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Sample records for automated sample preparation

  1. 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

  2. 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.

  3. Sample preparation automation for dosing plutonium in urine

    International Nuclear Information System (INIS)

    Jeanmaire, Lucien; Ballada, Jean; Ridelle Berger, Ariane

    1969-06-01

    After having indicated that dosing urinary plutonium by using the Henry technique can be divided into three stages (plutonium concentration by precipitation, passing the solution on an anionic resin column and plutonium elution, and eluate evaporation to obtain a source of which the radioactivity is measured), and recalled that the automation of the second stage has been reported in another document, this document describes the automation of the first stage, i.e. obtaining from urine a residue containing the plutonium, and sufficiently mineralized to be analyzed by means of ion exchanging resins. Two techniques are proposed, leading to slightly different devices. The different operations to be performed are indicated. The different components of the apparatus are described: beakers, hot plate stirrers, reagent circuits, a system for supernatant suction, and a control-command circuit. The operation and use are then described, and results are given

  4. An Automated Sample Preparation System for Large-Scale DNA Sequencing

    Science.gov (United States)

    Marziali, Andre; Willis, Thomas D.; Federspiel, Nancy A.; Davis, Ronald W.

    1999-01-01

    Recent advances in DNA sequencing technologies, both in the form of high lane-density gels and automated capillary systems, will lead to an increased requirement for sample preparation systems that operate at low cost and high throughput. As part of the development of a fully automated sequencing system, we have developed an automated subsystem capable of producing 10,000 sequence-ready ssDNA templates per day from libraries of M13 plaques at a cost of $0.29 per sample. This Front End has been in high throughput operation since June, 1997 and has produced > 400,000 high-quality DNA templates. PMID:10330125

  5. 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)

  6. 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.

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

    DEFF Research Database (Denmark)

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

    multiplexing readouts, but this has a natural limitation. High-content screening via image acquisition and analysis allows multiplexing of few parameters, but is connected to substantial time consumption and complex logistics. We report on integration of Reverse Phase Protein Arrays (RPPA)-based readouts...... 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...

  8. 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......High-throughput screening of genome wide siRNA- or compound libraries is currently applied for drug target and drug discovery. Commonly, these approaches deal with sample numbers ranging from 100,000 to several millions. Efforts to decrease costs and to increase information gained include......-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...

  9. 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.

  10. A simple and automated sample preparation system for subsequent halogens determination: Combustion followed by pyrohydrolysis.

    Science.gov (United States)

    Pereira, L S F; Pedrotti, M F; Vecchia, P Dalla; Pereira, J S F; Flores, E M M

    2018-06-20

    A simple and automated system based on combustion followed by a pyrohydrolysis reaction was proposed for further halogens determination. This system was applied for digestion of soils containing high (90%) and also low (10%) organic matter content for further halogens determination. The following parameters were evaluated: sample mass, use of microcrystalline cellulose and heating time. For analytes absorption, a diluted alkaline solution (6 mL of 25 mmol L -1  NH 4 OH) was used in all experiments. Up to 400 mg of soil with high organic matter content and 100 mg of soil with low organic matter content (mixed with 400 mg of cellulose) could be completely digested using the proposed system. Quantitative results for all halogens were obtained using less than 12 min of sample preparation step (about 1.8 min for sample combustion and 10 min for pyrohydrolysis). The accuracy was evaluated using a certified reference material of coal and spiked samples. No statistical difference was observed between the certified values and results obtained by the proposed method. Additionally, the recoveries obtained using spiked samples were in the range of 98-103% with relative standard deviation values lower than 5%. The limits of quantification obtained for F, Cl, Br and I for soil with high (400 mg of soil) and low (100 mg of soil) organic matter were in the range of 0.01-2 μg g -1 and 0.07-59 μg g -1 , respectively. The proposed system was considered as a simple and suitable alternative for soils digestion for further halogens determination by ion chromatography and inductively coupled plasma mass spectrometry techniques. Copyright © 2018 Elsevier B.V. All rights reserved.

  11. 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

    -mass spectrometry using several preparation techniques, including protein precipitation, solid-phase extraction and centrifugation, without any manual intervention. Pipetting of a known aliquot of whole blood was achieved by integrating a balance and performing gravimetric measurements. The system was able......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...... to handle 1,073 of 1,092 (98.3%) samples of whole blood from forensic material, including postmortem samples, without any need for repeating sample preparation. Only three samples required special treatment such as dilution. The addition of internal and calibration standards were validated by pipetting...

  12. 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

  13. Automated Gel Size Selection to Improve the Quality of Next-generation Sequencing Libraries Prepared from Environmental Water Samples.

    Science.gov (United States)

    Uyaguari-Diaz, Miguel I; Slobodan, Jared R; Nesbitt, Matthew J; Croxen, Matthew A; Isaac-Renton, Judith; Prystajecky, Natalie A; Tang, Patrick

    2015-04-17

    Next-generation sequencing of environmental samples can be challenging because of the variable DNA quantity and quality in these samples. High quality DNA libraries are needed for optimal results from next-generation sequencing. Environmental samples such as water may have low quality and quantities of DNA as well as contaminants that co-precipitate with DNA. The mechanical and enzymatic processes involved in extraction and library preparation may further damage the DNA. Gel size selection enables purification and recovery of DNA fragments of a defined size for sequencing applications. Nevertheless, this task is one of the most time-consuming steps in the DNA library preparation workflow. The protocol described here enables complete automation of agarose gel loading, electrophoretic analysis, and recovery of targeted DNA fragments. In this study, we describe a high-throughput approach to prepare high quality DNA libraries from freshwater samples that can be applied also to other environmental samples. We used an indirect approach to concentrate bacterial cells from environmental freshwater samples; DNA was extracted using a commercially available DNA extraction kit, and DNA libraries were prepared using a commercial transposon-based protocol. DNA fragments of 500 to 800 bp were gel size selected using Ranger Technology, an automated electrophoresis workstation. Sequencing of the size-selected DNA libraries demonstrated significant improvements to read length and quality of the sequencing reads.

  14. Automated Sample Preparation for Radiogenic and Non-Traditional Metal Isotopes: Removing an Analytical Barrier for High Sample Throughput

    Science.gov (United States)

    Field, M. Paul; Romaniello, Stephen; Gordon, Gwyneth W.; Anbar, Ariel D.; Herrmann, Achim; Martinez-Boti, Miguel A.; Anagnostou, Eleni; Foster, Gavin L.

    2014-05-01

    MC-ICP-MS has dramatically improved the analytical throughput for high-precision radiogenic and non-traditional isotope ratio measurements, compared to TIMS. The generation of large data sets, however, remains hampered by tedious manual drip chromatography required for sample purification. A new, automated chromatography system reduces the laboratory bottle neck and expands the utility of high-precision isotope analyses in applications where large data sets are required: geochemistry, forensic anthropology, nuclear forensics, medical research and food authentication. We have developed protocols to automate ion exchange purification for several isotopic systems (B, Ca, Fe, Cu, Zn, Sr, Cd, Pb and U) using the new prepFAST-MC™ (ESI, Nebraska, Omaha). The system is not only inert (all-flouropolymer flow paths), but is also very flexible and can easily facilitate different resins, samples, and reagent types. When programmed, precise and accurate user defined volumes and flow rates are implemented to automatically load samples, wash the column, condition the column and elute fractions. Unattended, the automated, low-pressure ion exchange chromatography system can process up to 60 samples overnight. Excellent reproducibility, reliability, recovery, with low blank and carry over for samples in a variety of different matrices, have been demonstrated to give accurate and precise isotopic ratios within analytical error for several isotopic systems (B, Ca, Fe, Cu, Zn, Sr, Cd, Pb and U). This illustrates the potential of the new prepFAST-MC™ (ESI, Nebraska, Omaha) as a powerful tool in radiogenic and non-traditional isotope research.

  15. 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.

  16. Automation and integration of multiplexed on-line sample preparation with capillary electrophoresis for DNA sequencing

    Energy Technology Data Exchange (ETDEWEB)

    Tan, H.

    1999-03-31

    The purpose of this research is to develop a multiplexed sample processing system in conjunction with multiplexed capillary electrophoresis for high-throughput DNA sequencing. The concept from DNA template to called bases was first demonstrated with a manually operated single capillary system. Later, an automated microfluidic system with 8 channels based on the same principle was successfully constructed. The instrument automatically processes 8 templates through reaction, purification, denaturation, pre-concentration, injection, separation and detection in a parallel fashion. A multiplexed freeze/thaw switching principle and a distribution network were implemented to manage flow direction and sample transportation. Dye-labeled terminator cycle-sequencing reactions are performed in an 8-capillary array in a hot air thermal cycler. Subsequently, the sequencing ladders are directly loaded into a corresponding size-exclusion chromatographic column operated at {approximately} 60 C for purification. On-line denaturation and stacking injection for capillary electrophoresis is simultaneously accomplished at a cross assembly set at {approximately} 70 C. Not only the separation capillary array but also the reaction capillary array and purification columns can be regenerated after every run. DNA sequencing data from this system allow base calling up to 460 bases with accuracy of 98%.

  17. 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.

  18. Automated Sample Preparation Platform for Mass Spectrometry-Based Plasma Proteomics and Biomarker Discovery

    Directory of Open Access Journals (Sweden)

    Vilém Guryča

    2014-03-01

    Full Text Available The identification of novel biomarkers from human plasma remains a critical need in order to develop and monitor drug therapies for nearly all disease areas. The discovery of novel plasma biomarkers is, however, significantly hampered by the complexity and dynamic range of proteins within plasma, as well as the inherent variability in composition from patient to patient. In addition, it is widely accepted that most soluble plasma biomarkers for diseases such as cancer will be represented by tissue leakage products, circulating in plasma at low levels. It is therefore necessary to find approaches with the prerequisite level of sensitivity in such a complex biological matrix. Strategies for fractionating the plasma proteome have been suggested, but improvements in sensitivity are often negated by the resultant process variability. Here we describe an approach using multidimensional chromatography and on-line protein derivatization, which allows for higher sensitivity, whilst minimizing the process variability. In order to evaluate this automated process fully, we demonstrate three levels of processing and compare sensitivity, throughput and reproducibility. We demonstrate that high sensitivity analysis of the human plasma proteome is possible down to the low ng/mL or even high pg/mL level with a high degree of technical reproducibility.

  19. Automated multi-dimensional liquid chromatography : sample preparation and identification of peptides from human blood filtrate

    NARCIS (Netherlands)

    Machtejevas, Egidijus; John, Harald; Wagner, Knut; Standker, Ludger; Marko-Varga, Gyorgy; Georg Forssmann, Wolf; Bischoff, Rainer; K. Unger, Klaus

    2004-01-01

    A comprehensive on-line sample clean-up with an integrated two-dimensional HPLC system was developed for the analysis of natural peptides. Samples comprised of endogenous peptides with molecular weights up to 20 kDa were generated from human hemofiltrate (HF) obtained from patients with chronic

  20. 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.

  1. 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.

  2. Automated radioanalytical system incorporating microwave-assisted sample preparation, chemical separation, and online radiometric detection for the monitoring of total 99Tc in nuclear waste processing streams.

    Science.gov (United States)

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

    2012-04-03

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

  3. Automated column liquid chromatographic determination of amoxicillin and cefadroxil in bovine serum and muscle tissue using on-line dialysis for sample preparation

    NARCIS (Netherlands)

    Snippe, N; van de Merbel, N C; Ruiter, F P; Steijger, O M; Lingeman, H; Brinkman, U A

    1994-01-01

    A fully automated method is described for the determination of amoxicillin and cefadroxil in bovine serum and muscle tissue. The method is based on the on-line combination of dialysis and solid-phase extraction for sample preparation, and column liquid chromatography with ultraviolet detection. In

  4. Automated microfluidic sample-preparation platform for high-throughput structural investigation of proteins by small-angle X-ray scattering

    DEFF Research Database (Denmark)

    Lafleur, Josiane P.; Snakenborg, Detlef; Nielsen, Søren Skou

    2011-01-01

    A new microfluidic sample-preparation system is presented for the structural investigation of proteins using small-angle X-ray scattering (SAXS) at synchrotrons. The system includes hardware and software features for precise fluidic control, sample mixing by diffusion, automated X-ray exposure...... control, UV absorbance measurements and automated data analysis. As little as 15 l of sample is required to perform a complete analysis cycle, including sample mixing, SAXS measurement, continuous UV absorbance measurements, and cleaning of the channels and X-ray cell with buffer. The complete analysis...... cycle can be performed in less than 3 min. Bovine serum albumin was used as a model protein to characterize the mixing efficiency and sample consumption of the system. The N2 fragment of an adaptor protein (p120-RasGAP) was used to demonstrate how the device can be used to survey the structural space...

  5. Reducing the cost of semi-automated in-gel tryptic digestion and GeLC sample preparation for high-throughput proteomics.

    Science.gov (United States)

    Ruelcke, Jayde E; Loo, Dorothy; Hill, Michelle M

    2016-10-21

    Peptide generation by trypsin digestion is typically the first step in mass spectrometry-based proteomics experiments, including 'bottom-up' discovery and targeted proteomics using multiple reaction monitoring. Manual tryptic digest and the subsequent clean-up steps can add variability even before the sample reaches the analytical platform. While specialized filter plates and tips have been designed for automated sample processing, the specialty reagents required may not be accessible or feasible due to their high cost. Here, we report a lower-cost semi-automated protocol for in-gel digestion and GeLC using standard 96-well microplates. Further cost savings were realized by re-using reagent tips with optimized sample ordering. To evaluate the methodology, we compared a simple mixture of 7 proteins and a complex cell-lysate sample. The results across three replicates showed that our semi-automated protocol had performance equal to or better than a manual in-gel digestion with respect to replicate variability and level of contamination. In this paper, we also provide the Agilent Bravo method file, which can be adapted to other liquid handlers. The simplicity, reproducibility, and cost-effectiveness of our semi-automated protocol make it ideal for routine in-gel and GeLC sample preparations, as well as high throughput processing of large clinical sample cohorts. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Automated solid-phase extraction for trace-metal analysis of seawater: sample preparation for total-reflection X-ray fluorescence measurements

    Science.gov (United States)

    Gerwinski, Wolfgang; Schmidt, Diether

    1998-08-01

    Solid-phase chromatography on silica gel columns can be used as a sample preparation technique for seawater, followed by total-reflection X-ray fluorescence analysis (TXRF). An automated extraction system (Zymark AutoTrace SPE Workstation) was studied for the analysis of blank solutions, seawater samples and certified reference materials. After replacing some stainless steel parts in the system, adequate blanks could be obtained to allow the analysis of seawater samples. Replicate analyses yielded low standard deviations and good recoveries for certified reference materials. Using a six-channel model and user-defined software, the time needed for a complete analytical run was about 100 min.

  7. 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.

  8. Manual versus automated blood sampling

    DEFF Research Database (Denmark)

    Teilmann, A C; Kalliokoski, Otto; Sørensen, Dorte B

    2014-01-01

    corticosterone metabolites, and expressed more anxious behavior than did the mice of the other groups. Plasma corticosterone levels of mice subjected to tail blood sampling were also elevated, although less significantly. Mice subjected to automated blood sampling were less affected with regard to the parameters......Facial vein (cheek blood) and caudal vein (tail blood) phlebotomy are two commonly used techniques for obtaining blood samples from laboratory mice, while automated blood sampling through a permanent catheter is a relatively new technique in mice. The present study compared physiological parameters......, glucocorticoid dynamics as well as the behavior of mice sampled repeatedly for 24 h by cheek blood, tail blood or automated blood sampling from the carotid artery. Mice subjected to cheek blood sampling lost significantly more body weight, had elevated levels of plasma corticosterone, excreted more fecal...

  9. 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.

  10. Influence of sample preparation and reliability of automated numerical refocusing in stain-free analysis of dissected tissues with quantitative phase digital holographic microscopy

    Science.gov (United States)

    Kemper, Björn; Lenz, Philipp; Bettenworth, Dominik; Krausewitz, Philipp; Domagk, Dirk; Ketelhut, Steffi

    2015-05-01

    Digital holographic microscopy (DHM) has been demonstrated to be a versatile tool for high resolution non-destructive quantitative phase imaging of surfaces and multi-modal minimally-invasive monitoring of living cell cultures in-vitro. DHM provides quantitative monitoring of physiological processes through functional imaging and structural analysis which, for example, gives new insight into signalling of cellular water permeability and cell morphology changes due to toxins and infections. Also the analysis of dissected tissues quantitative DHM phase contrast prospects application fields by stain-free imaging and the quantification of tissue density changes. We show that DHM allows imaging of different tissue layers with high contrast in unstained tissue sections. As the investigation of fixed samples represents a very important application field in pathology, we also analyzed the influence of the sample preparation. The retrieved data demonstrate that the quality of quantitative DHM phase images of dissected tissues depends strongly on the fixing method and common staining agents. As in DHM the reconstruction is performed numerically, multi-focus imaging is achieved from a single digital hologram. Thus, we evaluated the automated refocussing feature of DHM for application on different types of dissected tissues and revealed that on moderately stained samples highly reproducible holographic autofocussing can be achieved. Finally, it is demonstrated that alterations of the spatial refractive index distribution in murine and human tissue samples represent a reliable absolute parameter that is related of different degrees of inflammation in experimental colitis and Crohn's disease. This paves the way towards the usage of DHM in digital pathology for automated histological examinations and further studies to elucidate the translational potential of quantitative phase microscopy for the clinical management of patients, e.g., with inflammatory bowel disease.

  11. 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.

  12. Microfluidic Sample Preparation for Diagnostic Cytopathology

    Science.gov (United States)

    Mach, Albert J.; Adeyiga, Oladunni B.; Di Carlo, Dino

    2014-01-01

    The cellular components of body fluids are routinely analyzed to identify disease and treatment approaches. While significant focus has been placed on developing cell analysis technologies, tools to automate the preparation of cellular specimens have been more limited, especially for body fluids beyond blood. Preparation steps include separating, concentrating, and exposing cells to reagents. Sample preparation continues to be routinely performed off-chip by technicians, preventing cell-based point-of-care diagnostics, increasing the cost of tests, and reducing the consistency of the final analysis following multiple manually-performed steps. Here, we review the assortment of biofluids for which suspended cells are analyzed, along with their characteristics and diagnostic value. We present an overview of the conventional sample preparation processes for cytological diagnosis. We finally discuss the challenges and opportunities in developing microfluidic devices for the purpose of automating or miniaturizing these processes, with particular emphases on preparing large or small volume samples, working with samples of high cellularity, automating multi-step processes, and obtaining high purity subpopulations of cells. We hope to convey the importance of and help identify new research directions addressing the vast biological and clinical applications in preparing and analyzing the array of available biological fluids. Successfully addressing the challenges described in this review can lead to inexpensive systems to improve diagnostic accuracy while simultaneously reducing overall systemic healthcare costs. PMID:23380972

  13. Automated system for fractionation of blood samples

    Energy Technology Data Exchange (ETDEWEB)

    Lee, N. E.; Genung, R. K.; Johnson, W. F.; Mrochek, J. E.; Scott, C. D.

    1978-01-01

    A prototype system for preparing multiple fractions of blood components (plasma, washed red cells, and hemolysates) using automated techniques has been developed. The procedure is based on centrifugal separation and differential pressure-induced transfer in a rotor that has been designed to process numerous samples simultaneously. Red cells are sedimented against the outer walls of the sample chamber, and plasma is syphoned, by imposition of eithr a slight positive or negative pressure, into individual reservoirs in a collection ring. Washing of cells is performed in situ; samples of washed cells, either packed or in saline solution, can be recovered. Cellular hemolysates are prepared and automatically transferred to individual, commercially available collection vials ready for storage in liquid nitrogen or immediate analysis. The system has potential application in any biomedical area which requires high sample throughput and in which one or more of the blood fractions will be used. A separate unit has been designed and developed for the semiautomated cleaning of the blood processing vessel.

  14. Preparing the Nurse for Automation

    OpenAIRE

    Cumber, Denny

    1981-01-01

    The introduction of a computerized clinical information system into the hospital environment requires nursing involvement from the planning stages throughout implementation. Nurses are the largest segment of the health work force to be affected by the introduction of a new system. They are also the largest group of non-computer users. This paper discusses the preparation of the nursing staff at The Fairfax Hospital, a large community hospital, to accept the use of the computer as a tool in th...

  15. Non-Contact Conductivity Measurement for Automated Sample Processing Systems

    Science.gov (United States)

    Beegle, Luther W.; Kirby, James P.

    2012-01-01

    A new method has been developed for monitoring and control of automated sample processing and preparation especially focusing on desalting of samples before analytical analysis (described in more detail in Automated Desalting Apparatus, (NPO-45428), NASA Tech Briefs, Vol. 34, No. 8 (August 2010), page 44). The use of non-contact conductivity probes, one at the inlet and one at the outlet of the solid phase sample preparation media, allows monitoring of the process, and acts as a trigger for the start of the next step in the sequence (see figure). At each step of the muti-step process, the system is flushed with low-conductivity water, which sets the system back to an overall low-conductivity state. This measurement then triggers the next stage of sample processing protocols, and greatly minimizes use of consumables. In the case of amino acid sample preparation for desalting, the conductivity measurement will define three key conditions for the sample preparation process. First, when the system is neutralized (low conductivity, by washing with excess de-ionized water); second, when the system is acidified, by washing with a strong acid (high conductivity); and third, when the system is at a basic condition of high pH (high conductivity). Taken together, this non-contact conductivity measurement for monitoring sample preparation will not only facilitate automation of the sample preparation and processing, but will also act as a way to optimize the operational time and use of consumables

  16. 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.

  17. PROJECT ENGINEERING DATA MANAGEMENT AT AUTOMATED PREPARATION OF DESIGN DOCUMENTATION

    Directory of Open Access Journals (Sweden)

    A. V. Guryanov

    2017-01-01

    Full Text Available We have developed and realized instrumental means for automated support of end-to-end design process for design documentation on a product at the programming level. The proposed decision is based on processing of the engineering project data that are contained in interdependent design documents: tactical technical characteristics of products, data on the valuable metals contained in them, the list of components applied in a product and others. Processing of engineering data is based on their conversion to the form provided by requirements of industry standards for design documentation preparation. The general graph of the design documentation developed on a product is provided. The description of the developed software product is given. Automated preparation process of interdependent design documents is shown on the example of preparation of purchased products list. Results of work can be used in case of research and development activities on creation of perspective samples of ADP equipment.

  18. 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.

  19. Recent advances in column switching sample preparation in bioanalysis.

    Science.gov (United States)

    Kataoka, Hiroyuki; Saito, Keita

    2012-04-01

    Column switching techniques, using two or more stationary phase columns, are useful for trace enrichment and online automated sample preparation. Target fractions from the first column are transferred online to a second column with different properties for further separation. Column switching techniques can be used to determine the analytes in a complex matrix by direct sample injection or by simple sample treatment. Online column switching sample preparation is usually performed in combination with HPLC or capillary electrophoresis. SPE or turbulent flow chromatography using a cartridge column and in-tube solid-phase microextraction using a capillary column have been developed for convenient column switching sample preparation. Furthermore, various micro-/nano-sample preparation devices using new polymer-coating materials have been developed to improve extraction efficiency. This review describes current developments and future trends in novel column switching sample preparation in bioanalysis, focusing on innovative column switching techniques using new extraction devices and materials.

  20. Automated sampling and control of gaseous simulations

    KAUST Repository

    Huang, Ruoguan

    2013-05-04

    In this work, we describe a method that automates the sampling and control of gaseous fluid simulations. Several recent approaches have provided techniques for artists to generate high-resolution simulations based on a low-resolution simulation. However, often in applications the overall flow in the low-resolution simulation that an animator observes and intends to preserve is composed of even lower frequencies than the low resolution itself. In such cases, attempting to match the low-resolution simulation precisely is unnecessarily restrictive. We propose a new sampling technique to efficiently capture the overall flow of a fluid simulation, at the scale of user\\'s choice, in such a way that the sampled information is sufficient to represent what is virtually perceived and no more. Thus, by applying control based on the sampled data, we ensure that in the resulting high-resolution simulation, the overall flow is matched to the low-resolution simulation and the fine details on the high resolution are preserved. The samples we obtain have both spatial and temporal continuity that allows smooth keyframe matching and direct manipulation of visible elements such as smoke density through temporal blending of samples. We demonstrate that a user can easily configure a simulation with our system to achieve desired results. © 2013 Springer-Verlag Berlin Heidelberg.

  1. On the development of automatic sample preparation devices

    International Nuclear Information System (INIS)

    Oesselmann, J.

    1987-01-01

    Modern mass spectrometers for stable isotope analysis offer accurate isotope ratio results from gaseous samples (CO 2 , N 2 , H 2 , SO 2 ) in a completely automated fashion. However, most samples of interest either are associated with contaminant gases or the gas has to be liberated by a chemical procedure prior to measurement. In most laboratories this sample preparation step is performed manually. As a consequence, sample throughput is rather low and - despite skilful operation - the preparation procedure varies slightly from one sample to the next affecting mainly the reproducibility of the data. (author)

  2. 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...

  3. High throughput sample processing and automated scoring

    Directory of Open Access Journals (Sweden)

    Gunnar eBrunborg

    2014-10-01

    Full Text Available The comet assay is a sensitive and versatile method for assessing DNA damage in cells. In the traditional version of the assay, there are many manual steps involved and few samples can be treated in one experiment. High throughput modifications have been developed during recent years, and they are reviewed and discussed. These modifications include accelerated scoring of comets; other important elements that have been studied and adapted to high throughput are cultivation and manipulation of cells or tissues before and after exposure, and freezing of treated samples until comet analysis and scoring. High throughput methods save time and money but they are useful also for other reasons: large-scale experiments may be performed which are otherwise not practicable (e.g., analysis of many organs from exposed animals, and human biomonitoring studies, and automation gives more uniform sample treatment and less dependence on operator performance. The high throughput modifications now available vary largely in their versatility, capacity, complexity and costs. The bottleneck for further increase of throughput appears to be the scoring.

  4. 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...

  5. 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).

  6. Automated Cable Preparation for Robotized Stator Cable Winding

    Directory of Open Access Journals (Sweden)

    Erik Hultman

    2017-04-01

    Full Text Available A method for robotized cable winding of the Uppsala University Wave Energy Converter generator stator has previously been presented and validated. The purpose of this study is to present and validate further developments to the method: automated stand-alone equipment for the preparation of the winding cables. The cable preparation consists of three parts: feeding the cable from a drum, forming the cable end and cutting the cable. Forming and cutting the cable was previously done manually and only small cable drums could be handled. Therefore the robot cell needed to be stopped frequently. The new equipment was tested in an experimental robot stator cable winding setup. Through the experiments, the equipment was validated to be able to perform fully automated and robust cable preparation. Suggestions are also given on how to further develop the equipment with regards to performance, robustness and quality. Hence, this work represents another important step towards demonstrating completely automated robotized stator cable winding.

  7. Automated blood sampling systems for positron emission tomography

    International Nuclear Information System (INIS)

    Eriksson, L.; Holte, S.; Bohm, C.; Kesselberg, M.; Hovander, B.

    1988-01-01

    An automated blood sampling system has been constructed and evaluated. Two different detector units in the blood sampling system are compared. Results from studies of blood-brain barrier transfer of a C-11 labelled receptor antagonist will be discussed

  8. [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.

  9. The MEGAPIE PIE sample preparation

    International Nuclear Information System (INIS)

    Wohlmuther, M.; Boutellier, V.; Dai, Y.; Gavillet, D.; Geissmann, K.; Hahl, S.; Hammer, B.; Lagotzki, A.; Leu, H.; Linder, H.P.; Kalt, A.; Kuster, D.; Neuhausen, J.; Schumann, D.; Schwarz, R.; Schweikert, H.; Spahr, A.; Suter, P.; Teichmann, S.; Thomsen, K.; Wiese, H.; Wagner, W.; Zimmermann, U.; Zumbach, C.

    2015-01-01

    On the way towards Accelerator-driven Systems (ADS), the MEGAPIE (Mega-Watt Pilot Experiment) project is one of the key milestones. The MEGAPIE project aimed to prove that a liquid Lead-Bismuth-Eutectic (LBE) spallation target can be licensed, planned, built, operated, dismantled, examined and disposed. The project has finished the phase of producing the samples for Post-irradiation Examination (PIE). Samples to study structural material property changes due to the harsh environment of high temperatures, contact with flowing liquid metal (LBE), proton and neutron irradiation will be investigated by all partner laboratories (CEA, CNRS, ENEA, KIT, PSI and SCK-CEN). (authors)

  10. 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

  11. A 3D Printer Enabled, High Performing, Microgravity Compatible, and Versatile Sample Preparation Platform, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — AI Biosciences proposes to demonstrate the ability of a microgravity-compatible, compact, light-weight, and automated versatile sample preparation platform (VSPP)...

  12. Robotic, MEMS-based Multi Utility Sample Preparation Instrument for ISS Biological Workstation, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — This project will develop a multi-functional, automated sample preparation instrument for biological wet-lab workstations on the ISS. The instrument is based on a...

  13. 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

  14. 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)

  15. 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

  16. 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.

  17. INFORMATION SYSTEM OF AUTOMATION OF PREPARATION EDUCATIONAL PROCESS DOCUMENTS

    Directory of Open Access Journals (Sweden)

    V. A. Matyushenko

    2016-01-01

    Full Text Available Information technology is rapidly conquering the world, permeating all spheres of human activity. Education is not an exception. An important direction of information of education is the development of university management systems. Modern information systems improve and facilitate the management of all types of activities of the institution. The purpose of this paper is development of system, which allows automating process of formation of accounting documents. The article describes the problem of preparation of the educational process documents. Decided to project and create the information system in Microsoft Access environment. The result is four types of reports obtained by using the developed system. The use of this system now allows you to automate the process and reduce the effort required to prepare accounting documents. All reports was implement in Microsoft Excel software product and can be used for further analysis and processing.

  18. Automation of a dust sampling train | Akinola | Journal of Modeling ...

    African Journals Online (AJOL)

    The results obtained from this work show that the flue gas sampling process can be automated using microprocessor-based control system and a sampling train. Using the sampling train developed by the British Coal Utilization Research Association (BCURA) with both the internal and external flow-meter arrangements, the ...

  19. Sample preparation in biological mass spectrometry

    CERN Document Server

    Ivanov, Alexander R

    2011-01-01

    The aim of this book is to provide the researcher with important sample preparation strategies in a wide variety of analyte molecules, specimens, methods, and biological applications requiring mass spectrometric analysis as a detection end-point.

  20. Novel diffusion cell for in vitro transdermal permeation, compatible with automated dynamic sampling

    NARCIS (Netherlands)

    Bosman, I.J; Lawant, A.L; Avegaart, S.R.; Ensing, K; de Zeeuw, R.A

    The development of a new diffusion cell for in vitro transdermal permeation is described. The so-called Kelder cells were used in combination with the ASPEC system (Automatic Sample Preparation with Extraction Columns), which is designed for the automation of solid-phase extractions (SPE). Instead

  1. 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

  2. Screening library evolution through automation of solution preparation.

    Science.gov (United States)

    Schopfer, U; Höhn, F; Hueber, M; Girod, M; Engeloch, C; Popov, M; Muckenschnabel, I

    2007-08-01

    The quality of the compound library is a critical success factor in every high-throughput screening campaign. Screening solutions have to be prepared with a high level of process control to ensure the correct identity and initial concentration of each compound. However, even under optimized storage conditions, a certain level of degradation in solution cannot be avoided. Therefore, regular quality control and eventual removal of solutions from the screening deck is necessary. Because solution preparation, especially the weighing of compounds, is a tedious and often manual task, a regular resolubilization of compounds is difficult to achieve. By complete automation of the solution preparation, the authors have laid the foundation for a life cycle management of screening solutions. They demonstrate how a combination of quality and process control leads to a continuous improvement of the screening library. In presenting an automation concept, they show how a series of innovative process optimizations led to a high-performance system that achieves full industrialization of solution preparation.

  3. 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

  4. 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

  5. Reagent preparation and storage for amplification of microarray hybridization targets with a fully automated system.

    Science.gov (United States)

    Zhou, Mingjie; Marlowe, Jon; Graves, Jaime; Dahl, Jason; Riley, Zackery; Tian, Lena; Duenwald, Sven; Tokiwa, George; Fare, Thomas L

    2007-08-01

    The advent of automated systems for gene expression profiling has accentuated the need for the development of convenient and cost-effective methods for reagent preparation. We have developed a method for the preparation and storage of pre-aliquoted cocktail plates that contain all reagents required for amplification of nucleic acid by reverse transcription and in vitro transcription reactions. Plates can be stored at -80 degrees C for at least 1 month and kept in a hotel at 4 degrees C for at least 24 h prior to use. Microarray data quality generated from these pre-aliquoted reagent plates is not statistically different between cRNA amplified with stored cocktails and cRNA amplified with freshly prepared cocktails. Deployment of pre-aliquoted, stored cocktail plates in a fully automated system not only increases the throughput of amplifying cRNA targets from thousands of RNA samples, but could also considerably reduce reagent costs and potentially improve process robustness.

  6. Automated 741 document preparation: Oak Ridge National Laboratory's Automated Safeguards Information System (OASIS)

    International Nuclear Information System (INIS)

    Austin, H.C.; Gray, L.M.

    1982-01-01

    OASIS has been providing for Oak Ridge National Laboratory's total safeguards needs since being place on line in April 1980. The system supports near real-time nuclear materials safeguards and accountability control. The original design of OASIS called for an automated facsimile of a 741 document to be prepared as a functional by-product of updating the inventory. An attempt was made to utilize, intact, DOE-Albuquerque's automated 741 system to generate the facsimile; however, the five page document produced proved too cumbersome. Albuquerque's programs were modified to print an original 741 document utilizing standard DOE/NRC 741 forms. It is felt that the best features of both the automated and manually generated 741 documents have been incorporated. Automation of the source data for 741 shipping documents produces greater efficiency while reducing possible errors. Through utilization of the standard DOE/NRC form, continuity within the NMMSS system is maintained, thus minimizing the confusion and redundancy associated with facsimiles. OASIS now fulfills the original concept of near real-time accountability by furnishing a viable 741 document as a function of updating the inventory

  7. 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.

  8. Sample preparation for SEM of plant surfaces

    OpenAIRE

    A.K. Pathan; J. Bond; R.E. Gaskin

    2010-01-01

    Plant tissues must be dehydrated for observation in most electron microscopes. Although a number of sample processing techniques have been developed for preserving plant tissues in their original form and structure, none of them are guaranteed artefact-free. The current paper reviews common scanning electron microscopy techniques and the sample preparation methods employed for visualisation of leaves under specific types of electron microscopes. Common artefacts introduced by specific techniq...

  9. Automated spike preparation system for Isotope Dilution Mass Spectrometry (IDMS)

    International Nuclear Information System (INIS)

    Maxwell, S.L. III; Clark, J.P.

    1990-01-01

    Isotope Dilution Mass Spectrometry (IDMS) is a method frequently employed to measure dissolved, irradiated nuclear materials. A known quantity of a unique isotope of the element to be measured (referred to as the ''spike'') is added to the solution containing the analyte. The resulting solution is chemically purified then analyzed by mass spectrometry. By measuring the magnitude of the response for each isotope and the response for the ''unique spike'' then relating this to the known quantity of the ''spike'', the quantity of the nuclear material can be determined. An automated spike preparation system was developed at the Savannah River Site (SRS) to dispense spikes for use in IDMS analytical methods. Prior to this development, technicians weighed each individual spike manually to achieve the accuracy required. This procedure was time-consuming and subjected the master stock solution to evaporation. The new system employs a high precision SMI Model 300 Unipump dispenser interfaced with an electronic balance and a portable Epson HX-20 notebook computer to automate spike preparation

  10. Preparation of samples for coal analysis

    Energy Technology Data Exchange (ETDEWEB)

    Moucada, E.; Pazos, C.

    1986-11-01

    Taking and preparing coal samples for analysis is fundamental to obtaining reliable data. The sensitivity and precision of the monitoring equipment (calorimeters, devices for measuring sulphur content and for immediate elemental analysis, etc) are of little use if the samples analysed, normally less than 1 g, are not representative of the batch from which they are taken, a batch usually being of several tonnes. Moreover, as even the slightest error in results has major economic repercussions for the suppliers (mining companies) and buyers (power stations, cement works, etc), it is clear that sound criteria for use in the selection of equipment and sampling and preparation methods are of prime importance. The aim of this article is to give a general survey of this process describing the fundamental characteristics of each stage and, in terms of these, to provide basic selection criteria for the equipment. 5 refs., 15 figs., 1 tab.

  11. 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.

  12. 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.

  13. 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.

  14. Semi-automated library preparation for high-throughput DNA sequencing platforms.

    Science.gov (United States)

    Farias-Hesson, Eveline; Erikson, Jonathan; Atkins, Alexander; Shen, Peidong; Davis, Ronald W; Scharfe, Curt; Pourmand, Nader

    2010-01-01

    Next-generation sequencing platforms are powerful technologies, providing gigabases of genetic information in a single run. An important prerequisite for high-throughput DNA sequencing is the development of robust and cost-effective preprocessing protocols for DNA sample library construction. Here we report the development of a semi-automated sample preparation protocol to produce adaptor-ligated fragment libraries. Using a liquid-handling robot in conjunction with Carboxy Terminated Magnetic Beads, we labeled each library sample using a unique 6 bp DNA barcode, which allowed multiplex sample processing and sequencing of 32 libraries in a single run using Applied Biosystems' SOLiD sequencer. We applied our semi-automated pipeline to targeted medical resequencing of nuclear candidate genes in individuals affected by mitochondrial disorders. This novel method is capable of preparing as much as 32 DNA libraries in 2.01 days (8-hour workday) for emulsion PCR/high throughput DNA sequencing, increasing sample preparation production by 8-fold.

  15. Evaluation and optimisation of preparative semi-automated electrophoresis systems for Illumina library preparation.

    Science.gov (United States)

    Quail, Michael A; Gu, Yong; Swerdlow, Harold; Mayho, Matthew

    2012-12-01

    Size selection can be a critical step in preparation of next-generation sequencing libraries. Traditional methods employing gel electrophoresis lack reproducibility, are labour intensive, do not scale well and employ hazardous interchelating dyes. In a high-throughput setting, solid-phase reversible immobilisation beads are commonly used for size-selection, but result in quite a broad fragment size range. We have evaluated and optimised the use of two semi-automated preparative DNA electrophoresis systems, the Caliper Labchip XT and the Sage Science Pippin Prep, for size selection of Illumina sequencing libraries. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. An automated blood sampling system used in positron emission tomography

    International Nuclear Information System (INIS)

    Eriksson, L.; Bohm, C.; Kesselberg, M.

    1988-01-01

    Fast dynamic function studies with positron emission tomography (PET), has the potential to give accurate information of physiological functions of the brain. This capability can be realised if the positron camera system accurately quantitates the tracer uptake in the brain with sufficiently high efficiency and in sufficiently short time intervals. However, in addition, the tracer concentration in blood, as a function of time, must be accurately determined. This paper describes and evaluates an automated blood sampling system. Two different detector units are compared. The use of the automated blood sampling system is demonstrated in studies of cerebral blood flow, in studies of the blood-brain barrier transfer of amino acids and of the cerebral oxygen consumption. 5 refs.; 7 figs

  17. Optimizing centrifugation of coagulation samples in laboratory automation.

    Science.gov (United States)

    Suchsland, Juliane; Friedrich, Nele; Grotevendt, Anne; Kallner, Anders; Lüdemann, Jan; Nauck, Matthias; Petersmann, Astrid

    2014-08-01

    High acceleration centrifugation conditions are used in laboratory automation systems to reduce the turnaround time (TAT) of clinical chemistry samples, but not of coagulation samples. This often requires separate sample flows. The CLSI guideline and manufacturers recommendations for coagulation assays aim at reducing platelet counts. For measurement of prothrombin time (PT) and activated partial thromboplastin time (APTT) platelet counts (Plt) below 200×10(9)/L are recommended. Other coagulation assays may require even lower platelet counts, e.g., less than 10 × 10(9)/L. Unifying centrifugation conditions can facilitate the integration of coagulation samples in the overall workflow of a laboratory automation system. We evaluated centrifugation conditions of coagulation samples by using high acceleration centrifugation conditions (5 min; 3280×g) in a single and two consecutive runs. RESULTS of coagulation assays [PT, APTT, coagulation factor VIII (F. VIII) and protein S] and platelet counts were compared after the first and second centrifugation. Platelet counts below 200×10(9)/L were obtained in all samples after the first centrifugation and less than 10 × 10(9)/L was obtained in 73% of the samples after a second centrifugation. Passing-Bablok regression analyses showed an equal performance of PT, APTT and F. VIII after first and second centrifugation whereas protein S measurements require a second centrifugation. Coagulation samples can be integrated into the workflow of a laboratory automation system using high acceleration centrifugation. A single centrifugation was sufficient for PT, APTT and F. VIII whereas two successive centrifugations appear to be sufficient for protein S activity.

  18. Scanning Electron Microscopy Sample Preparation and Imaging.

    Science.gov (United States)

    Nguyen, Jenny Ngoc Tran; Harbison, Amanda M

    2017-01-01

    Scanning electron microscopes allow us to reach magnifications of 20-130,000× and resolve compositional and topographical images with intense detail. These images are created by bombarding a sample with electrons in a focused manner to generate a black and white image from the electrons that bounce off of the sample. The electrons are detected using positively charged detectors. Scanning electron microscopy permits three-dimensional imaging of desiccated specimens or wet cells and tissues by using variable pressure chambers. SEM ultrastructural analysis and intracellular imaging supplement light microscopy for molecular profiling of prokaryotes, plants, and mammals. This chapter demonstrates how to prepare and image samples that are (a) desiccated and conductive, (b) desiccated and nonconductive but coated with an electron conductive film using a gold sputter coater, and (c) wet and maintained in a hydrated state using a Deben Coolstage.

  19. 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)

  20. Applications of monolithic materials for sample preparation.

    Science.gov (United States)

    Nema, Tarang; Chan, Eric C Y; Ho, Paul C

    2014-01-01

    Recent advances in monolithic columns have made them an alternative to traditional packed columns used in liquid chromatography as well as capillary electrochromatography (CEC). The monolithic columns have been extensively studied and shown to possess several advantages that make them a promising and potential substitute for the particle packed columns. A large number of papers relating to monolithic columns have been published every year, focusing on different preparation techniques, characteristic evaluations as well as applications. This review highlighted the latest development of monoliths for other modes of analytical chemistry. In particular, this review will highlight the application of monoliths for sample preparation which is an important step of the entire analysis. Copyright © 2013 Elsevier B.V. All rights reserved.

  1. Trends and applications of integrated automated ultra-trace sample handling and analysis (T9)

    International Nuclear Information System (INIS)

    Kingston, H.M.S.; Ye Han; Stewart, L.; Link, D.

    2002-01-01

    Full text: Automated analysis, sub-ppt detection limits, and the trend toward speciated analysis (rather than just elemental analysis) force the innovation of sophisticated and integrated sample preparation and analysis techniques. Traditionally, the ability to handle samples at ppt and sub-ppt levels has been limited to clean laboratories and special sample handling techniques and equipment. The world of sample handling has passed a threshold where older or 'old fashioned' traditional techniques no longer provide the ability to see the sample due to the influence of the analytical blank and the fragile nature of the analyte. When samples require decomposition, extraction, separation and manipulation, application of newer more sophisticated sample handling systems are emerging that enable ultra-trace analysis and species manipulation. In addition, new instrumentation has emerged which integrate sample preparation and analysis to enable on-line near real-time analysis. Examples of those newer sample-handling methods will be discussed and current examples provided as alternatives to traditional sample handling. Two new techniques applying ultra-trace microwave energy enhanced sample handling have been developed that permit sample separation and refinement while performing species manipulation during decomposition. A demonstration, that applies to semiconductor materials, will be presented. Next, a new approach to the old problem of sample evaporation without losses will be demonstrated that is capable of retaining all elements and species tested. Both of those methods require microwave energy manipulation in specialized systems and are not accessible through convection, conduction, or other traditional energy applications. A new automated integrated method for handling samples for ultra-trace analysis has been developed. An on-line near real-time measurement system will be described that enables many new automated sample handling and measurement capabilities. This

  2. 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)

  3. Automating Groundwater Sampling At Hanford, The Next Step

    International Nuclear Information System (INIS)

    Connell, C.W.; Conley, S.F.; Hildebrand, R.D.; Cunningham, D.E.

    2010-01-01

    Historically, the groundwater monitoring activities at the Department of Energy's Hanford Site in southeastern Washington State have been very 'people intensive.' Approximately 1500 wells are sampled each year by field personnel or 'samplers.' These individuals have been issued pre-printed forms showing information about the well(s) for a particular sampling evolution. This information is taken from 2 official electronic databases: the Hanford Well information System (HWIS) and the Hanford Environmental Information System (HEIS). The samplers used these hardcopy forms to document the groundwater samples and well water-levels. After recording the entries in the field, the samplers turned the forms in at the end of the day and other personnel posted the collected information onto a spreadsheet that was then printed and included in a log book. The log book was then used to make manual entries of the new information into the software application(s) for the HEIS and HWIS databases. A pilot project for automating this extremely tedious process was lauched in 2008. Initially, the automation was focused on water-level measurements. Now, the effort is being extended to automate the meta-data associated with collecting groundwater samples. The project allowed electronic forms produced in the field by samplers to be used in a work flow process where the data is transferred to the database and electronic form is filed in managed records - thus eliminating manually completed forms. Elimating the manual forms and streamlining the data entry not only improved the accuracy of the information recorded, but also enhanced the efficiency and sampling capacity of field office personnel.

  4. 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.

  5. 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.

  6. Human mixed lymphocyte cultures. Evaluation of microculture technique utilizing the multiple automated sample harvester (MASH)

    Science.gov (United States)

    Thurman, G. B.; Strong, D. M.; Ahmed, A.; Green, S. S.; Sell, K. W.; Hartzman, R. J.; Bach, F. H.

    1973-01-01

    Use of lymphocyte cultures for in vitro studies such as pretransplant histocompatibility testing has established the need for standardization of this technique. A microculture technique has been developed that has facilitated the culturing of lymphocytes and increased the quantity of cultures feasible, while lowering the variation between replicate samples. Cultures were prepared for determination of tritiated thymidine incorporation using a Multiple Automated Sample Harvester (MASH). Using this system, the parameters that influence the in vitro responsiveness of human lymphocytes to allogeneic lymphocytes have been investigated. PMID:4271568

  7. 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

  8. 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...

  9. Automated high-resolution NMR with a sample changer

    International Nuclear Information System (INIS)

    Wade, C.G.; Johnson, R.D.; Philson, S.B.; Strouse, J.; McEnroe, F.J.

    1989-01-01

    Within the past two years, it has become possible to obtain high-resolution NMR spectra using automated commercial instrumentation. Software control of all spectrometer functions has reduced most of the tedious manual operations to typing a few computer commands or even making selections from a menu. Addition of an automatic sample changer is the next natural step in improving efficiency and sample throughput; it has a significant (and even unexpected) impact on how NMR laboratories are run and how it is taught. Such an instrument makes even sophisticated experiments routine, so that people with no previous exposure to NMR can run these experiments after a training session of an hour or less. This A/C Interface examines the impact of such instrumentation on both the academic and the industrial laboratory

  10. 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...

  11. Adapting RNAseq sample preparation for ISS

    Data.gov (United States)

    National Aeronautics and Space Administration — The primary innovation for this CIF will be the ability to accomplish library preparation of isolated RNA that will enable transcriptional (RNA instead of DNA)...

  12. Oak ridge national laboratory automated clean chemistry for bulk analysis of environmental swipe samples

    Energy Technology Data Exchange (ETDEWEB)

    Bostick, Debra A. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Hexel, Cole R. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Ticknor, Brian W. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Tevepaugh, Kayron N. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Metzger, Shalina C. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

    2016-11-01

    To shorten the lengthy and costly manual chemical purification procedures, sample preparation methods for mass spectrometry are being automated using commercial-off-the-shelf (COTS) equipment. This addresses a serious need in the nuclear safeguards community to debottleneck the separation of U and Pu in environmental samples—currently performed by overburdened chemists—with a method that allows unattended, overnight operation. In collaboration with Elemental Scientific Inc., the prepFAST-MC2 was designed based on current COTS equipment that was modified for U/Pu separations utilizing Eichrom™ TEVA and UTEVA resins. Initial verification of individual columns yielded small elution volumes with consistent elution profiles and good recovery. Combined column calibration demonstrated ample separation without crosscontamination of the eluent. Automated packing and unpacking of the built-in columns initially showed >15% deviation in resin loading by weight, which can lead to inconsistent separations. Optimization of the packing and unpacking methods led to a reduction in the variability of the packed resin to less than 5% daily. The reproducibility of the automated system was tested with samples containing 30 ng U and 15 pg Pu, which were separated in a series with alternating reagent blanks. These experiments showed very good washout of both the resin and the sample from the columns as evidenced by low blank values. Analysis of the major and minor isotope ratios for U and Pu provided values well within data quality limits for the International Atomic Energy Agency. Additionally, system process blanks spiked with 233U and 244Pu tracers were separated using the automated system after it was moved outside of a clean room and yielded levels equivalent to clean room blanks, confirming that the system can produce high quality results without the need for expensive clean room infrastructure. Comparison of the amount of personnel time necessary for successful manual vs

  13. Automated combustion accelerator mass spectrometry for the analysis of biomedical samples in the low attomole range.

    Science.gov (United States)

    van Duijn, Esther; Sandman, Hugo; Grossouw, Dimitri; Mocking, Johannes A J; Coulier, Leon; Vaes, Wouter H J

    2014-08-05

    The increasing role of accelerator mass spectrometry (AMS) in biomedical research necessitates modernization of the traditional sample handling process. AMS was originally developed and used for carbon dating, therefore focusing on a very high precision but with a comparably low sample throughput. Here, we describe the combination of automated sample combustion with an elemental analyzer (EA) online coupled to an AMS via a dedicated interface. This setup allows direct radiocarbon measurements for over 70 samples daily by AMS. No sample processing is required apart from the pipetting of the sample into a tin foil cup, which is placed in the carousel of the EA. In our system, up to 200 AMS analyses are performed automatically without the need for manual interventions. We present results on the direct total (14)C count measurements in <2 μL human plasma samples. The method shows linearity over a range of 0.65-821 mBq/mL, with a lower limit of quantification of 0.65 mBq/mL (corresponding to 0.67 amol for acetaminophen). At these extremely low levels of activity, it becomes important to quantify plasma specific carbon percentages. This carbon percentage is automatically generated upon combustion of a sample on the EA. Apparent advantages of the present approach include complete omission of sample preparation (reduced hands-on time) and fully automated sample analysis. These improvements clearly stimulate the standard incorporation of microtracer research in the drug development process. In combination with the particularly low sample volumes required and extreme sensitivity, AMS strongly improves its position as a bioanalysis method.

  14. Sample preparation system for microfluidic applications

    Science.gov (United States)

    Mosier, Bruce P [San Francisco, CA; Crocker, Robert W [Fremont, CA; Patel, Kamlesh D [Dublin, CA; Harnett, Cindy K [Livermore, CA

    2007-05-08

    An apparatus that couples automated injection with flow feedback to provide nanoliter accuracy in controlling microliter volumes. The apparatus comprises generally a source of hydraulic fluid pressure, a fluid isolator joined to the outlet of the hydraulic pressure source and a flow sensor to provide pressure-driven analyte metering. For operation generally and particularly in microfluidic systems the hydraulic pressure source is typically an electrokinetic (EK) pump that incorporates gasless electrodes. The apparatus is capable of metering sub-microliter volumes at flowrates of 1 100 .mu.L/min into microsystem load pressures of up to 1000 50 psi, respectively. Flowrates can be specified within 0.5 .mu.L/min and volumes as small as 80 nL can be metered.

  15. Sample Preparation and Processing for Nanopore Life Detection Instruments

    Data.gov (United States)

    National Aeronautics and Space Administration — The technical approach includes physically disrupting samples as a first step in sample preparation. Sample will then delivered for separation based on molecular...

  16. 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

  17. FISHprep: A Novel Integrated Device for Metaphase FISH Sample Preparation

    DEFF Research Database (Denmark)

    Shah, Pranjul Jaykumar; Vedarethinam, Indumathi; Kwasny, Dorota

    2011-01-01

    We present a novel integrated device for preparing metaphase chromosomes spread slides (FISHprep). The quality of cytogenetic analysis from patient samples greatly relies on the efficiency of sample pre-treatment and/or slide preparation. In cytogenetic slide preparation, cell cultures...... are routinely used to process samples (for culture, arrest and fixation of cells) and/or to expand limited amount of samples (in case of prenatal diagnostics). Arguably, this expansion and other sample pretreatments form the longest part of the entire diagnostic protocols spanning over 3–4 days. We present here...... with minimal handling for metaphase FISH slide preparation....

  18. 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.

  19. 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.

  20. Fluidics platform and method for sample preparation

    Science.gov (United States)

    Benner, Henry W.; Dzenitis, John M.

    2016-06-21

    Provided herein are fluidics platforms and related methods for performing integrated sample collection and solid-phase extraction of a target component of the sample all in one tube. The fluidics platform comprises a pump, particles for solid-phase extraction and a particle-holding means. The method comprises contacting the sample with one or more reagents in a pump, coupling a particle-holding means to the pump and expelling the waste out of the pump while the particle-holding means retains the particles inside the pump. The fluidics platform and methods herein described allow solid-phase extraction without pipetting and centrifugation.

  1. 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.

  2. 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.

  3. Whole-Genome Sequencing: Automated, Nonindexed Library Preparation.

    Science.gov (United States)

    Mardis, Elaine; McCombie, W Richard

    2017-03-01

    This protocol describes an automated procedure for constructing a nonindexed Illumina DNA library and relies on the use of a CyBi-SELMA automated pipetting machine, the Covaris E210 shearing instrument, and the epMotion 5075. With this method, genomic DNA fragments are produced by sonication, using high-frequency acoustic energy to shear DNA. Here, double-stranded DNA is fragmented when exposed to the energy of adaptive focused acoustic shearing (AFA). The resulting DNA fragments are ligated to adaptors, amplified by polymerase chain reaction (PCR), and subjected to size selection using magnetic beads. The product is suitable for use as template in whole-genome sequencing. © 2017 Cold Spring Harbor Laboratory Press.

  4. PROJECT ENGINEERING DATA MANAGEMENT AT AUTOMATED PREPARATION OF DESIGN DOCUMENTATION

    OpenAIRE

    A. V. Guryanov; A. V. Shukalov; I. O. Zharinov; S. A. Leonovets; E. Y. Didenko

    2017-01-01

    We have developed and realized instrumental means for automated support of end-to-end design process for design documentation on a product at the programming level. The proposed decision is based on processing of the engineering project data that are contained in interdependent design documents: tactical technical characteristics of products, data on the valuable metals contained in them, the list of components applied in a product and others. Processing of engineering data is based on their ...

  5. Automated MALDI Matrix Coating System for Multiple Tissue Samples for Imaging Mass Spectrometry

    Science.gov (United States)

    Mounfield, William P.; Garrett, Timothy J.

    2012-03-01

    Uniform matrix deposition on tissue samples for matrix-assisted laser desorption/ionization (MALDI) is key for reproducible analyte ion signals. Current methods often result in nonhomogenous matrix deposition, and take time and effort to produce acceptable ion signals. Here we describe a fully-automated method for matrix deposition using an enclosed spray chamber and spray nozzle for matrix solution delivery. A commercial air-atomizing spray nozzle was modified and combined with solenoid controlled valves and a Programmable Logic Controller (PLC) to control and deliver the matrix solution. A spray chamber was employed to contain the nozzle, sample, and atomized matrix solution stream, and to prevent any interference from outside conditions as well as allow complete control of the sample environment. A gravity cup was filled with MALDI matrix solutions, including DHB in chloroform/methanol (50:50) at concentrations up to 60 mg/mL. Various samples (including rat brain tissue sections) were prepared using two deposition methods (spray chamber, inkjet). A linear ion trap equipped with an intermediate-pressure MALDI source was used for analyses. Optical microscopic examination showed a uniform coating of matrix crystals across the sample. Overall, the mass spectral images gathered from tissues coated using the spray chamber system were of better quality and more reproducible than from tissue specimens prepared by the inkjet deposition method.

  6. Automated Clean Chemistry for Bulk Analysis of Environmental Swipe Samples - FY17 Year End Report

    Energy Technology Data Exchange (ETDEWEB)

    Ticknor, Brian W. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Metzger, Shalina C. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); McBay, Eddy H. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Hexel, Cole R. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Tevepaugh, Kayron N. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Bostick, Debra A. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

    2017-11-30

    Sample preparation methods for mass spectrometry are being automated using commercial-off-the-shelf (COTS) equipment to shorten lengthy and costly manual chemical purification procedures. This development addresses a serious need in the International Atomic Energy Agency’s Network of Analytical Laboratories (IAEA NWAL) to increase efficiency in the Bulk Analysis of Environmental Samples for Safeguards program with a method that allows unattended, overnight operation. In collaboration with Elemental Scientific Inc., the prepFAST-MC2 was designed based on COTS equipment. It was modified for uranium/plutonium separations using renewable columns packed with Eichrom TEVA and UTEVA resins, with a chemical separation method based on the Oak Ridge National Laboratory (ORNL) NWAL chemical procedure. The newly designed prepFAST-SR has had several upgrades compared with the original prepFAST-MC2. Both systems are currently installed in the Ultra-Trace Forensics Science Center at ORNL.

  7. One-step sample preparation of positive blood cultures for the direct detection of methicillin-sensitive and -resistant Staphylococcus aureus and methicillin-resistant coagulase-negative staphylococci within one hour using the automated GenomEra CDX™ PCR system.

    Science.gov (United States)

    Hirvonen, J J; von Lode, P; Nevalainen, M; Rantakokko-Jalava, K; Kaukoranta, S-S

    2012-10-01

    A method for the rapid detection of methicillin-sensitive and -resistant Staphylococcus aureus (MSSA and MRSA, respectively) and methicillin-resistant coagulase-negative staphylococci (MRCoNS) with a straightforward sample preparation protocol of blood cultures using an automated homogeneous polymerase chain reaction (PCR) assay, the GenomEra™ MRSA/SA (Abacus Diagnostica Oy, Turku, Finland), is presented. In total, 316 BacT/Alert (bioMérieux, Marcy l'Etoile, France) and 433 BACTEC (Becton Dickinson, Sparks, MD, USA) blood culture bottles were analyzed, including 725 positive cultures containing Gram-positive cocci in clusters (n = 419) and other Gram stain forms (n = 361), as well as 24 signal- and growth-negative bottles. Detection sensitivities for MSSA, MRSA, and MRCoNS were 99.4 % (158/159), 100.0 % (9/9), and 99.3 % (132/133), respectively. One false-positive MRSA result was detected from a non-staphylococci-containing bottle, yielding a specificity of 99.8 %. The lowest detectable amount of viable cells in the blood culture sample was 4 × 10(4) CFU/mL. The results were available within one hour after microbial growth detection and the two-step, time-resolved fluorometric (TRF) measurement mode employed by the GenomEra CDX™ instrument showed no interference from blood, charcoal, or culture media. The method described lacks all sample purification steps and allows reliable and simplified pathogen detection also in clinical microbiology laboratory settings without specialized molecular microbiology competence.

  8. Establishing a novel automated magnetic bead-based method for the extraction of DNA from a variety of forensic samples.

    Science.gov (United States)

    Witt, Sebastian; Neumann, Jan; Zierdt, Holger; Gébel, Gabriella; Röscheisen, Christiane

    2012-09-01

    Automated systems have been increasingly utilized for DNA extraction by many forensic laboratories to handle growing numbers of forensic casework samples while minimizing the risk of human errors and assuring high reproducibility. The step towards automation however is not easy: The automated extraction method has to be very versatile to reliably prepare high yields of pure genomic DNA from a broad variety of sample types on different carrier materials. To prevent possible cross-contamination of samples or the loss of DNA, the components of the kit have to be designed in a way that allows for the automated handling of the samples with no manual intervention necessary. DNA extraction using paramagnetic particles coated with a DNA-binding surface is predestined for an automated approach. For this study, we tested different DNA extraction kits using DNA-binding paramagnetic particles with regard to DNA yield and handling by a Freedom EVO(®)150 extraction robot (Tecan) equipped with a Te-MagS magnetic separator. Among others, the extraction kits tested were the ChargeSwitch(®)Forensic DNA Purification Kit (Invitrogen), the PrepFiler™Automated Forensic DNA Extraction Kit (Applied Biosystems) and NucleoMag™96 Trace (Macherey-Nagel). After an extensive test phase, we established a novel magnetic bead extraction method based upon the NucleoMag™ extraction kit (Macherey-Nagel). The new method is readily automatable and produces high yields of DNA from different sample types (blood, saliva, sperm, contact stains) on various substrates (filter paper, swabs, cigarette butts) with no evidence of a loss of magnetic beads or sample cross-contamination. Copyright © 2012 Elsevier Ireland Ltd. All rights reserved.

  9. Automated force volume image processing for biological samples.

    Directory of Open Access Journals (Sweden)

    Pavel Polyakov

    2011-04-01

    Full Text Available Atomic force microscopy (AFM has now become a powerful technique for investigating on a molecular level, surface forces, nanomechanical properties of deformable particles, biomolecular interactions, kinetics, and dynamic processes. This paper specifically focuses on the analysis of AFM force curves collected on biological systems, in particular, bacteria. The goal is to provide fully automated tools to achieve theoretical interpretation of force curves on the basis of adequate, available physical models. In this respect, we propose two algorithms, one for the processing of approach force curves and another for the quantitative analysis of retraction force curves. In the former, electrostatic interactions prior to contact between AFM probe and bacterium are accounted for and mechanical interactions operating after contact are described in terms of Hertz-Hooke formalism. Retraction force curves are analyzed on the basis of the Freely Jointed Chain model. For both algorithms, the quantitative reconstruction of force curves is based on the robust detection of critical points (jumps, changes of slope or changes of curvature which mark the transitions between the various relevant interactions taking place between the AFM tip and the studied sample during approach and retraction. Once the key regions of separation distance and indentation are detected, the physical parameters describing the relevant interactions operating in these regions are extracted making use of regression procedure for fitting experiments to theory. The flexibility, accuracy and strength of the algorithms are illustrated with the processing of two force-volume images, which collect a large set of approach and retraction curves measured on a single biological surface. For each force-volume image, several maps are generated, representing the spatial distribution of the searched physical parameters as estimated for each pixel of the force-volume image.

  10. 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...

  11. Whole-Genome Sequencing: Automated, Indexed Library Preparation.

    Science.gov (United States)

    Mardis, Elaine; McCombie, W Richard

    2017-03-01

    This protocol describes an automated procedure for constructing an indexed Illumina DNA library. With this method, genomic DNA fragments are produced by sonication, using high-frequency acoustic energy to shear DNA. Double-stranded DNA (dsDNA) will fragment when exposed to the energy of adaptive focused acoustic shearing (AFA). The resulting DNA fragments are ligated to adaptors, amplified by polymer chain reaction (PCR), and subjected to size selection using magnetic beads. The product is suitable for use as template in whole-genome sequencing. © 2017 Cold Spring Harbor Laboratory Press.

  12. 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)

  13. Automated Aqueous Sample Concentration Methods for in situ Astrobiological Instrumentation

    Science.gov (United States)

    Aubrey, A. D.; Grunthaner, F. J.

    2009-12-01

    The era of wet chemical experiments for in situ planetary science investigations is upon us, as evidenced by recent results from the surface of Mars by Phoenix’s microscopy, electrochemistry, and conductivity analyzer, MECA [1]. Studies suggest that traditional thermal volatilization methods for planetary science in situ investigations induce organic degradation during sample processing [2], an effect that is enhanced in the presence of oxidants [3]. Recent developments have trended towards adaptation of non-destructive aqueous extraction and analytical methods for future astrobiological instrumentation. Wet chemical extraction techniques under investigation include subcritical water extraction, SCWE [4], aqueous microwave assisted extraction, MAE, and organic solvent extraction [5]. Similarly, development of miniaturized analytical space flight instruments that require aqueous extracts include microfluidic capillary electrophoresis chips, μCE [6], liquid-chromatography mass-spectrometrometers, LC-MS [7], and life marker chips, LMC [8]. If organics are present on the surface of Mars, they are expected to be present at extremely low concentrations (parts-per-billion), orders of magnitude below the sensitivities of most flight instrument technologies. Therefore, it becomes necessary to develop and integrate concentration mechanisms for in situ sample processing before delivery to analytical flight instrumentation. We present preliminary results of automated solid-phase-extraction (SPE) sample purification and concentration methods for the treatment of highly saline aqueous soil extracts. These methods take advantage of the affinity of low molecular weight organic compounds with natural and synthetic scavenger materials. These interactions allow for the separation of target organic analytes from unfavorable background species (i.e. salts) during inline treatment, and a clever method for selective desorption is utilized to obtain concentrated solutions on the order

  14. 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

  15. Automated sampling and data processing derived from biomimetic membranes

    DEFF Research Database (Denmark)

    Perry, Mark; Vissing, Thomas; Boesen, P.

    2009-01-01

    Recent advances in biomimetic membrane systems have resulted in an increase in membrane lifetimes from hours to days and months. Long-lived membrane systems demand the development of both new automated monitoring equipment capable of measuring electrophysiological membrane characteristics and new...

  16. Automated sampling and data processing derived from biomimetic membranes

    International Nuclear Information System (INIS)

    Perry, M; Vissing, T; Hansen, J S; Nielsen, C H; Boesen, T P; Emneus, J

    2009-01-01

    Recent advances in biomimetic membrane systems have resulted in an increase in membrane lifetimes from hours to days and months. Long-lived membrane systems demand the development of both new automated monitoring equipment capable of measuring electrophysiological membrane characteristics and new data processing software to analyze and organize the large amounts of data generated. In this work, we developed an automated instrumental voltage clamp solution based on a custom-designed software controller application (the WaveManager), which enables automated on-line voltage clamp data acquisition applicable to long-time series experiments. We designed another software program for off-line data processing. The automation of the on-line voltage clamp data acquisition and off-line processing was furthermore integrated with a searchable database (DiscoverySheet(TM)) for efficient data management. The combined solution provides a cost efficient and fast way to acquire, process and administrate large amounts of voltage clamp data that may be too laborious and time consuming to handle manually. (communication)

  17. 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

  18. γ-ray spectrometry results versus sample preparation methods

    International Nuclear Information System (INIS)

    Su Qiong; Wang Xuewu; Chen Boxian

    2000-01-01

    According to recommended conditions two bio-samples, tea leave and flour, are prepared with different methods: grounding into powder and reducing to ash, then they were analyzed by γ ray spectrometry. Remarkable difference was shown between the measured values of tea samples prepared with these different methods. One of the reasons may be that the method of reducing to ash makes some nuclides lost. Compared with the 'non-destructive' method of grounding into powder, the method of reducing to ash can be much more sensible to the loss of some nuclides. The probable reasons are discussed for the varied influences of different preparation methods of tea leave and flour samples

  19. Sample preparation for atomic spectroscopy: evolution and future trends

    Directory of Open Access Journals (Sweden)

    Oliveira Elisabeth de

    2003-01-01

    Full Text Available Sample preparation is the critical step of any analytical protocol, and involves steps from simple dilution to partial or total dissolution. The methods include dry or wet decomposition of the samples in open or closed systems, using thermal, ultrasonic or radiant (infrared, ultraviolet and microwaves energy. This review emphasizes sample preparation for atomic spectroscopy. The present and future tendencies for sample preparation also involve on-line dissolution, extraction of the analytes, speciation, solid sample and slurry analysis, in situ and in vivo procedures, etc. Nowadays the goals are the best result, in the shortest time, with minimum contamination, using the smallest quantities of reagents and samples, and having low residue and waste generation, as well as maintaining the integrity of the sample and the traceability of the results, to have quality and confidence in the measurements as the primordial attributes required by the community and by the users.

  20. Clinical Chemistry Laboratory Automation in the 21st Century - Amat Victoria curam (Victory loves careful preparation)

    Science.gov (United States)

    Armbruster, David A; Overcash, David R; Reyes, Jaime

    2014-01-01

    The era of automation arrived with the introduction of the AutoAnalyzer using continuous flow analysis and the Robot Chemist that automated the traditional manual analytical steps. Successive generations of stand-alone analysers increased analytical speed, offered the ability to test high volumes of patient specimens, and provided large assay menus. A dichotomy developed, with a group of analysers devoted to performing routine clinical chemistry tests and another group dedicated to performing immunoassays using a variety of methodologies. Development of integrated systems greatly improved the analytical phase of clinical laboratory testing and further automation was developed for pre-analytical procedures, such as sample identification, sorting, and centrifugation, and post-analytical procedures, such as specimen storage and archiving. All phases of testing were ultimately combined in total laboratory automation (TLA) through which all modules involved are physically linked by some kind of track system, moving samples through the process from beginning-to-end. A newer and very powerful, analytical methodology is liquid chromatography-mass spectrometry/mass spectrometry (LC-MS/MS). LC-MS/MS has been automated but a future automation challenge will be to incorporate LC-MS/MS into TLA configurations. Another important facet of automation is informatics, including middleware, which interfaces the analyser software to a laboratory information systems (LIS) and/or hospital information systems (HIS). This software includes control of the overall operation of a TLA configuration and combines analytical results with patient demographic information to provide additional clinically useful information. This review describes automation relevant to clinical chemistry, but it must be recognised that automation applies to other specialties in the laboratory, e.g. haematology, urinalysis, microbiology. It is a given that automation will continue to evolve in the clinical laboratory

  1. Clinical Chemistry Laboratory Automation in the 21st Century - Amat Victoria curam (Victory loves careful preparation).

    Science.gov (United States)

    Armbruster, David A; Overcash, David R; Reyes, Jaime

    2014-08-01

    The era of automation arrived with the introduction of the AutoAnalyzer using continuous flow analysis and the Robot Chemist that automated the traditional manual analytical steps. Successive generations of stand-alone analysers increased analytical speed, offered the ability to test high volumes of patient specimens, and provided large assay menus. A dichotomy developed, with a group of analysers devoted to performing routine clinical chemistry tests and another group dedicated to performing immunoassays using a variety of methodologies. Development of integrated systems greatly improved the analytical phase of clinical laboratory testing and further automation was developed for pre-analytical procedures, such as sample identification, sorting, and centrifugation, and post-analytical procedures, such as specimen storage and archiving. All phases of testing were ultimately combined in total laboratory automation (TLA) through which all modules involved are physically linked by some kind of track system, moving samples through the process from beginning-to-end. A newer and very powerful, analytical methodology is liquid chromatography-mass spectrometry/mass spectrometry (LC-MS/MS). LC-MS/MS has been automated but a future automation challenge will be to incorporate LC-MS/MS into TLA configurations. Another important facet of automation is informatics, including middleware, which interfaces the analyser software to a laboratory information systems (LIS) and/or hospital information systems (HIS). This software includes control of the overall operation of a TLA configuration and combines analytical results with patient demographic information to provide additional clinically useful information. This review describes automation relevant to clinical chemistry, but it must be recognised that automation applies to other specialties in the laboratory, e.g. haematology, urinalysis, microbiology. It is a given that automation will continue to evolve in the clinical laboratory

  2. Automation Of University Report Documentation Preparation With Electronic Documents Circulation Elements

    Directory of Open Access Journals (Sweden)

    M. Melnik

    2009-11-01

    Full Text Available Considered are the questions of info-comunicational technology for university report information gathering and processing. It is proposed to automate the basic university reports preparation process. On the basis of the proposed system, it possible to provide electronic documents circulation between the Ministry of Education and universities of Ukraine.

  3. Isodisperse Telechelic Polymers and their Polyurethane Derivatives Sample Preparation

    National Research Council Canada - National Science Library

    Tuedoes, Ferenc

    1998-01-01

    ... (polyethylene) derivatives (HTPE). The polybutadiene samples, with nominal average molecular weights Mn of 1000, 1500, 2000, 3000, 5000, and 10000, have been prepared using the so-called "isodisperse telechelic polymerization" method...

  4. 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...... of cell structures that make it imprudent to blindly adopt protocols that were designed for a specific group of microorganisms. We have therefore reviewed and evaluated the whole sample preparation procedures for analysis of yeast metabolites. Our focus has been on the current needs in metabolome analysis...... with reduced pressure solvent evaporation and therefore represents an attractive sample preparation procedure for high-throughput metabolome analysis of yeasts. Copyright (c) 2005 John Wiley & Sons, Ltd....

  5. 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...

  6. 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.

  7. Automated washing of FTA Card punches and PCR setup for reference samples using a LIMS-controlled Sias Xantus automated liquid handler

    DEFF Research Database (Denmark)

    Stangegaard, Michael; Olsen, Addie Nina; Frøslev, Tobias G.

    2009-01-01

    We have implemented and validated automated methods for washing FTA Card punches containing buccal samples and subsequent PCR setup using a Sias Xantus automated liquid handler. The automated methods were controlled by worklists generated by our LabWare Laboratory Information Management System...

  8. 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.

  9. 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...

  10. 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

  11. 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

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. 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

  17. Validation of the Sysmex sp-1000i automated slide preparer-stainer in a clinical laboratory

    Directory of Open Access Journals (Sweden)

    Eberson Damiao dos Santos de Bitencourt

    2013-01-01

    Full Text Available Background: The speed and quality of information have become essential items in the release of laboratory reports. The Sysmex®SP1000-I device has been developed to prepare and stain smear slides. However, for a device to be cleared for use in the laboratory routine it must pass through a validation process. Objective: To evaluate the performance and reliability of the Sysmex® SP-1000i slide preparer-stainer incorporated into the routine of a hospital laboratory in Porto Alegre. Methods: Peripheral blood samples of patients attending the laboratory for ambulatory exams with leukocyte counts between 7000/°L and 12,000/°L were evaluated, independent of gender and age. Two slides were prepared for each sample using the Sysmex® SP-1000i equipment; one of the slides was used to perform quality control tests using the CellaVision® DM96 device, and the other slide was used to compare pre-classification by the same device and the classification performed by a pharmacist-biochemist. Results: The results of all the slides used as controls were acceptable according to the quality control test as established by the manufacturer of the device. In the comparison between the automated pre-classification and the classification made by the professional, there was an acceptable variation in the differential counts of leukocytes for 90% of the analyzed slides. Pearson correlation coefficient showed a strong correlation for band neutrophils (r = 0.802; p-value < 0.001, segmented neutrophils (r = 0.963; p-value < 0.001, eosinophils (r = 0.958; p-value < 0.001, lymphocytes (r = 0.985; p-value < 0.001 and atypical lymphocytes (r = 0.866; p-value < 0.001 using both methods. The red blood cell analysis was adequate for all slides analyzed by the equipment and by the professional. Conclusion: The new Sysmex®SP1000-i methodology was found to be reliable, fast and safe for the routines of medium and large laboratories, improving the quality of microscopic analysis in

  18. 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.

  19. 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.

  20. 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

  1. Plasma sample preparation by ultrafiltration for FTIR analysis

    International Nuclear Information System (INIS)

    Aslani, A.; Hansen, R.D.; Cooper, B.A.; Smith, R.C.

    2000-01-01

    Total body water (TBW) may be significantly altered with disease. Isotope dilution techniques, considered to be the 'gold standard' methods for measuring TBW, are expensive, time consuming and require considerable expertise, especially during the sample preparatory phase. In this study, a new method, ultrafiltration (UF), was hypothesised to be an efficient alternative to vacuum sublimation (VS) in the preparation of plasma samples for Fourier Transform Infra Red (FTIR) determination of TBW. Deuterium Oxide (D 2 O) concentrations were prepared in human plasma and subjected to both techniques. FTIR analysis was carried out on the resulting VS and UF solutions and on D 2 O concentrations in distilled water. The resulting absorbance values were then statistically compared. Urea concentrations prepared in D 2 O-containing plasma were also compared to 'blank' plasma to investigate the effect of high plasma urea concentration on the resulting H 2 O/D 2 O mixture obtained during UF Paired t-tests showed that the VS plasma samples (p=0.003), but not the UF samples (p=0.9), were significantly different to D 2 O standards prepared in distilled water. While there was no evidence of an effect of urea on UF at low (0.4 g/L) D 2 O concentration, a marginal (p=0.04) effect occurred at a higher (1.6 g/L) D 2 O level. Throughput of samples was much more efficient with the UF technique. These findings indicate that the new UF method is an accurate, more efficient method of plasma sample preparation than the VS method in the FTIR determination of TBW

  2. 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)

  3. SASSI: Subsystems for Automated Subsurface Sampling Instruments, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Future robotic planetary exploration missions will benefit greatly from the ability to capture rock and/or regolith core samples that deliver the stratigraphy of the...

  4. SASSI: Subsystems for Automated Subsurface Sampling Instruments, Phase II

    Data.gov (United States)

    National Aeronautics and Space Administration — Autonomous surface sampling systems are necessary, near term, to construct a historical view of planetary significant events; as well as allow for the identification...

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

    African Journals Online (AJOL)

    The objective of this study was to investigate the effect of method of sample preparation on the degradation kinetics of herbage when applying the in situ technique. Ryegrass (Lolium multiflorum cv. Midmar) was harvested at three and four weeks after cutting and fertilizing with 200 kg nitrogen (N)/ha. Freshly cut herbage ...

  6. 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

  7. New Methods of Sample Preparation for Atom Probe Specimens

    Science.gov (United States)

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

    2003-01-01

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

  8. The Effect of Sample Preparation and Testing Procedure

    African Journals Online (AJOL)

    handling and disturbance. Revisions to sample preparation and testing procedures are considered necessary and are proposed in utilizing these soils for civil engineering purposes. It is concluded that the plasticity chart should be regarded as a guidance tool only for evaluating the likely properties of laterite soils. It should.

  9. The effect of sample preparation and testing procedure on the ...

    African Journals Online (AJOL)

    The effect of sample preparation and testing procedure on the geotechnical properties of tropically weathered residual laterite soils of Ethiopia. ... A combination of classification based on structure, mineralogical composition, and geo-morphological impact on soil formation together with conventional classification systems is ...

  10. Automated modal parameter estimation using correlation analysis and bootstrap sampling

    Science.gov (United States)

    Yaghoubi, Vahid; Vakilzadeh, Majid K.; Abrahamsson, Thomas J. S.

    2018-02-01

    The estimation of modal parameters from a set of noisy measured data is a highly judgmental task, with user expertise playing a significant role in distinguishing between estimated physical and noise modes of a test-piece. Various methods have been developed to automate this procedure. The common approach is to identify models with different orders and cluster similar modes together. However, most proposed methods based on this approach suffer from high-dimensional optimization problems in either the estimation or clustering step. To overcome this problem, this study presents an algorithm for autonomous modal parameter estimation in which the only required optimization is performed in a three-dimensional space. To this end, a subspace-based identification method is employed for the estimation and a non-iterative correlation-based method is used for the clustering. This clustering is at the heart of the paper. The keys to success are correlation metrics that are able to treat the problems of spatial eigenvector aliasing and nonunique eigenvectors of coalescent modes simultaneously. The algorithm commences by the identification of an excessively high-order model from frequency response function test data. The high number of modes of this model provides bases for two subspaces: one for likely physical modes of the tested system and one for its complement dubbed the subspace of noise modes. By employing the bootstrap resampling technique, several subsets are generated from the same basic dataset and for each of them a model is identified to form a set of models. Then, by correlation analysis with the two aforementioned subspaces, highly correlated modes of these models which appear repeatedly are clustered together and the noise modes are collected in a so-called Trashbox cluster. Stray noise modes attracted to the mode clusters are trimmed away in a second step by correlation analysis. The final step of the algorithm is a fuzzy c-means clustering procedure applied to

  11. Use of automated irrigation pumps improves quality of bowel preparation for colonoscopy.

    Science.gov (United States)

    Ravi, Sujan; Sabbagh, Rana; Antaki, Fadi

    2016-03-25

    To evaluate the effectiveness of automated irrigation pumps (AIPs) in improving the quality of the bowel preparation and the yield of colonoscopy. A retrospective observational study was conducted at a single medical center. Outpatient colonoscopies performed during a 4-mo time period when AIPs were not in use, were compared to colonoscopies performed during control period. The main outcomes measured were quality of bowel preparation, procedures aborted due to poor preparation, recommendations to repeat at short interval due to sub-optimal bowel preparation and adenoma detection rates. One thousand and thirty-seven colonoscopies were included. A higher proportion of cases did not achieve a satisfactory bowel preparation when AIPs were not used (24.4% vs 10.3%, P preparation was not significantly different, however a repeat procedure at a short interval was recommended in a higher proportion of cases when AIPs were not used (21.3% vs 6.9%, P preparation was 2.91 (95%CI: 2.04-4.15) times more likely when AIPs were used. Detection of polyps and adenomas was not significantly different. AIP use during colonoscopy results in a higher proportion of colonic preparation rated as satisfactory, although polyp detection rate is not significantly affected. Recommendations for repeat colonoscopy at shorter interval significantly decrease with the use of AIPs. This study supports the use of the irrigation pumps in endoscopy units to improve the quality of colonoscopy.

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

    Science.gov (United States)

    Tseng, C M; Garraud, H; Amouroux, D; Donard, O F; 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 HNO(3) solution and complete dissolution of biomaterials by an alkaline solution, such as 25% TMAH solution, were obtained. Methylmercury compounds were kept intact without decomposition or losses by evaporation. Quantitative recoveries of total mercury were achieved with a two-step microwave attack using a combination of HNO(3) and H(2)0(2) solutions as extractant. The whole pretreatment procedure only takes 15 min, which can be further shortened by an automated robust operation with an open focused system. These analytical procedures were validated by the analysis of environmental certified reference materials. The results confirm that the open focused microwave technique is a promising tool for solid sample preparation in analytical and environmental chemistry.

  13. 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)

  14. Applications of reversible covalent chemistry in analytical sample preparation.

    Science.gov (United States)

    Siegel, David

    2012-12-07

    Reversible covalent chemistry (RCC) adds another dimension to commonly used sample preparation techniques like solid-phase extraction (SPE), solid-phase microextraction (SPME), molecular imprinted polymers (MIPs) or immuno-affinity cleanup (IAC): chemical selectivity. By selecting analytes according to their covalent reactivity, sample complexity can be reduced significantly, resulting in enhanced analytical performance for low-abundance target analytes. This review gives a comprehensive overview of the applications of RCC in analytical sample preparation. The major reactions covered include reversible boronic ester formation, thiol-disulfide exchange and reversible hydrazone formation, targeting analyte groups like diols (sugars, glycoproteins and glycopeptides, catechols), thiols (cysteinyl-proteins and cysteinyl-peptides) and carbonyls (carbonylated proteins, mycotoxins). Their applications range from low abundance proteomics to reversible protein/peptide labelling to antibody chromatography to quantitative and qualitative food analysis. In discussing the potential of RCC, a special focus is on the conditions and restrictions of the utilized reaction chemistry.

  15. 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.

  16. Automation systems for radioimmunoassay

    International Nuclear Information System (INIS)

    Yamasaki, Paul

    1974-01-01

    The application of automation systems for radioimmunoassay (RIA) was discussed. Automated systems could be useful in the second step, of the four basic processes in the course of RIA, i.e., preparation of sample for reaction. There were two types of instrumentation, a semi-automatic pipete, and a fully automated pipete station, both providing for fast and accurate dispensing of the reagent or for the diluting of sample with reagent. Illustrations of the instruments were shown. (Mukohata, S.)

  17. 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.

  18. 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.

  19. Automation of PacBio SMRTbell NGS library preparation for bacterial genome sequencing.

    Science.gov (United States)

    Kong, Nguyet; Ng, Whitney; Thao, Kao; Agulto, Regina; Weis, Allison; Kim, Kristi Spittle; Korlach, Jonas; Hickey, Luke; Kelly, Lenore; Lappin, Stephen; Weimer, Bart C

    2017-01-01

    The PacBio RS II provides for single molecule, real-time DNA technology to sequence genomes and detect DNA modifications. The starting point for high-quality sequence production is high molecular weight genomic DNA. To automate the library preparation process, there must be high-throughput methods in place to assess the genomic DNA, to ensure the size and amounts of the sheared DNA fragments and final library. The library construction automation was accomplished using the Agilent NGS workstation with Bravo accessories for heating, shaking, cooling, and magnetic bead manipulations for template purification. The quality control methods from gDNA input to final library using the Agilent Bioanalyzer System and Agilent TapeStation System were evaluated. Automated protocols of PacBio 10 kb library preparation produced libraries with similar technical performance to those generated manually. The TapeStation System proved to be a reliable method that could be used in a 96-well plate format to QC the DNA equivalent to the standard Bioanalyzer System results. The DNA Integrity Number that is calculated in the TapeStation System software upon analysis of genomic DNA is quite helpful to assure that the starting genomic DNA is not degraded. In this respect, the gDNA assay on the TapeStation System is preferable to the DNA 12000 assay on the Bioanalyzer System, which cannot run genomic DNA, nor can the Bioanalyzer work directly from the 96-well plates.

  20. 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.

  1. Sample preparation and electron microscopy of hydrocracking catalysts

    Science.gov (United States)

    Husain, S.; McComb, D. W.; Perkins, J. M.; Haswell, R.

    2008-08-01

    This work focuses on the preparation of zeolite and alumina hydrocracking catalysts for investigation by electron energy-loss spectroscopy (EELS). EELS can potentially give new insights into the location and structure of coke which can result in catalyst deactivation. Three sample preparation techniques have been used - microtoming, focussed ion beam milling (LIB) and conventional ion beam milling. Crushing and grinding the catalyst pellets has been discounted as a preparation technique as the spatial relationship between the coke and the catalyst is lost using this method. Microtomed sections show some mechanical damage while sections milled in a single beam LIB microscope show gallium decoration in pores and were too thick for EELS. Conventional ion beam milling has proved to be most successful as it results in extensive thin regions and maintains the spatial distribution of the zeolite and alumina phases.

  2. 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)

  3. Simple and fully automated preparation of [carbonyl-{sup 11}C]WAY-100635

    Energy Technology Data Exchange (ETDEWEB)

    Wadsak, W.; Ettlinger, D.E; Dudczak, R.; Kletter, K. [Medical Univ. of Vienna (Austria). Dept. of Nuclear Medicine; Mien, L.K. [Medical Univ. of Vienna (Austria). Dept. of Nuclear Medicine; Medical Univ. of Vienna (Austria). Dept. of Psychiatry; Vienna Univ. (Austria). Dept. of Pharmaceutical Technology and Biopharmaceutics; Lanzenberger, R.R. [Medical Univ. of Vienna (Austria). Dept. of Psychiatry; Haeusler, D. [Medical Univ. of Vienna (Austria). Dept. of Nuclear Medicine; Vienna Univ. (Austria). Dept. of Pharmaceutical Technology and Biopharmaceutics; Mitterhauser, M. [Medical Univ. of Vienna (Austria). Dept. of Nuclear Medicine; Vienna Univ. (Austria). Dept. of Pharmaceutical Technology and Biopharmaceutics; General Hospital of Vienna (Austria). Hospital Pharmacy

    2007-07-01

    So far, [carbonyl-{sup 11}C]WAY-100635 is the PET-tracer of choice for 5HT{sub 1A}-receptor-imaging. Since the preparation is still a challenge, we aimed at (1) the evaluation of various essential parameters for the successful preparation, (2) the simplification of the radiosynthesis and (3) the establishment of a safe and fully automated system. The preparation is based on a commercial synthesizer and all chemicals are used without further processing. We found a low failure rate (7.7%), high average yield (4.0 {+-} 1.0 GBq) and a specific radioactivity of 292 {+-} 168 GBq/{mu}mol (both at the end of synthesis, EOS). (orig.)

  4. 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 ...

  5. 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...

  6. Automated search-model discovery and preparation for structure solution by molecular replacement.

    Science.gov (United States)

    Keegan, Ronan M; Winn, Martyn D

    2007-04-01

    A novel automation pipeline for macromolecular structure solution by molecular replacement is described. There is a special emphasis on the discovery and preparation of a large number of search models, all of which can be passed to the core molecular-replacement programs. For routine molecular-replacement problems, the pipeline automates what a crystallographer might do and its value is simply one of convenience. For more difficult cases, the pipeline aims to discover the particular template structure and model edits required to produce a viable search model and may succeed in finding an efficacious combination that would be missed otherwise. The pipeline is described in detail and a number of examples are given. The examples are chosen to illustrate successes in real crystallography problems and also particular features of the pipeline. It is concluded that exploring a range of search models automatically can be valuable in many cases.

  7. 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

  8. [Evaluation of an automated streaking system of urine samples for urine cultures].

    Science.gov (United States)

    Bustamante, Verónica; Meza, Paulina; Román, Juan C; García, Patricia

    2014-12-01

    Automated systems have simplified laboratory workflow, improved standardization, traceability and diminished human errors and workload. Although microbiology laboratories have little automation, in recent years new tools for automating pre analytical steps have appeared. To assess the performance of an automated streaking machine for urine cultures and its agreement with the conventional manual plating method for semi quantitative colony counts. 495 urine samples for urinary culture were inoculated in CPS® agar using our standard protocol and the PREVI™ Isola. Rates of positivity, negativity, polymicrobial growth, bacterial species, colony counts and re-isolation requirements were compared. Agreement was achieved in 98.97% of the positive/negative results, in 99.39% of the polymicrobial growth, 99.76% of bacterial species isolated and in 98.56 % of colony counts. The need for re-isolation of colonies decreased from 12.1% to 1.1% using the automated system. PREVI™ Isola's performance was as expected, time saving and improving bacterial isolation. It represents a helpful tool for laboratory automation.

  9. An Automated Inpatient Split-dose Bowel Preparation System Improves Colonoscopy Quality and Reduces Repeat Procedures.

    Science.gov (United States)

    Yadlapati, Rena; Johnston, Elyse R; Gluskin, Adam B; Gregory, Dyanna L; Cyrus, Rachel; Werth, Lindsay; Ciolino, Jody D; Grande, David P; Keswani, Rajesh N

    2017-07-19

    Inpatient colonoscopy preparations are often inadequate, compromising patient safety and procedure quality, while resulting in greater hospital costs. The aims of this study were to: (1) design and implement an electronic inpatient split-dose bowel preparation order set; (2) assess the intervention's impact upon preparation adequacy, repeated colonoscopies, hospital days, and costs. We conducted a single center prospective pragmatic quasiexperimental study of hospitalized adults undergoing colonoscopy. The experimental intervention was designed using DMAIC (define, measure, analyze, improve, and control) methodology. Prospective data collected over 12 months were compared with data from a historical preintervention cohort. The primary outcome was bowel preparation quality and secondary outcomes included number of repeated procedures, hospital days, and costs. On the basis of a Delphi method and DMAIC process, we created an electronic inpatient bowel preparation order set inclusive of a split-dose bowel preparation algorithm, automated orders for rescue medications, and nursing bowel preparation checks. The analysis data set included 969 patients, 445 (46%) in the postintervention group. The adequacy of bowel preparation significantly increased following intervention (86% vs. 43%; P2.0% vs. 4.6%; P=0.03). Mean hospital days from bowel preparation initiation to discharge decreased from 8.0 to 6.9 days (P=0.02). The intervention resulted in an estimated 1-year cost-savings of $46,076 based on a reduction in excess hospital days associated with repeated and delayed procedures. Our interdisciplinary initiative targeting inpatient colonoscopy preparations significantly improved quality and reduced repeat procedures, and hospital days. Other institutions should consider utilizing this framework to improve inpatient colonoscopy value.

  10. 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

  11. 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)

  12. 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)

  13. Sample preparation and assay refinements for pathogen detection platforms

    Science.gov (United States)

    Lim, Daniel V.; Kearns, Elizabeth A.; Leskinen, Stephaney D.; Magaña, Sonia; Stroot, Joyce M.; Hunter, Dawn M.; Schlemmer, Sarah M.

    2009-02-01

    Food-borne and waterborne microbial pathogens are a potential problem in biowarfare and public health. Such pathogens can affect the health, combat readiness, and effectiveness of the warfighter in a battlefield environment and present potential threats to the civilian population through intentional or natural contamination of food and water. Conventional procedures to detect and identify microbial pathogens in food, water, and other materials can take days to perform and may provide inconclusive information. Research at the University of South Florida's Advanced Biosensors Laboratory (ABL) focuses on development of sample processing procedures and biosensor-based assays for rapid detection of biothreat agents. Rapid processing methods, including use of an automated concentrator of microorganisms in water, have been developed for complex matrix samples including ground beef, apple juice, produce, potable water and recreational water, enabling such samples to be directly tested by biosensor assays for target analytes. Bacillus atrophaeus spores and other bacteria can be concentrated from potable and recreational water at low levels with a dead-end hollow-fiber ultrafiltration concentration system. Target bacteria recovered by these processing procedures can be identified by evanescent wave, fiber optic biosensors or other detection platforms. Fiber optic biosensor assays have been improved to include subsequent PCR analysis and viability determination of captured target bacteria using broth enrichment and/or ATP luminescence.

  14. 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

  15. Sample preparation and detection device for infectious agents

    Science.gov (United States)

    Miles, Robin R.; Wang, Amy W.; Fuller, Christopher K.; Lemoff, Asuncion V.; Bettencourt, Kerry A.; Yu, June

    2003-06-10

    A sample preparation and analysis device which incorporates both immunoassays and PCR assays in one compact, field-portable microchip. The device provides new capabilities in fluid and particle control which allows the building of a fluidic chip with no moving parts, thus decreasing fabrication cost and increasing the robustness of the device. The device can operate in a true continuous (not batch) mode. The device incorporates magnetohydrodynamic (MHD) pumps to move the fluid through the system, acoustic mixing and fractionation, dielectropheretic (DEP) sample concentration and purification, and on-chip optical detection capabilities.

  16. Novel sample preparation for operando TEM of catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Miller, Benjamin K.; Barker, Trevor M. [School for Engineering of Matter, Transport and Energy, Arizona State University, Tempe, AZ 85287-6106 (United States); Crozier, Peter A., E-mail: crozier@asu.edu [School for Engineering of Matter, Transport and Energy, Arizona State University, Tempe, AZ 85287-6106 (United States)

    2015-09-15

    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{sub 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.

  17. A bench-top automated workstation for nucleic acid isolation from clinical sample types.

    Science.gov (United States)

    Thakore, Nitu; Garber, Steve; Bueno, Arial; Qu, Peter; Norville, Ryan; Villanueva, Michael; Chandler, Darrell P; Holmberg, Rebecca; Cooney, Christopher G

    2018-04-18

    Systems that automate extraction of nucleic acid from cells or viruses in complex clinical matrices have tremendous value even in the absence of an integrated downstream detector. We describe our bench-top automated workstation that integrates our previously-reported extraction method - TruTip - with our newly-developed mechanical lysis method. This is the first report of this method for homogenizing viscous and heterogeneous samples and lysing difficult-to-disrupt cells using "MagVor": a rotating magnet that rotates a miniature stir disk amidst glass beads confined inside of a disposable tube. Using this system, we demonstrate automated nucleic acid extraction from methicillin-resistant Staphylococcus aureus (MRSA) in nasopharyngeal aspirate (NPA), influenza A in nasopharyngeal swabs (NPS), human genomic DNA from whole blood, and Mycobacterium tuberculosis in NPA. The automated workstation yields nucleic acid with comparable extraction efficiency to manual protocols, which include commercially-available Qiagen spin column kits, across each of these sample types. This work expands the scope of applications beyond previous reports of TruTip to include difficult-to-disrupt cell types and automates the process, including a method for removal of organics, inside a compact bench-top workstation. Copyright © 2018 Elsevier B.V. All rights reserved.

  18. Sample preparation methods for quantitative detection of DNA by molecular assays and marine biosensors.

    Science.gov (United States)

    Cox, Annie M; Goodwin, Kelly D

    2013-08-15

    The need for quantitative molecular methods is growing in environmental, food, and medical fields but is hindered by low and variable DNA extraction and by co-extraction of PCR inhibitors. DNA extracts from Enterococcus faecium, seawater, and seawater spiked with E. faecium and Vibrio parahaemolyticus were tested by qPCR for target recovery and inhibition. Conventional and novel methods were tested, including Synchronous Coefficient of Drag Alteration (SCODA) and lysis and purification systems used on an automated genetic sensor (the Environmental Sample Processor, ESP). Variable qPCR target recovery and inhibition were measured, significantly affecting target quantification. An aggressive lysis method that utilized chemical, enzymatic, and mechanical disruption enhanced target recovery compared to commercial kit protocols. SCODA purification did not show marked improvement over commercial spin columns. Overall, data suggested a general need to improve sample preparation and to accurately assess and account for DNA recovery and inhibition in qPCR applications. Published by Elsevier Ltd.

  19. Feasibility of surface sampling in automated inspection of concrete aggregates during bulk transport on a conveyor

    NARCIS (Netherlands)

    Bakker, M.C.M.; Di Maio, F.; Lotfi, S.; Bakker, M.; Hu, M.; Vahidi, A.

    2017-01-01

    Automated optic inspection of concrete aggregates for pollutants (e.g. wood, plastics, gypsum and brick) is required to establish the suitability for reuse in new concrete products. Inspection is more efficient when directly sampling the materials on the conveyor belt instead of feeding them in a

  20. An automated high pressure reaction vessel for routine preparation of short-lived radiopharmaceuticals

    International Nuclear Information System (INIS)

    Ropchan, J.R.; Ricci, A.R.; Low, G.C.; Phelps, M.E.; Barrio, J.R.; California Univ., Los Angeles

    1986-01-01

    A remote, automated high-pressure/temperature system for preparation of radiopharmaceuticals is described. The system was routinely employed in our laboratories in the production of multimillicurie amounts of 11 C labeled D,L-amino acids in more than 90 production runs, with typical final D,L-product activities of 240-400 mCi. The high pressure system, however, is not restricted only to the production of 11 C labeled amino acids, but for application in any synthetic procedure requiring high pressure (approx. 300 psia) and temperature (>300 0 C). (author)

  1. 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.

  2. Rapid filtration separation-based sample preparation method for Bacillus spores in powdery and environmental matrices.

    Science.gov (United States)

    Isabel, Sandra; Boissinot, Maurice; Charlebois, Isabelle; Fauvel, Chantal M; Shi, Lu-E; Lévesque, Julie-Christine; Paquin, Amélie T; Bastien, Martine; Stewart, Gale; Leblanc, Eric; Sato, Sachiko; Bergeron, Michel G

    2012-03-01

    Authorities frequently need to analyze suspicious powders and other samples for biothreat agents in order to assess environmental safety. Numerous nucleic acid detection technologies have been developed to detect and identify biowarfare agents in a timely fashion. The extraction of microbial nucleic acids from a wide variety of powdery and environmental samples to obtain a quality level adequate for these technologies still remains a technical challenge. We aimed to develop a rapid and versatile method of separating bacteria from these samples and then extracting their microbial DNA. Bacillus atrophaeus subsp. globigii was used as a simulant of Bacillus anthracis. We studied the effects of a broad variety of powdery and environmental samples on PCR detection and the steps required to alleviate their interference. With a benchmark DNA extraction procedure, 17 of the 23 samples investigated interfered with bacterial lysis and/or PCR-based detection. Therefore, we developed the dual-filter method for applied recovery of microbial particles from environmental and powdery samples (DARE). The DARE procedure allows the separation of bacteria from contaminating matrices that interfere with PCR detection. This procedure required only 2 min, while the DNA extraction process lasted 7 min, for a total of sample preparation procedure allowed the recovery of cleaned bacterial spores and relieved detection interference caused by a wide variety of samples. Our procedure was easily completed in a laboratory facility and is amenable to field application and automation.

  3. 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)

  4. Thermophilic Campylobacter spp. in turkey samples: evaluation of two automated enzyme immunoassays and conventional microbiological techniques

    DEFF Research Database (Denmark)

    Borck, Birgitte; Stryhn, H.; Ersboll, A.K.

    2002-01-01

    Aims: To determine the sensitivity and specificity of two automated enzyme immunoassays (EIA), EiaFoss and Minividas, and a conventional microbiological culture technique for detecting thermophilic Campylobacter spp. in turkey samples. Methods and Results: A total of 286 samples (faecal, meat......, neckskin and environmental samples) were collected over a period of 4 months at a turkey slaughterhouse and meat-cutting plant in Denmark. Faecal and environmental samples were tested by the conventional culture method and by the two EIAs, whereas meat and neckskin samples were tested by the two EIAs only...

  5. [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.

  6. Feasibility of automated speech sample collection with stuttering children using interactive voice response (IVR) technology.

    Science.gov (United States)

    Vogel, Adam P; Block, Susan; Kefalianos, Elaina; Onslow, Mark; Eadie, Patricia; Barth, Ben; Conway, Laura; Mundt, James C; Reilly, Sheena

    2015-04-01

    To investigate the feasibility of adopting automated interactive voice response (IVR) technology for remotely capturing standardized speech samples from stuttering children. Participants were 10 6-year-old stuttering children. Their parents called a toll-free number from their homes and were prompted to elicit speech from their children using a standard protocol involving conversation, picture description and games. The automated IVR system was implemented using an off-the-shelf telephony software program and delivered by a standard desktop computer. The software infrastructure utilizes voice over internet protocol. Speech samples were automatically recorded during the calls. Video recordings were simultaneously acquired in the home at the time of the call to evaluate the fidelity of the telephone collected samples. Key outcome measures included syllables spoken, percentage of syllables stuttered and an overall rating of stuttering severity using a 10-point scale. Data revealed a high level of relative reliability in terms of intra-class correlation between the video and telephone acquired samples on all outcome measures during the conversation task. Findings were less consistent for speech samples during picture description and games. Results suggest that IVR technology can be used successfully to automate remote capture of child speech samples.

  7. 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

  8. 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)

  9. 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)

  10. Sample registration software for process automation in the Neutron Activation Analysis (NAA) Facility in Malaysia nuclear agency

    Energy Technology Data Exchange (ETDEWEB)

    Rahman, Nur Aira Abd, E-mail: nur-aira@nuclearmalaysia.gov.my; Yussup, Nolida; Ibrahim, Maslina Bt. Mohd; Mokhtar, Mukhlis B.; Soh Shaari, Syirrazie Bin Che; Azman, Azraf B. [Technical Support Division, Malaysian Nuclear Agency, 43000, Kajang, Selangor (Malaysia); Salim, Nazaratul Ashifa Bt. Abdullah [Division of Waste and Environmental Technology, Malaysian Nuclear Agency, 43000, Kajang, Selangor (Malaysia); Ismail, Nadiah Binti [Fakulti Kejuruteraan Elektrik, UiTM Pulau Pinang, 13500 Permatang Pauh, Pulau Pinang (Malaysia)

    2015-04-29

    Neutron Activation Analysis (NAA) had been established in Nuclear Malaysia since 1980s. Most of the procedures established were done manually including sample registration. The samples were recorded manually in a logbook and given ID number. Then all samples, standards, SRM and blank were recorded on the irradiation vial and several forms prior to irradiation. These manual procedures carried out by the NAA laboratory personnel were time consuming and not efficient. Sample registration software is developed as part of IAEA/CRP project on ‘Development of Process Automation in the Neutron Activation Analysis (NAA) Facility in Malaysia Nuclear Agency (RC17399)’. The objective of the project is to create a pc-based data entry software during sample preparation stage. This is an effective method to replace redundant manual data entries that needs to be completed by laboratory personnel. The software developed will automatically generate sample code for each sample in one batch, create printable registration forms for administration purpose, and store selected parameters that will be passed to sample analysis program. The software is developed by using National Instruments Labview 8.6.

  11. On sample preparation and dielectric breakdown in nanostructured epoxy resins

    Energy Technology Data Exchange (ETDEWEB)

    Reading, M; Xu, Z; Lewin, P L; Vaughan, A S, E-mail: asv@ecs.soton.ac.uk [Tony Davies High Voltage Laboratory, University of Southampton (United Kingdom)

    2011-08-12

    There are many methods available to achieve a good dispersion of fillers within a polymeric matrix. This investigation considered several methods of dispersing three chosen fillers within an epoxy resin; the same processes were also performed on unfilled materials to investigate any effects they may have on the host material. For this investigation, the epoxy system (EP) was combined with sodium montmorillonite (MMT), micrometric silicon dioxide (SD) or nanometric silicon dioxide (NSD) as fillers. The effect of the different sample preparation routes on breakdown behaviour was then evaluated. While more thorough mixing protocols were found to lead to improved breakdown behaviour in the case of the various filled systems, surprisingly, an entirely equivalent form of behaviour was also seen in the unfilled epoxy. The influence of changes in sample geometry on the breakdown strength was established.

  12. 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.

  13. Preparation of higher-actinide burnup and cross section samples

    International Nuclear Information System (INIS)

    Adair, H.L.; Kobisk, E.H.; Quinby, T.C.; Thomas, D.K.; Dailey, J.M.

    1981-01-01

    A joint research program involving the United States and the United Kingdom was instigated about four years ago for the purpose of studying burnup of higher actinides using in-core irradiation in the fast reactor at Dounreay, Scotland. Simultaneously, determination of cross sections of a wide variety of higher actinide isotopes was proposed. Coincidental neutron flux and energy spectral measurements were to be made using vanadium encapsulated dosimetry materials in the immediate region of the burnup and cross section samples. The higher actinide samples chosen for the burnup study were 241 Am and 244 Cm in the forms of Am 2 O 3 , Cm 2 O 3 , and Am 6 Cm(RE) 7 O 21 , where (RE) represents a mixture of lanthanide sesquioxides. It is the purpose of this paper to describe technology development and its application in the preparation of the fuel specimens and the cross section specimens that are being used in this cooperative program

  14. 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.

  15. Collection and preparation of water samples for hydrogeochemical reconnaissance

    International Nuclear Information System (INIS)

    Baucom, E.I.; Ferguson, R.B.; Wallace, R.M.

    1977-01-01

    A method based on ion exchange and neutron activation analysis (NAA) was developed and field-tested to determine uranium over the range 0.02 to 10,000 ppb in natural water using a single procedure. Water samples are filtered in the field using a specially-designed one-liter filter apparatus pressurized to 40 psig with an inert gas. The filtered water is treated with a high purity, mixed cation-anion resin in the hydronium-hydroxide form. All ions are removed from solution under the strong driving force of the neutralization reaction. Anionic, cationic, and natural complexes of uranium can be concentrated with this method. Field tests showed greater than 95 percent recovery of 13 elements analyzed (including greater than 99 percent recovery of uranium) and greater than or equal to 90 percent recovery of 4 other elements. Uranium collected on the resin was quantitatively determined by NAA. Coefficient of variation for sampling plus analysis was less than 20 percent for samples containing more than 0.1 ppb uranium. Advantages of this method include: (1) wide dynamic range, (2) low detection limit for uranium (0.02 ppb), (3) high precision and accuracy, (4) relatively low cost, (5) high-yield recovery from low-level aqueous samples without risk of loss to containers, (6) decreased risk of significant sample contamination compared with other low-level methods, (7) production of stable samples suitable for retrievable storage, and(8) concentration of other ions that can be determined by NAA. This paper presents (1) background regarding development of procedures for sample collection and preparation, (2) results of development programs, (3) description of equipment and field procedures, and (4) preliminary conclusions regarding use of this technology for hydrogeochemical reconnaissance for uranium

  16. NGSI FY15 Final Report. Innovative Sample Preparation for in-Field Uranium Isotopic Determinations

    Energy Technology Data Exchange (ETDEWEB)

    Yoshida, Thomas M. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Meyers, Lisa [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2015-11-10

    Our FY14 Final Report included an introduction to the project, background, literature search of uranium dissolution methods, assessment of commercial off the shelf (COTS) automated sample preparation systems, as well as data and results for dissolution of bulk quantities of uranium oxides, and dissolution of uranium oxides from swipe filter materials using ammonium bifluoride (ABF). Also, discussed were reaction studies of solid ABF with uranium oxide that provided a basis for determining the ABF/uranium oxide dissolution mechanism. This report details the final experiments for optimizing dissolution of U3O8 and UO2 using ABF and steps leading to development of a Standard Operating Procedure (SOP) for dissolution of uranium oxides on swipe filters.

  17. 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

  18. Small sample sorting of primary adherent cells by automated micropallet imaging and release.

    Science.gov (United States)

    Shah, Pavak K; Herrera-Loeza, Silvia Gabriela; Sims, Christopher E; Yeh, Jen Jen; Allbritton, Nancy L

    2014-07-01

    Primary patient samples are the gold standard for molecular investigations of tumor biology yet are difficult to acquire, heterogeneous in nature and variable in size. Patient-derived xenografts (PDXs) comprised of primary tumor tissue cultured in host organisms such as nude mice permit the propagation of human tumor samples in an in vivo environment and closely mimic the phenotype and gene expression profile of the primary tumor. Although PDX models reduce the cost and complexity of acquiring sample tissue and permit repeated sampling of the primary tumor, these samples are typically contaminated by immune, blood, and vascular tissues from the host organism while also being limited in size. For very small tissue samples (on the order of 10(3) cells) purification by fluorescence-activated cell sorting (FACS) is not feasible while magnetic activated cell sorting (MACS) of small samples results in very low purity, low yield, and poor viability. We developed a platform for imaging cytometry integrated with micropallet array technology to perform automated cell sorting on very small samples obtained from PDX models of pancreatic and colorectal cancer using antibody staining of EpCAM (CD326) as a selection criteria. These data demonstrate the ability to automate and efficiently separate samples with very low number of cells. © 2014 International Society for Advancement of Cytometry.

  19. Design aspects of automation system for initial processing of fecal samples

    International Nuclear Information System (INIS)

    Sawant, Pramilla D.; Prabhu, Supreetha P.; Suja, A.; Wankhede, Sonal; Chaudhary, Seema; Rao, D.D.; Pradeepkumar, K.S.; Das, A.P.; Badodkar, B.D.

    2014-01-01

    The procedure for initial handling of the fecal samples at Bioassay Lab., Trombay is as follows: overnight fecal samples are collected from the worker in a kit consisting of a polythene bag placed in a wide mouth polythene container closed with an inner lid and a screw cap. Occupational worker collects the sample in the polythene bag. On receiving the sample, the polythene container along with the sample is weighed, polythene bag containing fecal sample is lifted out of the container using a pair of tongs placed inside a crucible and ashed inside a muffle furnace at 450℃. After complete ashing, the crucible containing white ash is taken-up for further radiochemical processing. This paper describes the various steps in developing a prototype automated system for initial handling of fecal samples. The proposed system for handling and processing of fecal samples is proposed to automate the above. The system once developed will help eliminate manual intervention till the ashing stage and reduce the biological hazard involved in handling such samples mentioned procedure

  20. Preparation of tissue samples for X-ray fluorescence microscopy

    International Nuclear Information System (INIS)

    Chwiej, Joanna; Szczerbowska-Boruchowska, Magdalena; Lankosz, Marek; Wojcik, Slawomir; Falkenberg, Gerald; Stegowski, Zdzislaw; Setkowicz, Zuzanna

    2005-01-01

    As is well-known, trace elements, especially metals, play an important role in the pathogenesis of many disorders. The topographic and quantitative elemental analysis of pathologically changed tissues may shed some new light on processes leading to the degeneration of cells in the case of selected diseases. An ideal and powerful tool for such purpose is the Synchrotron Microbeam X-ray Fluorescence technique. It enables the carrying out of investigations of the elemental composition of tissues even at the single cell level. The tissue samples for histopathological investigations are routinely fixed and embedded in paraffin. The authors try to verify the usefulness of such prepared tissue sections for elemental analysis with the use of X-ray fluorescence microscopy. Studies were performed on rat brain samples. Changes in elemental composition caused by fixation in formalin or paraformaldehyde and embedding in paraffin were examined. Measurements were carried out at the bending magnet beamline L of the Hamburger Synchrotronstrahlungslabor HASYLAB in Hamburg. The decrease in mass per unit area of K, Br and the increase in P, S, Fe, Cu and Zn in the tissue were observed as a result of the fixation. For the samples embedded in paraffin, a lower level of most elements was observed. Additionally, for these samples, changes in the composition of some elements were not uniform for different analyzed areas of rat brain

  1. An automated system for the preparation of Large Size Dried (LSD) Spikes

    International Nuclear Information System (INIS)

    Verbruggen, A.; Bauwens, J.; Jakobsson, U.; Eykens, R.; Wellum, R.; Aregbe, Y.; Van De Steene, N.

    2008-01-01

    Large size dried (LSD) spikes have been produced to fulfill the existing requirement for reliable and traceable isotopic reference materials for nuclear safeguards. A system to produce certified nuclear isotopic reference material as a U/Pu mixture in the form of large size dried spikes, comparable to those produced using traditional methods has been installed in collaboration with Nucomat, a company with a recognized reputation in design and development of integrated automated systems. The major components of the system are a robot, two balances, a dispenser and a drying unit fitted into a glove box. The robot is software driven and designed to control all movements inside the glove-box, to identify unambiguously the penicillin vials with a bar-code reader, to dispense the LSD batch solution into the vials and to weigh the amount dispensed. The system functionality has been evaluated and the performance validated by comparing the results from a series of samples dispensed and weighed by the automated system with the results by manual substitution weighing. After applying the proper correction factors to the data from the automated system balance no significant difference was observed between the two. However, an additional component of uncertainty of 3*10 -4 is introduced in the uncertainty budget for the certified weights provided by the automatic system. (authors)

  2. Automatic sample changer control software for automation of neutron activation analysis process in Malaysian Nuclear Agency

    Science.gov (United States)

    Yussup, N.; Ibrahim, M. M.; Rahman, N. A. A.; Mokhtar, M.; Salim, N. A. A.; Soh@Shaari, S. C.; Azman, A.; Lombigit, L.; Azman, A.; Omar, S. A.

    2018-01-01

    Most of the procedures in neutron activation analysis (NAA) process that has been established in Malaysian Nuclear Agency (Nuclear Malaysia) since 1980s were performed manually. These manual procedures carried out by the NAA laboratory personnel are time consuming and inefficient especially for sample counting and measurement process. The sample needs to be changed and the measurement software needs to be setup for every one hour counting time. Both of these procedures are performed manually for every sample. Hence, an automatic sample changer system (ASC) that consists of hardware and software is developed to automate sample counting process for up to 30 samples consecutively. This paper describes the ASC control software for NAA process which is designed and developed to control the ASC hardware and call GammaVision software for sample measurement. The software is developed by using National Instrument LabVIEW development package.

  3. Portable Automation of Static Chamber Sample Collection for Quantifying Soil Gas Flux

    Energy Technology Data Exchange (ETDEWEB)

    Davis, Morgan P.; Groh, Tyler A.; Parkin, Timothy B.; Williams, Ryan J.; Isenhart, Thomas M.; Hofmockel, Kirsten S.

    2018-01-01

    Quantification of soil gas flux using the static chamber method is labor intensive. The number of chambers that can be sampled is limited by the spacing between chambers and the availability of trained research technicians. An automated system for collecting gas samples from chambers in the field would eliminate the need for personnel to return to the chamber during a flux measurement period and would allow a single technician to sample multiple chambers simultaneously. This study describes Chamber Automated Sampling Equipment (FluxCASE) to collect and store chamber headspace gas samples at assigned time points for the measurement of soil gas flux. The FluxCASE design and operation is described, and the accuracy and precision of the FluxCASE system is evaluated. In laboratory measurements of nitrous oxide (N2O), carbon dioxide (CO2), and methane (CH4) concentrations of a standardized gas mixture, coefficients of variation associated with automated and manual sample collection were comparable, indicating no loss of precision. In the field, soil gas fluxes measured from FluxCASEs were in agreement with manual sampling for both N2O and CO2. Slopes of regression equations were 1.01 for CO2 and 0.97 for N2O. The 95% confidence limits of the slopes of the regression lines included the value of one, indicating no bias. Additionally, an expense analysis found a cost recovery ranging from 0.6 to 2.2 yr. Implementing the FluxCASE system is an alternative to improve the efficiency of the static chamber method for measuring soil gas flux while maintaining the accuracy and precision of manual sampling.

  4. 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.

  5. Review of online coupling of sample preparation techniques with liquid chromatography.

    Science.gov (United States)

    Pan, Jialiang; Zhang, Chengjiang; Zhang, Zhuomin; Li, Gongke

    2014-03-07

    Sample preparation is still considered as the bottleneck of the whole analytical procedure, and efforts has been conducted towards the automation, improvement of sensitivity and accuracy, and low comsuption of organic solvents. Development of online sample preparation techniques (SP) coupled with liquid chromatography (LC) is a promising way to achieve these goals, which has attracted great attention. This article reviews the recent advances on the online SP-LC techniques. Various online SP techniques have been described and summarized, including solid-phase-based extraction, liquid-phase-based extraction assisted with membrane, microwave assisted extraction, ultrasonic assisted extraction, accelerated solvent extraction and supercritical fluids extraction. Specially, the coupling approaches of online SP-LC systems and the corresponding interfaces have been discussed and reviewed in detail, such as online injector, autosampler combined with transport unit, desorption chamber and column switching. Typical applications of the online SP-LC techniques have been summarized. Then the problems and expected trends in this field are attempted to be discussed and proposed in order to encourage the further development of online SP-LC techniques. Copyright © 2014 Elsevier B.V. All rights reserved.

  6. Automated Prediction of Catalytic Mechanism and Rate Law Using Graph-Based Reaction Path Sampling.

    Science.gov (United States)

    Habershon, Scott

    2016-04-12

    In a recent article [ J. Chem. Phys. 2015 , 143 , 094106 ], we introduced a novel graph-based sampling scheme which can be used to generate chemical reaction paths in many-atom systems in an efficient and highly automated manner. The main goal of this work is to demonstrate how this approach, when combined with direct kinetic modeling, can be used to determine the mechanism and phenomenological rate law of a complex catalytic cycle, namely cobalt-catalyzed hydroformylation of ethene. Our graph-based sampling scheme generates 31 unique chemical products and 32 unique chemical reaction pathways; these sampled structures and reaction paths enable automated construction of a kinetic network model of the catalytic system when combined with density functional theory (DFT) calculations of free energies and resultant transition-state theory rate constants. Direct simulations of this kinetic network across a range of initial reactant concentrations enables determination of both the reaction mechanism and the associated rate law in an automated fashion, without the need for either presupposing a mechanism or making steady-state approximations in kinetic analysis. Most importantly, we find that the reaction mechanism which emerges from these simulations is exactly that originally proposed by Heck and Breslow; furthermore, the simulated rate law is also consistent with previous experimental and computational studies, exhibiting a complex dependence on carbon monoxide pressure. While the inherent errors of using DFT simulations to model chemical reactivity limit the quantitative accuracy of our calculated rates, this work confirms that our automated simulation strategy enables direct analysis of catalytic mechanisms from first principles.

  7. RoboDiff: combining a sample changer and goniometer for highly automated macromolecular crystallography experiments.

    Science.gov (United States)

    Nurizzo, Didier; Bowler, Matthew W; Caserotto, Hugo; Dobias, Fabien; Giraud, Thierry; Surr, John; Guichard, Nicolas; Papp, Gergely; Guijarro, Matias; Mueller-Dieckmann, Christoph; Flot, David; McSweeney, Sean; Cipriani, Florent; Theveneau, Pascal; Leonard, Gordon A

    2016-08-01

    Automation of the mounting of cryocooled samples is now a feature of the majority of beamlines dedicated to macromolecular crystallography (MX). Robotic sample changers have been developed over many years, with the latest designs increasing capacity, reliability and speed. Here, the development of a new sample changer deployed at the ESRF beamline MASSIF-1 (ID30A-1), based on an industrial six-axis robot, is described. The device, named RoboDiff, includes a high-capacity dewar, acts as both a sample changer and a high-accuracy goniometer, and has been designed for completely unattended sample mounting and diffraction data collection. This aim has been achieved using a high level of diagnostics at all steps of the process from mounting and characterization to data collection. The RoboDiff has been in service on the fully automated endstation MASSIF-1 at the ESRF since September 2014 and, at the time of writing, has processed more than 20 000 samples completely automatically.

  8. Development and Testing of an Automated 4-Day Text Messaging Guidance as an Aid for Improving Colonoscopy Preparation.

    Science.gov (United States)

    Walter, Benjamin Michael; Klare, Peter; Neu, Bruno; Schmid, Roland M; von Delius, Stefan

    2016-06-21

    In gastroenterology a sufficient colon cleansing improves adenoma detection rate and prevents the need for preterm repeat colonoscopies due to invalid preparation. It has been shown that patient education is of major importance for improvement of colon cleansing. Objective of this study was to assess the function of an automated text messaging (short message service, SMS)-supported colonoscopy preparation starting 4 days before colonoscopy appointment. After preevaluation to assess mobile phone usage in the patient population for relevance of this approach, a Web-based, automated SMS text messaging system was developed, following which a single-center feasibility study at a tertiary care center was performed. Patients scheduled for outpatient colonoscopy were invited to participate. Patients enrolled in the study group received automated information about dietary recommendations and bowel cleansing during colonoscopy preparation. Data of outpatient colonoscopies with regular preparation procedure were used for pair matching and served as control. Primary end point was feasibility of SMS text messaging support in colonoscopy preparation assessed as stable and satisfactory function of the system. Secondary end points were quality of bowel preparation according to the Boston Bowel Preparation Scale (BBPS) and patient satisfaction with SMS text messaging-provided information assessed by a questionnaire. Web-based SMS text messaging-supported colonoscopy preparation was successful and feasible in 19 of 20 patients. Mean (standard error of the mean, SEM) total BBPS score was slightly higher in the SMS group than in the control group (7.3, SEM 0.3 vs 6.4, SEM 0.2) and for each colonic region (left, transverse, and right colon). Patient satisfaction regarding SMS text messaging-based information was high. Using SMS for colonoscopy preparation with 4 days' guidance including dietary recommendation is a new approach to improve colonoscopy preparation. Quality of colonoscopy

  9. Automated low energy photon absorption equipment for measuring internal moisture and density distributions of wood samples

    International Nuclear Information System (INIS)

    Tiitta, M.; Olkkonen, H.; Lappalainen, T.; Kanko, T.

    1993-01-01

    Automated equipment for measuring the moisture and density distributions of wood samples was developed. Using a narrow beam of gamma rays, the equipment scans the wood samples, which are placed on the moving belt. The moisture measurement is based on the 241 Am photon absorption technique (59.5 keV), where the difference of the linear absorption coefficients of the moist and dry wood is measured. The method requires no knowledge of the thickness of the specimen. The density estimation method is based on the measurement of the linear attenuation coefficient of wood. Comprehensive software including image processing was developed for treatment of the numerical values of the measurements. (author)

  10. Novel sample preparation for operando TEM of catalysts.

    Science.gov (United States)

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

    2015-09-01

    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. Copyright © 2015 Elsevier B.V. All rights reserved.

  11. AG-NGS: a powerful and user-friendly computing application for the semi-automated preparation of next-generation sequencing libraries using open liquid handling platforms.

    Science.gov (United States)

    Callejas, Sergio; Álvarez, Rebeca; Benguria, Alberto; Dopazo, Ana

    2014-01-01

    Next-generation sequencing (NGS) is becoming one of the most widely used technologies in the field of genomics. Library preparation is one of the most critical, hands-on, and time-consuming steps in the NGS workflow. Each library must be prepared in an independent well, increasing the number of hours required for a sequencing run and the risk of human-introduced error. Automation of library preparation is the best option to avoid these problems. With this in mind, we have developed automatic genomics NGS (AG-NGS), a computing application that allows an open liquid handling platform to be transformed into a library preparation station without losing the potential of an open platform. Implementation of AG-NGS does not require programming experience, and the application has also been designed to minimize implementation costs. Automated library preparation with AG-NGS generated high-quality libraries from different samples, demonstrating its efficiency, and all quality control parameters fell within the range of optimal values.

  12. Development testing of the chemical analysis automation polychlorinated biphenyl standard analysis method during surface soils sampling at the David Witherspoon 1630 site

    International Nuclear Information System (INIS)

    Hunt, M.A.; Klatt, L.N.; Thompson, D.H.

    1998-02-01

    The Chemical Analysis Automation (CAA) project is developing standardized, software-driven, site-deployable robotic laboratory systems with the objective of lowering the per-sample analysis cost, decreasing sample turnaround time, and minimizing human exposure to hazardous and radioactive materials associated with DOE remediation projects. The first integrated system developed by the CAA project is designed to determine polychlorinated biphenyls (PCB) content in soil matrices. A demonstration and development testing of this system was conducted in conjuction with surface soil characterization activities at the David Witherspoon 1630 Site in Knoxville, Tennessee. The PCB system consists of five hardware standard laboratory modules (SLMs), one software SLM, the task sequence controller (TSC), and the human-computer interface (HCI). Four of the hardware SLMs included a four-channel Soxhlet extractor, a high-volume concentrator, a column cleanup, and a gas chromatograph. These SLMs performed the sample preparation and measurement steps within the total analysis protocol. The fifth hardware module was a robot that transports samples between the SLMs and the required consumable supplies to the SLMs. The software SLM is an automated data interpretation module that receives raw data from the gas chromatograph SLM and analyzes the data to yield the analyte information. The TSC is a software system that provides the scheduling, management of system resources, and the coordination of all SLM activities. The HCI is a graphical user interface that presents the automated laboratory to the analyst in terms of the analytical procedures and methods. Human control of the automated laboratory is accomplished via the HCI. Sample information required for processing by the automated laboratory is entered through the HCI. Information related to the sample and the system status is presented to the analyst via graphical icons

  13. 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)

  14. Fully automated gamma spectrometry gauge observing possible radioactive contamination of melting-shop samples

    International Nuclear Information System (INIS)

    Kroos, J.; Westkaemper, G.; Stein, J.

    1999-01-01

    At Salzgitter AG, several monitoring systems have been installed to check the scrap transport by rail and by car. At the moment, the scrap transport by ship is reloaded onto wagons for monitoring afterwards. In the future, a detection system will be mounted onto a crane for a direct check on scrap upon the departure of ship. Furthermore, at Salzgitter AG Central Chemical Laboratory, a fully automated gamma spectrometry gauge is installed in order to observe a possible radioactive contamination of the products. The gamma spectrometer is integrated into the automated OE spectrometry line for testing melting shop samples after performing the OE spectrometry. With this technique the specific activity of selected nuclides and dose rate will be determined. The activity observation is part of the release procedure. The corresponding measurement data are stored in a database for quality management reasons. (author)

  15. 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

  16. Liquid-Based Medium Used to Prepare Cytological Breast Nipple Fluid Improves the Quality of Cellular Samples Automatic Collection

    Science.gov (United States)

    Zonta, Marco Antonio; Velame, Fernanda; Gema, Samara; Filassi, Jose Roberto; Longatto-Filho, Adhemar

    2014-01-01

    Background Breast cancer is the second cause of death in women worldwide. The spontaneous breast nipple discharge may contain cells that can be analyzed for malignancy. Halo® Mamo Cyto Test (HMCT) was recently developed as an automated system indicated to aspirate cells from the breast ducts. The objective of this study was to standardize the methodology of sampling and sample preparation of nipple discharge obtained by the automated method Halo breast test and perform cytological evaluation in samples preserved in liquid medium (SurePath™). Methods We analyzed 564 nipple fluid samples, from women between 20 and 85 years old, without history of breast disease and neoplasia, no pregnancy, and without gynecologic medical history, collected by HMCT method and preserved in two different vials with solutions for transport. Results From 306 nipple fluid samples from method 1, 199 (65%) were classified as unsatisfactory (class 0), 104 (34%) samples were classified as benign findings (class II), and three (1%) were classified as undetermined to neoplastic cells (class III). From 258 samples analyzed in method 2, 127 (49%) were classified as class 0, 124 (48%) were classified as class II, and seven (2%) were classified as class III. Conclusion Our study suggests an improvement in the quality and quantity of cellular samples when the association of the two methodologies is performed, Halo breast test and the method in liquid medium. PMID:29147397

  17. Automated, Ultra-Sterile Solid Sample Handling and Analysis on a Chip

    Science.gov (United States)

    Mora, Maria F.; Stockton, Amanda M.; Willis, Peter A.

    2013-01-01

    There are no existing ultra-sterile lab-on-a-chip systems that can accept solid samples and perform complete chemical analyses without human intervention. The proposed solution is to demonstrate completely automated lab-on-a-chip manipulation of powdered solid samples, followed by on-chip liquid extraction and chemical analysis. This technology utilizes a newly invented glass micro-device for solid manipulation, which mates with existing lab-on-a-chip instrumentation. Devices are fabricated in a Class 10 cleanroom at the JPL MicroDevices Lab, and are plasma-cleaned before and after assembly. Solid samples enter the device through a drilled hole in the top. Existing micro-pumping technology is used to transfer milligrams of powdered sample into an extraction chamber where it is mixed with liquids to extract organic material. Subsequent chemical analysis is performed using portable microchip capillary electrophoresis systems (CE). These instruments have been used for ultra-highly sensitive (parts-per-trillion, pptr) analysis of organic compounds including amines, amino acids, aldehydes, ketones, carboxylic acids, and thiols. Fully autonomous amino acid analyses in liquids were demonstrated; however, to date there have been no reports of completely automated analysis of solid samples on chip. This approach utilizes an existing portable instrument that houses optics, high-voltage power supplies, and solenoids for fully autonomous microfluidic sample processing and CE analysis with laser-induced fluorescence (LIF) detection. Furthermore, the entire system can be sterilized and placed in a cleanroom environment for analyzing samples returned from extraterrestrial targets, if desired. This is an entirely new capability never demonstrated before. The ability to manipulate solid samples, coupled with lab-on-a-chip analysis technology, will enable ultraclean and ultrasensitive end-to-end analysis of samples that is orders of magnitude more sensitive than the ppb goal given

  18. Preparation and purification of organic samples for selenium isotope studies.

    Science.gov (United States)

    Banning, Helena; Stelling, Monika; König, Stephan; Schoenberg, Ronny; Neumann, Thomas

    2018-01-01

    Selenium (Se) is an important micronutrient but also a strong toxin with a narrow tolerance range for many organisms. As such, a globally heterogeneous Se distribution in soils is responsible for various disease patterns (i.e. Se excess and deficiency) and environmental problems, whereby plants play a key role for the Se entrance into the biosphere. Selenium isotope variations were proved to be a powerful tracer for redox processes and are therefore promising for the exploration of the species dependent Se metabolism in plants and the Se cycling within the Critical Zone. Plant cultivation setups enable systematic controlled investigations, but samples derived from them-plant tissue and phytoagar-are particularly challenging and require specific preparation and purification steps to ensure precise and valid Se isotope analytics performed with HG-MC-ICP-MS. In this study, different methods for the entire process from solid tissue preparation to Se isotope measurements were tested, optimized and validated. A particular microwave digestion procedure for plant tissue and a vacuum filtration method for phytoagar led to full Se recoveries, whereby unfavorable organic residues were reduced to a minimum. Three purification methods predominantly described in the literature were systematically tested with pure Se solution, high concentrated multi-element standard solution as well as plant and phytoagar as target matrices. All these methods efficiently remove critical matrix elements, but differ in Se recovery and organic residues. Validation tests doping Se-free plant material and phytoagar with a reference material of known Se isotope composition revealed the high impact of organic residues on the accuracy of MC-ICP-MS measurements. Only the purification method with no detectable organic residues, hydride generation and trapping, results in valid mass bias correction for plant samples with an average deviation to true δ82/76Se values of 0.2 ‰ and a reproducibility (2 SD

  19. Construction and calibration of a low cost and fully automated vibrating sample magnetometer

    Energy Technology Data Exchange (ETDEWEB)

    El-Alaily, T.M., E-mail: toson_alaily@yahoo.com [Physics Department, Faculty of Science, Tanta University, Tanta (Egypt); El-Nimr, M.K.; Saafan, S.A.; Kamel, M.M.; Meaz, T.M. [Physics Department, Faculty of Science, Tanta University, Tanta (Egypt); Assar, S.T. [Engineering Physics and Mathematics Department, Faculty of Engineering, Tanta University, Tanta (Egypt)

    2015-07-15

    A low cost vibrating sample magnetometer (VSM) has been constructed by using an electromagnet and an audio loud speaker; where both are controlled by a data acquisition device. The constructed VSM records the magnetic hysteresis loop up to 8.3 KG at room temperature. The apparatus has been calibrated and tested by using magnetic hysteresis data of some ferrite samples measured by two scientifically calibrated magnetometers; model (Lake Shore 7410) and model (LDJ Electronics Inc. Troy, MI). Our VSM lab-built new design proved success and reliability. - Highlights: • A low cost automated vibrating sample magnetometer VSM has been constructed. • The VSM records the magnetic hysteresis loop up to 8.3 KG at room temperature. • The VSM has been calibrated and tested by using some measured ferrite samples. • Our VSM lab-built new design proved success and reliability.

  20. Automated Device for Asynchronous Extraction of RNA, DNA, or Protein Biomarkers from Surrogate Patient Samples.

    Science.gov (United States)

    Bitting, Anna L; Bordelon, Hali; Baglia, Mark L; Davis, Keersten M; Creecy, Amy E; Short, Philip A; Albert, Laura E; Karhade, Aditya V; Wright, David W; Haselton, Frederick R; Adams, Nicholas M

    2016-12-01

    Many biomarker-based diagnostic methods are inhibited by nontarget molecules in patient samples, necessitating biomarker extraction before detection. We have developed a simple device that purifies RNA, DNA, or protein biomarkers from complex biological samples without robotics or fluid pumping. The device design is based on functionalized magnetic beads, which capture biomarkers and remove background biomolecules by magnetically transferring the beads through processing solutions arrayed within small-diameter tubing. The process was automated by wrapping the tubing around a disc-like cassette and rotating it past a magnet using a programmable motor. This device recovered biomarkers at ~80% of the operator-dependent extraction method published previously. The device was validated by extracting biomarkers from a panel of surrogate patient samples containing clinically relevant concentrations of (1) influenza A RNA in nasal swabs, (2) Escherichia coli DNA in urine, (3) Mycobacterium tuberculosis DNA in sputum, and (4) Plasmodium falciparum protein and DNA in blood. The device successfully extracted each biomarker type from samples representing low levels of clinically relevant infectivity (i.e., 7.3 copies/µL of influenza A RNA, 405 copies/µL of E. coli DNA, 0.22 copies/µL of TB DNA, 167 copies/µL of malaria parasite DNA, and 2.7 pM of malaria parasite protein). © 2015 Society for Laboratory Automation and Screening.

  1. 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)

  2. Automated on-line liquid–liquid extraction system for temporal mass spectrometric analysis of dynamic samples

    Energy Technology Data Exchange (ETDEWEB)

    Hsieh, Kai-Ta; Liu, Pei-Han [Department of Applied Chemistry, National Chiao Tung University, 1001 University Rd, Hsinchu, 300, Taiwan (China); Urban, Pawel L. [Department of Applied Chemistry, National Chiao Tung University, 1001 University Rd, Hsinchu, 300, Taiwan (China); Institute of Molecular Science, National Chiao Tung University, 1001 University Rd, Hsinchu, 300, Taiwan (China)

    2015-09-24

    Most real samples cannot directly be infused to mass spectrometers because they could contaminate delicate parts of ion source and guides, or cause ion suppression. Conventional sample preparation procedures limit temporal resolution of analysis. We have developed an automated liquid–liquid extraction system that enables unsupervised repetitive treatment of dynamic samples and instantaneous analysis by mass spectrometry (MS). It incorporates inexpensive open-source microcontroller boards (Arduino and Netduino) to guide the extraction and analysis process. Duration of every extraction cycle is 17 min. The system enables monitoring of dynamic processes over many hours. The extracts are automatically transferred to the ion source incorporating a Venturi pump. Operation of the device has been characterized (repeatability, RSD = 15%, n = 20; concentration range for ibuprofen, 0.053–2.000 mM; LOD for ibuprofen, ∼0.005 mM; including extraction and detection). To exemplify its usefulness in real-world applications, we implemented this device in chemical profiling of pharmaceutical formulation dissolution process. Temporal dissolution profiles of commercial ibuprofen and acetaminophen tablets were recorded during 10 h. The extraction-MS datasets were fitted with exponential functions to characterize the rates of release of the main and auxiliary ingredients (e.g. ibuprofen, k = 0.43 ± 0.01 h{sup −1}). The electronic control unit of this system interacts with the operator via touch screen, internet, voice, and short text messages sent to the mobile phone, which is helpful when launching long-term (e.g. overnight) measurements. Due to these interactive features, the platform brings the concept of the Internet-of-Things (IoT) to the chemistry laboratory environment. - Highlights: • Mass spectrometric analysis normally requires sample preparation. • Liquid–liquid extraction can isolate analytes from complex matrices. • The proposed system automates

  3. Automated on-line liquid–liquid extraction system for temporal mass spectrometric analysis of dynamic samples

    International Nuclear Information System (INIS)

    Hsieh, Kai-Ta; Liu, Pei-Han; Urban, Pawel L.

    2015-01-01

    Most real samples cannot directly be infused to mass spectrometers because they could contaminate delicate parts of ion source and guides, or cause ion suppression. Conventional sample preparation procedures limit temporal resolution of analysis. We have developed an automated liquid–liquid extraction system that enables unsupervised repetitive treatment of dynamic samples and instantaneous analysis by mass spectrometry (MS). It incorporates inexpensive open-source microcontroller boards (Arduino and Netduino) to guide the extraction and analysis process. Duration of every extraction cycle is 17 min. The system enables monitoring of dynamic processes over many hours. The extracts are automatically transferred to the ion source incorporating a Venturi pump. Operation of the device has been characterized (repeatability, RSD = 15%, n = 20; concentration range for ibuprofen, 0.053–2.000 mM; LOD for ibuprofen, ∼0.005 mM; including extraction and detection). To exemplify its usefulness in real-world applications, we implemented this device in chemical profiling of pharmaceutical formulation dissolution process. Temporal dissolution profiles of commercial ibuprofen and acetaminophen tablets were recorded during 10 h. The extraction-MS datasets were fitted with exponential functions to characterize the rates of release of the main and auxiliary ingredients (e.g. ibuprofen, k = 0.43 ± 0.01 h −1 ). The electronic control unit of this system interacts with the operator via touch screen, internet, voice, and short text messages sent to the mobile phone, which is helpful when launching long-term (e.g. overnight) measurements. Due to these interactive features, the platform brings the concept of the Internet-of-Things (IoT) to the chemistry laboratory environment. - Highlights: • Mass spectrometric analysis normally requires sample preparation. • Liquid–liquid extraction can isolate analytes from complex matrices. • The proposed system automates the

  4. Automated gravimetric sample pretreatment using an industrial robot for the high-precision determination of plutonium by isotope dilution mass spectrometry.

    Science.gov (United States)

    Surugaya, Naoki; Hiyama, Toshiaki; Watahiki, Masaru

    2008-06-01

    A robotized sample-preparation method for the determination of Pu, which is recovered by extraction reprocessing of spent nuclear fuel, by isotope dilution mass spectrometry (IDMS) is described. The automated system uses a six-axis industrial robot, whose motility is very fast, accurate, and flexible, installed in a glove box. The automation of the weighing and dilution steps enables operator-unattended sample pretreatment for the high-precision analysis of Pu in aqueous solutions. Using the developed system, the Pu concentration in a HNO(3) medium was successfully determined using a set of subsequent mass spectrometric measurements. The relative uncertainty in determining the Pu concentration by IDMS using this system was estimated to be less than 0.1% (k = 2), which is equal to that expected of a talented analyst. The operation time required was the same as that for a skilled operator.

  5. Automated gravimetric sample pretreatment using an industrial robot for the high-precision determination of plutonium by isotope dilution mass spectrometry

    International Nuclear Information System (INIS)

    Surugaya, Naoki; Hiyama, Toshiaki; Watahiki, Masaru

    2008-01-01

    A robotized sample-preparation method for the determination of Pu, which is recovered by extraction reprocessing of spent nuclear fuel, by isotope dilution mass spectrometry (IDMS) is described. The automated system uses a six-axis industrial robot, whose motility is very fast, accurate, and flexible, installed in a glove box. The automation of the weighing and dilution steps enables operator-unattended sample pretreatment for the high-precision analysis of Pu in aqueous solutions. Using the developed system, the Pu concentration in a HNO 3 medium was successfully determined using a set of subsequent mass spectrometric measurements. The relative uncertainty in determining the Pu concentration by IDMS using this system was estimated to be less than 0.1% (k=2), which is equal to that expected of a talented analysis. The operation time required was the same as that for a skilled operator. (author)

  6. Sample preparation for measuring cow's progesterone in radioimmunoassay technique application

    International Nuclear Information System (INIS)

    Nuning Duria; Budi Santoso; Nuniek Lelananingtiyas; Wiranto Budi Santoso

    2010-01-01

    Sample preparation for measuring cow's progesterone in radioimmunoassay technique application has been done. Preparation includes the preparation of samples of cow's milk samples that has been carried out artificial insemination on day 0, 11 and 21. Then the standard making of progesterone in the form of fresh milk or skim milk (non fat) that has been removed its progesterone and through a series of chemical processes. The last is the preparation work on samples using the RIA kit I 125 . With this milk samples preparation, samples can be counted using RIA counter so that concentration of progesterone hormone can be determined accurately. (author)

  7. Automated sample exchange and tracking system for neutron research at cryogenic temperatures

    Science.gov (United States)

    Rix, J. E.; Weber, J. K. R.; Santodonato, L. J.; Hill, B.; Walker, L. M.; McPherson, R.; Wenzel, J.; Hammons, S. E.; Hodges, J.; Rennich, M.; Volin, K. J.

    2007-01-01

    An automated system for sample exchange and tracking in a cryogenic environment and under remote computer control was developed. Up to 24 sample "cans" per cycle can be inserted and retrieved in a programed sequence. A video camera acquires a unique identification marked on the sample can to provide a record of the sequence. All operations are coordinated via a LABVIEW™ program that can be operated locally or over a network. The samples are contained in vanadium cans of 6-10mm in diameter and equipped with a hermetically sealed lid that interfaces with the sample handler. The system uses a closed-cycle refrigerator (CCR) for cooling. The sample was delivered to a precooling location that was at a temperature of ˜25K, after several minutes, it was moved onto a "landing pad" at ˜10K that locates the sample in the probe beam. After the sample was released onto the landing pad, the sample handler was retracted. Reading the sample identification and the exchange operation takes approximately 2min. The time to cool the sample from ambient temperature to ˜10K was approximately 7min including precooling time. The cooling time increases to approximately 12min if precooling is not used. Small differences in cooling rate were observed between sample materials and for different sample can sizes. Filling the sample well and the sample can with low pressure helium is essential to provide heat transfer and to achieve useful cooling rates. A resistive heating coil can be used to offset the refrigeration so that temperatures up to ˜350K can be accessed and controlled using a proportional-integral-derivative control loop. The time for the landing pad to cool to ˜10K after it has been heated to ˜240K was approximately 20min.

  8. 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...

  9. Preparing and measuring ultra-small radiocarbon samples with the ARTEMIS AMS facility in Saclay, France

    Energy Technology Data Exchange (ETDEWEB)

    Delque-Kolic, E., E-mail: emmanuelle.delque-kolic@cea.fr [LMC14, CEA Saclay, Batiment 450 Porte 4E, 91191 Gif sur Yvette (France); Comby-Zerbino, C.; Ferkane, S.; Moreau, C.; Dumoulin, J.P.; Caffy, I.; Souprayen, C.; Quiles, A.; Bavay, D.; Hain, S.; Setti, V. [LMC14, CEA Saclay, Batiment 450 Porte 4E, 91191 Gif sur Yvette (France)

    2013-01-15

    The ARTEMIS facility in Saclay France measures, on average, 4500 samples a year for French organizations working in an array of fields, including environmental sciences, archeology and hydrology. In response to an increasing demand for the isolation of specific soil compounds and organic water fractions, we were motivated to evaluate our ability to reduce microgram samples using our standard graphitization lines and to measure the graphite thus obtained with our 3MV NEC Pelletron AMS. Our reduction facility consists of two fully automated graphitization lines. Each line has 12 reduction reactors with a reduction volume of 18 ml for the first line and 12 ml for the second. Under routine conditions, we determined that we could reduce the samples down to 10 {mu}g of carbon, even if the graphitization yield is consequently affected by the lower sample mass. Our results when testing different Fe/C ratios suggest that an amount of 1.5 mg of Fe powder was ideal (instead of lower amounts of catalyst) to prevent the sample from deteriorating too quickly under the Cs+ beam, and to facilitate pressing procedures. Several sets of microsamples produced from HOxI standard, international references and backgrounds were measured. When measuring {sup 14}C-free wood charcoal and HOxI samples we determined that our modern and dead blanks, due to the various preparation steps, were of 1.1 {+-} 0.8 and 0.2 {+-} 0.1 {mu}g, respectively. The results presented here were obtained for IAEA-C1, {sup 14}C-free wood, IAEA-C6, IAEA-C2 and FIRI C.

  10. 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.

  11. Rapid and Automated Determination of Plutonium and Neptunium in Environmental Samples

    DEFF Research Database (Denmark)

    Qiao, Jixin

    This thesis presents improved analytical methods for rapid and automated determination of plutonium and neptunium in environmental samples using sequential injection (SI) based chromatography and inductively coupled plasma mass spectrometry (ICP-MS). The progress of methodology development in thi...... environmental risk monitoring and assessment, emergency preparedness and surveillance of contaminated areas....... for rapid and simultaneous determination of plutonium and neptunium within an SI system (Paper VI). The results demonstrate that the developed methods in this study are reliable and efficient for accurate assays of trace levels of plutonium and neptunium as demanded in different situations including...

  12. A continuous flow from sample collection to data acceptability determination using an automated system

    International Nuclear Information System (INIS)

    Fisk, J.F.; Leasure, C.; Sauter, A.D.

    1993-01-01

    In its role as regulator, EPA is the recipient of enormous reams of analytical data, especially within the Superfund Program. In order to better manage the volume of paper that comes in daily, Superfund has required its laboratories to provide data that is contained on reporting forms to be delivered also on a diskette for uploading into data bases for various purposes, such as checking for contractual compliance, tracking quality assurance parameters, and, ultimately, for reviewing the data by computer. This last area, automated review of the data, has generated programs that are not necessarily appropriate for use by clients other than Superfund. Such is the case with Los Alamos National Laboratory's Environmental Chemistry Group and its emerging subcontractor community, designed to meet the needs of the remedial action program at LANL. LANL is in the process of implementing an automated system that will be used from the planning stage of sample collection to the production of a project-specific report on analytical data quality. Included are electronic scheduling and tracking of samples, data entry, checking and transmission, data assessment and qualification for use, and report generation that will tie the analytical data quality back to the performance criteria defined prior to sample collection. Industry standard products will be used (e.g., ORACLE, Microsoft Excel) to ensure support for users, prevent dependence on proprietary software, and to protect LANL's investment for the future

  13. Sample Preparation Report of the Fourth OPCW Confidence Building Exercise on Biomedical Sample Analysis

    Energy Technology Data Exchange (ETDEWEB)

    Udey, R. N. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Corzett, T. H. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Alcaraz, A. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2014-07-03

    Following the successful completion of the 3rd biomedical confidence building exercise (February 2013 – March 2013), which included the analysis of plasma and urine samples spiked at low ppb levels as part of the exercise scenario, another confidence building exercise was targeted to be conducted in 2014. In this 4th exercise, it was desired to focus specifically on the analysis of plasma samples. The scenario was designed as an investigation of an alleged use of chemical weapons where plasma samples were collected, as plasma has been reported to contain CWA adducts which remain present in the human body for several weeks (Solano et al. 2008). In the 3rd exercise most participants used the fluoride regeneration method to analyze for the presence of nerve agents in plasma samples. For the 4th biomedical exercise it was decided to evaluate the analysis of human plasma samples for the presence/absence of the VX adducts and aged adducts to blood proteins (e.g., VX-butyrylcholinesterase (BuChE) and aged BuChE adducts using a pepsin digest technique to yield nonapeptides; or equivalent). As the aging of VX-BuChE adducts is relatively slow (t1/2 = 77 hr at 37 °C [Aurbek et al. 2009]), soman (GD), which ages much more quickly (t1/2 = 9 min at 37 °C [Masson et al. 2010]), was used to simulate an aged VX sample. Additional objectives of this exercise included having laboratories assess novel OP-adducted plasma sample preparation techniques and analytical instrumentation methodologies, as well as refining/designating the reporting formats for these new techniques.

  14. Evaluation of an automated protocol for efficient and reliable DNA extraction of dietary samples.

    Science.gov (United States)

    Wallinger, Corinna; Staudacher, Karin; Sint, Daniela; Thalinger, Bettina; Oehm, Johannes; Juen, Anita; Traugott, Michael

    2017-08-01

    Molecular techniques have become an important tool to empirically assess feeding interactions. The increased usage of next-generation sequencing approaches has stressed the need of fast DNA extraction that does not compromise DNA quality. Dietary samples here pose a particular challenge, as these demand high-quality DNA extraction procedures for obtaining the minute quantities of short-fragmented food DNA. Automatic high-throughput procedures significantly decrease time and costs and allow for standardization of extracting total DNA. However, these approaches have not yet been evaluated for dietary samples. We tested the efficiency of an automatic DNA extraction platform and a traditional CTAB protocol, employing a variety of dietary samples including invertebrate whole-body extracts as well as invertebrate and vertebrate gut content samples and feces. Extraction efficacy was quantified using the proportions of successful PCR amplifications of both total and prey DNA, and cost was estimated in terms of time and material expense. For extraction of total DNA, the automated platform performed better for both invertebrate and vertebrate samples. This was also true for prey detection in vertebrate samples. For the dietary analysis in invertebrates, there is still room for improvement when using the high-throughput system for optimal DNA yields. Overall, the automated DNA extraction system turned out as a promising alternative to labor-intensive, low-throughput manual extraction methods such as CTAB. It is opening up the opportunity for an extensive use of this cost-efficient and innovative methodology at low contamination risk also in trophic ecology.

  15. 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.

  16. Development of an Automated and Sensitive Microfluidic Device for Capturing and Characterizing Circulating Tumor Cells (CTCs from Clinical Blood Samples.

    Directory of Open Access Journals (Sweden)

    Priya Gogoi

    Full Text Available Current analysis of circulating tumor cells (CTCs is hindered by sub-optimal sensitivity and specificity of devices or assays as well as lack of capability of characterization of CTCs with clinical biomarkers. Here, we validate a novel technology to enrich and characterize CTCs from blood samples of patients with metastatic breast, prostate and colorectal cancers using a microfluidic chip which is processed by using an automated staining and scanning system from sample preparation to image processing. The Celsee system allowed for the detection of CTCs with apparent high sensitivity and specificity (94% sensitivity and 100% specificity. Moreover, the system facilitated rapid capture of CTCs from blood samples and also allowed for downstream characterization of the captured cells by immunohistochemistry, DNA and mRNA fluorescence in-situ hybridization (FISH. In a subset of patients with prostate cancer we compared the technology with a FDA-approved CTC device, CellSearch and found a higher degree of sensitivity with the Celsee instrument. In conclusion, the integrated Celsee system represents a promising CTC technology for enumeration and molecular characterization.

  17. A Simple Method for Automated Solid Phase Extraction of Water Samples for Immunological Analysis of Small Pollutants.

    Science.gov (United States)

    Heub, Sarah; Tscharner, Noe; Kehl, Florian; Dittrich, Petra S; Follonier, Stéphane; Barbe, Laurent

    2016-01-01

    A new method for solid phase extraction (SPE) of environmental water samples is proposed. The developed prototype is cost-efficient and user friendly, and enables to perform rapid, automated and simple SPE. The pre-concentrated solution is compatible with analysis by immunoassay, with a low organic solvent content. A method is described for the extraction and pre-concentration of natural hormone 17β-estradiol in 100 ml water samples. Reverse phase SPE is performed with octadecyl-silica sorbent and elution is done with 200 µl of methanol 50% v/v. Eluent is diluted by adding di-water to lower the amount of methanol. After preparing manually the SPE column, the overall procedure is performed automatically within 1 hr. At the end of the process, estradiol concentration is measured by using a commercial enzyme-linked immune-sorbent assay (ELISA). 100-fold pre-concentration is achieved and the methanol content in only 10% v/v. Full recoveries of the molecule are achieved with 1 ng/L spiked de-ionized and synthetic sea water samples.

  18. Sample preparation methods for quantitative detection of DNA by molecular assays and marine biosensors

    International Nuclear Information System (INIS)

    Cox, Annie M.; Goodwin, Kelly D.

    2013-01-01

    Highlights: • DNA extraction methods affected measured qPCR target recovery. • Recovery and variability differed, sometimes by more than an order of magnitude. • SCODA did not offer significant improvement with PCR-inhibited seawater. • Aggressive lysis did appear to improve target recovery. • Reliable and affordable correction methods are needed for quantitative PCR. -- Abstract: The need for quantitative molecular methods is growing in environmental, food, and medical fields but is hindered by low and variable DNA extraction and by co-extraction of PCR inhibitors. DNA extracts from Enterococcus faecium, seawater, and seawater spiked with E. faecium and Vibrio parahaemolyticus were tested by qPCR for target recovery and inhibition. Conventional and novel methods were tested, including Synchronous Coefficient of Drag Alteration (SCODA) and lysis and purification systems used on an automated genetic sensor (the Environmental Sample Processor, ESP). Variable qPCR target recovery and inhibition were measured, significantly affecting target quantification. An aggressive lysis method that utilized chemical, enzymatic, and mechanical disruption enhanced target recovery compared to commercial kit protocols. SCODA purification did not show marked improvement over commercial spin columns. Overall, data suggested a general need to improve sample preparation and to accurately assess and account for DNA recovery and inhibition in qPCR applications

  19. An Energy Efficient Adaptive Sampling Algorithm in a Sensor Network for Automated Water Quality Monitoring.

    Science.gov (United States)

    Shu, Tongxin; Xia, Min; Chen, Jiahong; Silva, Clarence de

    2017-11-05

    Power management is crucial in the monitoring of a remote environment, especially when long-term monitoring is needed. Renewable energy sources such as solar and wind may be harvested to sustain a monitoring system. However, without proper power management, equipment within the monitoring system may become nonfunctional and, as a consequence, the data or events captured during the monitoring process will become inaccurate as well. This paper develops and applies a novel adaptive sampling algorithm for power management in the automated monitoring of the quality of water in an extensive and remote aquatic environment. Based on the data collected on line using sensor nodes, a data-driven adaptive sampling algorithm (DDASA) is developed for improving the power efficiency while ensuring the accuracy of sampled data. The developed algorithm is evaluated using two distinct key parameters, which are dissolved oxygen (DO) and turbidity. It is found that by dynamically changing the sampling frequency, the battery lifetime can be effectively prolonged while maintaining a required level of sampling accuracy. According to the simulation results, compared to a fixed sampling rate, approximately 30.66% of the battery energy can be saved for three months of continuous water quality monitoring. Using the same dataset to compare with a traditional adaptive sampling algorithm (ASA), while achieving around the same Normalized Mean Error (NME), DDASA is superior in saving 5.31% more battery energy.

  20. An Energy Efficient Adaptive Sampling Algorithm in a Sensor Network for Automated Water Quality Monitoring

    Directory of Open Access Journals (Sweden)

    Tongxin Shu

    2017-11-01

    Full Text Available Power management is crucial in the monitoring of a remote environment, especially when long-term monitoring is needed. Renewable energy sources such as solar and wind may be harvested to sustain a monitoring system. However, without proper power management, equipment within the monitoring system may become nonfunctional and, as a consequence, the data or events captured during the monitoring process will become inaccurate as well. This paper develops and applies a novel adaptive sampling algorithm for power management in the automated monitoring of the quality of water in an extensive and remote aquatic environment. Based on the data collected on line using sensor nodes, a data-driven adaptive sampling algorithm (DDASA is developed for improving the power efficiency while ensuring the accuracy of sampled data. The developed algorithm is evaluated using two distinct key parameters, which are dissolved oxygen (DO and turbidity. It is found that by dynamically changing the sampling frequency, the battery lifetime can be effectively prolonged while maintaining a required level of sampling accuracy. According to the simulation results, compared to a fixed sampling rate, approximately 30.66% of the battery energy can be saved for three months of continuous water quality monitoring. Using the same dataset to compare with a traditional adaptive sampling algorithm (ASA, while achieving around the same Normalized Mean Error (NME, DDASA is superior in saving 5.31% more battery energy.

  1. Automated high-volume aerosol sampling station for environmental radiation monitoring

    Energy Technology Data Exchange (ETDEWEB)

    Toivonen, H.; Honkamaa, T.; Ilander, T.; Leppaenen, A.; Nikkinen, M.; Poellaenen, R.; Ylaetalo, S

    1998-07-01

    An automated high-volume aerosol sampling station, known as CINDERELLA.STUK, for environmental radiation monitoring has been developed by the Radiation and Nuclear Safety Authority (STUK), Finland. The sample is collected on a glass fibre filter (attached into a cassette), the airflow through the filter is 800 m{sup 3}/h at maximum. During the sampling, the filter is continuously monitored with Na(I) scintillation detectors. After the sampling, the large filter is automatically cut into 15 pieces that form a small sample and after ageing, the pile of filter pieces is moved onto an HPGe detector. These actions are performed automatically by a robot. The system is operated at a duty cycle of 1 d sampling, 1 d decay and 1 d counting. Minimum detectable concentrations of radionuclides in air are typically 1Ae10 x 10{sup -6} Bq/m{sup 3}. The station is equipped with various sensors to reveal unauthorized admittance. These sensors can be monitored remotely in real time via Internet or telephone lines. The processes and operation of the station are monitored and partly controlled by computer. The present approach fulfils the requirements of CTBTO for aerosol monitoring. The concept suits well for nuclear material safeguards, too 10 refs.

  2. Amphiphilic mediated sample preparation for micro-flow cytometry

    Science.gov (United States)

    Clague, David S [Livermore, CA; Wheeler, Elizabeth K [Livermore, CA; Lee, Abraham P [Irvine, CA

    2009-03-17

    A flow cytometer includes a flow cell for detecting the sample, an oil phase in the flow cell, a water phase in the flow cell, an oil-water interface between the oil phase and the water phase, a detector for detecting the sample at the oil-water interface, and a hydrophobic unit operatively connected to the sample. The hydrophobic unit is attached to the sample. The sample and the hydrophobic unit are placed in an oil and water combination. The sample is detected at the interface between the oil phase and the water phase.

  3. Simple automated preparation of O-[{sup 11}C]methyl-L-tyrosine for routine clinical use

    Energy Technology Data Exchange (ETDEWEB)

    Ishikawa, Yoichi [CYRIC Tohoku University, Aramaki, Aoba-ku, Sendai 980-8578 (Japan); Iwata, Ren [CYRIC Tohoku University, Aramaki, Aoba-ku, Sendai 980-8578 (Japan)]. E-mail: rencyric@cyric.tohoku.ac.jp; Furumoto, Shozo [TUBERO, Tohoku University, Sendai 980-8575 (Japan); Pascali, Claudio [National Cancer Institute, 20133 Milan (Italy); Bogni, Anna [National Cancer Institute, 20133 Milan (Italy); Kubota, Kazuo [International Medical Center, Tokyo 162-8655 (Japan); Ishiwata, Kiichi [Tokyo Metropolitan Institute of Gerontology, Tokyo 173-0022 (Japan)

    2005-07-01

    The previously reported preparation of O-[{sup 11}C]methyl-L-tyrosine ([{sup 11}C]MT), a promising tumor imaging agent, has been now considerably simplified and automated. Main changes were the use of [{sup 11}C]methyl iodide ([{sup 11}C]MeI) in the reaction with L-tyrosine disodium and the use of solid phase extraction on commercially available cartridges instead of HPLC for the final purification. An injectable saline solution of [{sup 11}C]MT was obtained within 30 min after EOB with radiochemical yield of ca. 60% (decay-corrected, based on [{sup 11}C]MeI). Radiochemical purity was over 97%. The automated preparation was carried out using a miniature module employing manifold valves.

  4. Fully Automated Laser Ablation Liquid Capture Sample Analysis using NanoElectrospray Ionization Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Lorenz, Matthias [ORNL; Ovchinnikova, Olga S [ORNL; Van Berkel, Gary J [ORNL

    2014-01-01

    RATIONALE: Laser ablation provides for the possibility of sampling a large variety of surfaces with high spatial resolution. This type of sampling when employed in conjunction with liquid capture followed by nanoelectrospray ionization provides the opportunity for sensitive and prolonged interrogation of samples by mass spectrometry as well as the ability to analyze surfaces not amenable to direct liquid extraction. METHODS: A fully automated, reflection geometry, laser ablation liquid capture spot sampling system was achieved by incorporating appropriate laser fiber optics and a focusing lens into a commercially available, liquid extraction surface analysis (LESA ) ready Advion TriVersa NanoMate system. RESULTS: Under optimized conditions about 10% of laser ablated material could be captured in a droplet positioned vertically over the ablation region using the NanoMate robot controlled pipette. The sampling spot size area with this laser ablation liquid capture surface analysis (LA/LCSA) mode of operation (typically about 120 m x 160 m) was approximately 50 times smaller than that achievable by direct liquid extraction using LESA (ca. 1 mm diameter liquid extraction spot). The set-up was successfully applied for the analysis of ink on glass and paper as well as the endogenous components in Alstroemeria Yellow King flower petals. In a second mode of operation with a comparable sampling spot size, termed laser ablation/LESA , the laser system was used to drill through, penetrate, or otherwise expose material beneath a solvent resistant surface. Once drilled, LESA was effective in sampling soluble material exposed at that location on the surface. CONCLUSIONS: Incorporating the capability for different laser ablation liquid capture spot sampling modes of operation into a LESA ready Advion TriVersa NanoMate enhanced the spot sampling spatial resolution of this device and broadened the surface types amenable to analysis to include absorbent and solvent resistant

  5. Artificial Neural Network for Total Laboratory Automation to Improve the Management of Sample Dilution.

    Science.gov (United States)

    Ialongo, Cristiano; Pieri, Massimo; Bernardini, Sergio

    2017-02-01

    Diluting a sample to obtain a measure within the analytical range is a common task in clinical laboratories. However, for urgent samples, it can cause delays in test reporting, which can put patients' safety at risk. The aim of this work is to show a simple artificial neural network that can be used to make it unnecessary to predilute a sample using the information available through the laboratory information system. Particularly, the Multilayer Perceptron neural network built on a data set of 16,106 cardiac troponin I test records produced a correct inference rate of 100% for samples not requiring predilution and 86.2% for those requiring predilution. With respect to the inference reliability, the most relevant inputs were the presence of a cardiac event or surgery and the result of the previous assay. Therefore, such an artificial neural network can be easily implemented into a total automation framework to sensibly reduce the turnaround time of critical orders delayed by the operation required to retrieve, dilute, and retest the sample.

  6. Design of an automated rapid vapor concentrator and its application in nitroaromatic vapor sampling

    Science.gov (United States)

    Gehrke, Mark; Kapila, Shubhender; Hambacker, Kurt L.; Flanigan, Virgil I.

    2000-08-01

    An automated, rapid-cycling vapor concentrator and sample introduction device was designed and evaluated. The device consists of an inert deactivated fused silica capillary sampling loop. The temperature of the loop was manipulated through contact with a cold plate or a hot plate, maintained at pre-selected temperatures with a thermoelectric cooler and heating cartridge, respectively. The position of the loop was controlled with a stepper motor under microprocessor control. The low mass of the loop permit its rapid cooling and heating. This permits efficient trapping of adsorptive vapors such as the nitroaromatics from the air stream and also allows rapid and quantitative transfer of the trapped analytes to the detection system. The use of at thermoelectric cooler permits variable trapping temperatures and increased sampling selectivity without the use of cumbersome cryogenic fluids. Chemically inert sampling train surfaces prevent analyte loss due to irreversible adsorption and cross contamination between samples. The device was evaluated for rapid analysis of nitroaromatic and chlorinated aromatic vapors from air stream at trace concentrations with a selective electron capture detection system. Trapping efficiencies of > 95 percent can be readily obtained with the device for nitroaromatics at ppb and sub ppb concentrations.

  7. Quantum Hall samples prepared by helium-ion implantation

    International Nuclear Information System (INIS)

    Bruus, H.; Lindelof, P.E.; Veje, E.

    1990-01-01

    We have produced GaAs/GaAlAs heterostructure based quantum Hall samples with a wide range of electron mobilities using ion implantation. The purpose has been to optimize the samples for use in metrology. We have in particular studied the critical current and the non-ohmic behavior of our samples in the vicinity of a quantum Hall plateau. (orig.)

  8. A made in Brazil metallic sample preparation facility

    International Nuclear Information System (INIS)

    Holt, B.J.; Diaz, J.V.; Huber, J.G.; Luengo, C.A.

    A facility, built locally, for the preparation of metallic compounds and alloys of common use in solid state physics in described. This facility includes a multipurpose furnace (FORARCO I) and accessories which are capable of melting, quenching, casting and annealing. (author) [pt

  9. Restricted access materials and large particle supports for on-line sample preparation: an attractive approach for biological fluids analysis.

    Science.gov (United States)

    Souverain, S; Rudaz, S; Veuthey, J-L

    2004-03-05

    An analytical process generally involves four main steps: (1) sample preparation; (2) analytical separation; (3) detection; and (4) data handling. In the bioanalytical field, sample preparation is often considered as the time-limiting step. Indeed, the extraction techniques commonly used for biological matrices such as liquid-liquid extraction (LLE) and solid-phase extraction (SPE) are achieved in the off-line mode. In order to perform a high throughput analysis, efforts have been engaged in developing a faster sample purification process. Among different strategies, the introduction of special extraction sorbents, such as the restricted access media (RAM) and large particle supports (LPS), allowing the direct and repetitive injection of complex biological matrices, represents a very attractive approach. Integrated in a liquid chromatography (LC) system, these extraction supports lead to the automation, simplification and speeding up of the sample preparation process. In this paper, RAM and LPS are reviewed and particular attention is given to commercially available supports. Applications of these extraction supports, are presented in single column and column-switching configurations, for the direct analysis of compounds in various biological fluids.

  10. 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.

  11. Rapid and automated determination of plutonium and neptunium in environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Qiao, J.

    2011-03-15

    This thesis presents improved analytical methods for rapid and automated determination of plutonium and neptunium in environmental samples using sequential injection (SI) based chromatography and inductively coupled plasma mass spectrometry (ICP-MS). The progress of methodology development in this work consists of 5 subjects stated as follows: 1) Development and optimization of an SI-anion exchange chromatographic method for rapid determination of plutonium in environmental samples in combination of inductively coupled plasma mass spectrometry detection (Paper II); (2) Methodology development and optimization for rapid determination of plutonium in environmental samples using SI-extraction chromatography prior to inductively coupled plasma mass spectrometry (Paper III); (3) Development of an SI-chromatographic method for simultaneous determination of plutonium and neptunium in environmental samples (Paper IV); (4) Investigation of the suitability and applicability of 242Pu as a tracer for rapid neptunium determination using anion exchange chromatography in an SI-network coupled with inductively coupled plasma mass spectrometry (Paper V); (5) Exploration of macro-porous anion exchange chromatography for rapid and simultaneous determination of plutonium and neptunium within an SI system (Paper VI). The results demonstrate that the developed methods in this study are reliable and efficient for accurate assays of trace levels of plutonium and neptunium as demanded in different situations including environmental risk monitoring and assessment, emergency preparedness and surveillance of contaminated areas. (Author)

  12. 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.

  13. Rapid sample preparation for detection and identification of avian influenza virus from chicken faecal samples using magnetic bead microsystem

    DEFF Research Database (Denmark)

    Dhumpa, Raghuram; Bu, Minqiang; Handberg, Kurt

    2010-01-01

    -PCR is a sensitive method for detection of AIV, it requires sample preparation including separation and purification of AIV and concentrate viral RNA. It is laborious and complex process especially for diagnosis using faecal sample. In this study, magnetic beads were used for immunoseparation of AIV in chicken...... faecal sample by a magnetic microsystem. Using this system, all the 16 hemagglutinin (H) and 9 neuraminidase (N) subtypes of AIV were separated and detected in spiked faecal samples using RT-PCR, without an RNA extraction step. This rapid sample preparation method can be integrated with a total analysis...

  14. Automated Three-Dimensional Microbial Sensing and Recognition Using Digital Holography and Statistical Sampling

    Directory of Open Access Journals (Sweden)

    Inkyu Moon

    2010-09-01

    Full Text Available We overview an approach to providing automated three-dimensional (3D sensing and recognition of biological micro/nanoorganisms integrating Gabor digital holographic microscopy and statistical sampling methods. For 3D data acquisition of biological specimens, a coherent beam propagates through the specimen and its transversely and longitudinally magnified diffraction pattern observed by the microscope objective is optically recorded with an image sensor array interfaced with a computer. 3D visualization of the biological specimen from the magnified diffraction pattern is accomplished by using the computational Fresnel propagation algorithm. For 3D recognition of the biological specimen, a watershed image segmentation algorithm is applied to automatically remove the unnecessary background parts in the reconstructed holographic image. Statistical estimation and inference algorithms are developed to the automatically segmented holographic image. Overviews of preliminary experimental results illustrate how the holographic image reconstructed from the Gabor digital hologram of biological specimen contains important information for microbial recognition.

  15. Are Flow Injection-based Approaches Suitable for Automated Handling of Solid Samples?

    DEFF Research Database (Denmark)

    Miró, Manuel; Hansen, Elo Harald; Cerdà, Victor

    Flow-based approaches were originally conceived for liquid-phase analysis, implying that constituents in solid samples generally had to be transferred into the liquid state, via appropriate batch pretreatment procedures, prior to analysis. Yet, in recent years, much effort has been focused...... electrolytic or aqueous leaching, on-line dialysis/microdialysis, in-line filtration, and pervaporation-based procedures have been successfully implemented in continuous flow/flow injection systems. In this communication, the new generation of flow analysis, including sequential injection, multicommutated flow...... with the potential hyphenation with modern analytical instrumentation for automated monitoring of the content of targeted species in the on-line generated extracts [3,4]. [1] Z.-L. Zhi, A. Ríos, M. Valcárcel, Crit. Rev. Anal. Chem., 26 (1996) 239. [2] M. Miró, E.H. Hansen, R. Chomchoei, W. Frenzel, TRAC-Trends Anal...

  16. 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

  17. Protocol for Cohesionless Sample Preparation for Physical Experimentation

    Science.gov (United States)

    2016-05-01

    4.2 Correction for non-cylindrical solid specimen ............................................................ 35 5 Testing Apparatus Description...circular solid samples (b) circular hollow samples. ............................. 35 Figure 20. Analysis of ψ... sieve analysis verifies that the two test sands, SDA and SDB, are cohesionless materials and the grain-size distributions of the two sands are similar

  18. 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.

  19. An Automated Algorithm to Screen Massive Training Samples for a Global Impervious Surface Classification

    Science.gov (United States)

    Tan, Bin; Brown de Colstoun, Eric; Wolfe, Robert E.; Tilton, James C.; Huang, Chengquan; Smith, Sarah E.

    2012-01-01

    An algorithm is developed to automatically screen the outliers from massive training samples for Global Land Survey - Imperviousness Mapping Project (GLS-IMP). GLS-IMP is to produce a global 30 m spatial resolution impervious cover data set for years 2000 and 2010 based on the Landsat Global Land Survey (GLS) data set. This unprecedented high resolution impervious cover data set is not only significant to the urbanization studies but also desired by the global carbon, hydrology, and energy balance researches. A supervised classification method, regression tree, is applied in this project. A set of accurate training samples is the key to the supervised classifications. Here we developed the global scale training samples from 1 m or so resolution fine resolution satellite data (Quickbird and Worldview2), and then aggregate the fine resolution impervious cover map to 30 m resolution. In order to improve the classification accuracy, the training samples should be screened before used to train the regression tree. It is impossible to manually screen 30 m resolution training samples collected globally. For example, in Europe only, there are 174 training sites. The size of the sites ranges from 4.5 km by 4.5 km to 8.1 km by 3.6 km. The amount training samples are over six millions. Therefore, we develop this automated statistic based algorithm to screen the training samples in two levels: site and scene level. At the site level, all the training samples are divided to 10 groups according to the percentage of the impervious surface within a sample pixel. The samples following in each 10% forms one group. For each group, both univariate and multivariate outliers are detected and removed. Then the screen process escalates to the scene level. A similar screen process but with a looser threshold is applied on the scene level considering the possible variance due to the site difference. We do not perform the screen process across the scenes because the scenes might vary due to

  20. 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.

  1. 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.

  2. 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.

  3. Preview of the NASA NNWG NDE Sample Preparation Handbook

    Science.gov (United States)

    2010-01-01

    This viewgraph presents a step-by-step how-to fabrication documentation of every kind of sample that is fabricated for MSFC by UA Huntsville, including photos and illustrations. The tabulation of what kind of samples are being fabricated for what NDE method, detailed instructions/documentation of the inclusion/creation of defects, detailed specifications for materials, processes, and equipment, case histories and/or experiences with the different fabrication methods and defect inclusion techniques, discussion of pitfalls and difficulties associated with sample fabrication and defect inclusion techniques, and a discussion of why certain fabrication techniques are needed as related to the specific NDE methods are included in this presentation.

  4. 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.

  5. 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)

  6. Preparing for Automated Derivation of Products in a Software Product Line

    National Research Council Canada - National Science Library

    McGregor, John D

    2005-01-01

    ... to bring a product to market, or through other production improvements. Business goals such as these make automated product derivation an appealing strategy to a software product line organization...

  7. 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

  8. Automated on-line liquid-liquid extraction system for temporal mass spectrometric analysis of dynamic samples.

    Science.gov (United States)

    Hsieh, Kai-Ta; Liu, Pei-Han; Urban, Pawel L

    2015-09-24

    Most real samples cannot directly be infused to mass spectrometers because they could contaminate delicate parts of ion source and guides, or cause ion suppression. Conventional sample preparation procedures limit temporal resolution of analysis. We have developed an automated liquid-liquid extraction system that enables unsupervised repetitive treatment of dynamic samples and instantaneous analysis by mass spectrometry (MS). It incorporates inexpensive open-source microcontroller boards (Arduino and Netduino) to guide the extraction and analysis process. Duration of every extraction cycle is 17 min. The system enables monitoring of dynamic processes over many hours. The extracts are automatically transferred to the ion source incorporating a Venturi pump. Operation of the device has been characterized (repeatability, RSD = 15%, n = 20; concentration range for ibuprofen, 0.053-2.000 mM; LOD for ibuprofen, ∼0.005 mM; including extraction and detection). To exemplify its usefulness in real-world applications, we implemented this device in chemical profiling of pharmaceutical formulation dissolution process. Temporal dissolution profiles of commercial ibuprofen and acetaminophen tablets were recorded during 10 h. The extraction-MS datasets were fitted with exponential functions to characterize the rates of release of the main and auxiliary ingredients (e.g. ibuprofen, k = 0.43 ± 0.01 h(-1)). The electronic control unit of this system interacts with the operator via touch screen, internet, voice, and short text messages sent to the mobile phone, which is helpful when launching long-term (e.g. overnight) measurements. Due to these interactive features, the platform brings the concept of the Internet-of-Things (IoT) to the chemistry laboratory environment. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. Sample preparation of Medicago sativa L. hay for chemical analysis ...

    African Journals Online (AJOL)

    The objective of this study was to quantify the effect of the grinding procedure on the moisture and crude protein concentration of a ground Medicago sativa L. hay sample for quality grading. An additional aim was to investigate the accuracy of electronic moisture testers (EMT). Variance of analyses revealed significant ...

  10. Microfluidic desalination : capacitive deionization on chip for microfluidic sample preparation

    NARCIS (Netherlands)

    Roelofs, Susan Helena

    2015-01-01

    The main aim of the work described in this thesis is to implement the desalination technique capacitive deionization (CDI) on a microfluidic chip to improve the reproducibility in the analysis of biological samples for drug development. Secondly, microfluidic CDI allows for the in situ study of ion

  11. Sample preparation of Medicago sativa L. hay for chemical analysis

    African Journals Online (AJOL)

    UFS Campus

    Abstract. The objective of this study was to quantify the effect of the grinding procedure on the moisture and crude protein concentration of a ground Medicago sativa L. hay sample for quality grading. An additional aim was to investigate the accuracy of electronic moisture testers (EMT). Variance of analyses revealed.

  12. Microsystem strategies for sample preparation in biological detection.

    Energy Technology Data Exchange (ETDEWEB)

    James, Conrad D.; Galambos, Paul C.; Bennett, Dawn Jonita (University of Maryland Baltimore County, Baltimore, MD); Manginell, Monica; Okandan, Murat; Acrivos, Andreas (The City College of New York, NY); Brozik, Susan Marie; Khusid, Boris (New Jersey Institute of Technology, Newark, NJ)

    2005-03-01

    The objective of this LDRD was to develop microdevice strategies for dealing with samples to be examined in biological detection systems. This includes three sub-components: namely, microdevice fabrication, sample delivery to the microdevice, and sample processing within the microdevice. The first component of this work focused on utilizing Sandia's surface micromachining technology to fabricate small volume (nanoliter) fluidic systems for processing small quantities of biological samples. The next component was to develop interfaces for the surface-micromachined silicon devices. We partnered with Micronics, a commercial company, to produce fluidic manifolds for sample delivery to our silicon devices. Pressure testing was completed to examine the strength of the bond between the pressure-sensitive adhesive layer and the silicon chip. We are also pursuing several other methods, both in house and external, to develop polymer-based fluidic manifolds for packaging silicon-based microfluidic devices. The second component, sample processing, is divided into two sub-tasks: cell collection and cell lysis. Cell collection was achieved using dielectrophoresis, which employs AC fields to collect cells at energized microelectrodes, while rejecting non-cellular particles. Both live and dead Staph. aureus bacteria have been collected using RF frequency dielectrophoresis. Bacteria have been separated from polystyrene microspheres using frequency-shifting dielectrophoresis. Computational modeling was performed to optimize device separation performance, and to predict particle response to the dielectrophoretic traps. Cell lysis is continuing to be pursued using microactuators to mechanically disrupt cell membranes. Novel thermal actuators, which can generate larger forces than previously tested electrostatic actuators, have been incorporated with and tested with cell lysis devices. Significant cell membrane distortion has been observed, but more experiments need to be

  13. Invention and validation of an automated camera system that uses optical character recognition to identify patient name mislabeled samples.

    Science.gov (United States)

    Hawker, Charles D; McCarthy, William; Cleveland, David; Messinger, Bonnie L

    2014-03-01

    Mislabeled samples are a serious problem in most clinical laboratories. Published error rates range from 0.39/1000 to as high as 1.12%. Standardization of bar codes and label formats has not yet achieved the needed improvement. The mislabel rate in our laboratory, although low compared with published rates, prompted us to seek a solution to achieve zero errors. To reduce or eliminate our mislabeled samples, we invented an automated device using 4 cameras to photograph the outside of a sample tube. The system uses optical character recognition (OCR) to look for discrepancies between the patient name in our laboratory information system (LIS) vs the patient name on the customer label. All discrepancies detected by the system's software then require human inspection. The system was installed on our automated track and validated with production samples. We obtained 1 009 830 images during the validation period, and every image was reviewed. OCR passed approximately 75% of the samples, and no mislabeled samples were passed. The 25% failed by the system included 121 samples actually mislabeled by patient name and 148 samples with spelling discrepancies between the patient name on the customer label and the patient name in our LIS. Only 71 of the 121 mislabeled samples detected by OCR were found through our normal quality assurance process. We have invented an automated camera system that uses OCR technology to identify potential mislabeled samples. We have validated this system using samples transported on our automated track. Full implementation of this technology offers the possibility of zero mislabeled samples in the preanalytic stage.

  14. Microassay for interferon, using [3H]uridine, microculture plates, and a multiple automated sample harvester.

    Science.gov (United States)

    Richmond, J Y; Polatnick, J; Knudsen, R C

    1980-01-01

    A microassay for interferon is described which uses target cells grown in microculture wells, [3H]uridine to measure vesicular stomatitis virus replication in target cells, and a multiple automated sample harvester to collect the radioactively labeled viral ribonucleic acid onto glass fiber filter disks. The disks were placed in minivials, and radioactivity was counted in a liquid scintillation spectrophotometer. Interferon activity was calculated as the reciprocal of the highest titer which inhibited the incorporation of [3H]uridine into viral ribonucleic acid by 50%. Interferon titers determined by the microassay were similar to the plaque reduction assay when 100 plaque-forming units of challenge vesicular stomatitis virus was used. However, it was found that the interferon titers decreased approximately 2-fold for each 10-fold increase in the concentration of challenge vesicular stomatitis virus when tested in the range of 10(2) to 10(5) plaque-forming units. Interferon titers determined by the microassay show a high degree of repeatability, and the assay can be used to measure small and large numbers of interferon samples. PMID:6155105

  15. 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.

  16. 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...

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

    NARCIS (Netherlands)

    Switzar, L.; van Angeren, J.A; Pinkse, M; Kool, J.; Niessen, W.M.A.

    2013-01-01

    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

  18. An improved method of sample preparation on AnchorChip targets for MALDI-MS and MS/MS and its application in the liver proteome project

    DEFF Research Database (Denmark)

    Zhang, Xumin; Shi, Liang; Shu, Shaokung

    2007-01-01

    An improved method for sample preparation for MALDI-MS and MS/MS using AnchorChip targets is presented. The method, termed the SMW method (sample, matrix wash), results in better sensitivity for peptide mass fingerprinting as well as for sequencing by MS/MS than previously published methods....... The method allows up-concentration and desalting directly on the mass spectrometric target and should be amenable for automation. A draw back caused by extensive oxidation of methionine and tryptophan in the SMW method can be alleviated by the addition of n-octyl glucopyranoside and DTT to the sample...

  19. 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.

  20. PTR-ToF-MS Coupled with an Automated Sampling System and Tailored Data Analysis for Food Studies: Bioprocess Monitoring, Screening and Nose-space Analysis.

    Science.gov (United States)

    Capozzi, Vittorio; Yener, Sine; Khomenko, Iuliia; Farneti, Brian; Cappellin, Luca; Gasperi, Flavia; Scampicchio, Matteo; Biasioli, Franco

    2017-05-11

    Proton Transfer Reaction (PTR), combined with a Time-of-Flight (ToF) Mass Spectrometer (MS) is an analytical approach based on chemical ionization that belongs to the Direct-Injection Mass Spectrometric (DIMS) technologies. These techniques allow the rapid determination of volatile organic compounds (VOCs), assuring high sensitivity and accuracy. In general, PTR-MS requires neither sample preparation nor sample destruction, allowing real time and non-invasive analysis of samples. PTR-MS are exploited in many fields, from environmental and atmospheric chemistry to medical and biological sciences. More recently, we developed a methodology based on coupling PTR-ToF-MS with an automated sampler and tailored data analysis tools, to increase the degree of automation and, consequently, to enhance the potential of the technique. This approach allowed us to monitor bioprocesses (e.g. enzymatic oxidation, alcoholic fermentation), to screen large sample sets (e.g. different origins, entire germoplasms) and to analyze several experimental modes (e.g. different concentrations of a given ingredient, different intensities of a specific technological parameter) in terms of VOC content. Here, we report the experimental protocols exemplifying different possible applications of our methodology: i.e. the detection of VOCs released during lactic acid fermentation of yogurt (on-line bioprocess monitoring), the monitoring of VOCs associated with different apple cultivars (large-scale screening), and the in vivo study of retronasal VOC release during coffee drinking (nosespace analysis).

  1. Accelerated solvent extraction (ASE) - a fast and automated technique with low solvent consumption for the extraction of solid samples (T12)

    International Nuclear Information System (INIS)

    Hoefler, F.

    2002-01-01

    Full text: Accelerated solvent extraction (ASE) is a modern extraction technique that significantly streamlines sample preparation. A common organic solvent as well as water is used as extraction solvent at elevated temperature and pressure to increase extraction speed and efficiency. The entire extraction process is fully automated and performed within 15 minutes with a solvent consumption of 18 ml for a 10 g sample. For many matrices and for a variety of solutes, ASE has proven to be equivalent or superior to sonication, Soxhlet, and reflux extraction techniques while requiring less time, solvent and labor. First ASE has been applied for the extraction of environmental hazards from solid matrices. Within a very short time ASE was approved by the U.S. EPA for the extraction of BNAs, PAHs, PCBs, pesticides, herbicides, TPH, and dioxins from solid samples in method 3545. Especially for the extraction of dioxins the extraction time with ASE is reduced to 20 minutes in comparison to 18 h using Soxhlet. In food analysis ASE is used for the extraction of pesticide and mycotoxin residues from fruits and vegetables, the fat determination and extraction of vitamins. Time consuming and solvent intensive methods for the extraction of additives from polymers as well as for the extraction of marker compounds from herbal supplements can be performed with higher efficiencies using ASE. For the analysis of chemical weapons the extraction process and sample clean-up including derivatization can be automated and combined with GC-MS using an online ASE-APEC-GC system. (author)

  2. Sample preparation of metal alloys by electric discharge machining

    Science.gov (United States)

    Chapman, G. B., II; Gordon, W. A.

    1976-01-01

    Electric discharge machining was investigated as a noncontaminating method of comminuting alloys for subsequent chemical analysis. Particulate dispersions in water were produced from bulk alloys at a rate of about 5 mg/min by using a commercially available machining instrument. The utility of this approach was demonstrated by results obtained when acidified dispersions were substituted for true acid solutions in an established spectrochemical method. The analysis results were not significantly different for the two sample forms. Particle size measurements and preliminary results from other spectrochemical methods which require direct aspiration of liquid into flame or plasma sources are reported.

  3. A destructive sample preparation method for radioactive waste characterization

    International Nuclear Information System (INIS)

    Olteanu, M.; Bucur, C.

    2015-01-01

    Acid digestion, using the microwave power, was applied for ''dissolution'' of different materials corresponding to the radioactive waste matrices resulted from a nuclear power plant operation, including exchange resin (cationic and mixed), concrete, paper, textile and activated charcoals. A small aliquot of solid sample (0.1-0.5g) was mixed with a known volume of digestion reagents (HNO3 67% - H2O2 30% or HNO3 67% - HCl 37%, with HF addition if the SiO2 was present in matrices) in a 100 ml PTFE vessel and it was mineralized using a Berghof digestion system, Speedwave 4. Starting from the manufacturer procedures, the technical parameters (temperature and mineralization time), the types and quantities of digestion reagents were optimized. After the mineralization process, the samples were transferred in centrifuge tubes, separated at 3500 rot/min and visually analysed. The obtained solutions were clear, without suspended or deposed materials and separated phases, ready for future separation processes of the ''difficult to measure'' radioisotopes. (authors)

  4. Automated analysis of carbon in powdered geological and environmental samples by Raman spectroscopy.

    Science.gov (United States)

    Sparkes, Robert; Hovius, Niels; Galy, Albert; Kumar, R Vasant; Liu, James T

    2013-07-01

    Raman spectroscopy can be used to assess the structure of naturally occurring carbonaceous materials (CM), which exist in a wide range of crystal structures. The sources of these geological and environmental materials include rocks, soils, river sediments, and marine sediment cores, all of which can contain carbonaceous material ranging from highly crystalline graphite to amorphous-like organic compounds. In order to fully characterize a geological sample and its intrinsic heterogeneity, several spectra must be collected and analyzed in a precise and repeatable manner. Here, we describe a suitable processing and analysis technique. We show that short-period ball-mill grinding does not introduce structural changes to semi-graphitized material and allows for easy collection of Raman spectra from the resulting powder. Two automated peak-fitting procedures are defined that allow for rapid processing of large datasets. For very disordered CM, Lorentzian profiles are fitted to five characteristic peaks, for highly graphitized material, three Voigt profiles are fitted. Peak area ratios and peak width measurements are used to classify each spectrum and allow easy comparison between samples. By applying this technique to samples collected in Taiwan after Typhoon Morakot, sources of carbon to offshore sediments have been identified. Carbon eroded from different areas of Taiwan can be seen mixed and deposited in the offshore flood sediments, and both graphite and amorphous-like carbon have been recycled from terrestrial to marine deposits. The practicality of this application illustrates the potential for this technique to be deployed to sediment-sourcing problems in a wide range of geological settings.

  5. Interfacing click chemistry with automated oligonucleotide synthesis for the preparation of fluorescent DNA probes containing internal xanthene and cyanine dyes

    DEFF Research Database (Denmark)

    Astakhova, I Kira; Wengel, Jesper

    2013-01-01

    for the first time performed solid-phase copper(I)-catalyzed azide-alkyne cycloaddition (CuAAC) click labeling during the automated phosphoramidite oligonucleotide synthesis followed by postsynthetic click reactions in solution. We demonstrate that our novel strategy is rapid and efficient for the preparation...... Stokes shifts (40-110 nm), quenched fluorescence of single-stranded probes accompanied by up to 7.7-fold light-up effect of emission upon target DNA/RNA binding, remarkable sensitivity to single-nucleotide mismatches, generally high fluorescence brightness values (FB up to 26), and hence low limit...

  6. 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)

  7. Automated Diagnosis of Myocardial Infarction ECG Signals Using Sample Entropy in Flexible Analytic Wavelet Transform Framework

    Directory of Open Access Journals (Sweden)

    Mohit Kumar

    2017-09-01

    Full Text Available Myocardial infarction (MI is a silent condition that irreversibly damages the heart muscles. It expands rapidly and, if not treated timely, continues to damage the heart muscles. An electrocardiogram (ECG is generally used by the clinicians to diagnose the MI patients. Manual identification of the changes introduced by MI is a time-consuming and tedious task, and there is also a possibility of misinterpretation of the changes in the ECG. Therefore, a method for automatic diagnosis of MI using ECG beat with flexible analytic wavelet transform (FAWT method is proposed in this work. First, the segmentation of ECG signals into beats is performed. Then, FAWT is applied to each ECG beat, which decomposes them into subband signals. Sample entropy (SEnt is computed from these subband signals and fed to the random forest (RF, J48 decision tree, back propagation neural network (BPNN, and least-squares support vector machine (LS-SVM classifiers to choose the highest performing one. We have achieved highest classification accuracy of 99.31% using LS-SVM classifier. We have also incorporated Wilcoxon and Bhattacharya ranking methods and observed no improvement in the performance. The proposed automated method can be installed in the intensive care units (ICUs of hospitals to aid the clinicians in confirming their diagnosis.

  8. Sample preparation for mass spectrometry imaging of plant tissues: a review

    Directory of Open Access Journals (Sweden)

    Yonghui eDong

    2016-02-01

    Full Text Available 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 steps. 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 specific 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 various MSI techniques in plants are reviewed according to different classes of plant metabolites.

  9. 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.

  10. A novel flow injection chemiluminescence method for automated and miniaturized determination of phenols in smoked food samples.

    Science.gov (United States)

    Vakh, Christina; Evdokimova, Ekaterina; Pochivalov, Aleksei; Moskvin, Leonid; Bulatov, Andrey

    2017-12-15

    An easily performed fully automated and miniaturized flow injection chemiluminescence (CL) method for determination of phenols in smoked food samples has been proposed. This method includes the ultrasound assisted solid-liquid extraction coupled with gas-diffusion separation of phenols from smoked food sample and analytes absorption into a NaOH solution in a specially designed gas-diffusion cell. The flow system was designed to focus on automation and miniaturization with minimal sample and reagent consumption by inexpensive instrumentation. The luminol - N-bromosuccinimide system in an alkaline medium was used for the CL determination of phenols. The limit of detection of the proposed procedure was 3·10 -8 ·molL -1 (0.01mgkg -1 ) in terms of phenol. The presented method demonstrated to be a good tool for easy, rapid and cost-effective point-of-need screening phenols in smoked food samples. Copyright © 2017 Elsevier Ltd. All rights reserved.

  11. Preparing Future Managers for Effective Use of Technology in Automated Offices.

    Science.gov (United States)

    Graves, Charlotte

    1983-01-01

    Reports findings of a recent doctoral research study conducted to determine what changes are needed in collegiate business curricula as a result of office automation. Results were based on responses from office systems consultants, and faculty of office administration, management, marketing, accounting, and finance. Conclusions and recommendations…

  12. 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.

  13. 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

  14. Correction of an input function for errors introduced with automated blood sampling

    Energy Technology Data Exchange (ETDEWEB)

    Schlyer, D.J.; Dewey, S.L. [Brookhaven National Lab., Upton, NY (United States)

    1994-05-01

    Accurate kinetic modeling of PET data requires an precise arterial plasma input function. The use of automated blood sampling machines has greatly improved the accuracy but errors can be introduced by the dispersion of the radiotracer in the sampling tubing. This dispersion results from three effects. The first is the spreading of the radiotracer in the tube due to mass transfer. The second is due to the mechanical action of the peristaltic pump and can be determined experimentally from the width of a step function. The third is the adsorption of the radiotracer on the walls of the tubing during transport through the tube. This is a more insidious effect since the amount recovered from the end of the tube can be significantly different than that introduced into the tubing. We have measured the simple mass transport using [{sup 18}F]fluoride in water which we have shown to be quantitatively recovered with no interaction with the tubing walls. We have also carried out experiments with several radiotracers including [{sup 18}F]Haloperidol, [{sup 11}C]L-deprenyl, [{sup 18}]N-methylspiroperidol ([{sup 18}F]NMS) and [{sup 11}C]buprenorphine. In all cases there was some retention of the radiotracer by untreated silicone tubing. The amount retained in the tubing ranged from 6% for L-deprenyl to 30% for NMS. The retention of the radiotracer was essentially eliminated after pretreatment with the relevant unlabeled compound. For example less am 2% of the [{sup 18}F]NMS was retained in tubing treated with unlabelled NMS. Similar results were obtained with baboon plasma although the amount retained in the untreated tubing was less in all cases. From these results it is possible to apply a mathematical correction to the measured input function to account for mechanical dispersion and to apply a chemical passivation to the tubing to reduce the dispersion due to adsorption of the radiotracer on the tubing walls.

  15. 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.

  16. PET imaging of liposomes labeled with an [18F]-fluorocholesteryl ether probe prepared by automated radiosynthesis

    DEFF Research Database (Denmark)

    Jensen, Andreas Tue Ingemann; Binderup, Tina; Andresen, Thomas Lars

    2012-01-01

    A novel [F-18]-labeled cholesteryl ether lipid probe was prepared by synthesis of the corresponding mesylate, which was [F-18]-fluorinated by a [F-18]KF, Kryptofix-222, K2CO3 procedure. Fluorination was done for 10 minutes at 165 degrees C and took place with conversion between 3 and 17%, depending......, was observed, corresponding to expected liposomal pharmacokinetics. The tumor accumulation 8 hours postinjection accounted for 2.25 +/- 0.23 (mean +/- standard error of the mean) percent of injected dose per gram (%ID/g), and the tumor-to-muscle ratio reached 2.20 +/- 0.24 after 8 hours, which...... on conditions. Radiolabelling of the probe and subsequent in situ purification on SEP-Paks were done on a custom-built, fully automatic synthesis robot. Long-circulating liposomes were prepared by hydration (magnetic stirring) of a lipid film containing the radiolabeled probe, followed by fully automated...

  17. Flavourzyme, an Enzyme Preparation with Industrial Relevance: Automated Nine-Step Purification and Partial Characterization of Eight Enzymes.

    Science.gov (United States)

    Merz, Michael; Eisele, Thomas; Berends, Pieter; Appel, Daniel; Rabe, Swen; Blank, Imre; Stressler, Timo; Fischer, Lutz

    2015-06-17

    Flavourzyme is sold as a peptidase preparation from Aspergillus oryzae. The enzyme preparation is widely and diversely used for protein hydrolysis in industrial and research applications. However, detailed information about the composition of this mixture is still missing due to the complexity. The present study identified eight key enzymes by mass spectrometry and partially by activity staining on native polyacrylamide gels or gel zymography. The eight enzymes identified were two aminopeptidases, two dipeptidyl peptidases, three endopeptidases, and one α-amylase from the A. oryzae strain ATCC 42149/RIB 40 (yellow koji mold). Various specific marker substrates for these Flavourzyme enzymes were ascertained. An automated, time-saving nine-step protocol for the purification of all eight enzymes within 7 h was designed. Finally, the purified Flavourzyme enzymes were biochemically characterized with regard to pH and temperature profiles and molecular sizes.

  18. 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.

  19. 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.

  20. 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

  1. Advanced fluidic handling and use of two-phase flow for high throughput structural investigation of proteins on a microfluidic sample preparation platform

    DEFF Research Database (Denmark)

    Lafleur, Josiane P.; Snakenborg, Detlef; Møller, M.

    2010-01-01

    Research on the structure of proteins can bring forth a wealth of information about biological function and can be used to better understand the processes in living cells. This paper reports a new microfluidic sample preparation system for the structural investigation of proteins by Small Angle X......-ray Scattering (SAXS). The system includes hardware and software features for precise fluidic control, synchrotron beamline control, UV absorbance measurements and automated data analysis. The precise fluidic handling capabilities are used to transport and precisely position samples as small as 500 n...

  2. 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

  3. Preparation and investigation of bulk and thin film samples of strontium ferrite

    Directory of Open Access Journals (Sweden)

    A Poorbafrani

    2008-07-01

    Full Text Available   In this article, bulk and thin film samples of strontium ferrite have been studied. Due to the high electrical resistivity in strontium ferrite, energy loss due to eddy currents reduces and because of this, it can be used in high frequency magnetic circuits. On the other hand, strontium ferrite has attracted much attention as a permanent magnet. At first, we study the preparation process of bulk samples of strontium ferrite by a solid state reaction technique. In preparation of samples, to optimize the magnetic properties, we have used the stoichiometry factor (n = Fe2O3 / SrO of 5.25. In addition, we have used additives such as CaO and SiO2 to control grain growth. The samples have been prepared in two series: Isotropic and Anisotropic. For preparation of anisotropic samples, the magnetic field of 1T has been used for orientation of the grains during the press. Then, X-ray diffraction, Scanning Electron Microscopy (SEM, EDAX analysis and Magnetometer, was used for analyzing and comparing of structural and magnetic properties of isotropic and anisotropic samples. The results indicate that, due to the applied magnetic field, the structural and Magnetic properties of anisotropic samples improved efficiently because of the orientation of the grains during the press. In the next stage, we used bulk samples to prepare strontium ferrite thin films by Pulsed Laser Deposition technique (PLD. The Si (111 substrate has been used to prepare the thin films. Then we have studied the microstructure of thin films by X-ray diffraction, SEM and EDAX analysis. These studies on different samples show that for the preparation of crystalline phase of strontium ferrite thin films, the substrate temperature must be higher than 800˚C. The optimum conditions for preparation of strontium, ferrite thin films have been achieved on the substrate temperature of 840˚C and oxygen pressure of 75 mtorr.

  4. 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.

  5. 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...

  6. 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)

  7. 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.

  8. ASPIRE: An automated sample positioning and irradiation system for radiation biology experiments at Inter University Accelerator Centre, New Delhi

    International Nuclear Information System (INIS)

    Kothari, Ashok; Barua, P.; Archunan, M.; Rani, Kusum; Subramanian, E.T.; Pujari, Geetanjali; Kaur, Harminder; Satyanarayanan, V.V.V.; Sarma, Asitikantha; Avasthi, D.K.

    2015-01-01

    An automated irradiation setup for biology samples has been built at Inter University Accelerator Centre (IUAC), New Delhi, India. It can automatically load and unload 20 biology samples in a run of experiment. It takes about 20 min [2% of the cell doubling time] to irradiate all the 20 samples. Cell doubling time is the time taken by the cells (kept in the medium) to grow double in numbers. The cells in the samples keep growing during entire of the experiment. The fluence irradiated to the samples is measured with two silicon surface barrier detectors. Tests show that the uniformity of fluence and dose of heavy ions reaches to 2% at the sample area in diameter of 40 mm. The accuracy of mean fluence at the center of the target area is within 1%. The irradiation setup can be used to the studies of radiation therapy, radiation dosimetry and molecular biology at the heavy ion accelerator. - Highlights: • Automated positioning and irradiation setup for biology samples at IUAC is built. • Loading and unloading of 20 biology samples can be automatically carried out. • Biologicals cells keep growing during entire experiment. • Fluence and dose of heavy ions are measured by two silicon barrier detectors. • Uniformity of fluence and dose of heavy ions at sample position reaches to 2%

  9. 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 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.

  10. 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.

  11. History of target and special sample preparation at the Central Bureau for Nuclear Measurements

    International Nuclear Information System (INIS)

    Audenhove, J.V.; Pauwels, J.

    1981-01-01

    The Central Bureau for Nuclear Measurements is a laboratory whose special aim was the fabrication, analysis and distribution of foils, targets and other samples for nuclear measurements. Preparation and assaying techniques that have been used since 1963 are briefly reviewed

  12. 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...

  13. Proteoglycan and proteome profiling of central human pulmonary fibrotic tissue utilizing miniaturized sample preparation

    DEFF Research Database (Denmark)

    Malmström, Johan; Larsen, Kristoffer; Hansson, Lennart

    2002-01-01

    -dimensional electrophoresis was interfaced to miniaturized sample preparation techniques using microcapillary extraction. Four protein groups were identified; cytoskeletal, adhesion, scavenger and metabolic proteins. These patient's proteomes showed a high degree of heterogeneity between patients but larger homogeneity...

  14. In-Situ Sample Preparation Development for Extraterrestrial Life Detection and Characterization

    Science.gov (United States)

    Craft, K. L.; Bradburne, C.; Tiffany, J.; Hagedon, M.; Hibbitts, C.; Vandegriff, J.; Horst, S.

    2017-02-01

    In-situ life detection instrumentation require robust sample preparation techniques that need further development in the coming years to enable the exciting life discoveries we seek in both familiar and unfamiliar planetary environments.

  15. Automated non-stepwise preparation of bioanalytical calibration standards and quality controls using an ultra-low volume digitizing liquid dispenser.

    Science.gov (United States)

    Liao, Debra; Chen, Susan; Paton, Martin; Qian, Mark G

    2014-06-15

    Stepwise preparation of calibration standards and quality controls (QCs) is one of the most routine and laborious steps in bioanalysis. An alternative non-contact dispenser using low picoliter digitized dispensing technology is evaluated for its application in non-stepwise preparation of calibration curve and QCs in bioanalysis. Fluorescein was initially used to assess the accuracy and precision of dispense volumes with fluorescent measurement. Various concentrations of MX-1, an in-house proprietary small molecule compound, in neat solution and in dog plasma were prepared manually with calibrated pipettors and digitally by the digital dispenser. The plasma samples were extracted by protein precipitation. The resultant extracted samples and neat solutions of MX-1 were analyzed by liquid chromatography/tandem mass spectrometry (LC/MS/MS) using an electrospray ionization (ESI) source in positive ion mode with selected reaction monitoring (SRM) of the mass transitions. In the three-day precision and accuracy assessment of dispensing volumes between 13 pL to 411.2 nL, the intra-day precision and accuracy ranged from 1.4% to 10.3% and -12.7% to 12.8%, respectively. The inter-day precision and accuracy ranged from 3.5% to 7.8% and -6.6% to 10.4%, respectively. For real analysis of in vivo study samples, all 49 samples analyzed showed a less than 5% difference between calibrations with digital and manual curve preparations. The resultant pharmacokinetic (PK) parameters were physiologically comparable as well. Using the digitized picoliter dispensing technology, high-speed automated precise and accurate dispense of a wide range of volumes can be achieved and tests for bioanalytical standards and QC preparations passed the stringent criteria set forth for regulated bioanalysis using LC/MS/MS-based technology. The digital dispenser has been found to be a useful tool in drug discovery for automatically preparing standards and QCs in seconds with low consumption of stock

  16. Sample preparation device and its development of the sulfur isotope reactor for the sulfide and sulfate

    International Nuclear Information System (INIS)

    Li Zhentao; Liu Hanbin; Jin Guishan; Li Junjie; Zhong Fangwen

    2011-01-01

    A new type of sample preparation device and its reactor for sulfur isotope in sulfide and sulfate experiment is developed. The trial experiment proved that the sample preparation device and its reactor are characterized with good vacuum, easy to use, clean, high efficient and low cost to produce sulfur dioxide of high purity, and the analytical results are accurate and reliable. The device and reactor can fully meet for the analysis on the sulfur isotope in various sulfide and sulfate. (authors)

  17. 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.

  18. Analytical Chemistry Laboratory (ACL) procedure compendium. Volume 2, Sample preparation methods

    Energy Technology Data Exchange (ETDEWEB)

    1993-08-01

    This volume contains the interim change notice for sample preparation methods. Covered are: acid digestion for metals analysis, fusion of Hanford tank waste solids, water leach of sludges/soils/other solids, extraction procedure toxicity (simulate leach in landfill), sample preparation for gamma spectroscopy, acid digestion for radiochemical analysis, leach preparation of solids for free cyanide analysis, aqueous leach of solids for anion analysis, microwave digestion of glasses and slurries for ICP/MS, toxicity characteristic leaching extraction for inorganics, leach/dissolution of activated metal for radiochemical analysis, extraction of single-shell tank (SST) samples for semi-VOC analysis, preparation and cleanup of hydrocarbon- containing samples for VOC and semi-VOC analysis, receiving of waste tank samples in onsite transfer cask, receipt and inspection of SST samples, receipt and extrusion of core samples at 325A shielded facility, cleaning and shipping of waste tank samplers, homogenization of solutions/slurries/sludges, and test sample preparation for bioassay quality control program.

  19. Sample Preparation (SS) - Metabolonote | LSDB Archive [Life Science Database Archive metadata

    Lifescience Database Archive (English)

    Full Text Available switchLanguage; BLAST Search Image Search Home About Archive Update History Data List Contact us Metabol...ed to by S (Sample information). Data file File name: metabolonote_sample_prepara...tion_details.zip File URL: ftp://ftp.biosciencedbc.jp/archive/metabolonote/LATEST/metabolonote_sample_prepar...ation_details.zip File size: 13 KB Simple search URL http://togodb.biosciencedbc.jp/togodb/view/metabolonote...ption Download License Update History of This Database Site Policy | Contact Us Sample Preparation (SS) - Metabolonote | LSDB Archive ...

  20. Proteomic challenges: sample preparation techniques for microgram-quantity protein analysis from biological samples.

    Science.gov (United States)

    Feist, Peter; Hummon, Amanda B

    2015-02-05

    Proteins regulate many cellular functions and analyzing the presence and abundance of proteins in biological samples are central focuses in proteomics. The discovery and validation of biomarkers, pathways, and drug targets for various diseases can be accomplished using mass spectrometry-based proteomics. However, with mass-limited samples like tumor biopsies, it can be challenging to obtain sufficient amounts of proteins to generate high-quality mass spectrometric data. Techniques developed for macroscale quantities recover sufficient amounts of protein from milligram quantities of starting material, but sample losses become crippling with these techniques when only microgram amounts of material are available. To combat this challenge, proteomicists have developed micro-scale techniques that are compatible with decreased sample size (100 μg or lower) and still enable excellent proteome coverage. Extraction, contaminant removal, protein quantitation, and sample handling techniques for the microgram protein range are reviewed here, with an emphasis on liquid chromatography and bottom-up mass spectrometry-compatible techniques. Also, a range of biological specimens, including mammalian tissues and model cell culture systems, are discussed.

  1. Proteomic Challenges: Sample Preparation Techniques for Microgram-Quantity Protein Analysis from Biological Samples

    Science.gov (United States)

    Feist, Peter; Hummon, Amanda B.

    2015-01-01

    Proteins regulate many cellular functions and analyzing the presence and abundance of proteins in biological samples are central focuses in proteomics. The discovery and validation of biomarkers, pathways, and drug targets for various diseases can be accomplished using mass spectrometry-based proteomics. However, with mass-limited samples like tumor biopsies, it can be challenging to obtain sufficient amounts of proteins to generate high-quality mass spectrometric data. Techniques developed for macroscale quantities recover sufficient amounts of protein from milligram quantities of starting material, but sample losses become crippling with these techniques when only microgram amounts of material are available. To combat this challenge, proteomicists have developed micro-scale techniques that are compatible with decreased sample size (100 μg or lower) and still enable excellent proteome coverage. Extraction, contaminant removal, protein quantitation, and sample handling techniques for the microgram protein range are reviewed here, with an emphasis on liquid chromatography and bottom-up mass spectrometry-compatible techniques. Also, a range of biological specimens, including mammalian tissues and model cell culture systems, are discussed. PMID:25664860

  2. Biological Agent Sample Preparation for the Detection and Identification of Multiple Agents by Nucleic Acid-Based Analysis

    National Research Council Canada - National Science Library

    Fields, Robert

    2002-01-01

    .... The AutoLyser instrument which we have developed, provides fully automated purification of viral, bacterial and human genomic DNA and RNA from clinical samples, cell culture and swabs in as little...

  3. 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

  4. 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.

  5. 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

  6. 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.

  7. 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.

  8. Sample preparation for thermo-gravimetric determination and thermo-gravimetric characterization of refuse derived fuel.

    Science.gov (United States)

    Robinson, T; Bronson, B; Gogolek, P; Mehrani, P

    2016-02-01

    Thermo-gravimetric analysis (TGA) is a useful method for characterizing fuels. In the past it has been applied to the study of refuse derived fuel (RDF) and related materials. However, the heterogeneity of RDF makes the preparation of small representative samples very difficult and this difficulty has limited the effectiveness of TGA for characterization of RDF. A TGA method was applied to a variety of materials prepared from a commercially available RDF using a variety of procedures. Applicability of TGA method to the determination of the renewable content of RDF was considered. Cryogenic ball milling was found to be an effective means of preparing RDF samples for TGA. When combined with an effective sample preparation, TGA could be used as an alternative method for assessing the renewable content of RDF. Crown Copyright © 2015. Published by Elsevier Ltd. All rights reserved.

  9. 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

  10. Atypical antipsychotics: trends in analysis and sample preparation of various biological samples.

    Science.gov (United States)

    Fragou, Domniki; Dotsika, Spyridoula; Sarafidou, Parthena; Samanidou, Victoria; Njau, Samuel; Kovatsi, Leda

    2012-05-01

    Atypical antipsychotics are increasingly popular and increasingly prescribed. In some countries, they can even be obtained over-the-counter, without a prescription, making their abuse quite easy. Although atypical antipsychotics are thought to be safer than typical antipsychotics, they still have severe side effects. Intoxications are not rare and some of them have a fatal outcome. Drug interactions involving atypical antipsychotics complicate patient management in clinical settings and the determination of the cause of death in fatalities. In view of the above, analytical strategies that can efficiently isolate atypical antipsychotics from a variety of biological samples and quantify them accurately, sensitively and reliably, are of utmost importance both for the clinical, as well as for the forensic toxicologist. In this review, we will present and discuss novel analytical strategies that have been developed from 2004 to the present day for the determination of atypical antipsychotics in various biological samples.

  11. ARAM: an automated image analysis software to determine rosetting parameters and parasitaemia in Plasmodium samples.

    Science.gov (United States)

    Kudella, Patrick Wolfgang; Moll, Kirsten; Wahlgren, Mats; Wixforth, Achim; Westerhausen, Christoph

    2016-04-18

    Rosetting is associated with severe malaria and a primary cause of death in Plasmodium falciparum infections. Detailed understanding of this adhesive phenomenon may enable the development of new therapies interfering with rosette formation. For this, it is crucial to determine parameters such as rosetting and parasitaemia of laboratory strains or patient isolates, a bottleneck in malaria research due to the time consuming and error prone manual analysis of specimens. Here, the automated, free, stand-alone analysis software automated rosetting analyzer for micrographs (ARAM) to determine rosetting rate, rosette size distribution as well as parasitaemia with a convenient graphical user interface is presented. Automated rosetting analyzer for micrographs is an executable with two operation modes for automated identification of objects on images. The default mode detects red blood cells and fluorescently labelled parasitized red blood cells by combining an intensity-gradient with a threshold filter. The second mode determines object location and size distribution from a single contrast method. The obtained results are compared with standardized manual analysis. Automated rosetting analyzer for micrographs calculates statistical confidence probabilities for rosetting rate and parasitaemia. Automated rosetting analyzer for micrographs analyses 25 cell objects per second reliably delivering identical results compared to manual analysis. For the first time rosette size distribution is determined in a precise and quantitative manner employing ARAM in combination with established inhibition tests. Additionally ARAM measures the essential observables parasitaemia, rosetting rate and size as well as location of all detected objects and provides confidence intervals for the determined observables. No other existing software solution offers this range of function. The second, non-malaria specific, analysis mode of ARAM offers the functionality to detect arbitrary objects

  12. Cone-beam computed tomography analysis of the apical third of curved roots after mechanical preparation with different automated systems

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Cesar Augusto Pereira; Pascoalato, Cristina [University of Southern Santa Catarina (UNISUL), Tubarao, SC (Brazil); Meurer, Maria Ines [Federal University of Santa Catarina (UFSC), Florianopolis, SC (Brazil); Silva, Silvio Rocha Correa, E-mail: silvio@foar.unesp.b [Sao Paulo State University (UNESP), Araraquara, SP (Brazil)

    2009-07-01

    The present study evaluated by cone-beam computed tomography (CBCT) the apical canal transportation and centralizing ability of different automated systems after root canal preparation. The mesiobuccal canals of maxillary first molars (n=10 per group) were prepared with: GI - reciprocating system with K-Flexofile; GII - reciprocating system with NiTiFlex files; GIII - rotary system with K3 instruments; GIV - rotary system with RaCe instruments. CBCT scans were taken before and after biomechanical preparation up to a 40.02 diameter. Canal transportation was determined by measuring the smallest distance between the inner canal walls and the mesial and distal sides of the root. The centralization ability corresponded to the difference between the measurements from transportation evaluation, using the linear voxel to voxel method of analysis. The mean transportation was 0.06 +- 0.14 mm, with a tendency to deviate to the mesial side of the root (n=22), with no statistically significant difference among the groups (p=0.4153). The mean centralization index was 0.15 +- 0.65 also without statistically significant difference among the groups (p=0.0881). It may be concluded that apical canal transportation and centralization ability were not influenced by the type of mechanical movement and instruments used. (author)

  13. 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.

  14. 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.

  15. 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...

  16. 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

  17. 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.

  18. A simple approach to atom probe sample preparation by using shadow masks.

    Science.gov (United States)

    Felfer, Peter; McCarroll, Ingrid; Macauley, Chandra; Cairney, Julie M

    2016-01-01

    Here, we present a new method that utilises shadow masks in a broad ion beam system to prepare atom probe samples. It is particularly suited to non-conductors and materials with surface layers such as surface oxides, implanted layers or thin films. This new approach bypasses the focused ion beam (FIB) lift-out step, increasing the sample throughput, dramatically reducing the required FIB beam time and decreasing the complexity of sample preparation. Copyright © 2015 Elsevier B.V. All rights reserved.

  19. Sample preparation of biological macromolecular assemblies for the determination of high-resolution structures by cryo-electron microscopy.

    Science.gov (United States)

    Stark, Holger; Chari, Ashwin

    2016-02-01

    Single particle cryo-EM has recently developed into a powerful tool to determine the 3D structure of macromolecular complexes at near-atomic resolution, which allows structural biologists to build atomic models of proteins. All technical aspects of cryo-EM technology have been considerably improved over the last two decades, including electron microscopic hardware, image processing software and the ever growing speed of computers. This leads to a more widespread use of the technique, and it can be anticipated that further automation of electron microscopes and image processing tools will soon fully shift the focus away from the technological aspects, onto biological questions that can be answered. In single particle cryo-EM, no crystals of a macromolecule are required. In contrast to X-ray crystallography, this significantly facilitates structure determination by cryo-EM. Nevertheless, a relatively high level of biochemical control is still essential to obtain high-resolution structures by cryo-EM, and it can be anticipated that the success of the cryo-EM technology goes hand in hand with further developments of sample purification and preparation techniques. This will allow routine high-resolution structure determination of the many macromolecular complexes of the cell that until now represent evasive targets for X-ray crystallographers. Here we discuss the various biochemical tools that are currently available and the existing sample purification and preparation techniques for cryo-EM grid preparation that are needed to obtain high-resolution images for structure determination. © The Author 2015. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

  20. Microfluidic devices for sample preparation and rapid detection of foodborne pathogens

    DEFF Research Database (Denmark)

    Kant, Krishna; Shahbazi, Mohammad-Ali; Dave, Vivek Priy

    2018-01-01

    diagnosis competences. This has prompted researchers to call the current status of detection approaches into question and leverage new technologies for superior pathogen sensing outcomes. Novel strategies mainly rely on incorporating all the steps from sample preparation to detection in miniaturized devices...... streamlining the sample handling and concentrating procedures, which will subsequently reduce human errors and enhance the accuracy of the sensing methods. Integration of sample preparation techniques into these devices can effectively minimize the impact of complex food matrix on pathogen diagnosis...... recent advances in current state-of-the-art of sample preparation and concentration from food matrices with focus on bacterial capturing methods and sensing technologies, along with their advantages and limitations when integrated into microfluidic devices for online rapid detection of pathogens in foods...

  1. 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.

  2. High throughput detection of Coxiella burnetii by real-time PCR with internal control system and automated DNA preparation

    Directory of Open Access Journals (Sweden)

    Kramme Stefanie

    2008-05-01

    Full Text Available Abstract Background Coxiella burnetii is the causative agent of Q-fever, a widespread zoonosis. Due to its high environmental stability and infectivity it is regarded as a category B biological weapon agent. In domestic animals infection remains either asymptomatic or presents as infertility or abortion. Clinical presentation in humans can range from mild flu-like illness to acute pneumonia and hepatitis. Endocarditis represents the most common form of chronic Q-fever. In humans serology is the gold standard for diagnosis but is inadequate for early case detection. In order to serve as a diagnostic tool in an eventual biological weapon attack or in local epidemics we developed a real-time 5'nuclease based PCR assay with an internal control system. To facilitate high-throughput an automated extraction procedure was evaluated. Results To determine the minimum number of copies that are detectable at 95% chance probit analysis was used. Limit of detection in blood was 2,881 copies/ml [95%CI, 2,188–4,745 copies/ml] with a manual extraction procedure and 4,235 copies/ml [95%CI, 3,143–7,428 copies/ml] with a fully automated extraction procedure, respectively. To demonstrate clinical application a total of 72 specimens of animal origin were compared with respect to manual and automated extraction. A strong correlation between both methods was observed rendering both methods suitable. Testing of 247 follow up specimens of animal origin from a local Q-fever epidemic rendered real-time PCR more sensitive than conventional PCR. Conclusion A sensitive and thoroughly evaluated real-time PCR was established. Its high-throughput mode may show a useful approach to rapidly screen samples in local outbreaks for other organisms relevant for humans or animals. Compared to a conventional PCR assay sensitivity of real-time PCR was higher after testing samples from a local Q-fever outbreak.

  3. Automation impact study of Army training management 2: Extension of sampling and collection of installation resource data

    Energy Technology Data Exchange (ETDEWEB)

    Sanquist, T.F.; McCallum, M.C.; Hunt, P.S.; Slavich, A.L.; Underwood, J.A.; Toquam, J.L.; Seaver, D.A.

    1989-05-01

    This automation impact study of Army training management (TM) was performed for the Army Development and Employment Agency (ADEA) and the Combined Arms Training Activity (CATA) by the Battelle Human Affairs Research Centers and the Pacific Northwest Laboratory. The primary objective of the study was to provide the Army with information concerning the potential costs and savings associated with automating the TM process. This study expands the sample of units surveyed in Phase I of the automation impact effort (Sanquist et al., 1988), and presents data concerning installation resource management in relation to TM. The structured interview employed in Phase I was adapted to a self-administered survey. The data collected were compatible with that of Phase I, and both were combined for analysis. Three US sites, one reserve division, one National Guard division, and one unit in the active component outside the continental US (OCONUS) (referred to in this report as forward deployed) were surveyed. The total sample size was 459, of which 337 respondents contributed the most detailed data. 20 figs., 62 tabs.

  4. 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.

  5. 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

    Accurate and precise characterization of metrics such as size, mass, shape etc. of nanoparticles (NPs) remains a challenging task. In order to determine quantitative metrics that are relevant in food monitoring or in risk assessment, an instrumental separation method like asymmetric field flow...... fractionation (AFFF, or AF4) coupled on-line to various detectors including static and dynamic light scattering (LS), UV or fluorescence (FL) spectroscopies and ICP-MS have proven useful and powerful [1, 2, 3]. Furthermore, additional information obtained by an imaging method such as transmission electron...... 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...

  6. Magnetic resonance colonography with a limited bowel preparation and automated carbon dioxide insufflation in comparison to conventional colonoscopy: Patient burden and preferences

    International Nuclear Information System (INIS)

    Paardt, M.P. van der; Boellaard, T.N.; Zijta, F.M.; Baak, L.C.; Depla, A.C.T.M.; Dekker, E.; Nederveen, A.J.; Bipat, S.; Stoker, J.

    2015-01-01

    Highlights: • MR colonography with a limited bowel preparation and automated carbon dioxide insufflation demonstrated less burden compared to colonoscopy. • When discarding the bowel preparation, the examinations were rated equally burdensome. • The majority of patients preferred MR colonography over colonoscopy for their future examination of the bowel. - Abstract: Objectives: To evaluate patient burden and preferences for MR colonography with a limited bowel preparation and automated carbon dioxide insufflation in comparison to conventional colonoscopy. Methods: Symptomatic patients were consecutively recruited to undergo MR colonography with automated carbon dioxide insufflation and a limited bowel preparation followed within four weeks by colonoscopy with a standard bowel cleansing preparation. Four questionnaires regarding burden (on a five-point scale) and preferences (on a seven-point scale) were addressed after MR colonography and colonoscopy and five weeks after colonoscopy. Results: Ninety-nine patients (47 men, 52 women; mean age 62.3, SD 8.7) were included. None of the patients experienced severe or extreme burden from the MR colonography bowel preparation compared to 31.5% of the patients for the colonoscopy bowel preparation. Colonoscopy was rated more burdensome (25.6% severe or extreme burden) compared to MR colonography (5.2% severe or extreme burden) (P < 0.0001). When discarding the bowel preparations, the examinations were rated equally burdensome (P = 0.35). The majority of patients (61.4%) preferred MR colonography compared to colonoscopy (29.5%) immediately after the examinations and five weeks later (57.0% versus 39.5%). Conclusion: MR colonography with a limited bowel preparation and automated carbon dioxide insufflation demonstrated less burden compared to colonoscopy. The majority of patients preferred MR colonography over colonoscopy

  7. Magnetic resonance colonography with a limited bowel preparation and automated carbon dioxide insufflation in comparison to conventional colonoscopy: Patient burden and preferences

    Energy Technology Data Exchange (ETDEWEB)

    Paardt, M.P. van der, E-mail: m.p.vanderpaardt@amc.uva.nl [Department of Radiology, Academic Medical Center Amsterdam, Amsterdam (Netherlands); Boellaard, T.N., E-mail: t.n.boellaard@amc.uva.nl [Department of Radiology, Academic Medical Center Amsterdam, Amsterdam (Netherlands); Zijta, F.M., E-mail: fmzijta@yahoo.com [Department of Radiology, Medisch Centrum Haaglanden, Den Haag (Netherlands); Baak, L.C., E-mail: l.c.baak@olvg.nl [Department of Gastroenterology and Hepatology, Onze Lieve Vrouwe Gasthuis, Amsterdam (Netherlands); Depla, A.C.T.M., E-mail: actm.depla@slz.nl [Department of Gastroenterology and Hepatology, Slotervaartziekenhuis, Amsterdam (Netherlands); Dekker, E., E-mail: e.dekker@amc.uva.nl [Department of Gastroenterology and Hepatology, Academic Medical Center Amsterdam, Amsterdam (Netherlands); Nederveen, A.J., E-mail: a.j.nederveen@amc.uva.nl [Department of Radiology, Academic Medical Center Amsterdam, Amsterdam (Netherlands); Bipat, S., E-mail: s.bipat@amc.uva.nl [Department of Radiology, Academic Medical Center Amsterdam, Amsterdam (Netherlands); Stoker, J., E-mail: j.stoker@amc.uva.nl [Department of Radiology, Academic Medical Center Amsterdam, Amsterdam (Netherlands)

    2015-01-15

    Highlights: • MR colonography with a limited bowel preparation and automated carbon dioxide insufflation demonstrated less burden compared to colonoscopy. • When discarding the bowel preparation, the examinations were rated equally burdensome. • The majority of patients preferred MR colonography over colonoscopy for their future examination of the bowel. - Abstract: Objectives: To evaluate patient burden and preferences for MR colonography with a limited bowel preparation and automated carbon dioxide insufflation in comparison to conventional colonoscopy. Methods: Symptomatic patients were consecutively recruited to undergo MR colonography with automated carbon dioxide insufflation and a limited bowel preparation followed within four weeks by colonoscopy with a standard bowel cleansing preparation. Four questionnaires regarding burden (on a five-point scale) and preferences (on a seven-point scale) were addressed after MR colonography and colonoscopy and five weeks after colonoscopy. Results: Ninety-nine patients (47 men, 52 women; mean age 62.3, SD 8.7) were included. None of the patients experienced severe or extreme burden from the MR colonography bowel preparation compared to 31.5% of the patients for the colonoscopy bowel preparation. Colonoscopy was rated more burdensome (25.6% severe or extreme burden) compared to MR colonography (5.2% severe or extreme burden) (P < 0.0001). When discarding the bowel preparations, the examinations were rated equally burdensome (P = 0.35). The majority of patients (61.4%) preferred MR colonography compared to colonoscopy (29.5%) immediately after the examinations and five weeks later (57.0% versus 39.5%). Conclusion: MR colonography with a limited bowel preparation and automated carbon dioxide insufflation demonstrated less burden compared to colonoscopy. The majority of patients preferred MR colonography over colonoscopy.

  8. 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

  9. Independent assessment of matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) sample preparation quality: A novel statistical approach for quality scoring.

    Science.gov (United States)

    Kooijman, Pieter C; Kok, Sander J; Weusten, Jos J A M; Honing, Maarten

    2016-05-05

    Preparation of samples according to an optimized method is crucial for accurate determination of polymer sample characteristics by Matrix-Assisted Laser Desorption Ionization (MALDI) analysis. Sample preparation conditions such as matrix choice, cationization agent, deposition technique or even the deposition volume should be chosen to suit the sample of interest. Many sample preparation protocols have been developed and employed, yet finding the optimal sample preparation protocol remains a challenge. Because an objective comparison between the results of diverse protocols is not possible, "gut-feeling" or "good enough" is often decisive in the search for an optimum. This implies that sub-optimal protocols are used, leading to a loss of mass spectral information quality. To address this problem a novel analytical strategy based on MALDI imaging and statistical data processing was developed in which eight parameters were formulated to objectively quantify the quality of sample deposition and optimal MALDI matrix composition and finally sum up to an overall quality score of the sample deposition. These parameters can be established in a fully automated way using commercially available mass spectrometry imaging instruments without any hardware adjustments. With the newly developed analytical strategy the highest quality MALDI spots were selected, resulting in more reproducible and more valuable spectra for PEG in a variety of matrices. Moreover, our method enables an objective comparison of sample preparation protocols for any analyte and opens up new fields of investigation by presenting MALDI performance data in a clear and concise way. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Electromembrane extraction as a rapid and selective miniaturized sample preparation technique for biological fluids

    DEFF Research Database (Denmark)

    Gjelstad, Astrid; Pedersen-Bjergaard, Stig; Seip, Knut Fredrik

    2015-01-01

    This special report discusses the sample preparation method electromembrane extraction, which was introduced in 2006 as a rapid and selective miniaturized extraction method. The extraction principle is based on isolation of charged analytes extracted from an aqueous sample, across a thin film....... Technical aspects of electromembrane extraction, important extraction parameters as well as a handful of examples of applications from different biological samples and bioanalytical areas are discussed in the paper....

  11. 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.

  12. Potential Sources of Artifacts and Backgrounds Generated by the Sample Preparation of SAM

    OpenAIRE

    Buch, Arnaud; Belmahdi, Imène; Szopa, Cyril; Freissinet, Caroline; Glavin, Daniel P.; Coll, Patrice; Cabane, Michel; Millan, Maeva; Eigenbrode, Jennifer; Navarro-González, Rafael; Stern, Jennifer C.; Pinnick, Veronica; Coscia, David; Teinturier, Samuel; Morisson, M.

    2016-01-01

    International audience; Sample Analysis at Mars (SAM) is one of the instruments of the MSL mission. Three analytical devices are onboard SAM: the Tunable Laser Spectrometer (TLS), the Gas Chromatography (GC) and the Mass Spectrometer (MS). To adapt the nature of a sample to the analytical devices used, a sample preparation and gas processing system implemented with (a) a pyrolysis system, (b) wet chemistry: MTBSTFA and TMAH (c) the hydrocarbon trap (silica beads, Tenax® TA and Carbosieve G) a...

  13. Large sample neutron activation analysis avoids representative sub-sampling and sample preparation difficulties : An added value for forensic analysis

    NARCIS (Netherlands)

    Bode, P.; Romanò, Sabrina; Romolo, Francesco Saverio

    2017-01-01

    A crucial part of any chemical analysis is the degree of representativeness of the measurand(s) in the test portion for the same measurands in the object, originally collected for investigation. Such an object usually may have either to be homogenized and sub-sampled, or digested/dissolved. Any

  14. Automated preparation of Kepler time series of planet hosts for asteroseismic analysis

    DEFF Research Database (Denmark)

    Handberg, R.; Lund, M. N.

    2014-01-01

    . In this paper we present the KASOC Filter, which is used to automatically prepare data from the Kepler/K2 mission for asteroseismic analyses of solar-like planet host stars. The methods are very effective at removing unwanted signals of both instrumental and planetary origins and produce significantly cleaner...

  15. Lab on valve-multisyringe flow injection system (LOV-MSFIA) for fully automated uranium determination in environmental samples.

    Science.gov (United States)

    Avivar, Jessica; Ferrer, Laura; Casas, Montserrat; Cerdà, Víctor

    2011-06-15

    The hyphenation of lab-on-valve (LOV) and multisyringe flow analysis (MSFIA), coupled to a long path length liquid waveguide capillary cell (LWCC), allows the spectrophotometric determination of uranium in different types of environmental sample matrices, without any manual pre-treatment, and achieving high selectivity and sensitivity levels. On-line separation and preconcentration of uranium is carried out by means of UTEVA resin. The potential of the LOV-MSFIA makes possible the fully automation of the system by the in-line regeneration of the column. After elution, uranium(VI) is spectrophotometrically detected after reaction with arsenazo-III. The determination of levels of uranium present in environmental samples is required in order to establish an environmental control. Thus, we propose a rapid, cheap and fully automated method to determine uranium(VI) in environmental samples. The limit of detection reached is 1.9 ηg of uranium and depending on the preconcentrated volume; it results in ppt levels (10.3 ηg L(-1)). Different water sample matrices (seawater, well water, freshwater, tap water and mineral water) and a phosphogypsum sample (with natural uranium content) were satisfactorily analyzed. Copyright © 2010 Elsevier B.V. All rights reserved.

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

    DEFF Research Database (Denmark)

    Alimadadi, Hossein; Pantleon, Karen

    2009-01-01

    . 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......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...

  17. 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

  18. 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.

  19. 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.

  20. 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

  1. 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.

  2. 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...

  3. Integration of enabling methods for the automated flow preparation of piperazine-2-carboxamide.

    Science.gov (United States)

    Ingham, Richard J; Battilocchio, Claudio; Hawkins, Joel M; Ley, Steven V

    2014-01-01

    Here we describe the use of a new open-source software package and a Raspberry Pi(®) computer for the simultaneous control of multiple flow chemistry devices and its application to a machine-assisted, multi-step flow preparation of pyrazine-2-carboxamide - a component of Rifater(®), used in the treatment of tuberculosis - and its reduced derivative piperazine-2-carboxamide.

  4. Integration of enabling methods for the automated flow preparation of piperazine-2-carboxamide

    Directory of Open Access Journals (Sweden)

    Richard J. Ingham

    2014-03-01

    Full Text Available Here we describe the use of a new open-source software package and a Raspberry Pi® computer for the simultaneous control of multiple flow chemistry devices and its application to a machine-assisted, multi-step flow preparation of pyrazine-2-carboxamide – a component of Rifater®, used in the treatment of tuberculosis – and its reduced derivative piperazine-2-carboxamide.

  5. [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.

  6. Design and building of a homemade sample changer for automation of the irradiation in neutron activation analysis technique

    International Nuclear Information System (INIS)

    Gago, Javier; Hernandez, Yuri; Baltuano, Oscar; Bedregal, Patricia; Lopez, Yon; Urquizo, Rafael

    2014-01-01

    Because the RP-10 research reactor operates during weekends, it was necessary to design and build a sample changer for irradiation as part of the automation process of neutron activation analysis technique. The device is formed by an aluminum turntable disk which can accommodate 19 polyethylene capsules, containing samples to be sent using the pneumatic transfer system from the laboratory to the irradiation position. The system is operate by a control switchboard to send and return capsules in a variable preset time and by two different ways, allowing the determination of short, medium and long lived radionuclides. Also another mechanism is designed called 'exchange valve' for changing travel paths (pipelines) allowing the irradiated samples to be stored for a longer time in the reactor hall. The system design has allowed complete automation of this technique, enabling the irradiation of samples without the presence of an analyst. The design, construction and operation of the device is described and presented in this article. (authors).

  7. 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

  8. Analysis of aroma compounds of Roselle by Dynamic Headspace Sampling using different preparation methods

    DEFF Research Database (Denmark)

    Juhari, Nurul Hanisah Binti; Varming, Camilla; Petersen, Mikael Agerlin

    2015-01-01

    The influence of different methods of sample preparation on the aroma profiles of dried Roselle (Hibiscus sabdariffa) was studied. Least amounts of aroma compounds were recovered by analysis of whole dry calyxes (WD) followed by ground dry (GD), blended together with water (BTW), and ground...... and then mixed with water (GMW). The highest number of aroma compounds was found in Roselle treated in water bath (2hr/40°C) (GMWKB). GMW was chosen as the preparation method because it was shown to be an efficient extraction method without the possibility of excessive chemical changes of the sample....

  9. 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)

  10. 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

  11. HPLC analysis of oxindole alkaloids in Uncaria tomentosa: sample preparation and analysis optimisation by factorial design.

    Science.gov (United States)

    Bertol, Gustavo; Franco, Luzia; Oliveira, Brás Heleno de

    2012-01-01

    Uncaria tomentosa ("cat's claw") is widely used for the treatment of some infectious and inflammatory diseases. Oxindole alkaloids are regarded as the most important components responsible for the biological activities attributed to the plant. Their analysis require efficient sample preparation and suitable reference standards but few are commercially available. To develop and validate a HPLC analytical method for oxindole alkaloids in Uncaria tomentosa with emphasis on sample preparation. Factorial experimental designs were used for the optimisation of both sample preparation and chromatographic separation. The optimised sample preparation involved extraction with aqueous ethanol, and the granulometry of the powdered plant material significantly influenced extraction yields. Mitraphylline was used as a calibration reference for the determination of total alkaloids. The method was fully validated and showed good selectivity, linearity (r²  ≥ 0.9996), accuracy (≥ 96%) and precision (RSD < 2.4%). Detection and quantification limits for mitraphylline were 0.8 and 2.4 ppm, respectively. The optimised chromatographic method, using organic buffer in the mobile phase, provided baseline separation of tetracyclic and pentacyclic alkaloids in the samples. Calibration using mitraphylline provided more accurate estimates of total alkaloid content when compared to other available reference alkaloids. Copyright © 2011 John Wiley & Sons, Ltd.

  12. 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

  13. Instrument and method for X-ray diffraction, fluorescence, and crystal texture analysis without sample preparation

    Science.gov (United States)

    Gendreau, Keith (Inventor); Martins, Jose Vanderlei (Inventor); Arzoumanian, Zaven (Inventor)

    2010-01-01

    An X-ray diffraction and X-ray fluorescence instrument for analyzing samples having no sample preparation includes a X-ray source configured to output a collimated X-ray beam comprising a continuum spectrum of X-rays to a predetermined coordinate and a photon-counting X-ray imaging spectrometer disposed to receive X-rays output from an unprepared sample disposed at the predetermined coordinate upon exposure of the unprepared sample to the collimated X-ray beam. The X-ray source and the photon-counting X-ray imaging spectrometer are arranged in a reflection geometry relative to the predetermined coordinate.

  14. 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.

  15. MALDI (matrix assisted laser desorption ionization) Imaging Mass Spectrometry (IMS) of skin: Aspects of sample preparation.

    Science.gov (United States)

    de Macedo, Cristiana Santos; Anderson, David M; Schey, Kevin L

    2017-11-01

    MALDI (matrix assisted laser desorption ionization) Imaging Mass Spectrometry (IMS) allows molecular analysis of biological materials making possible the identification and localization of molecules in tissues, and has been applied to address many questions on skin pathophysiology, as well as on studies about drug absorption and metabolism. Sample preparation for MALDI IMS is the most important part of the workflow, comprising specimen collection and preservation, tissue embedding, cryosectioning, washing, and matrix application. These steps must be carefully optimized for specific analytes of interest (lipids, proteins, drugs, etc.), representing a challenge for skin analysis. In this review, critical parameters for MALDI IMS sample preparation of skin samples will be described. In addition, specific applications of MALDI IMS of skin samples will be presented including wound healing, neoplasia, and infection. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. EXPERIMENTS TOWARDS DETERMINING BEST TRAINING SAMPLE SIZE FOR AUTOMATED EVALUATION OF DESCRIPTIVE ANSWERS THROUGH SEQUENTIAL MINIMAL OPTIMIZATION

    Directory of Open Access Journals (Sweden)

    Sunil Kumar C

    2014-01-01

    Full Text Available With number of students growing each year there is a strong need to automate systems capable of evaluating descriptive answers. Unfortunately, there aren’t many systems capable of performing this task. In this paper, we use a machine learning tool called LightSIDE to accomplish auto evaluation and scoring of descriptive answers. Our experiments are designed to cater to our primary goal of identifying the optimum training sample size so as to get optimum auto scoring. Besides the technical overview and the experiments design, the paper also covers challenges, benefits of the system. We also discussed interdisciplinary areas for future research on this topic.

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

    International Nuclear Information System (INIS)

    Wall, Mark A.

    2016-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Wall, Mark A. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2016-10-25

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

  19. High-frequency, long-duration water sampling in acid mine drainage studies: a short review of current methods and recent advances in automated water samplers

    Science.gov (United States)

    Chapin, Thomas

    2015-01-01

    Hand-collected grab samples are the most common water sampling method but using grab sampling to monitor temporally variable aquatic processes such as diel metal cycling or episodic events is rarely feasible or cost-effective. Currently available automated samplers are a proven, widely used technology and typically collect up to 24 samples during a deployment. However, these automated samplers are not well suited for long-term sampling in remote areas or in freezing conditions. There is a critical need for low-cost, long-duration, high-frequency water sampling technology to improve our understanding of the geochemical response to temporally variable processes. This review article will examine recent developments in automated water sampler technology and utilize selected field data from acid mine drainage studies to illustrate the utility of high-frequency, long-duration water sampling.

  20. 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.

  1. 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.

  2. Sample Preparation for Determination of Biological Thiols by Liquid Chromatography and Electromigration Techniques

    OpenAIRE

    Bald, Edward

    2004-01-01

    Wydrukowano z dostarczonych Wydawnictwu UŁ gotowych materiałów Majority of the bioanalytical or environmental methods do not use just one chromatografie or electrophoretic step, but rather involve several sample pretreatment steps which simplfy the matrix, and often preconcentrate and chemically modify the analytes. This work surveys typical procedures for sample preparation for most commonly analyzed biofluids with particular emphasis placed on chemical derivatization of su...

  3. 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.

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

    Science.gov (United States)

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

    2012-01-01

    The effect of the embedding medium on the nano-indentation measurements of lignocellulosic materials was investigated experimentally using nano-indentation. Both the reduced elastic modulus and the hardness of nonembedded cell walls were found to be lower than those of the embedded samples, proving that the embedding medium used for specimen preparation on cellulosic...

  5. 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.

  6. 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

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

    Science.gov (United States)

    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, ...

  8. Reproducibility of measurement of the environmental carbon-14 samples prepared by the gel suspension method

    International Nuclear Information System (INIS)

    Ohura, Hirotaka; Wakabayashi, Genichiro; Nakamura, Kouji; Okai, Tomio; Matoba, Masaru; Kakiuchi, Hideki; Momoshima, Noriyuki; Kawamura, Hidehisa.

    1997-01-01

    Simple liquid scintillation counting technique for the assay of 14 C in the environment was developed. This technique was done by using gel suspension method, in which sample preparation is very simple and requires no special equipments. The reproducibility of this technique was considered and it was shown that the gel suspension method had enough reproducibility to monitor the environmental 14 C. (author)

  9. Sample preparation for combined chemical analysis and bioassay application in water quality assessment

    NARCIS (Netherlands)

    Kolkman, A.; Schriks, M.; Brand, W; Bäuerlein, P.S.; van der Kooi, M.M.E.; van Doorn, R.H.; Emke, E.; Reus, A.; van der Linden, S.; de Voogt, P.; Heringa, M.B.

    2013-01-01

    The combination of in vitro bioassays and chemical screening can provide a powerful toolbox to determine biologically relevant compounds in water extracts. In this study, a sample preparation method is evaluated for the suitability for both chemical analysis and in vitro bioassays. A set of 39

  10. Standardized Sample Preparation Using a Drop-on-Demand Printing Platform

    Directory of Open Access Journals (Sweden)

    Paul M. Pellegrino

    2013-05-01

    Full Text Available Hazard detection systems must be evaluated with appropriate test material concentrations under controlled conditions in order to accurately identify and quantify unknown residues commonly utilized in theater. The existing assortment of hazard reference sample preparation methods/techniques presents a range of variability and reproducibility concerns, making it increasingly difficult to accurately assess optically- based detection technologies. To overcome these challenges, we examined the optimization, characterization, and calibration of microdroplets from a drop-on-demand microdispenser that has a proven capability for the preparation of energetic reference materials. Research presented herein focuses on the development of a simplistic instrument calibration technique and sample preparation protocol for explosive materials testing based on drop-on-demand technology. Droplet mass and reproducibility were measured using ultraviolet-visible (UV-Vis absorption spectroscopy. The results presented here demonstrate the operational factors that influence droplet dispensing for specific materials (e.g., energetic and interferents. Understanding these parameters permits the determination of droplet and sample uniformity and reproducibility (typical R2 values of 0.991, relative standard deviation or RSD ≤ 5%, and thus the demonstrated maturation of a successful and robust methodology for energetic sample preparation.

  11. A large-capacity sample-changer for automated gamma-ray spectroscopy

    International Nuclear Information System (INIS)

    Andeweg, A.H.

    1980-01-01

    An automatic sample-changer has been developed at the National Institute for Metallurgy for use in gamma-ray spectroscopy with a lithium-drifted germanium detector. The sample-changer features remote storage, which prevents cross-talk and reduces background. It has a capacity for 200 samples and a sample container that takes liquid or solid samples. The rotation and vibration of samples during counting ensure that powdered samples are compacted, and improve the precision and reproducibility of the counting geometry [af

  12. An overview of sample preparation procedures for LC-MS multiclass antibiotic determination in environmental and food samples.

    Science.gov (United States)

    Moreno-Bondi, María Cruz; Marazuela, María Dolores; Herranz, Sonia; Rodriguez, Erika

    2009-10-01

    Antibiotics are a class of pharmaceuticals that are of great interest due to the large volumes of these substances that are consumed in both human and veterinary medicine, and due to their status as the agents responsible for bacterial resistance. They can be present in foodstuffs and in environmental samples as multicomponent chemical mixtures that exhibit a wide range of mechanisms of action. Moreover, they can be transformed into different metabolites by the action of microorganisms, as well as by other physical or chemical means, resulting in mixtures with higher ecotoxicities and risks to human health than those of the individual compounds. Therefore, there is growing interest in the availability of multiclass methods for the analysis of antimicrobial mixtures in environmental and food samples at very low concentrations. Liquid chromatography (LC) has become the technique of choice for multiclass analysis, especially when coupled to mass spectrometry (LC-MS) and tandem MS (LC-MS(2)). However, due to the complexity of the matrix, in most cases an extraction step for sample clean-up and preconcentration is required before analysis in order to achieve the required sensitivities. This paper reviews the most recent developments and applications of multiclass antimicrobial determination in environmental and food matrices, emphasizing the practical aspects of sample preparation for the simultaneous extraction of antimicrobials from the selected samples. Future trends in the application of LC-MS-based techniques to multiclass antibiotic analysis are also presented.

  13. 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.

  14. 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

  15. 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

  16. 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

  17. 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

  18. Advancement of Solidification Processing Technology Through Real Time X-Ray Transmission Microscopy: Sample Preparation

    Science.gov (United States)

    Stefanescu, D. M.; Curreri, P. A.

    1996-01-01

    Two types of samples were prepared for the real time X-ray transmission microscopy (XTM) characterization. In the first series directional solidification experiments were carried out to evaluate the critical velocity of engulfment of zirconia particles in the Al and Al-Ni eutectic matrix under ground (l-g) conditions. The particle distribution in the samples was recorded on video before and after the samples were directionally solidified. In the second series samples of the above two type of composites were prepared for directional solidification runs to be carried out on the Advanced Gradient Heating Facility (AGHF) aboard the space shuttle during the LMS mission in June 1996. X-ray microscopy proved to be an invaluable tool for characterizing the particle distribution in the metal matrix samples. This kind of analysis helped in determining accurately the critical velocity of engulfment of ceramic particles by the melt interface in the opaque metal matrix composites. The quality of the cast samples with respect to porosity and instrumented thermocouple sheath breakage or shift could be easily viewed and thus helped in selecting samples for the space shuttle experiments. Summarizing the merits of this technique it can be stated that this technique enabled the use of cast metal matrix composite samples since the particle location was known prior to the experiment.

  19. GeLC-MS: A Sample Preparation Method for Proteomics Analysis of Minimal Amount of Tissue.

    Science.gov (United States)

    Makridakis, Manousos; Vlahou, Antonia

    2017-10-10

    Application of various proteomics methodologies have been implemented for the global and targeted proteome analysis of many different types of biological samples such as tissue, urine, plasma, serum, blood, and cell lines. Among the aforementioned biological samples, tissue has an exceptional role into clinical research and practice. Disease initiation and progression is usually located at the tissue level of different organs, making the analysis of this material very important for the understanding of the disease pathophysiology. Despite the significant advances in the mass spectrometry instrumentation, tissue proteomics still faces several challenges mainly due to increased sample complexity and heterogeneity. However, the most prominent challenge is attributed to the invasive procedure of tissue sampling which restricts the availability of fresh frozen tissue to minimal amounts and limited number of samples. Application of GeLC-MS sample preparation protocol for tissue proteomics analysis can greatly facilitate making up for these difficulties. In this chapter, a step by step guide for the proteomics analysis of minute amounts of tissue samples using the GeLC-MS sample preparation protocol, as applied by our group in the analysis of multiple different types of tissues (vessels, kidney, bladder, prostate, heart) is provided.

  20. Client-server architecture applied to system automation radioactivity sampling in atmosphere

    Science.gov (United States)

    Hubbard, C. W.; McKinnon, A. D.

    1997-06-01

    Control software for an automated particulate air sampler is described. The software is divided into a number of small, cooperating server processes, each of which is responsible for the control of a particular device or subsystem. For each process, an effort was made to isolate the details of the underlying device or subsystem from the server interface. This made it possible to change the hardware without making changes to any of the server's client processes. A single supervisor process is responsible for overall system control. The design of the control algorithm was facilitated by employing a state machine model. Such a model is easy to study, easy to modify, and provides a clear understanding of the control mechanism to programmers and non-programmers alike. A state machine library was developed which greatly eased the task of implementing the design and ensured that the control algorithm detailed by the state machine model was the same algorithm that was actually employed.

  1. A METHOD FOR PREPARING A SUBSTRATE BY APPLYING A SAMPLE TO BE ANALYSED

    DEFF Research Database (Denmark)

    2017-01-01

    The invention relates to a method for preparing a substrate (105a) comprising a sample reception area (110) and a sensing area (111). The method comprises the steps of: 1) applying a sample on the sample reception area; 2) rotating the substrate around a predetermined axis; 3) during rotation......, at least part of the liquid travels from the sample reception area to the sensing area due to capillary forces acting between the liquid and the substrate; and 4) removing the wave of particles and liquid formed at one end of the substrate. The sensing area is closer to the predetermined axis than...... the sample reception area. The sample comprises a liquid part and particles suspended therein....

  2. 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.

  3. 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

  4. Applied Focused Ion Beam Techniques for Sample Preparation of Astromaterials for Integrated Nano-Analysis

    Energy Technology Data Exchange (ETDEWEB)

    Graham, G A; Teslich, N E; Kearsley, A T; Stadermann, F J; Stroud, R M; Dai, Z R; Ishii, H A; Hutcheon, I D; Bajt, S; Snead, C J; Weber, P K; Bradley, J P

    2007-02-20

    Sample preparation is always a critical step in study of micrometer sized astromaterials available for study in the laboratory, whether their subsequent analysis is by electron microscopy or secondary ion mass spectrometry. A focused beam of gallium ions has been used to prepare electron transparent sections from an interplanetary dust particle, as part of an integrated analysis protocol to maximize the mineralogical, elemental, isotopic and spectroscopic information extracted from one individual particle. In addition, focused ion beam techniques have been employed to extract cometary residue preserved on the rims and walls of micro-craters in 1100 series aluminum foils that were wrapped around the sample tray assembly on the Stardust cometary sample collector. Non-ideal surface geometries and inconveniently located regions of interest required creative solutions. These include support pillar construction and relocation of a significant portion of sample to access a region of interest. Serial sectioning, in a manner similar to ultramicrotomy, is a significant development and further demonstrates the unique capabilities of focused ion beam microscopy for sample preparation of astromaterials.

  5. Membrane biofouling characterization: effects of sample preparation procedures on biofilm structure and the microbial community

    KAUST Repository

    Xue, Zheng

    2014-07-15

    Ensuring the quality and reproducibility of results from biofilm structure and microbial community analysis is essential to membrane biofouling studies. This study evaluated the impacts of three sample preparation factors (ie number of buffer rinses, storage time at 4°C, and DNA extraction method) on the downstream analysis of nitrifying biofilms grown on ultrafiltration membranes. Both rinse and storage affected biofilm structure, as suggested by their strong correlation with total biovolume, biofilm thickness, roughness and the spatial distribution of EPS. Significant variations in DNA yields and microbial community diversity were also observed among samples treated by different rinses, storage and DNA extraction methods. For the tested biofilms, two rinses, no storage and DNA extraction with both mechanical and chemical cell lysis from attached biofilm were the optimal sample preparation procedures for obtaining accurate information about biofilm structure, EPS distribution and the microbial community. © 2014 © 2014 Taylor & Francis.

  6. 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.

  7. Automated method for simultaneous lead and strontium isotopic analysis applied to rainwater samples and airborne particulate filters (PM10).

    Science.gov (United States)

    Beltrán, Blanca; Avivar, Jessica; Mola, Montserrat; Ferrer, Laura; Cerdà, Víctor; Leal, Luz O

    2013-09-03

    A new automated, sensitive, and fast system for the simultaneous online isolation and preconcentration of lead and strontium by sorption on a microcolumn packed with Sr-resin using an inductively coupled plasma mass spectrometry (ICP-MS) detector was developed, hyphenating lab-on-valve (LOV) and multisyringe flow injection analysis (MSFIA). Pb and Sr are directly retained on the sorbent column and eluted with a solution of 0.05 mol L(-1) ammonium oxalate. The detection limits achieved were 0.04 ng for lead and 0.03 ng for strontium. Mass calibration curves were used since the proposed system allows the use of different sample volumes for preconcentration. Mass linear working ranges were between 0.13 and 50 ng and 0.1 and 50 ng for lead and strontium, respectively. The repeatability of the method, expressed as RSD, was 2.1% and 2.7% for Pb and Sr, respectively. Environmental samples such as rainwater and airborne particulate (PM10) filters as well as a certified reference material SLRS-4 (river water) were satisfactorily analyzed obtaining recoveries between 90 and 110% for both elements. The main features of the LOV-MSFIA-ICP-MS system proposed are the capability to renew solid phase extraction at will in a fully automated way, the remarkable stability of the column which can be reused up to 160 times, and the potential to perform isotopic analysis.

  8. Cross-sectional atom probe tomography sample preparation for improved analysis of fins on SOI

    Energy Technology Data Exchange (ETDEWEB)

    Martin, Andrew J., E-mail: andy.martin@globalfoundries.com; Weng, Weihao; Zhu, Zhengmao; Loesing, Rainer; Shaffer, James; Katnani, Ahmad

    2016-02-15

    Sample preparation for atom probe tomography of 3D semiconductor devices has proven to significantly affect field evaporation and the reliability of reconstructed data. A cross-sectional preparation method is applied to state-of-the-art Si finFET technology on SOI. This preparation approach advantageously provides a conductive path for voltage and heat, offers analysis of many fins within a single tip, and improves resolution across interfaces of particular interest. Measured B and Ge profiles exhibit good correlation with SIMS and EDX and show no signs of B clustering or pile-up near the Si/SiGe interface of the fin. - Highlights: • Cross-section atom probe tomography sample preparation of fins on SOI. • >5 fins captured in single atom probe tip via cross-section method. • Oxides affect collection efficiency, reconstruction accuracy, and data reliability. • Sample orientation affects field evaporation of dissimilar materials. • Data is well-matched to SIMS and EDX analysis.

  9. 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

  10. Surveillance cultures of samples obtained from biopsy channels and automated endoscope reprocessors after high-level disinfection of gastrointestinal endoscopes

    Directory of Open Access Journals (Sweden)

    Chiu King-Wah

    2012-09-01

    Full Text Available Abstract Background The instrument channels of gastrointestinal (GI endoscopes may be heavily contaminated with bacteria even after high-level disinfection (HLD. The British Society of Gastroenterology guidelines emphasize the benefits of manually brushing endoscope channels and using automated endoscope reprocessors (AERs for disinfecting endoscopes. In this study, we aimed to assess the effectiveness of decontamination using reprocessors after HLD by comparing the cultured samples obtained from biopsy channels (BCs of GI endoscopes and the internal surfaces of AERs. Methods We conducted a 5-year prospective study. Every month random consecutive sampling was carried out after a complete reprocessing cycle; 420 rinse and swabs samples were collected from BCs and internal surface of AERs, respectively. Of the 420 rinse samples collected from the BC of the GI endoscopes, 300 were obtained from the BCs of gastroscopes and 120 from BCs of colonoscopes. Samples were collected by flushing the BCs with sterile distilled water, and swabbing the residual water from the AERs after reprocessing. These samples were cultured to detect the presence of aerobic and anaerobic bacteria and mycobacteria. Results The number of culture-positive samples obtained from BCs (13.6%, 57/420 was significantly higher than that obtained from AERs (1.7%, 7/420. In addition, the number of culture-positive samples obtained from the BCs of gastroscopes (10.7%, 32/300 and colonoscopes (20.8%, 25/120 were significantly higher than that obtained from AER reprocess to gastroscopes (2.0%, 6/300 and AER reprocess to colonoscopes (0.8%, 1/120. Conclusions Culturing rinse samples obtained from BCs provides a better indication of the effectiveness of the decontamination of GI endoscopes after HLD than culturing the swab samples obtained from the inner surfaces of AERs as the swab samples only indicate whether the AERs are free from microbial contamination or not.

  11. Semi-automated separation of the epimeric dehydropyrrolizidine alkaloids lycopsamine and intermedine: preparation of their N-oxides and NMR comparison with diastereoisomeric rinderine and echinatine.

    Science.gov (United States)

    Colegate, Steven M; Gardner, Dale R; Betz, Joseph M; Panter, Kip E

    2014-01-01

    The diversity of structure and, particularly, stereochemical variation of the dehydropyrrolizidine alkaloids can present challenges for analysis and the isolation of pure compounds for the preparation of analytical standards and for toxicology studies. To investigate methods for the separation of gram-scale quantities of the epimeric dehydropyrrolizidine alkaloids lycopsamine and intermedine and to compare their NMR spectroscopic data with those of their heliotridine-based analogues echinatine and rinderine. Lycopsamine and intermedine were extracted, predominantly as their N-oxides and along with their acetylated derivatives, from commercial samples of comfrey (Symphytum officinale) root. Alkaloid enrichment involved liquid-liquid partitioning of the crude methanol extract between dilute aqueous acid and n-butanol, reduction of N-oxides and subsequent continuous liquid-liquid extraction of free base alkaloids into CHCl3 . The alkaloid-rich fraction was further subjected to semi-automated flash chromatography using boronated soda glass beads or boronated quartz sand. Boronated soda glass beads (or quartz sand) chromatography adapted to a Biotage Isolera Flash Chromatography System enabled large-scale separation (at least up to 1-2 g quantities) of lycopsamine and intermedine. The structures were confirmed using one- and two-dimensional (1) H- and (13) C-NMR spectroscopy. Examination of the NMR data for lycopsamine, intermedine and their heliotridine-based analogues echinatine and rinderine allowed for some amendments of literature data and provided useful comparisons for determining relative configurations in monoester dehydropyrrolizidine alkaloids. A similar NMR comparison of lycopsamine and intermedine with their N-oxides showed the effects of N-oxidation on some key chemical shifts. A levorotatory shift in specific rotation from +3.29° to -1.5° was observed for lycopsamine when dissolved in ethanol or methanol respectively. A semi-automated flash

  12. 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.

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

    Science.gov (United States)

    Ashley, Jon; Shahbazi, Mohammad-Ali; Kant, Krishna; Chidambara, Vinayaka Aaydha; Wolff, Anders; Bang, Dang Duong; Sun, Yi

    2017-05-15

    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 loading capacity. MIPs have been intensively employed in classical solid-phase extraction and solid-phase microextraction. More recently, MIPs have been combined with magnetic bead extraction, which greatly simplifies sample handling procedures. Studies have consistently shown that MIPs can effectively minimize complex food matrix effects, and improve recoveries and detection limits. In addition to sample preparation, MIPs have also been viewed as promising alternatives to bio-receptors due to the inherent molecular recognition abilities and the high stability in harsh chemical and physical conditions. MIPs have been utilized as receptors in biosensing platforms such as electrochemical, optical and mass biosensors to detect various analytes in food. In this review, we will discuss the current state-of-the-art of MIP synthesis and applications in the context of food analysis. We will highlight 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. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. Recent trends in sorption-based sample preparation and liquid chromatography techniques for food analysis.

    Science.gov (United States)

    Maciel, Edvaldo V Soares; de Toffoli, Ana Lúcia; Lanças, Fernando Mauro

    2018-04-20

    The accelerated rising of the world's population increased the consumption of food, thus demanding more rigors in the control of residue and contaminants in food-based products marketed for human consumption. In view of the complexity of most food matrices, including fruits, vegetables, different types of meat, beverages, among others, a sample preparation step is important to provide more reliable results when combined with high performance liquid chromatography separations. An adequate sample preparation step before the chromatographic analysis is mandatory in obtaining higher precision and accuracy in order to improve the extraction of the target analytes, one of the priorities in analytical chemistry. The recent discovery of new materials such as ionic liquids, graphene-derived materials, molecularly imprinted polymers, restricted access media, magnetic nanoparticles, and carbonaceous nanomaterials, provided high sensitivity and selectivity results in an extensive variety of applications. These materials, as well as their several possible combinations, have been demonstrated to be highly appropriate for the extraction of different analytes in complex samples such as food products. The main characteristics and application of these new materials in food analysis will be presented and discussed in this paper. Another topic discussed in this review covers the main advantages and limitations of sample preparation microtechniques, as well as their off-line and on-line combination with high performance liquid chromatography for food analysis. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

  15. 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.

  16. Cytology Preparations of Formalin Fixative Aid Detection of Giardia in Duodenal Biopsy Samples.

    Science.gov (United States)

    Panarelli, Nicole C; Gobara, Nariman; Hoda, Rana S; Chaump, Michael; Jessurun, Jose; Yantiss, Rhonda K

    2017-04-01

    Giardiasis is the most common intestinal parasitic infection in the United States. The organism elicits no, or minimal, inflammatory changes in duodenal biopsy samples, so it can be easily overlooked. We performed this study to determine whether Giardia could be isolated from the formalin fixative of biopsy samples, and to evaluate the value of fluid analysis in the assessment for potential infection. We prospectively evaluated duodenal biopsy samples from 92 patients with a clinical suspicion of giardiasis or symptoms compatible with that diagnosis (ie, diarrhea, bloating, or abdominal pain) Biopsy samples were routinely processed and stained with hematoxylin and eosin. Histologic diagnoses included giardiasis (5 cases, 4%), normal findings (64 cases, 70%), peptic injury/active duodenitis (12 cases, 13%), and intraepithelial lymphocytosis with villous blunting (10 cases, 12%). Fifteen cases (13%) showed detached degenerated epithelial cells or mucus droplets in the intervillous space that resembled Giardia. Cytology slides were prepared from formalin in the biopsy container using the standard Cytospin protocol and reviewed by a cytopathologist blinded to the biopsy findings. Cytologic evaluation revealed Giardia spp. in all 5 biopsy-proven cases, and identified an additional case that was not detected by biopsy analysis. Organisms were significantly more numerous (mean: 400 trophozoites; range, 120 to 810) and showed better morphologic features in cytology preparations compared with tissue sections (mean: 129 trophozoites; range, 37 to 253 organisms; P=0.05). Our findings suggest that cytology preparations from formalin fixative can resolve diagnostically challenging cases and even enhance Giardia detection in some cases.

  17. Diagnostic PCR: validation and sample preparation are two sides of the same coin

    DEFF Research Database (Denmark)

    Hoorfar, Jeffrey; Wolffs, Petra; Radstrøm, Peter

    2004-01-01

    of quantitative reference DNA material and reagents, production of stringent protocols and tools for thermal cycler performance testing, uncomplicated sample preparation techniques, and extensive ring trials for assessment of the efficacy of selected matrix/pathogen detection protocols.......Increased use of powerful PCR technology for the routine detection of pathogens has focused attention on the need for international validation and preparation of official non-commercial guidelines. Bacteria of epidemiological importance should be the prime focus, although a "validation...... infrastructure" once established could easily be adapted for PCR-based detection of viruses and parasites. The aim of standardization should be the widespread adoption of diagnostic PCR for routine pathogen testing. European experience provides the impetus for realization of this vision through preparation...

  18. Cross-sectional atom probe tomography sample preparation for improved analysis of fins on SOI.

    Science.gov (United States)

    Martin, Andrew J; Weng, Weihao; Zhu, Zhengmao; Loesing, Rainer; Shaffer, James; Katnani, Ahmad

    2016-02-01

    Sample preparation for atom probe tomography of 3D semiconductor devices has proven to significantly affect field evaporation and the reliability of reconstructed data. A cross-sectional preparation method is applied to state-of-the-art Si finFET technology on SOI. This preparation approach advantageously provides a conductive path for voltage and heat, offers analysis of many fins within a single tip, and improves resolution across interfaces of particular interest. Measured B and Ge profiles exhibit good correlation with SIMS and EDX and show no signs of B clustering or pile-up near the Si/SiGe interface of the fin. Copyright © 2015 Elsevier B.V. All rights reserved.

  19. 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.

  20. Improvement of the sample preparation method for AMS measurement of 36Cl in natural environment

    Science.gov (United States)

    Jiang, Songsheng; Lin, Yuanxian; Zhang, Huiying

    2004-08-01

    The isobaric interference, 36S, is a main problem in AMS measurement of 36Cl. The SO42- ion exists in the natural environment with an amount compared with the chlorine concentration. The chemical procedure should have a powerful capacity to remove sulfur from samples. Traditionally, precipitation of BaSO4 is used to separate S from the sample material. The sulfur reduction process should be repeated more than two times for measurement of the sample with a36Cl/Cl ratio down to 10-13. The multi-reduction processes take a long time and chlorine recovery is low. In the present work, a new cation-exchange-column method is used. The Ba column is used for separation of S. When the sample solution is passed through the Ba Column, SO42- are absorbed. After removal of SO42- the sample solution is passed through the H column to absorb metal ions and transfer Cl- to HCl. Then the HCl solution is passed through the Na column to convert HCl to NaCl. Finally, excess AgNO3 is added to the NaCl solution and AgCl is precipitated for AMS measurement. The chemical process only takes ∼6 h, the time much shorter than the traditional method, and the chlorine recovery is higher than ∼90%. The rainwater, groundwater and seawater samples were prepared with this method. The 36Cl/Cl ratios in those samples were measured in range of 10-13- 10-14. The method can also be used for soil, sediment and rock samples after extraction of chlorine (36Cl) from the sample materials. Some sediment and rock samples were prepared and 36Cl was measured.

  1. HPLC/DAD determination of rosmarinic acid in Salvia officinalis: sample preparation optimization by factorial design

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Karina B. de [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil). Dept. de Farmacia; Oliveira, Bras H. de, E-mail: bho@ufpr.br [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil). Dept. de Quimica

    2013-01-15

    Sage (Salvia officinalis) contains high amounts of the biologically active rosmarinic acid (RA) and other polyphenolic compounds. RA is easily oxidized, and may undergo degradation during sample preparation for analysis. The objective of this work was to develop and validate an analytical procedure for determination of RA in sage, using factorial design of experiments for optimizing sample preparation. The statistically significant variables for improving RA extraction yield were determined initially and then used in the optimization step, using central composite design (CCD). The analytical method was then fully validated, and used for the analysis of commercial samples of sage. The optimized procedure involved extraction with aqueous methanol (40%) containing an antioxidant mixture (ascorbic acid and ethylenediaminetetraacetic acid (EDTA)), with sonication at 45 deg C for 20 min. The samples were then injected in a system containing a C{sub 18} column, using methanol (A) and 0.1% phosphoric acid in water (B) in step gradient mode (45A:55B, 0-5 min; 80A:20B, 5-10 min) with flow rate of 1.0 mL min-1 and detection at 330 nm. Using this conditions, RA concentrations were 50% higher when compared to extractions without antioxidants (98.94 {+-} 1.07% recovery). Auto-oxidation of RA during sample extraction was prevented by the use of antioxidants resulting in more reliable analytical results. The method was then used for the analysis of commercial samples of sage. (author)

  2. Automated spectrometer interface for measurement of short half-life samples for neutron activation analysis

    Energy Technology Data Exchange (ETDEWEB)

    Lapolli, André L.; Secco, Marcello; Genezini, Frederico A.; Zahn, Guilherme S.; Moreira, Edson G., E-mail: alapolli@ipen.br [Instituto de Pesquisas Energéticas e Nucleares (IPEN/CNEN-SP), São Paulo, SP (Brazil)

    2017-07-01

    In this paper a source positioning system was developed, based on a HPGe detector coupled to a Canberra DAS 1000 data acquisition system and Canberra's GENIE2K software and libraries. The system is composed of a step motor coupled to an Arduino Uno microcontroller, which is programmed using C language to allow for a source-detector distance between 0.3 and 20 cm - both components are coupled to a PC computer using the USB interface. In order to allow automated data acquisition, two additional pieces of software were developed. The first one, a Human-Machine Interface (HMI) programmed in Visual Basic 6, allows the programming and monitoring of the data acquisition process, and the other, in REXX language, controls the data acquisition process in the background. The HMI is user-friendly and versatile, so that the even rather complex data acquisition processes may be easily programmed. When the experiment scheme is saved, two files are created and used by the REXX code to control the acquisition process so that the data acquisition is automatically stopped and saved after a user-defined time, then the source is repositioned and data acquisition is cleared and restarted. While in the present stage the system only offers three distinct source positions, finer source-position adjusting is under development. In its present configuration the system has been tested for stability and repeatability in all three positions, with an an excellent performance (author)

  3. Automated spectrometer interface for measurement of short half-life samples for neutron activation analysis

    International Nuclear Information System (INIS)

    Lapolli, André L.; Secco, Marcello; Genezini, Frederico A.; Zahn, Guilherme S.; Moreira, Edson G.

    2017-01-01

    In this paper a source positioning system was developed, based on a HPGe detector coupled to a Canberra DAS 1000 data acquisition system and Canberra's GENIE2K software and libraries. The system is composed of a step motor coupled to an Arduino Uno microcontroller, which is programmed using C language to allow for a source-detector distance between 0.3 and 20 cm - both components are coupled to a PC computer using the USB interface. In order to allow automated data acquisition, two additional pieces of software were developed. The first one, a Human-Machine Interface (HMI) programmed in Visual Basic 6, allows the programming and monitoring of the data acquisition process, and the other, in REXX language, controls the data acquisition process in the background. The HMI is user-friendly and versatile, so that the even rather complex data acquisition processes may be easily programmed. When the experiment scheme is saved, two files are created and used by the REXX code to control the acquisition process so that the data acquisition is automatically stopped and saved after a user-defined time, then the source is repositioned and data acquisition is cleared and restarted. While in the present stage the system only offers three distinct source positions, finer source-position adjusting is under development. In its present configuration the system has been tested for stability and repeatability in all three positions, with an an excellent performance (author)

  4. 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.

  5. A lab-on-a-chip system integrating tissue sample preparation and multiplex RT-qPCR for gene expression analysis in point-of-care hepatotoxicity assessment.

    Science.gov (United States)

    Lim, Geok Soon; Chang, Joseph S; Lei, Zhang; Wu, Ruige; Wang, Zhiping; Cui, Kemi; Wong, Stephen

    2015-10-21

    A truly practical lab-on-a-chip (LOC) system for point-of-care testing (POCT) hepatotoxicity assessment necessitates the embodiment of full-automation, ease-of-use and "sample-in-answer-out" diagnostic capabilities. To date, the reported microfluidic devices for POCT hepatotoxicity assessment remain rudimentary as they largely embody only semi-quantitative or single sample/gene detection capabilities. In this paper, we describe, for the first time, an integrated LOC system that is somewhat close to a practical POCT hepatotoxicity assessment device - it embodies both tissue sample preparation and multiplex real-time RT-PCR. It features semi-automation, is relatively easy to use, and has "sample-in-answer-out" capabilities for multiplex gene expression analysis. Our tissue sample preparation module incorporating both a microhomogenizer and surface-treated paramagnetic microbeads yielded high purity mRNA extracts, considerably better than manual means of extraction. A primer preloading surface treatment procedure and the single-loading inlet on our multiplex real-time RT-PCR module simplify off-chip handling procedures for ease-of-use. To demonstrate the efficacy of our LOC system for POCT hepatotoxicity assessment, we perform a preclinical animal study with the administration of cyclophosphamide, followed by gene expression analysis of two critical protein biomarkers for liver function tests, aspartate transaminase (AST) and alanine transaminase (ALT). Our experimental results depict normalized fold changes of 1.62 and 1.31 for AST and ALT, respectively, illustrating up-regulations in their expression levels and hence validating their selection as critical genes of interest. In short, we illustrate the feasibility of multiplex gene expression analysis in an integrated LOC system as a viable POCT means for hepatotoxicity assessment.

  6. An introduction to sample preparation and imaging by cryo-electron microscopy for structural biology

    Science.gov (United States)

    Thompson, Rebecca F.; Walker, Matt; Siebert, C. Alistair; Muench, Stephen P.; Ranson, Neil A.

    2016-01-01

    Transmission electron microscopy (EM) is a versatile technique that can be used to image biological specimens ranging from intact eukaryotic cells to individual proteins >150 kDa. There are several strategies for preparing samples for imaging by EM, including negative staining and cryogenic freezing. In the last few years, cryo-EM has undergone a ‘resolution revolution’, owing to both advances in imaging hardware, image processing software, and improvements in sample preparation, leading to growing number of researchers using cryo-EM as a research tool. However, cryo-EM is still a rapidly growing field, with unique challenges. Here, we summarise considerations for imaging of a range of specimens from macromolecular complexes to cells using EM. PMID:26931652

  7. Sample preparation for two-dimensional gel electrophoresis: considering the composition of biological material.

    Science.gov (United States)

    Knigge, Thomas; Letendre, Julie; Monsinjon, Tiphaine

    2013-11-01

    Comparative proteomic analyses in ecotoxicology and related fields require reproducible display of as many proteins as possible. In addition, it should be possible to carry out a quantitative comparison in a reliable manner. Sample preparation represents one of the essential steps toward these aims. In their work, Wu et al. describe how to deal with different recalcitrant tissues of varying species (Proteomics 2013, 13, 3205-3210). Their work underlines the necessity to adapt sample preparation to the specific requirements of the biological material. Beyond that Wu et al. present TRIzol® as feasible means for combined extraction of proteins and RNA. Indeed, using TRI-reagent extraction for proteomics, they resolve two problems at a time: that of removing contaminating compounds and that of simultaneous analysis of gene and protein expression. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Applications of Blue Light-curing Acrylic Resin to Forensic Sample Preparation and Microtomy.

    Science.gov (United States)

    Groves, Ethan; Palenik, Christopher S

    2016-03-01

    This study discusses the results of an evaluation of a one-part blue light-curing acrylic resin for embedding trace evidence prior to the preparation of thin sections with a microtome. Through a comparison to several epoxy resins, the physical properties relevant to both trace evidence examination and analytical microscopy in general, including as viscosity, clarity, color, hardness, and cure speed, were explored. Finally, thin sections from paint samples embedded in this acrylic resin were evaluated to determine if, through smearing or impregnation, the resin contributed to the infrared spectra. The results of this study show that blue light-curing acrylic resins provide the desired properties of an embedding medium, generate high-quality thin sections, and can significantly simplify the preparation of paint chips, fibers and a multitude of other types of microscopic samples in the forensic trace evidence laboratory. © 2015 American Academy of Forensic Sciences.

  9. Automated Microfluidic Droplet-Based Sample Chopper for Detection of Small Fluorescence Differences Using Lock-In Analysis.

    Science.gov (United States)

    Negou, Jean T; Avila, L Adriana; Li, Xiangpeng; Hagos, Tesfagebriel M; Easley, Christopher J

    2017-06-06

    Fluorescence is widely used for small-volume analysis and is a primary tool for on-chip detection in microfluidic devices, yet additional expertise, more elaborate optics, and phase-locked detectors are needed for ultrasensitive measurements. Recently, we designed a microfluidic analog to an optical beam chopper (μChopper) that alternated formation of picoliter volume sample and reference droplets. Without complex optics, the device negated large signal drifts (1/f noise), allowing absorbance detection in a mere 27 μm optical path. Here, we extend the μChopper concept to fluorescence detection with standard wide-field microscope optics. Precision of droplet control in the μChopper was improved by automation with pneumatic valves, allowing fluorescence measurements to be strictly phase locked at 0.04 Hz bandwidth to droplets generated at 3.50 Hz. A detection limit of 12 pM fluorescein was achieved when sampling 20 droplets, and as few as 310 zeptomoles (3.1 × 10 -19 mol) were detectable in single droplets (8.8 nL). When applied to free fatty acid (FFA) uptake in 3T3-L1 adipocytes, this μChopper permitted single-cell FFA uptake rates to be quantified at 3.5 ± 0.2 × 10 -15 mol cell -1 for the first time. Additionally, homogeneous immunoassays in droplets exhibited insulin detection limits of 9.3 nM or 190 amol (1.9 × 10 -16 mol). The combination of this novel, automated μChopper with lock-in detection provides a high-performance platform for detecting small differences with standard fluorescence optics, particularly in situations where sample volume is limited. The technique should be simple to implement into a variety of other droplet fluidics devices.

  10. 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.

  11. 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

  12. Sample preparation for accelerator mass spectrometry at the University of Washington

    International Nuclear Information System (INIS)

    Grootes, P.M.; Stuiver, M.; Farwell, G.W.; Schmidt, F.H.

    1981-01-01

    The adaptation of the University of Washington FN tandem Van de Graaff to accelerator mass spectrometry (AMS), as well as some of the results obtained, are described in another paper in this volume (Farwell et al., 1981). Here we discuss our experiences in preparing carbon and beryllium samples that give large and stable ion beams when used in our Extrion cesium sputter source with an inverted cesium beam geometry

  13. Standardized Sample Preparation Using a Drop-on-Demand Printing Platform

    Science.gov (United States)

    2013-05-07

    ring” effect , this effect is statistically negligible as compared to drop-and-dry methods. This is of particular concern with spatially sensitive ...Gillen, J.G. Fabrication of polymer microsphere particle standards containing trace explosives using an oil/water emulsion solvent extraction...technique and sample preparation protocol for explosive materials testing based on drop-on-demand technology. Droplet mass and reproducibility were measured

  14. [Preparation of sub-standard samples and XRF analytical method of powder non-metallic minerals].

    Science.gov (United States)

    Kong, Qin; Chen, Lei; Wang, Ling

    2012-05-01

    In order to solve the problem that standard samples of non-metallic minerals are not satisfactory in practical work by X-ray fluorescence spectrometer (XRF) analysis with pressed powder pellet, a method was studied how to make sub-standard samples according to standard samples of non-metallic minerals and to determine how they can adapt to analysis of mineral powder samples, taking the K-feldspar ore in Ebian-Wudu, Sichuan as an example. Based on the characteristic analysis of K-feldspar ore and the standard samples by X-ray diffraction (XRD) and chemical methods, combined with the principle of the same or similar between the sub-standard samples and unknown samples, the experiment developed the method of preparation of sub-standard samples: both of the two samples above mentioned should have the same kind of minerals and the similar chemical components, adapt mineral processing, and benefit making working curve. Under the optimum experimental conditions, a method for determination of SiO2, Al2O3, Fe2O3, TiO2, CaO, MgO, K2O and Na2O of K-feldspar ore by XRF was established. Thedetermination results are in good agreement with classical chemical methods, which indicates that this method was accurate.

  15. Simplified sample preparation using frame spotting method for direct counting of total bacteria by fluorescence microscopy.

    Science.gov (United States)

    Maruyama, Fumito; Yamaguchi, Nobuyasu; Kenzaka, Takehiko; Tani, Katsuji; Nasu, Masao

    2004-12-01

    A new preparation method for direct counting of bacteria in liquid samples with fluorescence microscope was developed using a glass slide coated with 3-aminopropyltriethoxy silane and ring-shaped polyester seal as a retainer. The experimental steps of this method were spotting samples onto the coated slides with the seal, drying under vacuum, staining with SYBR Green II, drying and covering with immersion oil and coverslip to allow counting. This simplified method provided consistent results when compared with the conventional filtration method for fluorescence microscopy, and is rapid, inexpensive and reproducible.

  16. Simulation of topography evolution and damage formation during TEM sample preparation using focused ion beams

    Energy Technology Data Exchange (ETDEWEB)

    Boxleitner, W. E-mail: wini@hobbit.fke.tuwien.ac.at; Hobler, G.; Klueppel, V.; Cerva, H

    2001-04-01

    Our recently developed simulation code FIBSIM is applied to topics related to transmission electron microscopy (TEM) sample preparation using focused ion beams (FIB). FIBSIM combines dynamic Monte Carlo simulation of collision cascades with two-dimensional, cell-based topography simulation. The influence of the scanning mode and of the beam current profile on the evolution of the surface contour is investigated. Furthermore, amorphous zones in silicon samples and damaged regions are predicted for different beam energies of 10, 30 and 50 keV. The thickness of the predicted amorphous regions is in good agreement with experimental TEM data.

  17. Error baseline rates of five sample preparation methods used to characterize RNA virus populations.

    Directory of Open Access Journals (Sweden)

    Jeffrey R Kugelman

    Full Text Available Individual RNA viruses typically occur as populations of genomes that differ slightly from each other due to mutations introduced by the error-prone viral polymerase. Understanding the variability of RNA virus genome populations is critical for understanding virus evolution because individual mutant genomes may gain evolutionary selective advantages and give rise to dominant subpopulations, possibly even leading to the emergence of viruses resistant to medical countermeasures. Reverse transcription of virus genome populations followed by next-generation sequencing is the only available method to characterize variation for RNA viruses. However, both steps may lead to the introduction of artificial mutations, thereby skewing the data. To better understand how such errors are introduced during sample preparation, we determined and compared error baseline rates of five different sample preparation methods by analyzing in vitro transcribed Ebola virus RNA from an artificial plasmid-based system. These methods included: shotgun sequencing from plasmid DNA or in vitro transcribed RNA as a basic "no amplification" method, amplicon sequencing from the plasmid DNA or in vitro transcribed RNA as a "targeted" amplification method, sequence-independent single-primer amplification (SISPA as a "random" amplification method, rolling circle reverse transcription sequencing (CirSeq as an advanced "no amplification" method, and Illumina TruSeq RNA Access as a "targeted" enrichment method. The measured error frequencies indicate that RNA Access offers the best tradeoff between sensitivity and sample preparation error (1.4-5 of all compared methods.

  18. 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.

  19. Preparation of Plant 41Ca Tracer Samples for Accelerator Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    ZHAO Qing-zhang1;JANG Ping-ping3;LIN De-yu4;YANG Xian-lin1;DOU Liang1;PANG Yi-jun1;WANG Xiao-ming1;ZHANG Hui1,5;YANG Xu-ran1;WU Shao-yong1;GAO Dong-sheng2;LI Ling2;WANG Lei2;SUN Ke-peng2;ZHOU Jun2;DONG Ke-jun1;HE Ming1

    2016-11-01

    Full Text Available Calcium plays an important role in the metabolism of plants and animals. In this paper, the preparation method of plant 41Ca for accelerator mass spectrometry (AMS measurement was developed for the first time in China. AMS, with its advantages of high sensitivity, small dose of radioactivity, high accuracy, large measuring range, and long tracer cycle, can be used to measure cosmogenic nuclide 41Ca , which has long half-life. The intensity of the beam in ion source is an important parameter for the sensitivity of AMS measurement. The high beam current can improve the sensitivity of AMS. The preparation methods of plant samples of 41Ca tracer were systematically studied to obtain high beam current using wet, dry and a combining method with wet and dry re-fluoride. A reliable preparation procedure of plant samples for 41Ca tracer and its optimization parameters were determined by testing beam currents of various samples and lay a foundation for the 41Ca-AMS technology at plant tracer applications.

  20. On the use of ultracentrifugal devices for routine sample preparation in biomolecular magic-angle-spinning NMR.

    Science.gov (United States)

    Mandal, Abhishek; Boatz, Jennifer C; Wheeler, Travis B; van der Wel, Patrick C A

    2017-03-01

    A number of recent advances in the field of magic-angle-spinning (MAS) solid-state NMR have enabled its application to a range of biological systems of ever increasing complexity. To retain biological relevance, these samples are increasingly studied in a hydrated state. At the same time, experimental feasibility requires the sample preparation process to attain a high sample concentration within the final MAS rotor. We discuss these considerations, and how they have led to a number of different approaches to MAS NMR sample preparation. We describe our experience of how custom-made (or commercially available) ultracentrifugal devices can facilitate a simple, fast and reliable sample preparation process. A number of groups have since adopted such tools, in some cases to prepare samples for sedimentation-style MAS NMR experiments. Here we argue for a more widespread adoption of their use for routine MAS NMR sample preparation.

  1. On the use of ultracentrifugal devices for routine sample preparation in biomolecular magic-angle-spinning NMR

    Energy Technology Data Exchange (ETDEWEB)

    Mandal, Abhishek; Boatz, Jennifer C. [University of Pittsburgh School of Medicine, Department of Structural Biology (United States); Wheeler, Travis B. [University of Pittsburgh School of Medicine, Department of Cell Biology (United States); Wel, Patrick C. A. van der, E-mail: vanderwel@pitt.edu [University of Pittsburgh School of Medicine, Department of Structural Biology (United States)

    2017-03-15

    A number of recent advances in the field of magic-angle-spinning (MAS) solid-state NMR have enabled its application to a range of biological systems of ever increasing complexity. To retain biological relevance, these samples are increasingly studied in a hydrated state. At the same time, experimental feasibility requires the sample preparation process to attain a high sample concentration within the final MAS rotor. We discuss these considerations, and how they have led to a number of different approaches to MAS NMR sample preparation. We describe our experience of how custom-made (or commercially available) ultracentrifugal devices can facilitate a simple, fast and reliable sample preparation process. A number of groups have since adopted such tools, in some cases to prepare samples for sedimentation-style MAS NMR experiments. Here we argue for a more widespread adoption of their use for routine MAS NMR sample preparation.

  2. Accelerated Evaluation of Automated Vehicles Safety in Lane-Change Scenarios Based on Importance Sampling Techniques.

    Science.gov (United States)

    Zhao, Ding; Lam, Henry; Peng, Huei; Bao, Shan; LeBlanc, David J; Nobukawa, Kazutoshi; Pan, Christopher S

    2017-03-01

    Automated vehicles (AVs) must be thoroughly evaluated before their release and deployment. A widely used evaluation approach is the Naturalistic-Field Operational Test (N-FOT), which tests prototype vehicles directly on the public roads. Due to the low exposure to safety-critical scenarios, N-FOTs are time consuming and expensive to conduct. In this paper, we propose an accelerated evaluation approach for AVs. The results can be used to generate motions of the other primary vehicles to accelerate the verification of AVs in simulations and controlled experiments. Frontal collision due to unsafe cut-ins is the target crash type of this paper. Human-controlled vehicles making unsafe lane changes are modeled as the primary disturbance to AVs based on data collected by the University of Michigan Safety Pilot Model Deployment Program. The cut-in scenarios are generated based on skewed statistics of collected human driver behaviors, which generate risky testing scenarios while preserving the statistical information so that the safety benefits of AVs in nonaccelerated cases can be accurately estimated. The cross-entropy method is used to recursively search for the optimal skewing parameters. The frequencies of the occurrences of conflicts, crashes, and injuries are estimated for a modeled AV, and the achieved accelerated rate is around 2000 to 20 000. In other words, in the accelerated simulations, driving for 1000 miles will expose the AV with challenging scenarios that will take about 2 to 20 million miles of real-world driving to encounter. This technique thus has the potential to greatly reduce the development and validation time for AVs.

  3. On-chip sample preparation for complete blood count from raw blood.

    Science.gov (United States)

    Nguyen, John; Wei, Yuan; Zheng, Yi; Wang, Chen; Sun, Yu

    2015-03-21

    This paper describes a monolithic microfluidic device capable of on-chip sample preparation for both RBC and WBC measurements from whole blood. For the first time, on-chip sample processing (e.g. dilution, lysis, and filtration) and downstream single cell measurement were fully integrated to enable sample preparation and single cell analysis from whole blood on a single device. The device consists of two parallel sub-systems that perform sample processing and electrical measurements for measuring RBC and WBC parameters. The system provides a modular environment capable of handling solutions of various viscosities by adjusting the length of channels and precisely controlling mixing ratios, and features a new 'offset' filter configuration for increased duration of device operation. RBC concentration, mean corpuscular volume (MCV), cell distribution width, WBC concentration and differential are determined by electrical impedance measurement. Experimental characterization of over 100,000 cells from 10 patient blood samples validated the system's capability for performing on-chip raw blood processing and measurement.

  4. Effects of sampling rate on automated fatigue recognition in surface EMG signals

    Directory of Open Access Journals (Sweden)

    Kahl Lorenz

    2015-09-01

    Full Text Available This study investigated the effects different sampling rates may produce on the quality of muscle fatigue detection algorithms. sEMG signals were obtained from isometric contractions of the arm. Subsampled signals resulting in technically relevant sampling rates were computationally deduced from the original recordings. The spectral based fatigue recognition methods mean and median frequency as well as spectral moment ratio were included in this investigation, as well as the sample and the fuzzy approximate entropy. The resulting fatigue indices were evaluated with respect to noise and separability of different load levels. We concluded that the spectral moment ratio provides the best results in fatigue detection over a wide range of sampling rates.

  5. Rapid DNA analysis for automated processing and interpretation of low DNA content samples.

    Science.gov (United States)

    Turingan, Rosemary S; Vasantgadkar, Sameer; Palombo, Luke; Hogan, Catherine; Jiang, Hua; Tan, Eugene; Selden, Richard F

    2016-01-01

    Short tandem repeat (STR) analysis of casework samples with low DNA content include those resulting from the transfer of epithelial cells from the skin to an object (e.g., cells on a water bottle, or brim of a cap), blood spatter stains, and small bone and tissue fragments. Low DNA content (LDC) samples are important in a wide range of settings, including disaster response teams to assist in victim identification and family reunification, military operations to identify friend or foe, criminal forensics to identify suspects and exonerate the innocent, and medical examiner and coroner offices to identify missing persons. Processing LDC samples requires experienced laboratory personnel, isolated workstations, and sophisticated equipment, requires transport time, and involves complex procedures. We present a rapid DNA analysis system designed specifically to generate STR profiles from LDC samples in field-forward settings by non-technical operators. By performing STR in the field, close to the site of collection, rapid DNA analysis has the potential to increase throughput and to provide actionable information in real time. A Low DNA Content BioChipSet (LDC BCS) was developed and manufactured by injection molding. It was designed to function in the fully integrated Accelerated Nuclear DNA Equipment (ANDE) instrument previously designed for analysis of buccal swab and other high DNA content samples (Investigative Genet. 4(1):1-15, 2013). The LDC BCS performs efficient DNA purification followed by microfluidic ultrafiltration of the purified DNA, maximizing the quantity of DNA available for subsequent amplification and electrophoretic separation and detection of amplified fragments. The system demonstrates accuracy, precision, resolution, signal strength, and peak height ratios appropriate for casework analysis. The LDC rapid DNA analysis system is effective for the generation of STR profiles from a wide range of sample types. The technology broadens the range of sample

  6. 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.

  7. Development of an automated method for determination of thorium in soil samples and aerosols

    International Nuclear Information System (INIS)

    Stuart, J.E.; Robertson, R.

    1986-09-01

    Methodology for determining trace thorium levels in a variety of sample types was further developed. Thorium in filtered water samples is concentrated by ferric hydroxide precipitation followed by dissolution and co-precipitation with lanthanum fluoride. Aerosols on glass fibre, cellulose ester, or teflon filters and solid soil and sediment samples are acid digested. Subsequently thorium is concentrated by lanthanum fluoride co-precipitation. Chemical separation and measurement is then done on a Technicon AA11-C autoanalyzer, using solvent extraction into thenoyltrifuoroacetone in kerosene followed by back extraction into 2 N H NO 3 , and colourometric measurement of the thorium arsenazo III complex. Chemical yields are determined by the addition of thorium-234 tracer using gamma-ray spectrometry. The sensitivities of the methods for water, aerosol and solid samples are approximately 1.0 μg/L, 0.5 μg/g and 1.0 μg/g respectively. At thorium levels about ten times the detection limit, accuracy is estimated to be ± 10% for liquids and aerosols and ± 15% for solid samples, and precision ± 5% for all samples

  8. 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.

  9. Microfluidic devices for sample preparation and rapid detection of foodborne pathogens.

    Science.gov (United States)

    Kant, Krishna; Shahbazi, Mohammad-Ali; Dave, Vivek Priy; Ngo, Tien Anh; Chidambara, Vinayaka Aaydha; Than, Linh Quyen; Bang, Dang Duong; Wolff, Anders

    2018-03-10

    Rapid detection of foodborne pathogens at an early stage is imperative for preventing the outbreak of foodborne diseases, known as serious threats to human health. Conventional bacterial culturing methods for foodborne pathogen detection are time consuming, laborious, and with poor pathogen diagnosis competences. This has prompted researchers to call the current status of detection approaches into question and leverage new technologies for superior pathogen sensing outcomes. Novel strategies mainly rely on incorporating all the steps from sample preparation to detection in miniaturized devices for online monitoring of pathogens with high accuracy and sensitivity in a time-saving and cost effective manner. Lab on chip is a blooming area in diagnosis, which exploits different mechanical and biological techniques to detect very low concentrations of pathogens in food samples. This is achieved through streamlining the sample handling and concentrating procedures, which will subsequently reduce human errors and enhance the accuracy of the sensing methods. Integration of sample preparation techniques into these devices can effectively minimize the impact of complex food matrix on pathogen diagnosis and improve the limit of detections. Integration of pathogen capturing bio-receptors on microfluidic devices is a crucial step, which can facilitate recognition abilities in harsh chemical and physical conditions, offering a great commercial benefit to the food-manufacturing sector. This article reviews recent advances in current state-of-the-art of sample preparation and concentration from food matrices with focus on bacterial capturing methods and sensing technologies, along with their advantages and limitations when integrated into microfluidic devices for online rapid detection of pathogens in foods and food production line. Copyright © 2018. Published by Elsevier Inc.

  10. Ferromagnetic particles as a rapid and robust sample preparation for the absolute quantification of seven eicosanoids in human plasma by UHPLC-MS/MS.

    Science.gov (United States)

    Suhr, Anna Catharina; Bruegel, Mathias; Maier, Barbara; Holdt, Lesca Miriam; Kleinhempel, Alisa; Teupser, Daniel; Grimm, Stefanie H; Vogeser, Michael

    2016-06-01

    We used ferromagnetic particles as a novel technique to deproteinize plasma samples prior to quantitative UHPLC-MS/MS analysis of seven eicosanoids [thromboxane B2 (TXB2), prostaglandin E2 (PGE2), PGD2, 5-hydroxyeicosatetraenoic acid (5-HETE), 11-HETE, 12-HETE, arachidonic acid (AA)]. A combination of ferromagnetic particle enhanced deproteination and subsequent on-line solid phase extraction (on-line SPE) realized quick and convenient semi-automated sample preparation-in contrast to widely used manual SPE techniques which are rather laborious and therefore impede the investigation of AA metabolism in larger patient cohorts. Method evaluation was performed according to a protocol based on the EMA guideline for bioanalytical method validation, modified for endogenous compounds. Calibrators were prepared in ethanol. The calibration curves were found to be linear in a range of 0.1-80ngmL(-1) (TXB2, PGE2, PGD2), 0.05-40ngmL(-1) (5-HETE, 11-HETE), 0.5-400ngmL(-1) (12-HETE) and 25-9800ngmL(-1) (AA). Regarding all analytes and all quality controls, the resulting precision data (inter-assay 2.6 %-15.5 %; intra-assay 2.5 %-15.1 %, expressed as variation coefficient) as well as the accuracy results (inter-assay 93.3 %-125 %; intra-assay 91.7 %-114 %) were adequate. Further experiments addressing matrix effect, recovery and robustness, yielded also very satisfying results. As a proof of principle, the newly developed LC-MS/MS assay was employed to determine the capacity of AA metabolite release after whole blood stimulation in healthy blood donors. For this purpose, whole blood specimens of 5 healthy blood donors were analyzed at baseline and after a lipopolysaccharide (LPS) induced blood cell activation. In several baseline samples some eicosanoids levels were below the Lower Limit of Quantification. However, in the stimulated samples all chosen eicosanoids (except PGD2) could be quantified. These results, in context with those obtained in validation, demonstrate the

  11. The T-lock: automated compensation of radio-frequency induced sample heating

    International Nuclear Information System (INIS)

    Hiller, Sebastian; Arthanari, Haribabu; Wagner, Gerhard

    2009-01-01

    Modern high-field NMR spectrometers can stabilize the nominal sample temperature at a precision of less than 0.1 K. However, the actual sample temperature may differ from the nominal value by several degrees because the sample heating caused by high-power radio frequency pulses is not readily detected by the temperature sensors. Without correction, transfer of chemical shifts between different experiments causes problems in the data analysis. In principle, the temperature differences can be corrected by manual procedures but this is cumbersome and not fully reliable. Here, we introduce the concept of a 'T-lock', which automatically maintains the sample at the same reference temperature over the course of different NMR experiments. The T-lock works by continuously measuring the resonance frequency of a suitable spin and simultaneously adjusting the temperature control, thus locking the sample temperature at the reference value. For three different nuclei, 13 C, 17 O and 31 P in the compounds alanine, water, and phosphate, respectively, the T-lock accuracy was found to be <0.1 K. The use of dummy scan periods with variable lengths allows a reliable establishment of the thermal equilibrium before the acquisition of an experiment starts

  12. Automation of the radiation measuring facilities for samples in health physics - MA 9

    International Nuclear Information System (INIS)

    Martini, M.

    1980-12-01

    Routine radation measurements of samples are performed by the HMI health physics department by means of test stations for individual samples and multiple samples (using a changing equipment). The basic device of these test stations is a SCALER/TIMER system (BF 22/25, BERTHOLD Corp.). This measuring facility has been extended by a CAMAC intrumentation which incorporates an autonomous CAMAC processor (CAPRO-1, INCAA B.V.) for monitoring an automatic control of the system. The programming language is BASIC. A DECwriter (LA 34) is used for user interaction and for printing the measurement results. This report describes the features of this system and present some examples of, the dialogue with the system and the printout of data. (orig.) [de

  13. 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.

  14. Automated flow-injection method for cadmium determination with pre-concentration and reagent preparation on-line

    Directory of Open Access Journals (Sweden)

    María S. Di Nezio

    2005-02-01

    Full Text Available The spectrophotometric determination of Cd(II using a flow injection system provided with a solid-phase reactor for cadmium preconcentration and on-line reagent preparation, is described. It is based on the formation of a dithizone-Cd complex in basic medium. The calibration curve is linear between 6 and 300 µg L-1 Cd(II, with a detection limit of 5.4 µg L-1, an RSD of 3.7% (10 replicates in duplicate and a sample frequency of 11.4 h-1. The proposed method was satisfactorily applied to the determination of Cd(II in surface, well and drinking waters.

  15. Portable automation of static chamber sample collection for quantifying soil gas flux

    Science.gov (United States)

    The collection of soil gas flux using the static chamber method is labor intensive. The number of chambers that can be sampled in a given time period is limited by the spacing between chambers and the availability of trained research technicians. However, the static chamber method can limit spatial ...

  16. [Automated serial diagnosis of donor blood samples. Ergonomic and economic organization structure].

    Science.gov (United States)

    Stoll, T; Fischer-Fröhlich, C L; Mayer, G; Hanfland, P

    1990-01-01

    A comprehensive computer-aided administration-system for blood-donors is presented. Ciphered informations of barcode-labels allow the automatic and nevertheless selective pipetting of samples by pipetting-robots. Self-acting analysis-results are transferred to a host-computer in order to actualize a donor data-base.

  17. Automated sample-processing and titration system for determining uranium in nuclear materials

    International Nuclear Information System (INIS)

    Harrar, J.E.; Boyle, W.G.; Breshears, J.D.; Pomernacki, C.L.; Brand, H.R.; Kray, A.M.; Sherry, R.J.; Pastrone, J.A.

    1977-01-01

    The system is designed for accurate, precise, and selective determination of from 10 to 180 mg of uranium in 2 to 12 cm 3 of solution. Samples, standards, and their solutions are handled on a weight basis. These weights, together with their appropriate identification numbers, are stored in computer memory and are used automatically in the assay calculations after each titration. The measurement technique (controlled-current coulometry) is based on the Davies-Gray and New Brunswick Laboratory method, in which U(VI) is reduced to U(IV) in strong H 3 PO 4 , followed by titration of the U(IV) with electrogenerated V(V). Solution pretreatment and titration are automatic. The analyzer is able to process 44 samples per loading of the sample changer, at a rate of 4 to 9 samples per hour. The system includes a comprehensive fault-monitoring system that detects analytical errors, guards against abnormal conditions which might cause errors, and prevents unsafe operation. A detailed description of the system, information on the reliability of the component subsystems, and a summary of its evaluation by the New Brunswick Laboratory are presented

  18. 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

  19. Novel sample preparation method for surfactant containing suppositories: effect of micelle formation on drug recovery.

    Science.gov (United States)

    Kalmár, Éva; Ueno, Konomi; Forgó, Péter; Szakonyi, Gerda; Dombi, György

    2013-09-01

    Rectal drug delivery is currently at the focus of attention. Surfactants promote drug release from the suppository bases and enhance the formulation properties. The aim of our work was to develop a sample preparation method for HPLC analysis for a suppository base containing 95% hard fat, 2.5% Tween 20 and 2.5% Tween 60. A conventional sample preparation method did not provide successful results as the recovery of the drug failed to fulfil the validation criterion 95-105%. This was caused by the non-ionic surfactants in the suppository base incorporating some of the drug, preventing its release. As guidance for the formulation from an analytical aspect, we suggest a well defined surfactant content based on the turbidimetric determination of the CMC (critical micelle formation concentration) in the applied methanol-water solvent. Our CMC data correlate well with the results of previous studies. As regards the sample preparation procedure, a study was performed of the effects of ionic strength and pH on the drug recovery with the avoidance of degradation of the drug during the procedure. Aminophenazone and paracetamol were used as model drugs. The optimum conditions for drug release from the molten suppository base were found to be 100 mM NaCl, 20-40 mM NaOH and a 30 min ultrasonic treatment of the final sample solution. As these conditions could cause the degradation of the drugs in the solution, this was followed by NMR spectroscopy, and the results indicated that degradation did not take place. The determined CMCs were 0.08 mM for Tween 20, 0.06 mM for Tween 60 and 0.04 mM for a combined Tween 20, Tween 60 system. Copyright © 2013 Elsevier B.V. All rights reserved.

  20. Enhancing sample preparation capabilities for accelerator mass spectrometry radiocarbon and radiocalcium studies

    International Nuclear Information System (INIS)

    Taylor, R.E.

    1991-01-01

    With support provided by the LLNL Accelerator Mass Spectrometry Laboratory, the UCR Radiocarbon Laboratory continued its studies involving sample pretreatment and target preparation for both AMS radiocarbon ( 14 C) and radiocalcium ( 41 Ca) involving applications to archaeologically -- and paleoanthropologically- related samples. With regard to AMS 14 C-related studies, we have extended the development of a series of procedures which have, as their initial goal, the capability to combust several hundred microgram amounts of a chemically-pretreated organic sample and convert the resultant CO 2 to graphitic carbon which will consistently yield relatively high 13 C - ion currents and blanks which will yield, on a consistent basis, 14 C count rates at or below 0.20% modern, giving an 2 sigma age limit of >50,000 yr BP

  1. Simple and Reproducible Sample Preparation for Single-Shot Phosphoproteomics with High Sensitivity

    DEFF Research Database (Denmark)

    Jersie-Christensen, Rosa R.; Sultan, Abida; Olsen, Jesper V

    2016-01-01

    The traditional sample preparation workflow for mass spectrometry (MS)-based phosphoproteomics is time consuming and usually requires multiple steps, e.g., lysis, protein precipitation, reduction, alkylation, digestion, fractionation, and phosphopeptide enrichment. Each step can introduce chemical...... artifacts, in vitro protein and peptide modifications, and contaminations. Those often result in sample loss and affect the sensitivity, dynamic range and accuracy of the mass spectrometric analysis. Here we describe a simple and reproducible phosphoproteomics protocol, where lysis, denaturation, reduction......, and alkylation are performed in a single step, thus reducing sample loss and increasing reproducibility. Moreover, unlike standard cell lysis procedures the cell harvesting is performed at high temperatures (99 °C) and without detergents and subsequent need for protein precipitation. Phosphopeptides are enriched...

  2. Advantages of infrared transflection micro spectroscopy and paraffin-embedded sample preparation for biological studies

    Science.gov (United States)

    Yao, Jie; Li, Qian; Zhou, Bo; Wang, Dan; Wu, Rie

    2018-04-01

    Fourier-Transform Infrared micro-spectroscopy is an excellent method for biological analyses. In this paper, series metal coating films on ITO glass were prepared by the electrochemical method and the different thicknesses of paraffin embedding rat's brain tissue on the substrates were studied by IR micro-spetroscopy in attenuated total reflection (ATR) mode and transflection mode respectively. The Co-Ni-Cu alloy coating film with low cost is good reflection substrates for the IR analysis. The infrared microscopic transflection mode needs not to touch the sample at all and can get the IR spectra with higher signal to noise ratios. The Paraffin-embedding method allows tissues to be stored for a long time for re-analysis to ensure the traceability of the sample. Also it isolates the sample from the metal and avoids the interaction of biological tissue with the metals. The best thickness of the tissues is 4 μm.

  3. Sources of variability in collection and preparation of paint and lead-coating samples.

    Science.gov (United States)

    Harper, S L; Gutknecht, W F

    2001-06-01

    Chronic exposure of children to lead (Pb) can result in permanent physiological impairment. Since surfaces coated with lead-containing paints and varnishes are potential sources of exposure, it is extremely important that reliable methods for sampling and analysis be available. The sources of variability in the collection and preparation of samples were investigated to improve the performance and comparability of methods and to ensure that data generated will be adequate for its intended use. Paint samples of varying sizes (areas and masses) were collected at different locations across a variety of surfaces including metal, plaster, concrete, and wood. A variety of grinding techniques were compared. Manual mortar and pestle grinding for at least 1.5 min and mechanized grinding techniques were found to generate similar homogenous particle size distributions required for aliquots as small as 0.10 g. When 342 samples were evaluated for sample weight loss during mortar and pestle grinding, 4% had 20% or greater loss with a high of 41%. Homogenization and sub-sampling steps were found to be the principal sources of variability related to the size of the sample collected. Analysis of samples from different locations on apparently identical surfaces were found to vary by more than a factor of two both in Pb concentration (mg cm-2 or %) and areal coating density (g cm-2). Analyses of substrates were performed to determine the Pb remaining after coating removal. Levels as high as 1% Pb were found in some substrate samples, corresponding to more than 35 mg cm-2 Pb. In conclusion, these sources of variability must be considered in development and/or application of any sampling and analysis methodologies.

  4. Rapid microbial sample preparation from blood using a novel concentration device.

    Directory of Open Access Journals (Sweden)

    Anna K Boardman

    Full Text Available Appropriate care for bacteremic patients is dictated by the amount of time needed for an accurate diagnosis. However, the concentration of microbes in the blood is extremely low in these patients (1-100 CFU/mL, traditionally requiring growth (blood culture or amplification (e.g., PCR for detection. Current culture-based methods can take a minimum of two days, while faster methods like PCR require a sample free of inhibitors (i.e., blood components. Though commercial kits exist for the removal of blood from these samples, they typically capture only DNA, thereby necessitating the use of blood culture for antimicrobial testing. Here, we report a novel, scaled-up sample preparation protocol carried out in a new microbial concentration device. The process can efficiently lyse 10 mL of bacteremic blood while maintaining the microorganisms' viability, giving a 30-μL final output volume. A suite of six microorganisms (Staphylococcus aureus, Streptococcus pneumoniae, Escherichia coli, Haemophilus influenzae, Pseudomonas aeruginosa, and Candida albicans at a range of clinically relevant concentrations was tested. All of the microorganisms had recoveries greater than 55% at the highest tested concentration of 100 CFU/mL, with three of them having over 70% recovery. At the lowest tested concentration of 3 CFU/mL, two microorganisms had recoveries of ca. 40-50% while the other four gave recoveries greater than 70%. Using a Taqman assay for methicillin-sensitive S. aureus (MSSAto prove the feasibility of downstream analysis, we show that our microbial pellets are clean enough for PCR amplification. PCR testing of 56 spiked-positive and negative samples gave a specificity of 0.97 and a sensitivity of 0.96, showing that our sample preparation protocol holds great promise for the rapid diagnosis of bacteremia directly from a primary sample.

  5. Sample preparation of waste water to determine metallic contaminants by X-ray fluorescence spectroscopy

    International Nuclear Information System (INIS)

    Gonzalez Olivos, Javier.

    1987-01-01

    Trace X-ray fluorescence spectroscopy analysis in liquid samples is preceded by sample preparation, which usually consists in the precipitation of the metallic ions and concentration over a thin cellulose filter. The samples preparation of waste water by this method is not efficient, due to the great amount of organic and insoluble matter that they contain. The purpose of this work was to determine the optimal value of pH in order to adsorbe all the insoluble matter contained in a waste water sample in the activated charcoal, so that the metallic ions could be precipitated and concentrated on a thin filter and determinated by X-ray fluorescence spectroscopy. A survey about the adsorption of some ions in activated charcoal in function of the pH was made for the following: Cr 3+ , Fe 3+ , Ni 2+ , Cu 2+ , Zn 2+ , Se 2+ , Hg 2+ , and Pb 2+ . It was observed that at pH 0, the ions are not adsorbed, but Cu 2+ and Zn 2+ are adsorbed in small amount; at pH 14, the ions are adsorbed, excluding Se, which is not adsorbed at any value of pH. If a waste water sample is treated at pH 0 with activated charcoal to adsorbe the organic and insoluble matter, most of the metallic ions are not adsorbed by the activated charcoal and could be precipitated with APDC (ammonium 1-pirrolidine dithio carbamate salt) and concentrated on a thin filter. The analysis of the metallic ions contained on the filter and those adsorbed in the activated charcoal by X-ray fluorescence spectroscopy, gave the total amount of the ions in the sample. (author)

  6. Trichlorosilane and silicon tetrachloride sample preparation for determination of boron, phosphorus and arsenic microelements

    International Nuclear Information System (INIS)

    Stolyarova, I.V.; Orlova, V.A.

    1995-01-01

    The conditions of sample preparation ensuring virtually complete elimination of boron, phosphorus, and arsenic losses are elaborated. Analysis procedures are proposed that involve hydrolysis in an autoclave for exothermic reactions and/or in an open reaction reservoir on frozen twice-distilled water with complexing-agent and oxidant solutionsd applied layer-by-layer, with the possible subsequent atomic-emission, extraction-spectrophotometric, or extraction-colorimetric determination of boron, phosphorus, and arsenic. The procedures improve the accuracy and precision of the results and reduce the duration of chemical preparation due to the quantitative preconcentration of boron, phosphorus, and arsenic; they almost completely eliminate the possibility of the formation of volatile fluoride forms of these elements. 11 refs.; 3 tabs

  7. Improved sample preparation for CE-LIF analysis of plant N-glycans.

    Science.gov (United States)

    Nagels, Bieke; Santens, Francis; Weterings, Koen; Van Damme, Els J M; Callewaert, Nico

    2011-12-01

    In view of glycomics studies in plants, it is important to have sensitive tools that allow one to analyze and characterize the N-glycans present on plant proteins in different species. Earlier methods combined plant-based sample preparations with CE-LIF N-glycan analysis but suffered from background contaminations, often resulting in non-reproducible results. This publication describes a reproducible and sensitive protocol for the preparation and analysis of plant N-glycans, based on a combination of the 'in-gel release method' and N-glycan analysis on a multicapillary DNA sequencer. Our protocol makes it possible to analyze plant N-glycans starting from low amounts of plant material with highly reproducible results. The developed protocol was validated for different plant species and plant cells. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Sorbent Tube Sampling and an Automated Thermal Desorption System for Halocarbon Analysis

    Directory of Open Access Journals (Sweden)

    Md. Anwar Hossain Khan

    2009-01-01

    Full Text Available Development and deployment of the analytical sys tem, ATD-GC-ECD has been established to monitor a suite of halogenated com pounds found in the atmosphere at trace concentrations. The instrument has been used to monitor urban back ground emission flux levels in Bristol, UK as well as Yellow stone National Park, USA and an in door rain forest (Wild Walk@Bristol, UK. The newly established sorbent tube sampling system is small and easily portable and has been used for large volume sample collection from remote areas. Auto mated Thermal Desorption (ATD provides routine atmospheric measurements with out cryogenic pre-concentration. The instrument provides good precision where the detection limit was _T_n3 pptv for the species of interest and the reproducibility was within 4% for all of the selected halocarbons. The results from two field experiments have also pro vided insight about natural missing sources of some ozone depleting halocarbons.

  9. Analysis of polycyclic aromatic hydrocarbons in soil: minimizing sample pretreatment using automated Soxhlet with ethyl acetate as extraction solvent.

    Science.gov (United States)

    Szolar, Oliver H J; Rost, Helmut; Braun, Rudolf; Loibner, Andreas P

    2002-05-15

    A simplified sample pretreatment method for industrially PAH-contaminated soils applying automated Soxhlet (Soxtherm) with ethyl acetate as extraction solvent is presented. Laborious pretreatment steps such as drying of samples, cleanup of crude extracts, and solvent exchange were allowed to be bypassed without notable performance impact. Moisture of the soil samples did not significantly influence recoveries of PAHs at a wide range of water content for the newly developed method. However, the opposite was true for the standard procedure using the more apolar 1:1 (v/v) n-hexane/acetone solvent mixture including postextraction treatments recommended by the U.S. EPA. Moreover, ethyl acetate crude extracts did not appreciably effect the chromatographic performance (HPLC-(3D)FLD), which was confirmed by a comparison of the purity of PAH spectra from both pretreatment methods. Up to 20% (v/v) in acetonitrile, ethyl acetate proved to be fully compatible with the mobile phase of the HPLC whereas the same concentration of n-hexane/acetone in acetonitrile resulted in significant retention time shifts. The newly developed pretreatment method was applied to three historically contaminated soils from different sources with extraction efficiencies not being significantly different compared to the standard procedure. Finally, the certified reference soil CRM 524 was subjected to the simplified procedure resulting in quantitative recoveries (>92%) for all PAHs analyzed.

  10. 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.

  11. 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.

  12. Advancing haemostasis automation--successful implementation of robotic centrifugation and sample processing in a tertiary service hospital.

    Science.gov (United States)

    Sédille-Mostafaie, Nazanin; Engler, Hanna; Lutz, Susanne; Korte, Wolfgang

    2013-06-01

    Laboratories today face increasing pressure to automate operations due to increasing workloads and the need to reduce expenditure. Few studies to date have focussed on the laboratory automation of preanalytical coagulation specimen processing. In the present study, we examined whether a clinical chemistry automation protocol meets the preanalytical requirements for the analyses of coagulation. During the implementation of laboratory automation, we began to operate a pre- and postanalytical automation system. The preanalytical unit processes blood specimens for chemistry, immunology and coagulation by automated specimen processing. As the production of platelet-poor plasma is highly dependent on optimal centrifugation, we examined specimen handling under different centrifugation conditions in order to produce optimal platelet deficient plasma specimens. To this end, manually processed models centrifuged at 1500 g for 5 and 20 min were compared to an automated centrifugation model at 3000 g for 7 min. For analytical assays that are performed frequently enough to be targets for full automation, Passing-Bablok regression analysis showed close agreement between different centrifugation methods, with a correlation coefficient between 0.98 and 0.99 and a bias between -5% and +6%. For seldom performed assays that do not mandate full automation, the Passing-Bablok regression analysis showed acceptable to poor agreement between different centrifugation methods. A full automation solution is suitable and can be recommended for frequent haemostasis testing.

  13. microPREP: a new laser tool for high-volume sample preparation

    Science.gov (United States)

    Wagner, Uwe; Petsch, Tino; Krause, Michael; Höche, Thomas

    2016-03-01

    Over the past fifty year, lasers have perpetuated to find new, often groundbreaking applications in science and technology. The most important features of lasers are that photons are inherently free of elemental contamination, extremely high energy densities can be focused in very small areas and the laser beam can be precisely positioned using deflection mirrors. By reducing pulse lengths from a few nanoseconds down to the picosecond or femtosecond range, material's ablation is becoming increasingly "athermal", i.e. structure damage by local heating is reduced to well below a few microns. In view of these outstanding characteristics of lasers as tools for micromachining, it is very surprising that sample preparation for microstructure diagnostics so far hasn't made use of laser technology. microPREPTM, the all-new, patented laser-micromachining tool developed by 3D-Micromac is the first instrument to make fast, clean, and efficient laser ablation available for the preparation of samples for microstructure diagnostics. Exemplified for a sample to be investigated by transmission electron microscopy (TEM) and following a three-stage approach, a supporting basic structure is cut from the feedstock first. Second, the supported structure is thinned down to a few micron of residual thickness and third, the supported and thinned structure is polished using an ion broad beam. Illustrated by numerous examples, it is shown that this technology is ready to be applied on different areas of microstructure diagnostics and has very high potential for failure diagnostics.

  14. Sample preparation for liquid chromatographic analysis of phytochemicals in biological fluids.

    Science.gov (United States)

    Oh, Ju-Hee; Lee, Young-Joo

    2014-01-01

    Natural products have been used traditionally for the treatment and prevention of diseases for thousands of years and are nowadays consumed as dietary supplements and herbal medicine. To ensure the safe and effective use of these herbal products, information about bioavailability of active compounds in plasma or target tissues should be provided via validated analytical methods combined with appropriate sampling methods. To provide comprehensive and abridged information about sample preparation methods for the quantification of phytochemicals in biological samples using liquid chromatography analysis. Sample pre-treatment procedures used in analytical methods for in vivo pharmacokinetic studies of natural compounds or herbal medicines were reviewed. These were categorised according to the biological matrices (plasma, bile, urine, faeces and tissues) and sample clean-up processes (protein precipitation, liquid-liquid extraction and solid-phase extraction). Although various kinds of sample pre-treatment methods have been developed, liquid-liquid extraction is still widely used and solid-phase extraction is becoming increasingly popular because of its efficiency for extensive clean up of complex matrix samples. However, protein precipitation is still favoured due to its simplicity. Sample treatment for phytochemical analysis in biological fluids is an indispensable and critical step to obtain high quality results. This step could dominate the overall analytical process because both the duration of the process as well as the reliability of the data depend in large part on its efficiency. Thus, special attention should be given to the choice of a proper sample treatment method that targets analytes and their biomatrix. Copyright © 2013 John Wiley & Sons, Ltd.

  15. Error baseline rates of five sample preparation methods used to characterize RNA virus populations

    Science.gov (United States)

    Kugelman, Jeffrey R.; Wiley, Michael R.; Nagle, Elyse R.; Reyes, Daniel; Pfeffer, Brad P.; Kuhn, Jens H.; Sanchez-Lockhart, Mariano; Palacios, Gustavo F.

    2017-01-01

    Individual RNA viruses typically occur as populations of genomes that differ slightly from each other due to mutations introduced by the error-prone viral polymerase. Understanding the variability of RNA virus genome populations is critical for understanding virus evolution because individual mutant genomes may gain evolutionary selective advantages and give rise to dominant subpopulations, possibly even leading to the emergence of viruses resistant to medical countermeasures. Reverse transcription of virus genome populations followed by next-generation sequencing is the only available method to characterize variation for RNA viruses. However, both steps may lead to the introduction of artificial mutations, thereby skewing the data. To better understand how such errors are introduced during sample preparation, we determined and compared error baseline rates of five different sample preparation methods by analyzing in vitro transcribed Ebola virus RNA from an artificial plasmid-based system. These methods included: shotgun sequencing from plasmid DNA or in vitro transcribed RNA as a basic “no amplification” method, amplicon sequencing from the plasmid DNA or in vitro transcribed RNA as a “targeted” amplification method, sequence-independent single-primer amplification (SISPA) as a “random” amplification method, rolling circle reverse transcription sequencing (CirSeq) as an advanced “no amplification” method, and Illumina TruSeq RNA Access as a “targeted” enrichment method. The measured error frequencies indicate that RNA Access offers the best tradeoff between sensitivity and sample preparation error (1.4−5) of all compared methods. PMID:28182717

  16. A novel, fully-automated, chemiluminescent assay for the detection of 1,25-dihydroxyvitamin D in biological samples.

    Science.gov (United States)

    Valcour, Andre; Zierold, Claudia; Podgorski, Angela L; Olson, Gregory T; Wall, John V; DeLuca, Hector F; Bonelli, Fabrizio

    2016-11-01

    1,25-Dihydroxyvitamin D (1,25-(OH) 2 D), the hormonal form of vitamin D, is difficult to measure because of its low circulating levels (pg/mL), and similarity to more abundant metabolites. Here a fully-automated chemiluminescent assay that accurately and precisely measures 1,25-(OH) 2 D is described. The novel 1,25-(OH) 2 D assay was conceived based on four pillars: (1) the VDR's ligand binding domain (LBD) as a capture molecule; (2) reaction conditions wherein 1,25-(OH) 2 D favors binding to LBD vs. the vitamin D binding protein; (3) exploitation of liganded-LBD's conformational change; (4) a monoclonal antibody specific to liganded-LBD. This specific, conformational, sandwich approach, unique for automated measurement of haptens, is superior to more cumbersome, conventional competitive formats. Accuracy of the 1,25-(OH) 2 D assay was corroborated by its alignment against LC-MS/MS with fit Deming regression equations of y=0.98x + 1.93 (r=0.92), and y=1.07x+3.77 (r=0.94) for different methods from Endocrine Sciences, Laboratory Corporation of America ® and the University of Washington, respectively. Good analytical precision was manifested by its low estimated limit of quantitation (1.57pg/mL), average intra-assay imprecision (3.5%CV; range 1.1-4.7%), and average inter-assay imprecision (4.5%CV; range 3.4-7.2%). Expected and measured recovery values were congruent (93.4% mean). The novel 1,25-(OH) 2 D method exhibited excellent correlation with well validated LC-MS/MS assays from two laboratories. Significantly, its 65min turn-around time is quicker, and sample volume smaller (75μl) than current methods. Copyright © 2015 The Authors. Published by Elsevier Ltd.. All rights reserved.

  17. Automated Image Sampling and Classification Can Be Used to Explore Perceived Naturalness of Urban Spaces.

    Directory of Open Access Journals (Sweden)

    Roger Hyam

    Full Text Available The psychological restorative effects of exposure to nature are well established and extend to just viewing of images of nature. A previous study has shown that Perceived Naturalness (PN of images correlates with their restorative value. This study tests whether it is possible to detect degree of PN of images using an image classifier. It takes images that have been scored by humans for PN (including a subset that have been assessed for restorative value and passes them through the Google Vision API image classification service. The resulting labels are assigned to broad semantic classes to create a Calculated Semantic Naturalness (CSN metric for each image. It was found that CSN correlates with PN. CSN was then calculated for a geospatial sampling of Google Street View images across the city of Edinburgh. CSN was found to correlate with PN in this sample also indicating the technique may be useful in large scale studies. Because CSN correlates with PN which correlates with restorativeness it is suggested that CSN or a similar measure may be useful in automatically detecting restorative images and locations. In an exploratory aside CSN was not found to correlate with an indicator of socioeconomic deprivation.

  18. Spectrophotometric Determination of Lamotrigine in Pharmaceutical Preparations and Urine Samples Using Bromothymol Blue and Bromophenol Blue

    International Nuclear Information System (INIS)

    Najib, F.M.; Aziz, K.H.H.

    2013-01-01

    Two simple and sensitive spectrophotometric methods have been developed for the determination of the antiepileptic drug lamotrigine (LMT) in pharmaceutical preparations and urine samples. The methods are based on the interaction of LMT with two sulphonphthalein dyes, namely, bromothymol blue (BTB) and bromophenol blue (BPB) in dichloromethane (DCM) medium to form stable and yellow-colored ion-pairs with λ max 410 and 413 nm respectively. The ion-pair LMT-BPB has been extracted from aqueous solutions at pH 3.25±0.25 using DCM; while LMT-BTB ion-pair was directly prepared in DCM. Interferences from the compounds of the urine samples, in case of LMT-BPB were removed using a suppressing solution (S.S.) prepared from the salts of the interfering ions. In LMT-BTB method, the urine of normal person not taking LMT, was used as a blank to remove the effect of interferences. Under optimum conditions, the calibration curve of LMT-BTB was linear over the range of 1-12 μg.ml -1 , ε=1.97x10 4 L.mole -1 .cm -1 , r 2 = 0.9983, and D.L of 0.13 μg.ml -1 . The corresponding values for (LMT-BPB) ion-pair were 0.5-12 μg.ml -1 linear range, ε=1.92x10 4 , r 2 = 0.9980, and D.L= 0.24 μg.ml -1 . The stoichiometry of the ion-pairs were found to be 1:1, based on Jobs, mole ratio and slope ratio methods. The recoveries (%R) for both methods were in the range of 97-101.8 % and 95-97.1 % with RSD≤1.68 and 3.1 % respectively. For LMT- spiked urine samples, the recoveries were 98.5-106.6 % with RSD≤1.66 %. Interferences from phenobarbital and carbamazepine were in the range of 25-40 folds. Statistical comparison of the results with a published method using F and t-tests showed no significant differences between each of the two methods and the reported one at 95 % confidence level. A standard addition method, gave high accuracy with LMT-BPB method. The proposed methods were successfully applied for the determination of LMT in pharmaceutical preparation and urine samples. (author)

  19. Preparation of quality control samples in radioimmunoassay for thyroid stimulating hormone (TSH)

    International Nuclear Information System (INIS)

    Ali, O.M.

    2006-03-01

    To days, the radioimmunoassay is becomes the best technique to analysis different concentrations of substance, especially in medical and research laboratories. Although the specificity of RIA techniques, the quality controls must takes place to give good results as possible. In this dissertation i prepared quality control samples of thyroid stimulating hormone (TSH), to use it in RIA techniques and to control the reliability results of those laboratories which used these methods. We used China production kits of RIA method to determine the level of hormone (low-normal-high) concentration. Statistical parameters were used to drown the control chart of the mean to these data.(Author)

  20. Sampling theory and automated simulations for vertical sections, applied to human brain.

    Science.gov (United States)

    Cruz-Orive, L M; Gelšvartas, J; Roberts, N

    2014-02-01

    In recent years, there have been substantial developments in both magnetic resonance imaging techniques and automatic image analysis software. The purpose of this paper is to develop stereological image sampling theory (i.e. unbiased sampling rules) that can be used by image analysts for estimating geometric quantities such as surface area and volume, and to illustrate its implementation. The methods will ideally be applied automatically on segmented, properly sampled 2D images - although convenient manual application is always an option - and they are of wide applicability in many disciplines. In particular, the vertical sections design to estimate surface area is described in detail and applied to estimate the area of the pial surface and of the boundary between cortex and underlying white matter (i.e. subcortical surface area). For completeness, cortical volume and mean cortical thickness are also estimated. The aforementioned surfaces were triangulated in 3D with the aid of FreeSurfer software, which provided accurate surface area measures that served as gold standards. Furthermore, a software was developed to produce digitized trace curves of the triangulated target surfaces automatically from virtual sections. From such traces, a new method (called the 'lambda method') is presented to estimate surface area automatically. In addition, with the new software, intersections could be counted automatically between the relevant surface traces and a cycloid test grid for the classical design. This capability, together with the aforementioned gold standard, enabled us to thoroughly check the performance and the variability of the different estimators by Monte Carlo simulations for studying the human brain. In particular, new methods are offered to split the total error variance into the orientations, sectioning and cycloid components. The latter prediction was hitherto unavailable--one is proposed here and checked by way of simulations on a given set of digitized

  1. Effect of sample preparation method on quantification of polymorphs using PXRD.

    Science.gov (United States)

    Alam, Shahnwaz; Patel, Sarsvatkumar; Bansal, Arvind Kumar

    2010-01-01

    The purpose of this study was to improve the sensitivity and accuracy of quantitative analysis of polymorphic mixtures. Various techniques such as hand grinding and mixing (in mortar and pestle), air jet milling and ball milling for micronization of particle and mixing were used to prepare binary mixtures. Using these techniques, mixtures of form I and form II of clopidogrel bisulphate were prepared in various proportions from 0-5% w/w of form I in form II and subjected to x-ray powder diffraction analysis. In order to obtain good resolution in minimum time, step time and step size were varied to optimize scan rate. Among the six combinations, step size of 0.05 degrees with step time of 5 s demonstrated identification of maximum characteristic peaks of form I in form II. Data obtained from samples prepared using both grinding and mixing in ball mill showed good analytical sensitivity and accuracy compared to other methods. Powder x-ray diffraction method was reproducible, precise with LOD of 0.29% and LOQ of 0.91%. Validation results showed excellent correlation between actual and predicted concentration with R2 > 0.9999.

  2. 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.

  3. Improved sample preparation method for environmental plutonium analysis by ICP-SFMS and alpha-spectrometry

    International Nuclear Information System (INIS)

    Varga, Z.; Stefanka, Z.; Suranyi, G.; Vajda, N.

    2007-01-01

    A rapid and simple sample preparation method for plutonium determination in environmental samples by inductively coupled plasma sector field mass spectrometry (ICP-SFMS) and alpha-spectrometry is described. The developed procedure involves a selective CaF 2 co-precipitation for preconcentration followed by extraction chromatographic separation. The proposed method effectively eliminates the possible interferences in mass spectrometric analysis and also removes interfering radionuclides that may disturb alpha-spectrometric measurement. For 239 Pu, 240 Pu and 241 Pu limits of detection of 9.0 fg x g -1 (0.021 mBq), 1.7 fg x g -1 (0.014 mBq) and 3.1 fg x g -1 (11.9 mBq) were achieved by ICP-SFMS, respectively, and 0.02 mBq by alpha-spectrometry. Results of certified reference materials agreed well with the recommended values. (author)

  4. 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

    loading capacity. MIPs have been intensively employed in classical solid-phase extraction and solid-phase microextraction. More recently, MIPs have been combined with magnetic bead extraction, which greatly simplifies sample handling procedures. Studies have consistently shown that MIPs can effectively...... minimize complex food matrix effects, and improve recoveries and detection limits. In addition to sample preparation, MIPs have also been viewed as promising alternatives to bio-receptors due to the inherent molecular recognition abilities and the high stability in harsh chemical and physical conditions....... MIPs have been utilized as receptors in biosensing platforms such as electrochemical, optical and mass biosensors to detect various analytes in food. In this review, we will discuss the current state-of-the-art of MIP synthesis and applications in the context of food analysis. We will highlight...

  5. Determination of oxygen in uranium carbide: importance of sample preparation method

    International Nuclear Information System (INIS)

    Handa, Muneo; Maeda, Atsushi; Yahata, Taneaki; Hoshino, Akira.

    1979-01-01

    The determination of oxygen in uranium carbide with new sample preparation method is described. To prevent the oxygen contamination of chemically reactive uranium carbide, it is sealed air-tight in a platinum capsule in an argon-atmosphere glove box containing less than 1 ppm of both oxygen and water vapor. The capsule is the transferred into an air-atmosphere glove box, and the oxygen determination is made by inert gas fusion-coulometry. Oxygen analysis by this method was made for the analyzed uranium carbide sample and about half value was obtained. The reason may be in the difference of the procedure of determination described. The oxygen contamination is kept lower by the method, and the determination of oxygen in carbide fuel can be performed precisely. (author)

  6. Campylobacter in Broiler Chicken and Broiler Meat in Sri Lanka: Influence of Semi-Automated vs. Wet Market Processing on Campylobacter Contamination of Broiler Neck Skin Samples

    Directory of Open Access Journals (Sweden)

    Kottawattage S. A. Kottawatta

    2017-11-01

    Full Text Available Broiler meat can become contaminated with Campylobacter of intestinal origin during processing. The present study aimed to identify the prevalence of Campylobacter in broiler flocks and meat contamination at retail shops, and determine the influence of semi-automated and wet market processing on Campylobacter contamination of neck skin samples. Samples were collected from semi-automated plants (n = 102 and wet markets (n = 25. From each batch of broilers, pooled caecal samples and neck skin samples were tested for Campylobacter. Broiler meat purchased from retail outlets (n = 37 was also tested. The prevalence of Campylobacter colonized broiler flocks was 67%. The contamination of meat at retail was 59%. Both semi-automated and wet market processing resulted to contaminate the broiler neck skins to the levels of 27.4% and 48%, respectively. When Campylobacter-free broiler flocks were processed in semi-automated facilities 15% (5/33 of neck skin samples became contaminated by the end of processing whereas 25% (2/8 became contaminated after wet market processing. Characterization of isolates revealed a higher proportion of C. coli compared to C. jejuni. Higher proportions of isolates were resistant to important antimicrobials. This study shows the importance of Campylobacter in poultry industry in Sri Lanka and the need for controlling antimicrobial resistance.

  7. Campylobacter in Broiler Chicken and Broiler Meat in Sri Lanka: Influence of Semi-Automated vs. Wet Market Processing on Campylobacter Contamination of Broiler Neck Skin Samples.

    Science.gov (United States)

    Kottawatta, Kottawattage S A; Van Bergen, Marcel A P; Abeynayake, Preeni; Wagenaar, Jaap A; Veldman, Kees T; Kalupahana, Ruwani S

    2017-11-29

    Broiler meat can become contaminated with Campylobacter of intestinal origin during processing. The present study aimed to identify the prevalence of Campylobacter in broiler flocks and meat contamination at retail shops, and determine the influence of semi-automated and wet market processing on Campylobacter contamination of neck skin samples. Samples were collected from semi-automated plants ( n = 102) and wet markets ( n = 25). From each batch of broilers, pooled caecal samples and neck skin samples were tested for Campylobacter . Broiler meat purchased from retail outlets ( n = 37) was also tested. The prevalence of Campylobacter colonized broiler flocks was 67%. The contamination of meat at retail was 59%. Both semi-automated and wet market processing resulted to contaminate the broiler neck skins to the levels of 27.4% and 48%, respectively. When Campylobacter -free broiler flocks were processed in semi-automated facilities 15% (5/33) of neck skin samples became contaminated by the end of processing whereas 25% (2/8) became contaminated after wet market processing. Characterization of isolates revealed a higher proportion of C. coli compared to C. jejuni . Higher proportions of isolates were resistant to important antimicrobials. This study shows the importance of Campylobacter in poultry industry in Sri Lanka and the need for controlling antimicrobial resistance.

  8. Campylobacter in Broiler Chicken and Broiler Meat in Sri Lanka: Influence of Semi-Automated vs. Wet Market Processing on Campylobacter Contamination of Broiler Neck Skin Samples

    Science.gov (United States)

    Kottawatta, Kottawattage S. A.; Van Bergen, Marcel A. P.; Abeynayake, Preeni; Wagenaar, Jaap A.; Veldman, Kees T.; Kalupahana, Ruwani S.

    2017-01-01

    Broiler meat can become contaminated with Campylobacter of intestinal origin during processing. The present study aimed to identify the prevalence of Campylobacter in broiler flocks and meat contamination at retail shops, and determine the influence of semi-automated and wet market processing on Campylobacter contamination of neck skin samples. Samples were collected from semi-automated plants (n = 102) and wet markets (n = 25). From each batch of broilers, pooled caecal samples and neck skin samples were tested for Campylobacter. Broiler meat purchased from retail outlets (n = 37) was also tested. The prevalence of Campylobacter colonized broiler flocks was 67%. The contamination of meat at retail was 59%. Both semi-automated and wet market processing resulted to contaminate the broiler neck skins to the levels of 27.4% and 48%, respectively. When Campylobacter-free broiler flocks were processed in semi-automated facilities 15% (5/33) of neck skin samples became contaminated by the end of processing whereas 25% (2/8) became contaminated after wet market processing. Characterization of isolates revealed a higher proportion of C. coli compared to C. jejuni. Higher proportions of isolates were resistant to important antimicrobials. This study shows the importance of Campylobacter in poultry industry in Sri Lanka and the need for controlling antimicrobial resistance. PMID:29186018

  9. The Upgrade Programme for the Structural Biology beamlines at the European Synchrotron Radiation Facility – High throughput sample evaluation and automation

    International Nuclear Information System (INIS)

    Theveneau, P; Baker, R; Barrett, R; Beteva, A; Bowler, M W; Carpentier, P; Caserotto, H; Sanctis, D de; Dobias, F; Flot, D; Guijarro, M; Giraud, T; Lentini, M; Leonard, G A; Mattenet, M; McSweeney, S M; Morawe, C; Nurizzo, D; McCarthy, A A; Nanao, M

    2013-01-01

    Automation and advances in technology are the key elements in addressing the steadily increasing complexity of Macromolecular Crystallography (MX) experiments. Much of this complexity is due to the inter-and intra-crystal heterogeneity in diffraction quality often observed for crystals of multi-component macromolecular assemblies or membrane proteins. Such heterogeneity makes high-throughput sample evaluation an important and necessary tool for increasing the chances of a successful structure determination. The introduction at the ESRF of automatic sample changers in 2005 dramatically increased the number of samples that were tested for diffraction quality. This 'first generation' of automation, coupled with advances in software aimed at optimising data collection strategies in MX, resulted in a three-fold increase in the number of crystal structures elucidated per year using data collected at the ESRF. In addition, sample evaluation can be further complemented using small angle scattering experiments on the newly constructed bioSAXS facility on BM29 and the micro-spectroscopy facility (ID29S). The construction of a second generation of automated facilities on the MASSIF (Massively Automated Sample Screening Integrated Facility) beam lines will build on these advances and should provide a paradigm shift in how MX experiments are carried out which will benefit the entire Structural Biology community.

  10. 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.

  11. 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.

  12. Impact of automated dispensing cabinets on medication selection and preparation error rates in an emergency department: a prospective and direct observational before-and-after study.

    Science.gov (United States)

    Fanning, Laura; Jones, Nick; Manias, Elizabeth

    2016-04-01

    The implementation of automated dispensing cabinets (ADCs) in healthcare facilities appears to be increasing, in particular within Australian hospital emergency departments (EDs). While the investment in ADCs is on the increase, no studies have specifically investigated the impacts of ADCs on medication selection and preparation error rates in EDs. Our aim was to assess the impact of ADCs on medication selection and preparation error rates in an ED of a tertiary teaching hospital. Pre intervention and post intervention study involving direct observations of nurses completing medication selection and preparation activities before and after the implementation of ADCs in the original and new emergency departments within a 377-bed tertiary teaching hospital in Australia. Medication selection and preparation error rates were calculated and compared between these two periods. Secondary end points included the impact on medication error type and severity. A total of 2087 medication selection and preparations were observed among 808 patients pre and post intervention. Implementation of ADCs in the new ED resulted in a 64.7% (1.96% versus 0.69%, respectively, P = 0.017) reduction in medication selection and preparation errors. All medication error types were reduced in the post intervention study period. There was an insignificant impact on medication error severity as all errors detected were categorised as minor. The implementation of ADCs could reduce medication selection and preparation errors and improve medication safety in an ED setting. © 2015 John Wiley & Sons, Ltd.

  13. Evaluation of sample preparation methods for water activity determination in jerky and kippered beef: a research note.

    Science.gov (United States)

    Harper, N M; Getty, K J K; Boyle, E A E

    2010-10-01

    Commercially available packaged whole muscle beef jerky, chopped and formed beef jerky, and kippered beef steak were obtained from retail stores to determine the effect of two sample preparation methods on water activity (a(w)). Intact samples were prepared by cutting product into a hexagonal shape with a 3.2 cm diameter. Diced samples were prepared by cutting the product into 0.4 x 0.4 cm squares. Whole muscle jerky a(w) was higher (0.016 units; P0.05) in a(w) levels between the two preparation methods for chopped and formed jerky or kippered beef steak. An intact sample preparation method is recommended for a(w) determination of whole muscle jerky to obtain a more conservative value, especially if a(w) is near the margin of safety. Copyright (c) 2010 The American Meat Science Association. Published by Elsevier Ltd. All rights reserved.

  14. Methodology for sample preparation and size measurement of commercial ZnO nanoparticles

    Directory of Open Access Journals (Sweden)

    Pei-Jia Lu

    2018-04-01

    Full Text Available This study discusses the strategies on sample preparation to acquire images with sufficient quality for size characterization by scanning electron microscope (SEM using two commercial ZnO nanoparticles of different surface properties as a demonstration. The central idea is that micrometer sized aggregates of ZnO in powdered forms need to firstly be broken down to nanosized particles through an appropriate process to generate nanoparticle dispersion before being deposited on a flat surface for SEM observation. Analytical tools such as contact angle, dynamic light scattering and zeta potential have been utilized to optimize the procedure for sample preparation and to check the quality of the results. Meanwhile, measurements of zeta potential values on flat surfaces also provide critical information and save lots of time and efforts in selection of suitable substrate for particles of different properties to be attracted and kept on the surface without further aggregation. This simple, low-cost methodology can be generally applied on size characterization of commercial ZnO nanoparticles with limited information from vendors. Keywords: Zinc oxide, Nanoparticles, Methodology

  15. Effect of sample preparation on components and liver toxicity of Polygonum multiflorum.

    Science.gov (United States)

    Lv, G P; Meng, L Z; Han, D Q; Li, H Y; Zhao, J; Li, S P

    2015-05-10

    It was shown that different extracts had significant differences in the toxicity of Polygonum multiflorum. In this study, the effect of sample preparation on components and liver toxicity of different extracts from P. multiflorum were determined. Hepatoxic components were discovered based on biomembrane extraction. Comparative chemistry and toxicology between ethanol and water extracts were also performed. The results showed that ethanol extract had much stronger hepatotoxicity, the content of emodin-8-O-β-d-glucopyranoside, physcion-8-O-β-d-glucopyranoside, emodin and physcion was significantly higher in ethanol extract than in water extract, while the human hepatocytes extraction showed that 2,3,5,4'-tetrahydroxystilbene-2-O-β-d-glucopyranoside, emodin-8-O-β-d-glucopyranoside, physcion-8-O-β-d-glucopyranoside, emodin and physcion had interaction with human hepatocytes. The hepatotoxic effect of these components was investigated on human hepatocytes LO2 cells and emodin-8-O-β-d-glucopyranoside, physcion-8-O-β-d-glucopyranoside, emodin and physcion were finally confirmed to be, at least partial, hepatotoxic components. The results showed that sample preparation has significant effect on components in extracts of P. multiflorum especially the components related to hepatotoxicity. Water extract, the conventional administration form of Chinese herbs, is prefer for phytotherapy before well understanding their chemistry and biological activities. Copyright © 2015 Elsevier B.V. All rights reserved.

  16. Preparation and evaluation of a novel molecularly imprinted polymer coating for selective extraction of indomethacin from biological samples by electrochemically controlled in-tube solid phase microextraction

    Energy Technology Data Exchange (ETDEWEB)

    Asiabi, Hamid [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Yamini, Yadollah, E-mail: yyamini@modares.ac.ir [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Seidi, Shahram; Ghahramanifard, Fazel [Department of Analytical Chemistry, Faculty of Chemistry, K.N. Toosi University of Technology, Tehran (Iran, Islamic Republic of)

    2016-03-24

    In the present work, an automated on-line electrochemically controlled in-tube solid-phase microextraction (EC-in-tube SPME) coupled with HPLC-UV was developed for the selective extraction and preconcentration of indomethacin as a model analyte in biological samples. Applying an electrical potential can improve the extraction efficiency and provide more convenient manipulation of different properties of the extraction system including selectivity, clean-up, rate, and efficiency. For more enhancement of the selectivity and applicability of this method, a novel molecularly imprinted polymer coated tube was prepared and applied for extraction of indomethacin. For this purpose, nanostructured copolymer coating consisting of polypyrrole doped with ethylene glycol dimethacrylate was prepared on the inner surface of a stainless-steel tube by electrochemical synthesis. The characteristics and application of the tubes were investigated. Electron microscopy provided a cross linked porous surface and the average thickness of the MIP coating was 45 μm. Compared with the non-imprinte