Sample preparation

International Nuclear Information System (INIS)

Anon.

1992-01-01

Sample preparation prior to HPLC analysis is certainly one of the most important steps to consider in trace or ultratrace analysis. For many years scientists have tried to simplify the sample preparation process. It is rarely possible to inject a neat liquid sample or a sample where preparation may not be any more complex than dissolution of the sample in a given solvent. The last process alone can remove insoluble materials, which is especially helpful with the samples in complex matrices if other interactions do not affect extraction. Here, it is very likely a large number of components will not dissolve and are, therefore, eliminated by a simple filtration process. In most cases, the process of sample preparation is not as simple as dissolution of the component interest. At times, enrichment is necessary, that is, the component of interest is present in very large volume or mass of material. It needs to be concentrated in some manner so a small volume of the concentrated or enriched sample can be injected into HPLC. 88 refs

Design and device construction for plane tables preparation for counter alpha/beta total

International Nuclear Information System (INIS)

Galicia C, F. J.; Monroy G, F.

2014-10-01

This work presents the design and assembly of a device for plane tables preparation for quantification alpha/beta total of radioactive waste samples. The determination of the activity index alpha/beta total is used to detect a wide variety of matrices quickly and the concentration of alpha and/or beta emitters of the contained radionuclides in different samples. In particular, the determination of the activity index alpha and beta total of radioactive wastes involves the digestion of samples in aggressive means that will be evaporated to dryness for its quantification. With the purpose of controlling the emission of corrosive gases during the preparation of the plane tables for the quantification of the index alpha and beta total, was designed and built the device in the Radioactive Waste Laboratory that allows to prepare plane tables for proportional counters in a sure and efficient way. The device is constituted by heating equipment, evaporation cylinder and a gases cleaning system. The self-absorption curve got ready starting from the device. (Author)

Use of a holder-vacuum tube device to save on-site hands in preparing urine samples for head-space gas-chromatography, and its application to determine the time allowance for sample sealing.

Science.gov (United States)

Kawai, Toshio; Sumino, Kimiaki; Ohashi, Fumiko; Ikeda, Masayuki

2011-01-01

To facilitate urine sample preparation prior to head-space gas-chromatographic (HS-GC) analysis. Urine samples containing one of the five solvents (acetone, methanol, methyl ethyl ketone, methyl isobutyl ketone and toluene) at the levels of biological exposure limits were aspirated into a vacuum tube via holder, a device commercially available for venous blood collection (the vacuum tube method). The urine sample, 5 ml, was quantitatively transferred to a 20-ml head-space vial prior to HS-GC analysis. The loaded tubes were stored at +4 ℃ in dark for up to 3 d. The vacuum tube method facilitated on-site procedures of urine sample preparation for HS-GC with no significant loss of solvents in the sample and no need of skilled hands, whereas on-site sample preparation time was significantly reduced. Furthermore, no loss of solvents was detected during the 3-d storage, irrespective of hydrophilic (acetone) or lipophilic solvent (toluene). In a pilot application, high performance of the vacuum tube method in sealing a sample in an air-tight space succeeded to confirm that no solvent will be lost when sealing is completed within 5 min after urine voiding, and that the allowance time is as long as 30 min in case of toluene in urine. The use of the holder-vacuum tube device not only saves hands for transfer of the sample to air-tight space, but facilitates sample storage prior to HS-GC analysis.

Pressure-driven one-step solid phase-based on-chip sample preparation on a microfabricated plastic device and integration with flow-through polymerase chain reaction (PCR).

Science.gov (United States)

Tran, Hong Hanh; Trinh, Kieu The Loan; Lee, Nae Yoon

2013-10-01

In this study, we fabricate a monolithic poly(methylmethacrylate) (PMMA) microdevice on which solid phase-based DNA preparation and flow-through polymerase chain reaction (PCR) units were functionally integrated for one-step sample preparation and amplification operated by pressure. Chelex resin, which is used as a solid support for DNA preparation, can capture denatured proteins but releases DNA, and the purified DNA can then be used as a template in a subsequent amplification process. Using the PMMA microdevices, DNA was successfully purified from both Escherichia coli and human hair sample, and the plasmid vector inserted in E. coli and the D1S80 locus in human genomic DNA were successfully amplified from on-chip purified E. coli and human hair samples. Furthermore, the integration potential of the proposed sample preparation and flow-through PCR units was successfully demonstrate on a monolithic PMMA microdevice with a seamless flow, which could pave the way for a pressure-driven, simple one-step sample preparation and amplification with greatly decreased manufacture cost and enhanced device disposability. Copyright © 2013 Elsevier B.V. All rights reserved.

Photonic devices prepared by embossing in PDMS

Energy Technology Data Exchange (ETDEWEB)

Jandura, D., E-mail: jandura@fyzika.uniza.sk; Pudis, D.; Berezina, S.

2017-02-15

Highlights: • Fabrication technology of photonic devices based on embossing in PDMS is presented. • Analysis of morphological properties of prepared devices in PDMS by CLSM and AFM. • Spectral characterization of PDMS ring resonator proved the resonator functionality. - Abstract: In this paper, we present useful technique for fabrication of novel photonic devices created in the polydimethylsiloxane (PDMS). We use combination of direct laser writing in thin photoresist layer with embossing process of liquid PDMS. We prepared ring resonator and Mach-Zehnder interferometer in PDMS. The shape of prepared PDMS photonic devices was analyzed by confocal laser microscope and atomic force microscope. Optical characterization of these devices reveals extinction ratios of up to 20 dB.

Green sample preparation for liquid chromatography and capillary electrophoresis of anionic and cationic analytes.

Science.gov (United States)

Wuethrich, Alain; Haddad, Paul R; Quirino, Joselito P

2015-04-21

A sample preparation device for the simultaneous enrichment and separation of cationic and anionic analytes was designed and implemented in an eight-channel configuration. The device is based on the use of an electric field to transfer the analytes from a large volume of sample into small volumes of electrolyte that was suspended into two glass micropipettes using a conductive hydrogel. This simple, economical, fast, and green (no organic solvent required) sample preparation scheme was evaluated using cationic and anionic herbicides as test analytes in water. The analytical figures of merit and ecological aspects were evaluated against the state-of-the-art sample preparation, solid-phase extraction. A drastic reduction in both sample preparation time (94% faster) and resources (99% less consumables used) was observed. Finally, the technique in combination with high-performance liquid chromatography and capillary electrophoresis was applied to analysis of quaternary ammonium and phenoxypropionic acid herbicides in fortified river water as well as drinking water (at levels relevant to Australian guidelines). The presented sustainable sample preparation approach could easily be applied to other charged analytes or adopted by other laboratories.

Automated Blood Sample Preparation Unit (ABSPU) for Portable Microfluidic Flow Cytometry.

Science.gov (United States)

Chaturvedi, Akhil; Gorthi, Sai Siva

2017-02-01

Portable microfluidic diagnostic devices, including flow cytometers, are being developed for point-of-care settings, especially in conjunction with inexpensive imaging devices such as mobile phone cameras. However, two pervasive drawbacks of these have been the lack of automated sample preparation processes and cells settling out of sample suspensions, leading to inaccurate results. We report an automated blood sample preparation unit (ABSPU) to prevent blood samples from settling in a reservoir during loading of samples in flow cytometers. This apparatus automates the preanalytical steps of dilution and staining of blood cells prior to microfluidic loading. It employs an assembly with a miniature vibration motor to drive turbulence in a sample reservoir. To validate performance of this system, we present experimental evidence demonstrating prevention of blood cell settling, cell integrity, and staining of cells prior to flow cytometric analysis. This setup is further integrated with a microfluidic imaging flow cytometer to investigate cell count variability. With no need for prior sample preparation, a drop of whole blood can be directly introduced to the setup without premixing with buffers manually. Our results show that integration of this assembly with microfluidic analysis provides a competent automation tool for low-cost point-of-care blood-based diagnostics.

Reactor operation plan preparing device

International Nuclear Information System (INIS)

Sano, Hiroki; Maruyama, Hiromi; Kinoshita, Mitsuo; Fukuzaki, Koji; Banto, Masaru; Fukazawa, Yukihisa.

1993-01-01

The device comprises a means for retrieving a control rod pattern capable of satisfying a thermal limit upon aimed power/minimum flow rate and providing minimum xenon and a control rod pattern maximum xenon. It further comprises a means for selecting a control rod pattern corresponding to a xenon equilibrium condition, and selecting a control rod which provides a greater thermal margin to provide a control rod operation sequence for each of the patterns. Further, the device comprises an outline plan preparing means and a correction means therefor, a simplified sequence table reference means operated along with sequence change, an operation limit region input means, a control rod operation preferential region changing means, a thermal margin evaluation region and an input means. This can automatically prepare the operation plan, decrease the times for preparation of detailed plans by using the outline plan preparing function, thereby enabling to remarkably shorten the time for preparing of an operation plan. (N.H.)

Device for preparing combinatorial libraries in powder metallurgy.

Science.gov (United States)

Yang, Shoufeng; Evans, Julian R G

2004-01-01

This paper describes a powder-metering, -mixing, and -dispensing mechanism that can be used as a method for producing large numbers of samples for metallurgical evaluation or electrical or mechanical testing from multicomponent metal and cermet powder systems. It is designed to make use of the same commercial powders that are used in powder metallurgy and, therefore, to produce samples that are faithful to the microstructure of finished products. The particle assemblies produced by the device could be consolidated by die pressing, isostatic pressing, laser sintering, or direct melting. The powder metering valve provides both on/off and flow rate control of dry powders in open capillaries using acoustic vibration. The valve is simple and involves no relative movement, avoiding seizure with fine powders. An orchestra of such valves can be arranged on a building platform to prepare multicomponent combinatorial libraries. As with many combinatorial devices, identification and evaluation of sources of mixing error as a function of sample size is mandatory. Such an analysis is presented.

Use of robotic systems for radiochemical sample changing and for analytical sample preparation

International Nuclear Information System (INIS)

Delmastro, J.R.; Hartenstein, S.D.; Wade, M.A.

1989-01-01

Two uses of the Perkin-Elmer (PE) robotic system will be presented. In the first, a PE robot functions as an automatic sample changer for up to five low energy photon spectrometry (LEPS) detectors operated with a Nuclear Data ND 6700 system. The entire system, including the robot, is controlled by an IBM PC-AT using software written in compiled BASIC. Problems associated with the development of the system and modifications to the robot will be presented. In the second, an evaluation study was performed to assess the abilities of the PE robotic system for performing complex analytical sample preparation procedures. For this study, a robotic system based upon the PE robot and auxiliary devices was constructed and programmed to perform the preparation of final product samples (UO 3 ) for accountability and impurity specification analyses. These procedures require sample dissolution, dilution, and liquid-liquid extraction steps. The results of an in-depth evaluation of all system components will be presented

Bipolar Electrode Sample Preparation Devices

Science.gov (United States)

Wang, Yi (Inventor); Song, Hongjun (Inventor); Pant, Kapil (Inventor)

2017-01-01

An analyte selection device can include: a body defining a fluid channel having a channel inlet and channel outlet; a bipolar electrode (BPE) between the inlet and outlet; one of an anode or cathode electrically coupled with the BPE on a channel inlet side of the BPE and the other of the anode or cathode electrically coupled with the BPE on a channel outlet side of the BPE; and an electronic system operably coupled with the anode and cathode so as to polarize the BPE. The fluid channel can have any shape or dimension. The channel inlet and channel outlet can be longitudinal or lateral with respect to the longitudinal axis of the channel. The BPE can be any metallic member, such as a flat plate on a wall or mesh as a barrier BPE. The anode and cathode can be located at a position that polarizes the BPE.

Reactor water sampling device

International Nuclear Information System (INIS)

Sakamaki, Kazuo.

1992-01-01

The present invention concerns a reactor water sampling device for sampling reactor water in an in-core monitor (neutron measuring tube) housing in a BWR type reactor. The upper end portion of a drain pipe of the reactor water sampling device is attached detachably to an in-core monitor flange. A push-up rod is inserted in the drain pipe vertically movably. A sampling vessel and a vacuum pump are connected to the lower end of the drain pipe. A vacuum pump is operated to depressurize the inside of the device and move the push-up rod upwardly. Reactor water in the in-core monitor housing flows between the drain pipe and the push-up rod and flows into the sampling vessel. With such a constitution, reactor water in the in-core monitor housing can be sampled rapidly with neither opening the lid of the reactor pressure vessel nor being in contact with air. Accordingly, operator's exposure dose can be reduced. (I.N.)

Highly simplified lateral flow-based nucleic acid sample preparation and passive fluid flow control

Science.gov (United States)

Cary, Robert E.

2015-12-08

Highly simplified lateral flow chromatographic nucleic acid sample preparation methods, devices, and integrated systems are provided for the efficient concentration of trace samples and the removal of nucleic acid amplification inhibitors. Methods for capturing and reducing inhibitors of nucleic acid amplification reactions, such as humic acid, using polyvinylpyrrolidone treated elements of the lateral flow device are also provided. Further provided are passive fluid control methods and systems for use in lateral flow assays.

Highly simplified lateral flow-based nucleic acid sample preparation and passive fluid flow control

Energy Technology Data Exchange (ETDEWEB)

Cary, Robert B.

2018-04-17

Highly simplified lateral flow chromatographic nucleic acid sample preparation methods, devices, and integrated systems are provided for the efficient concentration of trace samples and the removal of nucleic acid amplification inhibitors. Methods for capturing and reducing inhibitors of nucleic acid amplification reactions, such as humic acid, using polyvinylpyrrolidone treated elements of the lateral flow device are also provided. Further provided are passive fluid control methods and systems for use in lateral flow assays.

Ultra-High-Throughput Sample Preparation System for Lymphocyte Immunophenotyping Point-of-Care Diagnostics.

Science.gov (United States)

Walsh, David I; Murthy, Shashi K; Russom, Aman

2016-10-01

Point-of-care (POC) microfluidic devices often lack the integration of common sample preparation steps, such as preconcentration, which can limit their utility in the field. In this technology brief, we describe a system that combines the necessary sample preparation methods to perform sample-to-result analysis of large-volume (20 mL) biopsy model samples with staining of captured cells. Our platform combines centrifugal-paper microfluidic filtration and an analysis system to process large, dilute biological samples. Utilizing commercialization-friendly manufacturing methods and materials, yielding a sample throughput of 20 mL/min, and allowing for on-chip staining and imaging bring together a practical, yet powerful approach to microfluidic diagnostics of large, dilute samples. © 2016 Society for Laboratory Automation and Screening.

40 CFR 761.323 - Sample preparation.

Science.gov (United States)

2010-07-01

... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Sample preparation. 761.323 Section... Remediation Waste Samples § 761.323 Sample preparation. (a) The comparison study requires analysis of a... concentrations by dilution. Any excess material resulting from the preparation of these samples, which is not...

A Improved Seabed Surface Sand Sampling Device

Science.gov (United States)

Luo, X.

2017-12-01

In marine geology research it is necessary to obtain a suf fcient quantity of seabed surface samples, while also en- suring that the samples are in their original state. Currently,there are a number of seabed surface sampling devices available, but we fnd it is very diffcult to obtain sand samples using these devices, particularly when dealing with fne sand. Machine-controlled seabed surface sampling devices are also available, but generally unable to dive into deeper regions of water. To obtain larger quantities of seabed surface sand samples in their original states, many researchers have tried to improve upon sampling devices,but these efforts have generally produced ambiguous results, in our opinion.To resolve this issue, we have designed an improved andhighly effective seabed surface sand sampling device that incorporates the strengths of a variety of sampling devices. It is capable of diving into deepwater to obtain fne sand samples and is also suited for use in streams, rivers, lakes and seas with varying levels of depth (up to 100 m). This device can be used for geological mapping, underwater prospecting, geological engineering and ecological, environmental studies in both marine and terrestrial waters.

Sample preparation in foodomic analyses.

Science.gov (United States)

Martinović, Tamara; Šrajer Gajdošik, Martina; Josić, Djuro

2018-04-16

Representative sampling and adequate sample preparation are key factors for successful performance of further steps in foodomic analyses, as well as for correct data interpretation. Incorrect sampling and improper sample preparation can be sources of severe bias in foodomic analyses. It is well known that both wrong sampling and sample treatment cannot be corrected anymore. These, in the past frequently neglected facts, are now taken into consideration, and the progress in sampling and sample preparation in foodomics is reviewed here. We report the use of highly sophisticated instruments for both high-performance and high-throughput analyses, as well as miniaturization and the use of laboratory robotics in metabolomics, proteomics, peptidomics and genomics. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

Firewood preparation devices in 1994

International Nuclear Information System (INIS)

Mutikainen, A.

1994-01-01

A review of the market situation regarding firewood preparation devices is presented. The information was collected from the answers to a mail questionnaire. The review is assumed to include all the leading manufacturers and importers. Firewood production devices were available from 26 manufacturers. The range of models amounted to over 70. These may be divided into three categories: 1. cutting devices: the most common solution being a cross-cutting circular saw. There were only a few of these on sale as it is quite easy to include a splitting device on the same frame. 2. Splitting devices: e.g. screw splitter and hydraulically powered splitter. About 20 models are available on the markets. Cross cutting and splitting devices: these are the most popular devices. A cross-cutting circular saw with screw or hydraulic splitter is the most common type. There are about 50 models available on the markets. Cross-cutting and splitting devices are often equipped with conveyor for transferring the split wood e.g. into a trailer. Chopping devices are delivered as tractor powered devices, as electric motor powered devices or as combustion engine powered devices. Some of them are equipped with a time saving feeding device enabling the next stem to be lifted into position while the previous one is being chopped. The Finnish Work Efficiency Institute's studies show that when cross-cutting and splitting of stems into pieces of 35-50 cm in length, productivity for one operator varies in between 0.8 - 3.2 m 3 /h, depending on the device and work method used. (6 refs., 1 fig., 2 tabs.)

Automated cellular sample preparation using a Centrifuge-on-a-Chip.

Science.gov (United States)

Mach, Albert J; Kim, Jae Hyun; Arshi, Armin; Hur, Soojung Claire; Di Carlo, Dino

2011-09-07

The standard centrifuge is a laboratory instrument widely used by biologists and medical technicians for preparing cell samples. Efforts to automate the operations of concentration, cell separation, and solution exchange that a centrifuge performs in a simpler and smaller platform have had limited success. Here, we present a microfluidic chip that replicates the functions of a centrifuge without moving parts or external forces. The device operates using a purely fluid dynamic phenomenon in which cells selectively enter and are maintained in microscale vortices. Continuous and sequential operation allows enrichment of cancer cells from spiked blood samples at the mL min(-1) scale, followed by fluorescent labeling of intra- and extra-cellular antigens on the cells without the need for manual pipetting and washing steps. A versatile centrifuge-analogue may open opportunities in automated, low-cost and high-throughput sample preparation as an alternative to the standard benchtop centrifuge in standardized clinical diagnostics or resource poor settings.

Portable sample preparation and analysis system for micron and sub-micron particle characterization using light scattering and absorption spectroscopy

Science.gov (United States)

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.

Synchrotron/crystal sample preparation

Science.gov (United States)

Johnson, R. Barry

1993-01-01

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

Standard methods for sampling and sample preparation for gamma spectroscopy

International Nuclear Information System (INIS)

Taskaeva, M.; Taskaev, E.; Nikolov, P.

1993-01-01

The strategy for sampling and sample preparation is outlined: necessary number of samples; analysis and treatment of the results received; quantity of the analysed material according to the radionuclide concentrations and analytical methods; the minimal quantity and kind of the data needed for making final conclusions and decisions on the base of the results received. This strategy was tested in gamma spectroscopic analysis of radionuclide contamination of the region of Eleshnitsa Uranium Mines. The water samples was taken and stored according to the ASTM D 3370-82. The general sampling procedures were in conformity with the recommendations of ISO 5667. The radionuclides was concentrated by coprecipitation with iron hydroxide and ion exchange. The sampling of soil samples complied with the rules of ASTM C 998, and their sample preparation - with ASTM C 999. After preparation the samples were sealed hermetically and measured. (author)

[Sample preparation and bioanalysis in mass spectrometry].

Science.gov (United States)

Bourgogne, Emmanuel; Wagner, Michel

2015-01-01

The quantitative analysis of compounds of clinical interest of low molecular weight (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.

Sampling device for radioactive molten salt

International Nuclear Information System (INIS)

Shindo, Masato

1998-01-01

The present invention provides a device for accurately sampling molten salts to which various kinds of metals in a molten salt storage tank are mixed for analyzing them during a spent fuel dry type reprocessing. Namely, the device comprises a sampling tube having an opened lower end to be inserted into the radioactive molten salts stored in a tank and keeps reduced pressure from the upper end, and a pressure reducing pipeline having one end connected to the sampling tube and other end connected to an evacuating pump. In this device, the top end of the sampling tube is inserted to a position for sampling the radioactive molten salts (molten salts). The pressure inside the evacuating pipeline connected to the upper portion of the sampling tube is reduced for a while. In this case, the inside of the pressure reducing pipeline is previously evacuated by the evacuating pump so as to keep a predetermined pressure. Since the pressure in the sampling tube is lowered, molten salts are inserted into the sampling tube, the sampling tube is withdrawn, and the molten salts flown in the sampling tube are analyzed. (I.S.)

Sample preparation guidelines for two-dimensional electrophoresis.

Science.gov (United States)

Posch, Anton

2014-12-01

Sample preparation is one of the key technologies for successful two-dimensional electrophoresis (2DE). Due to the great diversity of protein sample types and sources, no single sample preparation method works with all proteins; for any sample the optimum procedure must be determined empirically. This review is meant to provide a broad overview of the most important principles in sample preparation in order to avoid a multitude of possible pitfalls. Sample preparation protocols from the expert in the field were screened and evaluated. On the basis of these protocols and my own comprehensive practical experience important guidelines are given in this review. The presented guidelines will facilitate straightforward protocol development for researchers new to gel-based proteomics. In addition the available choices are rationalized in order to successfully prepare a protein sample for 2DE separations. The strategies described here are not limited to 2DE and can also be applied to other protein separation techniques.

Experimental study of glass sampling devices

International Nuclear Information System (INIS)

Jouan, A.; Moncouyoux, J.P.; Meyere, A.

1992-01-01

Two high-level liquid waste containment glass sampling systems have been designed and built. The first device fits entirely inside a standard glass storage canister, and may thus be used in facilities not initially designed for this function. It has been tested successfully in the nonradioactive prototype unit at Marcoule. The work primarily covered the design and construction of an articulated arm supporting the sampling vessel, and the mechanisms necessary for filling the vessel and recovering the sample. System actuation and operation are fully automatic, and the resulting sample is representative of the glass melt. Implementation of the device is delicate however, and its reliability is estimated at about 75%. A second device was designed specifically for new vitrification facilities. It is installed directly on the glass melting furnace, and meets process operating and quality control requirements. Tests conducted at the Marcoule prototype vitrification facility demonstrated the feasibility of the system. Special attention was given to the sampling vessel transfer mechanisms, with two filling and controlled sample cooling options

The automated sample preparation system MixMaster for investigation of volatile organic compounds with mid-infrared evanescent wave spectroscopy.

Science.gov (United States)

Vogt, F; Karlowatz, M; Jakusch, M; Mizaikoff, B

2003-04-01

For efficient development assessment, and calibration of new chemical analyzers a large number of independently prepared samples of target analytes is necessary. Whereas mixing units for gas analysis are readily available, there is a lack of instrumentation for accurate preparation of liquid samples containing volatile organic compounds (VOCs). Manual preparation of liquid samples containing VOCs at trace concentration levels is a particularly challenging and time consuming task. Furthermore, regularly scheduled calibration of sensors and analyzer systems demands for computer controlled automated sample preparation systems. In this paper we present a novel liquid mixing device enabling extensive measurement series with focus on volatile organic compounds, facilitating analysis of water polluted by traces of volatile hydrocarbons. After discussing the mixing system and control software, first results obtained by coupling with an FT-IR spectrometer are reported. Properties of the mixing system are assessed by mid-infrared attenuated total reflection (ATR) spectroscopy of methanol-acetone mixtures and by investigation of multicomponent samples containing volatile hydrocarbons such as 1,2,4-trichlorobenzene and tetrachloroethylene. Obtained ATR spectra are evaluated by principal component regression (PCR) algorithms. It is demonstrated that the presented sample mixing device provides reliable multicomponent mixtures with sufficient accuracy and reproducibility at trace concentration levels.

Device for sampling liquid radioactive materials

International Nuclear Information System (INIS)

Vlasak, L.

1987-01-01

Remote sampling of radioactive materials in the process of radioactive waste treatment is claimed by the Czechoslovak Patent Document 238599. The existing difficulties are eliminated consisting in a complex remote control of sampling featuring the control of sliding and rotary movements of the sampling device. The new device consists of a vertical pipe with an opening provided with a cover. A bend is provided above the opening level housing flow distributors. A sampling tray is pivoted in the cover. In sampling, the tray is tilted in the vertical pipe space while it tilts back when filled. The sample flows into a vessel below the tray. Only rotary movement is thus sufficient for controlling the tray. (Z.M.)

imFASP: An integrated approach combining in-situ filter-aided sample pretreatment with microwave-assisted protein digestion for fast and efficient proteome sample preparation.

Science.gov (United States)

Zhao, Qun; Fang, Fei; Wu, Ci; Wu, Qi; Liang, Yu; Liang, Zhen; Zhang, Lihua; Zhang, Yukui

2016-03-17

An integrated sample preparation method, termed "imFASP", which combined in-situ filter-aided sample pretreatment and microwave-assisted trypsin digestion, was developed for preparation of microgram and even nanogram amounts of complex protein samples with high efficiency in 1 h. For imFASP method, proteins dissolved in 8 M urea were loaded onto a filter device with molecular weight cut off (MWCO) as 10 kDa, followed by in-situ protein preconcentration, denaturation, reduction, alkylation, and microwave-assisted tryptic digestion. Compared with traditional in-solution sample preparation method, imFASP method generated more protein and peptide identifications (IDs) from preparation of 45 μg Escherichia coli protein sample due to the higher efficiency, and the sample preparation throughput was significantly improved by 14 times (1 h vs. 15 h). More importantly, when the starting amounts of E. coli cell lysate decreased to nanogram level (50-500 ng), the protein and peptide identified by imFASP method were improved at least 30% and 44%, compared with traditional in-solution preparation method, suggesting dramatically higher peptide recovery of imFASP method for trace amounts of complex proteome samples. All these results demonstrate that the imFASP method developed here is of high potential for high efficient and high throughput preparation of trace amounts of complex proteome samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Subperiosteal preparation using a new piezoelectric device: a histological examination

Directory of Open Access Journals (Sweden)

Stoetzer, Marcus

2014-12-01

Full Text Available Introduction: Subperiosteal preparation using a periosteal elevator leads to disturbances of local immunohistochemistry and periosteal histology due to a microtrauma. Usually soft-tissue damage can be considerably reduced by using piezoelectric technology. For this reason, the effects of a novel piezoelectric device on immunohistochemistry and periosteal histology were examined and compared to conventional preparation of the periosteum using a periosteal elevator.Material and methods: Lewis rats were randomly assigned to one of five groups (n=50. Subperiosteal preparation was performed using either a piezoelectric device or a periosteal elevator. Immunohistochemical and histological analyses were performed immediately after preparation as well as three and eight days postoperatively. A statistical analysis of the histological colouring was performed offline using analysis of variance (ANOVA on ranks (p<0.05. Results: At all times, immunohistochemical and histological analysis demonstrated a significantly more homogenous tissue structure in the group of rats that underwent piezosurgery than in the group of rats that underwent treatment with a periosteal elevator.Conclusion: The use of a piezoelectric device for subperiosteal preparation is associated with more harmonious immunohistochemical and histological results for the periosteum than the use of a conventional periosteal elevator. As a result, piezoelectric devices can be expected to have a positive effect primarily on soft tissue, in particular of the periosteal as well as on surrounding tissues.

Collection and preparation of samples for gamma spectrometry

International Nuclear Information System (INIS)

Pan Jingquan

1994-01-01

The paper presents the basic principles of sample collection and preparation: setting up unified sampling program, methods and procedures, sample packing, transportation and storage, determination of sample quantity, sample pretreatment and preparation of samples to be analysed, etc. for gamma spectrometry. And the paper also describes briefly the main methods and special issues of sampling and preparation for the same environmental and biological samples, such as, air, water, grass, soil and foods

Focused-microwave-assisted sample preparation (M8)

International Nuclear Information System (INIS)

Nobrega, J.A.; Santos, D.M.; Trevizan, L.C.; Costa, L.M.; Nogueira, A.R.A.

2002-01-01

Full text: Focused-microwave-assisted sample preparation is a suitable strategy when dealing with high masses of organic samples. However, the final acid concentration of the digestate can difficult routine analytical measurements using spectroscopic techniques. Acids could be evaporated, but this step could be slow even when using microwave-assisted heating and requires a scrubber system for acid vapor collection and neutralization. We are investigating two procedures to decrease the acid concentration of digestates. The first one is based on acid vapor phase digestion of samples contained in PTFE devices' inserted into the microwave flask. The acid solution is heated by absorption of microwave radiation, then the acid vapor partially condenses in the upper part of the reaction flask and it is partially collected in each sample container. Calcium, Fe, Mg, Mn, and Zn were quantitatively recovered in samples of animal and vegetable tissues. Better recoveries were attained when adding a small volume of sodium hypochlorite to the sample. This effect is probably related to the generation of chlorine in the sample container after collecting condensed acid. The second procedure developed is based on the gradual addition of liquid samples to a previously heated acid digestion mixture. This procedure was successfully applied for digestion of milk, fruit juices, and red wine. The main advantage is the possibility of digesting up to four-fold more sample using up to ten-fold lower amounts of concentrated acids. Results obtained using both digestion procedures and measurements by ICP-OES with axial view will be presented. (author)

Innovative methods for inorganic sample preparation

Energy Technology Data Exchange (ETDEWEB)

Essling, A.M.; Huff, E.A.; Graczyk, D.G.

1992-04-01

Procedures and guidelines are given for the dissolution of a variety of selected materials using fusion, microwave, and Parr bomb techniques. These materials include germanium glass, corium-concrete mixtures, and zeolites. Emphasis is placed on sample-preparation approaches that produce a single master solution suitable for complete multielement characterization of the sample. In addition, data are presented on the soil microwave digestion method approved by the Environmental Protection Agency (EPA). Advantages and disadvantages of each sample-preparation technique are summarized.

Innovative methods for inorganic sample preparation

International Nuclear Information System (INIS)

Essling, A.M.; Huff, E.A.; Graczyk, D.G.

1992-04-01

Procedures and guidelines are given for the dissolution of a variety of selected materials using fusion, microwave, and Parr bomb techniques. These materials include germanium glass, corium-concrete mixtures, and zeolites. Emphasis is placed on sample-preparation approaches that produce a single master solution suitable for complete multielement characterization of the sample. In addition, data are presented on the soil microwave digestion method approved by the Environmental Protection Agency (EPA). Advantages and disadvantages of each sample-preparation technique are summarized

Novel Sample-handling Approach for XRD Analysis with Minimal Sample Preparation

Science.gov (United States)

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.

Newly introduced sample preparation techniques: towards miniaturization.

Science.gov (United States)

Costa, Rosaria

2014-01-01

Sampling and sample preparation are of crucial importance in an analytical procedure, representing quite often a source of errors. The technique chosen for the isolation of analytes greatly affects the success of a chemical determination. On the other hand, growing concerns about environmental and human safety, along with the introduction of international regulations for quality control, have moved the interest of scientists towards specific needs. Newly introduced sample preparation techniques are challenged to meet new criteria: (i) miniaturization, (ii) higher sensitivity and selectivity, and (iii) automation. In this survey, the most recent techniques introduced in the field of sample preparation will be described and discussed, along with many examples of applications.

Miniaturized bead-beating device to automate full DNA sample preparation processes for gram-positive bacteria.

Science.gov (United States)

Hwang, Kyu-Youn; Kwon, Sung Hong; Jung, Sun-Ok; Lim, Hee-Kyun; Jung, Won-Jong; Park, Chin-Sung; Kim, Joon-Ho; Suh, Kahp-Yang; Huh, Nam

2011-11-07

We have developed a miniaturized bead-beating device to automate nucleic acids extraction from Gram-positive bacteria for molecular diagnostics. The microfluidic device was fabricated by sandwiching a monolithic flexible polydimethylsiloxane (PDMS) membrane between two glass wafers (i.e., glass-PDMS-glass), which acted as an actuator for bead collision via its pneumatic vibration without additional lysis equipment. The Gram-positive bacteria, S. aureus and methicillin-resistant S. aureus, were captured on surface-modified glass beads from 1 mL of initial sample solution and in situ lyzed by bead-beating operation. Then, 10 μL or 20 μL of bacterial DNA solution was eluted and amplified successfully by real-time PCR. It was found that liquid volume fraction played a crucial role in determining the cell lysis efficiency in a confined chamber by facilitating membrane deflection and bead motion. The miniaturized bead-beating operation disrupted most of S. aureus within 3 min, which turned out to be as efficient as the conventional benchtop vortexing machine or the enzyme-based lysis technique. The effective cell concentration was significantly enhanced with the reduction of initial sample volume by 50 or 100 times. Combination of such analyte enrichment and in situ bead-beating lysis provided an excellent PCR detection sensitivity amounting to ca. 46 CFU even for the Gram-positive bacteria. The proposed bead-beating microdevice is potentially useful as a nucleic acid extraction method toward a PCR-based sample-to-answer system. This journal is © The Royal Society of Chemistry 2011

Green approaches in sample preparation of bioanalytical samples prior to chromatographic analysis.

Science.gov (United States)

Filippou, Olga; Bitas, Dimitrios; Samanidou, Victoria

2017-02-01

Sample preparation is considered to be the most challenging step of the analytical procedure, since it has an effect on the whole analytical methodology, therefore it contributes significantly to the greenness or lack of it of the entire process. The elimination of the sample treatment steps, pursuing at the same time the reduction of the amount of the sample, strong reductions in consumption of hazardous reagents and energy also maximizing safety for operators and environment, the avoidance of the use of big amount of organic solvents, form the basis for greening sample preparation and analytical methods. In the last decade, the development and utilization of greener and sustainable microextraction techniques is an alternative to classical sample preparation procedures. In this review, the main green microextraction techniques (solid phase microextraction, stir bar sorptive extraction, hollow-fiber liquid phase microextraction, dispersive liquid - liquid microextraction, etc.) will be presented, with special attention to bioanalytical applications of these environment-friendly sample preparation techniques which comply with the green analytical chemistry principles. Copyright © 2016 Elsevier B.V. All rights reserved.

Sample preparation of environmental samples using benzene synthesis followed by high-performance LSC

International Nuclear Information System (INIS)

Filippis, S. De; Noakes, J.E.

1991-01-01

Liquid scintillation counting (LSC) techniques have been widely employed as the detection method for determining environmental levels of tritium and 14 C. Since anthropogenic and nonanthropogenic inputs to the environment are a concern, sampling the environment surrounding a nuclear power facility or fuel reprocessing operation requires the collection of many different sample types, including agriculture products, water, biota, aquatic life, soil, and vegetation. These sample types are not suitable for the direct detection of tritium of 14 C for liquid scintillation techniques. Each sample type must be initially prepared in order to obtain the carbon or hydrogen component of interest and present this in a chemical form that is compatible with common chemicals used in scintillation counting applications. Converting the sample of interest to chemically pure benzene as a sample preparation technique has been widely accepted for processing samples for radiocarbon age-dating applications. The synthesized benzene is composed of the carbon or hydrogen atoms from the original sample and is ideal as a solvent for LSC with excellent photo-optical properties. Benzene synthesis followed by low-background scintillation counting can be applied to the preparation and measurement of environmental samples yielding good detection sensitivities, high radionuclide counting efficiency, and shorter preparation time. The method of benzene synthesis provides a unique approach to the preparation of a wide variety of environmental sample types using similar chemistry for all samples

Quantitative sample preparation of some heavy elements

International Nuclear Information System (INIS)

Jaffey, A.H.

1977-01-01

A discussion is given of some techniques that have been useful in quantitatively preparing and analyzing samples used in the half-life determinations of some plutonium and uranium isotopes. Application of these methods to the preparation of uranium and plutonium samples used in neutron experiments is discussed

7 CFR 27.21 - Preparation of samples of cotton.

Science.gov (United States)

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...

Novel Electrosorption-Enhanced Solid-Phase Microextraction Device for Ultrafast In Vivo Sampling of Ionized Pharmaceuticals in Fish.

Science.gov (United States)

Qiu, Junlang; Wang, Fuxin; Zhang, Tianlang; Chen, Le; Liu, Yuan; Zhu, Fang; Ouyang, Gangfeng

2018-01-02

Decreasing the tedious sample preparation duration is one of the most important concerns for the environmental analytical chemistry especially for in vivo experiments. However, due to the slow mass diffusion paths for most of the conventional methods, ultrafast in vivo sampling remains challenging. Herein, for the first time, we report an ultrafast in vivo solid-phase microextraction (SPME) device based on electrosorption enhancement and a novel custom-made CNT@PPY@pNE fiber for in vivo sampling of ionized acidic pharmaceuticals in fish. This sampling device exhibited an excellent robustness, reproducibility, matrix effect-resistant capacity, and quantitative ability. Importantly, the extraction kinetics of the targeted ionized pharmaceuticals were significantly accelerated using the device, which significantly improved the sensitivity of the SPME in vivo sampling method (limits of detection ranged from 0.12 ng·g -1 to 0.25 ng·g -1 ) and shorten the sampling time (only 1 min). The proposed approach was successfully applied to monitor the concentrations of ionized pharmaceuticals in living fish, which demonstrated that the device and fiber were suitable for ultrafast in vivo sampling and continuous monitoring. In addition, the bioconcentration factor (BCF) values of the pharmaceuticals were derived in tilapia (Oreochromis mossambicus) for the first time, based on the data of ultrafast in vivo sampling. Therefore, we developed and validated an effective and ultrafast SPME sampling device for in vivo sampling of ionized analytes in living organisms and this state-of-the-art method provides an alternative technique for future in vivo studies.

Sample preparation in alkaline media

International Nuclear Information System (INIS)

Nobrega, Joaquim A.; Santos, Mirian C.; Sousa, Rafael A. de; Cadore, Solange; Barnes, Ramon M.; Tatro, Mark

2006-01-01

The use of tetramethylammonium hydroxide, tertiary amines and strongly alkaline reagents for sample treatment involving extraction and digestion procedures is discussed in this review. The preparation of slurries is also discussed. Based on literature data, alkaline media offer a good alternative for sample preparation involving an appreciable group of analytes in different types of samples. These reagents are also successfully employed in tailored speciation procedures wherein there is a critical dependence on maintenance of chemical forms. The effects of these reagents on measurements performed using spectroanalytical techniques are discussed. Several undesirable effects on transport and atomization processes necessitate use of the method of standard additions to obtain accurate results. It is also evident that alkaline media can improve the performance of techniques such as inductively coupled plasma mass spectrometry and accessories, such as autosamplers coupled to graphite furnace atomic absorption spectrometers

Urine sample preparation for proteomic analysis.

Science.gov (United States)

Olszowy, Pawel; Buszewski, Boguslaw

2014-10-01

Sample preparation for both environmental and more importantly biological matrices is a bottleneck of all kinds of analytical processes. In the case of proteomic analysis this element is even more important due to the amount of cross-reactions that should be taken into consideration. The incorporation of new post-translational modifications, protein hydrolysis, or even its degradation is possible as side effects of proteins sample processing. If protocols are evaluated appropriately, then identification of such proteins does not bring difficulties. However, if structural changes are provided without sufficient attention then protein sequence coverage will be reduced or even identification of such proteins could be impossible. This review summarizes obstacles and achievements in protein sample preparation of urine for proteome analysis using different tools for mass spectrometry analysis. The main aim is to present comprehensively the idea of urine application as a valuable matrix. This article is dedicated to sample preparation and application of urine mainly in novel cancer biomarkers discovery. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Improvement of fuel sampling device for STACY and TRACY

International Nuclear Information System (INIS)

Hirose, Hideyuki; Sakuraba, Koichi; Onodera, Seiji

1998-05-01

STACY and TRACY, static and transient experiment facilities in NUCEF, use solution fuel. It is important to analyze accurately fuel composition (uranium enrichment, uranium concentration, nitric acid morality, amount of impurities, radioactivity of FP) for their safety operation and improvement of experimental accuracy. Both STACY and TRACY have the sampling devices to sample fuel solution for that purpose. The previous sampling devices of STACY and TRACY had been designed to dilute fuel sample with nitric acid. Its sampling mechanism could pour fuel sample into sampling vessel by a piston drive of nitric acid in the burette. It was, however, sometimes found that sample fuel solution was diluted by mixing with nitric acid in the burette. Therefore, the sampling mechanism was change into a fixed quantity pump drive which didn't use nitric acid. The authors confirmed that the performance of the new sampling device was improved by changing sampling mechanism. It was confirmed through the function test that the uncertainty in uranium concentration measurement using the improved sampling device was 0.14%, and less than the designed value of 0.2% (coefficient of variation). (author)

Design and device construction for plane tables preparation for counter alpha/beta total; Diseno y construccion de dispositivo para preparacion de planchetas para contador alfa/beta total

Energy Technology Data Exchange (ETDEWEB)

Galicia C, F. J.; Monroy G, F., E-mail: fgalicia82@yahoo.com [ININ, Carretera Mexico-Toluca s/n, 52750 Ocoyoacac, Estado de Mexico (Mexico)

2014-10-15

This work presents the design and assembly of a device for plane tables preparation for quantification alpha/beta total of radioactive waste samples. The determination of the activity index alpha/beta total is used to detect a wide variety of matrices quickly and the concentration of alpha and/or beta emitters of the contained radionuclides in different samples. In particular, the determination of the activity index alpha and beta total of radioactive wastes involves the digestion of samples in aggressive means that will be evaporated to dryness for its quantification. With the purpose of controlling the emission of corrosive gases during the preparation of the plane tables for the quantification of the index alpha and beta total, was designed and built the device in the Radioactive Waste Laboratory that allows to prepare plane tables for proportional counters in a sure and efficient way. The device is constituted by heating equipment, evaporation cylinder and a gases cleaning system. The self-absorption curve got ready starting from the device. (Author)

30 CFR 90.206 - Approved sampling devices; equivalent concentrations.

Science.gov (United States)

2010-07-01

... 30 Mineral Resources 1 2010-07-01 2010-07-01 false Approved sampling devices; equivalent... LABOR COAL MINE SAFETY AND HEALTH MANDATORY HEALTH STANDARDS-COAL MINERS WHO HAVE EVIDENCE OF THE DEVELOPMENT OF PNEUMOCONIOSIS Sampling Procedures § 90.206 Approved sampling devices; equivalent...

Tube closure device, especially for sample irradiation

International Nuclear Information System (INIS)

Klahn, F.C.; Nolan, J.H.; Wills, C.

1979-01-01

Device for closing the outlet of a bore and temporarily locking components in this bore. Specifically, it concerns a device for closing a tube containing a set of samples for monitoring irradiation in a nuclear reactor [fr

Recent Trends in Microextraction Techniques Employed in Analytical and Bioanalytical Sample Preparation

Directory of Open Access Journals (Sweden)

Abuzar Kabir

2017-12-01

Full Text Available Sample preparation has been recognized as a major step in the chemical analysis workflow. As such, substantial efforts have been made in recent years to simplify the overall sample preparation process. Major focusses of these efforts have included miniaturization of the extraction device; minimizing/eliminating toxic and hazardous organic solvent consumption; eliminating sample pre-treatment and post-treatment steps; reducing the sample volume requirement; reducing extraction equilibrium time, maximizing extraction efficiency etc. All these improved attributes are congruent with the Green Analytical Chemistry (GAC principles. Classical sample preparation techniques such as solid phase extraction (SPE and liquid-liquid extraction (LLE are being rapidly replaced with emerging miniaturized and environmentally friendly techniques such as Solid Phase Micro Extraction (SPME, Stir bar Sorptive Extraction (SBSE, Micro Extraction by Packed Sorbent (MEPS, Fabric Phase Sorptive Extraction (FPSE, and Dispersive Liquid-Liquid Micro Extraction (DLLME. In addition to the development of many new generic extraction sorbents in recent years, a large number of molecularly imprinted polymers (MIPs created using different template molecules have also enriched the large cache of microextraction sorbents. Application of nanoparticles as high-performance extraction sorbents has undoubtedly elevated the extraction efficiency and method sensitivity of modern chromatographic analyses to a new level. Combining magnetic nanoparticles with many microextraction sorbents has opened up new possibilities to extract target analytes from sample matrices containing high volumes of matrix interferents. The aim of the current review is to critically audit the progress of microextraction techniques in recent years, which has indisputably transformed the analytical chemistry practices, from biological and therapeutic drug monitoring to the environmental field; from foods to phyto

Recent advances in applications of nanomaterials for sample preparation.

Science.gov (United States)

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.

Liquid scintillation: Sample preparation and counting atypical emissions

International Nuclear Information System (INIS)

Anon.

1991-01-01

Liquid scintillation sample preparation has the most published information but the least amount of definitive technical direction because the chemical and physical nature of the samples from biological investigations varies widely. This chapter discusses the following related topics: Aqueous Samples; Tissue Solubilizers; Absorption of 14 CO 2 ; Sample Combustion Methods; Heterogeneous Systems; Sample Preparation Problems (colored samples, chemiluminescence, photoluminescence, static electricity); Counting Various Types of Emitters; Counting Atypical Emissions. 2 refs., 2 figs

Homogeneous immunosubtraction integrated with sample preparation is enabled by a microfluidic format

Science.gov (United States)

Apori, Akwasi A.; Herr, Amy E.

2011-01-01

Immunosubtraction is a powerful and resource-intensive laboratory medicine assay that reports both protein mobility and binding specificity. To expedite and automate this electrophoretic assay, we report on advances to the electrophoretic immunosubtraction assay by introducing a homogeneous, not heterogeneous, format with integrated sample preparation. To accomplish homogeneous immunosubtraction, a step-decrease in separation matrix pore-size at the head of a polyacrylamide gel electrophoresis (PAGE) separation channel enables ‘subtraction’ of target analyte when capture antibody is present (as the large immune-complex is excluded from PAGE), but no subtraction when capture antibody is absent. Inclusion of sample preparation functionality via small pore size polyacrylamide membranes is also key to automated operation (i.e., sample enrichment, fluorescence sample labeling, and mixing of sample with free capture antibody). Homogenous sample preparation and assay operation allows on-the-fly, integrated subtraction of one to multiple protein targets and reuse of each device. Optimization of the assay is detailed which allowed for ~95% subtraction of target with 20% non-specific extraction of large species at the optimal antibody-antigen ratio, providing conditions needed for selective target identification. We demonstrate the assay on putative markers of injury and inflammation in cerebrospinal fluid (CSF), an emerging area of diagnostics research, by rapidly reporting protein mobility and binding specificity within the sample matrix. We simultaneously detect S100B and C-reactive protein, suspected biomarkers for traumatic brain injury (TBI), in ~2 min. Lastly, we demonstrate S100B detection (65 nM) in raw human CSF with a lower limit of detection of ~3.25 nM, within the clinically relevant concentration range for detecting TBI in CSF. Beyond the novel CSF assay introduced here, a fully automated immunosubtraction assay would impact a spectrum of routine but labor

Sieve-based device for MALDI sample preparation. III. Its power for quantitative measurements.

Science.gov (United States)

Molin, Laura; Cristoni, Simone; Seraglia, Roberta; Traldi, Pietro

2011-02-01

The solid sample inhomogeneity is a weak point of traditional MALDI deposition techniques that reflects negatively on quantitative analysis. The recently developed sieve-based device (SBD) sample deposition method, based on the electrospraying of matrix/analyte solutions through a grounded sieve, allows the homogeneous deposition of microcrystals with dimensions smaller than that of the laser spot. In each microcrystal the matrix/analyte molar ratio can be considered constant. Then, by irradiating different portions of the microcrystal distribution an identical response is obtained. This result suggests the employment of SBD in the development of quantitative procedures. For this aim, mixtures of different proteins of known molarity were analyzed, showing a good relationship between molarity and intensity ratios. This behaviour was also observed in the case of proteins with quite different ionic yields. The power of the developed method for quantitative evaluation was also tested by the measurement of the abundance of IGPP[Oxi]GPP[Oxi]GLMGPP (m/z 1219) present in the collagen-α-5(IV) chain precursor, differently expressed in urines from healthy subjects and diabetic-nephropathic patients, confirming its overexpression in the presence of nephropathy. The data obtained indicate that SBD is a particularly effective method for quantitative analysis also in biological fluids of interest. Copyright © 2011 John Wiley & Sons, Ltd.

Modular microfluidic system for biological sample preparation

Science.gov (United States)

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.

Applications of Liquid-Phase Microextraction in the Sample Preparation of Environmental Solid Samples

Directory of Open Access Journals (Sweden)

Helena Prosen

2014-05-01

Full Text Available Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc. published in the last decade. Several innovative liquid-phase microextraction (LPME techniques that have emerged recently have also been applied as an aid in sample preparation of these samples: single-drop microextraction (SDME, hollow fiber-liquid phase microextraction (HF-LPME, dispersive liquid-liquid microextraction (DLLME. Besides the common organic solvents, surfactants and ionic liquids are also used. However, these techniques have to be combined with another technique to release the analytes from the solid sample into an aqueous solution. In the present review, the published methods were categorized into three groups: LPME in combination with a conventional solvent extraction; LPME in combination with an environmentally friendly extraction; LPME without previous extraction. The applicability of these approaches to the sample preparation for the determination of pollutants in solid environmental samples is discussed, with emphasis on their strengths, weak points and environmental impact.

Applications of liquid-phase microextraction in the sample preparation of environmental solid samples.

Science.gov (United States)

Prosen, Helena

2014-05-23

Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc.) published in the last decade. Several innovative liquid-phase microextraction (LPME) techniques that have emerged recently have also been applied as an aid in sample preparation of these samples: single-drop microextraction (SDME), hollow fiber-liquid phase microextraction (HF-LPME), dispersive liquid-liquid microextraction (DLLME). Besides the common organic solvents, surfactants and ionic liquids are also used. However, these techniques have to be combined with another technique to release the analytes from the solid sample into an aqueous solution. In the present review, the published methods were categorized into three groups: LPME in combination with a conventional solvent extraction; LPME in combination with an environmentally friendly extraction; LPME without previous extraction. The applicability of these approaches to the sample preparation for the determination of pollutants in solid environmental samples is discussed, with emphasis on their strengths, weak points and environmental impact.

Reagentless mechanical cell lysis by nanoscale barbs in microchannels for sample preparation.

Science.gov (United States)

Di Carlo, Dino; Jeong, Ki-Hun; Lee, Luke P

2003-11-01

A highly effective, reagentless, mechanical cell lysis device integrated in microfluidic channels is reported. Sample preparation, specifically cell lysis, is a critical element in 'lab-on-chip' applications. However, traditional methods of cell lysis require purification steps or complicated fabrication steps that a simple mechanical method of lysis may avoid. A simple and effective mechanical cell lysis system is designed, microfabricated, and characterized to quantify the efficiency of cell lysis and biomolecule accessibility. The device functionality is based on a microfluidic filter region with nanostructured barbs created using a modified deep reactive ion etching process. Mechanical lysis is characterized by using a membrane impermeable dye. Three main mechanisms of micro-mechanical lysis are described. Quantitative measurements of accessible protein as compared to a chemically lysed sample are acquired with optical absorption measurements at 280 and 414 nm. At a flow rate of 300 microL min(-1) within the filter region total protein and hemoglobin accessibilities of 4.8% and 7.5% are observed respectively as compared to 1.9% and 3.2% for a filter without nanostructured barbs.

Indigenous development of automated metallographic sample preparation system

International Nuclear Information System (INIS)

Kulkarni, A.P.; Pandit, K.M.; Deshmukh, A.G.; Sahoo, K.C.

2005-01-01

Surface preparation of specimens for Metallographic studies on irradiated material involves a lot of remote handling of radioactive material by skilled manpower. These are laborious and man-rem intensive activities and put limitations on number of samples that can be prepared for the metallographic studies. To overcome these limitations, automated systems have been developed for surface preparation of specimens in PIE division. The system includes (i) Grinding and polishing stations (ii) Water jet cleaning station (iii) Ultrasonic cleaning stations (iv) Drying station (v) Sample loading and unloading station (vi) Dispenser for slurries and diluents and (vii) Automated head for movement of the sample holder disc from one station to other. System facilities the operator for programming/changing sequence of the sample preparations including remote changing of grinding/polishing discs from the stations. Two such systems have been installed and commissioned in Hot Cell for PIE Division. These are being used for preparation of irradiated samples from nuclear fuels and structural components. This development has increased the throughput of metallography work and savings in terms of (man-severts) radiation exposure to operators. This presentation will provide details of the challenges in undertaking this developmental work. (author)

Applications of Liquid-Phase Microextraction in the Sample Preparation of Environmental Solid Samples

OpenAIRE

Helena Prosen

2014-01-01

Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc.) published in the last decade. Several...

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

Directory of Open Access Journals (Sweden)

Mohd Farhan Siddiqui

2018-03-01

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

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

Science.gov (United States)

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

2018-03-04

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

New materials for sample preparation techniques in bioanalysis.

Science.gov (United States)

Nazario, Carlos Eduardo Domingues; Fumes, Bruno Henrique; da Silva, Meire Ribeiro; Lanças, Fernando Mauro

2017-02-01

The analysis of biological samples is a complex and difficult task owing to two basic and complementary issues: the high complexity of most biological matrices and the need to determine minute quantities of active substances and contaminants in such complex sample. To succeed in this endeavor samples are usually subject to three steps of a comprehensive analytical methodological approach: sample preparation, analytes isolation (usually utilizing a chromatographic technique) and qualitative/quantitative analysis (usually with the aid of mass spectrometric tools). Owing to the complex nature of bio-samples, and the very low concentration of the target analytes to be determined, selective sample preparation techniques is mandatory in order to overcome the difficulties imposed by these two constraints. During the last decade new chemical synthesis approaches has been developed and optimized, such as sol-gel and molecularly imprinting technologies, allowing the preparation of novel materials for sample preparation including graphene and derivatives, magnetic materials, ionic liquids, molecularly imprinted polymers, and much more. In this contribution we will review these novel techniques and materials, as well as their application to the bioanalysis niche. Copyright © 2016 Elsevier B.V. All rights reserved.

Device for sampling HTGR recycle fuel particles

International Nuclear Information System (INIS)

Suchomel, R.R.; Lackey, W.J.

1977-03-01

Devices for sampling High-Temperature Gas-Cooled Reactor fuel microspheres were evaluated. Analysis of samples obtained with each of two specially designed passive samplers were compared with data generated by more common techniques. A ten-stage two-way sampler was found to produce a representative sample with a constant batch-to-sample ratio

Wideband 4-diode sampling circuit

Science.gov (United States)

Wojtulewicz, Andrzej; Radtke, Maciej

2016-09-01

The objective of this work was to develop a wide-band sampling circuit. The device should have the ability to collect samples of a very fast signal applied to its input, strengthen it and prepare for further processing. The study emphasizes the method of sampling pulse shaping. The use of ultrafast pulse generator allows sampling signals with a wide frequency spectrum, reaching several gigahertzes. The device uses a pulse transformer to prepare symmetrical pulses. Their final shape is formed with the help of the step recovery diode, two coplanar strips and Schottky diode. Made device can be used in the sampling oscilloscope, as well as other measurement system.

Sample Preparation for Electron Probe Microanalysis-Pushing the Limits.

Science.gov (United States)

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

Water sampling device for fuel rod failure monitoring

International Nuclear Information System (INIS)

Oogami, Hideaki; Echigoya, Hironori; Matsuoka, Tesshi.

1991-01-01

The device of the present invention accurately samples coolants in a channel box as sampling water even if the upper end of the channel box of a fuel assembly is positioned at the same height or lower than the upper end of an upper lattice plate. An existent device comprises an outer cap, an inner cap, an air supply pipe and a water sampling tube. In addition, the device of the present invention comprises a sealing material disposed at the end of the outer cap for keeping liquid sealing with the upper lattice plate and a water level monitoring pipe extended to lower than the inner cap passing through the liquid sealing of the outer cap for sucking the atmosphere in the outer cap. Pressurized air is sent through the air supply pipe, to lower the water level of the coolants in the outer cap and the water level monitoring pipe sucks the pressurized air, by which the inside and the outside of the channel box are partitioned. Subsequently, if the sample water is sampled by a sampling tube, sampling water which enables accurate evaluation for radioactivity concentration in the fuel assembly can be obtained. (I.S.)

Preparation of honey sample for tritium monitoring

International Nuclear Information System (INIS)

Chen Bingru; Wang Chenlian; Wang Weihua

1989-01-01

The method of preparation of honey sample for tritium monitoring was described. The equipments consist of an air and honey supply system, a quartz combustor with CM-type monolithic combustion catalyst and a condensation system. In the equipments, honey sample was converted into cooling water by the distilling, cracking and carbonizing procedures for tritium counting. The recovery ratio is 99.0 ± 4.5 percent for tritiated water and 96.0 ± 2.0 for tritiated organic compounds. It is a feasible preparing method for the total tritium monitoring in honey sample

Platelet-rich fibrin prepared from stored whole-blood samples.

Science.gov (United States)

Isobe, Kazushige; Suzuki, Masashi; Watanabe, Taisuke; Kitamura, Yutaka; Suzuki, Taiji; Kawabata, Hideo; Nakamura, Masayuki; Okudera, Toshimitsu; Okudera, Hajime; Uematsu, Kohya; Nakata, Koh; Tanaka, Takaaki; Kawase, Tomoyuki

2017-12-01

In regenerative therapy, self-clotted platelet concentrates, such as platelet-rich fibrin (PRF), are generally prepared on-site and are immediately used for treatment. If blood samples or prepared clots can be preserved for several days, their clinical applicability will expand. Here, we prepared PRF from stored whole-blood samples and examined their characteristics. Blood samples were collected from non-smoking, healthy male donors (aged 27-67 years, N = 6), and PRF clots were prepared immediately or after storage for 1-2 days. Fibrin fiber was examined by scanning electron microscopy. Bioactivity was evaluated by means of a bioassay system involving human periosteal cells, whereas PDGF-BB concentrations were determined by an enzyme-linked immunosorbent assay. Addition of optimal amounts of a 10% CaCl 2 solution restored the coagulative ability of whole-blood samples that contained an anticoagulant (acid citrate dextrose) and were stored for up to 2 days at ambient temperature. In PRF clots prepared from the stored whole-blood samples, the thickness and cross-links of fibrin fibers were almost identical to those of freshly prepared PRF clots. PDGF-BB concentrations in the PRF extract were significantly lower in stored whole-blood samples than in fresh samples; however, both extracts had similar stimulatory effects on periosteal-cell proliferation. Quality of PRF clots prepared from stored whole-blood samples is not reduced significantly and can be ensured for use in regenerative therapy. Therefore, the proposed method enables a more flexible treatment schedule and choice of a more suitable platelet concentrate immediately before treatment, not after blood collection.

The effect of sample preparation on uranium hydriding

International Nuclear Information System (INIS)

Banos, A.; Stitt, C.A.; Scott, T.B.

2016-01-01

Highlights: • Distinct differences in uranium hydride growth rates and characteristics between different surface preparation methods. • The primary difference between the categories of sample preparations is the level of strain present in the surface. • Greater surface-strain, leads to higher nucleation number density, implying a preferred attack of strained vs unstrained metal. • As strain is reduced, surface features such as carbides and grain boundaries become more important in controlling the UH3 location. - Abstract: The influence of sample cleaning preparation on the early stages of uranium hydriding has been examined, by using four identical samples but concurrently prepared using four different methods. The samples were reacted together in the same corrosion cell to ensure identical exposure conditions. From the analysis, it was found that the hydride nucleation rate was proportional to the level of strain exhibiting higher number density for the more strained surfaces. Additionally, microstructure of the metal plays a secondary role regarding initial hydrogen attack on the highly strained surfaces yet starts to dominate the system while moving to more pristine samples.

Efficient sample preparation from complex biological samples using a sliding lid for immobilized droplet extractions.

Science.gov (United States)

Casavant, Benjamin P; Guckenberger, David J; Beebe, David J; Berry, Scott M

2014-07-01

Sample preparation is a major bottleneck in many biological processes. Paramagnetic particles (PMPs) are a ubiquitous method for isolating analytes of interest from biological samples and are used for their ability to thoroughly sample a solution and be easily collected with a magnet. There are three main methods by which PMPs are used for sample preparation: (1) removal of fluid from the analyte-bound PMPs, (2) removal of analyte-bound PMPs from the solution, and (3) removal of the substrate (with immobilized analyte-bound PMPs). In this paper, we explore the third and least studied method for PMP-based sample preparation using a platform termed Sliding Lid for Immobilized Droplet Extractions (SLIDE). SLIDE leverages principles of surface tension and patterned hydrophobicity to create a simple-to-operate platform for sample isolation (cells, DNA, RNA, protein) and preparation (cell staining) without the need for time-intensive wash steps, use of immiscible fluids, or precise pinning geometries. Compared to other standard isolation protocols using PMPs, SLIDE is able to perform rapid sample preparation with low (0.6%) carryover of contaminants from the original sample. The natural recirculation occurring within the pinned droplets of SLIDE make possible the performance of multistep cell staining protocols within the SLIDE by simply resting the lid over the various sample droplets. SLIDE demonstrates a simple easy to use platform for sample preparation on a range of complex biological samples.

Sample Preparation for Electron Probe Microanalysis—Pushing the Limits

Science.gov (United States)

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

40 CFR 205.160-2 - Test sample selection and preparation.

Science.gov (United States)

2010-07-01

... 40 Protection of Environment 24 2010-07-01 2010-07-01 false Test sample selection and preparation... sample selection and preparation. (a) Vehicles comprising the sample which are required to be tested... maintained in any manner unless such preparation, tests, modifications, adjustments or maintenance are part...

Subperiosteal preparation using a new piezoelectric device: a histological examination

OpenAIRE

Stoetzer, Marcus; Magel, Anja; Kampmann, Andreas; Lemound, Juliana; Gellrich, Nils-Claudius; von See, Constantin

2014-01-01

Introduction: Subperiosteal preparation using a periosteal elevator leads to disturbances of local immunohistochemistry and periosteal histology due to a microtrauma. Usually soft-tissue damage can be considerably reduced by using piezoelectric technology. For this reason, the effects of a novel piezoelectric device on immunohistochemistry and periosteal histology were examined and compared to conventional preparation of the periosteum using a periosteal elevator.Material and methods: Lewis...

Application of a Dual-Arm Robot in Complex Sample Preparation and Measurement Processes.

Science.gov (United States)

Fleischer, Heidi; Drews, Robert Ralf; Janson, Jessica; Chinna Patlolla, Bharath Reddy; Chu, Xianghua; Klos, Michael; Thurow, Kerstin

2016-10-01

Automation systems with applied robotics have already been established in industrial applications for many years. In the field of life sciences, a comparable high level of automation can be found in the areas of bioscreening and high-throughput screening. Strong deficits still exist in the development of flexible and universal fully automated systems in the field of analytical measurement. Reasons are the heterogeneous processes with complex structures, which include sample preparation and transport, analytical measurements using complex sensor systems, and suitable data analysis and evaluation. Furthermore, the use of nonstandard sample vessels with various shapes and volumes results in an increased complexity. The direct use of existing automation solutions from bioscreening applications is not possible. A flexible automation system for sample preparation, analysis, and data evaluation is presented in this article. It is applied for the determination of cholesterol in biliary endoprosthesis using gas chromatography-mass spectrometry (GC-MS). A dual-arm robot performs both transport and active manipulation tasks to ensure human-like operation. This general robotic concept also enables the use of manual laboratory devices and equipment and is thus suitable in areas with a high standardization grade. © 2016 Society for Laboratory Automation and Screening.

Independent assessment of matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) sample preparation quality: Effect of sample preparation on MALDI-MS of synthetic polymers.

Science.gov (United States)

Kooijman, Pieter C; Kok, Sander; Honing, Maarten

2017-02-28

Matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) provides detailed and in-depth information about the molecular characteristics of synthetic polymers. To obtain the most accurate results the sample preparation parameters should be chosen to suit the sample and the aim of the experiment. Because the underlying principles of MALDI are still not fully known, a priori determination of optimal sample preparation protocols is often not possible. Employing an automated sample preparation quality assessment method recently presented by us we quantified the sample preparation quality obtained using various sample preparation protocols. Six conventional matrices with and without added potassium as a cationization agent and six ionic liquid matrices (ILMs) were assessed using poly(ethylene glycol) (PEG), polytetrahydrofuran (PTHF) and poly(methyl methacrylate) (PMMA) as samples. All sample preparation protocols were scored and ranked based on predefined quality parameters and spot-to-spot repeatability. Clearly distinctive preferences were observed in matrix identity and cationization agent for PEG, PTHF and PMMA, as the addition of an excess of potassium cationization agent results in an increased score for PMMA and a contrasting matrix-dependent effect for PTHF and PEG. The addition of excess cationization agent to sample mixtures dissipates any overrepresentation of high molecular weight polymer species. Our results show reduced ionization efficiency and similar sample deposit homogeneity for all tested ILMs, compared with well-performing conventional MALDI matrices. The results published here represent a start in the unsupervised quantification of sample preparation quality for MALDI samples. This method can select the best sample preparation parameters for any synthetic polymer sample and the results can be used to formulate hypotheses on MALDI principles. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

30 CFR 90.204 - Approved sampling devices; maintenance and calibration.

Science.gov (United States)

2010-07-01

... 30 Mineral Resources 1 2010-07-01 2010-07-01 false Approved sampling devices; maintenance and... LABOR COAL MINE SAFETY AND HEALTH MANDATORY HEALTH STANDARDS-COAL MINERS WHO HAVE EVIDENCE OF THE DEVELOPMENT OF PNEUMOCONIOSIS Sampling Procedures § 90.204 Approved sampling devices; maintenance and...

30 CFR 90.205 - Approved sampling devices; operation; air flowrate.

Science.gov (United States)

2010-07-01

... 30 Mineral Resources 1 2010-07-01 2010-07-01 false Approved sampling devices; operation; air... LABOR COAL MINE SAFETY AND HEALTH MANDATORY HEALTH STANDARDS-COAL MINERS WHO HAVE EVIDENCE OF THE DEVELOPMENT OF PNEUMOCONIOSIS Sampling Procedures § 90.205 Approved sampling devices; operation; air flowrate...

Congener Production in Blood Samples During Preparation and Storage

DEFF Research Database (Denmark)

Felby, Søren; Nielsen, Erik

1995-01-01

Retsmedicin, congener production, preparation, head space GC, acetone, isobutanol, storage, blood samples, n-propanol, methanol, methylethylketone......Retsmedicin, congener production, preparation, head space GC, acetone, isobutanol, storage, blood samples, n-propanol, methanol, methylethylketone...

A device for fresh water sampling before radioactive measurements

International Nuclear Information System (INIS)

Maubert, Henri; Picat, Philippe.

1982-06-01

On account of the many field operations carried out by the laboratory, a water sampling device has been developed. This portable autonomous device performs in situ water filtration and concentration on ion exchange resins and activated carbon columns. The device is described and the trapping performance for 8 radionuclides is given. A comparison is made with the so-called evaporation method. The effects of the treatment of the filtrating elements on the radioactive results are studied. This sampling method is very sensitive [fr

Trends in sample preparation 2002. Development and application. Book of abstracts

International Nuclear Information System (INIS)

Wenzl, T.; Eberl, M.; Zischka, M.; Knapp, G.

2002-01-01

This conference comprised topics dealing with sample preparation such as: sample decomposition, solvent extraction, derivatization techniques and uncertainty in sample preparation. In particular microwave assisted sample preparation techniques and equipment were discussed. The papers were organized under the general topics: trace element analysis, trace analysis of organic compounds, high performance instrumentation in sample preparation, speciation analysis and posters session. Those papers of INIS interest are cited individually. (nevyjel)

Trends in sample preparation 2002. Development and application. Book of abstracts

Energy Technology Data Exchange (ETDEWEB)

Wenzl, T; Eberl, M; Zischka, M; Knapp, G [eds.

2002-07-01

This conference comprised topics dealing with sample preparation such as: sample decomposition, solvent extraction, derivatization techniques and uncertainty in sample preparation. In particular microwave assisted sample preparation techniques and equipment were discussed. The papers were organized under the general topics: trace element analysis, trace analysis of organic compounds, high performance instrumentation in sample preparation, speciation analysis and posters session. Those papers of INIS interest are cited individually. (nevyjel)

On-line Automated Sample Preparation-Capillary Gas Chromatography for the Analysis of Plasma Samples.

NARCIS (Netherlands)

Louter, A.J.H.; van der Wagt, R.A.C.A.; Brinkman, U.A.T.

1995-01-01

An automated sample preparation module, (the automated sample preparation with extraction columns, ASPEC), was interfaced with a capillary gas chromatograph (GC) by means of an on-column interface. The system was optimised for the determination of the antidepressant trazodone in plasma. The clean-up

Cr(VI) generation during sample preparation of solid samples – A ...

African Journals Online (AJOL)

Cr(VI) generation during sample preparation of solid samples – A chromite ore case study. R.I Glastonbury, W van der Merwe, J.P Beukes, P.G van Zyl, G Lachmann, C.J.H Steenkamp, N.F Dawson, M.H Stewart ...

A Lab on a chip device for rapid identification of Avian Influenza virus by on-chip sample preparation and solid phase PCR

DEFF Research Database (Denmark)

Yi, Sun; Dhumpa, Raghuram; Bang, Dang Duong

2009-01-01

In this paper, we describe a novel lab-on-a-chip device for fast AIV screening by integrating DNA microarray-based solid phase PCR on microchip. The device can handle viral samples in an automatic way. Moreover, multiplex PCR and sequence detection are done in one-step, which greatly simplifies...

Device for radioactivity measurement of liquid samples

International Nuclear Information System (INIS)

Lamaziere, J.

1983-01-01

The device for low activity gamma measurements comprises an automatic changer for sample transfer from a conveyor to a measuring chamber. The conveyor includes a horizontal table were are regularly distributed sample holders. A lift allows a vertical motion of a plate for the exposition in front of a detector [fr

Integrated microfabricated biodevices. New advances in sample preparation (T2)

International Nuclear Information System (INIS)

Guttman, A.

2002-01-01

Full text: Interdisciplinary science and technologies have converged in the past few years to create exciting challenges and opportunities, which involve novel, integrated microfabricated systems, facilitating large-scale analytical applications. These new devices are referred to as lab-on-a-chip or micro Total Analysis Systems (uTAS). Their development involves both established and evolving technologies, which include microlithography, micromachining, micro-electromechanical systems (MEMS) technology, microfluidics and nanotechnology. The advent of this extremely powerful and rapid analysis technique opens up new horizons in analytical chemistry and molecular biology, capable of revealing global changes in gene expression levels by enabling genome, proteome and metabolome analysis on microchips. This presentation will provide an overview of the key device subject areas and the basic interdisciplinary technologies. It will also give a better understanding of how to utilize these miniaturized technologies as well as to provide appropriate technical solutions to problems perceived as being more fundamental. Theoretical and practical aspects of integrating sample preparation/purification and analysis units with chemical and biochemical reactors in monolithic microdevices are going to be thoroughly discussed. Important applications for this novel 'synergized' technology in high throughput analysis of biologically important molecules will also be addressed. (author)

Current trends in sample preparation for cosmetic analysis.

Science.gov (United States)

Zhong, Zhixiong; Li, Gongke

2017-01-01

The widespread applications of cosmetics in modern life make their analysis particularly important from a safety point of view. There is a wide variety of restricted ingredients and prohibited substances that primarily influence the safety of cosmetics. Sample preparation for cosmetic analysis is a crucial step as the complex matrices may seriously interfere with the determination of target analytes. In this review, some new developments (2010-2016) in sample preparation techniques for cosmetic analysis, including liquid-phase microextraction, solid-phase microextraction, matrix solid-phase dispersion, pressurized liquid extraction, cloud point extraction, ultrasound-assisted extraction, and microwave digestion, are presented. Furthermore, the research and progress in sample preparation techniques and their applications in the separation and purification of allowed ingredients and prohibited substances are reviewed. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The Recent Developments in Sample Preparation for Mass Spectrometry-Based Metabolomics.

Science.gov (United States)

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.

Soil sample preparation using microwave digestion for uranium analysis

International Nuclear Information System (INIS)

Mohagheghi, Amir H.; Preston, Rose; Akbarzadeh, Mansoor; Bakthiar, Steven

2000-01-01

A new sample preparation procedure has been developed for digestion of soil samples for uranium analysis. The technique employs a microwave oven digestion system to digest the sample and to prepare it for separation chemistry and analysis. The method significantly reduces the volume of acids used, eliminates a large fraction of acid vapor emissions, and speeds up the analysis time. The samples are analyzed by four separate techniques: Gamma Spectrometry, Alpha Spectroscopy using the open digestion method, Kinetic Phosphorescence Analysis (KPA) using open digestion, and KPA by Microwave digestion technique. The results for various analytical methods are compared and used to confirm the validity of the new procedure. The details of the preparation technique along with its benefits are discussed

7 CFR 61.34 - Drawing and preparation of sample.

Science.gov (United States)

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...

New trends in sample preparation techniques for environmental analysis.

Science.gov (United States)

Ribeiro, Cláudia; Ribeiro, Ana Rita; Maia, Alexandra S; Gonçalves, Virgínia M F; Tiritan, Maria Elizabeth

2014-01-01

Environmental samples include a wide variety of complex matrices, with low concentrations of analytes and presence of several interferences. Sample preparation is a critical step and the main source of uncertainties in the analysis of environmental samples, and it is usually laborious, high cost, time consuming, and polluting. In this context, there is increasing interest in developing faster, cost-effective, and environmentally friendly sample preparation techniques. Recently, new methods have been developed and optimized in order to miniaturize extraction steps, to reduce solvent consumption or become solventless, and to automate systems. This review attempts to present an overview of the fundamentals, procedure, and application of the most recently developed sample preparation techniques for the extraction, cleanup, and concentration of organic pollutants from environmental samples. These techniques include: solid phase microextraction, on-line solid phase extraction, microextraction by packed sorbent, dispersive liquid-liquid microextraction, and QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe).

Tooth enamel sample preparation using alkaline treatment in ESR dosimetry

International Nuclear Information System (INIS)

Yongzeng, Zhou; Jiadong, Wang; Xiaomei, Jia; Ke, Wu; Jianbo, Cong

2002-01-01

Tooth enamel sample preparation using alkaline treatment was studied and compared with traditional mechanical method in this paper. 20 adult teeth were used. Samples were placed into NaOH solution. This method requires 4-5 weeks and the enamel was separated from dentin. Experimental results show that 8M NaOH was appropriate for separating enamel from dentin and that there is no difference in background signal relative intensity between samples prepared by mechanical and by chemical methods. There is also no difference in radiosensitivity between samples prepared by two methods mentioned above. Dose response curve for tooth enamel samples isolated by 8M NaOH solution was obtained

High-throughput automated microfluidic sample preparation for accurate microbial genomics.

Science.gov (United States)

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

2017-01-27

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.

Optoelectronic devices, low temperature preparation methods, and improved electron transport layers

KAUST Repository

Eita, Mohamed S.

2016-08-04

An optoelectronic device such as a photovoltaic device which has at least one layer, such as an electron transport layer, which comprises a plurality of alternating, oppositely charged layers including metal oxide layers. The metal oxide can be zinc oxide. The plurality of layers can be prepared by layer-by-layer processing in which alternating layers are built up step-by-step due to electrostatic attraction. The efficiency of the device can be increased by this processing method compared to a comparable method like sputtering. The number of layers can be controlled to improve device efficiency. Aqueous solutions can be used which is environmentally friendly. Annealing can be avoided. A quantum dot layer can be used next to the metal oxide layer to form a quantum dot heterojunction solar device.

Sample preparations for spark source mass spectrography

International Nuclear Information System (INIS)

Catlett, C.W.; Rollins, M.B.; Griffin, E.B.; Dorsey, J.G.

1977-10-01

Methods have been developed for the preparation of various materials for spark source mass spectrography. The essential features of these preparations (all which can provide adequate precision in a cost-effective manner) consist in obtaining spark-stable electrode sample pieces, a common matrix, a reduction of anomolous effects in the spark, the incorporation of a suitable internal standard for plate response normalization, and a reduction in time

Present status of NMCC and sample preparation method for bio-samples

International Nuclear Information System (INIS)

Futatsugawa, S.; Hatakeyama, S.; Saitou, S.; Sera, K.

1993-01-01

In NMCC(Nishina Memorial Cyclotron Center) we are doing researches on PET of nuclear medicine (Positron Emission Computed Tomography) and PIXE analysis (Particle Induced X-ray Emission) using a small cyclotron of compactly designed. The NMCC facilities have been opened to researchers of other institutions since April 1993. The present status of NMCC is described. Bio-samples (medical samples, plants, animals and environmental samples) have mainly been analyzed by PIXE in NMCC. Small amounts of bio-samples for PIXE are decomposed quickly and easily in a sealed PTFE (polytetrafluoroethylene) vessel with a microwave oven. This sample preparation method of bio-samples also is described. (author)

Finding even more anthropogenic indicators in mildly prepared sediment samples

DEFF Research Database (Denmark)

Enevold, Renée; Odgaard, Bent Vad

2016-01-01

be worth the effort to prepare the NPP samples with as mild a preparation method as possible. We have mildly prepared NPP samples from a small forest hollow, Tårup Lund, Denmark. From the recovered NPP assemblages we attempt identifying anthropogenic indicators by comparing to the environmental information......NPPs in anthropogenic soils and archaeological samples are often numerous in types as well as in abundance. Preparing these soil samples with methods based on acid digestion holds the potential of severe bias leaving the NPP assemblages devoid of acid vulnerable NPPs. In many cases it might...... derived from sediment, pollen and macrofossil analyses. The sediment from the forest hollow encompasses environmental information from the last 6000 years, including a period of locally intense pastoral and/or agricultural activity during the Iron Age. Keywords: NPP diversity, forest hollow, anthropogenic...

Sampling, storage and sample preparation procedures for X ray fluorescence analysis of environmental materials

International Nuclear Information System (INIS)

1997-06-01

X ray fluorescence (XRF) method is one of the most commonly used nuclear analytical technique because of its multielement and non-destructive character, speed, economy and ease of operation. From the point of view of quality assurance practices, sampling and sample preparation procedures are the most crucial steps in all analytical techniques, (including X ray fluorescence) applied for the analysis of heterogeneous materials. This technical document covers recent modes of the X ray fluorescence method and recent developments in sample preparation techniques for the analysis of environmental materials. Refs, figs, tabs

Influences of different sample preparation methods on tooth enamel ESR signals

International Nuclear Information System (INIS)

Zhang Wenyi; Jiao Ling; Zhang Liang'an; Pan Zhihong; Zeng Hongyu

2005-01-01

Objective: To study the influences of different sample preparation methods on tooth enamel ESR signals in order to reduce the effect of dentine on their sensitivities to radiation. Methods: The enamel was separated from dentine of non-irradiated adult teeth by mechanical, chemical, or both methods. The samples of different preparations were scanned by an ESR spectrometer before and after irradiation. Results: The response of ESR signals of samples prepared with different methods to radiation dose was significantly different. Conclusion: The selection of sample preparation method is very important for dose reconstruction by tooth enamel ESR dosimetry, especially in the low dose range. (authors)

Global metabolite analysis of yeast: evaluation of sample preparation methods

DEFF Research Database (Denmark)

Villas-Bôas, Silas Granato; Højer-Pedersen, Jesper; Åkesson, Mats Fredrik

2005-01-01

Sample preparation is considered one of the limiting steps in microbial metabolome analysis. Eukaryotes and prokaryotes behave very differently during the several steps of classical sample preparation methods for analysis of metabolites. Even within the eukaryote kingdom there is a vast diversity...

Fluidics platform and method for sample preparation and analysis

Science.gov (United States)

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.

Sampling device for withdrawing a representative sample from single and multi-phase flows

Science.gov (United States)

Apley, Walter J.; Cliff, William C.; Creer, James M.

1984-01-01

A fluid stream sampling device has been developed for the purpose of obtaining a representative sample from a single or multi-phase fluid flow. This objective is carried out by means of a probe which may be inserted into the fluid stream. Individual samples are withdrawn from the fluid flow by sampling ports with particular spacings, and the sampling parts are coupled to various analytical systems for characterization of the physical, thermal, and chemical properties of the fluid flow as a whole and also individually.

Combining Electrochemical Sensors with Miniaturized Sample Preparation for Rapid Detection in Clinical Samples

Science.gov (United States)

Bunyakul, Natinan; Baeumner, Antje J.

2015-01-01

Clinical analyses benefit world-wide from rapid and reliable diagnostics tests. New tests are sought with greatest demand not only for new analytes, but also to reduce costs, complexity and lengthy analysis times of current techniques. Among the myriad of possibilities available today to develop new test systems, amperometric biosensors are prominent players—best represented by the ubiquitous amperometric-based glucose sensors. Electrochemical approaches in general require little and often enough only simple hardware components, are rugged and yet provide low limits of detection. They thus offer many of the desirable attributes for point-of-care/point-of-need tests. This review focuses on investigating the important integration of sample preparation with (primarily electrochemical) biosensors. Sample clean up requirements, miniaturized sample preparation strategies, and their potential integration with sensors will be discussed, focusing on clinical sample analyses. PMID:25558994

Test plan for K Basin Sludge Canister and Floor Sampling Device

International Nuclear Information System (INIS)

Meling, T.A.

1995-01-01

This document provides the test plan and procedure forms for conducting the functional and operational acceptance testing of the K Basin Sludge Canister and Floor Sampling Device(s). These samplers samples sludge off the floor of the 100K Basins and out of 100K fuel storage canisters

Sample preparation techniques in trace element analysis by X-ray emission spectroscopy

International Nuclear Information System (INIS)

Valkovic, V.

1983-11-01

The report, written under a research contract with the IAEA, contains a detailed presentation of the most difficult problem encountered in the trace element analysis by methods of the X-ray emission spectroscopy, namely the sample preparation techniques. The following items are covered. Sampling - with specific consideration of aerosols, water, soil, biological materials, petroleum and its products, storage of samples and their handling. Pretreatment of samples - preconcentration, ashing, solvent extraction, ion exchange and electrodeposition. Sample preparations for PIXE - analysis - backings, target uniformity and homogeneity, effects of irradiation, internal standards and specific examples of preparation (aqueous, biological, blood serum and solid samples). Sample preparations for radioactive sources or tube excitation - with specific examples (water, liquid and solid samples, soil, geological, plants and tissue samples). Finally, the problem of standards and reference materials, as well as that of interlaboratory comparisons, is discussed

Quantitating morphological changes in biological samples during scanning electron microscopy sample preparation with correlative super-resolution microscopy.

Science.gov (United States)

Zhang, Ying; Huang, Tao; Jorgens, Danielle M; Nickerson, Andrew; Lin, Li-Jung; Pelz, Joshua; Gray, Joe W; López, Claudia S; Nan, Xiaolin

2017-01-01

Sample preparation is critical to biological electron microscopy (EM), and there have been continuous efforts on optimizing the procedures to best preserve structures of interest in the sample. However, a quantitative characterization of the morphological changes associated with each step in EM sample preparation is currently lacking. Using correlative EM and superresolution microscopy (SRM), we have examined the effects of different drying methods as well as osmium tetroxide (OsO4) post-fixation on cell morphology during scanning electron microscopy (SEM) sample preparation. Here, SRM images of the sample acquired under hydrated conditions were used as a baseline for evaluating morphological changes as the sample went through SEM sample processing. We found that both chemical drying and critical point drying lead to a mild cellular boundary retraction of ~60 nm. Post-fixation by OsO4 causes at least 40 nm additional boundary retraction. We also found that coating coverslips with adhesion molecules such as fibronectin prior to cell plating helps reduce cell distortion from OsO4 post-fixation. These quantitative measurements offer useful information for identifying causes of cell distortions in SEM sample preparation and improving current procedures.

Sample Preparation for Mass Spectrometry Imaging of Plant Tissues: A Review

Science.gov (United States)

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

Sample Preparation for Mass Spectrometry Imaging of Plant Tissues: A Review.

Science.gov (United States)

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.

15N sample preparation for mass spectroscopy analysis

International Nuclear Information System (INIS)

Trivelin, P.C.O.; Salati, E.; Matsui, E.

1973-01-01

Technics for preparing 15 N samples to be analised is presented. Dumas method and oxidation by sodium hypobromite method are described in order to get the appropriate sample. Method to calculate 15 N ratio from mass spectrometry dates is also discussed [pt

Preparation of archaeological samples for its dating by thermoluminescence

International Nuclear Information System (INIS)

Mejia F, D.

2000-01-01

The present work shows the results of the preparation of archaeological samples for their dating by thermoluminescence (Tl) using the Fine grain technique established by Zimmerman but with the varying of such preparation was realized in normal daylight conditions, only the taking of the Tl readings were realized in dark room and red light. In the chapter 1 basic concepts are described about: matter constitution, radioactivity, units and radiation magnitudes, and thermoluminescence. In the chapter 2 some theoretical aspects on dating are showed. It is described how realizing the samples collection, the fine grain method, the determination of the accumulated dose through the years or paleodoses (P=Q+I) by mean of the increasing to obtain the dose equivalent dose (Q) and the signal regeneration method to obtain the correction factor by supra linearity (1), the determination of the annual dose rate to apply the age equation and the evaluation of the age uncertainty with the error limits. The development of experimental part with samples from the archaeological site named Edzna in Campeche, Mexico is described in the chapter 3. The results are presented in the chapter 4. It was obtained an age for the sample named CH7 it was obtained an age of 389 ± years. In conclusion the preparation of the archaeological samples for their dating by Tl in the conditions before mentioned is reliable, but they must be realized more studies with samples of well known age, preparing them in normal daylight conditions and simultaneously in dark room with red light. In order to observe how respond the minerals present in the sample at different dose rapidity, the same samples must be radiated with radiation sources with different dose rate. (Author)

Development of a magnetic measurement device for thin ribbon samples

International Nuclear Information System (INIS)

Sato, Yuta; Todaka, Takashi; Enokizono, Masato

2008-01-01

This paper presents a magnetic measurement device for thin ribbon samples, which are produced by rapid cooling technique. This device enables us to measure magnetic properties easily by only inserting a ribbon sample into a sample holder. The sample holder was made by bakelite to fix any width sample. A long solenoid coil was used to generate a uniform magnetic field and the sample holder was placed at the mid part of the solenoid. The magnetic field strength was measured using a shunt resistor and the magnetic flux density and magnetization in sample ribbons were evaluated by using search coils. The accuracy of measurement was verified with an amorphous metal ribbon sample. Next, we have measured magnetic properties of some magnetic shape memory alloys, which have different compositions. The measured results are compared and we clarified the effect of Sm contents on the magnetic properties

Sample preparation and EFTEM of Meat Samples for Nanoparticle Analysis in Food

International Nuclear Information System (INIS)

Lari, L; Dudkiewicz, A

2014-01-01

Nanoparticles are used in industry for personal care products and the preparation of food. In the latter application, their functions include the prevention of microbes' growth, increase of the foods nutritional value and sensory quality. EU regulations require a risk assessment of the nanoparticles used in foods and food contact materials before the products can reach the market. However, availability of validated analytical methodologies for detection and characterisation of the nanoparticles in food hampers appropriate risk assessment. As part of a research on the evaluation of the methods for screening and quantification of Ag nanoparticles in meat we have tested a new TEM sample preparation alternative to resin embedding and cryo-sectioning. Energy filtered TEM analysis was applied to evaluate thickness and the uniformity of thin meat layers acquired at increasing input of the sample demonstrating that the protocols used ensured good stability under the electron beam, reliable sample concentration and reproducibility

Sample preparation and EFTEM of Meat Samples for Nanoparticle Analysis in Food

Science.gov (United States)

Lari, L.; Dudkiewicz, A.

2014-06-01

Nanoparticles are used in industry for personal care products and the preparation of food. In the latter application, their functions include the prevention of microbes' growth, increase of the foods nutritional value and sensory quality. EU regulations require a risk assessment of the nanoparticles used in foods and food contact materials before the products can reach the market. However, availability of validated analytical methodologies for detection and characterisation of the nanoparticles in food hampers appropriate risk assessment. As part of a research on the evaluation of the methods for screening and quantification of Ag nanoparticles in meat we have tested a new TEM sample preparation alternative to resin embedding and cryo-sectioning. Energy filtered TEM analysis was applied to evaluate thickness and the uniformity of thin meat layers acquired at increasing input of the sample demonstrating that the protocols used ensured good stability under the electron beam, reliable sample concentration and reproducibility.

Final LDRD report : development of sample preparation methods for ChIPMA-based imaging mass spectrometry of tissue samples.

Energy Technology Data Exchange (ETDEWEB)

Maharrey, Sean P.; Highley, Aaron M.; Behrens, Richard, Jr.; Wiese-Smith, Deneille

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 includes 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.

Sample preparation composite and replicate strategy for assay of solid oral drug products.

Science.gov (United States)

Harrington, Brent; Nickerson, Beverly; Guo, Michele Xuemei; Barber, Marc; Giamalva, David; Lee, Carlos; Scrivens, Garry

2014-12-16

In pharmaceutical analysis, the results of drug product assay testing are used to make decisions regarding the quality, efficacy, and stability of the drug product. In order to make sound risk-based decisions concerning drug product potency, an understanding of the uncertainty of the reportable assay value is required. Utilizing the most restrictive criteria in current regulatory documentation, a maximum variability attributed to method repeatability is defined for a drug product potency assay. A sampling strategy that reduces the repeatability component of the assay variability below this predefined maximum is demonstrated. The sampling strategy consists of determining the number of dosage units (k) to be prepared in a composite sample of which there may be a number of equivalent replicate (r) sample preparations. The variability, as measured by the standard error (SE), of a potency assay consists of several sources such as sample preparation and dosage unit variability. A sampling scheme that increases the number of sample preparations (r) and/or number of dosage units (k) per sample preparation will reduce the assay variability and thus decrease the uncertainty around decisions made concerning the potency of the drug product. A maximum allowable repeatability component of the standard error (SE) for the potency assay is derived using material in current regulatory documents. A table of solutions for the number of dosage units per sample preparation (r) and number of replicate sample preparations (k) is presented for any ratio of sample preparation and dosage unit variability.

Study of microtip-based extraction and purification of DNA from human samples for portable devices

Science.gov (United States)

Fotouhi, Gareth

DNA sample preparation is essential for genetic analysis. However, rapid and easy-to-use methods are a major challenge to obtaining genetic information. Furthermore, DNA sample preparation technology must follow the growing need for point-of-care (POC) diagnostics. The current use of centrifuges, large robots, and laboratory-intensive protocols has to be minimized to meet the global challenge of limited access healthcare by bringing the lab to patients through POC devices. To address these challenges, a novel extraction method of genomic DNA from human samples is presented by using heat-cured polyethyleneimine-coated microtips generating a high electric field. The microtip extraction method is based on recent work using an electric field and capillary action integrated into an automated device. The main challenges to the method are: (1) to obtain a stable microtip surface for the controlled capture and release of DNA and (2) to improve the recovery of DNA from samples with a high concentration of inhibitors, such as human samples. The present study addresses these challenges by investigating the heat curing of polyethyleneimine (PEI) coated on the surface of the microtip. Heat-cured PEI-coated microtips are shown to control the capture and release of DNA. Protocols are developed for the extraction and purification of DNA from human samples. Heat-cured PEI-coated microtip methods of DNA sample preparation are used to extract genomic DNA from human samples. It is discovered through experiment that heat curing of a PEI layer on a gold-coated surface below 150°C could inhibit the signal of polymerase chain reaction (PCR). Below 150°C, the PEI layer is not completely cured and dissolved off the gold-coated surface. Dissolved PEI binds with DNA to inhibit PCR. Heat curing of a PEI layer above 150°C on a gold-coated surface prevents inhibition to PCR and gel electrophoresis. In comparison to gold-coated microtips, the 225°C-cured PEI-coated microtips improve the

Microbial profiling of cpn60 universal target sequences in artificial mixtures of vaginal bacteria sampled by nylon swabs or self-sampling devices under different storage conditions.

Science.gov (United States)

Schellenberg, John J; Oh, Angela Yena; Hill, Janet E

2017-05-01

The vaginal microbiome is increasingly characterized by deep sequencing of universal genes. However, there are relatively few studies of how different specimen collection and sample storage and processing influence these molecular profiles. Here, we evaluate molecular microbial community profiles of samples collected using the HerSwab™ self-sampling device, compared to nylon swabs and under different storage conditions. In order to minimize technical variation, mixtures of 11 common vaginal bacteria in simulated vaginal fluid medium were sampled and DNA extracts prepared for massively parallel sequencing of the cpn60 universal target (UT). Three artificial mixtures imitating commonly observed vaginal microbiome profiles were easily distinguished and proportion of sequence reads correlated with the estimated proportion of the organism added to the artificial mixtures. Our results indicate that cpn60 UT amplicon sequencing quantifies the proportional abundance of member organisms in these artificial communities regardless of swab type or storage conditions, although some significant differences were observed between samples that were stored frozen and thawed prior to DNA extraction, compared to extractions from samples stored at room temperature for up to 7days. Our results indicate that an on-the-market device developed for infectious disease diagnostics may be appropriate for vaginal microbiome profiling, an approach that is increasingly facilitated by rapidly dropping deep sequencing costs. Copyright © 2017 Elsevier B.V. All rights reserved.

Sample preparation of energy materials for X-ray nanotomography with micromanipulation.

Science.gov (United States)

Chen-Wiegart, Yu-chen Karen; Camino, Fernando E; Wang, Jun

2014-06-06

X-ray nanotomography presents an unprecedented opportunity to study energy storage/conversion materials at nanometer scales in three dimensions, with both elemental and chemical sensitivity. A critical step in obtaining high-quality X-ray nanotomography data is reliable sample preparation to ensure that the entire sample fits within the field of view of the X-ray microscope. Although focused-ion-beam lift-out has previously been used for large sample (few to tens of microns) preparation, a difficult undercut and lift-out procedure results in a time-consuming sample preparation process. Herein, we propose a much simpler and direct sample preparation method to resolve the issues that block the view of the sample base after milling and during the lift-out process. This method is applied on a solid-oxide fuel cell and a lithium-ion battery electrode, before numerous critical 3D morphological parameters are extracted, which are highly relevant to their electrochemical performance. A broad application of this method for microstructure study with X-ray nanotomography is discussed and presented. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Optimizing Frozen Sample Preparation for Laser Microdissection: Assessment of CryoJane Tape-Transfer System®.

Directory of Open Access Journals (Sweden)

Yelena G Golubeva

Full Text Available Laser microdissection is an invaluable tool in medical research that facilitates collecting specific cell populations for molecular analysis. Diversity of research targets (e.g., cancerous and precancerous lesions in clinical and animal research, cell pellets, rodent embryos, etc. and varied scientific objectives, however, present challenges toward establishing standard laser microdissection protocols. Sample preparation is crucial for quality RNA, DNA and protein retrieval, where it often determines the feasibility of a laser microdissection project. The majority of microdissection studies in clinical and animal model research are conducted on frozen tissues containing native nucleic acids, unmodified by fixation. However, the variable morphological quality of frozen sections from tissues containing fat, collagen or delicate cell structures can limit or prevent successful harvest of the desired cell population via laser dissection. The CryoJane Tape-Transfer System®, a commercial device that improves cryosectioning outcomes on glass slides has been reported superior for slide preparation and isolation of high quality osteocyte RNA (frozen bone during laser dissection. Considering the reported advantages of CryoJane for laser dissection on glass slides, we asked whether the system could also work with the plastic membrane slides used by UV laser based microdissection instruments, as these are better suited for collection of larger target areas. In an attempt to optimize laser microdissection slide preparation for tissues of different RNA stability and cryosectioning difficulty, we evaluated the CryoJane system for use with both glass (laser capture microdissection and membrane (laser cutting microdissection slides. We have established a sample preparation protocol for glass and membrane slides including manual coating of membrane slides with CryoJane solutions, cryosectioning, slide staining and dissection procedure, lysis and RNA extraction

Paper Capillary Enables Effective Sampling for Microfluidic Paper Analytical Devices.

Science.gov (United States)

Shangguan, Jin-Wen; Liu, Yu; Wang, Sha; Hou, Yun-Xuan; Xu, Bi-Yi; Xu, Jing-Juan; Chen, Hong-Yuan

2018-06-06

Paper capillary is introduced to enable effective sampling on microfluidic paper analytical devices. By coupling mac-roscale capillary force of paper capillary and microscale capillary forces of native paper, fluid transport can be flexibly tailored with proper design. Subsequently, a hybrid-fluid-mode paper capillary device was proposed, which enables fast and reliable sampling in an arrayed form, with less surface adsorption and bias for different components. The resulting device thus well supports high throughput, quantitative, and repeatable assays all by hands operation. With all these merits, multiplex analysis of ions, proteins, and microbe have all been realized on this platform, which has paved the way to level-up analysis on μPADs.

Sample preparation optimization in fecal metabolic profiling.

Science.gov (United States)

Deda, Olga; Chatziioannou, Anastasia Chrysovalantou; Fasoula, Stella; Palachanis, Dimitris; Raikos, Νicolaos; Theodoridis, Georgios A; Gika, Helen G

2017-03-15

Metabolomic analysis of feces can provide useful insight on the metabolic status, the health/disease state of the human/animal and the symbiosis with the gut microbiome. As a result, recently there is increased interest on the application of holistic analysis of feces for biomarker discovery. For metabolomics applications, the sample preparation process used prior to the analysis of fecal samples is of high importance, as it greatly affects the obtained metabolic profile, especially since feces, as matrix are diversifying in their physicochemical characteristics and molecular content. However there is still little information in the literature and lack of a universal approach on sample treatment for fecal metabolic profiling. The scope of the present work was to study the conditions for sample preparation of rat feces with the ultimate goal of the acquisition of comprehensive metabolic profiles either untargeted by NMR spectroscopy and GC-MS or targeted by HILIC-MS/MS. A fecal sample pooled from male and female Wistar rats was extracted under various conditions by modifying the pH value, the nature of the organic solvent and the sample weight to solvent volume ratio. It was found that the 1/2 (w f /v s ) ratio provided the highest number of metabolites under neutral and basic conditions in both untargeted profiling techniques. Concerning LC-MS profiles, neutral acetonitrile and propanol provided higher signals and wide metabolite coverage, though extraction efficiency is metabolite dependent. Copyright © 2016 Elsevier B.V. All rights reserved.

Comparison of sample preparation procedures on metal(loid) fractionation patterns in lichens.

Science.gov (United States)

Kroukamp, E M; Godeto, T W; Forbes, P B C

2017-08-13

The effects of different sample preparation strategies and storage on metal(loid) fractionation trends in plant material is largely underresearched. In this study, a bulk sample of lichen Parmotrema austrosinense (Zahlbr.) Hale was analysed for its total extractable metal(loid) content by ICP-MS, and was determined to be adequately homogenous (sample were prepared utilising a range of sample preservation techniques and subjected to a modified sequential extraction procedure or to total metal extraction. Both experiments were repeated after 1-month storage at 4 °C. Cryogenic freezing gave the best reproducibility for total extractable elemental concentrations between months, indicating this to be the most suitable method of sample preparation in such studies. The combined extraction efficiencies were >82% for As, Cu, Mn, Pb, Sr and Zn but poor for other elements, where sample preparation strategies 'no sample preparation' and 'dried in a desiccator' had the best extraction recoveries. Cryogenic freezing procedures had a significantly (p sample cleaning and preservation when species fractionation patterns are of interest. This study also shows that the assumption that species stability can be ensured through cryopreservation and freeze drying techniques needs to be revisited.

Field Sample Preparation Method Development for Isotope Ratio Mass Spectrometry

International Nuclear Information System (INIS)

Leibman, C.; Weisbrod, K.; Yoshida, T.

2015-01-01

Non-proliferation and International Security (NA-241) established a working group of researchers from Los Alamos National Laboratory (LANL), Pacific Northwest National Laboratory (PNNL) and Savannah River National Laboratory (SRNL) to evaluate the utilization of in-field mass spectrometry for safeguards applications. The survey of commercial off-the-shelf (COTS) mass spectrometers (MS) revealed no instrumentation existed capable of meeting all the potential safeguards requirements for performance, portability, and ease of use. Additionally, fieldable instruments are unlikely to meet the International Target Values (ITVs) for accuracy and precision for isotope ratio measurements achieved with laboratory methods. The major gaps identified for in-field actinide isotope ratio analysis were in the areas of: 1. sample preparation and/or sample introduction, 2. size reduction of mass analyzers and ionization sources, 3. system automation, and 4. decreased system cost. Development work in 2 through 4, numerated above continues, in the private and public sector. LANL is focusing on developing sample preparation/sample introduction methods for use with the different sample types anticipated for safeguard applications. Addressing sample handling and sample preparation methods for MS analysis will enable use of new MS instrumentation as it becomes commercially available. As one example, we have developed a rapid, sample preparation method for dissolution of uranium and plutonium oxides using ammonium bifluoride (ABF). ABF is a significantly safer and faster alternative to digestion with boiling combinations of highly concentrated mineral acids. Actinides digested with ABF yield fluorides, which can then be analyzed directly or chemically converted and separated using established column chromatography techniques as needed prior to isotope analysis. The reagent volumes and the sample processing steps associated with ABF sample digestion lend themselves to automation and field

Reproducible preparation of nanospray tips for capillary electrophoresis coupled to mass spectrometry using 3D printed grinding device.

Science.gov (United States)

Tycova, Anna; Prikryl, Jan; Foret, Frantisek

2016-04-01

The use of high quality fused silica capillary nanospray tips is critical for obtaining reliable and reproducible electrospray/MS data; however, reproducible laboratory preparation of such tips is a challenging task. In this work, we report on the design and construction of low-cost grinding device assembled from 3D printed and commercially easily available components. Detailed description and characterization of the grinding device is complemented by freely accessible files in stl and skp format allowing easy laboratory replication of the device. The process of sharpening is aimed at achieving maximal symmetricity, surface smoothness and repeatability of the conus shape. Moreover, the presented grinding device brings possibility to fabricate the nanospray tips of desired dimensions regardless of the commercial availability. On several samples of biological nature (reserpine, rabbit plasma, and the mixture of three aminoacids), performance of fabricated tips is shown on CE coupled to MS analysis. The special interest is paid to the effect of tip sharpness. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Air-deployable oil spill sampling devices review phase 2 testing. Volume 1

International Nuclear Information System (INIS)

Hawke, L.; Dumouchel, A.; Fingas, M.; Brown, C.E.

2007-01-01

SAIC Canada tested air deployable oil sampling devices for the Emergencies Science and Technology Division of Environment Canada in order to determine the applicability and status of these devices. The 3 devices tested were: Canada's SABER (sampling autonomous buoy for evidence recovery), the United States' POPEIE (probe for oil pollution evidence in the environment); and, Sweden's SAR Floatation 2000. They were tested for buoyancy properties, drift behaviour and sampler sorbent pickup ratios. The SAR and SABER both had lesser draft and greater freeboard, while the POPEIE had much greater draft than freeboard. All 3 devices could be used for oil sample collection in that their drift characteristics would allow for the SABER and SAR devices to be placed upwind of the slick while the POPEIE device could be placed downwind of an oil spill. The sorbent testing revealed that Sefar sorbent and Spectra sorbent used in the 3 devices had negative pickup ratios for diesel but performance improved as oil viscosity increased. Both sorbents are inert and capable of collecting oil in sufficient volumes for consistent fingerprinting analysis. 10 refs., 8 tabs., 8 figs

Choice and preparation of standard samples for X-ray spectral microanalysis

International Nuclear Information System (INIS)

Gavrilenko, I.S.; Surzhko, V.F.

1989-01-01

Choice, preparation and certification of standard samples for X-ray spectral microanalysis are considered. Requirements for standard samples in terms of concentration and volume, porosity, corrosion, conductivity distribution are formulated. Stages of sample preparation process, including composition choice, heat treatment, section production, certification, are considered in detail. The choice of composition is based on studying phase equilibrium diagrams, subdivided into 6 types

Novel strategies for sample preparation in forensic toxicology.

Science.gov (United States)

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.

TEM sample preparation by FIB for carbon nanotube interconnects

International Nuclear Information System (INIS)

Ke, Xiaoxing; Bals, Sara; Romo Negreira, Ainhoa; Hantschel, Thomas; Bender, Hugo; Van Tendeloo, Gustaaf

2009-01-01

A powerful method to study carbon nanotubes (CNTs) grown in patterned substrates for potential interconnects applications is transmission electron microscopy (TEM). However, high-quality TEM samples are necessary for such a study. Here, TEM specimen preparation by focused ion beam (FIB) has been used to obtain lamellae of patterned samples containing CNTs grown inside contact holes. A dual-cap Pt protection layer and an extensive 5 kV cleaning procedure are applied in order to preserve the CNTs and avoid deterioration during milling. TEM results show that the inner shell structure of the carbon nanotubes has been preserved, which proves that focused ion beam is a useful technique to prepare TEM samples of CNT interconnects.

TEM sample preparation by FIB for carbon nanotube interconnects

Energy Technology Data Exchange (ETDEWEB)

Ke, Xiaoxing, E-mail: xiaoxing.ke@ua.ac.be [EMAT, University of Antwerp, Groenenborgerlaan 171, B-2020 Antwerp (Belgium); Bals, Sara [EMAT, University of Antwerp, Groenenborgerlaan 171, B-2020 Antwerp (Belgium); Romo Negreira, Ainhoa [IMEC, Kapeldreef 75, B-3001 Leuven (Belgium); Metallurgy and Materials Engineering Department, KU Leuven, Kasteelpark Arenberg 44, Leuven B-3001 (Belgium); Hantschel, Thomas; Bender, Hugo [IMEC, Kapeldreef 75, B-3001 Leuven (Belgium); Van Tendeloo, Gustaaf [EMAT, University of Antwerp, Groenenborgerlaan 171, B-2020 Antwerp (Belgium)

2009-10-15

A powerful method to study carbon nanotubes (CNTs) grown in patterned substrates for potential interconnects applications is transmission electron microscopy (TEM). However, high-quality TEM samples are necessary for such a study. Here, TEM specimen preparation by focused ion beam (FIB) has been used to obtain lamellae of patterned samples containing CNTs grown inside contact holes. A dual-cap Pt protection layer and an extensive 5 kV cleaning procedure are applied in order to preserve the CNTs and avoid deterioration during milling. TEM results show that the inner shell structure of the carbon nanotubes has been preserved, which proves that focused ion beam is a useful technique to prepare TEM samples of CNT interconnects.

78 FR 25308 - Proposed Collection; Comment Request; Coal Mine Dust Sampling Devices

Science.gov (United States)

2013-04-30

...; Coal Mine Dust Sampling Devices AGENCY: Mine Safety and Health Administration, Labor. ACTION: 60-Day... mines. CPDMs must be designed and constructed for coal miners to wear and operate without impeding their... related to Coal Mine Dust Sampling Devices. MSHA is particularly interested in comments that: Evaluate...

Supporting Sampling and Sample Preparation Tools for Isotope and Nuclear Analysis

International Nuclear Information System (INIS)

2016-03-01

Nuclear and related techniques can help develop climate-smart agricultural practices by optimizing water and nutrient use efficiency, assessing organic carbon sequestration in soil, and assisting in the evaluation of soil erosion control measures. Knowledge on the behaviour of radioactive materials in soil, water and foodstuffs is also essential in enhancing nuclear emergency preparedness and response. Appropriate sampling and sample preparation are the first steps to ensure the quality and effective use of the measurements and this publication provides comprehensive detail on the necessary steps

Preparation of irritant polymer samples for an in vitro round robin study.

NARCIS (Netherlands)

Coleman, Kelly P; Grailer, Thomas P; McNamara, Lori R; Rollins, Beau L; Christiano, Nicholas J; Kandárová, Helena; De Jong, Wim H

2018-01-01

A round robin study using reconstructed human epidermis (RhE) tissues was conducted to test medical device polymer extracts for skin irritation potential. Test samples were four irritant and three non-irritant medical device polymers. Five of these polymer samples were developed and two were

Selecting Sample Preparation Workflows for Mass Spectrometry-Based Proteomic and Phosphoproteomic Analysis of Patient Samples with Acute Myeloid Leukemia.

Science.gov (United States)

Hernandez-Valladares, Maria; Aasebø, Elise; Selheim, Frode; Berven, Frode S; Bruserud, Øystein

2016-08-22

Global mass spectrometry (MS)-based proteomic and phosphoproteomic studies of acute myeloid leukemia (AML) biomarkers represent a powerful strategy to identify and confirm proteins and their phosphorylated modifications that could be applied in diagnosis and prognosis, as a support for individual treatment regimens and selection of patients for bone marrow transplant. MS-based studies require optimal and reproducible workflows that allow a satisfactory coverage of the proteome and its modifications. Preparation of samples for global MS analysis is a crucial step and it usually requires method testing, tuning and optimization. Different proteomic workflows that have been used to prepare AML patient samples for global MS analysis usually include a standard protein in-solution digestion procedure with a urea-based lysis buffer. The enrichment of phosphopeptides from AML patient samples has previously been carried out either with immobilized metal affinity chromatography (IMAC) or metal oxide affinity chromatography (MOAC). We have recently tested several methods of sample preparation for MS analysis of the AML proteome and phosphoproteome and introduced filter-aided sample preparation (FASP) as a superior methodology for the sensitive and reproducible generation of peptides from patient samples. FASP-prepared peptides can be further fractionated or IMAC-enriched for proteome or phosphoproteome analyses. Herein, we will review both in-solution and FASP-based sample preparation workflows and encourage the use of the latter for the highest protein and phosphorylation coverage and reproducibility.

Device for sampling radioactive and aggressive liquid and vaporous media

International Nuclear Information System (INIS)

Przibram, E.; Halm, G.

1974-01-01

The equipment enables the taking of samples even of radioactive media from a main pipeline in the through-flow in a closed system. A tap device is attached to the main pipeline which branches into two parts. The one branch contains the actual tap which is closed to both sides with snap closure coupling. It is only used for taking samples. The other branch bridges the tap position as a bypass so that a representative sample is always available. Both branches join up again and lead back to the main pipeline. The sampling can be used in a nuclear power plant for the determination of O 2 , CI, SiO 2 , and Cu. A millilitre collecting cylinder and a millipore filtration device can be connected to the tap for liquid sampling and solid analysis, respectively. The system can be extended to several tap positions. Permanent measuring equipment is attached to the bypass pipe to control the sample liquid. (DG) [de

Development of sample preparation method for honey analysis using PIXE

International Nuclear Information System (INIS)

Saitoh, Katsumi; Chiba, Keiko; Sera, Koichiro

2008-01-01

We developed an original preparation method for honey samples (samples in paste-like state) specifically designed for PIXE analysis. The results of PIXE analysis of thin targets prepared by adding a standard containing nine elements to honey samples demonstrated that the preparation method bestowed sufficient accuracy on quantitative values. PIXE analysis of 13 kinds of honey was performed, and eight mineral components (Si, P, S, K, Ca, Mn, Cu and Zn) were detected in all honey samples. The principal mineral components were K and Ca, and the quantitative value for K accounted for the majority of the total value for mineral components. K content in honey varies greatly depending on the plant source. Chestnuts had the highest K content. In fact, it was 2-3 times that of Manuka, which is known as a high quality honey. K content of false-acacia, which is produced in the greatest abundance, was 1/20 that of chestnuts. (author)

Witness sample preparation for measuring antireflection coatings.

Science.gov (United States)

Willey, Ronald R

2014-02-01

Measurement of antireflection coating of witness samples from across the worldwide industry has been shown to have excess variability from a sampling taken for the OSA Topical Meeting on Optical Interference Coatings: Measurement Problem. Various sample preparation techniques have been discussed with their limitations, and a preferred technique is recommended with its justification, calibration procedures, and limitations. The common practice of grinding the second side to reduce its reflection is less than satisfactory. One recommended practice is to paint the polished second side, which reduces its reflection to almost zero. A method to evaluate the suitability of given paints is also described.

Sample preparation method for scanning force microscopy

CERN Document Server

Jankov, I R; Szente, R N; Carreno, M N P; Swart, J W; Landers, R

2001-01-01

We present a method of sample preparation for studies of ion implantation on metal surfaces. The method, employing a mechanical mask, is specially adapted for samples analysed by Scanning Force Microscopy. It was successfully tested on polycrystalline copper substrates implanted with phosphorus ions at an acceleration voltage of 39 keV. The changes of the electrical properties of the surface were measured by Kelvin Probe Force Microscopy and the surface composition was analysed by Auger Electron Spectroscopy.

Status report of AMS sample preparation laboratory at GADAM Centre, Gliwice, Poland

Energy Technology Data Exchange (ETDEWEB)

Piotrowska, N., E-mail: natalia.piotrowska@polsl.pl [GADAM Centre of Excellence, Department of Radioisotopes, Institute of Physics, Silesian University of Technology, Gliwice (Poland)

2013-01-15

The laboratory for {sup 14}C AMS sample preparation in the Gliwice Radiocarbon Laboratory has gradually evolved since its start in 1999 to cater for an increase in volume and variety of radiocarbon dating samples. To date, nearly 2000 graphite targets have been produced from materials such as plant macrofossils, charcoal, peat, bones, shells and wood. The equipment comprises a station for chemical preparation and high vacuum lines for production, purification and graphitization of sample carbon dioxide. The present capacity allows preparation of up to 400 targets annually for the needs of scientific projects and external orders for radiocarbon dating continuously received by the GADAM Centre of Excellence. The laboratory's sample preparation protocols and recent improvements are described and its performance during the 10 years of activity is discussed in terms of parameters obtained from reference materials prepared in this laboratory and demonstrated with a few science applications.

Sample preparation techniques of biological material for isotope analysis

International Nuclear Information System (INIS)

Axmann, H.; Sebastianelli, A.; Arrillaga, J.L.

1990-01-01

Sample preparation is an essential step in all isotope-aided experiments but often it is not given enough attention. The methods of sample preparation are very important to obtain reliable and precise analytical data and for further interpretation of results. The size of a sample required for chemical analysis is usually very small (10mg-1500mg). On the other hand the amount of harvested plant material from plots in a field experiment is often bulky (several kilograms) and the entire sample is too large for processing. In addition, while approaching maturity many crops show not only differences in physical consistency but also a non-uniformity in 15 N content among plant parts, requiring a plant fractionation or separation into parts (vegetative and reproductive) e.g. shoots and spikes, in case of small grain cereals, shoots and pods in case of grain legumes and tops and roots or beets (including crown) in case of sugar beet, etc. In any case the ultimate goal of these procedures is to obtain representative subsample harvested from greenhouse or field experiments for chemical analysis. Before harvesting an isotopic-aided experiment the method of sampling has to be selected. It should be based on the type of information required in relation to the objectives of the research and the availability of resources (staff, sample preparation equipment, analytical facilities, chemicals and supplies, etc.). 10 refs, 3 figs, 3 tabs

[Progress in sample preparation and analytical methods for trace polar small molecules in complex samples].

Science.gov (United States)

Zhang, Qianchun; Luo, Xialin; Li, Gongke; Xiao, Xiaohua

2015-09-01

Small polar molecules such as nucleosides, amines, amino acids are important analytes in biological, food, environmental, and other fields. It is necessary to develop efficient sample preparation and sensitive analytical methods for rapid analysis of these polar small molecules in complex matrices. Some typical materials in sample preparation, including silica, polymer, carbon, boric acid and so on, are introduced in this paper. Meanwhile, the applications and developments of analytical methods of polar small molecules, such as reversed-phase liquid chromatography, hydrophilic interaction chromatography, etc., are also reviewed.

Considerations for Sample Preparation Using Size-Exclusion Chromatography for Home and Synchrotron Sources.

Science.gov (United States)

Rambo, Robert P

2017-01-01

The success of a SAXS experiment for structural investigations depends on two precise measurements, the sample and the buffer background. Buffer matching between the sample and background can be achieved using dialysis methods but in biological SAXS of monodisperse systems, sample preparation is routinely being performed with size exclusion chromatography (SEC). SEC is the most reliable method for SAXS sample preparation as the method not only purifies the sample for SAXS but also almost guarantees ideal buffer matching. Here, I will highlight the use of SEC for SAXS sample preparation and demonstrate using example proteins that SEC purification does not always provide for ideal samples. Scrutiny of the SEC elution peak using quasi-elastic and multi-angle light scattering techniques can reveal hidden features (heterogeneity) of the sample that should be considered during SAXS data analysis. In some cases, sample heterogeneity can be controlled using a small molecule additive and I outline a simple additive screening method for sample preparation.

A Method for Microalgae Proteomics Analysis Based on Modified Filter-Aided Sample Preparation.

Science.gov (United States)

Li, Song; Cao, Xupeng; Wang, Yan; Zhu, Zhen; Zhang, Haowei; Xue, Song; Tian, Jing

2017-11-01

With the fast development of microalgal biofuel researches, the proteomics studies of microalgae increased quickly. A filter-aided sample preparation (FASP) method is widely used proteomics sample preparation method since 2009. Here, a method of microalgae proteomics analysis based on modified filter-aided sample preparation (mFASP) was described to meet the characteristics of microalgae cells and eliminate the error caused by over-alkylation. Using Chlamydomonas reinhardtii as the model, the prepared sample was tested by standard LC-MS/MS and compared with the previous reports. The results showed mFASP is suitable for most of occasions of microalgae proteomics studies.

Selecting Sample Preparation Workflows for Mass Spectrometry-Based Proteomic and Phosphoproteomic Analysis of Patient Samples with Acute Myeloid Leukemia

Directory of Open Access Journals (Sweden)

Maria Hernandez-Valladares

2016-08-01

Full Text Available Global mass spectrometry (MS-based proteomic and phosphoproteomic studies of acute myeloid leukemia (AML biomarkers represent a powerful strategy to identify and confirm proteins and their phosphorylated modifications that could be applied in diagnosis and prognosis, as a support for individual treatment regimens and selection of patients for bone marrow transplant. MS-based studies require optimal and reproducible workflows that allow a satisfactory coverage of the proteome and its modifications. Preparation of samples for global MS analysis is a crucial step and it usually requires method testing, tuning and optimization. Different proteomic workflows that have been used to prepare AML patient samples for global MS analysis usually include a standard protein in-solution digestion procedure with a urea-based lysis buffer. The enrichment of phosphopeptides from AML patient samples has previously been carried out either with immobilized metal affinity chromatography (IMAC or metal oxide affinity chromatography (MOAC. We have recently tested several methods of sample preparation for MS analysis of the AML proteome and phosphoproteome and introduced filter-aided sample preparation (FASP as a superior methodology for the sensitive and reproducible generation of peptides from patient samples. FASP-prepared peptides can be further fractionated or IMAC-enriched for proteome or phosphoproteome analyses. Herein, we will review both in-solution and FASP-based sample preparation workflows and encourage the use of the latter for the highest protein and phosphorylation coverage and reproducibility.

Final Report for X-ray Diffraction Sample Preparation Method Development

Energy Technology Data Exchange (ETDEWEB)

Ely, T. M. [Hanford Site (HNF), Richland, WA (United States); Meznarich, H. K. [Hanford Site (HNF), Richland, WA (United States); Valero, T. [Hanford Site (HNF), Richland, WA (United States)

2018-01-30

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.

Sample taking device for toxic and/or radioactive substances

International Nuclear Information System (INIS)

Finsterwalder, L.; Zeh, H.; Schaarschmidt, U.

1979-01-01

An apparatus for taking samples of toxic and/or radioactive liquid substances by introducing such substances into sample vessels includes a holder for holding such a vessel, at least one needle head filling system composed of upwardly pointing hollow needles for introducing a sample of one such substance into such a vessel at a filling position, and inlet and outlet conduits for pneumatically conveying vessels to or from the holder at a transfer position. The holder is composed of a turntable having a sleeve for accommodating such vessel and is mounted to undergo rotary movement to convey a sample vessel held in the sleeve between the filling and transfer positions. The apparatus further includes a stand supporting the filling system below the holder and a lifting device connected for imparting a translational movement to the holder to bring a vessel in the holder to operative association with the filling system. The lifting device is arranged so that the translational movement which it produces is independent of the rotary movement of the turntable

Protocol for Cohesionless Sample Preparation for Physical Experimentation

Science.gov (United States)

2016-05-01

Standard test method for consolidated drained triaxial compression test for soils . In Annual book of ASTM standards. West Conshohocken, PA: ASTM...derived wherein uncertainties and laboratory scatter associated with soil fabric-behavior variance during sample preparation are mitigated. Samples of...wherein comparable analysis between different laboratory tests’ results can be made by ensuring a comparable soil fabric prior to laboratory testing

Sample Preparation (SS): SE51_SS01 [Metabolonote[Archive

Lifescience Database Archive (English)

Full Text Available e Master NEO, BMS, Tokyo, Japan), and the seed powder was extracted with 1 mL of extraction buffer (0.1% HCO...trifugation (4 ℃, 10,000 rpm, 5 min), the sample tubes were subjected to sample preparation (buffer transfer

Recent developments on field gas extraction and sample preparation methods for radiokrypton dating of groundwater

Science.gov (United States)

Yokochi, Reika

2016-09-01

Current and foreseen population growths will lead to an increased demand in freshwater, large quantities of which is stored as groundwater. The ventilation age is crucial to the assessment of groundwater resources, complementing the hydrological model approach based on hydrogeological parameters. Ultra-trace radioactive isotopes of Kr (81 Kr and 85 Kr) possess the ideal physical and chemical properties for groundwater dating. The recent advent of atom trap trace analyses (ATTA) has enabled determination of ultra-trace noble gas radioisotope abundances using 5-10 μ L of pure Kr. Anticipated developments will enable ATTA to analyze radiokrypton isotope abundances at high sample throughput, which necessitates simple and efficient sample preparation techniques that are adaptable to various sample chemistries. Recent developments of field gas extraction devices and simple and rapid Kr separation method at the University of Chicago are presented herein. Two field gas extraction devices optimized for different sampling conditions were recently designed and constructed, aiming at operational simplicity and portability. A newly developed Kr purification system enriches Kr by flowing a sample gas through a moderately cooled (138 K) activated charcoal column, followed by a gentle fractionating desorption. This simple process uses a single adsorbent and separates 99% of the bulk atmospheric gases from Kr without significant loss. The subsequent two stages of gas chromatographic separation and a hot Ti sponge getter further purify the Kr-enriched gas. Abundant CH4 necessitates multiple passages through one of the gas chromatographic separation columns. The presented Kr separation system has a demonstrated capability of extracting Kr with > 90% yield and 99% purity within 75 min from 1.2 to 26.8 L STP of atmospheric air with various concentrations of CH4. The apparatuses have successfully been deployed for sampling in the field and purification of groundwater samples.

Microfluidic devices and methods for integrated flow cytometry

Science.gov (United States)

Srivastava, Nimisha [Goleta, CA; Singh, Anup K [Danville, CA

2011-08-16

Microfluidic devices and methods for flow cytometry are described. In described examples, various sample handling and preparation steps may be carried out within a same microfluidic device as flow cytometry steps. A combination of imaging and flow cytometry is described. In some examples, spiral microchannels serve as incubation chambers. Examples of automated sample handling and flow cytometry are described.

Challenges in TEM sample preparation of solvothermally grown CuInS2 films.

Science.gov (United States)

Frank, Anna; Changizi, Rasa; Scheu, Christina

2018-06-01

Transmission electron microscopy (TEM) is a widely used tool to characterize materials. The required samples need to be electron transparent which should be achieved without changing the microstructure. This work describes different TEM sample preparation techniques of nanostructured CuInS 2 thin films on fluorine-doped tin oxide substrates, synthesized solvothermally using l-cysteine as sulfur source. Focused ion beam lamellae, conventional cross section samples and scratch samples have been prepared and investigated. It was possible to prepare appropriate samples with each technique, however, each technique brings with it certain advantages and disadvantages. FIB preparation of solvothermally synthesized CuInS 2 suffers from two main drawbacks. First, the whole CuInS 2 layer displays a strongly increased Cu content caused by Cu migration and preferential removal of In. Further, electron diffraction shows the formation of an additional CuS phase after Ga + bombardment. Second, diffraction analysis is complicated by a strong contribution of crystalline Pt introduced during the FIB preparation and penetrating into the porous film surface. The conventional cross sectional CuInS 2 sample also shows a Cu signal enhancement which is caused by contribution of the brass tube material used for embedding. Additionally, Cu particles have been observed inside the CuInS 2 which have been sputtered on the film during preparation. Only the scratch samples allow an almost artefact-free and reliable elemental quantification using energy-dispersive X-ray spectroscopy. However, scratch samples suffer from the drawback that it is not possible to determine the layer thickness, which is possible for both cross sectional preparation techniques. Consequently, it is concluded that the type of sample preparation should be chosen dependent on the required information. A full characterization can only be achieved when the different techniques are combined. Copyright © 2018 Elsevier Ltd. All

Automated SEM and TEM sample preparation applied to copper/low k materials

Science.gov (United States)

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.

Device for the analysis of fine dusts

International Nuclear Information System (INIS)

Riemer, F.; Tausch, W.; Torge, R.

1978-01-01

The invention deals with a device that brings graphite bulbs containing samples of fine dusts automatically to the spectrometer for analysis and transports them away afterwards, a great number of individual measurements thus being quickly performed. The device consists of magazines, means of transport for them etc., and, if necessary, also a furnace for thermal preparation of the samples. (RW) 891 RW/RW 892 MKO [de

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

Science.gov (United States)

Chikhani, Madelen; Wuhrer, Richard; Green, Hayley

2018-03-30

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

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

Science.gov (United States)

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

2014-12-01

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

Accumulation of brevetoxins by passive sampling devices | Shea ...

African Journals Online (AJOL)

We report on initial investigations into the use of polymer-based passive sampling devices for the chronic time-integrated measure of brevetoxins in natural waters. Polyethylene membranes readily accumulated brevetoxins, but reached steady state within a few days, likely owing to surface saturation on the polyethylene ...

State of the art in sample preparation for trace element analysis (M1)

International Nuclear Information System (INIS)

Barnes, R.M.

2002-01-01

Full text: The accelerated capabilities of modern trace element analysis techniques, especially inductively coupled plasma mass spectrometry (ICP-MS), have challenged the sample preparation competence of most laboratories. Exceptional analytical sensitivity, remarkable analysis speed, automated sample presentation, and intelligent sample sequencing of modern spectroscopic instrumentation have lead to demanding requirements for appropriate sample preparation steps needed for ultra trace concentration and speciation measurements. Contamination control, reliable digestion and extraction techniques, presentation of chemical forms, sample matrix management, and intelligent sample processing available today are often inadequate for the most demanding measurements. Some commercial instrumentation provides convenient implementation of well-established contamination control measures, and reagent and container purity are steadily being improved. Direct sample introduction approaches offer alternatives to conventional solution samples, but achieving calibration reliability is difficult. Developing new sample preparation chemistry is especially arduous and rare, yet progress exists in characterizing microwave-assisted reactions. This presentation will describe contemporary targets for modern sample preparation approaches for ultra trace elemental analysis and the likelihood that they can be reasonably achieved. (author)

Latex Rubber Gloves as a Sampling Dosimeter Using a Novel Surrogate Sampling Device.

Science.gov (United States)

Sankaran, Gayatri; Lopez, Terry; Ries, Steve; Ross, John; Vega, Helen; Eastmond, David A; Krieger, Robert I

2015-01-01

Pesticide exposure during harvesting of crops occurs primarily to the workers' hands. When harvesters wear latex rubber gloves for personal safety and hygiene harvesting reasons, gloves accumulate pesticide residues. Hence, characterization of the gloves' properties may be useful for pesticide exposure assessments. Controlled field studies were conducted using latex rubber gloves to define the factors that influence the transfer of pesticides to the glove and that would affect their use as a residue monitoring device. A novel sampling device called the Brinkman Contact Transfer Unit (BCTU) was constructed to study the glove characteristics and residue transfer and accumulation under controlled conditions on turf. The effectiveness of latex rubber gloves as sampling dosimeters was evaluated by measuring the transferable pesticide residues as a function of time. The validation of latex rubber gloves as a residue sampling dosimeter was performed by comparing pesticide transfer and dissipation from the gloves, with the turf transferable residues sampled using the validated California (CA) Roller, a standard measure of residue transfer. The observed correlation (Pearson's correlation coefficient R(2)) between the two methods was .84 for malathion and .96 for fenpropathrin, indicating that the BCTU is a useful, reliable surrogate tool for studying available residue transfer to latex rubber gloves under experimental conditions. Perhaps more importantly, these data demonstrate that latex gloves worn by workers may be useful quantifiable matrices for measuring pesticide exposure.

Sequencing of real-world samples using a microfabricated hybrid device having unconstrained straight separation channels.

Science.gov (United States)

Liu, Shaorong; Elkin, Christopher; Kapur, Hitesh

2003-11-01

We describe a microfabricated hybrid device that consists of a microfabricated chip containing multiple twin-T injectors attached to an array of capillaries that serve as the separation channels. A new fabrication process was employed to create two differently sized round channels in a chip. Twin-T injectors were formed by the smaller round channels that match the bore of the separation capillaries and separation capillaries were incorporated to the injectors through the larger round channels that match the outer diameter of the capillaries. This allows for a minimum dead volume and provides a robust chip/capillary interface. This hybrid design takes full advantage, such as sample stacking and purification and uniform signal intensity profile, of the unique chip injection scheme for DNA sequencing while employing long straight capillaries for the separations. In essence, the separation channel length is optimized for both speed and resolution since it is unconstrained by chip size. To demonstrate the reliability and practicality of this hybrid device, we sequenced over 1000 real-world samples from Human Chromosome 5 and Ciona intestinalis, prepared at Joint Genome Institute. We achieved average Phred20 read of 675 bases in about 70 min with a success rate of 91%. For the similar type of samples on MegaBACE 1000, the average Phred20 read is about 550-600 bases in 120 min separation time with a success rate of about 80-90%.

Carbon nanotubes for gas detection: materials preparation and device assembly

International Nuclear Information System (INIS)

Terranova, M L; Lucci, M; Orlanducci, S; Tamburri, E; Sessa, V; Reale, A; Carlo, A Di

2007-01-01

An efficient sensing device for NH 3 and NO x detection has been realized using ordered arrays of single-walled C nanotubes deposited onto an interdigitated electrode platform operating at room temperature. The sensing material has been prepared using several chemical-physical techniques for purification and positioning of the nanotubes inside the electrode gaps. In particular, both DC and AC fields have been applied in order to move and to align the nanostructures by electrophoresis and dielectrophoresis processes. We investigated the effects of different voltages applied to a gate contact on the back side of the substrate on the performances of the device and found that for different gas species (NH 3 , NO x ) a constant gate bias increases the sensitivity for gas detection. Moreover, in this paper we demonstrate that a pulsed bias applied to the gate contact facilitates the gas interaction with the nanotubes, either reducing the absorption times or accelerating the desorption times, thus providing a fast acceleration and a dramatic improvement of the time dependent behaviour of the device

The effect of sample preparation methods on glass performance

International Nuclear Information System (INIS)

Oh, M.S.; Oversby, V.M.

1990-01-01

A series of experiments was conducted using SRL 165 synthetic waste glass to investigate the effects of surface preparation and leaching solution composition on the alteration of the glass. Samples of glass with as-cast surfaces produced smooth reaction layers and some evidence for precipitation of secondary phases from solution. Secondary phases were more abundant in samples reacted in deionized water than for those reacted in a silicate solution. Samples with saw-cut surfaces showed a large reduction in surface roughness after 7 days of reaction in either solution. Reaction in silicate solution for up to 91 days produced no further change in surface morphology, while reaction in DIW produced a spongy surface that formed the substrate for further surface layer development. The differences in the surface morphology of the samples may create microclimates that control the details of development of alteration layers on the glass; however, the concentrations of elements in leaching solutions show differences of 50% or less between samples prepared with different surface conditions for tests of a few months duration. 6 refs., 7 figs., 1 tab

Preparation of Cytology Samples: Tricks of the Trade.

Science.gov (United States)

Moore, A Russell

2017-01-01

General principles and techniques for collection, preparation, and staining of cytologic samples in the general practice setting are reviewed. Tips for collection of digital images are also discussed. Copyright © 2016 Elsevier Inc. All rights reserved.

Sample preparation procedures utilized in microbial metabolomics: An overview.

Science.gov (United States)

Patejko, Małgorzata; Jacyna, Julia; Markuszewski, Michał J

2017-02-01

Bacteria are remarkably diverse in terms of their size, structure and biochemical properties. Due to this fact, it is hard to develop a universal method for handling bacteria cultures during metabolomic analysis. The choice of suitable processing methods constitutes a key element in any analysis, because only appropriate selection of procedures may provide accurate results, leading to reliable conclusions. Because of that, every analytical experiment concerning bacteria requires individually and very carefully planned research methodology. Although every study varies in terms of sample preparation, there are few general steps to follow while planning experiment, like sampling, separation of cells from growth medium, stopping their metabolism and extraction. As a result of extraction, all intracellular metabolites should be washed out from cell environment. What is more, extraction method utilized cannot cause any chemical decomposition or degradation of the metabolome. Furthermore, chosen extraction method should correlate with analytical technique, so it will not disturb or prolong following sample preparation steps. For those reasons, we observe a need to summarize sample preparation procedures currently utilized in microbial metabolomic studies. In the presented overview, papers concerning analysis of extra- and intracellular metabolites, published over the last decade, have been discussed. Presented work gives some basic guidelines that might be useful while planning experiments in microbial metabolomics. Copyright © 2016 Elsevier B.V. All rights reserved.

Sample preparation techniques for (p, X) spectrometry

International Nuclear Information System (INIS)

Whitehead, N.E.

1985-01-01

Samples are ashed at low temperature, using oxygen plasma; a rotary evaporator, and freeze drying speeded up the ashing. The new design of apparatus manufactured was only 10 watt but was as efficient as a 200 watt commercial machine; a circuit diagram is included. Samples of hair and biopsy samples of skin were analysed by the technique. A wool standard was prepared for interlaboratory comparison exercises. It was based on New Zealand merino sheep wool and was 2.9 kg in weight. A washing protocol was developed, which preserves most of the trace element content. The wool was ground in liquid nitrogen using a plastic pestle and beaker, driven by a rotary drill press. (author)

Comparative study of the characteristics of some suction devices for gas sampling applications

International Nuclear Information System (INIS)

Donguy, R.; Drouet, J.

1959-06-01

Gas sampling (used to determine the characteristics of dusts or aerosols contained in a gas) needs a suction device. In order to select the right device and the right conditions of use, the characteristics and performances of various suction devices (helicoidal and centrifugal aspirators, air pumps, volumetric pumps) have been experimentally measured: flow rate, head loss, sampling volume and duration, aerosol and dust concentration, gas density, nature of the gas, suction circuit configuration, etc

Evaluation of a new simple collection device for sampling of microparticles in exhaled breath.

Science.gov (United States)

Seferaj, Sabina; Ullah, Shahid; Tinglev, Åsa; Carlsson, Sten; Winberg, Jesper; Stambeck, Peter; Beck, Olof

2018-03-12

The microparticle fraction of exhaled breath is of interest for developing clinical biomarkers. Exhaled particles may contain non-volatile components from all parts of the airway system, formed during normal breathing. This study aimed to evaluate a new, simple sampling device, based on impaction, for collecting microparticles from exhaled breath. Performance of the new device was compared with that of the existing SensAbues membrane filter device. The analytical work used liquid chromatography-tandem mass spectrometry methods. The new device collected three subsamples and these were separately analysed from eight individuals. No difference was observed between the centre position (0.91 ng/sample) and the side positions (1.01 ng/sample) using major phosphatidylcholine (PC) 16:0/16:0 as the analyte. Exhaled breath was collected from eight patients on methadone maintenance treatment. The intra-individual variability in measured methadone concentration between the three collectors was 8.7%. In another experiment using patients on methadone maintenance treatment, the sampling efficiency was compared with an established filter device. Compared to the existing device, the efficiency of the new device was 121% greater for methadone and 1450% greater for DPPC. The data from lipid analysis also indicated that a larger fraction of the collected material was from the distal parts. Finally, a study using an optical particle counter indicated that the device preferentially collects the larger particle fraction. In conclusion, this study demonstrates the usefulness of the new device for collecting non-volatile components from exhaled breath. The performance of the device was superior to the filter device in several aspects.

Traceability and measurement uncertainty in sample preparation (W5)

International Nuclear Information System (INIS)

Wegscheider, W.; Walner, U.; Moser, J.

2002-01-01

Full text: Very few chemical measurements are being made directly on the object of interest and sample preparation is thus the rule rather than the exception in daily practice. Unfortunately the operations undertaken in the course of sample preparation are prone to rendering a sample useless for the purpose of interpreting a measurement performed on it, as it might not represent the original and relevant status any longer. Sample preparation along with sampling itself constitutes therefore a procedure that leads to a loss of representation of the original specimen or population. On the other hand it is also not sufficient to confine aspects of traceability and measurement uncertainty to the ultimate measurement, as the key purpose of measuring is to supply adequate data for some kind of decision, be it in production, in health, in the environment, or indeed in any other circumstance. These considerations have led to severe confusion in the community as to what traceability really means in chemistry. CITAC and EURACHEM have only recently issued a preliminary document that clarifies these issues and gives a firm handle on the future development of quality assurance in analytical chemistry. In this talk it will be attempted to outline the general ideas and procedures that lead to traceability of analytical chemical results accompanied by valid statements of their uncertainty. It will be argued that the central element in achieving these goals is a well-designed validation study that frequently goes beyond those requirements currently laid out in official documents. (author)

Development and application of a micro-digestion device for biological samples

International Nuclear Information System (INIS)

Bohlen, A. von; Klockenkaemper, R.; Messerschmidt, J.; Alt, F.

2000-01-01

The analytical characterization of small amounts of a sample is of increasing importance for various research projects in biology, biochemistry and medicine. Reliable determinations of minor and trace elements in microsamples can be performed by total reflection x-ray fluorescence analysis (TXRF). This microanalytical method is suitable for direct multielement analyses of a tiny amount of a liquid or solid sample. Instead of a direct analysis, however, a complete digestion or mineralisation of the sample material prior to analysis can be recommendable. It can be advantageous for a favorable presentation, for a preconcentration and/or homogenization of the material and particularly for an accurate quantification. Unfortunately, commercially available digestion devices are optimized for amounts of 50 to 400 mg of a sample. For smaller amounts, a microdigestion device was constructed and adapted to an equipment of high pressure ashing, which is commercially available. Digestions of very different microsamples between some μg and some mg were carried out, followed by quantitative determinations of a lot of elements. Besides, different Standard Reference Materials (SRM) were analyzed. The homogeneity of these materials could be investigated by comparing the results found for microsamples with those obtained for samples of 200 mg, the latter after digestion in a conventional device. (author)

Device for taking gaseous samples from irradiated fuel elements

International Nuclear Information System (INIS)

Lengacker, B.

1983-01-01

The described device allows to take gaseous samples from irradiated fuel elements. It is connected with a gas analyzer and a pressure gage, so that in opening the fuel can the internal pressure can be determined

Mechanical Conversion for High-Throughput TEM Sample Preparation

International Nuclear Information System (INIS)

Kendrick, Anthony B; Moore, Thomas M; Zaykova-Feldman, Lyudmila

2006-01-01

This paper presents a novel method of direct mechanical conversion from lift-out sample to TEM sample holder. The lift-out sample is prepared in the FIB using the in-situ liftout Total Release TM method. The mechanical conversion is conducted using a mechanical press and one of a variety of TEM coupons, including coupons for both top-side and back-side thinning. The press joins a probe tip point with attached TEM sample to the sample coupon and separates the complete assembly as a 3mm diameter TEM grid, compatible with commercially available TEM sample holder rods. This mechanical conversion process lends itself well to the high through-put requirements of in-line process control and to materials characterization labs where instrument utilization and sample security are critically important

A low-temperature sample orienting device for single crystal spectroscopy at the SNS

Energy Technology Data Exchange (ETDEWEB)

Sherline, T E; Solomon, L; Roberts, C K II; Bruce, D; Gaulin, B; Granroth, G E, E-mail: sherlinete@ornl.gov

2010-11-01

A low temperature sample orientation device providing three axes of rotation has been successfully built and is in testing for use on several spectrometers at the spallation neutron source (SNS). Sample rotation about the vertical ({omega}) axis of nearly 360 deg. and out of plane tilts ({phi} and v) of from -3.4 deg. to 4.4 deg. and from -2.8 deg. to 3.5 deg., respectively, are possible. An off-the-shelf closed cycle refrigerator (CCR) is mounted on a room temperature sealed rotary flange providing {omega} rotations of the sample. Out-of-plane tilts are made possible by piezoelectric actuated angular positioning devices mounted on the low temperature head of the CCR. Novel encoding devices based on magnetoresistive sensors have been developed to measure the tilt stage angles. This combination facilitates single crystal investigations from room temperature to 3.1 K. Commissioning experiments of the rotating CCR for both powder and single crystal samples have been performed on the ARCS spectrometer at the SNS. For the powder sample this device was used to continuously rotate the sample and thus average out any partial orientation of the powder. The powder rings observed in S(Q) are presented. For the single crystal sample, the rotation was used to probe different regions of momentum transfer (Q-space). Laue patterns obtained from a single crystal sample at two rotation angles are presented.

Preparation of porous titanium oxide films onto indium tin oxide for application in organic photovoltaic devices

Energy Technology Data Exchange (ETDEWEB)

Macedo, Andreia G. [Laboratorio de Dispositivos Nanoestruturados, Departamento de Fisica, Universidade Federal do Parana, Curitiba, Parana (Brazil); Mattos, Luana L.; Spada, Edna R.; Serpa, Rafael B.; Campos, Cristiani S. [Laboratorio de Sistemas Nanoestruturados, Departamento de Fisica, Universidade Federal de Santa Catarina, Florianopolis, Santa Catarina (Brazil); Grova, Isabel R.; Ackcelrud, Leni [Laboratorio de Polimeros Paulo Scarpa, Departamento de Quimica, Universidade Federal do Parana, Curitiba, Parana (Brazil); Reis, Francoise T.; Sartorelli, Maria L. [Laboratorio de Sistemas Nanoestruturados, Departamento de Fisica, Universidade Federal de Santa Catarina, Florianopolis, Santa Catarina (Brazil); Roman, Lucimara S., E-mail: lsroman@fisica.ufpr.br [Laboratorio de Dispositivos Nanoestruturados, Departamento de Fisica, Universidade Federal do Parana, Curitiba, Parana (Brazil)

2012-05-01

In this work, porous ordered TiO{sub 2} films were prepared through sol gel route by using a monolayer of polystyrene spheres as template on indium-tin oxide/glass substrate. These films were characterized by SEM, AFM, Raman spectroscopy, UV-vis absorbance and XRD. The UV-vis absorbance spectrum show a pseudo band gap (PBG) with maxima at 460 nm arising from the light scattering and partial or total suppression of the photon density of states, this PBG can be controlled by the size of the pore. We also propose the use of this porous film as electron acceptor electrode in organic photovoltaic cells; we show that devices prepared with porous titania displayed higher efficiencies than devices using compact titania films as electrode. Such behaviour was observed in both bilayer and bulk heterojunction devices.

Preparation of porous titanium oxide films onto indium tin oxide for application in organic photovoltaic devices

International Nuclear Information System (INIS)

Macedo, Andreia G.; Mattos, Luana L.; Spada, Edna R.; Serpa, Rafael B.; Campos, Cristiani S.; Grova, Isabel R.; Ackcelrud, Leni; Reis, Françoise T.; Sartorelli, Maria L.; Roman, Lucimara S.

2012-01-01

In this work, porous ordered TiO 2 films were prepared through sol gel route by using a monolayer of polystyrene spheres as template on indium-tin oxide/glass substrate. These films were characterized by SEM, AFM, Raman spectroscopy, UV-vis absorbance and XRD. The UV-vis absorbance spectrum show a pseudo band gap (PBG) with maxima at 460 nm arising from the light scattering and partial or total suppression of the photon density of states, this PBG can be controlled by the size of the pore. We also propose the use of this porous film as electron acceptor electrode in organic photovoltaic cells; we show that devices prepared with porous titania displayed higher efficiencies than devices using compact titania films as electrode. Such behaviour was observed in both bilayer and bulk heterojunction devices.

40 CFR 205.171-2 - Test exhaust system sample selection and preparation.

Science.gov (United States)

2010-07-01

... Systems § 205.171-2 Test exhaust system sample selection and preparation. (a)(1) Exhaust systems... 40 Protection of Environment 24 2010-07-01 2010-07-01 false Test exhaust system sample selection and preparation. 205.171-2 Section 205.171-2 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY...

Droplet Size-Aware and Error-Correcting Sample Preparation Using Micro-Electrode-Dot-Array Digital Microfluidic Biochips.

Science.gov (United States)

Li, Zipeng; Lai, Kelvin Yi-Tse; Chakrabarty, Krishnendu; Ho, Tsung-Yi; Lee, Chen-Yi

2017-12-01

Sample preparation in digital microfluidics refers to the generation of droplets with target concentrations for on-chip biochemical applications. In recent years, digital microfluidic biochips (DMFBs) have been adopted as a platform for sample preparation. However, there remain two major problems associated with sample preparation on a conventional DMFB. First, only a (1:1) mixing/splitting model can be used, leading to an increase in the number of fluidic operations required for sample preparation. Second, only a limited number of sensors can be integrated on a conventional DMFB; as a result, the latency for error detection during sample preparation is significant. To overcome these drawbacks, we adopt a next generation DMFB platform, referred to as micro-electrode-dot-array (MEDA), for sample preparation. We propose the first sample-preparation method that exploits the MEDA-specific advantages of fine-grained control of droplet sizes and real-time droplet sensing. Experimental demonstration using a fabricated MEDA biochip and simulation results highlight the effectiveness of the proposed sample-preparation method.

A novel needle-type sampling device for flexible ultrathin bronchoscopy

International Nuclear Information System (INIS)

Suda, Yuji; Hayashi, Katsutoshi; Shindoh, Yuriko; Iijima, Hideya; Tanaka, Akiko

2008-01-01

Diagnosis of suspected cancer in the periphery of the lung is difficult. A flexible ultrathin bronchoscope has been developed for the diagnosis of peripherally located pulmonary lesions that cannot be reached with the sampling devices for standard flexible bronchoscopes. The diagnostic yield with forceps and a brush for ultrathin bronchoscopes, however, is not adequate, especially when a lesion is not exposed to the bronchial lumen. We have thus developed a novel needle-type sampling device and tested its yield in transbronchial cytology. The device consists of an elongated dental H-file (0.4 mm in diameter and 110 cm in length), a housing sheath (1.0 mm in outer diameter), and a novel handle, which enables rapid out-and-in motion of the needle. Ten consecutive patients with a peripheral pulmonary lesion who had an indication for diagnostic procedure with a flexible ultrathin bronchoscope were enrolled. The optimal bronchial route to the lesion was analyzed with virtual bronchoscopy in a data set obtained with high-resolution computed tomography, and a novel bronchial route labeling system (prior-ridge-based relative orientation nomenclature) was employed to guide insertion of the bronchoscope. Sampling with the novel needle was performed prior to use of the forceps and brush under conventional fluoroscopy. In all the cases, sampling with the needle was successful and the amount of the specimen was sufficient for cytology. Our novel sampling system with flexible ultrathin bronchoscopes may contribute to accurate and minimally invasive diagnosis of peripheral pulmonary lesions. (author)

Error Analysis of Ceramographic Sample Preparation for Coating Thickness Measurement of Coated Fuel Particles

International Nuclear Information System (INIS)

Liu Xiaoxue; Li Ziqiang; Zhao Hongsheng; Zhang Kaihong; Tang Chunhe

2014-01-01

The thicknesses of four coatings of HTR coated fuel particle are very important parameters. It is indispensable to control the thickness of four coatings of coated fuel particles for the safety of HTR. A measurement method, ceramographic sample-microanalysis method, to analyze the thickness of coatings was developed. During the process of ceramographic sample-microanalysis, there are two main errors, including ceramographic sample preparation error and thickness measurement error. With the development of microscopic techniques, thickness measurement error can be easily controlled to meet the design requirements. While, due to the coated particles are spherical particles of different diameters ranged from 850 to 1000μm, the sample preparation process will introduce an error. And this error is different from one sample to another. It’s also different from one particle to another in the same sample. In this article, the error of the ceramographic sample preparation was calculated and analyzed. Results show that the error introduced by sample preparation is minor. The minor error of sample preparation guarantees the high accuracy of the mentioned method, which indicates this method is a proper method to measure the thickness of four coatings of coated particles. (author)

Miniaturizing EM Sample Preparation: Opportunities, Challenges, and "Visual Proteomics".

Science.gov (United States)

Arnold, Stefan A; Müller, Shirley A; Schmidli, Claudio; Syntychaki, Anastasia; Rima, Luca; Chami, Mohamed; Stahlberg, Henning; Goldie, Kenneth N; Braun, Thomas

2018-03-01

This review compares and discusses conventional versus miniaturized specimen preparation methods for transmission electron microscopy (TEM). The progress brought by direct electron detector cameras, software developments and automation have transformed transmission cryo-electron microscopy (cryo-EM) and made it an invaluable high-resolution structural analysis tool. In contrast, EM specimen preparation has seen very little progress in the last decades and is now one of the main bottlenecks in cryo-EM. Here, we discuss the challenges faced by specimen preparation for single particle EM, highlight current developments, and show the opportunities resulting from the advanced miniaturized and microfluidic sample grid preparation methods described, such as visual proteomics and time-resolved cryo-EM studies. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Optimized preparation of urine samples for two-dimensional electrophoresis and initial application to patient samples

DEFF Research Database (Denmark)

Lafitte, Daniel; Dussol, Bertrand; Andersen, Søren

2002-01-01

OBJECTIVE: We optimized of the preparation of urinary samples to obtain a comprehensive map of urinary proteins of healthy subjects and then compared this map with the ones obtained with patient samples to show that the pattern was specific of their kidney disease. DESIGN AND METHODS: The urinary...

Analytical characterization of high-level mixed wastes using multiple sample preparation treatments

International Nuclear Information System (INIS)

King, A.G.; Baldwin, D.L.; Urie, M.W.; McKinley, S.G.

1994-01-01

The Analytical Chemistry Laboratory at the Pacific Northwest Laboratory in Richland, Washington, is actively involved in performing analytical characterization of high-level mixed waste from Hanford's single shell and double shell tank characterization programs. A full suite of analyses is typically performed on homogenized tank core samples. These analytical techniques include inductively-coupled plasma-atomic emission spectroscopy, total organic carbon methods and radiochemistry methods, as well as many others, all requiring some type of remote sample-preparation treatment to solubilize the tank sludge material for analysis. Most of these analytical methods typically use a single sample-preparation treatment, inherently providing elemental information only. To better understand and interpret tank chemistry and assist in identifying chemical compounds, selected analytical methods are performed using multiple sample-preparation treatments. The sample preparation treatments used at Pacific Northwest Laboratory for this work with high-level mixed waste include caustic fusion, acid digestion, and water leach. The type of information available by comparing results from different sample-prep treatments includes evidence for the presence of refractory compounds, acid-soluble compounds, or water-soluble compounds. Problems unique to the analysis of Hanford tank wastes are discussed. Selected results from the Hanford single shell ferrocyanide tank, 241-C-109, are presented, and the resulting conclusions are discussed

Novel sample preparation for operando TEM of catalysts

International Nuclear Information System (INIS)

Miller, Benjamin K.; Barker, Trevor M.; Crozier, Peter A.

2015-01-01

A new TEM sample preparation method is developed to facilitate operando TEM of gas phase catalysis. A porous Pyrex-fiber pellet TEM sample was produced, allowing a comparatively large amount of catalyst to be loaded into a standard Gatan furnace-type tantalum heating holder. The increased amount of catalyst present inside the environmental TEM allows quantitative determination of the gas phase products of a catalytic reaction performed in-situ at elevated temperatures. The product gas concentration was monitored using both electron energy loss spectroscopy (EELS) and residual gas analysis (RGA). Imaging of catalyst particles dispersed over the pellet at atomic resolution is challenging, due to charging of the insulating glass fibers. To overcome this limitation, a metal grid is placed into the holder in addition to the pellet, allowing catalyst particles dispersed over the grid to be imaged, while particles in the pellet, which are assumed to experience identical conditions, contribute to the overall catalytic conversion inside the environmental TEM cell. The gas within the cell is determined to be well-mixed, making this assumption reasonable. - Highlights: • High in-situ conversion of CO to CO 2 achieved by a novel TEM sample preparation method. • A 3 mm fiber pellet increases the TEM sample surface area by 50×. • Operando atomic resolution is maintained by also including a 3 mm grid in the sample. • Evidence for a well-mixed gas composition inside the ETEM cell is given

Fabrication of quantum-dot devices in graphene

Directory of Open Access Journals (Sweden)

Satoshi Moriyama, Yoshifumi Morita, Eiichiro Watanabe, Daiju Tsuya, Shinya Uji, Maki Shimizu and Koji Ishibashi

2010-01-01

Full Text Available We describe our recent experimental results on the fabrication of quantum-dot devices in a graphene-based two-dimensional system. Graphene samples were prepared by micromechanical cleavage of graphite crystals on a SiO2/Si substrate. We performed micro-Raman spectroscopy measurements to determine the number of layers of graphene flakes during the device fabrication process. By applying a nanofabrication process to the identified graphene flakes, we prepared a double-quantum-dot device structure comprising two lateral quantum dots coupled in series. Measurements of low-temperature electrical transport show the device to be a series-coupled double-dot system with varied interdot tunnel coupling, the strength of which changes continuously and non-monotonically as a function of gate voltage.

78 FR 27442 - Coal Mine Dust Sampling Devices; Correction

Science.gov (United States)

2013-05-10

... DEPARTMENT OF LABOR Mine Safety and Health Administration Coal Mine Dust Sampling Devices; Correction AGENCY: Mine Safety and Health Administration, Labor. ACTION: Notice; correction. SUMMARY: On April 30, 2013, Mine Safety and Health Administration (MSHA) published a notice in the Federal Register...

A microfluidic dialysis device for complex biological mixture SERS analysis

KAUST Repository

Perozziello, Gerardo; Candeloro, Patrizio; Gentile, Francesco T.; Coluccio, Maria Laura; Tallerico, Marco; De Grazia, Antonio; Nicastri, Annalisa; Perri, Angela Mena; Parrotta, Elvira; Pardeo, Francesca; Catalano, Rossella; Cuda, Giovanni; Di Fabrizio, Enzo M.

2015-01-01

In this paper, we present a microfluidic device fabricated with a simple and inexpensive process allowing rapid filtering of peptides from a complex mixture. The polymer microfluidic device can be used for sample preparation in biological

Modern methods of sample preparation for GC analysis

NARCIS (Netherlands)

de Koning, S.; Janssen, H.-G.; Brinkman, U.A.Th.

2009-01-01

Today, a wide variety of techniques is available for the preparation of (semi-) solid, liquid and gaseous samples, prior to their instrumental analysis by means of capillary gas chromatography (GC) or, increasingly, comprehensive two-dimensional GC (GC × GC). In the past two decades, a large number

Collection and preparation of wet and dry stream-sediment samples

International Nuclear Information System (INIS)

Puchlik, K.

1977-03-01

Lawrence Livermore Laboratory is responsible for the Hydrogeochemistry and Stream Sediment Reconnaissance (HSSR) program for uranium in the seven far western states. The work thus far has concentrated on the arid to semi-arid regions of the West and this paper discusses the collection and preparation of sediment samples in the Basin and Range province. The sample collection and preparation procedures described here may not be applicable to other parts of the far western states or other areas. These procedures also differ somewhat from those used by the other three laboratories involved in the HSSR program

Sampling and sample preparation methods for the analysis of trace elements in biological material

International Nuclear Information System (INIS)

Sansoni, B.; Iyengar, V.

1978-05-01

The authors attempt to give a most systamtic possible treatment of the sample taking and sample preparation of biological material (particularly in human medicine) for trace analysis (e.g. neutron activation analysis, atomic absorption spectrometry). Contamination and loss problems are discussed as well as the manifold problems of the different consistency of solid and liquid biological materials, as well as the stabilization of the sample material. The process of dry and wet ashing is particularly dealt with, where new methods are also described. (RB) [de

Sample preparation with solid phase microextraction and exhaustive extraction approaches: Comparison for challenging cases.

Science.gov (United States)

Boyacı, Ezel; Rodríguez-Lafuente, Ángel; Gorynski, Krzysztof; Mirnaghi, Fatemeh; Souza-Silva, Érica A; Hein, Dietmar; Pawliszyn, Janusz

2015-05-11

In chemical analysis, sample preparation is frequently considered the bottleneck of the entire analytical method. The success of the final method strongly depends on understanding the entire process of analysis of a particular type of analyte in a sample, namely: the physicochemical properties of the analytes (solubility, volatility, polarity etc.), the environmental conditions, and the matrix components of the sample. Various sample preparation strategies have been developed based on exhaustive or non-exhaustive extraction of analytes from matrices. Undoubtedly, amongst all sample preparation approaches, liquid extraction, including liquid-liquid (LLE) and solid phase extraction (SPE), are the most well-known, widely used, and commonly accepted methods by many international organizations and accredited laboratories. Both methods are well documented and there are many well defined procedures, which make them, at first sight, the methods of choice. However, many challenging tasks, such as complex matrix applications, on-site and in vivo applications, and determination of matrix-bound and free concentrations of analytes, are not easily attainable with these classical approaches for sample preparation. In the last two decades, the introduction of solid phase microextraction (SPME) has brought significant progress in the sample preparation area by facilitating on-site and in vivo applications, time weighted average (TWA) and instantaneous concentration determinations. Recently introduced matrix compatible coatings for SPME facilitate direct extraction from complex matrices and fill the gap in direct sampling from challenging matrices. Following introduction of SPME, numerous other microextraction approaches evolved to address limitations of the above mentioned techniques. There is not a single method that can be considered as a universal solution for sample preparation. This review aims to show the main advantages and limitations of the above mentioned sample

Automated dried blood spots standard and QC sample preparation using a robotic liquid handler.

Science.gov (United States)

Yuan, Long; Zhang, Duxi; Aubry, Anne-Francoise; Arnold, Mark E

2012-12-01

A dried blood spot (DBS) bioanalysis assay involves many steps, such as the preparation of standard (STD) and QC samples in blood, the spotting onto DBS cards, and the cutting-out of the spots. These steps are labor intensive and time consuming if done manually, which, therefore, makes automation very desirable in DBS bioanalysis. A robotic liquid handler was successfully applied to the preparation of STD and QC samples in blood and to spot the blood samples onto DBS cards using buspirone as the model compound. This automated preparation was demonstrated to be accurate and consistent. However the accuracy and precision of automated preparation were similar to those from manual preparation. The effect of spotting volume on accuracy was evaluated and a trend of increasing concentrations of buspirone with increasing spotting volumes was observed. The automated STD and QC sample preparation process significantly improved the efficiency, robustness and safety of DBS bioanalysis.

Bio-sample detection on paper-based devices with inkjet printer-sprayed reagents.

Science.gov (United States)

Liang, Wun-Hong; Chu, Chien-Hung; Yang, Ruey-Jen

2015-12-01

The reagent required for bio-sample detection on paper-based analytical devices is generally introduced manually using a pipette. Such an approach is time-consuming; particularly if a large number of devices are required. Automated methods provide a far more convenient solution for large-scale production, but incur a substantial cost. Accordingly, the present study proposes a low-cost method for the paper-based analytical devices in which the biochemical reagents are sprayed onto the device directly using a modified commercial inkjet printer. The feasibility of the proposed method is demonstrated by performing aspartate aminotransferase (AST) and alanine aminotransferase (ALT) tests using simple two-dimensional (2D) paper-based devices. In both cases, the reaction process is analyzed using an image-processing-based colorimetric method. The experimental results show that for AST detection within the 0-105 U/l concentration range, the optimal observation time is around four minutes, while for ALT detection in the 0-125 U/l concentration range, the optimal observation time is approximately one minute. Finally, for both samples, the detection performance of the sprayed-reagent analytical devices is insensitive to the glucose concentration. Copyright © 2015 Elsevier B.V. All rights reserved.

Independent assessment of matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) sample preparation quality : Effect of sample preparation on MALDI-MS of synthetic polymers

NARCIS (Netherlands)

Kooijman, Pieter C.; Kok, Sander; Honing, Maarten

2017-01-01

Rationale: Matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) provides detailed and in-depth information about the molecular characteristics of synthetic polymers. To obtain the most accurate results the sample preparation parameters should be chosen to suit the sample and the

A hybrid approach to device integration on a genetic analysis platform

International Nuclear Information System (INIS)

Brennan, Des; Justice, John; Aherne, Margaret; Galvin, Paul; Jary, Dorothee; Kurg, Ants; Berik, Evgeny; Macek, Milan

2012-01-01

Point-of-care (POC) systems require significant component integration to implement biochemical protocols associated with molecular diagnostic assays. Hybrid platforms where discrete components are combined in a single platform are a suitable approach to integration, where combining multiple device fabrication steps on a single substrate is not possible due to incompatible or costly fabrication steps. We integrate three devices each with a specific system functionality: (i) a silicon electro-wetting-on-dielectric (EWOD) device to move and mix sample and reagent droplets in an oil phase, (ii) a polymer microfluidic chip containing channels and reservoirs and (iii) an aqueous phase glass microarray for fluorescence microarray hybridization detection. The EWOD device offers the possibility of fully integrating on-chip sample preparation using nanolitre sample and reagent volumes. A key challenge is sample transfer from the oil phase EWOD device to the aqueous phase microarray for hybridization detection. The EWOD device, waveguide performance and functionality are maintained during the integration process. An on-chip biochemical protocol for arrayed primer extension (APEX) was implemented for single nucleotide polymorphism (SNiP) analysis. The prepared sample is aspirated from the EWOD oil phase to the aqueous phase microarray for hybridization. A bench-top instrumentation system was also developed around the integrated platform to drive the EWOD electrodes, implement APEX sample heating and image the microarray after hybridization. (paper)

Sample Preparation of Corn Seed Tissue to Prevent Analyte Relocations for Mass Spectrometry Imaging

Science.gov (United States)

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.

Sample Preparation of Corn Seed Tissue to Prevent Analyte Relocations for Mass Spectrometry Imaging.

Science.gov (United States)

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. Graphical Abstract ᅟ.

Universal Sample Preparation Module for Molecular Analysis in Space, Phase I

Data.gov (United States)

National Aeronautics and Space Administration — Lynntech proposes to develop and demonstrate the ability of a compact, light-weight, and automated universal sample preparation module (USPM) to process samples from...

Elaboration of a semiconductive thin film device technology on the basis of monocrystalline gallium arsenide

International Nuclear Information System (INIS)

Antoshenko, V.; Taurbaev, T.; Skirnevskaya, E.; Shorin, V.; Mihajlov, L.; Bajganatova, Sh.

1996-01-01

The aim of the project: To elaborate the economical technological process of preparing super thin monocrystalline GaAs substrates and device structures for semiconductive electronics. To realize the project it is necessary to solve following problems: o to elaborate and produce the equipment for preparing of separated films and thin film multilayer structures with p-n-junction; - to study conditions of preparing plane crystal perfect separated Ga(Al)As - films; - to optimize regimes of preparing thin film structures with p- and n-conductive - layers; - to determine the optimal methods of transferring autonomous films and structures over the second substrates; - to work out preparing methods of ohmic contacts and electrical commutation; - to optimize the process of repeated use of initial monocrystalline GaAs substrate; - to prepare the samples of discrete thin film photo- and emitting devices. As the result of project realization there will be created cheap ecological technology of heterojunction optoelectronic devices on the basis of GaAs and AlGaAs solid solutions, the laboratory samples of thin film devices will be presented

Solid recovered fuels in the cement industry--semi-automated sample preparation unit as a means for facilitated practical application.

Science.gov (United States)

Aldrian, Alexia; Sarc, Renato; Pomberger, Roland; Lorber, Karl E; Sipple, Ernst-Michael

2016-03-01

One of the challenges for the cement industry is the quality assurance of alternative fuel (e.g., solid recovered fuel, SRF) in co-incineration plants--especially for inhomogeneous alternative fuels with large particle sizes (d95⩾100 mm), which will gain even more importance in the substitution of conventional fuels due to low production costs. Existing standards for sampling and sample preparation do not cover the challenges resulting from these kinds of materials. A possible approach to ensure quality monitoring is shown in the present contribution. For this, a specially manufactured, automated comminution and sample divider device was installed at a cement plant in Rohožnik. In order to prove its practical suitability with methods according to current standards, the sampling and sample preparation process were validated for alternative fuel with a grain size >30 mm (i.e., d95=approximately 100 mm), so-called 'Hotdisc SRF'. Therefore, series of samples were taken and analysed. A comparison of the analysis results with the yearly average values obtained through a reference investigation route showed good accordance. Further investigations during the validation process also showed that segregation or enrichment of material throughout the comminution plant does not occur. The results also demonstrate that compliance with legal standards regarding the minimum sample amount is not sufficient for inhomogeneous and coarse particle size alternative fuels. Instead, higher sample amounts after the first particle size reduction step are strongly recommended in order to gain a representative laboratory sample. © The Author(s) 2016.

Development of gas-sampling device for 13N monitoring system

International Nuclear Information System (INIS)

Zhao Lihong; Gong Xueyu

2003-01-01

The 13 N monitoring system is used in the monitoring of the rate of leakage of the primary coolant circuit in nuclear power stations. The author introduces a gas-sampling device of the 13 Nmonitoring system. It is with a close-loop flow control system with intelligent control of Single Chip Micyoco (SCM), and has the ability to monitor and replace the filter paper automatically, to increase the automation of the device and stable operation in long time

Recent developments in sample preparation and data pre-treatment in metabonomics research.

Science.gov (United States)

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.

Current advances and strategies towards fully automated sample preparation for regulated LC-MS/MS bioanalysis.

Science.gov (United States)

Zheng, Naiyu; Jiang, Hao; Zeng, Jianing

2014-09-01

Robotic liquid handlers (RLHs) have been widely used in automated sample preparation for liquid chromatography-tandem mass spectrometry (LC-MS/MS) bioanalysis. Automated sample preparation for regulated bioanalysis offers significantly higher assay efficiency, better data quality and potential bioanalytical cost-savings. For RLHs that are used for regulated bioanalysis, there are additional requirements, including 21 CFR Part 11 compliance, software validation, system qualification, calibration verification and proper maintenance. This article reviews recent advances in automated sample preparation for regulated bioanalysis in the last 5 years. Specifically, it covers the following aspects: regulated bioanalysis requirements, recent advances in automation hardware and software development, sample extraction workflow simplification, strategies towards fully automated sample extraction, and best practices in automated sample preparation for regulated bioanalysis.

Synthesis and application of magnetic molecularly imprinted polymers in sample preparation.

Science.gov (United States)

Huang, Shuyao; Xu, Jianqiao; Zheng, Jiating; Zhu, Fang; Xie, Lijun; Ouyang, Gangfeng

2018-04-12

Magnetic molecularly imprinted polymers (MMIPs) have superior advantages in sample pretreatment because of their high selectivity for target analytes and the fast and easy isolation from samples. To meet the demand of both good magnetic property and good extraction performance, MMIPs with various structures, from traditional core-shell structures to novel composite structures with a larger specific surface area and more accessible binding sites, are fabricated by different preparation technologies. Moreover, as the molecularly imprinted polymer (MIP) layers determine the affinity, selectivity, and saturated adsorption amount of MMIPs, the development and innovation of the MIP layer are attracting attention and are reviewed here. Many studies that used MMIPs as sorbents in dispersive solid-phase extraction of complex samples, including environmental, food, and biofluid samples, are summarized. Graphical abstract The application of magnetic molecularly imprinted polymers (MIPs) in the sample preparation procedure improves the analytical performances for complex samples. MITs molecular imprinting technologies.

Device to investigate samples by means of flameless atomic absorption measurement

International Nuclear Information System (INIS)

Sperling, K.R.

1977-01-01

An improvement on a device to investigate samples by means of flameless atomic absorption measurement is suggested in which one aims to produce a most complete possible atomic clond from the sample to be investigated within the sample space defined by the beam bundle, through which the measuring beam bundle is passed. According to the invention, the tubular sample space should be closed by an optically penetrable window on one side. (RW) [de

Fluid control structures in microfluidic devices

Science.gov (United States)

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

2017-05-09

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

High-resolution X-ray diffraction with no sample preparation.

Science.gov (United States)

Hansford, G M; Turner, S M R; Degryse, P; Shortland, A J

2017-07-01

It is shown that energy-dispersive X-ray diffraction (EDXRD) implemented in a back-reflection geometry is extremely insensitive to sample morphology and positioning even in a high-resolution configuration. This technique allows high-quality X-ray diffraction analysis of samples that have not been prepared and is therefore completely non-destructive. The experimental technique was implemented on beamline B18 at the Diamond Light Source synchrotron in Oxfordshire, UK. The majority of the experiments in this study were performed with pre-characterized geological materials in order to elucidate the characteristics of this novel technique and to develop the analysis methods. Results are presented that demonstrate phase identification, the derivation of precise unit-cell parameters and extraction of microstructural information on unprepared rock samples and other sample types. A particular highlight was the identification of a specific polytype of a muscovite in an unprepared mica schist sample, avoiding the time-consuming and difficult preparation steps normally required to make this type of identification. The technique was also demonstrated in application to a small number of fossil and archaeological samples. Back-reflection EDXRD implemented in a high-resolution configuration shows great potential in the crystallographic analysis of cultural heritage artefacts for the purposes of scientific research such as provenancing, as well as contributing to the formulation of conservation strategies. Possibilities for moving the technique from the synchrotron into museums are discussed. The avoidance of the need to extract samples from high-value and rare objects is a highly significant advantage, applicable also in other potential research areas such as palaeontology, and the study of meteorites and planetary materials brought to Earth by sample-return missions.

Application of immunoaffinity columns for different food item samples preparation in micotoxins determination

Directory of Open Access Journals (Sweden)

Ćurčić Marijana

2016-01-01

Full Text Available In analytical methods used for monitoring of what special attention is paid to sample preparation. Therefore, the objective of this study was testing the efficiency of immunoaffinity columns (IAC that are based on solid phase extraction principles used for samples preparation in determining aflatoxins and ochratoxins. Aflatoxins and ochratoxins concentrations were determined in totally 56 samples of food items: wheat, corn, rice, barley and other grains (19 samples, flour and flour products from grain and additives for the bakery industry (7 samples, fruits and vegetables (3 samples, hazelnut, walnut, almond, coconut flour (4 samples, roasted cocoa beans, peanuts, tea, coffee (16 samples, spices (4 samples and meat and meat products (4 samples. Obtained results indicate advantage of IAC use for sample preparation based on enhanced specificity due to binding of extracted molecules to incorporated specific antibodies and rinsing the rest molecules from sample which could interfere with further analysis. Additional advantage is the usage of small amount of organic solvents and consequently decreased exposure of staff who conduct micotoxins determination. Of special interest is increase in method sensitivity since limit of quantification for aflatoxins and ochratoxins determination method is lower than maximal allowed concentration of these toxines prescribed by national rule book.

HASE - The Helsinki adaptive sample preparation line

Energy Technology Data Exchange (ETDEWEB)

Palonen, V., E-mail: vesa.palonen@helsinki.fi [Department of Physics, University of Helsinki, P.O. Box 43, FI-00014 (Finland); Pesonen, A. [Laboratory of Chronology, Finnish Museum of Natural History, P.O. Box 64, FI-00014 (Finland); Herranen, T.; Tikkanen, P. [Department of Physics, University of Helsinki, P.O. Box 43, FI-00014 (Finland); Oinonen, M. [Laboratory of Chronology, Finnish Museum of Natural History, P.O. Box 64, FI-00014 (Finland)

2013-01-15

We have designed and built an adaptive sample preparation line with separate modules for combustion, molecular sieve handling, CO{sub 2} gas cleaning, CO{sub 2} storage, and graphitization. The line is also connected to an elemental analyzer. Operation of the vacuum equipment, a flow controller, pressure sensors, ovens, and graphitization reactors are automated with a reliable NI-cRIO real-time system. Stepped combustion can be performed in two ovens at temperatures up to 900 Degree-Sign C. Depending on the application, CuO or O{sub 2}-flow combustion can be used. A flow controller is used to adjust the O{sub 2} flow and pressure during combustion. For environmental samples, a module for molecular sieve regeneration and sample desorption is attached to the line replacing the combustion module. In the storage module, CO{sub 2} samples can be stored behind a gas-tight diaphragm valve and either stored for later graphitization or taken for measurements with separate equipment (AMS gas ion source or a separate mass spectrometer). The graphitization module consists of four automated reactors, capable of graphitizing samples with masses from 3 mg down to 50 {mu}g.

Gel-aided sample preparation (GASP)--a simplified method for gel-assisted proteomic sample generation from protein extracts and intact cells.

Science.gov (United States)

Fischer, Roman; Kessler, Benedikt M

2015-04-01

We describe a "gel-assisted" proteomic sample preparation method for MS analysis. Solubilized protein extracts or intact cells are copolymerized with acrylamide, facilitating denaturation, reduction, quantitative cysteine alkylation, and matrix formation. Gel-aided sample preparation has been optimized to be highly flexible, scalable, and to allow reproducible sample generation from 50 cells to milligrams of protein extracts. This methodology is fast, sensitive, easy-to-use on a wide range of sample types, and accessible to nonspecialists. © 2014 The Authors. PROTEOMICS published by Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

A Proteomics Sample Preparation Method for Mature, Recalcitrant Leaves of Perennial Plants

Science.gov (United States)

Na, Zhang; Chengying, Lao; Bo, Wang; Dingxiang, Peng; Lijun, Liu

2014-01-01

Sample preparation is key to the success of proteomics studies. In the present study, two sample preparation methods were tested for their suitability on the mature, recalcitrant leaves of six representative perennial plants (grape, plum, pear, peach, orange, and ramie). An improved sample preparation method was obtained: Tris and Triton X-100 were added together instead of CHAPS to the lysis buffer, and a 20% TCA-water solution and 100% precooled acetone were added after the protein extraction for the further purification of protein. This method effectively eliminates nonprotein impurities and obtains a clear two-dimensional gel electrophoresis array. The method facilitates the separation of high-molecular-weight proteins and increases the resolution of low-abundance proteins. This method provides a widely applicable and economically feasible technology for the proteomic study of the mature, recalcitrant leaves of perennial plants. PMID:25028960

A proteomics sample preparation method for mature, recalcitrant leaves of perennial plants.

Directory of Open Access Journals (Sweden)

Deng Gang

Full Text Available Sample preparation is key to the success of proteomics studies. In the present study, two sample preparation methods were tested for their suitability on the mature, recalcitrant leaves of six representative perennial plants (grape, plum, pear, peach, orange, and ramie. An improved sample preparation method was obtained: Tris and Triton X-100 were added together instead of CHAPS to the lysis buffer, and a 20% TCA-water solution and 100% precooled acetone were added after the protein extraction for the further purification of protein. This method effectively eliminates nonprotein impurities and obtains a clear two-dimensional gel electrophoresis array. The method facilitates the separation of high-molecular-weight proteins and increases the resolution of low-abundance proteins. This method provides a widely applicable and economically feasible technology for the proteomic study of the mature, recalcitrant leaves of perennial plants.

Advances in modern sample preparation techniques using microwaves assisted chemistry for metal species determination (W1)

International Nuclear Information System (INIS)

Ponard, O.F.X.

2002-01-01

Full text: Sample preparation has long been the bottleneck of environmental analysis for both total and species specific analysis. Digestion, extraction and preparation of the analytes are relying on a series of chemical reactions. The introduction of microwave assisted sample preparation has first been viewed as a mean to accelerate the kinetics of digestion of the matrix for total elements and fast samples preparation procedures. However, the extensive development and success of microwave digestion procedures in total elemental analysis has now allowed to have a larger insight of the perspectives offered by this technique. Microwave technologies now offer to have a precise control of the temperature and indirectly control the reaction kinetics taking place during the sample preparation procedures. Microwave assisted chemistry permits to perform simultaneously the fundamental steps required for metal species extraction and derivatization. The number of sample preparation steps used for organotin or organomercury species have been reduced to one and the total time of sample preparation brought down for a few hours to some minutes. Further, the developments of GC/ICP/MS techniques allow to routinely use speciated isotopic dilution methods has internal probe of the chemical reactions. These new approaches allow us to use the addition of the labeled species for isotopic dilution as a mean to evaluate and follow the chemical processes taking place during the extraction procedure. These procedures will help us to understand and check for the stability of the analytes during the chemistry of the sample preparation procedure and bring some insights of the chemistry taking place during the extraction. Understanding the different mechanisms involved in the sample preparation steps will allow us in return to further improve all theses procedures and bring us to the horizon of 'on-line sample preparation and detection'. (author)

Development of a One-Handed, Environmental Surface-Sampling Device

Science.gov (United States)

2016-05-01

individual packaging, an operator can generate a large amount of waste that needs to be managed during a sampling mission. The U.S. Army Edgewood...prepared and spore spotting was performed in a biological safety cabinet. For the spore- spotting procedures, the surfaces were spotted with 1 mL of...260 nm (A260) and 280 nm (A280). To determine the DNA concentration for each sample, the NanoDrop software used a modified Beer –Lambert equation and

A core handling device for the Mars Sample Return Mission

Science.gov (United States)

Gwynne, Owen

1989-01-01

A core handling device for use on Mars is being designed. To provide a context for the design study, it was assumed that a Mars Rover/Sample Return (MRSR) Mission would have the following characteristics: a year or more in length; visits by the rover to 50 or more sites; 100 or more meter-long cores being drilled by the rover; and the capability of returning about 5 kg of Mars regolith to Earth. These characteristics lead to the belief that in order to bring back a variegated set of samples that can address the range of scientific objetives for a MRSR mission to Mars there needs to be considerable analysis done on board the rover. Furthermore, the discrepancy between the amount of sample gathered and the amount to be returned suggests that there needs to be some method of choosing the optimal set of samples. This type of analysis will require pristine material-unaltered by the drilling process. Since the core drill thermally and mechanically alters the outer diameter (about 10 pct) of the core sample, this outer area cannot be used. The primary function of the core handling device is to extract subsamples from the core and to position these subsamples, and the core itself if needed, with respect to the various analytical instruments that can be used to perform these analyses.

Difficulties in preparing a standard sample of uranium metal having traces of nitrogen

International Nuclear Information System (INIS)

Toteja, R.S.D.; Jangida, B.L.; Sundaresan, M.

1991-01-01

Normally in the analysis of uranium for nitrogen, the nitrides are hydrolysed to give NH 3 and that for standardisation purposes to approximate the closest conditions of analysis of ammonia, NH 4 Cl is added to the sample and the recovery is tested. An appropriate method will be to have a standard sample of uranium with known amounts of nitrogen to be used as reference sample. The present work describes the efforts made in the preparation of such a reference sample and a general assessment of such methods available. In present work, known microamounts of nitrogen in an enclosed volume were allowed to react at a temperature of 773 K with a fixed amount of uranium metal of nitrogen content determined chemically. As the reaction of nitrogen with uranium is essentially a surface reaction, a sample had to be homogenised by allowing the nitrided sample to melt at about 1500 K and allow the nitrogen to diffuse through so that the concentration gradient along the profile will disappear. Attempts were made to prepare such samples in the range to 40 to 100 ppm of nitrogen. The density differences of uranium nitride and uranium metal made this diffusion and homogenisation process difficult. The prepared samples were analysed by the micro-kjeldahl's method and the recoveries tested. The equipment used for the preparation of the nitrided samples, for homogenisation and analysis of the results obtained are detailed in the paper together with the assessment of the general methods. (author). 2 refs., 1 fig., 1 tab

Biological samples positioning device for irradiations on a radial channel at the nuclear research reactor

International Nuclear Information System (INIS)

Rodriguez Gual, Maritza; Mas Milian, Felix; Deppman, Airton; Pinto Coelho, Paulo Rogerio

2010-01-01

For the demand of an experimental device for biological samples positioning system for irradiations on a radial channel at the nuclear research reactor in operation was constructed and started up a device for the place and remove of the biological samples from the irradiation channels without interrupting the operation of the reactor. The economical valuations are effected comparing with another type of device with the same functions. This work formed part of an international project between Cuba and Brazil that undertook the study of the induced damages by various types of ionizing radiation in DNA molecules. Was experimentally tested the proposed solution, which demonstrates the practical validity of the device. As a result of the work, the experimental device for biological samples irradiations are installed and operating in the radial beam hole No3(BH3) for more than five years at the IEA-R1 Brazilian research reactor according to the solicited requirements the device. The designed device increases considerably the type of studies can be conducted in this reactor. Its practical application in research taking place in that facility, in the field of radiobiology and dosimetry, and so on is immediate

Skin sample preparation by collagenase digestion for diclofenac quantification using LC-MS/MS after topical application.

Science.gov (United States)

Nirogi, Ramakrishna; Padala, Naga Surya Prakash; Boggavarapu, Rajesh Kumar; Kalaikadhiban, Ilayaraja; Ajjala, Devender Reddy; Bhyrapuneni, Gopinadh; Muddana, Nageswara Rao

2016-06-01

Skin is the target site to evaluate the pharmacokinetic parameters of topical applications. Sample preparation is one of the influential steps in the bioanalysis of drugs in the skin. Evaluation of dermatopharmacokinetics at preclinical stage is challenging due to lack of proper sample preparation method. There is a need for an efficient sample preparation procedure for quantification of drugs in the skin using LC-MS/MS. The skin samples treated with collagenase followed by homogenization using a bead beater represents a best-fit method resulting in uniform homogenate for reproducible results. A new approach involving enzymatic treatment and mechanical homogenization techniques were evaluated for efficient sample preparation of skin samples in the bioanalysis.

A review of sample preparation and its influence on pH determination in concrete samples

International Nuclear Information System (INIS)

Manso, S.; Aguado, A.

2017-01-01

If we are to monitor the chemical processes in cementitious materials, then pH assays in the pore solutions of cement pastes, mortars, and concretes are of key importance. However, there is no standard method that regulates the sample-preparation method for pH determination. The state-of-the-art of different methods for pH determination in cementitious materials is presented in this paper and the influence of sample preparation in each case. Moreover, an experimental campaign compares three different techniques for pH determination. Its results contribute to establishing a basic criterion to help researchers select the most suitable method, depending on the purpose of the research. A simple tool is described for selecting the easiest and the most economic pH determination method, depending on the objective; especially for researchers and those with limited experience in this field.

A user-friendly robotic sample preparation program for fully automated biological sample pipetting and dilution to benefit the regulated bioanalysis.

Science.gov (United States)

Jiang, Hao; Ouyang, Zheng; Zeng, Jianing; Yuan, Long; Zheng, Naiyu; Jemal, Mohammed; Arnold, Mark E

2012-06-01

Biological sample dilution is a rate-limiting step in bioanalytical sample preparation when the concentrations of samples are beyond standard curve ranges, especially when multiple dilution factors are needed in an analytical run. We have developed and validated a Microsoft Excel-based robotic sample preparation program (RSPP) that automatically transforms Watson worklist sample information (identification, sequence and dilution factor) to comma-separated value (CSV) files. The Freedom EVO liquid handler software imports and transforms the CSV files to executable worklists (.gwl files), allowing the robot to perform sample dilutions at variable dilution factors. The dynamic dilution range is 1- to 1000-fold and divided into three dilution steps: 1- to 10-, 11- to 100-, and 101- to 1000-fold. The whole process, including pipetting samples, diluting samples, and adding internal standard(s), is accomplished within 1 h for two racks of samples (96 samples/rack). This platform also supports online sample extraction (liquid-liquid extraction, solid-phase extraction, protein precipitation, etc.) using 96 multichannel arms. This fully automated and validated sample dilution and preparation process has been applied to several drug development programs. The results demonstrate that application of the RSPP for fully automated sample processing is efficient and rugged. The RSPP not only saved more than 50% of the time in sample pipetting and dilution but also reduced human errors. The generated bioanalytical data are accurate and precise; therefore, this application can be used in regulated bioanalysis.

Compact low temperature scanning tunneling microscope with in-situ sample preparation capability

Energy Technology Data Exchange (ETDEWEB)

Kim, Jungdae [Department of Physics, The University of Texas, Austin, Texas 78712 (United States); Department of Physics and EHSRC, University of Ulsan, Ulsan 680-749 (Korea, Republic of); Nam, Hyoungdo; Schroeder, Allan; Shih, Chih-Kang, E-mail: shih@physics.utexas.edu [Department of Physics, The University of Texas, Austin, Texas 78712 (United States); Qin, Shengyong [Department of Physics, The University of Texas, Austin, Texas 78712 (United States); Department of Physics, University of Science and Technology of China, Hefei, Anhui 230026 (China); ICQD, Hefei National Laboratory for Physical Sciences at the Microscale, University of Science and Technology of China, Hefei, Anhui 230026 (China); Kim, Sang-ui [Department of Physics and EHSRC, University of Ulsan, Ulsan 680-749 (Korea, Republic of); Eom, Daejin [Korea Research Institute of Standards and Science, Daejeon 305-340 (Korea, Republic of)

2015-09-15

We report on the design of a compact low temperature scanning tunneling microscope (STM) having in-situ sample preparation capability. The in-situ sample preparation chamber was designed to be compact allowing quick transfer of samples to the STM stage, which is ideal for preparing temperature sensitive samples such as ultra-thin metal films on semiconductor substrates. Conventional spring suspensions on the STM head often cause mechanical issues. To address this problem, we developed a simple vibration damper consisting of welded metal bellows and rubber pads. In addition, we developed a novel technique to ensure an ultra-high-vacuum (UHV) seal between the copper and stainless steel, which provides excellent reliability for cryostats operating in UHV. The performance of the STM was tested from 2 K to 77 K by using epitaxial thin Pb films on Si. Very high mechanical stability was achieved with clear atomic resolution even when using cryostats operating at 77 K. At 2 K, a clean superconducting gap was observed, and the spectrum was easily fit using the BCS density of states with negligible broadening.

Compact low temperature scanning tunneling microscope with in-situ sample preparation capability.

Science.gov (United States)

Kim, Jungdae; Nam, Hyoungdo; Qin, Shengyong; Kim, Sang-ui; Schroeder, Allan; Eom, Daejin; Shih, Chih-Kang

2015-09-01

We report on the design of a compact low temperature scanning tunneling microscope (STM) having in-situ sample preparation capability. The in-situ sample preparation chamber was designed to be compact allowing quick transfer of samples to the STM stage, which is ideal for preparing temperature sensitive samples such as ultra-thin metal films on semiconductor substrates. Conventional spring suspensions on the STM head often cause mechanical issues. To address this problem, we developed a simple vibration damper consisting of welded metal bellows and rubber pads. In addition, we developed a novel technique to ensure an ultra-high-vacuum (UHV) seal between the copper and stainless steel, which provides excellent reliability for cryostats operating in UHV. The performance of the STM was tested from 2 K to 77 K by using epitaxial thin Pb films on Si. Very high mechanical stability was achieved with clear atomic resolution even when using cryostats operating at 77 K. At 2 K, a clean superconducting gap was observed, and the spectrum was easily fit using the BCS density of states with negligible broadening.

Methods and devices for hyperpolarising and melting NMR samples in a cryostat

DEFF Research Database (Denmark)

Ardenkjaer-Larsen, Jan Henrik; Axelsson, Oskar H. E.; Golman, Klaes Koppel

2006-01-01

The present invention relates to devices and method for melting solid polarised sample while retaining a high level of polarisation. In an embodiment of the present invention a sample is polarised in a sample-retaining cup 9 in a strong magnetic field in a polarising means 3a, 3b, 3c in a cryosta...

Novel Biomedical Device Utilizing Light-Emitting Nanostructures Developed

Science.gov (United States)

Scardelletti, Maximilian C.; Goldman, Rachel

2004-01-01

Sketches and chemical diagrams of state-of-the-art device and novel proposed device are presented. Current device uses a diode laser that emits into a fluorescent fluid only one wavelength and a photodetector diode that detects only one wavelength. Only one type of bacteria can be detected. The proposed device uses a quantum dot array that emits into a fluorescent fluid multiple wavelengths and an NIR 512 spectrometer that scans 0.8- to 1.7-mm wavelengths. Hundreds of different bacteria and viruses can be detected. A novel biomedical device is being developed at the NASA Glenn Research Center in cooperation with the University of Michigan. This device uses nano-structured quantum dots that emit light in the near-infrared (IR) region. The nanostructured quantum dots are used as a source and excite fluorochrome polymers coupled with antibodies that seek out and attach to specific bacteria and viruses. The fluorochrome polymers/antibodies fluoresce at specific wavelengths in the near-IR spectrum, but these wavelengths are offset from the excitation wavelength and can be detected with a tunable spectrometer. The device will be used to detect the presence of viruses and bacteria in simple fluids and eventually in more complex fluids, such as blood. Current state-of-the-art devices are limited to single bacteria or virus detection and a considerable amount of time and effort is required to prepare samples for analysis. Most importantly, the devices are quite large and cumbersome, which prohibits them from being used on the International Space Station and the space shuttles. This novel device uses nanostructured quantum dots which, through molecular beam epitaxy and highly selective annealing processes, can be developed into an illumination source that could potentially generate hundreds of specific wavelengths. As a result, this device will be able to excite hundreds of antibody/fluorochrome polymer combinations, which in turn could be used to detect hundreds of bacteria

Highly Reproducible Automated Proteomics Sample Preparation Workflow for Quantitative Mass Spectrometry.

Science.gov (United States)

Fu, Qin; Kowalski, Michael P; Mastali, Mitra; Parker, Sarah J; Sobhani, Kimia; van den Broek, Irene; Hunter, Christie L; Van Eyk, Jennifer E

2018-01-05

Sample preparation for protein quantification by mass spectrometry requires multiple processing steps including denaturation, reduction, alkylation, protease digestion, and peptide cleanup. Scaling these procedures for the analysis of numerous complex biological samples can be tedious and time-consuming, as there are many liquid transfer steps and timed reactions where technical variations can be introduced and propagated. We established an automated sample preparation workflow with a total processing time for 96 samples of 5 h, including a 2 h incubation with trypsin. Peptide cleanup is accomplished by online diversion during the LC/MS/MS analysis. In a selected reaction monitoring (SRM) assay targeting 6 plasma biomarkers and spiked β-galactosidase, mean intraday and interday cyclic voltammograms (CVs) for 5 serum and 5 plasma samples over 5 days were samples repeated on 3 separate days had total CVs below 20%. Similar results were obtained when the workflow was transferred to a second site: 93% of peptides had CVs below 20%. An automated trypsin digestion workflow yields uniformly processed samples in less than 5 h. Reproducible quantification of peptides was observed across replicates, days, instruments, and laboratory sites, demonstrating the broad applicability of this approach.

An unattended device for high-voltage sampling and passive measurement of thoron decay products

Energy Technology Data Exchange (ETDEWEB)

Gierl, Stefanie; Meisenberg, Oliver, E-mail: oliver.meisenberg@helmholtz-muenchen.de; Wielunski, Marek; Tschiersch, Jochen [Helmholtz Zentrum München, German Research Center for Environmental Health, Institute of Radiation Protection, Ingolstädter Landstr. 1, 85764 Neuherberg (Germany); Haninger, Thomas [Helmholtz Zentrum München, German Research Center for Environmental Health, Auswertungsstelle für Strahlendosimeter, Otto-Hahn-Ring 6, 81739 München (Germany)

2014-02-15

An integrating measurement device for the concentration of airborne thoron decay products was designed and calibrated. It is suitable for unattended use over up to several months also in inhabited dwellings. The device consists of a hemispheric capacitor with a wire mesh as the outer electrode on ground potential and the sampling substrates as the inner electrode on +7.0 kV. Negatively charged and neutral thoron decay products are accelerated to and deposited on the sampling substrates. As sampling substrates, CR39 solid-state nuclear track detectors are used in order to record the alpha decay of the sampled decay products. Nuclide discrimination is achieved by covering the detectors with aluminum foil of different thickness, which are penetrated only by alpha particles with sufficient energy. Devices of this type were calibrated against working level monitors in a thoron experimental house. The sensitivity was measured as 9.2 tracks per Bq/m{sup 3} × d of thoron decay products. The devices were used over 8 weeks in several houses built of earthen material in southern Germany, where equilibrium equivalent concentrations of 1.4–9.9 Bq/m{sup 3} of thoron decay products were measured.

Ionic liquids: solvents and sorbents in sample preparation.

Science.gov (United States)

Clark, Kevin D; Emaus, Miranda N; Varona, Marcelino; Bowers, Ashley N; Anderson, Jared L

2018-01-01

The applications of ionic liquids (ILs) and IL-derived sorbents are rapidly expanding. By careful selection of the cation and anion components, the physicochemical properties of ILs can be altered to meet the requirements of specific applications. Reports of IL solvents possessing high selectivity for specific analytes are numerous and continue to motivate the development of new IL-based sample preparation methods that are faster, more selective, and environmentally benign compared to conventional organic solvents. The advantages of ILs have also been exploited in solid/polymer formats in which ordinarily nonspecific sorbents are functionalized with IL moieties in order to impart selectivity for an analyte or analyte class. Furthermore, new ILs that incorporate a paramagnetic component into the IL structure, known as magnetic ionic liquids (MILs), have emerged as useful solvents for bioanalytical applications. In this rapidly changing field, this Review focuses on the applications of ILs and IL-based sorbents in sample preparation with a special emphasis on liquid phase extraction techniques using ILs and MILs, IL-based solid-phase extraction, ILs in mass spectrometry, and biological applications. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Development of a sample preparation system for AMS radiocarbon dating at CRICH, Korea

Energy Technology Data Exchange (ETDEWEB)

Kim, Myung-Jin; Lee, Byeong-Cheol; Lim, Eun-Soo [Cultural Research Institute of Chungcheong Heritage, Gongju (Korea, Republic of); Hong, Duk-Geun [Kangwon National University, Chuncheon (Korea, Republic of); Park, Soon-Bal [Chungnam National University, Daejeon (Korea, Republic of); Youn, Min-Young [Seoul National University, Seoul (Korea, Republic of)

2010-01-15

We developed a sample preparation system for radiocarbon dating by using AMS measurement at Cultural Research Institute of Chungcheong Heritage, Korea. From the investigation of the reduction process, the optimum graphitization temperature was chosen as 625 .deg. C. Using Aldrich graphite powder of 0.75 {+-} 0.023 pMC, the background value of our preparation system was controlled at a low level. The robustness against chemical treatment and contamination was also observed from samples of Oxalic acid II and IAEA-C4. The resultant values, 134.04 {+-} 0.99 pMC and 0.38 {+-} 0.043 pMC, were in good agreement with the consensus values. Based on comparison, our conventional ages agreed very well with those of Beta Analytic Co. and SNU-AMS. No memory effect existed in the preparation system. Therefore, we concluded that the sample preparation system was operated in a stable manner and that the basic radiocarbon dating procedures were completely verified.

TCLP Preparation and Analysis of K East Basin Composite Sludge Samples

International Nuclear Information System (INIS)

Silvers, K.L.; Wagner, J.J.; Steele, R.T.

2000-01-01

Sludge samples from the Hanford K East Basin were analyzed by the Toxicity Characterization Leaching Procedure (TCLP) to assist in the appropriate Resource Conservation and Recovery Act (RCIL4) designation of this material. Sludge samples were collected by Fluor Hanford, Inc. using the consolidated sludge sampling system (system that allows collection of a single sample from multiple sample locations). These samples were shipped to the Postirradiation Testing Laboratory (PTL, 327 Building) and then transferred to the Pacific Northwest National Laboratory (PNNL) Radiochemical Processing Laboratory (RPL, 325 Building) for recovery and testing. Two sludge composites were prepared, using the consolidated sludge samples, to represent K East canister sludge (sample KC Can Comp) and K East floor sludge (sample KC Floor Comp). Each composite was extracted in duplicate and analyzed in duplicate following pre-approved(a) TCLP extraction and analyses procedures. In addition, these samples and duplicates were analyzed for total RCRA metals (via acid digestion preparation). The work was conducted in accordance with the requirements of the Hanford Analytical Quality Assurance Requirements Document (HASQARD). A PNNL Quality Assurance Program compliant with J HASQARD was implemented for this effort. The results from the TCLP analyses showed that all RCRA metal concentrations were less than the TCLP limits for both the canister and floor composite samples and their respective duplicates

Capacitive deionization on-chip as a method for microfluidic sample preparation

NARCIS (Netherlands)

Roelofs, Susan Helena; Kim, Bumjoo; Eijkel, Jan C.T.; Han, Jongyoon; van den Berg, Albert; Odijk, Mathieu

2015-01-01

Desalination as a sample preparation step is essential for noise reduction and reproducibility of mass spectrometry measurements. A specific example is the analysis of proteins for medical research and clinical applications. Salts and buffers that are present in samples need to be removed before

Study of measurement of the alcohol biomarker phosphatidylethanol (PEth) in dried blood spot (DBS) samples and application of a volumetric DBS device.

Science.gov (United States)

Beck, Olof; Kenan Modén, Naama; Seferaj, Sabina; Lenk, Gabriel; Helander, Anders

2018-04-01

Phosphatidylethanol (PEth) is a group of phospholipids formed in cell membranes following alcohol consumption. PEth measurement in whole blood samples is established as a specific alcohol biomarker with clinical and medico-legal applications. This study further evaluated the usefulness of dried blood spot (DBS) samples collected on filter paper for PEth measurement. Specimens used were surplus volumes of venous whole blood sent for routine LC-MS/MS quantification of PEth 16:0/18:1, the major PEth homolog. DBS samples were prepared by pipetting blood on Whatman 903 Protein Saver Cards and onto a volumetric DBS device (Capitainer). The imprecision (CV) of the DBS sample amount based on area and weight measurements of spot punches were 23-28%. Investigation of the relationship between blood hematocrit and PEth concentration yielded a linear, positive correlation, and at around 1.0-1.5μmol/L PEth 16:0/18:1, the PEth concentration increased by ~0.1μmol/L for every 5% increase in hematocrit. There was a close agreement between the PEth concentrations obtained with whole blood samples and the corresponding results using Whatman 903 (PEth DBS =1.026 PEth WB +0.013) and volumetric device (PEth DBS =1.045 PEth WB +0.016) DBS samples. The CV of PEth quantification in DBS samples at concentrations≥0.05μmol/L were ≤15%. The present results further confirmed the usefulness of DBS samples for PEth measurement. Copyright © 2018 Elsevier B.V. All rights reserved.

LC-MS analysis of the plasma metabolome–a novel sample preparation strategy

DEFF Research Database (Denmark)

Skov, Kasper; Hadrup, Niels; Smedsgaard, Jørn

2015-01-01

Blood plasma is a well-known body fluid often analyzed in studies on the effects of toxic compounds as physiological or chemical induced changes in the mammalian body are reflected in the plasma metabolome. Sample preparation prior to LC-MS based analysis of the plasma metabolome is a challenge...... as plasma contains compounds with very different properties. Besides, proteins, which usually are precipitated with organic solvent, phospholipids, are known to cause ion suppression in electrospray mass spectrometry. We have compared two different sample preparation techniques prior to LC-qTOF analysis...... of plasma samples: The first is protein precipitation; the second is protein precipitation followed by solid phase extraction with sub-fractionation into three sub-samples; a phospholipid, a lipid and a polar sub-fraction. Molecular feature extraction of the data files from LC-qTOF analysis of the samples...

Use of passive sampling devices to determine soil contaminant concentrations

Energy Technology Data Exchange (ETDEWEB)

Johnson, K.A. [Clemson Univ., Pendleton, SC (United States)]|[Washington State Univ., Richland, WA (United States); Hooper, M.J. [Clemson Univ., Pendleton, SC (United States); Weisskopf, C.P. [Washington State Univ., Richland, WA (United States)

1996-12-31

The effective remediation of contaminated sites requires accurate identification of chemical distributions. A rapid sampling method using passive sampling devices (PSDs) can provide a thorough site assessment. We have been pursuing their application in terrestrial systems and have found that they increase the ease and speed of analysis, decrease solvent usage and overall cost, and minimize the transport of contaminated soils. Time and cost savings allow a higher sampling frequency than is generally the case using traditional methods. PSDs have been used in the field in soils of varying physical properties and have been successful in estimating soil concentrations ranging from 1 {mu}g/kg (parts per billion) to greater than 200 mg/kg (parts per million). They were also helpful in identifying hot spots within the sites. Passive sampling devices show extreme promise as an analytical tool to rapidly characterize contaminant distributions in soil. There are substantial time and cost savings in laboratory personnel and supplies. By selectively excluding common interferences that require sample cleanup, PSDs can be retrieved from the field and processed rapidly (one technician can process approximately 90 PSDs in an 8-h work day). The results of our studies indicate that PSDs can be used to accurately estimate soil contaminant concentrations and provide lower detection limits. Further, time and cost savings will allow a more thorough and detailed characterization of contaminant distributions. 13 refs., 4 figs., 2 tabs.

[Sample preparation methods for chromatographic analysis of organic components in atmospheric particulate matter].

Science.gov (United States)

Hao, Liang; Wu, Dapeng; Guan, Yafeng

2014-09-01

The determination of organic composition in atmospheric particulate matter (PM) is of great importance in understanding how PM affects human health, environment, climate, and ecosystem. Organic components are also the scientific basis for emission source tracking, PM regulation and risk management. Therefore, the molecular characterization of the organic fraction of PM has become one of the priority research issues in the field of environmental analysis. Due to the extreme complexity of PM samples, chromatographic methods have been the chief selection. The common procedure for the analysis of organic components in PM includes several steps: sample collection on the fiber filters, sample preparation (transform the sample into a form suitable for chromatographic analysis), analysis by chromatographic methods. Among these steps, the sample preparation methods will largely determine the throughput and the data quality. Solvent extraction methods followed by sample pretreatment (e. g. pre-separation, derivatization, pre-concentration) have long been used for PM sample analysis, and thermal desorption methods have also mainly focused on the non-polar organic component analysis in PM. In this paper, the sample preparation methods prior to chromatographic analysis of organic components in PM are reviewed comprehensively, and the corresponding merits and limitations of each method are also briefly discussed.

A review of sample preparation and its influence on pH determination in concrete samples

Directory of Open Access Journals (Sweden)

S. Manso

2017-01-01

Full Text Available If we are to monitor the chemical processes in cementitious materials, then pH assays in the pore solutions of cement pastes, mortars, and concretes are of key importance. However, there is no standard method that regulates the sample-preparation method for pH determination. The state-of-the-art of different methods for pH determination in cementitious materials is presented in this paper and the influence of sample preparation in each case. Moreover, an experimental campaign compares three different techniques for pH determination. Its results contribute to establishing a basic criterion to help researchers select the most suitable method, depending on the purpose of the research. A simple tool is described for selecting the easiest and the most economic pH determination method, depending on the objective; especially for researchers and those with limited experience in this field.

A developed wedge fixtures assisted high precision TEM samples pre-thinning method: Towards the batch lamella preparation

Directory of Open Access Journals (Sweden)

Dandan Wang

2017-04-01

Full Text Available Ion milling, wedge cutting or polishing, and focused ion beam (FIB milling are widely-used techniques for the transmission electron microscope (TEM sample preparation. Especially, the FIB milling provides a site-specific analysis, deposition, and ablation of materials in the micrometer and nanometer scale. However, the cost of FIB tools has been always a significant concern. Since it is inevitable to use the FIB technique, the improvement of efficiency is a key point. Traditional TEM sample preparation with FIB was routinely implemented on a single sample each time. Aiming at cost efficiency, a new pre-thinning technique for batch sample preparation was developed in this paper. The present proposal combines the sample preparation techniques with multi-samples thinning, cross-section scanning electron microscopy (SEM, wedge cutting, FIB and other sample pre-thinning techniques. The new pre-thinning technique is to prepare an edge TEM sample on a grinding and polishing fixture with a slant surface. The thickness of the wedges sample can be measured to 1∼2 μm under optical microscope. Therefore, this fixture is superior to the traditional optical method of estimating the membrane thickness. Moreover, by utilizing a multi-sample holding fixture, more samples can be pre-thinned simultaneously, which significantly improved the productivity of TEM sample preparation.

Experience-Sampling Methodology with a Mobile Device in Fibromyalgia

Directory of Open Access Journals (Sweden)

Castilla Diana

2012-01-01

Full Text Available This work describes the usability studies conducted in the development of an experience-sampling methodology (ESM system running in a mobile device. The goal of the system is to improve the accuracy and ecology in gathering daily self-report data in individuals suffering a chronic pain condition, fibromyalgia. The usability studies showed that the developed software to conduct ESM with mobile devices (smartphones, cell phones can be successfully used by individuals with fibromyalgia of different ages and with low level of expertise in the use of information and communication technologies. 100% of users completed the tasks successfully, although some have completely illiterate. Also there seems to be a clear difference in the way of interaction obtained in the two studies carried out.

Preparation and characterization of Sb2Se3 devices for memory applications

Science.gov (United States)

Shylashree, N.; Uma B., V.; Dhanush, S.; Abachi, Sagar; Nisarga, A.; Aashith, K.; Sangeetha B., G.

2018-05-01

In this paper, A phase change material of Sb2Se3 was proposed for non volatile memory application. The thin film device preparation and characterization were carried out. The deposition method used was vapor evaporation technique and a thickness of 180nm was deposited. The switching between the SET and RESET state is shown by the I-V characterization. The change of phase was studied using R-V characterization. Different fundamental modes were also identified using Raman spectroscopy.

Automated injection of a radioactive sample for preparative HPLC with feedback control

International Nuclear Information System (INIS)

Iwata, Ren; Yamazaki, Shigeki

1990-01-01

The injection of a radioactive reaction mixture into a preparative HPLC column has been automated with computer control for rapid purification of routinely prepared positron emitting radiopharmaceuticals. Using pneumatic valves, a motor-driven pump and a liquid level sensor, two intelligent injection methods for the automation were compared with regard to efficient and rapid sample loading into a 2 mL loop of the 6-way valve. One, a precise but rather slow method, was demonstrated to be suitable for purification of 18 F-radiopharmaceuticals, while the other, due to its rapid operation, was more suitable for 11 C-radiopharmaceuticals. A sample volume of approx 0.5 mL can be injected onto a preparative HPLC column with over 90% efficiency with the present automated system. (author)

Design of sample analysis device for iodine adsorption efficiency test in NPPs

International Nuclear Information System (INIS)

Ji Jinnan

2015-01-01

In nuclear power plants, iodine adsorption efficiency test is used to check the iodine adsorption efficiency of the iodine adsorber. The iodine adsorption efficiency can be calculated through the analysis of the test sample, and thus to determine if the performance of the adsorber meets the requirement on the equipment operation and emission. Considering the process of test and actual demand, in this paper, a special device for the analysis of this kind of test sample is designed. The application shows that the device is with convenient operation and high reliability and accurate calculation, and improves the experiment efficiency and reduces the experiment risk. (author)

Sample preparation and fractionation for proteome analysis and cancer biomarker discovery by mass spectrometry.

Science.gov (United States)

Ahmed, Farid E

2009-03-01

Sample preparation and fractionation technologies are one of the most crucial processes in proteomic analysis and biomarker discovery in solubilized samples. Chromatographic or electrophoretic proteomic technologies are also available for separation of cellular protein components. There are, however, considerable limitations in currently available proteomic technologies as none of them allows for the analysis of the entire proteome in a simple step because of the large number of peptides, and because of the wide concentration dynamic range of the proteome in clinical blood samples. The results of any undertaken experiment depend on the condition of the starting material. Therefore, proper experimental design and pertinent sample preparation is essential to obtain meaningful results, particularly in comparative clinical proteomics in which one is looking for minor differences between experimental (diseased) and control (nondiseased) samples. This review discusses problems associated with general and specialized strategies of sample preparation and fractionation, dealing with samples that are solution or suspension, in a frozen tissue state, or formalin-preserved tissue archival samples, and illustrates how sample processing might influence detection with mass spectrometric techniques. Strategies that dramatically improve the potential for cancer biomarker discovery in minimally invasive, blood-collected human samples are also presented.

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

Energy Technology Data Exchange (ETDEWEB)

Adamic, M.L., E-mail: Mary.Adamic@inl.gov [Idaho National Laboratory, P.O. Box 1625, Idaho Falls, ID 83402 (United States); Lister, T.E.; Dufek, E.J.; Jenson, D.D.; Olson, J.E. [Idaho National Laboratory, P.O. Box 1625, Idaho Falls, ID 83402 (United States); Vockenhuber, C. [Laboratory of Ion Beam Physics, ETH Zurich, Otto-Stern-Weg 5, 8093 Zurich (Switzerland); Watrous, M.G. [Idaho National Laboratory, P.O. Box 1625, Idaho Falls, ID 83402 (United States)

2015-10-15

This paper presents an evaluation of an alternate method for preparing environmental samples for {sup 129}I 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. Precipitated silver iodide samples are usually mixed with niobium or silver powder 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.

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

International Nuclear Information System (INIS)

Adamic, M.L.; Lister, T.E.; Dufek, E.J.; Jenson, D.D.; Olson, J.E.; Vockenhuber, C.; Watrous, M.G.

2015-01-01

This paper presents an evaluation of an alternate method for preparing environmental samples for "1"2"9I 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. Precipitated silver iodide samples are usually mixed with niobium or silver powder 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.

A high-throughput sample preparation method for cellular proteomics using 96-well filter plates.

Science.gov (United States)

Switzar, Linda; van Angeren, Jordy; Pinkse, Martijn; Kool, Jeroen; Niessen, Wilfried M A

2013-10-01

A high-throughput sample preparation protocol based on the use of 96-well molecular weight cutoff (MWCO) filter plates was developed for shotgun proteomics of cell lysates. All sample preparation steps, including cell lysis, buffer exchange, protein denaturation, reduction, alkylation and proteolytic digestion are performed in a 96-well plate format, making the platform extremely well suited for processing large numbers of samples and directly compatible with functional assays for cellular proteomics. In addition, the usage of a single plate for all sample preparation steps following cell lysis reduces potential samples losses and allows for automation. The MWCO filter also enables sample concentration, thereby increasing the overall sensitivity, and implementation of washing steps involving organic solvents, for example, to remove cell membranes constituents. The optimized protocol allowed for higher throughput with improved sensitivity in terms of the number of identified cellular proteins when compared to an established protocol employing gel-filtration columns. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Simple-to-prepare multipoint field emitter

Science.gov (United States)

Sominskii, G. G.; Taradaev, E. P.; Tumareva, T. A.; Mishin, M. V.; Kornishin, S. Yu.

2015-07-01

We investigate multitip field emitters prepared by electroerosion treatment of the surface of molybdenum samples. Their characteristics are determined for operation with a protecting activated fullerene coating. Our experiments indicate that such cathodes are promising for high-voltage electron devices operating in technical vacuum.

Review of sample preparation techniques for the analysis of pesticide residues in soil.

Science.gov (United States)

Tadeo, José L; Pérez, Rosa Ana; Albero, Beatriz; García-Valcárcel, Ana I; Sánchez-Brunete, Consuelo

2012-01-01

This paper reviews the sample preparation techniques used for the analysis of pesticides in soil. The present status and recent advances made during the last 5 years in these methods are discussed. The analysis of pesticide residues in soil requires the extraction of analytes from this matrix, followed by a cleanup procedure, when necessary, prior to their instrumental determination. The optimization of sample preparation is a very important part of the method development that can reduce the analysis time, the amount of solvent, and the size of samples. This review considers all aspects of sample preparation, including extraction and cleanup. Classical extraction techniques, such as shaking, Soxhlet, and ultrasonic-assisted extraction, and modern techniques like pressurized liquid extraction, microwave-assisted extraction, solid-phase microextraction and QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) are reviewed. The different cleanup strategies applied for the purification of soil extracts are also discussed. In addition, the application of these techniques to environmental studies is considered.

Ergonomic analysis of radiopharmaceuticals samples preparation process

International Nuclear Information System (INIS)

Gomes, Luciene Betzler C.; Santos, Isaac Luquetti dos; Fonseca, Antonio Carlos C. da; Pellini, Marcos Pinto; Rebelo, Ana Maria

2005-01-01

The doses of radioisotopes to be administrated in patients for diagnostic effect or therapy are prepared in the radiopharmacological sector. The preparation process adopts techniques that are aimed to reduce the exposition time of the professionals and the absorption of excessive doses for patients. The ergonomic analysis of this process contributes in the prevention of occupational illnesses and to prevent risks of accidents during the routines, providing welfare and security to the involved users and conferring to the process an adequate working standard. In this context it is perceived relevance of studies that deal with the analysis of factors that point with respect to the solution of problems and for establishing proposals that minimize risks in the exercise of the activities. Through a methodology that considers the application of the concepts of Ergonomics, it is searched the improvement of the effectiveness or the quality and reduction of the difficulties lived for the workers. The work prescribed, established through norms and procedures codified will be faced with the work effectively carried through, the real work, shaped to break the correct appreciation, with focus in the activities. This work has as objective to argue an ergonomic analysis of samples preparation process of radioisotopes in the Setor de Radiofarmacia do Hospital Universitario Clementino Fraga Filho da Universidade Federal do Rio de Janeiro (UFRJ). (author)

Improved sample preparation and counting techniques for enhanced tritium measurement sensitivity

Science.gov (United States)

Moran, J.; Aalseth, C.; Bailey, V. L.; Mace, E. K.; Overman, C.; Seifert, A.; Wilcox Freeburg, E. D.

2015-12-01

Tritium (T) measurements offer insight to a wealth of environmental applications including hydrologic tracking, discerning ocean circulation patterns, and aging ice formations. However, the relatively short half-life of T (12.3 years) limits its effective age dating range. Compounding this limitation is the decrease in atmospheric T content by over two orders of magnitude (from 1000-2000 TU in 1962 to testing in the 1960's. We are developing sample preparation methods coupled to direct counting of T via ultra-low background proportional counters which, when combined, offer improved T measurement sensitivity (~4.5 mmoles of H2 equivalent) and will help expand the application of T age dating to smaller sample sizes linked to persistent environmental questions despite the limitations above. For instance, this approach can be used to T date ~ 2.2 mmoles of CH4 collected from sample-limited systems including microbial communities, soils, or subsurface aquifers and can be combined with radiocarbon dating to distinguish the methane's formation age from C age in a system. This approach can also expand investigations into soil organic C where the improved sensitivity will permit resolution of soil C into more descriptive fractions and provide direct assessments of the stability of specific classes of organic matter in soils environments. We are employing a multiple step sample preparation system whereby organic samples are first combusted with resulting CO2 and H2O being used as a feedstock to synthesize CH4. This CH4 is mixed with Ar and loaded directly into an ultra-low background proportional counter for measurement of T β decay in a shallow underground laboratory. Analysis of water samples requires only the addition of geologic CO2 feedstock with the sample for methane synthesis. The chemical nature of the preparation techniques enable high sample throughput with only the final measurement requiring T decay with total sample analysis time ranging from 2 -5 weeks

Preparation and application of radioactive soil samples for intercomparison

International Nuclear Information System (INIS)

Gao Zequan; Li Zhou; Li Pengxiang; Wang Ruijun; Ren Xiaona

2014-01-01

This article summarized the preparation process and intercomparison results of the simulated environmental radioactive soil samples. The components of the matrix were: SiO 2 , Al 2 O 3 , Fe 2 O 3 , MgO, CaO, NaCl, KCl and TiO 2 . All of the components were milled, oven-dried, sieved and then blended together. The homogeneity test was according to GB 15000. 5-1994, and no significant differences were observed. The 3 H analysis soils were spiked natural soils with the moisture content of 15%. Eight laboratories attended this intercomparison. The results proves that the preparation of the simulated soils were suitable for the inter-laboratories comparison. (authors)

Preparation of rock samples for measurement of the thermal neutron macroscopic absorption cross-section

International Nuclear Information System (INIS)

Czubek, J.A.; Burda, J.; Drozdowicz, K.; Igielski, A.; Kowalik, W.; Krynicka-Drozdowicz, E.; Woznicka, U.

1986-03-01

Preparation of rock samples for the measurement of the thermal neutron macroscopic absorption cross-section in small cylindrical two-region systems by a pulsed technique is presented. Requirements which should be fulfilled during the preparation of the samples due to physical assumptions of the method are given. A cylindrical vessel is filled with crushed rock and saturated with a medium strongly absorbing thermal neutrons. Water solutions of boric acid of well-known macroscopic absorption cross-section are used. Mass contributions of the components in the sample are specified. This is necessary for the calculation of the thermal neutron macroscopic absorption cross-section of the rock matrix. The conditions necessary for assuring the required accuracy of the measurement are given and the detailed procedure of preparation of the rock sample is described. (author)

Should the mass of a nanoferrite sample prepared by autocombustion method be considered as a realistic preparation parameter?

Energy Technology Data Exchange (ETDEWEB)

Wahba, Adel Maher, E-mail: adel.mousa@f-eng.tanta.edu.eg [Department of Engineering Physics and Mathematics, Faculty of Engineering, Tanta University (Egypt); Mohamed, Mohamed Bakr [Ain shams University, Faculty of Science, Physics Department, Cairo (Egypt)

2017-02-15

Detectable variations in structural, elastic and magnetic properties have been reported depending on the mass of the cobalt nanoferrite sample prepared by citrate autocombustion method. Heat released during the autocombustion process and its duration are directly proportional to the mass to be prepared, and is thus expected to affect both the crystallite size and the cation distribution giving rise to the reported variations in microstrain, magnetization, and coercivity. Formation of a pure spinel phase has been validated using X-ray diffraction patterns (XRD) and Fourier-transform infrared (FTIR) spectra. Crystallite sizes obtained from Williamson-Hall (W-H) method range from 28–87 nm, being further supported by images of high-resolution transmission electron microscope (HRTEM). Saturation magnetization and coercivity deduced from M-H hysteresis loops show a clear correlation with the cation distribution, which was proposed on the basis of experimentally obtained data of XRD, VSM, and IR. Elastic parameters have been estimated using the cation distribution and FTIR data, with a resulting trend quite opposite to that of the lattice parameter. - Highlights: • Samples with different masses of CoFe{sub 2}O{sub 4} were prepared by autocombustion method. • XRD and IR data confirmed a pure spinel cubic structure for all samples. • Structural and magnetic properties show detectable changes with the mass prepared. • Cation distribution was suggested from experimental data of XRD, IR, and M-H loops.

Experiences from Refurbishment of Metallography Hot Cells and Application of a New Preparation Concept for Materialography Samples

International Nuclear Information System (INIS)

Oberlander, B. C.; Espeland, M.; Solum, N. O.

2001-01-01

After more than 30 years of operation the lead shielded metallography hot cells needed a basic renewal and modernisation not least of the specimen preparation equipment. Preparation in hot cells of radioactive samples for metallography and ceramography is challenging and time consuming. It demands a special design and quality of all in-cell equipment and skill and patience from the operator. Essentials in the preparation process are: simplicity and reliability of the machines, and a good quality, reproducibility and efficiency in performance. Desirable is process automation, flexibility and an alara amounto of radioactive waste produced per sample prepared. State of the art preparation equipment for materialography seems to meet most of the demands, however, it cannot be used in hot cells without modifications. Therefore. IFE and Struers in Copenhagen modified a standard model of a Strues precision cutting machine and a microprocessor controlled grinding and polishing machine for Hot Cell application. Hot cell utilisation of the microcomputer controlled grinding and polishing machine and the existing automatic dosing equipment made the task of preparing radioactive samples more attractive. The new grinding and polishing system for hot cells provides good sample preparation quality and reproductibility at reduced preparation time and reduced amount of contaminated waste produced per sample prepared. the sample materials examined were irradiated cladding materials and fuels

Radiocarbon accelerator mass spectrometry (AMS) sample preparation laboratory in Brazil

International Nuclear Information System (INIS)

Macario, Kita D.; Gomes, Paulo R. S.; Anjos, Roberto M. dos; Linares, Roberto; Queiroz, Eduardo; Oliveira, Fabiana M. de; Cardozo, Laio; Carvalho, Carla R.A.

2011-01-01

Full text: For decades Accelerator Mass Spectrometry has been widely used for radiocarbon measurements all over the world with application in several fields of science from archaeology to geosciences. This technique provides ultrasensitive analysis of reduced size samples or even specific compounds since sample atoms are accelerated to high energies and measured using nuclear particle detectors. Sample preparation is extremely important for accurate radiocarbon measurement and includes chemical pre-treatment to remove all possible contaminants. For beam extraction in the accelerator ion source, samples are usually converted to graphite. In this work we report a new radiocarbon sample preparation facility installed at the Physics Institute of Universidade Federal Fluminense (UFF), in Brazil. At the Nuclear Chronology Laboratory (LACRON) samples are chemically treated and converted to carbon dioxide by hydrolysis or combustion. A stainless steel based vacuum line was constructed for carbon dioxide separation and graphitization is performed in sealed quartz tubes in a muffle oven. Successful graphite production is important to provide stable beam currents and to minimize isotopic fractionation. Performance tests for graphite production are currently under way and isotopic analysis will soon be possible with the acquisition of a Single Stage AMS System by our group. The Single Stage Accelerator produced by National Electrostatic Corporation is a 250 kV air insulated accelerator especially constructed to measure the amount of 14 C in small modern graphite samples to a precision of 0.3 % or better. With the installation of such equipment in the first half of 2012, UFF will be ready to perform the 14C -AMS technique. (author)

TruSeq Stranded mRNA and Total RNA Sample Preparation Kits

Science.gov (United States)

Total RNA-Seq enabled by ribosomal RNA (rRNA) reduction is compatible with formalin-fixed paraffin embedded (FFPE) samples, which contain potentially critical biological information. The family of TruSeq Stranded Total RNA sample preparation kits provides a unique combination of unmatched data quality for both mRNA and whole-transcriptome analyses, robust interrogation of both standard and low-quality samples and workflows compatible with a wide range of study designs.

Preparation and characterisation of magnetic nanostructured samples for inelastic neutron scattering experiments

Energy Technology Data Exchange (ETDEWEB)

Kreuzpaintner, Wolfgang

2010-06-22

Recent advances in thin-film structuring techniques have generated significant interest in the dynamics of spin waves in magnetic nanostructures and the possible use of inelastic neutron scattering (INS) for their investigation. This thesis describes the design and implementation, at GKSS Research Centre, of equipment for preparation of large and laterally submicron and nanometre structured magnetic samples for such future INS experiments. After a brief resume on spin waves in nanostructures, the development work on new purpose-designed equipment, including high vacuum (HV) argon ion beam milling and ultra high vacuum (UHV) e-beam evaporation setups, is described. Ni nanodot as well as Ni and novel Gd nanowire samples were prepared using combinations of sputter deposition, laser interference lithography, argon ion beam milling, e-beam evaporation and self organisation techniques. With reference to sample preparation, epitaxial growth studies for Ni on Si(100) substrate were performed, resulting in the development of a new deposition process, which by thermal tuning allows for the direct epitaxial growth of Ni on Si with unprecedented crystalline quality. The results of various characterisation experiments on the prepared nanostructured samples, including Scanning Electron Microscopy (SEM), microprobe analysis, Atomic and Magnetic Force Microscopy (AFM/MFM), Vibrating Sample Magnetometry (VSM), X-ray Diffraction (XRD) and Reflectivity (XRR), unpolarised and Polarised Neutron Scattering (PNR) and off-specular scattering by X-rays and neutrons using rocking scans and Time-Of-Flight Grazing Incidence Small Angle Neutron Scattering (TOF-GISANS), together with various analysis procedures such as Distorted-Wave Born Approximation (DWBA), are reported. The analysis of a Gd nanowire sample by TOF-GISANS led to a novel evaluation technique which in comparison with single wavelength methods allows portions of reciprocal space to be scanned without changing the angle of

Preparation and characterisation of magnetic nanostructured samples for inelastic neutron scattering experiments

International Nuclear Information System (INIS)

Kreuzpaintner, Wolfgang

2010-01-01

Recent advances in thin-film structuring techniques have generated significant interest in the dynamics of spin waves in magnetic nanostructures and the possible use of inelastic neutron scattering (INS) for their investigation. This thesis describes the design and implementation, at GKSS Research Centre, of equipment for preparation of large and laterally submicron and nanometre structured magnetic samples for such future INS experiments. After a brief resume on spin waves in nanostructures, the development work on new purpose-designed equipment, including high vacuum (HV) argon ion beam milling and ultra high vacuum (UHV) e-beam evaporation setups, is described. Ni nanodot as well as Ni and novel Gd nanowire samples were prepared using combinations of sputter deposition, laser interference lithography, argon ion beam milling, e-beam evaporation and self organisation techniques. With reference to sample preparation, epitaxial growth studies for Ni on Si(100) substrate were performed, resulting in the development of a new deposition process, which by thermal tuning allows for the direct epitaxial growth of Ni on Si with unprecedented crystalline quality. The results of various characterisation experiments on the prepared nanostructured samples, including Scanning Electron Microscopy (SEM), microprobe analysis, Atomic and Magnetic Force Microscopy (AFM/MFM), Vibrating Sample Magnetometry (VSM), X-ray Diffraction (XRD) and Reflectivity (XRR), unpolarised and Polarised Neutron Scattering (PNR) and off-specular scattering by X-rays and neutrons using rocking scans and Time-Of-Flight Grazing Incidence Small Angle Neutron Scattering (TOF-GISANS), together with various analysis procedures such as Distorted-Wave Born Approximation (DWBA), are reported. The analysis of a Gd nanowire sample by TOF-GISANS led to a novel evaluation technique which in comparison with single wavelength methods allows portions of reciprocal space to be scanned without changing the angle of

Infrared biospectroscopy for a fast qualitative evaluation of sample preparation in metabolomics.

Science.gov (United States)

Kuligowski, Julia; Pérez-Guaita, David; Escobar, Javier; Lliso, Isabel; de la Guardia, Miguel; Lendl, Bernhard; Vento, Máximo; Quintás, Guillermo

2014-09-01

Liquid chromatography-mass spectrometry (LC-MS) has been increasingly used in biomedicine to study the dynamic metabolomic responses of biological systems under different physiological or pathological conditions. To obtain an integrated snapshot of the system, metabolomic methods in biomedicine typically analyze biofluids (e.g. plasma) that require clean-up before being injected into LC-MS systems. However, high resolution LC-MS is costly in terms of resources required for sample and data analysis and care must be taken to prevent chemical (e.g. ion suppression) or statistical artifacts. Because of that, the effect of sample preparation on the metabolomic profile during metabolomic method development is often overlooked. This work combines an Attenuated Total Reflectance-Fourier transform infrared (ATR-FTIR) and a multivariate exploratory data analysis for a cost-effective qualitative evaluation of major changes in sample composition during sample preparation. ATR-FTIR and LC-time of flight mass spectrometry (TOFMS) data from the analysis of a set of plasma samples precipitated using acetonitrile, methanol and acetone performed in parallel were used as a model example. Biochemical information obtained from the analysis of the ATR-FTIR and LC-TOFMS data was thoroughly compared to evaluate the strengths and shortcomings of FTIR biospectroscopy for assessing sample preparation in metabolomics studies. Results obtained show the feasibility of ATR-FTIR for the evaluation of major trends in the plasma composition changes among different sample pretreatments, providing information in terms of e.g., amino acids, proteins, lipids and carbohydrates overall contents comparable to those found by LC-TOFMS. Copyright © 2014 Elsevier B.V. All rights reserved.

Highly oriented Bi-system bulk sample prepared by a decomposition-crystallization process

International Nuclear Information System (INIS)

Xi Zhengping; Zhou Lian; Ji Chunlin

1992-01-01

A decomposition-crystallization method, preparing highly oriented Bi-system bulk sample is reported. The effects of processing parameter, decomposition temperature, cooling rate and post-treatment condition on texture and superconductivity are investigated. The method has successfully prepared highly textured Bi-system bulk samples. High temperature annealing does not destroy the growing texture, but the cooling rate has some effect on texture and superconductivity. Annealing in N 2 /O 2 atmosphere can improve superconductivity of the textured sample. The study on the superconductivity of the Bi(Pb)-Sr-Ca-Cu-O bulk material has been reported in numerous papers. The research on J c concentrates on the tape containing the 2223 phase, with very few studies on the J c of bulk sample. The reason for the lack of studies is that the change of superconducting phases at high temperatures has not been known. The authors have reported that the 2212 phase incongruently melted at about 875 degrees C and proceeded to orient the c-axis perpendicular to the surface in the process of crystallization of the 2212 phase. Based on that result, a decomposition-crystallization method was proposed to prepare highly oriented Bi-system bulk sample. In this paper, the process is described in detail and the effects of processing parameters on texture and superconductivity are reported

X-ray diffraction without sample preparation: Proof-of-principle experiments

International Nuclear Information System (INIS)

Hansford, Graeme M.

2013-01-01

The properties of a novel X-ray diffraction (XRD) technique having very low sensitivity to the sample morphology were previously elucidated through theoretical considerations and model simulations (Hansford, 2011). This technique opens up the possibility of mineralogical analysis by XRD without sample preparation. Here, the results of proof-of-principle experimental tests are presented. Two sets of experiments were performed using a vacuum chamber equipped with an X-ray tube source, sample holder and charge-coupled detector. Firstly, a pressed-powder pellet of α-quartz was placed in three different positions relative to the X-ray source and detector. The changes in position represent gross sample movements which would be inconceivable in conventional XRD analysis. The resulting back-reflection energy-dispersive spectra show a very high degree of correspondence other than an overall intensity factor dependent on the distance between the sample and detector. Secondly, the back-reflection spectrum of an unprepared limestone hand specimen, having mm-scale surface morphology, was compared to the spectrum of a calcite pressed-powder pellet. The correspondence of the diffraction peaks in the spectra demonstrate that the limestone is comprised dominantly of calcite. In both cases, the claims of the earlier paper are fully supported by the results of these experimental tests. -- Highlights: • Proof-of-principle tests of a novel X-ray diffraction (XRD) method were conducted. • Very low sensitivity to sample position and orientation was demonstrated. • Insensitivity to sample morphology is inferred. • A simple analysis of an unprepared limestone hand specimen was performed. • This technique enables mineralogical analysis by XRD without sample preparation

pH adjustment of human blood plasma prior to bioanalytical sample preparation

NARCIS (Netherlands)

Hendriks, G.; Uges, D. R. A.; Franke, J. P.

2008-01-01

pH adjustment in bioanalytical sample preparation concerning ionisable compounds is one of the most common sample treatments. This is often done by mixing an aliquot of the sample with a proper buffer adjusted to the proposed pH. The pH of the resulting mixture however, does not necessarily have to

The role of graphene-based sorbents in modern sample preparation techniques.

Science.gov (United States)

de Toffoli, Ana Lúcia; Maciel, Edvaldo Vasconcelos Soares; Fumes, Bruno Henrique; Lanças, Fernando Mauro

2018-01-01

The application of graphene-based sorbents in sample preparation techniques has increased significantly since 2011. These materials have good physicochemical properties to be used as sorbent and have shown excellent results in different sample preparation techniques. Graphene and its precursor graphene oxide have been considered to be good candidates to improve the extraction and concentration of different classes of target compounds (e.g., parabens, polycyclic aromatic hydrocarbon, pyrethroids, triazines, and so on) present in complex matrices. Its applications have been employed during the analysis of different matrices (e.g., environmental, biological and food). In this review, we highlight the most important characteristics of graphene-based material, their properties, synthesis routes, and the most important applications in both off-line and on-line sample preparation techniques. The discussion of the off-line approaches includes methods derived from conventional solid-phase extraction focusing on the miniaturized magnetic and dispersive modes. The modes of microextraction techniques called stir bar sorptive extraction, solid phase microextraction, and microextraction by packed sorbent are discussed. The on-line approaches focus on the use of graphene-based material mainly in on-line solid phase extraction, its variation called in-tube solid-phase microextraction, and on-line microdialysis systems. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A microfluidic DNA library preparation platform for next-generation sequencing.

Science.gov (United States)

Kim, Hanyoup; Jebrail, Mais J; Sinha, Anupama; Bent, Zachary W; Solberg, Owen D; Williams, Kelly P; Langevin, Stanley A; Renzi, Ronald F; Van De Vreugde, James L; Meagher, Robert J; Schoeniger, Joseph S; Lane, Todd W; Branda, Steven S; Bartsch, Michael S; Patel, Kamlesh D

2013-01-01

Next-generation sequencing (NGS) is emerging as a powerful tool for elucidating genetic information for a wide range of applications. Unfortunately, the surging popularity of NGS has not yet been accompanied by an improvement in automated techniques for preparing formatted sequencing libraries. To address this challenge, we have developed a prototype microfluidic system for preparing sequencer-ready DNA libraries for analysis by Illumina sequencing. Our system combines droplet-based digital microfluidic (DMF) sample handling with peripheral modules to create a fully-integrated, sample-in library-out platform. In this report, we use our automated system to prepare NGS libraries from samples of human and bacterial genomic DNA. E. coli libraries prepared on-device from 5 ng of total DNA yielded excellent sequence coverage over the entire bacterial genome, with >99% alignment to the reference genome, even genome coverage, and good quality scores. Furthermore, we produced a de novo assembly on a previously unsequenced multi-drug resistant Klebsiella pneumoniae strain BAA-2146 (KpnNDM). The new method described here is fast, robust, scalable, and automated. Our device for library preparation will assist in the integration of NGS technology into a wide variety of laboratories, including small research laboratories and clinical laboratories.

A microfluidic DNA library preparation platform for next-generation sequencing.

Directory of Open Access Journals (Sweden)

Hanyoup Kim

Full Text Available Next-generation sequencing (NGS is emerging as a powerful tool for elucidating genetic information for a wide range of applications. Unfortunately, the surging popularity of NGS has not yet been accompanied by an improvement in automated techniques for preparing formatted sequencing libraries. To address this challenge, we have developed a prototype microfluidic system for preparing sequencer-ready DNA libraries for analysis by Illumina sequencing. Our system combines droplet-based digital microfluidic (DMF sample handling with peripheral modules to create a fully-integrated, sample-in library-out platform. In this report, we use our automated system to prepare NGS libraries from samples of human and bacterial genomic DNA. E. coli libraries prepared on-device from 5 ng of total DNA yielded excellent sequence coverage over the entire bacterial genome, with >99% alignment to the reference genome, even genome coverage, and good quality scores. Furthermore, we produced a de novo assembly on a previously unsequenced multi-drug resistant Klebsiella pneumoniae strain BAA-2146 (KpnNDM. The new method described here is fast, robust, scalable, and automated. Our device for library preparation will assist in the integration of NGS technology into a wide variety of laboratories, including small research laboratories and clinical laboratories.

Preparation and validation of gross alpha/beta samples used in EML's quality assessment program

International Nuclear Information System (INIS)

Scarpitta, S.C.

1997-10-01

A set of water and filter samples have been incorporated into the existing Environmental Measurements Laboratory's (EML) Quality Assessment Program (QAP) for gross alpha/beta determinations by participating DOE laboratories. The participating laboratories are evaluated by comparing their results with the EML value. The preferred EML method for measuring water and filter samples, described in this report, uses gas flow proportional counters with 2 in. detectors. Procedures for sample preparation, quality control and instrument calibration are presented. Liquid scintillation (LS) counting is an alternative technique that is suitable for quantifying both the alpha ( 241 Am, 230 Th and 238 Pu) and beta ( 90 Sr/ 90 Y) activity concentrations in the solutions used to prepare the QAP water and air filter samples. Three LS counting techniques (Cerenkov, dual dpm and full spectrum analysis) are compared. These techniques may be used to validate the activity concentrations of each component in the alpha/beta solution before the QAP samples are actually prepared

Sample preparation and characterization of technetium metal

International Nuclear Information System (INIS)

Minato, Kazuo; Serizawa, Hiroyuki; Fukuda, Kousaku; Itoh, Mitsuo

1997-10-01

Technetium-99 is a long-lived fission product with a half-life of about 2.1 x 10 5 years, which decays by β-emission. For the transmutation of 99 Tc, research on solid technetium was started. Technetium metal powder purchased was analyzed by X-ray diffraction, γ-ray spectrometry, and inductively coupled plasma-atomic emission spectrometry and -mass spectrometry. The lattice parameters obtained were agreed with the reported values. The metallic impurity was about 15 ppm, where aluminum and iron contributed mainly. No impurity nuclide with γ-emission was found. Using the technetium metal powder, button-, rod-, and disk-shaped samples of technetium metal were prepared by arc-melting technique. Thermal diffusivity of technetium metal was measured on a disk sample from room temperature to 1173 K by laser flash method. The thermal diffusivity decreased with increasing temperature though it was almost constant above 600 K. (author)

Determination of total alpha activity index in samples of radioactive wastes

International Nuclear Information System (INIS)

Galicia C, F. J.

2015-01-01

This study aimed to develop a methodology of preparation and quantification of samples containing radionuclides beta and/or alpha emitters, to determine the rates of alpha and beta total activity of radioactive waste samples. For this, a device of planchettes preparer was designed, to assist the planchettes preparation in a controlled environment and free of corrosive vapors. Planchettes were prepared in three means: nitrate, carbonate and sulfate, to different mass thickness, natural uranium (alpha and beta emitter) and in case of Sr-90 (beta emitter pure) only in half nitrate; and these planchettes were quantified in an alpha/beta counter, in order to construct the self-absorption curves for alpha and beta particles. These curves are necessary to determine the rate of alpha-beta activity of any sample because they provide the self-absorption correction factor to be applied in calculating the index. Samples with U were prepared with the help of the device of planchettes preparer and subsequently were analyzed in the proportional counter Mpc-100 Pic brand. Samples with Sr-90 were prepared without the device to see if there was a different behavior with respect to obtaining mass thickness. Similarly they were calcined and carried out count in the Mpc-100. To perform the count, first the parameters of counter operating were determined: operating voltages for alpha and beta particles 630 and 1500 V respectively, a count routine was generated where the time and count type were adjusted, and counting efficiencies for alpha and beta particles, with the aid of calibration sources of 210 Po for alphas and 90 Sr for betas. According to the results, the counts per minute will decrease as increasing the mass thickness of the sample (self-absorption curve), adjusting this behavior to an exponential function in all cases studied. The minor self-absorption of alpha and beta particles in the case of U was obtained in sulfate medium. The self-absorption curves of Sr-90 follow the

Comparison of leach results from field and laboratory prepared samples

International Nuclear Information System (INIS)

Oblath, S.B.; Langton, C.A.

1985-01-01

The leach behavior of saltstone prepared in the laboratory agrees well with that from samples mixed in the field using the Littleford mixer. Leach rates of nitrates and cesium from the current reference formulation saltstone were compared. The laboratory samples were prepared using simulated salt solution; those in the field used Tank 50 decontaminated supernate. For both nitrate and cesium, the field and laboratory samples showed nearly identical leach rates for the first 30 to 50 days. For the remaining period of the test, the field samples showed higher leach rates with the maximum difference being less than a factor of three. Ruthenium and antimony were present in the Tank 50 supernate in known amounts. Antimony-125 was observed in the leachate and a fractional leach rate was calculated to be at least a factor of ten less than that of 137 Cs. No 106 Ru was observed in the leachate, and the release rate was not calculated. However, based on the detection limits for the analysis, the ruthenium leach rate must also be at least a factor of ten less than cesium. These data are the first measurements of the leach rates of Ru and Sb from saltstone. The nitrate leach rates for these samples were 5 x 10 -5 grams of nitrate per square cm per day after 100 days for the laboratory samples and after 200 days for the field samples. These values are consistent with the previously measured leach rates for reference formulation saltstone. The relative standard deviation in the leach rate is about 15% for the field samples, which all were produced from one batch of saltstone, and about 35% for the laboratory samples, which came from different batches. These are the first recorded estimates of the error in leach rates for saltstone

A Chip-Capillary Hybrid Device for Automated Transfer of Sample Pre-Separated by Capillary Isoelectric Focusing to Parallel Capillary Gel Electrophoresis for Two-Dimensional Protein Separation

Science.gov (United States)

Lu, Joann J.; Wang, Shili; Li, Guanbin; Wang, Wei; Pu, Qiaosheng; Liu, Shaorong

2012-01-01

In this report, we introduce a chip-capillary hybrid device to integrate capillary isoelectric focusing (CIEF) with parallel capillary sodium dodecyl sulfate – polyacrylamide gel electrophoresis (SDS-PAGE) or capillary gel electrophoresis (CGE) toward automating two-dimensional (2D) protein separations. The hybrid device consists of three chips that are butted together. The middle chip can be moved between two positions to re-route the fluidic paths, which enables the performance of CIEF and injection of proteins partially resolved by CIEF to CGE capillaries for parallel CGE separations in a continuous and automated fashion. Capillaries are attached to the other two chips to facilitate CIEF and CGE separations and to extend the effective lengths of CGE columns. Specifically, we illustrate the working principle of the hybrid device, develop protocols for producing and preparing the hybrid device, and demonstrate the feasibility of using this hybrid device for automated injection of CIEF-separated sample to parallel CGE for 2D protein separations. Potentials and problems associated with the hybrid device are also discussed. PMID:22830584

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

International Nuclear Information System (INIS)

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

2000-01-01

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

Collection and preparation of bottom sediment samples for analysis of radionuclides and trace elements

International Nuclear Information System (INIS)

2003-07-01

The publication is the first in a series of TECDOCs on sampling and sample handling as part of the IAEA support to improve reliability of nuclear analytical techniques (NATs) in Member State laboratories. The purpose of the document is to provide information on the methods for collecting sediments, the equipment used, and the sample preparation techniques for radionuclide and elemental analysis. The most appropriate procedures for defining the strategies and criteria for selecting sampling locations, for sample storage and transportation are also given. Elements of QA/QC and documentation needs for sampling and sediment analysis are discussed. Collection and preparation of stream and river bottom sediments, lake bottom sediments, estuary bottom sediments, and marine (shallow) bottom sediments are covered. The document is intended to be a comprehensive manual for the collection and preparation of bottom sediments as a prerequisite to obtain representative and meaningful results using NATs. Quality assurance and quality control (QA/QC) is emphasized as an important aspect to ensure proper collection, transportation, preservation, and analysis since it forms the basis for interpretation and legislation. Although there are many approaches and methods available for sediment analyses, the scope of the report is limited to sample preparation for (1) analysis of radionuclides (including sediment dating using radionuclides such as Pb-210 and Cs-137) and (2) analysis of trace, minor and major elements using nuclear and related analytical techniques such as NAA, XRF and PIXE

Collection and preparation of bottom sediment samples for analysis of radionuclides and trace elements

Energy Technology Data Exchange (ETDEWEB)

NONE

2003-07-01

The publication is the first in a series of TECDOCs on sampling and sample handling as part of the IAEA support to improve reliability of nuclear analytical techniques (NATs) in Member State laboratories. The purpose of the document is to provide information on the methods for collecting sediments, the equipment used, and the sample preparation techniques for radionuclide and elemental analysis. The most appropriate procedures for defining the strategies and criteria for selecting sampling locations, for sample storage and transportation are also given. Elements of QA/QC and documentation needs for sampling and sediment analysis are discussed. Collection and preparation of stream and river bottom sediments, lake bottom sediments, estuary bottom sediments, and marine (shallow) bottom sediments are covered. The document is intended to be a comprehensive manual for the collection and preparation of bottom sediments as a prerequisite to obtain representative and meaningful results using NATs. Quality assurance and quality control (QA/QC) is emphasized as an important aspect to ensure proper collection, transportation, preservation, and analysis since it forms the basis for interpretation and legislation. Although there are many approaches and methods available for sediment analyses, the scope of the report is limited to sample preparation for (1) analysis of radionuclides (including sediment dating using radionuclides such as Pb-210 and Cs-137) and (2) analysis of trace, minor and major elements using nuclear and related analytical techniques such as NAA, XRF and PIXE.

Rapid immunohistochemical diagnosis of tobacco mosaic virus disease by microwave-assisted plant sample preparation

Science.gov (United States)

Zellnig, Günther; Möstl, Stefan; Zechmann, Bernd

2013-01-01

Immunoelectron microscopy is a powerful method to diagnose viral diseases and to study the distribution of the viral agent within plant cells and tissues. Nevertheless, current protocols for the immunological detection of viral diseases with transmission electron microscopy (TEM) in plants take between 3 and 6 days and are therefore not suited for rapid diagnosis of virus diseases in plants. In this study, we describe a method that allows rapid cytohistochemical detection of tobacco mosaic virus (TMV) in leaves of tobacco plants. With the help of microwave irradiation, sample preparation of the leaves was reduced to 90 min. After sample sectioning, virus particles were stained on the sections by immunogold labelling of the viral coat protein, which took 100 min. After investigation with the TEM, a clear visualization of TMV in tobacco cells was achieved altogether in about half a day. Comparison of gold particle density by image analysis revealed that samples prepared with the help of microwave irradiation yielded significantly higher gold particle density as samples prepared conventionally at room temperature. This study clearly demonstrates that microwave-assisted plant sample preparation in combination with cytohistochemical localization of viral coat protein is well suited for rapid diagnosis of plant virus diseases in altogether about half a day by TEM. PMID:23580761

Protocols for the analytical characterization of therapeutic monoclonal antibodies. II - Enzymatic and chemical sample preparation.

Science.gov (United States)

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.

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

Energy Technology Data Exchange (ETDEWEB)

Gagnon, Alan R. E-mail: agagnon@whoi.edu; McNichol, Ann P.; Donoghue, Joanne C.; Stuart, Dana R.; Reden, Karl von

2000-10-01

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

Sample preparation method for induced mutation on orchid

International Nuclear Information System (INIS)

Suhaimi Musa; Sakinah Ariffin

2005-01-01

Studies on the induction of mutation in Dendrobium orchid at MINT has produced a number of new orchid mutant cultivars. Tissue culture techniques on orchid seeds and meristem cloning are employed in preparing the samples for the mutation induction. Solid medium based on the Murashige and Skoog (1962) and liquid medium based on Vacin and Went (1949) were found to be suitable in producing protocorm like bodies (PLBs) that are required for the irradiation treatment. (Author)

[Standard sample preparation method for quick determination of trace elements in plastic].

Science.gov (United States)

Yao, Wen-Qing; Zong, Rui-Long; Zhu, Yong-Fa

2011-08-01

Reference sample was prepared by masterbatch method, containing heavy metals with known concentration of electronic information products (plastic), the repeatability and precision were determined, and reference sample preparation procedures were established. X-Ray fluorescence spectroscopy (XRF) analysis method was used to determine the repeatability and uncertainty in the analysis of the sample of heavy metals and bromine element. The working curve and the metrical methods for the reference sample were carried out. The results showed that the use of the method in the 200-2000 mg x kg(-1) concentration range for Hg, Pb, Cr and Br elements, and in the 20-200 mg x kg(-1) range for Cd elements, exhibited a very good linear relationship, and the repeatability of analysis methods for six times is good. In testing the circuit board ICB288G and ICB288 from the Mitsubishi Heavy Industry Company, results agreed with the recommended values.

Cytotoxicity of Light-Cured Dental Materials according to Different Sample Preparation Methods

Directory of Open Access Journals (Sweden)

Myung-Jin Lee

2017-03-01

Full Text Available Dental light-cured resins can undergo different degrees of polymerization when applied in vivo. When polymerization is incomplete, toxic monomers may be released into the oral cavity. The present study assessed the cytotoxicity of different materials, using sample preparation methods that mirror clinical conditions. Composite and bonding resins were used and divided into four groups according to sample preparation method: uncured; directly cured samples, which were cured after being placed on solidified agar; post-cured samples were polymerized before being placed on agar; and “removed unreacted layer” samples had their oxygen-inhibition layer removed after polymerization. Cytotoxicity was evaluated using an agar diffusion test, MTT assay, and confocal microscopy. Uncured samples were the most cytotoxic, while removed unreacted layer samples were the least cytotoxic (p < 0.05. In the MTT assay, cell viability increased significantly in every group as the concentration of the extracts decreased (p < 0.05. Extracts from post-cured and removed unreacted layer samples of bonding resin were less toxic than post-cured and removed unreacted layer samples of composite resin. Removal of the oxygen-inhibition layer resulted in the lowest cytotoxicity. Clinicians should remove unreacted monomers on the resin surface immediately after restoring teeth with light-curing resin to improve the restoration biocompatibility.

Sample preparation prior to the LC-MS-based metabolomics/metabonomics of blood-derived samples.

Science.gov (United States)

Gika, Helen; Theodoridis, Georgios

2011-07-01

Blood represents a very important biological fluid and has been the target of continuous and extensive research for diagnostic, or health and drug monitoring reasons. Recently, metabonomics/metabolomics have emerged as a new and promising 'omics' platform that shows potential in biomarker discovery, especially in areas such as disease diagnosis, assessment of drug efficacy or toxicity. Blood is collected in various establishments in conditions that are not standardized. Next, the samples are prepared and analyzed using different methodologies or tools. When targeted analysis of key molecules (e.g., a drug or its metabolite[s]) is the aim, enforcement of certain measures or additional analyses may correct and harmonize these discrepancies. In omics fields such as those performed by holistic analytical approaches, no such rules or tools are available. As a result, comparison or correlation of results or data fusion becomes impractical. However, it becomes evident that such obstacles should be overcome in the near future to allow for large-scale studies that involve the assaying of samples from hundreds of individuals. In this case the effect of sample handling and preparation becomes very serious, in order to avoid wasting months of work from experts and expensive instrument time. The present review aims to cover the different methodologies applied to the pretreatment of blood prior to LC-MS metabolomic/metabonomic studies. The article tries to critically compare the methods and highlight issues that need to be addressed.

Recent advances in sample preparation techniques and methods of sulfonamides detection - A review.

Science.gov (United States)

Dmitrienko, Stanislava G; Kochuk, Elena V; Apyari, Vladimir V; Tolmacheva, Veronika V; Zolotov, Yury A

2014-11-19

Sulfonamides (SAs) have been the most widely used antimicrobial drugs for more than 70 years, and their residues in foodstuffs and environmental samples pose serious health hazards. For this reason, sensitive and specific methods for the quantification of these compounds in numerous matrices have been developed. This review intends to provide an updated overview of the recent trends over the past five years in sample preparation techniques and methods for detecting SAs. Examples of the sample preparation techniques, including liquid-liquid and solid-phase extraction, dispersive liquid-liquid microextraction and QuEChERS, are given. Different methods of detecting the SAs present in food and feed and in environmental, pharmaceutical and biological samples are discussed. Copyright © 2014 Elsevier B.V. All rights reserved.

Low-Cost 3D Printers Enable High-Quality and Automated Sample Preparation and Molecular Detection.

Directory of Open Access Journals (Sweden)

Kamfai Chan

Full Text Available Most molecular diagnostic assays require upfront sample preparation steps to isolate the target's nucleic acids, followed by its amplification and detection using various nucleic acid amplification techniques. Because molecular diagnostic methods are generally rather difficult to perform manually without highly trained users, automated and integrated systems are highly desirable but too costly for use at point-of-care or low-resource settings. Here, we showcase the development of a low-cost and rapid nucleic acid isolation and amplification platform by modifying entry-level 3D printers that cost between $400 and $750. Our modifications consisted of replacing the extruder with a tip-comb attachment that houses magnets to conduct magnetic particle-based nucleic acid extraction. We then programmed the 3D printer to conduct motions that can perform high-quality extraction protocols. Up to 12 samples can be processed simultaneously in under 13 minutes and the efficiency of nucleic acid isolation matches well against gold-standard spin-column-based extraction technology. Additionally, we used the 3D printer's heated bed to supply heat to perform water bath-based polymerase chain reactions (PCRs. Using another attachment to hold PCR tubes, the 3D printer was programmed to automate the process of shuttling PCR tubes between water baths. By eliminating the temperature ramping needed in most commercial thermal cyclers, the run time of a 35-cycle PCR protocol was shortened by 33%. This article demonstrates that for applications in resource-limited settings, expensive nucleic acid extraction devices and thermal cyclers that are used in many central laboratories can be potentially replaced by a device modified from inexpensive entry-level 3D printers.

Low-Cost 3D Printers Enable High-Quality and Automated Sample Preparation and Molecular Detection

Science.gov (United States)

Chan, Kamfai; Coen, Mauricio; Hardick, Justin; Gaydos, Charlotte A.; Wong, Kah-Yat; Smith, Clayton; Wilson, Scott A.; Vayugundla, Siva Praneeth; Wong, Season

2016-01-01

Most molecular diagnostic assays require upfront sample preparation steps to isolate the target’s nucleic acids, followed by its amplification and detection using various nucleic acid amplification techniques. Because molecular diagnostic methods are generally rather difficult to perform manually without highly trained users, automated and integrated systems are highly desirable but too costly for use at point-of-care or low-resource settings. Here, we showcase the development of a low-cost and rapid nucleic acid isolation and amplification platform by modifying entry-level 3D printers that cost between $400 and $750. Our modifications consisted of replacing the extruder with a tip-comb attachment that houses magnets to conduct magnetic particle-based nucleic acid extraction. We then programmed the 3D printer to conduct motions that can perform high-quality extraction protocols. Up to 12 samples can be processed simultaneously in under 13 minutes and the efficiency of nucleic acid isolation matches well against gold-standard spin-column-based extraction technology. Additionally, we used the 3D printer’s heated bed to supply heat to perform water bath-based polymerase chain reactions (PCRs). Using another attachment to hold PCR tubes, the 3D printer was programmed to automate the process of shuttling PCR tubes between water baths. By eliminating the temperature ramping needed in most commercial thermal cyclers, the run time of a 35-cycle PCR protocol was shortened by 33%. This article demonstrates that for applications in resource-limited settings, expensive nucleic acid extraction devices and thermal cyclers that are used in many central laboratories can be potentially replaced by a device modified from inexpensive entry-level 3D printers. PMID:27362424

Monolith Chromatography as Sample Preparation Step in Virome Studies of Water Samples.

Science.gov (United States)

Gutiérrez-Aguirre, Ion; Kutnjak, Denis; Rački, Nejc; Rupar, Matevž; Ravnikar, Maja

2018-01-01

Viruses exist in aquatic media and many of them use this media as transmission route. Next-generation sequencing (NGS) technologies have opened new doors in virus research, allowing also to reveal a hidden diversity of viral species in aquatic environments. Not surprisingly, many of the newly discovered viruses are found in environmental fresh and marine waters. One of the problems in virome research can be the low amount of viral nucleic acids present in the sample in contrast to the background ones (host, eukaryotic, prokaryotic, environmental). Therefore, virus enrichment prior to NGS is necessary in many cases. In water samples, an added problem resides in the low concentration of viruses typically present in aquatic media. Different concentration strategies have been used to overcome such limitations. CIM monoliths are a new generation of chromatographic supports that due to their particular structural characteristics are very efficient in concentration and purification of viruses. In this chapter, we describe the use of CIM monolithic chromatography for sample preparation step in NGS studies targeting viruses in fresh or marine water. The step-by-step protocol will include a case study where CIM concentration was used to study the virome of a wastewater sample using NGS.

A novel electroluminescent PPV copolymer and silsesquioxane nanocomposite film for the preparation of efficient PLED devices.

Science.gov (United States)

Venegoni, Ivan; Carniato, Fabio; Olivero, Francesco; Bisio, Chiara; Pira, Nello Li; Lambertini, Vito Guido; Marchese, Leonardo

2012-11-02

Polymer light-emitting diodes (PLEDs) have attracted growing interest in recent years for their potential use in displays and lighting fields. Nevertheless, PLED devices have some disadvantages in terms of low optoelectronic efficiency, high cost, short lifetimes and low thermal stability, which limit their final applications. Huge efforts have been made recently to improve the performances of these devices. The addition of inorganic or hybrid organic-inorganic nanoparticles to the light-emitting polymers, for example, allows their thermal stability and electroluminescent efficiency to be increased. Following this approach, novel PLED devices based on composite films of PPV-derivative copolymer (commercial name Super Yellow, SY) and octaisobutil POSS, were developed in this study. The device containing Super Yellow loaded with 1 wt% of POSS showed higher efficiency (ca. +30%) and improved lifetime in comparison to PLED prepared with the pure electroluminescent polymer. The PLED devices developed in this study are suitable candidates for automotive dashboards and, in general, for lighting applications.

Electrodeposition as a sample preparation technique for TXRF analysis

International Nuclear Information System (INIS)

Griesel, S.; Reus, U.; Prange, A.

2000-01-01

TXRF analysis of trace elements at concentrations in the μg/L range and below in high salt matrices normally requires a number of sample preparation steps that include separation of the salt matrix and preconcentration of the trace elements. A neat approach which allows samples to be prepared straightforwardly in a single step involves the application of electrochemical deposition using the TXRF sample support itself as an electrode. For this work a common three-electrode arrangement (radiometer analytical) with a rotating disc electrode as the working electrode, as is frequently employed in voltametric analysis, has been used. A special electrode tip has been constructed as a holder for the sample carrier which consists of polished glassy carbon. This material has been proven to be suitable for both its electrical and chemical properties. Measurements of the trace elements were performed using the ATOMIKA 8030C TXRF spectrometer, with the option of variable incident angles. In first experiments an artificial sea water matrix containing various trace elements in the μg/L range has been used. Elements such as Cr, Mn, Fe, Co, Ni, Cu, Zn, Ag, Cd, Hg, and Pb deposited on glassy carbon carriers. The deposition can be optimized by controlling the potential of the working electrode with respect to the reference electrode. Metal ions with a suitable standard potential are reduced to the metallic state and plated onto the electrode surface. When deposition is finished the sample carrier is demounted, rinsed with ultra-pure water and measured directly. Deposition yields for the elements under investigation are quite similar, and with an appropriate choice of the reference element, quantification can be achieved directly by internal standardization. The influence of parameters such as time, pH value, and trace element concentration on the deposition yield has been examined, and the results will be presented along with reproducibility studies. (author)

Liquid-phase sample preparation method for real-time monitoring of airborne asbestos fibers by dual-mode high-throughput microscopy.

Science.gov (United States)

Cho, Myoung-Ock; Kim, Jung Kyung; Han, Hwataik; Lee, Jeonghoon

2013-01-01

Asbestos that had been used widely as a construction material is a first-level carcinogen recognized by the World Health Organization. It can be accumulated in body by inhalation causing virulent respiratory diseases including lung cancer. In our previous study, we developed a high-throughput microscopy (HTM) system that can minimize human intervention accompanied by the conventional phase contrast microscopy (PCM) through automated counting of fibrous materials and thus significantly reduce analysis time and labor. Also, we attempted selective detection of chrysotile using DksA protein extracted from Escherichia coli through a recombinant protein production technique, and developed a dual-mode HTM (DM-HTM) by upgrading the HTM device. We demonstrated that fluorescently-labeled chrysotile asbestos fibers can be identified and enumerated automatically among other types of asbestos fibers or non-asbestos particles in a high-throughput manner through a newly modified HTM system for both reflection and fluorescence imaging. However there is a limitation to apply DM-HTM to airborne sample with current air collecting method due to the difficulty of applying the protein to dried asbestos sample. Here, we developed a technique for preparing liquid-phase asbestos sample using an impinger normally used to collect odor molecules in the air. It would be possible to improve the feasibility of the dual-mode HTM by integrating a sample preparation unit for making collected asbestos sample dispersed in a solution. The new technique developed for highly sensitive and automated asbestos detection can be a potential alternative to the conventional manual counting method, and it may be applied on site as a fast and reliable environmental monitoring tool.

Guidance document for preparing water sampling and analysis plans for UMTRA Project sites. Revision 1

International Nuclear Information System (INIS)

1995-09-01

A water sampling and analysis plan (WSAP) is prepared for each Uranium Mill Tailings Remedial Action (UMTRA) Project site to provide the rationale for routine ground water sampling at disposal sites and former processing sites. The WSAP identifies and justifies the sampling locations, analytical parameters, detection limits, and sampling frequency for the routine ground water monitoring stations at each site. This guidance document has been prepared by the Technical Assistance Contractor (TAC) for the US Department of Energy (DOE). Its purpose is to provide a consistent technical approach for sampling and monitoring activities performed under the WSAP and to provide a consistent format for the WSAP documents. It is designed for use by the TAC in preparing WSAPs and by the DOE, US Nuclear Regulatory Commission, state and tribal agencies, other regulatory agencies, and the public in evaluating the content of WSAPS

Sample preparation for large-scale bioanalytical studies based on liquid chromatographic techniques.

Science.gov (United States)

Medvedovici, Andrei; Bacalum, Elena; David, Victor

2018-01-01

Quality of the analytical data obtained for large-scale and long term bioanalytical studies based on liquid chromatography depends on a number of experimental factors including the choice of sample preparation method. This review discusses this tedious part of bioanalytical studies, applied to large-scale samples and using liquid chromatography coupled with different detector types as core analytical technique. The main sample preparation methods included in this paper are protein precipitation, liquid-liquid extraction, solid-phase extraction, derivatization and their versions. They are discussed by analytical performances, fields of applications, advantages and disadvantages. The cited literature covers mainly the analytical achievements during the last decade, although several previous papers became more valuable in time and they are included in this review. Copyright © 2017 John Wiley & Sons, Ltd.

Sample Preparation and Identification of Biological, Chemical and Mid-Spectrum Agents

National Research Council Canada - National Science Library

Hancock, J. R; Dragon, D. C

2005-01-01

A general survey of sample preparation and identification techniques for biological, chemical and mid-spectrum agents was conducted as part of Canada's contribution to a joint NATO Allied Engineering Publication (AEP) handbook...

Guide for the preparation of applications for licenses for the use of sealed sources in portable gauging devices

International Nuclear Information System (INIS)

1985-01-01

The purpose of this regulatory guide is to provide assistance to applicants and licensees in preparing applications for new licenses, license amendments, and license renewals for the use of sealed sources in portable gauging devices. An example of a portable gauging device is a moisture-density gauge that contains a gamma-emitting sealed source, cesium-137, and a sealed neutron source, americium-242-beryllium

Bovine liver sample preparation and micro-homogeneity study for Cu and Zn determination by solid sampling electrothermal atomic absorption spectrometry

International Nuclear Information System (INIS)

Nomura, Cassiana S.; Silva, Cintia S.; Nogueira, Ana R.A.; Oliveira, Pedro V.

2005-01-01

This work describes a systematic study for the bovine liver sample preparation for Cu and Zn determination by solid sampling electrothermal atomic absorption spectrometry. The main parameters investigated were sample drying, grinding process, particle size, sample size, microsample homogeneity, and their relationship with the precision and accuracy of the method. A bovine liver sample was prepared using different drying procedures: (1) freeze drying, and (2) drying in a household microwave oven followed by drying in a stove at 60 deg. C until constant mass. Ball and cryogenic mills were used for grinding. Less sensitive wavelengths for Cu (216.5 nm) and Zn (307.6 nm), and Zeeman-based three-field background correction for Cu were used to diminish the sensitivities. The pyrolysis and atomization temperatures adopted were 1000 deg. C and 2300 deg. C for Cu, and 700 deg. C and 1700 deg. C for Zn, respectively. For both elements, it was possible to calibrate the spectrometer with aqueous solutions. The use of 250 μg of W + 200 μg of Rh as permanent chemical modifier was imperative for Zn. Under these conditions, the characteristic mass and detection limit were 1.4 ng and 1.6 ng for Cu, and 2.8 ng and 1.3 ng for Zn, respectively. The results showed good agreement (95% confidence level) for homogeneity of the entire material (> 200 mg) when the sample was dried in microwave/stove and ground in a cryogenic mill. The microsample homogeneity study showed that Zn is more dependent on the sample pretreatment than Cu. The bovine liver sample prepared in microwave/stove and ground in a cryogenic mill presented results with the lowest relative standard deviation for Cu than Zn. Good accuracy and precision were observed for bovine liver masses higher than 40 μg for Cu and 30 μg for Zn. The concentrations of Cu and Zn in the prepared bovine liver sample were 223 mg kg - 1 and 128 mg kg - 1 , respectively. The relative standard deviations were lower than 6% (n = 5). The

Sample preparation: a critical step in the analysis of cholesterol oxidation products.

Science.gov (United States)

Georgiou, Christiana A; Constantinou, Michalis S; Kapnissi-Christodoulou, Constantina P

2014-02-15

In recent years, cholesterol oxidation products (COPs) have drawn scientific interest, particularly due to their implications on human health. A big number of these compounds have been demonstrated to be cytotoxic, mutagenic, and carcinogenic. The main source of COPs is through diet, and particularly from the consumption of cholesterol-rich foods. This raises questions about the safety of consumers, and it suggests the necessity for the development of a sensitive and a reliable analytical method in order to identify and quantify these components in food samples. Sample preparation is a necessary step in the analysis of COPs in order to eliminate interferences and increase sensitivity. Numerous publications have, over the years, reported the use of different methods for the extraction and purification of COPs. However, no method has, so far, been established as a routine method for the analysis of COPs in foods. Therefore, it was considered important to overview different sample preparation procedures and evaluate the different preparative parameters, such as time of saponification, the type of organic solvents for fat extraction, the stationary phase in solid phase extraction, etc., according to recovery, precision and simplicity. Copyright © 2013 Elsevier Ltd. All rights reserved.

Consumers' Use of Personal Electronic Devices in the Kitchen.

Science.gov (United States)

Lando, Amy M; Bazaco, Michael C; Chen, Yi

2018-02-23

Smartphones, tablets, and other personal electronic devices have become ubiquitous in Americans' daily lives. These devices are used by people throughout the day, including while preparing food. For example, a device may be used to look at recipes and therefore be touched multiple times during food preparation. Previous research has indicated that cell phones can harbor bacteria, including opportunistic human pathogens such as Staphylococcus and Klebsiella spp. This investigation was conducted with data from the 2016 Food Safety Survey (FSS) and from subsequent focus groups to determine the frequency with which consumers use personal electronic devices in the kitchen while preparing food, the types of devices used, and hand washing behaviors after handling these devices. The 2016 FSS is the seventh wave of a repeated cross-sectional survey conducted by the U.S. Food and Drug Administration in collaboration with the U.S. Department of Agriculture. The goal of the FSS is to evaluate U.S. adult consumer attitudes, behaviors, and knowledge about food safety. The FSS included 4,169 adults that were contacted using a dual-frame (land line and cell phone interviews) random-digit-dial sampling process. The personal electronics module was the first of three food safety topics discussed by each of eight consumer focus groups, which were convened in four U.S. cities in fall 2016. Results from the 2016 FSS revealed that of those individuals who use personal electronic devices while cooking, only about one third reported washing hands after touching the device and before continuing cooking. This proportion is significantly lower than that for self-reported hand washing behaviors after touching risky food products such as raw eggs, meat, chicken, or fish. Results from the focus groups highlight the varied usage of these devices during food preparation and the related strategies consumers are using to incorporate personal electric devices into their cooking routines.

Preparation of solid-state samples of a transition metal coordination compound for synchrotron radiation photoemission studies

CERN Document Server

Crotti, C; Celestino, T; Fontana, S

2003-01-01

The aim of this research was to identify a sample preparation method suitable for the study of transition metal complexes by photoemission spectroscopy with synchrotron radiation as the X-ray source, even in the case where the compound is not evaporable. Solid-phase samples of W(CO) sub 4 (dppe) [dppe=1,2-bis(diphenylphosphino)ethane] were prepared according to different methods and their synchrotron radiation XPS spectra measured. The spectra acquired from samples prepared by spin coating show core level peaks only slightly broader than the spectrum recorded from UHV evaporated samples. Moreover, for these samples the reproducibility of the binding energy values is excellent. The dependence of the spin coating technique on parameters such as solvent and solution concentration, spinning speed and support material was studied. The same preparation method also allowed the acquisition of valence band spectra, the main peaks of which were clearly resolved. The results suggest that use of the spin coating techniqu...

Sample preparation method for the combined extraction of ethyl glucuronide and drugs of abuse in hair.

Science.gov (United States)

Meier, Ulf; Briellmann, Thomas; Scheurer, Eva; Dussy, Franz

2018-04-01

Often in hair analysis, a small hair sample is available while the analysis of a multitude of structurally diverse substances with different concentration ranges is demanded. The analysis of the different substances often requires different sample preparation methods, increasing the amount of required hair sample. When segmental hair analysis is necessary, the amount of hair sample needed is further increased. Therefore, the required sample amount for a full analysis can quickly exceed what is available. To combat this problem, a method for the combined hair sample preparation using a single extraction procedure for analysis of ethyl glucuronide with liquid chromatography-multistage fragmentation mass spectrometry/multiple reaction monitoring (LC-MS 3 /MRM) and common drugs of abuse with LC-MRM was developed. The combined sample preparation is achieved by separating ethyl glucuronide from the drugs of abuse into separate extracts by fractionation in the solid-phase extraction step during sample clean-up. A full validation for all substances for the parameters selectivity, linearity, limit of detection, limit of quantification, accuracy, precision, matrix effects, and recovery was successfully completed. The following drugs of abuse were included in the method: Amphetamine; methamphetamine; 3,4-methylenedioxy-N-methylamphetamine (MDMA); 3,4-methylenedioxyamphetamine (MDA); 3,4-methylenedioxy-N-ethylamphetamine (MDE); morphine; 6-monoacetylmorphine; codeine; acetylcodeine; cocaine; benzoylecgonine; norcocaine; cocaethylene; methadone; 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine (EDDP) and methylphenidate. In conclusion, as only 1 sample preparation is needed with 1 aliquot of hair, the presented sample preparation allows an optimal analysis of both ethyl glucuronide and of the drugs of abuse, even when the sample amount is a limiting factor. Copyright © 2017 John Wiley & Sons, Ltd.

Second generation laser-heated microfurnace for the preparation of microgram-sized graphite samples

Energy Technology Data Exchange (ETDEWEB)

Yang, Bin; Smith, A.M.; Long, S.

2015-10-15

We present construction details and test results for two second-generation laser-heated microfurnaces (LHF-II) used to prepare graphite samples for Accelerator Mass Spectrometry (AMS) at ANSTO. Based on systematic studies aimed at optimising the performance of our prototype laser-heated microfurnace (LHF-I) (Smith et al., 2007 [1]; Smith et al., 2010 [2,3]; Yang et al., 2014 [4]), we have designed the LHF-II to have the following features: (i) it has a small reactor volume of 0.25 mL allowing us to completely graphitise carbon dioxide samples containing as little as 2 μg of C, (ii) it can operate over a large pressure range (0–3 bar) and so has the capacity to graphitise CO{sub 2} samples containing up to 100 μg of C; (iii) it is compact, with three valves integrated into the microfurnace body, (iv) it is compatible with our new miniaturised conventional graphitisation furnaces (MCF), also designed for small samples, and shares a common vacuum system. Early tests have shown that the extraneous carbon added during graphitisation in each LHF-II is of the order of 0.05 μg, assuming 100 pMC activity, similar to that of the prototype unit. We use a ‘budget’ fibre packaged array for the diode laser with custom built focusing optics. The use of a new infrared (IR) thermometer with a short focal length has allowed us to decrease the height of the light-proof safety enclosure. These innovations have produced a cheaper and more compact device. As with the LHF-I, feedback control of the catalyst temperature and logging of the reaction parameters is managed by a LabVIEW interface.

Study of sample preparation in the measurement of 36Ar(n, p)36Cl reaction cross section

International Nuclear Information System (INIS)

Jiang Songsheng; Hemick, T.K.

1992-01-01

The preparation of enriched 36 Ar gas samples and 36 Cl samples for the use in the AMS measurement of 36 Ar(n, p) 36 Cl reaction cross section was described. The 36 Ar samples prepared had the volumes of about 0.4 ml and the weights of about 0.5 mg. The uncertainty in atomic numbers of 36 Ar was (0.3∼0.4)%. The reaction product, 36 Cl, in the 36 Ar was collected and the AgCl samples were prepared

Dynamic Headspace Sampling as an Initial Step for Sample Preparation in Chromatographic Analysis.

Science.gov (United States)

Wojnowski, Wojciech; Majchrzak, Tomasz; Dymerski, Tomasz; Gębicki, Jacek; Namieśnik, Jacek

2017-11-01

This work represents a brief summary of the use of dynamic headspace (DHS) as a technique for sample preparation in chromatographic analysis. Despite numerous developments in the area of analyte isolation and enrichment, DHS remains one of the fundamental methods used with GC. In our opinion, interest in this technique will not diminish significantly because it conforms to stipulations of green analytical chemistry. Moreover, DHS fulfills the need for methods that facilitate detection and determination of analytes present at ultratrace levels in complex matrixes. The main focus of this work was placed on the theoretical fundamentals of this method. Also described herein were DHS development, the advantages and disadvantages of this technique compared with other headspace sampling techniques, and selected examples of its applications in food and environmental analyses.

Ultrasonic assisted extraction - an alternative for sample preparation (M4)

International Nuclear Information System (INIS)

Santos Junior, P.; Barbosa Junior, F.; Krug, F.J.; Trevizan, L.C.; Nobrega, J.A.

2002-01-01

Full text: In the last years the ultrasound assisted metal extraction has been frequency proposed as a simple and inexpensive alternative for sample preparation of biological and inorganic samples. The extraction effect is considered as being caused by acoustic cavitation, that is, bubble formation and subsequent disruptive action. The collapse of bubbles created by sonication of solutions results in the generation of extremely high local temperature and pressure gradients, which may be regarded as localized 'hot spots'. On a timescale of about 10 -10 s, effective local pressures and temperature of about 10 5 atm and about 5000 K, respectively, are generated under sonochemical conditions. Usually, this method uses a diluted acid medium decreasing blank values and reducing both reagents and time consumption compared to traditional wet digestion systems using conductive or microwave-assisted heating. Furthermore, sonication can also allow the preparation of samples directly within the sample container, thereby preventing sample losses and minimizing sample contamination. Although some controversial results concerning metals extraction behavior have been reported, they could be explained by analyte-matrix interaction and the ability of the ultrasonic processor to generate ultrasound (i.e. the use of an ultrasonic bath or an ultrasonic probe at different power, frequency, and amplitude). This contribution presents a review of ultrasound assisted metal extraction and recent performance data obtained in our laboratory for determination of elements in biological materials, soils and sediments by ICP-OES and ETAAS. The effect of extraction parameters, such as type and concentration of the leaching solution, sonication time and performance of ultrasonic processor (bath or probe) will be presented. (author)

An automatic device for sample insertion and extraction to/from reactor irradiation facilities

International Nuclear Information System (INIS)

Alloni, L.; Venturelli, A.; Meloni, S.

1990-01-01

At the previous European Triga Users Conference in Vienna,a paper was given describing a new handling tool for irradiated samples at the L.E.N.A plant. This tool was the first part of an automatic device for the management of samples to be irradiated in the TRIGA MARK ii reactor and successively extracted and stored. So far sample insertion and extraction to/from irradiation facilities available on reactor top (central thimble,rotatory specimen rack and channel f),has been carried out manually by reactor and health-physics operators using the ''traditional'' fishing pole provided by General Atomic, thus exposing reactor personnel to ''unjustified'' radiation doses. The present paper describes the design and the operation of a new device, a ''robot''type machine,which, remotely operated, takes care of sample insertion into the different irradiation facilities,sample extraction after irradiation and connection to the storage pits already described. The extraction of irradiated sample does not require the presence of reactor personnel on the reactor top and,therefore,radiation doses are strongly reduced. All work from design to construction has been carried out by the personnel of the electronic group of the L.E.N.A plant. (orig.)

Effect of sample preparation methods on photometric determination of the tellurium and cobalt content in the samples of copper concentrates

Directory of Open Access Journals (Sweden)

Viktoriya Butenko

2016-03-01

Full Text Available Methods of determination of cobalt and nickel in copper concentrates currently used in factory laboratories are very labor intensive and time consuming. The limiting stage of the analysis is preliminary chemical sample preparation. Carrying out the decomposition process of industrial samples with concentrated mineral acids in open systems does not allow to improve the metrological characteristics of the methods, for this reason improvement the methods of sample preparation is quite relevant and has a practical interest. The work was dedicated to the determination of the optimal conditions of preliminary chemical preparation of copper concentrate samples for the subsequent determination of cobalt and tellurium in the obtained solution using tellurium-spectrophotometric method. Decomposition of the samples was carried out by acid dissolving in individual mineral acids and their mixtures by heating in an open system as well as by using ultrasonification and microwave radiation in a closed system. In order to select the optimal conditions for the decomposition of the samples in a closed system the phase contact time and ultrasonic generator’s power were varied. Intensification of the processes of decomposition of copper concentrates with nitric acid (1:1, ultrasound and microwave radiation allowed to transfer quantitatively cobalt and tellurium into solution spending 20 and 30 min respectively. This reduced the amount of reactants used and improved the accuracy of determination by running the process in strictly identical conditions.

Robotic sample preparation for radiochemical plutonium and americium analyses

International Nuclear Information System (INIS)

Stalnaker, N.; Beugelsdijk, T.; Thurston, A.; Quintana, J.

1985-01-01

A Zymate robotic system has been assembled and programmed to prepare samples for plutonium and americium analyses by radioactivity counting. The system performs two procedures: a simple dilution procedure and a TTA (xylene) extraction of plutonium. To perform the procedures, the robotic system executes 11 unit operations such as weighing, pipetting, mixing, etc. Approximately 150 programs, which require 64 kilobytes of memory, control the system. The system is now being tested with high-purity plutonium metal and plutonium oxide samples. Our studies indicate that the system can give results that agree within 5% at the 95% confidence level with determinations performed manually. 1 ref., 1 fig., 1 tab

Sample preparation composite and replicate strategy case studies for assay of solid oral drug products.

Science.gov (United States)

Nickerson, Beverly; Harrington, Brent; Li, Fasheng; Guo, Michele Xuemei

2017-11-30

Drug product assay is one of several tests required for new drug products to ensure the quality of the product at release and throughout the life cycle of the product. Drug product assay testing is typically performed by preparing a composite sample of multiple dosage units to obtain an assay value representative of the batch. In some cases replicate composite samples may be prepared and the reportable assay value is the average value of all the replicates. In previously published work by Harrington et al. (2014) [5], a sample preparation composite and replicate strategy for assay was developed to provide a systematic approach which accounts for variability due to the analytical method and dosage form with a standard error of the potency assay criteria based on compendia and regulatory requirements. In this work, this sample preparation composite and replicate strategy for assay is applied to several case studies to demonstrate the utility of this approach and its application at various stages of pharmaceutical drug product development. Copyright © 2017 Elsevier B.V. All rights reserved.

Integrated Automation of High-Throughput Screening and Reverse Phase Protein Array Sample Preparation

DEFF Research Database (Denmark)

Pedersen, Marlene Lemvig; Block, Ines; List, Markus

into automated robotic high-throughput screens, which allows subsequent protein quantification. In this integrated solution, samples are directly forwarded to automated cell lysate preparation and preparation of dilution series, including reformatting to a protein spotter-compatible format after the high......-throughput screening. Tracking of huge sample numbers and data analysis from a high-content screen to RPPAs is accomplished via MIRACLE, a custom made software suite developed by us. To this end, we demonstrate that the RPPAs generated in this manner deliver reliable protein readouts and that GAPDH and TFR levels can...

Influence of rice sample preparation and milling procedures on milling quality appraisals

Science.gov (United States)

The objective of this research was to investigate the effect of sample preparation and milling procedure on milling quality appraisals of rough rice. Samples of freshly harvested medium-grain rice (M202) with different initial moisture contents (MCs) ranging from 20.2% to 25.1% (w.b.) were used for...

Microextraction sample preparation techniques in biomedical analysis.

Science.gov (United States)

Szultka, Malgorzata; Pomastowski, Pawel; Railean-Plugaru, Viorica; Buszewski, Boguslaw

2014-11-01

Biologically active compounds are found in biological samples at relatively low concentration levels. The sample preparation of target compounds from biological, pharmaceutical, environmental, and food matrices is one of the most time-consuming steps in the analytical procedure. The microextraction techniques are dominant. Metabolomic studies also require application of proper analytical technique for the determination of endogenic metabolites present in biological matrix on trace concentration levels. Due to the reproducibility of data, precision, relatively low cost of the appropriate analysis, simplicity of the determination, and the possibility of direct combination of those techniques with other methods (combination types on-line and off-line), they have become the most widespread in routine determinations. Additionally, sample pretreatment procedures have to be more selective, cheap, quick, and environmentally friendly. This review summarizes the current achievements and applications of microextraction techniques. The main aim is to deal with the utilization of different types of sorbents for microextraction and emphasize the use of new synthesized sorbents as well as to bring together studies concerning the systematic approach to method development. This review is dedicated to the description of microextraction techniques and their application in biomedical analysis. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Device for the analysis of feedwater and condensation samples from power plants

International Nuclear Information System (INIS)

Mostofin, A.A.; Sorokina, N.S.

1978-01-01

An improved version of a device for automatic measurement of the salt and NH 3 contents of feedwater and condensate samples from nuclear power plants is described. Only one sample is required for determining both values. The invention proposes on the one hand to change the dimensions of a throttle opening and on the other to install a second measuring instrument (conductivity measuring instrument). (UWI) [de

ZnO-nanorod-array/p-GaN high-performance ultra-violet light emitting devices prepared by simple solution synthesis

Science.gov (United States)

Jha, Shrawan Kumar; Luan, Chunyan; To, Chap Hang; Kutsay, Oleksandr; Kováč, Jaroslav; Zapien, Juan Antonio; Bello, Igor; Lee, Shuit-Tong

2012-11-01

Pure ultra-violet (UV) (378 nm) electroluminescence (EL) from zinc oxide (ZnO)-nanorod-array/p-gallium nitride (GaN) light emitting devices (LEDs) is demonstrated at low bias-voltages (˜4.3 V). Devices were prepared merely by solution-synthesis, without any involvement of sophisticated material growth techniques or preparation methods. Three different luminescence characterization techniques, i.e., photo-luminescence, cathodo-luminescence, and EL, provided insight into the nature of the UV emission mechanism in solution-synthesized LEDs. Bias dependent EL behaviour revealed blue-shift of EL peaks and increased peak sharpness, with increasing the operating voltage. Accelerated bias stress tests showed very stable and repeatable electrical and EL performance of the solution-synthesized nanorod LEDs.

Notes on sample preparation of food: food of plant and animal origins, and daily meals

International Nuclear Information System (INIS)

Heilgeist, M.

1992-01-01

The procedure of food sample preparation to determine their specific radioactivity, analogous to chemical residue analysis, is laid down in the relevant sets of regulations. Several procedural steps of sample preparation of single food and composite food are dealt with. The sample size necessary for gamma spectroscopy and Sr-89/Sr-90 analysis, and the incineration step to enrich radionuclides are explained. Finally, enrichment by freeze drying of the high-volatile radionuclide I-131 is considered. (orig.) [de

Sampling technologies and air pollution control devices for gaseous and particulate arsenic: a review

International Nuclear Information System (INIS)

Helsen, Lieve

2005-01-01

Direct measurement of arsenic release requires a good sampling and analysis procedure in order to capture and detect the total amount of metals emitted. The literature is extensively reviewed in order to evaluate the efficiency of full field-scale and laboratory scale techniques for capturing particulate and gaseous emissions of arsenic from the thermo-chemical treatment of different sources of arsenic. Furthermore, trace arsenic concentrations in ambient air, national standard sampling methods and arsenic analysis methods are considered. Besides sampling techniques, the use of sorbents is also reviewed with respect to both approaches (1) to prevent the metals from exiting with the flue gas and (2) to react or combine with the metals in order to be collected in air pollution control systems. The most important conclusion is that submicron arsenic fumes are difficult to control in conventional air pollution control devices. Complete capture of the arsenic species requires a combination of particle control and vapour control devices. - Submicron arsenic fumes are difficult to control in conventional air pollution control devices

Sample collection and preparation of biofluids and extracts for gas chromatography-mass spectrometry.

Science.gov (United States)

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.

Open focused microwave-assisted sample preparation for rapid total and mercury species determination in environmental solid samples

OpenAIRE

Tseng, C. M.; Garraud, H.; Amouroux, D.; Donard, O. F. X.; de Diego, A.

1998-01-01

This paper describes rapid, simple microwave-assisted leaching/ digestion procedures for total and mercury species determination in sediment samples and biomaterials. An open focused microwave system allowed the sample preparation time to be dramatically reduced to only 24 min when a power of 40-80 W was applied. Quantitative leaching of methylmercury from sediments by HNO3 solution and complete dissolution of biomaterials by an alkaline solution, such as 25% TMAH solution, were obtained. Met...

Sample preparation strategies for food and biological samples prior to nanoparticle detection and imaging

DEFF Research Database (Denmark)

Larsen, Erik Huusfeldt; Löschner, Katrin

2014-01-01

microscopy (TEM) proved to be necessary for trouble shooting of results obtained from AFFF-LS-ICP-MS. Aqueous and enzymatic extraction strategies were tested for thorough sample preparation aiming at degrading the sample matrix and to liberate the AgNPs from chicken meat into liquid suspension. The resulting...... AFFF-ICP-MS fractograms, which corresponded to the enzymatic digests, showed a major nano-peak (about 80 % recovery of AgNPs spiked to the meat) plus new smaller peaks that eluted close to the void volume of the fractograms. Small, but significant shifts in retention time of AFFF peaks were observed...... for the meat sample extracts and the corresponding neat AgNP suspension, and rendered sizing by way of calibration with AgNPs as sizing standards inaccurate. In order to gain further insight into the sizes of the separated AgNPs, or their possible dissolved state, fractions of the AFFF eluate were collected...

Effect of method of sample preparation on ruminal in situ ...

African Journals Online (AJOL)

Midmar) was harvested at three and four weeks after cutting and fertilizing with 200 kg nitrogen (N)/ha. Freshly cut herbage was used to investigate the following four sample preparation methods. In trial 1, herbage was (1) chopped with a paper-cutting guillotine into 5-10 mm lengths, representing fresh (FR) herbage; ...

Soybean and lactose in meat products and preparations sampled at retail

Directory of Open Access Journals (Sweden)

Filomena Piccolo

2016-06-01

Full Text Available Food allergies and intolerances have increased during the last decades and regulatory authorities have taken different measures to prevent and manage consumers’ adverse reactions, including correct labelling of foods. Aim of this work was to search for soybean and lactose in meat products and meat preparations taken from retail in some provinces of Campania Region (Southern Italy and to evaluate the food labels compliance with Regulation (EU n.1169/2011. Soybean and lactose were searched using commercial kits in n. 58 samples of meat products produced in or distributed by 19 establishments, and in n. 55 samples of meat products and n. 8 of meat preparations produced in 21 plants. All samples were selected on the basis of the absence of any information on the labels about the presence of the two searched allergens, with the exception of n. 5 samples tested for lactose. Traces of soybean were detected in 50 out of the 58 examined samples, at concentrations up to 0.93 mg kg–1. Only two samples contained levels above the detection limit of 0.31 mg kg–1. Lactose levels ranging from 0.11 to 2.95 g/100 g, i.e. above the detection limit, were found in all the tested samples (n. 63. The results of the present research underline the need for careful controls and planning by operators as part of the self-control plans, and deserve attention from the competent authorities considering not only the consumers’ health but also the great attention media pay to regulations providing consumers with information on food.

Influence of sample preparation on the microstructure of tooth enamel apatite

Czech Academy of Sciences Publication Activity Database

Kallistová, Anna; Skála, Roman; Horáček, I.; Miyajima, N.; Malíková, R.

2015-01-01

Roč. 48, č. 3 (2015), s. 763-768 ISSN 0021-8898 Institutional support: RVO:67985831 Keywords : X-ray powder diffraction * sample preparation * microstructure * dental hydroxyapatite Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 3.720, year: 2014

Comparison of two sample preparation procedures for HPLC determination of ochratoxin A

Directory of Open Access Journals (Sweden)

Vuković Gorica L.

2009-01-01

Full Text Available In preparation of samples for chromatographic determination of ochratoxin A, two types of columns were used for sample cleanup (SPE and immunoaffinity columns. The first method consisted of liquid-liquid extraction with a mixture of chloroform and phosphoric acid, followed by ion-exchange cleanup on Waters Oasis MAX columns. The sec­ond method consisted of extraction with a mixture of water and methanol, followed by LCTech OtaCLEAN immunoaf­finity column cleanup. Recoveries of the methods were determined at three levels in three repetitions for maize flour, and they were 84% (%RSD = 19.2 for the first method of sample preparation and 101% (%RSD = 2.2 for the second method. Values of LOQ for OTA were 0.25 and 1.00 μg/kg for the IAC and SPE clean-up procedures, respectively. Both methods comply with present regulations, but the MAX sample clean-up procedure should be used as an alternative, since the immunoaffinity column clean-up procedure is characterized by better reproducibility, accuracy, and efficiency.

An electrodeposition method for the preparation of actinides and Ra samples for α spectrometry

International Nuclear Information System (INIS)

Garcia-Tenorio, R.; Garcia-Leon, M.; Madurga, G.; Piazza, C.

1986-01-01

As it is confirmed in this work, electrodeposition of α radionuclides gives a simple method for preparing α samples of high spectrometric quality, compared to those prepared by evaporation. Then we give the methods for electrodepositon or α emitters use in our Department. Actinides α emitters are electroplated from a 1% H 2 SO 4 medium with a recovery of about 90%. The samples of Ra are prepared by electrodeposition from a HCl + CH 3 -COONH 4 medium at pH approx.= 5. In this case the recovery reaches a value that ranges from 70 to 90%. For these measurements a Si surface barrier detector has been used. Some of its features are discussed in the text. (author)

On the preparation of as-produced and purified single-walled carbon nanotube samples for standardized X-ray diffraction characterization

International Nuclear Information System (INIS)

Allaf, Rula M.; Rivero, Iris V.; Spearman, Shayla S.; Hope-Weeks, Louisa J.

2011-01-01

The aim of this research was to specify proper sample conditioning for acquiring representative X-ray diffraction (XRD) profiles for single-walled carbon nanotube (SWCNT) samples. In doing so, a specimen preparation method for quantitative XRD characterization of as-produced and purified arc-discharge SWCNT samples has been identified. Series of powder XRD profiles were collected at different temperatures, states, and points of time to establish appropriate conditions for acquiring XRD profiles without inducing much change to the specimen. It was concluded that heating in the 300-450 deg. C range for 20 minutes, preferably vacuum-assisted, and then sealing the sample is an appropriate XRD specimen preparation technique for purified arc-discharge SWCNT samples, while raw samples do not require preconditioning for characterization. - Graphical Abstract: A sample preparation method for XRD characterization of as-produced and purified arc-discharge SWCNT samples is identified. The preparation technique seeks to acquire representative XRD profiles without inducing changes to the samples. Purified samples required 20 minutes of heating at (300-450)deg. C, while raw samples did not require preconditioning for characterization. Highlights: → Purification routines may induce adsorption onto the SWCNT samples. → Heating a SWCNT sample may result in material loss, desorption, and SWCNTs closing. → Raw arc-discharge samples do not require preparation for XRD characterization. → Heating is appropriate specimen preparation for purified and heat-treated samples. → XRD data fitting is required for structural analysis of SWCNT bundles.

A Simple Device for Lens-to-Sample Distance Adjustment in Laser-Induced Breakdown Spectroscopy (LIBS).

Science.gov (United States)

Cortez, Juliana; Farias Filho, Benedito B; Fontes, Laiane M; Pasquini, Celio; Raimundo, Ivo M; Pimentel, Maria Fernanda; de Souza Lins Borba, Flávia

2017-04-01

A simple device based on two commercial laser pointers is described to assist in the analysis of samples that present uneven surfaces and/or irregular shapes using laser-induced breakdown spectroscopy (LIBS). The device allows for easy positioning of the sample surface at a reproducible distance from the focusing lens that conveys the laser pulse to generate the micro-plasma in a LIBS system, with reproducibility better than ±0.2 mm. In this way, fluctuations in the fluence (J cm -2 ) are minimized and the LIBS analytical signals can be obtained with a better precision even when samples with irregular surfaces are probed.

Short communication: Influence of the sampling device on somatic cell count variation in cow milk samples (by official recording)

International Nuclear Information System (INIS)

Fouz, R.; Vilar, M.J.; Yus, E.; Sanjuán, M.L.; Diéguez, F.J.

2016-01-01

The objective of this study was to investigate the variability in cow´s milk somatic cell counts (SCC) depending on the type of milk meter used by dairy farms for official milk recording. The study was performed in 2011 and 2012 in the major cattle area of Spain. In total, 137,846 lactations of Holstein-Friesian cows were analysed at 1,912 farms. A generalised least squares regression model was used for data analysis. The model showed that the milk meter had a substantial effect on the SCC for individual milk samples obtained for official milk recording. The results suggested an overestimation of the SCC in milk samples from farms that had electronic devices in comparison with farms that used portable devices and underestimation when volumetric meters are used. A weak positive correlation was observed between the SCC and the percentage of fat in individual milk samples. The results underline the importance of considering this variable when using SCC data from milk recording in the dairy herd improvement program or in quality milk programs. (Author)

Short communication: Influence of the sampling device on somatic cell count variation in cow milk samples (by official recording)

Energy Technology Data Exchange (ETDEWEB)

Fouz, R.; Vilar, M.J.; Yus, E.; Sanjuán, M.L.; Diéguez, F.J.

2016-11-01

The objective of this study was to investigate the variability in cow´s milk somatic cell counts (SCC) depending on the type of milk meter used by dairy farms for official milk recording. The study was performed in 2011 and 2012 in the major cattle area of Spain. In total, 137,846 lactations of Holstein-Friesian cows were analysed at 1,912 farms. A generalised least squares regression model was used for data analysis. The model showed that the milk meter had a substantial effect on the SCC for individual milk samples obtained for official milk recording. The results suggested an overestimation of the SCC in milk samples from farms that had electronic devices in comparison with farms that used portable devices and underestimation when volumetric meters are used. A weak positive correlation was observed between the SCC and the percentage of fat in individual milk samples. The results underline the importance of considering this variable when using SCC data from milk recording in the dairy herd improvement program or in quality milk programs. (Author)

[In vitro study of the flow duration of antibiotics solutions prepared in elastomeric infusion devices: effect of cold storage for 3 to 7days].

Science.gov (United States)

Grangeon-Chapon, C; Robein-Dobremez, M-J; Pin, I; Trouiller, P; Allenet, B; Foroni, L

2015-09-01

Within the cystic fibrosis patients' home care, EMERAA network ("Together against Cystic fibrosis in Rhone-Alpes and Auvergne") organizes parenteral antibiotics cures at home prepared in elastomeric infusion devices by hospital pharmacies. However, patients and nurses found that the durations of infusion with these devices were often longer than the nominal duration of infusion indicated by their manufacturer. This study aimed to identify the potential different causes in relation to these discordances. Three hundred and ninety devices of two different manufacturers are tested in different experimental conditions: three antibiotics each at two different doses, duration of cold storage (three days or seven days) or immediate tests without cold storage, preparation and storage of the solution in the device (protocol Device) or transfer in the device just before measurement (protocol Pocket). All tests highlighted a longer flow duration for devices prepared according to the protocol Device versus the protocol Pocket (P=0.004). Flow duration is increased in the case of high doses of antibiotics with high viscosity such as piperacilline/tazobactam. The results of this in vitro study showed the impact of: (1) the time between the filling of the device and the flow of the solution; (2) cold storage of elastomeric infusion devices; (3) concentration of antibiotics and therefore the viscosity of the solution to infuse. It is therefore essential that health care teams are aware of factors, which may lead to longer infusion durations with these infusion devices. When the additional time for infusion remain acceptable, it should be necessary to inform the patient and to relativize these lengthening compared to many benefits that these devices provide for home care. Copyright © 2015 Elsevier Masson SAS. All rights reserved.

Validation of a fully automated robotic setup for preparation of whole blood samples for LC-MS toxicology analysis

DEFF Research Database (Denmark)

Andersen, David Wederkinck; Rasmussen, Brian; Linnet, Kristian

2012-01-01

A fully automated setup was developed for preparing whole blood samples using a Tecan Evo workstation. By integrating several add-ons to the robotic platform, the flexible setup was able to prepare samples from sample tubes to a 96-well sample plate ready for injection on liquid chromatography...

A microfluidic device for the automated derivatization of free fatty acids to fatty acid methyl esters.

Science.gov (United States)

Duong, Cindy T; Roper, Michael G

2012-02-21

Free fatty acid (FFA) compositions are examined in feedstock for biodiesel production, as source-specific markers in soil, and because of their role in cellular signaling. However, sample preparation of FFAs for gas chromatography-mass spectrometry (GC-MS) analysis can be time and labor intensive. Therefore, to increase sample preparation throughput, a glass microfluidic device was developed to automate derivatization of FFAs to fatty acid methyl esters (FAMEs). FFAs were delivered to one input of the device and methanolic-HCl was delivered to a second input. FAME products were produced as the reagents traversed a 29 μL reaction channel held at 55 °C. A Design of Experiment protocol was used to determine the combination of derivatization time (T(der)) and ratio of methanolic-HCl:FFA (R(der)) that maximized the derivatization efficiencies of tridecanoic acid and stearic acid to their methyl ester forms. The combination of T(der) = 0.8 min and R(der) = 4.9 that produced optimal derivatization conditions for both FFAs within a 5 min total sample preparation time was determined. This combination of T(der) and R(der) was used to derivatize 12 FFAs with a range of derivatization efficiencies from 18% to 93% with efficiencies of 61% for tridecanoic acid and 84% for stearic acid. As compared to a conventional macroscale derivatization of FFA to FAME, the microfluidic device decreased the volume of methanolic-HCl and FFA by 20- and 1300-fold, respectively. The developed microfluidic device can be used for automated preparation of FAMEs to analyze the FFA compositions of volume-limited samples.

A sample preparation method for recovering suppressed analyte ions in MALDI TOF MS

NARCIS (Netherlands)

Lou, X.; Waal, de B.F.M.; Milroy, L.G.; Dongen, van J.L.J.

2015-01-01

In matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI TOF MS), analyte signals can be substantially suppressed by other compounds in the sample. In this technical note, we describe a modified thin-layer sample preparation method that significantly reduces the analyte

Implementation of antimicrobial peptides for sample preparation prior to nucleic acid amplification in point-of-care settings.

Science.gov (United States)

Krõlov, Katrin; Uusna, Julia; Grellier, Tiia; Andresen, Liis; Jevtuševskaja, Jekaterina; Tulp, Indrek; Langel, Ülo

2017-12-01

A variety of sample preparation techniques are used prior to nucleic acid amplification. However, their efficiency is not always sufficient and nucleic acid purification remains the preferred method for template preparation. Purification is difficult and costly to apply in point-of-care (POC) settings and there is a strong need for more robust, rapid, and efficient biological sample preparation techniques in molecular diagnostics. Here, the authors applied antimicrobial peptides (AMPs) for urine sample preparation prior to isothermal loop-mediated amplification (LAMP). AMPs bind to many microorganisms such as bacteria, fungi, protozoa and viruses causing disruption of their membrane integrity and facilitate nucleic acid release. The authors show that incubation of E. coli with antimicrobial peptide cecropin P1 for 5 min had a significant effect on the availability of template DNA compared with untreated or even heat treated samples resulting in up to six times increase of the amplification efficiency. These results show that AMPs treatment is a very efficient sample preparation technique that is suitable for application prior to nucleic acid amplification directly within biological samples. Furthermore, the entire process of AMPs treatment was performed at room temperature for 5 min thereby making it a good candidate for use in POC applications.

Evaluation of sample preparation protocols for spider venom profiling by MALDI-TOF MS.

Science.gov (United States)

Bočánek, Ondřej; Šedo, Ondrej; Pekár, Stano; Zdráhal, Zbyněk

2017-07-01

Spider venoms are highly complex mixtures containing biologically active substances with potential for use in biotechnology or pharmacology. Fingerprinting of venoms by Matrix-Assisted Laser Desorption-Ionization - Time of Flight Mass Spectrometry (MALDI-TOF MS) is a thriving technology, enabling the rapid detection of peptide/protein components that can provide comparative information. In this study, we evaluated the effects of sample preparation procedures on MALDI-TOF mass spectral quality to establish a protocol providing the most reliable analytical outputs. We adopted initial sample preparation conditions from studies already published in this field. Three different MALDI matrixes, three matrix solvents, two sample deposition methods, and different acid concentrations were tested. As a model sample, venom from Brachypelma albopilosa was used. The mass spectra were evaluated on the basis of absolute and relative signal intensities, and signal resolution. By conducting three series of analyses at three weekly intervals, the reproducibility of the mass spectra were assessed as a crucial factor in the selection for optimum conditions. A sample preparation protocol based on the use of an HCCA matrix dissolved in 50% acetonitrile with 2.5% TFA deposited onto the target by the dried-droplet method was found to provide the best results in terms of information yield and repeatability. We propose that this protocol should be followed as a standard procedure, enabling the comparative assessment of MALDI-TOF MS spider venom fingerprints. Copyright © 2017 Elsevier Ltd. All rights reserved.

Challenges of sample preparation for cross sectional EBSD analysis of electrodeposited nickel films

DEFF Research Database (Denmark)

Alimadadi, Hossein; Pantleon, Karen

2009-01-01

Thorough microstructure and crystallographic orientation analysis of thin films by means of electron backscatter diffraction requires cross section preparation of the film-substrate compound. During careful preparation, changes of the rather non-stable as-deposited microstructure must be avoided....... Different procedures for sample preparation including mechanical grinding and polishing, electropolishing and focused ion beam milling have been applied to a nickel film electrodeposited on top of an amorphous Ni-P layer on a Cu-substrate. Reliable EBSD analysis of the whole cross section can be obtained...

Transmission Electron Microscopy (TEM) Sample Preparation of Si(1-x)Gex in c-Plane Sapphire Substrate

Science.gov (United States)

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.

Molecularly imprinted polymers for sample preparation and biosensing in food analysis: Progress and perspectives

DEFF Research Database (Denmark)

Ashley, Jon; Shahbazi, Mohammad-Ali; Kant, Krishna

2017-01-01

Molecularly imprinted polymers (MIPs) are biomimetics which can selectively bind to analytes of interest. One of the most interesting areas where MIPs have shown the biggest potential is food analysis. MIPs have found use as sorbents in sample preparation attributed to the high selectivity and high...... the imprinting methods which are applicable for imprinting food templates, summarize the recent progress in using MIPs for preparing and analysing food samples, and discuss the current limitations in the commercialisation of MIPs technology. Finally, future perspectives will be given....

An On-Target Desalting and Concentration Sample Preparation Protocol for MALDI-MS and MS/MS Analysis

DEFF Research Database (Denmark)

Zhang, Xumin; Wang, Quanhui; Lou, Xiaomin

2012-01-01

2DE coupled with MALDI-MS is one of the most widely used and powerful analytic technologies in proteomics study. The MALDI sample preparation method has been developed and optimized towards the combination of simplicity, sample-cleaning, and sample concentration since its introduction. Here we...... present a protocol of the so-called Sample loading, Matrix loading, and on-target Wash (SMW) method which fulfills the three criteria by taking advantage of the AnchorChip™ targets. Our method is extremely simple and no pre-desalting or concentration is needed when dealing with samples prepared from 2DE...

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

Science.gov (United States)

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.

Atomic absorption determination of metals in soils using ultrasonic sample preparation

International Nuclear Information System (INIS)

Chmilenko, F.A.; Smityuk, N.M.; Baklanov, A.N.

2002-01-01

It was shown that ultrasonic treatment accelerates sample preparation of soil extracts from chernozem into different solvents by a factor of 6 to 60. These extracts are used for the atomic absorption determination of soluble species of Cd, Co, Cr, Cu, Ni, Pb, and Zn. The optimum ultrasound parameters (frequency, intensity, and treatment time) were found for preparing soil extracts containing analytes in concentrations required in agrochemical procedures. Different extractants used to extract soluble heavy metals from soils of an ordinary chernozem type in agrochemical procedures using ultrasonic treatment were classified in accordance with the element nature [ru

9 CFR 147.8 - Procedures for preparing egg yolk samples for diagnostic tests.

Science.gov (United States)

2010-01-01

... 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... for diagnostic testing. (b) The authorized laboratory must identify each egg as to the breeding flock...

Analytical sample preparation strategies for the determination of antimalarial drugs in human whole blood, plasma and urine

DEFF Research Database (Denmark)

Casas, Monica Escolà; Hansen, Martin; Krogh, Kristine A

2014-01-01

the available sample preparation strategies combined with liquid chromatographic (LC) analysis to determine antimalarials in whole blood, plasma and urine published over the last decade. Sample preparation can be done by protein precipitation, solid-phase extraction, liquid-liquid extraction or dilution. After...

A Simple and Reproducible Method to Prepare Membrane Samples from Freshly Isolated Rat Brain Microvessels.

Science.gov (United States)

Brzica, Hrvoje; Abdullahi, Wazir; Reilly, Bianca G; Ronaldson, Patrick T

2018-05-07

The blood-brain barrier (BBB) is a dynamic barrier tissue that responds to various pathophysiological and pharmacological stimuli. Such changes resulting from these stimuli can greatly modulate drug delivery to the brain and, by extension, cause considerable challenges in the treatment of central nervous system (CNS) diseases. Many BBB changes that affect pharmacotherapy, involve proteins that are localized and expressed at the level of endothelial cells. Indeed, such knowledge on BBB physiology in health and disease has sparked considerable interest in the study of these membrane proteins. From a basic science research standpoint, this implies a requirement for a simple but robust and reproducible method for isolation of microvessels from brain tissue harvested from experimental animals. In order to prepare membrane samples from freshly isolated microvessels, it is essential that sample preparations be enriched in endothelial cells but limited in the presence of other cell types of the neurovascular unit (i.e., astrocytes, microglia, neurons, pericytes). An added benefit is the ability to prepare samples from individual animals in order to capture the true variability of protein expression in an experimental population. In this manuscript, details regarding a method that is utilized for isolation of rat brain microvessels and preparation of membrane samples are provided. Microvessel enrichment, from samples derived, is achieved by using four centrifugation steps where dextran is included in the sample buffer. This protocol can easily be adapted by other laboratories for their own specific applications. Samples generated from this protocol have been shown to yield robust experimental data from protein analysis experiments that can greatly aid the understanding of BBB responses to physiological, pathophysiological, and pharmacological stimuli.

Improvement of a sample preparation method assisted by sodium deoxycholate for mass-spectrometry-based shotgun membrane proteomics.

Science.gov (United States)

Lin, Yong; Lin, Haiyan; Liu, Zhonghua; Wang, Kunbo; Yan, Yujun

2014-11-01

In current shotgun-proteomics-based biological discovery, the identification of membrane proteins is a challenge. This is especially true for integral membrane proteins due to their highly hydrophobic nature and low abundance. Thus, much effort has been directed at sample preparation strategies such as use of detergents, chaotropes, and organic solvents. We previously described a sample preparation method for shotgun membrane proteomics, the sodium deoxycholate assisted method, which cleverly circumvents many of the challenges associated with traditional sample preparation methods. However, the method is associated with significant sample loss due to the slightly weaker extraction/solubilization ability of sodium deoxycholate when it is used at relatively low concentrations such as 1%. Hence, we present an enhanced sodium deoxycholate sample preparation strategy that first uses a high concentration of sodium deoxycholate (5%) to lyse membranes and extract/solubilize hydrophobic membrane proteins, and then dilutes the detergent to 1% for a more efficient digestion. We then applied the improved method to shotgun analysis of proteins from rat liver membrane enriched fraction. Compared with other representative sample preparation strategies including our previous sodium deoxycholate assisted method, the enhanced sodium deoxycholate method exhibited superior sensitivity, coverage, and reliability for the identification of membrane proteins particularly those with high hydrophobicity and/or multiple transmembrane domains. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

Energy Technology Data Exchange (ETDEWEB)

Jubin, Robert Thomas [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Bruffey, Stephanie H. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Jordan, Jacob A. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

2017-10-01

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

Paper-Based Analytical Device for Zinc Ion Quantification in Water Samples with Power-Free Analyte Concentration

Directory of Open Access Journals (Sweden)

Hiroko Kudo

2017-04-01

Full Text Available Insufficient sensitivity is a general issue of colorimetric paper-based analytical devices (PADs for trace analyte detection, such as metal ions, in environmental water. This paper demonstrates the colorimetric detection of zinc ions (Zn2+ on a paper-based analytical device with an integrated analyte concentration system. Concentration of Zn2+ ions from an enlarged sample volume (1 mL has been achieved with the aid of a colorimetric Zn2+ indicator (Zincon electrostatically immobilized onto a filter paper substrate in combination with highly water-absorbent materials. Analyte concentration as well as sample pretreatment, including pH adjustment and interferent masking, has been elaborated. The resulting device enables colorimetric quantification of Zn2+ in environmental water samples (tap water, river water from a single sample application. The achieved detection limit of 0.53 μM is a significant improvement over that of a commercial colorimetric Zn2+ test paper (9.7 μM, demonstrating the efficiency of the developed analyte concentration system not requiring any equipment.

Collection and preparation of marine samples for radionuclide analysis

International Nuclear Information System (INIS)

Holm, E.

1997-01-01

The ultimate goal of research in radioecology is to be able to predict the pathways of radioactive material in the environment and hence estimate possible doses to the population in various regions. Knowledge of levels of contamination are necessary to maintain control of operations of nuclear facilities. Correct methods of sample collection, handling and preparation are among the most important parts for a correct assessment. On basis of the final results of radionuclide concentrations, scientific, medical and political decisions are taken. (author)

Preparing Monodisperse Macromolecular Samples for Successful Biological Small-Angle X-ray and Neutron Scattering Experiments

Science.gov (United States)

Jeffries, Cy M.; Graewert, Melissa A.; Blanchet, Clément E.; Langley, David B.; Whitten, Andrew E.; Svergun, Dmitri I

2017-01-01

Small-angle X-ray and neutron scattering (SAXS and SANS) are techniques used to extract structural parameters and determine the overall structures and shapes of biological macromolecules, complexes and assemblies in solution. The scattering intensities measured from a sample contain contributions from all atoms within the illuminated sample volume including the solvent and buffer components as well as the macromolecules of interest. In order to obtain structural information, it is essential to prepare an exactly matched solvent blank so that background scattering contributions can be accurately subtracted from the sample scattering to obtain the net scattering from the macromolecules in the sample. In addition, sample heterogeneity caused by contaminants, aggregates, mismatched solvents, radiation damage or other factors can severely influence and complicate data analysis so it is essential that the samples are pure and monodisperse for the duration of the experiment. This Protocol outlines the basic physics of SAXS and SANS and reveals how the underlying conceptual principles of the techniques ultimately ‘translate’ into practical laboratory guidance for the production of samples of sufficiently high quality for scattering experiments. The procedure describes how to prepare and characterize protein and nucleic acid samples for both SAXS and SANS using gel electrophoresis, size exclusion chromatography and light scattering. Also included are procedures specific to X-rays (in-line size exclusion chromatography SAXS) and neutrons, specifically preparing samples for contrast matching/variation experiments and deuterium labeling of proteins. PMID:27711050

Sulfonate-terminated carbosilane dendron-coated nanotubes: a greener point of view in protein sample preparation.

Science.gov (United States)

González-García, Estefanía; Gutiérrez Ulloa, Carlos E; de la Mata, Francisco Javier; Marina, María Luisa; García, María Concepción

2017-09-01

Reduction or removal of solvents and reagents in protein sample preparation is a requirement. Dendrimers can strongly interact with proteins and have great potential as a greener alternative to conventional methods used in protein sample preparation. This work proposes the use of single-walled carbon nanotubes (SWCNTs) functionalized with carbosilane dendrons with sulfonate groups for protein sample preparation and shows the successful application of the proposed methodology to extract proteins from a complex matrix. SEM images of nanotubes and mixtures of nanotubes and proteins were taken. Moreover, intrinsic fluorescence intensity of proteins was monitored to observe the most significant interactions at increasing dendron generations under neutral and basic pHs. Different conditions for the disruption of interactions between proteins and nanotubes after protein extraction and different concentrations of the disrupting reagent and the nanotube were also tried. Compatibility of extraction and disrupting conditions with the enzymatic digestion of proteins for obtaining bioactive peptides was also studied. Finally, sulfonate-terminated carbosilane dendron-coated SWCNTs enabled the extraction of proteins from a complex sample without using non-environmentally friendly solvents that were required so far. Graphical Abstract Green protein extraction from a complex sample employing carbosilane dendron coated nanotubes.

Preparation Of Deposited Sediment Sample By Casting Method For Environmental Study

International Nuclear Information System (INIS)

Hutabarat, Tommy; Ristin PI, Evarista

2000-01-01

The preparation of deposited sediment sample by c asting m ethod for environmental study has been carried out. This method comprises separation of size fraction and casting process. The deposited sediment samples were wet sieved to separate the size fraction of >500 mum, (250-500) mum, (125-250) mum and (63-125) mum and settling procedures were followed for the separation of (40-63) mum, (20-40) mum, (10-20) mum and o C, ashed at 450 o C, respectively. In the casting process of sample, it was used polyester rapid cure resin and methyl ethyl ketone peroxide (MEKP) hardener. The moulded sediment sample was poured onto caster, allow for 60 hours long. The aim of this method is to get the casted sample which can be used effectively, efficiently and to be avoided from contamination of each other samples. Before casting, samples were grinded up to be fine. The result shows that casting product is ready to be used for natural radionuclide analysis

Minimizing technical variation during sample preparation prior to label-free quantitative mass spectrometry.

Science.gov (United States)

Scheerlinck, E; Dhaenens, M; Van Soom, A; Peelman, L; De Sutter, P; Van Steendam, K; Deforce, D

2015-12-01

Sample preparation is the crucial starting point to obtain high-quality mass spectrometry data and can be divided into two main steps in a bottom-up proteomics approach: cell/tissue lysis with or without detergents and a(n) (in-solution) digest comprising denaturation, reduction, alkylation, and digesting of the proteins. Here, some important considerations, among others, are that the reagents used for sample preparation can inhibit the digestion enzyme (e.g., 0.1% sodium dodecyl sulfate [SDS] and 0.5 M guanidine HCl), give rise to ion suppression (e.g., polyethylene glycol [PEG]), be incompatible with liquid chromatography-tandem mass spectrometry (LC-MS/MS) (e.g., SDS), and can induce additional modifications (e.g., urea). Taken together, all of these irreproducible effects are gradually becoming a problem when label-free quantitation of the samples is envisioned such as during the increasingly popular high-definition mass spectrometry (HDMS(E)) and sequential window acquisition of all theoretical fragment ion spectra (SWATH) data-independent acquisition strategies. Here, we describe the detailed validation of a reproducible method with sufficient protein yield for sample preparation without any known LC-MS/MS interfering substances by using 1% sodium deoxycholate (SDC) during both cell lysis and in-solution digest. Copyright © 2015 The Authors. Published by Elsevier Inc. All rights reserved.

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

Science.gov (United States)

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

2018-05-15

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

Use of passive sampling devices for monitoring and compliance checking of POP concentrations in water

NARCIS (Netherlands)

Lohmann, R.; Booij, K.; Smedes, F.; Vrana, B.

2012-01-01

The state of the art of passive water sampling of (nonpolar) organic contaminants is presented. Its suitability for regulatory monitoring is discussed, with an emphasis on the information yielded by passive sampling devices (PSDs), their relevance and associated uncertainties. Almost all persistent

A Microfluidic Device for Preparing Next Generation DNA Sequencing Libraries and for Automating Other Laboratory Protocols That Require One or More Column Chromatography Steps

Science.gov (United States)

Tan, Swee Jin; Phan, Huan; Gerry, Benjamin Michael; Kuhn, Alexandre; Hong, Lewis Zuocheng; Min Ong, Yao; Poon, Polly Suk Yean; Unger, Marc Alexander; Jones, Robert C.; Quake, Stephen R.; Burkholder, William F.

2013-01-01

Library preparation for next-generation DNA sequencing (NGS) remains a key bottleneck in the sequencing process which can be relieved through improved automation and miniaturization. We describe a microfluidic device for automating laboratory protocols that require one or more column chromatography steps and demonstrate its utility for preparing Next Generation sequencing libraries for the Illumina and Ion Torrent platforms. Sixteen different libraries can be generated simultaneously with significantly reduced reagent cost and hands-on time compared to manual library preparation. Using an appropriate column matrix and buffers, size selection can be performed on-chip following end-repair, dA tailing, and linker ligation, so that the libraries eluted from the chip are ready for sequencing. The core architecture of the device ensures uniform, reproducible column packing without user supervision and accommodates multiple routine protocol steps in any sequence, such as reagent mixing and incubation; column packing, loading, washing, elution, and regeneration; capture of eluted material for use as a substrate in a later step of the protocol; and removal of one column matrix so that two or more column matrices with different functional properties can be used in the same protocol. The microfluidic device is mounted on a plastic carrier so that reagents and products can be aliquoted and recovered using standard pipettors and liquid handling robots. The carrier-mounted device is operated using a benchtop controller that seals and operates the device with programmable temperature control, eliminating any requirement for the user to manually attach tubing or connectors. In addition to NGS library preparation, the device and controller are suitable for automating other time-consuming and error-prone laboratory protocols requiring column chromatography steps, such as chromatin immunoprecipitation. PMID:23894273

A microfluidic device for preparing next generation DNA sequencing libraries and for automating other laboratory protocols that require one or more column chromatography steps.

Directory of Open Access Journals (Sweden)

Swee Jin Tan

Full Text Available Library preparation for next-generation DNA sequencing (NGS remains a key bottleneck in the sequencing process which can be relieved through improved automation and miniaturization. We describe a microfluidic device for automating laboratory protocols that require one or more column chromatography steps and demonstrate its utility for preparing Next Generation sequencing libraries for the Illumina and Ion Torrent platforms. Sixteen different libraries can be generated simultaneously with significantly reduced reagent cost and hands-on time compared to manual library preparation. Using an appropriate column matrix and buffers, size selection can be performed on-chip following end-repair, dA tailing, and linker ligation, so that the libraries eluted from the chip are ready for sequencing. The core architecture of the device ensures uniform, reproducible column packing without user supervision and accommodates multiple routine protocol steps in any sequence, such as reagent mixing and incubation; column packing, loading, washing, elution, and regeneration; capture of eluted material for use as a substrate in a later step of the protocol; and removal of one column matrix so that two or more column matrices with different functional properties can be used in the same protocol. The microfluidic device is mounted on a plastic carrier so that reagents and products can be aliquoted and recovered using standard pipettors and liquid handling robots. The carrier-mounted device is operated using a benchtop controller that seals and operates the device with programmable temperature control, eliminating any requirement for the user to manually attach tubing or connectors. In addition to NGS library preparation, the device and controller are suitable for automating other time-consuming and error-prone laboratory protocols requiring column chromatography steps, such as chromatin immunoprecipitation.

Challenges of biological sample preparation for SIMS imaging of elements and molecules at subcellular resolution

International Nuclear Information System (INIS)

Chandra, Subhash

2008-01-01

Secondary ion mass spectrometry (SIMS) based imaging techniques capable of subcellular resolution characterization of elements and molecules are becoming valuable tools in many areas of biology and medicine. Due to high vacuum requirements of SIMS, the live cells cannot be analyzed directly in the instrument. The sample preparation, therefore, plays a critical role in preserving the native chemical composition for SIMS analysis. This work focuses on the evaluation of frozen-hydrated and frozen freeze-dried sample preparations for SIMS studies of cultured cells with a CAMECA IMS-3f dynamic SIMS ion microscope instrument capable of producing SIMS images with a spatial resolution of 500 nm. The sandwich freeze-fracture method was used for fracturing the cells. The complimentary fracture planes in the plasma membrane were characterized by field-emission secondary electron microscopy (FESEM) in the frozen-hydrated state. The cells fractured at the dorsal surface were used for SIMS analysis. The frozen-hydrated SIMS analysis of individual cells under dynamic primary ion beam (O 2 + ) revealed local secondary ion signal enhancements correlated with the water image signals of 19 (H 3 O) + . A preferential removal of water from the frozen cell matrix in the Z-axis was also observed. These complications render the frozen-hydrated sample type less desirable for subcellular dynamic SIMS studies. The freeze-drying of frozen-hydrated cells, either inside the instrument or externally in a freeze-drier, allowed SIMS imaging of subcellular chemical composition. Morphological evaluations of fractured freeze-dried cells with SEM and confocal laser scanning microscopy (CLSM) revealed well-preserved mitochondria, Golgi apparatus, and stress fibers. SIMS analysis of fractured freeze-dried cells revealed well-preserved chemical composition of even the most highly diffusible ions like K + and Na + in physiologically relevant concentrations. The high K-low Na signature in individual cells

Challenges of biological sample preparation for SIMS imaging of elements and molecules at subcellular resolution

Science.gov (United States)

Chandra, Subhash

2008-12-01

Secondary ion mass spectrometry (SIMS) based imaging techniques capable of subcellular resolution characterization of elements and molecules are becoming valuable tools in many areas of biology and medicine. Due to high vacuum requirements of SIMS, the live cells cannot be analyzed directly in the instrument. The sample preparation, therefore, plays a critical role in preserving the native chemical composition for SIMS analysis. This work focuses on the evaluation of frozen-hydrated and frozen freeze-dried sample preparations for SIMS studies of cultured cells with a CAMECA IMS-3f dynamic SIMS ion microscope instrument capable of producing SIMS images with a spatial resolution of 500 nm. The sandwich freeze-fracture method was used for fracturing the cells. The complimentary fracture planes in the plasma membrane were characterized by field-emission secondary electron microscopy (FESEM) in the frozen-hydrated state. The cells fractured at the dorsal surface were used for SIMS analysis. The frozen-hydrated SIMS analysis of individual cells under dynamic primary ion beam (O 2+) revealed local secondary ion signal enhancements correlated with the water image signals of 19(H 3O) +. A preferential removal of water from the frozen cell matrix in the Z-axis was also observed. These complications render the frozen-hydrated sample type less desirable for subcellular dynamic SIMS studies. The freeze-drying of frozen-hydrated cells, either inside the instrument or externally in a freeze-drier, allowed SIMS imaging of subcellular chemical composition. Morphological evaluations of fractured freeze-dried cells with SEM and confocal laser scanning microscopy (CLSM) revealed well-preserved mitochondria, Golgi apparatus, and stress fibers. SIMS analysis of fractured freeze-dried cells revealed well-preserved chemical composition of even the most highly diffusible ions like K + and Na + in physiologically relevant concentrations. The high K-low Na signature in individual cells

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

Science.gov (United States)

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.

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

International Nuclear Information System (INIS)

Sydoff, Marie; Stenstroem, Kristina

2010-01-01

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 14 C 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.

Preparation and performance optimization of TPBISi green-light organic luminescent material devices

Directory of Open Access Journals (Sweden)

Zheng Huajing

2017-01-01

Full Text Available The Study analyzed and tested the absorption spectrum, photoluminescence spectrum, and device’s electroluminescence spectrum of a new silole material. The device with Silol as an emitting layer, emitted green-light whose structure is ITO/NPB/2,2,3,3-tetraphenyl-4,4-bisthienylsilole(TPBTSi/Alq3/Mg: A by improvement of preparation technology and optimization of thin film. It reaches the maximum luminescence of 11290.2 cd/m2, the maximum luminous efficiency of 0.84 lm/W, luminescence spectrum of 516 nm, chromaticity diagram CIE coordinate of(0.275, 0.4568 when voltage is 15V. All of the above is the green characteristic spectrum of TPBTSi.

The role of sample preparation in interpretation of trace element concentration variability in moss bioindication studies

Science.gov (United States)

Migaszewski, Z.M.; Lamothe, P.J.; Crock, J.G.; Galuszka, A.; Dolegowska, S.

2011-01-01

Trace element concentrations in plant bioindicators are often determined to assess the quality of the environment. Instrumental methods used for trace element determination require digestion of samples. There are different methods of sample preparation for trace element analysis, and the selection of the best method should be fitted for the purpose of a study. Our hypothesis is that the method of sample preparation is important for interpretation of the results. Here we compare the results of 36 element determinations performed by ICP-MS on ashed and on acid-digested (HNO3, H2O2) samples of two moss species (Hylocomium splendens and Pleurozium schreberi) collected in Alaska and in south-central Poland. We found that dry ashing of the moss samples prior to analysis resulted in considerably lower detection limits of all the elements examined. We also show that this sample preparation technique facilitated the determination of interregional and interspecies differences in the chemistry of trace elements. Compared to the Polish mosses, the Alaskan mosses displayed more positive correlations of the major rock-forming elements with ash content, reflecting those elements' geogenic origin. Of the two moss species, P. schreberi from both Alaska and Poland was also highlighted by a larger number of positive element pair correlations. The cluster analysis suggests that the more uniform element distribution pattern of the Polish mosses primarily reflects regional air pollution sources. Our study has shown that the method of sample preparation is an important factor in statistical interpretation of the results of trace element determinations. ?? 2010 Springer-Verlag.

VAPOR SAMPLING DEVICE FOR INTERFACE WITH MICROTOX ASSAY FOR SCREENING TOXIC INDUSTRIAL CHEMICALS

Science.gov (United States)

A time-integrated sampling system interfaced with a toxicity-based assay is reported for monitoring volatile toxic industrial chemicals (TICs). Semipermeable membrane devices (SPMDs) using dimethyl sulfoxide (DMSO) as the fill solvent accumulated each of 17 TICs from the vapor...

Sample preparation for the HAW project and experimental results from the HFR

International Nuclear Information System (INIS)

Garcia Celma, A.; Wees, H. van; Miralles, L.

1990-09-01

This report deals with the preparation and analysis of samples, during the period May 1989-November 1989, for the High-Active Waste (HAW) project, a large-scale in situ test being performed underground in the Asse salt mine, Remlingen FRG. The development of the technical procedures required, and the scientific results, which regard mostly characterization of Potasas del Llobregat sample, are reported. Prior to using the samples in both the H.A.W. and the H.F.R. experiments they have to be machined to fit their holders. Technical improvements for machining samples of salt are reported. (H.W.). 9 refs.; 68 figs.; 10 tabs

Sample preparation method for ICP-MS measurement of 99Tc in a large amount of environmental samples

International Nuclear Information System (INIS)

Kondo, M.; Seki, R.

2002-01-01

Sample preparation for measurement of 99 Tc in a large amount of soil and water samples by ICP-MS has been developed using 95m Tc as a yield tracer. This method is based on the conventional method for a small amount of soil samples using incineration, acid digestion, extraction chromatography (TEVA resin) and ICP-MS measurement. Preliminary concentration of Tc has been introduced by co-precipitation with ferric oxide. The matrix materials in a large amount of samples were more sufficiently removed with keeping the high recovery of Tc than previous method. The recovery of Tc was 70-80% for 100 g soil samples and 60-70% for 500 g of soil and 500 L of water samples. The detection limit of this method was evaluated as 0.054 mBq/kg in 500 g soil and 0.032 μBq/L in 500 L water. The determined value of 99 Tc in the IAEA-375 (soil sample collected near the Chernobyl Nuclear Reactor) was 0.25 ± 0.02 Bq/kg. (author)

A critical review of microextraction by packed sorbent as a sample preparation approach in drug bioanalysis.

Science.gov (United States)

Alves, Gilberto; Rodrigues, Márcio; Fortuna, Ana; Falcão, Amílcar; Queiroz, João

2013-06-01

Sample preparation is widely accepted as the most labor-intensive and error-prone part of the bioanalytical process. The recent advances in this field have been focused on the miniaturization and integration of sample preparation online with analytical instrumentation, in order to reduce laboratory workload and increase analytical performance. From this perspective, microextraction by packed sorbent (MEPS) has emerged in the last few years as a powerful sample preparation approach suitable to be easily automated with liquid and gas chromatographic systems applied in a variety of bioanalytical areas (pharmaceutical, clinical, toxicological, environmental and food research). This paper aims to provide an overview and a critical discussion of recent bioanalytical methods reported in literature based on MEPS, with special emphasis on those developed for the quantification of therapeutic drugs and/or metabolites in biological samples. The advantages and some limitations of MEPS, as well as its comparison with other extraction techniques, are also addressed herein.

Quality Assessment of Platelet-Rich Fibrin-Like Matrix Prepared from Whole Blood Samples after Extended Storage

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Hideo Kawabata

2017-09-01

Full Text Available The platelet-rich fibrin–like matrix (PRFM is usually prepared onsite and immediately used for regenerative therapy. Nonetheless, to meet the clinical necessity of preserving the PRFM without quality deterioration, we developed a method for preparation of PRFMs from short-term-stored whole blood (WB samples. In this study, to evaluate the practical expiration date of storage, we extended the storage time of WB samples from 2 to 7 days and assessed the quality of the resulting PRFMs. WB samples collected with acid-citrate-dextrose were stored with gentle agitation at ambient temperature. To prepare PRFMs, the stored WB samples were mixed with CaCl2 in glass tubes and centrifuged. Fibrin fiber networks, CD41 and CD62P expression, and Platelet Derived Growth Factor-BB (PDGF-BB levels were examined by scanning electron microscopy (SEM, flow cytometry, and an Enzyme-Linked ImmunoSorbent Assay (ELISA, respectively. Long-term storage had no significant effect on either blood cell counts or platelet functions tested. The resulting PRFMs were visually identical to freshly prepared ones. PDGF-BB levels did not markedly decrease in a time-dependent manner. However, fibrin fibers gradually became thinner after storage. Although the coagulation activity may diminish, we propose that PRFMs can be prepared—without evident loss of quality—from WB samples stored for up to 7 days by our previously developed method.

14CO2 analysis of soil gas: Evaluation of sample size limits and sampling devices

Science.gov (United States)

Wotte, Anja; Wischhöfer, Philipp; Wacker, Lukas; Rethemeyer, Janet

2017-12-01

Radiocarbon (14C) analysis of CO2 respired from soils or sediments is a valuable tool to identify different carbon sources. The collection and processing of the CO2, however, is challenging and prone to contamination. We thus continuously improve our handling procedures and present a refined method for the collection of even small amounts of CO2 in molecular sieve cartridges (MSCs) for accelerator mass spectrometry 14C analysis. Using a modified vacuum rig and an improved desorption procedure, we were able to increase the CO2 recovery from the MSC (95%) as well as the sample throughput compared to our previous study. By processing series of different sample size, we show that our MSCs can be used for CO2 samples of as small as 50 μg C. The contamination by exogenous carbon determined in these laboratory tests, was less than 2.0 μg C from fossil and less than 3.0 μg C from modern sources. Additionally, we tested two sampling devices for the collection of CO2 samples released from soils or sediments, including a respiration chamber and a depth sampler, which are connected to the MSC. We obtained a very promising, low process blank for the entire CO2 sampling and purification procedure of ∼0.004 F14C (equal to 44,000 yrs BP) and ∼0.003 F14C (equal to 47,000 yrs BP). In contrast to previous studies, we observed no isotopic fractionation towards lighter δ13C values during the passive sampling with the depth samplers.

Soil and Water – What is Detectable through Microbiological Sample Preparation Techniques

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The concerns of a potential terrorist’s use of biological agents in soil and ground water are articulated by comparisons to major illnesses in this Country involving contaminated drinking water sources. Objectives are focused on the importance of sample preparation in the rapid, ...

Fluoroquinolone antibiotics in environmental waters: sample preparation and determination.

Science.gov (United States)

Speltini, Andrea; Sturini, Michela; Maraschi, Federica; Profumo, Antonella

2010-04-01

The aim of this review is to provide a general overview on the analytical methods proposed in the last decade for trace fluoroquinolone (FQ) determination in environmental waters. A large number of studies have been developed on this topic in reason of the importance of their monitoring in the studies of environmental mobility and potential degradation pathways. Every step of the analysis has been carefully considered, with a particular attention to sample preparation, in relationship with the problems involved in the analysis of real matrices. The different strategies to minimise interference from organic matter and to achieve optimal sensitivity, especially important in those samples with lower FQ concentrations, were also highlighted. Results and progress in this field have been described and critically commented. Moreover, a worldwide overview on the presence of FQs in the environmental waters has been reported.

Ultrasonic-based membrane aided sample preparation of urine proteomes.

Science.gov (United States)

Jesus, Jemmyson Romário; Santos, Hugo M; López-Fernández, H; Lodeiro, Carlos; Arruda, Marco Aurélio Zezzi; Capelo, J L

2018-02-01

A new ultrafast ultrasonic-based method for shotgun proteomics as well as label-free protein quantification in urine samples is developed. The method first separates the urine proteins using nitrocellulose-based membranes and then proteins are in-membrane digested using trypsin. The enzymatic digestion process is accelerated from overnight to four minutes using a sonoreactor ultrasonic device. Overall, the sample treatment pipeline comprising protein separation, digestion and identification is done in just 3h. The process is assessed using urine of healthy volunteers. The method shows that male can be differentiated from female using the protein content of urine in a fast, easy and straightforward way. 232 and 226 proteins are identified in urine of male and female, respectively. From this, 162 are common to both genders, whilst 70 are unique to male and 64 to female. From the 162 common proteins, 13 are present at levels statistically different (p minimalism concept as outlined by Halls, as each stage of this analysis is evaluated to minimize the time, cost, sample requirement, reagent consumption, energy requirements and production of waste products. Copyright © 2017 Elsevier B.V. All rights reserved.