences and more recently for their role in the extracellular milieu as chaperokines. In this chapter, we describe the latest techniques for quantitating the expression of molecular chaperones in human clinical samples.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Oosthoek, J. L. M.; Kooi, B. J., E-mail: B.J.Kooi@rug.nl; Voogt, F. C.
2015-02-14
Phase-change memory line cells, where the active material has a thickness of 15 nm, were prepared for transmission electron microscopy (TEM) observation such that they still could be switched and characterized electrically after the preparation. The result of these observations in comparison with detailed electrical characterization showed (i) normal behavior for relatively long amorphous marks, resulting in a hyperbolic dependence between SET resistance and SET current, indicating a switching mechanism based on initially long and thin nanoscale crystalline filaments which thicken gradually, and (ii) anomalous behavior, which holds for relatively short amorphous marks, where initially directly a massive crystalline filament ismore » formed that consumes most of the width of the amorphous mark only leaving minor residual amorphous regions at its edges. The present results demonstrate that even in (purposely) thick TEM samples, the TEM sample preparation hampers the probability to observe normal behavior and it can be debated whether it is possible to produce electrically switchable TEM specimen in which the memory cells behave the same as in their original bulk embedded state.« less
NASA Astrophysics Data System (ADS)
Oosthoek, J. L. M.; Voogt, F. C.; Attenborough, K.; Verheijen, M. A.; Hurkx, G. A. M.; Gravesteijn, D. J.; Kooi, B. J.
2015-02-01
Phase-change memory line cells, where the active material has a thickness of 15 nm, were prepared for transmission electron microscopy (TEM) observation such that they still could be switched and characterized electrically after the preparation. The result of these observations in comparison with detailed electrical characterization showed (i) normal behavior for relatively long amorphous marks, resulting in a hyperbolic dependence between SET resistance and SET current, indicating a switching mechanism based on initially long and thin nanoscale crystalline filaments which thicken gradually, and (ii) anomalous behavior, which holds for relatively short amorphous marks, where initially directly a massive crystalline filament is formed that consumes most of the width of the amorphous mark only leaving minor residual amorphous regions at its edges. The present results demonstrate that even in (purposely) thick TEM samples, the TEM sample preparation hampers the probability to observe normal behavior and it can be debated whether it is possible to produce electrically switchable TEM specimen in which the memory cells behave the same as in their original bulk embedded state.
Skin Sterility After Application of a Vapocoolant Spray Part 2.
Mlynek, Karolina; Lyahn, Hwang; Richards, Bryson; Schleicher, William; Bassiri Gharb, Bahar; Procop, Gary; Tuohy, Marion; Zins, James
2015-08-01
Refrigerant sprays have been used for pain relief at the time of minor office procedures. However, their sterility remains in question. This study investigates the microbiologic effect of this vapocoolant when sprayed after 70 % isopropyl alcohol skin preparation. In 50 healthy volunteers, three skin culture samples were collected: Group 1 prior to alcohol application; Group 2 after preparation with alcohol, and Group 3 after preparation with alcohol followed with vapocoolant spray. Samples were cultured in a blinded fashion and analyzed after 5 days of incubation. Gram staining was performed when cultures were positive. Bacterial growth was found in 98 % of samples prior to any skin preparation. This was reduced to 54 % after alcohol use (Group 2). Spraying with the skin refrigerant further reduced bacterial growth to 46 % (Group 3). The results showed a significant reduction in the number of positive bacterial cultures following skin preparation with alcohol and when alcohol prep was followed by vapocoolant spray (p < 0.001) compared to initial cultures. No statistical difference was observed between Groups 2 and 3 (p = 0.74). The use of the vapocoolant spray does not compromise the sterility of the skin following alcohol prep. Both 70 % isopropyl alcohol antiseptic preparation and skin preparation followed by vapocoolant spray significantly reduce skin colonization when compared to unprepared skin (p < 0.001).
Chiral stability of an extemporaneously prepared clopidogrel bisulfate oral suspension.
Tynes, Clay R; Livingston, Brad; Patel, Hetesh; Arnold, John J
2014-01-01
The purpose of this study was to evaluate the chiral stability of clopidogrel bisulfate in an extemporaneously compounded oral suspension for a period of 60 days. A 5 mg/mL oral suspension of clopidogrel bisulfate was prepared from commercially available Plavix tablets. The clopidogrel suspension was then evenly divided between two light-resistant prescription bottles and stored either under refrigeration (4°C) or at room temperature (25°C). Samples were drawn from the stored suspensions immediately after preparation and on days 7, 14, 28, and 60. Samples were subsequently analyzed at each time point by high-performance liquid chromatography using a reversed-phase column, with chemical stability defined as the retention of at least 90% of the initial intact clopidogrel concentration measured. To determine the chiral stability of the suspension, samples were also analyzed by high-performance liquid chromatography using a chiral column to investigate possible enantiomeric inversion. Chiral stability was defined as the retention of at least 90% of the initial concentration of the suspension as the S-enantiomer, the active moiety of Plavix. Regardless of storage conditions, the oral suspension of clopidogrel retained at least 98% of the active S-enantiomer for 60 days after preparation. Compared with the clopidogrel suspension stored in the refrigerator, more chiral inversion was noted in the clopidogrel suspension stored at room temperature. Our investigation of chiral stability indicates that a 5 mg/mL clopidogrel oral suspension stored under refrigeration and at room temperature maintains chiral stability as the active S-enantiomer.
Cryochemical modification, activity, and toxicity of dioxidine
NASA Astrophysics Data System (ADS)
Vernaya, O. I.; Shabatin, V. P.; Shabatina, T. I.; Khvatov, D. I.; Semenov, A. M.; Yudina, T. P.; Danilov, V. S.
2017-02-01
Dioxidine nanoparticles are prepared via cryochemical modification of the pharmacopoeial dioxidine substance. The form of the cryomodified dioxidine is characterized by data from 1H NMR spectroscopy; X-ray diffraction analysis; such thermal analytical methods as TG and DSC; low-temperature argon adsorption; and transmission electron microscopy. It is shown that the cryomodified samples are synthesized in the form of dioxidine nanocrystals 50-300 nm in size, with a crystal structure differing from that of the initial pharmacopoeial substance. The prepared cryomodified dioxidine nanoparticles inhibit the growth of E. coli 52, S. aureus 144, M. cyaneum 98, and B. cereus 9 better than the initial pharmacopoeial substance, and have comparable chronic toxicity.
Sosnowska, Katarzyna; Winnicka, Katarzyna; Czajkowska-Kośnik, Anna
2009-01-01
In this paper, the stability of enalapril maleate in oral formulations prepared from commercially available tablets was investigated. Extemporaneously compounded, 0.1 mg/mL and 1.0 mg/mL, oral suspensions of enalapril maleate in sugar-containing and sugar-free vehicles were stored in the absence of light at 4 degrees and 25 degrees C for 30 days. Enalapril maleate stability was quantified after 7, 14, 21, and 30 days using HPLC method. Viscosities and pH of prepared suspensions were measured on each study day and no appreciable changes from the initial pH and initial viscosities occurred in any of the samples both at 25 degrees and 4 degrees C. It was shown that all the formulations retain minimum 98% of the initial enalapril maleate concentration after 30 days of storage at 25 degrees and 4 degrees C and they may provide an option in situations where the marketed suspension is unavailable.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Bannochie, C. J.; Diprete, D. P.; Pareizs, J. M.
Presented in this report are radionuclide concentrations required as part of the program of qualifying Sludge Batch 9 (SB9) for processing in the Defense Waste Processing Facility (DWPF). The SB9 material is currently in Tank 51 and has been washed and prepared for transfer to Tank 40. The acceptance evaluation needs to be completed prior to the transfer of the material in Tank 51 to Tank 40. The sludge slurry in Tank 40 has already been qualified for DWPF processing and is currently being processed as Sludge Batch 8 (SB8). The radionuclide concentrations were measured or estimated in the Tankmore » 51 SB9 Washed Qualification Sample prepared at Savannah River National Laboratory (SRNL). This sample was prepared from a three liter sample of Tank 51 sludge slurry (HTF-51-15-81) taken on July 23, 2015. The sample was delivered to SRNL where it was initially characterized in the Shielded Cells. Under the direction of Savannah River Remediation (SRR) it was then adjusted per the Tank Farm washing strategy as of October 20, 2015. This final slurry now has a composition expected to be similar to that of the slurry in Tank 51 after final preparations have been made for transfer of that slurry to Tank 40.« less
DOE Office of Scientific and Technical Information (OSTI.GOV)
Bannochie, C.; Diprete, D.; Pareizs, J.
Presented in this report are radionuclide concentrations required as part of the program of qualifying Sludge Batch 9 (SB9) for processing in the Defense Waste Processing Facility (DWPF). The SB9 material is currently in Tank 51 and has been washed and prepared for transfer to Tank 40. The acceptance evaluation needs to be completed prior to the transfer of the material in Tank 51 to Tank 40. The sludge slurry in Tank 40 has already been qualified for DWPF processing and is currently being processed as Sludge Batch 8 (SB8). The radionuclide concentrations were measured or estimated in the Tankmore » 51 SB9 Washed Qualification Sample prepared at Savannah River National Laboratory (SRNL). This sample was prepared from a three liter sample of Tank 51 sludge slurry (HTF-51-15-81) taken on July 23, 2015. The sample was delivered to SRNL where it was initially characterized in the Shielded Cells. Under the direction of Savannah River Remediation (SRR) it was then adjusted per the Tank Farm washing strategy as of October 20, 2015. This final slurry now has a compositioniv expected to be similar to that of the slurry in Tank 51 after final preparations have been made for transfer of that slurry to Tank 40.« less
DOE Office of Scientific and Technical Information (OSTI.GOV)
Lazarević, Zorica Ž., E-mail: lzorica@yahoo.com; Jovalekić, Čedomir; Sekulić, Dalibor L.
2013-10-15
Graphical abstract: - Highlights: • Sintered NiFe{sub 2}O{sub 4} was prepared by a soft mechanochemical route from mixture powders. • XRD and Raman measurements indicate that the prepared samples have spinel structure. • The activation energy ΔE are 0.653 and 0.452 eV for NiFe{sub 2}O{sub 4} samples. • Ferrite from Ni(OH){sub 2}/Fe{sub 2}O{sub 3} has lower DC conductivity than from Ni(OH){sub 2}/Fe(OH){sub 3} powders. • The values of dielectric constant of samples NiFe{sub 2}O{sub 4} are 70 and 200, respectively. - Abstract: Nickel ferrite, NiFe{sub 2}O{sub 4} was prepared by a soft mechanochemical route from a mixture of (1) Ni(OH){submore » 2} and α-Fe{sub 2}O{sub 3} and (2) Ni(OH){sub 2} and Fe(OH){sub 3} powders in a planetary ball mill for 25 h. The powder samples were sintered at 1100 °C for 2 h and were characterized by X-ray diffraction (XRD), Raman spectroscopy and scanning electron microscopy (SEM). Impedance spectroscopy techniques were used to study the effect of grain and grain boundary on the electrical properties of the prepared samples. A difference in dielectric constant (ε) and dielectric loss tangent (tan δ) of NiFe{sub 2}O{sub 4} samples obtained by the same methods but starting from different initial components was observed.« less
The effect of initial pressure on growth of FeNPs in amorphous carbon films
NASA Astrophysics Data System (ADS)
Mashayekhi, Fatemeh; Shafiekhani, Azizollah; Sebt, S. Ali; Darabi, Elham
2018-04-01
Iron nanoparticles in amorphous hydrogenated carbon films (FeNPs@a-C:H) were prepared with RF-sputtering and RFPECVD methods by acetylene gas and Fe target. In this paper, deposition and sputtering process were carried out under influence of different initial pressure gas. The morphology and roughness of surface of samples were studied by AFM technique and also TEM images show the exact size of FeNPs and encapsulated FeNPs@a-C:H. The localized surface plasmon resonance peak (LSPR) of FeNPs was studied using UV-vis absorption spectrum. The results show that the intensity and position of LSPR peak are increased by increasing initial pressure. Also, direct energy gap of samples obtained by Tauc law is decreased with respect to increasing initial pressure.
Seixas, Fábio Heredia; Estrela, Carlos; Bueno, Mike Reis; Sousa-Neto, Manoel Damião; Pécora, Jesus Djalma
2015-06-01
The aim of this study was to determine the root canal area before and after the instrumentation 1 mm short of the apical foramen by clinical and cone beam computed tomography (CBCT) methods, and to evaluate the cleanliness of the apical region in mesiodistal flattened teeth by using optical microscopy. Forty-two human single-canal mandibular incisors were instrumented using the Free Tip Preparation technique up to three, four or five instruments from the initial. Cone beam computed tomography scans were acquired of the samples before and after root canal preparation (RCP). Irrigation was performed by conventional or hydrodynamic means, using 2.5% sodium hypochlorite. The samples were prepared for observation under an optical microscope. Images were digitally obtained, analyzed and the results were submitted to statistical analysis (two-way ANOVA complemented by Bonferroni's post-test). There was no significant difference between the studied anatomical areas with both CBCT and clinical methods. There were no differences between irrigation methods. It was verified differences between instrumentation techniques. Instrumentation with four instruments from the initial instrument determined a significant increase in the contact area when compared to preparation with three instruments, but RCP with 5 instruments did not result in a better cleanliness. The analysis with CBCT was not capable to determine the precise shape of surgical apical area comparing to the clinical method. Both the conventional and hydrodynamic irrigation techniques were not able to promote root canals debris-free. The instruments action in root canal walls was proportional to the number of instruments used from the initial apical instrument.
Robust Sub-nanomolar Library Preparation for High Throughput Next Generation Sequencing.
Wu, Wells W; Phue, Je-Nie; Lee, Chun-Ting; Lin, Changyi; Xu, Lai; Wang, Rong; Zhang, Yaqin; Shen, Rong-Fong
2018-05-04
Current library preparation protocols for Illumina HiSeq and MiSeq DNA sequencers require ≥2 nM initial library for subsequent loading of denatured cDNA onto flow cells. Such amounts are not always attainable from samples having a relatively low DNA or RNA input; or those for which a limited number of PCR amplification cycles is preferred (less PCR bias and/or more even coverage). A well-tested sub-nanomolar library preparation protocol for Illumina sequencers has however not been reported. The aim of this study is to provide a much needed working protocol for sub-nanomolar libraries to achieve outcomes as informative as those obtained with the higher library input (≥ 2 nM) recommended by Illumina's protocols. Extensive studies were conducted to validate a robust sub-nanomolar (initial library of 100 pM) protocol using PhiX DNA (as a control), genomic DNA (Bordetella bronchiseptica and microbial mock community B for 16S rRNA gene sequencing), messenger RNA, microRNA, and other small noncoding RNA samples. The utility of our protocol was further explored for PhiX library concentrations as low as 25 pM, which generated only slightly fewer than 50% of the reads achieved under the standard Illumina protocol starting with > 2 nM. A sub-nanomolar library preparation protocol (100 pM) could generate next generation sequencing (NGS) results as robust as the standard Illumina protocol. Following the sub-nanomolar protocol, libraries with initial concentrations as low as 25 pM could also be sequenced to yield satisfactory and reproducible sequencing results.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Brady, D.N.; Church, B.W.; White, M.G.
Soil sampling activities during 1974 were concentrated in Area 5 of the Nevada Test Site (NTS). Area 5 has been assigned the highest priority because of the number of atmospheric test events held and a wide distribution of contaminants. Improved sampling techniques are described. Preliminary data analysis aided in designing a program to infer $sup 239-240$Pu results by Ge(Li) scanning techniques. (auth)
Effect of ultrasonic treatment and temperature on nanocrystalline TiO 2
NASA Astrophysics Data System (ADS)
Kim, D. H.; Ryu, H. W.; Moon, J. H.; Kim, J.
Nanocrystalline TiO 2 particles were precipitated from the ethanol solution of titanium isopropoxide (Ti(O- iPr) 4) and H 2O 2 by refluxing at 80 °C for 48 h. The obtained particles were filtered and dried at 100 °C for 12 h. The dried powder itself, the sample with heating at 400 °C, and the sample with ultrasonically treating were prepared to investigate the effects of post treatments on materials characteristics and electrochemical properties of nanocrystalline TiO 2. The X-ray diffraction patterns of all of the samples were fitted well to the anatase phase. The field emission-TEM image of as-prepared sample shows a uniform spherical morphology with 5 nm particle size and the sample heated at 400 °C shows slightly increased particle size of about 10 nm while maintaining spherical shape. The sample treated with ultrasonic for 5 h or more at room temperature shows high aspect ratio particle shape with an average diameter of 5 nm and a length of 20 nm. According to the results of the electrochemical testing, as-prepared sample, the sample heated at 400 °C for 3 h, and the sample treated with ultrasonic show initial capacities of 270, 310 and 340 mAh g -1, respectively.
Compatibility of butorphanol and droperidol in 0.9% sodium chloride injection.
Chen, Fu-Chao; Fang, Bao-Xia; Li, Peng; Yang, Jin-Guo; Zhou, Ben-Hong
2013-03-15
The compatibility and stability of butorphanol tartrate and droperidol in polyvinyl chloride (PVC) bags and glass bottles stored at 4°C and 25°C for up to 15 days were studied. Admixtures were assessed initially and for 15 days after preparation in PVC bags and glass bottles using 0.9% sodium chloride injection as a diluent and stored at 4°C and 25°C. The initial drug concentrations were 0.08 mg/mL for butorphanol tartrate and 0.05 mg/mL for droperidol. Samples were withdrawn from each container immediately after preparation and at predetermined intervals (2, 4, 8, 24, 48, 72, 120, 168, 240, and 360 hours after preparation). The solutions were visually inspected for precipitation, cloudiness, and discoloration at each sampling interval. Drug concentrations were determined using a validated high-pressure liquid chromatography method. After 15 days of storage, all formulations tested retained >98% of the initial concentrations of both drugs. The drug mixtures were clear in appearance, and no color change or precipitation was observed. Throughout this period, pH values remained stable. Admixtures of butorphanol tartrate 0.08 mg/mL and droperidol 0.05 mg/mL in 0.9% sodium chloride injection were stable for at least 360 hours when stored in PVC bags or glass bottles at 4°C and 25°C and protected from light.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Kumar, P.; Nath, M.; Ghosh, A.
2015-03-15
Mullite–zirconia composites containing 20 wt.% zirconia were prepared by reaction sintering of zircon flour, sillimanite beach sand and calcined alumina. 0 to 8 mol% of La{sub 2}O{sub 3} with respect to zirconia was used as sintering aid. The effect of additive on the various physical, microstructures, mechanical and thermo-mechanical properties was studied. Quantitative phase analysis shows the change in tetragonal zirconia content with incorporation of lanthanum oxide. La{sub 2}O{sub 3} addition has significantly improved the thermal shock resistance of the samples. Samples without additive retained only 20% of initial flexural strength after 5 cycles, whereas samples containing 5 mol% La{submore » 2}O{sub 3} retained almost 78% of its initial flexural strength even after 15 thermal shock cycles. - Highlights: • Mullite–zirconia composites were prepared by reaction sintering route utilizing zircon and sillimanite beach sand. • Lanthanum oxide was used as sintering aid. • The presence of lanthanum oxide decreased the densification temperature. • Lanthanum oxide significantly improved the thermal shock resistance of the composites.« less
NASA Astrophysics Data System (ADS)
Liang, Yan-Yu; Bao, Shu-Juan; Li, Hu-Lin
2006-07-01
A series of spinel-structured materials have been prepared by a simple hydrothermal procedure in an aqueous medium. The new synthetic method is time and energy saving i.e., no further thermal treatment and extended grinding. The main experimental process involved the insertion of lithium into electrolytic manganese dioxide with glucose as a mild reductant in an autoclave. Both the hydrothermal temperature and the presence of glucose play the critical roles in determining the final spinel integrity. Particular electrochemical performance has also been systematically explored, and the results show that Al 3+, F - co-substituted spinels have the best combination of initial capacity and capacity retention among all these samples, exhibited the initial capacity of 115 mAh/g and maintained more than 90% of the initial value at the 50th cycle.
Richard S. Reiner; Alan W. Rudie
2013-01-01
The Fiber and Chemical Sciences Research Work Unit at the Forest Products Laboratory began working out the preparation of cellulose nanocrystals in 2006, using the method of Dong, Revol, and Gray. Initial samples were provided to several scientists within the Forest Service. Continued requests for this material forced scale-up from the initial 20 g scale to kg...
Chen, Yi; Allard, Emma; Wooten, Anna; Hur, Minji; Sheth, Ishani; Laasri, Anna; Hammack, Thomas S; Macarisin, Dumitru
2016-01-01
The recovery and growth potential of Listeria monocytogenes was evaluated in three flavors of milkshakes (vanilla, strawberry, and chocolate) that were prepared from naturally contaminated ice cream linked to a listeriosis outbreak in the U.S. in 2015, and were subsequently held at room temperature for 14 h. The average lag phase duration of L. monocytogenes was 9.05 h; the average generation time was 1.67 h; and the average population level increase per sample at 14 h was 1.14 log CFU/g. Milkshake flavors did not significantly affect these parameters. The average lag phase duration of L. monocytogenes in milkshakes with initial contamination levels ≤ 3 CFU/g (9.50 h) was significantly longer (P < 0.01) than that with initial contamination levels > 3 CFU/g (8.60 h). The results highlight the value of using samples that are contaminated with very low levels of L. monocytogenes for recovery and growth evaluations. The behavior of L. monocytogenes populations in milkshakes prepared from naturally contaminated ice cream linked to the listeriosis outbreak should be taken into account when performing risk based analysis using this outbreak as a case study.
Chen, Yi; Allard, Emma; Wooten, Anna; Hur, Minji; Sheth, Ishani; Laasri, Anna; Hammack, Thomas S.; Macarisin, Dumitru
2016-01-01
The recovery and growth potential of Listeria monocytogenes was evaluated in three flavors of milkshakes (vanilla, strawberry, and chocolate) that were prepared from naturally contaminated ice cream linked to a listeriosis outbreak in the U.S. in 2015, and were subsequently held at room temperature for 14 h. The average lag phase duration of L. monocytogenes was 9.05 h; the average generation time was 1.67 h; and the average population level increase per sample at 14 h was 1.14 log CFU/g. Milkshake flavors did not significantly affect these parameters. The average lag phase duration of L. monocytogenes in milkshakes with initial contamination levels ≤ 3 CFU/g (9.50 h) was significantly longer (P < 0.01) than that with initial contamination levels > 3 CFU/g (8.60 h). The results highlight the value of using samples that are contaminated with very low levels of L. monocytogenes for recovery and growth evaluations. The behavior of L. monocytogenes populations in milkshakes prepared from naturally contaminated ice cream linked to the listeriosis outbreak should be taken into account when performing risk based analysis using this outbreak as a case study. PMID:27242775
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.
[Effect of Ti bonder on the bond strength between porcelain and titanium].
Yao, Hai; Luo, Xiao-ping
2009-12-01
To investigate the influence of GC Initial Ti Bonder on bond strength between Vita Titankeramik porcelain and titanium. Forty titanium samples were prepared and randomly assigned to 4 groups with 10 samples in each group. Samples in each group were subjected to one of the following surface treatments, burnishing (Group B), sandblasting (Group S), firing GC Initial Ti Bonder after burnishing (Group BG) and firing GC Initial Ti Bonder after sandblasting (Group SG). Vita Titankeramik porcelain were fired on the surface of each sample in the middle. Three-point bending tests were conducted on each sample according to the ISO 9693. The fracture patterns of all specimens were recorded using zoom stereo microscope (ZSM) and the fracture surfaces were observed under scanning electron microscope (SEM). With fired GC Initial Ti Bonder, the bond strength of Vita Titankeramik porcelain to titanium in Group BG and Group SG were (32.72 +/- 4.46) and (34.25 +/- 6.52) MPa respectively, which reach the ISO 9693 standard for clinical use and were significantly higher than those in Group B [(20.70 +/- 3.15) MPa] and Group S [(23.92 +/- 5.02) MPa]. GC Initial Ti Bonder can significantly improve bond strength between Vita Titankeramik porcelain and titanium.
Stability of dolasetron in two oral liquid vehicles.
Johnson, Cary E; Wagner, Deborah S; Bussard, Wendy E
2003-11-01
The stability of dolasetron 10 mg/mL over 90 days when prepared as an oral liquid formulation from commercially available tablets in both strawberry syrup and a sugar-free vehicle was studied. A liquid suspension of dolasetron mesylate 10 mg/mL was prepared from commercially available dolasetron tablets, OraPlus, and Ora-Sweet or strawberry syrup. Six samples of each formulation were prepared and stored in amber plastic bottles. Three samples of each formulation were refrigerated (3-5 degrees C) and three were stored at room temperature (23-25 degrees C). A 1-mL sample was withdrawn from each of the 12 bottles immediately and after 7, 14, 30, 60, and 90 days. After further dilution to an expected concentration of 10 micrograms/mL with sample diluent, the solutions were assayed in duplicate using high-performance liquid chromatography. The samples were also inspected for color and odor changes, and the pH of each sample was determined. The stability-indicating capability of the dolasetron assay was determined by forced degradation of four separate 10-mg/mL samples exposed to direct sunlight for 90 days. There were no detectable changes in color, odor, or taste and no visible microbial growth in any sample. At least 98% of the initial dolasetron concentration remained throughout the 90-day study period for all samples. An extemporaneously compounded oral liquid preparation of dolasetron mesylate 10 mg/mL in a 1:1 mixture of Ora-Plus and strawberry syrup or Ora-Sweet was stable for at least 90 days when stored at 3-5 or 23-25 degrees C.
Adsorption of NO on alumina-supported oxides and oxide-hydroxides of manganese.
Spasova, I; Nikolov, P; Mehandjiev, D
2005-10-15
The adsorption capacity for NO of alumina-supported oxides and oxide-hydroxides of manganese have been studied. Two series of samples have been prepared by precipitation on gamma-alumina and appropriate thermal treatment. The samples have been characterized by adsorption methods, magnetic methods, electronic paramagnetic resonance (EPR), transient response technique, and temperature-programmed desorption (TPD). The influence of the concentration of the initial manganese-containing solution has been investigated. The sample, prepared with a solution with Mn concentration of 4 g/100 ml, has been shown to be the best adsorbent for NO under the conditions of the experiment. It has been found that the presence mainly of Mn3+ ions on the surface of the support is probably responsible for the enhanced adsorption capacity.
Properties of ZnO nanocrystals prepared by radiation method
NASA Astrophysics Data System (ADS)
Čuba, Václav; Gbur, Tomáš; Múčka, Viliam; Nikl, Martin; Kučerková, Romana; Pospíšil, Milan; Jakubec, Ivo
2010-01-01
Zinc oxide nanoparticles were prepared by irradiation of aqueous solutions containing zinc(II) ions, propan-2-ol, polyvinyl alcohol, and hydrogen peroxide. Zinc oxide was found in solid phase either directly after irradiation, or after additional heat treatment. Various physicochemical parameters, including scintillation properties of prepared materials, were studied. After decomposition of impurities and annealing of oxygen vacancies, the samples showed intensive emission in visible spectral range and well-shaped exciton luminescence at 390-400 nm. The best scintillating properties had zinc oxide prepared from aqueous solutions containing zinc formate as initial precursor and hydrogen peroxide. Size of the crystalline particles ranged from tens to hundreds nm, depending on type of irradiated solution and post-irradiation thermal treatment.
NASA Astrophysics Data System (ADS)
Xiao, Liguang; Pang, Bo
2017-09-01
This experiment used zinc nitrate as precursor, ethanol as solvent and polyethylene glycol as dispersant, diatomite as carrier, diatomite loaded nano Zinc Oxide was prepared by sol-gel method, in addition, the formaldehyde degradation was studied by two kinds of experimental methods: preparation and loading, preparation and post loading, The samples were characterized by SEM, XRD, BET and IR. Experimental results showed that: Diatomite based nano Zinc Oxide had a continuous adsorption and degradation of formaldehyde, formaldehyde gas with initial concentration was 0.7mg/m3, after 36h degradation, the concentration reached 0.238mg/m3, the degradation rate reached to 66%.
3D imaging of cells and tissues by focused ion beam/scanning electron microscopy (FIB/SEM).
Drobne, Damjana
2013-01-01
Integration of a scanning electron microscope (SEM) and focused ion beam (FIB) technology into a single FIB/SEM system permits use of the FIB as a nano-scalpel to reveal site-specific subsurface microstructures which can be examined in great detail by SEM. The FIB/SEM technology is widely used in the semiconductor industry and material sciences, and recently its use in the life sciences has been initiated. Samples for FIB/SEM investigation can be either embedded in a plastic matrix, the traditional means of preparation of transmission electron microscopy (TEM) specimens, or simply dried as in samples prepared for SEM imaging. Currently, FIB/SEM is used in the life sciences for (a) preparation by the lift-out technique of lamella for TEM analysis, (b) tomography of samples embedded in a matrix, and (c) in situ site-specific FIB milling and SEM imaging using a wide range of magnifications. Site-specific milling and imaging has attracted wide interest as a technique in structural research of single eukaryotic and prokaryotic cells, small animals, and different animal tissue, but it still remains to be explored more thoroughly. In the past, preparation of samples for site-specific milling and imaging by FIB/SEM has typically adopted the embedding techniques used for TEM samples, and which have been very well described in the literature. Sample preparation protocols for the use of dried samples in FIB/SEM have been less well investigated. The aim of this chapter is to encourage application of FIB/SEM on dried biological samples. A detailed description of conventional dried sample preparation and FIB/SEM investigation of dried biological samples is presented. The important steps are described and illustrated, and direct comparison between embedded and dried samples of same tissues is provided. The ability to discover links between gross morphology of the tissue or organ, surface characteristics of any selected region, and intracellular structural details on the nanometer scale is an appealing application of electron microscopy in the life sciences and merits further exploration.
Initial Morphologic Evolution of Perdido Key Berm Nourishment, Florida
2013-08-01
December 18, 2011). METHODOLOGY : This study is based on beach-nearshore profiles, sediment samples, and wave data collected during the first 6 months...preparation). Vicksburg, MS: US Army Engineering Reserach and Development Center. NOTE: The contents of this technical note are not to be used for
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...
Gignac, Lynne M; Mittal, Surbhi; Bangsaruntip, Sarunya; Cohen, Guy M; Sleight, Jeffrey W
2011-12-01
The ability to prepare multiple cross-section transmission electron microscope (XTEM) samples from one XTEM sample of specific sub-10 nm features was demonstrated. Sub-10 nm diameter Si nanowire (NW) devices were initially cross-sectioned using a dual-beam focused ion beam system in a direction running parallel to the device channel. From this XTEM sample, both low- and high-resolution transmission electron microscope (TEM) images were obtained from six separate, specific site Si NW devices. The XTEM sample was then re-sectioned in four separate locations in a direction perpendicular to the device channel: 90° from the original XTEM sample direction. Three of the four XTEM samples were successfully sectioned in the gate region of the device. From these three samples, low- and high-resolution TEM images of the Si NW were taken and measurements of the NW diameters were obtained. This technique demonstrated the ability to obtain high-resolution TEM images in directions 90° from one another of multiple, specific sub-10 nm features that were spaced 1.1 μm apart.
Myers, Alan L; Zhang, Yanping; Kawedia, Jitesh D; Shank, Brandon R; Deaver, Melissa A; Kramer, Mark A
2016-12-15
The chemical stability and physical compatibility of tacrolimus i.v. infusion solutions prepared in Excel bags and stored at 23 or 4 °C for up to nine days were studied. Tacrolimus admixtures (2, 4, and 8 μg/mL) were prepared in Excel bags using 0.9% sodium chloride injection and stored at 23 °C without protection from light or at 4 °C in the dark. Test samples were withdrawn from triplicate bag solutions immediately after preparation and at predetermined time intervals (1, 3, 5, 7, and 9 days). Chemical stability was assessed by measuring tacrolimus concentrations using a validated stability-indicating high-performance liquid chromatography assay. The physical stability of the admixtures was assessed by visual examination and by measuring turbidity, particle size, and drug content. All test solutions stored at 23 or 4 °C had a no greater than 6% loss of the initial tacrolimus concentration throughout the nine-day study period. All test samples of tacrolimus admixtures, under both storage conditions, were without precipitation and remained clear initially and throughout the nine-day observation period. Changes in turbidities were minor; measured particulates remained few in number in all samples throughout the study. Extemporaneously prepared infusion solutions of tacrolimus 2, 4, and 8 μg/mL in 0.9% sodium chloride injection in Excel bags were chemically and physically stable for at least nine days when stored at room temperature (23 °C) without protection from light and when stored in a refrigerator (4 °C) in the dark. Copyright © 2016 by the American Society of Health-System Pharmacists, Inc. All rights reserved.
Phosphate removal from aqueous solutions using raw and activated red mud and fly ash.
Li, Yanzhong; Liu, Changjun; Luan, Zhaokun; Peng, Xianjia; Zhu, Chunlei; Chen, Zhaoyang; Zhang, Zhongguo; Fan, Jinghua; Jia, Zhiping
2006-09-01
The effect of acidification and heat treatment of raw red mud (RM) and fly ash (FA) on the sorption of phosphate was studied in parallel experiments. The result shows that a higher efficiency of phosphate removal was acquired by the activated samples than by the raw ones. The sample prepared by using the RM stirred with 0.25 M HCl for 2h (RM0.25), as well as another sample prepared by heating the RM at 700 degrees C for 2h (RM700), registered the maximum removal of phosphate (99% removal of phosphate). This occurred when they were used in the phosphate sorption studies conducted at pH 7.0 and 25 degrees C with the initial PO(4)(3-) concentration of 155 mg P/l. The FA samples treated in the same way described above can achieve 7.0 and 8.2 mg P/l phosphate removal for FA0.25 and FA700 respectively, corresponding to 45.2% and 52.9% removal. The activated materials performed higher phosphate removal over broader pH range compared with the raw ones. The influences of various factors, such as initial pH and initial phosphate concentration on the sorption capacity were also studied in batch equilibration technique. Solution pH significantly influenced the sorption. Each sample achieved the maximal removal of phosphate at pH 7.0. The amount of phosphate removal increased with the solute concentration. The Freundlich and Langmuir models were used to simulate the sorption equilibrium. The results indicate that the Langmuir model has a better correlation with the experimental data than the Freundlich model.
Sudhakaran, R; Mekata, T; Kono, T; Supamattaya, K; Linh, N T H; Suzuki, Y; Sakai, M; Itami, T
2009-07-01
White spot syndrome virus (WSSV) is an important shrimp pathogen responsible for large economic losses for the shrimp culture industry worldwide. The nucleic acids of the virus must be adequately preserved and transported from the field to the laboratory before molecular diagnostic analysis is performed. Here, we developed a new method to isolate WSSV-DNA using Flinders Technology Associates filter paper (FTA matrix card; Whatman) without centrifugation or hazardous steps involved. FTA technology is a new method allowing the simple collection, shipment and archiving of nucleic acids from haemolymph samples providing DNA protection against nucleases, oxidation, UV damage, microbial and fungal attack. DNA samples prepared from 10-fold dilutions of moribund shrimp haemolymph using FTA matrix cards were analysed using semi-quantitative and quantitative polymerase chain reaction (PCR) and were compared with two commercially available DNA isolation methods, the blood GenomicPrep Mini Spin Kit (GE Healthcare) and the DNAzol (Invitrogen). Sequence analysis was performed for the DNA samples prepared using the various isolation procedures and no differences in the sequence among these methods were identified. Results based on the initial copy number of DNA prepared from the GenomicPrep Mini Spin Kit are a little more sensitive than the DNA prepared from FTA matrix cards, whereas the DNAzol method is not suitable for blood samples. Our data shows the efficiency of retention capacity of WSSV-DNA samples from impregnated FTA matrix cards. Matrix cards were easy to store and ship for long periods of time. They provide ease of handling and are a reliable alternative for sample collection and for molecular detection and characterization of WSSV isolates.
Hossain, Mirza Akram; Friciu, Mihaela; Aubin, Sebastien; Leclair, Grégoire
2014-04-15
The stability of penicillin G sodium solutions stored in polyvinyl chloride (PVC) bags or elastomeric pump containers was studied. Test samples were prepared by diluting powdered penicillin G sodium (10 million units/10-mL vial) to solutions of 2,500 or 50,000 units/mL with 0.9% sodium chloride injection or 5% dextrose injection. The preparations were transferred to 250-mL PVC bags and elastomeric pump containers. All samples were prepared in triplicate and stored at 5°C. Chemical stability was measured by a stability-indicating high-performance liquid chromatographic (HPLC) assay and by pH evaluation. Particulate matter was evaluated according to compendial standards using a light-obscuration particle count test. Preparations were visually examined throughout the study. After 21 days of storage, all test samples remained chemically stable, with an HPLC assay recovery value of more than 90% of the initial value. After 28 days, all samples prepared with either diluent and stored in PVC bags, as well as the samples diluted to 2,500 units/mL with sodium chloride injection and stored in elastomeric pump containers, did not meet the recovery acceptance limit. For all test samples, the mean pH consistently decreased during storage, from about 6.4 to about 5.5. Particle counts remained acceptable throughout the study, and no change in appearance was observed. Penicillin G for injection (2,500 and 50,000 units/mL) diluted in 0.9% sodium chloride injection or 5% dextrose injection and stored at 5°C in PVC containers or elastomeric pump containers was physically and chemically stable for a period of at least 21 days.
Stability of extemporaneously prepared rufinamide oral suspensions.
Hutchinson, David J; Liou, Yayin; Best, Robert; Zhao, Fang
2010-03-01
Rufinamide is an oral antiepileptic drug indicated for adjunctive therapy in treating generalized seizures associated with Lennox-Gastaut syndrome. Currently, rufinamide is available as 200-mg and 400-mg tablets. A liquid dosage form does not exist at the present time. Lack of a suspension formulation may present an administration problem for many children and adults who are unable to swallow tablets. The availability of a liquid dosage form will provide an easy and accurate way to measure and administer the medication. To determine the stability of both sugar-containing and sugar-free rufinamide suspensions over a 90-day period. A suspension of rufinamide 40 mg/mL was prepared by grinding twelve 400-mg tablets of rufinamide tablets in a glass mortar. Sixty milliliters of Ora-Plus and 60 mL of either Ora-Sweet or Ora-Sweet SF (sugar free) were mixed and added to the powder to make a final volume of 120 mL. Three identical samples of each formulation were prepared and placed in 60-mL amber plastic bottles and were stored at room temperature. A 1-mL sample was withdrawn from each of the 6 bottles with a micropipette immediately after preparation and at 7, 14, 28, 56, and 90 days. After further dilution to an expected concentration of 0.4 mg/mL, the samples were assayed using high-performance liquid chromatography. Stability was defined as the retention of at least 90% of the initial concentration. At least 90% of the initial rufinamide concentration remained throughout the 90-day study period in both preparations. There were no detectable changes in color, odor, taste, and pH and no visible microbial growth. Extemporaneously compounded suspensions of rufinamide 40 mg/mL in a 1:1 mixture of Ora-Plus and Ora-Sweet or Ora-Sweet SF were stable for at least 90 days when stored in 59-mL amber polypropylene plastic bottles at room temperature.
Protocol for Initial Purification of Bacteriocin
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
A Molecular Framework for Understanding DCIS
2016-10-01
frozen patient biopsies, these have been annotated by our pathologist and prepared to be taken on for sequencing. The tissue includes DCIS, IDC...stroma adjacent to DCIS/IDC and normal tissue . We have initiated the RNA sequencing from these samples and also the DNA sequencing 15. SUBJECT TERMS DCIS...before they reach 55. Utilizing a unique bank of frozen mammary biopsies, containing samples with DCIS alone, and a combination of DCIS and IDC, we aim
Development of a sustained fluoride delivery system.
Baturina, Olga; Tufekci, Eser; Guney-Altay, Ozge; Khan, Shadeed M; Wnek, Gary E; Lindauer, Steven J
2010-11-01
To develop a novel delivery system by which fluoride incorporated into elastomeric rings, such as those used to ligate orthodontic wires, will be released in a controlled and constant manner. Polyethylene co-vinyl acetate (PEVA) was used as the model elastomer. Samples (N = 3) were prepared by incorporating 0.02 to 0.4 g of sodium fluoride (NaF) into previously prepared PEVA solution. Another group of samples prepared in the same manner were additionally dip-coated in PEVA to create an overcoat. Fluoride release studies were conducted in vitro using an ion selective electrode over a period of 45 days. The amount of fluoride released was compared to the optimal therapeutic dose of 0.7 microg F(-)/ring/d. Only coated samples with the highest fluoride content (group D, 0.4 g of NaF) were able to release fluoride at therapeutic levels. When fluoride release from coated and uncoated samples with the same amount of NaF were compared, it was shown that the dip-coating technique resulted in a fluoride release in a controlled manner while eliminating the initial burst effect. This novel fluoride delivery matrix provided fluoride release at a therapeutically effective rate and profile.
NASA Astrophysics Data System (ADS)
García-Vela, A.
2000-05-01
A definition of a quantum-type phase-space distribution is proposed in order to represent the initial state of the system in a classical dynamics simulation. The central idea is to define an initial quantum phase-space state of the system as the direct product of the coordinate and momentum representations of the quantum initial state. The phase-space distribution is then obtained as the square modulus of this phase-space state. The resulting phase-space distribution closely resembles the quantum nature of the system initial state. The initial conditions are sampled with the distribution, using a grid technique in phase space. With this type of sampling the distribution of initial conditions reproduces more faithfully the shape of the original phase-space distribution. The method is applied to generate initial conditions describing the three-dimensional state of the Ar-HCl cluster prepared by ultraviolet excitation. The photodissociation dynamics is simulated by classical trajectories, and the results are compared with those of a wave packet calculation. The classical and quantum descriptions are found in good agreement for those dynamical events less subject to quantum effects. The classical result fails to reproduce the quantum mechanical one for the more strongly quantum features of the dynamics. The properties and applicability of the phase-space distribution and the sampling technique proposed are discussed.
Evaluation of Sampling and Sample Preparation Modifications for Soil Containing Metallic Residues
2012-01-01
assessed the procedures devel- oped and adopted for energetics using USEPA Method 8330B and whether they are applicable to soils containing metals. The...initially encourage the use of MI at sites where soil is contam- inated with petroleum hydrocarbons only. However, MI sampling may be applicable to...602 793 962 974 733 723 1065 839 162 19 Mn 41 38 54 54 39 42 90 51 19 37 Pb 277 345 549 549 264 720 370 445 175 39 W 429 625 1374 1374 292 142 777
2014-06-01
layer of epoxy and ensure crack is filled in. Let sit for at least 1 hour, but no longer than 3 hours. (Do not allow base layer to harden before...10 mmHg and hold for 8 hours. • Once hardened remove excess epoxy and test sample. C. TENSILE TESTING For the purpose of this study, total fracture...hardened remove excess epoxy and test sample. 2. Final Changes Changes were made from this initial sample preparation to the final one shown in the
Chemical stability of extemporaneously prepared Lorazepam suspension at two temperatures.
Lee, Wan-Man Ellaria; Lugo, Ralph A; Rusho, William J; Mackay, Mark; Sweeley, John
2004-10-01
The objective of this study was to determine the chemical stability of extemporaneously prepared lorazepam suspension (1 mg/mL) stored at two temperatures (4°C and 22°C) for 3 months. Lorazepam tablets marketed by two manufacturers (Mylan Pharmaceuticals and Watson Laboratories) were used to extemporaneously formulate two independently prepared suspensions. Each suspension was prepared using sterile water, Ora-Plus(®) and Ora-Sweet(®) to achieve a final concentration of 1 mg/mL. The two brands of tablets required different volumes of vehicles to prepare a pharmaceutically optimal suspension. The suspensions were stored in amber glass bottles at 4°C and 22°C for 91 days. Samples were analyzed by high performance liquid chromatography at baseline and on days 2, 3, 7, 14, 21, 28, 42, 63, and 91. The suspensions were considered stable if the mean lorazepam concentration remained greater than 90% of the initial concentration.The chemical stabilities of these two extemporaneously prepared lorazepam suspensions were comparable throughout the study. Both lorazepam suspensions were stable for 63 days when stored at 4°C or 22°C, and both were stable for 91 days when refrigerated at 4°C. When stored at room temperature, the suspension prepared from the Watson tablet retained 88.9 ± 1.4% of the initial concentration on day 91 and was therefore considered unstable, while the suspension prepared from the Mylan tablet was stable for the entire 91-day study.
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.
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
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
Comparison of analytical methods for profiling N- and O-linked glycans from cultured cell lines
Togayachi, Akira; Azadi, Parastoo; Ishihara, Mayumi; Geyer, Rudolf; Galuska, Christina; Geyer, Hildegard; Kakehi, Kazuaki; Kinoshita, Mitsuhiro; Karlsson, Niclas G.; Jin, Chunsheng; Kato, Koichi; Yagi, Hirokazu; Kondo, Sachiko; Kawasaki, Nana; Hashii, Noritaka; Kolarich, Daniel; Stavenhagen, Kathrin; Packer, Nicolle H.; Thaysen-Andersen, Morten; Nakano, Miyako; Taniguchi, Naoyuki; Kurimoto, Ayako; Wada, Yoshinao; Tajiri, Michiko; Yang, Pengyuan; Cao, Weiqian; Li, Hong; Rudd, Pauline M.; Narimatsu, Hisashi
2016-01-01
The Human Disease Glycomics/Proteome Initiative (HGPI) is an activity in the Human Proteome Organization (HUPO) supported by leading researchers from international institutes and aims at development of disease-related glycomics/glycoproteomics analysis techniques. Since 2004, the initiative has conducted three pilot studies. The first two were N- and O-glycan analyses of purified transferrin and immunoglobulin-G and assessed the most appropriate analytical approach employed at the time. This paper describes the third study, which was conducted to compare different approaches for quantitation of N- and O-linked glycans attached to proteins in crude biological samples. The preliminary analysis on cell pellets resulted in wildly varied glycan profiles, which was probably the consequence of variations in the pre-processing sample preparation methodologies. However, the reproducibility of the data was not improved dramatically in the subsequent analysis on cell lysate fractions prepared in a specified method by one lab. The study demonstrated the difficulty of carrying out a complete analysis of the glycome in crude samples by any single technology and the importance of rigorous optimization of the course of analysis from preprocessing to data interpretation. It suggests that another collaborative study employing the latest technologies in this rapidly evolving field will help to realize the requirements of carrying out the large-scale analysis of glycoproteins in complex cell samples. PMID:26511985
A major diesel emissions research program has been initiated by the US Environmental Protection Agency to assess the human health risk associated with increased use of diesel automobiles. This program is intended to establish the mutagenic and carcinogenic potency of complex orga...
NASA Astrophysics Data System (ADS)
Liu, Hongxia; Deng, Shuping; Shen, Lanxian; Wang, Jinsong; Feng, Cheng; Deng, Shukang
2017-03-01
β-Zn4Sb3 is a promising p-type thermoelectric material for utilization in moderate temperatures. This study prepares a group of single-crystalline β-Zn4Sb3 samples using the Zn-Sn mixed-flux method based on the stoichiometric ratios of Zn4+ x Sb3Sn y . The effect of Zn-to-Sn proportion in the flux on the structure and electrical transport properties is investigated. All samples are strip-shaped single crystals of different sizes. The actual Zn content of the present samples is improved (>3.9) compared with that of the samples prepared through the Sn flux method. Larger lattice parameters are also obtained. The carrier concentration of all the samples is in the order of over 1019 cm-3. With increasing Sn rate in the flux, this carrier concentration decreases, whereas mobility is significantly enhanced. The electrical conductivity and Seebeck coefficients of all the samples exhibit a behavior that of a degenerate semiconductor transport. Electrical conductivity initially increases and then decreases as the Sn ratio in the flux increases. The electrical conductivity of the x: y = 5:1 sample reaches 6.45 × 104 S m-1 at 300 K. Benefitting from the electrical conductivity and Seebeck coefficient, the flux proportion of the x: y = 7:1 sample finally achieves the highest power factor value of 1.4 × 10-3 W m-1 K-2 at 598 K.
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.
Li induced effects in the core level and π-band electronic structure of graphene grown on C-face SiC
DOE Office of Scientific and Technical Information (OSTI.GOV)
Johansson, Leif I., E-mail: lij@ifm.liu.se; Xia, Chao; Virojanadara, Chariya
Studies of the effects induced in the electronic structure after Li deposition, and subsequent heating, on graphene samples prepared on C-face SiC are reported. The as prepared graphene samples are essentially undoped, but after Li deposition, the Dirac point shifts down to 1.2 eV below the Fermi level due to electron doping. The shape of the C 1s level also indicates a doping concentration of around 10{sup 14 }cm{sup −2} after Li deposition, when compared with recent calculated results of core level spectra of graphene. The C 1s, Si 2p, and Li 1s core level results show little intercalation directly after depositionmore » but that most of the Li has intercalated after heating at 280 °C. Heating at higher temperatures leads to desorption of Li from the sample, and at 1030 °C, Li can no longer be detected on the sample. The single π-band observable from multilayer C-face graphene samples in conventional angle resolved photoelectron spectroscopy is reasonably sharp both on the initially prepared sample and after Li deposition. After heating at 280 °C, the π-band appears more diffuse and possibly split. The Dirac point becomes located at 0.4 eV below the Fermi level, which indicates occurrence of a significant reduction in the electron doping concentration. Constant energy photoelectron distribution patterns extracted from the as prepared graphene C-face sample and also after Li deposition and heating at 280 °C look very similar to earlier calculated distribution patterns for monolayer graphene.« less
Thermal-history dependent magnetoelastic transition in (Mn,Fe){sub 2}(P,Si)
DOE Office of Scientific and Technical Information (OSTI.GOV)
Miao, X. F., E-mail: x.f.miao@tudelft.nl; Dijk, N. H. van; Brück, E.
The thermal-history dependence of the magnetoelastic transition in (Mn,Fe){sub 2}(P,Si) compounds has been investigated using high-resolution neutron diffraction. As-prepared samples display a large difference in paramagnetic-ferromagnetic (PM-FM) transition temperature compared to cycled samples. The initial metastable state transforms into a lower-energy stable state when the as-prepared sample crosses the PM-FM transition for the first time. This additional transformation is irreversible around the transition temperature and increases the energy barrier which needs to be overcome through the PM-FM transition. Consequently, the transition temperature on first cooling is found to be lower than on subsequent cycles characterizing the so-called “virgin effect.” High-temperaturemore » annealing can restore the cycled sample to the high-temperature metastable state, which leads to the recovery of the virgin effect. A model is proposed to interpret the formation and recovery of the virgin effect.« less
Ptachcinski, R J; Logue, L W; Burckart, G J; Venkataramanan, R
1986-01-01
The stability of cyclosporine in commonly used i.v. solutions and the percentage of the drug delivered via polyvinyl chloride administration tubing were studied. Cyclosporine injection was prepared according to the manufacturer's instructions and diluted with 5% dextrose injection (D5W) or with 0.9% sodium chloride injection (NS). Admixtures containing cyclosporine 2 mg/mL were prepared in polyvinyl chloride minibags (five for each solution) and in glass containers (three for each solution). The sample obtained at time zero from a glass container protected from light was the control. Additional samples were prepared in minibags and run through 70-inch polyvinyl chloride administration sets. An HPLC assay for cyclosporine was used. Exposure to room light did not significantly affect cyclosporine concentrations. More than 90% of the initial drug concentration remained after 24 hours under all storage conditions, but less than 95% remained after 6 hours in samples diluted with NS and stored in plastic. At times up to 60 minutes, cyclosporine concentrations were significantly different in solutions infused from the minibags through polyvinyl chloride tubing from those in control solutions. Under these conditions, cyclosporine is stable in D5W in glass containers or polyvinyl chloride minibags for 24 hours and in NS for 6 hours (polyvinyl chloride) to 12 hours (glass). However, because of the potential for leaching of plasticizers, cyclosporine admixtures should be stored in glass or used within six hours if stored in polyvinyl chloride minibags. Approximately 10% of the initial drug concentration is lost to 70-inch length polyvinyl chloride infusion tubing.
Cai, Zhu-Yun; Peng, Fan; Zi, Yun-Peng; Chen, Feng; Qian, Qi-Rong
2015-01-01
Synthetic calcium phosphate (CaP)-based materials have attracted much attention in the biomedical field. In this study, we have investigated the effect of pH values on CaP nanostructures prepared using a microwave-assisted hydrothermal method. The hierarchical nanosheet-assembled hydroxyapatite (HAP) nanostructure was prepared under weak acidic conditions (pH 5), while the HAP nanorod was prepared under neutral (pH 7) and weak alkali (pH 9) condition. However, when the pH value increases to 11, a mixed product of HAP nanorod and tri-calcium phosphate nanoparticle was obtained. The results indicated that the pH value of the initial reaction solution played an important role in the phase and structure of the CaP. Furthermore, the protein adsorption and release performance of the as-prepared CaP nanostructures were investigated by using hemoglobin (Hb) as a model protein. The sample that was prepared at pH = 11 and consisted of mixed morphologies of nanorods and nanoprisms showed a higher Hb protein adsorption capacity than the sample prepared at pH 5, which could be explained by its smaller size and dispersed structure. The results revealed the relatively high protein adsorption capacity of the as-prepared CaP nanostructures, which show promise for applications in various biomedical fields such as drug delivery and protein adsorption. PMID:28347064
Cai, Zhu-Yun; Peng, Fan; Zi, Yun-Peng; Chen, Feng; Qian, Qi-Rong
2015-07-31
Synthetic calcium phosphate (CaP)-based materials have attracted much attention in the biomedical field. In this study, we have investigated the effect of pH values on CaP nanostructures prepared using a microwave-assisted hydrothermal method. The hierarchical nanosheet-assembled hydroxyapatite (HAP) nanostructure was prepared under weak acidic conditions (pH 5), while the HAP nanorod was prepared under neutral (pH 7) and weak alkali (pH 9) condition. However, when the pH value increases to 11, a mixed product of HAP nanorod and tri-calcium phosphate nanoparticle was obtained. The results indicated that the pH value of the initial reaction solution played an important role in the phase and structure of the CaP. Furthermore, the protein adsorption and release performance of the as-prepared CaP nanostructures were investigated by using hemoglobin (Hb) as a model protein. The sample that was prepared at pH = 11 and consisted of mixed morphologies of nanorods and nanoprisms showed a higher Hb protein adsorption capacity than the sample prepared at pH 5, which could be explained by its smaller size and dispersed structure. The results revealed the relatively high protein adsorption capacity of the as-prepared CaP nanostructures, which show promise for applications in various biomedical fields such as drug delivery and protein adsorption.
Lee, Se Hee; Jung, Ji Young; Jeon, Che Ok
2014-01-01
To investigate the effects of salt concentration on saeu-jeot (salted shrimp) fermentation, four sets of saeu-jeot samples with 20%, 24%, 28%, and 32% salt concentrations were prepared, and the pH, bacterial and archaeal abundances, bacterial communities, and metabolites were monitored during the entire fermentation period. Quantitative PCR showed that Bacteria were much more abundant than Archaea in all saeu-jeot samples, suggesting that bacterial populations play more important roles than archaeal populations even in highly salted samples. Community analysis indicated that Vibrio, Photobacterium, Psychrobacter, Pseudoalteromonas, and Enterovibrio were identified as the initially dominant genera, and the bacterial successions were significantly different depending on the salt concentration. During the early fermentation period, Salinivibrio predominated in the 20% salted samples, whereas Staphylococcus, Halomonas, and Salimicrobium predominated in the 24% salted samples; eventually, Halanaerobium predominated in the 20% and 24% salted samples. The initially dominant genera gradually decreased as the fermentation progressed in the 28% and 32% salted samples, and eventually Salimicrobium became predominant in the 28% salted samples. However, the initially dominant genera still remained until the end of fermentation in the 32% salted samples. Metabolite analysis showed that the amino acid profile and the initial glycerol increase were similar in all saeu-jeot samples regardless of the salt concentration. After 30–80 days of fermentation, the levels of acetate, butyrate, and methylamines in the 20% and 24% salted samples increased with the growth of Halanaerobium, even though the amino acid concentrations steadily increased until approximately 80–107 days of fermentation. This study suggests that a range of 24–28% salt concentration in saeu-jeot fermentation is appropriate for the production of safe and tasty saeu-jeot. PMID:24587230
DOE Office of Scientific and Technical Information (OSTI.GOV)
Clark, Scarlett R.; Leonard, Keith J.
The goal of the Mechanisms of Irradiation Assisted Stress Corrosion Cracking (IASCC) task in the LWRS Program is to conduct experimental research into understanding how multiple variables influence the crack initiation and crack growth in materials subjected to stress under corrosive conditions. This includes understanding the influences of alloy composition, radiation condition, water chemistry and metallurgical starting condition (i.e., previous cold work or heat treatments and the resulting microstructure) has on the behavior of materials. Testing involves crack initiation and growth testing on irradiated specimens of single-variable alloys in simulated Light Water Reactor (LWR) environments, tensile testing, hardness testing, microstructuralmore » and microchemical analysis, and detailed efforts to characterize localized deformation. Combined, these single-variable experiments will provide mechanistic understanding that can be used to identify key operational variables to mitigate or control IASCC, optimize inspection and maintenance schedules to the most susceptible materials/locations, and, in the long-term, design IASCC-resistant materials. In support of this research, efforts are currently underway to arrange shipment of “free” high fluence austenitic alloys available through Électricité de France (EDF) for post irradiation testing at the Oak Ridge National Laboratory (ORNL) and IASCC testing at the University of Michigan. These high fluence materials range in damage values from 45 to 125 displacements per atom (dpa). The samples identified for transport to the United States, which include nine, no-cost, 304, 308 and 316 tensile bars, were relocated from the Research Institute of Atomic Reactors (RIAR) in Dimitrovgrad, Ulyanovsk Oblast, Russia, and received at the Halden Reactor in Halden, Norway, on August 23, 2016. ORNL has been notified that a significant amount of work is required to prepare the samples for further shipment to Oak Ridge, Tennessee. The preliminary work for sample shipment between Halden and Oak Ridge includes fabrication of an inner cask sample container, decontamination and preparation of a Type A container, preparation of new activity calculations, all necessary paperwork, and handling. ORNL will continue to work to track progress of sample preparation and shipment status, and to work toward an agreement that covers material shipping costs between the Halden Reactor and the Oak Ridge National Laboratory.« less
Electro-Chemical-Mechanical, Low Stress, Automatic Polishing (ECMP) Device (Preprint)
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
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.
Ion mobility analysis of lipoproteins
Benner, W Henry [Danville, CA; Krauss, Ronald M [Berkeley, CA; Blanche, Patricia J [Berkeley, CA
2007-08-21
A medical diagnostic method and instrumentation system for analyzing noncovalently bonded agglomerated biological particles is described. The method and system comprises: a method of preparation for the biological particles; an electrospray generator; an alpha particle radiation source; a differential mobility analyzer; a particle counter; and data acquisition and analysis means. The medical device is useful for the assessment of human diseases, such as cardiac disease risk and hyperlipidemia, by rapid quantitative analysis of lipoprotein fraction densities. Initially, purification procedures are described to reduce an initial blood sample to an analytical input to the instrument. The measured sizes from the analytical sample are correlated with densities, resulting in a spectrum of lipoprotein densities. The lipoprotein density distribution can then be used to characterize cardiac and other lipid-related health risks.
Kitagawa, Koichi; Shigemura, Katsumi; Onuma, Ken-Ichiro; Nishida, Masako; Fujiwara, Mayu; Kobayashi, Saori; Yamasaki, Mika; Nakamura, Tatsuya; Yamamichi, Fukashi; Shirakawa, Toshiro; Tokimatsu, Issei; Fujisawa, Masato
2018-03-01
Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) contributes to rapid identification of pathogens in the clinic but has not yet performed especially well for Gram-positive cocci (GPC) causing complicated urinary tract infection (UTI). The goal of this study was to investigate the possible clinical use of MALDI-TOF MS as a rapid method for bacterial identification directly from urine in complicated UTI. MALDI-TOF MS was applied to urine samples gathered from 142 suspected complicated UTI patients in 2015-2017. We modified the standard procedure (Method 1) for sample preparation by adding an initial 10 minutes of ultrasonication followed by centrifugation at 500 g for 1 minutes to remove debris such as epithelial cells and leukocytes from the urine (Method 2). In 133 urine culture-positive bacteria, the rate of corresponded with urine culture in GPC by MALDI-TOF MS in urine with standard sample preparation (Method 1) was 16.7%, but the modified sample preparation (Method 2) significantly improved that rate to 52.2% (P=.045). Method 2 also improved the identification accuracy for Gram-negative rods (GNR) from 77.1% to 94.2% (P=.022). The modified Method 2 significantly improved the average MALDI score from 1.408±0.153 to 2.166±0.045 (P=.000) for GPC and slightly improved the score from 2.107±0.061 to 2.164±0.037 for GNR. The modified sample preparation for MALDI-TOF MS can improve identification accuracy for complicated UTI causative bacteria. This simple modification offers a rapid and accurate routine diagnosis for UTI, and may possibly be a substitute for urine cultures. © 2017 Wiley Periodicals, Inc.
A brief overview on radon measurements in drinking water.
Jobbágy, Viktor; Altzitzoglou, Timotheos; Malo, Petya; Tanner, Vesa; Hult, Mikael
2017-07-01
The aim of this paper is to present information about currently used standard and routine methods for radon analysis in drinking waters. An overview is given about the current situation and the performance of different measurement methods based on literature data. The following parameters are compared and discussed: initial sample volume and sample preparation, detection systems, minimum detectable activity, counting efficiency, interferences, measurement uncertainty, sample capacity and overall turnaround time. Moreover, the parametric levels for radon in drinking water from the different legislations and directives/guidelines on radon are presented. Copyright © 2016 The Authors. Published by Elsevier Ltd.. All rights reserved.
Spectral Characterization of Analog Samples in Anticipation of OSIRIS-REx's Arrival at Bennu
NASA Technical Reports Server (NTRS)
Donaldson Hanna, K. L.; Schrader, D. L.; Bowles, N. E.; Clark, B. E.; Cloutis, E. A.; Connolly, H. C., Jr.; Hamilton, V. E.; Keller, L. P.; Lauretta, D. S.; Lim, L. F.;
2017-01-01
NASA's Origins, Spectral Interpretation, Resource Identification, and Security-Regolith Explorer (OSIRIS-REx) mission successfully launched on September 8th, 2016. During its rendezvous with near-Earth asteroid (101955) Bennu beginning in 2018, OSIRIS-REx will characterize the asteroid's physical, mineralogical, and chemical properties in an effort to globally map the properties of Bennu, a primitive carbonaceous asteroid, and choose a sampling location]. In preparation for these observations, analog samples were spectrally characterized across visible, near- and thermal-infrared wavelengths and were used in initial tests on mineral-phase-detection and abundance-determination software algorithms.
"Paper Machine" for Molecular Diagnostics.
Connelly, John T; Rolland, Jason P; Whitesides, George M
2015-08-04
Clinical tests based on primer-initiated amplification of specific nucleic acid sequences achieve high levels of sensitivity and specificity. Despite these desirable characteristics, these tests have not reached their full potential because their complexity and expense limit their usefulness to centralized laboratories. This paper describes a device that integrates sample preparation and loop-mediated isothermal amplification (LAMP) with end point detection using a hand-held UV source and camera phone. The prototype device integrates paper microfluidics (to enable fluid handling) and a multilayer structure, or a "paper machine", that allows a central patterned paper strip to slide in and out of fluidic path and thus allows introduction of sample, wash buffers, amplification master mix, and detection reagents with minimal pipetting, in a hand-held, disposable device intended for point-of-care use in resource-limited environments. This device creates a dynamic seal that prevents evaporation during incubation at 65 °C for 1 h. This interval is sufficient to allow a LAMP reaction for the Escherichia coli malB gene to proceed with an analytical sensitivity of 1 double-stranded DNA target copy. Starting with human plasma spiked with whole, live E. coli cells, this paper demonstrates full integration of sample preparation with LAMP amplification and end point detection with a limit of detection of 5 cells. Further, it shows that the method used to prepare sample enables concentration of DNA from sample volumes commonly available from fingerstick blood draw.
Liu, Junguo; Song, Jiuxue; Huang, Karen; Michel, Deborah; Fang, Jim
2018-05-01
A high-performance liquid chromatography tandem-mass spectrometry (HPLC-MS/MS) method has been developed to analyze anthocyanins in urine and plasma to further understand their absorption, distribution, metabolism and excretion. The method employed a Synergi RP-Max column (250 × 4.6 mm, 4 μm) and an API 4000 mass spectrometer. A gradient elution system consisted of mobile phase A (water-1% formic acid) and mobile phase B (acetonitrile) with a flow rate of 0.60 mL/min. The gradient was initiated at 5% B, increased to 21% B at 20 min, and then increased to 40% B at 35 min. The analysis of anthocyanins presents a challenge because of the poor stability of anthocyanins during sample preparation, especially during solvent evaporation. In this method, the degradation of anthocyanins was minimized using protein precipitation and dilute-and-shoot and sample preparation methods for plasma and urine, respectively. No interferences were observed from endogenous compounds. The method has been used to analyze anthocyanin concentrations in urine and plasma samples from volunteers administered saskatoon berries. Cyanidin-3-galactoside, cyanidin-3-glucoside, cyanidin-3-arabinoside, cyanidin-3-xyloside and quercetin-3-galactoside, the five major flavonoid components in saskatoon berries, were identified in plasma and urine samples. Copyright © 2017 John Wiley & Sons, Ltd.
Yang, Qin; Wang, Yuzhi; Zhang, Hongmei; Xu, Kaijia; Wei, Xiaoxiao; Xu, Panli; Zhou, Yigang
2017-11-01
A novel magnetic extractant, PEG 4000 modified Fe 3 O 4 nanomaterial that coated with dianionic amino acid ionic liquid (Fe 3 O 4 @PEG@DAAAIL), was successfully synthesized and characterized. X-ray diffraction (XRD), transmission electron microscope (TEM), vibrating sample magnetometer (VSM), fourier transform infrared spectrometry (FT-IR), thermal gravimetric analysis (TGA) and zeta potentials were used to confirm that the novel nanocomposite was successfully synthesized. Subsequently, the prepared Fe 3 O 4 @PEG@DAAAIL nanocomposite was used as the extractant for trypsin coupled with magnetic solid-phase extraction (MSPE). The concentrations of trypsin in the supernatant were detected by UV-vis spectrophotometer at 278nm. The extraction ability turned out to be better than the other four kinds of extractants prepared in this work. Furthermore, the influence of a series of factors, such as extraction time and temperature, initial trypsin concentration, the value of pH and ionic strength, was systematically investigated. Under the optimal extraction condition, the extraction capacity for trypsin could reach up to 718.73mg/g, absolutely higher than that of other adsorbents reported. This satisfactory extraction capacity could be maintained unchangeable after at least eight days, and kept over 90% of initial extraction capacity after eight recycles. What's more, the activity of trypsin after extraction retained 92.29% of initial activity, verifying the biocompatibility of the prepared extractant. Finally, the developed Fe 3 O 4 @PEG@DAAAIL-MSPE method was successfully applied to the real sample analysis with satisfactory results. All of above proves the potential value of Fe 3 O 4 @PEG@DAAAIL-MSPE in the analysis of biomass. Copyright © 2017 Elsevier B.V. All rights reserved.
NASA Astrophysics Data System (ADS)
Velayi, Elmira; Norouzbeigi, Reza
2017-12-01
Robust superhydrophobic ZnO surfaces with micro/nano hybrid hierarchical structures were synthesized on the stainless steel mesh by a facile single-step chemical bath deposition (CBD) method without using further low surface energy materials. The Taguchi L16 experimental design was applied to evaluate the effects of reaction time, type and concentration of the additive, type of the chelating agent, and the molar ratio of the chelating agent to the initial zinc (II) ions. The prepared sample at the optimal conditions exhibited a sustainable and time-independent superhydrophobic behavior with the water contact angle (WCA) of 162.8° ± 2.5° and contact angle hysteresis (CAH) of 1.8° ± 0.5°. The XRD, SEM, TEM and FTIR analyses were used to characterize the prepared samples. Surface characterization using scanning electron microscopy (SEM) indicated accumulation of micro/nano branched ZnO needles on the substrate with the average diameters of ∼85 nm. After 20 abrasion cycles the optimum sample indicated an excellent mechanical robustness via exposure to the pressure of 4.7 kPa. A suitable chemical resistance to the acidic and basic droplets with the pH range of 4 and 9 was observed.
Properties of Foamed Mortar Prepared with Granulated Blast-Furnace Slag.
Zhao, Xiao; Lim, Siong-Kang; Tan, Cher-Siang; Li, Bo; Ling, Tung-Chai; Huang, Runqiu; Wang, Qingyuan
2015-01-30
Foamed mortar with a density of 1300 kg/m³ was prepared. In the initial laboratory trials, water-to-cement (w/c) ratios ranging from 0.54 to 0.64 were tested to determine the optimal value for foamed mortar corresponding to the highest compressive strength without compromising its fresh state properties. With the obtained optimal w/c ratio of 0.56, two types of foamed mortar were prepared, namely cement-foamed mortar (CFM) and slag-foamed mortar (SFM, 50% cement was replaced by slag weight). Four different curing conditions were adopted for both types of foamed mortar to assess their compressive strength, ultrasonic pulse velocity (UPV) and thermal insulation performance. The test results indicated that utilizing 50% of slag as cement replacement in the production of foamed mortar improved the compressive strength, UPV and thermal insulation properties. Additionally, the initial water curing of seven days gained higher compressive strength and increased UPV values as compared to the air cured and natural weather curing samples. However, this positive effect was more pronounced in the case of compressive strength than in the UPV and thermal conductivity of foamed mortar.
630 A MARITIME NUCLEAR STEAM GENERATOR. Progress Report No. 2
DOE Office of Scientific and Technical Information (OSTI.GOV)
None
1962-09-28
A layout of a reduced-height 630A assembly (34 to 23 ft) was prepared and is presently being evaluated for use in a merchant vessel. While shielding studies indicate the need for some rearrangement of the shield materials, the desired radiation constraint can be obtained without an increase in shielding weight. A preliminary stress analysis of the pressure vessel, flow path analysis, and insulation evaluation was completed and showed no major problems. Evaluation of the total containment design indicates a design pressure of 45 psig. The Critical Experiment (CE) mockup is about 80% complete. The CE tank and dolly is aboutmore » 50% complete. The CE hazards report was reviewed and approved. The draft of the test program and procedures document is 75% complete. The LPT control room modifications were made, and the draft of the standard operating procedures completed. The CE fuel was inspected and a significant portion was found to be of no use, about 60% requires recoating. Creep and oxidation test time on some of the fuel sheet has exceeded 3000 hr with no significant oxidation or elongation on any of the samples. The nickel -chromium alloy sheet high- temperature (1750 F) stress and oxidating testing have exceeded 5000 hr with elongations below 0.8% except for one sample of 2.3%. Experimental fuel sheet samples were prepared and comparative property studies were ini-tiated. Fabrication of the ring test assembly, 3-F-1, for test in the MTR is essentially complete. The design of the test ring for seal evaluations was initiated. A detailed schedule for the work in FY 63 was prepared and issued for comments and concurrence. (auth)« less
Çapar, İsmail Davut; Uysal, Banu; Ok, Evren; Arslan, Hakan
2015-02-01
The purpose of this study was to investigate the incidence of apical crack initiation and propagation in root dentin after several endodontic procedures. Sixty intact mandibular premolars were sectioned perpendicular to the long axis at 1 mm from the apex, and the apical surface was polished. Thirty teeth were left unprepared and served as a control, and the remaining 30 teeth were instrumented with ProTaper Universal instruments (Dentsply Maillefer, Ballaigues, Switzerland) up to size F5. The root canals were filled with the single-cone technique. Gutta-percha was removed with drills of the Rebilda post system (VOCO, Cuxhaven, Germany). Glass fiber-reinforced composite fiber posts were cemented using a dual-cure resin cement. The fiber posts were removed with a drill of the post system. Retreatment was completed after the removal of the gutta-percha. Crack initiation and propagation in the apical surfaces of the samples were examined with a stereomicroscope after each procedure. The absence/presence of cracks was recorded. Logistic regression was performed to analyze statistically the incidence of crack initiation and propagation with each procedure. The initiation of the first crack and crack propagation was associated with F2 and F4 instruments, respectively. The logistic regression analysis revealed that instrumentation and F2 instrument significantly affected apical crack initiation (P < .001). Post space preparation had a significant effect on crack propagation (P = .0004). The other procedures had no significant effects on crack initiation and propagation (P > .05). Rotary nickel-titanium instrumentation had a significant effect on apical crack initiation, and post space preparation with drills had a significant impact on crack propagation. Copyright © 2015 American Association of Endodontists. Published by Elsevier Inc. All rights reserved.
Filova, Elena; Fojt, Jaroslav; Kryslova, Marketa; Moravec, Hynek; Joska, Ludek; Bacakova, Lucie
2015-01-01
Ti-6Al-4V-based nanotubes were prepared on a Ti-6Al-4V surface by anodic oxidation on 10 V, 20 V, and 30 V samples. The 10 V, 20 V, and 30 V samples and a control smooth Ti-6Al-4V sample were evaluated in terms of their chemical composition, diameter distribution, and cellular response. The surfaces of the 10 V, 20 V, and 30 V samples consisted of nanotubes of a relatively wide range of diameters that increased with the voltage. Saos-2 cells had a similar initial adhesion on all nanotube samples to the control Ti-6Al-4V sample, but it was lower than on glass. On day 3, the highest concentrations of both vinculin and talin measured by enzyme-linked immunosorbent assay and intensity of immunofluorescence staining were on 30 V nanotubes. On the other hand, the highest concentrations of ALP, type I collagen, and osteopontin were found on 10 V and 20 V samples. The final cellular densities on 10 V, 20 V, and 30 V samples were higher than on glass. Therefore, the controlled anodization of Ti-6Al-4V seems to be a useful tool for preparing nanostructured materials with desirable biological properties. PMID:26648719
NASA Astrophysics Data System (ADS)
Kebede, Mesfin A.; Ozoemena, Kenneth I.
2017-02-01
A molten salt synthesis technique has been used to prepare nanorods of Mn2O3 and single-crystal LiMn2O4 nanorods cathode material with superior capacity retention. The molten salt-directed synthesis involved the use of NaCl as the eutectic melt. The as-synthesized LiMn2O4 nanorods cathode material showed superior electrochemical performance compared to the LiMn2O4 sample obtained via the solid state method. The as-synthesized LiMn2O4 nanorods maintained more than 95% of the initial discharge capacity of 107 mA h g-1 over 100 cycles at a rate of 0.1 C, whereas the LiMn2O4 sample synthesized using the solid state reaction method maintained 88% of the initial discharge capacity of 98 mA h g-1 over 100 cycles at a rate of 0.1 C. Compared to the literature, the molten salt-directed method for the preparation of high-performance LiMn2O4 is simpler and less expensive, with greater potential for industrial scale-up.
High performance supercapacitor from activated carbon derived from waste orange skin
NASA Astrophysics Data System (ADS)
Ahmed, Sultan; Hussain, S.; Ahmed, Ahsan; Rafat, M.
2018-05-01
Activated carbon due to its inherent properties such as large surface area and low cost is most frequently used electrode material for supercapacitor. Activated carbon has been previously derived from various biomass such as coconut shell, coffee bean etc. Herein, we report the synthesis of activated carbon from waste orange skin. The material was synthesized employing chemical activation method and the success of synthesis was confirmed by its physical and electrochemical properties. The physical properties of the as-prepared sample were studied using the techniques of XRD, SEM, Raman spectroscopy and N2 adsorption/desorption analysis while its electrochemical properties were studied in two-electrode assembly using liquid electrolyte (consisting of 1 M solution of LiTFSI dispersed in ionic liquid EMITFSI) and employing the techniques of cyclic voltammetry, electrochemical impedance spectroscopy and galvanostatic charge- discharge. The synthesized sample of activated carbon exhibits high specific capacitance of 115 F g-1 at 10 mV s-1. Also, the activated carbon electrode shows the retention of ˜75% in initial capacitance value for more than 2000 initial cycles, indicating the as-prepared activated carbon can be profitably used as electrode material for energy storage devices.
Preparing Pediatric Healthcare Professionals for End-of-Life Care Discussions: An Exploratory Study.
Henderson, Amanda; Young, Jeanine; Herbert, Anthony; Bradford, Natalie; Pedersen, Lee-Anne
2017-06-01
Preparedness to initiate end-of-life (EoL) discussions is a confronting and daunting task for all healthcare professionals. We conducted a group interview to explore healthcare professionals' experiences of preparing for EoL discussions with the patient and their family in a pediatric context. To identify what pediatric healthcare professionals consider important when preparing for an EoL discussion. A qualitative design using a group interview. Two open-ended questions were asked: (1) How could preparedness to initiate EoL care discussions between healthcare professionals and the patient and family be enhanced? (2) What education resources/strategies could be developed to support preparation for EoL care discussions? Healthcare professionals, including medical, nursing, and allied health professionals working in pediatric palliative care settings across Queensland, Australia. These settings included major tertiary hospitals, general practice, community, and nongovernment organizations. A convenience sample of 36 healthcare professionals consented to participate in the study. An analysis of the data identified seven themes that had relevance for preparing for an EoL discussion: communication, healthcare professional perspectives, interdisciplinary team role, patient and family perspectives, practical issues, addressing mistakes, and healthcare professional education. Pediatric healthcare professionals confirmed that gaps exist in preparing for an EoL discussion. The findings support a need for further research in two areas. First, a systematic review of interdisciplinary resources that are available to support healthcare professionals in preparing for EoL discussions is recommended. Second, evidence-based interdisciplinary interventions to support pediatric EoL discussions need to be developed and evaluated.
Stability of rifabutin in two extemporaneously compounded oral liquids.
Haslam, J L; Egodage, K L; Chen, Y; Rajewski, R A; Stella, V
1999-02-15
The stability of rifabutin 20 mg/mL in two oral liquids was studied. Powder from 100 150-mg rifabutin capsules was placed in a glass mortar. Cherry syrup (pH 2.9) or a 1:1 mixture of Ora-Sweet and Ora-Plus (Paddock Laboratories) was added to produce 750 mL of each formulation, which was then stored in 2-oz plastic prescription bottles. Three bottles of each formulation were stored at 4, 25, 30, and 40 degrees C. At 0, 1, 2, 4, 8, and 12 weeks, the bottles were collected and allowed to remain at room temperature for one hour; samples of about 1 mL were collected from each bottle, weighed, and assayed for rifabutin content by high-performance liquid chromatography. The rifabutin liquids prepared with cherry syrup and stored at 4, 25, and 30 degrees C lost a mean of < 8% of the initial drug concentration during the 12-week study; at 40 degrees C, the liquids lost > 10% of the initial drug concentration by 12 weeks. There was a mean loss of < 5% of the initial rifabutin concentration in all the liquids prepared with Ora-Sweet and Ora-Plus. The liquid prepared with cherry syrup, upon standing, showed a tendency for some of the ingredients to float. The suspension prepared with Ora-Sweet and Ora-Plus had a tendency to retain bubbles after it was shaken, but the ingredients did not settle upon standing. Rifabutin 20 mg/mL in two extemporaneously compounded oral liquids prepared from capsules and sweetened vehicles was stable for at least 12 weeks at 4, 25, 30, and 40 degrees C with the exception of rifabutin in cherry syrup, which was stable for only 8 weeks at 40 degrees C.
Determining the risk of cardiovascular disease using ion mobility of lipoproteins
Benner, W. Henry; Krauss, Ronald M.; Blanche, Patricia J.
2010-05-11
A medical diagnostic method and instrumentation system for analyzing noncovalently bonded agglomerated biological particles is described. The method and system comprises: a method of preparation for the biological particles; an electrospray generator; an alpha particle radiation source; a differential mobility analyzer; a particle counter; and data acquisition and analysis means. The medical device is useful for the assessment of human diseases, such as cardiac disease risk and hyperlipidemia, by rapid quantitative analysis of lipoprotein fraction densities. Initially, purification procedures are described to reduce an initial blood sample to an analytical input to the instrument. The measured sizes from the analytical sample are correlated with densities, resulting in a spectrum of lipoprotein densities. The lipoprotein density distribution can then be used to characterize cardiac and other lipid-related health risks.
ERIC Educational Resources Information Center
Kleinhammer-Tramill, Jeannie
2003-01-01
This article describes federal initiatives to support preparation of regular educators to serve students with disabilities through the eras of mainstreaming, the Regular Education Initiative, inclusion, and promoting access to the general education curriculum. Trends in the number of personnel preparation projects that support preparation of…
Magnetically separable polymer (Mag-MIP) for selective analysis of biotin in food samples.
Uzuriaga-Sánchez, Rosario Josefina; Khan, Sabir; Wong, Ademar; Picasso, Gino; Pividori, Maria Isabel; Sotomayor, Maria Del Pilar Taboada
2016-01-01
This work presents an efficient method for the preparation of magnetic nanoparticles modified with molecularly imprinted polymers (Mag-MIP) through core-shell method for the determination of biotin in milk food samples. The functional monomer acrylic acid was selected from molecular modeling, EGDMA was used as cross-linking monomer and AIBN as radical initiator. The Mag-MIP and Mag-NIP were characterized by FTIR, magnetic hysteresis, XRD, SEM and N2-sorption measurements. The capacity of Mag-MIP for biotin adsorption, its kinetics and selectivity were studied in detail. The adsorption data was well described by Freundlich isotherm model with adsorption equilibrium constant (KF) of 1.46 mL g(-1). The selectivity experiments revealed that prepared Mag-MIP had higher selectivity toward biotin compared to other molecules with different chemical structure. The material was successfully applied for the determination of biotin in diverse milk samples using HPLC for quantification of the analyte, obtaining the mean value of 87.4% recovery. Copyright © 2015 Elsevier Ltd. All rights reserved.
Patterning of ultrathin polymethylmethacrylate films by in-situ photodirecting of the Marangoni flow
NASA Astrophysics Data System (ADS)
Elashnikov, Roman; Fitl, Premysl; Svorcik, Vaclav; Lyutakov, Oleksiy
2017-02-01
Laser heating and Marangoni flow result in the formation of surface structures with different geometries and shape on thin polymer films. By laser beam irradiation combined with a sample movement the solid polymethylmethacrylate (PMMA) films are heated and undergo phase transition which leads to a material flow. Since the laser beam has a non-linear distribution of energy, the PMMA film is heated inhomogeneously and a surface tension gradient in a lateral direction is introduced. During this procedure additional phenomena such as "reversible" or cyclic polymer flow also take place. The careful choice of experimental conditions enables the preparation of patterns with sophisticated geometries and with hierarchical pattern organization. Depending on initial PMMA film thickness and speed of the sample movement line arrays are created, which can subsequently be transformed into the crimped lines or system of circular holes. In addition, the introduction of a constant acceleration in the sample movement or a laser beam distortion enables the preparation of regularly crimped lines, ordered hexagonal holes or overlapped plates.
Duan, Qiannan; Lee, Jianchao; Chen, Han; Zheng, Yunyun
2017-12-01
A novel magnetically separable magnetic activated carbon supporting-copper (MCAC) catalyst for catalytic wet peroxide oxidation (CWPO) was prepared by chemical impregnation. The prepared samples were characterized by X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) method, and scanning electron microscopy (SEM) equipped with energy dispersive spectrometry (EDS). The catalytic performance of the catalysts was evaluated by direct violet (D-BL) degradation in CWPO experiments. The influence of preparative and operational parameters (dipping conditions, calcination temperature, catalyst loading H 2 O 2 dosage, pH, reaction temperature, additive salt ions and initial D-BL concentration) on degradation performance of CWPO process was investigated. The resulting MCAC catalyst showed higher reusability in direct violet oxidation than the magnetic activated carbon (MAC). Besides, dynamic tests also showed the maximal degradation rate reached 90.16% and its general decoloring ability of MCAC was 34 mg g -1 for aqueous D-BL.
Stability of extemporaneously prepared preservative-free prochlorperazine nasal spray.
Yellepeddi, Venkata K
2018-01-01
The stability of an extemporaneously prepared preservative-free prochlorperazine 5-mg/mL nasal spray was evaluated. The preservative-free prochlorperazine nasal spray was prepared by adding 250 mg of prochlorperazine edisylate to 50 mL of citrate buffer in a low-density polyethylene nasal spray bottle. A stability-indicating high-performance liquid chromatography (HPLC) method was developed and validated using the major degradant prochlorperazine sulfoxide and by performing forced-degradation studies. For chemical stability studies, 3 100-μL samples of the preservative-free prochlorperazine from 5 nasal spray bottles stored at room temperature were collected at days 0, 20, 30, 45, and 60 and were assayed in triplicate using the stability-indicating HPLC method. Microbiological testing involved antimicrobial effectiveness testing based on United States Pharmacopeia ( USP ) chapter 51 and quantitative microbiological enumeration of aerobic bacteria, yeasts, and mold based on USP chapter 61. Samples for microbiological testing were collected at days 0, 30, and 60. The stability-indicating HPLC method clearly identified the degradation product prochlorperazine sulfoxide without interference from prochlorperazine. All tested solutions retained over 90% of the initial prochlorperazine concentration for the 60-day study period. There were no detectable changes in color, pH, and viscosity in any sample. There was no growth of bacteria, yeast, and mold for 60 days in all samples tested. An extemporaneously prepared preservative-free nasal spray solution of prochlorperazine edisylate 5 mg/mL was physically, chemically, and microbiologically stable for 60 days when stored at room temperature in low-density polyethylene bottles. Copyright © 2018 by the American Society of Health-System Pharmacists, Inc. All rights reserved.
Garrigues, P; Narbonne, J F; Lafaurie, M; Ribera, D; Lemaire, P; Raoux, C; Michel, X; Salaun, J P; Monod, J L; Romeo, M
1993-11-01
The GICBEM (Groupe Interface Chimie Biologie des Ecosystèmes Marins) program consists of an evaluation of the ecosystem health status in the Mediterranean Sea mainly based on chemical and biochemical approaches. Specific chemical contaminants (polycyclic aromatic hydrocarbons (PAH), polychlorobiphenyls (PCB), heavy metals) in waters, sediments, and related biotransformation indicators in target organisms (mussels, fish) have been selected for a complete survey of the coastal waters. In order to provide an appropriate sampling program for standardization for each sampling cruise, various aspects have been studied: (a) parameters for the choice of the sample sites; (b) ways of collection the samples (waters, sediments, marine organisms); and (c) preparation of the samples for a short term storage on board ship and for further analyses in the ground laboratory. Methods of preparation and storage of the samples are described and could be used to initiate an environmental banking program including both possible retrospective analyses of chemical pollutants and biochemical indicators. Moreover, the correlation between chemicals (PAH) and biochemical (mixed function oxygenase activities) parameters has been studied and this demonstrates the capability of the enzyme activities as reliable pollution biomarkers.
Sheng, Le; Jin, Yulong; He, Yonghuan; Huang, Yanyan; Yan, Liushui; Zhao, Rui
2017-11-01
Superparamagnetic core-shell molecularly imprinted polymer nanoparticles (MIPs) were prepared via surface initiated reversible-addition fragmentation chain transfer (si-RAFT) polymerization for the selective recognition of 2,4-dichlorophenoxyacetic acid (2,4-D) in real samples. The construction of uniform core-shell structure with a 50nm MIP layer was successfully accomplished, which favored mass transfer and resulted in fast recognition kinetics. The static equilibrium experiments revealed the satisfied adsorption capacity and imprinting efficiency of Fe 3 O 4 @MIP. Moreover, the Fe 3 O 4 @MIP exhibited high selectivity and affinity towards 2,4-D over structural analogues. The prepared Fe 3 O 4 @MIP nanoparticles were used for the selective enrichment of 2,4-D in tap water and Chinese cabbage samples. Combined with RP-HPLC, the recoveries of 2,4-D were calculated from 93.1% to 103.3% with RSD of 1.7-5.4% (n = 3) in Chinese cabbage samples. This work provides a versatile approach for fabricating well-constructed core-shell MIP nanoparticles for rapid enrichment and highly selective separation of target molecules in real samples. Copyright © 2017 Elsevier B.V. All rights reserved.
Dynamic evolution of interface roughness during friction and wear processes.
Kubiak, K J; Bigerelle, M; Mathia, T G; Dubois, A; Dubar, L
2014-01-01
Dynamic evolution of surface roughness and influence of initial roughness (S(a) = 0.282-6.73 µm) during friction and wear processes has been analyzed experimentally. The mirror polished and rough surfaces (28 samples in total) have been prepared by surface polishing on Ti-6Al-4V and AISI 1045 samples. Friction and wear have been tested in classical sphere/plane configuration using linear reciprocating tribometer with very small displacement from 130 to 200 µm. After an initial period of rapid degradation, dynamic evolution of surface roughness converges to certain level specific to a given tribosystem. However, roughness at such dynamic interface is still increasing and analysis of initial roughness influence revealed that to certain extent, a rheology effect of interface can be observed and dynamic evolution of roughness will depend on initial condition and history of interface roughness evolution. Multiscale analysis shows that morphology created in wear process is composed from nano, micro, and macro scale roughness. Therefore, mechanical parts working under very severe contact conditions, like rotor/blade contact, screws, clutch, etc. with poor initial surface finishing are susceptible to have much shorter lifetime than a quality finished parts. © Wiley Periodicals, Inc.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Prathibha, G.; Rosaiah, P.; Reddy, B. Purusottam
Lithium ion (Li-ion) batteries are currently the energy source of choice for cell phones, laptops, and other mobile electronic devices due to their balance of high energy density with high power density compared to other electrochemical energy carriers. In the present study, mixed hydroxide method is used to prepare Li[Ni{sub 0.5}Co{sub 0.25}Mn{sub 0.25}]O{sub 2} from the precursors and analyze qualitatively and studied the electrochemical properties. The XRD spectrum exhibited predominant (003) orientation at 2θ =18.39{sup o} corresponding to hexagonal layered structure of R3m symmetry with evaluated lattice parameters are a= 2.84 Å, c= 14.43 Å. Raman measurements were performed tomore » understand the microstructure and vibrational modes of the prepared sample. From the electrochemical (EC) studies an initial discharge capacity of about 140 mAhg{sup −1} with good cyclic stability was observed for the prepared sample in the potential range 0.0 −1.0V in aqueous medium.« less
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.
ERIC Educational Resources Information Center
Amankwah, Francis; Oti-Agyen, Philip; Sam, Francis Kwame
2017-01-01
The descriptive survey design was used to find out the perception of pre-service teachers on teaching practice (on-campus) as an initial teacher preparation programme in University of Education, Winneba. A simple random sampling was used to select 226 pre-service teachers from the College of Technology Education, Kumasi. Data for the study were…
Pacifici, Roberta; Marchei, Emilia; Salvatore, Francesco; Guandalini, Luca; Busardò, Francesco Paolo; Pichini, Simona
2017-08-28
Cannabis has been used since ancient times to relieve neuropathic pain, to lower intraocular pressure, to increase appetite and finally to decrease nausea and vomiting. The combination of the psychoactive cannabis alkaloid Δ9-tetrahydrocannabinol (THC) with the non-psychotropic alkaloids cannabidiol (CBD) and cannabinol (CBN) demonstrated a higher activity than THC alone. The Italian National Institute of Health sought to establish conditions and indications on how to correctly use nationally produced cannabis to guarantee therapeutic continuity in individuals treated with medical cannabis. The evaluation of cannabinoids concentration and stability in standardized preparations of cannabis tea and cannabis oil was conducted using an easy and fast ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) assay. Extraction efficiency of oil was significantly higher than that of water with respect to the different cannabinoids. This was especially observed in the case of the pharmacologically active THC, CBD and their acidic precursors. Fifteen minutes boiling was sufficient to achieve the highest concentrations of cannabinoids in the cannabis tea solutions. At ambient temperature, a significant THC and CBD decrease to 50% or less of the initial concentration was observed over 3 and 7 days, respectively. When refrigerated at 4 °C, similar decreasing profiles were observed for the two compounds. The cannabinoids profile in cannabis oil obtained after pre-heating the flowering tops at 145 °C for 30 min in a static oven resulted in a complete decarboxylation of cannabinoid acids CBDA and THCA-A. Nevertheless, it was apparent that heat not only decarboxylated acidic compounds, but also significantly increased the final concentrations of cannabinoids in oil. The stability of cannabinoids in oil samples was higher than that in tea samples since the maximum decrease (72% of initial concentration) was observed in THC coming from unheated flowering tops at ambient temperature. In the case of the other cannabinoids, at ambient and refrigerated temperatures, 80%-85% of the initial concentrations were measured up to 14 days after oil preparation. As the first and most important aim of the different cannabis preparations is to guarantee therapeutic continuity in treated individuals, a strictly standardized preparation protocol is necessary to assure the availability of a homogeneous product of defined stability.
Lambrechts, Nicolaas E; Hurter, Karin; Picard, Jackie A; Goldin, Jeremy P; Thompson, Peter N
2004-01-01
To compare the efficacy of 0.3% stabilized glutaraldehyde and alcohol (SG+A), 0.3% SG and water (SG+W), and 4% chlorhexidine gluconate tincture (CG+A), as skin disinfectants in dogs undergoing ovariohysterectomy. Prospective, blinded clinical study. One hundred and twenty-one dogs. Cutaneous bacterial colony forming units (CFU) from the perioperative site after skin preparation, after antisepsis, and after surgery (incisional and paramedian), were quantified. The influence of high initial bacterial counts (> or =150 CFU) and surgical time on antibacterial efficacy was examined and the proportion of dogs from which Staphylococcus intermedius was cultured, determined. Perioperative skin reactions and wound infections were documented. All 3 antiseptic solutions significantly and equally reduced CFU to all post-antisepsis sampling levels irrespective of surgical duration (mean surgical times 151.6, 136.2, and 149.6 minutes for CG+A, SG+A and SG+W, respectively). Median percentage reductions in CFU ranged between 99.3% and 100%. In dogs with initial high counts and disinfected with CG+A and SG+W, the incisional samples had significantly higher counts than the post-antisepsis samples. In the CG+A and SG+W groups, the proportion of post-surgery samples yielding S. intermedius was significantly higher at the incisional than the paramedian sites. Eight mild cutaneous reactions were recorded in equal proportions for the 3 solutions. There were no recorded infections. All 3 preparations had an equal ability to reduce and maintain low CFU counts, with minimal cutaneous reactions. SG solutions are safe and effective preoperative skin antiseptics for elective clean-contaminated surgical procedures.
NASA Astrophysics Data System (ADS)
Rady, K. E.; Shams, M. S.
2017-03-01
Ferrite samples with general chemical formula Mn0.9Zn0.1Ni0.05Ti0.05GdtFe1.9-tO4; (0.0≤ t≤0.05; step 0.01) were prepared using solid state reaction technique and the effect of Gd3+ ions incorporation on its physical properties has been studied. From the obtained results, XRD analysis reveals that the samples have a cubic spinel single phase structure for 0.0≤ t≤0.02; while for t≥0.03 a small peak of secondary phase (Gd3Fe5O12) appears and becomes more noticeable with increasing Gd content. The lattice parameter (a) of the prepared samples was found to be initially increases and then decreases with increasing Gd content which may be attributed to the difference in the ionic radii of the cations involved and the solubility limit of Gd3+ ions. The crystallite size of the samples was estimated using Scherrer's equation and ranged from 96 nm to 107 nm. A vibrating sample magnetometer (VSM) was used at room temperature in order to study the effect of Gd content on the magnetic hysteresis parameters of the prepared ferrites such as saturation magnetization and coercivity. DC molar magnetic susceptibility (χM) for the prepared samples was measured using Faraday's method as a function of temperature and the Curie temperature was calculated from the magnetic susceptibility measurements. Also the DC resistivity of the samples was measured at room temperature. The obtained results show that, the substitution by Gd3+ ions improves the electrical properties of the samples by increasing it DC electrical resistivity by 118% and consequently decreases it eddy current loss while the saturation magnetization slightly decreased by 14% only. The sample of t=0.01 shows a high dc magnetic susceptibility, high saturation magnetization (43.1 emu/g), high electric resistivity 12×103 Ω.m and high Curie temperature (496 K), which is useful in some technological applications such as transformer and inductor cores.
Weiss, Agnes; Jérôme, Valérie; Freitag, Ruth
2007-06-15
The goal of the project was the extraction of PCR-compatible genomic DNA representative of the entire microbial community from municipal biogas plant samples (mash, bioreactor content, process water, liquid fertilizer). For the initial isolation of representative DNA from the respective lysates, methods were used that employed adsorption, extraction, or precipitation to specifically enrich the DNA. Since no dedicated method for biogas plant samples was available, preference was given to kits/methods suited to samples that resembled either the bioreactor feed, e.g. foodstuffs, or those intended for environmental samples including wastewater. None of the methods succeeded in preparing DNA that was directly PCR-compatible. Instead the DNA was found to still contain considerable amounts of difficult-to-remove enzyme inhibitors (presumably humic acids) that hindered the PCR reaction. Based on the isolation method that gave the highest yield/purity for all sample types, subsequent purification was attempted by agarose gel electrophoresis followed by electroelution, spermine precipitation, or dialysis through nitrocellulose membrane. A combination of phenol/chloroform extraction followed by purification via dialysis constituted the most efficient sample treatment. When such DNA preparations were diluted 1:100 they did no longer inhibit PCR reactions, while they still contained sufficient genomic DNA to allow specific amplification of specific target sequences.
Method of assessing a lipid-related health risk based on ion mobility analysis of lipoproteins
Benner, W. Henry; Krauss, Ronald M.; Blanche, Patricia J.
2010-12-14
A medical diagnostic method and instrumentation system for analyzing noncovalently bonded agglomerated biological particles is described. The method and system comprises: a method of preparation for the biological particles; an electrospray generator; an alpha particle radiation source; a differential mobility analyzer; a particle counter; and data acquisition and analysis means. The medical device is useful for the assessment of human diseases, such as cardiac disease risk and hyperlipidemia, by rapid quantitative analysis of lipoprotein fraction densities. Initially, purification procedures are described to reduce an initial blood sample to an analytical input to the instrument. The measured sizes from the analytical sample are correlated with densities, resulting in a spectrum of lipoprotein densities. The lipoprotein density distribution can then be used to characterize cardiac and other lipid-related health risks.
Farhangdoust, S; Zamanian, A; Yasaei, M; Khorami, M
2013-01-01
The design and fabrication of macroporous hydroxyapatite scaffolds, which could overcome current bone tissue engineering limitations, have been considered in recent years. In the current study, controlled unidirectional freeze-casting at different cooling rates was investigated. In the first step, different slurries with initial hydroxyapatite concentrations of 7-37.5 vol.% were prepared. In the next step, different cooling rates from 2 to 14 °C/min were applied to synthesize the porous scaffold. Additionally, a sintering temperature of 1350 °C was chosen as an optimum temperature. Finally, the phase composition (by XRD), microstructure (by SEM), mechanical characteristics, and the porosity of sintered samples were assessed. The porosity of the sintered samples was in a range of 45-87% and the compressive strengths varied from 0.4 MPa to 60 MPa. The mechanical strength of the scaffolds increased as a function of initial concentration, cooling rate, and sintering temperature. With regards to mechanical strength and pore size, the samples with the initial concentration and the cooling rate of 15 vol.% and 5 °C/min, respectively, showed better results. Copyright © 2012 Elsevier B.V. All rights reserved.
Adsorption of (99m)Tc-radiopharmaceuticals onto injection vials and syringes.
Mushtaq, Ahmad; Ur Rehman, Taj; Safdar Mansur, Muhammad; Jehangir, Mustanser
2008-06-01
Many groups have reported the adsorption or retention of (99m)Tc-radiopharmaceuticals on injection vials and disposable plastic syringes. Such an enormously high loss of radioactivity would result in poor images, radiation exposure, waste, and economic burdens. We therefore decided to investigate the extent of adsorption or retention of several (99m)Tc-radiopharmaceuticals on injection vials, rubber stoppers, and plastic syringes. These radiopharmaceuticals are produced as lyophilized kits in our department and supplied to various hospitals practicing nuclear medicine in Pakistan. A vial containing lyophilized material was reconstituted with 3 mL of freshly eluted Na(99m)TcO(4). A 1-mL aliquot of the resulting solution was withdrawn into a syringe at 0.25, 0.5, 1, 3, and 5 h after preparation. All preparations were stored at room temperature ( approximately 22 degrees C). After each withdrawal, the vial was reweighed and the activity remaining in the vial was measured using a radioisotope calibrator. The sample was reinjected into the vial. From the original weight and activity of solution in the vial, the initial activity per gram was calculated. From the weight and activity remaining in the vial after withdrawal of the sample, the activity per gram of the sample was calculated. From the difference between the initial activity per gram and the activity per gram of the sample, the percentage of (99m)Tc adsorbed on the vial was calculated. All preparations were kept in the syringe for 15 min, and the activity was measured before and after the syringe was emptied. The needle and plunger of the syringe were separated, and activity in the needle and plunger was also measured. The labeling efficiency of all radiopharmaceuticals used during these studies was more than 95%. In most cases, the activity of (99m)Tc found on the rubber stopper was less than 1%. Adsorption of (99m)Tc onto vials increased gradually with storage time. Adsorption was minimal at the initial stages, whereas maximum retention was noted after 5 h. Nearly 5% adsorption of activity was observed after 5 h of storage time on vials of sestamibi, mercaptoacetyltriglycine, dextran, ciprofloxacin, and dimercaptosuccinic acid (III and V). Retention of activity on needles ranged from 1% to 2% for all preparations studied. Plungers did not show any significant retention of radioactivity; in most cases, retention was less than 0.5%. The maximum retention of radioactivity on plastic syringe bodies was more than 3% for sestamibi, dimercaptosuccinic acid, dextran, pyrophosphate, and phytate. The results revealed that losses of radioactivity from (99m)Tc-radiopharmaceuticals in these objects (glass vial, rubber stopper, plastic syringes, plungers, and needles) are not alarming in our setup.
Properties of Foamed Mortar Prepared with Granulated Blast-Furnace Slag
Zhao, Xiao; Lim, Siong-Kang; Tan, Cher-Siang; Li, Bo; Ling, Tung-Chai; Huang, Runqiu; Wang, Qingyuan
2015-01-01
Foamed mortar with a density of 1300 kg/m3 was prepared. In the initial laboratory trials, water-to-cement (w/c) ratios ranging from 0.54 to 0.64 were tested to determine the optimal value for foamed mortar corresponding to the highest compressive strength without compromising its fresh state properties. With the obtained optimal w/c ratio of 0.56, two types of foamed mortar were prepared, namely cement-foamed mortar (CFM) and slag-foamed mortar (SFM, 50% cement was replaced by slag weight). Four different curing conditions were adopted for both types of foamed mortar to assess their compressive strength, ultrasonic pulse velocity (UPV) and thermal insulation performance. The test results indicated that utilizing 50% of slag as cement replacement in the production of foamed mortar improved the compressive strength, UPV and thermal insulation properties. Additionally, the initial water curing of seven days gained higher compressive strength and increased UPV values as compared to the air cured and natural weather curing samples. However, this positive effect was more pronounced in the case of compressive strength than in the UPV and thermal conductivity of foamed mortar. PMID:28787950
NASA Technical Reports Server (NTRS)
Snead, C. J.; McCubbin, F. M.; Nakamura-Messenger, K.; Righter, K.
2018-01-01
The Astromaterials Acquisition and Curation office at NASA Johnson Space Center has established an Advanced Curation program that is tasked with developing procedures, technologies, and data sets necessary for the curation of future astromaterials collections as envisioned by NASA exploration goals. One particular objective of the Advanced Curation program is the development of new methods for the collection, storage, handling and characterization of small (less than 100 micrometer) particles. Astromaterials Curation currently maintains four small particle collections: Cosmic Dust that has been collected in Earth's stratosphere by ER2 and WB-57 aircraft, Comet 81P/Wild 2 dust returned by NASA's Stardust spacecraft, interstellar dust that was returned by Stardust, and asteroid Itokawa particles that were returned by the JAXA's Hayabusa spacecraft. NASA Curation is currently preparing for the anticipated return of two new astromaterials collections - asteroid Ryugu regolith to be collected by Hayabusa2 spacecraft in 2021 (samples will be provided by JAXA as part of an international agreement), and asteroid Bennu regolith to be collected by the OSIRIS-REx spacecraft and returned in 2023. A substantial portion of these returned samples are expected to consist of small particle components, and mission requirements necessitate the development of new processing tools and methods in order to maximize the scientific yield from these valuable acquisitions. Here we describe initial progress towards the development of applicable sample handling methods for the successful curation of future small particle collections.
Comprehensive Marine Particle Analysis System
2001-09-30
October. A second HRS cruise will conduct sampling at the HyCODE/ECOHAB: Florida site from November 1-7 and complete the investigation of seasonal ...HyCODE/ECOHAB: Florida modeling site. Following our November cruise this year, a manuscript will be prepared investigating the seasonal dynamics of...zooplankton distribution and grazing on the West Florida Shelf as a follow-up to our initial paper (Sutton et al., 2001). Multiple- season optical and
Comprehensive Marine Particle Analysis System
2002-09-30
October. A second HRS cruise will conduct sampling at the HyCODE/ECOHAB: Florida site from November 1-7 and complete the investigation of seasonal ...HyCODE/ECOHAB: Florida modeling site. Following our November cruise this year, a manuscript will be prepared investigating the seasonal dynamics of...zooplankton distribution and grazing on the West Florida Shelf as a follow-up to our initial paper (Sutton et al., 2001). Multiple- season optical and
Novel Diffusion-Weighted MRI for High-Grade Prostate Cancer Detection
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
DOE Office of Scientific and Technical Information (OSTI.GOV)
Kronewitter, Scott R.; Marginean, Ioan; Cox, Jonathan T.
The N-glycan diversity of human serum glycoproteins, i.e. the human blood serum N-glycome, is complex due to the range of glycan structures potentially synthesizable by human glycosylation enzymes. The reported glycome, however, is limited by methods of sample preparation, available analytical platforms, e.g., based upon electrospray ionization-mass spectrometry (ESI-MS), and software tools for data analysis. In this report, several improvements have been implemented in sample preparation and analysis to extend ESI-MS glycan characterization and to provide an improved view of glycan diversity. Sample preparation improvements include acidified, microwave-accelerated, PNGase F N-glycan release, and sodium borohydride reduction were optimized to improvemore » quantitative yields and conserve the number of glycoforms detected. Two-stage desalting (during solid phase extraction and on the analytical column) increased the sensitivity by reducing analyte signal division between multiple reducing-end-forms or cation adducts. On-line separations were improved by using extended length graphitized carbon columns and adding TFA as an acid modifier to a formic acid/reversed phase gradient which provides additional resolving power and significantly improved desorption of both large and heavily sialylated glycans. To improve MS sensitivity and provide gentler ionization conditions at the source-MS interface, subambient pressure ionization with nanoelectrospray (SPIN) has been utilized. When method improvements are combined together with the Glycomics Quintavariate Informed Quantification (GlyQ-IQ) recently described1 these technologies demonstrate the ability to significantly extend glycan detection sensitivity and provide expanded glycan coverage. We demonstrate application of these advances in the context of the human serum glycome, and for which our initial observations include detection of a new class of heavily sialylated N-glycans, including polysialylated N-glycans.« less
Lehmann, Roland; Schmidt, André; Pastuschek, Jana; Müller, Mario M; Fritzsche, Andreas; Dieterle, Stefan; Greb, Robert R; Markert, Udo R; Slevogt, Hortense
2018-06-25
The proteomic analysis of complex body fluids by liquid chromatography tandem mass spectrometry (LC-MS/MS) analysis requires the selection of suitable sample preparation techniques and optimal parameter settings in data analysis software packages to obtain reliable results. Proteomic analysis of follicular fluid, as a representative of a complex body fluid similar to serum or plasma, is difficult as it contains a vast amount of high abundant proteins and a variety of proteins with different concentrations. However, the accessibility of this complex body fluid for LC-MS/MS analysis is an opportunity to gain insights into the status, the composition of fertility-relevant proteins including immunological factors or for the discovery of new diagnostic and prognostic markers for, for example, the treatment of infertility. In this study, we compared different sample preparation methods (FASP, eFASP and in-solution digestion) and three different data analysis software packages (Proteome Discoverer with SEQUEST, Mascot and MaxQuant with Andromeda) combined with semi- and full-tryptic databank search options to obtain a maximum coverage of the follicular fluid proteome. We found that the most comprehensive proteome coverage is achieved by the eFASP sample preparation method using SDS in the initial denaturing step and the SEQUEST-based semi-tryptic data analysis. In conclusion, we have developed a fractionation-free methodical workflow for in depth LC-MS/MS-based analysis for the standardized investigation of human follicle fluid as an important representative of a complex body fluid. Taken together, we were able to identify a total of 1392 proteins in follicular fluid. © 2018 John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.
Former foster youth's perspectives on independent living preparation six months after discharge.
Jones, Loring P
2014-01-01
Research findings have developed a troubling narrative of youth leaving foster care. Congress attempted to address the post-discharge difficulties of foster youth by passing the Independent Living Initiative in 1986, which mandated that the states develop services that would prepare youth for life after foster care. However, it is unclear what effect these programs have on post-foster care trajectories. This largely qualitative study examined the perceptions of a sample of discharged foster six months after leaving care. Most youth felt prepared for life and foster care. They were also for the most part were satisfied with their independent living program, but had significant dissatisfactions with elements of the program. These satisfactions and dissatisfactions are reported along with suggestions for improvement. The policy and practice implications of these suggestions are considered.
Ground truth crop proportion summaries for US segments, 1976-1979
NASA Technical Reports Server (NTRS)
Horvath, R. (Principal Investigator); Rice, D.; Wessling, T.
1981-01-01
The original ground truth data was collected, digitized, and registered to LANDSAT data for use in the LACIE and AgRISTARS projects. The numerous ground truth categories were consolidated into fewer classes of crops or crop conditions and counted occurrences of these classes for each segment. Tables are presented in which the individual entries are the percentage of total segment area assigned to a given class. The ground truth summaries were prepared from a 20% sample of the scene. An analysis indicates that this size of sample provides sufficient accuracy for use of the data in initial segment screening.
Beyond-use dating of lidocaine alone and in two "magic mouthwash" preparations.
Kirk, Loren Madden; Brown, Stacy D; Luu, Yao; Ogle, Amanda; Huffman, Jessica; Lewis, Paul O
2017-05-01
Beyond-use dating (BUD) of lidocaine alone and in two "magic mouthwash" preparations stored in amber oral syringes at room temperature was determined. Two formulations of mouthwash containing oral topical lidocaine 2% (viscous), diphenhydramine 2.5 mg/mL, and aluminum hydroxide-magnesium hydroxide-simethicone were prepared in 1:1:1 and 1:2.5:2.5 ratios, divided into 3-mL samples, and stored in unit-dose oral amber syringes. Unit-dose single-product lidocaine samples were also prepared to serve as controls and stored in oral amber syringes. The lidocaine concentrations in these samples were measured periodically for 90 days. A stability-indicating high-performance liquid chromatographic method was developed and validated for system suitability, accuracy, repeatability, intermediate precision, specificity, linearity, and robustness. Based on the calculated percentages versus the initial concentration and the results from an analysis of variance comparing the two formulations, a BUD of 21 days is deemed appropriate for both magic mouthwash formulations. Based on the stability data, published safety concerns, and lack of efficacy in combination, packaging and dispensing lidocaine separately from other ingredients are recommended when administering magic mouthwash mixtures. Utilizing a 90-day BUD, lidocaine can be packaged separately from other magic mouthwash ingredients in individual dosage units and applied to the oral cavity using the swish-and-spit method. The delivery of the diphenhydramine and aluminum hydroxide-magnesium hydroxide-simethicone could be separated, allowing for a swish-and-swallow method of administration. A BUD of 21 days is recommended for lidocaine prepared with diphenhydramine and aluminum hydroxide-magnesium hydroxide-simethicone in ratios of 1:1:1 and 1:2.5:2.5 and stored at room temperature in amber oral plastic syringes. Copyright © 2017 by the American Society of Health-System Pharmacists, Inc. All rights reserved.
Leonardo, Mário R; Guillén-Carías, M G; Pécora, J D; Ito, I Y; Silva, L A B
2005-06-01
Our goal in this study was to evaluate the antimicrobial effect of Er:YAG laser applied after biomechanical preparation of the root canals of dog's teeth with apical periodontitis. Various in vitro studies have reported effective bacterial reduction in infected root canals using Er:YAG laser. However, there is no in vivo research to support these results. Forty root canals of dogs' premolar teeth with pulp necrosis and chronic periapical lesions were used. An initial microbiological sample was taken, and after biomechanical preparation was carried out, a second microbiological sample was taken. The teeth were divided into two groups: Group I-biomechanical preparation was taken of root canals without Er:YAG laser application; Group II-biomechanical preparation was taken of root canals with Er:YAG laser application using 140-mJ input, 63-mJ output/15 Hz. After coronal sealing, the root canals were left empty for 7 days at which time a third microbiological sample was taken. The collected material was removed from the root canal with a #40 K file and placed in transport media. It was serially diluted and seeded on culture dishes selective for anaerobes, aerobes, and total streptococci. Colony-forming units per milliliter (CFU/mL) were counted. Groups I and II showed an increase of CFU/mL for all microorganisms 7 days after treatment, being statistically significant for anaerobes in Group I and for anaerobes and total streptococci in Group II. When comparing CFU/mL of Groups I and II, there was a statistically significant increase after 7 d for total streptococci in Group II. Er:YAG laser applied after biomechanical preparation did not reduce microorganisms in the root canal system.
NASA Astrophysics Data System (ADS)
Kadirova, Zukhra C.; Katsumata, Ken-ichi; Isobe, Toshihiro; Matsushita, Nobuhiro; Nakajima, Akira; Okada, Kiyoshi
2013-11-01
The photocatalytic adsorbents BAU-OA, BAU-CL and BAU-HA with varying iron oxide content (9-10 mass%) were prepared by heat treatment at 250 °C from commercial activated carbon (BAU) impregnated with iron oxalate, chloride, tris-benzohydroxamate, respectively. The XRD patterns showed amorphous structure in the BAU-CL sample (SBET 50 m2/g) and low crystallinity (as FeOOH and Fe2O3 phases) in the BAU-HA and BAU-OA samples (SBET 4 and 111 m2/g, respectively). The methylene blue adsorption capacities was decreased in order of BAU-OA < BAU-CL < BAU-HA sample and the adsorption followed Langmuir model. The apparent MB photodegradation rate constant (kapp) was increased in same order BAU-HA < BAU-CL < BAU-OA under the standard experimental conditions (initial MB concentrations 0.015-0.025 mM; sample content - 10 mg/l; initial oxalic acid concentration - 0.43 mM; pH 3-4; UV illumination). The process included high efficiency combination of adsorption, heterogeneous and homogeneous catalysis under UV and solar lights illumination without addition of hydrogen peroxide. The detoxification of water sample containing organic dyes was confirmed after combined sorption-photocatalytic treatment.
NASA Astrophysics Data System (ADS)
Furtak-Wrona, K.; Kozik-Ostrówka, P.; Jadwiszczak, K.; Maigret, J. E.; Aguié-Béghin, V.; Coqueret, X.
2018-01-01
A water-based polyurethane (PUR) acrylate water emulsion was selected as a radiation curable matrix for preparing nanocomposites including cellulose nanocrystals (CNC) prepared by controlled hydrolysis of Ramie fibers. Cross-linking polymerization of samples prepared in the form of films or of 1 mm-thick bars was either initiated by exposure to the 395 nm light of a high intensity LED lamp or by treatment with low energy electron beam (EB). The conversion level of acrylate functions in samples submitted to increasing radiation doses was monitored by Fourier Transform Infrared Spectroscopy (FTIR). Differential Scanning Calorimetry (DSC) and Dynamic Mechanical Analysis (DMA) were used to characterize changes in the glass transition temperature of the PUR-CNC nanocomposites as a function of acrylate conversion and of CNC content. Micromechanical testing indicates the positive effect of 1 wt% CNC on Young's modulus and on the tensile strength at break (σ) of cured nanocomposites. The presence of CNC in the PUR acrylate matrix was shown to double the σ value of the nanocomposite cured to an acrylate conversion level of 85% by treatment with a 25 kGy dose under EB, whereas no increase of σ was observed in UV-cured samples exhibiting the same acrylate conversion level. The occurrence of grafting reactions inducing covalent linkages between the polysaccharide nanofiller and the PUR acrylate matrix during the EB treatment is advanced as an explanation to account for the improvement observed in samples cured under ionizing radiation.
NASA Astrophysics Data System (ADS)
Niaz Akhtar, Majid; Azhar Khan, Muhammad; Ahmad, Mukhtar; Murtaza, G.; Raza, Rizwan; Shaukat, S. F.; Asif, M. H.; Nasir, Nadeem; Abbas, Ghazanfar; Nazir, M. S.; Raza, M. R.
2014-11-01
The effects of synthesis methods such as sol-gel (SG), self combustion (SC) and modified conventional mixed oxide (MCMO) on the structure, morphology and magnetic properties of the (Y3Fe5O12) garnet ferrites have been studied in the present work. The samples of Y3Fe5O12 were sintered at 950 °C and 1150 °C (by SG and SC methods). For MCMO route the sintering was done at 1350 °C for 6 h. Synthesized samples prepared by various routes were investigated using X-ray diffraction (XRD) analysis, Field emission scanning electron microscopy (FESEM), Impedance network analyzer and transmission electron microscopy (TEM). The structural analysis reveals that the samples are of single phase structure and shows variations in the particle sizes and cells volumes, prepared by various routes. FESEM and TEM images depict that grain size increases with the increase of sintering temperature from 40 nm to 100 nm.Magnetic measurements reveal that garnet ferrite synthesized by sol gel method has high initial permeability (60.22) and low magnetic loss (0.0004) as compared to other garnet ferrite samples, which were synthesized by self combustion and MCMO methods. The M-H loops exhibit very low coercivity which enables the use of these materials in relays and switching devices fabrications. Thus, the garnet nanoferrites with low magnetic loss prepared by different methods may open new horizon for electronic industry for their use in high frequency applications.
Global metabolic profiling procedures for urine using UPLC-MS.
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.
Self-powered integrated microfluidic point-of-care low-cost enabling (SIMPLE) chip
Yeh, Erh-Chia; Fu, Chi-Cheng; Hu, Lucy; Thakur, Rohan; Feng, Jeffrey; Lee, Luke P.
2017-01-01
Portable, low-cost, and quantitative nucleic acid detection is desirable for point-of-care diagnostics; however, current polymerase chain reaction testing often requires time-consuming multiple steps and costly equipment. We report an integrated microfluidic diagnostic device capable of on-site quantitative nucleic acid detection directly from the blood without separate sample preparation steps. First, we prepatterned the amplification initiator [magnesium acetate (MgOAc)] on the chip to enable digital nucleic acid amplification. Second, a simplified sample preparation step is demonstrated, where the plasma is separated autonomously into 224 microwells (100 nl per well) without any hemolysis. Furthermore, self-powered microfluidic pumping without any external pumps, controllers, or power sources is accomplished by an integrated vacuum battery on the chip. This simple chip allows rapid quantitative digital nucleic acid detection directly from human blood samples (10 to 105 copies of methicillin-resistant Staphylococcus aureus DNA per microliter, ~30 min, via isothermal recombinase polymerase amplification). These autonomous, portable, lab-on-chip technologies provide promising foundations for future low-cost molecular diagnostic assays. PMID:28345028
Surface characteristics and bioactivity of oxide film on titanium metal formed by thermal oxidation.
Park, Yeong-Joon; Song, Ho-Jun; Kim, In; Yang, Hong-So
2007-04-01
In this study, we characterized the surface of oxide film formed on titanium metal through the use of thermal treatment and investigated the effect of surface characteristics on the bioactivity of titanium. The as-received sample group was prepared by polishing and cleaning CP-Ti as a control group, and thermally oxidized sample groups were prepared by heat treating at 530, 600, 700, 800, 900, and 1000 degrees C respectively. Micro-morphology, crystalline structure, chemical composition, and binding state were evaluated using FE-SEM, XRD, and XPS. The bioactivity of sample groups was investigated by observing the degree of calcium phosphate formation from immersion testing in MEM. The surface characterization tests showed that hydroxyl group content in titanium oxide film was increased, as the density of titanium atoms was high and the surface area was large. In MEM immersion test, initial calcium phosphate formation was dependent upon the thickness of titanium oxide, and resultant calcium phosphate formation depended on the content of the hydroxyl group of the titanium oxide film surface.
Ramírez Restrepo, Andrés; Gallo Ortiz, Andrés Fernando; Hoyos Ossa, Duvan Esteban; Peñuela Mesa, Gustavo Antonio
2014-09-01
The objective of this study was to validate (SANCO/12495/2011 and NTC-ISO/IEC 17025) multi-residue multi-class methods using QuEChERS sample preparation and GC-MS for the analysis of regulated pesticides in tomatoes (Solanum lycopersicum), tamarillos (Solanum betaceum) and goldenberries (Physalis peruviana). These Latin American products are representative and widely produced in Antioquia (Colombia). Sample preparation followed the UNE-EN 15662 method (150 mg MgSO4, 25mg primary secondary amines and 25mg of octadecylsiloxane for cleanup; graphitized carbon black was added for tomatoes). Extracts were injected using a programmed temperature-vaporizing injector. The residues were validated over a range from 0.02 mg/kg to 0.20 mg/kg, with 24 analytes validated in tomatoes, 33 in tamarillos and 28 in goldenberries. An initial risk assessment was enabled by monitoring 24 samples in the municipalities of El Peñol, Marinilla and San Vicente Ferrer. Risks were found for tomatoes, but no significant risks were found for tamarillos or goldenberries. Copyright © 2014 Elsevier Ltd. All rights reserved.
NASA Astrophysics Data System (ADS)
Malys, Brian J.; Piotrowski, Michelle L.; Owens, Kevin G.
2018-02-01
Frustrated by worse than expected error for both peak area and time-of-flight (TOF) in matrix assisted laser desorption ionization (MALDI) experiments using samples prepared by electrospray deposition, it was finally determined that there was a correlation between sample location on the target plate and the measured TOF/peak area. Variations in both TOF and peak area were found to be due to small differences in the initial position of ions formed in the source region of the TOF mass spectrometer. These differences arise largely from misalignment of the instrument sample stage, with a smaller contribution arising from the non-ideal shape of the target plates used. By physically measuring the target plates used and comparing TOF data collected from three different instruments, an estimate of the magnitude and direction of the sample stage misalignment was determined for each of the instruments. A correction method was developed to correct the TOFs and peak areas obtained for a given combination of target plate and instrument. Two correction factors are determined, one by initially collecting spectra from each sample position used and another by using spectra from a single position for each set of samples on a target plate. For TOF and mass values, use of the correction factor reduced the error by a factor of 4, with the relative standard deviation (RSD) of the corrected masses being reduced to 12-24 ppm. For the peak areas, the RSD was reduced from 28% to 16% for samples deposited twice onto two target plates over two days.
NASA Astrophysics Data System (ADS)
Malys, Brian J.; Piotrowski, Michelle L.; Owens, Kevin G.
2017-12-01
Frustrated by worse than expected error for both peak area and time-of-flight (TOF) in matrix assisted laser desorption ionization (MALDI) experiments using samples prepared by electrospray deposition, it was finally determined that there was a correlation between sample location on the target plate and the measured TOF/peak area. Variations in both TOF and peak area were found to be due to small differences in the initial position of ions formed in the source region of the TOF mass spectrometer. These differences arise largely from misalignment of the instrument sample stage, with a smaller contribution arising from the non-ideal shape of the target plates used. By physically measuring the target plates used and comparing TOF data collected from three different instruments, an estimate of the magnitude and direction of the sample stage misalignment was determined for each of the instruments. A correction method was developed to correct the TOFs and peak areas obtained for a given combination of target plate and instrument. Two correction factors are determined, one by initially collecting spectra from each sample position used and another by using spectra from a single position for each set of samples on a target plate. For TOF and mass values, use of the correction factor reduced the error by a factor of 4, with the relative standard deviation (RSD) of the corrected masses being reduced to 12-24 ppm. For the peak areas, the RSD was reduced from 28% to 16% for samples deposited twice onto two target plates over two days. [Figure not available: see fulltext.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Bai, Ying; Wang, Zhen; Wu, Chuan
2015-02-27
Two types of hard carbon materials were synthesized through direct pyrolysis of commercial polyvinyl chloride (PVC) particles and pyrolysis of PVC nanofibers at 600-800 degrees C, respectively, where the nanofibers were prepared by an electrospinning PVC precursors method. These as-prepared hard carbon samples were used as anode materials for Na-ion batteries. The hard carbon obtained from PVC nanofibers achieved a high reversible capacity of 271 mAh/g and an initial Coulombic efficiency of 69.9%, which were much superior to the one from commercial PVC, namely, a reversible capacity of 206 mAh/g and an initial Coulombic efficiency of 60.9%. In addition, themore » hard carbon originated from the PVC nanofibers exhibited good cycling stability and rate performance: the initial discharge capacities were 389, 228, 194, 178, 147 mAh/g at the current density of 12, 24, 60, 120, and 240 mA/g, respectively, retaining 211 mAh/g after 150 cycles. Such excellent cycle performance, high reversible capacity, and good rate capability enabled this hard carbon to be a promising candidate as anode material for Na-ion battery application.« less
Bai, Ying; Wang, Zhen; Wu, Chuan; Xu, Rui; Wu, Feng; Liu, Yuanchang; Li, Hui; Li, Yu; Lu, Jun; Amine, Khalil
2015-03-11
Two types of hard carbon materials were synthesized through direct pyrolysis of commercial polyvinyl chloride (PVC) particles and pyrolysis of PVC nanofibers at 600-800 °C, respectively, where the nanofibers were prepared by an electrospinning PVC precursors method. These as-prepared hard carbon samples were used as anode materials for Na-ion batteries. The hard carbon obtained from PVC nanofibers achieved a high reversible capacity of 271 mAh/g and an initial Coulombic efficiency of 69.9%, which were much superior to the one from commercial PVC, namely, a reversible capacity of 206 mAh/g and an initial Coulombic efficiency of 60.9%. In addition, the hard carbon originated from the PVC nanofibers exhibited good cycling stability and rate performance: the initial discharge capacities were 389, 228, 194, 178, 147 mAh/g at the current density of 12, 24, 60, 120, and 240 mA/g, respectively, retaining 211 mAh/g after 150 cycles. Such excellent cycle performance, high reversible capacity, and good rate capability enabled this hard carbon to be a promising candidate as anode material for Na-ion battery application.
Weng, Neng-Chiao; Wu, Chih-Fu; Tsen, Wen-Chin; Wu, Cheng-Lung; Suen, Maw-Cherng
2018-01-01
Abstract In this study, 4,4′-diphenylmethane diisocyanate and polytetramethylene glycol were used to prepare a prepolymer; N,N′-bis(4-hydroxybenzylidene)-2,6-diaminopyridine (BHBP) was used as a chain extender; and these elements were combined to prepare a novel polyurethane, BHBP/PU. Gel permeation chromatography revealed that the molecular weight of the BHBP/PU samples increased as the BHBP content was increased. Fourier transform infrared spectroscopy demonstrated that high BHBP content facilitated strong hydrogen bonding in the samples. Differential thermogravimetry indicated that the initial decomposition temperature of BHBP/PU-3 was approximately 10 °C higher than that of BHBP/PU-1. Differential scanning calorimetry and dynamic mechanical analysis revealed that increasing the BHBP content substantially increased both the glass transition and dynamic glass transition temperatures of the BHBP/PU samples. The tensile strengths of BHBP/PU-1, BHBP/PU-2, and BHBP/PU-3 were 7.7, 10.9, and 21.6 MPa, respectively, with corresponding Young’s moduli of 0.7, 1.9, and 3.3 MPa. These results demonstrated that both the tensile strength and Young’s modulus of the BHBP/PU samples increased as the BHBP content was increased. Moreover, the BHBP/PU samples exhibited excellent shape recovery of >90%. PMID:29706848
Stability of Drugs of Abuse in Urine Samples at Room Temperature by Use of a Salts Mixture.
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.
Flagg, Lee A; Sen, Bisakha; Kilgore, Meredith; Locher, Julie L
2014-09-01
To examine the extent to which the gendered division of labour persists within households in the USA in regard to meal planning/preparation and food shopping activities. Secondary analysis of cross-sectional data. 2007-2008 US National Health and Nutrition Examination Survey. Sub-sample of 3195 adults at least 20 years old who had a spouse or partner. Analyses revealed that the majority of women and men reported they shared in both meal planning/preparing and food shopping activities (meal planning/preparation: women 54 % and men 56 %; food shopping: women 60 % and men 57 %). Results from multinomial logistic regression analyses indicated that, compared with men, women were more likely to take primary responsibility than to share this responsibility and less likely to report having no responsibility for these tasks. Gender differences were observed for age/cohort, education and household size. This study may have implications for public health nutritional initiatives and the well-being of families in the USA.
Stability of an extemporaneous alcohol-free melatonin suspension.
Johnson, Cary E; Cober, Mary Petrea; Thome, Tennille; Rouse, Emily
2011-03-01
The stability of alcohol-free oral suspensions of melatonin 1 mg/mL, extemporaneously prepared from two commercially available melatonin tablet products, was studied. Four 1-mg/mL melatonin suspensions were prepared. Formulations A and B contained 20 crushed 3-mg tablets of melatonin combined with a 1:1 mixture of Ora-Plus and either Ora-Sweet or Ora-Sweet SF to produce a volume of 60 mL. Formulations C and D were prepared by crushing 20 combination tablets containing melatonin 3 mg and pyridoxine hydrochloride 10 mg and then combining the powder with a 1:1 mixture of Ora-Plus and either Ora-Sweet or Ora-Sweet SF to produce a 60-mL volume. The suspensions were prepared in triplicate and stored at room temperature in amber plastic prescription bottles. Immediately after preparation and on days 7, 15, 30, 60, and 90, the samples were assayed in duplicate by stability-indicating high-performance liquid chromatography (HPLC). The samples were also evaluated for any changes in color, odor, and taste. HPLC analysis demonstrated that at least 94% of the initial melatonin concentration in formulations A and B, and at least 98% of that in formulations C and D, remained throughout the 90-day study period. Detectable changes in color, odor, or taste occurred in all of the formulations. Extemporaneously prepared, alcohol-free, 1-mg/mL suspensions of melatonin and melatonin-pyridoxine hydrochloride in a 1:1 mixture of Ora-Plus and either Ora Sweet or Ora Sweet SF were stable for at least 90 days when stored in 2-oz amber plastic bottles at room temperature.
Initial versus final fracture of metal-free crowns, analyzed via acoustic emission.
Ereifej, Nadia; Silikas, Nick; Watts, David C
2008-09-01
To discriminate between initial and final fracture failure loads of four metal-free crown systems by the conjoint detection of acoustic emission signals during compressive loading. Teeth were prepared and used for crown construction with four crown systems; Vita Mark II (VM II) (Vita Zahnfabrik), IPS e.max Ceram/CAD (CAD) (Ivoclar-Vivadent), IPS e.max Ceram/ZirCAD (ZirCAD) (Ivoclar-Vivadent) and BelleGlass/EverStick (BGES) (Kerr/Stick Tech Ltd.). All samples were loaded in compression via a Co/Cr maxillary first molar tooth at 0.2mm/min and released acoustic signals were collected and analyzed. A minimum number of 15 crowns per group were loaded to final failure and values of loading at initial and final fracture were compared. Additional four samples per group were loaded till fracture initiation and were fractographically examined under the optical microscope. A lower threshold of 50dB was selected to exclude spurious background signals. Initial fracture forces were significantly lower than those of final fracture (p<0.05) in all groups and initial failure AE amplitudes were lower than those of final fracture. Mean initial fracture force of ZirCAD samples (1029.1N) was higher than those of VMII (744.4N), CAD (808.8 N) and BGES (979.7 N). Final fracture of ZirCAD also occurred at significantly higher force values (2091.7 N) than the rest of the groups; VMII (1120.9 N), CAD (1468.9 N) and BGES (1576.6 N). Significantly higher values of initial failure AE amplitude were found in VMII than CAD and BGES while those of final fracture were similar. All crowns observed under the microscope at initial fracture had signs of failure. Whereas the metal-free crowns examined showed significant variations in final failure loads, acoustic emission data showed that they all manifested initial failures at significantly lower load values.
Rush, Steven D; Vernak, Charlene; Zhao, Fang
2017-01-01
Dehydroepiandrosterone supplementation is used to treat a variety of conditions. Rapid-dissolving tablets are a relatively novel choice for compounded dehydroepiandrosterone dosage forms. While rapid-dissolving tablets offer ease of administration, there are uncertainties about the physical and chemical stability of the drug and dosage form during preparation and over long-term storage. This study was designed to evaluate the stability of dehydroepiandrosterone rapid-dissolving tablets just after preparation and over six months of storage. The Professional Compounding Centers of America rapid-dissolving tablet mold and base formula were used to prepare 10-mg strength dehydroepiandrosterone rapid-dissolving tablets. The formulation was heated at 100°C to 110°C for 30 minutes, released from the mold, and cooled at room temperature for 30 minutes. The resulting rapid-dissolving tablets were individually packaged in amber blister packs and stored in a stability chamber maintained at 25°C and 60% relative humidity. The stability samples were pulled at pre-determined time points for evaluation, which included visual inspection, tablet weight check, United States Pharmacopeia disintegration test, and stability-indicating high-performance liquid chromatography. The freshly prepared dehydroepiandrosterone rapiddissolving tablets exhibited satisfactory chemical and physical stability. Time 0 samples disintegrated within 40 seconds in water kept at 37°C. The high-performance liquid chromatographic results confirmed that the initial potency was 101.9% of label claim and that there was no chemical degradation from the heating procedure. Over six months of storage, there were no significant changes in visual appearance, physical integrity, or disintegration time for any of the stability samples. The high-performance liquid chromatographic results also indicated that dehydroepiandrosterone rapid-dissolving tablets retained >95% label claim with no detectable degradation products. The dehydroepiandrosterone rapid-dissolving tablets investigated in this pilot study were physically and chemically stable during preparation and over six months of storage at 25°C and 60% relative humidity. Copyright© by International Journal of Pharmaceutical Compounding, Inc.
Three Dimensional Immobilization of Beta-Galactosidase on a Silicon Surface (Preprint)
2006-12-01
initial activity after 10 days at 24°C. The ability to generate three- dimensional structures with enhanced loading capacity for biosensing molecules...dimensional structures for biosensors (Charles et al. 2004). Silicon samples that had been washed but not activated with APTS did not retain any enzyme...preparation. The use of silica particles to build a 3-dimensional structure not only provides an increased capacity for the immobilization of β
Experiments in fault tolerant software reliability
NASA Technical Reports Server (NTRS)
Mcallister, David F.; Tai, K. C.; Vouk, Mladen A.
1987-01-01
The reliability of voting was evaluated in a fault-tolerant software system for small output spaces. The effectiveness of the back-to-back testing process was investigated. Version 3.0 of the RSDIMU-ATS, a semi-automated test bed for certification testing of RSDIMU software, was prepared and distributed. Software reliability estimation methods based on non-random sampling are being studied. The investigation of existing fault-tolerance models was continued and formulation of new models was initiated.
Photochemical Degradation of Composition B and Its Components
2007-09-01
recorded on the toluene (5.7 mg yield ), ether I (35 mg), and aceto- nitrile (17.8 mg) fractions. Irradiation of solution explosives in soils A...the soil was Soxhlet extracted with acetonitrile for 93 hours. The acetonitrile was removed with a rotary evaporator and the residue redissolved in...ionization to yield an anion of m/z 226. The traces show differences observed in samples with different initial preparation protocols at 15 days. Distance
Vapor deposition routes to conformal polymer thin films
Moni, Priya; Al-Obeidi, Ahmed
2017-01-01
Vapor phase syntheses, including parylene chemical vapor deposition (CVD) and initiated CVD, enable the deposition of conformal polymer thin films to benefit a diverse array of applications. This short review for nanotechnologists, including those new to vapor deposition methods, covers the basic theory in designing a conformal polymer film vapor deposition, sample preparation and imaging techniques to assess film conformality, and several applications that have benefited from vapor deposited, conformal polymer thin films. PMID:28487816
Prevention of Ovarian High-Grade Serous Carcinoma by Elucidating its Early Changes
We will determine the early molecular changes in STIC and their biological significance in developing high-grade serous carcinoma. marker selection...and sample preparation will begin in the next coming months. Project 2 We will evaluate whether the presence of a STIC is associated with different...clinical manifestations and/or outcome compare to those patients in whom a STIC was not identified. Molecular profiling will be initiated after quality
NASA Astrophysics Data System (ADS)
Yano, H.; Fujiwara, A.
After the successful launch in May 2003, the Hayabusa (MUSES-C) mission of JAXA/ISAS will collect surface materials (e.g., regolith) of several hundred mg to several g in total from the S-type near Earth asteroid (25143) Itokawa in late 2005 and bring them back to ground laboratories in the summer of 2007. The retrieved samples will be given initial analysis at the JAXA/ISAS astromaterial curation facility, which is currently in the preparation for its construction, by the Hayabusa Asteroidal Sample Preliminary Examination Team (HASPET). HASPET is consisted of the ISAS Hayabusa team, the international partners from NASA and Australia and all-Japan meteoritic scientists to be selected as outsourcing parts of the initial analyses. The initial analysis to characterize general aspects of returned samples can consume only 15 % of its total mass and must complete the whole analyses including the database building before international AO for detailed analyses within the maximum of 1 year. Confident exercise of non-destructive, micro-analyses whenever possible are thus vital for the HASPET analysis. In the purpose to survey what kinds and levels of micro-analysis techniques in respective fields, from major elements and mineralogy to trace and isotopic elements and organics, are available in Japan at present, ISAS has conducted the HASPET open competitions in 2000-01 and 2004. The initial evaluation was made by multiple domestic peer reviews. Applicants were then provided two kinds of unknown asteroid sample analogs in order to conduct proposed analysis with self-claimed amount of samples in self-claimed duration. After the completion of multiple, international peer reviews, the Selection Committee compiled evaluations and recommended the finalists of each round. The final members of the HASPET will be appointed about 2 years prior to the Earth return. Then they will conduct a test-run of the whole initial analysis procedures at the ISAS astromaterial curation facility and their respective analysis facilities. This talk also summarizes the curation facility design and plans of initial analysis procedure flow.
Federal Register 2010, 2011, 2012, 2013, 2014
2013-08-12
... DEPARTMENT OF DEFENSE Department of Air Force Intent To Prepare an Environmental Impact Statement for the Gulf Regional Airspace Strategic Initiative (GRASI) Landscape Initiative AGENCY: Department of... Airspace Strategic Initiative (GRASI) Landscape Initiative (GLI) is a U.S Air Force-led partnership with...
NASA Astrophysics Data System (ADS)
Managadze, G. G.; Safronova, A. A.; Luchnikov, K. A.; Vorobyova, E. A.; Duxbury, N. S.; Wurz, P.; Managadze, N. G.; Chumikov, A. E.; Khamizov, R. Kh.
2017-05-01
We propose a new technique for the detection of microorganisms by elemental composition analyses of a sample extracted from regolith, permafrost, and ice of extraterrestrial bodies. We also describe the design of the ABIMAS instrument, which consists of the onboard time-of-flight laser mass-reflectron (TOF LMR) and the sample preparation unit (SPU) for biomass extraction. This instrument was initially approved to fly on board the ExoMars 2020 lander mission. The instrument can be used to analyze the elemental composition of possible extraterrestrial microbial communities and compare it to that of terrestrial microorganisms. We have conducted numerous laboratory studies to confirm the possibility of biomass identification via the following biomarkers: P/S and Ca/K ratios, and C and N abundances. We underline that only the combination of these factors will allow one to discriminate microbial samples from geological ones. Our technique has been tested experimentally in numerous laboratory trials on cultures of microorganisms and polar permafrost samples as terrestrial analogues for martian polar soils. We discuss various methods of extracting microorganisms and sample preparation. The developed technique can be used to search for and identify microorganisms in different martian samples and in the subsurface of other planets, satellites, comets, and asteroids—in particular, Europa, Ganymede, and Enceladus.
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.
Blackwood, Kym S; Burdz, Tamara V; Turenne, Christine Y; Sharma, Meenu K; Kabani, Amin M; Wolfe, Joyce N
2005-01-24
In the field of clinical mycobacteriology, Mycobacterium tuberculosis (MTB) can be a difficult organism to manipulate due to the restrictive environment of a containment level 3 (CL3) laboratory. Tests for rapid diagnostic work involving smears and molecular methods do not require CL3 practices after the organism has been rendered non-viable. While it has been assumed that after organism deactivation these techniques can be performed outside of a CL3, no conclusive study has consistently confirmed that the organisms are noninfectious after the theoretical 'deactivation' steps. Previous studies have shown that initial steps (such as heating/chemical fixation) may not consistently kill MTB organisms. An inclusive viability study (n = 226) was undertaken to determine at which point handling of culture extraction materials does not necessitate a CL3 environment. Four different laboratory protocols tested for viability included: standard DNA extractions for IS6110 fingerprinting, crude DNA preparations for PCR by boiling and mechanical lysis, protein extractions, and smear preparations. For each protocol, laboratory staff planted a proportion of the resulting material to Bactec 12B medium that was observed for growth for 8 weeks. Of the 208 isolates initially tested, 21 samples grew within the 8-week period. Sixteen (7.7%) of these yielded positive results for MTB that included samples of: deactivated culture resuspensions exposed to 80 degrees C for 20 minutes, smear preparations and protein extractions. Test procedures were consequently modified and tested again (n = 18), resulting in 0% viability. This study demonstrates that it cannot be assumed that conventional practices (i.e. smear preparation) or extraction techniques render the organism non-viable. All methodologies, new and existing, should be examined by individual laboratories to validate the safe removal of material derived from MTB to the outside of a CL3 laboratory. This process is vital to establish in house biosafety-validated practices with the aim of protecting laboratory workers conducting these procedures.
DOE Office of Scientific and Technical Information (OSTI.GOV)
L. Phillips; G. K. Davis; J. R. Delayen
2005-07-10
In order to measure the superconducting surface properties of niobium that are of interest to SRF applications, a facility which utilizes a Nb cavity operating in the TE011 mode at 7.65 GHz which provides a well-defined RF field on a disk shaped sample has been designed and fabricated. The RF losses due to the sample's surface impedance are determined by using a calorimetric technique. The system has the capability to measure such properties as Rs,(T), and penetration depth, which can then be correlated with surface properties and preparation processes. The design, fabrication, and results from initial commissioning operations will bemore » discussed, along with the near term sample evaluation program.« less
Examination Of Sulfur Measurements In DWPF Sludge Slurry And SRAT Product Materials
DOE Office of Scientific and Technical Information (OSTI.GOV)
Bannochie, C. J.; Wiedenman, B. J.
2012-11-29
Savannah River National Laboratory (SRNL) was asked to re-sample the received SB7b WAPS material for wt. % solids, perform an aqua regia digestion and analyze the digested material by inductively coupled plasma - atomic emission spectroscopy (ICP-AES), as well as re-examine the supernate by ICP-AES. The new analyses were requested in order to provide confidence that the initial analytical subsample was representative of the Tank 40 sample received and to replicate the S results obtained on the initial subsample collected. The ICP-AES analyses for S were examined with both axial and radial detection of the sulfur ICP-AES spectroscopic emission linesmore » to ascertain if there was any significant difference in the reported results. The outcome of this second subsample of the Tank 40 WAPS material is the first subject of this report. After examination of the data from the new subsample of the SB7b WAPS material, a team of DWPF and SRNL staff looked for ways to address the question of whether there was in fact insoluble S that was not being accounted for by ion chromatography (IC) analysis. The question of how much S is reaching the melter was thought best addressed by examining a DWPF Slurry Mix Evaporator (SME) Product sample, but the significant dilution of sludge material, containing the S species in question, that results from frit addition was believed to add additional uncertainty to the S analysis of SME Product material. At the time of these discussions it was believed that all S present in a Sludge Receipt and Adjustment Tank (SRAT) Receipt sample would be converted to sulfate during the course of the SRAT cycle. A SRAT Product sample would not have the S dilution effect resulting from frit addition, and hence, it was decided that a DWPF SRAT Product sample would be obtained and submitted to SRNL for digestion and sample preparation followed by a round-robin analysis of the prepared samples by the DWPF Laboratory, F/H Laboratories, and SRNL for S and sulfate. The results of this round-robin analytical study are the second subject of this report.« less
Aging of ceramic carbonized hydroxyapatite at room temperature
NASA Astrophysics Data System (ADS)
Tkachenko, M. V.; Kamzin, A. S.
2016-08-01
The process of aging of ceramic carbonized hydroxyapatite (CHA) produced in a dry carbon dioxide atmosphere at temperatures of 800-1200°C has been studied by chemical and X-ray structural analysis, infrared spectroscopy, and scanning electron microscopy methods. The phase composition and structure of initial prepared ceramics samples and those aged for a year have been compared. It has been shown that relaxation of internal stresses occurring during pressed sample sintering causes plastic deformation of crystallites at room temperature, accompanied by redistribution of carbonate ions between A1, A2, B1, and B2 sites and CHA decomposition with the formation of CaO separations.
Hatch, Joseph R.; Bullock, John H.; Finkelman, Robert B.
2006-01-01
In 1999, the USGS initiated the National Coal Quality Inventory (NaCQI) project to address a need for quality information on coals that will be mined during the next 20-30 years. At the time this project was initiated, the publicly available USGS coal quality data was based on samples primarily collected and analyzed between 1973 and 1985. The primary objective of NaCQI was to create a database containing comprehensive, accurate and accessible chemical information on the quality of mined and prepared United States coals and their combustion byproducts. This objective was to be accomplished through maintaining the existing publicly available coal quality database, expanding the database through the acquisition of new samples from priority areas, and analysis of the samples using updated coal analytical chemistry procedures. Priorities for sampling include those areas where future sources of compliance coal are federally owned. This project was a cooperative effort between the U.S. Geological Survey (USGS), State geological surveys, universities, coal burning utilities, and the coal mining industry. Funding support came from the Electric Power Research Institute (EPRI) and the U.S. Department of Energy (DOE).
Williamson, J H; Lacy-Hulbert, S J
2014-01-01
To compare clinical and bacteriological cure rates of clinical mastitis following treatment with either antimicrobials or homeopathic preparations. Seven spring-calving herds from the Waikato region of New Zealand were used to source cases of clinical mastitis (n = 263 glands) during the first 90 days following calving. Duplicate milk samples were collected for bacteriology from each clinically infected gland at diagnosis and 25 (SD 5.3) days after initial treatment. Affected glands were treated with either an antimicrobial formulation or a homeopathic remedy. Generalised linear models with binomial error distribution and logit link were used to analyse the proportion of cows that were clinical treatment cures and the proportion of glands that were classified as bacteriological cures, based on initial and post-treatment milk samples. Mean cumulative incidence of clinical mastitis was 7% (range 2-13% across herds) of cows. Streptococcus uberis was the most common pathogen isolated from culture-positive samples from affected glands (140/209; 67%). The clinical cure rate was higher for cows treated with antimicrobials (107/113; 95%) than for cows treated with homeopathic remedies (72/114; 63%) (p < 0.001) based on the observance of clinical signs following initial treatment. Across all pathogen types bacteriological cure rate at gland level was higher for those cows treated with antimicrobials (75/102; 74%) than for those treated with a homeopathic preparation (39/107; 36%) (p < 0.001). Using herds located in the Waikato region of New Zealand, homeopathic remedies had significantly lower clinical and bacteriological cure rates compared with antimicrobials when used to treat post-calving clinical mastitis where S. uberis was the most common pathogen. The proportion of cows that needed retreatment was significantly higher for the homeopathic treated cows. This, combined with lower bacteriological cure rates, has implications for duration of infection, individual cow somatic cell count, costs associated with treatment and animal welfare.
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.
Chen, Grace Dongqing; Alberts, Catharina Johanna
2009-01-01
The low concentration and complex sample matrix of many clinical and environmental viral samples presents a significant challenge in the development of low cost, point-of-care viral assays. To address this problem, we investigated the use of a microfluidic passive magnetic separator combined with on-chip mixer to both purify and concentrate whole particle HIV-1 virions. Virus-containing plasma samples are first mixed to allow specific binding of the viral particles with antibody-conjugated superparamagnetic nanoparticles, and several passive mixer geometries were assessed for their mixing efficiencies. The virus-nanoparticle complexes are then separated from the plasma in a novel magnetic separation chamber, where packed micron-sized ferromagnetic particles serve as high magnetic gradient concentrators for an externally applied magnetic field. Thereafter, a viral lysis buffer was flowed through the chip and the released HIV proteins were assayed off-chip. Viral protein extraction efficiencies of 62% and 45% were achieved at 10uL/min and 30uL/min throughputs respectively. More importantly, an 80-fold concentration was observed for an initial sample volume of 1mL, and a 44-fold concentration for an initial sample volume of 0.5mL. The system is broadly applicable to microscale sample preparation of any viral sample and can be used for nucleic acid extraction as well as 40–80 fold enrichment of target viruses. PMID:19954210
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...
Li, Chuchu; Wang, Min
2017-08-01
Three sets of experiments using the picture naming tasks with the form preparation paradigm investigated the influence of orthographic experience on the development of phonological preparation unit in spoken word production in native Mandarin-speaking children. Participants included kindergarten children who have not received formal literacy instruction, Grade 1 children who are comparatively more exposed to the alphabetic pinyin system and have very limited Chinese character knowledge, Grades 2 and 4 children who have better character knowledge and more exposure to characters, and skilled adult readers who have the most advanced character knowledge and most exposure to characters. Only Grade 1 children showed the form preparation effect in the same initial consonant condition (i.e., when a list of target words shared the initial consonant). Both Grade 4 children and adults showed the preparation effect when the initial syllable (but not tone) among target words was shared. Kindergartners and Grade 2 children only showed the preparation effect when the initial syllable including tonal information was shared. These developmental changes in phonological preparation could be interpreted as a joint function of the modification of phonological representation and attentional shift. Extensive pinyin experience encourages speakers to attend to and select onset phoneme in phonological preparation, whereas extensive character experience encourages speakers to prepare spoken words in syllables.
NASA Technical Reports Server (NTRS)
Miller, Teresa Y.; Williams, George O.; Snyder, Robert S.
1985-01-01
The resolution of continuous flow electrophoresis systems is generally measured by the spread of the sample bands in the direction of the electrophoretic migration. This paper evaluates the cross section of the sample bands in the plane perpendicular to the flow and shows that the spread in the direction perpendicular to the migration increased significantly with the applied electric field. Concentrated samples of monodisperse latex particles and vinyltoluene T-butylstyrene particles in sample buffers of different electrical conductivities were used to map the shape of the sample bands relative to the zero electric field case. As the electric field was applied, the sample band spread from an initial diameter of only one-third the chamber thickness until it approached the chamber walls where electroosmosis significantly reduced the resolution of separation. It can be shown, however, that it is possible to minimize these distortions by careful sample preparation and experiment design.
A (13)C NMR analysis of the effects of electron radiation on graphite/polyetherimide composites
NASA Technical Reports Server (NTRS)
Ferguson, Milton W.
1989-01-01
Initial investigations have been made into the use of high resolution nuclear magnetic resonance (NMR) for the characterization of radiation effects in graphite and Kevlar fibers, polymers, and the fiber/matrix interface in graphite/polyetherimide composites. Sample preparation techniques were refined. Essential equipment has been procured. A new NMR probe was constructed to increase the proton signal-to-noise ratio. Problem areas have been identified and plans developed to resolve them.
Ga2O3-In2O3 thin films on sapphire substrates: Synthesis and ultraviolet photoconductivity
NASA Astrophysics Data System (ADS)
Muslimov, A. E.; Butashin, A. V.; Kolymagin, A. B.; Nabatov, B. V.; Kanevsky, V. M.
2017-11-01
The structure and electrical and optical properties of β-Ga2O3-In2O3 thin films on sapphire substrates with different orientations have been investigated. The samples have been prepared by annealing of gallium-indium metallic films on sapphire substrates in air at different gallium-to-indium ratios in the initial mixture. The photoconductivity of these structures in the solar-blind ultraviolet spectral region has been examined.
NASA Astrophysics Data System (ADS)
Dawande, Kiran; Patel, Swarnim; Bajpai, Rakesh; Keller, J. M.
2018-05-01
Thermally stimulated discharge currents in PVFO: PVDF blend samples of weight percentage ratio 80:20 and 95:05 prepared by the solution cast technique have been studied as function of polarizing temperature. Three distinct peaks are found at 60±10, 100±10, and 140 ±10 °C respectively. Activation energy values been calculated by initial rise method and it were found to range from 0.22 to 1.0 eV.
Ono, Hiroshi; Nishio, Shoko; Tsurii, Jun; Kawamoto, Tetsuhiro; Sonomoto, Kenji; Nakayama, Jiro
2014-11-01
Nukadoko is a fermented rice bran mash traditionally used for pickling vegetables in Japan. To date, the production of both homemade and commercial nukadoko depends on natural fermentation without using starter cultures. Here, we monitored chemical and microbiological changes in the initial batch fermentation of nukadoko. Nukadoko samples were prepared by spontaneous fermentation of four different brands of rice bran, and microbiome dynamics were analyzed for 2 months. In the first week, non-Lactobacillales lactic acid bacteria (LAB) species, which differed among the samples, grew proportionally to pH decrease and lactate increase. Thereafter, Lactobacillus plantarum started growing and consumed residual sugars, causing further lactate increase in nukadoko. Finally, microbial communities in all tested nukadoko samples were dominated by L. plantarum. Taken together, our results suggest that the mixture of the fast-growing LAB species and slow-growing L. plantarum may be used as a suitable starter culture to promote the initial fermentation of nukadoko. Copyright © 2014 The Society for Biotechnology, Japan. Published by Elsevier B.V. All rights reserved.
NASA Technical Reports Server (NTRS)
Mcgrath, J. E.
1982-01-01
The radiation degradation of poly(arylene ether sulfones) and related materials is studied. These basic studies are important both as a means to developing stronger, more stable matrix resins for composite materials, as well as to improve the data base in regard to chemical structure-physical property relationships. Thirty homo and copolymers were synthesized, at least partially characterized and, in several cases suitable film casting techniques were developed. Four samples were chosen for initial radiation degradation. Poly(dimethyl siloxane) soft bocks/segments can preferentially migrate to the surface of copolymer films. Since siloxanes are utilized as thermal control coatings, this form of 'molecular' coating is of interest. The chemistry for preparing such copolymers with any of the polymers described was demonstrated.
230Th/U ages Supporting Hanford Site-Wide Probabilistic Seismic Hazard Analysis
DOE Office of Scientific and Technical Information (OSTI.GOV)
Paces, James B.
This product represents a USGS Administrative Report that discusses samples and methods used to conduct uranium-series isotope analyses and resulting ages and initial 234U/238U activity ratios of pedogenic cements developed in several different surfaces in the Hanford area middle to late Pleistocene. Samples were collected and dated to provide calibration of soil development in surface deposits that are being used in the Hanford Site-Wide probabilistic seismic hazard analysis conducted by AMEC. The report includes description of sample locations and physical characteristics, sample preparation, chemical processing and mass spectrometry, analytical results, and calculated ages for individual sites. Ages of innermost rindsmore » on a number of samples from five sites in eastern Washington are consistent with a range of minimum depositional ages from 17 ka for cataclysmic flood deposits to greater than 500 ka for alluvium at several sites.« less
230Th/U ages Supporting Hanford Site‐Wide Probabilistic Seismic Hazard Analysis
Paces, James B.
2014-01-01
This product represents a USGS Administrative Report that discusses samples and methods used to conduct uranium-series isotope analyses and resulting ages and initial 234U/238U activity ratios of pedogenic cements developed in several different surfaces in the Hanford area middle to late Pleistocene. Samples were collected and dated to provide calibration of soil development in surface deposits that are being used in the Hanford Site-Wide probabilistic seismic hazard analysis conducted by AMEC. The report includes description of sample locations and physical characteristics, sample preparation, chemical processing and mass spectrometry, analytical results, and calculated ages for individual sites. Ages of innermost rinds on a number of samples from five sites in eastern Washington are consistent with a range of minimum depositional ages from 17 ka for cataclysmic flood deposits to greater than 500 ka for alluvium at several sites.
Characterization of Neutron Transmutation Doped (NTD) Ge for low temperature sensor development
NASA Astrophysics Data System (ADS)
Mathimalar, S.; Singh, V.; Dokania, N.; Nanal, V.; Pillay, R. G.; Pal, S.; Ramakrishnan, S.; Shrivastava, A.; Maheshwari, Priya; Pujari, P. K.; Ojha, S.; Kanjilal, D.; Jagadeesan, K. C.; Thakare, S. V.
2015-02-01
Development of NTD Ge sensors has been initiated for low temperature (mK) thermometry in The India-based TIN detector (TIN.TIN). NTD Ge sensors are prepared by thermal neutron irradiation of device grade Ge samples at Dhruva reactor, BARC, Mumbai. Detailed measurements have been carried out in irradiated samples for estimating the carrier concentration and fast neutron induced defects. The Positron Annihilation Lifetime Spectroscopy (PALS) measurements indicated monovacancy type defects for all irradiated samples, while Channeling studies employing RBS with 2 MeV alpha particles, revealed no significant defects in the samples exposed to fast neutron fluence of ∼ 4 ×1016 /cm2 . Both PALS and Channeling studies have shown that vacuum annealing at 600 °C for ∼ 2 h is sufficient to recover the damage in the irradiated samples, thereby making them suitable for the sensor development.
ERIC Educational Resources Information Center
European Commission, 2017
2017-01-01
"Preparing Teachers for Diversity: The Role of Initial Teacher Education. Annex 2 To the Final Report to DG Education, Youth, Sport and Culture of the European Commission. Case Study Summaries" is designed as a companion document to the final report "Preparing Teachers for Diversity: The Role of Initial Teacher Education. Final…
Beyki, Mostafa Hossein; Shemirani, Farzaneh; Khani, Rouhollah
2014-01-01
In this work, the nanoclay was intercalated with acyclovir (9-[(2-hydroxyethoxy) methyl] guanine), the toxicity of which to mammalian cells is very low. We used no organic solvents for preparation of modified clay and desorption of Cu ions from the sorbent. Batch and column methods were used, and sorption of Cu was quantitative (>98%) in the pH range of 7.5 to 10.0. Quantitative desorption occurred with 5.0 mL of 3.0 M HCl, and the amount of Cu(II) was measured by using flame atomic absorption spectrometry. In the initial solution the linear dynamic range and the LOD were 3.0-1000.0 and 0.58 μg/L, respectively. With 500.0 mL of sample, an enrichment factor of 100 was obtained. The RSD was 2.0% (n = 8, concentration = 0.5 mg/L), and the maximum capacity of the sorbent was 45.0 mg/g. The influence of experimental parameters including sample pH, ionic strength, type and volume of the eluent, and interference of some ions on the recoveries of Cu was investigated. The proposed method using a new and easier prepared solid sorbent was applied to the determination of Cu in different real samples with satisfactory results.
Analysis of laboratory compaction methods of roller compacted concrete
NASA Astrophysics Data System (ADS)
Trtík, Tomáš; Chylík, Roman; Bílý, Petr; Fládr, Josef
2017-09-01
Roller-Compacted Concrete (RCC) is an ordinary concrete poured and compacted with machines typically used for laying of asphalt road layers. One of the problems connected with this technology is preparation of representative samples in the laboratory. The aim of this work was to analyse two methods of preparation of RCC laboratory samples with bulk density as the comparative parameter. The first method used dynamic compaction by pneumatic hammer. The second method of compaction had a static character. The specimens were loaded by precisely defined force in laboratory loading machine to create the same conditions as during static rolling (in the Czech Republic, only static rolling is commonly used). Bulk densities obtained by the two compaction methods were compared with core drills extracted from real RCC structure. The results have shown that the samples produced by pneumatic hammer tend to overestimate the bulk density of the material. For both compaction methods, immediate bearing index test was performed to verify the quality of compaction. A fundamental difference between static and dynamic compaction was identified. In static compaction, initial resistance to penetration of the mandrel was higher, after exceeding certain limit the resistance was constant. This means that the samples were well compacted just on the surface. Specimens made by pneumatic hammer actively resisted throughout the test, the whole volume was uniformly compacted.
NASA Technical Reports Server (NTRS)
Strutzenberg, Louise L.; Grugel, R. N.; Trivedi, R. K.
2005-01-01
A series of experiments performed using the Pore Formation and Mobility Investigation (PFMI) apparatus within the glovebox facility (GBX) on board the International Space Station (ISS) has provided video images of the morphological evolution of a three-dimensional interface in a diffusion controlled regime. The experimental samples were prepared on ground by filling glass tubes, 1 cm ID and approximately 30 cm in length, with "alloys" of succinonitrile (SCN) and water in an atmosphere of nitrogen at 450 millibar pressure. The compositions of the samples processed and analyzed are 0.25,0.5 and 1.0 wt% water. Experimental processing parameters of temperature gradient and translation speed, as well as camera settings, were remotely monitored and manipulated from the ground Telescience Center (TSC) at the Marshall !3pace Flight Center. During the experiments, the sample was first subjected to a unidirectional melt back, generally at 10 microns per second, with a constant temperature gradient ahead of the melting interface. Following the melt back, the interface was allowed to stabilize before translation is initiated. The temperatures in the sample were monitored by six in situ thermocouples and the position is monitored by an optical linear encoder. For the experiments performed and analyzed, the gradients ranged from 2.5 - 3.3 K/mm and the initial pulling velocities ranged from 0.7 micron per second to 1 micron per second with subsequent transition velocities of up to 100 microns per second. The data provided by the PFMI for analysis includes near-real-time (NRT) video captured on the ground during the experiment runs, ISS Video Tape Recorder (VTR) data dumped from the VTR at the end of the experiment run and recorded on the ground, telemetry data including temperature and position measurements, and limited flight HI-8 tapes in 2 camera views of experiment runs for which tapes have been returned to the investigators from ISS. Because of limited down mass from the ISS, the majority of the initial analysis has been performed using the NRT and VTR video data but will be supplemented with the HI-8 video as it becomes available. hardware and procedures required to prepare samples for correlation to flight samples is described. Using this ground-based system, a series of experiments have been performed for direct comparison with the flight data. The results of these comparisons as well as implications to future microgravity experiments are presented and discussed. A ground-based thin-sample directional solidification system as well as all associated
Thermo-mechanical properties and microfabric of fly ash-stabilized gold tailings.
Lee, Joon Kyu; Shang, Julie Q; Jeong, Sangseom
2014-07-15
This paper studies the changes in thermal conductivity, temperature, and unconfined compressive strength of gold tailings and fly ash mixtures during the curing period of 5 days. The microfabric of the cured mixtures was investigated with mercury intrusion porosimetry (MIP). The mixture samples were prepared at their maximum dry unit weight and optimum moisture content. Effect of adding fly ash to gold tailings (i.e., 0, 20, and 40% of the dry weight of tailings) was examined, and a comparison was made on samples prepared at the same fly ash content by replacing gold tailings with humic acid (i.e., gold tailings and humic acid ratios of 100:0, 90:10, and 80:20 by weight) or by varying pore fluid chemistry (i.e., water and salt solutions of 1M NaCl and CaCl2). The results show that the initial thermal conductivity of the samples is sensitive to the mixture proportion and a declination in the thermal conductivity is observed due to hydration of fly ash and evaporation. Inclusion of fly ash and salts into gold tailings improves the unconfined compressive strength but the presence of humic acid in samples leads to the decrease of the strength. MIP results reveal the pore structure changes associated with the packing states of the samples that reflect the influential factors considered. Copyright © 2014 Elsevier B.V. All rights reserved.
Toward An Understanding of Cluster Evolution: A Deep X-Ray Selected Cluster Catalog from ROSAT
NASA Technical Reports Server (NTRS)
Jones, Christine; Oliversen, Ronald (Technical Monitor)
2002-01-01
In the past year, we have focussed on studying individual clusters found in this sample with Chandra, as well as using Chandra to measure the luminosity-temperature relation for a sample of distant clusters identified through the ROSAT study, and finally we are continuing our study of fossil groups. For the luminosity-temperature study, we compared a sample of nearby clusters with a sample of distant clusters and, for the first time, measured a significant change in the relation as a function of redshift (Vikhlinin et al. in final preparation for submission to Cape). We also used our ROSAT analysis to select and propose for Chandra observations of individual clusters. We are now analyzing the Chandra observations of the distant cluster A520, which appears to have undergone a recent merger. Finally, we have completed the analysis of the fossil groups identified in ROM observations. In the past few months, we have derived X-ray fluxes and luminosities as well as X-ray extents for an initial sample of 89 objects. Based on the X-ray extents and the lack of bright galaxies, we have identified 16 fossil groups. We are comparing their X-ray and optical properties with those of optically rich groups. A paper is being readied for submission (Jones, Forman, and Vikhlinin in preparation).
Soni, Dileep; Raisingani, Deepak; Mathur, Rachit; Madan, Nidha; Visnoi, Suchita
2016-01-01
To evaluate the incidence of apical crack initiation during canal preparation with stainless steel K-files and hand protaper files (in vitro study). Sixty extracted mandibular premo-lar teeth are randomly selected and embedded in an acrylic tube filled with autopolymerizing resin. A baseline image of the apical surface of each specimen was recorded under a digital microscope (80×). The cervical and middle thirds of all samples were flared with #2 and #1 Gates-Glidden (GG) drills, and a second image was recorded. The teeth were randomly divided into four groups of 15 teeth each according to the file type (hand K-file and hand-protaper) and working length (WL) (instrumented at WL and 1 mm less than WL). Final image after dye penetration and photomicrograph of the apical root surface were digitally recorded. Maximum numbers of cracks were observed with hand protaper files compared with hand K-file at the WL and 1 mm short of WL. Chi-square testing revealed a highly significant effect of WL on crack formation at WL and 1 mm short of WL (p = 0.000). Minimum numbers of cracks at WL and 1 mm short of WL were observed with hand K-file and maximum with hand protaper files. Soni D, Raisingani D, Mathur R, Madan N, Visnoi S. Incidence of Apical Crack Initiation during Canal Preparation using Hand Stainless Steel (K-File) and Hand NiTi (Protaper) Files. Int J Clin Pediatr Dent 2016;9(4):303-307.
NASA Astrophysics Data System (ADS)
Jafari, Meysam; Garrison, Warren M.; Tsuzaki, Kaneaki
2014-02-01
A medium-carbon low-alloy steel was prepared with initial structures of either martensite or bainite. For both initial structures, warm caliber-rolling was conducted at 773 K (500 °C) to obtain ultrafine elongated grain (UFEG) structures with strong <110>//rolling direction (RD) fiber deformation textures. The UFEG structures consisted of spheroidal cementite particles distributed uniformly in a ferrite matrix of a transverse grain size of about 331 and 311 nm in samples with initial martensite and bainite structures, respectively. For both initial structures, the UFEG materials had similar tensile properties, upper shelf energy (145 J), and ductile-to-brittle transition temperatures 98 K (500 °C). Obtaining the martensitic structure requires more rapid cooling than is needed to obtain the bainitic structure and this more rapid cooling promote cracking. As the UFEG structures obtained from initial martensitic and bainitic structures have almost identical properties, but obtaining the bainitic structure does not require a rapid cooling which promotes cracking suggests the use of a bainitic structure in obtaining UFEG structures should be examined further.
Heat Effects of Promoters and Determination of Burn Criterion in Promoted Combustion Testing
NASA Technical Reports Server (NTRS)
Sparks, Kyle M.; Stoltzfus, Joel M.; Steinberg, Theodore A.; Lynn, David
2010-01-01
Promoted ignition testing (NASA Test 17) [1] is used to determine the relative flammability of metal rods in oxygen-enriched atmospheres. A promoter is used to ignite a metal sample rod, initiating sample burning. If a predetermined length of the sample burns, beyond the promoter, the material is considered flammable at the condition tested. Historically, this burn length has been somewhat arbitrary. Experiments were performed to better understand this test by obtaining insight into the effect a burning promoter has on the preheating of a test sample. Test samples of several metallic materials were prepared and coupled to fast-responding thermocouples along their length. Thermocouple measurements and test video were synchronized to determine temperature increase with respect to time and length along each test sample. A recommended flammability burn length, based on a sample preheat of 500 F, was determined based on the preheated zone measured from these tests. This length was determined to be 30 mm (1.18 in.). Validation of this length and its rationale are presented.
Paul, Baboo Joseph; Gim, Jihyeon; Baek, Sora; Kang, Jungwon; Song, Jinju; Kim, Sungjin; Kim, Jaekook
2015-08-01
Nanocrystalline LiFePO4/C has been synthesized under a very short period of time (90 sec) using a polyol-assisted microwave heating synthesis technique. The X-ray diffraction (XRD) data indicates that the rapidly synthesized materials correspond to phase pure olivine. Post-annealing of the as-prepared sample at 600 °C in argon atmosphere yields highly crystalline LiFePO4/C. The morphology of the samples studied using scanning electron microscopy (SEM) reveals the presence of secondary particles formed from aggregation of primary particles in the range of 30-50 nm. Transmission electron microscopy (TEM) images reveal a thin carbon layer coating on the surface of the primary particle. The charge/discharge studies indicate that the as-prepared and annealed LiFePO4/C samples delivered initial discharge capacities of 126 and 160 mA h g-1, respectively, with good capacity retentions at 0.05 mA cm-2 current densities. The post-annealing process indeed improves the crystallinity of the LiFePO4 nanocrystals, which enhances the electrode performance of LiFePO4/C.
NASA Astrophysics Data System (ADS)
AbdulRahman, A.; Latiff, A. A. A.; Daud, Z.; Ridzuan, M. B.; D, N. F. M.; Jagaba, A. H.
2016-07-01
Several studies have been conducted on the removal of heavy metals from palm oil mill effluent. In this study, cow bones were developed as an adsorbent for the removal of cadmium II from POME. A batch experiment was conducted to investigate the effectiveness of the prepared activated cow bone powder for the sorption of cadmium II from raw POME. The experiment was carried out under fixed conditions using 100mg/L raw POME combined with different adsorbent dosage of CBP of 184.471 Ra(nm) surface roughness. The equilibrium adsorption capacity of the hydrophobic CBP of average contact angle 890 was determined from the relationship between the initial and equilibrium liquid phase concentrations of POME. The optimum adsorption of cadmium II on CBP was at 10g adsorbent dosage for sample 1 and 2 at 97.8% and 96.93% respectively. The least uptake was at 30g adsorbent weight for both samples at average of 95.1% for both samples. The effective removal of cadmium ion showed that CBP has a great potential for the treatment of heavy metal in POME.
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.
NASA Astrophysics Data System (ADS)
Jalaiah, K.; Vijaya Babu, K.; Rajashekhar Babu, K.; Chandra Mouli, K.
2018-06-01
Zr and Co substituted Ni0.5Zn0.5 ZrxCuxFe2-2xO4 with x values varies from the 0.0 to 0.4 in steps of 0.08 wt% ferrites synthesized by using sol-gel auto combustion method. The XRD patterns give evidence for formation of the single phase cubic spinel. The lattice constant was initially decreased from 8.3995 Å to 8.3941 Å with dopant concentration for x = 0.00-0.08 thereafter the lattice parameter steeply increased up to 8.4129 Å fox x = 0.4 with increasing dopant concentration. The estimated crystallite size and measured particle sizes are in comparable nano size. The grain size initially increased 2.3137-3.0430 μm, later it decreased to 2.2952 μm with increasing dopant concentration. The prepared samples porosity shows the opposite trend to grain size. The FT-IR spectrum for prepared samples shows the Fd3m (O7h). The wavenumber for tetrahedral site increased from 579 cm-1 to 593 cm-1 with increasing dopant concentration and the wavenumber of octahedral site are initially decreased from 414 cm-1 to 400 cm-1 for x = 0.00 to x = 0.08 later increased to 422 cm-1 with increasing dopant concentration. The dielectric constant increased from 8.85 to 34.5127 with dopant increasing concentration. The corresponding loss factor was fallows the similar trend as dielectric constant. The AC conductivity increased with increasing dopant concentration from 3.0261 × 10-7 S/m to 4.4169 × 10-6 S/m.
Stability of tacrolimus solutions in polyolefin containers.
Lee, Jun H; Goldspiel, Barry R; Ryu, Sujung; Potti, Gopal K
2016-02-01
Results of a study to determine the stability of tacrolimus solutions stored in polyolefin containers under various temperature conditions are reported. Triplicate solutions of tacrolimus (0.001, 0.01, and 0.1 mg/mL) in 0.9% sodium chloride injection or 5% dextrose injection were prepared in polyolefin containers. Some samples were stored at room temperature (20-25 °C); others were refrigerated (2-8 °C) for 20 hours and then stored at room temperature for up to 28 hours. The solutions were analyzed by stability-indicating high-performance liquid chromatography (HPLC) assay at specified time points over 48 hours. Solution pH was measured and containers were visually inspected at each time point. Stability was defined as retention of at least 90% of the initial tacrolimus concentration. All tested solutions retained over 90% of the initial tacrolimus concentration at all time points, with the exception of the 0.001-mg/mL solution prepared in 0.9% sodium chloride injection, which was deemed unstable beyond 24 hours. At all evaluated concentrations, mean solution pH values did not change significantly over 48 hours; no particle formation was detected. During storage in polyolefin bags at room temperature, a 0.001-mg/mL solution of tacrolimus was stable for 24 hours when prepared in 0.9% sodium chloride injection and for at least 48 hours when prepared in 5% dextrose injection. Solutions of 0.01 and 0.1 mg/mL prepared in either diluent were stable for at least 48 hours, and the 0.01-mg/mL tacrolimus solution was also found to be stable throughout a sequential temperature protocol. Copyright © 2016 by the American Society of Health-System Pharmacists, Inc. All rights reserved.
NASA Astrophysics Data System (ADS)
Lee, Sojin; Song, Chul-han; Park, Rae Seol; Park, Mi Eun; Han, Kyung man; Kim, Jhoon; Choi, Myungje; Ghim, Young Sung; Woo, Jung-Hun
2016-04-01
To improve short-term particulate matter (PM) forecasts in South Korea, the initial distribution of PM composition, particularly over the upwind regions, is primarily important. To prepare the initial PM composition, the aerosol optical depth (AOD) data retrieved from a geostationary equatorial orbit (GEO) satellite sensor, GOCI (Geostationary Ocean Color Imager) which covers a part of Northeast Asia (113-146° E; 25-47° N), were used. Although GOCI can provide a higher number of AOD data in a semicontinuous manner than low Earth orbit (LEO) satellite sensors, it still has a serious limitation in that the AOD data are not available at cloud pixels and over high-reflectance areas, such as desert and snow-covered regions. To overcome this limitation, a spatiotemporal-kriging (STK) method was used to better prepare the initial AOD distributions that were converted into the PM composition over Northeast Asia. One of the largest advantages in using the STK method in this study is that more observed AOD data can be used to prepare the best initial AOD fields compared with other methods that use single frame of observation data around the time of initialization. It is demonstrated in this study that the short-term PM forecast system developed with the application of the STK method can greatly improve PM10 predictions in the Seoul metropolitan area (SMA) when evaluated with ground-based observations. For example, errors and biases of PM10 predictions decreased by ˜ 60 and ˜ 70{%}, respectively, during the first 6 h of short-term PM forecasting, compared with those without the initial PM composition. In addition, the influences of several factors on the performances of the short-term PM forecast were explored in this study. The influences of the choices of the control variables on the PM chemical composition were also investigated with the composition data measured via PILS-IC (particle-into-liquid sampler coupled with ion chromatography) and low air-volume sample instruments at a site near Seoul. To improve the overall performances of the short-term PM forecast system, several future research directions were also discussed and suggested.
Recent advances in applications of nanomaterials for sample preparation.
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.
Islam, Md Azharul; Ahmed, M J; Khanday, W A; Asif, M; Hameed, B H
2017-04-01
Hydrothermal carbonization of biomass wastes presents a promising step in the production of cost-effective activated carbon. In the present work, mesoporous activated carbon (HAC) was prepared by the hydrothermal carbonization of rattan furniture wastes followed by NaOH activation. The textural and morphological characteristics, along with adsorption performance of prepared HAC toward methylene blue (MB) dye, were evaluated. The effects of common adsorption variables on performance resulted in a removal efficiency of 96% for the MB sample at initial concentration of 25mg/L, solution pH of 7, 30°C, and 8h. The Langmuir equation showed the best isotherm data correlation, with a maximum uptake of 359mg/g. The adsorbed amount versus time data was well fitted by a pseudo-second order kinetic model. The prepared HAC with a high surface area of 1135m 2 /g and an average pore size distribution of 35.5Å could be an efficient adsorbent for treatment of synthetic dyes in wastewaters. Copyright © 2017 Elsevier Inc. All rights reserved.
Jha, Vinay Kumar; Kameshima, Yoshikazu; Nakajima, Akira; Okada, Kiyoshi; MacKenzie, Kenneth J D
2005-08-31
A series of nCaO.Al2O3.2SiO2 samples (n=1-4) were prepared by solid-state reaction of mechanochemically treated mixtures of kaolinite and calcite fired at 600-1000 degrees C for 24 h. All the samples were X-ray amorphous after firing at 600-800 degrees C but had crystallized by 900 degrees C. The main crystalline phases were anorthite (n=1), gehlenite (n=2 and 3) and larnite (n=4). The uptake of Ni2+ by nCaO.Al2O3.2SiO2 samples fired at 800 and 900 degrees C was investigated at room temperature using solutions with initial Ni2+ concentrations of 0.1-50 mmol/l. Amorphous samples (fired at 800 degrees C) showed a higher Ni2+ uptake capacity than crystalline samples (fired at 900 degrees C). Ni2+ uptake was found to increase with increasing of CaO content. Amorphous 4CaO.Al2O3.2SiO2 showed the highest Ni2+ uptake capacity (about 9 mmol/g). The Ni2+ uptake abilities of the present samples are higher than those of other materials reported in the literature. Since the sorbed Ni2+/released Ca2+ ratios of these samples are close to unity, ion replacement of Ni2+ for Ca2+ is thought to be the principal mechanism of Ni2+ uptake by the present samples.
ERIC Educational Resources Information Center
Gonzales, Alberto
2010-01-01
Schools are constantly engaged in implementing reform strategies to prepare students for post-secondary education leading to their career choices. Challenges here involve education initiatives addressing programs not strategically planned, educators not prepared for transition, and no follow-up support beyond initial implementation stages. This…
ERIC Educational Resources Information Center
Gonzales, Alberto; Jones, Don; Ruiz, Alberto
2014-01-01
Schools are constantly engaged in implementing reform strategies to prepare students for postsecondary education leading to their career choices. Challenges here involve education initiatives addressing programs not strategically planned, educators not prepared for transition, and no follow-up support beyond initial implementation stages. This…
Initial and Ongoing Teacher Preparation and Support: Current Problems and Possible Solutions
ERIC Educational Resources Information Center
Johnson, Harold A.
2013-01-01
The effective initial preparation and ongoing support of teachers of students who are deaf and hard of hearing has always been a difficult and controversial task. Changes in student demographic characteristics and educational settings, combined with the rapidly diminishing number and diversity of deaf education teacher preparation (DETP) programs,…
The Recent Developments in Sample Preparation for Mass Spectrometry-Based Metabolomics.
Gong, Zhi-Gang; Hu, Jing; Wu, Xi; Xu, Yong-Jiang
2017-07-04
Metabolomics is a critical member in systems biology. Although great progress has been achieved in metabolomics, there are still some problems in sample preparation, data processing and data interpretation. In this review, we intend to explore the roles, challenges and trends in sample preparation for mass spectrometry- (MS-) based metabolomics. The newly emerged sample preparation methods were also critically examined, including laser microdissection, in vivo sampling, dried blood spot, microwave, ultrasound and enzyme-assisted extraction, as well as microextraction techniques. Finally, we provide some conclusions and perspectives for sample preparation in MS-based metabolomics.
Infrared Extinction and the Initial Conditions For Star and Planet Formation
NASA Technical Reports Server (NTRS)
Lada, Charles J.
2003-01-01
This grant funds a research program to use infrared extinction measurements to probe the detailed structure of dark molecular clouds and investigate the physical conditions which give rise to star and planet formation. The goals of the this program are to: 1) acquire deep infrared and molecular-line observations of a carefully selected sample of nearby dark clouds, 2) reduce and analyze the data obtained in order to produce detailed extinction maps of the clouds, 3) prepare results, where appropriate, for publication.
Infrared Extinction and the Initial Conditions for Star and Planet Formation
NASA Technical Reports Server (NTRS)
Lada, Charles J.
2002-01-01
This grant funds a research program to use infrared extinction measurements to probe the detailed structure of dark molecular clouds and investigate the physical conditions which give rise to star and planet formation. The goals of the this program are to: (1) acquire deep infrared and molecular-line observations of a carefully selected sample of nearby dark clouds; (2) reduce and analyze the data obtained in order to produce detailed extinction maps of the clouds; and (3) prepare results, where appropriate, for publication.
Development and Evaluation of Integrity Assessment Tests for Polymeric Hermetic Seals
2006-02-19
Knoxville, the wires were pulled from the seals and then the packages were dipped in the microorganism Enterobacter aerogene . The polytrays were exposed for...inoculated) 5 samples Total Polytrays 80 Microorganism Washes 1. Prepare Cultures of Enterobacter aerogenes a. 5 tubes (10 mL each) in...initial number – 6 log CFU/mL a. Add two tubes (20 mL) of Enterobacter aerogenes culture to 5 gallons of water with sodium thiosulfate b. Ca. 9 log CFU
Effect of Passive Ultrasonic Irrigation on Enterococcus faecalis from Root Canals: An Ex Vivo Study.
Guerreiro-Tanomaru, Juliane Maria; Chávez-Andrade, Gisselle Moraima; de Faria-Júnior, Norberto Batista; Watanabe, Evandro; Tanomaru-Filho, Mário
2015-01-01
Endodontic irrigation aims to clean and disinfect the root canal system. Passive ultrasonic irrigation (PUI) is based on the use of an ultrasound-activated instrument into the root canal filled with irrigant. The aim of this study was to evaluate, ex vivo, the effectiveness of PUI in eliminating Enterococcus faecalis from root canals. Seventy-five extracted human single-root teeth were used. After root canal preparation, specimens were inoculated with E. faecalis and incubated at 37 °C for 21 days. Specimens were distributed into five groups (n=15), according to the irrigation method: PUI + saline solution (PUI/SS); PUI + 1% NaOCl (PUI/NaOCl); conventional needle irrigation (CNI) + saline solution (CNI/SS); CNI + 1% NaOCl (CNI/NaOCl); No irrigation (control). Microbiological samples were collected at three time points: initial (21 days after inoculation), post-irrigation (immediately after irrigation), and final (7 days after irrigation). Data were obtained in CFU mL-1 and subjected to analysis by ANOVA and Tukey's tests at 5% significance level. The post-irrigation samples did not demonstrate statistical difference between PUI/SS and CNI/SS nor between PUI/NaOCl and CNI/NaOCl (p>0.05), but PUI/NaOCl and CNI/NaOCl had lower CFU mL-1 number than the other groups (p>0.05). Statistically significant difference was observed between the initial and post-irrigation samples and between the post-irrigation and final samples (p<0.05) in all groups, except in the control. The final samples of all groups presented bacterial counts similar to the initial samples. PUI or CNI with 1% NaOCl contribute to disinfection, but are unable to eradicate E. faecalis from the root canal system.
Managadze, G G; Safronova, A A; Luchnikov, K A; Vorobyova, E A; Duxbury, N S; Wurz, P; Managadze, N G; Chumikov, A E; Khamizov, R Kh
2017-05-01
We propose a new technique for the detection of microorganisms by elemental composition analyses of a sample extracted from regolith, permafrost, and ice of extraterrestrial bodies. We also describe the design of the ABIMAS instrument, which consists of the onboard time-of-flight laser mass-reflectron (TOF LMR) and the sample preparation unit (SPU) for biomass extraction. This instrument was initially approved to fly on board the ExoMars 2020 lander mission. The instrument can be used to analyze the elemental composition of possible extraterrestrial microbial communities and compare it to that of terrestrial microorganisms. We have conducted numerous laboratory studies to confirm the possibility of biomass identification via the following biomarkers: P/S and Ca/K ratios, and C and N abundances. We underline that only the combination of these factors will allow one to discriminate microbial samples from geological ones. Our technique has been tested experimentally in numerous laboratory trials on cultures of microorganisms and polar permafrost samples as terrestrial analogues for martian polar soils. We discuss various methods of extracting microorganisms and sample preparation. The developed technique can be used to search for and identify microorganisms in different martian samples and in the subsurface of other planets, satellites, comets, and asteroids-in particular, Europa, Ganymede, and Enceladus. Key Words: Mass spectrometry-Life-detection instruments-Biomarkers-Earth Mars-Biomass spectra. Astrobiology 17, 448-458.
Liquid-based cytology for primary cervical cancer screening: a multi-centre study
Monsonego, J; Autillo-Touati, A; Bergeron, C; Dachez, R; Liaras, J; Saurel, J; Zerat, L; Chatelain, P; Mottot, C
2001-01-01
The aim of this six-centre, split-sample study was to compare ThinPrep fluid-based cytology to the conventional Papanicolaou smear. Six cytopathology laboratories and 35 gynaecologists participated. 5428 patients met the inclusion criteria (age > 18 years old, intact cervix, informed consent). Each cervical sample was used first to prepare a conventional Pap smear, then the sampling device was rinsed into a PreservCyt vial, and a ThinPrep slide was made. Screening of slide pairs was blinded (n = 5428). All non-negative concordant cases (n = 101), all non-concordant cases (n = 206), and a 5% random sample of concordant negative cases (n = 272) underwent review by one independent pathologist then by the panel of 6 investigators. Initial (blinded) screening results for ThinPrep and conventional smears were correlated. Initial diagnoses were correlated with consensus cytological diagnoses. Differences in disease detection were evaluated using McNemar's test. On initial screening, 29% more ASCUS cases and 39% more low-grade squamous intraepithelial lesions (LSIL) and more severe lesions (LSIL+) were detected on the ThinPrep slides than on the conventional smears (P = 0.001), including 50% more LSIL and 18% more high-grade SIL (HSIL). The ASCUS:SIL ratio was lower for the ThinPrep method (115:132 = 0.87:1) than for the conventional smear method (89:94 = 0.95:1). The same trend was observed for the ASCUS/AGUS:LSIL ratio. Independent and consensus review confirmed 145 LSIL+ diagnoses; of these, 18% more had been detected initially on the ThinPrep slides than on the conventional smears (P = 0.041). The ThinPrep Pap Test is more accurate than the conventional Pap test and has the potential to optimize the effectiveness of primary cervical cancer screening. © 2001 Cancer Research Campaign http://www.bjcancer.com PMID:11161401
Chen, Yi; Allard, Emma; Wooten, Anna; ...
2016-05-18
The recovery and growth potential of Listeria monocytogenes was evaluated in three flavors of milkshakes (vanilla, strawberry, and chocolate) that were prepared from naturally contaminated ice cream linked to a listeriosis outbreak in the U.S. in 2015, and were subsequently held at room temperature for 14 h. The average lag phase duration of L. monocytogenes was 9.05 h; the average generation time was 1.67 h; and the average population level increase per sample at 14 h was 1.14 log CFU/g. Milkshake flavors did not significantly affect these parameters. The average lag phase duration of L. monocytogenes in milkshakes with initialmore » contamination levels ≤ 3 CFU/g (9.50 h) was significantly longer (P < 0.01) than that with initial contamination levels > 3 CFU/g (8.60 h). The results highlight the value of using samples that are contaminated with very low levels of L. monocytogenes for recovery and growth evaluations. The behavior of L. monocytogenes populations in milkshakes prepared from naturally contaminated ice cream linked to the listeriosis outbreak should be taken into account when performing risk based analysis using this outbreak as a case study.« less
NASA Astrophysics Data System (ADS)
Tong, Wei; Huang, Yudai; Cai, Yanjun; Guo, Yong; Wang, Xingchao; Jia, Dianzeng; Sun, Zhipeng; Pang, Weikong; Guo, Zaiping; Zong, Jun
2018-01-01
Hierarchical mesoporous LiNi1/3Co1/3Mn1/3O2 spheres have been synthesized by urea-assisted solvothermal method with adding Triton X-100. The structure and morphology of the as-prepared materials were analyzed by X-ray diffraction and electron microscope. The results show that the as-prepared samples can be indexed as hexagonal layered structure with hierarchical architecture, and the possible formation mechanism is speculated. When evaluated as cathode material, the hierarchical mesoporous LiNi1/3Co1/3Mn1/3O2 spheres show good electrochemical properties with high initial discharge capacity of 129.9 mAh g-1, and remain the discharge capacity of 95.5 mAh g-1 after 160 cycles at 10C. The excellent electrochemical performance of the as-prepared sample can be attributed to its stable hierarchical mesoporous framework in conjunction with large specific surface, low cation mixing and small particle size. They not only provide a large number of reaction sites for surface or interface reaction, but also shorten the diffusion length of Li+ ions. Meanwhile, the mesoporous spheres composed of nanoparticles can contribute to high rate ability and buffer volume changes during charge/discharge process.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Chen, Yi; Allard, Emma; Wooten, Anna
The recovery and growth potential of Listeria monocytogenes was evaluated in three flavors of milkshakes (vanilla, strawberry, and chocolate) that were prepared from naturally contaminated ice cream linked to a listeriosis outbreak in the U.S. in 2015, and were subsequently held at room temperature for 14 h. The average lag phase duration of L. monocytogenes was 9.05 h; the average generation time was 1.67 h; and the average population level increase per sample at 14 h was 1.14 log CFU/g. Milkshake flavors did not significantly affect these parameters. The average lag phase duration of L. monocytogenes in milkshakes with initialmore » contamination levels ≤ 3 CFU/g (9.50 h) was significantly longer (P < 0.01) than that with initial contamination levels > 3 CFU/g (8.60 h). The results highlight the value of using samples that are contaminated with very low levels of L. monocytogenes for recovery and growth evaluations. The behavior of L. monocytogenes populations in milkshakes prepared from naturally contaminated ice cream linked to the listeriosis outbreak should be taken into account when performing risk based analysis using this outbreak as a case study.« less
Shojania, S; Oleschuk, R D; McComb, M E; Gesser, H D; Chow, A
1999-08-23
A new and simple method of solventless extraction of volatile organic compounds (VOCs) from air is presented. The sampling device has an adsorbing carbon coating on the interior surface of a hollow needle, and is called the inside needle capillary adsorption trap (INCAT). This paper describes a study of the reproducibility in the preparation and sampling of the INCAT device. In addition, this paper examines the effects of sample volume in active sampling and exposure time in passive sampling on the analyte adsorption. Analysis was achieved by sampling the air from an environmental chamber doped with benzene, toluene, ethyl benzene and xylenes (BTEX) compounds. Initial rates of adsorption were found to vary among the different compounds, but ranged from 0.0099 to 0.016 nmol h(-1) for passive sampling and from 2.2 to 10 nmol h(-1) for active sampling. Analysis was done by thermal desorption of the adsorbed compounds directly into a gas chromatograph injection port. Quantification of the analysis was done by comparison to actively sampled activated carbon solid phase extraction (SPE) measurements.
Mandal, Abhishek; Boatz, Jennifer C.; Wheeler, Travis; van der Wel, Patrick C. A.
2017-01-01
A number of recent advances in the field of magic-angle-spinning (MAS) solid-state NMR have enabled its application to a range of biological systems of ever increasing complexity. To retain biological relevance, these samples are increasingly studied in a hydrated state. At the same time, experimental feasibility requires the sample preparation process to attain a high sample concentration within the final MAS rotor. We discuss these considerations, and how they have led to a number of different approaches to MAS NMR sample preparation. We describe our experience of how custom-made (or commercially available) ultracentrifugal devices can facilitate a simple, fast and reliable sample preparation process. A number of groups have since adopted such tools, in some cases to prepare samples for sedimentation-style MAS NMR experiments. Here we argue for a more widespread adoption of their use for routine MAS NMR sample preparation. PMID:28229262
Banerjee, Chiranjib; Westberg, Michael; Breitenbach, Thomas; Bregnhøj, Mikkel; Ogilby, Peter R
2017-06-06
The oxidation of lipids is an important phenomenon with ramifications for disciplines that range from food science to cell biology. The development and characterization of tools and techniques to monitor lipid oxidation are thus relevant. Of particular significance in this regard are tools that facilitate the study of oxidations at interfaces in heterogeneous samples (e.g., oil-in-water emulsions, cell membranes). In this article, we establish a proof-of-principle for methods to initiate and then monitor such oxidations with high spatial resolution. The experiments were performed using oil-in-water emulsions of polyunsaturated fatty acids (PUFAs) prepared from cod liver oil. We produced singlet oxygen at a point near the oil-water interface of a given PUFA droplet in a spatially localized two-photon photosensitized process. We then followed the oxidation reactions initiated by this process with the fluorescence-based imaging technique of structured illumination microscopy (SIM). We conclude that the approach reported herein has attributes well-suited to the study of lipid oxidation in heterogeneous samples.
Hydrothermal Synthesized of CoMoO4 Microspheres as Excellent Electrode Material for Supercapacitor.
Li, Weixia; Wang, Xianwei; Hu, Yanchun; Sun, Lingyun; Gao, Chang; Zhang, Cuicui; Liu, Han; Duan, Meng
2018-04-24
The single-phase CoMoO 4 was prepared via a facile hydrothermal method coupled with calcination treatment at 400 °C. The structures, morphologies, and electrochemical properties of samples with different hydrothermal reaction times were investigated. The microsphere structure, which consisted of nanoflakes, was observed in samples. The specific capacitances at 1 A g -1 are 151, 182, 243, 384, and 186 F g -1 for samples with the hydrothermal times of 1, 4, 8, 12, and 24 h, respectively. In addition, the sample with the hydrothermal time of 12 h shows a good rate capability, and there is 45% retention of initial capacitance when the current density increases from 1 to 8 A g -1 . The high retain capacitances of samples show the fine long-cycle stability after 1000 charge-discharge cycles at current density of 8 A g -1 . The results indicate that CoMoO 4 samples could be a choice of excellent electrode materials for supercapacitor.
Hydrothermal Synthesized of CoMoO4 Microspheres as Excellent Electrode Material for Supercapacitor
NASA Astrophysics Data System (ADS)
Li, Weixia; Wang, Xianwei; Hu, Yanchun; Sun, Lingyun; Gao, Chang; Zhang, Cuicui; Liu, Han; Duan, Meng
2018-04-01
The single-phase CoMoO4 was prepared via a facile hydrothermal method coupled with calcination treatment at 400 °C. The structures, morphologies, and electrochemical properties of samples with different hydrothermal reaction times were investigated. The microsphere structure, which consisted of nanoflakes, was observed in samples. The specific capacitances at 1 A g-1 are 151, 182, 243, 384, and 186 F g-1 for samples with the hydrothermal times of 1, 4, 8, 12, and 24 h, respectively. In addition, the sample with the hydrothermal time of 12 h shows a good rate capability, and there is 45% retention of initial capacitance when the current density increases from 1 to 8 A g-1. The high retain capacitances of samples show the fine long-cycle stability after 1000 charge-discharge cycles at current density of 8 A g-1. The results indicate that CoMoO4 samples could be a choice of excellent electrode materials for supercapacitor.
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.
The Response of Simple Polymer Structures Under Dynamic Loading
NASA Astrophysics Data System (ADS)
Proud, William; Ellison, Kay; Yapp, Su; Cole, Cloe; Galimberti, Stefano; Institute of Shock Physics Team
2017-06-01
The dynamic response of polymeric materials has been widely studied with the effects of degree of crystallinity, strain rate, temperature and sample size being commonly reported. This study uses a simple PMMA structure, a right cylindrical sample, with structural features such as holes. The features are added an varied in a systematic fashion. Samples were dynamically loaded using a Split Hopkinson Pressure Bar up to failure. The resulting stress-strain curves are presented showing the change in sample response. The strain to failure is shown to increase initially with the presence of holes, while failure stress is relatively unaffected. The fracture patterns seen in the failed samples change, with tensile cracks, Hertzian cones, shear effects being dominant for different holes sizes and geometries. The sample were prepared by laser cutting and checked for residual stress before experiment. The data is used to validate predictive model predictions where material, structure and damage are included.. The Institute of Shock Physics acknowledges the support of Imperial College London and the Atomic Weapons Establishment.
ERIC Educational Resources Information Center
Murphy, Joseph; Moorman, Hunter N.; McCarthy, Martha
2008-01-01
Background/Context: This study examines the extent of reform in preparation programs in school leadership in six states employing a comprehensive, whole-state intervention design. Although no studies of these or other comprehensive reform designs are available, there is a rich context surrounding preparation reform work that informed our…
NASA Astrophysics Data System (ADS)
Liang, Pan; Du, Lu; Wang, Xia; Liu, Zhi-Hong
2014-11-01
A novel flower-like nickel borate of Ni3B2O6 nanostructure was prepared through a hydrothermal treatment and sequential thermal decomposition of precursor without employing any template or surfactant. All the samples were characterized by XRD, IR, XPS, TG-DTA, nitrogen adsorption, SEM and TEM. The flower-like Ni3B2O6 nanostructure was self-assembled by nanosheets with the thickness of about 40 nm. The electrochemical properties in lithium-ion battery of flower-like Ni3B2O6 nanostructure were studied by the cyclic voltammetry, galvanostatic cycling test, and electrochemical impedance spectroscopy, which showed it had a high initial discharge capacity and a good reversibility.
Stability of levothyroxine sodium 0.4 microg/mL in 0.9% sodium chloride injection.
Stadalman, Kelli A; Kelner, Michael J; Box, Kevin; Dominguez, Alex; Rigby, Joseph F
2009-12-01
Intravenous levothyroxine therapy decreases vasopressor requirements and prevents cardiovascular collapse in hemodynamically unstable patients eligible for organ donation. The stability of levothyroxine when used in this manner is unknown. To determine the stability of levothyroxine solution for intravenous use at a concentration of 0.4 microg/mL diluted in 0.9% sodium chloride. Triplicate sample sets were prepared by reconstituting levothyroxine 200 microg for injection with 5 mL of 0.9% sodium chloride with further dilution in 500 mL of 0.9% sodium chloride. One sample set was protected from light and the other was left unprotected. Both sample sets were stored at room temperature, and samples from each were analyzed for initial concentration and 4, 8, 12, and 24 hours later. Levothyroxine sodium 0.4 microg/mL in 500 mL 0.9% sodium chloride is stable for 24 hours at room temperature when protected from light.
Spectral Characterization of Analog Samples in Anticipation of OSIRIS-REx's Arrival at Bennu
NASA Technical Reports Server (NTRS)
Donaldson Hanna, K. L.; Schrader, D. L.; Bowles, N. E.; Clark, B. E.; Cloutis, E. A.; Connolly, H. C., Jr.; Hamilton, V. E.; Keller, L. P.; Lauretta, D. S.; Lim, L. F.;
2017-01-01
NASA's Origins, Spectral Interpretation, Resource Identification, and Security-Regolith Explorer (OSIRIS-REx) mission successfully launched on September 8th, 2016. During its rendezvous with near-Earth asteroid (101955) Bennu beginning in 2018, OSIRIS-REx will characterize the asteroid's physical, mineralogical, and chemical properties in an effort to globally map the properties of Bennu, a primitive carbonaceous asteroid, and choose a sampling location [e.g. 1]. In preparation for these observations, we spectrally characterized a suite of analog samples across visible, near- and thermal-infrared wavelengths and used these in initial tests of phase detection and abundance determination software algorithms. Here we present the thermal infrared laboratory measurements of the analog sample suite measured under asteroidlike conditions, which are relevant to the interpretation of spectroscopic observations by the OSIRIS-REx Thermal Emission Spectrometer (OTES) [2, 3]. This suite of laboratory measurements of asteroid analogs under asteroid-like conditions is the first of their kind.
NASA Astrophysics Data System (ADS)
Liu, Zhiyuan; Zhong, Mou; Sun, Yuhua; Chen, Junhong; Feng, Bo
2018-03-01
Titanium with hybrid microporous/nanotubes (TMNT) structure on its surface was fabricated by acid etching and subsequently anodization at different voltages. Bovine lactoferricin, a kind of antimicrobial peptide, and sodium alginate (NaAlg) were loaded onto titanium surface through layer by layer assembly. The drug release, cytocompatibility and antimicrobial property against S.aureus and E.coil were studied by release experiment, osteoblast and bacterial cultures. Results indicated that samples with nanotubes of bigger diameter carried more drugs and had better biocompatibility, and drug-loaded samples acquired better biocompatibility compared with drug-free samples. Furthermore, the drug-loaded samples exhibited good initial antimicrobial property, but weak long-term antimicrobial property. Therefore, drug-loaded titanium with micro/nano structure, especially, of big diameter nanotubes, could be a promise material for medical implants, such as internal/external fixation devices.
ERIC Educational Resources Information Center
Blanton, Linda P.; Boveda, Mildred; Munoz, Lorena R.; Pugach, Marleen C.
2017-01-01
Initial licensure polices in special education were examined to determine how these policies support or hinder reform efforts to develop teacher education programs that prepare graduates for the increasingly complex needs of diverse students. Initial special education licensure policies are described with an emphasis on the differences across…
Tablet Technology in Teacher Preparation: A Case Study--The Nook Initiative
ERIC Educational Resources Information Center
Jordan, Hope; Hunter, Elizabeth; Douglas, Maegan; Wighting, Mervyn
2015-01-01
Regent University's Special Education and Reading Specialist Programs introduced the Nook Initiative fall 2013. This paper discusses the implementation, the need for integrated tablet technology in teacher preparation, initial outcomes of the study, and offers suggestions for practice. A second tablet pilot program introducing the iPad mini in the…
Skucha-Nowak, Małgorzata
2015-01-01
The resin infiltration technique, a minimally invasive method, involves the saturation, strengthening, and stabilization of demineralized enamel by a mixture of polymer resins without the need to use rotary tools or the risk of losing healthy tooth structures. To design and synthesize an experimental infiltrant with potential bacteriostatic properties.To compare the depth of infiltration of the designed experimental preparation with the infiltrant available in the market using a scanning electron microscope. Composition of the experimental infiltrant was established after analysis of 1H NMR spectra of the commercially available compounds that can penetrate pores of demineralized enamel. As the infiltrant should have bacteriostatic features by definition, an addition of 1% of monomer containing metronidazole was made. Thirty extracted human teeth were soaked in an acidic solution, which was to provide appropriate conditions for demineralization of enamel. Afterward, each tooth was divided along the coronal-root axis into two zones. One zone had experimental preparation applied to it (the test group), while the other had commercially available Icon (the control group). The teeth were dissected along the long axis and described above underwent initial observation with use of a Hitachi S-4200 scanning electron microscope. It was found that all samples contained only oxygen and carbon, regardless of the concentration of additions introduced into them. The occurrence of carbon is partially because it is a component of the preparation in question and partially because of sputtering of the sample with it. Hydrogen is also a component of the preparation, as a result of its phase composition; however, it cannot be detected by the EDS method. SEM, in combination with X-ray microanalysis, does not allow one to explicitly assess the depth of penetration of infiltration preparations into enamel.In order to assess the depth of penetration of infiltration preparations with use of X-ray microanalysis, it is recommended to introduce a contrast agent that is approved for use in dental materials, such as ytterbium III fluoride.
Harmonisation of seven common enzyme results through EQA.
Weykamp, Cas; Franck, Paul; Gunnewiek, Jacqueline Klein; de Jonge, Robert; Kuypers, Aldy; van Loon, Douwe; Steigstra, Herman; Cobbaert, Christa
2014-11-01
Equivalent results between different laboratories enable optimal patient care and can be achieved with harmonisation. We report on EQA-initiated national harmonisation of seven enzymes using commutable samples. EQA samples were prepared from human serum spiked with human recombinant enzymes. Target values were assigned with the IFCC Reference Measurement Procedures. The same samples were included at four occasions in the EQA programmes of 2012 and 2013. Laboratories were encouraged to report IFCC traceable results. A parallel study was done to confirm commutability of the samples. Of the 223 participating laboratories, 95% reported IFCC traceable results, ranging from 98% (ASAT) to 87% (amylase). Users of Roche and Siemens (97%) more frequently reported in IFCC traceable results than users of Abbott (91%), Beckman (90%), and Olympus (87%). The success of harmonisation, expressed as the recovery of assigned values and the inter-laboratory CV was: ALAT (recovery 100%; inter-lab CV 4%), ASAT (102%; 4%), LD (98%; 3%), CK (101%; 5%), GGT (98%; 4%), AP (96%; 6%), amylase (99%; 4%). There were no significant differences between the manufacturers. Commutability was demonstrated in the parallel study. Equal results in the same sample in the 2012 and 2013 EQA programmes demonstrated stability of the samples. The EQA-initiated national harmonisation of seven enzymes, using stable, commutable human serum samples, spiked with human recombinant enzymes, and targeted with the IFCC Reference Measurement Procedures, was successful in terms of implementation of IFCC traceable results (95%), recovery of the target (99%), and inter-laboratory CV (4%).
Bansil, Pooja; Wittet, Scott; Lim, Jeanette L; Winkler, Jennifer L; Paul, Proma; Jeronimo, Jose
2014-06-12
Vaginal self-sampling with HPV-DNA tests is a promising primary screening method for cervical cancer. However, women's experiences, concerns and the acceptability of such tests in low-resource settings remain unknown. In India, Nicaragua, and Uganda, a mixed-method design was used to collect data from surveys (N = 3,863), qualitative interviews (N = 72; 20 providers and 52 women) and focus groups (N = 30 women) on women's and providers' experiences with self-sampling, women's opinions of sampling at home, and their future needs. Among surveyed women, 90% provided a self- collected sample. Of these, 75% reported it was easy, although 52% were initially concerned about hurting themselves and 24% were worried about not getting a good sample. Most surveyed women preferred self-sampling (78%). However it was not clear if they responded to the privacy of self-sampling or the convenience of avoiding a pelvic examination, or both. In follow-up interviews, most women reported that they didn't mind self-sampling, but many preferred to have a provider collect the vaginal sample. Most women also preferred clinic-based screening (as opposed to home-based self-sampling), because the sample could be collected by a provider, women could receive treatment if needed, and the clinic was sanitary and provided privacy. Self-sampling acceptability was higher when providers prepared women through education, allowed women to examine the collection brush, and were present during the self-collection process. Among survey respondents, aids that would facilitate self-sampling in the future were: staff help (53%), additional images in the illustrated instructions (31%), and a chance to practice beforehand with a doll/model (26%). Self-and vaginal-sampling are widely acceptable among women in low-resource settings. Providers have a unique opportunity to educate and prepare women for self-sampling and be flexible in accommodating women's preference for self-sampling.
Stability of amlodipine besylate in two liquid dosage forms.
Nahata, M C; Morosco, R S; Hipple, T F
1999-01-01
To determine the stability of amlodipine besylate in two liquid dosage forms under refrigeration and at room temperature. Commercially available amlodipine tablets (Norvasc-Pfizer) were used to prepare two suspensions: one in extemporaneously prepared 1% methylcellulose in syrup (1:1), and another in equal volumes of commercially available OraPlus/OraSweet. Each suspension containing amlodipine 1 mg/mL was stored in 10 plastic prescription bottles; 5 were stored at 4 degrees C and 5 at 25 degrees C. Samples were collected immediately after preparation (day 0) and on days 7, 14, 28, 42, 56, 70, and 91. Amlodipine concentration was measured by stability-indicating HPLC method (n = 15). Research laboratory at Children's Hospital. Physical and chemical stability (> 90% of the initial concentration) of amlodipine in the two extemporaneously prepared suspensions during storage in plastic prescription bottles at 4 degrees C and 25 degrees C. Observed mean concentrations exceeded 90% of the initial concentrations in both suspensions for 91 days at 4 degrees C and 56 days at 25 degrees C. No noticeable change in physical appearance or odor was observed; pH changed slightly in the methylcellulose-containing formulation stored at 25 degrees C. Amlodipine was stable in two suspensions when stored in plastic prescription bottles for 91 days at 4 degrees C or 56 days at 25 degrees C. These formulations may be considered for pediatric or elderly patients who are unable to swallow tablets. The liquid dosage form would also permit accurate administration of amlodipine doses to infants and young children based on their body weight.
Yang, Zhihong; Xie, Changsheng; Xia, Xianping; Cai, Shuizhou
2008-11-01
To decrease the side effects of the existing copper-bearing intrauterine devices, the zinc/low-density polyethylene (Zn/LDPE) nanocomposite and zinc-oxide/low-density polyethylene (ZnO/LDPE) nanocomposite have been developed in our research for intrauterine devices (IUDs). In this study, the influences of preparation methods of nanocomposites and particle sizes of zinc and zinc oxide on Zn(2+) release from composites incubated in simulated uterine solution were investigated. All release profiles are biphasic: an initial rapid release phase is followed by a near zero-order release period. Zn(2+) release rates of nanocomposites prepared by compressing moulding are higher than those of the nanocomposites prepared by hot-melt extrusing. Compared with Zn(2+) release from the microcomposites, the release profiles of the nanocomposites exhibit a sharp decrease in Zn(2+) release rate in the first 18 days, an early onset of the zero-order release period and a high release rate of Zn(2+) at the later stage. The microstructure of the Zn/LDPE sample and the ZnO/LDPE sample after being incubated for 200 days was characterized by SEM, XRD and EDX techniques. The results show that the dissolution depth of ZnO/LDPE nanocomposite is about 60 mum. Lots of pores were formed on the surface of the Zn/LDPE sample and ZnO/LDPE sample, indicating that these pores can provide channels for the dissolution of nanoparticles in the matrix. The undesirable deposits that are composed of ZnO are only detected on the surface of Zn/LDPE nanocomposite, which may increase the risk of side effects associated with IUDs. It can be expected that ZnO/LDPE nanocomposite is more suitable for IUDs than Zn/LDPE nanocomposite.
NASA Astrophysics Data System (ADS)
Nasser, Ramzi; Othmen, Walid Ben Haj; Elhouichet, Habib; Férid, Mokhtar
2017-01-01
In the present study, undoped and antimony (Sb) doped ZnO nanocrystals (NCs) were prepared by a simple and economical sol-gel method. X-ray diffraction (XRD) and transmission electron microscopy (TEM) revealed the purity of the obtained phase and its high crystallinity. Raman analysis confirms the hexagonal Wurtzite ZnO structure. According to the diffuse reflectance results, the band gap was found to decrease up to 3% of Sb doping (ZSb3 sample). The results of X-ray photoelectron spectroscopy (XPS) measurements reveal that Sb ions occupied both Zn and interstitials sites. The successful substitution of antimony in ZnO lattice suggests the formation of the complex (SbZn-2 VZn) acceptor level above the valence band. Particularly for ZSb3 sample, the UV photoluminescence (PL) band presents an obvious red-shift attributed to the formation of this complex. Rhodamine B (RhB) was used to evaluate the photocatalytic activity of Sb-doped ZnO NCs under sunlight irradiation. It was found that oxygen vacancies play a major role in the photocatalytic process by trapping the excited electrons and inhibiting the radiative recombination. During the photocatalytic mechanism, the Sb doping, expressed through the apparition of the (SbZn-2 VZn) correspondent acceptor level, enhances the sunlight absorption within the ZnO band gap, which stimulates the generation of hydroxyl radicals and promotes the photocatalytics reaction rates. Such important contribution of the hydroxyl radicals was confirmed experimentally when using ethanol as scavenger in the photocatalytic reaction. The photodegradation experiments reveal that ZSb3 sample exhibits the highest photocatalytic activity among all the prepared samples and presents a good cycling stability and reusability. The influence of the initial pH in the photodegradation efficiency was also monitored and discussed.
Total morphine stability in urine specimens stored under various conditions.
Chang, B L; Huang, M K; Tsai, Y Y
2000-09-01
The stability of total morphine in urine stored under various conditions was studied using control and experimental specimens. Samples in the control group were prepared using drug-free urine spiked with morphine at three concentration levels (300, 1000, and 2500 ng/mL), each with the pH adjusted to 5.5, 6.5, and 7.5. Samples in the experimental group came from 20 alleged heroin addicts (provided by Taipei Municipal Psychiatric Hospital). Samples in both groups were divided into two categories--one with and one without the precipitate (formed at 0 degrees C) removed. Samples in each of these two categories were further divided into two sub-groups--one with and one without sodium azide (0.05%) added. Total morphine contents in these samples were first determined by gas chromatography-mass spectrometry prior to storage and at 6, 12, 18, and 24 months following storage at -20, 4, 25, and 35 degrees C. Effects of sample treatment (azide addition and precipitate removal), pH, and storage temperature and length were evaluated by examining the percentage of total morphine remaining at the four time intervals following the initial determination. Major findings were as follows: (1) total morphine decomposition was minimal when stored for 12 months at -20 degrees C, which is a common current practice; (2) samples with lower initial sample pH had slower total morphine decomposition rates; and (3) azide addition appeared to have no detectable effect, whereas precipitate removal appeared to marginally reduce the decomposition rate, especially for samples with lower pH.
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.
Atsukawa, Yoshiko; Kawakami, Sayoko; Asahara, Miwa; Ishigaki, Shinobu; Tanaka, Takashi; Ono, Yasuo; Nishiya, Hajime; Fujisaki, Ryuichi; Koga, Ichiro; Ota, Yasuo; Miyazawa, Yukihisa
2011-08-01
Gram staining is a useful technique for detecting bacteria but is highly questionable in detecting Mycobacterium tuberculosis. Its detection generally requires special staining, such as Ziehl-Neelsen staining. We experienced three cases in which tuberculosis was first suggested by Gram staining of sputum or pus, confirmed by Ziehl-Neelsen staining, and diagnosed by polymerase chain reaction or culture. To find colorless tubercle bacilli in clinical samples with various organisms, varying the focus to slightly longer and shorter during study of the slides is indispensable. We present criteria for detecting infective pulmonary tuberculosis in Gram staining. First, in the ordinary focus, weakly stained, thin, gram-positive bacilli are found; second, with a slightly longer focus distance, the thin, cord-like, conspicuous gram-positive bacilli can be observed; and third, with a shorter focus distance, the gram-positive bacilli have changed into the brightened, colorless, or ghost ones. Four laboratory technologists each evaluated 20 Gram-stained samples after being lectured on the criteria, with no prior information about the sample. They accurately evaluated the presence of the bacilli in Gram-stained preparations in more than 90% of samples containing 3+ bacilli on Ziehl-Neelsen staining. Gram staining is available as an easy and rapid initial clue to recognize highly infective tuberculosis.
Braze Development of Graphite Fiber for Use in Phase Change Material Heat Sinks
NASA Technical Reports Server (NTRS)
Quinn, Gregory; Beringer, Woody; Gleason, Brian; Stephan, Ryan
2011-01-01
Hamilton Sundstrand (HS), together with NASA Johnson Space Center, developed methods to metallurgically join graphite fiber to aluminum. The goal of the effort was to demonstrate improved thermal conductance, tensile strength and manufacturability compared to existing epoxy bonded techniques. These improvements have the potential to increase the performance and robustness of phase change material heat sinks that use graphite fibers as an interstitial material. Initial work focused on evaluating joining techniques from four suppliers, each consisting of a metallization step followed by brazing or soldering of one inch square blocks of Fibercore graphite fiber material to aluminum end sheets. Results matched the strength and thermal conductance of the epoxy bonded control samples, so two suppliers were down-selected for a second round of braze development. The second round of braze samples had up to a 300% increase in strength and up to a 132% increase in thermal conductance over the bonded samples. However, scalability and repeatability proved to be significant hurdles with the metallization approach. An alternative approach was pursued which used a nickel braze allow to prepare the carbon fibers for joining with aluminum. Initial results on sample blocks indicate that this approach should be repeatable and scalable with good strength and thermal conductance when compared with epoxy bonding.
Standardized Sample Preparation Using a Drop-on-Demand Printing Platform
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
Kirkham, Kylian; Munson, Jessica M; McCluskey, Susan V; Graner, Kevin K
2017-01-01
The stability of dalteparin 1,000 units/mL in 0.9% sodium chloride for injection stored in polypropylene syringes under refrigeration was examined. Dalteparin 1,000-units/mL syringes were prepared by adding 9 mL of 0.9% sodium chloride for injection to 1 mL of dalteparin sodium 10,000 unit/mL from commercial single-use syringes. Compounded solutions in 0.5-mL aliquots were transferred to 1-mL polypropylene syringes and sealed with a Luer lock tip cap and stored at refrigerated temperatures (2°C to 8°C) with ambient fluorescent light exposure. Syringes from three batches of dalteparin 1,000 units/mL were potency tested in duplicate by a stability-indicating high-performance liquid chromatography assay using a 0.5-mL sample at specified intervals. Visual and pH testing were performed on each batch. Samples were visually inspected for container integrity, color, and clarity. Samples for pH testing were prepared using a 1:1 dilution of dalteparin 1,000 units/mL in sterile water for injection and underwent duplicate analysis at each time point. High-performance liquid chromatography analyses showed a remaining percent of the initial dalteparin content at day 30 of 94.88% ± 2.11%. Samples remained colorless and clear with no signs of container compromise and no visual particulate matter at each time point. Throughout the 30-day study period, pH values remained within 0.3-pH units from the initial value of 5.84. Dalteparin 1,000 unit/mL in 0.9% sodium chloride for injection, packaged in 1-mL polypropylene syringes was stable for at least 30 days while stored at refrigerated conditions with ambient fluorescent light exposure. Copyright© by International Journal of Pharmaceutical Compounding, Inc.
NASA Astrophysics Data System (ADS)
Tarasov, Konstantin; Beaunier, Patricia; Che, Michel; Marceau, Eric; Li, Yanling
2011-05-01
Following procedures formerly developed for the preparation of supported heterogeneous catalysts, carbon-coated cobalt nanoparticles dispersed on porous alumina have been prepared by impregnation of γ-Al2O3 with (NH4)2[Co(EDTA)] and thermal decomposition in inert atmosphere. Below 350 °C, Co(II) ions are complexed in a hexa-coordinated way by the EDTA ligand. The thermal treatment at 400-900 °C leads to the EDTA ligand decomposition and recovering of the support porosity, initially clogged by the impregnated salt. According to X-ray absorption spectroscopy, and due to in situ redox reactions between the organic ligand and Co(II), both oxidic and metallic cobalt phases are formed. Characterisation by transmission electron microscopy, X-ray diffraction and magnetic measurements reveals that an increase in the treatment temperature leads to an increase of the degree of cobalt reduction as well as to a growth of the cobalt metal particles. As a consequence, the samples prepared at 400-700 °C exhibit superparamagnetism and a saturation magnetisation of 1.7-6.5 emu g-1 at room temperature, whilst the sample prepared at 900 °C has a weak coercivity (0.1 kOe) and a saturation magnetisation of 12 emu g-1. Metal particles are homogeneously dispersed on the support and appear to be protected by carbon; its elimination by a heating in H2 at 400 °C is demonstrated to cause sintering of the metal particles. The route investigated here can be of interest for obtaining porous magnetic adsorbents or carriers with high magnetic moments and low coercivities, in which the magnetic nanoparticles are protected from chemical aggression and sintering by their coating.
Del Mar, P.
1993-12-28
A process is presented of sample preparation prior to analysis for the concentration of an organic contaminant in an aqueous medium by (a) passing an initial aqueous medium including a minor amount of the organic contaminant through a composite tube comprised of a blend of a polyolefin and a polyester, the composite tube having an internal diameter of from about 0.1 to about 2.0 millimeters and being of sufficient length to permit the organic contaminant to adhere to the composite tube, (b) passing a solvent through the composite tube. The solvent is capable of separating the adhered organic contaminant from the composite tube. Further, an extraction apparatus is presented for sample preparation prior to analysis for the concentration of an organic contaminant in an aqueous medium. The apparatus includes a composite tube comprised of a blend of a polyolefin and a polyester. The composite tube has an internal diameter of from about 0.1 to about 2.0 millimeters and has sufficient length to permit an organic contaminant contained within an aqueous medium passed therethrough to adhere to the composite tube. 2 figures.
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.
Raisingani, Deepak; Mathur, Rachit; Madan, Nidha; Visnoi, Suchita
2016-01-01
Aim To evaluate the incidence of apical crack initiation during canal preparation with stainless steel K-files and hand protaper files (in vitro study). Materials and methods Sixty extracted mandibular premo-lar teeth are randomly selected and embedded in an acrylic tube filled with autopolymerizing resin. A baseline image of the apical surface of each specimen was recorded under a digital microscope (80×). The cervical and middle thirds of all samples were flared with #2 and #1 Gates-Glidden (GG) drills, and a second image was recorded. The teeth were randomly divided into four groups of 15 teeth each according to the file type (hand K-file and hand-protaper) and working length (WL) (instrumented at WL and 1 mm less than WL). Final image after dye penetration and photomicrograph of the apical root surface were digitally recorded. Results Maximum numbers of cracks were observed with hand protaper files compared with hand K-file at the WL and 1 mm short of WL. Chi-square testing revealed a highly significant effect of WL on crack formation at WL and 1 mm short of WL (p = 0.000). Conclusion Minimum numbers of cracks at WL and 1 mm short of WL were observed with hand K-file and maximum with hand protaper files. How to cite this article Soni D, Raisingani D, Mathur R, Madan N, Visnoi S. Incidence of Apical Crack Initiation during Canal Preparation using Hand Stainless Steel (K-File) and Hand NiTi (Protaper) Files. Int J Clin Pediatr Dent 2016;9(4):303-307. PMID:28127160
Blackwood, Kym S; Burdz, Tamara V; Turenne, Christine Y; Sharma, Meenu K; Kabani, Amin M; Wolfe, Joyce N
2005-01-01
Background In the field of clinical mycobacteriology, Mycobacterium tuberculosis (MTB) can be a difficult organism to manipulate due to the restrictive environment of a containment level 3 (CL3) laboratory. Tests for rapid diagnostic work involving smears and molecular methods do not require CL3 practices after the organism has been rendered non-viable. While it has been assumed that after organism deactivation these techniques can be performed outside of a CL3, no conclusive study has consistently confirmed that the organisms are noninfectious after the theoretical 'deactivation' steps. Previous studies have shown that initial steps (such as heating /chemical fixation) may not consistently kill MTB organisms. Methods An inclusive viability study (n = 226) was undertaken to determine at which point handling of culture extraction materials does not necessitate a CL3 environment. Four different laboratory protocols tested for viability included: standard DNA extractions for IS6110 fingerprinting, crude DNA preparations for PCR by boiling and mechanical lysis, protein extractions, and smear preparations. For each protocol, laboratory staff planted a proportion of the resulting material to Bactec 12B medium that was observed for growth for 8 weeks. Results Of the 208 isolates initially tested, 21 samples grew within the 8-week period. Sixteen (7.7%) of these yielded positive results for MTB that included samples of: deactivated culture resuspensions exposed to 80°C for 20 minutes, smear preparations and protein extractions. Test procedures were consequently modified and tested again (n = 18), resulting in 0% viability. Conclusions This study demonstrates that it cannot be assumed that conventional practices (i.e. smear preparation) or extraction techniques render the organism non-viable. All methodologies, new and existing, should be examined by individual laboratories to validate the safe removal of material derived from MTB to the outside of a CL3 laboratory. This process is vital to establish in house biosafety-validated practices with the aim of protecting laboratory workers conducting these procedures. PMID:15667662
2013-01-01
Background The etiology of fibromyalgia and chronic fatigue syndrome (FM/CFS) is currently unknown. A recurrent viral infection is an attractive hypothesis repeatedly found in the literature since it would explain the persistent pain and tiredness these patients suffer from. The initial striking link of two distinct orphan retroviruses: the gamma retroviruses murine leukemia virus (MLV)-related virus and the delta retrovirus T-lymphotropic virus type 2 (HTLV-2) to chronic fatigue have not been confirmed to date. Results Genomic DNA (gDNA) from 75 fibromyalgia patients suffering from chronic fatigue and 79 age-matched local healthy controls were screened for the presence of MLV-related and HTLV-2 related proviral sequences. The XMRV env gene was amplified in 20% of samples tested (24% patients/15% healthy controls). Unexpectedly, no PCR amplifications from independent gDNA preparations of the same individuals were obtained. None of the positive samples showed presence of contaminating murine sequences previously reported by other investigators, neither contained additional regions of the virus making us conclude that the initial env amplification came from spurious air-driven amplicon contaminants. No specific HTLV-2 sequences were obtained at any time from any of the 154 quality-controlled gDNA preparations screened. Conclusions Previous associations between MLV-related or HTLV-2 retrovirus infection with chronic fatigue must be discarded. Thus, studies showing positive amplification of HTLV-2 sequences from chronic fatigue participants should be revised for possible undetected technical problems. To avoid false positives of viral infection, not only extreme precautions should be taken when nested-PCR reactions are prepared and exhaustive foreign DNA contamination controls performed, but also consistent amplification of diverse regions of the virus in independent preparations from the same individual must be demanded. The fact that our cohort of patients did not present evidence of any of the two types of retroviral infection formerly associated to chronic fatigue does not rule out the possibility that other viruses are involved in inciting or maintaining fibromyalgia and/or chronic fatigue conditions. PMID:24216038
Experimental Study of Factors Affecting Soil Erodibility
NASA Astrophysics Data System (ADS)
Larionov, G. A.; Bushueva, O. G.; Gorobets, A. V.; Dobrovolskaya, N. G.; Kiryukhina, Z. P.; Krasnov, S. F.; Litvin, L. F.; Maksimova, I. A.; Sudnitsyn, I. I.
2018-03-01
The effect of different factors and preparation conditions of monofraction samples from the arable horizon of leached chernozem on soil erodibility and its relationship with soil tensile strength (STS) has been studied. The exposure of samples at 38°C reduces their erodibility by two orders of magnitude. The drying of samples, on the contrary, increases their erodibility. It has been shown that erodibility decreases during the experiment. It has been found that the inoculation of soil with yeast cultures ( Naganishia albida, Lipomyces tetrasporus) reliably increases the STS value in 1.5-1.9 times. The sterile soil is eroded more intensively than the unsterile soil: at 4.9 and 0.3 g/(m2 s), respectively. The drying of soil followed by wetting to the initial water content (30%) has no significant effect on the STS value in almost all experimental treatments.
Lack of latex allergen contamination of solutions withdrawn from vials with natural rubber stoppers.
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 preparation and bioanalysis in mass spectrometry].
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.
Sabino, Bruno Duarte; Torraca, Tathiana Guilliod; Moura, Claudia Melo; Rozenbaum, Hannah Felicia; de Castro Faria, Mauro Velho
2010-05-01
Foods contaminated with a granulated material similar to Temik (a commercial pesticide formulation containing the carbamate insecticide aldicarb) are often involved in accidental ingestion, suicides, and homicides in Brazil. We developed a simple technique to detect aldicarb. This technique is based on the inhibition of a stable preparation of the enzyme acetylcholinesterase, and it is specially adapted for forensic purposes. It comprises an initial extraction step with the solvent methylene chloride followed by a colorimetric acetylcholinesterase assay. We propose that results of testing contaminated forensic samples be expressed in aldicarb equivalents because, even though all other carbamates are also potent enzyme inhibitors, aldicarb is the contaminant most frequently found in forensic samples. This method is rapid (several samples can be run in a period of 2 h) and low cost. This method also proved to be precise and accurate, detecting concentrations as low as 40 microg/kg of aldicarb in meat samples.
Estimated content percentages of volatile liquids and fat extractables in ready-to-eat foods.
Daft, J L; Cline, J K; Palmer, R E; Sisk, R L; Griffitt, K R
1996-01-01
Content percentages of volatile liquids and fat extractables in 340 samples of ready-to-eat foods were determined gravimetrically. Volatile liquids were determined by drying samples in a microwave oven with a self-contained balance; results were printed out automatically. Fat extractables were extracted from the samples with mixed ethers; extracts were dried and weighed manually. The samples, 191 nonfat and 149 fatty (containing ca 2% or more fat) foods, represent about 5000 different food items and include infant and toddler, ethnic, fast, and imported items. Samples were initially prepared for screening of essential and toxic elements and chemical contamination by chopping and mixing into homogenous composites. Content determinations were then made on separate portions from each composite. Content results were put into a database for evaluation. Overall, mean results from both determinations agree with published data for moisture and fat contents of similar food items. Coefficients of variation, however, were lower for determination of volatile liquids than for that of fat extractables.
Rapley, Pat; Davidson, Laura; Nathan, Pauline; Dhaliwal, Satvinder S
2008-01-01
There is a shortage of registered nurses (RN) globally and equally in rural areas of Australia. The sparsely populated areas of rural Australia prompted the development of an external-mode EN-to-RN pathway course for enrolled nurses (EN) who want to complete a nursing degree. However, the awarding of advanced standing for EN clinical experience, regardless of educational background, is a new initiative that needs to be evaluated. Hence, this paper reports on the link between initial EN educational preparation and its impact on course completion. This exploratory correlation study used existing course data from four cohorts between 2000 and 2003. The comparisons included educational background, years of experience, and location of the EN-to-RN students. Significant differences were not found between rural and metropolitan students who completed or who withdrew from the course. Logistic regression analysis indicated that ENs in this sample with a hospital-based certificate rather than a technical college qualification were more likely to complete the course: Location and years of experience as an EN did not contribute significantly to course completion. The findings provide support for the same recognition of prior learning, regardless of educational background, for ENs entering a bachelor level nursing degree. The findings have relevance for Australia and other countries with similar challenges for ENs who want to become RNs without relocating to a city.
Hor, M M; Chan, S Y; Yow, K L; Lim, L Y; Chan, E
1997-01-01
To study the stability of admixtures of pethidine and metoclopramide in aqueous solution, 0.9% sodium chloride and 5% dextrose preparations. Aqueous mixtures of 1 ml of 50 mg/ml pethidine with 2ml of 5 mg/ml metoclopramide were prepared in plastic syringes, while the 0.9% sodium chloride and 5% dextrose admixtures, each containing 7.35 mg/ml of pethidine and 0.15 mg/ml of metoclopramide, were prepared in infusion bags. The preparations were stored under light and dark conditions at 32 degrees C for 48 h. Samples were collected at 0, 0.5, 1, 2, 4, 6, 8, 24, 32 and 48 h. A high-performance liquid chromatographic method was developed to separate and quantify both drugs. All preparations were found to be physically and chemically stable for at least 48h, as concentration changes were within 10% of their initial level, with no development of haze, precipitate or colour. Light appeared to have a negligible effect. Although pH changes were observed, they were inconsistent and were within the ranges in which the drugs are expected to remain stable. Pethidine and metoclopramide admixtures can, therefore, on stability grounds be used for the concomitant management of pain, nausea and vomiting.
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.
Rahman, Siti Khadijah Ab.; Yusof, Nor Azah; Abdullah, Abdul Halim; Idris, Azni; Al-lohedan, Hamad A.
2018-01-01
In the present study, ion imprinted polymer monoliths (IIPMs) were developed to overcome the limitations of ion imprinted polymer particles (IIPPs) used for the removal of Hg(II) ions from waste water samples. The adsorbents preparation, characterization and Hg(II) removal were very well reported. The IIPMs on porogen optimization was prepared using the molding technique with Hg(II) as a template ion, [2-(methacryloyloxy)ethyl]trimethylammonium cysteine (MAETC) as ligand, methacrylic acid (MAA) as functional monomer, ethylene glycol dimethacrylamide (EGDMA) as cross-linker, benzoyl peroxide as an initiator and methanol and acetonitrile as porogen in the polypropylene tube (drinking straw) as mold. The IIPMs prepared with higher volumes of porogen were indicated to have a good adsorption rate for the Hg(II) removal along with good water permeability and larger porosity as compared to a lower volume of porogen. The IIPMs prepared using the binary porogen were able to improve the porosity and surface area of the monolithic polymers as compared to the single porogen added IIPMs. Finally, we indicate from our analysis that the IIPM having the efficient capacity for the Hg(II) ions is easy to prepare, and has higher water permeability along with high porosity and high adsorption capacity and all these factors making it one of the suitable adsorbent for the successful removal of Hg(II) ions. PMID:29649325
Synthesis and Electrochemical Properties of LiFePO4/C for Lithium Ion Batteries.
Gao, Hong; Wang, Jiazhao; Yin, Shengyu; Zheng, Hao; Wang, Shengfu; Feng, Chuanqi; Wang, Shiquan
2015-03-01
LiFePO4/C was prepared through a facile rheological phase reaction method by using Fe3(PO4)2, Li3PO4 · 8H2O, and glucose as reactants. The LiFePO4/C samples were characterized by X-ray diffraction, scanning electron microscopy, and thermogravimetric analysis. The electrochemical properties of the samples were investigated. The results show that the LiFePO4/C samples have single-phase olivine-type structure, and their particles feature a spherical shape. The carbon coating on the particles of LiFePO4 is about 1.8% of the LiFePO4/C by weight. The particle size was distributed from 0.2 to 1 µm. The initial discharge capacity of LiFePO4/C reached 154 mA h/g at 0.1 C. The retained discharge capacity of LiFePO4/C was 152.9 mA h g(-1) after 50 cycles. The LiFePO4/C also showed better cycling performance than that of the bare LiPeO4 at a higher charge/discharge rate (1 C). The LIFePO4/C prepared in this way could be a promising cathode material for lithium ion battery application.
Clarke, B; Carroll, W; Rochev, Y; Hynes, M; Bradley, D; Plumley, D
2006-10-01
Medical implants and devices are now used successfully in surgical procedures on a daily basis. Alloys of nickel and titanium, and in particular Nitinol are of special interest in the medical device industry, because of their shape memory and superelastic properties. The corrosion behavior of nitinol in the body is also of critical importance because of the known toxicological effects of nickel. The stability of a NiTi alloy in the physiological environment is dependant primarily on the properties of the mostly TiO(2) oxide layer that is present on the surface. For the present study, a range of nitinol wires have been prepared using different drawing processes and a range of surface preparation procedures. It is clear from the results obtained that the wire samples with very thick oxides also contain a high nickel content in the oxide layer. The untreated samples with the thicker oxides show the lowest pitting potential values and greater nickel release in both long and short-term experiments. It was also found that after long-term immersion tests breakdown potentials increased for samples that exhibited lower values initially. From these results it would appear that surface treatment is essential for the optimum bioperformance of nitinol. (c) 2006 Wiley Periodicals, Inc
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.
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.
Clinically relevant advances in on-chip affinity-based electrophoresis and electrochromatography.
Hou, Chenlu; Herr, Amy E
2008-08-01
Clinical and point-of-care disease diagnostics promise to play an important role in personalized medicine, new approaches to global health, and health monitoring. Emerging instrument platforms based on lab-on-a-chip technology can confer performance advantages successfully exploited in electrophoresis and electrochromatography to affinity-based electrokinetic separations. This review surveys lab-on-a-chip diagnostic developments in affinity-based electrokinetic separations for quantitation of proteins, integration of preparatory functions needed for subsequent analysis of diverse biological samples, and initial forays into multiplexed analyses. The technologies detailed here underpin new clinical and point-of-care diagnostic strategies. The techniques and devices promise to advance translation of until now laboratory-based sample preparation and analytical assays to near-patient settings.
Hodnik, Nejc; Jeyabharathi, Chinnaiah; Meier, Josef C; Kostka, Alexander; Phani, Kanala L; Rečnik, Aleksander; Bele, Marjan; Hočevar, Stanko; Gaberšček, Miran; Mayrhofer, Karl J J
2014-07-21
In this study the performance enhancement effect of structural ordering for the oxygen reduction reaction (ORR) is systematically studied. Two samples of PtCu3 nanoparticles embedded on a graphitic carbon support are carefully prepared with identical initial composition, particle dispersion and size distribution, yet with different degrees of structural ordering. Thus we can eliminate all coinciding effects and unambiguously relate the improved activity of the ORR and more importantly the enhanced stability to the ordered nanostructure. Interestingly, the electrochemically induced morphological changes are common to both ordered and disordered samples. The observed effect could have a groundbreaking impact on the future directions in the rational design of active and stable platinum alloyed ORR catalysts.
Hot Spots from Generated Defects in HMX Crystals
NASA Astrophysics Data System (ADS)
Sorensen, Christian; Cummock, Nicholas; O'Grady, Caitlin; Gunduz, I. Emre; Son, Steven
2017-06-01
There are several hot spot initiation mechanisms that have been proposed. However, direct observation of shock or impact compression of these mechanisms at macroscopic scale in explosives is difficult. Phase contrast imaging (PCI) may be applied to these systems. Here, high-speed video was used to record optical spectrum and for x-ray Phase Contrast Imaging (PCI) of shockwave interaction with low defect HMX crystals and crystals with engineered defects. Additionally, multiple crystals were arranged and observed under shock loading with PCI and optical high-speed video. Sample preparation techniques for generating voids and other engineered defects will be discussed. These methods include drilled holes and laser machined samples. Insight into hot spot mechanisms was obtained. Funding from ONR's PC@Xtreme MURI.
NASA Technical Reports Server (NTRS)
Lee, S. S.; Sengupta, S.
1978-01-01
A mathematical model package for thermal pollution analyses and prediction is presented. These models, intended as user's manuals, are three dimensional and time dependent using the primitive equation approach. Although they have sufficient generality for application at sites with diverse topographical features; they also present specific instructions regarding data preparation for program execution and sample problems. The mathematical formulation of these models is presented including assumptions, approximations, governing equations, boundary and initial conditions, numerical method of solution, and same results.
1974-02-01
least one of the board members shall be a certified boiler inspector. c. Each board will be a permanently established examining board reporting to the...Initial Light-Off Examination - to be conducted prior to lighting the first fire in any boiler during a regular overhaul, major conversion, or fitting... boiler water and feed water sampling and analysis and casualty control walk-thru drills may be conducted at the discretion of the senior member (or his
Infrared Extinction and the Initial Conditions for Star and Planet Formation
NASA Technical Reports Server (NTRS)
Lada, Charles J.
2004-01-01
This grant funds a research program to use infrared extinction measurements to probe the detailed structure of dark molecular clouds and investigate the physical conditions which give rise to star and planet formation. The goals of the this program are to: 1) acquire deep infrared and molecular-line observations of a carefully selected sample of nearby dark clouds, 2) reduce and analyze the data obtained in order to produce detailed extinction maps of the clouds, 3) prepare results, where appropriate, for publication. A description of how these goals were met are included.
NASA Astrophysics Data System (ADS)
Zhang, Yaoyao; Li, Mengyao; Guo, Yinli
2018-01-01
A series of Ag-doped TiO2 powder photocatalysts were prepared by the sol-gel method. The phase structure and morphology of the samples were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The persistent organic pollutant sodium pentachlorophenol ate (PCP-Na) was selected as the target pollutant, and the photocatalytic property of the material Ag/TiO2 was evaluated by PCP-Na degradation rate. It was found that the calcination at 450 °C was conducive to form the anatase structure with high catalytic activity, and the catalytic activity was higher when the silver mole fraction of Ag/TiO2 was 0.50%. The influence of Ag/TiO2 dosage, hydrogen peroxide volume, silver mole fraction and PCP-Na initial concentration was investigated by the single factor experiment.
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.
MARS: bringing the automation of small-molecule bioanalytical sample preparations to a new frontier.
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.
Centrifugal Pump Effect on Average Particle Diameter of Oil-Water Emulsion
NASA Astrophysics Data System (ADS)
Morozova, A.; Eskin, A.
2017-11-01
In this paper we review the process of oil-water emulsion particles fragmentation in a turbulent flow created by a centrifugal pump. We examined the influence of time necessary for oil-water emulsion preparation on the particle size of oil products and the dependence of a centrifugal pump emulsifying capacity on the initial emulsion dispersion. The investigated emulsion contained the brand fuel oil M-100 and tap water; it was sprayed with a nozzle in a gas-water flare. After preparation of the emulsion, the centrifugal pump was turned on and the emulsion samples were taken before and after the pump passing in 15, 30 and 45 minutes of spraying. To determine the effect the centrifugal pump has on the dispersion of the oil-water emulsion, the mean particle diameter of the emulsion particles was determined by the optical and microscopic method before and after the pump passing. A dispersion analysis of the particles contained in the emulsion was carried out by a laser diffraction analyzer. By analyzing the pictures of the emulsion samples, it was determined that after the centrifugal pump operation a particle size of oil products decreases. This result is also confirmed by the distribution of the obtained analyzer where the content of fine particles with a diameter less than 10 μm increased from 12% to 23%. In case of increasing emulsion preparation time, a particle size of petroleum products also decreases.
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.
System for autonomous monitoring of bioagents
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.
Comparison of Crack Initiation, Propagation and Coalescence Behavior of Concrete and Rock Materials
NASA Astrophysics Data System (ADS)
Zengin, Enes; Abiddin Erguler, Zeynal
2017-04-01
There are many previously studies carried out to identify crack initiation, propagation and coalescence behavior of different type of rocks. Most of these studies aimed to understand and predict the probable instabilities on different engineering structures such as mining galleries or tunnels. For this purpose, in these studies relatively smaller natural rock and synthetic rock-like models were prepared and then the required laboratory tests were performed to obtain their strength parameters. By using results provided from these models, researchers predicted the rock mass behavior under different conditions. However, in the most of these studies, rock materials and models were considered as contains none or very few discontinuities and structural flaws. It is well known that rock masses naturally are extremely complex with respect to their discontinuities conditions and thus it is sometimes very difficult to understand and model their physical and mechanical behavior. In addition, some vuggy rock materials such as basalts and limestones also contain voids and gaps having various geometric properties. Providing that the failure behavior of these type of rocks controlled by the crack initiation, propagation and coalescence formed from their natural voids and gaps, the effect of these voids and gaps over failure behavior of rocks should be investigated. Intact rocks are generally preferred due to relatively easy side of their homogeneous characteristics in numerical modelling phases. However, it is very hard to extract intact samples from vuggy rocks because of their complex pore sizes and distributions. In this study, the feasibility of concrete samples to model and mimic the failure behavior vuggy rocks was investigated. For this purpose, concrete samples were prepared at a mixture of %65 cement dust and %35 water and their physical and mechanical properties were determined by laboratory experiments. The obtained physical and mechanical properties were used to constitute numerical models, and then uniaxial compressive strength (UCS) tests were performed on these models by using a commercial software called as Particle Flow Code (PFC2D). When the crack behavior of concrete samples obtained from both laboratory tests and numerical models are compared with the results of previous studies, a significant similarity was found. As a result, due to the observed similarity crack behavior between concretes and rocks, it can be concluded that intact concrete samples can be used for modelling purposes to understand the effect of voids and gaps on failure characteristics of vuggy rocks.
Sample Preparation for Mass Spectrometry Imaging of Plant Tissues: A Review
Dong, Yonghui; Li, Bin; Malitsky, Sergey; Rogachev, Ilana; Aharoni, Asaph; Kaftan, Filip; Svatoš, Aleš; Franceschi, Pietro
2016-01-01
Mass spectrometry imaging (MSI) is a mass spectrometry based molecular ion imaging technique. It provides the means for ascertaining the spatial distribution of a large variety of analytes directly on tissue sample surfaces without any labeling or staining agents. These advantages make it an attractive molecular histology tool in medical, pharmaceutical, and biological research. Likewise, MSI has started gaining popularity in plant sciences; yet, information regarding sample preparation methods for plant tissues is still limited. Sample preparation is a crucial step that is directly associated with the quality and authenticity of the imaging results, it therefore demands in-depth studies based on the characteristics of plant samples. In this review, a sample preparation pipeline is discussed in detail and illustrated through selected practical examples. In particular, special concerns regarding sample preparation for plant imaging are critically evaluated. Finally, the applications of MSI techniques in plants are reviewed according to different classes of plant metabolites. PMID:26904042
[Comparison of the Conventional Centrifuged and Filtrated Preparations in Urine Cytology].
Sekita, Nobuyuki; Shimosakai, Hirofumi; Nishikawa, Rika; Sato, Hiroaki; Kouno, Hiroyoshi; Fujimura, Masaaki; Mikami, Kazuo
2016-03-01
The urine cytology test is one of the most important tools for the diagnosis of malignant urinary tract tumors. This test is also of great value for predicting malignancy. However, the sensitivity of this test is not high enough to screen for malignant cells. In our laboratory, we were able to attain a high sensitivity of urine cytology tests after changing the preparation method of urine samples. The differences in the cytodiagnosis between the two methods are discussed here. From January 2012 to June 2013, 2,031 urine samples were prepared using the conventional centrifuge method (C method) ; and from September 2013 to March 2015, 2,453 urine samples were prepared using the filtration method (F method) for the cytology test. When the samples included in category 4 or 5, were defined as cytological positive, the sensitivities of this test with samples prepared using the F method were significantly high compared with samples prepared using the C method (72% vs 28%, p<0.001). The number of cells on the glass slides prepared by the F method was significantly higher than that of the samples prepared by the C method (p<0.001). After introduction of the F method, the number of f alse negative cases was decreased in the urine cytology test because a larger number of cells was seen and easily detected as atypical or malignant epithelial cells. Therefore, this method has a higher sensitivity than the conventional C method as the sensitivity of urine cytology tests relies partially on the number of cells visualized in the prepared samples.
Minimizing Segregation during the Controlled Directional Solidification of Dendric Alloys
NASA Technical Reports Server (NTRS)
Grugel, Richard N.; Fedoseyev, Alex; Kim, Shin-Woo
2003-01-01
Gravity-driven convection induced in the liquid by density gradients of temperature or composition disrupts uniform dendritic growth during controlled directional solidification and promotes severe macrosegregation. The solute-rich region about the dendrite tip appears to play a pivotal role in channel initiation. Allen and Hunt referred to this region as an "initial transient" or dynamic region constituting steep concentration gradients. Experimental investigation also point to the role the tip region plays in developing microstructure. Hellawell and co-workers showed that flow-through dendritic channels could be effectively disrupted, and segregation minimized, during the gradient freezing of bulk castings by rotating the melt through a slight angle with respect to Earth's gravity vector. Adapting this principle to controlled directional solidification, it has been shown" that segregation in dendritic alloys can be minimized, and properties improved, by processing the sample near horizontal in conjunction with a slow axial rotation of the crucible. It is postulated that the observed microstructural uniformity arises by maintaining the developing solute field about the dendrite tip. Solute rejected during vertical directional solidification will rise or sink parallel to the primary dendrite arms during axial rotation setting the stage for accumulation, instabilities, and segregation. In contrast, during horizontal growth, the rejected solute will sink or rise perpendicular to the primary dendrite. Now, in the presence of a slight axial rotation, solute that was initially sinking (or rising) will find itself above (or below) its parent dendrite, i.e., still about the tip region. The following is intended to experimentally demonstrate the viability of this concept in coordination with a model that gives predictive insight regarding solute distribution about growing dendrites. Alloys based on the lead-tin eutectic system were used in this study. The system is well characterized, the constituent metals are available in a very pure form, and the thermophysical properties are well known. During solidification of hypoeutectic alloys, e.g., 55 wt pct Pb, the primary dendrites reject the less dense tin, and for the hypereutectic alloys, e.g., 75 wt pct Sn, the primary dendrites reject denser lead. Alloys were prepared by melting appropriate amounts of lead and tin in a glass crucible after which the homogeneous liquid was sucked directly into 5-mm i.d. glass tubes. The sample tube, containing approximately 30 cm of alloy, was then mechanically driven into the directional solidification furnace assembly and positioned such that approx. 20 cm of the sample was remelted. Subsequently, directional solidification was initiated by withdrawing the sample through a water-cooled jacket at a constant growth velocity of 2 ,microns/s. After 5 to 6 cm of growth, the sample was quickly removed from the furnace and quenched in a water bath to preserve the solid-liquid interface. Samples were directionally solidified vertically upward, nearly horizontally, and some in conjunction with an applied axial rotation of the crucible. Temperature gradients at the solid-liquid interface were measured with an in-siru K-type thermocouple. Solidified samples were cut perpendicular and parallel to the growth direction and conventionally prepared for microscopic examination.
Yoshida, Yasuyuki; Takata, Kazuyuki; Takai, Hiroki; Kawahara, Keisuke; Kuzuya, Akinori; Ohya, Yuichi
2017-10-01
On clinical application of biodegradable injectable polymer (IP) systems, quick extemporaneous preparation of IP formulations and longer duration time gel state after injection into the body are the important targets to be developed. Previously, we had reported temperature-responsive covalent gelation systems via bio-orthogonal thiol-ene reaction by 'mixing strategy' of amphiphilic biodegradable tri-block copolymer (tri-PCG) attaching acryloyl groups on both termini (tri-PCG-Acryl) with reactive polythiol. In other previous works, we found 'freeze-dry with PEG/dispersion' method as quick extemporaneous preparation method of biodegradable IP formulations. In this study, we applied this quick preparative method to the temperature-triggered covalent gelation system. The instant formulation (D-sample) could be prepared by 'freeze-dry with PEG/dispersion' just mixing of tri-PCG-Acryl micelle dispersion and tri-PCG/DPMP micelle dispersion with PEG, that can be prepared in 30 s from the dried samples. The obtained D-sample showed irreversible gelation and long duration time of gel state, which was basically the same as the formulations prepared by the usual heating dissolution method (S-sample). Interestingly, the D-sample could maintain its sol state for a longer time (24 h) after preparing the formulation at r.t. compared with the S-sample, which became a gel in 3 h after preparing. The IP system showed good biocompatibility and long duration time of the gel state after subcutaneous implantation. These characteristics of D-samples, quick extemporaneous preparation and high stability in the sol state before injection, would be very convenient in a clinical setting.
Effect of Genetic Database Comprehensiveness on Fractional Proteomics of Escherichia coli O157:H7
2014-01-01
proteins would be observed in the extracellular fraction. 15. SUBJECT TERMS Escherichia coli O157:H7 Liquid chromatography Mass spectrometry...Preparation ...............1 2.2 Liquid Chromatography /Mass Spectrometry Sample Preparation ....................2 2.3 Liquid Chromatography /Mass... Chromatography /Mass Spectrometry Sample Preparation. Samples were prepared for liquid chromatography tandem mass spectrometry (LC-MS/MS) in a similar
Stability of nitroglycerin in intravenous admixtures.
Klamerus, K J; Ueda, C T; Newton, D W
1984-02-01
The stability of nitroglycerin in intravenous admixtures was studied. Admixtures containing nitroglycerin 400 micrograms/ml and each of seven injectable drugs in concentrations used clinically were prepared in triplicate in 5% dextrose and 0.9% sodium chloride injections. Admixtures were stored in glass bottles at room temperature for 24 hours in the upright position and then for 24 hours in the inverted position to ensure contact of the solution with the rubber stopper of the container. At 0, 24, and 48 hours, samples of each admixture were assayed by high-performance liquid chromatography for nitroglycerin concentration. The pH of one randomly chosen bottle of each admixture was measured at 0, 24, and 48 hours. A significant loss of nitroglycerin potency at 48 hours was observed only in admixtures containing phenytoin; in these solutions, a 9% decrease in initial nitroglycerin concentration was noted. Phenytoin crystallization was present in all phenytoin admixtures by 24 hours. Compared with initial values, no significant differences in the pH values of any admixture samples assayed at 24 and 48 hours were noted; however, admixtures containing phenytoin had the most alkaline pH values. Under the conditions studied, nitroglycerin concentrations remained above 90% of their initial values for 48 hours in all tested admixtures; however, phenytoin crystallization limits the stability of phenytoin admixtures.
Optimization of a biomimetic bone cement: role of DCPD.
Panzavolta, Silvia; Bracci, Barbara; Rubini, Katia; Bigi, Adriana
2011-08-01
We previously proposed a biomimetic α-tricalcium phosphate (α-TCP) bone cement where gelatin controls the transformation of α-TCP into calcium deficient hydroxyapatite (CDHA), leading to improved mechanical properties. In this study we investigated the setting and hardening processes of biomimetic cements containing increasing amounts of CaHPO(4)·2H2O (DCPD) (0, 2.5, 5, 10, 15 wt.%), with the aim to optimize composition. Both initial and final setting times increased significantly when DCPD content accounts for 10 wt.%, whereas cements containing 15 wt.% DCPD did not set at all. Differential scanning calorimetry (DSC), X-ray diffraction (XRD), thermogravimetry (TG) and scanning electron microscopy (SEM) investigations were performed on samples maintained in physiological solution for different times. DCPD dissolution starts soon after cement preparation, but the rate of transformation decreases on increasing DCPD initial content in the samples. The rate of α-TCP to CDHA conversion during hardening decreases on increasing DCPD initial content. Moreover, the presence of DCPD prevents gelatin release during hardening. The combined effects of gelatin and DCPD on the rate of CDHA formation and porosity lead to significantly improved mechanical properties, with the best composition displaying a compressive strength of 35 MPa and a Young modulus of 1600 MPa. Copyright © 2011 Elsevier Inc. All rights reserved.
Abazari, Reza; Salehi, Ghazal; Mahjoub, Ali Reza
2018-09-01
Using a green and simple route with ultrasound illumination under atmospheric pressure and at room temperature, the nanosized preparation of a Zn(II) metal-organic framework, [Zn(ATA)(BPD)] ∞ (ATA = 2-aminoterephthalic acid), BPD = 1,4-bis(4-pyridyl)-2,3-diaza-1,3-butadiene), having nano-plate shape and 3D channel framework, was considered and the product was named as compound 1. The X-ray diffraction (XRD), scanning electron microscopy (SEM), IR spectroscopy, Brunauer-Emmett-Teller (BET), and thermogravimetric analysis (TGA) were used for characterization of the synthesized micro/nano-structures. Further, impact of different sonication times and initial reagent contents on the shape and size of the micro/nano-structures was investigated. The results show that under ultrasound irradiation non-aggregated plates with uniform morphology can be obtained with content of [0.0125] M of the initial reagents in the presence of triethylamine (TEA) at 120 min. Moreover, through N 2 adsorption, effect of the preparation route on the porosity was explored. The bulk and nano-plates of compound 1 were also studied for adsorption of 2,4-dichlorophenol as a pollutant sample. Kinetic studies indicated that 2,4-dichlorophenol adsorption via MOF nano-plates are of first-order kinetics. Also, MOF nano-plates have significantly been reutilized for five times while their adsorption properties have remained unchanged. Copyright © 2018 Elsevier B.V. All rights reserved.
NASA Astrophysics Data System (ADS)
Wang, Xuejiang; Song, Jingke; Huang, Jiayu; Zhang, Jing; Wang, Xin; Ma, RongRong; Wang, Jiayi; Zhao, Jianfu
2016-12-01
Magnetic photocatalyst - iodine and nitrogen codoped TiO2 based on chitosan decorated magnetic activated carbon (I-N-T/CMAC) was prepared via simple coprecipitation and sol-gel method. The characteristics of photocatalysts were investigated by X-ray diffraction (XRD), N2 adsorption-desorption isotherm, field emission scanning electron microscopy (FESEM), energy dispersive spectrometry (EDS), fourier transform infrared (FTIR), X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflection spectroscopy (UV-vis DRS), photoluminescence (PL) spectroscopy and vibrating sample magnetometer (VSM). It turned out that the prepared material had large surface area, enhanced absorption of visible light, and magnetically separable properties when mole ratio of I/Ti was 0.1. Iodine-nitrogen codoped magnetic photocatalyst was used for the removal of salicylic acid (SA), and the rate of adsorption reaction for SA by I0.1-N-T/CMAC followed the pseudo second-order kinetic. Under visible light irradiation, 89.71% SA with initial concentration = 30 mg/L could be removed by I0.1-N-T/CMAC, and photodegradation rate of SA on I0.1-N-T/CMAC composites was 0.0084 min-1 which is about 4 times higher than that of magnetic photocatalyst with nitrogen doped only. The effects of SA initial concentration, pH, coexisting anions and humic acid to the degradation of SA with the prepared material were also investigated. Main oxidative species in the photodegradation process are rad OH and h+.
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.
Corrosion Propagation of Rebar Embedded in High Performance Concrete
NASA Astrophysics Data System (ADS)
Nazim, Manzurul
The FDOT has been using supplementary cementitious materials while constructing steel reinforced concrete marine bridge structures for over 3 decades. Previous findings indicated that such additions in concrete mix make the concrete more durable. To better understand corrosion propagation of rebar in high performance concrete: mature concrete samples that were made (2008/2009) with Portland cement, a binary mix, a ternary mix and recently prepared (April 2016 with 50% OPC + 50% slag and 80% OPC + 20% Fly ash) concrete samples were considered. None of these concretes had any admixed chloride to start with. An accelerated chloride transport process was used to drive chloride ions into the concrete so that chlorides reach and exceed the chloride threshold at the rebar surface and initiate corrosion. Electrochemical measurements were taken at regular intervals (during and after the electro-migration process) to observe the corrosion propagation in each sample.
Extending the solvent-free MALDI sample preparation method.
Hanton, Scott D; Parees, David M
2005-01-01
Matrix-assisted laser desorption/ionization (MALDI) mass spectrometry is an important technique to characterize many different materials, including synthetic polymers. MALDI mass spectral data can be used to determine the polymer average molecular weights, repeat units, and end groups. One of the key issues in traditional MALDI sample preparation is making good solutions of the analyte and the matrix. Solvent-free sample preparation methods have been developed to address these issues. Previous results of solvent-free or dry prepared samples show some advantages over traditional wet sample preparation methods. Although the results of the published solvent-free sample preparation methods produced excellent mass spectra, we found the method to be very time-consuming, with significant tool cleaning, which presents a significant possibility of cross contamination. To address these issues, we developed an extension of the solvent-free method that replaces the mortar and pestle grinding with ball milling the sample in a glass vial with two small steel balls. This new method generates mass spectra with equal quality of the previous methods, but has significant advantages in productivity, eliminates cross contamination, and is applicable to liquid and soft or waxy analytes.
Two New Nuclear Isolation Buffers for Plant DNA Flow Cytometry: A Test with 37 Species
Loureiro, João; Rodriguez, Eleazar; Doležel, Jaroslav; Santos, Conceição
2007-01-01
Background and Aims After the initial boom in the application of flow cytometry in plant sciences in the late 1980s and early 1990s, which was accompanied by development of many nuclear isolation buffers, only a few efforts were made to develop new buffer formulas. In this work, recent data on the performance of nuclear isolation buffers are utilized in order to develop new buffers, general purpose buffer (GPB) and woody plant buffer (WPB), for plant DNA flow cytometry. Methods GPB and WPB were used to prepare samples for flow cytometric analysis of nuclear DNA content in a set of 37 plant species that included herbaceous and woody taxa with leaf tissues differing in structure and chemical composition. The following parameters of isolated nuclei were assessed: forward and side light scatter, propidium iodide fluorescence, coefficient of variation of DNA peaks, quantity of debris background, and the number of particles released from sample tissue. The nuclear genome size of 30 selected species was also estimated using the buffer that performed better for a given species. Key Results In unproblematic species, the use of both buffers resulted in high quality samples. The analysis of samples obtained with GPB usually resulted in histograms of DNA content with higher or similar resolution than those prepared with the WPB. In more recalcitrant tissues, such as those from woody plants, WPB performed better and GPB failed to provide acceptable results in some cases. Improved resolution of DNA content histograms in comparison with previously published buffers was achieved in most of the species analysed. Conclusions WPB is a reliable buffer which is also suitable for the analysis of problematic tissues/species. Although GPB failed with some plant species, it provided high-quality DNA histograms in species from which nuclear suspensions are easy to prepare. The results indicate that even with a broad range of species, either GPB or WPB is suitable for preparation of high-quality suspensions of intact nuclei suitable for DNA flow cytometry. PMID:17684025
Sample Preparation for Electron Probe Microanalysis—Pushing the Limits
Geller, Joseph D.; Engle, Paul D.
2002-01-01
There are two fundamental considerations in preparing samples for electron probe microanalysis (EPMA). The first one may seem obvious, but we often find it is overlooked. That is, the sample analyzed should be representative of the population from which it comes. The second is a direct result of the assumptions in the calculations used to convert x-ray intensity ratios, between the sample and standard, to concentrations. Samples originate from a wide range of sources. During their journey to being excited under the electron beam for the production of x rays there are many possibilities for sample alteration. Handling can contaminate samples by adding extraneous matter. In preparation, the various abrasives used in sizing the sample by sawing, grinding and polishing can embed themselves. The most accurate composition of a contaminated sample is, at best, not representative of the original sample; it is misleading. Our laboratory performs EPMA analysis on customer submitted samples and prepares over 250 different calibration standards including pure elements, compounds, alloys, glasses and minerals. This large variety of samples does not lend itself to mass production techniques, including automatic polishing. Our manual preparation techniques are designed individually for each sample. The use of automated preparation equipment does not lend itself to this environment, and is not included in this manuscript. The final step in quantitative electron probe microanalysis is the conversion of x-ray intensities ratios, known as the “k-ratios,” to composition (in mass fraction or atomic percent) and/or film thickness. Of the many assumptions made in the ZAF (where these letters stand for atomic number, absorption and fluorescence) corrections the localized geometry between the sample and electron beam, or takeoff angle, must be accurately known. Small angular errors can lead to significant errors in the final results. The sample preparation technique then becomes very important, and, under certain conditions, may even be the limiting factor in the analytical uncertainty budget. This paper considers preparing samples to get known geometries. It will not address the analysis of samples with irregular, unprepared surfaces or unknown geometries. PMID:27446757
DOE Office of Scientific and Technical Information (OSTI.GOV)
Youngman, A.L.; Lydy, M.J.; Williams, T.L.
1998-12-31
The purpose of this study was to determine whether a duckweed bioassay could be used to evaluate the downward migration of heavy metals in smelter soils. The duckweed bioassay was initially used to evaluate elutriates prepared from samples of smelter soils. These initial tests verified that the elutriates would elicit toxic responses. Elutriate testing was followed with an evaluation of leachate from untreated soil cores or soil cores that had been amended with organic matter either unplanted or planted to a grass-forb seed mixture. There was an inverse linear relationship between heavy-metal concentrations in leachate and NOEC and IC{sub 50}more » values expressed as percentages among all soil cores. Based on these preliminary duckweed bioassays, there were no differences between soil types or organic amended or non-amended soil, but leachate from vegetated soil cores were less toxic than were leachates from non-vegetated soil cores. Overall, the duckweed bioassays were useful in detecting heavy metal availability in elutriate and leachate samples from smelter soils.« less
Nucleation and growth of electrodeposited Mn oxide rods for supercapacitor electrodes
NASA Astrophysics Data System (ADS)
Clark, Michael; Ivey, Douglas G.
2015-09-01
The nucleation and growth of electrodeposited Mn oxide rods has been investigated by preparing deposits on Au coated Si at varying deposition times between 0.5 s and 10 min. The deposits were investigated using high resolution scanning and transmission electron microscopy. A model for the nucleation and growth of Mn oxide rods has been proposed. Nucleation begins as thin sheets along Au grain boundaries and triple points. As these nucleation sites are consumed, nucleation spreads across the grains. Nucleation of sheets in close proximity causes agglomeration and the formation of rounded particles. Some of these rounded particles then accelerate in growth, initially in all directions and then primarily in the direction normal to the sample surface. Accelerated growth normal to the sample surface leads to the formation of rods. As rods grow, the growth of other particles accelerates and they become rods themselves. Eventually the entire sample surface is covered with rods 15-20 μm long and about 2 μm wide. The sheet-like morphology of the deposits is retained at all stages of deposition. Electron diffraction analysis of 3 s and 6 s deposits shows that the sheets are initially amorphous and then begin to crystallize into a cubic spinel Mn3O4 crystal structure. High resolution imaging of the 6 s sample shows small crystalline regions (˜5 nm in size) within an amorphous matrix.
Magnetic and microwave absorbing properties of magnetite-thermoplastic natural rubber nanocomposites
NASA Astrophysics Data System (ADS)
Kong, Ing; Hj Ahmad, Sahrim; Hj Abdullah, Mustaffa; Hui, David; Nazlim Yusoff, Ahmad; Puryanti, Dwi
2010-11-01
Magnetic and microwave absorbing properties of thermoplastic natural rubber (TPNR) filled magnetite (Fe 3O 4) nanocomposites were investigated. The TPNR matrix was prepared from polypropylene (PP), natural rubber (NR) and liquid natural rubber (LNR) in the ratio of 70:20:10 with the LNR as the compatibilizer. TPNR-Fe 3O 4 nanocomposites with 4-12 wt% Fe 3O 4 as filler were prepared via a Thermo Haake internal mixer using a melt-blending method. XRD reveals the presence of cubic spinel structure of Fe 3O 4 with the lattice parameter of a=8.395 Å. TEM micrograph shows that the Fe 3O 4 nanoparticles are almost spherical with the size ranging 20-50 nm. The values of saturation magnetization ( MS), remanence ( MR), initial magnetic susceptibility ( χi) and initial permeability ( μi) increase, while the coercivity ( HC) decreases with increasing filler content for all compositions. For nanocomposites, the values of the real ( ɛr') and imaginary permittivity ( ɛr'') and imaginary permeability ( μr'') increase, while the value of real permeability ( μr') decreases as the filler content increases. The absorption or minimum reflection loss ( RL) continuously increases and the dip shifts to a lower frequency region with the increasing of both filler content in nanocomposites and the sample thickness. The RL is -25.51 dB at 12.65 GHz and the absorbing bandwidth in which the RL is less than -10 dB is 2.7 GHz when the filler content is 12 wt% at 9 mm sample thickness.
Production and stability of mechanochemically exfoliated graphene in water and culture media
NASA Astrophysics Data System (ADS)
León, V.; González-Domínguez, J. M.; Fierro, J. L. G.; Prato, M.; Vázquez, E.
2016-07-01
The preparation of graphene suspensions in water, without detergents or any other additives is achieved using freeze-dried graphene powders, produced by mechanochemical exfoliation of graphite. These powders of graphene can be safely stored or shipped, and promptly dissolved in aqueous media. The suspensions are relatively stable in terms of time, with a maximum loss of ~25% of the initial concentration at 2 h. This work provides an easy and general access to aqueous graphene suspensions of chemically non-modified graphene samples, an otherwise (almost) impossible task to achieve by other means. A detailed study of the stability of the relative dispersions is also reported.The preparation of graphene suspensions in water, without detergents or any other additives is achieved using freeze-dried graphene powders, produced by mechanochemical exfoliation of graphite. These powders of graphene can be safely stored or shipped, and promptly dissolved in aqueous media. The suspensions are relatively stable in terms of time, with a maximum loss of ~25% of the initial concentration at 2 h. This work provides an easy and general access to aqueous graphene suspensions of chemically non-modified graphene samples, an otherwise (almost) impossible task to achieve by other means. A detailed study of the stability of the relative dispersions is also reported. Electronic supplementary information (ESI) available: A video showing the dispersion process, the N 1s XPS spectrum of BMG, image of the graphite test in CCM, and the characterization of the GO employed. See DOI: 10.1039/c6nr03246j
Novel Sample-handling Approach for XRD Analysis with Minimal Sample Preparation
NASA Technical Reports Server (NTRS)
Sarrazin, P.; Chipera, S.; Bish, D.; Blake, D.; Feldman, S.; Vaniman, D.; Bryson, C.
2004-01-01
Sample preparation and sample handling are among the most critical operations associated with X-ray diffraction (XRD) analysis. These operations require attention in a laboratory environment, but they become a major constraint in the deployment of XRD instruments for robotic planetary exploration. We are developing a novel sample handling system that dramatically relaxes the constraints on sample preparation by allowing characterization of coarse-grained material that would normally be impossible to analyze with conventional powder-XRD techniques.
Synthesis carbon foams prepared from gelatin (CFG) for cadmium ion adsorption
NASA Astrophysics Data System (ADS)
Ulfa, M.; Ulfa, D. K.
2018-01-01
In this paper, carbon foam from gelatin (CFG) was synthesized by acid-catalyzed carbonization of gelatin solution on mild condition by the simple method. Gelatin (Ge) were used as sacrificial template and source of carbon. Sulphuric acid was used as acid catalyst. Carbon foam CFG sample were characterized by scanning electron microscope (SEM), nitrogen adsorption desorption and FTIR for knowing textural and structural properties of the sample. Carbon foam CFG sample demonstrated macro pipes-channel like with pore size that varies between 30-40 μ and surface area m 60-100 m2g-1. The carbon foams CFG sample were tested by using adsorption process for obtained their performance for decreasing Cd(II) ions from aqueous solutions. The adsorption capacities for cadmium was 46.7 mg/g obtained by using adsorbent dose 50 mg, initial concentration 50 ppm, contact time, 3 h; room temperature, stirring rate 150 rpm) which reached equilibrium at 55 min. Adsorption process fits using using Lagergren and Ho and McKay equation and measuring data
Ozay, Guner; Seyhan, Ferda; Yilmaz, Aysun; Whitaker, Thomas B; Slate, Andrew B; Giesbrecht, Francis
2006-01-01
The variability associated with the aflatoxin test procedure used to estimate aflatoxin levels in bulk shipments of hazelnuts was investigated. Sixteen 10 kg samples of shelled hazelnuts were taken from each of 20 lots that were suspected of aflatoxin contamination. The total variance associated with testing shelled hazelnuts was estimated and partitioned into sampling, sample preparation, and analytical variance components. Each variance component increased as aflatoxin concentration (either B1 or total) increased. With the use of regression analysis, mathematical expressions were developed to model the relationship between aflatoxin concentration and the total, sampling, sample preparation, and analytical variances. The expressions for these relationships were used to estimate the variance for any sample size, subsample size, and number of analyses for a specific aflatoxin concentration. The sampling, sample preparation, and analytical variances associated with estimating aflatoxin in a hazelnut lot at a total aflatoxin level of 10 ng/g and using a 10 kg sample, a 50 g subsample, dry comminution with a Robot Coupe mill, and a high-performance liquid chromatographic analytical method are 174.40, 0.74, and 0.27, respectively. The sampling, sample preparation, and analytical steps of the aflatoxin test procedure accounted for 99.4, 0.4, and 0.2% of the total variability, respectively.
A probabilistic drought forecasting framework: A combined dynamical and statistical approach
DOE Office of Scientific and Technical Information (OSTI.GOV)
Yan, Hongxiang; Moradkhani, Hamid; Zarekarizi, Mahkameh
In order to improve drought forecasting skill, this study develops a probabilistic drought forecasting framework comprised of dynamical and statistical modeling components. The novelty of this study is to seek the use of data assimilation to quantify initial condition uncertainty with the Monte Carlo ensemble members, rather than relying entirely on the hydrologic model or land surface model to generate a single deterministic initial condition, as currently implemented in the operational drought forecasting systems. Next, the initial condition uncertainty is quantified through data assimilation and coupled with a newly developed probabilistic drought forecasting model using a copula function. The initialmore » condition at each forecast start date are sampled from the data assimilation ensembles for forecast initialization. Finally, seasonal drought forecasting products are generated with the updated initial conditions. This study introduces the theory behind the proposed drought forecasting system, with an application in Columbia River Basin, Pacific Northwest, United States. Results from both synthetic and real case studies suggest that the proposed drought forecasting system significantly improves the seasonal drought forecasting skills and can facilitate the state drought preparation and declaration, at least three months before the official state drought declaration.« less
Brar, Pardeepinder K; Strawn, Laura K; Danyluk, Michelle D
2016-03-01
In-shell pecan samples (500 g) were collected over four harvest seasons (2010 to 2014) from seven pecan shelling facilities located in five U.S. states. Four varieties of pecans were analyzed: Mexican Improved, Native Seedlings, Southern Improved, and Western Improved. Pecan samples (100 g) were sent to a third party laboratory for initial Salmonella screening. When a sample was positive for Salmonella, the pathogen level was determined by the most-probable-number (MPN) method (25, 2.5, and 0.25 g). Two sample preparation strategies were used for the MPN analysis, and both strategies were combined for the reported MPN values. Forty-four (0.95%) of 4,641 in-shell pecan samples were positive for Salmonella during initial screening; prevalence by year was 0.47 to 1.4%. Prevalence was not significantly different between varieties: Mexican Improved, 1.2%; Native/Seedling, 0.99%; Southern Improved, 0.97%; and Western Improved, 0.75%. Salmonella was not isolated from 31 of 44 samples upon retesting during MPN analysis (<0.47 MPN/100 g). When Salmonella was detected, the levels were 0.47 to 39 MPN/100 g, with a mean of 2.4 MPN/100 g. Thirty-one Salmonella serotypes were obtained from 42 Salmonella-positive pecan samples; Enteritidis was the most common (12% of samples) followed by Javiana (9%) and Braenderup (7%). All Salmonella Enteritidis isolates were phage type 8. Pulsed-field gel electrophoresis analysis (XbaI) revealed within-serotype diversity, indicating introduction of contamination from a variety of sources. Most (64%) of the isolates were resistant to streptomycin or tetracycline, and 13% were resistant to three or more antibiotics. Salmonella prevalence and level on in-shell pecans is comparable to that on other nuts.
Wallace, Ellen; Dranow, David; Laible, Philip D.; Christensen, Jeff; Nollert, Peter
2011-01-01
The crystallization of membrane proteins in amphiphile-rich materials such as lipidic cubic phases is an established methodology in many structural biology laboratories. The standard procedure employed with this methodology requires the generation of a highly viscous lipidic material by mixing lipid, for instance monoolein, with a solution of the detergent solubilized membrane protein. This preparation is often carried out with specialized mixing tools that allow handling of the highly viscous materials while minimizing dead volume to save precious membrane protein sample. The processes that occur during the initial mixing of the lipid with the membrane protein are not well understood. Here we show that the formation of the lipidic phases and the incorporation of the membrane protein into such materials can be separated experimentally. Specifically, we have investigated the effect of different initial monoolein-based lipid phase states on the crystallization behavior of the colored photosynthetic reaction center from Rhodobacter sphaeroides. We find that the detergent solubilized photosynthetic reaction center spontaneously inserts into and concentrates in the lipid matrix without any mixing, and that the initial lipid material phase state is irrelevant for productive crystallization. A substantial in-situ enrichment of the membrane protein to concentration levels that are otherwise unobtainable occurs in a thin layer on the surface of the lipidic material. These results have important practical applications and hence we suggest a simplified protocol for membrane protein crystallization within amphiphile rich materials, eliminating any specialized mixing tools to prepare crystallization experiments within lipidic cubic phases. Furthermore, by virtue of sampling a membrane protein concentration gradient within a single crystallization experiment, this crystallization technique is more robust and increases the efficiency of identifying productive crystallization parameters. Finally, we provide a model that explains the incorporation of the membrane protein from solution into the lipid phase via a portal lamellar phase. PMID:21909395
7 CFR 61.34 - Drawing and preparation of sample.
Code of Federal Regulations, 2010 CFR
2010-01-01
... 7 Agriculture 3 2010-01-01 2010-01-01 false Drawing and preparation of sample. 61.34 Section 61.34 Agriculture Regulations of the Department of Agriculture (Continued) AGRICULTURAL MARKETING SERVICE (Standards... Cottonseed Samplers § 61.34 Drawing and preparation of sample. Each licensed cottonseed sampler shall draw...
The method for extracting and preparing indoor and outdoor air samples for analysis of polar persistent organic pollutants is summarized in this SOP. It covers the preparation of samples that are to be analyzed by gas chromatography/mass spectrometry.
40 CFR 761.392 - Preparing validation study samples.
Code of Federal Regulations, 2010 CFR
2010-07-01
... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Preparing validation study samples..., AND USE PROHIBITIONS Comparison Study for Validating a New Performance-Based Decontamination Solvent Under § 761.79(d)(4) § 761.392 Preparing validation study samples. (a)(1) To validate a procedure to...
40 CFR 761.392 - Preparing validation study samples.
Code of Federal Regulations, 2011 CFR
2011-07-01
... 40 Protection of Environment 31 2011-07-01 2011-07-01 false Preparing validation study samples..., AND USE PROHIBITIONS Comparison Study for Validating a New Performance-Based Decontamination Solvent Under § 761.79(d)(4) § 761.392 Preparing validation study samples. (a)(1) To validate a procedure to...
CSPAP Professional Preparation and Research Initiatives at the University of South Carolina
ERIC Educational Resources Information Center
Webster, Collin
2017-01-01
Several comprehensive school physical activity program (CSPAP) professional preparation and research initiatives are underway in the Department of Physical Education and Athletic Training at the University of South Carolina. The CSPAP learning experiences have been mostly integrated into existing courses to help candidates in physical education…
Preparation and characterization of poly(acrylic acid)-hydroxyethyl cellulose graft copolymer.
Abdel-Halim, E S
2012-10-01
Poly(acrylic acid) hydroxyethyl cellulose [poly(AA)-HEC] graft copolymer was prepared by polymerizing acrylic acid (AA) with hydroxyethyl cellulose (HEC) using potassium bromate/thiourea dioxide (KBrO(3)/TUD) as redox initiation system. The polymerization reaction was carried out under a variety of conditions including concentrations of AA, KBrO(3) and TUD, material to liquor ratio and polymerization temperature. The polymerization reaction was monitored by withdrawing samples from the reaction medium and measuring the total conversion. The rheological properties of the poly(AA)-HEC graft copolymer were investigated. The total conversion and rheological properties of the graft copolymer depended on the ratio of KBrO(3) to TUD and on acrylic acid concentration as well as temperature and material to liquor ratio. Optimum conditions of the graft copolymer preparation were 30 mmol KBrO(3) and 30 mmol TUD/100g HEC, 100% AA (based on weight of HEC), duration 2h at temperature 50 °C using a material to liquor ratio of 1:10. Copyright © 2012. Published by Elsevier Ltd.
Kinetic Spectrophotometric Determination of Biotin in Pharmaceutical Preparations
Walash, M. I.; Rizk, M.; Sheribah, Z. A.; Salim, M. M.
2008-01-01
A simple accurate kinetic spectrophotometric method was developed for the determination of biotin in pure form and pharmaceutical preparations. The proposed method is based on a catalytic acceleration of biotin on the reaction between sodium azide and tri-iodide in an aqueous solution. Concentration range of 4-16 μg/mL for biotin was determined by measuring the decrease in the absorbance of tri-iodide at 348 nm by a fixed time method. The decrease in absorbance after 14 min from the initiation of the reaction was markedly correlated to the concentration with correlation coefficient of 0.9999. The detection limit (LOD) of biotin was 0.18 μg/mL while quantitation limit (LOQ) was 0.54 μg/mL. The percentage recovery of the spiked samples was 100.08 ± 0.761. The proposed procedure was successfully applied for the determination of biotin in its pharmaceutical preparations with mean recoveries of 101.17 ± 2.05 and 97.87 ± 1.50 for biotin ampoules and capsules, respectively. The results obtained were in good agreement with those obtained using official method. PMID:23675096
Bottoli, Carla B G; Vigna, Camila R M; Fischer, Gerd; Albert, Klaus; Collins, Kenneth E; Collins, Carol H
2004-03-19
Batches of poly(methyloctylsiloxane) (PMOS)-loaded silica were prepared by the deposition of PMOS, into the pores of HPLC silica. Portions of PMOS-loaded silica were allowed to remain at ambient temperature, without further treatment for 2, 9, 20, 31, 51, 105 and 184 days after preparation to undergo self-immobilization (irreversible adsorption of a layer of polymer on silica at ambient temperature in the absence of initiators). Other portions were subjected to a thermal treatment (100 degrees C for 4h) after 1, 2, 5, 7, 9, 15, 20, 25, 70, 111 and 184 days. Self-immobilized and thermally treated samples were characterized by % C, 29Si cross-polarization magic angle spinning (CP/MAS) NMR spectroscopy and reversed-phase column performance. The results show that thermal immobilization accelerates the distribution and rearrangement of the polymer on the silica surface. However, from the time that a monolayer has been formed by self-immobilization (approximately 100 days for PMOS on Kromasil silica), the thermal treatment does not alter this configuration and, thus, does not change the resulting chromatographic parameters.
Response (re-)programming in aging: a kinematic analysis.
Bellgrove, M A; Phillips, J G; Bradshaw, J L; Gallucci, R M
1998-05-01
Age-related motor slowing may reflect either motor programming deficits, poorer movement execution, or mere strategic preferences for online guidance of movement. We controlled such preferences, limiting the extent to which movements could be programmed. Twenty-four young and 24 older adults performed a line drawing task that allowed movements to be prepared in advance in one case (i.e., cue initially available indicating target location) and not in another (i.e., no cue initially available as to target location). Participants connected large or small targets illuminated by light-emitting diodes upon a graphics tablet that sampled pen tip position at 200 Hz. Older adults had a disproportionate difficulty initiating movement when prevented from programming in advance. Older adults produced slower, less efficient movements, particularly when prevented from programming under greater precision requirements. The slower movements of older adults do not simply reflect a preference for online control, as older adults have less efficient movements when forced to reprogram their movements. Age-related motor slowing kinematically resembles that seen in patients with cerebellar dysfunction.
Repetitive Interrogation of 2-Level Quantum Systems
NASA Technical Reports Server (NTRS)
Prestage, John D.; Chung, Sang K.
2010-01-01
Trapped ion clocks derive information from a reference atomic transition by repetitive interrogations of the same quantum system, either a single ion or ionized gas of many millions of ions. Atomic beam frequency standards, by contrast, measure reference atomic transitions in a continuously replenished "flow through" configuration where initial ensemble atomic coherence is zero. We will describe some issues and problems that can arise when atomic state selection and preparation of the quantum atomic system is not completed, that is, optical pumping has not fully relaxed the coherence and also not fully transferred atoms to the initial state. We present a simple two-level density matrix analysis showing how frequency shifts during the state-selection process can cause frequency shifts of the measured clock transition. Such considerations are very important when a low intensity lamp light source is used for state selection, where there is relatively weak relaxation and re-pumping of ions to an initial state and much weaker 'environmental' relaxation of the atomic coherence set-up in the atomic sample.
7 CFR 27.89 - Expenses; inspection; sampling.
Code of Federal Regulations, 2011 CFR
2011-01-01
... 7 Agriculture 2 2011-01-01 2011-01-01 false Expenses; inspection; sampling. 27.89 Section 27.89... Micronaire § 27.89 Expenses; inspection; sampling. Expense of inspection and sampling, the preparation of the... Office, the expense of inspection, sampling, preparation of samples, and delivery of the samples to the...
7 CFR 27.89 - Expenses; inspection; sampling.
Code of Federal Regulations, 2010 CFR
2010-01-01
... 7 Agriculture 2 2010-01-01 2010-01-01 false Expenses; inspection; sampling. 27.89 Section 27.89... Micronaire § 27.89 Expenses; inspection; sampling. Expense of inspection and sampling, the preparation of the... Office, the expense of inspection, sampling, preparation of samples, and delivery of the samples to the...
Imaging Gallium Nitride High Electron Mobility Transistors to Identify Point Defects
2014-03-01
streamline the sample preparation procedure to maximize the yield of successful samples to be analyzed chemically in an energy dispersive spectrometry...transmission electron microscope (STEM), sample preparation 15. NUMBER OF PAGES 103 16. PRICE CODE 17. SECURITY CLASSIFICATION OF REPORT...Computer Engineering iii THIS PAGE INTENTIONALLY LEFT BLANK iv ABSTRACT The purpose of this thesis is to streamline the sample preparation
Independence of Movement Preparation and Movement Initiation.
Haith, Adrian M; Pakpoor, Jina; Krakauer, John W
2016-03-09
Initiating a movement in response to a visual stimulus takes significantly longer than might be expected on the basis of neural transmission delays, but it is unclear why. In a visually guided reaching task, we forced human participants to move at lower-than-normal reaction times to test whether normal reaction times are strictly necessary for accurate movement. We found that participants were, in fact, capable of moving accurately ∼80 ms earlier than their reaction times would suggest. Reaction times thus include a seemingly unnecessary delay that accounts for approximately one-third of their duration. Close examination of participants' behavior in conventional reaction-time conditions revealed that they generated occasional, spontaneous errors in trials in which their reaction time was unusually short. The pattern of these errors could be well accounted for by a simple model in which the timing of movement initiation is independent of the timing of movement preparation. This independence provides an explanation for why reaction times are usually so sluggish: delaying the mean time of movement initiation relative to preparation reduces the risk that a movement will be initiated before it has been appropriately prepared. Our results suggest that preparation and initiation of movement are mechanistically independent and may have a distinct neural basis. The results also demonstrate that, even in strongly stimulus-driven tasks, presentation of a stimulus does not directly trigger a movement. Rather, the stimulus appears to trigger an internal decision whether to make a movement, reflecting a volitional rather than reactive mode of control. Copyright © 2016 the authors 0270-6474/16/363007-10$15.00/0.
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
High-throughput automated microfluidic sample preparation for accurate microbial genomics
Kim, Soohong; De Jonghe, Joachim; Kulesa, Anthony B.; Feldman, David; Vatanen, Tommi; Bhattacharyya, Roby P.; Berdy, Brittany; Gomez, James; Nolan, Jill; Epstein, Slava; Blainey, Paul C.
2017-01-01
Low-cost shotgun DNA sequencing is transforming the microbial sciences. Sequencing instruments are so effective that sample preparation is now the key limiting factor. Here, we introduce a microfluidic sample preparation platform that integrates the key steps in cells to sequence library sample preparation for up to 96 samples and reduces DNA input requirements 100-fold while maintaining or improving data quality. The general-purpose microarchitecture we demonstrate supports workflows with arbitrary numbers of reaction and clean-up or capture steps. By reducing the sample quantity requirements, we enabled low-input (∼10,000 cells) whole-genome shotgun (WGS) sequencing of Mycobacterium tuberculosis and soil micro-colonies with superior results. We also leveraged the enhanced throughput to sequence ∼400 clinical Pseudomonas aeruginosa libraries and demonstrate excellent single-nucleotide polymorphism detection performance that explained phenotypically observed antibiotic resistance. Fully-integrated lab-on-chip sample preparation overcomes technical barriers to enable broader deployment of genomics across many basic research and translational applications. PMID:28128213
Carbon distribution profiles in lunar fines
NASA Technical Reports Server (NTRS)
Hart, R. K.
1977-01-01
Radial distribution profiles of elemental carbon in lunar soils consisting of particles in the size range of 50 to 150 microns were investigated. Initial experiments on specimen preparation and the analysis of prepared specimens by Auger electron spectrometry (AES) and scanning electron microscopy (SEM) are described. Results from splits of samples 61501,84 and 64421,11, which were mounted various ways in several specimen holders, are presented. A low carbon content was observed in AES spectra from soil particles that were subjected to sputter-ion cleaning with 960eV argon ions for periods of time up to a total exposure for one hour. This ion charge was sufficient to remove approximately 70 nm of material from the surface. All of the physically adsorbed carbon (as well as water vapor, etc.) would normally be removed in the first few minutes, leaving only carbon in the specimen, and metal support structure, to be detected thereafter.
National Delphi study to determine competencies for nursing leadership in public health.
Misener, T R; Alexander, J W; Blaha, A J; Clarke, P N; Cover, C M; Felton, G M; Fuller, S G; Herman, J; Rodes, M M; Sharp, H F
1997-01-01
To identify competencies needed by nurse leaders in public health programs. Five-round national Delphi. Convenience sample of members of major public health nursing associations and nurse and non-nurse public health leaders in the USA. Mailed survey in 1994-1995 using a modified snowball technique based on a modification of the Pew Foundation health professions' competencies for Round 1. Four additional rounds produced consensus. Initially, 62 competencies were identified. Factor analysis resulted in four factors: political competencies, business acumen, program leadership, and management capabilities; 57 competencies were clustered in the four groupings and accounted for 91.4% of the variance. Graduate schools in nursing and public health must prepare students with broad-based competencies from a variety of disciplines. Findings of this national survey provide a database for curriculum development and evaluation of programs to prepare nurse leaders for roles in public health-based delivery systems.
Behavior of Aluminum in Solid Propellant Combustion
1982-06-01
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 second sample used pre...34propellant" formulations. The formulations included dry pressed AP/AI, and AP/AI/ Wax samples. Sandwiches were also prepared consisting of an aluminum...Binder flame instead of by aluminum exposure during accumulate break-up. Combustion of AP/AI/ Wax Samples A set of propellant samples were prepared by
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.
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.
Solving satisfiability problems using a novel microarray-based DNA computer.
Lin, Che-Hsin; Cheng, Hsiao-Ping; Yang, Chang-Biau; Yang, Chia-Ning
2007-01-01
An algorithm based on a modified sticker model accompanied with an advanced MEMS-based microarray technology is demonstrated to solve SAT problem, which has long served as a benchmark in DNA computing. Unlike conventional DNA computing algorithms needing an initial data pool to cover correct and incorrect answers and further executing a series of separation procedures to destroy the unwanted ones, we built solutions in parts to satisfy one clause in one step, and eventually solve the entire Boolean formula through steps. No time-consuming sample preparation procedures and delicate sample applying equipment were required for the computing process. Moreover, experimental results show the bound DNA sequences can sustain the chemical solutions during computing processes such that the proposed method shall be useful in dealing with large-scale problems.
High volumetric supercapacitor with a long life span based on polymer dots and graphene sheets
NASA Astrophysics Data System (ADS)
Wei, Ji-Shi; Chen, Jie; Ding, Hui; Zhang, Peng; Wang, Yong-Gang; Xiong, Huan-Ming
2017-10-01
A series of polymer dots/graphene sheets composites with high densities are prepared and tested for supercapacitors. Polymer dots (PDs) are synthesized by one-step method at room temperature. They can effectively increase surface areas of the composites (almost 10 times), and the functional groups from PDs produce high pseudocapacitance, so that the samples exhibit high specific capacitances (e. g., 364.2 F cm-3 at 1 A g-1) and high cycling stability (e. g., more than 95% of the initial capacity retention over 10 000 cycles at different current densities). The optimal sample is employed to fabricate a symmetric supercapacitor, which exhibits an energy density up to 8 Wh L-1 and a power density up to 11 800 W L-1, respectively.
NASA Technical Reports Server (NTRS)
Lauretta, D. S.
2004-01-01
The primary goal of our research in this program is to develop new techniques for the analysis of volatile trace elements in very small samples using inductively coupled plasma mass spectrometry (ICP-MS) in preparation for samples returned by the Stardust mission. The instrument that will serve as the basis of our experiments is the ELEMENT2 high-resolution ICP-MS. We have spent the past year designing the laboratory to house this instrument as well as space to store and prepare samples returned by the Stardust mission. Unfortunately, the location that we had initially selected for the instrument turned out to be insufficient for our needs. This was determined almost eight months into the first year of our funding cycle, after extensive work including the production of engineering drawings. However, during this time the Lunar and Planetary Laboratory was selected to lead Phoenix, the first Mars Scout mission. As a result of this award LPL purchased a new, 50,000 square foot building. We have acquired 1400 square feet of laboratory space in this new facility. Four-hundred square feet will be used for a class-100 clean room. This area is designated for storage and preparation of extraterrestrial materials. The additional 1000 square feet will house the ELEMENT2 ICP-MS and peripheral devices. This is an enormous amount of space for this instrument, but it provides plenty of room for expansion in the future. The ICP-MS and the clean room facilities have been purchased. The instrument has been delivered. The startup time for this instrument is relatively short and we expect to be collecting our first data by mid-summer.
Kline, Margaret C; Duewer, David L; Travis, John C; Smith, Melody V; Redman, Janette W; Vallone, Peter M; Decker, Amy E; Butler, John M
2009-06-01
Modern highly multiplexed short tandem repeat (STR) assays used by the forensic human-identity community require tight control of the initial amount of sample DNA amplified in the polymerase chain reaction (PCR) process. This, in turn, requires the ability to reproducibly measure the concentration of human DNA, [DNA], in a sample extract. Quantitative PCR (qPCR) techniques can determine the number of intact stretches of DNA of specified nucleotide sequence in an extremely small sample; however, these assays must be calibrated with DNA extracts of well-characterized and stable composition. By 2004, studies coordinated by or reported to the National Institute of Standards and Technology (NIST) indicated that a well-characterized, stable human DNA quantitation certified reference material (CRM) could help the forensic community reduce within- and among-laboratory quantitation variability. To ensure that the stability of such a quantitation standard can be monitored and that, if and when required, equivalent replacement materials can be prepared, a measurement of some stable quantity directly related to [DNA] is required. Using a long-established conventional relationship linking optical density (properly designated as decadic attenuance) at 260 nm with [DNA] in aqueous solution, NIST Standard Reference Material (SRM) 2372 Human DNA Quantitation Standard was issued in October 2007. This SRM consists of three quite different DNA extracts: a single-source male, a multiple-source female, and a mixture of male and female sources. All three SRM components have very similar optical densities, and thus very similar conventional [DNA]. The materials perform very similarly in several widely used gender-neutral assays, demonstrating that the combination of appropriate preparation methods and metrologically sound spectrophotometric measurements enables the preparation and certification of quantitation [DNA] standards that are both maintainable and of practical utility.
Secondary Physical Science Teachers' Conceptions of Science Teaching in a Context of Change
NASA Astrophysics Data System (ADS)
Taylor, Dale L.; Booth, Shirley
2015-05-01
Pre-service teachers enter initial teacher education programmes with conceptions of teaching gleaned from their own schooling. These conceptions, which include teachers' beliefs, may be resistant to change, which is a challenge in contexts where teacher educators hope that teachers will teach in ways different from their own schooling. Conceptions of teaching found in different cultural and disciplinary contexts have contextual differences but have resonances with the results of research into teacher beliefs. Our sample of eight South African secondary physical science teachers was schooled in a system which encouraged knowledge transmission, but they were prepared in their initial teacher education for a learner-centred approach. After they had taught for a few years, we explored their conceptions of science teaching, using phenomenographic interviews. Four conceptions emerged inductively from the analysis: transferring science knowledge from mind to mind; transferring problematic science knowledge from mind to mind; creating space for learning science knowledge and creating space for learning problematic science knowledge. Internally these conceptions are constituted by three dimensions of variation: the nature of the science knowledge to be learnt, the role of the students and the role of the teacher. Media and practical work play different roles in the external horizon of these conceptions. These conceptions reflect the disciplinary context as well as the emphases of the sample's initial teacher education programme. This suggests that initial teacher education can significantly shape teachers' conceptions of teaching.
Compatibility and activity of enoxaparin sodium in 0.9% sodium chloride injection for 48 hours.
Mewborn, A L; Kessler, J M; Joyner, K A
1996-01-15
The stability of enoxaparin sodium in 0.9% sodium chloride injection in polyvinyl chloride (PVC) containers was studied. Triplicate solutions of 120 mg (1.2 mL) of enoxaparin (as the sodium salt) and 98.8 mL of 0.9% sodium chloride injection were prepared in 250-mL PVC containers and stored at room temperature (20-22 degrees C). Samples were taken immediately after preparation and at 0.25, 0.5, 0.75, 1, 4, 12, 16, 24, and 48 hours. Inspections for color change and precipitation were performed with a clarity inspection station and a magnifying glass. Samples of the three admixtures were evaluated in duplicate for pharmacologic activity by an automated coagulation heparin assay. Throughout the 48-hour study period, the enoxaparin admixtures were free of color change, evolution of gas, and precipitates. The pharmacologic activity of enoxaparin in the PVC containers remained > 94% of the initial measured activity for 48 hours. Enoxaparin 1.2 mg/mL (as the sodium salt) in 0.9% sodium chloride injection in PVC containers was stable for up to 48 hours at 20-22 degrees C.
Time-resolved analysis of nonlinear optical limiting for laser synthesized carbon nanoparticles
NASA Astrophysics Data System (ADS)
Chen, G. X.; Hong, M. H.
2010-11-01
Nonlinear optical limiting materials have attracted much research interest in recent years. Carbon nanoparticles suspended in liquids show a strong nonlinear optical limiting function. It is important to investigate the nonlinear optical limiting process of carbon nanoparticles for further improving their nonlinear optical limiting performance. In this study, carbon nanoparticles were prepared by laser ablation of a carbon target in tetrahydrofuran (THF). Optical limiting properties of the samples were studied with 532-nm laser light, which is in the most sensitive wavelength band for human eyes. The shape of the laser pulse plays an important role for initializing the nonlinear optical limiting effect. Time-resolved analysis of laser pulses discovered 3 fluence stages of optical limiting. Theoretical simulation indicates that the optical limiting is initialized by a near-field optical enhancement effect.
Preparation of Chemical Samples On Relevant Surfaces Using Inkjet Technology
2013-04-01
PREPARATION OF CHEMICAL SAMPLES ON RELEVANT SURFACES USING INKJET TECHNOLOGY...2012 4. TITLE AND SUBTITLE 5a. CONTRACT NUMBER Preparation of Chemical Samples on Relevant Surfaces Using Inkjet Technology 5b. GRANT NUMBER...SUBJECT TERMS Surface detection Inkjet Simulant deposition 16. SECURITY CLASSIFICATION OF: 17. LIMITATION OF ABSTRACT 18. NUMBER OF
DOE Office of Scientific and Technical Information (OSTI.GOV)
Takayama, Yuki; Nakasako, Masayoshi; RIKEN Harima Institute/SPring-8, 1-1-1 Kouto, Mikaduki, Sayo, Hyogo 679-5148
2012-05-15
Coherent x-ray diffraction microscopy (CXDM) has the potential to visualize the structures of micro- to sub-micrometer-sized biological particles, such as cells and organelles, at high resolution. Toward advancing structural studies on the functional states of such particles, here, we developed a system for the preparation of frozen-hydrated biological samples for cryogenic CXDM experiments. The system, which comprised a moist air generator, microscope, micro-injector mounted on a micromanipulator, custom-made sample preparation chamber, and flash-cooling device, allowed for the manipulation of sample particles in the relative humidity range of 20%-94%rh at 293 K to maintain their hydrated and functional states. Here, wemore » report the details of the system and the operation procedure, including its application to the preparation of a frozen-hydrated chloroplast sample. Sample quality was evaluated through a cryogenic CXDM experiment conducted at BL29XUL of SPring-8. Taking the performance of the system and the quality of the sample, the system was suitable to prepare frozen-hydrated biological samples for cryogenic CXDM experiments.« less
Preparation of bone samples in the Gliwice Radiocarbon Laboratory for AMS radiocarbon dating.
Piotrowska, N; Goslar, T
2002-12-01
In the Gliwice Radiocarbon Laboratory, a system for preparation of samples for AMS dating has been built. At first it was used to produce graphite targets from plant macrofossils and sediments. In this study we extended its capabilities with the preparation of bones. We dealt with 3 methods; the first was the classical Longin method of collagen extraction, the second one included additional treatment of powdered bone in alkali solution, while in the third one carboxyl carbon was separated from amino acids obtained after hydrolysis of protein. The suitability of the methods was tested on 2 bone samples. Most of our samples gave ages > 40 kyr BP, suggesting good performance of the adapted methods, except for one sample prepared with simple Longin method. For routine preparation of bones we chose the Longin method with additional alkali treatment.
Effect Of Neodymium Substitution In Structural Characteristics Of Magnesium Ferrite
DOE Office of Scientific and Technical Information (OSTI.GOV)
Thankachan, Smitha; Binu, P. J.; Xavier, Sheena
2011-10-20
The effect of Nd{sup 3+} substitution on the structural properties of Magnesium ferrite was studied in the series MgNd{sub x}Fe{sub 2-x}O{sub 4}, where x = 0 to 0.3 in steps of 0.05. The series was prepared by sol-gel technique which is one of the novel technique to prepare nanosized samples. Structural characterization was done using X-ray diffractometer and Fourier Transform Infrared Spectrometer. XRD analysis reveals the prepared samples are single phasic till x = 0.2. From x0 = .25, a secondary phase of iron neodymium oxide appears along with the spinel phase. Particle size calculation shows the prepared samples aremore » in the 9nm to 11 nm regime. Lattice parameter was found to increase with concentration of Nd. XRD and FTIR analysis confirmed spinel structure of the prepared samples. XRF result shows the expected composition of prepared samples. The frequency dependence of the dielectric constant in the range 100 Hz--120MHz was also studied« less
[Effects of TWP on capacity of muscle contraction].
Zhang, Yun; Yu, Jingrui; Lü, Guangneng; Li, Keyong; Xu, Jianguo
2003-04-01
To investigate the direct effects of Tripterygium Wilfordii Polyglycosidium (TWP) on capability of muscle contraction. Using electronic stimulator to stimulate the phrenic nerve of the isolated phrenic nerve diaphragm preparation of 30 rats or directly stimulate the isolated gastrocnemius muscle preparation of 45 toads in vitro, we studied the effects of TWP on capability of muscle intrinsic contraction. TWP in 20 mg/L increased the amplitude of muscle contraction in initial 60 min but did not make further increase of the amplitude of muscle contraction from 60 min to 90 min in the isolated phrenic nerve diaphragm preparation of rat under one-third optimal stimulus. TWP in 40 mg/L and in 60 mg/L did not cause decrease of amplitude of muscle contraction in initial 60 min in isolated phrenic nerve diaphragm preparation of rat under one-third optimal stimulus. TWP in 60 mg/L did not cause decrease of tension of signal-contraction in initial 30 min in isolated gastrocnemius muscle preparation of toad under one-third optimal direct stimulus. Solvent DMSO could obviously reduce the tension of muscle contraction both in isolated phrenic nerve diaphragm preparation of rat and in isolated gastrocnemius muscle preparation of toad under one-third optimal stimulus. TWP can limitedly enhance the capability of muscle contraction; Solvent DMSO can restrain muscle contraction.
Tandem catalysis for the preparation of cylindrical polypeptide brushes.
Rhodes, Allison J; Deming, Timothy J
2012-11-28
Here, we report a method for synthesis of cylindrical copolypeptide brushes via N-carboxyanhydride (NCA) polymerization utilizing a new tandem catalysis approach that allows preparation of brushes with controlled segment lengths in a straightforward, one-pot procedure requiring no intermediate isolation or purification steps. To obtain high-density brush copolypeptides, we used a "grafting from" approach where alloc-α-aminoamide groups were installed onto the side chains of NCAs to serve as masked initiators. These groups were inert during cobalt-initiated NCA polymerization and gave allyloxycarbonyl-α-aminoamide-substituted polypeptide main chains. The alloc-α-aminoamide groups were then activated in situ using nickel to generate initiators for growth of side-chain brush segments. This use of stepwise tandem cobalt and nickel catalysis was found to be an efficient method for preparation of high-chain-density, cylindrical copolypeptide brushes, where both the main chains and side chains can be prepared with controlled segment lengths.
Deng, Liandong; He, Xiaohua; Li, Aigui; Yang, Qiuxia; Dong, Anjie
2007-02-01
Poly(methacrylic acid-grafted-poly(ethylene glycol)) (P(MAA-g-EG)) hydrogel nanoparticles (HNPs) were prepared by a thermally-initiated free radical dispersion polymerization method. The effects of various reaction parameters on the preparation of HNPs were investigated, including the quantity of monomer, temperature, initiator dosage, crosslinker dosage, and co-stabilizer concentration. The reaction temperature at 75 degrees C was found to be suitable for preparing stable and small P(MAA-g-EG) HNPs. By adding a little amount of polyvinyl alcohol in the reaction media, P(MAA-g-EG) HNPs with narrow size distribution could be obtained. The effects of pH and the crosslinker dosage on the equilibrium swelling behavior of P(MAA-g-EG) HNPs were also studied. The P(MAA-g-EG) HNPs perform pH-responsive swelling behavior, which is strongly influenced by the crosslinker dosage.
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.
School of Education - Teacher Preparation Program.
ERIC Educational Resources Information Center
University of the Pacific, Stockton, CA.
In recognition of the fact that teachers in this pluralistic society must have a multiplicity of skills, the School of Education of the University of the Pacific in 1970 initiated a self-study structure which resulted in a critical evaluation of its existing programs for the preparation of teachers. Programs were initiated and strengthened in…
Plant Response to Soils, Site Preparation, and Initial Pine Planting Density
Henry A. Pearson; Gale L. Wolters; Ronald E. Thill; Alton Martin; V. Clark Baldwin
1995-01-01
This study described the effects of soils, site preparation, and initial pine regeneration spacings on tree growth and the associated understory woody and herbaceous plant succession. Although Sawyer soils appeared more productive than Ruston soils before the harvest and regeneration treatments, woody and herbaceous plant differences were not apparent between the...
Integrating Experiential and Academic Learning in Teacher Preparation for Development Education
ERIC Educational Resources Information Center
Ryan, Anne
2012-01-01
With a view to linking ideals with action in development education, the preparation of teachers for practice in this area merits consideration. Given the theory/practice disconnect associated with initial teacher education, it is appropriate to explore means of effectively initiating beginning teachers into development education. To that end, a…
ERIC Educational Resources Information Center
Swank, Jacqueline M.; Huber, Peter
2013-01-01
Employment preparation and life skill development are crucial in assisting students identified as having emotional and behavioral disabilities with successfully transitioning to adulthood following high school. This article outlines four initiatives that a school counselor developed with other school personnel to promote work skills, life skills,…
Who Withdraws from Initial Teacher Preparation Programmes and Why?
ERIC Educational Resources Information Center
Hobson, Andrew J.; Giannakaki, Marina-Stefania; Chambers, Gary N.
2009-01-01
Background: In recent years, withdrawal from initial teacher preparation (ITP) programmes, in England and elsewhere, has become a cause for concern amongst both ITP providers and policy-makers. Purpose: This paper seeks to enhance the presently underdeveloped evidence base on the causes of withdrawal from ITP and on the characteristics of student…
Fabrication of Natural Uranium UO 2 Disks (Phase II): Texas A&M Work for Others Summary Document
DOE Office of Scientific and Technical Information (OSTI.GOV)
Gerczak, Tyler J.; Baldwin, Charles A.; Schmidlin, Joshua E.
The steps to fabricate natural UO 2 disks for an irradiation campaign led by Texas A&M University are outlined. The process was initiated with stoichiometry adjustment of parent, U 3O 8 powder. The next stage of sample preparation involved exploratory pellet pressing and sintering to achieve the desired natural UO 2 pellet densities. Ideal densities were achieved through the use of a bimodal powder size blend. The steps involved with disk fabrication are also presented, describing the coring and thinning process executed to achieve final dimensionality.
Final report on cermet high-level waste forms
DOE Office of Scientific and Technical Information (OSTI.GOV)
Kobisk, E.H.; Quinby, T.C.; Aaron, W.S.
1981-08-01
Cermets are being developed as an alternate method for the fixation of defense and commercial high level radioactive waste in a terminal disposal form. Following initial feasibility assessments of this waste form, consisting of ceramic particles dispersed in an iron-nickel base alloy, significantly improved processing methods were developed. The characterization of cermets has continued through property determinations on samples prepared by various methods from a variety of simulated and actual high-level wastes. This report describes the status of development of the cermet waste form as it has evolved since 1977. 6 tables, 18 figures.
Postmenopausal estrogen and progestin effects on the serum proteome
2009-01-01
Background Women's Health Initiative randomized trials of postmenopausal hormone therapy reported intervention effects on several clinical outcomes, with some important differences between estrogen alone and estrogen plus progestin. The biologic mechanisms underlying these effects, and these differences, have yet to be fully elucidated. Methods Baseline serum samples were compared with samples drawn 1 year later for 50 women assigned to active hormone therapy in both the estrogen-plus-progestin and estrogen-alone randomized trials, by applying an in-depth proteomic discovery platform to serum pools from 10 women per pool. Results In total, 378 proteins were quantified in two or more of the 10 pooled serum comparisons, by using strict identification criteria. Of these, 169 (44.7%) showed evidence (nominal P < 0.05) of change in concentration between baseline and 1 year for one or both of estrogen-plus-progestin and estrogen-alone groups. Quantitative changes were highly correlated between the two hormone-therapy preparations. A total of 98 proteins had false discovery rates < 0.05 for change with estrogen plus progestin, compared with 94 for estrogen alone. Of these, 84 had false discovery rates <0.05 for both preparations. The observed changes included multiple proteins relevant to coagulation, inflammation, immune response, metabolism, cell adhesion, growth factors, and osteogenesis. Evidence of differential changes also was noted between the hormone preparations, with the strongest evidence in growth factor and inflammation pathways. Conclusions Serum proteomic analyses yielded a large number of proteins similarly affected by estrogen plus progestin and by estrogen alone and identified some proteins and pathways that appear to be differentially affected between the two hormone preparations; this may explain their distinct clinical effects. PMID:20034393
DOE Office of Scientific and Technical Information (OSTI.GOV)
Madden, Jeremy T.; Toth, Scott J.; Dettmar, Christopher M.
Nonlinear optical (NLO) instrumentation has been integrated with synchrotron X-ray diffraction (XRD) for combined single-platform analysis, initially targeting applications for automated crystal centering. Second-harmonic-generation microscopy and two-photon-excited ultraviolet fluorescence microscopy were evaluated for crystal detection and assessed by X-ray raster scanning. Two optical designs were constructed and characterized; one positioned downstream of the sample and one integrated into the upstream optical path of the diffractometer. Both instruments enabled protein crystal identification with integration times between 80 and 150 µs per pixel, representing a ~10 3–10 4-fold reduction in the per-pixel exposure time relative to X-ray raster scanning. Quantitative centering andmore » analysis of phenylalanine hydroxylase fromChromobacterium violaceumcPAH,Trichinella spiralisdeubiquitinating enzyme TsUCH37, human κ-opioid receptor complex kOR-T4L produced in lipidic cubic phase (LCP), intimin prepared in LCP, and α-cellulose samples were performed by collecting multiple NLO images. The crystalline samples were characterized by single-crystal diffraction patterns, while α-cellulose was characterized by fiber diffraction. Good agreement was observed between the sample positions identified by NLO and XRD raster measurements for all samples studied.« less
Boonna, Sureeporn; Tongta, Sunanta
2018-07-01
Structural transformation of crystallized debranched cassava starch prepared by temperature cycling (TC) treatment and then subjected to annealing (ANN), heat-moisture treatment (HMT) and dual hydrothermal treatments of ANN and HMT was investigated. The relative crystallinity, lateral crystal size, melting temperature and resistant starch (RS) content increased for all hydrothermally treated samples, but the slowly digestible starch (SDS) content decreased. The RS content followed the order: HMT → ANN > HMT > ANN → HMT > ANN > TC, respectively. The HMT → ANN sample showed a larger lateral crystal size with more homogeneity, whereas the ANN → HMT sample had a smaller lateral crystal size with a higher melting temperature. After cooking at 50% moisture, the increased RS content of samples was observed, particularly for the ANN → HMT sample. These results suggest that structural changes of crystallized debranched starch during hydrothermal treatments depend on initial crystalline characteristics and treatment sequences, influencing thermal stability, enzyme digestibility, and cooking stability. Copyright © 2018 Elsevier Ltd. All rights reserved.
Recent advances of mesoporous materials in sample preparation.
Zhao, Liang; Qin, Hongqiang; Wu, Ren'an; Zou, Hanfa
2012-03-09
Sample preparation has been playing an important role in the analysis of complex samples. Mesoporous materials as the promising adsorbents have gained increasing research interest in sample preparation due to their desirable characteristics of high surface area, large pore volume, tunable mesoporous channels with well defined pore-size distribution, controllable wall composition, as well as modifiable surface properties. The aim of this paper is to review the recent advances of mesoporous materials in sample preparation with emphases on extraction of metal ions, adsorption of organic compounds, size selective enrichment of peptides/proteins, specific capture of post-translational peptides/proteins and enzymatic reactor for protein digestion. Copyright © 2011 Elsevier B.V. All rights reserved.
Birnbaum, D T; Kosmala, J D; Henthorn, D B; Brannon-Peppas, L
2000-04-03
To determine the effect of the organic solvent used during microparticle preparation on the in vitro release of beta-estradiol, a number of formulations were evaluated in terms of size, shape and drug delivery performance. Biodegradable microparticles of poly(lactide-co-glycolide) were prepared containing beta-estradiol that utilized dichloromethane, ethyl acetate or a mixture of dichloromethane and methanol as the organic phase solvent during the particle preparation. The drug delivery behavior from the microparticles was studied and comparisons were made of their physical properties for different formulations. The varying solubilities of beta-estradiol and poly(lactide-co-glycolide) in the solvents studied resulted in biodegradable microparticles with very different physical characteristics. Microparticles prepared from solid suspensions of beta-estradiol using dichloromethane as the organic phase solvent were similar in appearance to microparticles prepared without drug. Microparticles prepared from dichloromethane/methanol solutions appeared transparent to translucent depending on the initial amount of drug used in the formulation. Microparticles prepared using ethyl acetate appeared to have the most homogeneous encapsulation of beta-estradiol, appearing as solid white spheres regardless of initial drug content. Studies showed that microparticles prepared from either ethyl acetate or a mixture of dichloromethane and methanol gave a more constant release profile of beta-estradiol than particles prepared using dichloromethane alone. For all formulations, an initial burst of release increased with increasing drug loading, regardless of the organic solvent used.
Stability of urea in solution and pharmaceutical preparations.
Panyachariwat, Nattakan; Steckel, Hartwig
2014-01-01
The stability of urea in solution and pharmaceutical preparations was analyzed as a function of temperature (25°-60°C), pH (3.11-9.67), and initial urea concentration (2.5%-20%). This study was undertaken to (i) obtain more extensive, quantitative information relative to the degradation of urea in both aqueous and non-aqueous solutions and in pharmaceutical preparations, and (ii) test the effects of initial urea concentration, pH, buffer, and temperature values on urea degradation. The stability analysis shows that urea is more stable at the pH range of 4-8 and the stability of urea decreases by increase in temperature for all pH values. Within the experimental range of temperature and initial urea concentration values, the lowest urea degradation was found with lactate buffer pH 6.0. The urea decomposition rate in solution and pharmaceutical preparations shows the dependence of the initial urea concentrations. At higher initial urea concentrations, the rate of degradation is a decreasing function with time. This suggests that the reverse reaction is a factor in the degradation of concentrated urea solution. For non-aqueous solvents, isopropanol showed the best effort in retarding the decomposition of urea. Since the losses in urea is directly influenced by its stability at a given temperature and pH, the stability analysis of urea by the proposed model can be used to prevent the loss and optimize the operating condition for urea-containing pharmaceutical preparations.
40 CFR 761.323 - Sample preparation.
Code of Federal Regulations, 2013 CFR
2013-07-01
... 761.323 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL... Remediation Waste Samples § 761.323 Sample preparation. (a) The comparison study requires analysis of a minimum of 10 samples weighing at least 300 grams each. Samples of PCB remediation waste used in the...
40 CFR 761.323 - Sample preparation.
Code of Federal Regulations, 2014 CFR
2014-07-01
... 761.323 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL... Remediation Waste Samples § 761.323 Sample preparation. (a) The comparison study requires analysis of a minimum of 10 samples weighing at least 300 grams each. Samples of PCB remediation waste used in the...
40 CFR 761.323 - Sample preparation.
Code of Federal Regulations, 2012 CFR
2012-07-01
... 761.323 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL... Remediation Waste Samples § 761.323 Sample preparation. (a) The comparison study requires analysis of a minimum of 10 samples weighing at least 300 grams each. Samples of PCB remediation waste used in the...
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.
46 CFR 164.009-15 - Test procedure.
Code of Federal Regulations, 2010 CFR
2010-10-01
... material, is less than 47 mm, the specimens prepared consist of layers of the sample. (3) If the sample is a composite material and has a height that is not 50 ±3mm, the layers of the specimen prepared are proportional in thickness to the layers of the sample. (4) The top and bottom faces of each specimen prepared...
9 CFR 147.8 - Procedures for preparing egg yolk samples for diagnostic tests.
Code of Federal Regulations, 2014 CFR
2014-01-01
... 9 Animals and Animal Products 1 2014-01-01 2014-01-01 false Procedures for preparing egg yolk samples for diagnostic tests. 147.8 Section 147.8 Animals and Animal Products ANIMAL AND PLANT HEALTH... IMPROVEMENT PLAN Blood Testing Procedures § 147.8 Procedures for preparing egg yolk samples for diagnostic...
9 CFR 147.8 - Procedures for preparing egg yolk samples for diagnostic tests.
Code of Federal Regulations, 2013 CFR
2013-01-01
... 9 Animals and Animal Products 1 2013-01-01 2013-01-01 false Procedures for preparing egg yolk samples for diagnostic tests. 147.8 Section 147.8 Animals and Animal Products ANIMAL AND PLANT HEALTH... IMPROVEMENT PLAN Blood Testing Procedures § 147.8 Procedures for preparing egg yolk samples for diagnostic...
9 CFR 147.8 - Procedures for preparing egg yolk samples for diagnostic tests.
Code of Federal Regulations, 2012 CFR
2012-01-01
... 9 Animals and Animal Products 1 2012-01-01 2012-01-01 false Procedures for preparing egg yolk samples for diagnostic tests. 147.8 Section 147.8 Animals and Animal Products ANIMAL AND PLANT HEALTH... IMPROVEMENT PLAN Blood Testing Procedures § 147.8 Procedures for preparing egg yolk samples for diagnostic...
9 CFR 147.8 - Procedures for preparing egg yolk samples for diagnostic tests.
Code of Federal Regulations, 2011 CFR
2011-01-01
... 9 Animals and Animal Products 1 2011-01-01 2011-01-01 false Procedures for preparing egg yolk samples for diagnostic tests. 147.8 Section 147.8 Animals and Animal Products ANIMAL AND PLANT HEALTH... IMPROVEMENT PLAN Blood Testing Procedures § 147.8 Procedures for preparing egg yolk samples for diagnostic...
DOE Office of Scientific and Technical Information (OSTI.GOV)
Haab, Brian B.; Geierstanger, Bernhard H.; Michailidis, George
2005-08-01
Four different immunoassay and antibody microarray methods performed at four different sites were used to measure the levels of a broad range of proteins (N = 323 assays; 39, 88, 168, and 28 assays at the respective sites; 237 unique analytes) in the human serum and plasma reference specimens distributed by the Plasma Proteome Project (PPP) of the HUPO. The methods provided a means to (1) assess the level of systematic variation in protein abundances associated with blood preparation methods (serum, citrate-anticoagulated-plasma, EDTA-anticoagulated-plasma, or heparin-anticoagulated-plasma) and (2) evaluate the dependence on concentration of MS-based protein identifications from data sets usingmore » the HUPO specimens. Some proteins, particularly cytokines, had highly variable concentrations between the different sample preparations, suggesting specific effects of certain anticoagulants on the stability or availability of these proteins. The linkage of antibody-based measurements from 66 different analytes with the combined MS/MS data from 18 different laboratories showed that protein detection and the quality of MS data increased with analyte concentration. The conclusions from these initial analyses are that the optimal blood preparation method is variable between analytes and that the discovery of blood proteins by MS can be extended to concentrations below the ng/mL range under certain circumstances. Continued developments in antibody-based methods will further advance the scientific goals of the PPP.« less
Survivability of Vibrio cholerae O1 in Cooked Rice, Coffee, and Tea
Tang, John Yew Huat; Izenty, Bariah Ibrahim; Nur' Izzati, Ahmad Juanda; Masran, Siti Rahmah; Yeo, Chew Chieng; Roslan, Arshad; Abu Bakar, Che Abdullah
2013-01-01
This study aimed to investigate the survival of Vibrio cholerae O1 in 3 types of preparation for cooked rice, Oryza sativa L., (plain rice, rice with coconut milk, and rice with ginger); coffee, Coffea canephora, (plain coffee, coffee with sugar, and coffee with sweetened condensed milk); and tea, Camellia sinensis, (plain tea, tea with sugar, and tea with sweetened condensed milk) held at room temperature (27°C). The survival of V. cholerae O1 was determined by spread plate method on TCBS agar. Initial cultures of 8.00 log CFU/mL were inoculated into each food sample. After 6 h incubation, significant growth was only detected in rice with coconut milk (9.67 log CFU/mL; P < 0.05). However, all 3 types of rice preparation showed significant growth of V. cholerae after 24 h (P < 0.05). For coffee and tea preparations, V. cholerae survived up to 6 h in tea with condensed milk (4.72 log CFU/mL) but not in similar preparation of coffee. This study showed evidence for the survivability of V. cholerae in rice, coffee, and tea. Thus, holding these food and beverages for an extended period of time at room temperature should be avoided. PMID:26904604
La 2-xSr xCuO 4-δ superconducting samples prepared by the wet-chemical method
NASA Astrophysics Data System (ADS)
Loose, A.; Gonzalez, J. L.; Lopez, A.; Borges, H. A.; Baggio-Saitovitch, E.
2009-10-01
In this work, we report on the physical properties of good-quality polycrystalline superconducting samples of La 2-xSr xCu 1-yZn yO 4-δ ( y=0, 0.02) prepared by a wet-chemical method, focusing on the temperature dependence of the critical current. Using the wet-chemical method, we were able to produce samples with improved homogeneity compared to the solid-state method. A complete set of samples with several carrier concentrations, ranging from the underdoped (strontium concentration x≈0.05) to the highly overdoped ( x≈0.25) region, were prepared and investigated. The X-ray diffraction analysis, zero-field cooling magnetization and electrical resistivity measurements were reported on earlier. The structural parameters of the prepared samples seem to be slightly modified by the preparation method and their critical temperatures were lower than reported in the literature. The temperature dependence of the critical current was explained by a theoretical model which took the granular structure of the samples into account.
Automated SEM and TEM sample preparation applied to copper/low k materials
NASA Astrophysics Data System (ADS)
Reyes, R.; Shaapur, F.; Griffiths, D.; Diebold, A. C.; Foran, B.; Raz, E.
2001-01-01
We describe the use of automated microcleaving for preparation of both SEM and TEM samples as done by SELA's new MC500 and TEMstation tools. The MC500 is an automated microcleaving tool that is capable of producing cleaves with 0.25 μm accuracy resulting in SEM-ready samples. The TEMstation is capable of taking a sample output from the MC500 (or from SELA's earlier MC200 tool) and producing a FIB ready slice of 25±5 μm, mounted on a TEM-washer and ready for FIB thinning to electron transparency for TEM analysis. The materials selected for the tool set evaluation mainly included the Cu/TaN/HOSP low-k system. The paper is divided into three sections, experimental approach, SEM preparation and analysis of HOSP low-k, and TEM preparation and analysis of Cu/TaN/HOSP low-k samples. For the samples discussed, data is presented to show the quality of preparation provided by these new automated tools.
Struwe, Weston B; Agravat, Sanjay; Aoki-Kinoshita, Kiyoko F; Campbell, Matthew P; Costello, Catherine E; Dell, Anne; Ten Feizi; Haslam, Stuart M; Karlsson, Niclas G; Khoo, Kay-Hooi; Kolarich, Daniel; Liu, Yan; McBride, Ryan; Novotny, Milos V; Packer, Nicolle H; Paulson, James C; Rapp, Erdmann; Ranzinger, Rene; Rudd, Pauline M; Smith, David F; Tiemeyer, Michael; Wells, Lance; York, William S; Zaia, Joseph; Kettner, Carsten
2016-09-01
The minimum information required for a glycomics experiment (MIRAGE) project was established in 2011 to provide guidelines to aid in data reporting from all types of experiments in glycomics research including mass spectrometry (MS), liquid chromatography, glycan arrays, data handling and sample preparation. MIRAGE is a concerted effort of the wider glycomics community that considers the adaptation of reporting guidelines as an important step towards critical evaluation and dissemination of datasets as well as broadening of experimental techniques worldwide. The MIRAGE Commission published reporting guidelines for MS data and here we outline guidelines for sample preparation. The sample preparation guidelines include all aspects of sample generation, purification and modification from biological and/or synthetic carbohydrate material. The application of MIRAGE sample preparation guidelines will lead to improved recording of experimental protocols and reporting of understandable and reproducible glycomics datasets. © The Author 2016. Published by Oxford University Press. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.
[Recent advances in sample preparation methods of plant hormones].
Wu, Qian; Wang, Lus; Wu, Dapeng; Duan, Chunfeng; Guan, Yafeng
2014-04-01
Plant hormones are a group of naturally occurring trace substances which play a crucial role in controlling the plant development, growth and environment response. With the development of the chromatography and mass spectroscopy technique, chromatographic analytical method has become a widely used way for plant hormone analysis. Among the steps of chromatographic analysis, sample preparation is undoubtedly the most vital one. Thus, a highly selective and efficient sample preparation method is critical for accurate identification and quantification of phytohormones. For the three major kinds of plant hormones including acidic plant hormones & basic plant hormones, brassinosteroids and plant polypeptides, the sample preparation methods are reviewed in sequence especially the recently developed methods. The review includes novel methods, devices, extractive materials and derivative reagents for sample preparation of phytohormones analysis. Especially, some related works of our group are included. At last, the future developments in this field are also prospected.
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.
Sample preparation techniques for the determination of trace residues and contaminants in foods.
Ridgway, Kathy; Lalljie, Sam P D; Smith, Roger M
2007-06-15
The determination of trace residues and contaminants in complex matrices, such as food, often requires extensive sample extraction and preparation prior to instrumental analysis. Sample preparation is often the bottleneck in analysis and there is a need to minimise the number of steps to reduce both time and sources of error. There is also a move towards more environmentally friendly techniques, which use less solvent and smaller sample sizes. Smaller sample size becomes important when dealing with real life problems, such as consumer complaints and alleged chemical contamination. Optimal sample preparation can reduce analysis time, sources of error, enhance sensitivity and enable unequivocal identification, confirmation and quantification. This review considers all aspects of sample preparation, covering general extraction techniques, such as Soxhlet and pressurised liquid extraction, microextraction techniques such as liquid phase microextraction (LPME) and more selective techniques, such as solid phase extraction (SPE), solid phase microextraction (SPME) and stir bar sorptive extraction (SBSE). The applicability of each technique in food analysis, particularly for the determination of trace organic contaminants in foods is discussed.
Monitoring nitrite and nitrate residues in frankfurters during processing and storage.
Pérez-Rodríguez, M L; Bosch-Bosch, N; Garciá-Mata, M
1996-09-01
Frankfurter-type sausages were prepared in a pilot plant with different concentrations of NaNO(2) (75, 125 or 250 ppm) combined or not with 200 ppm KNO(3). A meat system, free of curing agents, was also used as control. Nitrite and nitrate levels were tested in various processing steps and over 120 days storage at 3 °C of the vacuum-packaged frankfurters. Little influence of the originally added nitrite level on the amount of nitrate formed was observed. Important losses of nitrite and nitrate were due to cooking. Thereafter about 50% of the nitrite added initially remained in this form in all samples (39, 59 and 146 ppm, respectively) and between 10 and 15% as nitrate. When only nitrate was initially added, formation of nitrite after cooking was observed (maximum level 43 ppm NaNO(2)). Formulations prepared with both nitrate and nitrite showed no significant differences (p < 0.01) respect to their nitrite or nitrate counterparts. A good correlation among nitrite and nitrate levels and storage time was showed by multiple linear regression analysis. It is concluded that the use of nitrate in combination with nitrite in cooked meat products seems to have little technological significance and adds to the total body burden of nitrite.
Huang, Qiang; Liu, Meiying; Mao, Liucheng; Xu, Dazhuang; Zeng, Guangjian; Huang, Hongye; Jiang, Ruming; Deng, Fengjie; Zhang, Xiaoyong; Wei, Yen
2017-08-01
Monodispersed SiO 2 particles functionalized with cationic polymers poly-((3-acrylamidopropyl)trimethylammonium chloride) (PAPTCl) were prepared using mussel inspired surface modification strategy and surface initiated atom transfer radical polymerization (SI-ATRP). Fourier transform infrared spectroscopy, transmission electron microscope, thermogravimetric analysis, X-ray photoelectron spectroscopy, and zeta potential were employed to characterize these SiO 2 samples. The adsorption performance of the functionalized SiO 2 (donated as SiO 2 -PDA-PAPTCl) towards anionic organic dye Congo red (CR) was investigated to evaluate their potential environmental applications. We demonstrated that the surface of SiO 2 particles can be successfully functionalized with cationic PAPTCl. The adsorption capability of as-prepared SiO 2 was found to increases from 28.70 and 106.65mg/g after surface grafted with cationic polymers. The significant enhancement in the adsorption capability of SiO 2 -PDA-PAPTCl is mainly attributed to the introduction of cationic polymers. More importantly, this strategy is expected to be promising for fabrication of many other functional polymer nanocomposites for environmental applications due to the universality of mussel inspired chemistry and well designability and good monomer adaptability of SI-ATRP. Copyright © 2017 Elsevier Inc. All rights reserved.
Sample Preparation Techniques for Grain Boundary Characterization of Annealed TRISO-Coated Particles
DOE Office of Scientific and Technical Information (OSTI.GOV)
Dunzik-Gougar, M. L.; van Rooyen, I. J.; Hill, C. M.
Crystallographic information about chemical vapor deposition layers of silicon carbide (SiC) is essential to understanding layer performance, especially when the layers are in non planar geometries, such as spherical. We performed electron Back Scatter Diffraction (EBSD) analysis of spherical SiC layers using a different approach to sample focus ion beam milling technique to avoid the negative impacts of traditional sample polishing and to address the need of very small samples of irradiated materials for analysis. Mechanical and chemical grinding and polishing of sample surfaces can introduce lattice strains and result in unequal removal of SiC and surrounding layers of differentmore » material due to the hardness differences of these materials. The nature of layer interfaces is thought to play a key role in performance of the SiC; therefore, analysis of representative samples at these interfacial areas is crucial. In work reported here, a focused ion beam (FIB) was employed in a novel manner to prepare a more representative sample for EBSD analysis from TRISO layers free of effects introduced by mechanical and chemical preparation methods. In addition, the difficulty of handling neutron irradiated microscopic samples such as those analyzed in this work has been simplified with pre tilted mounting stages. Our study showed that although the average grain size of samples may be similar, the grain boundary characteristics may differ significantly. It was also found that low angle grain boundaries, comprises 25% in the FIB-prepared sample vs only 1-2% in the polished sample measured in the same particle. From this study it was determined that results of FIB prepared sample will provide more repeatable results, as the role of sample preparation is eliminated.« less
Sample Preparation Techniques for Grain Boundary Characterization of Annealed TRISO-Coated Particles
Dunzik-Gougar, M. L.; van Rooyen, I. J.; Hill, C. M.; ...
2016-08-25
Crystallographic information about chemical vapor deposition layers of silicon carbide (SiC) is essential to understanding layer performance, especially when the layers are in non planar geometries, such as spherical. We performed electron Back Scatter Diffraction (EBSD) analysis of spherical SiC layers using a different approach to sample focus ion beam milling technique to avoid the negative impacts of traditional sample polishing and to address the need of very small samples of irradiated materials for analysis. Mechanical and chemical grinding and polishing of sample surfaces can introduce lattice strains and result in unequal removal of SiC and surrounding layers of differentmore » material due to the hardness differences of these materials. The nature of layer interfaces is thought to play a key role in performance of the SiC; therefore, analysis of representative samples at these interfacial areas is crucial. In work reported here, a focused ion beam (FIB) was employed in a novel manner to prepare a more representative sample for EBSD analysis from TRISO layers free of effects introduced by mechanical and chemical preparation methods. In addition, the difficulty of handling neutron irradiated microscopic samples such as those analyzed in this work has been simplified with pre tilted mounting stages. Our study showed that although the average grain size of samples may be similar, the grain boundary characteristics may differ significantly. It was also found that low angle grain boundaries, comprises 25% in the FIB-prepared sample vs only 1-2% in the polished sample measured in the same particle. From this study it was determined that results of FIB prepared sample will provide more repeatable results, as the role of sample preparation is eliminated.« less
DOE Office of Scientific and Technical Information (OSTI.GOV)
B. D. Miller; J. Gan; J. Madden
2012-05-01
Transmission electron microscopy (TEM), scanning electron microscopy (SEM), and focused ion beam (FIB) milling were performed on an irradiated U-10Mo monolithic fuel to understand its irradiation microstructure. This is the first reported TEM work of irradiated fuel sample prepared using a FIB. Advantages and disadvantages of using the FIB to create TEM samples from this irradiated fuel will be presented along with some results from the work. Sample preparation techniques used to create SEM and FIB samples from the brittle irradiated monolithic sample will also be discussed.
ERIC Educational Resources Information Center
Yontz, Brian David
2010-01-01
The stewardship of schools is central to the renewal and preservation of that which is precious in our nation's schools. This study examined perceptions of future teachers as to the degree to which their teacher preparation program emphasized the idea of stewarding schools. With a theoretical foundation that initial teacher preparation provides…
40 CFR 761.323 - Sample preparation.
Code of Federal Regulations, 2010 CFR
2010-07-01
... Remediation Waste Samples § 761.323 Sample preparation. (a) The comparison study requires analysis of a minimum of 10 samples weighing at least 300 grams each. Samples of PCB remediation waste used in the... PCB remediation waste at the cleanup site, or must be the same kind of material as that waste. For...
NASA Astrophysics Data System (ADS)
Wu, Tao
We describe two new methodologies leading to the formation of novel surface-anchored polymer assemblies on solid substrates. While the main goal is to understand the fundamentals pertaining to the preparation and properties of the surface-bound polymer assemblies (including neutral and chargeable polymers), several examples also are mentioned throughout the Thesis that point out to practical applications of such structures. The first method is based on generating assemblies comprising anchored polymers with a gradual variation of grafting densities on solid substrates. These structures are prepared by first covering the substrate with a molecular gradient of the polymerization initiator, followed by polymerization from these substrate-bound initiator centers ("grafting from"). We apply this technique to prepare grafting density gradients of poly(acryl amide) (PAAm) and poly(acrylic acid) (PAA) on silica-covered substrates. We show that using the grafting density gradient geometry, the characteristics of surface-anchored polymers in both the low grafting density ("mushroom") regime as well as the high grafting density ("brush") regime can be accessed conveniently on a single sample. We use a battery of experimental methods, including Fourier transform infrared spectroscopy (FTIR), Near-edge absorption fine structure spectroscopy (NEXAFS), contact angle, ellipsometry, to study the characteristics of the surface-bound polymer layers. We also probe the scaling laws of neutral polymer as a function of grafting density, and for weak polyelectrolyte, in addition to the grafting density, we study the affect of solution ionic strength and pH values. In the second novel method, which we coined as "mechanically assisted polymer assembly" (MAPA), we form surface anchored polymers by "grafting from" polymerization initiators deposited on elastic surfaces that have been previously extended uniaxially by a certain length increment, Deltax. Upon releasing the strain in the substrate after completion of polymerization, we show the grafting density of the polymers grafted to flexible substrates can be tuned as a function of Deltax.
NASA Astrophysics Data System (ADS)
Peebles, D. E.; Peebles, H. C.; Ohlhausen, J. A.; Hurst, M. J.
1996-02-01
A specially designed ultrahigh vacuum in situ surface analysis and wetting system has been constructed to study the spreading of liquid metal solders on carefully prepared and well-characterized solid substrates. The system consists of a standard ultrahigh vacuum surface analysis chamber linked to a reaction chamber for wetting or other experiments at pressures up to atmospheric. A sophisticated video system allows real-time monitoring of the spreading of the liquid metal through both side and top views. An infrared imaging system allows accurate remote temperature measurements. Sample surfaces are prepared and spreading experiments performed without intermediate exposure of the surfaces to the contaminating atmospheres. Solder spreading is performed under 50 Torr of highly purified helium gas to allow for adequate thermal coupling between the solder and the substrate. Initial studies have been completed for the spreading of pure tin solder on copper substrates in the absence of any fluxing agent. Three types of copper substrate surfaces were investigated in these experiments: the sputter-cleaned, air-exposed, and the as-received surface. Surface chemical analysis by x-ray photoelectron spectroscopy showed the air-exposed surface to consist of about 3 nm of Cu2O, while the as-received surface consisted of about 8 nm of Cu2O. The sputter-cleaned surface contained less than one monolayer (0.3 nm) of Cu2O. Spreading experiments utilizing a linear temperature ramp show that pure tin solder spreads readily on oxidized copper surfaces at elevated temperatures. The initiation temperature for rapid tin spreading on the as-received copper surface was 325 °C. Decreasing the thickness of the oxide on the surface lowered the observed temperature for the initiation of spreading and increased the rate of spreading. On the sputter-cleaned copper surface, rapid solder spreading was observed immediately upon melting of the solder.
Modular microfluidic system for biological sample preparation
Rose, Klint A.; Mariella, Jr., Raymond P.; Bailey, Christopher G.; Ness, Kevin Dean
2015-09-29
A reconfigurable modular microfluidic system for preparation of a biological sample including a series of reconfigurable modules for automated sample preparation adapted to selectively include a) a microfluidic acoustic focusing filter module, b) a dielectrophoresis bacteria filter module, c) a dielectrophoresis virus filter module, d) an isotachophoresis nucleic acid filter module, e) a lyses module, and f) an isotachophoresis-based nucleic acid filter.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Wen, Haiming; Lin, Yaojun; Seidman, David N.
The preparation of transmission electron microcopy (TEM) samples from powders with particle sizes larger than ~100 nm poses a challenge. The existing methods are complicated and expensive, or have a low probability of success. Herein, we report a modified methodology for preparation of TEM samples from powders, which is efficient, cost-effective, and easy to perform. This method involves mixing powders with an epoxy on a piece of weighing paper, curing the powder–epoxy mixture to form a bulk material, grinding the bulk to obtain a thin foil, punching TEM discs from the foil, dimpling the discs, and ion milling the dimpledmore » discs to electron transparency. Compared with the well established and robust grinding–dimpling–ion-milling method for TEM sample preparation for bulk materials, our modified approach for preparing TEM samples from powders only requires two additional simple steps. In this article, step-by-step procedures for our methodology are described in detail, and important strategies to ensure success are elucidated. Furthermore, our methodology has been applied successfully for preparing TEM samples with large thin areas and high quality for many different mechanically milled metallic powders.« less
Wen, Haiming; Lin, Yaojun; Seidman, David N.; ...
2015-09-09
The preparation of transmission electron microcopy (TEM) samples from powders with particle sizes larger than ~100 nm poses a challenge. The existing methods are complicated and expensive, or have a low probability of success. Herein, we report a modified methodology for preparation of TEM samples from powders, which is efficient, cost-effective, and easy to perform. This method involves mixing powders with an epoxy on a piece of weighing paper, curing the powder–epoxy mixture to form a bulk material, grinding the bulk to obtain a thin foil, punching TEM discs from the foil, dimpling the discs, and ion milling the dimpledmore » discs to electron transparency. Compared with the well established and robust grinding–dimpling–ion-milling method for TEM sample preparation for bulk materials, our modified approach for preparing TEM samples from powders only requires two additional simple steps. In this article, step-by-step procedures for our methodology are described in detail, and important strategies to ensure success are elucidated. Furthermore, our methodology has been applied successfully for preparing TEM samples with large thin areas and high quality for many different mechanically milled metallic powders.« less
Critical evaluation of sample pretreatment techniques.
Hyötyläinen, Tuulia
2009-06-01
Sample preparation before chromatographic separation is the most time-consuming and error-prone part of the analytical procedure. Therefore, selecting and optimizing an appropriate sample preparation scheme is a key factor in the final success of the analysis, and the judicious choice of an appropriate procedure greatly influences the reliability and accuracy of a given analysis. The main objective of this review is to critically evaluate the applicability, disadvantages, and advantages of various sample preparation techniques. Particular emphasis is placed on extraction techniques suitable for both liquid and solid samples.
Preparation of protein samples for mass spectrometry and N-terminal sequencing.
Glenn, Gary
2014-01-01
The preparation of protein samples for mass spectrometry and N-terminal sequencing is a key step in successfully identifying proteins. Mass spectrometry is a very sensitive technique, and as such, samples must be prepared carefully since they can be subject to contamination of the sample (e.g., due to incomplete subcellular fractionation or purification of a multiprotein complex), overwhelming of the sample by highly abundant proteins, and contamination from skin or hair (keratin can be a very common hit). One goal of sample preparation for mass spec is to reduce the complexity of the sample - in the example presented here, mitochondria are purified, solubilized, and fractionated by sucrose density gradient sedimentation prior to preparative 1D SDS-PAGE. It is important to verify the purity and integrity of the sample so that you can have confidence in the hits obtained. More protein is needed for N-terminal sequencing and ideally it should be purified to a single band when run on an SDS-polyacrylamide gel. The example presented here involves stably expressing a tagged protein in HEK293 cells and then isolating the protein by affinity purification and SDS-PAGE. © 2014 Elsevier Inc. All rights reserved.
NASA Astrophysics Data System (ADS)
Taer, E.; Taslim, R.; Deraman, M.
2016-02-01
Preparation of activated carbon monolith (ACM) from rubber wood was investigated. Two kind of preparation method were carried out by pre-carbonized of rubber wood saw dust and rubber wood material as it is naturally. The samples were prepared with pelletizing method and small cutting of rubber wood in cross sectional method. Both of samples were characterized by physical and electrochemical technique. The physical properties such as morphology and porosity were investigated. The electrochemical properties of both samples such as equivalent series resistances (ESR) and specific capacitances were also compared. In conclusion, this study showed that both of different preparation method would propose a simple method of ACM electrode preparation technique for supercapacitor applications.
Wei, Binnian; Feng, June; Rehmani, Imran J; Miller, Sharyn; McGuffey, James E; Blount, Benjamin C; Wang, Lanqing
2014-09-25
Most sample preparation methods characteristically involve intensive and repetitive labor, which is inefficient when preparing large numbers of samples from population-scale studies. This study presents a robotic system designed to meet the sampling requirements for large population-scale studies. Using this robotic system, we developed and validated a method to simultaneously measure urinary anatabine, anabasine, nicotine and seven major nicotine metabolites: 4-Hydroxy-4-(3-pyridyl)butanoic acid, cotinine-N-oxide, nicotine-N-oxide, trans-3'-hydroxycotinine, norcotinine, cotinine and nornicotine. We analyzed robotically prepared samples using high-performance liquid chromatography (HPLC) coupled with triple quadrupole mass spectrometry in positive electrospray ionization mode using scheduled multiple reaction monitoring (sMRM) with a total runtime of 8.5 min. The optimized procedure was able to deliver linear analyte responses over a broad range of concentrations. Responses of urine-based calibrators delivered coefficients of determination (R(2)) of >0.995. Sample preparation recovery was generally higher than 80%. The robotic system was able to prepare four 96-well plate (384 urine samples) per day, and the overall method afforded an accuracy range of 92-115%, and an imprecision of <15.0% on average. The validation results demonstrate that the method is accurate, precise, sensitive, robust, and most significantly labor-saving for sample preparation, making it efficient and practical for routine measurements in large population-scale studies such as the National Health and Nutrition Examination Survey (NHANES) and the Population Assessment of Tobacco and Health (PATH) study. Published by Elsevier B.V.
The FASES instrument development and experiment preparation for the ISS
NASA Astrophysics Data System (ADS)
Picker, Gerold; Gollinger, Klaus; Greger, Ralf; Dettmann, Jan; Winter, Josef; Dewandre, Thierry; Castiglione, Luigi; Vincent-Bonnieu, Sebastien; Liggieri, Libero; Clausse, Daniele; Antoni, Mickael
The FASES experiments target the investigation of the stability of emulsions. The main objec-tives are the study of the surfactant adsorption at the liquid / liquid interfaces, the interaction of the droplets as well as the behaviour of the liquid film between nearby drops. Particular focus is given to the dynamic droplet evolution during emulsion destabilisation. The results of the experiments shall support development of methods for the modelling of droplet size distri-butions, which are important to many industries using stable emulsions like food production, cosmetics and pharmaceutics or unstable emulsions as required for applications in waste water treatment or crude oil recovery. The development of the experimental instrumentation was initiated in 2002. The flight instru-ment hardware development was started in 2004 and finally the flight unit was completed in 2009. Currently the final flight preparation is proceeding targeting a launch to the International Space Station (ISS) with Progress 39P in September 2010. The experiment setup of the instrument is accommodated in a box type insert called Experiment Container (EC), which will be installed in the Fluid Science Laboratory part of the European Columbus module of the ISS. The EC is composed of two diagnostics instruments for the investigation of transparent and opaque liquid emulsion. The transparent emulsions will be subject to the experiment called "Investigations on drop/drop interactions in Transparent Emulsions" (ITEM). The opaque emulsion samples will be studied in the experiment called "Investigations on concentrated or opaque Emulsions and on Phase Inversions" (EMPI). The thermal conditioning unit (TCU) allows performing homogeneous thermalization, tem-perature sweeps, emulsion preparation by stirrer, and optical diagnostics with a scanning mi-croscope. The objective of the instrument is the 3D reconstruction of the emulsion droplet distribution in the liquid matrix in terms of the droplet sizes, location and their time depen-dent evolution. The TCU will be used for the stability experiment ITEM-S and the droplet freezing experiment ITEM-F. The Differential Scanning Calorimeter (DSC) will give an information about the evolution of the emulsion through the droplet size distribution and the dispersion state of the droplets within the emulsion during a controlled temperature sweep by measuring the latent heat of droplet freezing and melting during the EMPI experiments. For this purpose the calorimeter is equipped with a reference sample filled with a pure liquid matrix and a similar measurement sample filled with the specific emulsion under investigation. The differential heat flux between measurement sample and reference sample is measured with a sensitive heat flux sensor. Each instrument is serviced by a robotic sample stowage system, which accommodates in total 44 different ITEM and EMPI emulsion samples each filled with a specific composition of the emulsion. Currently the flight preparation is ongoing with particular focus on the preparation of the emulsion flight sample set and the instrument's operating parameters. The FASES flight instrument was developed by ASTRIUM Space Transportation Germany with support of RUAG Aerospace Wallisellen under ESA / ESTEC contract. The science team of FASES is supported by ESA/ESTEC (Microgravity Application Programme, AO99-052).
NASA Astrophysics Data System (ADS)
Ferguson, P. P.; Martine, M. L.; George, A. E.; Dahn, J. R.
Samples of Sn 30TM 30C 40 and of Sn 30Co 15TM 15C 40, with TM = 3d transition metals, were prepared by vertical-axis attritor milling. The structure and performance of these samples were studied by X-ray diffraction (XRD) and by electrochemical testing. The XRD patterns of Sn 30TM 30C 40 show an amorphous-like diffraction pattern only for the sample with TM = Co. The other prepared samples show broadened Bragg peaks of their main starting material, along with an amorphous-like background, even after 32 h of milling. Samples with TM = Co and TM = Ni show stable differential capacity versus potential plots and stable cycling for at least 100 cycles with reversible capacities of 425 and 250 mAh g -1, respectively. All samples prepared with 15 at.% Co show good capacity retention for at least 100 cycles ranging from 270 mAh g -1 for samples with TM = Ni to 500 mAh g -1 for samples with TM = Ti. The differential capacity versus potential plots for all the prepared Sn 30Co 15TM 15C 40 samples show similar structure to that of Sn 30Co 30C 40 except when TM = Cu. This shows the possibility of preparing tin-based negative electrode materials using a combination of cobalt and TM, especially if one looks to reduce the cobalt content.
Non-Contact Conductivity Measurement for Automated Sample Processing Systems
NASA Technical Reports Server (NTRS)
Beegle, Luther W.; Kirby, James P.
2012-01-01
A new method has been developed for monitoring and control of automated sample processing and preparation especially focusing on desalting of samples before analytical analysis (described in more detail in Automated Desalting Apparatus, (NPO-45428), NASA Tech Briefs, Vol. 34, No. 8 (August 2010), page 44). The use of non-contact conductivity probes, one at the inlet and one at the outlet of the solid phase sample preparation media, allows monitoring of the process, and acts as a trigger for the start of the next step in the sequence (see figure). At each step of the muti-step process, the system is flushed with low-conductivity water, which sets the system back to an overall low-conductivity state. This measurement then triggers the next stage of sample processing protocols, and greatly minimizes use of consumables. In the case of amino acid sample preparation for desalting, the conductivity measurement will define three key conditions for the sample preparation process. First, when the system is neutralized (low conductivity, by washing with excess de-ionized water); second, when the system is acidified, by washing with a strong acid (high conductivity); and third, when the system is at a basic condition of high pH (high conductivity). Taken together, this non-contact conductivity measurement for monitoring sample preparation will not only facilitate automation of the sample preparation and processing, but will also act as a way to optimize the operational time and use of consumables
Novel sustained-release dosage forms of proteins using polyglycerol esters of fatty acids.
Yamagata, Y; Iga, K; Ogawa, Y
2000-02-03
In order to develop a novel delivery system for proteins based on polyglycerol esters of fatty acids (PGEFs), we studied a model system using interferon-alpha (IFN-alpha) as the test protein. A cylindrical matrix was prepared by a heat extrusion technique using a lyophilized powder of the protein and 11 different types of synthetic PGEFs, which varied in degree of glycerol polymerization (di- and tetra-), chain length of fatty acids (myristate, palmitate and stearate) and degree of fatty acid esterification (mono-, di- and tri-). In an in-vitro release study using an enzyme-linked immunosorbent assay (ELISA) as a detection method, the matrices prepared from a monoglyceride (used for comparison) and from diglycerol esters exhibited a biphasic release pattern with a large initial burst followed by slow release. In contrast, the matrices prepared from tetraglycerol esters showed a steady rate of release without a large initial burst. In an in vivo release study, initial bursts of IFN-alpha release were, also, dramatically reduced when the matrices were prepared from the tetraglycerol esters of palmitate and stearate, and the mean residence time (MRT) of IFN-alpha was prolonged, whereas the matrices prepared from monoglyceride and from diglycerol esters showed large initial bursts of IFN-alpha release. Since the release rates from the matrices prepared from the tetraglycerol esters of palmitate and stearate were governed by Jander's equation modified for a cylindrical matrix, the release from those matrices was concluded to be a diffusion-controlled process. The bioavailability of IFN-alpha after implantation of the matrix formulation prepared using all types of PGEFs, except for tetraglycerol triesters, was almost equivalent to that after injection of IFN-alpha solution; consequently, IFN-alpha in these matrices appears to remain stable during the release period.
Negreira, N; Rodríguez, I; Rubí, E; Cela, R
2010-06-30
A novel, single step method for the determination of seven ink photo-initiators in carton packed milk samples is described. Solid-phase microextraction (SPME) and gas chromatography (GC), combined with mass spectrometry (MS), were used as sample preparation and determination techniques, respectively. Parameters affecting the performance of the microextraction process were thoroughly evaluated using uni- and multivariate optimization strategies, based on the use of experimental factorial designs. The coating of the SPME fibre, together with the sampling mode and the temperature were the factors playing a major influence on the efficiency of the extraction. Under final conditions, 1.5 mL of milk and 8.5 mL of ultrapure water were poured in a glass vessel, which was closed and immersed in a water boiling bath. A poly(dimethylsiloxane)-divinylbenzene (PDMS-DVB) coated fibre was exposed directly to the diluted sample for 40 min. After that, the fibre was desorbed in the injector of the GC-MS system for 3 min. The optimized method provided limits of quantification (LOQs) between 0.2 and 1 microg L(-1) and a good linearity in the range between 1 and 250 microg L(-1). The inter-day precision remained below 15% for all compounds in spiked whole milk. The efficiency of the extraction changed for whole, semi-skimmed and skimmed milk; however, no differences were noticed among the relative recoveries achieved for milk samples, from different brands, with the same fat content. Copyright 2010 Elsevier B.V. All rights reserved.
Comparison of stored umbilical cord blood and adult donor blood: transfusion feasibility.
Tokan, Rola Sahyoun; Arsan, Saadet; Erdeve, Omer; Solaz, Nuri; Avcı, Aslıhan; Ulkar, Serenay Elgün; Gülyapar, Elif; Ustünyurt, Zeynep; Bıyıklı, Zeynep; Kemahlı, Sabri
2012-09-01
This study aimed to compare the storage properties of red blood cell (RBC) concentrates of umbilical cordblood (UCB) and adult donor blood (ADB), and to evaluate the feasibility of UCB-RBC concentrate as an autologoussource for blood transfusion in very low birth weight (VLBW) preterm neonates. In all, 30 newborn (10 preterm, 20 full term) UCB and 31 ADB units were collected.RBC concentrates were stored and compared with regard to pH, potassium (K(+)), 2,3-biphosphoglycerate (2-3-BPG),adenosine tri-phosphate (ATP), plasma Hb, and bacterial contamination on d 1, 21, and 35 of storage. The K(+) level increased with time and differed significantly between storage d 1 and 21, and between storaged 1 and 35 in both the UCB and ADB units. Initial and d 21 K(+) levels were higher in the UCB units than in the ADBunits. The 2,3-BPG level did not differ significantly between the UCB-PRC and ADB-PRC samples. After 35 d of storageboth UCB-PRC and ADB-PRC samples exhibited significant differences from the initial free Hb, intracellular ATP, andpH values. Significant differences in intracellular ATP and pH were also observed between the UCB-PRC and ADB-PRCsamples. The volume of harvested and prepared UCB-PRC can be used for some of the blood transfusions requiredduring the neonatal period and thus may decrease the number of allogeneic transfusions, especially in preterm newborns.The hematological and biochemical changes that occurred in UCB during storage were comparable with those observedin ADB, and do not pose a risk to the immature metabolism of neonates. UCB-RPC prepared and stored under standardconditions can be a safe alternative RBC source for transfusions in VLBW newborns.
Tu, Xijuan; Sun, Fanyi; Wu, Siyuan; Liu, Weiyi; Gao, Zhaosheng; Huang, Shaokang; Chen, Wenbin
2018-01-15
Homogeneous liquid-liquid extraction (h-LLE) has been receiving considerable attention as a sample preparation method due to its simple and fast partition of compounds with a wide range of polarities. To better understand the differences between the two h-LLE extraction approaches, salting-out assisted liquid-liquid extraction (SALLE) and sugaring-out assisted liquid-liquid extraction (SULLE), have been compared for the partition of 10-hydroxy-2-decenoic acid (10-HDA) from royal jelly, and for the co-extraction of proteins. Effects of the amount of phase partition agents and the concentration of acetonitrile (ACN) on the h-LLE were discussed. Results showed that partition efficiency of 10-HDA depends on the phase ratio in both SALLE and SULLE. Though the partition triggered by NaCl and glucose is less efficient than MgSO 4 in the 50% (v/v) ACN-water mixture, their extraction yields can be improved to be similar with that in MgSO 4 SALLE by increasing the initial concentration of ACN in the ACN-water mixture. The content of co-extracted protein was correlated with water concentration in the obtained upper phase. MgSO 4 showed the largest protein co-extraction at the low concentration of salt. Glucose exhibited a large protein co-extraction in the high phase ratio condition. Furthermore, NaCl with high initial ACN concentration is recommended because it produced high extraction yield for 10-HDA and the lowest amount of co-extracted protein. These observations would be valuable for the sample preparation of royal jelly. Copyright © 2017 Elsevier B.V. All rights reserved.
NASA Astrophysics Data System (ADS)
Bugaj, Joseph E.; Dorshow, Richard B.
2014-03-01
The fluorescent tracer agent 2,5-bis[N-(1-carboxy-2-hydroxy)]carbamoyl-3,6-diaminopyrazine, designated APC-2, has been developed with properties and attributes necessary for use as a direct measure of glomerular filtration rate (GFR). Comparison to known standard exogenous GFR agents in animal models has demonstrated an excellent correlation. A clinical trial to demonstrate this same correlation in humans is in preparation. A battery of formal toxicity tests necessary for regulatory clearance to proceed with a clinical trial has been recently completed on this new fluorescent tracer agent. These include single dose toxicity studies in rats and dogs to determine overall toxicity and toxicokinetics of the compound. Blood compatibility, mutation assay, chromosomal aberration assay, and several other assays were also completed. Toxicity assessments were based on mortality, clinical signs, body weight, food consumption and anatomical pathology. Blood samples were collected to assess pharmacokinetic parameters including half-life, area under the curve, and clearance. Urine samples were collected to assess distribution. Doses of up to 200-300 times the estimated human dose were administered. No test-article related effects were noted on body weight, food consumption, ophthalmic observations and no abnormal pathology was seen in either macroscopic or microscopic evaluations of any organs or tissues. All animals survived to scheduled sacrifice. Transient discoloration of skin and urine was noted at the higher dose levels in both species as expected from a highly fluorescent compound and was not considered pathological. Thus initial toxicology studies of this new fluorescent tracer agent APC-2 have resulted in no demonstrable pathological test article concerns.
Results of Hg speciation testing on DWPF SMECT-4, SMECT-6, and RCT-2 samples
DOE Office of Scientific and Technical Information (OSTI.GOV)
Bannochie, C. J.
2016-02-04
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 fifteenth shipment of samples was designated to include Defense Waste Processing Facility (DWPF) Slurry Mix Evaporator Condensate Tank (SMECT) samples from Sludge Receipt and Adjustment Tank (SRAT) Batch 738 and a Recycle Condensate Tank (RCT) sample from SRAT Batch 736. The DWPF sample designations for the three samples analyzed are provided in Table 1. The Batch 738 ‘Baseline’ SMECT sample was taken priormore » to Precipitate Reactor Feed Tank (PRFT) addition and concentration and therefore, precedes the SMECT-5 sample reported previously. iii The Batch 738 ‘End of SRAT Cycle’ SMECT sample was taken at the conclusion of SRAT operations for this batch (PRFT addition/concentration, acid additions, initial concentration, MCU addition, and steam stripping). 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 SRAT Cycle’ SMECT-6 sample. The Batch 736 ‘After SME’ RCT sample was taken after completion of SMECT transfers at the end of the SME cycle.« less
Lessons learnt on recruitment and fieldwork from a pilot European human biomonitoring survey.
Fiddicke, Ulrike; Becker, Kerstin; Schwedler, Gerda; Seiwert, Margarete; Joas, Reinhard; Joas, Anke; Biot, Pierre; Aerts, Dominique; Casteleyn, Ludwine; Dumez, Birgit; Castaño, Argelia; Esteban, Marta; Angerer, Jürgen; Koch, Holger M; Schoeters, Greet; Den Hond, Elly; Sepai, Ovnair; Exley, Karen; Knudsen, Lisbeth E; Horvat, Milena; Bloemen, Louis; Katsonouri, Andromachi; Hadjipanayis, Adamos; Cerna, Milena; Krsková, Andrea; Jensen, Janne Fangel; Nielsen, Jeanette K S; Rudnai, Peter; Közepésy, Szilvia; Gutleb, Arno C; Fischer, Marc E; Ligocka, Danuta; Kamińska, Joanna; Reis, M Fátima; Namorado, Sónia; Lupsa, Ioana-Rodica; Gurzau, Anca E; Halzlová, Katarína; Mazej, Darja; Tratnik, Janja Snoj; Rivas, Teresa C; Gómez, Silvia; Berglund, Marika; Larsson, Kristin; Lehmann, Andrea; Crettaz, Pierre; Dewolf, Marie-Christine; Burns, Damien; Kellegher, Anne; Kolossa-Gehring, Marike
2015-08-01
Within the European Environment and Health Action Plan an initiative to establish a coherent human biomonitoring approach in Europe was started. The project COPHES (COnsortium to Perform Human biomonitoring on a European Scale ) developed recommendations for a harmonized conduct of a human biomonitoring (HBM) survey which came into action as the pilot study DEMOCOPHES (DEMOnstration of a study to COordinate and Perform Human biomonitoring on a European Scale). Seventeen European countries conducted a survey with harmonized instruments for, inter alia, recruitment, fieldwork and sampling, in autumn/winter 2011/2012. Based on the countries' experiences of conducting the pilot study, following lessons learnt were compiled: the harmonized fieldwork instruments (basic questionnaire, urine and hair sampling) turned out to be very valuable for future HBM surveys on the European scale. A school approach was favoured by most of the countries to recruit school-aged children according to the established guidelines and country specific experiences. To avoid a low participation rate, intensive communication with the involved institutions and possible participants proved to be necessary. The communication material should also include information on exclusion criteria and offered incentives. Telephone contact to the participants the day before fieldwork during the survey can prevent the forgetting of appointments and first morning urine samples. To achieve comparable results on the European scale, training of interviewers in all issues of recruitment, fieldwork and sampling through information material and training sessions is crucial. A survey involving many European countries needs time for preparation and conduct. Materials for quality control prepared for all steps of recruitment, fieldwork and sampling proved to be important to warrant reliable results. Copyright © 2014 Elsevier Inc. All rights reserved.
Li, Mengqing; Forest, Jean-Marc; Coursol, Christian; Leclair, Grégoire
2011-09-01
The stability of cyclosporine diluted to 0.2 or 2.5 mg/mL with 0.9% sodium chloride injection or 5% dextrose injection and stored in polypropylene-polyolefin containers or polypropylene syringes was evaluated. Intravenous cyclosporine solutions (0.2 and 2.5 mg/mL) were aseptically prepared and transferred to 250-mL polypropylene-polyolefin bags or 60-mL polypropylene syringes. Chemical stability was measured using a stability-indicating high-performance liquid chromatography (HPLC) assay. Physical stability was assessed by visual inspection and a dynamic light scattering (DLS) method. After 14 days, HPLC assay showed that the samples of i.v. cyclosporine stored in polypropylene-polyolefin bags remained chemically stable (>98% of initial amount remaining); the physical stability of the samples was confirmed by DLS and visual inspection. The samples stored in polypropylene syringes were found to contain an impurity (attributed to leaching of a syringe component by the solution) that could be detected by HPLC after 1 day; on further investigation, no leaching was detected when the syringes were exposed to undiluted i.v. cyclosporine 50 mg/mL for 10 minutes. Samples of i.v. cyclosporine solutions of 0.2 and 2.5 mg/mL diluted in 0.9% sodium chloride injection or 5% dextrose injection and stored at 25 °C in polypropylene-polyolefin bags were physically and chemically stable for at least 14 days. When stored in polypropylene syringes, the samples were contaminated by an impurity within 1 day; however, the short-term (i.e., ≤10 minutes) use of the syringes for the preparation and transfer of i.v. cyclosporine solution is considered safe.
NASA Astrophysics Data System (ADS)
Pfisterer, Kaylen J.; Amelard, Robert; Wong, Alexander
2018-02-01
Dysphagia (swallowing difficulty) increases risk for malnutrition and affects at least 15% of American older adults, and 590 million people worldwide. Malnutrition is associated with increased mortality, increased morbidity, decreased quality of life, and accounts for over $15 billion (USD) health-care related costs each year. While modified texture diets (e.g., puréed food) reduce the risk of choking, quality assurance is necessary for monitoring nutrient density to ensure food meets nutritional requirements. However, current methods are subjective and time consuming. The purpose of this study was to investigate the feasibility of optical techniques for an objective assessment of food nutrient density in puréed samples. Motivated by a theoretical optical dilution model, broadband spectral images of commercially prepared purée samples were acquired. Specifically, 13 flavors at five dilutions relative to initial concentration, each with six replicates, were acquired for a total of 390 samples. Purée samples were prepared and loaded onto a white reflectance back plane to maximize photon traversal path length through the purée. The sample was illuminated with a tungsten-halogen illumination source fitted with a front glass fabric diffuser for spatially homogeneous illumination. This broadband illuminant was chosen to observe as many food-light spectral absorbance interactions as possible. Flavor-stratified correlation analysis was performed on this food image dataset to investigate the relationship between nutritional information and color space transformations. A special case of blueberry is presented as the effect of anthocyanins was quantitatively observed through normalized spectral trends in response to pH perturbations across dilutions.
SU-F-T-550: Radiochromic Plastic Thin Sheet Dosimeter: Initial Performance
DOE Office of Scientific and Technical Information (OSTI.GOV)
Jordan, K; Adamovics, J
Purpose: Thin sheets, of a high sensitivity formulation of radiochromic dosimeter, Presage were prepared and evaluated for optical readout. Methods: Sheets of radiochromic polyurethane, 12 cm long, 10 cm wide and 0.2 cm thick were prepared with leuco crystal violet as the reporter molecule. Sample transmission was evaluated at a wavelength of 590 nm with in-house constructed instruments: optical cone beam laser CT scanner, fixed and scanning spot densitometers. Sample sequential irradiations to a total dose of 40 Gy were conducted with a modified, Theratron 60, cobalt radiotherapy machine at dose rates of 1 or 0.25 Gy per minute. Exposuremore » to ambient and readout light was minimized to limit background photochromic signals. Samples were stored at 4°C. Optical activity was assessed from linearly polarized transmission images. Comparison sensitivity measurements with EBT3 film were conducted. Results: Samples were transparent, smooth and pale purple before irradiation. Radiochromic reaction was completed in less than 5 minutes. A linear dose response with a sensitivity of 0.5 cm-1Gy-1 was observed. Micrometer measurements found sheet thickness variations up to 20%. Uniform dose, 2 Gy attenuation images, correlated with local sheet thicknesses. Comparable measurements with EBT3 film were 3 times more sensitive at 1 Gy but above 15 Gy, EBT3 film had lower sensitivity than 0.2 cm thick Presage sheet dosimeter due to its non-linear response. Conclusion: Dose sensitivity provided a 10% decrease in transmission for a 1 Gy dose. Improvements in mold design are expected to allow production of sheets with less than 5% variation in thickness. Above, 10 Gy, Presage sheet dosimeter performance expected to exceed EBT3 film based on linearity, sensitivity, transparency and smoothness of samples. J Adamovics is owner of Heuris Inc.« less
Nestić, Marina; Babić, Sandra; Pavlović, Dragana Mutavdžić; Sutlović, Davorka
2013-09-10
In presented paper analytical method based on solid-phase extraction using molecularly imprinted polymer and gas chromatography-mass spectrometry has been developed and validated for the confirmation of THC, THC-OH and THC-COOH in urine samples. Non-covalent molecularly imprinted polymers of THC-OH were prepared using different functional monomers (methacrylic acid, 4-vinylpyridine, and 2-hydroxyethyl methacrylate), ethylene glycol dimethacrylate as a cross-linker and 2,2'-azobis-isobutyronitrile as an initiator of radical polymerization. Analytes were extracted from urine samples using prepared polymer sorbent with highest binding selectivity and capability. Before extraction, urine samples were hydrolyzed with alkaline. Elution was performed with chloroform:ethyl acetate (60:40, v/v). Dry extracts were silylated with BSTFA+1% TMCS. Detection and quantification were performed using gas chromatography-mass spectrometry in single ion recording mode. The developed method was linear over the range from LOQ to 150 ng mL(-1) for all three analytes. For THC, THC-OH and THC-COOH LOD was 2.5, 1 and 1 ng mL(-1), and LOQ was 3, 2 and 2 ng mL(-1), respectively. The precision, accuracy, recovery and matrix effect were investigated at 5, 25 and 50 ng mL(-1). In the investigated concentration range recoveries were 71.9% for THC, 78.6% for THC-OH and 75.2% for THC-COOH. Matrix effect was not significant (<10%) for all analytes in the concentration range from 5 ng mL(-1) to 50 ng mL(-1). Extraction recovery on non-imprinted polymer was relatively high indicating high non-specific binding. Optimized and validated method was applied to 15 post-mortem urine samples. Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.
Rutten, Niels; Gonzales, José L.; Elbers, Armin R. W.; Velthuis, Annet G. J.
2012-01-01
Background As low pathogenic avian influenza viruses can mutate into high pathogenic viruses the Dutch poultry sector implemented a surveillance system for low pathogenic avian influenza (LPAI) based on blood samples. It has been suggested that egg yolk samples could be sampled instead of blood samples to survey egg layer farms. To support future decision making about AI surveillance economic criteria are important. Therefore a cost analysis is performed on systems that use either blood or eggs as sampled material. Methodology/Principal Findings The effectiveness of surveillance using egg or blood samples was evaluated using scenario tree models. Then an economic model was developed that calculates the total costs for eight surveillance systems that have equal effectiveness. The model considers costs for sampling, sample preparation, sample transport, testing, communication of test results and for the confirmation test on false positive results. The surveillance systems varied in sampled material (eggs or blood), sampling location (farm or packing station) and location of sample preparation (laboratory or packing station). It is shown that a hypothetical system in which eggs are sampled at the packing station and samples prepared in a laboratory had the lowest total costs (i.e. € 273,393) a year. Compared to this a hypothetical system in which eggs are sampled at the farm and samples prepared at a laboratory, and the currently implemented system in which blood is sampled at the farm and samples prepared at a laboratory have 6% and 39% higher costs respectively. Conclusions/Significance This study shows that surveillance for avian influenza on egg yolk samples can be done at lower costs than surveillance based on blood samples. The model can be used in future comparison of surveillance systems for different pathogens and hazards. PMID:22523543
Stability of Levothyroxine in Sodium Chloride for IV Administration.
Strong, Dawn K; Decarie, Diane; Ensom, Mary H H
2010-11-01
Levothyroxine by IV administration is often prescribed in the intensive care unit for the management of potential solid organ donors, following declaration of brain death and provision of consent for organ donation. Published data on the stability of levothyroxine in IV solutions are limited. To evaluate the physical compatibility and chemical stability, over a 24-h period, of 2 concentrations of levothyroxine in 0.9% sodium chloride with storage at room temperature and with exposure to or protection from light. Levothyroxine solutions (0.4 μg/mL and 2.0 μg/mL) were prepared in 50-mL minibags of 0.9% NaCl and stored at room temperature (25°C) with exposure to or protection from light. Samples were collected from each minibag at time 0 and after 0.5, 1.0, 1.5, 2.0, 3.0, 4.0, 8.0, 12.0, and 24.0 h. The samples were analyzed in triplicate with a validated stability-indicating high-performance liquid chromatography method using ultraviolet detection. A solution was considered stable if it maintained 90% of its initial concentration of levothyroxine. Changes in colour, clarity, and pH were assessed to determine the physical compatibility of the solutions. All samples remained clear, colourless, and free of precipitate throughout the study, and there were no significant changes in pH. Based on the 95% confidence interval of the slope of the curve relating concentration to time determined by linear regression, solutions of levothyroxine with concentration 0.4 μg/mL would maintain at least 90% of the initial concentration for 16.9 h with exposure to light and for 18.0 h if kept in the dark. Solutions of levothyroxine with concentration 2.0 μg/mL would maintain at least 90% of the initial concentration for 6.5 h with exposure to light and for 12.0 h if kept in the dark, with 95% confidence. Extemporaneously prepared solutions of levothyroxine in 0.9% NaCl can be expected to remain stable for at least 6.5 h if stored without protection from light and at least 12 h if stored in the dark. Stability is related to concentration, with more dilute solutions having greater stability.
Stability of levamisole oral solutions prepared from tablets and powder.
Chiadmi, Fouad; Lyer, Abdel; Cisternino, Salvatore; Toledano, Audrey; Schlatter, Joël; Ratiney, Robert; Fontan, Jean-Eudes
2005-08-12
To study the stability of levamisole oral solutions (25 mg/mL) prepared from powder and tablets stored at 4 +/- 3 degrees C and 23 +/- 2 degrees C in amber glass prescription bottles. Levamisole 25 mg/mL solutions were prepared from commercially available 50-mg tablets or from pure powder in sterile water. Levamisole concentrations were determined in duplicate by a stability-indicating HPLC method at 0, 1, 2, 3, 4, 7, 14, 30, 60 and 90 days. The initial and final pHs of solutions were measured. The recovery of levamisole from tablets was 100 +/- 2.1%. No color or odour changes were observed during the study period. The oral solutions prepared from powder were stable at least 90 days stored at 4 and 23 degrees C. The oral solutions prepared from tablets were stable at least 90 days at 4 degrees C and 15 days when stored at 23 degrees C. The initial pH of solutions prepared from powder and tablets were 5.30 and 4.55, respectively. Initial and final pH values were significantly different (p<0.001) for the two solutions. Levamisole 25 mg/mL oral solutions can be prepared from tablets or powder with sterile water for irrigation and stored for 90 days under refrigeration, taking account of the lack of microbiological contamination.
NASA Technical Reports Server (NTRS)
Fraser, A. S.; Wells, A. F.; Tenoso, H. J. (Inventor)
1978-01-01
The performance of a waste water reclamation system is monitored by introducing a non-pathogenic marker virus, bacteriophage F2, into the waste-water prior to treatment and, thereafter, testing the reclaimed water for the presence of the marker virus. A test sample is first concentrated by absorbing any marker virus onto a cellulose acetate filter in the presence of a trivalent cation at low pH and then flushing the filter with a limited quantity of a glycine buffer solution to desorb any marker virus present on the filter. Photo-optical detection of indirect passive immune agglutination by polystyrene beads indicates the performance of the water reclamation system in removing the marker virus. A closed system provides for concentrating any marker virus, initiating and monitoring the passive immune agglutination reaction, and then flushing the system to prepare for another sample.
NASA Astrophysics Data System (ADS)
Faraji, Nastaran; Mahmood Mat Yunus, W.; Kharazmi, Alireza; Saion, Elias; Behzad, Kasra
2014-01-01
CdS nanofluids were prepared by the gamma-radiation method at different radiation doses. The samples were characterized by UV-Vis spectroscopy and transmission electron microscopy. The open cell photoacoustic technique was used to measure the thermal effusivity of the CdS nanocomposites. In this technique a He-Ne laser was used as the excitation source and was operated at 632.8 nm with an output power of 70 mW. The precision and accuracy of this technique were initially established by measuring the thermal effusivity of distilled water and ethylene glycol. The thermal-effusivity values of these two samples were found to be close to the values reported in the literature. The thermal effusivity of CdS nanofluids decreased from (0.453 to 0.268) with increased dosage of gamma radiation.
Wang, Hao; Tian, Zhixin
2018-06-06
Analysis of phosphoproteins always faces the challenge of low stoichiometry, which demands highly selective and efficient enrichment in the initial sample preparation. Here we report our synthesis of the novel titanium (IV) ion immobilized adenosine triphosphate functionalized silica nanoparticles (Ti 4+ -ATP-NPs) for efficient enrichment of intact phosphoproteins. The average diameter of Ti 4+ -ATP-NPs was about 128 nm with good dispersibility and the saturated adsorption capacity for β-casein was 1046.5 mg/g. In addition, Ti 4+ -ATP-NPs exhibited high specificity and selectivity in enriching phosphoproteins from both standard protein mixtures and complex biological samples (non-fat milk, chicken egg white and mouse heart tissue extract) as demonstrated by SDS-PAGE. Copyright © 2018 Elsevier B.V. All rights reserved.
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.
Saed, Mohand O; Torbati, Amir H; Nair, Devatha P; Yakacki, Christopher M
2016-01-19
This study presents a novel two-stage thiol-acrylate Michael addition-photopolymerization (TAMAP) reaction to prepare main-chain liquid-crystalline elastomers (LCEs) with facile control over network structure and programming of an aligned monodomain. Tailored LCE networks were synthesized using routine mixing of commercially available starting materials and pouring monomer solutions into molds to cure. An initial polydomain LCE network is formed via a self-limiting thiol-acrylate Michael-addition reaction. Strain-to-failure and glass transition behavior were investigated as a function of crosslinking monomer, pentaerythritol tetrakis(3-mercaptopropionate) (PETMP). An example non-stoichiometric system of 15 mol% PETMP thiol groups and an excess of 15 mol% acrylate groups was used to demonstrate the robust nature of the material. The LCE formed an aligned and transparent monodomain when stretched, with a maximum failure strain over 600%. Stretched LCE samples were able to demonstrate both stress-driven thermal actuation when held under a constant bias stress or the shape-memory effect when stretched and unloaded. A permanently programmed monodomain was achieved via a second-stage photopolymerization reaction of the excess acrylate groups when the sample was in the stretched state. LCE samples were photo-cured and programmed at 100%, 200%, 300%, and 400% strain, with all samples demonstrating over 90% shape fixity when unloaded. The magnitude of total stress-free actuation increased from 35% to 115% with increased programming strain. Overall, the two-stage TAMAP methodology is presented as a powerful tool to prepare main-chain LCE systems and explore structure-property-performance relationships in these fascinating stimuli-sensitive materials.
Hashemzadeh, Fatemeh; Gaffarinejad, Ali; Rahimi, Rahmatollah
2015-04-09
Porous NiO/Nb2O5 nanocomposites with Ni/Nb molar ratio of 0.4, 0.8 and 1.2 have been obtained via the EISA route using P123 copolymer as organic template, and are assigned as NiNb0.4, NiNb0.8 and NiNb1.2, respectively. For comparison, pure Nb2O5 sample assigned as NiNb0.0 was also synthesized by the same method. Structural and textural features of the as prepared samples were investigated by XRD, FTIR, FE-SEM, EDX, UV-vis DRS and BET techniques. The results indicated that the porous p-NiO/n-Nb2O5 junction nanocomposites were formed and coupling of NiO with Nb2O5 resulted a remarkable red shift in the optical response of the nanocomposite samples. The photocatalytic properties of the nanocomposite samples, and also synthesized pure Nb2O5 (NiNb0.0) and commercial Nb2O5 as reference catalysts were evaluated for the first time by simultaneous Cr(VI) reduction and MO decolorization in aqueous suspension under visible light irradiation at pH 2. NiNb0.4 was found to be the most active photocatalyst, which might be attributed to the extended absorption in the visible light region and the effective photogenerated electron-hole separation by the photosynergistic effects of the p-NiO/n-Nb2O5 composite powder. The photocatalytic efficiency of the most active photocatalyst, NiNb0.4, was found to be rather low for either single Cr(VI) solution or single MO solution. However, the photocatalytic reduction of Cr(VI) and photocatalytic decolorization of MO proceed more rapidly for the coexistence system of Cr(VI) and MO than for the single process, showing synergetic effect between the reduction and decolorization reactions. The effects of initial concentration of Cr(VI), MO and the initial pH value on the rate of simultaneous photoreactions over NiNb0.4 sample, were also investigated. The Cr(VI) and MO removal rates were further enhanced by increasing MO and Cr (VI) concentration to an optimal value, respectively, and/or decreasing solution pH. Copyright © 2014 Elsevier B.V. All rights reserved.
Song, Wenji; Zhao, Chen; Lercher, Johannes A
2013-07-22
Improved synthetic approaches for preparing small-sized Ni nanoparticles (d=3 nm) supported on HBEA zeolite have been explored and compared with the traditional impregnation method. The formation of surface nickel silicate/aluminate involved in the two precipitation processes are inferred to lead to the stronger interaction between the metal and the support. The lower Brønsted acid concentrations of these two Ni/HBEA catalysts compared with the parent zeolite caused by the partial exchange of Brønsted acid sites by Ni(2+) cations do not influence the hydrodeoxygenation rates, but alter the product selectivity. Higher initial rates and higher stability have been achieved with these optimized catalysts for the hydrodeoxygenation of stearic acid and microalgae oil. Small metal particles facilitate high initial catalytic activity in the fresh sample and size uniformity ensures high catalyst stability. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
ERIC Educational Resources Information Center
Christian, Karen Jeanne
2011-01-01
Students often use study groups to prepare for class or exams; yet to date, we know very little about how these groups actually function. This study looked at the ways in which undergraduate organic chemistry students prepared for exams through self-initiated study groups. We sought to characterize the methods of social regulation, levels of…
Hydrologic characteristics of benchmark soils of Hawaii’s forest watersheds-
L. R. Ahuja; S. A. El-Swaify
1975-01-01
The project was initiated in May, 1972. the initial effort involved mapping of forest soils on the islands of Oahu and Kawaii, and collection of relevant literature for preparing the study plan. The detailed study plan (el-Swaify, 1972) was prepared after cooperative discussions with staff of the Institute of Pacific Islands Forestry, Honolulu, Hawaii, and set forth...
A Simplified Extemporaneously Prepared Potassium Chloride Oral Solution.
Tannous, Elias; Tal, Yana; Amarny, Kamal
2016-01-01
Although commercial preparations of oral potassium supplements are usually available, there are times when our Medical Center is faced with situations in which the oral solution of potassium chloride is not available. This solution is necessary for our pediatric outpatients who cannot swallow tablets and need an oral solution. Moreover, there are no studies available which describe an extemporaneously prepared potassium chloride oral solution on which we can rely for assigning a beyond-use date. The aim of this study was to formulate an extemporaneous pediatric oral solution of potassium chloride and to determine the physical and chemical stability of this preparation. We prepared 1 mMoL/mL by withdrawing 25 mL of potassium chloride 14.9%. Ora-Sweet SF was added to 50 mL in a metered flask. The solution was kept refrigerated (2°C to 8°C). Samples were withdrawn to measure potassium concentration, pH, and microbial overgrowth. The test was performed by our biochemical laboratory. The oral solution of potassium chloride 1 mMoL/mL stored at 2°C to 8°C maintained at least 91% of the initial concentration for 28 days. There were no notable changes in pH, and the solution remained physically stable with no visual microbial growth. The oral solution of potassium chloride 1 mMoL/mL prepared in Ora-Sweet and stored at 2°C to 8°C in amber glass bottles is expected to remain stable for 28 days. Copyright© by International Journal of Pharmaceutical Compounding, Inc.
Posterior quantum dynamics for a continuous diffusion observation of a coherent channel
NASA Astrophysics Data System (ADS)
Dąbrowska, Anita; Staszewski, Przemysław
2012-11-01
We present the Belavkin filtering equation for the intense balanced heterodyne detection in a unitary model of an indirect observation. The measuring apparatus modelled by a Bose field is initially prepared in a coherent state and the observed process is a diffusion one. We prove that this filtering equation is relaxing: any initial square-integrable function tends asymptotically to a coherent state with an amplitude depending on the coupling constant and the initial state of the apparatus. The time-development of a squeezed coherent state is studied and compared with the previous results obtained for the measuring apparatus prepared initially in the vacuum state.
Initial dissolution kinetics of cocrystal of carbamazepine with nicotinamide.
Hattori, Yusuke; Sato, Maiko; Otsuka, Makoto
2015-11-01
Objectives of this study are investigating the initial dissolution kinetics of the cocrystal of carbamazepine (CBZ) with nicotinamide (NIC) and understanding its initial dissolution process. Cocrystal solids of CBZ with NIC were prepared by co-milling and solvent evaporation methods. The formation of cocrystal solid was verified via X-ray diffraction measurement. Dissolution tests of the solids were performed using an original flow cell and ultraviolet-visible spectroscopic detector. The spectra monitored in situ were analyzed to determine the dissolved compounds separately using the classical least squares regression method. The initial dissolution profiles were interpreted using simultaneous model of dissolution and phase changes. In the initial dissolution, CBZ in the cocrystal structure dissolved in water and it was suggested that CBZ reached a metastable intermediate state simultaneously with dissolution. The cocrystal solid prepared by solvent evaporation provided a higher rate constant of the phase change than that prepared by co-milling. Our results thus support the use of evaporation as the method of choice to produce ordered cocrystal structures. We suggest that CBZ forms dihydrate during the dissolution process; however, during the initial phase of dissolution, CBZ changes to a metastable intermediate phase. © 2015 Royal Pharmaceutical Society.
Zhang, Jie; Wei, Shimin; Ayres, David W; Smith, Harold T; Tse, Francis L S
2011-09-01
Although it is well known that automation can provide significant improvement in the efficiency of biological sample preparation in quantitative LC-MS/MS analysis, it has not been widely implemented in bioanalytical laboratories throughout the industry. This can be attributed to the lack of a sound strategy and practical procedures in working with robotic liquid-handling systems. Several comprehensive automation assisted procedures for biological sample preparation and method validation were developed and qualified using two types of Hamilton Microlab liquid-handling robots. The procedures developed were generic, user-friendly and covered the majority of steps involved in routine sample preparation and method validation. Generic automation procedures were established as a practical approach to widely implement automation into the routine bioanalysis of samples in support of drug-development programs.
A high-throughput semi-automated preparation for filtered synaptoneurosomes.
Murphy, Kathryn M; Balsor, Justin; Beshara, Simon; Siu, Caitlin; Pinto, Joshua G A
2014-09-30
Synaptoneurosomes have become an important tool for studying synaptic proteins. The filtered synaptoneurosomes preparation originally developed by Hollingsworth et al. (1985) is widely used and is an easy method to prepare synaptoneurosomes. The hand processing steps in that preparation, however, are labor intensive and have become a bottleneck for current proteomic studies using synaptoneurosomes. For this reason, we developed new steps for tissue homogenization and filtration that transform the preparation of synaptoneurosomes to a high-throughput, semi-automated process. We implemented a standardized protocol with easy to follow steps for homogenizing multiple samples simultaneously using a FastPrep tissue homogenizer (MP Biomedicals, LLC) and then filtering all of the samples in centrifugal filter units (EMD Millipore, Corp). The new steps dramatically reduce the time to prepare synaptoneurosomes from hours to minutes, increase sample recovery, and nearly double enrichment for synaptic proteins. These steps are also compatible with biosafety requirements for working with pathogen infected brain tissue. The new high-throughput semi-automated steps to prepare synaptoneurosomes are timely technical advances for studies of low abundance synaptic proteins in valuable tissue samples. Copyright © 2014 Elsevier B.V. All rights reserved.
Thermoluminescence property of nano scale Al{sub 2}O{sub 3}: C by combustion method
DOE Office of Scientific and Technical Information (OSTI.GOV)
Bharthasaradhi, R.; Nehru, L. C.
In this study, thermoluminescence dosimetry material of carbon doped aluminium oxide by combustion method using Aluminium nitrate and Glycine. The Structure of the prepared Sample was carried out by XRD. The sample was nano crystalline in nature. Having hexagonal structure with unit cell parameters a=4.75Å, C=12.99Å. The surface morphology of the prepared nanopowder was carried out through (SEM). The morphology of the prepared sample is platelet structure and functional group analysis carried out through FT-IR Spectrum. The prepared sample was irradiated through γ-ray CO{sup 60} (100 Gy) was used as γ-ray source. The thermoluminescence glow curve of the irradiated samplemore » showed an isolated peak at around 200°C. The result suggest the prepared nanopowder is suitable for medical radiation dosimetry.« less
NASA Astrophysics Data System (ADS)
Quintela, Irwin A.; de Los Reyes, Benildo G.; Lin, Chih-Sheng; Wu, Vivian C. H.
2015-01-01
A simultaneous direct detection of Shiga-toxin producing strains of E. coli (STEC; ``Big Six'' - O26, O45, O103, O111, O121, and O145) as well as O157 strains by optical biosensing with oligonucleotide-functionalized gold nanoparticles (AuNPs) was developed. Initially, conserved regions of stx genes were amplified by asymmetric polymerase chain reaction (asPCR). Pairs of single stranded thiol-modified oligonucleotides (30-mer) were immobilized onto AuNPs and used as probes to capture regions of stx1 (119-bp) and/or stx2 (104-bp) genes from STEC strains. DNA samples from pure cultures and food samples were sandwich hybridized with AuNP-oligo probes at optimal conditions (50 °C, 30 min). A complex was formed from the hybridization of AuNP-probes and target DNA fragments that retained the initial red color of the reaction solutions. For non-target DNA, a color change from red to purplish-blue was observed following an increase in salt concentration, thus providing the basis of simultaneous direct colorimetric detection of target DNA in the samples. Enrichment and pooling systems were incorporated to efficiently process a large number of food samples (ground beef and blueberries) and detection of live targets. The detection limit was <1 log CFU g-1, requiring less than 1 h to complete after DNA sample preparation with 100% specificity. Gel electrophoresis verified AuNP-DNA hybridization while spectrophotometric data and transmission electron microscope (TEM) images supported color discrimination based on the occurrence of molecular aggregation. In conclusion, the significant features of this approach took advantage of the unique colorimetric properties of AuNPs as a low-cost and simple approach yet with high specificity for simultaneous detection of STEC strains.A simultaneous direct detection of Shiga-toxin producing strains of E. coli (STEC; ``Big Six'' - O26, O45, O103, O111, O121, and O145) as well as O157 strains by optical biosensing with oligonucleotide-functionalized gold nanoparticles (AuNPs) was developed. Initially, conserved regions of stx genes were amplified by asymmetric polymerase chain reaction (asPCR). Pairs of single stranded thiol-modified oligonucleotides (30-mer) were immobilized onto AuNPs and used as probes to capture regions of stx1 (119-bp) and/or stx2 (104-bp) genes from STEC strains. DNA samples from pure cultures and food samples were sandwich hybridized with AuNP-oligo probes at optimal conditions (50 °C, 30 min). A complex was formed from the hybridization of AuNP-probes and target DNA fragments that retained the initial red color of the reaction solutions. For non-target DNA, a color change from red to purplish-blue was observed following an increase in salt concentration, thus providing the basis of simultaneous direct colorimetric detection of target DNA in the samples. Enrichment and pooling systems were incorporated to efficiently process a large number of food samples (ground beef and blueberries) and detection of live targets. The detection limit was <1 log CFU g-1, requiring less than 1 h to complete after DNA sample preparation with 100% specificity. Gel electrophoresis verified AuNP-DNA hybridization while spectrophotometric data and transmission electron microscope (TEM) images supported color discrimination based on the occurrence of molecular aggregation. In conclusion, the significant features of this approach took advantage of the unique colorimetric properties of AuNPs as a low-cost and simple approach yet with high specificity for simultaneous detection of STEC strains. Electronic supplementary information (ESI) available. See DOI: 10.1039/c4nr05869k
Deepwater Gulf of Mexico turbidites -- Compaction effects on porosity and permeability
DOE Office of Scientific and Technical Information (OSTI.GOV)
Ostermeier, R.M.
1995-06-01
The deepwater Gulf of Mexico is now a major area of activity for the US oil industry. Compaction causes particular concern because most prospective deepwater reservoirs are highly geo-pressured and many have limited aquifer support; water injection may also be problematic. To address some of the issues associated with compaction, the authors initiated a special core-analysis program to study compaction effects on turbidite sand porosity and permeability specifically. This program also addressed a number of subsidiary but no less important issues, such as sample characterization and quality, sample preparation, and test procedures. These issues are particularly pertinent, because Gulf ofmore » Mexico turbidites are generally unconsolidated, loose sands, and are thus susceptible to a whole array of potentially serious core-disturbing processes. One key result of the special core analysis program is that turbidite compressibilities exhibit large variations in both magnitude and stress dependence. These variations correlate with creep response in the laboratory measurements. The effects of compaction on permeability are significant. To eliminate complicating effects caused by fines movement, the authors made oil flow measurements at initial water saturation. The measurements indicate compaction reduces permeability four to five times more than porosity on a relative basis.« less
NASA Astrophysics Data System (ADS)
Mikhailov, Ivan; Levina, Vera; Leybo, Denis; Masov, Vsevolod; Tagirov, Marat; Kuznetsov, Denis
Nanostructured zero-valent iron (NSZVI) particles were synthesized by the method of ferric ion reduction with sodium borohydride with subsequent drying and passivation at room temperature in technical grade nitrogen. The obtained sample was characterized by means of X-ray powder diffraction, scanning electron microscopy, transmission electron microscopy and dynamic light scattering studies. The prepared NSZVI particles represent 100-200nm aggregates, which consist of 20-30nm iron nanoparticles in zero-valent oxidation state covered by thin oxide shell. The reactivity of the NSZVI sample, as the removal efficiency of refractory azo dyes, was investigated in this study. Two azo dye compounds, namely, orange G and methyl orange, are commonly detected in waste water of textile production. Experimental variables such as NSZVI dosage, initial dye concentration and solution pH were investigated. The kinetic rates of degradation of both dyes by NSZVI increased with the decrease of solution pH from 10 to 3 and with the increase of NSZVI dosage, but decreased with the increase of initial dye concentration. The removal efficiencies achieved for both orange G and methyl orange were higher than 90% after 80min of treatment.
NASA Astrophysics Data System (ADS)
Schumann, Dorothea; Sibbens, Goedele; Stolarz, Anna; Eberhardt, Klaus; Lommel, Bettina; Stodel, Christelle
2018-05-01
A wide number of research fields in the nuclear sector requires high-quality and well-characterized samples and targets. Currently, only a few laboratories own or have access to the equipment allowing fulfilling such demands. Coordination of activities and sharing resources is therefore mandatory to meet the increasing needs. This very urgent issue has now been addressed by six European target laboratories with an initiative called ANITA (Advanced Network for Isotope and TArget laboratories). The global aim of ANITA is to establish an overarching research infrastructure service for isotope and target production and develop a tight cooperation between the target laboratories in Europe in order to transfer the knowledge and improve the production techniques of well-characterized samples and targets. Moreover, the interaction of the target producers with the users shall be encouraged and intensified to deliver tailor-made targets best-suited to the envisaged experiments. For the realization of this ambitious goal, efforts within the European Commission and strong support by the target-using communities will be necessary. In particular, an appropriate funding instrument has to be found and applied, enabling ANITA to develop from an initiative employed by the interested parties to a real coordination platform.
Final Report for X-ray Diffraction Sample Preparation Method Development
DOE Office of Scientific and Technical Information (OSTI.GOV)
Ely, T. M.; Meznarich, H. K.; Valero, T.
WRPS-1500790, “X-ray Diffraction Saltcake Sample Preparation Method Development Plan/Procedure,” was originally prepared with the intent of improving the specimen preparation methodology used to generate saltcake specimens suitable for XRD-based solid phase characterization. At the time that this test plan document was originally developed, packed powder in cavity supports with collodion binder was the established XRD specimen preparation method. An alternate specimen preparation method less vulnerable, if not completely invulnerable to preferred orientation effects, was desired as a replacement for the method.
Bobaly, Balazs; D'Atri, Valentina; Goyon, Alexandre; Colas, Olivier; Beck, Alain; Fekete, Szabolcs; Guillarme, Davy
2017-08-15
The analytical characterization of therapeutic monoclonal antibodies and related proteins usually incorporates various sample preparation methodologies. Indeed, quantitative and qualitative information can be enhanced by simplifying the sample, thanks to the removal of sources of heterogeneity (e.g. N-glycans) and/or by decreasing the molecular size of the tested protein by enzymatic or chemical fragmentation. These approaches make the sample more suitable for chromatographic and mass spectrometric analysis. Structural elucidation and quality control (QC) analysis of biopharmaceutics are usually performed at intact, subunit and peptide levels. In this paper, general sample preparation approaches used to attain peptide, subunit and glycan level analysis are overviewed. Protocols are described to perform tryptic proteolysis, IdeS and papain digestion, reduction as well as deglycosylation by PNGase F and EndoS2 enzymes. Both historical and modern sample preparation methods were compared and evaluated using rituximab and trastuzumab, two reference therapeutic mAb products approved by Food and Drug Administration (FDA) and European Medicines Agency (EMA). The described protocols may help analysts to develop sample preparation methods in the field of therapeutic protein analysis. Copyright © 2017 Elsevier B.V. All rights reserved.
NASA Astrophysics Data System (ADS)
Remund, Stefan M.; Jaeggi, Beat; Kramer, Thorsten; Neuenschwander, Beat
2017-03-01
The resulting surface roughness and waviness after processing with ultra-short pulsed laser radiation depend on the laser parameters as well as on the machining strategy and the scanning system. However the results depend on the material and its initial surface quality and finishing as well. The improvement of surface finishing represents effort and produces additional costs. For industrial applications it is important to reduce the preparation of a workpiece for laser micro-machining to optimize quality and reduce costs. The effects of the ablation process and the influence of the machining strategy and scanning system onto the surface roughness and waviness can be differenced due to their separate manner. By using the optimal laser parameters on an initially perfect surface, the ablation process mainly increases the roughness to a certain value for most metallic materials. However, imperfections in the scanning system causing a slight variation in the scanning speed lead to a raise of the waviness on the sample surface. For a basic understanding of the influence of grinding marks, the sample surfaces were initially furnished with regular grooves of different depths and spatial frequencies to gain a homogenous and well-defined original surface. On these surfaces the effect of different beam waists and machining strategy are investigated and the results are compared with a simulation of the process. Furthermore the behaviors of common surface finishes used in industrial applications for laser micro-machining are studied and the relation onto the resulting surface roughness and waviness is presented.
Exploring the initial steps of the testing process: frequency and nature of pre-preanalytic errors.
Carraro, Paolo; Zago, Tatiana; Plebani, Mario
2012-03-01
Few data are available on the nature of errors in the so-called pre-preanalytic phase, the initial steps of the testing process. We therefore sought to evaluate pre-preanalytic errors using a study design that enabled us to observe the initial procedures performed in the ward, from the physician's test request to the delivery of specimens in the clinical laboratory. After a 1-week direct observational phase designed to identify the operating procedures followed in 3 clinical wards, we recorded all nonconformities and errors occurring over a 6-month period. Overall, the study considered 8547 test requests, for which 15 917 blood sample tubes were collected and 52 982 tests undertaken. No significant differences in error rates were found between the observational phase and the overall study period, but underfilling of coagulation tubes was found to occur more frequently in the direct observational phase (P = 0.043). In the overall study period, the frequency of errors was found to be particularly high regarding order transmission [29 916 parts per million (ppm)] and hemolysed samples (2537 ppm). The frequency of patient misidentification was 352 ppm, and the most frequent nonconformities were test requests recorded in the diary without the patient's name and failure to check the patient's identity at the time of blood draw. The data collected in our study confirm the relative frequency of pre-preanalytic errors and underline the need to consensually prepare and adopt effective standard operating procedures in the initial steps of laboratory testing and to monitor compliance with these procedures over time.
Synthesis of SrFe12O19 magnetic nanoparticles by EDTA complex method
NASA Astrophysics Data System (ADS)
Wang, Shifa; Li, Danming; Xiao, Yuhua; Dang, Wenqiang; Feng, Jie
2017-10-01
A modified polyacrylamide gel route was used to prepare SrFe12O19 magnetic nanoparticles; ethylenediaminetetraacetic acid (EDTA) was used as a carboxyl chelating agent. The phase purity, morphology and magnetic properties of as-prepared samples were analyzed via X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and vibrating sample magnetometery (VSM). XRD analysis indicates that high-purity SrFe12O19 magnetic nanoparticles can be synthesized at 700°C in air. The characteristic peaks of as-prepared sample at 210, 283, 321, 340, 381, 411, 432, 475, 532, 618, 686, and 726 cm-1 were observed in Raman spectra. SEM and TEM show that the synthesized SrFe12O19 magnetic nanoparticles are uniform with the mean particle size of 60 nm. VSM measurement shows that the maximum magnetic energy product (BH)max of sample prepared using EDTA as a chelating agent is higher than that of sample prepared using citric acid as a chelating agent.
Nuclear Magnetic Resonance Spectroscopy-Based Identification of Yeast.
Himmelreich, Uwe; Sorrell, Tania C; Daniel, Heide-Marie
2017-01-01
Rapid and robust high-throughput identification of environmental, industrial, or clinical yeast isolates is important whenever relatively large numbers of samples need to be processed in a cost-efficient way. Nuclear magnetic resonance (NMR) spectroscopy generates complex data based on metabolite profiles, chemical composition and possibly on medium consumption, which can not only be used for the assessment of metabolic pathways but also for accurate identification of yeast down to the subspecies level. Initial results on NMR based yeast identification where comparable with conventional and DNA-based identification. Potential advantages of NMR spectroscopy in mycological laboratories include not only accurate identification but also the potential of automated sample delivery, automated analysis using computer-based methods, rapid turnaround time, high throughput, and low running costs.We describe here the sample preparation, data acquisition and analysis for NMR-based yeast identification. In addition, a roadmap for the development of classification strategies is given that will result in the acquisition of a database and analysis algorithms for yeast identification in different environments.
Progress Towards an Indirect Neutron Capture Capability at LANSCE
DOE Office of Scientific and Technical Information (OSTI.GOV)
Koehler, Paul E.; Ullmann, John Leonard; Couture, Aaron Joseph
2017-09-20
There are many neutron-capture cross sections of importance to radiochemical diagnostics and nuclear forensics which are beyond the reach of direct measurements. Hence, we have been developing an apparatus on flight path (FP) 13 at target 1 at LANSCE for tightly constraining these cross sections via determination of the underlying physical quantities. FP-13 was initially a cold-neutron beam line for materials science and therefore required substantial modification for use for nuclear physics. In FY17, we made several improvements to FP-13, demonstrated improved performance due to these changes via measurements on a variety of samples, identified a few more needed improvements,more » and reconfigured the beam line to implement the most important of these. New measurements to assess the impact of the most recent improvement will commence when beam is restored to LANSCE. Although FP-13 has not yet reached the performance required for small radioactive samples, measurements on a gold sample have led to an important science result which we are preparing for publication.« less
Inter-laboratory exercise on antibiotic drugs analysis in aqueous samples.
Roig, B; Brogat, M; Mompelat, S; Leveque, J; Cadiere, A; Thomas, O
2012-08-30
An inter-laboratory exercise was organized under the PHARMAS EU project, by the Advanced School of Public Health (EHESP), in order to evaluate the performances of analytical methods for the measurement of antibiotics in waters (surface and tap). This is the first time such an exercise on antibiotics has been organized in Europe, using different kinds of analytical methods and devices. In this exercise thirteen laboratories from five countries (Canada, France, Italy, the Netherlands and Portugal) participated, and a total number of 78 samples were distributed. During the exercise, 2 testing samples (3 bottles of each) prepared from tap water and river water, respectively, spiked with antibiotics, were sent to participants and analyzed over a period of one month. A final number of 77 (98.7%) testing samples were considered. Depending on substances studied by each participant, 305 values in duplicate were collected, with the results for each sample being expressed as the target concentration. A statistical study was initiated using 611 results. The mean value, standard deviation, coefficient of variation, standard uncertainty of the mean, median, the minimum and maximum values of each series as well as the 95% confidence interval were obtained from each participant laboratory. In this exercise, 36 results (6% of accounted values) were outliers according to the distribution over the median (box plot). The outlier results were excluded. In order to establish the stability of testing samples in the course of the exercise, differences between variances obtained for every type of sample at different intervals were evaluated. The results showed no representative variations and it can be considered that all samples were stable during the exercise. The goals of this inter-laboratory study were to assess results variability when analysis is conducted by different laboratories, to evaluate the influence of different matrix samples, and to determine the rate at which participating laboratories successfully completed the tests initiated. Copyright © 2012 Elsevier B.V. All rights reserved.
Schieltz, David M; McGrath, Sara C; McWilliams, Lisa G; Rees, Jon; Bowen, Michael D; Kools, John J; Dauphin, Leslie A; Gomez-Saladin, Eduardo; Newton, Bruce N; Stang, Heather L; Vick, Michael J; Thomas, Jerry; Pirkle, James L; Barr, John R
2011-06-15
In late February 2008, law enforcement officials in Las Vegas, Nevada, discovered in a hotel room, a copy of The Anarchist Cookbook, suspected castor beans and a "white powder" thought to be a preparation of ricin. Ricin is a deadly toxin from the seed of the castor bean plant (Ricinus communis). The United States regulates the possession, use, and transfer of ricin and it is the only substance considered a warfare agent in both the Chemical and the Biological Weapons Conventions. Six samples obtained from the hotel room were analyzed by laboratories at the Centers for Disease Control and Prevention using a panel of biological and mass spectrometric assays. The biological assays (real time-PCR, time resolved fluorescence and cytotoxicity) provided presumptive evidence of active ricin in each of the samples. This initial screen was followed by an in-depth analysis using a novel, state-of-the-art mass spectrometry-based ricin functional assay and high sensitivity tandem mass spectrometry for protein identification. Mass spectrometric analysis positively identified ricin and confirmed that in each of the samples it was enzymatically active. The tandem mass spectrometry analysis used here is the most selective method available to detect ricin toxin. In each sample, ricin was unequivocally identified along with other R. communis plant proteins, including the highly homologous protein RCA120. Although database searches using tandem mass spectra acquired from the samples indicated that additional controlled substances were not present in these samples, the mass spectrometric results did provide extensive detail about the sample contents. To the best of our knowledge following a review of the available literature, this report describes the most detailed analysis of a white powder for a public health or forensic investigation involving ricin. Published by Elsevier Ireland Ltd.
A microfluidics-based technique for automated and rapid labeling of cells for flow cytometry
NASA Astrophysics Data System (ADS)
Patibandla, Phani K.; Estrada, Rosendo; Kannan, Manasaa; Sethu, Palaniappan
2014-03-01
Flow cytometry is a powerful technique capable of simultaneous multi-parametric analysis of heterogeneous cell populations for research and clinical applications. In recent years, the flow cytometer has been miniaturized and made portable for application in clinical- and resource-limited settings. The sample preparation procedure, i.e. labeling of cells with antibodies conjugated to fluorescent labels, is a time consuming (˜45 min) and labor-intensive procedure. Microfluidics provides enabling technologies to accomplish rapid and automated sample preparation. Using an integrated microfluidic device consisting of a labeling and washing module, we demonstrate a new protocol that can eliminate sample handling and accomplish sample and reagent metering, high-efficiency mixing, labeling and washing in rapid automated fashion. The labeling module consists of a long microfluidic channel with an integrated chaotic mixer. Samples and reagents are precisely metered into this device to accomplish rapid and high-efficiency mixing. The mixed sample and reagents are collected in a holding syringe and held for up to 8 min following which the mixture is introduced into an inertial washing module to obtain ‘analysis-ready’ samples. The washing module consists of a high aspect ratio channel capable of focusing cells to equilibrium positions close to the channel walls. By introducing the cells and labeling reagents in a narrow stream at the center of the channel flanked on both sides by a wash buffer, the elution of cells into the wash buffer away from the free unbound antibodies is accomplished. After initial calibration experiments to determine appropriate ‘holding time’ to allow antibody binding, both modules were used in conjunction to label MOLT-3 cells (T lymphoblast cell line) with three different antibodies simultaneously. Results confirm no significant difference in mean fluorescence intensity values for all three antibodies labels (p < 0.01) between the conventional procedure (45 min) and our microfluidic approach (12 min).
Zhang, Shasha; Fang, Yunting; Xi, Dan
2015-07-30
There are several preparation methods for the measurement of the nitrogen (N) isotopic composition of ammonium (NH4 (+) ) in different types of samples (freshwater, saltwater and soil extracts). The diffusion method is the most popular and it involves NH4 (+) in solutions being released under alkaline conditions and then immediately trapped by an acidified filter. However, the traditional preparation is designed for samples with large volume and relatively high N concentrations. The performance of diffusion for small-volume samples (e.g., a few milliliters) remains unknown. We examined the overall performance of micro-diffusion on 5 mL samples on varying the incubation time, temperature and initial NH4 (+) concentration. The trapped ammonia was chemically converted into nitrous oxide (N2 O) with hypobromite and hydroxylamine in sequence. The produced N2 O was analyzed by a commercially available purge and cryogenic trap system coupled to an isotope ratio mass spectrometer. We found that diffusion can be complete with no more than 7 days of treatment at 37 °C. Increasing the temperature to 50 °C and the incubation time to 11 days did not improve the overall performance. There were no significant differences in the overall performance during diffusion with NH4 (+) concentrations from 15 to 60 μM. The blank size was relatively large, and the N contamination might come from the reagents especially KCl salts. The method presented here combines micro-diffusion and hypobromite oxidation and hydroxylamine reduction. It is suitable for samples with small volume and low NH4 (+) concentrations. Our study demonstrates that the NH4 (+) concentrations in samples can be as low as 15 μM, and a volume of 5 mL is sufficient for this method. We suggest that this method can be used for the routine determination of (15) N/(14) N for either natural abundance or (15) N-enriched NH4 (+) . Copyright © 2015 John Wiley & Sons, Ltd.
Black, Jennifer L; Velazquez, Cayley E; Ahmadi, Naseam; Chapman, Gwen E; Carten, Sarah; Edward, Joshua; Shulhan, Stephanie; Stephens, Teya; Rojas, Alejandro
2015-09-01
To describe the development and application of the School Food Environment Assessment Tools and a novel scoring system to assess the integration of healthy and environmentally sustainable food initiatives in elementary and secondary schools. The cross-sectional study included direct observations of physical food environments and interviews with key school personnel regarding food-related programmes and policies. A five-point scoring system was then developed to assess actions across six domains: (i) food gardens; (ii) composting systems; (iii) food preparation activities; (iv) food-related teaching and learning activities; and availability of (v) healthy food; and (vi) environmentally sustainable food. Vancouver, Canada. A purposive sample of public schools (n 33) from all six sectors of the Vancouver Board of Education. Schools scored highest in the areas of food garden and compost system development and use. Regular integration of food-related teaching and learning activities and hands-on food preparation experiences were also commonly reported. Most schools demonstrated rudimentary efforts to make healthy and environmentally sustainable food choices available, but in general scored lowest on these two domains. Moreover, no schools reported widespread initiatives fully supporting availability or integration of healthy or environmentally sustainable foods across campus. More work is needed in all areas to fully integrate programmes and policies that support healthy, environmentally sustainable food systems in Vancouver schools. The assessment tools and proposed indicators offer a practical approach for researchers, policy makers and school stakeholders to assess school food system environments, identify priority areas for intervention and track relevant changes over time.
Gas chromatography-mass spectrometry of biofluids and extracts.
Emwas, Abdul-Hamid M; Al-Talla, Zeyad A; Yang, Yang; Kharbatia, Najeh M
2015-01-01
Gas chromatography-mass spectrometry (GC-MS) has been widely used in metabonomics analyses of biofluid samples. Biofluids provide a wealth of information about the metabolism of the whole body and from multiple regions of the body that can be used to study general health status and organ function. Blood serum and blood plasma, for example, can provide a comprehensive picture of the whole body, while urine can be used to monitor the function of the kidneys, and cerebrospinal fluid (CSF) will provide information about the status of the brain and central nervous system (CNS). Different methods have been developed for the extraction of metabolites from biofluids, these ranging from solvent extracts, acids, heat denaturation, and filtration. These methods vary widely in terms of efficiency of protein removal and in the number of metabolites extracted. Consequently, for all biofluid-based metabonomics studies, it is vital to optimize and standardize all steps of sample preparation, including initial extraction of metabolites. In this chapter, recommendations are made of the optimum experimental conditions for biofluid samples for GC-MS, with a particular focus on blood serum and plasma samples.
NASA Astrophysics Data System (ADS)
Tumey, Scott J.; Brown, Thomas A.; Hamilton, Terry E.; Hillegonds, Darren J.
2008-05-01
Strontium-90 is one of the most hazardous materials managed by agencies charged with protecting the public from radiation. Traditional radiometric methods have been limited by low sample throughput and slow turnaround times. Mass spectrometry offers the advantage of shorter analysis times and the ability to measure samples immediately after processing, however conventional mass spectrometric techniques are susceptible to molecular isobaric interferences that limit their overall sensitivity. In contrast, accelerator mass spectrometry is insensitive to molecular interferences and we have therefore begun developing a method for determination of 90Sr by accelerator mass spectrometry. Despite a pervasive interference from 90Zr, our initial development has yielded an instrumental background of ∼108 atoms (75 mBq) per sample. Further refinement of our system (e.g. redesign of our detector, use of alternative target materials) is expected to push the background below 106 atoms, close to the theoretical limit for AMS. Once we have refined our system and developed suitable sample preparation protocols, we will utilize our capability in applications to homeland security, environmental monitoring and human health.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Hoogheem, T.J.; Woods, L.A.
The Monsanto Analytical Testing (MAT) program was devised and implemented in order to provide analytical standards to Monsanto manufacturing plants involved in the self-monitoring of plant discharges as required by National Pollutant Discharge Elimination System (NPDES) permit conditions. Standards are prepared and supplied at concentration levels normally observed at each individual plant. These levels were established by canvassing all Monsanto plants having NPDES permits and by determining which analyses and concentrations were most appropriate. Standards are prepared by Monsanto's analyses and concentrations were most appropriate. Standards are prepared by Monsanto's Environmental Sciences Center (ESC) using Environmental Protection Agency (EPA) methods.more » Eleven standards are currently available, each in three concentrations. Standards are issued quarterly in a company internal round-robin program or on a per request basis or both. Since initiation of the MAT program in 1981, the internal round-robin program has become an integral part of Monsanto's overall Good Laboratory Practices (GLP) program. Overall, results have shown that the company's plant analytical personnel can accurately analyze and report standard test samples. More importantly, such personnel have gained increased confidence in their ability to report accurate values for compounds regulated in their respective plant NPDES permits. 3 references, 3 tables.« less
Preparation of ZnO Photocatalyst for the Efficient and Rapid Photocatalytic Degradation of Azo Dyes.
Chen, Xiaoqing; Wu, Zhansheng; Liu, Dandan; Gao, Zhenzhen
2017-12-01
Zinc oxide (ZnO) photocatalysts were synthesized by sol-gel method using zinc acetate as precursor for degradation of azo dyes under UV irradiation. The resultant samples were characterized by different techniques, such as XRD, SEM, and EDX. The influence of preparation conditions such as calcination temperature and composite ratio on the degradation of methyl orange (MO) was investigated. ZnO prepared with a composite ratio of 4:1 and calcination temperature of 400 °C exhibited 99.70% removal rate for MO. The effect of operation parameters on the degradation was also studied. Results showed that the removal rate of azo dyes increased with the increased dosage of catalyst and decreased initial concentration of azo dyes and the acidic condition is favorable for degradation. Furthermore, the kinetics and scavengers of the reactive species during the degradation were also investigated. It was found that the degradation of azo dyes fitted the first-order kinetics and superoxide ions were the main species. The proposed photocatalyst can efficiently and rapidly degrade azo dyes; thus, this economical and environment-friendly photocatalyst can be applied to the treatment of wastewater contaminated with synthetic dyes.
NASA Astrophysics Data System (ADS)
Zhang, J.; Yu, X. C.; Nie, Z. W.; Guo, M. C.; Liu, J. H.; Wang, L. P.
2017-12-01
The ZnO/SnO2 composite nanophotocatalyst studied in this paper was prepared by a chemical precipitation method, which were characterized by XRD and SEM. The results show that the prepared samples were rutile SnO2 particles and the average grain size is 8.41 nm. In this paper, the factors for the degradation efficiency of marine diesel oil degraded by ZnO/SnO2 composite nanophotocatalyst are the catalysts’ doping ratio, the initial concentration of oil, the pH value of seawater, the dosage of catalyst and the dosage of hydrogen peroxide. The results show that the ZnO/SnO2 composite nanophotocatalyst can effectively degrade seawater diesel oil under UV light. When the doping ratio of ZnO and SnO2 is 0.35, the reaction time is 2.5 hours, the pH value of seawater with oil is 7, The concentration of diesel oil is 0.1g/L, the dosage of catalyst is 0.3g/L and the dosage of hydrogen peroxide is 0.1 g/L, the highest degradation rate is 91.54%.
NASA Astrophysics Data System (ADS)
Zhang, Min; Xu, Bajin; Ling, Guoping
2015-03-01
In this paper, α-Al2O3 film was prepared by low temperature thermal oxidation of Al8Cr5 coating. The Al8Cr5 alloy coating was prepared on SUS430 stainless steel through a two-step approach including electrodepositing Cr/Al composite coating and subsequent heat treatment at 740 °C for 16 h. After mechanical polishing removal of voids on the surface, the Al8Cr5 coating was thermal oxidized at 720 °C in argon for 100 h. The samples were characterized by SEM, EDX, XRD, XPS and TEM. XPS detection on the surface of oxidized Al8Cr5 coating showed that the oxide film mainly consisted of Al2O3. TEM characterization of the oxide film showed that it was α-Al2O3 films ca. 110 nm. The formation of α-Al2O3 films at low temperature can be attributed to the formation of Cr2O3 nuclei at the initial stage of oxidation which lowers the nucleation energy barrier of α-Al2O3.
Orr, Elizabeth M J; Moscovitch, David A
2014-01-01
Video feedback (VF) interventions effectively reduce social anxiety symptoms and negative self-perception, particularly when they are preceded by cognitive preparation (CP) and followed by cognitive review. In the current study, we re-examined data from a study on the efficacy of a novel VF intervention for individuals high in social anxiety to test the hypothesis that physical appearance anxiety would moderate the effects of VF. Data were analyzed from 68 socially anxious participants who performed an initial public speech, and were randomly assigned to an Elaborated VF condition (VF plus cognitive preparation and cognitive review), a Standard VF condition (VF plus cognitive preparation) or a No VF condition (exposure alone), and then performed a second speech. As hypothesized, when appearance concerns were low, both participants who received Elaborated and Standard VF were significantly less anxious during speech 2 than those in the No VF condition. However, when levels of appearance concern were high, neither Elaborated nor Standard VF reduced anxiety levels during speech 2 beyond the No VF condition. Results from our analog sample suggest the importance of tailoring treatment protocols to accommodate the idiosyncratic concerns of socially anxious patients.
Monolithic methacrylate packed 96-tips for high throughput bioanalysis.
Altun, Zeki; Skoglund, Christina; Abdel-Rehim, Mohamed
2010-04-16
In the pharmaceutical industry the growing number of samples to be analyzed requires high throughput and fully automated analytical techniques. Commonly used sample-preparation methods are solid-phase extraction (SPE), liquid-liquid extraction (LLE) and protein precipitation. In this paper we will discus a new sample-preparation technique based on SPE for high throughput drug extraction developed and used by our group. This new sample-preparation method is based on monolithic methacrylate polymer as packing sorbent for 96-tip robotic device. Using this device a 96-well plate could be handled in 2-4min. The key aspect of the monolithic phase is that monolithic material can offer both good binding capacity and low back-pressure properties compared to e.g. silica phases. The present paper presents the successful application of monolithic 96-tips and LC-MS/MS by the sample preparation of busulphan, rescovitine, metoprolol, pindolol and local anaesthetics from human plasma samples and cyklophosphamid from mice blood samples. Copyright 2009 Elsevier B.V. All rights reserved.
Electrodeposition as an alternate method for preparation of environmental samples for iodide by AMS
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
DOE Office of Scientific and Technical Information (OSTI.GOV)
Tomar, Vikas
Irradiations and post characterization experiments were performed first on Zr samples. This step will help understand the effect of the 2.5% alloying elements on the behavior of Zircaloy-4 (PWR cladding material) when compared to pure Zr. Irradiation flux measurements and sample temperature calibrations were performed at different energies prior to the irradiation experiments. Irradiations were performed with two different energy regimes1: non-displacment energies and displacement energies. Time was also dedicated to optimize transmission electron microscopy (TEM) sample preparation conditions via electropolishing technique. This step is crucial to prepare TEM samples for the in-situ TEM/irradiation experiments (Year 2). In addition, Zircaloy-4more » samples are being prepared for irradiation, and a setup is built by one of our collaborators (Dr. Mert Efe) to prepare ultrafine (UF) and nanocrystalline (NC) Zircaloy-4 samples for comparison with the commercial Zircaloy-4 samples.« less
NASA Astrophysics Data System (ADS)
Stosnach, Hagen; Mages, Margarete
2009-04-01
In clinical service laboratories, one of the most common analytical tasks with regard to inorganic traces is the determination of the nutrition-relevant elements Fe, Cu, Zn, and Se. Because of the high numbers of samples and the commercial character of these analyses, a time-consuming sample preparation must be avoided. In this presentation, the results of total reflection X-ray fluorescence measurements with a low-power system and different sample preparation procedures are compared with those derived from analysis with common methods like Atomic Absorption Spectroscopy (AAS) and Inductively Coupled Plasma Mass Spectroscopy (ICP-MS). The results of these investigations indicate that the optimal total reflection X-ray fluorescence analysis of the nutrition-relevant elements Fe, Cu, Zn, and Se can be performed by preparing whole blood and serum samples after dilution with ultrapure water and transferring 10 μl of internally standardized sample to an unsiliconized quartz glass sample carrier with subsequent drying in a laboratory oven. Suitable measurement time was found to be 600 s. The enhanced sample preparation by means of microwave or open digestion, in parts combined with cold plasma ashing, led to an improvement of detection limits by a factor of 2 for serum samples while for whole blood samples an improvement was only observed for samples prepared by means of microwave digestion. As the matrix elements P, S, Cl, and for whole blood Fe have a major influence on the detection limits, most probably a further enhancement of analytical quality requires the removal of the organic matrix. However, for the routine analysis of the nutrition-relevant elements, the dilution preparation was found to be sufficient.
Wang, Chaoli; Hu, Xiaoling; Guan, Ping; Wu, Danfeng; Qian, Liwei; Li, Ji; Song, Renyuan
2015-01-01
The synthesis and performance of molecularly imprinted membranes (MIMs) as a solid phase extraction packing materials for the separation and purification of thymopentin from crude samples was described. In order to increase structural selectivity and imprinting efficiency, surface-initiated ATRP and ionic liquid (1-vinyl-3-ethyl acetate imidazolium chloride) were used to prepare molecularly imprinting membranes. The results demonstrated that solid phase extraction disks stuffed by MIMs with ionic liquids as functional monomer demonstrated high isolation and purification of performance to the thymopentin. The molecular recognition of thymopentin was analyzed by using molecular modeling software. Copyright © 2014 Elsevier B.V. All rights reserved.
The laboratory astrophysics facility at University College
NASA Astrophysics Data System (ADS)
Hyland, A. R.; Smith, R. G.; Robinson, G.
A laboratory astrophysics facility for the study of the terrestrial analogues of interstellar dust grains is being developed in the Physics Department, University College, Australian Defence Force Academy. The facility consists of a gas handling system for the preparation of samples, a closed-cycle cooler and specimen chamber, and a Fourier Transform Infrared (FTIR) Spectrometer capable of high resolution (0.3/cm) and high sensitivity measurements, currently from 1-25 microns. The layout and construction of the laboratory are described, and the proposed initial experimental program aimed at determining the optical constants of ices, over a wide wavelength range for comparison with astronomical observations, is discussed.
ERIC Educational Resources Information Center
Kopas-Vukašinovic, Emina; Stevanovic, Jelena; Stanojevic, Vladimir
2017-01-01
The preparation of children for the teaching of initial writing is a problem which is, in the system of unique institutional education, addressed by the preschool institution and the school. The open preschool education system includes the engagement of parents in these activities. The aim of this paper was to determine the attitudes of parents…
ERIC Educational Resources Information Center
Chambers, Gary N.; Hobson, Andrew J.; Tracey, Louise
2010-01-01
Retention in initial teacher preparation (ITP) and the teaching profession, in England and elsewhere, has been the subject of numerous articles in academic and professional journals. Whilst a number of common findings are beginning to emerge from research on this subject, notably on the causes of student teacher withdrawal, studies have tended to…
ERIC Educational Resources Information Center
Vote, Carol J.
A literature review examined the legislation to eliminate sex bias and stereotyping in education and the guidance and counseling curricula and programs that are integral components of the legislation. Six questions guided the preparation of the review: (1) How have legislative initiatives intended to reform education, affected the career…
Robinson, T; Bronson, B; Gogolek, P; Mehrani, P
2016-02-01
Thermo-gravimetric analysis (TGA) is a useful method for characterizing fuels. In the past it has been applied to the study of refuse derived fuel (RDF) and related materials. However, the heterogeneity of RDF makes the preparation of small representative samples very difficult and this difficulty has limited the effectiveness of TGA for characterization of RDF. A TGA method was applied to a variety of materials prepared from a commercially available RDF using a variety of procedures. Applicability of TGA method to the determination of the renewable content of RDF was considered. Cryogenic ball milling was found to be an effective means of preparing RDF samples for TGA. When combined with an effective sample preparation, TGA could be used as an alternative method for assessing the renewable content of RDF. Crown Copyright © 2015. Published by Elsevier Ltd. All rights reserved.
FC and ZFC magnetic properties of ferro-spinels (MFe2O4) prepared by solution-combustion method
NASA Astrophysics Data System (ADS)
Aravind, G.; Kumar, R. Vijaya; Nathaniyal, V.; Rambabu, T.; Ravinder, D.
2017-07-01
Magnetic ferro-spinels MFe2O4 (M= Co and Ni) prepared by citrate-gel solution combustion method using metal nitrates with low sintering temperature (500°C). From the XRD and TEM studies confirm that a nano crystalline nature of the prepared samples. Field Cooled (FC) and Zero Field Cooled (ZFC) magnetic studies of the prepared ferro-spinels are measured by using vibrating sample magnetometer (VSM). The resultant magnetization of the prepared samples as a function of an applied magnetic field 10 T was measured at two different temperatures 5 K and 310 K. Field Cooled (FC) and Zero Field Cooled (ZFC) magnetization measurements under an applied field of 100 Oe and 1000 Oe in the temperature range of 5-375 K were carried out, which shows the blocking temperature of these two samples at around 350 K.
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.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Miller, J.T.
1994-09-01
Guidelines are given for using abbreviations, acronyms, and initialisms (AAIs) in documents prepared by US Department of Energy facilities managed by Martin Marietta Energy Systems, Inc., in Oak Ridge, Tennessee. The more than 10,000 AAIs listed represent only a small portion of those found in recent documents prepared by contributing editors of the Information Management Services organization of Oak Ridge National Laboratory, the Oak Ridge K-25 Site, and the Oak Ridge Y-12 Plant. This document expands on AAIs listed in the Document Preparation Guide and is intended as a companion document
Reuter, Benedikt; Elsner, Björn; Möllers, David; Kathmann, Norbert
2016-11-01
Clinical and theoretical models suggest deficient volitional initiation of action in schizophrenia patients. Recent research provided an experimental model of testing this assumption using saccade tasks. However, inconsistent findings necessitate a specification of conditions on which the deficit may occur. The present study sought to detect mechanisms that may contribute to poor performance. Sixteen schizophrenia patients and 16 healthy control participants performed visually guided and two types of volitional saccade tasks. All tasks varied as to whether the initial fixation stimulus disappeared (fixation stimulus offset) or continued during saccade initiation, and whether a direction cue allowed motor preparation of the specific saccade. Saccade latencies of the two groups were differentially affected by task type, fixation stimulus offset, and cueing, suggesting abnormal volitional saccade generation, fixation release, and motor preparation in schizophrenia. However, substantial performance deficits may only occur if all affected processes are required in a task. © 2016 Society for Psychophysiological Research.
Recent developments in sample preparation and data pre-treatment in metabonomics research.
Li, Ning; Song, Yi peng; Tang, Huiru; Wang, Yulan
2016-01-01
Metabonomics is a powerful approach for biomarker discovery and an effective tool for pinpointing endpoint metabolic effects of external stimuli, such as pathogens and disease development. Due to its wide applications, metabonomics is required to deal with various biological samples of different properties. Hence sample preparation and corresponding data pre-treatment become important factors in ensuring validity of an investigation. In this review, we summarize some recent developments in metabonomics sample preparation and data-pretreatment procedures. Copyright © 2015 Elsevier Inc. 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.
Fluidics platform and method for sample preparation and analysis
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.
Stability of Extemporaneously Prepared Hydroxycarbamide Oral Suspensions.
Kabiche, Djamila; Balde, Issa-Bella; Majoul, Elyes; Kabiche, Sofiane; Bourguignon, Elodie; Fontan, Jean-Eudes; Cisternino, Salvatore; Schlatter, Jöel
2017-01-01
Hydroxycarbamide, available as tablets, is a pharmacological agent for fetal hemoglobin induction such as sickle cell anemia. The need for alternative dosage form options for patients unable to take tablets led hospital pharmacies to prepare solutions and suspensions. The objective of this study was to determine the stability of hydroxycarbamide in Ora-Plus in combination with either Ora-Sweet or Ora-Sweet SF, Ora-Blend, or Ora-Blend SF suspending agents. The studied samples were compounded into 100-mg/mL suspensions and stored in 60-mL amber glass bottles at room (22°C to 25°C) or refrigerated (4°C to 8°C) temperature. Samples were assayed at each time point out to 120 days by a stability-indicating high-performance liquid chromatography method. The samples were examined for any change in color, odor, visual microbiology, and pH on initial and final day of analysis. At least 90% of hydroxycarbamide concentration remained in all suspensions at the end of the 120-day study period in both conditions. There was no appreciable change in color, odor, or taste. The pH values of suspensions stored at 25°C changed by at least 1 unit at the end of the study period. Based on the data collected, the beyond-use date of these suspensions is 120 days when stored in 60-mL amber glass bottles at both temperature storage conditions. Copyright© by International Journal of Pharmaceutical Compounding, Inc.
Magnetic nanoparticles coated with polyaniline to stabilize immobilized trypsin
NASA Astrophysics Data System (ADS)
Maciel, J. C.; D. Mercês, A. A.; Cabrera, M.; Shigeyosi, W. T.; de Souza, S. D.; Olzon-Dionysio, M.; Fabris, J. D.; Cardoso, C. A.; Neri, D. F. M.; C. Silva, M. P.; Carvalho, L. B.
2016-12-01
It is reported the synthesis of magnetic nanoparticles via the chemical co-precipitation of Fe 3+ ions and their preparation by coating them with polyaniline. The electronic micrograph analysis showed that the mean diameter for the nanoparticles is ˜15 nm. FTIR, powder X-ray diffraction and Mössbauer spectroscopy were used to understand the chemical, crystallographic and 57Fe hyperfine structures for the two samples. The nanoparticles, which exhibited magnetic behavior with relatively high spontaneous magnetization at room temperature, were identified as being mainly formed by maghemite ( γFe2O3). The coated magnetic nanoparticles (sample labeled "mPANI") presented a real ability to bind biological molecules such as trypsin, forming the magnetic enzyme derivative (sample "mPANIG-Trypsin"). The amount of protein and specific activity of the immobilized trypsin were found to be 13±5 μg of protein/mg of mPANI (49.3 % of immobilized protein) and 24.1±0.7 U/mg of immobilized protein, respectively. After 48 days of storage at 4 ∘C, the activity of the immobilized trypsin was found to be 89 % of its initial activity. This simple, fast and low-cost procedure was revealed to be a promising way to prepare mPANI nanoparticles if technological applications addressed to covalently link biomolecules are envisaged. This route yields chemically stable derivatives, which can be easily recovered from the reaction mixture with a magnetic field and recyclable reused.
Roushani, Mahmoud; Abbasi, Shahryar; Khani, Hossein
2015-04-01
Novel Cu(II) ion-imprinted polymers (Cu-IIP) nanoparticles were prepared by using Cu(II) ion-thiosemicarbazide complex as the template molecule and methacrylic acid, ethylene glycol dimethacrylate (EGDMA), and 2,2'azobisisobutyronitrile (AIBN) as the functional monomer, cross-linker, and the radical initiator, respectively. The synthesized polymer nanoparticles were characterized by using infrared spectroscopy (IR), thermo gravimetric analysis (TGA), X-ray diffraction (XRD), and scanning electron microscopic (SEM) techniques. Some parameters such as pH, weight of the polymer, adsorption time, elution time, eluent type, and eluent volume which affect the extraction efficiency of the polymer were studied. In the proposed method, the maximum sorbent capacity of the ion-imprinted polymer was calculated to be 38.8 mg g(-1). The preconcentration factor, relative standard deviation, and limit of detection of the method were found to be 80, 1.7%, and 0.003 μg mL(-1), respectively. The prepared ion-imprinted polymer nanoparticles have an increased selectivity toward Cu(II) ions over a range of competing metal ions with the same charge and similar ionic radius. The method was applied to the determination of ultra trace levels of Cu2+ in environmental water samples with satisfactory results.
Fu, Zhiqiang; Wang, Chengbiao
2014-01-01
Ultrafine tungsten carbide-nickel (WC-Ni) cemented carbides with varied fractions of silicon carbide (SiC) nanowhisker (0–3.75 wt.%) were fabricated by spark plasma sintering at 1350°C under a uniaxial pressure of 50 MPa with the assistance of vanadium carbide (VC) and tantalum carbide (TaC) as WC grain growth inhibitors. The effects of SiC nanowhisker on the microstructure and mechanical properties of the as-prepared WC-Ni cemented carbides were investigated. X-ray diffraction analysis revealed that during spark plasma sintering (SPS) Ni may react with the applied SiC nanowhisker, forming Ni2Si and graphite. Scanning electron microscopy examination indicated that, with the addition of SiC nanowhisker, the average WC grain size decreased from 400 to 350 nm. However, with the additional fractions of SiC nanowhisker, more and more Si-rich aggregates appeared. With the increase in the added fraction of SiC nanowhisker, the Vickers hardness of the samples initially increased and then decreased, reaching its maximum of about 24.9 GPa when 0.75 wt.% SiC nanowhisker was added. However, the flexural strength of the sample gradually decreased with increasing addition fraction of SiC nanowhisker. PMID:25003143
NASA Astrophysics Data System (ADS)
Bhowmik, R. N.; Kazhugasalamoorthy, S.; Sinha, A. K.
2017-12-01
We have prepared a composite of ferrimagnetic ferrite Co1.75Fe1.25O4 and non-magnetic oxide BaTiO3. The ferrite composition Co1.75Fe1.25O4 has been prepared by chemical co-precipitation and subsequently heated at different temperatures. The heat treated ferrite powder has been mixed with BaTiO3 powder with mass ratio 1:1 and the mixed powder has been finally heated at 1000 °C to form composite material. Structural phase of the composite material has been confirmed by high quality Synchrotron X-ray diffraction pattern and Micro-Raman spectra. The grain surface morphology and elemental composition have been studied by Scanning electron microscope and Energy dispersive X-ray analysis. The distribution of magnetic exchange interactions and blocking behavior of the ferrimagnetic grains in composite samples has been understood by analyzing the temperature and magnetic field dependence of dc magnetization. Finally, information on modified micro-structure and ferrimagnetic parameters in composite samples has been obtained as the variation of annealing temperature of the ferrite component before making composite.
Su, Xiaomeng; Li, Xiaoyan; Li, Junjie; Liu, Min; Lei, Fuhou; Tan, Xuecai; Li, Pengfei; Luo, Weiqiang
2015-03-15
Core-shell magnetic molecularly imprinted polymers (MIPs) nanoparticles (NPs), in which a Rhodamine B-imprinted layer was coated on Fe3O4 NPs. were synthesized. First, Fe3O4 NPs were prepared by a coprecipitation method. Then, amino-modified Fe3O4 NPs (Fe3O4@SiO2-NH2) was prepared. Finally, the MIPs were coated on the Fe3O4@SiO2-NH2 surface by the copolymerization with functional monomer, acrylamide, using a cross-linking agent, ethylene glycol dimethacrylate; an initiator, azobisisobutyronitrile and a template molecule, Rhodamine B. The Fe3O4@MIPs were characterized using a scanning electron microscope, Fourier transform infrared spectrometer, vibrating sample magnetometer, and re-binding experiments. The Fe3O4@MIPs showed a fast adsorption equilibrium, a highly improved imprinting capacity, and significant selectivity; they could be used as a solid-phase extraction material and detect illegal addition Rhodamine B in food. A method was developed for the selective isolation and enrichment of Rhodamine B in food samples with recoveries in the range 78.47-101.6% and the relative standard deviation was <2%. Copyright © 2014 Elsevier Ltd. All rights reserved.
Mg-Al and Zn-Fe layered double hydroxides used for organic species storage and controlled release.
Seftel, E M; Cool, P; Lutic, D
2013-12-01
Layered double hydroxides (LDH) containing (Mg and Al) or (Zn and Fe) were prepared by coprecipitation at constant pH, using NaOH and urea as precipitation agents. The most pure LDH phase in the Zn/Fe system was obtained with urea and in Mg/Al system when using NaOH. The incorporation of phenyl-alanine (Phe) anions in the interlayer of the LDH was performed by direct coprecipitation, ionic exchange and structure reconstruction of the mixed oxide obtained by the calcination of the coprecipitated product at 400°C. The reconstruction method and the direct coprecipitation in a medium containing Phe in the initial mixture were less successful in terms of high yields of organic-mineral composite than the ionic exchange method. A spectacular change in sample morphology and yield in exchanged solid was noticed for the Zn3Fe sample obtained by ionic exchange for 6h with Phe solution. A delivery test in PBS of pH=7.4 showed the release of the Phe in several steps up to 25 h indicating different host-guest interactions between the Phe and the LDH matrix. This behavior makes the preparation useful to obtain late delivery drugs, by the incorporation of the anion inside the LDH layer. © 2013.
Del Mar, Peter
1995-01-01
A process of sample preparation prior to analysis for the concentration of an organic contaminant in an aqueous medium by (a) passing an initial aqueous medium including a minor amount of the organic contaminant through a composite tube including a polymeric base material selected from the group of polyolefins and polyfluorocarbons and particles of a carbon allotrope material adfixed to the inner wall of the polymeric base material, the composite tube having an internal diameter of from about 0.1 to about 2.0 millimeters and being of sufficient length to permit the organic contaminant to adhere to the composite tube, (b) passing a solvent through the composite tube, said solvent capable of separating the adhered organic contaminant from the composite tube. Further, an extraction apparatus for sample preparation prior to analysis for the concentration of an organic contaminant in an aqueous medium, said apparatus including a composite tube including a polymeric base material selected from the group of polyolefins and polyfluorocarbons and particles of a carbon allotrope material adfixed to the inner wall of the polymeric base material, the composite tube having an internal diameter of from about 0.1 to about 2.0 millimeters and being of sufficient length to permit an organic contaminant contained within an aqueous medium passed therethrough to adhere to the composite tube is disclosed.
Mar, Peter D.
1994-01-01
A process of sample preparation prior to analysis for the concentration of an organic contaminant in an aqueous medium by (a) passing an initial aqueous medium including a minor amount of the organic contaminant through a composite tube including a polymeric base material selected from the group of polyolefins and polyfluorocarbons and particles of a carbon allotrope material adfixed to the inner wall of the polymeric base material, the composite tube having an internal diameter of from about 0.1 to about 2.0 millimeters and being of sufficient length to permit the organic contaminant to adhere to the composite tube, (b) passing a solvent through the composite tube, said solvent capable of separating the adhered organic contaminant from the composite tube. Further, an extraction apparatus for sample preparation prior to analysis for the concentration of an organic contaminant in an aqueous medium, said apparatus including a composite tube including a polymeric base material selected from the group of polyolefins and polyfluorocarbons and particles of a carbon allotrope material adfixed to the inner wall of the polymeric base material, the composite tube having an internal diameter of from about 0.1 to about 2.0 millimeters and being of sufficient length to permit an organic contaminant contained within an aqueous medium passed therethrough to adhere to the composite tube is disclosed.
NASA Astrophysics Data System (ADS)
Kozai, Naofumi; Inada, Koichi; Adachi, Yoshifusa; Kawamura, Sachi; Kashimoto, Yusuke; Kozaki, Tamotsu; Sato, Seichi; Ohnuki, Toshihiko; Sakai, Takuro; Sato, Takahiro; Oikawa, Masakazu; Esaka, Fumitaka; Mitamura, Hisayoshi
2007-08-01
Fe 2+-montmorillonite with Fe 2+ ions occupying cation exchange sites is an ideal transformation product in bentonite buffer material. In our previous study on preparation and characterization of Fe 2+-montmorillonite, the montmorillonite sample that adsorbed Fe 2+ ions on almost all of the cation exchange sites was prepared using a FeCl 2 solution under an inert gas condition [N. Kozai, Y. Adachi, S. Kawamura, K. Inada, T. Kozaki, S. Sato, H. Ohashi, T. Ohnuki, T. Banba, J. Nucl. Sci. Technol. 38 (2001) 1141]. In view of the unstable nature of iron(II) chemical species, this study attempted to determine the potential contaminant iron chemical species in the sample. Nondestructive elemental analysis revealed that a small amount of chloride ions remained dispersed throughout the clay particles. The chloride ion retention may be due to the adsorption of FeCl + ion pairs in the initial FeCl 2 solution and the subsequent containment of the Cl - ions that are dissociated from the FeCl + ion pairs during excess salt removal treatment. Two explanations are advanced for the second process: the slow release of the remaining Cl - ions from the collapsed interlayer of the montmorillonite, and the transformation of a minor fraction of the remaining FeCl + ion pairs to iron(III) hydroxide chloride complexes having low solubility.
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.
Schmitt, Christopher J.; Finger, Susan E.
1987-01-01
The influence of sample preparation on measured concentrations of eight elements in the edible tissues of two black basses (Centrarchidae), two catfishes (Ictaluridae), and the black redhorse,Moxostoma duquesnei (Catostomidae) from two rivers in southeastern Missouri contaminated by mining and related activities was investigated. Concentrations of Pb, Cd, Cu, Zn, Fe, Mn, Ba, and Ca were measured in two skinless, boneless samples of axial muscle from individual fish prepared in a clean room. One sample (normally-processed) was removed from each fish with a knife in a manner typically used by investigators to process fish for elemental analysis and presumedly representative of methods employed by anglers when preparing fish for home consumption. A second sample (clean-processed) was then prepared from each normally-processed sample by cutting away all surface material with acid-cleaned instruments under ultraclean conditions. The samples were analyzed as a single group by atomic absorption spectrophotometry. Of the elements studied, only Pb regularly exceeded current guidelines for elemental contaminants in foods. Concentrations were high in black redhorse from contaminated sites, regardless of preparation method; for the other fishes, whether or not Pb guidelines were exceeded depended on preparation technique. Except for Mn and Ca, concentrations of all elements measured were significantly lower in cleanthan in normally-processed tissue samples. Absolute differences in measured concentrations between clean- and normally-processed samples were most evident for Pb and Ba in bass and catfish and for Cd and Zn in redhorse. Regardless of preparation method, concentrations of Pb, Ca, Mn, and Ba in individual fish were closely correlated; samples that were high or low in one of these four elements were correspondingly high or low in the other three. In contrast, correlations between Zn, Fe, and Cd occurred only in normallyprocessed samples, suggesting that these correlations resulted from high concentrations on the surfaces of some samples. Concentrations of Pb and Ba in edible tissues of fish from contaminated sites were highly correlated with Ca content, which was probably determined largely by the amount of tissue other than muscle in the sample because fish muscle contains relatively little Ca. Accordingly, variation within a group of similar samples can be reduced by normalizing Pb and Ba concentrations to a standard Ca concentration. When sample size (N) is large, this can be accomplished statistically by analysis of covariance; whenN is small, molar ratios of [Pb]/[Ca] and [Ba]/[Ca] can be computed. Without such adjustments, unrealistically large Ns are required to yield statistically reliable estimates of Pb concentrations in edible tissues. Investigators should acknowledge that reported concentrations of certain elements are only estimates, and that regardless of the care exercised during the collection, preparation, and analysis of samples, results should be interpreted with the awareness that contamination from external sources may have occurred.
40 CFR 205.171-2 - Test exhaust system sample selection and preparation.
Code of Federal Regulations, 2013 CFR
2013-07-01
... 40 Protection of Environment 26 2013-07-01 2013-07-01 false Test exhaust system sample selection... Systems § 205.171-2 Test exhaust system sample selection and preparation. (a)(1) Exhaust systems comprising the sample which are required to be tested under a test request in accordance with this subpart...
Paul, Atish T; Vir, Sanjay; Bhutani, K K
2008-10-24
A new liquid chromatography-mass spectrometry (LC-MS)-based method coupled with pressurized liquid extraction (PLE) as an efficient sample preparation technique has been developed for the quantification and fingerprint analysis of Solanum xanthocarpum. Optimum separations of the samples were achieved on a Waters MSC-18 XTerra column, using 0.5% (v/v) formic acid in water (A) and acetonitrile (ACN):2-propanol:formic acid (94.5:5:0.5, v/v/v) (B) as mobile phase. The separation was carried out using linear gradient elution with a flow rate of 1.0mL/min. The gradient was: 0min, 20% B; 14min, 30% B; 20min, 30% B; 27min, 60% B and the column was re-equilibrated to the initial condition (20% B) for 10min prior to next injection. The steroidal glycoalkaloids (SGAs) which are the major active constituents were isolated as pure compounds from the crude methanolic extract of S. xanthocarpum by preparative LC-MS and after characterization were used as external standards for the development and validation of the method. Extracts prepared by conventional Soxhlet extraction, PLE and ultrasonication were used for analysis. The method was validated for repeatability, precision (intra- and inter-day variation), accuracy (recovery) and sensitivity (limit of detection and limit of quantitation). The purpose of the work was to develop a validated method, which can be used for the quantification of SGAs in commercialized S. xanthocarpum products and the fingerprint analysis for their routine quality control.
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.
28 CFR 91.63 - Preparing an Environmental Impact Statement
Code of Federal Regulations, 2010 CFR
2010-07-01
... 28 Judicial Administration 2 2010-07-01 2010-07-01 false Preparing an Environmental Impact... CORRECTIONAL FACILITIES Environmental Impact Review Procedures for VOI/TIS Grant Program Environmental Review Procedures § 91.63 Preparing an Environmental Impact Statement (a) Initial determination. OJP will determine...
Redesigning Personnel Preparation: Lessons Learned and Considerations for Program Enhancement
ERIC Educational Resources Information Center
Little, Mary E.; Sobel, Donna; McCray, Erica D.; Wang, Jun
2015-01-01
Changing legal requirements, economic demands, accountability, and student demographics focus the need for reform among personnel preparation programs. Although redesign efforts in general and special education teacher preparation programs have increased, little evidence from research describes enhancement initiatives. In this article, the authors…
NASA Astrophysics Data System (ADS)
Kohga, Makoto; Handa, Saori
2018-01-01
The thermal decomposition behaviors and burning characteristics of propellants prepared with combined ammonium perchlorate (AP)/ammonium nitrate (AN) particles greatly depended on the AN content (χ) of the AP/AN sample. The thermal decomposition behaviors of the propellants prepared with the combined samples almost matched those of the propellants prepared by physically mixing AP and AN particles, while their burning characteristics differed. The use of combined AP/AN particles decreased the heterogeneity of the combustion waves of the AP/AN propellants because of the difference in the combustion wave structure. In contrast, the addition of Fe2O3 caused unsteady combustion of the propellants prepared using samples with χ values lower than 8.1%.
NASA Astrophysics Data System (ADS)
Shamsipur, Mojtaba; Rajabi, Hamid Reza; Pourmortazavi, Seied Mahdi; Roushani, Mahmoud
2014-01-01
Preparation of Zn2+ ion-imprinted polymer (Zn-IIP) nanoparticles is presented in this report. The Zn-IIP nanoparticles are prepared by dissolving stoichiometric amounts of zinc nitrate and selected chelating ligand, 3,5,7,20,40-pentahydroxyflavone, in 15 mL ethanol-acetonitrile (2:1; v/v) mixture as a porogen solvent in the presence of ethylene glycol-dimethacrylate (EGDMA) as cross-linking, methacrylic acid (MAA) as functional monomer, and 2,2-azobisisobutyronitrile (AIBN) as initiator. After polymerization, Cavities in the polymer particles corresponding to the Zn2+ ions were created by leaching the polymer in HCl aqueous solution. The synthesized IIPs were characterized by scanning electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy, fluorescence spectroscopy and thermal analysis techniques. Also, the pH range for rebinding of Zn2+ ion on the IIP and equilibrium binding time were optimized, using flame atomic absorption spectrometry. In selectivity study, it was found that imprinting results increased affinity of the material toward Zn2+ ion over other competitor metal ions with the same charge and close ionic radius. The prepared IIPs were repeatedly used and regenerated for six times without any significant decrease in polymer binding affinities. Finally, the prepared sorbent was successfully applied to the selective recognition and determination of zinc ion in different real samples.
Bo, Chunmiao; Wang, Xiaomeng; Wang, Chaozhan; Wei, Yinmao
2017-03-03
Development of mixed-mode chromatography (MMC) stationary phase with adjustable selectivity is beneficial to meet the needs of complex samples. In this work, surface-initiated atom transfer radical polymerization (SI-ATRP) using the mixture of two functional monomers was proposed as a new preparation strategy for MMC stationary phase with adjustable selectivity. The mixture of sodium 4-styrenesulfonate (NASS) and dimethylaminoethyl methacrylate (DMAEMA) underwent SI-ATRP to bond poly(NASS-co-DMAEMA) on the surface of silica to prepare hydrophilic interaction/ion-exchange mixed-mode stationary phase. Various analytes (neutral, acidic, basic analytes and strong polar nucleosides) were employed to investigate the retention behaviors. The influences of water content and pH of the mobile phase on the retention validated the mixed-mode retention mechanisms of HILIC and ion-exchange. The charge and polarity of stationary phase as well as the separation selectivity were conveniently manipulated by the ratio of NASS to DMAEMA monomer, and the use of DMAEMA in the mixture additionally endowed the column with the temperature-responsive characteristics. Moreover, the application of the developed column was demonstrated by the successful separation of nucleosides, β-agonists and safflower injection. In a word, the proposed strategy can be potentially applied in the controllable preparation of MMC stationary phase with adjustable selectivity. Copyright © 2017 Elsevier B.V. All rights reserved.
Madden, Jeremy T.; Toth, Scott J.; Dettmar, Christopher M.; Newman, Justin A.; Oglesbee, Robert A.; Hedderich, Hartmut G.; Everly, R. Michael; Becker, Michael; Ronau, Judith A.; Buchanan, Susan K.; Cherezov, Vadim; Morrow, Marie E.; Xu, Shenglan; Ferguson, Dale; Makarov, Oleg; Das, Chittaranjan; Fischetti, Robert; Simpson, Garth J.
2013-01-01
Nonlinear optical (NLO) instrumentation has been integrated with synchrotron X-ray diffraction (XRD) for combined single-platform analysis, initially targeting applications for automated crystal centering. Second-harmonic-generation microscopy and two-photon-excited ultraviolet fluorescence microscopy were evaluated for crystal detection and assessed by X-ray raster scanning. Two optical designs were constructed and characterized; one positioned downstream of the sample and one integrated into the upstream optical path of the diffractometer. Both instruments enabled protein crystal identification with integration times between 80 and 150 µs per pixel, representing a ∼103–104-fold reduction in the per-pixel exposure time relative to X-ray raster scanning. Quantitative centering and analysis of phenylalanine hydroxylase from Chromobacterium violaceum cPAH, Trichinella spiralis deubiquitinating enzyme TsUCH37, human κ-opioid receptor complex kOR-T4L produced in lipidic cubic phase (LCP), intimin prepared in LCP, and α-cellulose samples were performed by collecting multiple NLO images. The crystalline samples were characterized by single-crystal diffraction patterns, while α-cellulose was characterized by fiber diffraction. Good agreement was observed between the sample positions identified by NLO and XRD raster measurements for all samples studied. PMID:23765294
Mohamed, Lamiaa Z; Ghanem, Wafaa A; El Kady, Omayma A; Lotfy, Mohamed M; Ahmed, Hafiz A; Elrefaie, Fawzi A
2017-11-01
The oxidation behavior of two types of inhomogeneous nickel was investigated in air at 1273 K for a total oxidation time of 100 h. The two types were porous sintered-nickel and microstructurally inhomogeneous cast-nickel. The porous-nickel samples were fabricated by compacting Ni powder followed by sintering in vacuum at 1473 K for 2 h. The oxidation kinetics of the samples was determined gravimetrically. The topography and the cross-section microstructure of each oxidized sample were observed using optical and scanning electron microscopy. X-ray diffractometry and X-ray energy dispersive analysis were used to determine the nature of the formed oxide phases. The kinetic results revealed that the porous-nickel samples had higher trend for irreproducibility. The average oxidation rate for porous- and cast-nickel samples was initially rapid, and then decreased gradually to become linear. Linear rate constants were 5.5 × 10 -8 g/cm 2 s and 3.4 × 10 -8 g/cm 2 s for the porous- and cast-nickel samples, respectively. Initially a single-porous non-adherent NiO layer was noticed on the porous- and cast-nickel samples. After a longer time of oxidation, a non-adherent duplex NiO scale was formed. The two layers of the duplex scales were different in color. NiO particles were observed in most of the pores of the porous-nickel samples. Finally, the linear oxidation kinetics and the formation of porous non-adherent duplex oxide scales on the inhomogeneous nickel substrates demonstrated that the addition of new layers of NiO occurred at the scale/metal interface due to the thermodynamically possible reaction between Ni and the molecular oxygen migrating inwardly.
NASA Astrophysics Data System (ADS)
Mousavi, M.; Kompany, A.; Shahtahmasebi, N.; Bagheri-Mohagheghi, M.-M.
2013-08-01
Vanadium oxide thin films were grown on glass substrates using spray pyrolysis technique. The effects of substrate temperature, vanadium concentration in the initial solution and the solution spray rate on the nanostructural and the electrochromic properties of deposited films are investigated. Characterization and the electrochromic measurements were carried out using X-ray diffraction, scanning electron microscopy and cyclic voltammogram. XRD patterns showed that the prepared films have polycrystalline structure and are mostly mixed phases of orthorhombic α-V2O5 along with minor β-V2O5 and V4O9 tetragonal structures. The preferred orientation of the deposited films was found to be along [101] plane. The cyclic voltammogram results obtained for different samples showed that only the films with 0.2 M solution concentration, 5 ml/min solution spray rate and 450°C substrate temperature exhibit two-step electrochromic properties. The results show a correlation between cycle voltammogram, morphology and resistance of the films.
Bellucci, F S; Salmazo, L O; Budemberg, E R; da Silva, M R; Rodríguez-Pérez, M A; Nobre, M A L; Job, A E
2012-03-01
Single-phase polycrystalline mixed nickel-zinc ferrites belonging to Ni0.5Zn0.5Fe2O4 were prepared on a nanometric scale (mean crystallite size equal to 14.7 nm) by chemical synthesis named the modified poliol method. Ferrite nanopowder was then incorporated into a natural rubber matrix producing nanocomposites. The samples were investigated by means of infrared spectroscopy, X-ray diffraction, scanning electron microscopy and magnetic measurements. The obtained results suggest that the base concentration of nickel-zinc ferrite nanoparticles inside the polymer matrix volume greatly influences the magnetic properties of nanocomposites. A small quantity of nanoparticles, less than 10 phr, in the nanocomposite is sufficient to produce a small alteration in the semi-crystallinity of nanocomposites observed by X-ray diffraction analysis and it produces a flexible magnetic composite material with a saturation magnetization, a coercivity field and an initial magnetic permeability equal to 3.08 emu/g, 99.22 Oe and 9.42 x 10(-5) respectively.
Eu-doped ZnO nanoparticles: Sonochemical synthesis, characterization, and sonocatalytic application.
Khataee, Alireza; Karimi, Atefeh; Zarei, Mahmoud; Joo, Sang Woo
2015-03-30
Undoped and europium (III)-doped ZnO nanoparticles were prepared by a sonochemical method. The prepared samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and X-ray photoelectron spectroscopy (XPS) analysis. The crystalline sizes of undoped and 3% Eu-doped ZnO were found to be 16.04 and 8.22nm, respectively. The particle size of Eu-doped ZnO nanoparticles was much smaller than that of pure ZnO. The synthesized nanocatalysts were used for the sonocatalytic degradation of Acid Red 17. Among the Eu-doped ZnO catalysts, 3% Eu-doped ZnO nanoparticles showed the highest sonocatalytic activity. The effects of various parameters such as catalyst loading, initial dye concentration, pH, ultrasonic power, the effect of oxidizing agents, and the presence of anions were investigated. The produced intermediates of the sonocatalytic process were monitored by GC-Mass (GC-MS) spectrometry. Copyright © 2015 Elsevier B.V. All rights reserved.
Characterization of food additive-potato starch complexes by FTIR and X-ray diffraction.
Dankar, Iman; Haddarah, Amira; Omar, Fawaz E L; Pujolà, Montserrat; Sepulcre, Francesc
2018-09-15
Fourier-transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD) techniques were used to study the effect of four food additives, agar, alginate, lecithin and glycerol, at three different concentrations, 0.5, 1 and 1.5%, on the molecular structure of potato puree prepared from commercial potato powder. Vibrational spectra revealed that the amylose-amylopectin skeleton present in the raw potato starch was missing in the potato powder but could be fully recovered upon water addition when the potato puree was prepared. FTIR peaks corresponding to water were clearly present in the potato powder, indicating the important structural role of water molecules in the recovery of the initial molecular conformation. None of the studied puree samples presented a crystalline structure or strong internal order. A comparison of the FTIR and XRD results revealed that the additives exerted some effects, mainly on the long-range order of the starch structure via interacting with and changing -OH and hydrogen bond interactions. Copyright © 2018 Elsevier Ltd. All rights reserved.
Araújo, B C; Moraes, M S; Costa, L E O; Nascimento, J S
2015-04-01
Infant milk formulas are not sterile products, and pathogenic bacteria can survive and multiply in these products. This study was performed, initially, to detect the presence of Salmonella spp. in reconstituted infant milk formula and on utensils previously sanitized used in their preparation or distribution in a nursery of a public hospital in Rio de Janeiro. None of the samples tested carried Salmonellaspp. However, further identification of colonies growing on the selective media revealed the presence of several other gram-negative bacteria. Seventeen isolates were identified as belonging to Acinetobacter baumannii-calcoaceticus complex. Fourteen isolates presented a multidrug-resistance profile, by disc diffusion assays, and one of them--JE4--was also resistant to imipenem. The detection of Acinetobacter isolates in this work demonstrates inadequate hygiene practices in the preparation or distribution of infant milk formula. Copyright © 2015 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.
New potentiometric sensor based on molecularly imprinted nanoparticles for cocaine detection.
Smolinska-Kempisty, K; Ahmad, O Sheej; Guerreiro, A; Karim, K; Piletska, E; Piletsky, S
2017-10-15
Here we present a potentiometric sensor for cocaine detection based on molecularly imprinted polymer nanoparticles (nanoMIPs) produced by the solid-phase imprinting method. The composition of polymers with high affinity for cocaine was optimised using molecular modelling. Four compositions were selected and polymers prepared using two protocols: chemical polymerisation in water and UV-initiated polymerisation in organic solvent. All synthesised nanoparticles had very good affinity to cocaine with dissociation constants between 0.6nM and 5.3nM. Imprinted polymers produced in organic solvent using acrylamide as a functional monomer demonstrated the highest yield and affinity, and so were selected for further sensor development. For this, nanoparticles were incorporated within a PVC matrix which was then used to prepare an ion-selective membrane integrated with a potentiometric transducer. It was demonstrated that the sensor was able to quantify cocaine in blood serum samples in the range of concentrations between 1nM and 1mM. Copyright © 2017 Elsevier B.V. All rights reserved.
NASA Astrophysics Data System (ADS)
Gui, Chen; Wang, Kan; Li, Chao; Dai, Xuan; Cui, Daxiang
2014-02-01
Immunochromatographic assays are widely used to detect many analytes. CagA is proved to be associated closely with initiation of gastric carcinoma. Here, we reported that a charge-coupled device (CCD)-based test strip reader combined with CdS quantum dot-labeled lateral flow strips for quantitative detection of CagA was developed, which used 365-nm ultraviolet LED as the excitation light source, and captured the test strip images through an acquisition module. Then, the captured image was transferred to the computer and was processed by a software system. A revised weighted threshold histogram equalization (WTHE) image processing algorithm was applied to analyze the result. CdS quantum dot-labeled lateral flow strips for detection of CagA were prepared. One hundred sera samples from clinical patients with gastric cancer and healthy people were prepared for detection, which demonstrated that the device could realize rapid, stable, and point-of-care detection, with a sensitivity of 20 pg/mL.
40 CFR 761.323 - Sample preparation.
Code of Federal Regulations, 2011 CFR
2011-07-01
... PROHIBITIONS Self-Implementing Alternative Extraction and Chemical Analysis Procedures for Non-liquid PCB Remediation Waste Samples § 761.323 Sample preparation. (a) The comparison study requires analysis of a... of use in this chemical extraction and chemical analysis comparison study, a person may adjust PCB...
Bo, Chun Miao; Wang, Chaozhan; Wei, Yin Mao
2017-12-01
A novel approach that involved the grafting of diblock copolymer with two types of monomer onto substrate by sequential surface initiated-atom transfer radical polymerization was proposed to prepare a mixed-mode chromatographic stationary phase. The distinguishing feature of this method is that it can be applied in the preparation of various mixed-mode stationary phases. In this study, a new reverse-phase/ion-exchange stationary phase was prepared by grafting hydrophobic styrene and cationic sodium 4-styrenesulfonate by the proposed approach onto silica surface. The chromatographic properties of the prepared stationary phase were evaluated by the separation of benzene derivatives, anilines, and β-agonists, and by the effect of pH values and acetonitrile content on the retention. Compared with typical RP columns, the prepared stationary phase achieved the better resolution and higher selectivity at a shorter separation time and lower organic content. Moreover, the application of the prepared column was proved by separating widely distributed polar and charged compounds simultaneously. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
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.
Microfluidic Sample Preparation for Diagnostic Cytopathology
Mach, Albert J.; Adeyiga, Oladunni B.; Di Carlo, Dino
2014-01-01
The cellular components of body fluids are routinely analyzed to identify disease and treatment approaches. While significant focus has been placed on developing cell analysis technologies, tools to automate the preparation of cellular specimens have been more limited, especially for body fluids beyond blood. Preparation steps include separating, concentrating, and exposing cells to reagents. Sample preparation continues to be routinely performed off-chip by technicians, preventing cell-based point-of-care diagnostics, increasing the cost of tests, and reducing the consistency of the final analysis following multiple manually-performed steps. Here, we review the assortment of biofluids for which suspended cells are analyzed, along with their characteristics and diagnostic value. We present an overview of the conventional sample preparation processes for cytological diagnosis. We finally discuss the challenges and opportunities in developing microfluidic devices for the purpose of automating or miniaturizing these processes, with particular emphases on preparing large or small volume samples, working with samples of high cellularity, automating multi-step processes, and obtaining high purity subpopulations of cells. We hope to convey the importance of and help identify new research directions addressing the vast biological and clinical applications in preparing and analyzing the array of available biological fluids. Successfully addressing the challenges described in this review can lead to inexpensive systems to improve diagnostic accuracy while simultaneously reducing overall systemic healthcare costs. PMID:23380972
Joshi, C; Dwivedi, A; Rai, S B
2014-08-14
Infrared-to-visible upconverting rare earths Er(3+)/Yb(3+) co-doped Y2O3 nano-crystalline phosphor samples have been prepared by solution combustion method followed by post-heat treatment at higher temperatures. A slight increase in average crystallite size has been found on calcinations verified by X-ray analysis. Transmission electron microscopy (TEM) confirms the nano-crystalline nature of the as-prepared and calcinated samples. Fourier transform infrared (FTIR) analysis shows the structural changes in as-prepared and calcinated samples. Upconversion and downconversion emission recorded using 976 and 532 nm laser sources clearly demonstrates a better luminescence properties in the calcinated samples as compared to as-prepared sample. Upconversion emission has been quantified in terms of standard chromaticity diagram (CIE) showing a shift in overall upconversion emission of as-prepared and calcinated samples. Temperature sensing behaviour of this material has also been investigated by measurement of fluorescence intensity ratio (FIR) of various signals in green emission in the temperature range of 315 to 555 K under 976 nm laser excitation. Copyright © 2014 Elsevier B.V. All rights reserved.
Zhang, Zhenbin; Sun, Liangliang; Zhu, Guijie; Cox, Olivia F; Huber, Paul W; Dovichi, Norman J
2016-01-05
A sulfonate-silica hybrid strong cation exchange monolith microreactor was synthesized and coupled to a linear polyacrylamide coated capillary for online sample preparation and capillary zone electrophoresis-tandem mass spectrometry (CZE-MS/MS) bottom-up proteomic analysis. The protein sample was loaded onto the microreactor in an acidic buffer. After online reduction, alkylation, and digestion with trypsin, the digests were eluted with 200 mM ammonium bicarbonate at pH 8.2 for CZE-MS/MS analysis using 1 M acetic acid as the background electrolyte. This combination of basic elution and acidic background electrolytes results in both sample stacking and formation of a dynamic pH junction. 369 protein groups and 1274 peptides were identified from 50 ng of Xenopus laevis zygote homogenate, which is comparable with an offline sample preparation method, but the time required for sample preparation was decreased from over 24 h to less than 40 min. Dramatically improved performance was produced by coupling the reactor to a longer separation capillary (∼100 cm) and a Q Exactive HF mass spectrometer. 975 protein groups and 3749 peptides were identified from 50 ng of Xenopus protein using the online sample preparation method.
Dietary hyperoxaluria is not reduced by treatment with lactic acid bacteria
2013-01-01
Background Secondary hyperoxaluria either based on increased intestinal absorption of oxalate (enteric), or high oxalate intake (dietary), is a major risk factor of calcium oxalate urolithiasis. Oxalate-degrading bacteria might have beneficial effects on urinary oxalate excretion resulting from decreased intestinal oxalate concentration and absorption. Methods Twenty healthy subjects were studied initially while consuming a diet normal in oxalate. Study participants were then placed on a controlled oxalate-rich diet for a period of 6 weeks. Starting with week 2 of the oxalate-rich diet, participants received 2.6 g/day of a lactic acid bacteria preparation for 5 weeks. Finally, subjects were examined 4 weeks after treatment while consuming again a normal-oxalate diet. Participants provided weekly 24-hour urine specimens. Analyses of blood samples were performed before and at the end of treatment. Results Urinary oxalate excretion increased significantly from 0.354 ± 0.097 at baseline to 0.542 ± 0.163 mmol/24 h under the oxalate-rich diet and remained elevated until the end of treatment, as did relative supersaturation of calcium oxalate. Plasma oxalate concentration was significantly higher after 5 weeks of treatment compared to baseline. Four weeks after treatment, urinary oxalate excretion and relative supersaturation of calcium oxalate fell to reach initial values. Conclusions Persistent dietary hyperoxaluria and increased plasma oxalate concentration can already be induced in healthy subjects without disorders of oxalate metabolism. The study preparation neither reduced urinary oxalate excretion nor plasma oxalate concentration. The preparation may be altered to select for lactic acid bacteria strains with the highest oxalate-degrading activity. PMID:24330782
ERIC Educational Resources Information Center
European Commission, 2017
2017-01-01
This document, "Annex 1 to the Final Report to DG Education, Youth, Sport and Culture of the European Commission" is intended as a companion piece to European Commission report "Preparing Teachers for Diversity: The Role of Initial Teacher Education. Final Report". It contains country fiches which are overviews of available…
Flexible automated approach for quantitative liquid handling of complex biological samples.
Palandra, Joe; Weller, David; Hudson, Gary; Li, Jeff; Osgood, Sarah; Hudson, Emily; Zhong, Min; Buchholz, Lisa; Cohen, Lucinda H
2007-11-01
A fully automated protein precipitation technique for biological sample preparation has been developed for the quantitation of drugs in various biological matrixes. All liquid handling during sample preparation was automated using a Hamilton MicroLab Star Robotic workstation, which included the preparation of standards and controls from a Watson laboratory information management system generated work list, shaking of 96-well plates, and vacuum application. Processing time is less than 30 s per sample or approximately 45 min per 96-well plate, which is then immediately ready for injection onto an LC-MS/MS system. An overview of the process workflow is discussed, including the software development. Validation data are also provided, including specific liquid class data as well as comparative data of automated vs manual preparation using both quality controls and actual sample data. The efficiencies gained from this automated approach are described.
Freitas, Mírian Luisa Faria; Dutra, Mariana Borges de Lima; Bolini, Helena Maria André
2016-12-01
The objective of this study was to evaluate the sensory properties and acceptability of pitanga nectar samples prepared with sucrose and different sweeteners (sucralose, aspartame, stevia with 40% rebaudioside A, stevia with 95% rebaudioside A, neotame, and a 2:1 cyclamate/saccharin blend). A total of 13 assessors participated in a quantitative descriptive analysis and evaluated the samples in relation to the descriptor terms. The acceptability test was carried out by 120 fruit juice consumers. The results of the quantitative descriptive analysis of pitanga nectar showed that samples prepared with sucralose, aspartame, and the 2:1 cyclamate/saccharin blend had sensory profiles similar to that of the sample prepared with sucrose. Consumers' most accepted samples were prepared with sucrose, sucralose, aspartame, and neotame. The sweeteners that have the greatest potential to replace sucrose in pitanga nectar are sucralose and aspartame. © The Author(s) 2016.
The occurrence of Salmonella in airline meals.
Hatakka, M; Asplund, K
1993-01-01
The occurrence of Salmonella in airline meals was studied in 1989-1992. Samples were collected from flight kitchens in 29 countries. The material consisted of 400 cold dishes and 1,288 hot dishes as well as salads, cheese plates and deserts. Total number of samples was 2211. Salmonella spp. were isolated from 6 samples; 1 contaminated sample was a cold dish prepared in Bangkok, 1 was a hot dish prepared in Mombasa and the remaining 4 contaminated samples were hot dishes prepared within one week in Beijing. The isolated serotypes were S. ohio, S. manchester and S. braenderup. The contaminated cold dish prepared by a flight kitchen in Bangkok was found to be connected with a Salmonella outbreak which occurred in Finland in 1990. Cold airline dishes containing food of animal origin seems to be more risky as a source of Salmonella infections among airline passengers.
30 CFR 7.48 - Acid resistance test.
Code of Federal Regulations, 2010 CFR
2010-07-01
...) Test procedures. (1) Prepare one sample each of the insulated surfaces of the battery box and of the... for the battery box and cover, only one sample need be prepared and tested. (2) Prepare a 30 percent... insulation plus the battery cover or box material. The insulation thickness shall be representative of that...
30 CFR 7.48 - Acid resistance test.
Code of Federal Regulations, 2014 CFR
2014-07-01
...) Test procedures. (1) Prepare one sample each of the insulated surfaces of the battery box and of the... for the battery box and cover, only one sample need be prepared and tested. (2) Prepare a 30 percent... insulation plus the battery cover or box material. The insulation thickness shall be representative of that...
30 CFR 7.48 - Acid resistance test.
Code of Federal Regulations, 2013 CFR
2013-07-01
...) Test procedures. (1) Prepare one sample each of the insulated surfaces of the battery box and of the... for the battery box and cover, only one sample need be prepared and tested. (2) Prepare a 30 percent... insulation plus the battery cover or box material. The insulation thickness shall be representative of that...
NASA Astrophysics Data System (ADS)
De la Calle, Inmaculada; Menta, Mathieu; Séby, Fabienne
2016-11-01
Due to the increasing use of nanoparticles (NPs) in consumer products, it becomes necessary to develop different strategies for their detection, identification, characterization and quantification in a wide variety of samples. Since the analysis of NPs in consumer products and environmental samples is particularly troublesome, a detailed description of challenges and limitations is given here. This review mainly focuses on sample preparation procedures applied for the mostly used techniques for metallic and metal oxide NPs characterization in consumer products and most outstanding publications of biological and environmental samples (from 2006 to 2015). We summarize the procedures applied for total metal content, extraction/separation and/or preconcentration of NPs from the matrix, separation of metallic NPs from their ions or from larger particles and NPs' size fractionation. Sample preparation procedures specifically for microscopy are also described. Selected applications in cosmetics, food, other consumer products, biological tissues and environmental samples are presented. Advantages and inconveniences of those procedures are considered. Moreover, selected simplified schemes for NPs sample preparation, as well as usual techniques applied are included. Finally, promising directions for further investigations are discussed.
Tvedt, Tor Henrik Anderson; Rye, Kristin Paulsen; Reikvam, Håkon; Brenner, Annette K; Bruserud, Øystein
2015-03-01
Cytokines, soluble adhesion molecules and metalloproteinases can be detected in human serum or plasma samples. Such systemic levels are widely used as biomarkers in epidemiological and clinical studies. We prepared serum samples and three types of plasma samples (EDTA, heparin, citric acid) from 20 healthy individuals. The levels of 31 cytokines, four soluble adhesion molecules and eight matrix metalloproteinases were analyzed by Luminex technology. Most mediators showed detectable levels in both plasma and serum. Several mediators that can be released by platelets showed increased serum levels, especially CCL5 and CD40L, but for the other mediators the serum levels did not correlate with peripheral blood platelet counts and for these last mediators serum and plasma levels often showed strong correlations. The use of bivalirudin for anticoagulation significantly increased and citric acid combined with platelet inhibitors (ticagrelor, acetylsalicylic acid plus prostaglandin E2) did not alter plasma levels of platelet-store mediators compared with citric acid alone. The impact of sample preparation differed between mediators; for many mediators strong correlations were seen between serum and plasma levels even when absolute levels differed. Soluble adhesion molecule levels showed only minor differences between samples. Unsupervised hierarchical clustering suggested that the effect of sampling/preparation was strongest for serum and heparin plasma samples. Careful standardization of sample preparation is usually necessary when analyzing systemic mediator levels, and differences caused by sample preparation should be considered as a possible explanation if studies show conflicting results. Copyright © 2015 Elsevier B.V. All rights reserved.
An Overview of Conventional and Emerging Analytical Methods for the Determination of Mycotoxins
Cigić, Irena Kralj; Prosen, Helena
2009-01-01
Mycotoxins are a group of compounds produced by various fungi and excreted into the matrices on which they grow, often food intended for human consumption or animal feed. The high toxicity and carcinogenicity of these compounds and their ability to cause various pathological conditions has led to widespread screening of foods and feeds potentially polluted with them. Maximum permissible levels in different matrices have also been established for some toxins. As these are quite low, analytical methods for determination of mycotoxins have to be both sensitive and specific. In addition, an appropriate sample preparation and pre-concentration method is needed to isolate analytes from rather complicated samples. In this article, an overview of methods for analysis and sample preparation published in the last ten years is given for the most often encountered mycotoxins in different samples, mainly in food. Special emphasis is on liquid chromatography with fluorescence and mass spectrometric detection, while in the field of sample preparation various solid-phase extraction approaches are discussed. However, an overview of other analytical and sample preparation methods less often used is also given. Finally, different matrices where mycotoxins have to be determined are discussed with the emphasis on their specific characteristics important for the analysis (human food and beverages, animal feed, biological samples, environmental samples). Various issues important for accurate qualitative and quantitative analyses are critically discussed: sampling and choice of representative sample, sample preparation and possible bias associated with it, specificity of the analytical method and critical evaluation of results. PMID:19333436
NASA Technical Reports Server (NTRS)
Kim, Hyun Jung; Choi, Sang H.; Bae, Hyung-Bin; Lee, Tae Woo
2012-01-01
The National Aeronautics and Space Administration-invented X-ray diffraction (XRD) methods, including the total defect density measurement method and the spatial wafer mapping method, have confirmed super hetero epitaxy growth for rhombohedral single crystalline silicon germanium (Si1-xGex) on a c-plane sapphire substrate. However, the XRD method cannot observe the surface morphology or roughness because of the method s limited resolution. Therefore the authors used transmission electron microscopy (TEM) with samples prepared in two ways, the focused ion beam (FIB) method and the tripod method to study the structure between Si1-xGex and sapphire substrate and Si1?xGex itself. The sample preparation for TEM should be as fast as possible so that the sample should contain few or no artifacts induced by the preparation. The standard sample preparation method of mechanical polishing often requires a relatively long ion milling time (several hours), which increases the probability of inducing defects into the sample. The TEM sampling of the Si1-xGex on sapphire is also difficult because of the sapphire s high hardness and mechanical instability. The FIB method and the tripod method eliminate both problems when performing a cross-section TEM sampling of Si1-xGex on c-plane sapphire, which shows the surface morphology, the interface between film and substrate, and the crystal structure of the film. This paper explains the FIB sampling method and the tripod sampling method, and why sampling Si1-xGex, on a sapphire substrate with TEM, is necessary.
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.
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