WorldWideScience

Sample records for automated sample preparation

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

    Science.gov (United States)

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

    2016-04-01

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

  2. Development of automated preparation system for isotopocule analysis of N2O in various air samples

    Science.gov (United States)

    Toyoda, Sakae; Yoshida, Naohiro

    2016-05-01

    Nitrous oxide (N2O), an increasingly abundant greenhouse gas in the atmosphere, is the most important stratospheric ozone-depleting gas of this century. Natural abundance ratios of isotopocules of N2O, NNO molecules substituted with stable isotopes of nitrogen and oxygen, are a promising index of various sources or production pathways of N2O and of its sink or decomposition pathways. Several automated methods have been reported to improve the analytical precision for the isotopocule ratio of atmospheric N2O and to reduce the labor necessary for complicated sample preparation procedures related to mass spectrometric analysis. However, no method accommodates flask samples with limited volume or pressure. Here we present an automated preconcentration system which offers flexibility with respect to the available gas volume, pressure, and N2O concentration. The shortest processing time for a single analysis of typical atmospheric sample is 40 min. Precision values of isotopocule ratio analysis are < 0.1 ‰ for δ15Nbulk (average abundances of 14N15N16O and 15N14N16O relative to 14N14N16O), < 0.2 ‰ for δ18O (relative abundance of 14N14N18O), and < 0.5 ‰ for site preference (SP; difference between relative abundance of 14N15N16O and 15N14N16O). This precision is comparable to that of other automated systems, but better than that of our previously reported manual measurement system.

  3. Fast detection of Noroviruses using a real-time PCR assay and automated sample preparation

    Directory of Open Access Journals (Sweden)

    Schmid Michael

    2004-06-01

    Full Text Available Abstract Background Noroviruses (NoV have become one of the most commonly reported causative agents of large outbreaks of non-bacterial acute gastroenteritis worldwide as well as sporadic gastroenteritis in the community. Currently, reverse transcriptase polymerase chain reaction (RT-PCR assays have been implemented in NoV diagnosis, but improvements that simplify and standardize sample preparation, amplification, and detection will be further needed. The combination of automated sample preparation and real-time PCR offers such refinements. Methods We have designed a new real-time RT-PCR assay on the LightCycler (LC with SYBR Green detection and melting curve analysis (Tm to detect NoV RNA in patient stool samples. The performance of the real-time PCR assay was compared with that obtained in parallel with a commercially available enzyme immunoassay (ELISA for antigen detection by testing a panel of 52 stool samples. Additionally, in a collaborative study with the Baden-Wuerttemberg State Health office, Stuttgart (Germany the real-time PCR results were blindly assessed using a previously well-established nested PCR (nPCR as the reference method, since PCR-based techniques are now considered as the "gold standard" for NoV detection in stool specimens. Results Analysis of 52 clinical stool samples by real-time PCR yielded results that were consistent with reference nPCR results, while marked differences between the two PCR-based methods and antigen ELISA were observed. Our results indicate that PCR-based procedures are more sensitive and specific than antigen ELISA for detecting NoV in stool specimens. Conclusions The combination of automated sample preparation and real-time PCR provided reliable diagnostic results in less time than conventional RT-PCR assays. These benefits make it a valuable tool for routine laboratory practice especially in terms of rapid and appropriate outbreak-control measures in health-care facilities and other settings.

  4. Two Methods for High-Throughput NGS Template Preparation for Small and Degraded Clinical Samples Without Automation

    OpenAIRE

    Kamberov, E.; Tesmer, T.; Mastronardi, M.; Langmore, John

    2012-01-01

    Clinical samples are difficult to prepare for NGS, because of the small amounts or degraded states of formalin-fixed tissue, plasma, urine, and single-cell DNA. Conventional whole genome amplification methods are too biased for NGS applications, and the existing NGS preparation kits require intermediate purifications and excessive time to prepare hundreds of samples in a day without expensive automation. We have tested two 96-well manual methods to make NGS templates from FFPE tissue, plasma,...

  5. Automated sample preparation and analysis using a sequential-injection-capillary electrophoresis (SI-CE) interface.

    Science.gov (United States)

    Kulka, Stephan; Quintás, Guillermo; Lendl, Bernhard

    2006-06-01

    A fully automated sequential-injection-capillary electrophoresis (SI-CE) system was developed using commercially available components as the syringe pump, the selection and injection valves and the high voltage power supply. The interface connecting the SI with the CE unit consisted of two T-pieces, where the capillary was inserted in one T-piece and a Pt electrode in the other (grounded) T-piece. By pressurising the whole system using a syringe pump, hydrodynamic injection was feasible. For characterisation, the system was applied to a mixture of adenosine and adenosine monophosphate at different concentrations. The calibration curve obtained gave a detection limit of 0.5 microg g(-1) (correlation coefficient of 0.997). The reproducibility of the injection was also assessed, resulting in a RSD value (5 injections) of 5.4%. The total time of analysis, from injection, conditioning and separation to cleaning the capillary again was 15 minutes. In another application, employing the full power of the automated SIA-CE system, myoglobin was mixed directly using the flow system with different concentrations of sodium dodecyl sulfate (SDS), a known denaturing agent. The different conformations obtained in this way were analysed with the CE system and a distinct shift in migration time and decreasing of the native peak of myoglobin (Mb) could be observed. The protein samples prepared were also analysed with off-line infrared spectroscopy (IR), confirming these results. PMID:16732362

  6. 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.

  7. A self-contained polymeric cartridge for automated biological sample preparation.

    Science.gov (United States)

    Xu, Guolin; Lee, Daniel Yoke San; Xie, Hong; Chiew, Deon; Hsieh, Tseng-Ming; Ali, Emril Mohamed; Lun Looi, Xing; Li, Mo-Huang; Ying, Jackie Y

    2011-09-01

    Sample preparation is one of the most crucial processes for nucleic acids based disease diagnosis. Several steps are required for nucleic acids extraction, impurity washes, and DNA/RNA elution. Careful sample preparation is vital to the obtaining of reliable diagnosis, especially with low copies of pathogens and cells. This paper describes a low-cost, disposable lab cartridge for automatic sample preparation, which is capable of handling flexible sample volumes of 10 μl to 1 ml. This plastic cartridge contains all the necessary reagents for pathogen and cell lysis, DNA/RNA extraction, impurity washes, DNA/RNA elution and waste processing in a completely sealed cartridge. The entire sample preparation processes are automatically conducted within the cartridge on a desktop unit using a pneumatic fluid manipulation approach. Reagents transportation is achieved with a combination of push and pull forces (with compressed air and vacuum, respectively), which are connected to the pneumatic inlets at the bottom of the cartridge. These pneumatic forces are regulated by pinch valve manifold and two pneumatic syringe pumps within the desktop unit. The performance of this pneumatic reagent delivery method was examined. We have demonstrated the capability of the on-cartridge RNA extraction and cancer-specific gene amplification from 10 copies of MCF-7 breast cancer cells. The on-cartridge DNA recovery efficiency was 54-63%, which was comparable to or better than the conventional manual approach using silica spin column. The lab cartridge would be suitable for integration with lab-chip real-time polymerase chain reaction devices in providing a portable system for decentralized disease diagnosis. PMID:22662036

  8. 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%.

  9. Automated sample preparation for radiogenic and non-traditional metal isotope analysis by MC-ICP-MS

    Science.gov (United States)

    Field, M. P.; Romaniello, S. J.; Gordon, G. W.; Anbar, A. D.

    2012-12-01

    High throughput analysis is becoming increasingly important for many applications of radiogenic and non-traditional metal isotopes. While MC-ICP-MS instruments offer the potential for very high sample throughout, the requirement for labor-intensive sample preparation and purification procedures remains a substantial bottleneck. Current purification protocols require manually feeding gravity-driven separation columns, a process that is both costly and time consuming. This bottleneck is eliminated with the prepFAST-MC™, an automated, low-pressure ion exchange chromatography system that can process from 1 to 60 samples in unattended operation. The syringe-driven system allows sample loading, multiple acid washes, column conditioning and elution cycles necessary to isolate elements of interest and automatically collect up to 3 discrete eluent fractions at user-defined intervals (time, volume and flow rate). Newly developed protocols for automated purification of uranium illustrates high throughput (>30 per run), multiple samples processed per column (>30), complete (>99%) matrix removal, high recovery (> 98%, n=25), and excellent precision (2 sigma =0.03 permil, n=10). The prepFAST-MC™ maximizes sample throughput and minimizes costs associated with personnel and consumables providing an opportunity to greatly expand research horizons in fields where large isotopic data sets are required, including archeology, geochemistry, and climate/environmental science

  10. High-Throughput Serum 25-Hydroxy Vitamin D Testing with Automated Sample Preparation.

    Science.gov (United States)

    Stone, Judy

    2016-01-01

    Serum from bar-coded tubes, and then internal standard, are pipetted to 96-well plates with an 8-channel automated liquid handler (ALH). The first precipitation reagent (methanol:ZnSO4) is added and mixed with the 8-channel ALH. A second protein precipitating agent, 1 % formic acid in acetonitrile, is added and mixed with a 96-channel ALH. After a 4-min delay for larger precipitates to settle to the bottom of the plate, the upper 36 % of the precipitate/supernatant mix is transferred with the 96-channel ALH to a Sigma Hybrid SPE(®) plate and vacuumed through for removal of phospholipids and precipitated proteins. The filtrate is collected in a second 96-well plate (collection plate) which is foil-sealed, placed in the autosampler (ALS), and injected into a multiplexed LC-MS/MS system running AB Sciex Cliquid(®) and MPX(®) software. Two Shimadzu LC stacks, with multiplex timing controlled by MPX(®) software, inject alternately to one AB Sciex API-5000 MS/MS using positive atmospheric pressure chemical ionization (APCI) and a 1.87 min water/acetonitrile LC gradient with a 2.1 × 20 mm, 2.7 μm, C18 fused core particle column (Sigma Ascentis Express). LC-MS/MS through put is ~44 samples/h/LC-MS/MS system with dual-LC channel multiplexing. Plate maps are transferred electronically from the ALH and reformatted into LC-MS/MS sample table format using the Data Innovations LLC (DI) Instrument Manager middleware application. Before collection plates are loaded into the ALS, the plate bar code is manually scanned to download the sample table from the DI middleware to the LC-MS/MS. After acquisition-LC-MS/MS data is analyzed with AB Sciex Multiquant(®) software using customized queries, and then results are transferred electronically via a DI interface to the LIS. 2500 samples/day can be extracted by two analysts using four ALHs in 4-6 h. LC-MS/MS analysis of those samples on three dual-channel LC multiplexed LC-MS/MS systems requires 19-21 h and data analysis can be

  11. 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. PMID:26759433

  12. Adjustable virtual pore-size filter for automated sample preparation using acoustic radiation force

    Energy Technology Data Exchange (ETDEWEB)

    Jung, B; Fisher, K; Ness, K; Rose, K; Mariella, R

    2008-05-22

    We present a rapid and robust size-based separation method for high throughput microfluidic devices using acoustic radiation force. We developed a finite element modeling tool to predict the two-dimensional acoustic radiation force field perpendicular to the flow direction in microfluidic devices. Here we compare the results from this model with experimental parametric studies including variations of the PZT driving frequencies and voltages as well as various particle sizes and compressidensities. These experimental parametric studies also provide insight into the development of an adjustable 'virtual' pore-size filter as well as optimal operating conditions for various microparticle sizes. We demonstrated the separation of Saccharomyces cerevisiae and MS2 bacteriophage using acoustic focusing. The acoustic radiation force did not affect the MS2 viruses, and their concentration profile remained unchanged. With optimized design of our microfluidic flow system we were able to achieve yields of > 90% for the MS2 with > 80% of the S. cerevisiae being removed in this continuous-flow sample preparation device.

  13. 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 co...

  14. 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.

  15. 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.

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

    Science.gov (United States)

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

    2016-01-01

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

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

    Science.gov (United States)

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

    2016-01-01

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

  18. 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

    2012-04-01

    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.

  19. 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 o

  20. On-site detection of foot-and-mouth disease virus using a portable, automated sample preparation and PCR system

    International Nuclear Information System (INIS)

    Full text: Foot-and-mouth disease (FMD) is a highly contagious and economically devastating disease of farm livestock. The etiological agent, FMD virus (FMDV), is a single-stranded, positive-sense RNA virus belonging to the genus Aphthovirus within the family Picornaviridae. Rapid and accurate confirmation of the presence of FMDV is needed for effective control and eradication of the disease. An on-site detection test would be highly advantageous as the time taken to transport suspect clinical material to a central laboratory can often be lengthy, thus delaying a definitive diagnosis in the event of an outbreak. This study describes the development of a molecular assay for the detection of all seven serotypes of FMDV using novel technology, namely: Linear-After-The- Exponential (LATE)-PCR, for transfer onto a portable, easy-to-use, fully automated sample preparation and RT-PCR instrument. Primers and a mismatch tolerant probe were designed from consensus sequences in the FMDV 3D (RNA polymerase) gene to detect the target and its variants at low temperature. An internal control (IC) was included to validate negative results. After demonstrating that the LATE RT-PCR signal at end-point was proportional to number of target molecules over the range 10 to 1 million copies, the assay was compared with a one-step real-time RT-PCR (rRT-PCR) assay (also targeting the 3D) used routinely by reference laboratories. The LATE RT-PCR assay amplified RNA extracted from multiple strains of all FMDV serotypes. Of the 121 FMDV-positive samples tested, 119 were positive by both rRT-PCR and LATE RT-PCR tests while 118 had tested positive by virus isolation at the time of receipt. Twenty-eight FMDVnegative samples failed to react in all 3 tests. There were no false positive signals with RNA from other vesicular disease-causing viruses. Each FMDV-negative sample generated a signal from the IC, ruling out amplification failures. A dilution series of an FMDV reference strain demonstrated

  1. 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

    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...

  2. 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...

  3. AUTOMATING GROUNDWATER SAMPLING AT HANFORD

    Energy Technology Data Exchange (ETDEWEB)

    CONNELL CW; HILDEBRAND RD; CONLEY SF; CUNNINGHAM DE

    2009-01-16

    Until this past October, Fluor Hanford managed Hanford's integrated groundwater program for the U.S. Department of Energy (DOE). With the new contract awards at the Site, however, the CH2M HILL Plateau Remediation Company (CHPRC) has assumed responsibility for the groundwater-monitoring programs at the 586-square-mile reservation in southeastern Washington State. These programs are regulated by the Resource Conservation and Recovery Act (RCRA) and the Comprehensive Environmental Response Compensation and Liability Act (CERCLA). The purpose of monitoring is to track existing groundwater contamination from past practices, as well as other potential contamination that might originate from RCRA treatment, storage, and disposal (TSD) facilities. An integral part of the groundwater-monitoring program involves taking samples of the groundwater and measuring the water levels in wells scattered across the site. More than 1,200 wells are sampled each year. Historically, field personnel or 'samplers' have been issued pre-printed forms that have information about the well(s) for a particular sampling evolution. This information is taken from the Hanford Well Information System (HWIS) and the Hanford Environmental Information System (HEIS)--official electronic databases. 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 the collected information was posted 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. This is a pilot project for automating this tedious process by providing an electronic tool for automating water-level measurements and groundwater field-sampling activities. The automation will eliminate the manual forms and associated data entry, improve the

  4. Modular microfluidic system for biological sample preparation

    Energy Technology Data Exchange (ETDEWEB)

    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.

  5. Differential proteomic analysis of mouse macrophages exposed to adsorbate-loaded heavy fuel oil derived combustion particles using an automated sample-preparation workflow.

    Science.gov (United States)

    Kanashova, Tamara; Popp, Oliver; Orasche, Jürgen; Karg, Erwin; Harndorf, Horst; Stengel, Benjamin; Sklorz, Martin; Streibel, Thorsten; Zimmermann, Ralf; Dittmar, Gunnar

    2015-08-01

    Ship diesel combustion particles are known to cause broad cytotoxic effects and thereby strongly impact human health. Particles from heavy fuel oil (HFO) operated ships are considered as particularly dangerous. However, little is known about the relevant components of the ship emission particles. In particular, it is interesting to know if the particle cores, consisting of soot and metal oxides, or the adsorbate layers, consisting of semi- and low-volatile organic compounds and salts, are more relevant. We therefore sought to relate the adsorbates and the core composition of HFO combustion particles to the early cellular responses, allowing for the development of measures that counteract their detrimental effects. Hence, the semi-volatile coating of HFO-operated ship diesel engine particles was removed by stepwise thermal stripping using different temperatures. RAW 264.7 macrophages were exposed to native and thermally stripped particles in submersed culture. Proteomic changes were monitored by two different quantitative mass spectrometry approaches, stable isotope labeling by amino acids in cell culture (SILAC) and dimethyl labeling. Our data revealed that cells reacted differently to native or stripped HFO combustion particles. Cells exposed to thermally stripped particles showed a very differential reaction with respect to the composition of the individual chemical load of the particle. The cellular reactions of the HFO particles included reaction to oxidative stress, reorganization of the cytoskeleton and changes in endocytosis. Cells exposed to the 280 °C treated particles showed an induction of RNA-related processes, a number of mitochondria-associated processes as well as DNA damage response, while the exposure to 580 °C treated HFO particles mainly induced the regulation of intracellular transport. In summary, our analysis based on a highly reproducible automated proteomic sample-preparation procedure shows a diverse cellular response, depending on the

  6. Universal Sample Preparation Module for Molecular Analysis in Space Project

    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...

  7. Image analysis software and sample preparation demands

    Science.gov (United States)

    Roth, Karl n.; Wenzelides, Knut; Wolf, Guenter; Hufnagl, Peter

    1990-11-01

    Image analysis offers the opportunity to analyse many processes in medicine, biology and engeneering in a quantitative manner. Experience shows that it is only by awareness of preparation methods and attention to software design that full benefit can be reaped from a picture processing system in the fields of cytology and histology. Some examples of special stains for automated analysis are given here and the effectiveness of commercially available software packages is investigated. The application of picture processing and development of related special hardware and software has been increasing within the last years. As PC-based picture processing systems can be purchased at reasonable costs more and more users are confronted with these problems. Experience shows that the quality of commercially available software packages differ and the requirements on the sample preparation needed for successful problem solutions are often underestimated. But as always, sample preparation is still the key to success in automated image analysis for cells and tissues. Hence, a problem solution requires the permanent interaction between sample preparation methods and algorithm development.

  8. 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.

  9. Microfluidic Sample Preparation for Immunoassays

    Energy Technology Data Exchange (ETDEWEB)

    Visuri, S; Benett, W; Bettencourt, K; Chang, J; Fisher, K; Hamilton, J; Krulevitch, P; Park, C; Stockton, C; Tarte, L; Wang, A; Wilson, T

    2001-08-09

    Researchers at Lawrence Livermore National Laboratory are developing means to collect and identify fluid-based biological pathogens in the forms of proteins, viruses, and bacteria. to support detection instruments, they are developing a flexible fluidic sample preparation unit. The overall goal of this Microfluidic Module is to input a fluid sample, containing background particulates and potentially target compounds, and deliver a processed sample for detection. They are developing techniques for sample purification, mixing, and filtration that would be useful to many applications including immunologic and nucleic acid assays. Many of these fluidic functions are accomplished with acoustic radiation pressure or dielectrophoresis. They are integrating these technologies into packaged systems with pumps and valves to control fluid flow through the fluidic circuit.

  10. Robotic, MEMS-based Multi Utility Sample Preparation Instrument for ISS Biological Workstation Project

    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...

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

    Science.gov (United States)

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

    2015-11-01

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

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

    Science.gov (United States)

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

    2015-11-01

    High-throughput individual diagnostic dose assessment is essential for medical management of radiation-exposed subjects after a mass casualty. Cytogenetic assays such as the Dicentric Chromosome Assay (DCA) are recognized as the gold standard by international regulatory authorities. DCA is a multi-step and multi-day bioassay. DCA, as described in the IAEA manual, can be used to assess dose up to 4-6 weeks post-exposure quite accurately but throughput is still a major issue and automation is very essential. The throughput is limited, both in terms of sample preparation as well as analysis of chromosome aberrations. Thus, there is a need to design and develop novel solutions that could utilize extensive laboratory automation for sample preparation, and bioinformatics approaches for chromosome-aberration analysis to overcome throughput issues. We have transitioned the bench-based cytogenetic DCA to a coherent process performing high-throughput automated biodosimetry for individual dose assessment ensuring quality control (QC) and quality assurance (QA) aspects in accordance with international harmonized protocols. A Laboratory Information Management System (LIMS) is designed, implemented and adapted to manage increased sample processing capacity, develop and maintain standard operating procedures (SOP) for robotic instruments, avoid data transcription errors during processing, and automate analysis of chromosome-aberrations using an image analysis platform. Our efforts described in this paper intend to bridge the current technological gaps and enhance the potential application of DCA for a dose-based stratification of subjects following a mass casualty. This paper describes one such potential integrated automated laboratory system and functional evolution of the classical DCA towards increasing critically needed throughput. PMID:26520383

  13. An Automated Home Made Low Cost Vibrating Sample Magnetometer

    Science.gov (United States)

    Kundu, S.; Nath, T. K.

    2011-07-01

    The design and operation of a homemade low cost vibrating sample magnetometer is described here. The sensitivity of this instrument is better than 10-2 emu and found to be very efficient for the measurement of magnetization of most of the ferromagnetic and other magnetic materials as a function of temperature down to 77 K and magnetic field upto 800 Oe. Both M(H) and M(T) data acquisition are fully automated employing computer and Labview software.

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

    OpenAIRE

    Vogeser, Michael; Spöhrer, Ute

    2006-01-01

    Background: Liquid chromatography tandem-mass spectrometry (LC-MS/MS) is an efficient technology for routine determination of immunosuppressants in whole blood; however, time-consuming manual sample preparation remains a significant limitation of this technique. Methods: Using a commercially available robotic pipetting system (Tecan Freedom EVO), we developed an automated sample-preparation protocol for quantification of tacrolimus in whole blood by LC-MS/MS. Barcode reading, sample resuspens...

  15. AUTOMATING GROUNDWATER SAMPLING AT HANFORD THE NEXT STEP

    Energy Technology Data Exchange (ETDEWEB)

    CONNELL CW; CONLEY SF; HILDEBRAND RD; CUNNINGHAM DE; R_D_Doug_Hildebrand@rl.gov; DeVon_E_Cunningham@rl.gov

    2010-01-21

    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.

  16. Sample preparation for x-ray analysis

    International Nuclear Information System (INIS)

    Full text: In my experience over many years it is not uncommon for a geologist to present a suite of rocks or powders for analysis and demand results of high analytical precision which are not warranted for the following reasons: 1. Sample collection is unsatisfactory. 2. Little or no attention has been given to cleaning and splitting the sample. The ultimate aim of the preparation laboratory is to produce a homogeneous, uncontaminated aliquot of the total sample pulverised to a grain size of less than 10 microns. Clearly this is not possible as the grinding equipment will always impart some level of contamination to the sample and there is no grinder available which can produce powders of grain size less than 10 microns without imparting unacceptable levels of contamination to the sample. Modern x-ray spectrometers are extremely stable instruments. Most laboratories run a drift monitor at the start of each shift or when starting analyses requiring a different calibration. Depending on the method of sample preparation errors from this source can be up to two orders of magnitude greater than instrumental errors. For this reason it is imperative that sample preparation methods for a particular analysis are carefully set up and that these procedures are followed implicitly by the sample preparation laboratory. All too often sample preparation is relegated to a secondary role carried out in poorly designed work areas with inappropriate equipment by poorly trained unsupervised staff. Over the past few years staffing reductions and the requirement to crush an increasingly large volume of sample has given the impetus to develop improved jaw crushers. An example of this is the Boyd Crusher which has been designed to minimise these problems, ie this crusher has high throughput, can be easily cleaned and produces minimal contamination. Copyright (1999) Australian X-ray Analytical Association Inc

  17. Sample preparations for spark source mass spectrography

    International Nuclear Information System (INIS)

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

  18. 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.

  19. Automated Training Sample Extraction for Global Land Cover Mapping

    Directory of Open Access Journals (Sweden)

    Julien Radoux

    2014-05-01

    Full Text Available Land cover is one of the essential climate variables of the ESA Climate Change Initiative (CCI. In this context, the Land Cover CCI (LC CCI project aims at building global land cover maps suitable for climate modeling based on Earth observation by satellite sensors.  The  challenge  is  to  generate  a  set  of  successive  maps  that  are  both  accurate and consistent over time. To do so, operational methods for the automated classification of optical images are investigated. The proposed approach consists of a locally trained classification using an automated selection of training samples from existing, but outdated land cover information. Combinations of local extraction (based on spatial criteria and self-cleaning of training samples (based on spectral criteria are quantitatively assessed. Two large study areas, one in Eurasia and the other in South America, are considered. The proposed morphological cleaning of the training samples leads to higher accuracies than the statistical outlier removal in the spectral domain. An optimal neighborhood has been identified for the local sample extraction. The results are coherent for the two test areas, showing an improvement of the overall accuracy compared with the original reference datasets and a significant reduction of macroscopic errors. More importantly, the proposed method partly controls the reliability of existing land cover maps as sources of training samples for supervised classification.

  20. An instrument for automated purification of nucleic acids from contaminated forensic samples.

    Science.gov (United States)

    Broemeling, David J; Pel, Joel; Gunn, Dylan C; Mai, Laura; Thompson, Jason D; Poon, Hiron; Marziali, Andre

    2008-02-01

    Forensic crime scene sample analysis, by its nature, often deals with samples in which there are low amounts of nucleic acids, on substrates that often lead to inhibition of subsequent enzymatic reactions such as PCR amplification for STR profiling. Common substrates include denim from blue jeans, which yields indigo dye as a PCR inhibitor, and soil, which yields humic substances as inhibitors. These inhibitors frequently co-extract with nucleic acids in standard column or bead-based preps, leading to frequent failure of STR profiling. We present a novel instrument for DNA purification of forensic samples that is capable of highly effective concentration of nucleic acids from soil particulates, fabric, and other complex samples including solid components. The novel concentration process, known as SCODA, is inherently selective for long charged polymers such as DNA, and therefore is able to effectively reject known contaminants. We present an automated sample preparation instrument based on this process, and preliminary results based on mock forensic samples.

  1. Total Integrated Sample Preparation for Microfluidic Immunoassays in Complex Biological Matrices

    OpenAIRE

    Apori, Akwasi Asare

    2011-01-01

    A high-throughput protein analysis platform with integrated sample preparation is developed to address the identified technology gaps in biomarker validation, clinical and point-of-care diagnostics. The goals of the technology are to automate and integrate protein sample preparation with electrokinetic separations, implement immunoassays capable of processing raw biological fluids, and perform high-throughput protein assays targeted for disease diagnosis.Integration of multiple functions is ...

  2. On-chip Ultrasonic Sample Preparation

    OpenAIRE

    Iranmanesh, Ida Sadat

    2015-01-01

    Acoustofluidics has become a well-established technology in the lab-on-a-chip scientific community. The technology involves primarily the manipulation of fluids and/or particles in microfluidic systems. It is used today for variety of applications such as handling, sorting, washing and separation of cells or micro-particles, and for mixing and pumping of fluids. When such manipulation functions are integrated in micro-devices, the technology has been used for clinical sample preparation as we...

  3. 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

    2014-08-01

    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. PMID:25033319

  4. Sample preparation for SEM of plant surfaces

    Directory of Open Access Journals (Sweden)

    A.K. Pathan

    2010-01-01

    Full Text Available 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 techniques on different leaf types are discussed. Comparative examples are depicted from our lab using similar techniques; the pros and cons for specific techniques are discussed. New promising techniques and microscopes, which can alleviate some of the problems encountered in conventional methods of leaf sample processing and visualisation, are also discussed. It is concluded that the choice of technique for a specific leaf sample is dictated by the surface features that need to be preserved (such as trichomes, epidermal cells or wax microstructure, the resolution to be achieved, availability of the appropriate processing equipment and the technical capabilities of the available electron microscope.

  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. Reducing Workload in Systematic Review Preparation Using Automated Citation Classification

    OpenAIRE

    Cohen, A M; Hersh, W R; Peterson, K; Yen, Po-Yin

    2006-01-01

    Objective: To determine whether automated classification of document citations can be useful in reducing the time spent by experts reviewing journal articles for inclusion in updating systematic reviews of drug class efficacy for treatment of disease.

  7. 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...

  8. Design Automation Systems for Production Preparation : Applied on the Rotary Draw Bending Process

    OpenAIRE

    Johansson, Joel

    2008-01-01

    Intensive competition on the global market puts great pressure on manufacturing companies to develop and produce products that meet requirements from customers and investors. One key factor in meeting these requirements is the efficiency of the product development and the production preparation process. Design automation is a powerful tool to increase efficiency in these two processes. The benefits of automating the production preparation process are shortened led-time, improved product perfo...

  9. 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.

  10. Sample preparation for measurement of plasma mycophenolic acid concentrations using chromatographically functionalized magnetic micro-particles.

    Science.gov (United States)

    König, Katrin; Vogeser, Michael

    2012-01-01

    Utilizing chromatographically modified magnetic micro-particles is an innovative principle of sample preparation for quantitative analysis of small molecules in complex biomedical samples by liquid chromatography tandem mass spectrometry. Since no vacuum or pressure has to be applied-in contrast to cartridge based solid phase extraction protocols-the principle's main characteristics are potentially straightforward automation and a high extraction performance (in terms of µg of extraction material per µL of sample). Following first descriptions of the approach, this article reports, the validation of a magnetic particle-based, analytical method for the quantification of the immunosuppressant mycophenolic acid in plasma. This sample preparation technology has shown a good performance for this clinically relevant analyte. As a result, we conclude that further work towards the implementation of this technology in a multi- analyte approach on robotic systems, aiming towards a fully automated process, is justified. PMID:23221116

  11. 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.

  12. 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 routin...... with minimal handling for metaphase FISH slide preparation....

  13. 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...

  14. Automated sampling and data processing derived from biomimetic membranes

    DEFF Research Database (Denmark)

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

    2009-01-01

    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...... 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....... 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...

  15. Expanding the application of the tablet processing workstation to support the sample preparation of oral suspensions.

    Science.gov (United States)

    Opio, Alex Manuel; Nickerson, Beverly; Xue, Gang; Warzeka, John; Norris, Ken

    2011-06-01

    Sample preparation is the most time-consuming part of the analytical method for powder for oral suspension (POS) assay, purity, and preservative analysis, as this involves multiple dilution and filtration steps. The Tablet Processing Workstation (TPW) was used to automate the sample preparation of a POS formulation. Although the TPW is typically used to automate the preparation of solid oral dosage forms and powders, it contains all of the necessary components to perform POS sample preparation. The TPW exhibited acceptable repeatability in testing 3 lots using 10 replicate preparations per lot. Acceptable linearity of the drug and preservative in the presence of excipients was demonstrated over the range corresponding to 50-150% of intent. Accuracy showed suitable recoveries for all points evaluated. TPW results were shown to correlate to results obtained with the manual method. The TPW method was used to prepare samples in support of manufacturing scale-up efforts. With the efficiencies gained using the TPW, it was possible to analyze a large number of samples generated during process development activities for the POS formulation with minimal human intervention. The extensive data enabled trending of the manufacturing development runs and helped to identify optimization strategies for the process.

  16. 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...

  17. Evaluation of the measurement uncertainty in automated long-term sampling of PCDD/PCDFs.

    Science.gov (United States)

    Vicaretti, M; D'Emilia, G; Mosca, S; Guerriero, E; Rotatori, M

    2013-12-01

    Since the publication of the first version of European standard EN-1948 in 1996, long-term sampling equipment has been improved to a high standard for the sampling and analysis of polychlorodibenzo-p-dioxin (PCDD)/polychlorodibenzofuran (PCDF) emissions from industrial sources. The current automated PCDD/PCDF sampling systems enable to extend the measurement time from 6-8 h to 15-30 days in order to have data values better representative of the real pollutant emission of the plant in the long period. EN-1948:2006 is still the European technical reference standard for the determination of PCDD/PCDF from stationary source emissions. In this paper, a methodology to estimate the measurement uncertainty of long-term automated sampling is presented. The methodology has been tested on a set of high concentration sampling data resulting from a specific experience; it is proposed with the intent that it is to be applied on further similar studies and generalized. A comparison between short-term sampling data resulting from manual and automated parallel measurements has been considered also in order to verify the feasibility and usefulness of automated systems and to establish correlations between results of the two methods to use a manual method for calibration of automatic long-term one. The uncertainty components of the manual method are analyzed, following the requirements of EN-1948-3:2006, allowing to have a preliminary evaluation of the corresponding uncertainty components of the automated system. Then, a comparison between experimental data coming from parallel sampling campaigns carried out in short- and long-term sampling periods is realized. Long-term sampling is more reliable to monitor PCDD/PCDF emissions than occasional short-term sampling. Automated sampling systems can assure very useful emission data both in short and long sampling periods. Despite this, due to the different application of the long-term sampling systems, the automated results could not be

  18. A Semi-automated Approach to Preparing Antibody Cocktails for Immunophenotypic Analysis of Human Peripheral Blood.

    Science.gov (United States)

    Koguchi, Yoshinobu; Gonzalez, Iliana L; Meeuwsen, Tanisha L; Miller, William L; Haley, Daniel P; Tanibata-Branham, Alice N; Bahjat, Keith S

    2016-01-01

    Immunophenotyping of peripheral blood by flow cytometry determines changes in the frequency and activation status of peripheral leukocytes during disease and treatment. It has the potential to predict therapeutic efficacy and identify novel therapeutic targets. Whole blood staining utilizes unmanipulated blood, which minimizes artifacts that can occur during sample preparation. However, whole blood staining must also be done on freshly collected blood to ensure the integrity of the sample. Additionally, it is best to prepare antibody cocktails on the same day to avoid potential instability of tandem-dyes and prevent reagent interaction between brilliant violet dyes. Therefore, whole blood staining requires careful standardization to control for intra and inter-experimental variability. Here, we report deployment of an automated liquid handler equipped with a two-dimensional (2D) barcode reader into a standard process of making antibody cocktails for flow cytometry. Antibodies were transferred into 2D barcoded tubes arranged in a 96 well format and their contents compiled in a database. The liquid handler could then locate the source antibody vials by referencing antibody names within the database. Our method eliminated tedious coordination for positioning of source antibody tubes. It provided versatility allowing the user to easily change any number of details in the antibody dispensing process such as specific antibody to use, volume, and destination by modifying the database without rewriting the scripting in the software method for each assay. A proof of concept experiment achieved outstanding inter and intra- assay precision, demonstrated by replicate preparation of an 11-color, 17-antibody flow cytometry assay. These methodologies increased overall throughput for flow cytometry assays and facilitated daily preparation of the complex antibody cocktails required for the detailed phenotypic characterization of freshly collected anticoagulated peripheral blood

  19. Influences of sample preparations on dentine ESR signals

    International Nuclear Information System (INIS)

    The work is to study influences of sample preparations on dentine ESR (electron spin resonance) signals, in order to use dentine samples for dose reconstruction, which has been performed with enamel samples. The dentine and enamel samples were collected from non-irradiated adult teeth and prepared by mechanical or mechanical plus chemical methods. The samples were scanned by an ESR spectrometer before and after their irradiation by 60Co γ-rays. The sensitivities of ESR signals of dentine and enamel samples to irradiation dose differed significantly among different sample preparation methods. The results show that dentine samples mechanically and chemically prepared have good enough ESR response to low dose γ-ray irradiations, and it is possible to use the dentine samples for dose reconstruction, as a substitution to enamel samples when they are short of supply. (authors)

  20. Sample preparation techniques in trace element analysis of water

    Science.gov (United States)

    Nagj, Marina; Jakšić, M.; Orlić, I.; Valković, V.

    1985-06-01

    Sample preparation techniques for the analysis of water for trace elements using X-ray emission spectroscopy are described. Fresh water samples for the analysis of transition metals were prepared by complexation with ammonium-pyrrolidine-dithiocarbamate (APDC) and filtering through a membrane filter. Analyses of water samples for halogenes was done on samples prepared by precipitation with AgNO 3 and subsequent filtration. Two techniques for seawater preparation for uranium determination are described, viz. precipitation with APDC in the presence of iron (II) as a carrier and complexation with APDC followed with adsorption on activated carbon. In all cases trace element levels at 10 -3 μg/g were measured.

  1. Fluidics platform and method for sample preparation

    Energy Technology Data Exchange (ETDEWEB)

    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.

  2. Preparation of protein samples for gel electrophoresis by sequential extraction

    Institute of Scientific and Technical Information of China (English)

    钟伯雄; 翁宏飚; 等

    2002-01-01

    Since preparation and solubilization of protein samples are crucial factors in proteome research,the authors established a sequential extraction technique to prepare protein samples from the body wall of the 5th instar larvae of silkworm.Bombyx mori.Two kinds of protein samples were obtained from the body wall using the method.Between the two types of samples only about 15% proteins were identical;the majority were different,indicating that more species of proteins could be obtained with the sequential extraction method;which will be useful for preparation of protein samples for proteome study.

  3. 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...

  4. Development of an automated data processing method for sample to sample comparison of seized methamphetamines.

    Science.gov (United States)

    Choe, Sanggil; Lee, Jaesin; Choi, Hyeyoung; Park, Yujin; Lee, Heesang; Pyo, Jaesung; Jo, Jiyeong; Park, Yonghoon; Choi, Hwakyung; Kim, Suncheun

    2012-11-30

    The information about the sources of supply, trafficking routes, distribution patterns and conspiracy links can be obtained from methamphetamine profiling. The precursor and synthetic method for the clandestine manufacture can be estimated from the analysis of minor impurities contained in methamphetamine. Also, the similarity between samples can be evaluated using the peaks that appear in chromatograms. In South Korea, methamphetamine was the most popular drug but the total seized amount of methamphetamine whole through the country was very small. Therefore, it would be more important to find the links between samples than the other uses of methamphetamine profiling. Many Asian countries including Japan and South Korea have been using the method developed by National Research Institute of Police Science of Japan. The method used gas chromatography-flame ionization detector (GC-FID), DB-5 column and four internal standards. It was developed to increase the amount of impurities and minimize the amount of methamphetamine. After GC-FID analysis, the raw data have to be processed. The data processing steps are very complex and require a lot of time and effort. In this study, Microsoft Visual Basic Application (VBA) modules were developed to handle these data processing steps. This module collected the results from the data into an Excel file and then corrected the retention time shift and response deviation generated from the sample preparation and instruments analysis. The developed modules were tested for their performance using 10 samples from 5 different cases. The processed results were analyzed with Pearson correlation coefficient for similarity assessment and the correlation coefficient of the two samples from the same case was more than 0.99. When the modules were applied to 131 seized methamphetamine samples, four samples from two different cases were found to have the common origin and the chromatograms of the four samples were appeared visually identical

  5. An automated atmospheric sampling system operating on 747 airliners

    Science.gov (United States)

    Perkins, P. J.; Gustafsson, U. R. C.

    1976-01-01

    An air sampling system that automatically measures the temporal and spatial distribution of particulate and gaseous constituents of the atmosphere is collecting data on commercial air routes covering the world. Measurements are made in the upper troposphere and lower stratosphere (6 to 12 km) of constituents related to aircraft engine emissions and other pollutants. Aircraft operated by different airlines sample air at latitudes from the Arctic to Australia. This unique system includes specialized instrumentation, a special air inlet probe for sampling outside air, a computerized automatic control, and a data acquisition system. Air constituent and related flight data are tape recorded in flight for later computer processing on the ground.

  6. Miniaturized sample preparation based on carbon nanostructures

    OpenAIRE

    Cárdenas Soledad

    2014-01-01

    The evolution of analytical methodologies has been driven by the objective to reduce the complexity of sample treatment while increasing the efficiency of the overall analytical process. For this reason, the analytical chemist takes into consideration advances in other scientific areas and systematically evaluates the potential influence that such discoveries might have on its own discipline. This is the present situation with nanostructured materials, which have alrea...

  7. SASSI: Subsystems for Automated Subsurface Sampling Instruments Project

    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...

  8. Automated biowaste sampling system, solids subsystem operating model, part 2

    Science.gov (United States)

    Fogal, G. L.; Mangialardi, J. K.; Stauffer, R. E.

    1973-01-01

    The detail design and fabrication of the Solids Subsystem were implemented. The system's capacity for the collection, storage or sampling of feces and vomitus from six subjects was tested and verified.

  9. SASSI: Subsystems for Automated Subsurface Sampling Instruments Project

    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...

  10. 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...

  11. Snow White Trench Prepared for Sample Collection

    Science.gov (United States)

    2008-01-01

    The informally named 'Snow White' trench is the source for the next sample to be acquired by NASA's Phoenix Mars Lander for analysis by the wet chemistry lab. The Surface Stereo Imager on Phoenix took this shadow-enhanced image of the trench, on the eastern end of Phoenix's work area, on Sol 103, or the 103rd day of the mission, Sept. 8, 2008. The trench is about 23 centimeters (9 inches) wide. The wet chemistry lab is part of Phoenix's Microscopy, Electrochemistry and Conductivity suite of instruments. The Phoenix Mission is led by the University of Arizona, Tucson, on behalf of NASA. Project management of the mission is by NASA's Jet Propulsion Laboratory, Pasadena, Calif. Spacecraft development is by Lockheed Martin Space Systems, Denver.

  12. Automated biowaste sampling system urine subsystem operating model, part 1

    Science.gov (United States)

    Fogal, G. L.; Mangialardi, J. K.; Rosen, F.

    1973-01-01

    The urine subsystem automatically provides for the collection, volume sensing, and sampling of urine from six subjects during space flight. Verification of the subsystem design was a primary objective of the current effort which was accomplished thru the detail design, fabrication, and verification testing of an operating model of the subsystem.

  13. Sequential automated fusion/extraction chromatography methodology for the dissolution of uranium in environmental samples for mass spectrometric determination

    International Nuclear Information System (INIS)

    An improved methodology has been developed, based on dissolution by automated fusion followed by extraction chromatography for the detection and quantification of uranium in environmental matrices by mass spectrometry. A rapid fusion protocol (2/LiBr melts were used. The use of a M4 fusion unit also improved repeatability in sample preparation over muffle furnace fusion. Instrumental issues originating from the presence of high salt concentrations in the digestate after lithium metaborate fusion was also mitigated using an extraction chromatography (EXC) protocol aimed at removing lithium and interfering matrix constituants prior to the elution of uranium. The sequential methodology, which can be performed simultaneously on three samples, requires less than 20 min per sample for fusion and separation. It was successfully coupled to inductively coupled plasma mass spectrometry (ICP-MS) achieving detection limits below 100 pg kg-1 for 5-300 mg of sample.

  14. A self-contained polymeric cartridge for automated biological sample preparationa

    OpenAIRE

    Xu, Guolin; Lee, Daniel Yoke San; Xie, Hong; Chiew, Deon; Hsieh, Tseng-Ming; Ali, Emril Mohamed; Lun Looi, Xing; Li, Mo-Huang; Ying, Jackie Y.

    2011-01-01

    Sample preparation is one of the most crucial processes for nucleic acids based disease diagnosis. Several steps are required for nucleic acids extraction, impurity washes, and DNA/RNA elution. Careful sample preparation is vital to the obtaining of reliable diagnosis, especially with low copies of pathogens and cells. This paper describes a low-cost, disposable lab cartridge for automatic sample preparation, which is capable of handling flexible sample volumes of 10 μl to 1 ml. This plastic ...

  15. γ-ray spectrometry results versus sample preparation methods

    Institute of Scientific and Technical Information of China (English)

    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.

  16. Overview and perspectives on automation strategies in (68)Ga radiopharmaceutical preparations.

    Science.gov (United States)

    Boschi, Stefano; Malizia, Claudio; Lodi, Filippo

    2013-01-01

    The renaissance of (68)Ga radiopharmacy has led to great advances in automation technology. The availability of a highly efficient, reliable, long-lived (68)Ge/(68)Ga generator system along with a well-established coordination chemistry based on bifunctional chelating agents have been the bases of this development in (68)Ga radiopharmacy. Syntheses of (68)Ga peptides were originally performed by manual or semiautomated systems, but increasing clinical demand, radioprotection, and regulatory issues have driven extensive automation of their production process. Several automated systems, based on different post-processing of the (68)Ga generator eluate, on different engineering, and on fixed tubing or disposable cassette approaches, have been developed and are discussed in this chapter. Since automatic systems for preparation of radiopharmaceuticals should comply with qualification and validation protocols established by regulations such as current Good Manufacturing Practices (cGMP) and local regulations, some regulatory issues and the more relevant qualification protocols are also discussed.

  17. Automated Genotyping of Biobank Samples by Multiplex Amplification of Insertion/Deletion Polymorphisms

    OpenAIRE

    Lucy Mathot; Elin Falk-Sörqvist; Lotte Moens; Marie Allen; Tobias Sjöblom; Mats Nilsson

    2012-01-01

    The genomic revolution in oncology will entail mutational analyses of vast numbers of patient-matched tumor and normal tissue samples. This has meant an increased risk of patient sample mix up due to manual handling. Therefore, scalable genotyping and sample identification procedures are essential to pathology biobanks. We have developed an efficient alternative to traditional genotyping methods suited for automated analysis. By targeting 53 prevalent deletions and insertions found in human p...

  18. Efficient Sample Preparation from Complex Biological Samples Using a Sliding Lid for Immobilized Droplet Extractions

    OpenAIRE

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

    2014-01-01

    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...

  19. 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

  20. Application of bar codes to the automation of analytical sample data collection

    International Nuclear Information System (INIS)

    The Health Protection Department at the Savannah River Plant collects 500 urine samples per day for tritium analyses. Prior to automation, all sample information was compiled manually. Bar code technology was chosen for automating this program because it provides a more accurate, efficient, and inexpensive method for data entry. The system has three major functions: sample labeling is accomplished at remote bar code label stations composed of an Intermec 8220 (Intermec Corp.) interfaced to an IBM-PC, data collection is done on a central VAX 11/730 (Digital Equipment Corp.). Bar code readers are used to log-in samples to be analyzed on liquid scintillation counters. The VAX 11/730 processes the data and generates reports, data storage is on the VAX 11/730 and backed up on the plant's central computer. A brief description of several other bar code applications at the Savannah River Plant is also presented

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

    OpenAIRE

    Qiao, Jixin

    2011-01-01

    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 combina...

  2. 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

  3. RapTOR: Automated sequencing library preparation and suppression for rapid pathogen characterization ( 7th Annual SFAF Meeting, 2012)

    Energy Technology Data Exchange (ETDEWEB)

    Lane, Todd [SNL

    2012-06-01

    Todd Lane on "RapTOR: Automated sequencing library preparation and suppression for rapid pathogen characterization" at the 2012 Sequencing, Finishing, Analysis in the Future Meeting held June 5-7, 2012 in Santa Fe, New Mexico.

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

    Science.gov (United States)

    Rahman, Nur Aira Abd; Yussup, Nolida; Salim, Nazaratul Ashifa Bt. Abdullah; Ibrahim, Maslina Bt. Mohd; Mokhtar, Mukhlis B.; Soh@Shaari, Syirrazie Bin Che; Azman, Azraf B.; Ismail, Nadiah Binti

    2015-04-01

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

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

    International Nuclear Information System (INIS)

    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

  6. Fluidics platform and method for sample preparation and analysis

    Energy Technology Data Exchange (ETDEWEB)

    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.

  7. Microfluidic Sample Preparation Methods for the Analysis of Milk Contaminants

    Directory of Open Access Journals (Sweden)

    Andrea Adami

    2016-01-01

    Full Text Available In systems for food analysis, one of the major challenges is related to the quantification of specific species into the complex chemical and physical composition of foods, that is, the effect of “matrix”; the sample preparation is often the key to a successful application of biosensors to real measurements but little attention is traditionally paid to such aspects in sensor research. In this critical review, we discuss several microfluidic concepts that can play a significant role in sample preparation, highlighting the importance of sample preparation for efficient detection of food contamination. As a case study, we focus on the challenges related to the detection of aflatoxin M1 in milk and we evaluate possible approaches based on inertial microfluidics, electrophoresis, and acoustic separation, compared with traditional laboratory and industrial methods for phase separation as a baseline of thrust and well-established techniques.

  8. 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......, which is the analysis of a large number of metabolites with very diverse chemical and physical properties. This work reports the leakage of intracellular metabolites observed during quenching yeast cells with cold methanol solution, the efficacy of six different methods for the extraction...

  9. Functional profiling of live melanoma samples using a novel automated platform.

    Directory of Open Access Journals (Sweden)

    Adam Schayowitz

    Full Text Available AIMS: This proof-of-concept study was designed to determine if functional, pharmacodynamic profiles relevant to targeted therapy could be derived from live human melanoma samples using a novel automated platform. METHODS: A series of 13 melanoma cell lines was briefly exposed to a BRAF inhibitor (PLX-4720 on a platform employing automated fluidics for sample processing. Levels of the phosphoprotein p-ERK in the mitogen-activated protein kinase (MAPK pathway from treated and untreated sample aliquots were determined using a bead-based immunoassay. Comparison of these levels provided a determination of the pharmacodynamic effect of the drug on the MAPK pathway. A similar ex vivo analysis was performed on fine needle aspiration (FNA biopsy samples from four murine xenograft models of metastatic melanoma, as well as 12 FNA samples from patients with metastatic melanoma. RESULTS: Melanoma cell lines with known sensitivity to BRAF inhibitors displayed marked suppression of the MAPK pathway in this system, while most BRAF inhibitor-resistant cell lines showed intact MAPK pathway activity despite exposure to a BRAF inhibitor (PLX-4720. FNA samples from melanoma xenografts showed comparable ex vivo MAPK activity as their respective cell lines in this system. FNA samples from patients with metastatic melanoma successfully yielded three categories of functional profiles including: MAPK pathway suppression; MAPK pathway reactivation; MAPK pathway stimulation. These profiles correlated with the anticipated MAPK activity, based on the known BRAF mutation status, as well as observed clinical responses to BRAF inhibitor therapy. CONCLUSION: Pharmacodynamic information regarding the ex vivo effect of BRAF inhibitors on the MAPK pathway in live human melanoma samples can be reproducibly determined using a novel automated platform. Such information may be useful in preclinical and clinical drug development, as well as predicting response to targeted therapy in

  10. Preparation of archaeological samples for its dating by thermoluminescence

    International Nuclear Information System (INIS)

    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)

  11. 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.

  12. 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.

    2016-01-01

    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. PMID:27487827

  13. 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. PMID:27487827

  14. 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.

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

    International Nuclear Information System (INIS)

    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

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

    DEFF Research Database (Denmark)

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

    , multisyringe flow injection, and micro-Lab-on-valve are presented as appealing approaches for on-line handling of solid samples. Special emphasis is given to the capability of flow systems to accommodate sequential extraction protocols for partitioning of trace elements and nutrients in environmental solids (e......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...... on the design and characterisation of sample processings units coupled with flowing systems aiming to enable the direct introduction and treatment of solid samples of environmental and agricultural origin in an automated fashion [1]. In this respect, various sample pre-treatment techniques including...

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

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Löschner, Katrin

    2014-01-01

    microscopy (TEM) proved to be necessary for trouble shooting of results obtained from AFFF-LS-ICP-MS. Aqueous and enzymatic extraction strategies were tested for thorough sample preparation aiming at degrading the sample matrix and to liberate the AgNPs from chicken meat into liquid suspension. The resulting...... 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......-ICP-MS analysis of their content of gold nanoparticles (AuNPs) was tested and compared with enzymatic sample preparation [3]. The results showed that the same results, with respect to the obtained number-based size distribution for AuNPs, were obtained for the two preparation methods. In contrast, the alkaline...

  18. 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)

    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

  19. 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

  20. 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.

  1. 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.

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

    International Nuclear Information System (INIS)

    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

  3. 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 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 SIextraction 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...

  4. Sample preparation methods for determination of drugs of abuse in hair samples: A review.

    Science.gov (United States)

    Vogliardi, Susanna; Tucci, Marianna; Stocchero, Giulia; Ferrara, Santo Davide; Favretto, Donata

    2015-02-01

    Hair analysis has assumed increasing importance in the determination of substances of abuse, both in clinical and forensic toxicology investigations. Hair analysis offers particular advantages over other biological matrices (blood and urine), including a larger window of detection, ease of collection and sample stability. In the present work, an overview of sample preparation techniques for the determination of substances of abuse in hair is provided, specifically regarding the principal steps in hair sample treatment-decontamination, extraction and purification. For this purpose, a survey of publications found in the MEDLINE database from 2000 to date was conducted. The most widely consumed substances of abuse and psychotropic drugs were considered. Trends in simplification of hair sample preparation, washing procedures and cleanup methods are discussed. Alternative sample extraction techniques, such as head-space solid phase microextraction (HS-SPDE), supercritical fluid extraction (SFE) and molecularly imprinted polymers (MIP) are also reported. PMID:25604816

  5. Sample preparation method for induced mutation on orchid

    International Nuclear Information System (INIS)

    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)

  6. Preparation of TEM samples for hard ceramic powders.

    Science.gov (United States)

    Xu, Qiang; Kumar, Vikas; de Kruijff, Tom; Jansen, Jacob; Zandbergen, Henny W

    2008-12-01

    It is challenging to prepare a good sample for high-resolution electron microscopy of polycrystalline ceramic powders containing hard particles or particles with a strong preferential cleavage. Here we demonstrate that embedding the particles in a Cu matrix in a pressed pellet allows for straightforward conventional ion milling. The method is applied to powders of Mg10Ir19B16 and Na0.5CoO2 to show its feasibility, whereby transmission electron microscopy (TEM) samples with crystalline areas thinner than 10 nm can be obtained easily. PMID:18722061

  7. Preparation of TEM samples for hard ceramic powders

    International Nuclear Information System (INIS)

    It is challenging to prepare a good sample for high-resolution electron microscopy of polycrystalline ceramic powders containing hard particles or particles with a strong preferential cleavage. Here we demonstrate that embedding the particles in a Cu matrix in a pressed pellet allows for straightforward conventional ion milling. The method is applied to powders of Mg10Ir19B16 and Na0.5CoO2 to show its feasibility, whereby transmission electron microscopy (TEM) samples with crystalline areas thinner than 10 nm can be obtained easily.

  8. Preparation of TEM samples for hard ceramic powders

    Energy Technology Data Exchange (ETDEWEB)

    Xu Qiang [National Centre for HREM, Kavli Institute of Nanoscience, Delft University of Technology, 2628 CJ Lorentzweg 1, Delft (Netherlands)], E-mail: q.xu@tudelft.nl; Kumar, Vikas [National Centre for HREM, Kavli Institute of Nanoscience, Delft University of Technology, 2628 CJ Lorentzweg 1, Delft (Netherlands)], E-mail: V.Kumar@tudelft.nl; Kruijff, Tom de [National Centre for HREM, Kavli Institute of Nanoscience, Delft University of Technology, 2628 CJ Lorentzweg 1, Delft (Netherlands)], E-mail: t.r.dekruijff@tudelft.nl; Jansen, Jacob [National Centre for HREM, Kavli Institute of Nanoscience, Delft University of Technology, 2628 CJ Lorentzweg 1, Delft (Netherlands)], E-mail: joukj@hrem.nano.tudelft.nl; Zandbergen, Henny W. [National Centre for HREM, Kavli Institute of Nanoscience, Delft University of Technology, 2628 CJ Lorentzweg 1, Delft (Netherlands)], E-mail: h.w.zandbergen@tudelft.nl

    2008-12-15

    It is challenging to prepare a good sample for high-resolution electron microscopy of polycrystalline ceramic powders containing hard particles or particles with a strong preferential cleavage. Here we demonstrate that embedding the particles in a Cu matrix in a pressed pellet allows for straightforward conventional ion milling. The method is applied to powders of Mg{sub 10}Ir{sub 19}B{sub 16} and Na{sub 0.5}CoO{sub 2} to show its feasibility, whereby transmission electron microscopy (TEM) samples with crystalline areas thinner than 10 nm can be obtained easily.

  9. Apparatus for preparing a sample for mass spectrometry

    Science.gov (United States)

    Villa-Aleman, Eliel

    1994-01-01

    An apparatus for preparing a sample for analysis by a mass spectrometer system. The apparatus has an entry chamber and an ionization chamber separated by a skimmer. A capacitor having two space-apart electrodes followed by one or more ion-imaging lenses is disposed in the ionization chamber. The chamber is evacuated and the capacitor is charged. A valve injects a sample gas in the form of sample pulses into the entry chamber. The pulse is collimated by the skimmer and enters the ionization chamber. When the sample pulse passes through the gap between the electrodes, it discharges the capacitor and is thereby ionized. The ions are focused by the imaging lenses and enter the mass analyzer, where their mass and charge are analyzed.

  10. Novel sample preparation for operando TEM of catalysts

    International Nuclear Information System (INIS)

    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 CO2 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

  11. 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.

  12. Automated sample-changing robot for solution scattering experiments at the EMBL Hamburg SAXS station X33

    OpenAIRE

    Round, A R; D. Franke; S. Moritz; Huchler, R.; Fritsche, M.; Malthan, D.; Klaering, R.; Svergun, D I; Roessle, M.

    2008-01-01

    There is a rapidly increasing interest in the use of synchrotron small-angle X-ray scattering (SAXS) for large-scale studies of biological macromolecules in solution, and this requires an adequate means of automating the experiment. A prototype has been developed of an automated sample changer for solution SAXS, where the solutions are kept in thermostatically controlled well plates allowing for operation with up to 192 samples. The measuring protocol involves controlled loading of protein so...

  13. Optimization for Peptide Sample Preparation for Urine Peptidomics

    Energy Technology Data Exchange (ETDEWEB)

    Sigdel, Tara K.; Nicora, Carrie D.; Hsieh, Szu-Chuan; Dai, Hong; Qian, Weijun; Camp, David G.; Sarwal, Minnie M.

    2014-02-25

    Analysis of native or endogenous peptides in biofluids can provide valuable insights into disease mechanisms. Furthermore, the detected peptides may also have utility as potential biomarkers for non-invasive monitoring of human diseases. The non-invasive nature of urine collection and the abundance of peptides in the urine makes analysis by high-throughput ‘peptidomics’ methods , an attractive approach for investigating the pathogenesis of renal disease. However, urine peptidomics methodologies can be problematic with regards to difficulties associated with sample preparation. The urine matrix can provide significant background interference in making the analytical measurements that it hampers both the identification of peptides and the depth of the peptidomics read when utilizing LC-MS based peptidome analysis. We report on a novel adaptation of the standard solid phase extraction (SPE) method to a modified SPE (mSPE) approach for improved peptide yield and analysis sensitivity with LC-MS based peptidomics in terms of time, cost, clogging of the LC-MS column, peptide yield, peptide quality, and number of peptides identified by each method. Expense and time requirements were comparable for both SPE and mSPE, but more interfering contaminants from the urine matrix were evident in the SPE preparations (e.g., clogging of the LC-MS columns, yellowish background coloration of prepared samples due to retained urobilin, lower peptide yields) when compared to the mSPE method. When we compared data from technical replicates of 4 runs, the mSPE method provided significantly improved efficiencies for the preparation of samples from urine (e.g., mSPE peptide identification 82% versus 18% with SPE; p = 8.92E-05). Additionally, peptide identifications, when applying the mSPE method, highlighted the biology of differential activation of urine peptidases during acute renal transplant rejection with distinct laddering of specific peptides, which was obscured for most proteins

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

    Energy Technology Data Exchange (ETDEWEB)

    Macario, Kita D.; Gomes, Paulo R. S.; Anjos, Roberto M. dos; Linares, Roberto; Queiroz, Eduardo; Oliveira, Fabiana M. de; Cardozo, Laio [Universidade Federal Fluminense (UFF), Niteroi, RJ (Brazil); Carvalho, Carla R.A. [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil)

    2011-07-01

    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 {sup 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)

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

    International Nuclear Information System (INIS)

    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

  16. 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

  17. Scalable Transcriptome Preparation for Massive Parallel Sequencing

    OpenAIRE

    Stranneheim, Henrik; Werne, Beata; Sherwood, Ellen; Lundeberg, Joakim

    2011-01-01

    Background The tremendous output of massive parallel sequencing technologies requires automated robust and scalable sample preparation methods to fully exploit the new sequence capacity. Methodology In this study, a method for automated library preparation of RNA prior to massively parallel sequencing is presented. The automated protocol uses precipitation onto carboxylic acid paramagnetic beads for purification and size selection of both RNA and DNA. The automated sample preparation was comp...

  18. Scalable Transcriptome Preparation for Massive Parallel Sequencing

    OpenAIRE

    Henrik Stranneheim; Beata Werne; Ellen Sherwood; Joakim Lundeberg

    2011-01-01

    BACKGROUND: The tremendous output of massive parallel sequencing technologies requires automated robust and scalable sample preparation methods to fully exploit the new sequence capacity. METHODOLOGY: In this study, a method for automated library preparation of RNA prior to massively parallel sequencing is presented. The automated protocol uses precipitation onto carboxylic acid paramagnetic beads for purification and size selection of both RNA and DNA. The automated sample preparation was co...

  19. A fast method to prepare water samples for 15N analysis

    Institute of Scientific and Technical Information of China (English)

    肖化云; 刘丛强

    2001-01-01

    Automatic element analyser is often used to prepare organic matters tor 15N analysis. It is seldom used to prepare water samples. Water samples are conventionally dealt with by Kjeldahl-Rittenberg technique. But it requires tedious and labor-intensive sample preparation. A fast and reliable method is proposed in this paper to prepare water samples for 15N analysis.

  20. Deuterium and oxygen-18 determination of microliter quantities of a water sample using an automated equilibrator.

    Science.gov (United States)

    Uemura, Ryu; Matsui, Yohei; Motoyama, Hideaki; Yoshida, Naohiro

    2007-01-01

    We describe a modified version of the equilibration method and a correction algorithm for isotope ratio measurements of small quantities of water samples. The deltaD and the delta(18)O of the same water sample can both be analyzed using an automated equilibrator with sample sizes as small as 50 microL. Conventional equilibration techniques generally require water samples of several microL. That limitation is attributable mainly to changes in the isotope ratio ((18)O/(16)O or D/H) of water samples during isotopic exchange between the equilibration gas (CO(2) or H(2)) and water, and therefore the technique for microL quantities of water requires mass-balance correction using the water/gas (CO(2) or H(2)) mole ratio to correct this isotopic effect. We quantitatively evaluate factors controlling the variability of the isotopic effect due to sample size. Theoretical consideration shows that a simple linear equation corrects for the effects without determining parameters such as isotope fractionation factors and water/gas mole ratios. Precisions (1-sigma) of 50-microL meteoric water samples whose isotopic compositions of -1.4 to -396.2 per thousand for deltaD are +/-0.5 to +/-0.6 per thousand, and of -0.37 to -51.37 per thousand for delta(18)O are +/-0.01 to +/-0.11 per thousand. PMID:17487828

  1. Robowell: An automated process for monitoring ground water quality using established sampling protocols

    Science.gov (United States)

    Granato, G.E.; Smith, K.P.

    1999-01-01

    Robowell is an automated process for monitoring selected ground water quality properties and constituents by pumping a well or multilevel sampler. Robowell was developed and tested to provide a cost-effective monitoring system that meets protocols expected for manual sampling. The process uses commercially available electronics, instrumentation, and hardware, so it can be configured to monitor ground water quality using the equipment, purge protocol, and monitoring well design most appropriate for the monitoring site and the contaminants of interest. A Robowell prototype was installed on a sewage treatment plant infiltration bed that overlies a well-studied unconfined sand and gravel aquifer at the Massachusetts Military Reservation, Cape Cod, Massachusetts, during a time when two distinct plumes of constituents were released. The prototype was operated from May 10 to November 13, 1996, and quality-assurance/quality-control measurements demonstrated that the data obtained by the automated method was equivalent to data obtained by manual sampling methods using the same sampling protocols. Water level, specific conductance, pH, water temperature, dissolved oxygen, and dissolved ammonium were monitored by the prototype as the wells were purged according to U.S Geological Survey (USGS) ground water sampling protocols. Remote access to the data record, via phone modem communications, indicated the arrival of each plume over a few days and the subsequent geochemical reactions over the following weeks. Real-time availability of the monitoring record provided the information needed to initiate manual sampling efforts in response to changes in measured ground water quality, which proved the method and characterized the screened portion of the plume in detail through time. The methods and the case study described are presented to document the process for future use.

  2. Improved synthesis of anti-[18F]FACBC: improved preparation of labeling precursor and automated radiosynthesis.

    Science.gov (United States)

    McConathy, Jonathan; Voll, Ronald J; Yu, Weiping; Crowe, Ronald J; Goodman, Mark M

    2003-06-01

    The non-natural amino acid anti-1-amino-3-[18F]fluorocyclobutyl-1-carboxylic acid (FACBC) has shown promise for tumor imaging with positron emission tomography. An improved synthesis of the precursor of anti-[18F]FACBC has been devised which demonstrates high stereoselectivity and suitability for large-scale preparations. An automated radiosynthesis has been developed which provides anti-[18F]FACBC in 24% decay-corrected yield. Additionally, the major non-radioactive species present in doses of anti-[18F]FACBC has been identified as anti-1-amino-3-hydroxycyclobutane-1-carboxylic acid. Together, these results are important steps towards the routine production of anti-[18F]FACBC for human use.

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

    CERN Document Server

    Handberg, R

    2014-01-01

    One of the tasks of the Kepler Asteroseismic Science Operations Center (KASOC) is to provide asteroseismic analyses on Kepler Objects of Interest (KOIs). However, asteroseismic analysis of planetary host stars presents some unique complications with respect to data preprocessing, compared to pure asteroseismic targets. If not accounted for, the presence of planetary transits in the photometric time series often greatly complicates or even hinders these asteroseismic analyses. This drives the need for specialised methods of preprocessing data to make them suitable for asteroseismic analysis. 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 photometric time series than the original data. The methods are automated and can therefore easily be applied to a ...

  4. 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.

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

    International Nuclear Information System (INIS)

    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)

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

    International Nuclear Information System (INIS)

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

  7. 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.

  8. Automated high-throughput in vitro screening of the acetylcholine esterase inhibiting potential of environmental samples, mixtures and single compounds.

    Science.gov (United States)

    Froment, Jean; Thomas, Kevin V; Tollefsen, Knut Erik

    2016-08-01

    A high-throughput and automated assay for testing the presence of acetylcholine esterase (AChE) inhibiting compounds was developed, validated and applied to screen different types of environmental samples. Automation involved using the assay in 96-well plates and adapting it for the use with an automated workstation. Validation was performed by comparing the results of the automated assay with that of a previously validated and standardised assay for two known AChE inhibitors (paraoxon and dichlorvos). The results show that the assay provides similar concentration-response curves (CRCs) when run according to the manual and automated protocol. Automation of the assay resulted in a reduction in assay run time as well as in intra- and inter-assay variations. High-quality CRCs were obtained for both of the model AChE inhibitors (dichlorvos IC50=120µM and paraoxon IC50=0.56µM) when tested alone. The effect of co-exposure of an equipotent binary mixture of the two chemicals were consistent with predictions of additivity and best described by the concentration addition model for combined toxicity. Extracts of different environmental samples (landfill leachate, wastewater treatment plant effluent, and road tunnel construction run-off) were then screened for AChE inhibiting activity using the automated bioassay, with only landfill leachate shown to contain potential AChE inhibitors. Potential uses and limitations of the assay were discussed based on the present results. PMID:27085000

  9. 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

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

    Science.gov (United States)

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

    2005-12-01

    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.

  11. Waste minimization in analytical chemistry through innovative sample preparation techniques

    International Nuclear Information System (INIS)

    Because toxic solvents and other hazardous materials are commonly used in analytical methods, characterization procedures result in significant and costly amount of waste. We are developing alternative analytical methods in the radiological and organic areas to reduce the volume or form of the hazardous waste produced during sample analysis. For the radiological area, we have examined high-pressure, closed-vessel microwave digestion as a way to minimize waste from sample preparation operations. Heated solutions of strong mineral acids can be avoided for sample digestion by using the microwave approach. Because reactivity increases with pressure, we examined the use of less hazardous solvents to leach selected contaminants from soil for subsequent analysis. We demonstrated the feasibility of this approach by extracting plutonium from a NET reference material using citric and tartaric acids with microwave digestion. Analytical results were comparable to traditional digestion methods, while hazardous waste was reduced by a factor often. We also evaluated the suitability of other natural acids, determined the extraction performance on a wider variety of soil types, and examined the extraction efficiency of other contaminants. For the organic area, we examined ways to minimize the wastes associated with the determination of polychlorinated biphenyls (PCBs) in environmental samples. Conventional methods for analyzing semivolatile organic compounds are labor intensive and require copious amounts of hazardous solvents. For soil and sediment samples, we have a method to analyze PCBs that is based on microscale extraction using benign solvents (e.g., water or hexane). The extraction is performed at elevated temperatures in stainless steel cells containing the sample and solvent. Gas chromatography-mass spectrometry (GC/MS) was used to quantitate the analytes in the isolated extract. More recently, we developed a method utilizing solid-phase microextraction (SPME) for natural

  12. 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

    protein excretion patterns of 49 healthy men and 4 patients with renal disease were obtained by 2D electrophoresis. Silver nitrate stained protein spots were identified by mass spectrometry. RESULTS: Reproductive 2D gels identified 5 classes of proteins systematically found in healthy subjects......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...

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

    International Nuclear Information System (INIS)

    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)

  14. 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)

  15. 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.

  16. 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

  17. AMS 14C performance test of a new automated bone preparation system

    International Nuclear Information System (INIS)

    Complete text of publication follows. Bone is one of the most complex sample materials for radiocarbon dating. After burial, its physical state and chemical composition can be affected by many environmental processes. In case of our new AMS bone preparation technique, after ultrasonication in distilled water, drying, surface cleaning and grinding, the sample is sieved to get the appropriate sized sample fraction (0.5 - 1 mm) out of which 500 - 1000 mg is measured, depending on the state of the bone. We have developed our own continuous flow bone sample preparation equipment. In this unit OMNIFITTM columns are used as flow cells to construct our own automatic ABA (acid-base-acid) cleaning system. From 3 types of reagent, each one is injected via a 4 way valve and inert plastic tubing to an IsmatechTM IPC 12 channel peristaltic pump to ensure a constant flow rate. Reagents are selectively pumped to the reaction cells containing the powdered bone samples, with a sequence of 0.5 M HCl and 0.1 M NaOH solution, interspersed with flushing with distilled water. During the sixteen-hour-long process, reagents follow a well-defined sequence that is controlled by a computer program and a special electronic driver device. The cleaned sample is inserted into a test tube containing 5 ml, pH 3 aqueous solutions, and it is placed into a heating block at 75 deg C for 24 hours. Dissolved collagen is filtered via a 45 μm glass fibre filter (WhatmanTM AUTOVIAL 5) into a clean vial, and after freezing, it gets freeze-dried, a process which takes at least a day. To investigate the sample-preparation reproducibility and possible extra contamination effect by an optional ultra-filtration process a known-age bone sample, previously dated by an independent method (GPC at HEKAL), was prepared several times using the new AMS preparation line for 14C analyses. The results obtained (Figure 1.) showed very good reproducibility and excellent agreement with the classical GPC measured 14C age in

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

    International Nuclear Information System (INIS)

    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 (UO3) 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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1989-05-15

    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{sub 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.

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

    International Nuclear Information System (INIS)

    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)

  1. 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. PMID:25974880

  2. 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. PMID:26423626

  3. Plasma cortisol and noradrenalin concentrations in pigs: automated sampling of freely moving pigs housed in PigTurn versus manually sampled and restrained pigs

    Science.gov (United States)

    Minimizing the effects of restraint and human interaction on the endocrine physiology of animals is essential for collection of accurate physiological measurements. Our objective was to compare stress-induced cortisol (CORT) and noradrenalin (NorA) responses in automated versus manual blood sampling...

  4. 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.

  5. 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.

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

    International Nuclear Information System (INIS)

    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

  7. 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.

  8. Evaluation of two automated enzyme-immunoassays for detection of thermophilic campylobacters in faecal samples from cattle and swine

    DEFF Research Database (Denmark)

    Hoorfar, Jeffrey; Nielsen, E.M.; Stryhn, H.;

    1999-01-01

    We evaluated the performance of two enzyme-immunoassays (EIA) for the detection of naturally occurring, thermophilic Campylobacter spp. found in faecal samples from cattle (n = 21 and n = 26) and swine (n = 43) relative to the standard culture method, and also assuming that none of the tests......-2 method resulted in a rather low specificity (32%). This seemed to be partially due to the isolation of nonthermophilic species. In conclusion, EIA-1 method may provide a simple and fast tool with good accuracy in cattle and swine samples for automated screening of large number of samples....

  9. 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.

  10. 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

    2016-05-01

    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.

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

    International Nuclear Information System (INIS)

    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

  12. An automated synthesis module for preparation of L-3-[I-123]iodo-alpha-methyl tyrosine

    NARCIS (Netherlands)

    Luurtsema, G; Jager, PL; Piers, A; de Hooge, MN

    2001-01-01

    L-3-[I-123]iodo-alpha-methyl tyrosine (IMT) is an artificial amino acid suitable for SPECT imaging of various tumours. Manual synthesis of this radiopharmaceutical is reliable, but time-consuming and may require handling of large quantities of radioactivity. We developed an automated IMT synthesis m

  13. Sample Preparation for Monolithic Refractories Part 1: Refractory Castables

    Institute of Scientific and Technical Information of China (English)

    Zhang Xiaohui; Peng Xigao

    2010-01-01

    @@ 1 Scope This standard specifies the definition and test methods of flowability of dense and insulating refractory castables,and moulding equipment,moulding methods,curing and drying conditions of castables samples.

  14. Sample Preparation (SS): SE52_SS01 [Metabolonote[Archive

    Lifescience Database Archive (English)

    Full Text Available Tokyo, Japan) using a mixer mill (MM 300, Retsch) with a zirconia bead for 6 min... at 20 Hz. Next, the samples were centrifuged at 15,000 g for 10 min and filtered (Ultrafree-MC filter, 0.2 μm; Mil...lipore, Bedford, MA, USA). The sample extracts were then applied to an HLB μElution plate (Waters, Mil

  15. 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.

  16. 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. PMID:26671943

  17. 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...

  18. 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...... of novel oligonucleotide probes containing internally positioned xanthene and cyanine dye pairs and thus represents a significant step forward for the preparation of advanced fluorescent oligonucleotide probes. Furthermore, we demonstrate that the novel xanthene and cyanine labeled probes display unusual...... and very promising photophysical properties resulting from energy-transfer interactions between the fluorophores controlled by nucleic acid assembly. Potential benefits of using these novel fluorescent probes within, for example, molecular diagnostics and fluorescence microscopy include: Considerable...

  19. Automated sample-changing robot for solution scattering experiments at the EMBL Hamburg SAXS station X33.

    Science.gov (United States)

    Round, A R; Franke, D; Moritz, S; Huchler, R; Fritsche, M; Malthan, D; Klaering, R; Svergun, D I; Roessle, M

    2008-10-01

    There is a rapidly increasing interest in the use of synchrotron small-angle X-ray scattering (SAXS) for large-scale studies of biological macromolecules in solution, and this requires an adequate means of automating the experiment. A prototype has been developed of an automated sample changer for solution SAXS, where the solutions are kept in thermostatically controlled well plates allowing for operation with up to 192 samples. The measuring protocol involves controlled loading of protein solutions and matching buffers, followed by cleaning and drying of the cell between measurements. The system was installed and tested at the X33 beamline of the EMBL, at the storage ring DORIS-III (DESY, Hamburg), where it was used by over 50 external groups during 2007. At X33, a throughput of approximately 12 samples per hour, with a failure rate of sample loading of less than 0.5%, was observed. The feedback from users indicates that the ease of use and reliability of the user operation at the beamline were greatly improved compared with the manual filling mode. The changer is controlled by a client-server-based network protocol, locally and remotely. During the testing phase, the changer was operated in an attended mode to assess its reliability and convenience. Full integration with the beamline control software, allowing for automated data collection of all samples loaded into the machine with remote control from the user, is presently being implemented. The approach reported is not limited to synchrotron-based SAXS but can also be used on laboratory and neutron sources. PMID:25484841

  20. Sample Preparation (SS): SE55_SS01 [Metabolonote[Archive

    Lifescience Database Archive (English)

    Full Text Available .1% acetic acid, 0.5 mg/L of lidocaine, and d-camphor sulfonic acid (Tokyo Kasei) using a mixer mill (MM 300...,000g for 10 min and filtration (Ultrafree-MC filter, 0.2 mm, Millipore), the sample extracts were applied t

  1. 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

  2. 9 CFR 147.8 - Procedures for preparing egg yolk samples for diagnostic tests.

    Science.gov (United States)

    2010-01-01

    ... 9 Animals and Animal Products 1 2010-01-01 2010-01-01 false Procedures for preparing egg yolk samples for diagnostic tests. 147.8 Section 147.8 Animals and Animal Products ANIMAL AND PLANT HEALTH... IMPROVEMENT PLAN Blood Testing Procedures § 147.8 Procedures for preparing egg yolk samples for...

  3. Technical Note: An improved guideline for rapid and precise sample preparation of tree-ring stable isotope analysis

    Directory of Open Access Journals (Sweden)

    K. Schollaen

    2015-07-01

    Full Text Available The procedure of wood sample preparation, including tree-ring dissection, cellulose extraction, homogenization and finally weighing and packing for stable isotope analysis is labour intensive and time consuming. We present an elaborated methodical guideline from pre-analyses considerations, wood sample preparation through semi-automated chemical extraction of cellulose directly from tree-ring cross-sections to tree-ring dissection for high-precision isotope ratio mass spectrometry. This guideline reduces time and maximizes the tree-ring stable isotope data throughput significantly. The method was applied to ten different tree species (coniferous and angiosperm wood with different wood growth rates and differently shaped tree-ring boundaries. The tree-ring structures of the cellulose cross-sections largely remained well identifiable. FTIR (Fourier transform infrared spectrometry and the comparison of stable isotope values with classical method confirm chemical purity of the resultant cellulose. Sample homogenization is no longer necessary. Cellulose extraction is now faster, cheaper and more user friendly allowing (i the simultaneous treatment of wood cross-sections of a total length of 180 cm (equivalent to 6 increment cores of 30 cm length and thickness of 0.5 to 2 mm, and (ii precise tree-ring separation at annual to high-resolution scale utilizing manual devices or UV-laser microdissection microscopes.

  4. 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 nL into the...

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

    Science.gov (United States)

    Jensen, Andreas Tue Ingemann; Binderup, Tina; Andresen, Thomas L; Kjær, Andreas; Rasmussen, Palle H

    2012-12-01

    A novel [¹⁸F]-labeled cholesteryl ether lipid probe was prepared by synthesis of the corresponding mesylate, which was [¹⁸F]-fluorinated by a [¹⁸F]KF, Kryptofix-222, K₂CO₃ procedure. Fluorination was done for 10 minutes at 165°C and took place with conversion between 3 and 17%, depending 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 extrusion through 100-nm filters. The [¹⁸F]-labeled liposomes were injected into nude, tumor-bearing mice, and positron emission tomography (PET) scans were performed several times over 8 hours to investigate the in vivo biodistribution. Clear tumor accumulation, as well as hepatic and splenic uptake, 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 is satisfactorily high for visualization of pathological lesions. Moreover, the blood concentration was still at a high level (13.9 ± 1.5 %ID/g) at the end of the 8-hour time frame. The present work demonstrates the methodology for automated preparation of radiolabeled liposomes, and shows that [¹⁸F]-labeled liposomes could be suitable as a methodology for visualization of tumors and obtaining short-term pharmacokinetics in vivo. PMID:22803638

  6. High-resolution laboratory lysimeter for automated sampling of tracers through a 0.5 m soil block

    OpenAIRE

    K. N. Andrew; Worsfold, P. J.; Matthews, G. P.; Patel, D.; Mathews, T.J.; Johnson, A

    2003-01-01

    A computer-controlled, automated sample collection from a 0.5-m lysimeter, designed to give superior temporal and spatial resolution for monitoring the movement of chemical tracers through a large undisturbed soil block, is described. The soil block, 0.520.520.5 m, was monitored for saturation using eight time domain reflectometry probes. Rainfall was applied at approximately 1600 ml hm1 using a 12212 array of 23-gauge (0.318 mm internal diameter) hypodermic needles. Soil leachates were colle...

  7. Sample preparation for atomic-resolution STEM at low voltages by FIB

    Energy Technology Data Exchange (ETDEWEB)

    Schaffer, Miroslava, E-mail: mschaffer@SuperSTEM.org [SuperSTEM, STFC Daresbury Laboratories, Keckwick Lane, Warrington WA4 4AD (United Kingdom); Department of Engineering, George Holt Building, Ashton Street, Liverpool L69 3BX (United Kingdom); Schaffer, Bernhard [SuperSTEM, STFC Daresbury Laboratories, Keckwick Lane, Warrington WA4 4AD (United Kingdom); Kelvin Nanocharacterisation Centre, SUPA School of Physics and Astronomy, University of Glasgow, Glasgow G12 8QQ, Scotland (United Kingdom); Ramasse, Quentin [SuperSTEM, STFC Daresbury Laboratories, Keckwick Lane, Warrington WA4 4AD (United Kingdom); Department of Engineering, George Holt Building, Ashton Street, Liverpool L69 3BX (United Kingdom)

    2012-03-15

    While FIB sample preparation for transmission electron microscopy is a well established technique, few examples exist of samples of sufficient quality for atomic resolution imaging by aberration corrected (scanning) transmission electron microscopy (STEM). In this work we demonstrate the successful preparation of such samples from five different materials and present the refined lift-out preparation technique, which was applied here. Samples with parallel surfaces and a general thickness between 20 and 40 nm over a range of several {mu}m were repeatedly prepared and analyzed by Cs-corrected STEM at 60 and 100 kV. Here, a novel 'wedge pre-milling' step helps to keep the protective surface layers intact during the whole milling process, allowing features close to or at the sample surface to be analyzed without preparation damage. Another example shows the cross-sectional preparation of a working thin film solar cell device to a final thickness of 10 to 20 nm over {mu}m sized areas in the region of interest, enabling atomic resolution imaging and elemental mapping across general grain boundaries without projection artefacts. All sample preparation has been carried out in modern Dual-Beam FIB microscopes capable of low-kV Ga{sup +} ion milling, but without additional preparation steps after the FIB lift-out procedure. -- Highlights: Black-Right-Pointing-Pointer Suitability of stand-alone FIB preparation for atomic resolution STEM is shown. Black-Right-Pointing-Pointer Reproducible preparation of 10-40 nm thick samples from 5 different materials. Black-Right-Pointing-Pointer Low-kV milling and adjusted procedure for crystalline, homogeneously thin specimen. Black-Right-Pointing-Pointer Wedge pre-milling to protect surface-near features.

  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;

    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...

  9. Method for sample preparation for cryoelectron microscopy (CEM) microreactor and loading platform

    NARCIS (Netherlands)

    Zandbergen, H.W.; Ahn, C.W.

    2008-01-01

    A method for sample preparation for cryoelectron microscopy (CEM), wherein the sample is held in a microreactor, wherein the conditions in the microreactor are regulated relative to the environment, wherein the sample in the microreactor is frozen according to a quench freeze process, whereupon the

  10. 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.

  11. 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.

  12. Non-destructive automated sampling of mycotoxins in bulk food and feed - A new tool for required harmonization.

    Science.gov (United States)

    Spanjer, M; Stroka, J; Patel, S; Buechler, S; Pittet, A; Barel, S

    2001-06-01

    Mycotoxins contamination is highly non-uniformly distributed as is well recog-nized by the EC, by not only setting legal limits in a series of commodities, but also schedule a sampling plan that takes this heterogeneity into account. In practice however, it turns out that it is very difficult to carry out this sampling plan in a harmonised way. Applying the sampling plan to a container filled with pallets of bags (i.e. with nuts or coffee beans) varies from very laborious to almost impossible. The presented non-destructive automated method to sample bulk food could help to overcome these practical problems and to enforcing of EC directives. It is derived from a tested and approved technology for detection of illicit substances in security applications. It has capability to collect and iden-tify ultra trace contaminants, i.e. from a fingerprint of chemical substance in a bulk of goods, a cargo pallet load (~ 1000 kg) with boxes and commodities.The technology, patented for explosives detection, uses physical and chemistry processes for excitation and remote rapid enhanced release of contaminant residues, vapours and particulate, of the inner/outer surfaces of inspected bulk and collect them on selective probes. The process is automated, takes only 10 minutes, is non-destructive and the bulk itself remains unharmed. The system design is based on applicable international regulations for shipped cargo hand-ling and transportation by road, sea and air. After this process the pallet can be loaded on a truck, ship or plane. Analysis can be carried out before the cargo leaves the place of shipping. The potent application of this technology for myco-toxins detection, has been demonstrated by preliminary feasibility experiments. Aflatoxins were detected in pistachios and ochratoxin A in green coffee beans bulk. Both commodities were naturally contaminated, priory found and confirm-ed by common methods as used at routine inspections. Once the contaminants are extracted from a

  13. 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)

  14. Automated production of copper radioisotopes and preparation of high specific activity [64Cu]Cu-ATSM for PET studies

    International Nuclear Information System (INIS)

    60Cu and 64Cu are useful radioisotopes for positron emission tomography (PET) radiopharmaceuticals and may be used for the preparation of promising agents for diagnosis and radiotherapy. In this study, the production and purification of 60/64Cu starting from 60/64Ni using a new automated system, namely Alceo, is described. A dynamic process for electrodeposition and dissolution of 60/64Ni/60/64Cu was developed. Preliminary production yields of 60Cu and 64Cu were 400 and 300 mCi, respectively. 64Cu was used to radiolabel the hypoxia detection tracer ATSM with a specific activity of 2.2±1.3 Ci/μmol.

  15. Automated production of copper radioisotopes and preparation of high specific activity [{sup 64}Cu]Cu-ATSM for PET studies

    Energy Technology Data Exchange (ETDEWEB)

    Matarrese, Mario [Institute of Molecular Bioimaging and Physiology-CNR, University of Milano-Bicocca, San Raffaele Scientific Institute, Via Olgettina 60, 20132 Milano (Italy); Technological Oncologyc Laboratory (LaTO), Contrada Pietrapollastra Pisciotto, 90015 Cefalu (Italy)], E-mail: matarrese.mario@hsr.it; Bedeschi, Paolo [Comecer S.p.A., Via Emilia Ponente 390, 48014 Castelbolognese (Italy); Scardaoni, Roberto [Technological Oncologyc Laboratory (LaTO), Contrada Pietrapollastra Pisciotto, 90015 Cefalu (Italy); Sudati, Francesco; Savi, Annarita; Pepe, Annalisa; Masiello, Valeria; Todde, Sergio; Gianolli, Luigi; Messa, Cristina; Fazio, Ferruccio [Institute of Molecular Bioimaging and Physiology-CNR, University of Milano-Bicocca, San Raffaele Scientific Institute, Via Olgettina 60, 20132 Milano (Italy)

    2010-01-15

    {sup 60}Cu and {sup 64}Cu are useful radioisotopes for positron emission tomography (PET) radiopharmaceuticals and may be used for the preparation of promising agents for diagnosis and radiotherapy. In this study, the production and purification of {sup 60/64}Cu starting from {sup 60/64}Ni using a new automated system, namely Alceo, is described. A dynamic process for electrodeposition and dissolution of {sup 60/64}Ni/{sup 60/64}Cu was developed. Preliminary production yields of {sup 60}Cu and {sup 64}Cu were 400 and 300 mCi, respectively. {sup 64}Cu was used to radiolabel the hypoxia detection tracer ATSM with a specific activity of 2.2{+-}1.3 Ci/{mu}mol.

  16. Improved synthesis of anti-[{sup 18}F]FACBC: improved preparation of labeling precursor and automated radiosynthesis

    Energy Technology Data Exchange (ETDEWEB)

    McConathy, Jonathan; Voll, Ronald J.; Yu Weiping; Crowe, Ronald J.; Goodman, Mark M. E-mail: mgoodma@emory.edu

    2003-06-01

    The non-natural amino acid anti-1-amino-3-[{sup 18}F]fluorocyclobutyl-1-carboxylic acid (FACBC) has shown promise for tumor imaging with positron emission tomography. An improved synthesis of the precursor of anti-[{sup 18}F]FACBC has been devised which demonstrates high stereoselectivity and suitability for large-scale preparations. An automated radiosynthesis has been developed which provides anti-[{sup 18}F]FACBC in 24% decay-corrected yield. Additionally, the major non-radioactive species present in doses of anti-[{sup 18}F]FACBC has been identified as anti-1-amino-3-hydroxycyclobutane-1-carboxylic acid. Together, these results are important steps towards the routine production of anti-[{sup 18}F]FACBC for human use.

  17. Automation and environment of a sample of the modernized installation YuMO

    International Nuclear Information System (INIS)

    New possibilities of the modernized installation YuMO due to automation of separate units are shown. Main unique devices due to modernization are presented. Advantages of the upgraded spectrometer are shown. The basic approaches to creation of control systems by executive mechanisms of spectrometers on the basis of their unification and standardization are formulated. Circuits of the block of management by step-by-step engines, the switchboard-amplifier of step-by-step motors, the circuit of the system of stabilization of the period and phase of the chopper, and the block diagram of the control system of executive mechanisms of the spectrometer YuMO are submitted. Main technical parameters of the basic original mechanical devices are given. (author)

  18. 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.

  19. 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.

  20. 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.

  1. Method for sample preparation for cryoelectron microscopy (CEM) microreactor and loading platform

    OpenAIRE

    H.W. Zandbergen; Ahn, C. W.

    2008-01-01

    A method for sample preparation for cryoelectron microscopy (CEM), wherein the sample is held in a microreactor, wherein the conditions in the microreactor are regulated relative to the environment, wherein the sample in the microreactor is frozen according to a quench freeze process, whereupon the sample, in frozen condition, is placed in the electron microscope. A microreactor for use with cryoelectron microscopy (CEM), comprising a first and second membrane, which membranes, at least in a ...

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

    International Nuclear Information System (INIS)

    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 (241Am, 230Th and 238Pu) and beta (90Sr/90Y) 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

  3. Novel sample preparation technique with needle-type micro-extraction device for volatile organic compounds in indoor air samples.

    Science.gov (United States)

    Ueta, Ikuo; Mizuguchi, Ayako; Fujimura, Koji; Kawakubo, Susumu; Saito, Yoshihiro

    2012-10-01

    A novel needle-type sample preparation device was developed for the effective preconcentration of volatile organic compounds (VOCs) in indoor air before gas chromatography-mass spectrometry (GC-MS) analysis. To develop a device for extracting a wide range of VOCs typically found in indoor air, several types of particulate sorbents were tested as the extraction medium in the needle-type extraction device. To determine the content of these VOCs, air samples were collected for 30min with the packed sorbent(s) in the extraction needle, and the extracted VOCs were thermally desorbed in a GC injection port by the direct insertion of the needle. A double-bed sorbent consisting of a needle packed with divinylbenzene and activated carbon particles exhibited excellent extraction and desorption performance and adequate extraction capacity for all the investigated VOCs. The results also clearly demonstrated that the proposed sample preparation method is a more rapid, simpler extraction/desorption technique than traditional sample preparation methods. PMID:22975183

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

    NARCIS (Netherlands)

    Duijn, E. van; Sandman, H.; Grossouw, D.; Mocking, J.A.J.; Coulier, L.; Vaes, W.H.J.

    2014-01-01

    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. H

  5. 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. PMID:24778715

  6. 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.

  7. 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.

  8. Reducing Spatial Heterogeneity of MALDI Samples with Marangoni Flows During Sample Preparation

    Science.gov (United States)

    Lai, Yin-Hung; Cai, Yi-Hong; Lee, Hsun; Ou, Yu-Meng; Hsiao, Chih-Hao; Tsao, Chien-Wei; Chang, Huan-Tsung; Wang, Yi-Sheng

    2016-08-01

    This work demonstrates a method to prepare homogeneous distributions of analytes to improve data reproducibility in matrix-assisted laser desorption/ionization (MALDI) mass spectrometry (MS). Natural-air drying processes normally result in unwanted heterogeneous spatial distributions of analytes in MALDI crystals and make quantitative analysis difficult. This study demonstrates that inducing Marangoni flows within drying droplets can significantly reduce the heterogeneity problem. The Marangoni flows are accelerated by changing substrate temperatures to create temperature gradients across droplets. Such hydrodynamic flows are analyzed semi-empirically. Using imaging mass spectrometry, changes of heterogeneity of molecules with the change of substrate temperature during drying processes are demonstrated. The observed heterogeneities of the biomolecules reduce as predicted Marangoni velocities increase. In comparison to conventional methods, drying droplets on a 5 °C substrate while keeping the surroundings at ambient conditions typically reduces the heterogeneity of biomolecular ions by 65%-80%. The observation suggests that decreasing substrate temperature during droplet drying processes is a simple and effective means to reduce analyte heterogeneity for quantitative applications.

  9. Reducing Spatial Heterogeneity of MALDI Samples with Marangoni Flows During Sample Preparation.

    Science.gov (United States)

    Lai, Yin-Hung; Cai, Yi-Hong; Lee, Hsun; Ou, Yu-Meng; Hsiao, Chih-Hao; Tsao, Chien-Wei; Chang, Huan-Tsung; Wang, Yi-Sheng

    2016-08-01

    This work demonstrates a method to prepare homogeneous distributions of analytes to improve data reproducibility in matrix-assisted laser desorption/ionization (MALDI) mass spectrometry (MS). Natural-air drying processes normally result in unwanted heterogeneous spatial distributions of analytes in MALDI crystals and make quantitative analysis difficult. This study demonstrates that inducing Marangoni flows within drying droplets can significantly reduce the heterogeneity problem. The Marangoni flows are accelerated by changing substrate temperatures to create temperature gradients across droplets. Such hydrodynamic flows are analyzed semi-empirically. Using imaging mass spectrometry, changes of heterogeneity of molecules with the change of substrate temperature during drying processes are demonstrated. The observed heterogeneities of the biomolecules reduce as predicted Marangoni velocities increase. In comparison to conventional methods, drying droplets on a 5 °C substrate while keeping the surroundings at ambient conditions typically reduces the heterogeneity of biomolecular ions by 65%-80%. The observation suggests that decreasing substrate temperature during droplet drying processes is a simple and effective means to reduce analyte heterogeneity for quantitative applications. Graphical Abstract ᅟ. PMID:27126469

  10. Contribution to the sample preparation in the radionuclide X-ray fluorescence analysis of hair

    International Nuclear Information System (INIS)

    Methods of sample treatment in XRF analysis of hair are studied in view of the effect on analytical results. A new method is proposed based on the incomplete ashing of hair followed by pellet preparation. Its suitability is estimated on the XRF analysis of real hair samples collected from 4 healthy adults. (author) 12 refs.; 4 figs.; 1 tab

  11. A new method for preparing thin samples of pottery shards for PIXE analysis

    International Nuclear Information System (INIS)

    A novel method, based on the centrifugal precipitation technique, has been used for preparing thin (1 mg/cm2) uniform and homogeneous samples of pottery shards for PIXE analysis. The reproducibility of the results has been tested on standard Perlman-Asaro samples and ancient Greek pottery shards. The abundances of more than 12 elements can be reliably measured. (orig.)

  12. Preparation and characterization of microporous fibers for sample preparation and LC-MS determination of drugs.

    Science.gov (United States)

    Buszewski, Boguslaw; Nowaczyk, Jacek; Ligor, Tomasz; Olszowy, Pawel; Ligor, Magdalena; Wasiniak, Bartlomiej; Miekisch, Wolfram; Schubert, Jochen K; Amann, Anton

    2009-07-01

    The aim of this study was the preparation of polypyrrole (PPy) fibers for solid phase microextraction (SPME). PPy coatings were obtained during the electrochemical polymerization process. The utility of various metal wires (Fe, Cu, Ag, Cu/Ag, kanthal and medical stainless steel) as a support for polymers was compared. Various experimental conditions of the synthesis process such as scan rate, voltage limits and number of scans and deposition time were applied. The average polymer thickness was in the range of 7-125 microm and its weight was in the scope of 0.65-5.6 mg. Different techniques, mainly elemental analysis, Fourier transform infrared spectroscopy, microscopy, and chromatography were performed for the characterization of obtained fibers with microporous structure. The extraction efficiency of cardiovascular drugs (metoprolol, propranolol, oxprenolol, propafenone and mexiletine) by means of fibers was tested. The concentration of mentioned compounds in standard solution was in the span of 10-150 ng/mL. LC-MS was employed for determination of drugs in desorption solution. LODs varied from 0.013 to 1.51 ng/mL for metoprolol and mexiletine respectively. The repeatability of extraction was obtained with the RSD values lower than 10%. PMID:19569094

  13. An automated gas exchange tank for determining gas transfer velocities in natural seawater samples

    Directory of Open Access Journals (Sweden)

    K. Schneider-Zapp

    2014-02-01

    Full Text Available In order to advance understanding of the role of seawater surfactants in the air–sea exchange of climatically active trace gases via suppression of the gas transfer velocity (kw, we constructed a fully automated, closed air-water gas exchange tank and coupled analytical system. The system allows water-side turbulence in the tank to be precisely controlled with an electronically operated baffle. Two coupled gas chromatographs and an integral equilibrator, connected to the tank in a continuous gas-tight system, allow temporal changes in the partial pressures of SF6, CH4 and N2O to be measured simultaneously in the tank water and headspace at multiple turbulence settings, during a typical experimental run of 3.25 h. PC software developed by the authors controls all operations and data acquisition, enabling the optimisation of experimental conditions with high reproducibility. The use of three gases allows three independent estimates of kw for each turbulence setting; these values are subsequently normalised to a constant Schmidt number for direct comparison. The normalised kw estimates show close agreement. Repeated experiments with MilliQ water demonstrate a typical measurement accuracy of 4% for kw. Experiments with natural seawater show that the system clearly resolves the effects on kw of spatial and temporal trends in natural surfactant activity. The system is an effective tool with which to probe the relationships between kw, surfactant activity and biogeochemical indices of primary productivity, and should assist in providing valuable new insights into the air–sea gas exchange process.

  14. An automated gas exchange tank for determining gas transfer velocities in natural seawater samples

    Science.gov (United States)

    Schneider-Zapp, K.; Salter, M. E.; Upstill-Goddard, R. C.

    2014-07-01

    In order to advance understanding of the role of seawater surfactants in the air-sea exchange of climatically active trace gases via suppression of the gas transfer velocity (kw), we constructed a fully automated, closed air-water gas exchange tank and coupled analytical system. The system allows water-side turbulence in the tank to be precisely controlled with an electronically operated baffle. Two coupled gas chromatographs and an integral equilibrator, connected to the tank in a continuous gas-tight system, allow temporal changes in the partial pressures of SF6, CH4 and N2O to be measured simultaneously in the tank water and headspace at multiple turbulence settings, during a typical experimental run of 3.25 h. PC software developed by the authors controls all operations and data acquisition, enabling the optimisation of experimental conditions with high reproducibility. The use of three gases allows three independent estimates of kw for each turbulence setting; these values are subsequently normalised to a constant Schmidt number for direct comparison. The normalised kw estimates show close agreement. Repeated experiments with Milli-Q water demonstrate a typical measurement accuracy of 4% for kw. Experiments with natural seawater show that the system clearly resolves the effects on kw of spatial and temporal trends in natural surfactant activity. The system is an effective tool with which to probe the relationships between kw, surfactant activity and biogeochemical indices of primary productivity, and should assist in providing valuable new insights into the air-sea gas exchange process.

  15. Microwave radiation as a factor intensifying sample preparation: analysis of samples with an organic matrix

    International Nuclear Information System (INIS)

    Specific features of SHF-(mirowave) decomposition of a sample to ascertain microcomponents in objects with an organic matrix have been considered. The amount of organic substances remaining in solution after decomposition has been evaluated. It has been shown that they do not affect the subsequent determination of metallic impurities by the ICP-AES and ET-AAS methods. Methods of macro- and microcomponents determination in phyto-objects, vegetable oils, biological liquids, perfumery and cosmetics at the level of contents 10-2-10-3% Sr, 10-5-10-6% Cd have been elaborated

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

    OpenAIRE

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

    2016-01-01

    Background 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 f...

  17. An instrument for automated purification of nucleic acids from contaminated forensic samples

    OpenAIRE

    Broemeling, David J; Pel, Joel; Gunn, Dylan C; Mai, Laura; Thompson, Jason D.; Poon, Hiron; Marziali, Andre

    2008-01-01

    Forensic crime scene sample analysis, by its nature, often deals with samples in which there are low amounts of nucleic acids, on substrates that often lead to inhibition of subsequent enzymatic reactions such as PCR amplification for STR profiling. Common substrates include denim from blue jeans, which yields indigo dye as a PCR inhibitor, and soil, which yields humic substances as inhibitors. These inhibitors frequently co-extract with nucleic acids in standard column or bead-based preps, l...

  18. Automated Data Preparation and Physics Mining Tools for Space Weather Studies (Invited)

    Science.gov (United States)

    Karimabadi, H.; Sipes, T.

    2009-12-01

    Heliophysics is a data centric field which relies heavily on the use of spacecraft data for further advances. The prevalent approach to analysis of spacecraft data is based on visual inspection of data. As a result, the vast majority of the collected data from various missions has gone unexplored. The computer aided algorithmic approach to data analysis as facilitated through data mining techniques are essential for analysis of large data sets and enable discovery of hidden information and patterns in the data. Many data analysis problems in space weather stand to benefit from the application of data mining techniques. Examples include identifying spacecraft charging signatures in plasma detectors, identifying plasma frequency lines in wave spectrograms (and hence density), detecting and classifying substorm infection features, among others (R. Friedel, private communication). Thus while the need for advanced algorithmic approach to data exploration and knowledge discovery is generally recognized by experimentalists, the adoption of such techniques (“data mining”) has been slow. This has been partly due to the steep learning curve of some of the techniques and/or the requirement to have a working knowledge of statistics. Another factor is the existence of a plethora of data mining approaches, and it is often a daunting task for a scientist to determine the appropriate technique. Our goal has been to make such tools accessible to non-experts and remove it from gee-whiz domain to a practical tool that will become part of the standard arsenal of data analysis. To this end, we have developed an automated data mining technique called MineTool. Its first deployment to analysis of Cluster has been very successful (Karimabadi et al., JGR, 114, A06216 , 2009) and this tool is gaining adoption among experimentalists. In this talk, we will provide an overview of this tool, illustrate its use through examples, and discuss future directions of research.

  19. Automated Broad-Range Molecular Detection of Bacteria in Clinical Samples.

    Science.gov (United States)

    Budding, Andries E; Hoogewerf, Martine; Vandenbroucke-Grauls, Christina M J E; Savelkoul, Paul H M

    2016-04-01

    Molecular detection methods, such as quantitative PCR (qPCR), have found their way into clinical microbiology laboratories for the detection of an array of pathogens. Most routinely used methods, however, are directed at specific species. Thus, anything that is not explicitly searched for will be missed. This greatly limits the flexibility and universal application of these techniques. We investigated the application of a rapid universal bacterial molecular identification method, IS-pro, to routine patient samples received in a clinical microbiology laboratory. IS-pro is a eubacterial technique based on the detection and categorization of 16S-23S rRNA gene interspace regions with lengths that are specific for each microbial species. As this is an open technique, clinicians do not need to decide in advance what to look for. We compared routine culture to IS-pro using 66 samples sent in for routine bacterial diagnostic testing. The samples were obtained from patients with infections in normally sterile sites (without a resident microbiota). The results were identical in 20 (30%) samples, IS-pro detected more bacterial species than culture in 31 (47%) samples, and five of the 10 culture-negative samples were positive with IS-pro. The case histories of the five patients from whom these culture-negative/IS-pro-positive samples were obtained suggest that the IS-pro findings are highly clinically relevant. Our findings indicate that an open molecular approach, such as IS-pro, may have a high added value for clinical practice. PMID:26763956

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

    International Nuclear Information System (INIS)

    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, 13C, 17O and 31P 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

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

    International Nuclear Information System (INIS)

    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

  2. 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.

  3. A faster sample preparation method for determination of polonium-210 in fish

    International Nuclear Information System (INIS)

    In order to facilitate Health Canada’s study on background radiation levels in country foods, an in-house radio-analytical method has been developed for determination of polonium-210 (210Po) in fish samples. The method was validated by measurement of 210Po in a certified reference material. It was also evaluated by comparing 210Po concentrations in a number of fish samples by another method. The in-house method offers faster sample dissolution using an automated digestion system compared to currently used wet-ashing on a hot plate. It also utilizes pre-packed Sr-resin® cartridges for rapid and reproducible separation of 210Po versus time-consuming manually packed Sr-resin® columns. (author)

  4. [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.

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

    DEFF Research Database (Denmark)

    Handberg, R.; Lund, M. N.

    2014-01-01

    One of the tasks of the Kepler Asteroseismic Science Operations Center (KASOC) is to provide asteroseismic analyses on Kepler Objects of Interest (KOIs). However, asteroseismic analysis of planetary host stars presents some unique complications with respect to data preprocessing, compared to pure...... asteroseismic targets. If not accounted for, the presence of planetary transits in the photometric time series often greatly complicates or even hinders these asteroseismic analyses. This drives the need for specialised methods of preprocessing data to make them suitable for asteroseismic analysis....... 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...

  6. Automatic microemulsion preparation for metals determination in fuel samples using a flow-batch analyzer and graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Cunha, Francisco Antonio S. [Universidade Federal da Paraiba, CCEN, Departamento de Quimica, P. Box 5093, 58051-970, Joao Pessoa, PB (Brazil); Sousa, Rafael A. [Institute of Chemistry-University of Campinas, P.O. Box 6154, 13083-970, Campinas, SP (Brazil); Harding, David P. [Universidade Federal da Paraiba, CCEN, Departamento de Quimica, P. Box 5093, 58051-970, Joao Pessoa, PB (Brazil); Cadore, Solange [Institute of Chemistry-University of Campinas, P.O. Box 6154, 13083-970, Campinas, SP (Brazil); Almeida, Luciano F. [Universidade Federal da Paraiba, CCEN, Departamento de Quimica, P. Box 5093, 58051-970, Joao Pessoa, PB (Brazil); Araujo, Mario Cesar U., E-mail: laqa@quimica.ufpb.br [Universidade Federal da Paraiba, CCEN, Departamento de Quimica, P. Box 5093, 58051-970, Joao Pessoa, PB (Brazil)

    2012-05-21

    Highlights: Black-Right-Pointing-Pointer Micro-emulsion composition phase study to obtain low fuel dilutions. Black-Right-Pointing-Pointer Automated and instantaneous in-line preparation of micro-emulsions for metals determinations. Black-Right-Pointing-Pointer A versatile piston-driven form of 'Flow-batch Analysis'. Black-Right-Pointing-Pointer Rheological considerations explored including a mathematical derivation of flow parameters. - Abstract: The principal thermodynamic advantages of using microemulsions over standard emulsions for flow metal analysis are the greatly increased analyte stability and emulsive homogeneity that improve both the ease of sample preparation, and the analytical result. In this study a piston propelled flow-batch analyzer (PFBA) for the determination of Cu, Cr and Pb in gasoline and naphtha by graphite furnace atomic absorption spectrometry (GF AAS) was explored. Investigative phase modeling for low dilution was conducted both for gasoline and naphtha microemulsions. Rheological considerations were also explored including a mathematical flow derivation to fine tune the system's operational parameters, and the GF AAS coupling. Both manual and automated procedures for microemulsion preparation were compared. The results of the paired t test at a 95% confidence level showed no significant differences between them. Further recovery test results confirmed a negligible matrix effect of the sample on the analyte absorption signals and an efficient stabilization of the samples (with metals) submitted to microemulsion treatment. The accuracy of the developed procedure was attested by good recovery percentages in the ranges of 100.0 {+-} 3.5% for Pb in the naphtha samples, and 100.2 {+-} 3.4% and 100.7 {+-} 4.6% for Cu and Cr, respectively in gasoline samples.

  7. 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.

  8. [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.

  9. Electric transport measurements on bulk, polycrystalline MgB2 samples prepared at various reaction temperatures

    Science.gov (United States)

    Wiederhold, A.; Koblischka, M. R.; Inoue, K.; Muralidhar, M.; Murakami, M.; Hartmann, U.

    2016-03-01

    A series of disk-shaped, bulk MgB2 superconductors (sample diameter up to 4 cm) was prepared in order to improve the performance for superconducting super-magnets. Several samples were fabricated using a solid state reaction in pure Ar atmosphere from 750 to 950oC in order to determine the optimum processing parameters to obtain the highest critical current density as well as large trapped field values. Additional samples were prepared with added silver (up to 10 wt.-%) to the Mg and B powder. Magneto-resistance data and I/V-characteristics were recorded using an Oxford Instruments Teslatron system. From Arrhenius plots, we determine the TAFF pinning potential, U 0. The I/V-characteristics yield detailed information on the current flow through the polycrystalline samples. The current flow is influenced by the presence of pores in the samples. Our analysis of the achieved critical currents together with a thorough microstructure investigation reveals that the samples prepared at temperatures between 775°C and 805°C exhibit the smallest grains and the best connectivity between them, while the samples fabricated at higher reaction temperatures show a reduced connectivity and lower pinning potential. Doping the samples with silver leads to a considerable increase of the pinning potential and hence, the critical current densities.

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

    Science.gov (United States)

    Astakhova, I Kira; Wengel, Jesper

    2013-01-14

    Double-labeled oligonucleotide probes containing fluorophores interacting by energy-transfer mechanisms are essential for modern bioanalysis, molecular diagnostics, and in vivo imaging techniques. Although bright xanthene and cyanine dyes are gaining increased prominence within these fields, little attention has thus far been paid to probes containing these dyes internally attached, a fact which is mainly due to the quite challenging synthesis of such oligonucleotide probes. Herein, by using 2'-O-propargyl uridine phosphoramidite and a series of xanthenes and cyanine azide derivatives, we have 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 of novel oligonucleotide probes containing internally positioned xanthene and cyanine dye pairs and thus represents a significant step forward for the preparation of advanced fluorescent oligonucleotide probes. Furthermore, we demonstrate that the novel xanthene and cyanine labeled probes display unusual and very promising photophysical properties resulting from energy-transfer interactions between the fluorophores controlled by nucleic acid assembly. Potential benefits of using these novel fluorescent probes within, for example, molecular diagnostics and fluorescence microscopy include: Considerable 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 of target detection values (LOD down to <5 nM).

  11. Automated Large Scale Parameter Extraction of Road-Side Trees Sampled by a Laser Mobile Mapping System

    Science.gov (United States)

    Lindenbergh, R. C.; Berthold, D.; Sirmacek, B.; Herrero-Huerta, M.; Wang, J.; Ebersbach, D.

    2015-08-01

    In urbanized Western Europe trees are considered an important component of the built-up environment. This also means that there is an increasing demand for tree inventories. Laser mobile mapping systems provide an efficient and accurate way to sample the 3D road surrounding including notable roadside trees. Indeed, at, say, 50 km/h such systems collect point clouds consisting of half a million points per 100m. Method exists that extract tree parameters from relatively small patches of such data, but a remaining challenge is to operationally extract roadside tree parameters at regional level. For this purpose a workflow is presented as follows: The input point clouds are consecutively downsampled, retiled, classified, segmented into individual trees and upsampled to enable automated extraction of tree location, tree height, canopy diameter and trunk diameter at breast height (DBH). The workflow is implemented to work on a laser mobile mapping data set sampling 100 km of road in Sachsen, Germany and is tested on a stretch of road of 7km long. Along this road, the method detected 315 trees that were considered well detected and 56 clusters of tree points were no individual trees could be identified. Using voxels, the data volume could be reduced by about 97 % in a default scenario. Processing the results of this scenario took ~2500 seconds, corresponding to about 10 km/h, which is getting close to but is still below the acquisition rate which is estimated at 50 km/h.

  12. IHC Profiler: An Open Source Plugin for the Quantitative Evaluation and Automated Scoring of Immunohistochemistry Images of Human Tissue Samples

    Science.gov (United States)

    Malhotra, Renu; De, Abhijit

    2014-01-01

    In anatomic pathology, immunohistochemistry (IHC) serves as a diagnostic and prognostic method for identification of disease markers in tissue samples that directly influences classification and grading the disease, influencing patient management. However, till today over most of the world, pathological analysis of tissue samples remained a time-consuming and subjective procedure, wherein the intensity of antibody staining is manually judged and thus scoring decision is directly influenced by visual bias. This instigated us to design a simple method of automated digital IHC image analysis algorithm for an unbiased, quantitative assessment of antibody staining intensity in tissue sections. As a first step, we adopted the spectral deconvolution method of DAB/hematoxylin color spectra by using optimized optical density vectors of the color deconvolution plugin for proper separation of the DAB color spectra. Then the DAB stained image is displayed in a new window wherein it undergoes pixel-by-pixel analysis, and displays the full profile along with its scoring decision. Based on the mathematical formula conceptualized, the algorithm is thoroughly tested by analyzing scores assigned to thousands (n = 1703) of DAB stained IHC images including sample images taken from human protein atlas web resource. The IHC Profiler plugin developed is compatible with the open resource digital image analysis software, ImageJ, which creates a pixel-by-pixel analysis profile of a digital IHC image and further assigns a score in a four tier system. A comparison study between manual pathological analysis and IHC Profiler resolved in a match of 88.6% (P<0.0001, CI = 95%). This new tool developed for clinical histopathological sample analysis can be adopted globally for scoring most protein targets where the marker protein expression is of cytoplasmic and/or nuclear type. We foresee that this method will minimize the problem of inter-observer variations across labs and further help in

  13. Testing of an automated online EA-IRMS method for fast and simultaneous carbon content and stable isotope measurement of aerosol samples

    Science.gov (United States)

    Major, István; Gyökös, Brigitta; Túri, Marianna; Futó, István; Filep, Ágnes; Hoffer, András; Molnár, Mihály

    2016-04-01

    Comprehensive atmospheric studies have demonstrated that carbonaceous aerosol is one of the main components of atmospheric particulate matter over Europe. Various methods, considering optical or thermal properties, have been developed for quantification of the accurate amount of both organic and elemental carbon constituents of atmospheric aerosol. The aim of our work was to develop an alternative fast and easy method for determination of the total carbon content of individual aerosol samples collected on prebaked quartz filters whereby the mass and surface concentration becomes simply computable. We applied the conventional "elemental analyzer (EA) coupled online with an isotope ratio mass spectrometer (IRMS)" technique which is ubiquitously used in mass spectrometry. Using this technique we are able to measure simultaneously the carbon stable isotope ratio of the samples, as well. During the developing process, we compared the EA-IRMS technique with an off-line catalytic combustion method worked out previously at Hertelendi Laboratory of Environmental Studies (HEKAL). We tested the combined online total carbon content and stable isotope ratio measurement both on standard materials and real aerosol samples. Regarding the test results the novel method assures, on the one hand, at least 95% of carbon recovery yield in a broad total carbon mass range (between 100 and 3000 ug) and, on the other hand, a good reproducibility of stable isotope measurements with an uncertainty of ± 0.2 per mill. Comparing the total carbon results obtained by the EA-IRMS and the off-line catalytic combustion method we found a very good correlation (R2=0.94) that proves the applicability of both preparation method. Advantages of the novel method are the fast and simplified sample preparation steps and the fully automated, simultaneous carbon stable isotope ratio measurement processes. Furthermore stable isotope ratio results can effectively be applied in the source apportionment

  14. Radiostrontium and radium analysis in low-level environmental samples following a multi-stage semi-automated chromatographic sequential separation

    International Nuclear Information System (INIS)

    Strontium isotopes, 89Sr and 90Sr, and 226Ra being radiotoxic when ingested, are routinely monitored in milk and drinking water samples collected from different regions in Canada. In order to monitor environmental levels of activity, a novel semi-automated sensitive method has been developed at the Radiation Protection Bureau of Health Canada (Ottawa, Canada). This method allows the separation and quantification of both 89Sr and 90Sr and has also been adapted to quantify 226Ra during the same sample preparation procedure. The method uses a 2-stage purification process during which matrix constituents, such as magnesium and calcium that are rich in milk, are removed as well as the main beta-interferences (e.g., 40K, 87Rb, 134Cs, 137Cs, and 140Ba). The first purification step uses strong cation exchange (SCX) chromatography with commercially available resins. In a second step, fractions containing the radiostrontium analytes are further purified using high-performance ion chromatography (HPIC). While 89Sr is quantified by Cerenkov counting immediately after the second purification stage, the same vial is counted again after a latent period of 10-14 days to quantify the 90Sr activity based on 90Y ingrowth. Similarly, the activity of 226Ra, which is separated by SCX only, is determined via the emanation of 222Rn in a 2-phase aqueous/cocktail system using liquid scintillation counting. The minimum detectable concentration (MDC) for 89Sr and 90Sr for a 200 min count time at 95% confidence interval is 0.03 and 0.02 Bq/L, respectively. The MDC for 226Ra for a 100 min count time is 0.002 Bq/L. Semi-annual intercomparison samples from the USA Department of Energy Mixed Analyte Performance Evaluation Program (MAPEP) were used to validate the method for 89Sr and 90Sr. Spiked water samples prepared in-house and from International Atomic Energy Agency (IAEA) were used to validate the 226Ra assay.

  15. 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.

  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...

  17. On-chip sample preparation by controlled release of antibodies for simple CD4 counting

    NARCIS (Netherlands)

    Beck, M.; Brockhuis, S.; Velde, van der N.; Breukers, C.; Greve, J.; Terstappen, L.W.M.M.

    2012-01-01

    We present a simple system for CD4 and CD8 counting for point-of-care HIV staging in low-resource settings. Automatic sample preparation is achieved through a dried reagent coating inside a thin (26 μm) counting chamber, allowing the delayed release of fluorochrome conjugated monoclonal antibodies a

  18. QuEChERS sample preparation approach for mass spectrometric analysis of pesticide residues in foods

    Science.gov (United States)

    This chapter describes an easy, rapid, and low-cost sample preparation approach for the determination of pesticide residues in foods using gas and/or liquid chromatographic (GC and/or LC) analytical separation and mass spectrometric (MS) detection. The approach is known as QuEChERS, which stands fo...

  19. 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 t...

  20. Streamlining and automation of radioanalytical methods at a commercial laboratory

    Energy Technology Data Exchange (ETDEWEB)

    Harvey, J.T.; Dillard, J.W. [IT Corp., Knoxville, TN (United States)

    1993-12-31

    Through the careful planning and design of laboratory facilities and incorporation of modern instrumentation and robotics systems, properly trained and competent laboratory associates can efficiently and safely handle radioactive and mixed waste samples. This paper addresses the potential improvements radiochemistry and mixed waste laboratories can achieve utilizing robotics for automated sample analysis. Several examples of automated systems for sample preparation and analysis will be discussed.

  1. 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

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

    International Nuclear Information System (INIS)

    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

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

    Science.gov (United States)

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

    2016-03-01

    Community-level physiological profiling (CLPP) using BIOLOG® EcoPlates™ has become a popular method for characterizing and comparing the functional diversity, functional potential, and metabolic activity of heterotrophic microbial communities. The method was originally developed for profiling soil communities; however, its usage has expanded into the fields of ecotoxicology, agronomy, and the monitoring and profiling of microbial communities in various wastewater treatment systems, including constructed wetlands for water pollution control. When performing CLPP on aqueous samples from constructed wetlands, a wide variety of sample characteristics can be encountered and challenges may arise due to excessive solids, color, or turbidity. The aim of this study was to investigate the impacts of different sample preparation methods on CLPP performed on a variety of aqueous samples covering a broad range of physical and chemical characteristics. The results show that using filter paper, centrifugation, or settling helped clarify samples for subsequent CLPP analysis, however did not do so as effectively as dilution for the darkest samples. Dilution was able to provide suitable clarity for the darkest samples; however, 100-fold dilution significantly affected the carbon source utilization patterns (CSUPs), particularly with samples that were already partially or fully clear. Ten-fold dilution also had some effect on the CSUPs of samples which were originally clear; however, the effect was minimal. Based on these findings, for this specific set of samples, a 10-fold dilution provided a good balance between ease of use, sufficient clarity (for dark samples), and limited effect on CSUPs. The process and findings outlined here can hopefully serve future studies looking to utilize CLPP for functional analysis of microbial communities and also assist in comparing data from studies where different sample preparation methods were utilized. PMID:26563413

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

    Science.gov (United States)

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

    2016-03-01

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

  5. Preparation of samples taken from the Alshar mine for x-ray fluorescence spectrometry (Macedonia)

    International Nuclear Information System (INIS)

    Preparation of samples which contain a large amount of arsenic, antimony and thallium sulphides, by fusion with sodium or lithium tetraborate, for x-ray spectrochemical analysis, could not be applied directly, due to the volatility of the compounds which are of analytical interest and the destruction of Pt-crucibles. To prevent the evaporation of thallium, arsenic and antimony compounds during fusion, two different methods are described: fusion of the sample and the flux with the addition of oxidizing agents; and fusion of the dry residue which remains after dissolving the sample in nitric acid or in 'aqua regia' and evaporation of the excess of acids. (author). 3 refs., 7 tabs

  6. Sample Preparation for Fungal Community Analysis by High-Throughput Sequencing of Barcode Amplicons.

    Science.gov (United States)

    Clemmensen, Karina Engelbrecht; Ihrmark, Katarina; Durling, Mikael Brandström; Lindahl, Björn D

    2016-01-01

    Fungal species participate in vast numbers of processes in the landscape around us. However, their often cryptic growth, inside various substrates and in highly diverse species assemblages, has been a major obstacle to thorough analysis of fungal communities, hampering exhaustive description of the fungal kingdom. Recent technological developments allowing rapid, high-throughput sequencing of mixed communities from many samples at once are currently having a tremendous impact in fungal community ecology. Universal DNA extraction followed by amplification and sequencing of fungal species-level barcodes such as the nuclear internal transcribed spacer (ITS) region now enable identification and relative quantification of fungal community members across well-replicated experimental settings. Here, we present the sample preparation procedure presently used in our laboratory for fungal community analysis by high-throughput sequencing of amplified ITS2 markers. We focus on the procedure optimized for studies of total fungal communities in humus-rich soils, wood, and litter. However, this procedure can be applied to other sample types and markers. We focus on the laboratory-based part of sample preparation, that is, the procedure from the point where samples enter the laboratory until amplicons are submitted for sequencing. Our procedure comprises four main parts: (1) universal DNA extraction, (2) optimization of PCR conditions, (3) production of tagged ITS amplicons, and (4) preparation of the multiplexed amplicon mix to be sequenced. The presented procedure is independent of the specific high-throughput sequencing technology used, which makes it highly versatile. PMID:26791497

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

    Science.gov (United States)

    Xue, Zheng; Lu, Huijie; Liu, Wen-Tso

    2014-01-01

    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.

  8. 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.

  9. Automated Fast Screening Method for Cocaine Identification in Seized Drug Samples Using a Portable Fourier Transform Infrared (FT-IR) Instrument.

    Science.gov (United States)

    Mainali, Dipak; Seelenbinder, John

    2016-05-01

    Quick and presumptive identification of seized drug samples without destroying evidence is necessary for law enforcement officials to control the trafficking and abuse of drugs. This work reports an automated screening method to detect the presence of cocaine in seized samples using portable Fourier transform infrared (FT-IR) spectrometers. The method is based on the identification of well-defined characteristic vibrational frequencies related to the functional group of the cocaine molecule and is fully automated through the use of an expert system. Traditionally, analysts look for key functional group bands in the infrared spectra and characterization of the molecules present is dependent on user interpretation. This implies the need for user expertise, especially in samples that likely are mixtures. As such, this approach is biased and also not suitable for non-experts. The method proposed in this work uses the well-established "center of gravity" peak picking mathematical algorithm and combines it with the conditional reporting feature in MicroLab software to provide an automated method that can be successfully employed by users with varied experience levels. The method reports the confidence level of cocaine present only when a certain number of cocaine related peaks are identified by the automated method. Unlike library search and chemometric methods that are dependent on the library database or the training set samples used to build the calibration model, the proposed method is relatively independent of adulterants and diluents present in the seized mixture. This automated method in combination with a portable FT-IR spectrometer provides law enforcement officials, criminal investigators, or forensic experts a quick field-based prescreening capability for the presence of cocaine in seized drug samples. PMID:27006022

  10. Automated Fast Screening Method for Cocaine Identification in Seized Drug Samples Using a Portable Fourier Transform Infrared (FT-IR) Instrument.

    Science.gov (United States)

    Mainali, Dipak; Seelenbinder, John

    2016-05-01

    Quick and presumptive identification of seized drug samples without destroying evidence is necessary for law enforcement officials to control the trafficking and abuse of drugs. This work reports an automated screening method to detect the presence of cocaine in seized samples using portable Fourier transform infrared (FT-IR) spectrometers. The method is based on the identification of well-defined characteristic vibrational frequencies related to the functional group of the cocaine molecule and is fully automated through the use of an expert system. Traditionally, analysts look for key functional group bands in the infrared spectra and characterization of the molecules present is dependent on user interpretation. This implies the need for user expertise, especially in samples that likely are mixtures. As such, this approach is biased and also not suitable for non-experts. The method proposed in this work uses the well-established "center of gravity" peak picking mathematical algorithm and combines it with the conditional reporting feature in MicroLab software to provide an automated method that can be successfully employed by users with varied experience levels. The method reports the confidence level of cocaine present only when a certain number of cocaine related peaks are identified by the automated method. Unlike library search and chemometric methods that are dependent on the library database or the training set samples used to build the calibration model, the proposed method is relatively independent of adulterants and diluents present in the seized mixture. This automated method in combination with a portable FT-IR spectrometer provides law enforcement officials, criminal investigators, or forensic experts a quick field-based prescreening capability for the presence of cocaine in seized drug samples.

  11. Simultaneous extraction of PCDDs/PCDFs, PCBs and PBDEs. Extension of a sample preparation method for determination of PCDDs/PCDFs

    Energy Technology Data Exchange (ETDEWEB)

    Thomsen, C.; Nicolaysen, T.; Broadwell, S.L.; Haug, L.S.; Becher, G. [Norwegian Institute of Public Health, Oslo (Norway)

    2004-09-15

    Due to emission controls and regulatory measures, the levels of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDDs/PCDFs) and polychlorinated biphenyls (PCBs) have been steadily decreasing in the environment and in human samples the last decades. Nevertheless, the exposure of general populations is still considered to be high and many individuals may have a dietary intake above the established tolerable daily intake. During the recent years, several brominated flame retardants (BFRs) and especially the polybrominated diphenyl ethers (PBDEs) have been shown to be potential persistent organic pollutants (POPs)5. In contrast to PCDDs/PCDFs and PCBs, levels of BFRs seem to be increasing in several environmental compartments. Thus it is of great importance to obtain information on levels of both PCDDs/PCDFs, PCBs and BFRs. Traditionally, PCDDs/PCDFs have been extracted together with the non-ortho PCBs, while extracts of other POPs and PCBs have been prepared separately. Recently, efficient automated methods preparing PCDDs/PCDFs and PCBs extracts at the same time, have been described. A simultaneous sample preparation is advantageous in cases where limited amounts of sample is available, e.g. when analysing human milk or blood, and assures comparable results since the different POPs are determined in exactly the same sample aliquot. Also, due to the low concentration of PCDDs/PCDFs and non-ortho PCBs usually present, a relatively large amount of sample is applied for the extraction, which leads to the possibility of detecting other POPs that are normally not found. We present here a simple and inexpensive extension of our sample preparation method used for determination of PCDDs/PCDFs and non-ortho PCBs that leads to inclusion of both ortho PCBs and PBDEs.

  12. 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.

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

    OpenAIRE

    María S. Di Nezio; Miriam E. Palomeque; Fernández Band, Beatriz S.

    2005-01-01

    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 ap...

  14. Validation of three viable-cell counting methods: Manual, semi-automated, and automated

    Directory of Open Access Journals (Sweden)

    Daniela Cadena-Herrera

    2015-09-01

    Full Text Available A viable cell count is essential to evaluate the kinetics of cell growth. Since the hemocytometer was first used for counting blood cells, several variants of the methodology have been developed towards reducing the time of analysis and improving accuracy through automation of both sample preparation and counting. The successful implementation of automated techniques relies in the adjustment of cell staining, image display parameters and cell morphology to obtain equivalent precision, accuracy and linearity with respect to the hemocytometer. In this study we conducted the validation of three trypan blue exclusion-based methods: manual, semi-automated, and fully automated; which were used for the estimation of density and viability of cells employed for the biosynthesis and bioassays of recombinant proteins. Our results showed that the evaluated attributes remained within the same range for the automated methods with respect to the manual, providing an efficient alternative for analyzing a huge number of samples.

  15. Automatic microemulsion preparation for metals determination in fuel samples using a flow-batch analyzer and graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Cunha, Francisco Antônio S; Sousa, Rafael A; Harding, David P; Cadore, Solange; Almeida, Luciano F; Araújo, Mário César U

    2012-05-21

    The principal thermodynamic advantages of using microemulsions over standard emulsions for flow metal analysis are the greatly increased analyte stability and emulsive homogeneity that improve both the ease of sample preparation, and the analytical result. In this study a piston propelled flow-batch analyzer (PFBA) for the determination of Cu, Cr and Pb in gasoline and naphtha by graphite furnace atomic absorption spectrometry (GF AAS) was explored. Investigative phase modeling for low dilution was conducted both for gasoline and naphtha microemulsions. Rheological considerations were also explored including a mathematical flow derivation to fine tune the system's operational parameters, and the GF AAS coupling. Both manual and automated procedures for microemulsion preparation were compared. The results of the paired t test at a 95% confidence level showed no significant differences between them. Further recovery test results confirmed a negligible matrix effect of the sample on the analyte absorption signals and an efficient stabilization of the samples (with metals) submitted to microemulsion treatment. The accuracy of the developed procedure was attested by good recovery percentages in the ranges of 100.0±3.5% for Pb in the naphtha samples, and 100.2±3.4% and 100.7±4.6% for Cu and Cr, respectively in gasoline samples. PMID:22541820

  16. State-of-the-art technologies for rapid and high-throughput sample preparation and analysis of N-glycans from antibodies.

    Science.gov (United States)

    Aich, Udayanath; Lakbub, Jude; Liu, Aston

    2016-06-01

    Glycosylation is a PTM that occurs during production of many protein-based biologic drugs and can have a profound impact on their biological, clinical, and pharmacological properties. Quality by design, process optimization, and advance in manufacturing technology create a demand for robust, sensitive, and accurate profiling and quantification of antibody glycosylation. Potential drawbacks in antibody glycosylation profiling include the high hands-on time required for sample preparation and several hours for data acquisition and analysis. Rapid and high-throughput (HTP) N-glycan profiling and characterization along with automation for sample preparation and analysis are essential for extensive antibody glycosylation analysis due to the substantial improvement of turnaround time. The first part of this review article will focus on the recent progress in rapid and HTP sample preparation and analysis of antibody glycosylation. Subsequently, the article will cover a brief overview of various separation and mass spectrometric methods for the rapid and HTP analysis of N-glycans in antibodies. Finally, we will discuss the recent developments in process analytical technologies for the screening and quantification of N-glycans in antibodies.

  17. State-of-the-art technologies for rapid and high-throughput sample preparation and analysis of N-glycans from antibodies.

    Science.gov (United States)

    Aich, Udayanath; Lakbub, Jude; Liu, Aston

    2016-06-01

    Glycosylation is a PTM that occurs during production of many protein-based biologic drugs and can have a profound impact on their biological, clinical, and pharmacological properties. Quality by design, process optimization, and advance in manufacturing technology create a demand for robust, sensitive, and accurate profiling and quantification of antibody glycosylation. Potential drawbacks in antibody glycosylation profiling include the high hands-on time required for sample preparation and several hours for data acquisition and analysis. Rapid and high-throughput (HTP) N-glycan profiling and characterization along with automation for sample preparation and analysis are essential for extensive antibody glycosylation analysis due to the substantial improvement of turnaround time. The first part of this review article will focus on the recent progress in rapid and HTP sample preparation and analysis of antibody glycosylation. Subsequently, the article will cover a brief overview of various separation and mass spectrometric methods for the rapid and HTP analysis of N-glycans in antibodies. Finally, we will discuss the recent developments in process analytical technologies for the screening and quantification of N-glycans in antibodies. PMID:26829758

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-09-15

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

  19. Experimental improvements in sample preparation for the track registration technique from dry and solution media

    Energy Technology Data Exchange (ETDEWEB)

    Suarez-Navarro, M.J. [Universidad Politecnica de Madrid (UPM), E.T.S.I de Caminos, Canales y Puertos, Profesor Aranguren s/n, 28040 Madrid (Spain)]. E-mail: he04@caminos.upm.es; Pujol, Ll. [Centro de Estudios y Experimentacion de Obras Publicas (CEDEX), Alfonso XII, 3, 28014 Madrid (Spain); Gonzalez-Gonzalez, J.A. [Universidad Politecnica de Madrid (UPM), E.T.S.I de Caminos, Canales y Puertos, Profesor Aranguren s/n, 28040 Madrid (Spain)

    2006-04-15

    This paper describes the sample preparation studies carried out to determine gross alpha activities in waste materials by means of alpha-particle track counting using CR-39 detector. Sample preparation for the track registration technique using evaporation or electroplating methods (also known as conventional 'dry methods') has a number of drawbacks. The distribution of tracks in different areas of the detector surface is non-uniform, so accurate quantitative determinations depend on tedious and time-consuming counting of tracks under an optical microscope. In this paper, we propose the use of tensioactives in sample preparation to achieve uniform track distribution over the entire detector surface, which enables track density to be evaluated by scanning a small representative area. Under our counting conditions, uniform distribution was achieved with 0.2 ml of Teg from a planchetted source. Furthermore, track registration techniques using solution media (also known as the 'wet methods') and conventional 'dry methods' were analysed and compared with the proposed method. The reproducibility of the procedure described in the study was tested by analysing gross alpha activity in two low-level nuclear waste samples at two different laboratories.

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

    Science.gov (United States)

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

    2015-09-01

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

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

    International Nuclear Information System (INIS)

    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 C18 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)

  3. 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. PMID:26920773

  4. [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. PMID:22827101

  5. 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. PMID:27404623

  6. Sample preparation for the analysis of flavors and off-flavors in foods.

    Science.gov (United States)

    Wilkes, J G; Conte, E D; Kim, Y; Holcomb, M; Sutherland, J B; Miller, D W

    2000-06-01

    Off-flavors in foods may originate from environmental pollutants, the growth of microorganisms, oxidation of lipids, or endogenous enzymatic decomposition in the foods. The chromatographic analysis of flavors and off-flavors in foods usually requires that the samples first be processed to remove as many interfering compounds as possible. For analysis of foods by gas chromatography (GC), sample preparation may include mincing, homogenation, centrifugation, distillation, simple solvent extraction, supercritical fluid extraction, pressurized-fluid extraction, microwave-assisted extraction, Soxhlet extraction, or methylation. For high-performance liquid chromatography of amines in fish, cheese, sausage and olive oil or aldehydes in fruit juice, sample preparation may include solvent extraction and derivatization. Headspace GC analysis of orange juice, fish, dehydrated potatoes, and milk requires almost no sample preparation. Purge-and-trap GC analysis of dairy products, seafoods, and garlic may require heating, microwave-mediated distillation, purging the sample with inert gases and trapping the analytes with Tenax or C18, thermal desorption, cryofocusing, or elution with ethyl acetate. Solid-phase microextraction GC analysis of spices, milk and fish can involve microwave-mediated distillation, and usually requires adsorption on poly(dimethyl)siloxane or electrodeposition on fibers followed by thermal desorption. For short-path thermal desorption GC analysis of spices, herbs, coffee, peanuts, candy, mushrooms, beverages, olive oil, honey, and milk, samples are placed in a glass-lined stainless steel thermal desorption tube, which is purged with helium and then heated gradually to desorb the volatiles for analysis. Few of the methods that are available for analysis of food flavors and off-flavors can be described simultaneously as cheap, easy and good.

  7. Sample preparation for the analysis of flavors and off-flavors in foods.

    Science.gov (United States)

    Wilkes, J G; Conte, E D; Kim, Y; Holcomb, M; Sutherland, J B; Miller, D W

    2000-06-01

    Off-flavors in foods may originate from environmental pollutants, the growth of microorganisms, oxidation of lipids, or endogenous enzymatic decomposition in the foods. The chromatographic analysis of flavors and off-flavors in foods usually requires that the samples first be processed to remove as many interfering compounds as possible. For analysis of foods by gas chromatography (GC), sample preparation may include mincing, homogenation, centrifugation, distillation, simple solvent extraction, supercritical fluid extraction, pressurized-fluid extraction, microwave-assisted extraction, Soxhlet extraction, or methylation. For high-performance liquid chromatography of amines in fish, cheese, sausage and olive oil or aldehydes in fruit juice, sample preparation may include solvent extraction and derivatization. Headspace GC analysis of orange juice, fish, dehydrated potatoes, and milk requires almost no sample preparation. Purge-and-trap GC analysis of dairy products, seafoods, and garlic may require heating, microwave-mediated distillation, purging the sample with inert gases and trapping the analytes with Tenax or C18, thermal desorption, cryofocusing, or elution with ethyl acetate. Solid-phase microextraction GC analysis of spices, milk and fish can involve microwave-mediated distillation, and usually requires adsorption on poly(dimethyl)siloxane or electrodeposition on fibers followed by thermal desorption. For short-path thermal desorption GC analysis of spices, herbs, coffee, peanuts, candy, mushrooms, beverages, olive oil, honey, and milk, samples are placed in a glass-lined stainless steel thermal desorption tube, which is purged with helium and then heated gradually to desorb the volatiles for analysis. Few of the methods that are available for analysis of food flavors and off-flavors can be described simultaneously as cheap, easy and good. PMID:10890508

  8. Evaluation of Sample Stability and Automated DNA Extraction for Fetal Sex Determination Using Cell-Free Fetal DNA in Maternal Plasma

    Directory of Open Access Journals (Sweden)

    Elena Ordoñez

    2013-01-01

    Full Text Available Objective. The detection of paternally inherited sequences in maternal plasma, such as the SRY gene for fetal sexing or RHD for fetal blood group genotyping, is becoming part of daily routine in diagnostic laboratories. Due to the low percentage of fetal DNA, it is crucial to ensure sample stability and the efficiency of DNA extraction. We evaluated blood stability at 4°C for at least 24 hours and automated DNA extraction, for fetal sex determination in maternal plasma. Methods. A total of 158 blood samples were collected, using EDTA-K tubes, from women in their 1st trimester of pregnancy. Samples were kept at 4°C for at least 24 hours before processing. An automated DNA extraction was evaluated, and its efficiency was compared with a standard manual procedure. The SRY marker was used to quantify cfDNA by real-time PCR. Results. Although lower cfDNA amounts were obtained by automated DNA extraction (mean 107,35 GE/mL versus 259,43 GE/mL, the SRY sequence was successfully detected in all 108 samples from pregnancies with male fetuses. Conclusion. We successfully evaluated the suitability of standard blood tubes for the collection of maternal blood and assessed samples to be suitable for analysis at least 24 hours later. This would allow shipping to a central reference laboratory almost from anywhere in Europe.

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

    International Nuclear Information System (INIS)

    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

  10. On the preparation of electron sensor using LiRbSO4 samples

    Science.gov (United States)

    El-Muraikhi, M.; Kassem, M. E.; Gaafar, M.; Abdel Gawad, M. M. H.; Ragab, I. M.

    2005-01-01

    The dielectric spectroscopy of metal-metal sulfate LiRbSO4 samples are described with particular emphasis on sensor performance to be used in the field of radiation. The obtained results as the effect of different electron energy beams at fixed dose, 0.5 Gy, showed abrupt change of the electrical properties (electrical conductivity, capacitance, and loss tangent). The results can be explained on the basis of radiation-induced defects followed by radiation quenching. The prepared samples can be used in the field of radiation dosimeter.

  11. Automation in biological crystallization.

    Science.gov (United States)

    Stewart, Patrick Shaw; Mueller-Dieckmann, Jochen

    2014-06-01

    Crystallization remains the bottleneck in the crystallographic process leading from a gene to a three-dimensional model of the encoded protein or RNA. Automation of the individual steps of a crystallization experiment, from the preparation of crystallization cocktails for initial or optimization screens to the imaging of the experiments, has been the response to address this issue. Today, large high-throughput crystallization facilities, many of them open to the general user community, are capable of setting up thousands of crystallization trials per day. It is thus possible to test multiple constructs of each target for their ability to form crystals on a production-line basis. This has improved success rates and made crystallization much more convenient. High-throughput crystallization, however, cannot relieve users of the task of producing samples of high quality. Moreover, the time gained from eliminating manual preparations must now be invested in the careful evaluation of the increased number of experiments. The latter requires a sophisticated data and laboratory information-management system. A review of the current state of automation at the individual steps of crystallization with specific attention to the automation of optimization is given.

  12. Sample Preparation for in vitro Analysis of Iodine in Thyroid Tissue using X-ray Fluorescence

    Directory of Open Access Journals (Sweden)

    Gertrud Berg

    2008-01-01

    Full Text Available Iodine is enriched and stored in the thyroid gland. Due to several factors, the size of the thyroid iodine pool varies both between individuals and within individuals over time. Excess iodine as well as iodine deficiency may promote thyroid cancer. Therefore, knowledge of iodine content and distribution within thyroid cancer tissue is of interest. X-ray fluorescence analysis (XRF and secondary ion mass spectrometry (SIMS are two methods that can be used to assess iodine content in thyroid tissue. With both techniques, choice of sample preparation affects the results. Aldehyde fixatives are required for SIMS analysis while a freezing method might be satisfactory for XRF analysis. The aims of the present study were primarily to evaluate a simple freezing technique for preserving samples for XRF analysis and also to use XRF to evaluate the efficacy of using aldehyde fixatives to prepare samples for SIMS analysis. Ten porcine thyroids were sectioned into four pieces that were either frozen or fixed in formaldehyde, glutaraldehyde, or a modified Karnovsky fixative. The frozen samples were assessed for iodine content with XRF after 1 and 2 months, and the fixed samples were analyzed for iodine content after 1 week. Freezing of untreated tissue yielded no significant iodine loss, whereas fixation with aldehydes yielded an iodine loss of 14–30%, with Karnovsky producing the least loss.

  13. DNA isolation and sample preparation for quantification of adduct levels by accelerator mass spectrometry.

    Science.gov (United States)

    Dingley, Karen H; Ubick, Esther A; Vogel, John S; Ognibene, Ted J; Malfatti, Michael A; Kulp, Kristen; Haack, Kurt W

    2014-01-01

    Accelerator mass spectrometry (AMS) is a highly sensitive technique used for the quantification of adducts following exposure to carbon-14- or tritium-labeled chemicals, with detection limits in the range of one adduct per 10(11)-10(12) nucleotides. The protocol described in this chapter provides an optimal method for isolating and preparing DNA samples to measure isotope-labeled DNA adducts by AMS. When preparing samples, special precautions must be taken to avoid cross-contamination of isotope among samples and produce a sample that is compatible with AMS. The DNA isolation method described is based upon digestion of tissue with proteinase K, followed by extraction of DNA using Qiagen isolation columns. The extracted DNA is precipitated with isopropanol, washed repeatedly with 70 % ethanol to remove salt, and then dissolved in water. DNA samples are then converted to graphite or titanium hydride and the isotope content measured by AMS to quantify adduct levels. This method has been used to reliably generate good yields of uncontaminated, pure DNA from animal and human tissues for analysis of adduct levels.

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

    Science.gov (United States)

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

    2014-02-15

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

  15. Influence of commonly used primer systems on automated ribosomal intergenic spacer analysis of bacterial communities in environmental samples.

    Directory of Open Access Journals (Sweden)

    Witoon Purahong

    Full Text Available Due to the high diversity of bacteria in many ecosystems, their slow generation times, specific but mostly unknown nutrient requirements and syntrophic interactions, isolation based approaches in microbial ecology mostly fail to describe microbial community structure. Thus, cultivation independent techniques, which rely on directly extracted nucleic acids from the environment, are a well-used alternative. For example, bacterial automated ribosomal intergenic spacer analysis (B-ARISA is one of the widely used methods for fingerprinting bacterial communities after PCR-based amplification of selected regions of the operon coding for rRNA genes using community DNA. However, B-ARISA alone does not provide any taxonomic information and the results may be severely biased in relation to the primer set selection. Furthermore, amplified DNA stemming from mitochondrial or chloroplast templates might strongly bias the obtained fingerprints. In this study, we determined the applicability of three different B-ARISA primer sets to the study of bacterial communities. The results from in silico analysis harnessing publicly available sequence databases showed that all three primer sets tested are specific to bacteria but only two primers sets assure high bacterial taxa coverage (1406f/23Sr and ITSF/ITSReub. Considering the study of bacteria in a plant interface, the primer set ITSF/ITSReub was found to amplify (in silico sequences of some important crop species such as Sorghum bicolor and Zea mays. Bacterial genera and plant species potentially amplified by different primer sets are given. These data were confirmed when DNA extracted from soil and plant samples were analyzed. The presented information could be useful when interpreting existing B-ARISA results and planning B-ARISA experiments, especially when plant DNA can be expected.

  16. Particle analysis for uranium isotopes on swipe samples using new generation Cameca IMS 7f SIMS supported by SEM automated uranium detection

    International Nuclear Information System (INIS)

    Full text: Recent safeguard issues revealed a need for increasing swipe samples analysis capability within the Agency's Network of Analytical Laboratories (NWAL). Our laboratory is qualified for uranium isotopic analysis of particles based on fission track and Thermo-Ionization Mass Spectrometry method (FT-TIMS). In addition, we recently acquired a Secondary Ion Mass Spectrometer (SIMS) in order to broaden particle analysis capabilities in the laboratory. The SIMS technique enables to lower the response time for urgent analysis and to maintain a swipe sample analysis capacity even when our reactor for neutron irradiation is not available. This presentation focuses on the results that have been obtained on swipes particle analysis for uranium isotopes using our new generation Cameca IMS 7f. In this study, all sample processing steps have been examined with the view to improve the reliability of the results and to shorten analytical response time. The IMS 7f instrument mainly differs from other small radius magnetic sector SIMS by ultra high vacuum conditions (-10 mbar in the sample chamber) likely to improve sensitivity as well as to lower hydride ion formation rates. Sensitivity is critical in particle analysis, considering the very small amounts of uranium to be analyzed (∼ a few pg) whereas isobaric interferences due to uranium hydride ions have been shown to cause dramatic artifacts in 236U/238U ratio determination. Particle extraction and sample mounting -- All sample preparation operations have been conducted in a class 10 clean laboratory. A special attention has been paid to the choice of solvents in order to minimize uranium dissolution during liquid-phase particle extraction. Particle suspensions have been deposited and evaporated onto 1 inch diameter carbon disks. Several deposition techniques have been investigated in order to minimize deposition diameters. Sample mountings have been equipped with an internal reference consisting of 2 aluminum foil

  17. Removal of interfering substances in samples prepared for two-dimensional (2-D) electrophoresis.

    Science.gov (United States)

    Berkelman, Tom

    2008-01-01

    Biological samples may contain contaminants that interfere with analysis by two-dimensional (2-D) electrophoresis. Lysates or biological fluids are complex mixtures that contain a wide variety of nonprotein substances in addition to the proteins to be analyzed. These substances often interfere with the resolution of the electrophoretic separation or the visualization of the result. Macromolecules (e.g., polysaccharides and DNA) can interfere with electrophoretic separation by clogging gel pores. Small ionic molecules can impair isoelectric focusing (IEF) separation by rendering the sample too conductive. Other substances (e.g., phenolics and lipids) can bind to proteins, influencing their electrophoretic properties or solubility. In many cases, measures to remove interfering substances can result in significantly clearer 2-D patterns with more visible spots and better resolution. It should be borne in mind, however, that analysis of samples by 2-D electrophoresis is usually most successful and informative when performed with minimally processed samples, so it is important that any steps taken to remove interfering substance be appropriate to the sample and only performed when necessary. Procedures for the removal of interfering substances therefore represent a compromise between removing nonprotein contaminants, and minimizing interference with the integrity and relative abundances of the sample proteins. This chapter presents a number of illustrative examples of optimized sample preparation methods in which specific interfering substances are removed by a variety of different strategies.

  18. 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...... of organic solvent, and into an aqueous receiver solution. The extraction is promoted by application of an electrical field, causing electrokinetic migration of the charged analytes. The method has shown to perform excellent clean-up and selectivity from complicated aqueous matrices like biological fluids....... 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....

  19. 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......, 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...... 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...

  20. Evaluation of neon focused ion beam milling for TEM sample preparation.

    Science.gov (United States)

    Pekin, T C; Allen, F I; Minor, A M

    2016-10-01

    Gallium-based focused ion beams generated from liquid-metal sources are widely used in micromachining and sample preparation for transmission electron microscopy, with well-known drawbacks such as sample damage and contamination. In this work, an alternative (neon) focused ion beam generated by a gas field-ionization source is evaluated for the preparation of electron-transparent specimens. To do so, electron-transparent sections of Si and an Al alloy are prepared with both Ga and Ne ion beams for direct comparison. Diffraction-contrast imaging and energy dispersive x-ray spectroscopy are used to evaluate the relative damage induced by the two beams, and cross-sections of milled trenches are examined to compare the implantation depth with theoretical predictions from Monte Carlo simulations. Our results show that for the beam voltages and materials systems investigated, Ne ion beam milling does not significantly reduce the focused ion beam induced artefacts. However, the Ne ion beam does enable more precise milling and may be of interest in cases where Ga contamination cannot be tolerated.

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

    International Nuclear Information System (INIS)

    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: Cr3+, Fe3+, Ni2+, Cu2+, Zn2+, Se2+, Hg2+, and Pb2+. It was observed that at pH 0, the ions are not adsorbed, but Cu2+ and Zn2+ 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)

  2. Practical Guide to Using Cryoprotectants in Biological Sample Preparation at Cryogenic temperature for Electron Microscopic Studies

    Directory of Open Access Journals (Sweden)

    A-Reum Je

    2011-10-01

    Full Text Available Cryo-fixation enables the preservation of the fine structures of intracellular organelles in a condition that is as close to their native state as possible compared with chemical fixation and room temperature processing. Fixation is the initial step for biological sample preparation in electron microscopy. This step is critically important because the goals of electron microscopic observation are fundamentally dependent on well-preserved specimens resulting from this fixation. In the present work, key components of cryo-fixation, cryoprotectants, are tested with various cell types of interest. The results show that dextran can be easily adapted for use with animal cells and cyanobacteria, whereas 1-hexadecene is applicable to plant and yeast cells. The current report provides useful information on the preparation of cryo-fixed biological specimens using high pressure freezing and freeze-substitution aimed at electron microscopic observation.

  3. Preparation of carbon-nitride bulk samples in the presence of seed carbon-nitride films

    Energy Technology Data Exchange (ETDEWEB)

    Kim, J. I. [Korea University of Technology and Education, Chonan (Korea, Republic of); Zorov, N. B. [Moscow State University, Moscow (Russian Federation)

    2004-05-15

    A procedure was developed for preparing bulk carbon-nitride crystals from polymeric alpha-C{sub 3}N{sub 4.2} at high pressure and high temperature in the presence of seeds of crystalline carbon-nitride films prepared by using a high-voltage discharge plasma combined with pulsed laser ablation of a graphite target. The samples were evaluated by using X-ray photoelectron spectroscopy (XPS), infrared (IR) spectroscopy, Auger electron spectroscopy (AES), secondary-ion mass spectrometry (SIMS), scanning electron microscopy (SEM) and X-ray diffraction (XRD). Notably, XPS studies of the film composition before and after thermobaric treatments demonstrated that the nitrogen composition in the alpha-C{sub 3}N{sub 4.2} material, which initially contained more than 58 % nitrogen, decreased during the annealing process and reached a common, stable composition of approx 45 %. The thermobaric experiments were performed at 10 - 77 kbar and 350 - 1200 .deg. C.

  4. Automated determination of the stable carbon isotopic composition (δ13C) of total dissolved inorganic carbon (DIC) and total nonpurgeable dissolved organic carbon (DOC) in aqueous samples: RSIL lab codes 1851 and 1852

    Science.gov (United States)

    Révész, Kinga M.; Doctor, Daniel H.

    2014-01-01

    The purposes of the Reston Stable Isotope Laboratory (RSIL) lab codes 1851 and 1852 are to determine the total carbon mass and the ratio of the stable isotopes of carbon (δ13C) for total dissolved inorganic carbon (DIC, lab code 1851) and total nonpurgeable dissolved organic carbon (DOC, lab code 1852) in aqueous samples. The analysis procedure is automated according to a method that utilizes a total carbon analyzer as a peripheral sample preparation device for analysis of carbon dioxide (CO2) gas by a continuous-flow isotope ratio mass spectrometer (CF-IRMS). The carbon analyzer produces CO2 and determines the carbon mass in parts per million (ppm) of DIC and DOC in each sample separately, and the CF-IRMS determines the carbon isotope ratio of the produced CO2. This configuration provides a fully automated analysis of total carbon mass and δ13C with no operator intervention, additional sample preparation, or other manual analysis. To determine the DIC, the carbon analyzer transfers a specified sample volume to a heated (70 °C) reaction vessel with a preprogrammed volume of 10% phosphoric acid (H3PO4), which allows the carbonate and bicarbonate species in the sample to dissociate to CO2. The CO2 from the reacted sample is subsequently purged with a flow of helium gas that sweeps the CO2 through an infrared CO2 detector and quantifies the CO2. The CO2 is then carried through a high-temperature (650 °C) scrubber reactor, a series of water traps, and ultimately to the inlet of the mass spectrometer. For the analysis of total dissolved organic carbon, the carbon analyzer performs a second step on the sample in the heated reaction vessel during which a preprogrammed volume of sodium persulfate (Na2S2O8) is added, and the hydroxyl radicals oxidize the organics to CO2. Samples containing 2 ppm to 30,000 ppm of carbon are analyzed. The precision of the carbon isotope analysis is within 0.3 per mill for DIC, and within 0.5 per mill for DOC.

  5. Automated Liquid Microjunction Surface Sampling-HPLC-MS/MS Analysis of Drugs and Metabolites in Whole-Body Thin Tissue Sections

    Energy Technology Data Exchange (ETDEWEB)

    Kertesz, Vilmos [ORNL; Van Berkel, Gary J [ORNL

    2013-01-01

    A fully automated liquid extraction-based surface sampling system utilizing a commercially available autosampler coupled to high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) detection is reported. Discrete spots selected for droplet-based sampling and automated sample queue generation for both the autosampler and MS were enabled by using in-house developed software. In addition, co-registration of spatially resolved sampling position and HPLC-MS information to generate heatmaps of compounds monitored for subsequent data analysis was also available in the software. The system was evaluated with whole-body thin tissue sections from propranolol dosed rat. The hands-free operation of the system was demonstrated by creating heatmaps of the parent drug and its hydroxypropranolol glucuronide metabolites with 1 mm resolution in the areas of interest. The sample throughput was approximately 5 min/sample defined by the time needed for chromatographic separation. The spatial distributions of both the drug and its metabolites were consistent with previous studies employing other liquid extraction-based surface sampling methodologies.

  6. Automated extraction of DNA from blood and PCR setup using a Tecan Freedom EVO liquid handler for forensic genetic STR typing of reference samples.

    Science.gov (United States)

    Stangegaard, Michael; Frøslev, Tobias G; Frank-Hansen, Rune; Hansen, Anders J; Morling, Niels

    2011-04-01

    We have implemented and validated automated protocols for DNA extraction and PCR setup using a Tecan Freedom EVO liquid handler mounted with the Te-MagS magnetic separation device (Tecan, Männedorf, Switzerland). The protocols were validated for accredited forensic genetic work according to ISO 17025 using the Qiagen MagAttract DNA Mini M48 kit (Qiagen GmbH, Hilden, Germany) from fresh whole blood and blood from deceased individuals. The workflow was simplified by returning the DNA extracts to the original tubes minimizing the risk of misplacing samples. The tubes that originally contained the samples were washed with MilliQ water before the return of the DNA extracts. The PCR was setup in 96-well microtiter plates. The methods were validated for the kits: AmpFℓSTR Identifiler, SGM Plus and Yfiler (Applied Biosystems, Foster City, CA), GenePrint FFFL and PowerPlex Y (Promega, Madison, WI). The automated protocols allowed for extraction and addition of PCR master mix of 96 samples within 3.5h. In conclusion, we demonstrated that (1) DNA extraction with magnetic beads and (2) PCR setup for accredited, forensic genetic short tandem repeat typing can be implemented on a simple automated liquid handler leading to the reduction of manual work, and increased quality and throughput. PMID:21609694

  7. On reactivity of metallic zinc used for preparation of samples for hydrogen isotope ratio measurement

    International Nuclear Information System (INIS)

    As the reagent which is suitable to the reduction of water to hydrogen for preparing the samples for hydrogen isotope ratio measurement, the supply of the zinc of BDH Co. which has been widely used so far was stopped, consequently, for the purpose of searching for its substitute, several kinds of metallic zinc were obtained, and their reactivity was examined. As the criteria of the reactivity, the points that the experimental setup used so far can be used and that the accuracy of measurement and efficiency similar to those of heretofore can be obtained were selected, then, it was found that the zinc made by Bio Geochemical Laboratory, Indiana University, and the powder zinc on the market satisfied the criteria. In order to measure hydrogen isotope ratio within the measurement error of ±1%, it is necessary to maintain the quantities of zinc and water to be used and reaction temperature constant, to prepare the standard sample and an unknown sample under the same conditions, and to do the mass analysis as quickly as possible. The researches carried out so far, the reactivity test on various kinds of zinc and so on are reported. The optimum reaction conditions are shown. (K.I.)

  8. Sample preparation for laser-microdissection of soybean shoot apical meristem

    Directory of Open Access Journals (Sweden)

    Chui E. Wong

    2012-10-01

    Full Text Available The shoot apical meristem houses stem cells responsible for the continuous formation of aerial plant organs including leaves and stems throughout the life of plants. Laser-microdissection in combination with high-throughput technology such as next generation sequencing permits an in-depth analysis of molecular events associated with specific cell type of interest. Sample preparation is the most critical step in ensuring good quality RNA to be extracted from samples following laser-microdissection. Here, we optimized the sample preparation for a major legume crop, soybean. We used Farmer’s solution as a fixative and paraffin as the embedding medium for soybean shoot apical meristem tissue without the use of any specialized equipment. Shorter time for tissue fixation (two days was found to be critical for the preservation of RNA in soybean shoot apical meristem. We further demonstrated the utility of this method for different tissues derived from soybean and rice. The method outlined here shall facilitate studies on crop plants involving laser-microdissection.

  9. 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.

  10. Review of sample preparation strategies for MS-based metabolomic studies in industrial biotechnology.

    Science.gov (United States)

    Causon, Tim J; Hann, Stephan

    2016-09-28

    Fermentation and cell culture biotechnology in the form of so-called "cell factories" now play an increasingly significant role in production of both large (e.g. proteins, biopharmaceuticals) and small organic molecules for a wide variety of applications. However, associated metabolic engineering optimisation processes relying on genetic modification of organisms used in cell factories, or alteration of production conditions remain a challenging undertaking for improving the final yield and quality of cell factory products. In addition to genomic, transcriptomic and proteomic workflows, analytical metabolomics continues to play a critical role in studying detailed aspects of critical pathways (e.g. via targeted quantification of metabolites), identification of biosynthetic intermediates, and also for phenotype differentiation and the elucidation of previously unknown pathways (e.g. via non-targeted strategies). However, the diversity of primary and secondary metabolites and the broad concentration ranges encompassed during typical biotechnological processes means that simultaneous extraction and robust analytical determination of all parts of interest of the metabolome is effectively impossible. As the integration of metabolome data with transcriptome and proteome data is an essential goal of both targeted and non-targeted methods addressing production optimisation goals, additional sample preparation steps beyond necessary sampling, quenching and extraction protocols including clean-up, analyte enrichment, and derivatisation are important considerations for some classes of metabolites, especially those present in low concentrations or exhibiting poor stability. This contribution critically assesses the potential of current sample preparation strategies applied in metabolomic studies of industrially-relevant cell factory organisms using mass spectrometry-based platforms primarily coupled to liquid-phase sample introduction (i.e. flow injection, liquid

  11. A study of the Perkin-Elmer laboratory robotic system for analytical sample preparation

    Energy Technology Data Exchange (ETDEWEB)

    Hartenstein, S.D.; Delmastro, J.R.

    1988-09-01

    The purpose of this study was to evaluate the abilities of a Perkin-Elmer (PE) robotic system in performing complex analytical sample preparation procedures. Until this time, reports have been written describing the physical capabilities of the robotic arm marketed by PE and the use of this arm in a pick-and-place application at the Idaho Chemical Processing Plant (ICPP). Since the robotic arm is only capable of handling and transporting objects, the ability of the PE system is dependent upon the performance capabilities of the auxiliary devices marketed with the arm. 2 refs., 2 figs., 1 tab.

  12. Effects of sample preparation conditions on biomolecular solid-state NMR lineshapes

    International Nuclear Information System (INIS)

    Sample preparation conditions with the 46 kDa enzyme complex of 5-enolpyruvyl-shikimate-3-phosphate (EPSP) synthase, shikimate-3-phosphate (S3P) and glyphosate (GLP) have been examined in an attempt to reduce linewidths in solid-state NMR spectra. The linewidths of 13P resonances associated with enzyme bound S3P and GLP in the lyophilized ternary complex have been reduced to 150 ± 12 Hz and 125 ± 7 Hz respectively, by a variety of methods involving additives and freezing techniques

  13. Background and Artifacts Generated by the by the Sample Preparation Experiment on SAM

    Science.gov (United States)

    Belmahdi, Imene; Buch, Arnaud; Szopa, Cyril; Freissinet, Caroline; Glavin, Daniel; Coll, Patrice; Cabane, Michel; Millan, Maeva; Eigenbrode, Jennifer; Navarro-Gonzalez, Rafael; Stern, Jennifer; Coscia, David; Bonnet, Jean-Yves; Teinturier, Samuel; Morisson, Marietta; Stambouli, Moncef; Dequaire, Tristan; Mahaffy, Paul

    2016-04-01

    Sample Analysis at Mars (SAM) is one of the instruments of the Mars Science Laboratory mission. Three analytical devices composed the SAM experiment: 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) and the injection trap (Tenax® GR composed of Tenax® TA and 30% of graphite) are employed to concentrate volatiles released from the sample prior to GC-MS analysis. Our study investigates several propositions for chlorinated hydrocarbon formation detected in the SAM background by looking for: (a) all products coming from the interaction of Tenax® and perchlorates present on Mars, (b) also between some soil sample and perchlorates and (c) sources of chlorinated hydrocarbon precursors. Here we report on the detection of chlorohydrocarbon compounds and their potential origin.

  14. Preparing Electronic Clinical Data for Quality Improvement and Comparative Effectiveness Research: The SCOAP CERTAIN Automation and Validation Project

    Science.gov (United States)

    Devine, Emily Beth; Capurro, Daniel; van Eaton, Erik; Alfonso-Cristancho, Rafael; Devlin, Allison; Yanez, N. David; Yetisgen-Yildiz, Meliha; Flum, David R.; Tarczy-Hornoch, Peter

    2013-01-01

    Background: The field of clinical research informatics includes creation of clinical data repositories (CDRs) used to conduct quality improvement (QI) activities and comparative effectiveness research (CER). Ideally, CDR data are accurately and directly abstracted from disparate electronic health records (EHRs), across diverse health-systems. Objective: Investigators from Washington State’s Surgical Care Outcomes and Assessment Program (SCOAP) Comparative Effectiveness Research Translation Network (CERTAIN) are creating such a CDR. This manuscript describes the automation and validation methods used to create this digital infrastructure. Methods: SCOAP is a QI benchmarking initiative. Data are manually abstracted from EHRs and entered into a data management system. CERTAIN investigators are now deploying Caradigm’s Amalga™ tool to facilitate automated abstraction of data from multiple, disparate EHRs. Concordance is calculated to compare data automatically to manually abstracted. Performance measures are calculated between Amalga and each parent EHR. Validation takes place in repeated loops, with improvements made over time. When automated abstraction reaches the current benchmark for abstraction accuracy - 95% - itwill ‘go-live’ at each site. Progress to Date: A technical analysis was completed at 14 sites. Five sites are contributing; the remaining sites prioritized meeting Meaningful Use criteria. Participating sites are contributing 15–18 unique data feeds, totaling 13 surgical registry use cases. Common feeds are registration, laboratory, transcription/dictation, radiology, and medications. Approximately 50% of 1,320 designated data elements are being automatically abstracted—25% from structured data; 25% from text mining. Conclusion: In semi-automating data abstraction and conducting a rigorous validation, CERTAIN investigators will semi-automate data collection to conduct QI and CER, while advancing the Learning Healthcare System. PMID:25848565

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

    Science.gov (United States)

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

    2015-03-21

    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 analysis to improve the signal-to-noise ratio. Capacitive deionization is an electrostatic desalination (CDI) technique which uses two porous electrodes facing each other to remove ions from a solution. Upon the application of a potential of 0.5 V ions migrate to the electrodes and are stored in the electrical double layer. In this article we demonstrate CDI on a chip, and desalinate a solution by the removal of 23% of Na(+) and Cl(-) ions, while the concentration of a larger molecule (FITC-dextran) remains unchanged. For the first time impedance spectroscopy is introduced to monitor the salt concentration in situ in real-time in between the two desalination electrodes. PMID:25607349

  16. Sample preparation and separation techniques for bioanalysis of morphine and related substances.

    Science.gov (United States)

    Hansen, Steen Honoré

    2009-03-01

    In present time the use or misuse of morphine and its derivatives are monitored by assaying the presence of the drug and its metabolites in biofluids. In the present review, focus is placed on the sample preparation and on the separation techniques used in the current best practices of bioanalysis of morphine and its major metabolites. However, as methods for testing the misuse of heroin, a morphine derivative, often involve bioanalytical methods that cover a number of other illicit drug substances, such methods are also included in the review. Furthermore, the review also includes bioanalysis in a broader perspective as analysis of plant materials, cell cultures and environmental samples. The review is not intended to cover all publications that include bioanalysis of morphine but is more to be considered a view into the current best practices of bioanalysis of morphine, its metabolites and other related substances.

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

    Science.gov (United States)

    Yokochi, Reika

    2016-09-01

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

  18. Performance Evaluation of Fast Microfluidic Thermal Lysis of Bacteria for Diagnostic Sample Preparation

    Directory of Open Access Journals (Sweden)

    Evangelyn C. Alocilja

    2013-01-01

    Full Text Available Development of new diagnostic platforms that incorporate lab-on-a-chip technologies for portable assays is driving the need for rapid, simple, low cost methods to prepare samples for downstream processing or detection. An important component of the sample preparation process is cell lysis. In this work, a simple microfluidic thermal lysis device is used to quickly release intracellular nucleic acids and proteins without the need for additional reagents or beads used in traditional chemical or mechanical methods (e.g., chaotropic salts or bead beating. On-chip lysis is demonstrated in a multi-turn serpentine microchannel with external temperature control via an attached resistive heater. Lysis was confirmed for Escherichia coli by fluorescent viability assay, release of ATP measured with bioluminescent assay, release of DNA measured by fluorometry and qPCR, as well as bacterial culture. Results comparable to standard lysis techniques were achievable at temperatures greater than 65 °C and heating durations between 1 and 60 s.

  19. Matrix compatible solid phase microextraction coating, a greener approach to sample preparation in vegetable matrices.

    Science.gov (United States)

    Naccarato, Attilio; Pawliszyn, Janusz

    2016-09-01

    This work proposes the novel PDMS/DVB/PDMS fiber as a greener strategy for analysis by direct immersion solid phase microextraction (SPME) in vegetables. SPME is an established sample preparation approach that has not yet been adequately explored for food analysis in direct immersion mode due to the limitations of the available commercial coatings. The robustness and endurance of this new coating were investigated by direct immersion extractions in raw blended vegetables without any further sample preparation steps. The PDMS/DVB/PDMS coating exhibited superior features related to the capability of the external PDMS layer to protect the commercial coating, and showed improvements in terms of extraction capability and in the cleanability of the coating surface. In addition to having contributed to the recognition of the superior features of this new fiber concept before commercialization, the outcomes of this work serve to confirm advancements in the matrix compatibility of the PDMS-modified fiber, and open new prospects for the development of greener high-throughput analytical methods in food analysis using solid phase microextraction in the near future.

  20. High-efficiency sample preparation approach to determine acrylamide levels in high-fat foods.

    Science.gov (United States)

    Li, Xiaodan; Li, Jinwei; Cao, Peirang; Liu, Yuanfa

    2016-08-01

    An improved sample preparation method was developed to enhance acrylamide recovery in high-fat foods. Prior to concentration, distilled deionized water was added to protect acrylamide from degradation, resulting in a higher acrylamide recovery rate from fried potato chips. A Chrome-Matrix C18 column (2.6 μm, 2.1 × 100 mm) was used for the first time to analyze acrylamide levels using ultra high performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry, displaying good separation of acrylamide from interference. A solid-phase extraction procedure was avoided, and an average recovery of >89.00% was achieved from different food matrices for three different acrylamide spiking levels. Good reproducibility was observed, with an intraday relative standard deviation of 0.04-2.38%, and an interday relative standard deviation of 2.34-3.26%. Thus, combining the improved sample preparation method for acrylamide analysis with the separation on a Chrome-Matrix C18 column (2.6 μm, 2.1 × 100 mm) using ultra high performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry is highly useful for analyzing acrylamide levels in complex food matrices. PMID:27279364

  1. EVALUATION OF ARG-1 SAMPLES PREPARED BY CESIUM CARBONATE DISSOLUTION DURING THE ISOLOK SME ACCEPTABILITY TESTING

    Energy Technology Data Exchange (ETDEWEB)

    Edwards, T.; Hera, K.; Coleman, C.

    2011-12-05

    Evaluation of Defense Waste Processing Facility (DWPF) Chemical Process Cell (CPC) cycle time identified several opportunities to improve the CPC processing time. The Mechanical Systems & Custom Equipment Development (MS&CED) Section of the Savannah River National Laboratory (SRNL) recently completed the evaluation of one of these opportunities - the possibility of using an Isolok sampling valve as an alternative to the Hydragard valve for taking DWPF process samples at the Slurry Mix Evaporator (SME). The use of an Isolok for SME sampling has the potential to improve operability, reduce maintenance time, and decrease CPC cycle time. The SME acceptability testing for the Isolok was requested in Task Technical Request (TTR) HLW-DWPF-TTR-2010-0036 and was conducted as outlined in Task Technical and Quality Assurance Plan (TTQAP) SRNLRP-2011-00145. RW-0333P QA requirements applied to the task, and the results from the investigation were documented in SRNL-STI-2011-00693. Measurement of the chemical composition of study samples was a critical component of the SME acceptability testing of the Isolok. A sampling and analytical plan supported the investigation with the analytical plan directing that the study samples be prepared by a cesium carbonate (Cs{sub 2}CO{sub 3}) fusion dissolution method and analyzed by Inductively Coupled Plasma - Optical Emission Spectroscopy (ICP-OES). The use of the cesium carbonate preparation method for the Isolok testing provided an opportunity for an additional assessment of this dissolution method, which is being investigated as a potential replacement for the two methods (i.e., sodium peroxide fusion and mixed acid dissolution) that have been used at the DWPF for the analysis of SME samples. Earlier testing of the Cs{sub 2}CO{sub 3} method yielded promising results which led to a TTR from Savannah River Remediation, LLC (SRR) to SRNL for additional support and an associated TTQAP to direct the SRNL efforts. A technical report resulting

  2. Evaluation of sample preparation methods and optimization of nickel determination in vegetable tissues

    Directory of Open Access Journals (Sweden)

    Rodrigo Fernando dos Santos Salazar

    2011-02-01

    Full Text Available Nickel, although essential to plants, may be toxic to plants and animals. It is mainly assimilated by food ingestion. However, information about the average levels of elements (including Ni in edible vegetables from different regions is still scarce in Brazil. The objectives of this study were to: (a evaluate and optimize a method for preparation of vegetable tissue samples for Ni determination; (b optimize the analytical procedures for determination by Flame Atomic Absorption Spectrometry (FAAS and by Electrothermal Atomic Absorption (ETAAS in vegetable samples and (c determine the Ni concentration in vegetables consumed in the cities of Lorena and Taubaté in the Vale do Paraíba, State of São Paulo, Brazil. By means of the analytical technique for determination by ETAAS or FAAS, the results were validated by the test of analyte addition and recovery. The most viable method tested for quantification of this element was HClO4-HNO3 wet digestion. All samples but carrot tissue collected in Lorena contained Ni levels above the permitted by the Brazilian Ministry of Health. The most disturbing results, requiring more detailed studies, were the Ni concentrations measured in carrot samples from Taubaté, where levels were five times higher than permitted by Brazilian regulations.

  3. Preparation of Magnetic Hollow Molecularly Imprinted Polymers for Detection of Triazines in Food Samples.

    Science.gov (United States)

    Wang, Aixiang; Lu, Hongzhi; Xu, Shoufang

    2016-06-22

    Novel magnetic hollow molecularly imprinted polymers (M-H-MIPs) were proposed for highly selective recognition and fast enrichment of triazines in food samples. M-H-MIPs were prepared on the basis of multi-step swelling polymerization, followed by in situ growth of magnetic Fe3O4 nanoparticles on the surface of hollow molecularly imprinted polymers (H-MIPs). Transmission electron microscopy and scanning electron microscopy confirmed the successful immobilization of Fe3O4 nanoparticles on the surface of H-MIPs. M-H-MIPs could be separated simply using an external magnet. The binding adsorption results indicated that M-H-MIPs displayed high binding capacity and fast mass transfer property and class selective property for triazines. Langmuir isotherm and pseudo-second-order kinetic models fitted the best adsorption models for M-H-MIPs. M-H-MIPs were used to analyze atrazine, simazine, propazine, and terbuthylazine in corn, wheat, and soybean samples. Satisfactory recoveries were in the range of 80.62-101.69%, and relative standard deviation was lower than 5.2%. Limits of detection from 0.16 to 0.39 μg L(-1) were obtained. When the method was applied to test positive samples that were contaminated with triazines, the results agree well with those obtained from an accredited method. Thus, the M-H-MIP-based dispersive solid-phase extraction method proved to be a convenient and practical platform for detection of triazines in food samples. PMID:27257079

  4. Preparative divergent flow IEF without carrier ampholytes for separation of complex biological samples.

    Science.gov (United States)

    Stastna, Miroslava; Slais, Karel

    2010-01-01

    Efficient separation method is a crucial part of the process in which components of highly complex biological sample are identified and characterized. Based on the principles of recently newly established electrophoretic method called divergent flow IEF (DF IEF), we have tested the DF IEF instrument which is able to operate without the use of background carrier ampholytes. We have verified that during separation and focusing of sample consisting of high numbers of proteins (yeast lysate and wheat flour extract), the pH gradient of preparative DF IEF can be created by autofocusing of the sample components themselves without any addition of carrier ampholytes. In DF IEF, the proteins are separated, desalted and concentrated in one step. The fractions of yeast lysate sample, collected at the DF IEF output and subjected to gel IEF, contained the zones of proteins gradually covering the pI values from 3.7 to 8.5. In our experimental arrangement, the highest number of proteins has been found in fractions with pI values around 5.3 as detected by polyacrylamide gel IEF with CBB staining. During DF IEF, the selected protein bands have been concentrated up to 16.8-fold.

  5. Determination of bromine, fluorine and iodine in mineral supplements using pyrohydrolysis for sample preparation

    Energy Technology Data Exchange (ETDEWEB)

    Taflik, Ticiane; Antes, Fabiane G.; Paniz, Jose N.G.; Flores, Erico M.M.; Dressler, Valderi L., E-mail: valdres@quimica.ufsm.br [Departamento de Quimica, Universidade Federal de Santa Maria, RS (Brazil); Duarte, Fabio A. [Escola de Quimica e Alimentos, Universidade Federal do Rio Grande, Rio Grande, RS (Brazil); Flores, Eder L.M. [Coordenacao de Engenharia de Alimentos, Universidade Tecnologica Federal do Parana, Medianeira, PR (Brazil)

    2012-03-15

    Pyrohydrolysis was employed for mineral supplements decomposition prior to F, Br and I determination. Fluoride determination was carried out by potentiometry using a fluoride-ion selective electrode, whereas Br and I were determined by inductively coupled plasma mass spectrometry. The main parameters that influence on pyrohydrolysis were investigated. After evaluation, the following conditions were established: reactor temperature of 1000 deg C during 10 min; sample plus accelerator mass ratio of 1 + 5 and carrier gas (air) flow rate of 200 mL min{sup -1} . The accuracy of the proposed method was evaluated by analyte recovery tests and analysis of certified reference materials of phosphate rock and soil. Commercial mineral supplement samples were analyzed. The limits of quantification were 16, 0.3 and 0.07 {mu}g g{sup -1} for F, Br and I, respectively. By using a relatively simple and low cost pyrohydrolysis system up to 5 samples can be processed per hour. The developed sample preparation procedure can be routinely employed for F, Br and I determination in mineral supplements. (author)

  6. Preparation of Biological Samples Containing Metoprolol and Bisoprolol for Applying Methods for Quantitative Analysis

    Directory of Open Access Journals (Sweden)

    Corina Mahu Ştefania

    2015-12-01

    Full Text Available Arterial hypertension is a complex disease with many serious complications, representing a leading cause of mortality. Selective beta-blockers such as metoprolol and bisoprolol are frequently used in the management of hypertension. Numerous analytical methods have been developed for the determination of these substances in biological fluids, such as liquid chromatography coupled with mass spectrometry, gas chromatography coupled with mass spectrometry, high performance liquid chromatography. Due to the complex composition of biological fluids a biological sample pre-treatment before the use of the method for quantitative determination is required in order to remove proteins and potential interferences. The most commonly used methods for processing biological samples containing metoprolol and bisoprolol were identified through a thorough literature search using PubMed, ScienceDirect, and Willey Journals databases. Articles published between years 2005-2015 were reviewed. Protein precipitation, liquid-liquid extraction and solid phase extraction are the main techniques for the extraction of these drugs from plasma, serum, whole blood and urine samples. In addition, numerous other techniques have been developed for the preparation of biological samples, such as dispersive liquid-liquid microextraction, carrier-mediated liquid phase microextraction, hollow fiber-protected liquid phase microextraction, on-line molecularly imprinted solid phase extraction. The analysis of metoprolol and bisoprolol in human plasma, urine and other biological fluids provides important information in clinical and toxicological trials, thus requiring the application of appropriate extraction techniques for the detection of these antihypertensive substances at nanogram and picogram levels.

  7. Preparation of Environmental and Food Samples to Support the Heavy Metals Detection by Stripping Electrochemical

    International Nuclear Information System (INIS)

    Preparation of environmental and food samples to support the heavy metals detection by stripping electrochemistry was done. The water samples taken directly from the ground water were acidified with 1 mL of HNO3 acic suprapure was not digested, while the soils samples which have already dried in the oven at 105 oC, ware grinded and sieved through 150 μm, werte digested with HNO3 acic suprapure in the digestion bomb at 150 oC for 3-4 hours. The mussels samples which have already freezed in the freezer were peeled, dried with N2 liquid, grinded and dried again in the freeze drier at the pressure of ≅ 10-2 mBar, and then were grinded again, weighted, digested with HNO3 acic and HClO4 suprapure in the digestion bomb at 150 oC for 3 hours. Food samples were homogenized by electric mixer, dried with freeze dried, homogenized again by using ZrO2 ball mill, weighted, digested by HPA (high Pressure Asher). The heavy metals in the food samples solution of digestion product were detected by using Polarographic Analyzer EGandG of SWV and DPASV methods, while in the water, soils and the mussels solution were detected by using PDV 2000 and Polarograf E-505, DPASV method. The method validity were tested with SRM materials such as soil-5, soil-7, water W-4, and coppepoda. The heavy metals detection results in the water, soils, mussels, and food by electrochemical method were reported in this paper. (author)

  8. A Method to Prepare a Descemet's Stripping Automated Endothelial Keratoplasty (DSAEK) Graft Using Donor Corneas With Narrow Scleral Rims

    OpenAIRE

    Lin, Tzu-Yu; Hwang, Yih-Shiou; Ma, David Hui-Kang

    2015-01-01

    Abstract Donor corneas with narrow scleral rims are often disqualified for Descemet's Stripping Automated Endothelial Keratoplasty (DSAEK), mainly because of fluid leak and low pressure when they are mounted onto an artificial anterior chamber (AAC). This report describes a novel method to tight-lock a donor cornea with a narrow scleral rim so that microkeratome cutting is possible, allowing a DSAEK procedure to be completed. A 50-year-old male suffering from Epstein–Barr virus (EBV) endothel...

  9. Sample preparation with microwave. Experiences in the environmental- and industrial analytics laboratory of Voest Alpine (P1)

    International Nuclear Information System (INIS)

    Full text: Since around one and a half year two microwave sample preparation units tested and used in the environmental- and industrial analytics laboratory of Voest Alpine. On basis of the experiences the technique offered good results for the specific applications in a steel company. In comparison with the traditional sample preparation of iron oxides for ICP-OES determination through an open vessel wet-chemical acid pulping sample preparation with closed vessel microwave digestion got a large quantity of advantages. The problem with simultaneously sample preparation and determination of silica and other compounds in ultra-pure iron oxides could be solved. We obtained an excellent recovery and reproducibility with microwave pulping. In the range of environmental analytics the possibilities of microwave sample preparation to prepare typical dusts, landfill wastes, process and waste water of a steel company was analyzed. The microwave sample preparation showed good reproducibility to the conventional techniques, e.g. pulping and Soxleth-extraction. Someone of them are already replaced by the new method. Here also the microwave technique possess a large potential for more uses. (author)

  10. Preparation and examination of monolithic in-needle extraction (MINE) device for the direct analysis of liquid samples

    Energy Technology Data Exchange (ETDEWEB)

    Pietrzyńska, Monika, E-mail: monikapietrzynska@gmail.com; Voelkel, Adam; Bielicka-Daszkiewicz, Katarzyna

    2013-05-07

    Graphical abstract: -- Highlights: •MINE device for isolation of analytes from water samples. •Nine polymer poly(styrene-divinylbenzene) monoliths prepared in stainless steel needles. •High efficiency of in-needle extraction systems based on monolithic materials. •New possibilities in sample preparation area. -- Abstract: Combination of extraction and chromatographic techniques opens NEW possibilities in sample preparation area. Macroporous poly(styrene-divinylbenzene) (PS-DVB) monoliths were prepared by in situ polymerization in stainless steel needles. The surface of stainless steel needle was modified earlier by the silane coupling agent. Monolithic materials located inside needles were used as the in-needle extraction device. Scanning electron microscope (SEM) images were obtained for nine monoliths. Spectra of prepared materials were also performed with the use of two techniques: Attenuated Total Reflectance (ATR) and Fourier Transform Infrared Spectroscopy (FTIR). The new monolithic in-needle extraction (MINE) devices were used in the preparation of a series of test water samples for chromatographic analysis. The extraction of phenolic compounds from water samples was carried out by pumping liquid samples through the MINE device. Obtained results indicate a high efficiency of in-needle extraction systems based on monolithic materials. Breakthrough volume and the sorption efficiency of prepared monolithic in-needle extraction devices were determined experimentally. The achieved recovery was close to 90%, and determined LOQ values varied between 0.4 and 6 μg.

  11. Laboratory manual on sample preparation procedures for x-ray micro-analysis

    International Nuclear Information System (INIS)

    X-ray micro fluorescence is a non-destructive and sensitive method for studying the microscopic distribution of different elements in almost all kinds of samples. Since the beginning of this century, x-rays and electrons have been used for the analysis of many different kinds of material. Techniques which rely on electrons are mainly developed for microscopic studies, and are used in conventional Electron Microscopy (EM) or Scanning Electron Microscopy (SEM), while x-rays are widely used for chemical analysis at the microscopic level. The first chemical analysis by fluorescence spectroscopy using small x-ray beams was conducted in 1928 by Glockner and Schreiber. Since then much work has been devoted to developing different types of optical systems for focusing an x-ray beam, but the efficiency of these systems is still inferior to the conventional electron optical systems. However, even with a poor optical efficiency, the x-ray microbeam has many advantages compared with electron or proton induced x-ray emission methods. These include: The analyses are non-destructive, losses of mass are negligible, and due to the low thermal loading of x-rays, materials which may be thermally degraded can be analysed; Samples can be analysed in air, and no vacuum is required, therefore specimens with volatile components such as water in biological samples, can be imaged at normal pressure and temperature; No charging occurs during analysis and therefore coating of the sample with a conductive layer is not necessary; With these advantages, simpler sample preparation procedures including mounting and preservation can be used

  12. Using Exclusion-Based Sample Preparation (ESP to Reduce Viral Load Assay Cost.

    Directory of Open Access Journals (Sweden)

    Scott M Berry

    Full Text Available Viral load (VL measurements are critical to the proper management of HIV in developing countries. However, access to VL assays is limited by the high cost and complexity of existing assays. While there is a need for low cost VL assays, performance must not be compromised. Thus, new assays must be validated on metrics of limit of detection (LOD, accuracy, and dynamic range. Patient plasma samples from the Joint Clinical Research Centre in Uganda were de-identified and measured using both an existing VL assay (Abbott RealTime HIV-1 and our assay, which combines low cost reagents with a simplified method of RNA isolation termed Exclusion-Based Sample Preparation (ESP.71 patient samples with VLs ranging from 3,000,000 copies/mL were used to compare the two methods. We demonstrated equivalent LOD (~50 copies/mL and high accuracy (average difference between methods of 0.08 log, R2 = 0.97. Using expenditures from this trial, we estimate that the cost of the reagents and consumables for this assay to be approximately $5 USD. As cost is a significant barrier to implementation of VL testing, we anticipate that our assay will enhance access to this critical monitoring test in developing countries.

  13. Modular approach to customise sample preparation procedures for viral metagenomics: a reproducible protocol for virome analysis.

    Science.gov (United States)

    Conceição-Neto, Nádia; Zeller, Mark; Lefrère, Hanne; De Bruyn, Pieter; Beller, Leen; Deboutte, Ward; Yinda, Claude Kwe; Lavigne, Rob; Maes, Piet; Van Ranst, Marc; Heylen, Elisabeth; Matthijnssens, Jelle

    2015-11-12

    A major limitation for better understanding the role of the human gut virome in health and disease is the lack of validated methods that allow high throughput virome analysis. To overcome this, we evaluated the quantitative effect of homogenisation, centrifugation, filtration, chloroform treatment and random amplification on a mock-virome (containing nine highly diverse viruses) and a bacterial mock-community (containing four faecal bacterial species) using quantitative PCR and next-generation sequencing. This resulted in an optimised protocol that was able to recover all viruses present in the mock-virome and strongly alters the ratio of viral versus bacterial and 16S rRNA genetic material in favour of viruses (from 43.2% to 96.7% viral reads and from 47.6% to 0.19% bacterial reads). Furthermore, our study indicated that most of the currently used virome protocols, using small filter pores and/or stringent centrifugation conditions may have largely overlooked large viruses present in viromes. We propose NetoVIR (Novel enrichment technique of VIRomes), which allows for a fast, reproducible and high throughput sample preparation for viral metagenomics studies, introducing minimal bias. This procedure is optimised mainly for faecal samples, but with appropriate concentration steps can also be used for other sample types with lower initial viral loads.

  14. Sample Preparation for Headspace GC Analysis of Residual Solvents in Hyaluronic Acid Derivative Fiber

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Hoon Joo; Kim, Dong Min; Yang, Jeong Soo [LG life Sciences, Ltd./R and D Park, Daejeon (Korea, Republic of); Kim, Chan Wha [Korea University, Seoul (Korea, Republic of)

    2006-02-15

    The aim of this study is to develop efficient sample preparation method for HS-GC analysis of residual solvents in HA derivative fiber. Compared to direct extraction of residual solvents from HA derivative fiber, the extraction through the hydrolysis of HA derivative fiber by HAse gave more complete and higher reproducible quantification of residual solvent. To validate HS-GC analysis method of residual solvents, specificity, limits of detection and quantification, linearity, accuracy and precision are investigated in the study. HA derivative fiber was hydrolyzed using HAse for headspace gas chromatographic analysis of residual solvents of ethanol, acetone and isopropanol in HA derivative fiber. This study showed that the developed method had specificity, linearity, accuracy and precision. In addition, it demonstrated that HS-GC coupled with matrix-breaking method such as hydrolysis was available for the determination of residual solvents in a matrix like HA derivative fiber.

  15. Preparation and Application of Novel Magnetic Molecularly Imprinted Composites for Recognition of Sulfadimethoxine in Feed Samples.

    Science.gov (United States)

    Feng, Min; Li, Hengye; Zhang, Lin; Zhang, Jingyou; Dai, Jianping; Wang, Xiaojin; Zhang, Lingli; Wei, Yunji

    2016-01-01

    Novel magnetic molecularly imprinted composites were prepared through a facile method using sulfadimethoxine (SDM) as template. The inorganic magnetic nanoparticles were linked with the organic molecularly imprinted polymer (MIP) through irreversibly covalent bond. So, the resulted composites showed excellent stability and reusability under acidic elution conditions. The magnetic MIP composites showed good selectivity, high binding capacity and excellent kinetics toward SDM. Adopting the magnetic MIP composites as extraction material, an off-line magnetic solid-phase extraction (SPE)/high performance liquid chromatography (HPLC) method was established. The calibration curve was linear in the range of 0.05 - 15 mg kg(-1) (r(2) = 0.9976). The LOD and LOQ were 0.016 and 0.052 mg kg(-1), respectively, while the recoveries were in the range of 89.3 - 107.0%. These novel magnetic MIP composites may become a powerful tool for the extraction of template from complex samples with good efficiency. PMID:27169650

  16. Agarose- and alginate-based biopolymers for sample preparation: Excellent green extraction tools for this century.

    Science.gov (United States)

    Sanagi, Mohd Marsin; Loh, Saw Hong; Wan Ibrahim, Wan Nazihah; Pourmand, Neda; Salisu, Ahmed; Wan Ibrahim, Wan Aini; Ali, Imran

    2016-03-01

    Recently, there has been considerable interest in the use of miniaturized sample preparation techniques before the chromatographic monitoring of the analytes in unknown complex compositions. The use of biopolymer-based sorbents in solid-phase microextraction techniques has achieved a good reputation. A great variety of polysaccharides can be extracted from marine plants or microorganisms. Seaweeds are the major sources of polysaccharides such as alginate, agar, agarose, as well as carrageenans. Agarose and alginate (green biopolymers) have been manipulated for different microextraction approaches. The present review is focused on the classification of biopolymer and their applications in multidisciplinary research. Besides, efforts have been made to discuss the state-of-the-art of the new microextraction techniques that utilize commercial biopolymer interfaces such as agarose in liquid-phase microextraction and solid-phase microextraction.

  17. Preparation of 15N labelled protein sample by gene engineering technology

    International Nuclear Information System (INIS)

    Using the advanced multi-dimension heteronuclear pulses and isotope labelled protein technique, nuclear magnetic resonance spectroscopy has become an important tool in analysis of the solution conformation of protein. On the basis of the high level expression of a protein-trichosanthin in recombinant E.coli using DNA, 15N was used to label the protein, the 15N labelled trichosanthin was obtained by affinity chromatography on Ni-NTA agarose. Terminating pregnant effect in mice showed that this recombinant protein had the same activity as natural trichosanthin. A 1H-15N heteronuclear single-quantum coherence (HSQC) spectrum was obtained from an AM-500 NMR spectrometer, demonstrating that this method is suitable in preparing labelled protein sample for NMR

  18. Shear mechanical anisotropy of side chain liquid-crystal elastomers: Influence of sample preparation

    Science.gov (United States)

    Rogez, D.; Francius, G.; Finkelmann, H.; Martinoty, P.

    2006-08-01

    We study the mechanical anisotropy of a series of uniaxial side chain nematic elastomers prepared with the same chemical composition but with different preparation protocols. For all the compounds, the experiments performed as a function of temperature show no discontinuity in both G'// and G'⊥ (the labels // and ⊥ stand for the director parallel, respectively perpendicular to the shear displacement) around the nematic-isotropic (N-I) phase transition temperature determined by DSC. They also all show a small decrease in G'// starting at temperatures well above this temperature (from ˜ 4°C to ˜ 20°C depending on the compound studied) and leading to a small hydrodynamic value of the G'⊥/G'// ratio. The measurements taken as a function of frequency show that the second plateau in G'// and the associated dip in G//” expected from dynamic semi-soft elasticity are not observed. These results can be described by the de Gennes model, which predicts small elastic anisotropy in the hydrodynamic and linear regimes. They correspond to the behavior expected for compounds beyond the mechanical critical point, which is consistent with the NMR and specific heat measurements taken on similar compounds. We also show that a reduction in the cross-linking density does not change the non-soft character of the mechanical response. From the measurements taken as a function of frequency at several temperatures we deduce that the time-temperature superposition method does not apply. From these measurements, we also determine the temperature dependence of the longest relaxation time τE of the network for the situations where the director is either parallel or perpendicular to the shear velocity. Finally, we discuss the influence on the measurements of the mechanical constraint associated with the fact that the samples cannot change their shape around the pseudo phase transition, because of their strong adherence on the sample-bearing glass slides.

  19. Determination of Cd and Pb in food slurries by GFAAS using cryogenic grinding for sample preparation

    Energy Technology Data Exchange (ETDEWEB)

    Santos, D. Jr.; Barbosa, F. Jr.; Tomazelli, A.C.; Krug, F.J. [Centro de Energia Nuclear na Agricultura, Piracicaba (Brazil); Nobrega, J.A. [Departamento de Quimica, UFSCar, Sao Carlos (Brazil); Arruda, M.A.Z. [Instituto de Quimica, UNICAMP, Campinas (Brazil)

    2002-06-01

    A simple method combining slurry sampling after cryogenic grinding and the use of a permanent modification of the integrated platform inside the transversely heated graphite atomizer (THGA) was proposed for the determination of Cd and Pb in foods. Potentialities of the cryogenic grinding were evaluated for grinding different materials of difficult homogenization such as high fat and high fiber tissues. Animal and vegetal samples were cut into small pieces and ground in liquid nitrogen for 2 min. Slurries were prepared directly in the autosampler cup after cryogenic grinding by transferring an exact amount of homogeneous powdered material (5-20 mg) to the cup, followed by 1.00 mL of 0.2% (v/v) HNO{sub 3} containing 0.04% (v/v) Triton X-100 and sonication for 30 s, before transferring into the platform previously coated with 250 {mu}g W and 200 {mu}g Rh. Use of a tungsten carbide-rhodium permanent modifier combined with NH{sub 4}H{sub 2}PO{sub 4} conventional modifier improves tube lifetime and increases the pyrolysis temperature for Cd. Homogeneity tests, carried out by comparing the between- and within-batch precision for each kind of sample, showed no significant differences at the 95% confidence level, indicating good homogeneity for 5-20 mg masses. Detection limits were 3.3 ng g{sup -1} Cd and 75 ng g{sup -1} Pb for 1% m/v slurries. Results for determination of Cd and Pb in foods slurries were in agreement with those obtained with digested samples, since no statistical differences were found by the paired t-test at the 95% level. (orig.)

  20. State of the art of environmentally friendly sample preparation approaches for determination of PBDEs and metabolites in environmental and biological samples: A critical review.

    Science.gov (United States)

    Berton, Paula; Lana, Nerina B; Ríos, Juan M; García-Reyes, Juan F; Altamirano, Jorgelina C

    2016-01-28

    Green chemistry principles for developing methodologies have gained attention in analytical chemistry in recent decades. A growing number of analytical techniques have been proposed for determination of organic persistent pollutants in environmental and biological samples. In this light, the current review aims to present state-of-the-art sample preparation approaches based on green analytical principles proposed for the determination of polybrominated diphenyl ethers (PBDEs) and metabolites (OH-PBDEs and MeO-PBDEs) in environmental and biological samples. Approaches to lower the solvent consumption and accelerate the extraction, such as pressurized liquid extraction, microwave-assisted extraction, and ultrasound-assisted extraction, are discussed in this review. Special attention is paid to miniaturized sample preparation methodologies and strategies proposed to reduce organic solvent consumption. Additionally, extraction techniques based on alternative solvents (surfactants, supercritical fluids, or ionic liquids) are also commented in this work, even though these are scarcely used for determination of PBDEs. In addition to liquid-based extraction techniques, solid-based analytical techniques are also addressed. The development of greener, faster and simpler sample preparation approaches has increased in recent years (2003-2013). Among green extraction techniques, those based on the liquid phase predominate over those based on the solid phase (71% vs. 29%, respectively). For solid samples, solvent assisted extraction techniques are preferred for leaching of PBDEs, and liquid phase microextraction techniques are mostly used for liquid samples. Likewise, green characteristics of the instrumental analysis used after the extraction and clean-up steps are briefly discussed.

  1. Investigation into Alternative Sample Preparation Techniques for the Determination of Heavy Metals in Stationary Source Emission Samples Collected on Quartz Filters

    Directory of Open Access Journals (Sweden)

    Sharon L. Goddard

    2014-11-01

    Full Text Available Monitoring stationary source emissions for heavy metals generally requires the use of quartz filters to collect samples because of the high temperature and high moisture sampling environment. The documentary standard method sample preparation technique in Europe, EN 14385, uses digestion in hydrofluoric acid and nitric acid (HF/HNO3 followed by complexing with boric acid (H3BO3 prior to analysis. However, the use of this method presents a number of problems, including significant instrumental drift during analysis caused by the matrix components, often leading to instrument breakdown and downtime for repairs, as well as posing significant health and safety risks. The aim of this work was to develop an alternative sample preparation technique for emissions samples on quartz filters. The alternative techniques considered were: (i acid digestion in a fluoroboric acid (HBF4 and HNO3 mixture and (ii acid extraction in an aqua regia (AR mixture (HCl and HNO3. Assessment of the effectiveness of these options included determination of interferences and signal drift, as well as validating the different methods by measurement of matrix certified reference materials (CRMs, and comparing the results obtained from real test samples and sample blanks to determine limits of detection. The results showed that the HBF4/HNO3 mixture provides the most viable alternative to the documentary standard preparation technique.

  2. Preparation of chitosan grafted graphite composite for sensitive detection of dopamine in biological samples.

    Science.gov (United States)

    Palanisamy, Selvakumar; Thangavelu, Kokulnathan; Chen, Shen-Ming; Gnanaprakasam, P; Velusamy, Vijayalakshmi; Liu, Xiao-Heng

    2016-10-20

    The accurate detection of dopamine (DA) levels in biological samples such as human serum and urine are essential indicators in medical diagnostics. In this work, we describe the preparation of chitosan (CS) biopolymer grafted graphite (GR) composite for the sensitive and lower potential detection of DA in its sub micromolar levels. The composite modified electrode has been used for the detection of DA in biological samples such as human serum and urine. The GR-CS composite modified electrode shows an enhanced oxidation peak current response and low oxidation potential for the detection of DA than that of electrodes modified with bare, GR and CS discretely. Under optimum conditions, the fabricated GR-CS composite modified electrode shows the DPV response of DA in the linear response ranging from 0.03 to 20.06μM. The detection limit and sensitivity of the sensor were estimated as 0.0045μM and 6.06μA μM(-1)cm(-2), respectively. PMID:27474582

  3. Critical comparison of sample preparation strategies for shotgun proteomic analysis of formalin-fixed, paraffin-embedded samples: insights from liver tissue

    OpenAIRE

    Tanca, Alessandro; Abbondio, Marcello; Pisanu, Salvatore; Pagnozzi, Daniela; Uzzau, Sergio; Addis, Maria Filippa

    2014-01-01

    Background The growing field of formalin-fixed paraffin-embedded (FFPE) tissue proteomics holds promise for improving translational research. Direct tissue trypsinization (DT) and protein extraction followed by in solution digestion (ISD) or filter-aided sample preparation (FASP) are the most common workflows for shotgun analysis of FFPE samples, but a critical comparison of the different methods is currently lacking. Experimental design DT, FASP and ISD workflows were compared by subjecting ...

  4. New Sample Preparation Method for Quantification of Phenolic Compounds of Tea (Camellia sinensis L. Kuntze: A Polyphenol Rich Plant

    Directory of Open Access Journals (Sweden)

    P. A. Nimal Punyasiri

    2015-01-01

    Full Text Available Chemical analysis of the Sri Lankan tea (Camellia sinensis, L. germplasm would immensely contribute to the success of the tea breeding programme. However, the polyphenols, particularly catechins (flavan-3-ols, are readily prone to oxidation in the conventional method of sample preparation. Therefore, optimization of the present sample preparation methodology for the profiling of metabolites is much important. Two sample preparation methodologies were compared, fresh leaves (as in the conventional procedures and freeze-dried leaves (a new procedure, for quantification of major metabolites by employing two cultivars, one is known to be high quality black tea and the other low quality black tea. The amounts of major metabolites such as catechins, caffeine, gallic acid, and theobromine, recorded in the new sampling procedure via freeze-dried leaves, were significantly higher than those recorded in the conventional sample preparation procedure. Additionally new method required less amount of leaf sample for analysis of major metabolites and facilitates storage of samples until analysis. The freeze-dried method would be useful for high throughput analysis of large number of samples in shorter period without chemical deterioration starting from the point of harvest until usage. Hence, this method is more suitable for metabolite profiling of tea as well as other phenol rich plants.

  5. Solvent-assisted dispersive solid-phase extraction: A sample preparation method for trace detection of diazinon in urine and environmental water samples.

    Science.gov (United States)

    Aladaghlo, Zolfaghar; Fakhari, Alireza; Behbahani, Mohammad

    2016-09-01

    In this research, a sample preparation method termed solvent-assisted dispersive solid-phase extraction (SA-DSPE) was applied. The used sample preparation method was based on the dispersion of the sorbent into the aqueous sample to maximize the interaction surface. In this approach, the dispersion of the sorbent at a very low milligram level was received by inserting a solution of the sorbent and disperser solvent into the aqueous sample. The cloudy solution created from the dispersion of the sorbent in the bulk aqueous sample. After pre-concentration of the diazinon, the cloudy solution was centrifuged and diazinon in the sediment phase dissolved in ethanol and determined by gas chromatography-flame ionization detector. Under the optimized conditions (pH of solution=7.0, Sorbent: benzophenone, 2%, Disperser solvent: ethanol, 500μL, Centrifuge: centrifuged at 4000rpm for 3min), the method detection limit for diazinon was 0.2, 0.3, 0.3 and 0.3μgL(-1) for distilled water, lake water, waste water and urine sample, respectively. Furthermore, the pre-concentration factor was 363.8, 356.1, 360.7 and 353.38 in distilled water, waste water, lake water and urine sample, respectively. SA-DSPE was successfully used for trace monitoring of diazinon in urine, lake and waste water samples. PMID:27495366

  6. Estimation of uranium in columbite-tantalite samples: a method for sample solution preparation for fluorimetric estimation

    International Nuclear Information System (INIS)

    A method has been developed for obtaining a clear solution of columbite-tantalite samples in nitric acid medium before the fluorimetric estimation of uranium. Ammonium hydrogen fluoride is used to keep tantalum, niobium and titanium dissolved in the acid medium. The excess of fluoride is complexed with boric acid. The method has been successfully applied to a number of synthetic and natural columbite-tantalite samples. (author)

  7. Humidity-controlled preparation of frozen-hydrated biological samples for cryogenic coherent x-ray diffraction microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Takayama, Yuki; Nakasako, Masayoshi [Department of Physics, Faculty of Science and Technology, Keio University, 3-14-1 Hiyoshi, Kohoku-ku, Kanagawa 223-8522 (Japan); RIKEN Harima Institute/SPring-8, 1-1-1 Kouto, Mikaduki, Sayo, Hyogo 679-5148 (Japan)

    2012-05-15

    Coherent x-ray diffraction microscopy (CXDM) has the potential to visualize the structures of micro- to sub-micrometer-sized biological particles, such as cells and organelles, at high resolution. Toward advancing structural studies on the functional states of such particles, here, we developed a system for the preparation of frozen-hydrated biological samples for cryogenic CXDM experiments. The system, which comprised a moist air generator, microscope, micro-injector mounted on a micromanipulator, custom-made sample preparation chamber, and flash-cooling device, allowed for the manipulation of sample particles in the relative humidity range of 20%-94%rh at 293 K to maintain their hydrated and functional states. Here, we report the details of the system and the operation procedure, including its application to the preparation of a frozen-hydrated chloroplast sample. Sample quality was evaluated through a cryogenic CXDM experiment conducted at BL29XUL of SPring-8. Taking the performance of the system and the quality of the sample, the system was suitable to prepare frozen-hydrated biological samples for cryogenic CXDM experiments.

  8. The AS-76 interlaboratory experiment on the alpha spectrometric determinaion of Pu-238. Part 3: Preparation and characterization of samples

    International Nuclear Information System (INIS)

    Four plutonium samples containing 0.2, 0.8, 1.6 and 0.9 atom % of 238Pu have been prepared for the Interlaboratory Experiment AS-76. Of these three were input solutions from a reprocessing plant. The fourth sample was from a plutonium product solution. These samples have been characterized by two alpha spectrometry laboratories and two mass spectrometry laboratories to certify the ratio of alpha activities 238Pu/(239Pu + 240Pu) and the isotopic composition, respectively

  9. Automated extraction of DNA from blood and PCR setup using a Tecan Freedom EVO liquid handler for forensic genetic STR typing of reference samples

    DEFF Research Database (Denmark)

    Stangegaard, Michael; Frøslev, Tobias G; Frank-Hansen, Rune;

    2011-01-01

    We have implemented and validated automated protocols for DNA extraction and PCR setup using a Tecan Freedom EVO liquid handler mounted with the Te-MagS magnetic separation device (Tecan, Männedorf, Switzerland). The protocols were validated for accredited forensic genetic work according to ISO...... 17025 using the Qiagen MagAttract DNA Mini M48 kit (Qiagen GmbH, Hilden, Germany) from fresh whole blood and blood from deceased individuals. The workflow was simplified by returning the DNA extracts to the original tubes minimizing the risk of misplacing samples. The tubes that originally contained...... the samples were washed with MilliQ water before the return of the DNA extracts. The PCR was setup in 96-well microtiter plates. The methods were validated for the kits: AmpFlSTR Identifiler, SGM Plus and Yfiler (Applied Biosystems, Foster City, CA), GenePrint FFFL and PowerPlex Y (Promega, Madison, WI...

  10. A timer inventory based upon manual and automated analysis of ERTS-1 and supporting aircraft data using multistage probability sampling. [Plumas National Forest, California

    Science.gov (United States)

    Nichols, J. D.; Gialdini, M.; Jaakkola, S.

    1974-01-01

    A quasi-operational study demonstrating that a timber inventory based on manual and automated analysis of ERTS-1, supporting aircraft data and ground data was made using multistage sampling techniques. The inventory proved to be a timely, cost effective alternative to conventional timber inventory techniques. The timber volume on the Quincy Ranger District of the Plumas National Forest was estimated to be 2.44 billion board feet with a sampling error of 8.2 percent. Costs per acre for the inventory procedure at 1.1 cent/acre compared favorably with the costs of a conventional inventory at 25 cents/acre. A point-by-point comparison of CALSCAN-classified ERTS data with human-interpreted low altitude photo plots indicated no significant differences in the overall classification accuracies.

  11. Remote monitoring field trial. Application to automated air sampling. Report on Task FIN-E935 of the Finnish Support Programme to IAEA Safeguards

    International Nuclear Information System (INIS)

    An automated air sampling station has recently been developed by Radiation and Nuclear Safety Authority (STUK). The station is furnished with equipment that allows comprehensive remote monitoring of the station and the data. Under the Finnish Support Programme to IAEA Safeguards, STUK and Sandia National Laboratories (SNL) established a field trial to demonstrate the use of remote monitoring technologies. STUK provided means for real-lime radiation monitoring and sample authentication whereas SNL delivered means for authenticated surveillance of the equipment and its location. The field trial showed that remote monitoring can be carried out using simple means although advanced facilities are needed for comprehensive surveillance. Authenticated measurement data could be reliably transferred from the monitoring site to the headquarters without the presence of authorized personnel in the monitoring site. The operation of the station and the remote monitoring system were reliable. (orig.)

  12. Surface Cleaning Techniques: Ultra-Trace ICP-MS Sample Preparation and Assay of HDPE

    Energy Technology Data Exchange (ETDEWEB)

    Overman, Nicole R.; Hoppe, Eric W.; Addleman, Raymond S.

    2013-06-01

    The world’s most sensitive radiation detection and assay systems depend upon ultra-low background (ULB) materials to reduce unwanted radiological backgrounds. Herein, we evaluate methods to clean HDPE, a material of interest to ULB systems and the means to provide rapid assay of surface and bulk contamination. ULB level material and ultra-trace level detection of actinide elements is difficult to attain, due to the introduction of contamination from sample preparation equipment such as pipette tips, sample vials, forceps, etc. and airborne particulate. To date, literature available on the cleaning of such polymeric materials and equipment for ULB applications and ultra-trace analyses is limited. For these reasons, a study has been performed to identify an effective way to remove surface contamination from polymers in an effort to provide improved instrumental detection limits. Inductively Coupled Plasma Mass Spectroscopy (ICP-MS) was utilized to assess the effectiveness of a variety of leachate solutions for removal of inorganic uranium and thorium surface contamination from polymers, specifically high density polyethylene (HDPE). HDPE leaching procedures were tested to optimize contaminant removal of thorium and uranium. Calibration curves for thorium and uranium ranged from 15 ppq (fg/mL) to 1 ppt (pg/mL). Detection limits were calculated at 6 ppq for uranium and 7 ppq for thorium. Results showed the most effective leaching reagent to be clean 6 M nitric acid for 72 hour exposures. Contamination levels for uranium and thorium found in the leachate solutions were significant for ultralow level radiation detection applications.

  13. Surface cleaning techniques. Ultra-trace ICP-MS sample preparation and assay of HDPE

    International Nuclear Information System (INIS)

    The world's most sensitive radiation detection and assay systems depend upon ultra-low-background (ULB) materials to reduce unwanted radiological backgrounds. In this study, we evaluate methods to clean HDPE, a material of interest to ULB systems and the means to provide rapid assay of surface and bulk contamination. ULB-level material and ultra-trace-level detection of actinide elements is difficult to attain, due to the introduction of contamination from sample preparation equipment such as pipette tips, sample vials, forceps, etc and airborne particulate. To date, literature available on the cleaning of such polymeric materials and equipment for ULB applications and ultra-trace analyses is limited. For these reasons, a study has been performed to identify an effective way to remove surface contamination from polymers in an effort to provide improved instrumental detection limits. Inductively Coupled Plasma Mass Spectroscopy was utilized to assess the effectiveness of a variety of leachate solutions for removal of inorganic uranium and thorium surface contamination from polymers, specifically high density polyethylene (HDPE). Leaching procedures for HDPE were tested to optimize contaminant removal of thorium and uranium. Calibration curves for thorium and uranium ranged from 15 ppq (fg/mL) to 1 ppt (pg/mL). Detection limits were calculated at 6 ppq for uranium and 7 ppq for thorium. Results showed the most effective leaching reagent to be clean 6 M nitric acid for 72 h exposures. Contamination levels for uranium and thorium found in the leachate solutions were significant for ultra-low-level radiation detection applications. (author)

  14. Sample preparation for inductively coupled plasma mass spectrometric determination of the zinc-70 to zinc-68 isotope ratio in biological samples

    International Nuclear Information System (INIS)

    Sample preparation was optimized for the 70Zn:68Zn isotope ratio determinations performed with inductively coupled plasma mass spectrometry in blood, faeces and urine from human pre-term babies after oral or intravenous administration of enriched 70Zn. The preparation techniques achieved complete decomposition, matrix separation, maximum preconcentration and minimum contamination. After sample decomposition, Zn was extracted into CCl4 with ammonium pyrrolidin-1-yldithioformate and back extracted into 1.2 mol dm-3 HNO3 for analysis. Residual chloride resulting from dissolved CCl4 in the acid led to interference by 35Cl2+, and the procedure was modified to evaporate the CCl4. Extraction was unnecessary for faecal samples. Under optimized conditions the 70Zn:68Zn isotope ratio can be measured with acceptable precision (200 ng cm-3 in the analytical solution). (Author)

  15. Advances in Fourier transform infrared spectroscopy of natural glasses: From sample preparation to data analysis

    Science.gov (United States)

    von Aulock, F. W.; Kennedy, B. M.; Schipper, C. I.; Castro, J. M.; Martin, D. E.; Oze, C.; Watkins, J. M.; Wallace, P. J.; Puskar, L.; Bégué, F.; Nichols, A. R. L.; Tuffen, H.

    2014-10-01

    Fourier transform infrared spectroscopy (FTIR) is an analytical technique utilized to measure the concentrations of H and C species in volcanic glasses. Water and CO2 are the most abundant volatile species in volcanic systems. Water is present in magmas in higher concentrations than CO2 and is also more soluble at lower pressures, and, therefore it is the dominant volatile forming bubbles during volcanic eruptions. Dissolved water affects both phase equilibria and melt physical properties such as density and viscosity, therefore, water is important for understanding magmatic processes. Additionally, quantitative measurements of different volatile species using FTIR can be achieved at high spatial resolution. Recent developments in analytical equipment such as synchrotron light sources and the development of focal plane array (FPA) detectors allow higher resolution measurements and the acquisition of concentration maps. These new capabilities are being used to characterize spatial gradients (or lack thereof) around bubbles and other textural features, which in turn lead to new insights into the behavior of volcanic feeder systems. Here, practical insights about sample preparation and analysis of the distribution and speciation of volatiles in volcanic glasses using FTIR spectroscopy are discussed. New advances in the field of FTIR analysis produce reliable data at high spatial resolution that can be used to produce datasets on the distribution, dissolution and diffusion of volatiles in volcanic materials.

  16. Atmospheric pressure microwave sample preparation procedure for the combined analysis of total phosphorus and kjeldahl nitrogen.

    Science.gov (United States)

    Collins, L W; Chalk, S J; Kingston, H M

    1996-08-01

    An atmospheric pressure microwave digestion method has been developed for the combined analysis of total phosphorus and Kjeldahl nitrogen in complex matrices. In comparison to the digestion steps in EPA Methods 365.4 (total phosphorus) and 351.x (Kjeldahl nitrogen), this method requires less time, eliminates the need for a catalyst, and reduces the toxicity of the waste significantly. It employs a microwave-assisted digestion step, using refluxing borosilicate glass vessels at atmospheric pressure. Traditionally, this method has a time-consuming sample preparation step and generates toxic waste through the use of heavy metal catalysts. These advantages are gained by the combination of a high boiling point acid (sulfuric acid) and the application of focused microwave irradiation, which enhances the digestion process by direct energy coupling. NIST standard reference materials 1572 (citrus leaves), 1577a (bovine liver), and 1566 (oyster tissue) and tryptophan were analyzed to validate the method. Phosphorus concentrations were determined by the colorimetric ascorbic acid method outlined in EPA Method 365.3. Kjeldahl nitrogen concentrations were determined using EPA Method 351.1. The results of the analyses showed good precision and are in excellent agreement with the NIST published values for both elements.

  17. Reproducibility of NMR Analysis of Urine Samples: Impact of Sample Preparation, Storage Conditions, and Animal Health Status

    Directory of Open Access Journals (Sweden)

    Christina Schreier

    2013-01-01

    Full Text Available Introduction. Spectroscopic analysis of urine samples from laboratory animals can be used to predict the efficacy and side effects of drugs. This employs methods combining 1H NMR spectroscopy with quantification of biomarkers or with multivariate data analysis. The most critical steps in data evaluation are analytical reproducibility of NMR data (collection, storage, and processing and the health status of the animals, which may influence urine pH and osmolarity. Methods. We treated rats with a solvent, a diuretic, or a nephrotoxicant and collected urine samples. Samples were titrated to pH 3 to 9, or salt concentrations increased up to 20-fold. The effects of storage conditions and freeze-thaw cycles were monitored. Selected metabolites and multivariate data analysis were evaluated after 1H NMR spectroscopy. Results. We showed that variation of pH from 3 to 9 and increases in osmolarity up to 6-fold had no effect on the quantification of the metabolites or on multivariate data analysis. Storage led to changes after 14 days at 4°C or after 12 months at −20°C, independent of sample composition. Multiple freeze-thaw cycles did not affect data analysis. Conclusion. Reproducibility of NMR measurements is not dependent on sample composition under physiological or pathological conditions.

  18. 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%, dependi...

  19. Effort versus Reward: Preparing Samples for Fungal Community Characterization in High-Throughput Sequencing Surveys of Soils

    OpenAIRE

    Song, Zewei; Schlatter, Dan; Kennedy, Peter; Linda L Kinkel; Kistler, H. Corby; Nguyen, Nhu; Bates, Scott T

    2015-01-01

    Next generation fungal amplicon sequencing is being used with increasing frequency to study fungal diversity in various ecosystems; however, the influence of sample preparation on the characterization of fungal community is poorly understood. We investigated the effects of four procedural modifications to library preparation for high-throughput sequencing (HTS). The following treatments were considered: 1) the amount of soil used in DNA extraction, 2) the inclusion of additional steps (freeze...

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

    Science.gov (United States)

    Kim, Hyun Jung; Choi, Sang H.; Bae, Hyung-Bin; Lee, Tae Woo

    2012-01-01

    The National Aeronautics and Space Administration-invented X-ray diffraction (XRD) methods, including the total defect density measurement method and the spatial wafer mapping method, have confirmed super hetero epitaxy growth for rhombohedral single crystalline silicon germanium (Si1-xGex) on a c-plane sapphire substrate. However, the XRD method cannot observe the surface morphology or roughness because of the method s limited resolution. Therefore the authors used transmission electron microscopy (TEM) with samples prepared in two ways, the focused ion beam (FIB) method and the tripod method to study the structure between Si1-xGex and sapphire substrate and Si1?xGex itself. The sample preparation for TEM should be as fast as possible so that the sample should contain few or no artifacts induced by the preparation. The standard sample preparation method of mechanical polishing often requires a relatively long ion milling time (several hours), which increases the probability of inducing defects into the sample. The TEM sampling of the Si1-xGex on sapphire is also difficult because of the sapphire s high hardness and mechanical instability. The FIB method and the tripod method eliminate both problems when performing a cross-section TEM sampling of Si1-xGex on c-plane sapphire, which shows the surface morphology, the interface between film and substrate, and the crystal structure of the film. This paper explains the FIB sampling method and the tripod sampling method, and why sampling Si1-xGex, on a sapphire substrate with TEM, is necessary.

  1. Automation of the radiosynthesis and purification procedures for [18F]Fluspidine preparation, a new radiotracer for clinical investigations in PET imaging of σ1 receptors in brain

    International Nuclear Information System (INIS)

    The radiosynthesis of [18F]Fluspidine, a potent σ1 receptor imaging probe for pre-clinical/clinical studies, was implemented on a TRACERlabTM FX F-N synthesizer. [18F]2 was synthesized in 15 min at 85 °C starting from its tosylate precursor. Purification via semi-preparative RP-HPLC was investigated using different columns and eluent compositions and was most successful on a polar RP phase with acetonitrile/water buffered with NH4OAc. After solid phase extraction, [18F]Fluspidine was formulated and produced within 59±4 min with an overall radiochemical yield of 37±8%, a radiochemical purity of 99.3±0.5% and high specific activity (176.6±52.0 GBq/µmol). - Highlights: • [18F]Fluspidine is a promising radiotracer for PET imaging of sigma1 receptors. • A fully automated CGMP-oriented radiosynthesis of [18F]Fluspidine is described. • The purification was investigated using different semi-preparative HPLC systems. • [18F]Fluspidine was produced within 59±4 min with a radiochemical yield of 37±8%

  2. H++ 3.0: automating pK prediction and the preparation of biomolecular structures for atomistic molecular modeling and simulations.

    Science.gov (United States)

    Anandakrishnan, Ramu; Aguilar, Boris; Onufriev, Alexey V

    2012-07-01

    The accuracy of atomistic biomolecular modeling and simulation studies depend on the accuracy of the input structures. Preparing these structures for an atomistic modeling task, such as molecular dynamics (MD) simulation, can involve the use of a variety of different tools for: correcting errors, adding missing atoms, filling valences with hydrogens, predicting pK values for titratable amino acids, assigning predefined partial charges and radii to all atoms, and generating force field parameter/topology files for MD. Identifying, installing and effectively using the appropriate tools for each of these tasks can be difficult for novice and time-consuming for experienced users. H++ (http://biophysics.cs.vt.edu/) is a free open-source web server that automates the above key steps in the preparation of biomolecular structures for molecular modeling and simulations. H++ also performs extensive error and consistency checking, providing error/warning messages together with the suggested corrections. In addition to numerous minor improvements, the latest version of H++ includes several new capabilities and options: fix erroneous (flipped) side chain conformations for HIS, GLN and ASN, include a ligand in the input structure, process nucleic acid structures and generate a solvent box with specified number of common ions for explicit solvent MD.

  3. State of the art of environmentally friendly sample preparation approaches for determination of PBDEs and metabolites in environmental and biological samples: A critical review.

    Science.gov (United States)

    Berton, Paula; Lana, Nerina B; Ríos, Juan M; García-Reyes, Juan F; Altamirano, Jorgelina C

    2016-01-28

    Green chemistry principles for developing methodologies have gained attention in analytical chemistry in recent decades. A growing number of analytical techniques have been proposed for determination of organic persistent pollutants in environmental and biological samples. In this light, the current review aims to present state-of-the-art sample preparation approaches based on green analytical principles proposed for the determination of polybrominated diphenyl ethers (PBDEs) and metabolites (OH-PBDEs and MeO-PBDEs) in environmental and biological samples. Approaches to lower the solvent consumption and accelerate the extraction, such as pressurized liquid extraction, microwave-assisted extraction, and ultrasound-assisted extraction, are discussed in this review. Special attention is paid to miniaturized sample preparation methodologies and strategies proposed to reduce organic solvent consumption. Additionally, extraction techniques based on alternative solvents (surfactants, supercritical fluids, or ionic liquids) are also commented in this work, even though these are scarcely used for determination of PBDEs. In addition to liquid-based extraction techniques, solid-based analytical techniques are also addressed. The development of greener, faster and simpler sample preparation approaches has increased in recent years (2003-2013). Among green extraction techniques, those based on the liquid phase predominate over those based on the solid phase (71% vs. 29%, respectively). For solid samples, solvent assisted extraction techniques are preferred for leaching of PBDEs, and liquid phase microextraction techniques are mostly used for liquid samples. Likewise, green characteristics of the instrumental analysis used after the extraction and clean-up steps are briefly discussed. PMID:26755134

  4. Multi-element determination of Cu, Fe, Ni and Zn content in vegetable oils samples by high-resolution continuum source atomic absorption spectrometry and microemulsion sample preparation.

    Science.gov (United States)

    Nunes, Luana S; Barbosa, José T P; Fernandes, Andréa P; Lemos, Valfredo A; Santos, Walter N L Dos; Korn, Maria Graças A; Teixeira, Leonardo S G

    2011-07-15

    The aim of this work was to evaluate the microemulsification as sample preparation procedure for determination of Cu, Fe, Ni and Zn in vegetable oils samples by High-Resolution Continuum Source Flame Atomic Absorption Spectrometry (HR-CS FAAS). Microemulsions were prepared by mixing samples with propan-1-ol and aqueous acid solution, which allowed the use of inorganic aqueous standards for the calibration. To a sample mass of 0.5g, 100μL of hydrochloric acid and propan-1-ol were added and the resulting mixture diluted to a final volume of 10mL. The sample was manually shaken resulting in a visually homogeneous system. The main lines were selected for all studied metals and the detection limits (3σ, n=10) were 0.12, 0.62, 0.58 and 0.12mgkg(-1) for Cu, Fe, Ni and Zn, respectively. The relative standard deviation (RSD) ranged from 5% to 11 % in samples spiked with 0.25 and 1.5μgmL(-1) of each metal, respectively. Recoveries varied from 89% to 102%. The proposed method was applied to the determination of Cu, Fe, Ni and Zn in soybean, olive and sunflower oils. PMID:23140735

  5. Reproducibility of NMR Analysis of Urine Samples: Impact of Sample Preparation, Storage Conditions, and Animal Health Status

    OpenAIRE

    Christina Schreier; Werner Kremer; Fritz Huber; Sindy Neumann; Philipp Pagel; Kai Lienemann; Sabine Pestel

    2013-01-01

    Introduction. Spectroscopic analysis of urine samples from laboratory animals can be used to predict the efficacy and side effects of drugs. This employs methods combining 1H NMR spectroscopy with quantification of biomarkers or with multivariate data analysis. The most critical steps in data evaluation are analytical reproducibility of NMR data (collection, storage, and processing) and the health status of the animals, which may influence urine pH and osmolarity. Methods. We treated rats wit...

  6. Closer to the native state. Critical evaluation of cryo-techniques for Transmission Electron Microscopy: preparation of biological samples.

    Science.gov (United States)

    Mielanczyk, Lukasz; Matysiak, Natalia; Michalski, Marek; Buldak, Rafal; Wojnicz, Romuald

    2014-01-01

    Over the years Transmission Electron Microscopy (TEM) has evolved into a powerful technique for the structural analysis of cells and tissues at various levels of resolution. However, optimal sample preservation is required to achieve results consistent with reality. During the last few decades, conventional preparation methods have provided most of the knowledge about the ultrastructure of organelles, cells and tissues. Nevertheless, some artefacts can be introduced at all stagesofstandard electron microscopy preparation technique. Instead, rapid freezing techniques preserve biological specimens as close as possible to the native state. Our review focuses on different cryo-preparation approaches, starting from vitrification methods dependent on sample size. Afterwards, we discuss Cryo-Electron Microscopy Of VItreous Sections (CEMOVIS) and the main difficulties associated with this technique. Cryo-Focused Ion Beam (cryo-FIB) is described as a potential alternative for CEMOVIS. Another post-processing route for vitrified samples is freeze substitution and embedding in resin for structural analysis or immunolocalization analysis. Cryo-sectioning according to Tokuyasu is a technique dedicated to high efficiency immunogold labelling. Finally, we introduce hybrid techniques, which combine advantages of primary techniques originally dedicated to different approaches. Hybrid approaches permit to perform the study of difficult-to-fix samples and antigens or help optimize the sample preparation protocol for the integrated Laser and Electron Microscopy (iLEM) technique.

  7. Sample preparation methods for subsequent determination of metals and non-metals in crude oil--a review.

    Science.gov (United States)

    Mello, Paola A; Pereira, Juliana S F; Mesko, Marcia F; Barin, Juliano S; Flores, Erico M M

    2012-10-01

    In this review sample preparation strategies used for crude oil digestion in last ten years are discussed focusing on further metals and non-metals determination. One of the main challenges of proposed methods has been to overcome the difficulty to bring crude oil samples into solution, which should be compatible with analytical techniques used for element determination. On this aspect, this review summarizes the sample preparation methods for metals and non metals determination in crude oil including those based on wet digestion, combustion, emulsification, extraction, sample dilution with organic solvents, among others. Conventional methods related to wet digestion with concentrated acids or combustion are also covered, with special emphasis to closed systems. Trends in sample digestion, such as microwave-assisted digestion using diluted acids combined with high-efficiency decomposition systems are discussed. On the other hand, strategies based on sample dilution in organic solvents and procedures recommended for speciation analysis are reported as well as the use of direct analysis in view of the recent importance for crude oil field. A compilation concerning sample preparation for crude oil provided by official methods as well as certified reference materials available for accuracy evaluation is also presented and discussed. PMID:22975177

  8. Sample preparation and direct electrospray ionization on a tip column for rapid mass spectrometry analysis of complex samples.

    Science.gov (United States)

    Huang, Yun-Qing; You, Jin-Qing; Yuan, Bi-Feng; Feng, Yu-Qi

    2012-10-01

    A handheld pipette tip column electrospray ionization source (PTC-ESI source) was developed for rapid mass spectrometry analysis at ambient pressure. The PTC-ESI source was made up of three main component parts including a micro DC high voltage (HV) power supply, a micropipette and a disposable micropipette tip filled with a plug of adsorbent. A DC high voltage was applied to the sharp point of the micropipette tip column to induce electrospray ionization. The PTC-ESI source was successfully used for direct analysis of basic organic compounds, organic acids and peptides in a simple matrix. In the case of complex samples, micro-extraction based on the adsorbent phase filled in the pipette tip was used to remove impurities and concentrate target analytes prior to ionization. The eluting solution was not pipetted out, but directly dispersed in the form of electrospray from the pipette tip for ionization. The effectiveness of the PTC-ESI source has been further demonstrated by fast analysis of therapeutic compounds and endogenous bioactive chemicals in complex biological samples. PMID:22898704

  9. Application of laser ablation inductively coupled plasma mass spectrometry for soil analysis: a novel procedure for sample preparation

    International Nuclear Information System (INIS)

    A rapid, sensitive and reliable LA–ICP–MS method for simultaneous determination of micro and macro elements in soils and sediments was developed and optimized. Certified reference materials available in powder form (IAEA–SOIL–5, IAEA–SOIL–7, IAEA–SL–1, IAEA–SL–3 and STSD–3) were used for the optimization and validation of the sample preparation step and LA–ICP–MS analysis. Three types of soil pellets were prepared from each CRM: (i) original soil; (ii) soil, mixed with boric acid in ratio 1:5; and (iii) pellets, prepared by mixing the soil successively in hexane and dichloromethane and subjected to LA–ICP–MS measurement. The signal of the matrix elements was reduced by introducing the rejection parameter (RPa) to enable the high–mass cut off. Best accuracy and precision were obtained with the pellets, prepared in organic solvents. This approach can be recommended for sample preparation of soils and sediments for LA–ICP–MS analysis. Key words: LA–ICP–MS, pellet preparation, calibration, soil analysis

  10. A filter paper-based microdevice for low-cost, rapid, and automated DNA extraction and amplification from diverse sample types.

    Science.gov (United States)

    Gan, Wupeng; Zhuang, Bin; Zhang, Pengfei; Han, Junping; Li, Cai-Xia; Liu, Peng

    2014-10-01

    A plastic microfluidic device that integrates a filter disc as a DNA capture phase was successfully developed for low-cost, rapid and automated DNA extraction and PCR amplification from various raw samples. The microdevice was constructed by sandwiching a piece of Fusion 5 filter, as well as a PDMS (polydimethylsiloxane) membrane, between two PMMA (poly(methyl methacrylate)) layers. An automated DNA extraction from 1 μL of human whole blood can be finished on the chip in 7 minutes by sequentially aspirating NaOH, HCl, and water through the filter. The filter disc containing extracted DNA was then taken out directly for PCR. On-chip DNA purification from 0.25-1 μL of human whole blood yielded 8.1-21.8 ng of DNA, higher than those obtained using QIAamp® DNA Micro kits. To realize DNA extraction from raw samples, an additional sample loading chamber containing a filter net with an 80 μm mesh size was designed in front of the extraction chamber to accommodate sample materials. Real-world samples, including whole blood, dried blood stains on Whatman® 903 paper, dried blood stains on FTA™ cards, buccal swabs, saliva, and cigarette butts, can all be processed in the system in 8 minutes. In addition, multiplex amplification of 15 STR (short tandem repeat) loci and Sanger-based DNA sequencing of the 520 bp GJB2 gene were accomplished from the filters that contained extracted DNA from blood. To further prove the feasibility of integrating this extraction method with downstream analyses, "in situ" PCR amplifications were successfully performed in the DNA extraction chamber following DNA purification from blood and blood stains without DNA elution. Using a modified protocol to bond the PDMS and PMMA, our plastic PDMS devices withstood the PCR process without any leakage. This study represents a significant step towards the practical application of on-chip DNA extraction methods, as well as the development of fully integrated genetic analytical systems.

  11. Comparison of QuEChERS sample preparation methods for the analysis of pesticide residues in fruits and vegetables

    Science.gov (United States)

    This article describes the comparison of different versions of an easy, rapid, and low-cost sample preparation approach for the determination of pesticide residues in fruits and vegetables by concurrent use of gas and liquid chromatography (GC and LC) coupled to mass spectrometry (MS) for detection....

  12. Sludge batch 9 (SB9) accepance evaluation: Radionuclide concentrations in tank 51 SB9 qualification sample prepared at SRNL

    Energy Technology Data Exchange (ETDEWEB)

    Bannochie, C. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Diprete, D. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Pareizs, J. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2016-03-01

    Presented in this report are radionuclide concentrations required as part of the program of qualifying Sludge Batch 9 (SB9) for processing in the Defense Waste Processing Facility (DWPF). The SB9 material is currently in Tank 51 and has been washed and prepared for transfer to Tank 40. The acceptance evaluation needs to be completed prior to the transfer of the material in Tank 51 to Tank 40. The sludge slurry in Tank 40 has already been qualified for DWPF processing and is currently being processed as Sludge Batch 8 (SB8). The radionuclide concentrations were measured or estimated in the Tank 51 SB9 Washed Qualification Sample prepared at Savannah River National Laboratory (SRNL). This sample was prepared from a three liter sample of Tank 51 sludge slurry (HTF-51-15-81) taken on July 23, 2015. The sample was delivered to SRNL where it was initially characterized in the Shielded Cells. Under the direction of Savannah River Remediation (SRR) it was then adjusted per the Tank Farm washing strategy as of October 20, 2015. This final slurry now has a compositioniv expected to be similar to that of the slurry in Tank 51 after final preparations have been made for transfer of that slurry to Tank 40.

  13. Sludge batch 9 (SB9) acceptance evaluation. Radionuclide concentrations in tank 51 SB9 qualification sample prepared at SRNL

    Energy Technology Data Exchange (ETDEWEB)

    Bannochie, C. J. [Savannah River Site (SRS), Aiken, SC (United States); Diprete, D. P. [Savannah River Site (SRS), Aiken, SC (United States); Pareizs, J. M. [Savannah River Site (SRS), Aiken, SC (United States)

    2016-02-10

    Presented in this report are radionuclide concentrations required as part of the program of qualifying Sludge Batch 9 (SB9) for processing in the Defense Waste Processing Facility (DWPF). The SB9 material is currently in Tank 51 and has been washed and prepared for transfer to Tank 40. The acceptance evaluation needs to be completed prior to the transfer of the material in Tank 51 to Tank 40. The sludge slurry in Tank 40 has already been qualified for DWPF processing and is currently being processed as Sludge Batch 8 (SB8). The radionuclide concentrations were measured or estimated in the Tank 51 SB9 Washed Qualification Sample prepared at Savannah River National Laboratory (SRNL). This sample was prepared from a three liter sample of Tank 51 sludge slurry (HTF-51-15-81) taken on July 23, 2015. The sample was delivered to SRNL where it was initially characterized in the Shielded Cells. Under the direction of Savannah River Remediation (SRR) it was then adjusted per the Tank Farm washing strategy as of October 20, 2015. This final slurry now has a composition expected to be similar to that of the slurry in Tank 51 after final preparations have been made for transfer of that slurry to Tank 40.

  14. A novel sample preparation method of matrix-assisted laser desorption/ionization time of flight mass spectrometry for polystyrene

    Institute of Scientific and Technical Information of China (English)

    Shu Zhang; Zhen Wen Zhao; Lei Xiong; Bin Xin; Wei Hua Hu; Shao Xiang Xiong

    2007-01-01

    A novel sample preparation method of matrix-assisted laser desorption/ionization mass spectrometry for polystyrene was reported.Compared to the conventional dried-droplet method, the efficiency of ionization and signal intensity of mass spectra were improved.The mechanism was also analyzed.

  15. Automated large scale parameter extraction of road-side trees sampled by a laser mobile mapping system

    NARCIS (Netherlands)

    Lindenbergh, R.C.; Berthold, D.; Sirmacek, B.; Herrero-Huerta, M.; Wang, J.; Ebersbach, D.

    2015-01-01

    In urbanized Western Europe trees are considered an important component of the built-up environment. This also means that there is an increasing demand for tree inventories. Laser mobile mapping systems provide an efficient and accurate way to sample the 3D road surrounding including notable roadsid

  16. Automated determination of nitrate plus nitrite in aqueous samples with flow injection analysis using vanadium (III) chloride as reductant.

    Science.gov (United States)

    Wang, Shu; Lin, Kunning; Chen, Nengwang; Yuan, Dongxing; Ma, Jian

    2016-01-01

    Determination of nitrate in aqueous samples is an important analytical objective for environmental monitoring and assessment. Here we report the first automatic flow injection analysis (FIA) of nitrate (plus nitrite) using VCl3 as reductant instead of the well-known but toxic cadmium column for reducing nitrate to nitrite. The reduced nitrate plus the nitrite originally present in the sample react with the Griess reagent (sulfanilamide and N-1-naphthylethylenediamine dihydrochloride) under acidic condition. The resulting pink azo dye can be detected at 540 nm. The Griess reagent and VCl3 are used as a single mixed reagent solution to simplify the system. The various parameters of the FIA procedure including reagent composition, temperature, volume of the injection loop, and flow rate were carefully investigated and optimized via univariate experimental design. Under the optimized conditions, the linear range and detection limit of this method are 0-100 µM (R(2)=0.9995) and 0.1 µM, respectively. The targeted analytical range can be easily extended to higher concentrations by selecting alternative detection wavelengths or increasing flow rate. The FIA system provides a sample throughput of 20 h(-1), which is much higher than that of previously reported manual methods based on the same chemistry. National reference solutions and different kinds of aqueous samples were analyzed with our method as well as the cadmium column reduction method. The results from our method agree well with both the certified value and the results from the cadmium column reduction method (no significant difference with P=0.95). The spiked recovery varies from 89% to 108% for samples with different matrices, showing insignificant matrix interference in this method. PMID:26695325

  17. Phase analysis of aluminium modified GeSbTe bulk prepared from XRD of samples

    Science.gov (United States)

    Sandhu, Sharanjit; Singh, D.; Kumar, S.; Thangaraj, R.

    2016-05-01

    Various compositions of Aluminium modified GST as Alx(Ge2Sb2Te5)1-x x= 0, 0.15, 0.20, 0.25, 0.30 are prepared to study as a phase change material. Bulk prepared is studied with XRD scans for various phases formed. Phases other than Ge2Sb2Te5 do come in but dominated one is Ge2Sb2Te5 hexagonal phase.

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

    Science.gov (United States)

    Stark, Peter C.; Zurek, Eduardo; Wheat, Jeffrey V.; Dunbar, John M.; Olivares, Jose A.; Garcia-Rubio, Luis H.; Ward, Michael D.

    2011-07-26

    There is provided a method and device for remote sampling, preparation and optical interrogation of a sample using light scattering and light absorption methods. The portable device is a filtration-based device that removes interfering background particle material from the sample matrix by segregating or filtering the chosen analyte from the sample solution or matrix while allowing the interfering background particles to be pumped out of the device. The segregated analyte is then suspended in a diluent for analysis. The device is capable of calculating an initial concentration of the analyte, as well as diluting the analyte such that reliable optical measurements can be made. Suitable analytes include cells, microorganisms, bioparticles, pathogens and diseases. Sample matrixes include biological fluids such as blood and urine, as well as environmental samples including waste water.

  19. Thorium in the workplace: The preparation and validation of comparison samples for a European-based measurement comparison project

    International Nuclear Information System (INIS)

    The quality of any comparison exercise depends critically on the quality, accuracy and fitness for purpose of the comparison samples. The comparisons were designed to move progressively from the testing of the analysis capabilities for relatively simple, aqueous solutions through to the more complex natural matrix materials encountered in the workplace. In each case, it was imperative that the comparison samples were prepared and validated in such a way as to ensure traceability of their activity values to national and international standards of radioactivity, to enable a reasonable estimate to be made of the uncertainty on those values and to ensure homogeneity both within and between samples. The processes involved are discussed. (author)

  20. Automated preparation method for colloidal crystal arrays of monodisperse and binary colloid mixtures by contact printing with a pintool plotter.

    Science.gov (United States)

    Burkert, Klaus; Neumann, Thomas; Wang, Jianjun; Jonas, Ulrich; Knoll, Wolfgang; Ottleben, Holger

    2007-03-13

    Photonic crystals and photonic band gap materials with periodic variation of the dielectric constant in the submicrometer range exhibit unique optical properties such as opalescence, optical stop bands, and photonic band gaps. As such, they represent attractive materials for the active elements in sensor arrays. Colloidal crystals, which are 3D gratings leading to Bragg diffraction, are one potential precursor of such optical materials. They have gained particular interest in many technological areas as a result of their specific properties and ease of fabrication. Although basic techniques for the preparation of regular patterns of colloidal crystals on structured substrates by self-assembly of mesoscopic particles are known, the efficient fabrication of colloidal crystal arrays by simple contact printing has not yet been reported. In this article, we present a spotting technique used to produce a microarray comprising up to 9600 single addressable sensor fields of colloidal crystal structures with dimensions down to 100 mum on a microfabricated substrate in different formats. Both monodisperse colloidal crystals and binary colloidal crystal systems were prepared by contact printing of polystyrene particles in aqueous suspension. The array morphology was characterized by optical light microscopy and scanning electron microscopy, which revealed regularly ordered crystalline structures for both systems. In the case of binary crystals, the influence of the concentration ratio of the large and small particles in the printing suspension on the obtained crystal structure was investigated. The optical properties of the colloidal crystal arrays were characterized by reflection spectroscopy. To examine the stop bands of the colloidal crystal arrays in a high-throughput fashion, an optical setup based on a CCD camera was realized that allowed the simultaneous readout of all of the reflection spectra of several thousand sensor fields per array in parallel. In agreement with

  1. Powder Handling Device for X-ray Diffraction Analysis with Minimal Sample Preparation Project

    Data.gov (United States)

    National Aeronautics and Space Administration — This project consists of developing a Vibrating Sample Holder (VSH) for planetary X-Ray Diffraction (XRD) instruments. The principle of this novel sample handling...

  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

    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...... of more metabolomic information as compared to protein precipitation alone. Chromatography showed good separation of the metabolites with little retention time drift (method was investigated using plasma samples from rats...

  3. Shorter sampling periods and accurate estimates of milk volume and components are possible for pasture based dairy herds milked with automated milking systems.

    Science.gov (United States)

    Kamphuis, Claudia; Burke, Jennie K; Taukiri, Sarah; Petch, Susan-Fay; Turner, Sally-Anne

    2016-08-01

    Dairy cows grazing pasture and milked using automated milking systems (AMS) have lower milking frequencies than indoor fed cows milked using AMS. Therefore, milk recording intervals used for herd testing indoor fed cows may not be suitable for cows on pasture based farms. We hypothesised that accurate standardised 24 h estimates could be determined for AMS herds with milk recording intervals of less than the Gold Standard (48 hs), but that the optimum milk recording interval would depend on the herd average for milking frequency. The Gold Standard protocol was applied on five commercial dairy farms with AMS, between December 2011 and February 2013. From 12 milk recording test periods, involving 2211 cow-test days and 8049 cow milkings, standardised 24 h estimates for milk volume and milk composition were calculated for the Gold Standard protocol and compared with those collected during nine alternative sampling scenarios, including six shorter sampling periods and three in which a fixed number of milk samples per cow were collected. Results infer a 48 h milk recording protocol is unnecessarily long for collecting accurate estimates during milk recording on pasture based AMS farms. Collection of two milk samples only per cow was optimal in terms of high concordance correlation coefficients for milk volume and components and a low proportion of missed cow-test days. Further research is required to determine the effects of diurnal variations in milk composition on standardised 24 h estimates for milk volume and components, before a protocol based on a fixed number of samples could be considered. Based on the results of this study New Zealand have adopted a split protocol for herd testing based on the average milking frequency for the herd (NZ Herd Test Standard 8100:2015). PMID:27600967

  4. Comparison of pre-analytical FFPE sample preparation methods and their impact on massively parallel sequencing in routine diagnostics.

    Directory of Open Access Journals (Sweden)

    Carina Heydt

    Full Text Available Over the last years, massively parallel sequencing has rapidly evolved and has now transitioned into molecular pathology routine laboratories. It is an attractive platform for analysing multiple genes at the same time with very little input material. Therefore, the need for high quality DNA obtained from automated DNA extraction systems has increased, especially to those laboratories which are dealing with formalin-fixed paraffin-embedded (FFPE material and high sample throughput. This study evaluated five automated FFPE DNA extraction systems as well as five DNA quantification systems using the three most common techniques, UV spectrophotometry, fluorescent dye-based quantification and quantitative PCR, on 26 FFPE tissue samples. Additionally, the effects on downstream applications were analysed to find the most suitable pre-analytical methods for massively parallel sequencing in routine diagnostics. The results revealed that the Maxwell 16 from Promega (Mannheim, Germany seems to be the superior system for DNA extraction from FFPE material. The extracts had a 1.3-24.6-fold higher DNA concentration in comparison to the other extraction systems, a higher quality and were most suitable for downstream applications. The comparison of the five quantification methods showed intermethod variations but all methods could be used to estimate the right amount for PCR amplification and for massively parallel sequencing. Interestingly, the best results in massively parallel sequencing were obtained with a DNA input of 15 ng determined by the NanoDrop 2000c spectrophotometer (Thermo Fisher Scientific, Waltham, MA, USA. No difference could be detected in mutation analysis based on the results of the quantification methods. These findings emphasise, that it is particularly important to choose the most reliable and constant DNA extraction system, especially when using small biopsies and low elution volumes, and that all common DNA quantification techniques can

  5. Efficient lasing action from Rhodamine-110 (Rh-110) impregnated sol-gel silica samples prepared by dip method

    Energy Technology Data Exchange (ETDEWEB)

    Deshpande, Aparna V. [Department of Physics, Institute of Chemical Technology, Matunga, Nathalal Parikh Marg, Mumbai - 400 019 (India); Kumar, Uday, E-mail: udayphy@yahoo.co.i [Department of Physics, Institute of Chemical Technology, Matunga, Nathalal Parikh Marg, Mumbai - 400 019 (India)

    2010-05-15

    Rhodamine-110/sol-gel samples are prepared by sol-gel technique using dip method. Concentration dependent photophysical studies of these samples have indicated about the least possibility of aggregate formation. The lasing action of Rh-110 in silica samples is studied as a function of dye concentration. An efficient laser emission is observed when the samples are transversely pumped at 337.1 nm and 1.5 Hz repetition rate using a nitrogen laser (400 muJ energy/pulse and 4 ns pulse duration). The maximum of 166% laser efficiency of dye doped sol-gel samples compared to Rhodamine-6G (Rh-6G) in methanol is achieved. The photostability is also measured by using N{sub 2} laser at 1 Hz and it is found nearly 165 pulses. The possible reasons for the photodegradation of the dye molecules are discussed in detail.

  6. Optimization of crude enzyme preparation methods for analysis of glutamine synthetase activity in phytoplankton and field samples

    Institute of Scientific and Technical Information of China (English)

    WANG Yujue; WANG Dazhi; HONG Huasheng

    2009-01-01

    Glutamine synthetase (GS) is an important enzyme involved in nitrogen assimilation and metabolism in marine phytoplankton. However, little work has been done in situ due to the limitation of crude enzyme preparation methods. In this study, three enzyme preparation methods, high-speed centrifugation (HC, <10 000 g), ultracentrifugation (UC, 70 000 g), and ultrafiltration (UF) with 100 kμ, molecular weight cutoff, were compared using two diatom species (Asterionellopsis glacialis and Thalassiosira weissflogii), and two dinoflagellate species (Alexandrium catenella and Prorocentrum donghaiense) as experimental materials together with field samples collected from Xiamen Harbor, China. The results showed that HC is the best method to prepare crude enzymes for glutamine synthetase activity (GSA) in diatom species and diatom-dominant samples, while UF is the best method to extract GS from dinoflagellate species and dinoflagellate-dominant samples. For the HC method, the optimal centrifugal speed and time were 10 000 g and 35 min, respectively, and under these conditions, the highest GSA was obtained in all samples. This study indicates that both methods (HC and UF) overcome the limitation of centrifugal speed and could be applied to in situ GSA analysis, especially at sea.

  7. Study of sample preparation for quantitative analysis of amino acids in human sweat by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

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

    2016-01-01

    The determination of physiological levels of amino acids is important to aid in the diagnosis and treatment of several diseases and nutritional status of individuals. Amino acids are frequently determined in biofluids such as blood (serum or plasma) and urine; however, there are less common biofluids with different concentration profiles of amino acids that could be of interest. One of these biofluids is sweat that can be obtained in a non-invasive manner and is characterized by low complex composition. The analysis of amino acids in human sweat requires the development of sample preparation strategies according to the sample matrix and small collected volume. The influence of sample preparation on the quantitative analysis of amino acids in sweat by LC-MS/MS has been assessed through a comparison between two strategies: dilution of sweat and centrifugal microsolid-phase extraction (c-μSPE). In both cases, several dilution factors were assayed for in-depth knowledge of the matrix effects, and the use of c-μSPE provided the best results in terms of accuracy. The behavior of the target analytes was a function of the dilution factor, thus providing a pattern for sample preparation that depended on the amino acid to be determined. The concentration of amino acids in sweat ranges between 6.20 ng mL(-1) (for homocysteine) and 259.77 µg mL(-1) (for serine) with precision, expressed as relative standard deviation, within 1.1-21.4%.

  8. Comparison of Chlorhexidine and Tincture of Iodine for Skin Antisepsis in Preparation for Blood Sample Collection

    OpenAIRE

    Barenfanger, Joan; Drake, Cheryl; Lawhorn, Jerry; Verhulst, Steven J.

    2004-01-01

    Rates of contamination of blood cultures obtained when skin was prepared with iodine tincture versus chlorhexidine were compared. For iodine tincture, the contamination rate was 2.7%; for chlorhexidine, it was 3.1%. The 0.41% difference is not statistically significant. Chlorhexidine has comparable effectiveness and is safer, cheaper, and preferred by staff, so it is an alternative to iodine tincture.

  9. 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

    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...

  10. Sampling

    CERN Document Server

    Thompson, Steven K

    2012-01-01

    Praise for the Second Edition "This book has never had a competitor. It is the only book that takes a broad approach to sampling . . . any good personal statistics library should include a copy of this book." —Technometrics "Well-written . . . an excellent book on an important subject. Highly recommended." —Choice "An ideal reference for scientific researchers and other professionals who use sampling." —Zentralblatt Math Features new developments in the field combined with all aspects of obtaining, interpreting, and using sample data Sampling provides an up-to-date treat

  11. Effort versus Reward: Preparing Samples for Fungal Community Characterization in High-Throughput Sequencing Surveys of Soils.

    Science.gov (United States)

    Song, Zewei; Schlatter, Dan; Kennedy, Peter; Kinkel, Linda L; Kistler, H Corby; Nguyen, Nhu; Bates, Scott T

    2015-01-01

    Next generation fungal amplicon sequencing is being used with increasing frequency to study fungal diversity in various ecosystems; however, the influence of sample preparation on the characterization of fungal community is poorly understood. We investigated the effects of four procedural modifications to library preparation for high-throughput sequencing (HTS). The following treatments were considered: 1) the amount of soil used in DNA extraction, 2) the inclusion of additional steps (freeze/thaw cycles, sonication, or hot water bath incubation) in the extraction procedure, 3) the amount of DNA template used in PCR, and 4) the effect of sample pooling, either physically or computationally. Soils from two different ecosystems in Minnesota, USA, one prairie and one forest site, were used to assess the generality of our results. The first three treatments did not significantly influence observed fungal OTU richness or community structure at either site. Physical pooling captured more OTU richness compared to individual samples, but total OTU richness at each site was highest when individual samples were computationally combined. We conclude that standard extraction kit protocols are well optimized for fungal HTS surveys, but because sample pooling can significantly influence OTU richness estimates, it is important to carefully consider the study aims when planning sampling procedures. PMID:25974078

  12. A Loop-Mediated Isothermal Amplification Assay and Sample Preparation Procedure for Sensitive Detection of Xanthomonas fragariae in Strawberry.

    Directory of Open Access Journals (Sweden)

    Hehe Wang

    Full Text Available Xanthomonas fragariae is a bacterium that causes angular leaf spot of strawberry. Asymptomatic infection is common and contributes to the difficulties in disease management. The aim of this study was to develop a loop-mediated isothermal amplification (LAMP assay as an efficient method for detection of asymptomatic infections of X. fragariae. In addition, a new method of sample preparation was developed that allows sampling of a larger amount of plant tissue, hence increasing the detection rate in real-life samples. The sample preparation procedure includes an overnight incubation of strawberry tissues in phosphate-buffered saline (PBS, followed by a quick sample concentration and a boiling step to extract DNA for amplification. The detection limit of the LAMP assay was approximately 2×10(3 CFU/mL for pure bacteria culture and 300 CFU/mL for bacteria spiked strawberry leaf and petiole samples. LAMP provided a 2-3 fold lower detection limit than the standard qPCR assay but was faster, and more user-friendly. The LAMP assay should serve as a rapid, sensitive and cost-effective tool for detecting asymptomatic infections of X. fragariae in strawberry nursery stock and contribute to improved disease management.

  13. Effort versus Reward: Preparing Samples for Fungal Community Characterization in High-Throughput Sequencing Surveys of Soils.

    Directory of Open Access Journals (Sweden)

    Zewei Song

    Full Text Available Next generation fungal amplicon sequencing is being used with increasing frequency to study fungal diversity in various ecosystems; however, the influence of sample preparation on the characterization of fungal community is poorly understood. We investigated the effects of four procedural modifications to library preparation for high-throughput sequencing (HTS. The following treatments were considered: 1 the amount of soil used in DNA extraction, 2 the inclusion of additional steps (freeze/thaw cycles, sonication, or hot water bath incubation in the extraction procedure, 3 the amount of DNA template used in PCR, and 4 the effect of sample pooling, either physically or computationally. Soils from two different ecosystems in Minnesota, USA, one prairie and one forest site, were used to assess the generality of our results. The first three treatments did not significantly influence observed fungal OTU richness or community structure at either site. Physical pooling captured more OTU richness compared to individual samples, but total OTU richness at each site was highest when individual samples were computationally combined. We conclude that standard extraction kit protocols are well optimized for fungal HTS surveys, but because sample pooling can significantly influence OTU richness estimates, it is important to carefully consider the study aims when planning sampling procedures.

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

    Directory of Open Access Journals (Sweden)

    Yelena G Golubeva

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

  15. Home Automation

    OpenAIRE

    Ahmed, Zeeshan

    2010-01-01

    In this paper I briefly discuss the importance of home automation system. Going in to the details I briefly present a real time designed and implemented software and hardware oriented house automation research project, capable of automating house's electricity and providing a security system to detect the presence of unexpected behavior.

  16. Sample Preparation for Mass Spectrometry Analysis of Protein-Protein Interactions in Cancer Cell Lines and Tissues.

    Science.gov (United States)

    Beigbeder, Alice; Vélot, Lauriane; James, D Andrew; Bisson, Nicolas

    2016-01-01

    A precisely controlled network of protein-protein interactions constitutes the basis for functional signaling pathways. This equilibrium is more often than not disrupted in cancer cells, by the aberrant expression or activation of oncogenic proteins. Therefore, the analysis of protein interaction networks in cancer cells has become crucial to expand our comprehension of the molecular underpinnings of tumor formation and progression. This protocol describes a sample preparation method for the analysis of signaling complexes by mass spectrometry (MS), following the affinity purification of a protein of interest from a cancer cell line or a solid tumor. In particular, we provide a spin tip-based protease digestion procedure that offers a more rapid and controlled alternative to other gel-based and gel-free methods. This sample preparation protocol represents a useful strategy to identify protein interactions and to gain insight into the molecular mechanisms that contribute to a given cancer phenotype. PMID:27581032

  17. Automated solvent concentrator

    Science.gov (United States)

    Griffith, J. S.; Stuart, J. L.

    1976-01-01

    Designed for automated drug identification system (AUDRI), device increases concentration by 100. Sample is first filtered, removing particulate contaminants and reducing water content of sample. Sample is extracted from filtered residue by specific solvent. Concentrator provides input material to analysis subsystem.

  18. Sample preparation for an optimized extraction of localized metabolites in lichens: Application to Pseudevernia furfuracea.

    Science.gov (United States)

    Komaty, Sarah; Letertre, Marine; Dang, Huyen Duong; Jungnickel, Harald; Laux, Peter; Luch, Andreas; Carrié, Daniel; Merdrignac-Conanec, Odile; Bazureau, Jean-Pierre; Gauffre, Fabienne; Tomasi, Sophie; Paquin, Ludovic

    2016-04-01

    Lichens are symbiotic organisms known for producing unique secondary metabolites with attractive cosmetic and pharmacological properties. In this paper, we investigated three standard methods of preparation of Pseudevernia furfuracea (blender grinding, ball milling, pestle and mortar). The materials obtained were characterized by electronic microscopy, nitrogen adsorption and compared from the point of view of extraction. Their microscopic structure is related to extraction efficiency. In addition, it is shown using thalline reactions and mass spectrometry mapping (TOF-SIMS) that these metabolites are not evenly distributed throughout the organism. Particularly, atranorin (a secondary metabolite of interest) is mainly present in the cortex of P. furfuracea. Finally, using microwave assisted extraction (MAE) we obtained evidence that an appropriate preparation can increase the extraction efficiency of atranorin by a factor of five. PMID:26838439

  19. The beauty of being (label)-free: sample preparation methods for SWATH-MS and next-generation targeted proteomics

    OpenAIRE

    Jakob Vowinckel; Floriana Capuano; Kate Campbell; Deery, Michael J.; Lilley, Kathryn S.; Markus Ralser

    2013-01-01

    The combination of qualitative analysis with label-free quantification has greatly facilitated the throughput and flexibility of novel proteomic techniques. However, such methods rely heavily on robust and reproducible sample preparation procedures. Here, we benchmark a selection of in gel, on filter, and in solution digestion workflows for their application in label-free proteomics. Each procedure was associated with differing advantages and disadvantages. The in gel methods interrogated wer...

  20. Bead-releasing agents used in the preparation of solid samples as beads for WD-XRF measurement

    OpenAIRE

    Gazulla Barreda, María Fernanda; Barba Juan, Antonio; Orduña, Mónica; Rodrigo, Marta

    2008-01-01

    A study has been undertaken of bead-releasing agents that are widely used in preparing solid samples as fused beads for wavelength-dispersive X-ray fluorescence (WD-XRF)spectrometry measurement. The following bead-releasing agents were studied: NaI, LiBr, NH4I, and LiI. Each was incorporated in different quantities, as a solid and/or in an aqueous solution, together with a flux, into samples of ceramic raw materials. Release agent interference in the WD-XRF measurement was analyse...

  1. Preparation of quality control samples for its use in the radioimmunoassay de T3, T4 and TSH

    International Nuclear Information System (INIS)

    The use of quality control samples is necessary to evaluate, in a very simple way, the quality of the assays in the radioimmunoanalysis, since allows to settle down a quality control intra and inter analysis. In this work the methodology used for the preparation of these samples with low, media and high concentration for hormones related with the thyroid is shown, being obtained the following concentrations: 50, 200 and 500 ng/dl for T3; 5.6, 7.8 and 14.4 μ g/dl for T4 and 5.4, 13.4 and >50 μ U I/ml for TSH. (Author)

  2. The effects of water sample treatment, preparation, and storage prior to cyanotoxin analysis for cylindrospermopsin, microcystin and saxitoxin.

    Science.gov (United States)

    Kamp, Lisa; Church, Jennifer L; Carpino, Justin; Faltin-Mara, Erin; Rubio, Fernando

    2016-02-25

    Cyanobacterial harmful algal blooms occur in freshwater lakes, ponds, rivers, and reservoirs, and in brackish waters throughout the world. The wide variety of cyanotoxins and their congeners can lead to frequent exposure of humans through consumption of meat, fish, seafood, blue-green algal products and water, accidental ingestion of contaminated water and cyanobacterial scum during recreational activities, and inhalation of cyanobacterial aerosols. Cyanotoxins can also occur in the drinking water supply. In order to monitor human exposure, sensitive analytical methods such as enzyme linked immunosorbent assay and liquid chromatography-mass spectrometry are often used. Regardless of the analytical method of choice, some problems regularly occur during sample collection, treatment, storage, and preparation which cause toxin loss and therefore underestimation of the true concentration. To evaluate the potential influence of sample treatment, storage and preparation materials on surface and drinking water samples, the effects of different types of materials on toxin recovery were compared. Collection and storage materials included glass and various types of plastics. It was found that microcystin congeners LA and LF adsorbed to polystyrene, polypropylene, high density polyethylene and polycarbonate storage containers, leading to low recoveries (water samples immediately upon sample collection is critical for accurate analysis. In addition, the effect of various drinking water treatment chemicals on toxin recovery and the behavior of those chemicals in the enzyme linked immunosorbent assays were also studied and are summarized.

  3. Powder Handling Device for X-ray Diffraction Analysis with Minimal Sample Preparation Project

    Data.gov (United States)

    National Aeronautics and Space Administration — This project consists in developing a Vibrating Powder Handling System for planetary X-Ray Diffraction instruments. The principle of this novel sample handling...

  4. Sample preparation of sewage sludge and soil samples for the determination of polycyclic aromatic hydrocarbons based on one-pot microwave-assisted saponification and extraction.

    Science.gov (United States)

    Pena, M Teresa; Pensado, Luis; Casais, M Carmen; Mejuto, M Carmen; Cela, Rafael

    2007-04-01

    A microwave-assisted sample preparation (MASP) procedure was developed for the analysis of polycyclic aromatic hydrocarbons (PAHs) in sewage sludge and soil samples. The procedure involved the simultaneous microwave-assisted extraction of PAHs with n-hexane and the hydrolysis of samples with methanolic potassium hydroxide. Because of the complex nature of the samples, the extracts were submitted to further cleaning with silica and Florisil solid-phase extraction cartridges connected in series. Naphthalene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benz[a]anthracene, chrysene, benzo[e]pyrene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, dibenz[a,h]anthracene, benzo[g,h,i]perylene, and indeno[1,2,3-cd]pyrene, were considered in the study. Quantification limits obtained for all of these compounds (between 0.4 and 14.8 microg kg(-1) dry mass) were well below of the limits recommended in the USA and EU. Overall recovery values ranged from 60 to 100%, with most losses being due to evaporation in the solvent exchange stages of the procedure, although excellent extraction recoveries were obtained. Validation of the accuracy was carried out with BCR-088 (sewage sludge) and BCR-524 (contaminated industrial soil) reference materials. PMID:17268774

  5. Sample preparation of sewage sludge and soil samples for the determination of polycyclic aromatic hydrocarbons based on one-pot microwave-assisted saponification and extraction

    Energy Technology Data Exchange (ETDEWEB)

    Pena, M.T.; Pensado, Luis; Casais, M.C.; Mejuto, M.C.; Cela, Rafael [Universidad de Santiago de Compostela, Dpto. Quimica Analitica, Nutricion y Bromatologia. Instituto de Investigacion y Analisis Alimentario, Santiago de Compostela (Spain)

    2007-04-15

    A microwave-assisted sample preparation (MASP) procedure was developed for the analysis of polycyclic aromatic hydrocarbons (PAHs) in sewage sludge and soil samples. The procedure involved the simultaneous microwave-assisted extraction of PAHs with n-hexane and the hydrolysis of samples with methanolic potassium hydroxide. Because of the complex nature of the samples, the extracts were submitted to further cleaning with silica and Florisil solid-phase extraction cartridges connected in series. Naphthalene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benz[a]anthracene, chrysene, benzo[e]pyrene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, dibenz[a,h]anthracene, benzo[g,h,i]perylene, and indeno[1,2,3-cd]pyrene, were considered in the study. Quantification limits obtained for all of these compounds (between 0.4 and 14.8 {mu}g kg{sup -1} dry mass) were well below of the limits recommended in the USA and EU. Overall recovery values ranged from 60 to 100%, with most losses being due to evaporation in the solvent exchange stages of the procedure, although excellent extraction recoveries were obtained. Validation of the accuracy was carried out with BCR-088 (sewage sludge) and BCR-524 (contaminated industrial soil) reference materials. (orig.)

  6. Sample preparation of sewage sludge and soil samples for the determination of polycyclic aromatic hydrocarbons based on one-pot microwave-assisted saponification and extraction.

    Science.gov (United States)

    Pena, M Teresa; Pensado, Luis; Casais, M Carmen; Mejuto, M Carmen; Cela, Rafael

    2007-04-01

    A microwave-assisted sample preparation (MASP) procedure was developed for the analysis of polycyclic aromatic hydrocarbons (PAHs) in sewage sludge and soil samples. The procedure involved the simultaneous microwave-assisted extraction of PAHs with n-hexane and the hydrolysis of samples with methanolic potassium hydroxide. Because of the complex nature of the samples, the extracts were submitted to further cleaning with silica and Florisil solid-phase extraction cartridges connected in series. Naphthalene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benz[a]anthracene, chrysene, benzo[e]pyrene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, dibenz[a,h]anthracene, benzo[g,h,i]perylene, and indeno[1,2,3-cd]pyrene, were considered in the study. Quantification limits obtained for all of these compounds (between 0.4 and 14.8 microg kg(-1) dry mass) were well below of the limits recommended in the USA and EU. Overall recovery values ranged from 60 to 100%, with most losses being due to evaporation in the solvent exchange stages of the procedure, although excellent extraction recoveries were obtained. Validation of the accuracy was carried out with BCR-088 (sewage sludge) and BCR-524 (contaminated industrial soil) reference materials.

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

    Science.gov (United States)

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

    2015-06-07

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

  8. Sample preparation and biomass determination of SRF model mixture using cryogenic milling and the adapted balance method

    Energy Technology Data Exchange (ETDEWEB)

    Schnöller, Johannes, E-mail: johannes.schnoeller@chello.at; Aschenbrenner, Philipp; Hahn, Manuel; Fellner, Johann; Rechberger, Helmut

    2014-11-15

    Highlights: • An alternative sample comminution procedure for SRF is tested. • Proof of principle is shown on a SRF model mixture. • The biogenic content of the SRF is analyzed with the adapted balance method. • The novel method combines combustion analysis and a data reconciliation algorithm. • Factors for the variance of the analysis results are statistically quantified. - Abstract: The biogenic fraction of a simple solid recovered fuel (SRF) mixture (80 wt% printer paper/20 wt% high density polyethylene) is analyzed with the in-house developed adapted balance method (aBM). This fairly new approach is a combination of combustion elemental analysis (CHNS) and a data reconciliation algorithm based on successive linearisation for evaluation of the analysis results. This method shows a great potential as an alternative way to determine the biomass content in SRF. However, the employed analytical technique (CHNS elemental analysis) restricts the probed sample mass to low amounts in the range of a few hundred milligrams. This requires sample comminution to small grain sizes (<200 μm) to generate representative SRF specimen. This is not easily accomplished for certain material mixtures (e.g. SRF with rubber content) by conventional means of sample size reduction. This paper presents a proof of principle investigation of the sample preparation and analysis of an SRF model mixture with the use of cryogenic impact milling (final sample comminution) and the adapted balance method (determination of biomass content). The so derived sample preparation methodology (cutting mills and cryogenic impact milling) shows a better performance in accuracy and precision for the determination of the biomass content than one solely based on cutting mills. The results for the determination of the biogenic fraction are within 1–5% of the data obtained by the reference methods, selective dissolution method (SDM) and {sup 14}C-method ({sup 14}C-M)

  9. Accurate and Precise in Situ Zircon U-Pb age Dating With High Sample Throughput by Automated LA-SF-ICP-MS

    Science.gov (United States)

    Frei, D.; Gerdes, A.; Schersten, A.; Hollis, J. A.; Martina, F.; Knudsen, C.

    2006-12-01

    Zircon is an ubiquitous mineral in most crystalline rocks as well as clastic sediments. The high resistance to thermal resetting and physical erosion makes zircon an exceptionally useful mineral for precise and accurate dating of thermal geological events. For example, the analysis of the U-Pb ages of detrital zircon grains in clastic sediments is a powerful tool in sedimentary provenance studies. Accurate and precise U-Pb ages of > 100 zircon grains in a sample usually allow to detect all major sedimentary source age components with statistical confidence. U-Pb age dating of detrital zircons is generally the domain of high resolution ion microprobe techniques (high resolution SIMS), where relatively rapid in situ analysis can be achieved. The major limitations of these techniques are sample throughput (about 75 zircon age dates per 24 hours), the very high purchasing and operating costs of the equipment and the need for highly specialised personnel, resulting in high cost. These high costs usually impose uncomfortable restrictions on the number of samples that can be analysed in a provenance study. Here, we present a high sample throughput technique for highly accurate and precise U-Pb dating of zircons by laser ablation magnetic sectorfield inductively coupled plasma mass spectrometry (LA-SF-ICP-MS). This technique takes advantage of recent progress in laser technology and the introduction of magnetic sectorfield ICP-MS instruments. Based on a ThermoFinnigan Element2 magnetic sctorfield ICP-MS and a New Wave UP 213 laser ablation system, this techniques allows U-Pb dating of zircon grains with precision, accuray and spatial resolution comparable to high resolution SIMS. Because an individual analysis is carried out in less than two minutes and all data is acquired automated in pre-set mode with only minimal operator presence, the sample throughput is an order of magnitude higher compared to high resolution SIMS. Furthermore, the purchasing and operating costs of

  10. Solar UV-assisted sample preparation of river water for ultra-trace determination of uranium by adsorptive stripping voltammetry

    International Nuclear Information System (INIS)

    The article describes how solar ultraviolet-A radiation can be used to digest samples as needed for voltammetric ultratrace determination of uranium(VI) in river water. We applied adsorptive stripping voltammetry (AdSV) using chloranilic acid as the complexing agent. Samples from the river Warnow in Rostock (Germany) were pretreated with either soft solar UV or wit artificial hard UV from a 30-W source emitting 254-nm light. Samples were irradiated for 12 h, and both methods yielded the same results. We were able to detect around 1 μg.L-1 of uranium(VI) in a sample of river water that also contained dissolved organic carbon at a higher mg.L-1 levels. No AdSV signal was obtained for U(VI) without any UV pre-treatment. Pseudo-polarographic experiments confirmed the dramatic effect of both digestion techniques the the AdSV response. The new method is recommended for use in mobile ultratrace voltammetry of heavy metals for most kinds of natural water samples including tap, spring, ground, sea, and river waters. The direct use of solar radiation for sample pre-treatment represents a sustainable technique for sample preparation that does not consume large quantities of chemicals or energy. (author)

  11. Mercury Determination in Fish Samples by Chronopotentiometric Stripping Analysis Using Gold Electrodes Prepared from Recordable CDs

    Directory of Open Access Journals (Sweden)

    Andrei Florin Danet

    2008-11-01

    Full Text Available A simple method for manufacturing gold working electrodes for chronopotentiometric stripping measurements from recordable CD-R’s is described. These gold electrodes are much cheaper than commercially available ones. The electrochemical behavior of such an electrode and the working parameters for mercury determination by chronopotentiometric stripping analysis were studied. Detection limit was 0.30 μg Hg/L and determination limit was 1.0 μg Hg/L for a deposition time of 600 s. Using the developed working electrodes it was possible to determine the total mercury in fish samples. A method for fish sample digestion was developed by using a mixture of fuming nitric acid and both concentrated sulfuric and hydrochloric acids. The recovery degree for a known amount of mercury introduced in the sample before digestion was 95.3% (n=4.

  12. Optimisation Of Preparation And Measurement Protocols For Luminescence Dating Of Small Samples From A Suite Of Porcelains And Faiences

    Science.gov (United States)

    Burbridge, C. I.; Rodrigues, A. L.; Dias, M. I.; Prudencio, M. I.; Cardoso, G.

    Experiments designed to evaluate protocols for preparation and luminescence measurement of small samples (ceramics are described. These include: additive TL of untreatedmaterial; multiple stimulation (Predose TL, OSL, TL) of hydrofluoric washed fragments; Simplified Predose and SAR OSL of silicate powders from hydrochloric and fluorosilicic acid treatment. The 110°C TL signal in the Simplified Predose technique minimised required sample size, but growth with cumulative predose was sub-linear. For exponential extrapolations 11/26 faience samples yielded results within 1σ of typological expectations, but substantial scatter was interpreted as relating to radiation quenching effects. Extrapolation errors were investigated by deactivating samples and regenerating their predose responses. Acid treatment of cores drilled from sherds enabled preparation of mineral and grain-size fractions while avoiding crushing effects, and damage to or contamination by the glaze and decoration. Results of luminescence measurements indicate that future work should focus on the use of open detection filter combinations to increase signal levels, to enable quenching corrections in predose measurements and the use of high temperature TL signals.

  13. OPTIMAL METHOD FOR PREPARATION OF SILICATE ROCK SAMPLES FOR ANALYTICAL PURPOSES

    Directory of Open Access Journals (Sweden)

    Maja Vrkljan

    2004-12-01

    Full Text Available The purpose of this study was to determine an optimal dissolution method for silicate rock samples for further analytical purposes. Analytical FAAS method of determining cobalt, chromium, copper, nickel, lead and zinc content in gabbro sample and geochemical standard AGV-1 has been applied for verification. Dissolution in mixtures of various inorganic acids has been tested, as well as Na2CO3 fusion technique. The results obtained by different methods have been compared and dissolution in the mixture of HNO3 + HF has been recommended as optimal.

  14. Automation of NMR measurements and data evaluation for systematically screening interactions of small molecules with target proteins

    International Nuclear Information System (INIS)

    In this technical note we describe the setup and application of automated sample preparation and usage of flow-through NMR equipment for the characterization of ligand binding on proteins. In addition, we focus on the perspectives of automated analysis of 2D HSQC spectra to identify changes in patterns indicative for ligand binding or changes of sample conditions. In this context we discuss a combination of statistical and non-statistical data analysis

  15. A Filtration Based Technique for Simultaneous SEM and TEM Sample Preparation for the Rapid Detection of Pathogens

    Directory of Open Access Journals (Sweden)

    Daniel R. Beniac

    2014-09-01

    Full Text Available Diagnostic electron microscopy for infectious diseases has the advantage that “everything” in the specimen can be observed, without a priori knowledge of the likely identity of the microorganisms present in the sample. The classical specimen preparation method used employs a droplet of sample, which allows particles to adsorb to a support film, and is subsequently negative stained. This “grid on drop” procedure has a sensitivity range of approximately 106 viruses per mL if no enrichment procedures are used. In the current investigation we present a novel use of filtration that allows us to detect viruses at concentrations as low as 102 viruses per mL. We present here methods based on filtration, in which total virus, and not virus concentration, is the limiting factor for detection. We show that filtration is more sensitive than conventional negative staining and can detect as few as 5 × 103 particles per sample.

  16. Preparation and characterization of sup 35 Cl and sup 36 Cl samples for (n,p) cross section measurements

    Energy Technology Data Exchange (ETDEWEB)

    Eykens, R.; Goetz, A.; Lamberty, A.; Gestel, J. van; Pauwels, J. (Commission of the European Communities, Joint Research Centre, Central Bureau for Nuclear Measurements, Geel (Belgium)); Wagemans, C.; Druyts, S. (Nuclear Physics Lab., State Univ., Ghent (Belgium)); Hondt, P. d' (SCK/CEN, Mol (Belgium))

    1991-05-15

    The {sup 35}Cl(n,p) and the {sup 36}Cl(n,p) reactions are of great importance for astrophysics. Several silver chloride samples were evaporated on platinum coated aluminium backings. The sample definition has been achieved by combining destructive and non-destructive methods. The isotopic composition of the {sup 36}Cl-enriched material was verified. Pulse height spectra of {sup 35}Cl(n{sub th},p) and {sup 36}Cl(n{sub th},p) are shown. The samples prepared and assayed in this way have proven to fulfil the experimental requirements and have been used to determine the reaction cross sections of {sup 35}Cl(n{sub th},p) and {sup 36}Cl(n{sub th},p). (orig.).

  17. Influence Of Sample Preparation Method On Isothermal Studies During Compatibility Screening Of Ofloxacin; Correlation With DSC Data

    Directory of Open Access Journals (Sweden)

    M. Misra, A. K. MISRA,, G. M. Panpalia

    2011-05-01

    Full Text Available Objectives: The compatibility of ofloxacin with somecommonly used diluents has been investigated usingisothermal stability studies (IST to allow relative ranking.Materials and Methods: The samples were prepared usingthree methods namely physical admixtures (with 5% addedmoisture, slugging and kneading in order to evaluate theeffect of mechanical treatment on the physicochemical stabilityof drug. To further verify the results of IST fresh binarymixtures were subjected to thermal analysis and an attemptwas made to correlate the results obtained from the twostudies.Results: The results from both DSC and IST revealed thatofloxacin was compatible with all the diluents used in thestudy. Among the three methods of sample preparation usedfor the study, the extent of degradation was more or less samein all the three methods indicating least influence of method ofsample preparation on the results of IST.Conclusions: From the study it was concluded that a betterco-correlation could have been obtained had ofloxacin beenmore unstable with few of the excipients than rest, used in thestudy. This way the extent of degradation would bedistinguishing enough to rank the excipients in decreasingorder of stability.

  18. Molecularly imprinted polymeric stir bar: Preparation and application for the determination of naftopidil in plasma and urine samples.

    Science.gov (United States)

    Peng, Jun; Xiao, Deli; He, Hua; Zhao, Hongyan; Wang, Cuixia; Shi, Tian; Shi, Kexin

    2016-01-01

    In this study, molecularly imprinting technology and stir bar absorption technology were combined to develop a microextraction approach based on a molecularly imprinted polymeric stir bar. The molecularly imprinted polymer stir bar has a high performance, is specific, economical, and simple to prepare. The obtained naftopidil-imprinted polymer-coated bars could simultaneously agitate and adsorb naftopidil in the sample solution. The ratio of template/monomer/cross-linker and conditions of template removal were optimized to prepare a stir bar with highly efficient adsorption. Fourier transform infrared spectroscopy, scanning electron microscopy, selectivity, and extraction capacity experiments showed that the molecularly imprinted polymer stir bar was prepared successfully. To utilize the molecularly imprinted polymer stir bar for the determination of naftopidil in complex body fluid matrices, the extraction time, stirring speed, eluent, and elution time were optimized. The limits of detection of naftopidil in plasma and urine sample were 7.5 and 4.0 ng/mL, respectively, and the recoveries were in the range of 90-112%. The within-run precision and between-run precision were acceptable (relative standard deviation performance liquid chromatography was a convenient, rapid, efficient, and specific method for the precise determination of trace naftopidil in clinical analysis. PMID:26541792

  19. Preparation and applicability of fresh fruit samples for the identification of radiation treatment by EPR

    Energy Technology Data Exchange (ETDEWEB)

    Yordanov, Nicola D. [Laboratory EPR, Institute of Catalysis, Bulgarian Academy of Sciences, 1113 Sofia (Bulgaria)], E-mail: ndyepr@bas.bg; Aleksieva, Katerina [Laboratory EPR, Institute of Catalysis, Bulgarian Academy of Sciences, 1113 Sofia (Bulgaria)

    2009-03-15

    The results of electron paramagnetic resonance (EPR) study on fresh fruits (whole pulp of pears, apples, peaches, apricots, avocado, kiwi and mango) before and after gamma-irradiation are reported using two drying procedures before EPR investigation. In order to remove water from non-irradiated and irradiated samples of the first batch, the pulp of fresh fruits is pressed, and the solid residue is washed with alcohol and dried at room temperature. The fruits of the second batch are pressed and dried in a standard laboratory oven at 40 deg. C. The results obtained with both drying procedures are compared. All samples under study show a singlet EPR line with g=2.0048{+-}0.0005 before irradiation. Irradiation gives rise to typical 'cellulose-like' EPR spectrum featuring one intensive line with g=2.0048{+-}0.0005 and two very weak satellite lines situated 3 mT at left and right of the central line. Only mango samples show a singlet line after irradiation. The fading kinetics of radiation-induced EPR signal is studied for a period of 50 days after irradiation. When the irradiated fruit samples are stored in their natural state and dried just before each EPR measurement, the satellite lines are measurable for less than 17 days of storage. Irradiated fruit samples, when stored dried, lose for 50 days ca. 40% of their radiation-induced radicals if treated with alcohol or ca. 70% if dried in an oven. The reported results unambiguously show that the presence of the satellite lines in the EPR spectra could be used for identification of radiation processing of fresh fruits, thus extending the validity of European Protocol EN 1787 (2000). Foodstuffs-Detection of Irradiated Food Containing Cellulose by EPR Spectroscopy. European Committee for Standardisation. Brussels for dry herbs.

  20. Preparation and applicability of fresh fruit samples for the identification of radiation treatment by EPR

    Science.gov (United States)

    Yordanov, Nicola D.; Aleksieva, Katerina

    2009-03-01

    The results of electron paramagnetic resonance (EPR) study on fresh fruits (whole pulp of pears, apples, peaches, apricots, avocado, kiwi and mango) before and after gamma-irradiation are reported using two drying procedures before EPR investigation. In order to remove water from non-irradiated and irradiated samples of the first batch, the pulp of fresh fruits is pressed, and the solid residue is washed with alcohol and dried at room temperature. The fruits of the second batch are pressed and dried in a standard laboratory oven at 40 °C. The results obtained with both drying procedures are compared. All samples under study show a singlet EPR line with g=2.0048±0.0005 before irradiation. Irradiation gives rise to typical "cellulose-like" EPR spectrum featuring one intensive line with g=2.0048±0.0005 and two very weak satellite lines situated 3 mT at left and right of the central line. Only mango samples show a singlet line after irradiation. The fading kinetics of radiation-induced EPR signal is studied for a period of 50 days after irradiation. When the irradiated fruit samples are stored in their natural state and dried just before each EPR measurement, the satellite lines are measurable for less than 17 days of storage. Irradiated fruit samples, when stored dried, lose for 50 days ca. 40% of their radiation-induced radicals if treated with alcohol or ca. 70% if dried in an oven. The reported results unambiguously show that the presence of the satellite lines in the EPR spectra could be used for identification of radiation processing of fresh fruits, thus extending the validity of European Protocol EN 1787 (2000). Foodstuffs—Detection of Irradiated Food Containing Cellulose by EPR Spectroscopy. European Committee for Standardisation. Brussels for dry herbs.

  1. Preparation and applicability of fresh fruit samples for the identification of radiation treatment by EPR

    International Nuclear Information System (INIS)

    The results of electron paramagnetic resonance (EPR) study on fresh fruits (whole pulp of pears, apples, peaches, apricots, avocado, kiwi and mango) before and after gamma-irradiation are reported using two drying procedures before EPR investigation. In order to remove water from non-irradiated and irradiated samples of the first batch, the pulp of fresh fruits is pressed, and the solid residue is washed with alcohol and dried at room temperature. The fruits of the second batch are pressed and dried in a standard laboratory oven at 40 deg. C. The results obtained with both drying procedures are compared. All samples under study show a singlet EPR line with g=2.0048±0.0005 before irradiation. Irradiation gives rise to typical 'cellulose-like' EPR spectrum featuring one intensive line with g=2.0048±0.0005 and two very weak satellite lines situated 3 mT at left and right of the central line. Only mango samples show a singlet line after irradiation. The fading kinetics of radiation-induced EPR signal is studied for a period of 50 days after irradiation. When the irradiated fruit samples are stored in their natural state and dried just before each EPR measurement, the satellite lines are measurable for less than 17 days of storage. Irradiated fruit samples, when stored dried, lose for 50 days ca. 40% of their radiation-induced radicals if treated with alcohol or ca. 70% if dried in an oven. The reported results unambiguously show that the presence of the satellite lines in the EPR spectra could be used for identification of radiation processing of fresh fruits, thus extending the validity of European Protocol EN 1787 (2000). Foodstuffs-Detection of Irradiated Food Containing Cellulose by EPR Spectroscopy. European Committee for Standardisation. Brussels for dry herbs

  2. Fully automated ionic liquid-based headspace single drop microextraction coupled to GC-MS/MS to determine musk fragrances in environmental water samples.

    Science.gov (United States)

    Vallecillos, Laura; Pocurull, Eva; Borrull, Francesc

    2012-09-15

    A fully automated ionic liquid-based headspace single drop microextraction (IL-HS-SDME) procedure has been developed for the first time to preconcentrate trace amounts of ten musk fragrances extensively used in personal care products (six polycyclic musks, three nitro musks and one polycyclic musk degradation product) from wastewater samples prior to analysis by gas chromatography and ion trap tandem mass spectrometry (GC-IT-MS/MS). Due to the low volatility of the ILs, a large internal diameter liner (3.4 mm i.d.) was used to improve the ILs evaporation. Furthermore, a piece of glass wool was introduced into the liner to avoid the entrance of the ILs in the GC column and a guard column was used to prevent analytical column damages. The main factors influencing the IL-HS-SDME were optimized. For all species, the highest enrichments factors were achieved using 1 μL of 1-octyl-3-methylimidazolium hexafluorophosphate ([OMIM][PF(6)]) ionic liquid exposed in the headspace of 10 mL water samples containing 300 g L(-1) of NaCl and stirred at 750 rpm and 60 °C for 45 min. All compounds were determined by direct injection GC-IT-MS/MS with a chromatographic time of 19 min. Method detection limits were found in the low ng mL(-1) range between 0.010 ng mL(-1) and 0.030 ng mL(-1) depending on the target analytes. Also, under optimized conditions, the method gave good levels of intra-day and inter-day repeatabilities in wastewater samples with relative standard deviations varying between 3% and 6% and 5% and 11%, respectively (n=3, 1 ng mL(-1)). The applicability of the method was tested with different wastewater samples from influent and effluent urban wastewater treatment plants (WWTPs) and one potable treatment plant (PTP). The analysis of influent urban wastewater revealed the presence of galaxolide and tonalide at concentrations of between 2.10 ng mL(-1) and 0.29 ng mL(-1) and 0.32 ng mL(-1) and waters from PTP only galaxolide was found at a concentration higher than MQL.

  3. Comparison of sample preparation methods for reliable plutonium and neptunium urinalysis using automatic extraction chromatography

    DEFF Research Database (Denmark)

    Qiao, Jixin; Xu, Yihong; Hou, Xiaolin;

    2014-01-01

    This paper describes improvement and comparison of analytical methods for simultaneous determination of trace-level plutonium and neptunium in urine samples by inductively coupled plasma mass spectrometry (ICP-MS). Four sample pre-concentration techniques, including calcium phosphate, iron...... by manganese dioxide co-precipitation. The need of drying ashing (>= 7 h) for calcium phosphate co-precipitation and long-term aging (5 d) for iron hydroxide co-precipitation, respectively, rendered time-consuming analytical protocols. Despite the fact that evaporation is also somewhat time-consuming (1.5 d...... of plutonium and neptunium associated with organic compounds in real urine assays. In this work, different protocols for decomposing organic matter in urine were investigated, of which potassium persulfate (K2S2O8) treatment provided the highest chemical yield of neptunium in the iron hydroxide co...

  4. Preparation of Samples for Leaf Architecture Studies, A Method for Mounting Cleared Leaves

    Directory of Open Access Journals (Sweden)

    Alejandra Vasco

    2014-09-01

    Full Text Available Premise of the study: Several recent waves of interest in leaf architecture have shown an expanding range of approaches and applications across a number of disciplines. Despite this increased interest, examination of existing archives of cleared and mounted leaves shows that current methods for mounting, in particular, yield unsatisfactory results and deterioration of samples over relatively short periods. Although techniques for clearing and staining leaves are numerous, published techniques for mounting leaves are scarce. Methods and Results: Here we present a complete protocol and recommendations for clearing, staining, and imaging leaves, and, most importantly, a method to permanently mount cleared leaves. Conclusions: The mounting protocol is faster than other methods, inexpensive, and straightforward; moreover, it yields clear and permanent samples that can easily be imaged, scanned, and stored. Specimens mounted with this method preserve well, with leaves that were mounted more than 35 years ago showing no signs of bubbling or discoloration.

  5. Digestion and preparation methods of different samples determine elements produced hydride generation

    International Nuclear Information System (INIS)

    The aim of this work is to explain the principle of hydride generation technique, which is another technique of atomic absorption spectrometry, in addition to flame and graphite techniques. This technique is used to determine some metals and nonmetals (Se, Sn, Te, Sb, Bi, AS, Hg ) which produce volatile compounds in their reactions. The study focuses on the analytical capabilities of the hydride generation technique, the principle of hydride generation process, the interferences that affect the analysis process (spectra interference, chemical interference, kinetic interference, oxidation state interference, gas layer interference) and the methods to overcome these interferences. The working steps of the technique have been reported, finally some experimental work has been performed on different kind of samples such as: waste, tripolyphosphate, volcanic rock and phosphogypsum to determine mercury and blood sample to determine arsenic. (Authors)

  6. Considerations for the preparation of peat samples for palynology, and for the counting of pollen and non-pollen palynomorphs

    Directory of Open Access Journals (Sweden)

    F.M. Chambers

    2011-09-01

    Full Text Available Peat deposits are valuable archives for studying palaeoclimate, the history of local and regional vegetation, and human impact. The most widely applied laboratory analytical technique has been palynology (pollen analysis, which is often limited to the study of pollen and a few easily recognisable spores; however, a variety of other microfossils can be studied in peat deposits and can provide information on past environmental conditions. Among the so-called non-pollen palynomorphs (NPPs are fungal and algal spores that can be used as indicators for local hydrological changes and trophic conditions. This article provides an overview of aspects to consider and sample preparation methods for pollen, spores and other non-pollen palynomorph microfossils in peat deposits; advice on aids to pollen identification and counting; and a brief guide to the range of NPPs that can be counted from prepared subfossil-pollen microslides.

  7. Preparation and standardization of a sample of P 32 by liquid scintillation

    International Nuclear Information System (INIS)

    A procedure to standardize P 32 in liquid scintillation counting by labelling a tsributyl phosphate organic molecule is described. This method shows a high counting efficiency, over 99%, while keeping a good stability of samples in PCS or toluene, which vary less that 1% in two weed periods. The global uncertainty that results for calibrating the radioactive solution through this method has been less that 2.2%. (Author)

  8. Comparison of sample preparation methods for reliable plutonium and neptunium urinalysis using automatic extraction chromatography.

    Science.gov (United States)

    Qiao, Jixin; Xu, Yihong; Hou, Xiaolin; Miró, Manuel

    2014-10-01

    This paper describes improvement and comparison of analytical methods for simultaneous determination of trace-level plutonium and neptunium in urine samples by inductively coupled plasma mass spectrometry (ICP-MS). Four sample pre-concentration techniques, including calcium phosphate, iron hydroxide and manganese dioxide co-precipitation and evaporation were compared and the applicability of different techniques was discussed in order to evaluate and establish the optimal method for in vivo radioassay program. The analytical results indicate that the various sample pre-concentration approaches afford dissimilar method performances and care should be taken for specific experimental parameters for improving chemical yields. The best analytical performances in terms of turnaround time (6h) and chemical yields for plutonium (88.7 ± 11.6%) and neptunium (94.2 ± 2.0%) were achieved by manganese dioxide co-precipitation. The need of drying ashing (≥ 7h) for calcium phosphate co-precipitation and long-term aging (5d) for iron hydroxide co-precipitation, respectively, rendered time-consuming analytical protocols. Despite the fact that evaporation is also somewhat time-consuming (1.5d), it endows urinalysis methods with better reliability and repeatability compared with co-precipitation techniques. In view of the applicability of different pre-concentration techniques proposed previously in the literature, the main challenge behind relevant method development is pointed to be the release of plutonium and neptunium associated with organic compounds in real urine assays. In this work, different protocols for decomposing organic matter in urine were investigated, of which potassium persulfate (K2S2O8) treatment provided the highest chemical yield of neptunium in the iron hydroxide co-precipitation step, yet, the occurrence of sulfur compounds in the processed sample deteriorated the analytical performance of the ensuing extraction chromatographic separation with chemical

  9. Preparation of polyethylene sacks for collection of precipitation samples for chemical analysis

    Science.gov (United States)

    Schroder, L.J.; Bricker, A.W.

    1985-01-01

    Polyethylene sacks are used to collect precipitation samples. Washing polyethylene with acetone, hexane, methanol, or nitric acid can change the adsorptive characteristics of the polyethylene. In this study, simulated precipitation at pH 4.5 was in contact with the polyethylene sacks for 21 days; subsamples were removed for chemical analysis at 7, 14, and 21 days after intitial contact. Sacks washed with acetone adsorbed iron and lithium; sacks washed with hexane adsorbed barium, iron , and lithium; sacks washed with methanol adsorbed calcium and iron; and sacks washed with 0.30 N nitric acid adsorbed iron. Leaching the plastic sacks with 0.15 N nitric acid did not result in 100-percent recovery of any of the adsorbed metals. Washing polyethylene sacks with dilute nitric acid caused the pH of the simulated precipitation to be decreased by 0.2 pH unit after 1 week of contact with the polyethylene. The specific conductance increased by 10 microsiemens per centimeter. Contamination of precipitation samples by lead was determined to be about 0.1 microgram per liter from contact with precleaned polyethylene sacks. No measurable contamination of precipitation samples by zinc occurred. (USGS)

  10. The effects of water sample treatment, preparation, and storage prior to cyanotoxin analysis for cylindrospermopsin, microcystin and saxitoxin.

    Science.gov (United States)

    Kamp, Lisa; Church, Jennifer L; Carpino, Justin; Faltin-Mara, Erin; Rubio, Fernando

    2016-02-25

    Cyanobacterial harmful algal blooms occur in freshwater lakes, ponds, rivers, and reservoirs, and in brackish waters throughout the world. The wide variety of cyanotoxins and their congeners can lead to frequent exposure of humans through consumption of meat, fish, seafood, blue-green algal products and water, accidental ingestion of contaminated water and cyanobacterial scum during recreational activities, and inhalation of cyanobacterial aerosols. Cyanotoxins can also occur in the drinking water supply. In order to monitor human exposure, sensitive analytical methods such as enzyme linked immunosorbent assay and liquid chromatography-mass spectrometry are often used. Regardless of the analytical method of choice, some problems regularly occur during sample collection, treatment, storage, and preparation which cause toxin loss and therefore underestimation of the true concentration. To evaluate the potential influence of sample treatment, storage and preparation materials on surface and drinking water samples, the effects of different types of materials on toxin recovery were compared. Collection and storage materials included glass and various types of plastics. It was found that microcystin congeners LA and LF adsorbed to polystyrene, polypropylene, high density polyethylene and polycarbonate storage containers, leading to low recoveries (effect of various drinking water treatment chemicals on toxin recovery and the behavior of those chemicals in the enzyme linked immunosorbent assays were also studied and are summarized. PMID:26740478

  11. Combination of direct swim-up technique and discontinuous Percoll gradient centrifugation for sperm preparation of oligoasthenozoospermic samples.

    Science.gov (United States)

    Chen, S U; Ho, H N; Chen, H F; Chao, K H; Wu, M Y; Chen, C D; Huang, S C; Lee, T Y; Yang, Y S

    1996-01-01

    Sperm recovery for assisted reproduction in oligoasthenozoospermic patients is not satisfying either by the swim-up technique or by Percoll gradient centrifugation, and no single technique is constantly preferred. The design of this study was to evaluate the effects of combining the two methods on improving the efficacy of sperm preparation in these poor samples. For each semen sample, 1 mL was treated with a combination method, which used direct swim-up technique to recover motile sperm swimming to the supernatant, and then the residual semen was subjected to two-layer discontinuous Percoll gradient procedure for further recovery of motile sperm. Another 1 mL was prepared with two-layer discontinuous Percoll gradient centrifugation alone for comparison. Parameters measured included sperm concentration, number of progressively motile sperm, percentage of progressive motility, percentage of motile sperm recovery, amount of debris, percentage of normal forms according to Kruger's strict criteria, and motion characteristics of sperm using computer-aided motility analysis. The results of 30 oligoasthenozoospermic samples demonstrated that the combination method achieved a significantly greater recovery of motile sperm than the two-layer discontinuous Percoll gradient centrifugation did (43.2 +/- 19.7% vs. 32.2 +/- 14.3%, p method than in those of Percoll gradient centrifugation alone, but the difference was not significant (63.7 +/- 21.8% vs. 58.7 +/- 20.1%). The debris of semen was removed equally well by both methods. The percentage of normal forms as well as motion characteristics, including curvilinear velocity, straight-line velocity, mean amplitude of lateral head displacement, and linearity, were similar in the samples treated by these two procedures. The combination of the direct swim-up technique and discontinuous Percoll gradient centrifugation combines the advantages of each procedure and results in greater recovery of motile sperm in oligoasthenozoospermic

  12. High Throughput Sample Preparation and Analysis for DNA Sequencing, PCR and Combinatorial Screening of Catalysis Based on Capillary Array Technique

    Energy Technology Data Exchange (ETDEWEB)

    Yonghua Zhang

    2002-05-27

    Sample preparation has been one of the major bottlenecks for many high throughput analyses. The purpose of this research was to develop new sample preparation and integration approach for DNA sequencing, PCR based DNA analysis and combinatorial screening of homogeneous catalysis based on multiplexed capillary electrophoresis with laser induced fluorescence or imaging UV absorption detection. The author first introduced a method to integrate the front-end tasks to DNA capillary-array sequencers. protocols for directly sequencing the plasmids from a single bacterial colony in fused-silica capillaries were developed. After the colony was picked, lysis was accomplished in situ in the plastic sample tube using either a thermocycler or heating block. Upon heating, the plasmids were released while chromsomal DNA and membrane proteins were denatured and precipitated to the bottom of the tube. After adding enzyme and Sanger reagents, the resulting solution was aspirated into the reaction capillaries by a syringe pump, and cycle sequencing was initiated. No deleterious effect upon the reaction efficiency, the on-line purification system, or the capillary electrophoresis separation was observed, even though the crude lysate was used as the template. Multiplexed on-line DNA sequencing data from 8 parallel channels allowed base calling up to 620 bp with an accuracy of 98%. The entire system can be automatically regenerated for repeated operation. For PCR based DNA analysis, they demonstrated that capillary electrophoresis with UV detection can be used for DNA analysis starting from clinical sample without purification. After PCR reaction using cheek cell, blood or HIV-1 gag DNA, the reaction mixtures was injected into the capillary either on-line or off-line by base stacking. The protocol was also applied to capillary array electrophoresis. The use of cheaper detection, and the elimination of purification of DNA sample before or after PCR reaction, will make this approach an

  13. Optimized sample preparation for two-dimensional gel electrophoresis of soluble proteins from chicken bursa of Fabricius

    Directory of Open Access Journals (Sweden)

    Zheng Xiaojuan

    2009-10-01

    Full Text Available Abstract Background Two-dimensional gel electrophoresis (2-DE is a powerful method to study protein expression and function in living organisms and diseases. This technique, however, has not been applied to avian bursa of Fabricius (BF, a central immune organ. Here, optimized 2-DE sample preparation methodologies were constructed for the chicken BF tissue. Using the optimized protocol, we performed further 2-DE analysis on a soluble protein extract from the BF of chickens infected with virulent avibirnavirus. To demonstrate the quality of the extracted proteins, several differentially expressed protein spots selected were cut from 2-DE gels and identified by matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS. Results An extraction buffer containing 7 M urea, 2 M thiourea, 2% (w/v 3-[(3-cholamidopropyl-dimethylammonio]-1-propanesulfonate (CHAPS, 50 mM dithiothreitol (DTT, 0.2% Bio-Lyte 3/10, 1 mM phenylmethylsulfonyl fluoride (PMSF, 20 U/ml Deoxyribonuclease I (DNase I, and 0.25 mg/ml Ribonuclease A (RNase A, combined with sonication and vortex, yielded the best 2-DE data. Relative to non-frozen immobilized pH gradient (IPG strips, frozen IPG strips did not result in significant changes in the 2-DE patterns after isoelectric focusing (IEF. When the optimized protocol was used to analyze the spleen and thymus, as well as avibirnavirus-infected bursa, high quality 2-DE protein expression profiles were obtained. 2-DE maps of BF of chickens infected with virulent avibirnavirus were visibly different and many differentially expressed proteins were found. Conclusion These results showed that method C, in concert extraction buffer IV, was the most favorable for preparing samples for IEF and subsequent protein separation and yielded the best quality 2-DE patterns. The optimized protocol is a useful sample preparation method for comparative proteomics analysis of chicken BF tissues.

  14. Determination of aflatoxins in food samples by automated on-line in-tube solid-phase microextraction coupled with liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Nonaka, Y; Saito, K; Hanioka, N; Narimatsu, S; Kataoka, H

    2009-05-15

    A simple and sensitive automated method for determination of aflatoxins (B1, B2, G1, and G2) in nuts, cereals, dried fruits, and spices was developed consisting of in-tube solid-phase microextraction (SPME) coupled with liquid chromatography-mass spectrometry (LC-MS). Aflatoxins were separated within 8 min by high-performance liquid chromatography using a Zorbax Eclipse XDB-C8 column with methanol/acetonitrile (60/40, v/v): 5mM ammonium formate (45:55) as the mobile phase. Electrospray ionization conditions in the positive ion mode were optimized for MS detection of aflatoxins. The pseudo-molecular ions [M+H](+) were used to detect aflatoxins in selected ion monitoring (SIM) mode. The optimum in-tube SPME conditions were 25draw/eject cycles of 40 microL of sample using a Supel-Q PLOT capillary column as an extraction device. The extracted aflatoxins were readily desorbed from the capillary by passage of the mobile phase, and no carryover was observed. Using the in-tube SPME LC-MS with SIM method, good linearity of the calibration curve (r>0.9994) was obtained in the concentration range of 0.05-2.0 ng/mL using aflatoxin M1 as an internal standard, and the detection limits (S/N=3) of aflatoxins were 2.1-2.8 pg/mL. The in-tube SPME method showed >23-fold higher sensitivity than the direct injection method (10 microL injection volume). The within-day and between-day precision (relative standard deviations) at the concentration of 1 ng/mL aflatoxin mixture were below 3.3% and 7.7% (n=5), respectively. This method was applied successfully to analysis of food samples without interference peaks. The recoveries of aflatoxins spiked into nuts and cereals were >80%, and the relative standard deviations were Aflatoxins were detected at <10 ng/g in several commercial food samples. PMID:19328492

  15. Preparation of {sup 183,184}Re samples for modelling a rapid gas phase chemistry of Nielsbohrium (Ns), element 107

    Energy Technology Data Exchange (ETDEWEB)

    Eichler, R.; Gaeggeler, H.W.; Eichler, B.; Tuerler, A. [Paul Scherrer Inst. (PSI), Villigen (Switzerland)

    1997-09-01

    Chemical gas phase reactions of the heavier group 7 elements in the system O{sub 2}/H{sub 2}O are presumably best suited for a separation of Nielsbohrium from the lighter transactinides. We expect a higher reaction velocity using the more reactive gas system O{sub 3}/H{sub 2}O{sub 2}. For the experimental verification of this idea we prepared {sup 183}Re/{sup 184}Re samples for thermochromatography experiments with both gas systems. (author) 8 refs.

  16. Neutron beam preparation with Am-Be source for analysis of biological samples with PGNAA method

    International Nuclear Information System (INIS)

    Material analysis with prompt gamma neutron activation analysis (PGNAA) requires a proper geometrical arrangement for equipments in laboratory. Application of PGNAA in analysis of biological samples, due to small size of sample, needs attention to the dimension of neutron beam. In our work, neutron source has been made of 241Am-Be type. Activity of 241Am was 20 Ci which lead to neutron source strength of 4.4 x 107 neutrons per second. Water has been considered as the basic shielding material for the neutron source. The effect of various concentration of boric acid in the reduction of intensity of fast and thermal components of the neutron beam and gamma ray has been investigated. Gamma ray is produced by (α, n) reaction in Am-Be source (4.483 MeV), neutron capture by hydrogen (2.224 MeV), and neutron capture by boron (0.483 MeV). Various types of neutron and gamma ray dosimeters have been employed including BF3 and NE-213 detectors to detect fast and thermal neutrons. BGO scintillation detector has been used for gamma ray spectroscopy. It is shown that the gamma and neutron radiation dose due to direct beam is of the same magnitude as the dose due to radiation scattered in the laboratory ambient. It is concluded that 14 kg boric acid dissolved in 1,000 kg water is the optimum solution to surround the neutron source. The experimental results have been compared with Monte Carlo simulation. (author)

  17. Preparation of magnetic molecularly imprinted polymer for the separation of tetracycline antibiotics from egg and tissue samples.

    Science.gov (United States)

    Chen, Ligang; Liu, Jun; Zeng, Qinglei; Wang, Hui; Yu, Aimin; Zhang, Hanqi; Ding, Lan

    2009-05-01

    Magnetic molecularly imprinted polymers were prepared using hydrophobic Fe(3)O(4) magnetite as the magnetically susceptible component, oxytetracycline as template molecule, methacrylic acid as functional monomer, and styrene and divinylbenzene as polymeric matrix components. The polymers were applied to the separation of tetracycline antibiotics from egg and tissue samples. The extraction and clean-up procedures were carried out in a single step by blending and stirring the sample, extraction solvent and polymers. The analytes can be transferred from the sample matrix to the polymers directly or through the extraction solvent as medium. When the extraction was complete, the polymers adsorbing the analytes were easily separated from the sample matrix by an adscititious magnet. The analytes eluted from the polymers were determined by liquid chromatography-tandem mass spectrometry. The recoveries ranging from 72.8% to 96.5% were obtained with relative standard deviations in the range of 2.9-12.3%. The limit of detection was less than 0.2 ng g(-1). The feasibility of this method was validated by analysis of incurred egg and tissue samples, and the results were compared with those obtained by the classical method in which solvent extraction, centrifugation, and subsequent clean-up and concentration by solid-phase extraction were applied. The proposed method reduced the complicacy of classical method and improved the reliability of method. PMID:19268956

  18. Sample preparation for avian and porcine influenza virus cDNA amplification simplified: Boilign vs. conventional RNA extraction

    International Nuclear Information System (INIS)

    Full text: RNA extraction and purification is a fundamental step that allows for highly sensitive amplification of specific RNA targets in PCR applications. However, commercial extraction kits that are broadly used because of their robustness and high yield of purified RNA are expensive and labor-intensive. In this study, boiling in distilled water or a commerical lysis buffer of different sample matrices containing avian or porcine influenza viruses was tested as an alternative. Real-time PCR (RTaPCR) for nucleoprotein gene fragment was used as read out. Results were compared with freshly extracted RNA by use of a commercial extraction kit. Different batches of virus containing material materials, including diluted virus positive allontoic fluid or cell culture supernatnat, and avian faecal, cloacal or oropharyngeal swab samples were used in this study. Simple boiling of samples without any additional purification steps can be used as an alternative RNA preparation method to detect influenza A virus nucleoprotein RNA in oropharyngeal swab samples, allantoic fluid or cell-culture supernatant. The boiling method is not applicable for sample matrices containing faecal material. (author)

  19. A Microbiome DNA Enrichment Method for Next-Generation Sequencing Sample Preparation.

    Science.gov (United States)

    Yigit, Erbay; Feehery, George R; Langhorst, Bradley W; Stewart, Fiona J; Dimalanta, Eileen T; Pradhan, Sriharsa; Slatko, Barton; Gardner, Andrew F; McFarland, James; Sumner, Christine; Davis, Theodore B

    2016-01-01

    "Microbiome" is used to describe the communities of microorganisms and their genes in a particular environment, including communities in association with a eukaryotic host or part of a host. One challenge in microbiome analysis concerns the presence of host DNA in samples. Removal of host DNA before sequencing results in greater sequence depth of the intended microbiome target population. This unit describes a novel method of microbial DNA enrichment in which methylated host DNA such as human genomic DNA is selectively bound and separated from microbial DNA before next-generation sequencing (NGS) library construction. This microbiome enrichment technique yields a higher fraction of microbial sequencing reads and improved read quality resulting in a reduced cost of downstream data generation and analysis. © 2016 by John Wiley & Sons, Inc. PMID:27366894

  20. Sample preparation and system calibration for proton-induced X-ray emission analysis of hair from occupationally exposed workers

    International Nuclear Information System (INIS)

    Blood and urine collections are commonly used to monitor trace element concentration in the body. Hair may also be used. The concentration of many elements is much higher in hair than in either blood or urine and may provide a ready record of a period of exposure to heavy metals. Proton-induced X-ray emission (PIXE) has been used to study trace elements in hair. A method of preparing samples by charring hair and mixing with yttrium-spiked graphite has been developed. Thick targets suitable for PIXE analysis are made. The trace elements K, Ca, Tl, Mn, Fe, Ni, Cu, Zn, Pb, Br, Rb, and Sr are routinely measured in most samples and Cr, Co, As, Bi, Se, Zr, and Cd can be measured in occupationally exposed workers. Helium backscattering and elastic recoil detection are used to determine the major component H, C, N, O, and S. 23 references, 5 figures, 3 tables

  1. Simple and rapid sample preparation system for the molecular detection of antibiotic resistant pathogens in human urine.

    Science.gov (United States)

    Valiadi, Martha; Kalsi, Sumit; Jones, Isaac G F; Turner, Carrie; Sutton, J Mark; Morgan, Hywel

    2016-02-01

    Antibiotic resistance in urinary tract infections (UTIs) can cause significant complications without quick detection and appropriate treatment. We describe a new approach to capture, concentrate and prepare amplification-ready DNA from antibiotic resistant bacteria in human urine samples. Klebsiella pneumoniae NCTC13443 (bla CTX-M-15 positive) spiked into filtered human urine was used as a model system. Bacteria were captured using anion exchange diaethylaminoethyl (DEAE) magnetic microparticles and concentrated 200-fold within ~3.5 min using a custom, valve-less microfluidic chip. Eight samples were processed in parallel, and DNA was released using heat lysis from an integrated resistive heater. The crude cell lysate was used for real time Recombinase Polymerase Amplification (RPA) of the bla CTX-M-15 gene. The end to end processing time was approximately 15 min with a limit of detection of 1000 bacteria in 1 mL urine. PMID:26846875

  2. Taking samples from the reactor components in preparation for dismantling the TRIGA reactor at the Medical University of Hannover

    International Nuclear Information System (INIS)

    After shutting down the facility at the end of 1996 the spent TRIGA fuel elements from the research reactor at the Medical University of Hanover (MHH) were returned to the United States in the summer of 1999 and thus disposed of for the MHH. Consequently one of the main prerequisites for dismantling the TRIGA reactor as planned has been fulfilled. In preparation for dismantling the facility a number of samples were taken from the various reactor components in 2000. The aim of the samples being taken was to establish the radiological condition of the facility in more detail, in particular the condition of the activated components in the reactor tank and the biological shield in the core area. Up to now the calculated estimates for these components had been based mainly on the details provided in the facility documentation when operation started at the beginning of the 1970s, showing that the evaluation of the activity and dose rates was too high. This was confirmed in 1998 in the course of measuring contamination and dose rates when samples were taken from some reactor components before the fuel elements were removed. For example, drill samples were taken from the bottom part of a graphite blind element and from the central radiation beam tube in the core area and then analyzed by the U.R.A. Laboratory of the University of Regensburg. As it is planned to dismantle the reactor facility completely by hand, it is necessary to have realistic radiological data in order to prepare for the dismantling procedure. Furthermore, both the release of radioactive materials into the environment and the costs for external disposal of the radioactive waste from the dismantling of the reactor are to be kept to a minimum. (orig.)

  3. Library Automation

    OpenAIRE

    Dhakne, B. N.; Giri, V. V; Waghmode, S. S.

    2010-01-01

    New technologies library provides several new materials, media and mode of storing and communicating the information. Library Automation reduces the drudgery of repeated manual efforts in library routine. By use of library automation collection, Storage, Administration, Processing, Preservation and communication etc.

  4. Rapid sample preparation procedure for determination of retinol and α-tocopherol in human breast milk.

    Science.gov (United States)

    Kašparová, Markéta; Plíšek, Jiří; Solichová, Dagmar; Krčmová, Lenka; Kučerová, Barbora; Hronek, Miloslav; Solich, Petr

    2012-05-15

    The liposoluble vitamins (retinol and α-tocopherol) concentration in human breast milk is of a cardinal knowledge especially for nutrition of prematurely born. It enables the feeding optimization of these important micronutrients for preterm infants. The novel rapid liquid-liquid extraction procedure for human breast milk investigation was developed and validated according to FDA guidelines. The recovery of retinol was 82-90% measured at three concentration levels 1.0, 2.5 and 5.0 μmol/L, for α-tocopherol 92-109% at concentration levels 2.5, 5.0 and 10.0 μmol/L. The repeatability of extraction procedure expressed as relative standard deviation was 3.26% for retinol and 4.79% for α-tocopherol. Developed extraction procedure was applied on 120 human breast milk samples. The separation of vitamins was completed using advantages of a monolithic column which accomplished demands of acceleration made by modern bio-analytical HPLC methodology. The analytes of interest were detected by diode-array detector at wavelengths 325 nm for retinol and 290 nm for α-tocopherol. PMID:22483891

  5. Nano-Scale Tensile Testing and Sample Preparation Techniques for Silicon Nanowires

    Science.gov (United States)

    Fujii, Tatsuya; Sudoh, Koichi; Sakakihara, Shouichi; Naito, Muneyuki; Inoue, Shozo; Namazu, Takahiro

    2013-11-01

    In this paper, we describe an experimental technique to achieve a highly reliable characterization of the mechanical properties of silicon (Si) nanowires (NWs). A reusable on-chip Si device consisting of comb-drive electrostatic actuator for generating tensile force and capacitive sensors for measuring tensile force and displacement was designed and developed for quasi-static tensile test of Si NWs. The combination of focused ion beam (FIB) fabrication, FIB-assisted chemical vapor deposition, and probe manipulation enabled us to directly fabricate the NWs on the device. This sampling technique led to high yielding percentage of nano-scale tensile testing. The NWs were made from 200-nm-thick Si membranes that were produced by using silicon-on-nothing membrane fabrication technique. Several Si NWs were annealed at 700 °C in ultrahigh vacuum (UHV) for 5 min in order to examine the influence of annealing on the mechanical characteristics. The mean Young's modulus for nonannealed NWs was 129.1+/-10.1 GPa. After UHV annealing, the mean value was improved to be 168.1+/-1.3 GPa, comparable to the ideal value for Si(001)[110]. The annealing process gave rise to improving the Young's modulus, whereas it degraded the strength. Transmission electron microscopy suggested that recrystallization and gallium nanoclusters formation by annealing would have changed the mechanical characteristics.

  6. Accelerating sample preparation through enzyme-assisted microfiltration of Salmonella in chicken extract.

    Science.gov (United States)

    Vibbert, Hunter B; Ku, Seockmo; Li, Xuan; Liu, Xingya; Ximenes, Eduardo; Kreke, Thomas; Ladisch, Michael R; Deering, Amanda J; Gehring, Andrew G

    2015-01-01

    Microfiltration of chicken extracts has the potential to significantly decrease the time required to detect Salmonella, as long as the extract can be efficiently filtered and the pathogenic microorganisms kept in a viable state during this process. We present conditions that enable microfiltration by adding endopeptidase from Bacillus amyloliquefaciens to chicken extracts or chicken rinse, prior to microfiltration with fluid flow on both retentate and permeate sides of 0.2 μm cutoff polysulfone and polyethersulfone hollow fiber membranes. After treatment with this protease, the distribution of micron, submicron, and nanometer particles in chicken extracts changes so that the size of the remaining particles corresponds to 0.4-1 μm. Together with alteration of dissolved proteins, this change helps to explain how membrane fouling might be minimized because the potential foulants are significantly smaller or larger than the membrane pore size. At the same time, we found that the presence of protein protects Salmonella from protease action, thus maintaining cell viability. Concentration and recovery of 1-10 CFU Salmonella/mL from 400 mL chicken rinse is possible in less than 4 h, with the microfiltration step requiring less than 25 min at fluxes of 0.028-0.32 mL/cm(2) min. The entire procedure-from sample processing to detection by polymerase chain reaction-is completed in 8 h.

  7. Investigation of the sample preparation and curing treatment effects on mechanical properties and bioactivity of silica rich metakaolin geopolymer.

    Science.gov (United States)

    Catauro, M; Bollino, F; Papale, F; Lamanna, G

    2014-03-01

    In many biomedical applications both the biological and mechanical behaviours of implants are of relevant interest; in the orthopaedic field, for example, favourable bioactivity and biocompatibility capabilities are necessary, but at the same time the mechanical characteristics of the implants must be such as to allow one to support the body weight. In the present work, the authors have examined the application of geopolymers with composition H24AlK7Si31O79 and ratio Si/Al=31 to be used in biomedical field, considering two different preparation methods: one of the activators (KOH) has been added as pellets in the potassium silicate solution, in the other as a water solution with 8M concentration. Moreover, a different water content was used and only some of the synthesized samples were heat treated. The chemical and microstructural characterizations of those materials have been carried out by Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM). Subsequently, the effects of the adopted preparation on the mechanical and biological properties have been studied: compressive strength tests have demonstrated that more fragile specimens were obtained when KOH was added as a solution. The bioactivity was successfully evaluated with the soaking of the samples in a simulated body fluid (SBF) for 3 weeks. The formation of a layer of hydroxyapatite on the surface of the materials has been shown both by SEM micrographs and EDS analyses.

  8. The beauty of being (label)-free: sample preparation methods for SWATH-MS and next-generation targeted proteomics.

    Science.gov (United States)

    Vowinckel, Jakob; Capuano, Floriana; Campbell, Kate; Deery, Michael J; Lilley, Kathryn S; Ralser, Markus

    2013-01-01

    The combination of qualitative analysis with label-free quantification has greatly facilitated the throughput and flexibility of novel proteomic techniques. However, such methods rely heavily on robust and reproducible sample preparation procedures. Here, we benchmark a selection of in gel, on filter, and in solution digestion workflows for their application in label-free proteomics. Each procedure was associated with differing advantages and disadvantages. The in gel methods interrogated were cost effective, but were limited in throughput and digest efficiency. Filter-aided sample preparations facilitated reasonable processing times and yielded a balanced representation of membrane proteins, but led to a high signal variation in quantification experiments. Two in solution digest protocols, however, gave optimal performance for label-free proteomics. A protocol based on the detergent RapiGest led to the highest number of detected proteins at second-best signal stability, while a protocol based on acetonitrile-digestion, RapidACN, scored best in throughput and signal stability but came second in protein identification. In addition, we compared label-free data dependent (DDA) and data independent (SWATH) acquisition on a TripleTOF 5600 instrument. While largely similar in protein detection, SWATH outperformed DDA in quantification, reducing signal variation and markedly increasing the number of precisely quantified peptides. PMID:24741437

  9. The beauty of being (label)-free: sample preparation methods for SWATH-MS and next-generation targeted proteomics

    Science.gov (United States)

    Campbell, Kate; Deery, Michael J.; Lilley, Kathryn S.; Ralser, Markus

    2014-01-01

    The combination of qualitative analysis with label-free quantification has greatly facilitated the throughput and flexibility of novel proteomic techniques. However, such methods rely heavily on robust and reproducible sample preparation procedures. Here, we benchmark a selection of in gel, on filter, and in solution digestion workflows for their application in label-free proteomics. Each procedure was associated with differing advantages and disadvantages. The in gel methods interrogated were cost effective, but were limited in throughput and digest efficiency. Filter-aided sample preparations facilitated reasonable processing times and yielded a balanced representation of membrane proteins, but led to a high signal variation in quantification experiments. Two in solution digest protocols, however, gave optimal performance for label-free proteomics. A protocol based on the detergent RapiGest led to the highest number of detected proteins at second-best signal stability, while a protocol based on acetonitrile-digestion, RapidACN, scored best in throughput and signal stability but came second in protein identification. In addition, we compared label-free data dependent (DDA) and data independent (SWATH) acquisition on a TripleTOF 5600 instrument. While largely similar in protein detection, SWATH outperformed DDA in quantification, reducing signal variation and markedly increasing the number of precisely quantified peptides. PMID:24741437

  10. Polypyrrole solid phase microextraction: A new approach to rapid sample preparation for the monitoring of antibiotic drugs

    Energy Technology Data Exchange (ETDEWEB)

    Szultka, Malgorzata [Department of Environmental Chemistry and Bioanalytics, Faculty of Chemistry, Nicolaus, Copernicus University, Gagarin 7, 87-100 Torun (Poland); Kegler, Ricarda [Institute of Clinical Pharmacology, University of Rostock, Schillingallee 70, D-18057 Rostock (Germany); Fuchs, Patricia [Department of Anaesthesia and Intensive Care, University of Rostock, Schillingallee 35, D-18057 Rostock (Germany); Olszowy, Pawel [Department of Environmental Chemistry and Bioanalytics, Faculty of Chemistry, Nicolaus, Copernicus University, Gagarin 7, 87-100 Torun (Poland); Miekisch, Wolfram; Schubert, Jochen K. [Department of Anaesthesia and Intensive Care, University of Rostock, Schillingallee 35, D-18057 Rostock (Germany); Buszewski, Boguslaw [Department of Environmental Chemistry and Bioanalytics, Faculty of Chemistry, Nicolaus, Copernicus University, Gagarin 7, 87-100 Torun (Poland); Mundkowski, Ralf G., E-mail: ralf.mundkowski@med.uni-rostock.de [Institute of Clinical Pharmacology, University of Rostock, Schillingallee 70, D-18057 Rostock (Germany)

    2010-05-14

    Simple or even rapid bioanalytical methods are rare, since they generally involve complicated, time-consuming sample preparation from the biological matrices like LLE or SPE. SPME provides a promising approach to overcome these limitations. The full potential of this innovative technique for medical diagnostics, pharmacotherapy or biochemistry has not been tapped yet. In-house manufactured SPME probes with polypyrrole (PPy) coating were evaluated using three antibiotics of high clinical relevance - linezolid, daptomycin, and moxifloxacin - from PBS, plasma, and whole blood. The PPy coating was characterised by scanning electron microscopy. Influences of pH, inorganic salt, and blood anticoagulants were studied for optimum performance. Extraction yields were determined from stagnant media as well as re-circulating human blood using the heart-and-lung machine model system. The PPy-SPME fibres showed high extraction yields, particularly regarding linezolid. The reproducibility of the method was optimised to achieve RSDs of 9% or 17% and 7% for SPME from stagnant or re-circulating blood using fresh and re-used fibres, respectively. The PPy-SPME approach was demonstrated to meet the requirements of therapeutic monitoring of the drugs tested, even from re-circulating blood at physiological flow rates. SPME represents a rapid and simple dual-step procedure with potency to significantly reduce the effort and expenditure of complicated sample preparations in biomedical analysis.

  11. Matrix-assisted laser desorption/ionization sample preparation optimization for structural characterization of poly(styrene-co-pentafluorostyrene) copolymers

    International Nuclear Information System (INIS)

    Graphical abstract: -- Highlights: •We optimized sample preparation for MALDI TOF poly(styrene-copentafluorostyrene) co-polymers. •Influence of matrix choice was investigated. •Influence of matrix/analyte ratio was examined. •Influence of analyte/salt ratio (for Ag+ salt) was studied. -- Abstract: The influence of the sample preparation parameters (the choice of the matrix, matrix:analyte ratio, salt:analyte ratio) was investigated and optimal conditions were established for the MALDI time-of-flight mass spectrometry analysis of the poly(styrene-co-pentafluorostyrene) copolymers. These were synthesized by atom transfer radical polymerization. Use of 2,5-dihydroxybenzoic acid as matrix resulted in spectra with consistently high ion yields for all matrix:analyte:salt ratios tested. The optimized MALDI procedure was successfully applied to the characterization of three copolymers obtained by varying the conditions of polymerization reaction. It was possible to establish the nature of the end groups, calculate molecular weight distributions, and determine the individual length distributions for styrene and pentafluorostyrene monomers, contained in the resulting copolymers. Based on the data obtained, it was concluded that individual styrene chain length distributions are more sensitive to the change in the composition of the catalyst (the addition of small amount of CuBr2) than is the pentafluorostyrene component distribution

  12. Extraction chromatographic methods in the sample preparation sequence for thermal ionization mass spectrometric analysis of plutonium isotopes.

    Science.gov (United States)

    Grate, Jay W; O'Hara, Matthew J; Farawila, Anne F; Douglas, Matthew; Haney, Morgan M; Petersen, Steven L; Maiti, Tapas C; Aardahl, Christopher L

    2011-12-01

    A sample preparation sequence for actinide isotopic analysis by thermal ionization mass spectrometry (TIMS) is described that includes column-based extraction chromatography as the first separation step, followed by anion-exchange column separations. The sequence is designed to include a wet ashing step after the extraction chromatography to prevent any leached extractant or oxalic acid eluent reagents from interfering with subsequent separations, source preparation, or TIMS ionization. TEVA resin and DGA resin materials, containing extractants that consist only of C, N, O, and H atoms, were investigated for isolation of plutonium. Radiotracer level studies confirmed expected high yields from column-based separation procedures. Femtogram-level studies were carried out with TIMS detection, using multiple monoisotopic spikes applied sequentially throughout the separation sequence. Pu recoveries were 87% and 86% for TEVA and DGA resin separations, respectively. The Pu recoveries from 400 μL anion-exchange column separation sequences were 89% and 93% for trial sequences incorporating TEVA and DGA resin. Thus, a prior extraction chromatography step in the sequence did not interfere with the subsequent anion-exchange separation when a simple wet ash step was carried out in between these column separations. The average measurement efficiency for Pu, encompassing the chemical separation recoveries and the TIMS ionization efficiency, was 2.73% ± 0.77% (2σ) for the DGA resin trials and 2.67% ± 0.54% for the TEVA resin trials, compared to 3.41% and 2.37% (average 2.89%) for two control trials. These compare with an average measurement efficiency of 2.78% ± 1.70%, n = 33 from process benchmark analyses using Pu spikes processed through a sequence of oxalate precipitation, wet ash, iron hydroxide precipitation, and anion-exchange column separations. We conclude that extraction chromatography can be a viable separation procedure as part of a multistep sequence for TIMS

  13. Extraction chromatographic methods in the sample preparation sequence for thermal ionization mass spectrometric analysis of plutonium isotopes.

    Science.gov (United States)

    Grate, Jay W; O'Hara, Matthew J; Farawila, Anne F; Douglas, Matthew; Haney, Morgan M; Petersen, Steven L; Maiti, Tapas C; Aardahl, Christopher L

    2011-12-01

    A sample preparation sequence for actinide isotopic analysis by thermal ionization mass spectrometry (TIMS) is described that includes column-based extraction chromatography as the first separation step, followed by anion-exchange column separations. The sequence is designed to include a wet ashing step after the extraction chromatography to prevent any leached extractant or oxalic acid eluent reagents from interfering with subsequent separations, source preparation, or TIMS ionization. TEVA resin and DGA resin materials, containing extractants that consist only of C, N, O, and H atoms, were investigated for isolation of plutonium. Radiotracer level studies confirmed expected high yields from column-based separation procedures. Femtogram-level studies were carried out with TIMS detection, using multiple monoisotopic spikes applied sequentially throughout the separation sequence. Pu recoveries were 87% and 86% for TEVA and DGA resin separations, respectively. The Pu recoveries from 400 μL anion-exchange column separation sequences were 89% and 93% for trial sequences incorporating TEVA and DGA resin. Thus, a prior extraction chromatography step in the sequence did not interfere with the subsequent anion-exchange separation when a simple wet ash step was carried out in between these column separations. The average measurement efficiency for Pu, encompassing the chemical separation recoveries and the TIMS ionization efficiency, was 2.73% ± 0.77% (2σ) for the DGA resin trials and 2.67% ± 0.54% for the TEVA resin trials, compared to 3.41% and 2.37% (average 2.89%) for two control trials. These compare with an average measurement efficiency of 2.78% ± 1.70%, n = 33 from process benchmark analyses using Pu spikes processed through a sequence of oxalate precipitation, wet ash, iron hydroxide precipitation, and anion-exchange column separations. We conclude that extraction chromatography can be a viable separation procedure as part of a multistep sequence for TIMS

  14. Microbial profile of a kefir sample preparations: grains in natura and lyophilized and fermented suspension

    Directory of Open Access Journals (Sweden)

    Rafaela Strada de Oliveira Bergmann

    2010-12-01

    Full Text Available Probiotics are supplementary foods developed by microbial strains that improve animal health beyond basic nutrition. Probiotics are consumed orally, regardless of being considered as normal inhabitants of the intestines, able to survive in enzimatic and biliary secretions. Kefir is a probiotic originated from the old continent, fermented by several bacteria and yeasts, encapsulated in a polyssacharide matrix, and resembles jelly grains. Kefir is also presented as its sourish product both in sugary or milky suspensions containing vitamins, aminoacids, peptides, carbohydrates, ethanol, and volatile compounds. Kefir is known to have a diverse microbial content depending on the country and fermentative substrates, which cause distinct probiotic effects. In this sense, the purpose of this work was to isolate, identify, and quantify the microbial content of a native sugary kefir sample (fermented suspension and lyophilized natural grains. Serial dilutions were plated on Rogosa agar (AR and De Man, Rogosa and Sharpe (MRS, for Lactobacillus; Brain Heart Infusion (BHI, for total bacteria; Sabouraud-Dextrose-Agar (SDA, for yeasts and filamentous fungi; Thioglycolate Agar (TA, for Streptococcus, Acetobacteria and Leuconostoc; and Coconut Water Agar (CWA, and CWA supplemented with yeast extract (CWAY, for various genera. Genera and species for all strains were identified through biochemical reactions and specific API systems. The microbial profile of kefir was different from other sources of grains despite the presence of similar microorganisms and others which have not been reported yet. The data obtained with the CWA and CWAE media suggest that both substrates are alternative and salutary media for culture of kefir strains.

  15. Validation of an automated ELISA system for detection of antibodies to Aleutian mink disease virus using blood samples collected in filter paper strips

    OpenAIRE

    Knuuttila, Anna; Aronen, Pirjo; Eerola, Majvor; Gardner, Ian A; Virtala, Anna-Maija K; Vapalahti, Olli

    2014-01-01

    Background Aleutian mink disease virus (AMDV) is the cause of a chronic immune complex disease, Aleutian disease (AD), which is common in mink-producing countries. In 2005, implementation of an AMDV eradication programme in Finland created a need for an automated high-throughput assay. The aim of this study was to validate an AMDV-VP2 -recombinant antigen ELISA, which we developed earlier, in an automated assay format for the detection of anti-AMDV antibodies in mink blood and to determine th...

  16. Process automation

    International Nuclear Information System (INIS)

    Process automation technology has been pursued in the chemical processing industries and to a very limited extent in nuclear fuel reprocessing. Its effective use has been restricted in the past by the lack of diverse and reliable process instrumentation and the unavailability of sophisticated software designed for process control. The Integrated Equipment Test (IET) facility was developed by the Consolidated Fuel Reprocessing Program (CFRP) in part to demonstrate new concepts for control of advanced nuclear fuel reprocessing plants. A demonstration of fuel reprocessing equipment automation using advanced instrumentation and a modern, microprocessor-based control system is nearing completion in the facility. This facility provides for the synergistic testing of all chemical process features of a prototypical fuel reprocessing plant that can be attained with unirradiated uranium-bearing feed materials. The unique equipment and mission of the IET facility make it an ideal test bed for automation studies. This effort will provide for the demonstration of the plant automation concept and for the development of techniques for similar applications in a full-scale plant. A set of preliminary recommendations for implementing process automation has been compiled. Some of these concepts are not generally recognized or accepted. The automation work now under way in the IET facility should be useful to others in helping avoid costly mistakes because of the underutilization or misapplication of process automation. 6 figs

  17. Analysis of dissected tissues with digital holographic microscopy: quantification of inflammation mediated tissue alteration, influence of sample preparation, and reliability of numerical autofocusing

    Science.gov (United States)

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

    2015-03-01

    Quantitative phase imaging with digital holographic microscopy (DHM) allows label-free imaging of tissue sections and quantification of the spatial refractive index distribution, which is of interest for applications in digital pathology. We show that DHM allows quantitative imaging of different layers in unstained tissue samples by detection of refractive index changes. In addition, we evaluate the automated refocussing feature of DHM for application on dissected tissues and could achieve highly reproducible holographic autofocusing for unstained and moderately stained samples. Finally, it is demonstrated that in human ulcerative colitis patients the average tissue refractive index is reduced significantly in all parts of the inflamed colonic wall in comparison to patients in remission.

  18. Secondary Ion Mass Spectrometry Imaging of Molecular Distributions in Cultured Neurons and Their Processes: Comparative Analysis of Sample Preparation

    Science.gov (United States)

    Tucker, Kevin R.; Li, Zhen; Rubakhin, Stanislav S.; Sweedler, Jonathan V.

    2012-11-01

    Neurons often exhibit a complex chemical distribution and topography; therefore, sample preparation protocols that preserve structures ranging from relatively large cell somata to small neurites and growth cones are important factors in secondary ion mass spectrometry (SIMS) imaging studies. Here, SIMS was used to investigate the subcellular localization of lipids and lipophilic species in neurons from Aplysia californica. Using individual neurons cultured on silicon wafers, we compared and optimized several SIMS sampling approaches. After an initial step to remove the high salt culturing media, formaldehyde, paraformaldehyde, and glycerol, and various combinations thereof, were tested for their ability to achieve cell stabilization during and after the removal of extracellular media. These treatments improved the preservation of cellular morphology as visualized with SIMS imaging. For analytes >250 Da, coating the cell surface with a 3.2 nm-thick gold layer increased the ion intensity; multiple analytes previously not observed or observed at low abundance were detected, including intact cholesterol and vitamin E molecular ions. However, once a sample was coated, many of the lower molecular mass (cultured neurons over a broad mass range with enhanced image contrast.

  19. Desorption electrospray ionisation mass spectrometry: A rapid screening tool for veterinary drug preparations and forensic samples from hormone crime investigations

    International Nuclear Information System (INIS)

    Hormone and veterinary drug screening and forensics can benefit from the recent developments in desorption electrospray ionisation (DESI) mass spectrometry (MS). In this work the feasibility of DESI application has been studied. Using a linear ion trap or quadrupole time-of-flight (TOF) MS instrument both full-scan and data-dependent collision-induced dissociation MSn spectra were acquired in seconds without sample preparation. Preliminary data are presented for the rapid screening of (pro)hormone supplement samples, an illegal steroid cocktail and forensic samples from veterinary drug investigations. The potential of this DESI approach is clearly demonstrated since compounds observed could be independently confirmed by liquid chromatography/TOFMS with accurate mass measurement, and/or proton nuclear magnetic resonance spectroscopy. Specific concerns related to false-positive and false-negative findings due to limitations in quantification and memory-effects are briefly discussed. It is envisaged that DESI will achieve a prominent role in hormone and veterinary drug analysis in the near future

  20. Rapid preparation of expanded graphite by microwave irradiation for the extraction of triazine herbicides in milk samples.

    Science.gov (United States)

    Zhang, Fengshuang; Zhao, Qi; Yan, Xu; Li, Huiyu; Zhang, Ping; Wang, Long; Zhou, Tianyu; Li, Yi; Ding, Lan

    2016-04-15

    In this study, we proposed a rapid and efficient method for the preparation of the expanded graphite (EG). The exfoliation process was accelerated by microwave irradiation, and the preparation time was greatly shortened. The obtained EG was worm-like in shape and exhibits well exfoliated structure. It was successfully applied as solid-phase extraction (SPE) adsorbent to extract and clean up the triazine herbicides in milk, followed by liquid chromatography tandem mass spectrometry (LC-MS) analysis. The parameters affecting the performance of extraction and LC-MS analysis were evaluated. Under the optimal conditions, the detection limits of triazines are in the range of 0.03-0.12 ng mL(-1). At the spiked level (0.4 ng mL(-1)), the recoveries of triazines are in the range of 82.5±2.5% to 97.5±7.5%. The proposed method was successfully applied to determine six triazines in six milk samples.

  1. Optimisation of sample preparation and analysis conditions for atom probe tomography characterisation of low concentration surface species

    Science.gov (United States)

    Douglas, J. O.; Bagot, P. A. J.; Johnson, B. C.; Jamieson, D. N.; Moody, M. P.

    2016-08-01

    The practicalities for atom probe tomography (APT) analysis of near-surface chemistry, particularly the distribution of low concentration elements, are presented in detail. Specifically, the challenges of surface analysis using APT are described through the characterisation of near-surface implantation profiles of low concentration phosphorus into single crystal silicon. This material system was chosen to illustrate this surface specific approach as low concentration phosphorus has significant mass spectra overlaps with silicon species and the near surface location requires particular attention to focused ion beam specimen preparation and deposition of various capping layers. Required changes to standard sample preparation procedure are described and the effects of changes in APT analysis parameters are discussed with regards to this specific material system. Implantation profiles of 14 kV phosphorus ions with a predicted peak concentration of 0.2 at .% were successfully analysed using APT using pulsed laser assisted evaporation. It is demonstrated that the most important factor in obtaining the most accurate implantation profile was to ensure all phosphorus mass peaks were as free of background noise as possible, with thermal tails from the Si2+ ions obscuring the P2+ ions being the major overlap in the mass spectrum. The false positive contribution to the phosphorus profiles from hydride species appears minimal at the capping layer/substrate interface. The initial capping layer selection of nickel was successful in allowing the analysis of the majority of the phosphorus profile but nickel and phosphorus mass spectra overlaps prevent optimum quantification of phosphorus at the surface.

  2. Rapid preparation of expanded graphite by microwave irradiation for the extraction of triazine herbicides in milk samples.

    Science.gov (United States)

    Zhang, Fengshuang; Zhao, Qi; Yan, Xu; Li, Huiyu; Zhang, Ping; Wang, Long; Zhou, Tianyu; Li, Yi; Ding, Lan

    2016-04-15

    In this study, we proposed a rapid and efficient method for the preparation of the expanded graphite (EG). The exfoliation process was accelerated by microwave irradiation, and the preparation time was greatly shortened. The obtained EG was worm-like in shape and exhibits well exfoliated structure. It was successfully applied as solid-phase extraction (SPE) adsorbent to extract and clean up the triazine herbicides in milk, followed by liquid chromatography tandem mass spectrometry (LC-MS) analysis. The parameters affecting the performance of extraction and LC-MS analysis were evaluated. Under the optimal conditions, the detection limits of triazines are in the range of 0.03-0.12 ng mL(-1). At the spiked level (0.4 ng mL(-1)), the recoveries of triazines are in the range of 82.5±2.5% to 97.5±7.5%. The proposed method was successfully applied to determine six triazines in six milk samples. PMID:26617038

  3. Sample preparation for nanoanalytical electron microscopy using the FIB lift-out method and low energy ion milling

    International Nuclear Information System (INIS)

    Thinning specimens to electron transparency for electron microscopy analysis can be done by conventional (2-4 kV) argon ion milling or focused ion beam (FIB) lift-out techniques. Both these methods tend to leave 'mottling' visible on thin specimen areas, and this is believed to be surface damage caused by ion implantation and amorphisation. A low energy (250-500 V) Argon ion polish has been shown to greatly improve specimen quality for crystalline silicon samples. Here we investigate the preparation of technologically important materials for nanoanalysis using conventional and lift-out methods followed by a low energy polish in a GentleMillTM low energy ion mill. We use a low energy, low angle (6-8 deg.) ion beam to remove the surface damage from previous processing steps. We assess this method for the preparation of technologically important materials, such as steel, silicon and GaAs. For these materials the ability to create specimens from specific sites, and to be able to image and analyse these specimens with the full resolution and sensitivity of the STEM, allows a significant increase of the power and flexibility of nanoanalytical electron microscopy

  4. Changes of the elemental distributions in marine diatoms as a reporter of sample preparation artefacts. A nuclear microscopy application

    Energy Technology Data Exchange (ETDEWEB)

    Godinho, R.M. [Instituto de Bioengenharia e Biociências, Instituto Superior Técnico, Universidade de Lisboa, Lisboa (Portugal); Instituto Português do Mar e da Atmosfera, Lisboa (Portugal); Centro Interdisciplinar de Investigação Marinha e Ambiental, Universidade do Porto, Porto (Portugal); Cabrita, M.T. [Instituto Português do Mar e da Atmosfera, Lisboa (Portugal); Centro Interdisciplinar de Investigação Marinha e Ambiental, Universidade do Porto, Porto (Portugal); Alves, L.C. [Centro de Ciências e Tecnologias Nucleares, Instituto Superior Técnico, Universidade de Lisboa, Sacavém (Portugal); Pinheiro, T., E-mail: murmur@ctn.ist.utl.pt [Instituto de Bioengenharia e Biociências, Instituto Superior Técnico, Universidade de Lisboa, Lisboa (Portugal)

    2015-04-01

    Studies of the elemental composition of whole marine diatoms cells have high interest as they constitute a direct measurement of environmental changes, and allow anticipating consequences of anthropogenic alterations to organisms, ecosystems and global marine geochemical cycles. Nuclear microscopy is a powerful tool allowing direct measurement of whole cells giving qualitative imaging of distribution, and quantitative determination of intracellular concentration. Major obstacles to the analysis of marine microalgae are high medium salinity and the recurrent presence of extracellular exudates produced by algae to maintain colonies in natural media and in vitro. The objective of this paper was to optimize the methodology of sample preparation of marine unicellular algae for elemental analysis with nuclear microscopy, allowing further studies on cellular response to metals. Primary cultures of Coscinodiscus wailesii maintained in vitro were used to optimize protocols for elemental analysis with nuclear microscopy techniques. Adequate cell preparation procedures to isolate the cells from media components and exudates were established. The use of chemical agents proved to be inappropriate for elemental determination and for intracellular morphological analysis. The assessment of morphology and elemental partitioning in cell compartments obtained with nuclear microscopy techniques enabled to infer their function in natural environment and imbalances in exposure condition. Exposure to metal affected C. wailesii morphology and internal elemental distribution.

  5. Automated headspace-solid-phase micro extraction-retention time locked-isotope dilution gas chromatography-mass spectrometry for the analysis of organotin compounds in water and sediment samples.

    Science.gov (United States)

    Devosa, Christophe; Vliegen, Maarten; Willaert, Bart; David, Frank; Moens, Luc; Sandra, Pat

    2005-06-24

    An automated method for the simultaneous determination of six important organotin compounds namely monobutyltin (MBT), dibutyltin (DBT), tributyltin (TBT), monophenyltin (MPhT), diphenyltin (DPhT) and triphenyltin (TPhT) in water and sediment samples is described. The method is based on derivatization with sodium tetraethylborate followed by automated headspace-solid-phase micro extraction (SPME) combined with GC-MS under retention time locked (RTL) conditions. Home-synthesized deuterated organotin analogues were used as internal standards. Two high abundant fragment ions corresponding to the main tin isotopes Sn118 and Sn120 were chosen; one for quantification and one as qualifier ion. The method was validated and excellent figures of merit were obtained. Limits of quantification (LOQs) are from 1.3 to 15 ng l(-1) (ppt) for water samples and from 1.0 to 6.3 microg kg(-1) (ppb) for sediment samples. Accuracy for sediment samples was tested on spiked real-life sediment samples and on a reference PACS-2 marine harbor sediment. The developed method was used in a case-study at the harbor of Antwerp where sediment samples in different areas were taken and subsequently screened for TBT contamination. Concentrations ranged from 15 microg kg(-1) in the port of Antwerp up to 43 mg kg(-1) near a ship repair unit. PMID:16038329

  6. Sample preparation followed by HPLC under harmless 100% aqueous conditions for determination of oxytetracycline in milk and eggs.

    Science.gov (United States)

    Furusawa, Naoto

    2004-05-01

    A simple and hazardous chemical-free method for the high-performance liquid chromatographic determination of oxytetracycline (OTC) residues in milk and eggs has been developed. Sample preparation consists in homogenization with an aqueous solution by means of a handheld ultrasonic homogenizer followed by centrifugal ultrafiltration. HPLC is performed with an isocratic aqueous mobile phase and a photodiode array detector. Average recoveries of OTC (0.05, 0.1, and 0.2 microg mL(-1) for milk; 0.1, 0.2, and 0.4 microg mL(-1) for eggs) were > or =84% with relative standard deviations of solvents or hazardous reagents were used. PMID:15335039

  7. Towards a complete {sup 14}C AMS facility at the Universidade Federal Fluminense (Niteroi, Brazil): Sample preparation laboratory tests

    Energy Technology Data Exchange (ETDEWEB)

    Anjos, R.M., E-mail: meigikos@if.uff.br [Instituto de Fisica, Universidade Federal Fluminense, Av. Gal Milton Tavares de Souza, s/no, Gragoata, 24210-346 Niteroi, RJ (Brazil); Macario, K.D.; Gomes, P.R.S.; Linares, R.; Queiroz, E.; Carvalho, C. [Instituto de Fisica, Universidade Federal Fluminense, Av. Gal Milton Tavares de Souza, s/no, Gragoata, 24210-346 Niteroi, RJ (Brazil)

    2013-01-15

    Highlights: Black-Right-Pointing-Pointer We report a new AMS facility at the Physics Institute of UFF in Brazil. Black-Right-Pointing-Pointer A NEC 250 kV single stage accelerator mass spectrometer (SSAMS). Black-Right-Pointing-Pointer The first lab to perform the {sup 14}C-AMS technique not only in Brazil but in Latin America. Black-Right-Pointing-Pointer We report preliminary results and plans for the future. - Abstract: The new radiocarbon sample preparation laboratory at the Physics Institute of the Universidade Federal Fluminense (UFF) in Brazil is discussed and early trials with reference materials are presented, leading up to the installation of a single-stage AMS system in early 2012.

  8. Cyclization of the N-Terminal X-Asn-Gly Motif during Sample Preparation for Bottom-Up Proteomics

    DEFF Research Database (Denmark)

    Zhang, Xumin; Højrup, Peter

    2010-01-01

    We, herein, report a novel -17 Da peptide modification corresponding to an N-terminal cyclization of peptides possessing the N-terminal motif of X-Asn-Gly. The cyclization occurs spontaneously during sample preparation for bottom-up proteomics studies. Distinct from the two well-known N......-terminal cyclizations, cyclization of N-terminal glutamine and S-carbamoylmethylcysteine, it is dependent on pH instead of [NH(4)(+)]. The data set from our recent study on large-scale N(α)-modified peptides revealed a sequence requirement for the cyclization event similar to the well-known deamidation of Asn to iso......Asp and Asp. Detailed analysis using synthetic peptides confirmed that the cyclization forms between the N-terminus and its neighboring Asn residue, and the reaction shares the same succinimide intermediate with the Asn deamidation event. As a result, we, here, propose a molecular mechanism for this specific...

  9. Determination of thromboxanes, leukotrienes and lipoxins using high-temperature capillary liquid chromatography-tandem mass spectrometry and on-line sample preparation

    DEFF Research Database (Denmark)

    Dahl, Sandra Rinne; Kleiveland, Charlotte Ramstad; Kassem, Moustapha;

    2009-01-01

    culture supernatants was developed and validated. In the present method, a high temperature (70 degrees C) was used for the separation on the analytical column to obtain efficient chromatography of the thromboxanes. An on-line sample preparation was performed, where peptides/proteins contained...... in the matrix were removed by the SCX column. Sample pre-treatment included dilution and filtration, and the analysis time including all sample preparation steps was 60min per sample. Limits of detection in the range of 1-4ng/mL cell culture supernatant, recoveries between 30% and 100%, within day precisions...

  10. Investigation of the sample preparation and curing treatment effects on mechanical properties and bioactivity of silica rich metakaolin geopolymer

    Energy Technology Data Exchange (ETDEWEB)

    Catauro, M., E-mail: michelina.catauro@unina2.it; Bollino, F.; Papale, F.; Lamanna, G.

    2014-03-01

    In many biomedical applications both the biological and mechanical behaviours of implants are of relevant interest; in the orthopaedic field, for example, favourable bioactivity and biocompatibility capabilities are necessary, but at the same time the mechanical characteristics of the implants must be such as to allow one to support the body weight. In the present work, the authors have examined the application of geopolymers with composition H{sub 24}AlK{sub 7}Si{sub 31}O{sub 79} and ratio Si/Al = 31 to be used in biomedical field, considering two different preparation methods: one of the activators (KOH) has been added as pellets in the potassium silicate solution, in the other as a water solution with 8 M concentration. Moreover, a different water content was used and only some of the synthesized samples were heat treated. The chemical and microstructural characterizations of those materials have been carried out by Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM). Subsequently, the effects of the adopted preparation on the mechanical and biological properties have been studied: compressive strength tests have demonstrated that more fragile specimens were obtained when KOH was added as a solution. The bioactivity was successfully evaluated with the soaking of the samples in a simulated body fluid (SBF) for 3 weeks. The formation of a layer of hydroxyapatite on the surface of the materials has been shown both by SEM micrographs and EDS analyses. - Highlights: • Rich metakaolin geopolymer activated with KOH/K{sub 2}SiO{sub 3} and thermal treatment • Mechanical and bioactivity test to evaluate consolidation and bone bonding ability • Order of addition of reactants and thermal treatment influence mechanical properties.

  11. Isochron burial dating of Danube terraces in the course of an interlaboratory comparison on sample preparation in Vienna and Budapest

    Science.gov (United States)

    Neuhuber, Stephanie; Ruszkiczay-Rüdiger, Zsófia; Decker, Kurt; Braucher, Regis; Fiebig, Markus; Braun, Mihály; Häuselmann, Philipp; Aster Team

    2016-04-01

    -depositional history, but have different pre-exposure and transport histories [4]. The sandy gravel of the Haslau terrace was sampled in an active gravel pit. At this location, two major sedimentary units are separated by an erosional hiatus of unknown duration. The upper sequence was sampled at 5.5 m depth and the lower one was sampled at 11.8 m depth. From both depths six quartzite or quartz-bearing cobbles were taken together with a bulk sample from the matrix for isochron burial duration determination. Five samples were split after crushing and sieving and were processed at both the Cosmogenic Nuclide Sample Preparation Laboratory at Vienna and at Budapest (http://www.geochem.hu/kozmogen/Lab_en.html), in order to assess and compare the sample processing preocedures of these recently operating sample preparation laboratories. AMS measurements were performed at the French national facility ASTER (CEREGE (Aix-en-Provence, France). Thanks to OTKA PD83610, NKM-96/2014, NKM-31/2015; OMAA 90öu17; LP2012-27/2012. INSU/CNRS, the ANR through the program "EQUIPEX Investissement d'Avenir", IRD and CEA. [1] Decker et al., 2005. QSR 24, 307-322 [2] Hintersberger et al, 2013, EGU2013-12755 [3] Salcher et al. 2012. Tectonics, 31, TC3004, doi:10.1029/2011TC002979 [4] Balco and Rovey, 2008. AJS 908, 1083-1114 [5] Fuchs and Grill, 1984, Geologische Gebietskarte der Republik Österreich 1:200 000 Wien und Umgebung

  12. Development of a digital-analogue robotic system for input solution and mixed oxide samples

    International Nuclear Information System (INIS)

    Automated analytical systems for uranium and plutonium samples have been under development at the Nuclear Material Control Center (NMCC) since 1983. These include two systems for a large scale reprocessing plant for measurement of input solution samples and for measurement of mixed oxide (MOX) samples using automated destructive analysis procedures. Diverse tasks, such as designing the enclosures, developing the control systems and performing preparatory experiments, were combined. On the basis of NMCC's routine manual analysis, input solution sample analysis employing the isotope dilution method has been automated. A new method has been applied to automate the analysis of MOX powder samples. This method uses glass bead samples prepared by the system. Each sample may have different properties; therefore each is processed in different enclosures. The methods for the two analyses were quite different. The technical considerations were based on NMCC's ten years of expertise in nuclear material analysis. (author). 4 refs

  13. RNA-protein binding kinetics in an automated microfluidic reactor.

    Science.gov (United States)

    Ridgeway, William K; Seitaridou, Effrosyni; Phillips, Rob; Williamson, James R

    2009-11-01

    Microfluidic chips can automate biochemical assays on the nanoliter scale, which is of considerable utility for RNA-protein binding reactions that would otherwise require large quantities of proteins. Unfortunately, complex reactions involving multiple reactants cannot be prepared in current microfluidic mixer designs, nor is investigation of long-time scale reactions possible. Here, a microfluidic 'Riboreactor' has been designed and constructed to facilitate the study of kinetics of RNA-protein complex formation over long time scales. With computer automation, the reactor can prepare binding reactions from any combination of eight reagents, and is optimized to monitor long reaction times. By integrating a two-photon microscope into the microfluidic platform, 5-nl reactions can be observed for longer than 1000 s with single-molecule sensitivity and negligible photobleaching. Using the Riboreactor, RNA-protein binding reactions with a fragment of the bacterial 30S ribosome were prepared in a fully automated fashion and binding rates were consistent with rates obtained from conventional assays. The microfluidic chip successfully combines automation, low sample consumption, ultra-sensitive fluorescence detection and a high degree of reproducibility. The chip should be able to probe complex reaction networks describing the assembly of large multicomponent RNPs such as the ribosome.

  14. Elimination of the artefact peaks in capillary electrophoresis determination of glutamate by using organic solvents in sample preparation.

    Science.gov (United States)

    Campos, Camila Dalben Madeira; de Campos Braga, Patricia Aparecida; Reyes, Felix Guillermo Reyes; da Silva, José Alberto Fracassi

    2015-11-01

    Focusing on the demand from the food industry for fast and reliable alternative methods to control the quality of food products, we present in this paper a method for amino acid separation and glutamic acid quantification in complex matrices employing capillary electrophoresis with capacitively coupled contactless conductivity detection. We demonstrate by simulation and experimentally the use of organic solvents in sample preparation to prevent peak splitting and increase stacking in capillary electrophoretic separations of amino acids. Additionally, we obtained results for glutamic acid quantification comparable to those obtained via traditional methods used at industrial sites. We tested premium and low-cost samples with large variations in their glutamic acid content, which demonstrated the wide range of applicability of the method presented herein. The results of the proposed capacitively coupled contactless conductivity detection based capillary electrophoresis method agreed with those obtained by an enzymatic detector and ultra high performance liquid chromatography coupled to tandem mass spectrometry, considering a confidence level of 95%. PMID:26332708

  15. Thermoelectric properties of polycrystalline Zn{sub 4}Sb{sub 3} samples prepared by solid state reaction method

    Energy Technology Data Exchange (ETDEWEB)

    Cadavid, D. [Department of Physics, Universidad Nacional de Colombia, Bogota (Colombia); Rodriguez, J.E. [Department of Physics, Universidad Nacional de Colombia, Bogota (Colombia)], E-mail: jerodriguezl@unal.edu.co

    2008-11-30

    Seebeck coefficient S(T), electrical resistivity {rho}(T) and thermal conductivity {kappa}(T) measurements on polycrystalline Zn{sub 4}Sb{sub 3} compounds grown by solid state reaction method are presented; these transport properties were studied in the temperature range between 100 and 290 K. The Seebeck coefficient is positive over the measured temperature range and its magnitude increases with both temperature and the processing time up to reach values close to 240{mu}V/K. The electrical resistivity shows a weak semiconducting behavior, its magnitude increases with the processing time to reach values around 10m{omega}cm in the sample annealed during 5 h, then {rho}(T) decreases up to 0.5m{omega}cm. The thermal conductivity shows a linear temperature behavior, at room temperature, it reaches minimum values close to 0.5 W/K m. From {rho}(T), S(T) and {kappa}(T) data, it was possible to determine the thermoelectric power factor, PF and the dimensionless figure of merit ZT, which reach maximum values close to 14{mu}W/K{sup 2}cm and 0.2, respectively. The behavior of studied transport properties shows that these Zn{sub 4}Sb{sub 3} compounds can be prepared by using the solid state reaction method, which could allow to obtain proper samples to be used in technological thermoelectric applications.

  16. Determination of umckalin in commercial tincture and phytopreparations containing Pelargonium sidoides by HPLC: comparison of sample preparation procedures.

    Science.gov (United States)

    Franco, L; de Oliveira, B H

    2010-06-15

    Roots of Pelargonium sidoides D.C. are used for the production of phytomedicines. Current quality control of phytopreparations containing P. sidoides extracts has been made in terms of total phenolics content. In this work we describe the development and validation of an HPLC method for the analysis of P. sidoides tincture and commercial syrup phytopreparations using umckalin (7-hydroxy-5,6-dimethoxycoumarin) as chemical marker. Two sample preparation procedures, liquid-liquid extraction (LLE) and solid-phase extraction (SPE) were also developed and compared. The samples were analyzed by RP-HPLC and the two methods were then validated and compared. The repeatability of the two procedures showed coefficients of variation (CV) of 1.2% for SPE procedure, and 1.3% for LLE. Recovery for both methods was higher than 95.2%. The linearity showed correlation coefficients better than 0.999 for both methods. The detection and quantification limit were 0.0098 and 0.0298microgmL(-1), respectively. The validated procedure was then used for the analysis of tincture and five batches of two commercial phytopreparations containing P. sidoides tincture.

  17. Fully automated radiochemical preparation system for gamma-spectroscopy on fission products and the study of the intruder and vibrational levels in 83Se

    International Nuclear Information System (INIS)

    AUTOBATCH was developed to provide a usable source of short-lived neutron-rich nuclides through chemical preparation of the sample from fission products for detailed gamma-ray spectroscopy, which would complement the output of on-line isotope separators. With AUTOBATCH the gamma rays following the β- decay of 83As were studied to determine the ground state spin and parity of 83As to be 5/2-; the absolute intensity of the β- branch from 83As to 83Se/sup m/ to be 0.3%; the absolute intensity of the ground state β- branch from 83Se/sup m/ to 83Br to be 39%; the halflife of the 5/21+ level to be 3.2 ns; and the structure of 83Se49. Results are used to show that the intruder structure which had been previously observed in the odd mass 49In isotopes could be observed in the N = 49 isotones. The observed structure is discussed in terms of the unified model calculations of Heyde which has been used to describe the intruder structure in the indium nuclei. The intruder structure is most strongly developed, not at core mid-shell, 89Zr49, but rather at core mid-sub-shell 83Se. This difference is qualitatively understood to be due to the blocking of collectivity by the Z = 40 subshell closure which prevents the intruder structure from occurring in 87Sr49 and 89Zr49

  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 ...

  19. Preparation of biomorphic porous calcium titanate and its application for preconcentration of nickel in water and food samples

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Dong, E-mail: sylgdxdong@sina.com; Wang, Min; Ren, Guang-jun; Song, En-jun

    2013-12-01

    Biomorphic porous nanocrystalline-calcium titanate (SPCTO) was successfully prepared using the sol–gel method and with sorghum straw as the template. Characterization was conducted through XRD, SEM and FTIR. The ability of SPCTO to adsorb nickel ion in water was assessed. Elution and regeneration conditions, as well as the thermodynamics and kinetics of nickel adsorption, were also investigated. The result showed that the sorbent by the sol–gel template method was porous and has a perovskite structure with an average particle diameter of 26 nm. The nickel ion could be quantitatively retained at a pH value range of 4–8, but the adsorbed nickel ion could be completely eluted using 2 mol L{sup −1} HNO{sub 3}. The adsorption capacity of SPCTO for nickel was found to be 51.814 mg g{sup −1} and the adsorption behavior followed a Langmuir adsorption isotherm and a pseudo-second-order kinetic model. The enthalpy change (ΔH) of the adsorption process was 33.520 kJ mol{sup −1}. At various temperatures, Gibbs free energy changes (ΔG) were negative, and entropy changes (ΔS) were positive. The activation energy (E{sub a}) was 25.291 kJ mol{sup −1} for the adsorption. These results demonstrate that the adsorption was an endothermic and spontaneous physical process. This same method has been successfully applied in the preconcentration and determination of nickel in water and food samples with good results. - Highlights: • The biomorphic porous calcium titanate was prepared by sol–gel template method. • The porous calcium titanate was applied in adsorption of nickel. • The method has been applied in the determination of nickel in water and food.

  20. Fluoride and chloride determination in fossil fuels after sample preparation by pyrohydrolysis; Preparo de amostras de combustiveis fosseis por piroidrolise para a determinacao de fluor e cloro

    Energy Technology Data Exchange (ETDEWEB)

    Antes, Fabiane G.; Duarte, Fabio A.; Flores, Eder L. M.; Paniz, Jose Neri G.; Flores, Erico M. M.; Dressler, Valderi L., E-mail: valdres@quimica.ufsm.b [Universidade Federal de Santa Maria (DQ/UFSM), RS (Brazil). Dept. de Quimica

    2010-07-01

    Pyrohydrolysis is proposed for fossil fuels sample preparation for further fluorine and chlorine determination. Samples were heated during 10 min at temperatures up to 1000 deg C. Water vapor was passed through the reactor and the volatile products were condensed and collected in NH{sub 4}OH solution. Fluoride was determined by potentiometry using an ion selective electrode (ISE) and Cl by ICP OES and DRC-ICP-MS. The results are in good agreement with certified values and the precision is better than 10% (n = 4). Sample preparation by means of pyrohydrolysis is relatively simple, whereas chlorine and fluorine can be determined at low concentrations (author)

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

    Science.gov (United States)

    Straubinger, Rainer; Beyer, Andreas; Volz, Kerstin

    2016-06-01

    A reproducible way to transfer a single crystalline sample into a gas environmental cell holder for in situ transmission electron microscopic (TEM) analysis is shown in this study. As in situ holders have only single-tilt capability, it is necessary to prepare the sample precisely along a specific zone axis. This can be achieved by a very accurate focused ion beam lift-out preparation. We show a step-by-step procedure to prepare the sample and transfer it into the gas environmental cell. The sample material is a GaP/Ga(NAsP)/GaP multi-quantum well structure on Si. Scanning TEM observations prove that it is possible to achieve atomic resolution at very high temperatures in a nitrogen environment of 100,000 Pa. PMID:27026281

  2. The first 110 years of laboratory automation: technologies, applications, and the creative scientist.

    Science.gov (United States)

    Olsen, Kevin

    2012-12-01

    Prior to the widespread availability of electronic components after the Second World War, laboratory automation was constructed by end users and designed for specific tasks, mostly filtration, percolation, and washing operations. The earliest mention of automation in the chemical literature of the United States was in 1875, announcing a device to wash filtrates unattended. In the years that followed, a small number of commercial automated devices were sold, including large grinders for the preparation of coal samples. Around 1900, power stations began adopting automated carbon dioxide analysis. The development of electrical equipment for conductivity measurements enabled the first commercial, automated gas detection instruments for laboratory and field use around the time of the First World War. The growth of industrial production in the 1920s led to a desire for automated testing equipment, and the growing rubber industry was among the more successful early adapters. Photoelectric cells were first used in the early 1930s to create automatic titrators, and by the 1950s, automatic titration encompassed coulometric, potentiometric, and photometric devices. Combinations of chart recorders, photocells, and timers created other types of automated equipment such as stills and fraction collectors. The first true stand-alone automation for the laboratory included clinical chemistry analyzers, introduced during the 1950s. PMID:22893633

  3. Sample-first preparation: a method for surface-assisted laser desorption/ionization time-of-flight mass spectrometry analysis of cyclic oligosaccharides.

    Science.gov (United States)

    Wu, Hsin-Pin; Su, Chih-Lin; Chang, Hui-Chiu; Tseng, Wei-Lung

    2007-08-15

    A new sample preparation method for the analysis of cyclic oligosaccharides in surface-assisted laser desorption/ionization mass spectrometry (SALDI-MS) is presented. We call this new technique "sample first method", in which a sample is deposited first and then bare gold nanoparticles (AuNPs), which serve as the SALDI matrixes, are added to the top of the sample layer. The use of the sample first method offers significant advantages for improving shot-to-shot reproducibility, enhancing the ionization efficiency of the analyte, and reducing sample preparation time as compared to the dried-droplet method, wherein samples and bare AuNPs are mixed and dried together. The relative standard deviation (RSD) values of the signal intensity as calculated from 65 sample spots was 25% when the sample first methods were applied to the analysis of beta-cyclodextrin. The results were more homogeneous as compared to the outcome using dried-droplet preparation of AuNPs (RSD=66%) and 2,5-dihydroxybenzoic acid (RSD=209%). We also found out that the optimal concentration of AuNP for ionization efficiency is 7.4 nM (4.52x10(12) particles/mL) while the lowest detectable concentration of cyclic oligosaccharides through this approach is 0.25 microM. Except for the cyclic oligosaccharide, the proposed method was also applied to the analyses of other biological samples, including neutral carbohydrate and steroid, aminothiols, and peptides as well as proteins.

  4. Avaliação de procedimentos de preparo de amostra de amendoim in natura para análise de aflatoxinas Evaluation of sample preparation procedures for aflatoxin analysis in raw peanut

    Directory of Open Access Journals (Sweden)

    Maria Antonia Calori-Domingues

    2010-01-01

    Full Text Available The variability in aflatoxin B1 concentration among peanut subsamples of 4 sample preparation procedures was evaluated. For each procedure, 18 samples were prepared involving dry comminuting/homogenization or dry roughly comminuting followed by the preparation of a aqueous slurry. Ten analytical samples were withdrawn from each sample/procedure and analyzed by thin layer chromatography. The coefficient of variation (CV% among each set of 10 analytical samples was assumed to be associated with the sample preparation procedure. The procedure that made use of a subsample mill and preparation of a subsample slurry, showed lower variability (CV% among the analytical subsamples.

  5. Improved method for the preparation of TiN-coated WC-Co-based samples for cross-sectional AEM investigation.

    Science.gov (United States)

    Hefter, J; Ostreicher, K; Sung, C

    1992-11-01

    An improved method for the preparation of cross-sectional thin foils of coated WC-Co samples for studies by analytical electron microscopy is described. A braze alloy is used to join the sections of the sample together and the resulting sample is stable during subsequent grinding, dimpling, and milling operations. Cross-sectional micrographs provide examples of the efficacy of this method. No microstructural alteration associated with the brazing operation was observed. PMID:1472751

  6. [Preparation technique of S2OF10 gas standard sample and determination method of the trace S2OF10 in SF6].

    Science.gov (United States)

    Wang, L; Wang, J

    1999-09-01

    In this paper a series of methods and techniques for the S2OF10 standard sample preparation and quantitative determination are presented. They are, the preparation of S2OF10 by preparative chromatography with adsorption/thermal desorption, the standard sample of S2OF10 gas prepared by exponential dilution and the gas chromatography/flame photometric detector(GC/FPD) determination of trace S2OF10 from an SF6 sample with quantitative calibration factor. Especially, the S2OF10 gas from a used SF6 sample was directly separated and concentrated through a U-adsorbent-tube packed with 300 mg of Porasil A in a cold trap (-63 degrees C) with liquid-nitrogen and chloroform. Then it was purified by preparative-GC and to be injected into a preparative system of standard gas sample. In the meantime, the S2OF10 gas obtained was confirmed by the methods of GC/FPD, infrared spectrophotometer(IR) and gas chromatography/mass spectrometer(GC/MS) separately. The sub-ppm(by volume) level of the S2OF10 and SF6 mixture samples were prepared by use of the exponential dilution system. The GC/FPD experimental results showed that the detection linear range of S2OF10 gas concentration was 0.80 x 10(-6)-2.60 x 10(-4) (volume fraction) and the quantitative calibration factor of the S2OF10 was 0.197 based on SF6. The determination errors of quantitative calibration factor were 1.8%-20% and S2OF10 recovery of the adsorption/thermal desorption was 98.2% (n = 9) and its relative standard deviation was 6.2%. In addition, the results also showed that it is a simple and rapid method with good linearity and reproducibility. PMID:12552882

  7. Laboratory automation and LIMS in forensics

    DEFF Research Database (Denmark)

    Stangegaard, Michael; Hansen, Anders Johannes; Morling, Niels

    2013-01-01

    Implementation of laboratory automation and LIMS in a forensic laboratory enables the laboratory, to standardize sample processing. Automated liquid handlers can increase throughput and eliminate manual repetitive pipetting operations, known to result in occupational injuries to the technical staff....... Furthermore, implementation of automated liquid handlers reduces the risk of sample misplacement. A LIMS can efficiently control the sample flow through the laboratory and manage the results of the conducted tests for each sample. Integration of automated liquid handlers with a LIMS provides the laboratory...... with the tools required for setting up automated production lines of complex laboratory processes and monitoring the whole process and the results. Combined, this enables processing of a large number of samples. Selection of the best automated solution for an individual laboratory should be based on user...

  8. Preparation and characterization of superparamagnetic molecularly imprinted polymers for selective adsorption and separation of vanillin in food samples.

    Science.gov (United States)

    Ning, Fangjian; Peng, Hailong; Dong, Liling; Zhang, Zhong; Li, Jinhua; Chen, Lingxin; Xiong, Hua

    2014-11-19

    Novel water-compatible superparamagnetic molecularly imprinted polymers (M-MIPs) were prepared by coating superparamagnetic Fe3O4 nanoparticles with MIPs in a methanol-water reaction system. The M-MIPs were used for the selective adsorption and separation of vanillin from aqueous solution. The M-MIPs were characterized by X-ray powder diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, thermogravimetric analysis (TGA), vibrating sample magnetometry (VSM), and scanning electron microscopy (SEM). Results indicated that a core-shell structure of M-MIPs was obtained by coating a layer of silica and MIPs on the surface of the Fe3O4 nanoparticles. The obtained M-MIPs possess a loose and porous structure and can be rapidly separated from the solution using a magnet. The adsorption experiments showed that the binding capacity of the M-MIPs was significantly higher than that of the superparamagnetic non-molecularly imprinted polymers (M-NIPs). Meanwhile, the adsorption of M-MIPs reached equilibrium within 100 min, and the apparent maximum adsorption quantity (Qmax) and dissociation constant (Kd) were 64.12 μmol g(-1) and 58.82 μmol L(-1), respectively. The Scatchard analysis showed that homogeneous binding sites were formed on the M-MIP surface. The recoveries of 83.39-95.58% were achieved when M-MIPs were used for the pre-concentration and selective separation of vanillin in spiked food samples. These results provided the possibility for the separation and enrichment of vanillin from complicated food matrices by M-MIPs.

  9. Fabric phase sorptive extraction: An innovative sample preparation approach applied to the analysis of specific migration from food packaging.

    Science.gov (United States)

    Aznar, M; Alfaro, P; Nerin, C; Kabir, A; Furton, K G

    2016-09-14

    Additives added to food packaging materials can migrate to food in contact with them during storage and shelf life. A novel simple, fast and sensitive analyte extraction method based on fabric phase sorptive extraction (FPSE), followed by analysis using ultra-high performance liquid chromatography and mass spectrometry detection (UPLC-MS) was applied to the analysis of 18 common non-volatile plastic additives. Three FPSE media coated with different sol-gel sorbents characterized with different polarities including sol-gel poly(dimethylsiloxane), sol-gel poly(ethylene glycol) and sol-gel poly(tetrahydrofuran) were studied. All three FPSE media showed very satisfactory results. In general, compounds with low logP values seemed to have higher enrichment factors (EFs), especially with poly(tetrahydrofuran) and poly(ethylene glycol) media. For compounds with high logP values, the use of sol-gel poly(dimethylsiloxane) improved the enrichment capacity. Sample preparation time was optimized at 20 min for sample extraction and 10 min for solvent desorption. Acetonitrile was selected as desorption solvent since recoveries were over 70% for 13 out of 18 selected compounds in all FPSE media. The best extraction recovery values were obtained when compounds were dissolved in aqueous acetic acid solution (3%), where 17 out of 18 compounds showed improvement in their signal intensity after FPSE extraction and 10 obtained enrichment factors above 3 for all the tested FPSE media. When FPSE extracts were concentrated under nitrogen, 11 out of 18 compounds reached EFs values above 100. PMID:27566344

  10. An approach to optimize sample preparation for MALDI imaging MS of FFPE sections using fractional factorial design of experiments.

    Science.gov (United States)

    Oetjen, Janina; Lachmund, Delf; Palmer, Andrew; Alexandrov, Theodore; Becker, Michael; Boskamp, Tobias; Maass, Peter

    2016-09-01

    A standardized workflow for matrix-assisted laser desorption/ionization imaging mass spectrometry (MALDI imaging MS) is a prerequisite for the routine use of this promising technology in clinical applications. We present an approach to develop standard operating procedures for MALDI imaging MS sample preparation of formalin-fixed and paraffin-embedded (FFPE) tissue sections based on a novel quantitative measure of dataset quality. To cover many parts of the complex workflow and simultaneously test several parameters, experiments were planned according to a fractional factorial design of experiments (DoE). The effect of ten different experiment parameters was investigated in two distinct DoE sets, each consisting of eight experiments. FFPE rat brain sections were used as standard material because of low biological variance. The mean peak intensity and a recently proposed spatial complexity measure were calculated for a list of 26 predefined peptides obtained by in silico digestion of five different proteins and served as quality criteria. A five-way analysis of variance (ANOVA) was applied on the final scores to retrieve a ranking of experiment parameters with increasing impact on data variance. Graphical abstract MALDI imaging experiments were planned according to fractional factorial design of experiments for the parameters under study. Selected peptide images were evaluated by the chosen quality metric (structure and intensity for a given peak list), and the calculated values were used as an input for the ANOVA. The parameters with the highest impact on the quality were deduced and SOPs recommended. PMID:27485623

  11. Fractional Factorial Design of MALDI-TOF-MS Sample Preparations for the Optimized Detection of Phospholipids and Acylglycerols.

    Science.gov (United States)

    AlMasoud, Najla; Correa, Elon; Trivedi, Drupad K; Goodacre, Royston

    2016-06-21

    Matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS) has successfully been used for the analysis of high molecular weight compounds, such as proteins and nucleic acids. By contrast, analysis of low molecular weight compounds with this technique has been less successful due to interference from matrix peaks which have a similar mass to the target analyte(s). Recently, a variety of modified matrices and matrix additives have been used to overcome these limitations. An increased interest in lipid analysis arose from the feasibility of correlating these components with many diseases, e.g. atherosclerosis and metabolic dysfunctions. Lipids have a wide range of chemical properties making their analysis difficult with traditional methods. MALDI-TOF-MS shows excellent potential for sensitive and rapid analysis of lipids, and therefore this study focuses on computational-analytical optimization of the analysis of five lipids (4 phospholipids and 1 acylglycerol) in complex mixtures using MALDI-TOF-MS with fractional factorial design (FFD) and Pareto optimality. Five different experimental factors were investigated using FFD which reduced the number of experiments performed by identifying 720 key experiments from a total of 8064 possible analyses. Factors investigated included the following: matrices, matrix preparations, matrix additives, additive concentrations, and deposition methods. This led to a significant reduction in time and cost of sample analysis with near optimal conditions. We discovered that the key factors used to produce high quality spectra were the matrix and use of appropriate matrix additives. PMID:27228355

  12. Nanometer depth resolution in 3D topographic analysis of drug-loaded nanofibrous mats without sample preparation.

    Science.gov (United States)

    Paaver, Urve; Heinämäki, Jyrki; Kassamakov, Ivan; Hæggström, Edward; Ylitalo, Tuomo; Nolvi, Anton; Kozlova, Jekaterina; Laidmäe, Ivo; Kogermann, Karin; Veski, Peep

    2014-02-28

    We showed that scanning white light interferometry (SWLI) can provide nanometer depth resolution in 3D topographic analysis of electrospun drug-loaded nanofibrous mats without sample preparation. The method permits rapidly investigating geometric properties (e.g. fiber diameter, orientation and morphology) and surface topography of drug-loaded nanofibers and nanomats. Electrospun nanofibers of a model drug, piroxicam (PRX), and hydroxypropyl methylcellulose (HPMC) were imaged. Scanning electron microscopy (SEM) served as a reference method. SWLI 3D images featuring 29 nm by 29 nm active pixel size were obtained of a 55 μm × 40 μm area. The thickness of the drug-loaded non-woven nanomats was uniform, ranging from 2.0 μm to 3.0 μm (SWLI), and independent of the ratio between HPMC and PRX. The average diameters (n=100, SEM) for drug-loaded nanofibers were 387 ± 125 nm (HPMC and PRX 1:1), 407 ± 144 nm (HPMC and PRX 1:2), and 290 ± 100 nm (HPMC and PRX 1:4). We found advantages and limitations in both techniques. SWLI permits rapid non-contacting and non-destructive characterization of layer orientation, layer thickness, porosity, and surface morphology of electrospun drug-loaded nanofibers and nanomats. Such analysis is important because the surface topography affects the performance of nanomats in pharmaceutical and biomedical applications. PMID:24378328

  13. Optimization of Sample Preparation for the Identification and Quantification of Saxitoxin in Proficiency Test Mussel Sample using Liquid Chromatography-Tandem Mass Spectrometry

    OpenAIRE

    Kirsi Harju; Marja-Leena Rapinoja; Marc-André Avondet; Werner Arnold; Martin Schär; Stephen Burrell; Werner Luginbühl; Paula Vanninen

    2015-01-01

    Saxitoxin (STX) and some selected paralytic shellfish poisoning (PSP) analogues in mussel samples were identified and quantified with liquid chromatography-tandem mass spectrometry (LC-MS/MS). Sample extraction and purification methods of mussel sample were optimized for LC-MS/MS analysis. The developed method was applied to the analysis of the homogenized mussel samples in the proficiency test (PT) within the EQuATox project (Establishment of Quality Assurance for the Detection of Biological...

  14. Investigating how fundamental parameters of XRF sample preparation and analysis affect the observed elemental concentration: an experiment using fluvial sediment from Sabah, Borneo.

    Science.gov (United States)

    Higton, Sam; Walsh, Rory

    2015-04-01

    X-Ray Fluorescence (XRF) is an important technique for measuring the concentrations of geochemical elements and inorganic contaminants adsorbed to sediments as an input to sediment tracing methods used to evaluate sediment transport dynamics in river catchments. In addition to traditional laboratory-based XRF instruments, the advent of increasingly advanced portable handheld XRF devices now mean that samples of fluvial sediment can be analysed in the field or in the laboratory following appropriate sample preparation procedures. There are limitations and sources of error associated with XRF sample preparation and analysis, however. It is therefore important to understand how fundamental parameters involved in sample preparation and analysis, such as sample compression and measurement exposure duration, affect observed variability in measurement results. Such considerations become important if the resulting measurement variability is high relative to the natural variability in element concentrations at a sample site. This paper deployed a simple experimental design to assess the impacts of varying a number of sample preparation and XRF analysis parameters on recorded measurements of elemental concentrations of the fine fraction (XRF elemental analyser. Helium purging was used on both machines to enable measurement of lighter geochemical elements. Sediment sub-samples were taken from a larger homogenised sample from a sediment core taken from an in-channel lateral bench deposit of the Brantian river in Sabah, Borneo; the core site is being used for research into multi-proxy sediment fingerprinting as part of the Stability of Altered Forest Ecosystems (SAFE) project. Some fundamental sample preparation procedures consistent with US EPA Method 6200 were applied to all sediment samples in order to explore key variables of interest. All sediment samples were air-dried to constant weight and sample quantity was sufficient to satisfy the assumption of 'infinite thickness

  15. Automating Finance

    Science.gov (United States)

    Moore, John

    2007-01-01

    In past years, higher education's financial management side has been riddled with manual processes and aging mainframe applications. This article discusses schools which had taken advantage of an array of technologies that automate billing, payment processing, and refund processing in the case of overpayment. The investments are well worth it:…

  16. Evaluating focused ion beam and ultramicrotome sample preparation for analytical microscopies of the cathode layer of a polymer electrolyte membrane fuel cell

    Science.gov (United States)

    de A. Melo, Lis G.; Hitchcock, Adam P.; Berejnov, Viatcheslav; Susac, Darija; Stumper, Juergen; Botton, Gianluigi A.

    2016-04-01

    Optimizing the structure of the porous electrodes of polymer electrolyte membrane fuel cells (PEM-FC) can improve device power and durability. Analytical microscopy techniques are important tools for measuring the electrode structure, thereby providing guidance for structural optimization. Transmission Electron Microscopy (TEM), with either Energy Dispersive X-Ray (EDX) or Electron Energy Loss Spectroscopy (EELS) analysis, and Scanning Transmission X-Ray Microscopy (STXM) are complementary methods which, together, provide a powerful approach for PEM-FC electrode analysis. Both TEM and STXM require thin (50-200 nm) samples, which can be prepared either by Focused Ion Beam (FIB) milling or by embedding and ultramicrotomy. Here we compare TEM and STXM spectromicroscopy analysis of FIB and ultramicrotomy sample preparations of the same PEM-FC sample, with focus on how sample preparation affects the derived chemical composition and spatial distributions of carbon support and ionomer. The FIB lamella method, while avoiding pore-filling by embedding media, had significant problems. In particular, in the FIB sample the carbon support was extensively amorphized and the ionomer component suffered mass loss and structural damage. Although each sample preparation technique has a role to play in PEM-FC optimization studies, it is important to be aware of the limitations of each method.

  17. An overview of the contaminant analysis automation program

    International Nuclear Information System (INIS)

    The Department of Energy (DOE) has significant amounts of radioactive and hazardous wastes stored, buried, and still being generated at many sites within the United States. These wastes must be characterized to determine the elemental, isotopic, and compound content before remediation can begin. In this paper, the authors project that sampling requirements will necessitate generating more than 10 million samples by 1995, which will far exceed the capabilities of our current manual chemical analysis laboratories. The Contaminant Analysis Automation effort (CAA), with Los Alamos National Laboratory (LANL) as to the coordinating Laboratory, is designing and fabricating robotic systems that will standardize and automate both the hardware and the software of the most common environmental chemical methods. This will be accomplished by designing and producing several unique analysis systems called Standard Analysis Methods (SAM). Each SAM will automate a specific chemical method, including sample preparation, the analytical analysis, and the data interpretation, by using a building block known as the Standard Laboratory Module (SLM). This concept allows the chemist to assemble an automated environmental method using standardized SLMs easily and without the worry of hardware compatibility or the necessity of generating complicated control programs

  18. Comparison of the effects of sample preparation temperature, milling time, and carbon content on soft ferrite, hard ferrite, and Alnico magnet EM wave absorbers

    International Nuclear Information System (INIS)

    We compared the effects of sample preparation temperature, milling time, and carbon content on Mn-Zn ferrite (soft ferrite), Ba ferrite and Sr ferrite (hard ferrite), and Alnico magnet EM wave absorbers for preparing superior EM wave absorbers. The reflectivity of the EM wave absorbers depended on the particle size and the particle shape of ferrites. In the manufacturing process of the EM wave absorbers, the preparation temperature played a very important role in deciding the EM wave absorption properties. We confirmed that carbon strongly affects on the reflectivity of hard ferrite and Alnico magnet EM wave absorbers.

  19. 全自动定量浓缩-气相色谱法分析地表水中的有机氯农药%Determination of organochlorine Pesticides in Water Samples by Fully Automated Quantitative Concentrator-Gas Chromatography

    Institute of Scientific and Technical Information of China (English)

    曹旭静

    2016-01-01

    地表水中的有机氯农药用正己烷萃取后,用全自动定量蒸发浓缩仪在水浴温度35℃,真空度为300mbar时浓缩定容到1mL,一个样品只需要25min。用液液萃取-全自动定量浓缩仪-气相色谱法分析地表水水中的有机氯农药,该方法的检出限为为0.001~0.008μg/L,方法的平均回收率在78.6%~104%之间。该方法检出限低,精密度好,省时省力,自动化程度高,适合于大批量样品的监测。%Organochlorine pesticides in water were extracted by n-hexan,the extracted liquid was concentrated to 1mL with fully automated quantitative concentrator in the water bath temperature 35℃and the vacuum 300mbar.Which only need 25min. Organochlorine pesticides were determined by gas chromatograph after samples pre-treatment by liquid-liquid ex⁃traction with n-hexane and concentration with fully automated quantitative concentrator.The detection limits of method for organochlorine pesticides were in the range of 0.001~0.008μg/L.The average recoveries were 78.6%~104%. This method had advantages of good accuracy and precision,rapid,high degree of automation and was suitable for batch samples.

  20. Automation Security

    OpenAIRE

    Mirzoev, Dr. Timur

    2014-01-01

    Web-based Automated Process Control systems are a new type of applications that use the Internet to control industrial processes with the access to the real-time data. Supervisory control and data acquisition (SCADA) networks contain computers and applications that perform key functions in providing essential services and commodities (e.g., electricity, natural gas, gasoline, water, waste treatment, transportation) to all Americans. As such, they are part of the nation s critical infrastructu...

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

    OpenAIRE

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

    2015-01-01

    Laser microdissection followed by mass spectrometry has been successfully used for amyloid typing. However, sample contamination can interfere with proteomic analysis, and overnight digestion limits the analytical throughput. Moreover, current quantitative analysis methods are based on the spectrum count, which ignores differences in protein length and may lead to misdiagnoses. Here, we developed a microwave-assisted filter-aided sample preparation (maFASP) method that can efficiently remove ...

  2. Sample Preparation Problem Solving for Inductively Coupled Plasma-Mass Spectrometry with Liquid Introduction Systems I. Solubility, Chelation, and Memory Effects

    OpenAIRE

    Pappas, R. Steven

    2012-01-01

    This tutorial was adapted from the first half of a course presented at the 7th International Conference on Sector Field Inductively Coupled Plasma Mass Spectrometry in 2008 and the 2012 Winter Conference on Plasma Spectrochemistry on sample preparation for liquid introduction systems. Liquid introduction in general and flow injection specifically are the most widely used sample introduction methods for inductively coupled plasma-mass spectrometry. Nevertheless, problems persist in determinati...

  3. A lab-on-a-chip system with integrated sample preparation and loop-mediated isothermal amplification for rapid and quantitative detection of Salmonella spp. in food samples

    DEFF Research Database (Denmark)

    Sun, Yi; Than Linh, Quyen; Hung, Tran Quang;

    2015-01-01

    amplification (LAMP) for rapid and quantitative detection of Salmonella spp. in food samples. The whole diagnostic procedures including DNA isolation, isothermal amplification, and real-time detection were accomplished in a single chamber. Up to eight samples could be handled simultaneously and the system...... was capable to detect Salmonella at concentration of 50 cells per test within 40 min. The simple design, together with high level of integration, isothermal amplification, and quantitative analysis of multiple samples in short time will greatly enhance the practical applicability of the LOC system for rapid...

  4. Evaluation of automated analysis of 15N and total N in plant material and soil

    DEFF Research Database (Denmark)

    Jensen, E.S.

    1991-01-01

    was lower than 0.1%. The CV of repeated analyses of N-15-labelled plant material and soil samples varied between 0.3% and 1.1%. The reproducibility of repeated total N analyses using the automated method was comparable to results obtained with a semi-micro Kjeldahl procedure. However, the automated method...... gave results which were 3% to 5% higher than those obtained with the Kjeldahl procedure. Since only small samples can be analysed, careful sample homogenization and fine grinding are very important. Evaluation of a diffusion method for preparing nitrate and ammonium in solution for automated N-15......Simultaneous determination of N-15 and total N using an automated nitrogen analyser interfaced to a continuous-flow isotope ratio mass spectrometer (ANA-MS method) was evaluated. The coefficient of variation (CV) of repeated analyses of homogeneous standards and samples at natural abundance...

  5. A revolutionary graphitisation system: Fully automated, compact and simple

    Energy Technology Data Exchange (ETDEWEB)

    Wacker, L., E-mail: wacker@phys.ethz.c [Ion Beam Physics, Paul Scherrer Institute and ETH Zurich, 8093 Zurich (Switzerland); Nemec, M. [Department of Chemistry and Biochemistry, University of Bern, 3012 Bern (Switzerland); Bourquin, J. [Ion Beam Physics, Paul Scherrer Institute and ETH Zurich, 8093 Zurich (Switzerland)

    2010-04-15

    A new graphitisation system, directly coupled to an elemental analyser, has been developed for convenient, fast and efficient sample preparations for radiocarbon measurement by means of accelerator mass spectrometry. We demonstrate an alternative to the cryogenic transport of CO{sub 2} into the graphitisation reactors with liquid nitrogen, which is used by others. Instead, the CO{sub 2} coming from an EA is absorbed on a single column filled with zeolite. The CO{sub 2} can then be easily released by heating the zeolite trap and transferred to the reactor by gas expansion. The system is simple and fully automated for sample combustion and graphitisation.

  6. In situ liquid-liquid extraction as a sample preparation method for matrix-assisted laser desorption/ionization MS analysis of polypeptide mixtures

    DEFF Research Database (Denmark)

    Kjellström, Sven; Jensen, Ole Nørregaard

    2003-01-01

    A novel liquid-liquid extraction (LLE) procedure was investigated for preparation of peptide and protein samples for matrix-assisted laser desorption/ionization mass spectrometry (MALDI MS). LLE using ethyl acetate as the water-immiscible organic solvent enabled segregation of hydrophobic...

  7. 14C measurement: effect of variations in sample preparation and storage on the counting efficiency for 14C using a carbo-sorb/permafluor E+ liquid scintillation cocktail

    International Nuclear Information System (INIS)

    The effect of variations in sample preparation and storage on the counting efficiency for 14C using a Carbo-Sorb/PermafluorE+ liquid scintillation cocktail has been studied, and optimum conditions are recommended. (author). 2 refs., 2 tabs., 4 figs

  8. Extensible automated dispersive liquid–liquid microextraction

    Energy Technology Data Exchange (ETDEWEB)

    Li, Songqing; Hu, Lu; Chen, Ketao; Gao, Haixiang, E-mail: hxgao@cau.edu.cn

    2015-05-04

    method opens a new avenue for automated DLLME that not only greatly expands the range of viable extractants, especially functional ILs but also enhances its application for various detection methods. Furthermore, multiple samples can be processed simultaneously, which accelerates the sample preparation and allows the examination of a large number of samples.

  9. Sample Handling and Processing on Mars for Future Astrobiology Missions

    Science.gov (United States)

    Beegle, Luther; Kirby, James P.; Fisher, Anita; Hodyss, Robert; Saltzman, Alison; Soto, Juancarlos; Lasnik, James; Roark, Shane

    2011-01-01

    In most analytical investigations, there is a need to process complex field samples for the unique detection of analytes especially when detecting low concentration organic molecules that may identify extraterrestrial life. Sample processing for analytical instruments is time, resource and manpower consuming in terrestrial laboratories. Every step in this laborious process will have to be automated for in situ life detection. We have developed, and are currently demonstrating, an automated wet chemistry preparation system that can operate autonomously on Earth and is designed to operate under Martian ambient conditions. This will enable a complete wet chemistry laboratory as part of future missions. Our system, namely the Automated Sample Processing System (ASPS) receives fines, extracts organics through solvent extraction, processes the extract by removing non-organic soluble species and delivers sample to multiple instruments for analysis (including for non-organic soluble species).

  10. Colonization of Potato Rhizosphere by GFP-Tagged Bacillus subtilis MB73/2, Pseudomonas sp. P482 and Ochrobactrum sp. A44 Shown on Large Sections of Roots Using Enrichment Sample Preparation and Confocal Laser Scanning Microscopy

    Directory of Open Access Journals (Sweden)

    Sylwia Jafra

    2012-12-01

    Full Text Available The ability to colonize the host plants’ rhizospheres is a crucial feature to study in the case of Plant Growth Promoting Rhizobacteria (PGPRs with potential agricultural applications. In this work, we have created GFP-tagged derivatives of three candidate PGPRs: Bacillus subtilis MB73/2, Pseudomonas sp. P482 and Ochrobactrum sp. A44. The presence of these strains in the rhizosphere of soil-grown potato (Solanum tuberosum L. was detected with a classical fluorescence microscope and a confocal laser scanning microscope (CLSM. In this work, we have used a broad-field-of-view CLMS device, dedicated to in vivo analysis of macroscopic objects, equipped with an automated optical zoom system and tunable excitation and detection spectra. We show that features of this type of CLSM microscopes make them particularly well suited to study root colonization by microorganisms. To facilitate the detection of small and scattered bacterial populations, we have developed a fast and user-friendly enrichment method for root sample preparation. The described method, thanks to the in situ formation of mini-colonies, enables visualization of bacterial colonization sites on large root fragments. This approach can be easily modified to study colonization patterns of other fluorescently tagged strains. Additionally, dilution plating of the root extracts was performed to estimate the cell number of MB73/2, P482 and A44 in the rhizosphere of the inoculated plants.

  11. Automated preparation of the dopamine D{sub 2/3} receptor agonist ligand [{sup 11}C]-(+)-PHNO for human PET imaging studies

    Energy Technology Data Exchange (ETDEWEB)

    Plisson, Christophe, E-mail: Christophe.2.plisson@gsk.com [GlaxoSmithKline, Clinical Imaging Centre, Hammersmith Hospital, London W12 0NN (United Kingdom); Huiban, Mickael; Pampols-Maso, Sabina; Singleton, Goerkem; Hill, Samuel P.; Passchier, Jan [GlaxoSmithKline, Clinical Imaging Centre, Hammersmith Hospital, London W12 0NN (United Kingdom)

    2012-02-15

    Carbon-11 labelled (+)-4-Propyl-3,4,4a,5,6,10b-hexahydro-2H-naphtho[1,2-b][1,4]oxazin-9-ol ([{sup 11}C]-(+)-PHNO) is used as a high-affinity state, dopamine D{sub 2/3} receptor ligand in clinical PET studies. To facilitate its use, robust, rapid, efficient and GMP compliant methods are required for the manufacturing and QC testing processes. Additionally, to allow for full quantification of the resulting signal in the CNS, a reliable method is required to establish the parent plasma concentration over the course of the scan. This paper provides high-quality methods to support clinical application of [{sup 11}C]-(+)-PHNO. - Highlights: Black-Right-Pointing-Pointer Fully automated synthesis of [{sup 11}C]-(+)-PHNO. Black-Right-Pointing-Pointer Rapid multi-step synthesis and QC analysis. Black-Right-Pointing-Pointer Reproducible synthesis process typically yielding more than 3 GBq of [{sup 11}C]-(+)-PHNO. Black-Right-Pointing-Pointer Very low failure rate.

  12. Effect of Testing Conditions on Fibre-Bundle Tensile Properties Part Ⅰ: Sample Preparation, Bundle Mass and Fibre Alignment of Wool Bundles

    Institute of Scientific and Technical Information of China (English)

    YU Wei-dong; YAN Hao-jing; Ron Postle; Yang Shouren

    2002-01-01

    Due to the effects of samples and testing conditions on fibre-bundle tensile behaviour, it is necessary to investigate the relationships between experimental factors and tensile properties for the fibre-bumdle tensile tester (TENSOR). The effects of bundle sample preparation, fibre bundle mass and fibre alignment have been tested. The experimental results indicated that (1) the low damage in combing and no free-end fibres in the cut bundle are most important for the sample preparation; (2) the reasonable bundle mass is 400- 700tex, but the tensile properties measured should bemodified with the bundle mass because a small amount of bundle mass causes the scatter results, while the larger is the bundle mass, the more difficult to comb fibres parallel and to clamp fibre evenly; and (3) the fibre irregular arrangement forms a slack bundle resulting in interaction between fibres, which will affect the reproducibility and accuracy of the tensile testing.

  13. Optimization of chemical analysis methods for coal and fly ash. 1. Sampling, sample preparation and 'proximate' analysis. Optimalisatie analysemethoden voor steenkool en vliegas. 1. Monstername, monsterverwerking en 'proximate' analyse

    Energy Technology Data Exchange (ETDEWEB)

    Hissink, M.

    1983-01-01

    To support the experiments in the atmospheric fluid bed boiler (AFBB) many analyses of samples of fuel, additions and waste are needed. Therefore it was necessary to obtain experience with regard to sampling, sample preparation and analysis of these materials. For a correct interpretation of the experiments in the AFBB a knowledge of the accuracy of the results of these analyses is essential. This accuracy depends largely on the sampling method. As a guide for the methods to be used the instructions in the relevant ISO Standards have been followed usually. A description is given of the procedures for sampling and analysis as well as of the equipment used. The accuracy that can be expected for the various results of analysis has been established experimentally. It was found in general that the requirements were met.

  14. Optimization of chemical analysis methods for coal and fly ash. 1. Sampling, sample preparation and proximate analysis. Optimalisatie analysemethoden voor steenkool en vliegas. 1. Monstername monsterverwerking en 'proximate' analyse

    Energy Technology Data Exchange (ETDEWEB)

    Hissink, M.

    1983-01-01

    To support the experiments in the atmospheric fluid bed boiler (AFBB), many analyses of samples of fuel, additives and waste are needed. Therefore it was necessary to obtain experience with regard to sampling, sample preparation and analysis of these materials. For a correct interpretation of the experiments in the AFBB, a knowledge of accuracy of the results of these analyses is essential. This accuracy depends largely on the sampling method. As a guide for the methods to be used, the instructions in the relevant ISO Standards have been followed usually. A description is given of the procedures for sampling and analysis as well as of the equipment used. The accuracy that can be expected for the various results of analysis has been established experimentally. It was found in general that the requirements were met. (In Dutch)

  15. Automated activation-analysis system

    International Nuclear Information System (INIS)

    An automated delayed neutron counting and instrumental neutron activation analysis system has been developed at Los Alamos National Laboratory's Omega West Reactor (OWR) to analyze samples for uranium and 31 additional elements with a maximum throughput of 400 samples per day. The system and its mode of operation for a large reconnaissance survey are described

  16. Data on step-by-step atomic force microscopy monitoring of changes occurring in single melanoma cells undergoing ToF SIMS specialized sample preparation protocol.

    Science.gov (United States)

    Bobrowska, J; Pabijan, J; Wiltowska-Zuber, J; Jany, B R; Krok, F; Awsiuk, K; Rysz, J; Budkowski, A; Lekka, M

    2016-09-01

    Data included in this article are associated with the research article entitled 'Protocol of single cells preparation for time-of-flight secondary ion mass spectrometry' (Bobrowska et al., 2016 in press) [1]. This data file contains topography images of single melanoma cells recorded using atomic force microscopy (AFM). Single cells cultured on glass surface were subjected to the proposed sample preparation protocol applied to prepare biological samples for time-of-flight secondary ion mass spectrometry (ToF SIMS) measurements. AFM images were collected step-by-step for the single cell, after each step of the proposed preparation protocol. It consists of four main parts: (i) paraformaldehyde fixation, (ii) salt removal, (iii) dehydrating, and (iv) sample drying. In total 13 steps are required, starting from imaging of a living cell in a culture medium and ending up at images of a dried cell in the air. The protocol was applied to melanoma cells from two cell lines, namely, WM115 melanoma cells originated from primary melanoma site and WM266-4 ones being the metastasis of WM115 cells to skin. PMID:27570811

  17. 21 CFR 864.5680 - Automated heparin analyzer.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Automated heparin analyzer. 864.5680 Section 864....5680 Automated heparin analyzer. (a) Identification. An automated heparin analyzer is a device used to determine the heparin level in a blood sample by mixing the sample with protamine (a...

  18. Technology modernization assessment flexible automation

    Energy Technology Data Exchange (ETDEWEB)

    Bennett, D.W.; Boyd, D.R.; Hansen, N.H.; Hansen, M.A.; Yount, J.A.

    1990-12-01

    The objectives of this report are: to present technology assessment guidelines to be considered in conjunction with defense regulations before an automation project is developed to give examples showing how assessment guidelines may be applied to a current project to present several potential areas where automation might be applied successfully in the depot system. Depots perform primarily repair and remanufacturing operations, with limited small batch manufacturing runs. While certain activities (such as Management Information Systems and warehousing) are directly applicable to either environment, the majority of applications will require combining existing and emerging technologies in different ways, with the special needs of depot remanufacturing environment. Industry generally enjoys the ability to make revisions to its product lines seasonally, followed by batch runs of thousands or more. Depot batch runs are in the tens, at best the hundreds, of parts with a potential for large variation in product mix; reconfiguration may be required on a week-to-week basis. This need for a higher degree of flexibility suggests a higher level of operator interaction, and, in turn, control systems that go beyond the state of the art for less flexible automation and industry in general. This report investigates the benefits and barriers to automation and concludes that, while significant benefits do exist for automation, depots must be prepared to carefully investigate the technical feasibility of each opportunity and the life-cycle costs associated with implementation. Implementation is suggested in two ways: (1) develop an implementation plan for automation technologies based on results of small demonstration automation projects; (2) use phased implementation for both these and later stage automation projects to allow major technical and administrative risk issues to be addressed. 10 refs., 2 figs., 2 tabs. (JF)

  19. Sample preparation for semivolatile organics analysis of Hanford single-shell tank waste with high nitrate/nitrite and water content

    Energy Technology Data Exchange (ETDEWEB)

    Stromatt, R.W.; Hoppe, E.W.; Steele, M.J.

    1993-11-01

    This report describes research work carried out to solve sample preparation problems associated with applying gas chromatography with mass spectrometric detection (GC/MS) to the analysis of single shell tank (SST) samples from Hanford for semivolatile organic compounds. Poor performance was found when applying the procedures based on the U.S. Environmental Protection Agency (EPA), Contract Laboratory Program, Statement of Work (CLP SOW). Analysis work was carried out on simulated drainable liquid modeled after the SST core samples which had evidenced analysis problems. Some work was also conducted on true SST samples. It was found that the pH range was too broad in the original procedure. It was also found that by decreasing the amount of methanol used in the extraction process, problems associated with the formation of an azeotrope phase could be avoided. The authors suggest a new procedure, whose eventual application to a wide array of SST samples will lend itself to better quality control limits.

  20. Automated synthesis of sialylated oligosaccharides

    Directory of Open Access Journals (Sweden)

    Davide Esposito

    2012-09-01

    Full Text Available Sialic acid-containing glycans play a major role in cell-surface interactions with external partners such as cells and viruses. Straightforward access to sialosides is required in order to study their biological functions on a molecular level. Here, automated oligosaccharide synthesis was used to facilitate the preparation of this class of biomolecules. Our strategy relies on novel sialyl α-(2→3 and α-(2→6 galactosyl imidates, which, used in combination with the automated platform, provided rapid access to a small library of conjugation-ready sialosides of biological relevance.

  1. Comparison of sample preparation methods combined with gas chromatography with electron-capture detection for the analysis of multipesticide residues in lotus seeds.

    Science.gov (United States)

    Miao, Qing; Kong, Weijun; Yang, Shihai; Yang, Meihua

    2013-06-01

    Sample preparation is always the major bottleneck in analytical chemistry for the determination of pesticide residues. Different sample preparation methods have been proposed due to the wide variety of pesticides used and the inherent complexity of the matrices. In this study, different sample preparation methods including SPE, matrix solid-phase dispersion, the quick, easy, cheap, efficient, rugged, and safe method, and a one-step completion method were compared and evaluated for extracting pesticides from lotus seeds. Analysis was carried out using GC with electron-capture detection. The results showed that good recoveries for tested pesticides were obtained by using Florisil in the four methods, and the extraction efficiency of the one-step completion method was superior to the other three methods. The one-step completion method was confirmed to have good linearity, reproducibility, stability, and recovery for the detection of 36 pesticides in lotus seed samples. The data collected from this study are expected to prove useful in regulating the concentration of the residues in lotus seeds, as well as in protecting human health from the hazards posed by these residues.

  2. Determination of propoxur in environmental samples by automated solid-phase extraction followed by flow-injection analysis with tris(2,2'-bipyridyl)ruthenium(II) chemiluminescence detection

    Energy Technology Data Exchange (ETDEWEB)

    Perez-Ruiz, Tomas [Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, 30071 Murcia (Spain)]. E-mail: tpr@um.es; Martinez-Lozano, Carmen [Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, 30071 Murcia (Spain); Garcia, Maria Dolores [Department of Analytical Chemistry, Faculty of Chemistry, University of Murcia, 30071 Murcia (Spain)

    2007-02-19

    A sensitive method for the analysis of propoxur in environmental samples has been developed. It involves an automated solid-phase extraction (SPE) procedure using a Gilson Aspec XLi and flow-injection analysis (FI) with chemiluminescence (CL) detection. The FI-CL system relies on the photolysis of propoxur by irradiation using a low-pressure mercury lamp (main spectral line 254 nm). The resultant methylamine is subsequently detected by CL using tris(2,2'-bipyridyl)ruthenium(III), which is on-line generated by photo-oxidation of the ruthenium(II) complex in the presence of peroxydisulfate. The linear concentration range of application was 0.05-5 {mu}g mL{sup -1} of propoxur, with a detection limit of 5 ng mL{sup -1}. The repeatability was 0.82% expressed as relative standard deviation (n = 10) and the reproducibility, studied on 5 consecutive days, was 2.1%. The sample throughput was 160 injection per hour. Propoxur residues below ng mL{sup -1} levels could be determined in environmental water samples when an SPE preconcentration device was coupled on-line with the FI system. This SPE-FI-CL arrangement provides a detection limit as low as 5 ng L{sup -1} using only 500 mL of sample. In the analysis of fruits and vegetables, the detection limit was about 10 {mu}g kg{sup -1}.

  3. Determination of propoxur in environmental samples by automated solid-phase extraction followed by flow-injection analysis with tris(2,2'-bipyridyl)ruthenium(II) chemiluminescence detection.

    Science.gov (United States)

    Pérez-Ruiz, Tomás; Martínez-Lozano, Carmen; García, María Dolores

    2007-02-19

    A sensitive method for the analysis of propoxur in environmental samples has been developed. It involves an automated solid-phase extraction (SPE) procedure using a Gilson Aspec XLi and flow-injection analysis (FI) with chemiluminescence (CL) detection. The FI-CL system relies on the photolysis of propoxur by irradiation using a low-pressure mercury lamp (main spectral line 254 nm). The resultant methylamine is subsequently detected by CL using tris(2,2'-bipyridyl)ruthenium(III), which is on-line generated by photo-oxidation of the ruthenium(II) complex in the presence of peroxydisulfate. The linear concentration range of application was 0.05-5 microg mL(-1) of propoxur, with a detection limit of 5 ng mL(-1). The repeatability was 0.82% expressed as relative standard deviation (n=10) and the reproducibility, studied on 5 consecutive days, was 2.1%. The sample throughput was 160 injection per hour. Propoxur residues below ng mL(-1) levels could be determined in environmental water samples when an SPE preconcentration device was coupled on-line with the FI system. This SPE-FI-CL arrangement provides a detection limit as low as 5 ng L(-1) using only 500 mL of sample. In the analysis of fruits and vegetables, the detection limit was about 10 microg kg(-1).

  4. An automated image analysis framework for segmentation and division plane detection of single live Staphylococcus aureus cells which can operate at millisecond sampling time scales using bespoke Slimfield microscopy

    CERN Document Server

    Wollman, Adam J M; Foster, Simon; Leake, Mark C

    2016-01-01

    Staphylococcus aureus is an important pathogen, giving rise to antimicrobial resistance in cell strains such as Methicillin Resistant S. aureus (MRSA). Here we report an image analysis framework for automated detection and image segmentation of cells in S. aureus cell clusters, and explicit identification of their cell division planes. We use a new combination of several existing analytical tools of image analysis to detect cellular and subcellular morphological features relevant to cell division from millisecond time scale sampled images of live pathogens at a detection precision of single molecules. We demonstrate this approach using a fluorescent reporter GFP fused to the protein EzrA that localises to a mid-cell plane during division and is involved in regulation of cell size and division. This image analysis framework presents a valuable platform from which to study candidate new antimicrobials which target the cell division machinery, but may also have more general application in detecting morphological...

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

    Science.gov (United States)

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

    2015-07-01

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

  6. Automated Budget System

    Data.gov (United States)

    Department of Transportation — The Automated Budget System (ABS) automates management and planning of the Mike Monroney Aeronautical Center (MMAC) budget by providing enhanced capability to plan,...

  7. Detection of Giardia lamblia, Cryptosporidium spp. and Entamoeba histolytica in clinical stool samples by using multiplex real-time PCR after automated DNA isolation

    NARCIS (Netherlands)

    Van Lint, P; Rossen, J W; Vermeiren, S; Ver Elst, K; Weekx, S; Van Schaeren, J; Jeurissen, A

    2013-01-01

    Diagnosis of intestinal parasites in stool samples is generally still carried out by microscopy; however, this technique is known to suffer from a low sensitivity and is unable to discriminate between certain protozoa. In order to overcome these limitations, a real-time multiplex PCR was evaluated a

  8. Use of pooled urine samples and automated DNA isolation to achieve improved sensitivity and cost-effectiveness of large-scale testing for Chlamydia trachomatis in pregnant women.

    NARCIS (Netherlands)

    Rours, G.I.J.G.; Verkooyen, R.P.; Willemse, H.F.M.; Zwaan, E.A. van der; Belkum, A. van; Groot, R. de; Verbrugh, H.A.; Ossewaarde, J.M.

    2005-01-01

    The success of large-scale screening for Chlamydia trachomatis depends on the availability of noninvasive samples, low costs, and high-quality testing. To evaluate C. trachomatis testing with pregnant women, first-void urine specimens from 750 consecutive asymptomatic pregnant women from the Rotterd

  9. Use of pooled urine samples and automated DNA isolation to achieve improved sensitivity and cost-effectiveness of large-scale testing for Chlamydia trachomatis in pregnant women.

    NARCIS (Netherlands)

    G.I.J.G. Rours (Ingrid); R.P.A.J. Verkooyen (Roel); H.F. Willemse; E.A.E. van der Zwaan (Elizabeth); A.F. van Belkum (Alex); R. de Groot (Ronald); H.A. Verbrugh (Henri); J.M. Ossewaarde (Jacobus)

    2005-01-01

    textabstractThe success of large-scale screening for Chlamydia trachomatis depends on the availability of noninvasive samples, low costs, and high-quality testing. To evaluate C. trachomatis testing with pregnant women, first-void urine specimens from 750 consecutive asymptomatic pregnant women from

  10. Determination of benzoylureas in ground water samples by fully automated on-line pre-concentration and liquid chromatography-fluorescence detection.

    Science.gov (United States)

    Gil García, M D; Martínez Galera, M; Barranco Martínez, D; Gisbert Gallego, J

    2006-01-27

    An on-line pre-concentration method for the analysis of five benzoylureas (diflubenzuron, triflumuron, hexaflumuron, lufenuron and flufenoxuron) in ground water samples was evaluated using two C(18) columns, and fluorescence detection after photochemical induced fluorescence (PIF) post-column derivatization. The trace enrichment was carried out with 35 mL of ground water modified with 15 mL of MeOH on a 50 mm x 4.6 mm I.D. first enrichment column (C-1) packed with 5 microm Hypersil Elite C(18). Retention properties of pesticides and humic acids usually contained in ground water were studied on C-1 at concentration levels ranging between 0.04 and 14.00 microg/L in water samples. The results obtained in this study show that the pesticides are pre-concentrated in the first short column while the humic acids contained in the ground water samples are eluted to waste. Pesticides recoveries ranged between 92.3 and 109.5%. The methodology proposed was used to determine benzoylureas in ground water samples at levels lower than 0.1 microg/L (maximum levels established by the European Union). PMID:16337641

  11. The Effect of Sample Preparation on Yield and Composition of Certified Organic Ethanolic Extracts Produced from Icelandic Marine Algae Species

    OpenAIRE

    Coaten, Daniel James, 1976-

    2014-01-01

    During recent years, the natural product chemistry of marine organisms has received much attention as a promising new field of study. In particular, marine algae have proven to be a rich source of structurally diverse bioactive compounds with a high potential value to food, cosmetic, and pharmaceutical industries. Therefore, the main focus of this study was to investigate how preparation and extraction methods effect the yield and chemical composition of the crude extracts obtained from I...

  12. Analysis of sample preparation procedures for enumerating fecal coliforms in coarse southwestern U.S. bottom sediments by the most-probable-number method.

    OpenAIRE

    Doyle, J D; Tunnicliff, B; Kramer, R E; Brickler, S K

    1984-01-01

    The determination of bacterial densities in aquatic sediments generally requires that a dilution-mixing treatment be used before enumeration of organisms by the most-probable-number fermentation tube method can be done. Differential sediment and organism settling rates may, however, influence the distribution of the microbial population after the dilution-mixing process, resulting in biased bacterial density estimates. For standardization of sample preparation procedures, the influence of set...

  13. Preparation and Characterization of Mg1-xB2 Bulk Samples and Cu/Nb Sheathed Wires with Low Grade Amorphous Boron Powder

    DEFF Research Database (Denmark)

    Grivel, Jean-Claude; Alexiou, Aikaterini; Rubesova, Katerina;

    2014-01-01

    MgB2 bulk and wire samples were prepared using cheap, low grade amorphous boron powders. Based on chemical analysis performed on the starting reagents, three nominal stoichiometries were studied. It was found that the structural and superconducting properties of the bulk samples were not affected...... by the composition, but that residual Mg was left in the wires for the nominal MgB2 composition. In contrast, slightly Mg-deficient compositions were free from residual Mg and exhibited higher critical current densities. The MgB2 phase formation kinetics was not influenced by the variations in the nominal powder...

  14. Comparison of sample preparation methods for the quantitative analysis of eicosanoids and other oxylipins in plasma by means of LC-MS/MS.

    Science.gov (United States)

    Ostermann, Annika I; Willenberg, Ina; Schebb, Nils Helge

    2015-02-01

    Oxylipins are potent lipid mediators. For the evaluation of their biological roles, several LC-MS based methods have been developed. While these methods are similar, the described sample preparation procedures for the extraction of oxylipins differ considerably. In order to deduce the most appropriate method for the analysis of non-esterified oxylipins in human plasma, we evaluated the performance of seven established sample preparation procedures. Six commonly used solid phase extraction (SPE) and one liquid-liquid extraction (LLE) protocol were compared based on the recovery of 13 added internal standards, extraction efficacy of oxylipins from plasma and reduction of ion-suppressing matrix. Dramatic differences in the performance in all three parameters were found. LLE with ethyl acetate was overall not a sufficient sample preparation strategy. The protocols using Oasis- and StrataX-material insufficiently removed interfering matrix compounds. Extraction efficacy of oxylipins on anion-exchanging BondElut cartridges was low, while removal of matrix was nearly perfect. None of the protocols led to a high extraction efficacy of analytes while removing all interfering matrix components. However, SPE on a C18-material with removal of matrix by water and n-hexane prior elution with methyl formate showed the best performance for the analysis of a broad spectrum of oxylipins in plasma.

  15. Preparation, Microhardness Characterization on Untreated And Treated With Electric Stressed Samples on The Inorganic Tunable Laser Dye Rhodamine Doped PMMA

    Directory of Open Access Journals (Sweden)

    Pradeep Kumar Dubey, R. Bajpai , J. M. Keller

    2013-04-01

    Full Text Available Effect of Load, Load dependent nature of Microhardness measurement and Doping Effect on untreated samples and Microhardness studies on the effect of charge due to electrical stress on the samples of pure and Rhodamine doped PMMA with different weights proportions have been carried out using Vicker’s microhardness testing for hardened networks plasticization and crystallization. Some selected samples are used to study the electrical stress, with the help of thermostat controller at different polarizing temperatures and fields in thermally stimulated depolarization current due to dipole orientation or trapping of space charges, which gives the information about uniform polarization.

  16. US Environmental Protection Agency Method 314.1, an automated sample preconcentration/matrix elimination suppressed conductivity method for the analysis of trace levels (0.50 microg/L) of perchlorate in drinking water.

    Science.gov (United States)

    Wagner, Herbert P; Pepich, B V; Pohl, C; Later, D; Joyce, R; Srinivasan, K; Thomas, D; Woodruff, A; Deborba, B; Munch, D J

    2006-06-16

    Since 1997 there has been increasing interest in the development of analytical methods for the analysis of perchlorate. The US Environmental Protection Agency (EPA) Method 314.0, which was used during the first Unregulated Contaminant Monitoring Regulation (UCMR) cycle, supports a method reporting limit (MRL) of 4.0 microg/L. The non-selective nature of conductivity detection, combined with very high ionic strength matrices, can create conditions that make the determination of perchlorate difficult. The objective of this work was to develop an automated, suppressed conductivity method with improved sensitivity for use in the second UCMR cycle. The new method, EPA Method 314.1, uses a 35 mm x 4 mm cryptand concentrator column in the sample loop position to concentrate perchlorate from a 2 mL sample volume, which is subsequently rinsed with 10 mM NaOH to remove interfering anions. The cryptand concentrator column is combined with a primary AS16 analytical column and a confirmation AS20 analytical column. Unique characteristics of the cryptand column allow perchlorate to be desorbed from the cryptand trap and refocused on the head of the guard column for subsequent separation and analysis. EPA Method 314.1 has a perchlorate lowest concentration minimum reporting level (LCMRL) of 0.13 microg/L in both drinking water and laboratory synthetic sample matrices (LSSM) containing up to 1,000 microg/L each of chloride, bicarbonate and sulfate.

  17. Automated extraction of DNA from reference samples from various types of biological materials on the Qiagen BioRobot EZ1 Workstation

    DEFF Research Database (Denmark)

    Stangegaard, Michael; Jørgensen, Mads; Hansen, Anders Johannes;

    2009-01-01

    We have validated and implemented a protocol for DNA extraction from various types of biological materials using a Qiagen BioRobot EZ1 Workstation. The sample materials included whole blood, blood from deceased, buccal cells on Omni swabs and FTA Cards, blood on FTA Cards and cotton swabs......, and muscle biopsies. The DNA extraction was validated according to EN/ISO 17025 for the STR kits AmpFlSTR« Identifiler« and AmpFlSTR« Yfiler« (Applied Biosystems). Of 298 samples extracted, 11 (4%) did not yield acceptable results. In conclusion, we have demonstrated that extraction of DNA from various types...... of biological material can be performed quickly and without the use of hazardous chemicals, and that the DNA may be successfully STR typed according to the requirements of forensic genetic investigations accredited according to EN/ISO 17025...

  18. Full second order chromatographic/spectrometric data matrices for automated sample identification and component analysis by non-data-reducing image analysis

    DEFF Research Database (Denmark)

    Nielsen, Niles-Peter Vest; Smedsgaard, Jørn; Frisvad, Jens Christian

    1999-01-01

    A data analysis method is proposed for identification and for confirmation of classification schemes, based on single- or multiple-wavelength chromatographic profiles. The proposed method works directly on the chromatographic data without data reduction procedures such as peak area or retention...... index calculation, Chromatographic matrices from analysis of previously identified samples are used for generating a reference chromatogram for each class, and unidentified samples are compared with all reference chromatograms by calculating a resemblance measure for each reference. Once the method...... yielded over 90% agreement with accepted classifications. The method is highly accurate and may be used on all sorts of chromatographic profiles. Characteristic component analysis yielded results in good agreement with existing knowledge of characteristic components, but also succeeded in identifying new...

  19. Comparison between whole mount tissue preparations and virtual tissue microarray samples for measuring Ki-67 and apoptosis indices in human bladder cancer: A cross-sectional study.

    Science.gov (United States)

    Oshiro, Hisashi; Czerniak, Bogdan A; Sakamaki, Kentaro; Tsuta, Koji; Bondaruk, Jolanta; Keyhani, Afsaneh; Dinney, Colin P; Nagai, Takeshi; Kamat, Ashish M

    2016-08-01

    Recent tissue microarray (TMA)-based studies have shown that cell proliferation- and apoptosis-related biomarkers are associated with clinical outcomes in patients with bladder urothelial carcinoma. However, little is known about the differences in these biomarker measurements between whole mount tissue preparations and TMAs. This study aimed to elucidate the discrepancy in the measurements of Ki-67 indices (KIs) and apoptosis indices (AIs) between whole mount tissue preparations and TMAs of bladder urothelial carcinoma samples.Whole mount tissue preparations for Ki-67 immunohistochemistry and terminal deoxynucleotidyl transferase dUTP nick end labeling were made from 30 patients who underwent transurethral resection of bladder urothelial carcinoma. Digital microscopy-assisted virtual TMAs, consisting of 3 small round areas (1 or 0.6 mm in diameter), were generated from the same whole mount tissue preparations. The measurement results in highly reactive areas of biomarkers were compared between the whole mount tissue preparation- and the TMA-based methods. Bland-Altman plot analysis, regression analysis, and Kendall τ were performed to investigate differences in the measurement results, systematic biases, and correlations between biomarkers.Although the Bland-Altman plot analysis demonstrated that almost all the plots were within the limits of agreement, fixed biases were detected in the 1- and 0.6-mm TMAs for the KI (0.181 and 0.222, respectively) and the AI (0.055 and 0.063, respectively). Proportional biases were also detected in the 1- and 0.6-mm TMAs for the AI (P KIs and AIs were observed in whole mount tissue preparations (r = 0.260, P = 0.044) and in the 1 mm TMAs (r = 0.375, P = 0.004); however, no such correlation was observed in the 0.6 mm TMAs.Our study suggests that the measurement results for certain biomarkers of bladder urothelial carcinoma obtained from TMA-based samples can be susceptible to systematic bias, and the lack

  20. Comparison between whole mount tissue preparations and virtual tissue microarray samples for measuring Ki-67 and apoptosis indices in human bladder cancer

    Science.gov (United States)

    Oshiro, Hisashi; Czerniak, Bogdan A.; Sakamaki, Kentaro; Tsuta, Koji; Bondaruk, Jolanta; Keyhani, Afsaneh; Dinney, Colin P.; Nagai, Takeshi; Kamat, Ashish M.

    2016-01-01

    Abstract Recent tissue microarray (TMA)-based studies have shown that cell proliferation- and apoptosis-related biomarkers are associated with clinical outcomes in patients with bladder urothelial carcinoma. However, little is known about the differences in these biomarker measurements between whole mount tissue preparations and TMAs. This study aimed to elucidate the discrepancy in the measurements of Ki-67 indices (KIs) and apoptosis indices (AIs) between whole mount tissue preparations and TMAs of bladder urothelial carcinoma samples. Whole mount tissue preparations for Ki-67 immunohistochemistry and terminal deoxynucleotidyl transferase dUTP nick end labeling were made from 30 patients who underwent transurethral resection of bladder urothelial carcinoma. Digital microscopy-assisted virtual TMAs, consisting of 3 small round areas (1 or 0.6 mm in diameter), were generated from the same whole mount tissue preparations. The measurement results in highly reactive areas of biomarkers were compared between the whole mount tissue preparation- and the TMA-based methods. Bland–Altman plot analysis, regression analysis, and Kendall τ were performed to investigate differences in the measurement results, systematic biases, and correlations between biomarkers. Although the Bland–Altman plot analysis demonstrated that almost all the plots were within the limits of agreement, fixed biases were detected in the 1- and 0.6-mm TMAs for the KI (0.181 and 0.222, respectively) and the AI (0.055 and 0.063, respectively). Proportional biases were also detected in the 1- and 0.6-mm TMAs for the AI (P < 0.001 and P < 0.001, respectively). Furthermore, positive correlations between KIs and AIs were observed in whole mount tissue preparations (r = 0.260, P = 0.044) and in the 1 mm TMAs (r = 0.375, P = 0.004); however, no such correlation was observed in the 0.6 mm TMAs. Our study suggests that the measurement results for certain biomarkers of bladder