Science.gov

Sample records for afci sampling analysis

  1. Enhanced AFCI Sampling, Analysis, and Safeguards Technology Review

    SciTech Connect

    John Svoboda

    2009-09-01

    The focus of this study includes the investigation of sampling technologies used in industry and their potential application to nuclear fuel processing. The goal is to identify innovative sampling methods using state of the art techniques that could evolve into the next generation sampling and analysis system for metallic elements. Sampling and analysis of nuclear fuel recycling plant processes is required both to monitor the operations and ensure Safeguards and Security goals are met. In addition, environmental regulations lead to additional samples and analysis to meet licensing requirements. The volume of samples taken by conventional means, can restrain productivity while results samples are analyzed, require process holding tanks that are sized to meet analytical issues rather than process issues (and that create a larger facility footprint), or, in some cases, simply overwhelm analytical laboratory capabilities. These issues only grow when process flowsheets propose new separations systems and new byproduct material for transmutation purposes. Novel means of streamlining both sampling and analysis are being evaluated to increase the efficiency while meeting all requirements for information. This report addresses just a part of the effort to develop and study novel methods by focusing on the sampling and analysis of aqueous samples for metallic elements. It presents an overview of the sampling requirements, including frequency, sensitivity, accuracy, and programmatic drivers, to demonstrate the magnitude of the task. The sampling and analysis system needed for metallic element measurements is then discussed, and novel options being applied to other industrial analytical needs are presented. Inductively coupled mass spectrometry instruments are the most versatile for metallic element analyses and are thus chosen as the focus for the study. Candidate novel means of process sampling, as well as modifications that are necessary to couple such instruments to

  2. 2014 AFCI Glovebox Event Executive Summary

    SciTech Connect

    Campbell, Joseph Lenard

    2016-01-01

    One of the primary INL missions is to support development of advanced fuels with the goal of creating reactor fuels that produce less waste and are easier to store. The Advanced Fuel Cycle Initiative (AFCI) Glovebox in the Fuel Manufacturing Facility (FMF) is used for several fuel fabrication steps that involve transuranic elements, including americium. The AFCI glove box contains equipment used for fuel fabrication, including an arc melter – a small, laboratory-scale version of an electric arc furnace used to make new metal alloys for research – and an americium distillation apparatus. This overview summarizes key findings related to the investigation into the releases of airborne radioactivity that occurred in the AFCI glovebox room in late August and early September 2014. The full report (AFCI Glovebox Radiological Release – Evaluation, Corrective Actions and Testing, INL/INL-15-36996) provides details of the identified issues, corrective actions taken as well as lessons learned

  3. Quality Assurance Protocol for AFCI Advanced Structural Materials Testing

    SciTech Connect

    Busby, Jeremy T

    2009-05-01

    application of NQA-1 requirements at the site. The current program is being revised to incorporate changes imposed through the recently revised AFCI Technical Integration Office QA requirements. Testing conducted under the AFCI QA program for the advanced structural materials effort shall incorporate the following quality assurance expectations: (1) personnel are adequately trained to perform assigned work; (2) activities are controlled to ensure consistency of results; (3) records necessary to substantiate how the work was performed are maintained (dedicated laboratory notebooks will be used); (4) the pedigree and traceability of the various tested materials are maintained throughout the described processes using consistent sample numbering and adequate record keeping; (5) equipment with the potential to affect the quality of the planned work is calibrated and maintained in accordance with applicable operating requirements. In addition, all reporting or related dissemination by ORNL personnel of the results of the work described in this subcontract shall be conducted in accordance with the requirements described or referenced in the ORNL Standards Based Management System subject area entitled Scientific and Technical Information. Reporting or publications at other institutions will be conducted in accordance with the requirements of that institution. Successful implementation of these protocols will provide a sound basis for future decisions and research. In addition, these steps will also help ensure that results can also be applied to licensing discussions at a future date.

  4. AFCI Safeguards Enhancement Study: Technology Development Roadmap

    SciTech Connect

    Smith, Leon E.; Dougan, A.; Tobin, Stephen; Cipiti, B.; Ehinger, Michael H.; Bakel, A. J.; Bean, Robert; Grate, Jay W.; Santi, P.; Bryan, Steven; Kinlaw, M. T.; Schwantes, Jon M.; Burr, Tom; Lehn, Scott A.; Tolk, K.; Chichester, David; Menlove, H.; Vo, D.; Duckworth, Douglas C.; Merkle, P.; Wang, T. F.; Duran, F.; Nakae, L.; Warren, Glen A.; Friedrich, S.; Rabin, M.

    2008-12-31

    The Advanced Fuel Cycle Initiative (AFCI) Safeguards Campaign aims to develop safeguards technologies and processes that will significantly reduce the risk of proliferation in the U.S. nuclear fuel cycle of tomorrow. The Safeguards Enhancement Study was chartered with identifying promising research and development (R&D) directions over timescales both near-term and long-term, and under safeguards oversight both domestic and international. This technology development roadmap documents recognized gaps and needs in the safeguarding of nuclear fuel cycles, and outlines corresponding performance targets for each of those needs. Drawing on the collective expertise of technologists and user-representatives, a list of over 30 technologies that have the potential to meet those needs was developed, along with brief summaries of each candidate technology. Each summary describes the potential impact of that technology, key research questions to be addressed, and prospective development milestones that could lead to a definitive viability or performance assessment. Important programmatic linkages between U.S. agencies and offices are also described, reflecting the emergence of several safeguards R&D programs in the U.S. and the reinvigoration of nuclear fuel cycles across the globe.

  5. MDD Status Letter Report (AFCI CETE Milestone)

    SciTech Connect

    Vedder, Raymond James; Jubin, Robert Thomas

    2009-09-01

    understanding of the chemistry of the uranium-ammonium double nitrate salt was developed. Later pilot-scale studies produced kilogram quantities of UO{sub 3} using engineering-scale (1 kg/hour), continuously-operated equipment, while establishing the reliability of the process and equipment. The current work was performed in support of the Advanced Fuel Cycle Initiative (AFCI), utilizing glove-box-contained equipment (100 g/hour) to produce UO{sub 3}, PuO{sub 2}, and mixed oxides of uranium, plutonium, neptunium, and americium from a nitrate solution of those actinides. Then the MDD glove-box system was utilized in the Coupled-End-To-End (CETE) project to convert the U-Pu-Np and uranium product solutions into oxide powders. As part of the CETE project, a powder characterization laboratory was established in gloveboxes with instruments required for the determination of: (1) surface area by the BET methodology; (2) tap density by using a Quantachrome AutoTap; (3) flow properties by using a Freeman technology powder rheometer; (4) material composition and crystalline structure by using a powder X-ray diffractometer; (5) particle size distribution by using a laser light-scattering analyzer; and (6) imaging of the powders with a stereomicroscope. These instruments can be used to characterize the products and to determine the effects of MDD operating parameters on product powder morphology. Ultimately, the powder characteristics necessary to produce high-density, sintered MOX pellets can be determined.

  6. AFCI-2.0 Library of Neutron Cross Section Covariances

    SciTech Connect

    Herman, M.; Herman,M.; Oblozinsky,P.; Mattoon,C.; Pigni,M.; Hoblit,S.; Mughabghab,S.F.; Sonzogni,A.; Talou,P.; Chadwick,M.B.; Hale.G.M.; Kahler,A.C.; Kawano,T.; Little,R.C.; Young,P.G.

    2011-06-26

    Neutron cross section covariance library has been under development by BNL-LANL collaborative effort over the last three years. The primary purpose of the library is to provide covariances for the Advanced Fuel Cycle Initiative (AFCI) data adjustment project, which is focusing on the needs of fast advanced burner reactors. The covariances refer to central values given in the 2006 release of the U.S. neutron evaluated library ENDF/B-VII. The preliminary version (AFCI-2.0beta) has been completed in October 2010 and made available to the users for comments. In the final 2.0 release, covariances for a few materials were updated, in particular new LANL evaluations for {sup 238,240}Pu and {sup 241}Am were adopted. BNL was responsible for covariances for structural materials and fission products, management of the library and coordination of the work, while LANL was in charge of covariances for light nuclei and for actinides.

  7. AFCI-2.0 Neutron Cross Section Covariance Library

    SciTech Connect

    Herman, M.; Herman, M; Oblozinsky, P.; Mattoon, C.M.; Pigni, M.; Hoblit, S.; Mughabghab, S.F.; Sonzogni, A.; Talou, P.; Chadwick, M.B.; Hale, G.M.; Kahler, A.C.; Kawano, T.; Little, R.C.; Yount, P.G.

    2011-03-01

    The cross section covariance library has been under development by BNL-LANL collaborative effort over the last three years. The project builds on two covariance libraries developed earlier, with considerable input from BNL and LANL. In 2006, international effort under WPEC Subgroup 26 produced BOLNA covariance library by putting together data, often preliminary, from various sources for most important materials for nuclear reactor technology. This was followed in 2007 by collaborative effort of four US national laboratories to produce covariances, often of modest quality - hence the name low-fidelity, for virtually complete set of materials included in ENDF/B-VII.0. The present project is focusing on covariances of 4-5 major reaction channels for 110 materials of importance for power reactors. The work started under Global Nuclear Energy Partnership (GNEP) in 2008, which changed to Advanced Fuel Cycle Initiative (AFCI) in 2009. With the 2011 release the name has changed to the Covariance Multigroup Matrix for Advanced Reactor Applications (COMMARA) version 2.0. The primary purpose of the library is to provide covariances for AFCI data adjustment project, which is focusing on the needs of fast advanced burner reactors. Responsibility of BNL was defined as developing covariances for structural materials and fission products, management of the library and coordination of the work; LANL responsibility was defined as covariances for light nuclei and actinides. The COMMARA-2.0 covariance library has been developed by BNL-LANL collaboration for Advanced Fuel Cycle Initiative applications over the period of three years, 2008-2010. It contains covariances for 110 materials relevant to fast reactor R&D. The library is to be used together with the ENDF/B-VII.0 central values of the latest official release of US files of evaluated neutron cross sections. COMMARA-2.0 library contains neutron cross section covariances for 12 light nuclei (coolants and moderators), 78 structural

  8. Code qualification of structural materials for AFCI advanced recycling reactors.

    SciTech Connect

    Natesan, K.; Li, M.; Majumdar, S.; Nanstad, R.K.; Sham, T.-L.

    2012-05-31

    This report summarizes the further findings from the assessments of current status and future needs in code qualification and licensing of reference structural materials and new advanced alloys for advanced recycling reactors (ARRs) in support of Advanced Fuel Cycle Initiative (AFCI). The work is a combined effort between Argonne National Laboratory (ANL) and Oak Ridge National Laboratory (ORNL) with ANL as the technical lead, as part of Advanced Structural Materials Program for AFCI Reactor Campaign. The report is the second deliverable in FY08 (M505011401) under the work package 'Advanced Materials Code Qualification'. The overall objective of the Advanced Materials Code Qualification project is to evaluate key requirements for the ASME Code qualification and the Nuclear Regulatory Commission (NRC) approval of structural materials in support of the design and licensing of the ARR. Advanced materials are a critical element in the development of sodium reactor technologies. Enhanced materials performance not only improves safety margins and provides design flexibility, but also is essential for the economics of future advanced sodium reactors. Code qualification and licensing of advanced materials are prominent needs for developing and implementing advanced sodium reactor technologies. Nuclear structural component design in the U.S. must comply with the ASME Boiler and Pressure Vessel Code Section III (Rules for Construction of Nuclear Facility Components) and the NRC grants the operational license. As the ARR will operate at higher temperatures than the current light water reactors (LWRs), the design of elevated-temperature components must comply with ASME Subsection NH (Class 1 Components in Elevated Temperature Service). However, the NRC has not approved the use of Subsection NH for reactor components, and this puts additional burdens on materials qualification of the ARR. In the past licensing review for the Clinch River Breeder Reactor Project (CRBRP) and the

  9. SAMPLING AND ANALYSIS PROTOCOLS

    SciTech Connect

    Jannik, T; P Fledderman, P

    2007-02-09

    Radiological sampling and analyses are performed to collect data for a variety of specific reasons covering a wide range of projects. These activities include: Effluent monitoring; Environmental surveillance; Emergency response; Routine ambient monitoring; Background assessments; Nuclear license termination; Remediation; Deactivation and decommissioning (D&D); and Waste management. In this chapter, effluent monitoring and environmental surveillance programs at nuclear operating facilities and radiological sampling and analysis plans for remediation and D&D activities will be discussed.

  10. Lunar sample analysis

    NASA Technical Reports Server (NTRS)

    Housley, R. M.

    1986-01-01

    A wide variety of lunar sample and meteorite studies were performed. Abstracts of the most recent reports are also attached. Experimental techniques employed have included scanning electron microscopy, transmission electron microscopy, Mossbauer spectroscopy, atomic absorption analysis and a variety of simulation studies.

  11. Germanium-76 Sample Analysis

    SciTech Connect

    Kouzes, Richard T.; Engelhard, Mark H.; Zhu, Zihua

    2011-04-01

    The MAJORANA DEMONSTRATOR is a large array of ultra-low background high-purity germanium detectors, enriched in 76Ge, designed to search for zero-neutrino double-beta decay (0νββ). The DEMONSTRATOR will utilize 76Ge from Russia, and the first one gram sample was received from the supplier for analysis on April 24, 2011. The Environmental Molecular Sciences facility, a DOE user facility at PNNL, was used to make the required isotopic and chemical purity measurements that are essential to the quality assurance for the MAJORANA DEMONSTRATOR. The results of this first analysis are reported here.

  12. AFCI Transmutation Fuel Processes and By-Products Planning: Interim Report

    SciTech Connect

    Eric L. Shaber

    2005-09-01

    The goals of the Advanced Fuel Cycle Initiative (AFCI) Program are to reduce high-level waste volume, reduce long-lived and radiotoxic elements, and reclaim valuable energy content of spent nuclear fuel. The AFCI chartered the Fuel Development Working Group (FDWG) to develop advanced fuels in support of the AFCI goals. The FDWG organized a phased strategy of fuel development that is designed to match the needs of the AFCI program: Phase 1 - High-burnup fuels for light-water reactors (LWRs) and tri-isotopic (TRISO) fuel for gas-cooled reactors Phase 2 – Mixed oxide fuels with minor actinides for LWRs, Am transmutation targets for LWRs, inert matrix fuels for LWRs, and TRISO fuel containing Pu and other transuranium for gas-cooled reactors Phase 3 – Fertile free or low-fertile metal, ceramic, ceramic dispersed in a metal matrix (CERMET), and ceramics dispersed in a ceramic matrix (CERCER) that would be used primarily in fast reactors. Development of advanced fuels requires the fabrication, assembly, and irradiation of prototypic fuel under bounding reactor conditions. At specialized national laboratory facilities small quantities of actinides are being fabricated into such fuel for irradiation tests. Fabrication of demonstration quantities of selected fuels for qualification testing is needed but not currently feasible, because existing manual glovebox fabrication approaches result in significant radiation exposures when larger quantities of actinides are involved. The earliest demonstration test fuels needed in the AFCI program are expected to be variants of commercial mixed oxide fuel for use in an LWR as lead test assemblies. Manufacture of such test assemblies will require isolated fabrication lines at a facility not currently available in the U.S. Such facilities are now being planned as part of an Advanced Fuel Cycle Facility (AFCF). Adequate planning for and specification of actinide fuel fabrication facilities capable of producing transmutation fuels

  13. Revisiting sample entropy analysis

    NASA Astrophysics Data System (ADS)

    Govindan, R. B.; Wilson, J. D.; Eswaran, H.; Lowery, C. L.; Preißl, H.

    2007-03-01

    We modify the definition of sample entropy (SaEn) by incorporating a time delay between the components of the block (from which the densities are estimated) and show that the modified method characterizes the complexity of the system better than the original version. We apply the modified SaEn to the standard deterministic systems and stochastic processes (uncorrelated and long range correlated (LRC) processes) and show that the underlying complexity of the system is better quantified by the modified method. We extend this analysis to the RR intervals of the normal and congestive heart failure (CHF) subjects (available via www.physionet.org) and show that there is a good degree of separation between the two groups.

  14. Progress on Nuclear Data Covariances: AFCI-1.2 Covariance Library

    SciTech Connect

    Oblozinsky,P.; Oblozinsky,P.; Mattoon,C.M.; Herman,M.; Mughabghab,S.F.; Pigni,M.T.; Talou,P.; Hale,G.M.; Kahler,A.C.; Kawano,T.; Little,R.C.; Young,P.G

    2009-09-28

    Improved neutron cross section covariances were produced for 110 materials including 12 light nuclei (coolants and moderators), 78 structural materials and fission products, and 20 actinides. Improved covariances were organized into AFCI-1.2 covariance library in 33-energy groups, from 10{sup -5} eV to 19.6 MeV. BNL contributed improved covariance data for the following materials: {sup 23}Na and {sup 55}Mn where more detailed evaluation was done; improvements in major structural materials {sup 52}Cr, {sup 56}Fe and {sup 58}Ni; improved estimates for remaining structural materials and fission products; improved covariances for 14 minor actinides, and estimates of mubar covariances for {sup 23}Na and {sup 56}Fe. LANL contributed improved covariance data for {sup 235}U and {sup 239}Pu including prompt neutron fission spectra and completely new evaluation for {sup 240}Pu. New R-matrix evaluation for {sup 16}O including mubar covariances is under completion. BNL assembled the library and performed basic testing using improved procedures including inspection of uncertainty and correlation plots for each material. The AFCI-1.2 library was released to ANL and INL in August 2009.

  15. Summary of Off-Normal Events in US Fuel Cycle Facilities for AFCI Applications

    SciTech Connect

    L. C. Cadwallader; S. J. Piet; S. O. Sheetz; D. H. McGuire; W. B. Boore

    2005-09-01

    This report is a collection and review of system operation and failure experiences for facilities comprising the fission reactor fuel cycle, with the exception of reactor operations. This report includes mines, mills, conversion plants, enrichment plants, fuel fabrication plants, transportation of fuel materials between these centers, and waste storage facilities. Some of the facilities discussed are no longer operating; others continue to produce fuel for the commercial fission power plant industry. Some of the facilities discussed have been part of the military’s nuclear effort; these are included when the processes used are similar to those used for commercial nuclear power. When reading compilations of incidents and accidents, after repeated entries it is natural to form an opinion that there exists nothing but accidents. For this reason, production or throughput values are described when available. These adverse operating experiences are compiled to support the design and decisions needed for the Advanced Fuel Cycle Initiative (AFCI). The AFCI is to weigh options for a new fission reactor fuel cycle that is efficient, safe, and productive for US energy security.

  16. Sampling for Chemical Analysis.

    ERIC Educational Resources Information Center

    Kratochvil, Byron; And Others

    1984-01-01

    This review, designed to make analysts aware of uncertainties introduced into analytical measurements during sampling, is organized under these headings: general considerations; theory; standards; and applications related to mineralogy, soils, sediments, metallurgy, atmosphere, water, biology, agriculture and food, medical and clinical areas, oil…

  17. Lunar sample analysis

    NASA Technical Reports Server (NTRS)

    Tittmann, B. R.

    1975-01-01

    Previous studies have shown that very small amounts of absorbed volatiles only removed by outgassing in high vacuum and elevated temperatures-drastically increase the internal friction in terrestrial analogs of lunar basalt. Recently room temperature Q values as high as 2000 were achieved by thorough outgassing procedures in 10 to the 8th power torr. Results are presented on Q measurements for lunar rock 70215.85, along with some data on the effect on Q of a variety of gases. Data show that substantially greater increases in Q are obtainable in a lunar rock sample than in the terrestrial analog samples studied, and that in addition to H2O other gases also can make non-negligible contributions to the internal friction.

  18. Analysis of Pet Coke Samples

    EPA Pesticide Factsheets

    EPA required KCBX to submit samples of the petroleum coke stored at their North and South Chicago terminals to EPA's Chicago Regional Laboratory for analysis of pollutant levels. Results will be compared to coal and pet coke sampled in Detroit.

  19. AFCI Fuel Irradiation Test Plan, Test Specimens AFC-1Æ and AFC-1F

    SciTech Connect

    D. C. Crawford; S. L. Hayes; B. A. Hilton; M. K. Meyer; R. G. Ambrosek; G. S. Chang; D. J. Utterbeck

    2003-11-01

    The U. S. Advanced Fuel Cycle Initiative (AFCI) seeks to develop and demonstrate the technologies needed to transmute the long-lived transuranic actinide isotopes contained in spent nuclear fuel into shorter-lived fission products, thereby dramatically decreasing the volume of material requiring disposition and the long-term radiotoxicity and heat load of high-level waste sent to a geologic repository (DOE, 2003). One important component of the technology development is actinide-bearing transmutation fuel forms containing plutonium, neptunium, americium (and possibly curium) isotopes. There are little irradiation performance data available on non-fertile fuel forms, which would maximize the destruction rate of plutonium, and low-fertile (i.e., uranium-bearing) fuel forms, which would support a sustainable nuclear energy option. Initial scoping level irradiation tests on a variety of candidate fuel forms are needed to establish a transmutation fuel form design and evaluate deployment of transmutation fuels.

  20. AFCI UFP, Final Technical Report DE-FC07-00AL67053

    SciTech Connect

    Cathy Dixon

    2005-02-21

    The project ''Creating an Educational Consortium to Support the Recruitment and Retention of Expertise for the Nuclear Weapons Complex'' was also known as the Advanced Fuel Cycle Initiative (AFCI) University Fellowship Program. Since its inception, the Advanced Fuel Cycle Initiative program and its predecessor, the Advanced Accelerator Applications (AAA) program, have engaged university researchers and students in the sciences necessary to answer technical questions related to reducing high-level waste volumes, optimizing the economics and performance of Yucca Mountain, reducing the technical need for a second repository, reducing the long-term inventories of plutonium in spent fuel, and enabling the proliferation-resistant recovery of the energy contained in spent fuel. The Advanced Fuel Cycle University Fellowship Program is intended to support top students across the nation in a variety of disciplines that will be required to support transmutation research and technology development in the coming decades.

  1. GET electronics samples data analysis

    NASA Astrophysics Data System (ADS)

    Giovinazzo, J.; Goigoux, T.; Anvar, S.; Baron, P.; Blank, B.; Delagnes, E.; Grinyer, G. F.; Pancin, J.; Pedroza, J. L.; Pibernat, J.; Pollacco, E.; Rebii, A.; Roger, T.; Sizun, P.

    2016-12-01

    The General Electronics for TPCs (GET) has been developed to equip a generation of time projection chamber detectors for nuclear physics, and may also be used for a wider range of detector types. The goal of this paper is to propose first analysis procedures to be applied on raw data samples from the GET system, in order to correct for systematic effects observed on test measurements. We also present a method to estimate the response function of the GET system channels. The response function is required in analysis where the input signal needs to be reconstructed, in terms of time distribution, from the registered output samples.

  2. Reactor physics studies for the Advanced Fuel Cycle Initiative (AFCI) Reactor-Accelerator Coupling Experiments (RACE) Project

    NASA Astrophysics Data System (ADS)

    Stankovskiy, Evgeny Yuryevich

    In the recently completed RACE Project of the AFCI, accelerator-driven subcritical systems (ADS) experiments were conducted to develop technology of coupling accelerators to nuclear reactors. In these experiments electron accelerators induced photon-neutron reactions in heavy-metal targets to initiate fission reactions in ADS. Although the Idaho State University (ISU) RACE ADS was constructed only to develop measurement techniques for advanced experiments, many reactor kinetics experiments were conducted there. In the research reported in this dissertation, a method was developed to calculate kinetics parameters for measurement and calculation of the reactivity of ADS, a safety parameter that is necessary for control and monitoring of power production. Reactivity is measured in units of fraction of delayed versus prompt neutron from fission, a quantity that cannot be directly measured in far-subcritical reactors such as the ISU RACE configuration. A new technique is reported herein to calculate it accurately and to predict kinetic behavior of a far-subcritical ADS. Experiments conducted at ISU are first described and experimental data are presented before development of the kinetic theory used in the new computational method. Because of the complexity of the ISU ADS, the Monte-Carlo method as applied in the MCNP code is most suitable for modeling reactor kinetics. However, the standard method of calculating the delayed neutron fraction produces inaccurate values. A new method was developed and used herein to evaluate actual experiments. An advantage of this method is that its efficiency is independent of the fission yield of delayed neutrons, which makes it suitable for fuel with a minor actinide component (e.g. transmutation fuels). The implementation of this method is based on a correlated sampling technique which allows the accurate evaluation of delayed and prompt neutrons. The validity of the obtained results is indicated by good agreement between experimental

  3. 340 Representative sampling verification tank sampling and analysis plan

    SciTech Connect

    Olander, A.R., Westinghouse Hanford

    1996-08-21

    This Sampling and Analysis Plan contains requirements for characterizing the 340 vault tank 1. The objective of the sampling and characterization is to determine if the tank is homogeneous when agitated and which sampling method provides the most representative sample. A secondary objective is to collect and characterize solid samples.

  4. Sample Manipulation System for Sample Analysis at Mars

    NASA Technical Reports Server (NTRS)

    Mumm, Erik; Kennedy, Tom; Carlson, Lee; Roberts, Dustyn

    2008-01-01

    The Sample Analysis at Mars (SAM) instrument will analyze Martian samples collected by the Mars Science Laboratory Rover with a suite of spectrometers. This paper discusses the driving requirements, design, and lessons learned in the development of the Sample Manipulation System (SMS) within SAM. The SMS stores and manipulates 74 sample cups to be used for solid sample pyrolysis experiments. Focus is given to the unique mechanism architecture developed to deliver a high packing density of sample cups in a reliable, fault tolerant manner while minimizing system mass and control complexity. Lessons learned are presented on contamination control, launch restraint mechanisms for fragile sample cups, and mechanism test data.

  5. Sub-sampling and preparing forensic samples for pollen analysis.

    PubMed

    Horrocks, Mark

    2004-09-01

    The main forensic application of palynology is in providing associative evidence, assisting to prove or disprove a link between people and objects with places or with other people. Although identification and interpretation of pollen is a specialist job, sub-sampling and preparing pollen samples for analysis may be carried out by non-specialists. As few forensic laboratories have residing palynologists, laboratories may wish to reduce the cost of analysis or risk of contamination by doing their own sub-sampling and preparation. Presented is a practical guide for sub-sampling and preparing forensic samples for pollen analysis, providing a complete standard procedure for both the palynologist and non-specialist. Procedures for sub-sampling include a wide variety of materials commonly collected for forensic analysis (soil, clothing and other fabrics, footwear, twine and rope, firearms, granulated materials, plant and animal material, and illicit drugs), many of which palynologists will not be familiar with. Procedures for preparation of samples (pollen concentration) are presented as a detailed, step-by-step method. Minimizing the risks of laboratory and cross-sample contamination during sub-sampling and preparation is emphasized.

  6. Sampling and sample processing in pesticide residue analysis.

    PubMed

    Lehotay, Steven J; Cook, Jo Marie

    2015-05-13

    Proper sampling and sample processing in pesticide residue analysis of food and soil have always been essential to obtain accurate results, but the subject is becoming a greater concern as approximately 100 mg test portions are being analyzed with automated high-throughput analytical methods by agrochemical industry and contract laboratories. As global food trade and the importance of monitoring increase, the food industry and regulatory laboratories are also considering miniaturized high-throughput methods. In conjunction with a summary of the symposium "Residues in Food and Feed - Going from Macro to Micro: The Future of Sample Processing in Residue Analytical Methods" held at the 13th IUPAC International Congress of Pesticide Chemistry, this is an opportune time to review sampling theory and sample processing for pesticide residue analysis. If collected samples and test portions do not adequately represent the actual lot from which they came and provide meaningful results, then all costs, time, and efforts involved in implementing programs using sophisticated analytical instruments and techniques are wasted and can actually yield misleading results. This paper is designed to briefly review the often-neglected but crucial topic of sample collection and processing and put the issue into perspective for the future of pesticide residue analysis. It also emphasizes that analysts should demonstrate the validity of their sample processing approaches for the analytes/matrices of interest and encourages further studies on sampling and sample mass reduction to produce a test portion.

  7. Sampling and sample processing in pesticide residue analysis

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Proper sampling and sample processing in pesticide residue analysis of food and soil has always been essential to obtain accurate results, but the subject is becoming a greater concern as approximately 100 mg test portions are being analyzed with automated high-throughput analytical methods by agroc...

  8. IWTU Process Sample Analysis Report

    SciTech Connect

    Nick Soelberg

    2013-04-01

    CH2M-WG Idaho (CWI) requested that Battelle Energy Alliance (BEA) analyze various samples collected during June – August 2012 at the Integrated Waste Treatment Facility (IWTU). Samples of IWTU process materials were collected from various locations in the process. None of these samples were radioactive. These samples were collected and analyzed to provide more understanding of the compositions of various materials in the process during the time of the process shutdown that occurred on June 16, 2012, while the IWTU was in the process of nonradioactive startup.

  9. FIELD SAMPLING PROTOCOLS AND ANALYSIS

    EPA Science Inventory

    I have been asked to speak again to the environmental science class regarding actual research scenarios related to my work at Kerr Lab. I plan to discuss sampling protocols along with various field analyses performed during sampling activities. Many of the students have never see...

  10. 40 CFR 1065.1111 - Sample analysis.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 33 2014-07-01 2014-07-01 false Sample analysis. 1065.1111 Section... § 1065.1111 Sample analysis. This subpart does not specify chromatographic or analytical methods to... process by verifying the volume of sample injected for analysis....

  11. Sample collection, biobanking, and analysis.

    PubMed

    Ahsman, Maurice J; Tibboel, Dick; Mathot, Ron A A; de Wildt, Saskia N

    2011-01-01

    Pediatric pharmacokinetic studies require sampling of biofluids from neonates and children. Limitations on sampling frequency and sample volume complicate the design of these studies. In addition, strict guidelines, designed to guarantee patient safety, are in place. This chapter describes the practical implications of sample collection and their storage, with special focus on the selection of the appropriate type of biofluid and withdrawal technique. In addition, we describe appropriate measures for storage of these specimens, for example, in the context of biobanking, and the requirements on drug assay methods that they pose. Pharmacokinetic studies in children are possible, but they require careful selection of an appropriate sampling method, specimen volume, and assay method. The checklist provided could help prospective researchers with the design of an appropriate study protocol and infrastructure.

  12. Sample processor for chemical analysis

    NASA Technical Reports Server (NTRS)

    Boettger, Heinz G. (Inventor)

    1980-01-01

    An apparatus is provided which can process numerous samples that must be chemically analyzed by the application of fluids such as liquid reagents, solvents and purge gases, as well as the application of dumps for receiving the applied fluid after they pass across the sample, in a manner that permits numerous samples to be processed in a relatively short time and with minimal manpower. The processor includes a rotor which can hold numerous cartridges containing inert or adsorbent material for holding samples, and a pair of stators on opposite sides of the rotor. The stators form stations spaced along the path of the cartridges which lie in the rotor, and each station can include an aperture in one stator through which a fluid can be applied to a cartridge resting at that station, and an aperture in the other stator which can receive the fluid which has passed through the cartridge. The stators are sealed to the ends of the cartridges lying on the rotor, to thereby isolate the stations from one another.

  13. Microwave sample preparation for analysis of metals in environmental samples

    SciTech Connect

    Collins, L.W.

    1996-10-01

    The unique nature of microwave energy enhances heating efficiency and improves acid digestion sample preparation. Faster sample preparation and improved precision of the analysis occur. These results will be illustrated in this presentation using various standard reference materials and environmentally important samples. The analytical microwave system used offers accurate temperature and pressure feedback control through the use of a hand-held controller or PC-based control. Digestions are performed in patented, user-friendly microwave vessels. USEPA Method 3015, {open_quotes}Microwave-Assisted Acid Digestion of Aqueous Samples and Extracts,{close_quotes} is properly performed when the sample is heated to 170{degrees}C within 10 minutes, and maintained for an additional 10 minutes. USEPA Method 3051, {open_quotes}Microwave-Assisted Acid Digestion of Sediments, Sludges, Soils, and Oils,{close_quotes} is properly performed when the sample is heated to 175{degrees}C within 5.5 minutes, and maintained at 175{degrees}C for an additional 4.5 minutes. After the timesaving microwave digestion period, the samples were analyzed for metals by ICP-AES. Excellent accuracy and precision were obtained, in addition to 90% time reduction when using microwave sample preparation.

  14. Tank 12H residuals sample analysis report

    SciTech Connect

    Oji, L. N.; Shine, E. P.; Diprete, D. P.; Coleman, C. J.; Hay, M. S.

    2015-06-11

    The Savannah River National Laboratory (SRNL) was requested by Savannah River Remediation (SRR) to provide sample preparation and analysis of the Tank 12H final characterization samples to determine the residual tank inventory prior to grouting. Eleven Tank 12H floor and mound residual material samples and three cooling coil scrape samples were collected and delivered to SRNL between May and August of 2014.

  15. REPRESENTATIVE SAMPLING AND ANALYSIS OF HETEROGENEOUS SOILS

    EPA Science Inventory

    Standard sampling and analysis methods for hazardous substances in contaminated soils currently are available and routinely employed. Standard methods inherently assume a homogeneous soil matrix and contaminant distribution; therefore only small sample quantities typically are p...

  16. Integrated sampling procedure for metabolome analysis.

    PubMed

    Schaub, Jochen; Schiesling, Carola; Reuss, Matthias; Dauner, Michael

    2006-01-01

    Metabolome analysis, the analysis of large sets of intracellular metabolites, has become an important systems analysis method in biotechnological and pharmaceutical research. In metabolic engineering, the integration of metabolome data with fluxome and proteome data into large-scale mathematical models promises to foster rational strategies for strain and cell line improvement. However, the development of reproducible sampling procedures for quantitative analysis of intracellular metabolite concentrations represents a major challenge, accomplishing (i) fast transfer of sample, (ii) efficient quenching of metabolism, (iii) quantitative metabolite extraction, and (iv) optimum sample conditioning for subsequent quantitative analysis. In addressing these requirements, we propose an integrated sampling procedure. Simultaneous quenching and quantitative extraction of intracellular metabolites were realized by short-time exposure of cells to temperatures < or =95 degrees C, where intracellular metabolites are released quantitatively. Based on these findings, we combined principles of heat transfer with knowledge on physiology, for example, turnover rates of energy metabolites, to develop an optimized sampling procedure based on a coiled single tube heat exchanger. As a result, this sampling procedure enables reliable and reproducible measurements through (i) the integration of three unit operations into a one unit operation, (ii) the avoidance of any alteration of the sample due to chemical reagents in quenching and extraction, and (iii) automation. A sampling frequency of 5 s(-)(1) and an overall individual sample processing time faster than 30 s allow observing responses of intracellular metabolite concentrations to extracellular stimuli on a subsecond time scale. Recovery and reliability of the unit operations were analyzed. Impact of sample conditioning on subsequent IC-MS analysis of metabolites was examined as well. The integrated sampling procedure was validated

  17. Sampling almonds for aflatoxin, part I: estimation of uncertainty associated with sampling, sample preparation, and analysis.

    PubMed

    Whitaker, Thomas B; Slate, Andrew B; Jacobs, Merle; Hurley, J Michael; Adams, Julie G; Giesbrecht, Francis G

    2006-01-01

    Domestic and international regulatory limits have been established for aflatoxin in almonds and other tree nuts. It is difficult to obtain an accurate and precise estimate of the true aflatoxin concentration in a bulk lot because of the uncertainty associated with the sampling, sample preparation, and analytical steps of the aflatoxin test procedure. To evaluate the performance of aflatoxin sampling plans, the uncertainty associated with sampling lots of shelled almonds for aflatoxin was investigated. Twenty lots of shelled almonds were sampled for aflatoxin contamination. The total variance associated with measuring B1 and total aflatoxins in bulk almond lots was estimated and partitioned into sampling, sample preparation, and analytical variance components. All variances were found to increase with an increase in aflatoxin concentration (both B1 and total). By using regression analysis, mathematical expressions were developed to predict the relationship between each variance component (total, sampling, sample preparation, and analysis variances) and aflatoxin concentration. Variance estimates were the same for B1 and total aflatoxins. The mathematical relationships can be used to estimate each variance for a given sample size, subsample size, and number of analyses other than that measured in the study. When a lot with total aflatoxins at 15 ng/g was tested by using a 10 kg sample, a vertical cutter mixer type of mill, a 100 g subsample, and high-performance liquid chromatography analysis, the sampling, sample preparation, analytical, and total variances (coefficient of variation, CV) were 394.7 (CV, 132.4%), 14.7 (CV, 25.5%), 0.8 (CV, 6.1%), and 410.2 (CV, 135.0%), respectively. The percentages of the total variance associated with sampling, sample preparation, and analytical steps were 96.2, 3.6, and 0.2, respectively.

  18. Statistical Analysis Techniques for Small Sample Sizes

    NASA Technical Reports Server (NTRS)

    Navard, S. E.

    1984-01-01

    The small sample sizes problem which is encountered when dealing with analysis of space-flight data is examined. Because of such a amount of data available, careful analyses are essential to extract the maximum amount of information with acceptable accuracy. Statistical analysis of small samples is described. The background material necessary for understanding statistical hypothesis testing is outlined and the various tests which can be done on small samples are explained. Emphasis is on the underlying assumptions of each test and on considerations needed to choose the most appropriate test for a given type of analysis.

  19. Sampling hazelnuts for aflatoxin: uncertainty associated with sampling, sample preparation, and analysis.

    PubMed

    Ozay, Guner; Seyhan, Ferda; Yilmaz, Aysun; Whitaker, Thomas B; Slate, Andrew B; Giesbrecht, Francis

    2006-01-01

    The variability associated with the aflatoxin test procedure used to estimate aflatoxin levels in bulk shipments of hazelnuts was investigated. Sixteen 10 kg samples of shelled hazelnuts were taken from each of 20 lots that were suspected of aflatoxin contamination. The total variance associated with testing shelled hazelnuts was estimated and partitioned into sampling, sample preparation, and analytical variance components. Each variance component increased as aflatoxin concentration (either B1 or total) increased. With the use of regression analysis, mathematical expressions were developed to model the relationship between aflatoxin concentration and the total, sampling, sample preparation, and analytical variances. The expressions for these relationships were used to estimate the variance for any sample size, subsample size, and number of analyses for a specific aflatoxin concentration. The sampling, sample preparation, and analytical variances associated with estimating aflatoxin in a hazelnut lot at a total aflatoxin level of 10 ng/g and using a 10 kg sample, a 50 g subsample, dry comminution with a Robot Coupe mill, and a high-performance liquid chromatographic analytical method are 174.40, 0.74, and 0.27, respectively. The sampling, sample preparation, and analytical steps of the aflatoxin test procedure accounted for 99.4, 0.4, and 0.2% of the total variability, respectively.

  20. Electron spectroscopy for chemical analysis: Sample analysis

    NASA Technical Reports Server (NTRS)

    Carter, W. B.

    1989-01-01

    Exposure conditions in atomic oxygen (ESCA) was performed on an SSL-100/206 Small Spot Spectrometer. All data were taken with the use of a low voltage electron flood gun and a charge neutralization screen to minimize charging effects on the data. The X-ray spot size and electron flood gun voltage used are recorded on the individual spectra as are the instrumental resolutions. Two types of spectra were obtained for each specimen: (1) general surveys, and (2) high resolution spectra. The two types of data reduction performed are: (1) semiquantitative compositional analysis, and (2) peak fitting. The materials analyzed are: (1) kapton 4, 5, and 6, (2) HDPE 19, 20, and 21, and (3) PVDF 4, 5, and 6.

  1. Automated Sample collection and Analysis unit

    SciTech Connect

    Latner, Norman; Sanderson, Colin G.; Negro, Vincent C.

    1999-03-31

    Autoramp is an atmospheric radionuclide collection and analysis unit designed for unattended operation. A large volume of air passes through one of 31 filter cartridges which is then moved from a sampling chamber and past a bar code reader, to a shielded enclosure. The collected dust-borne radionuclides are counted with a high resolution germanium gamma-ray detector. An analysis is made and the results are transmitted to a central station that can also remotely control the unit.

  2. Sampling of illicit drugs for quantitative analysis--part III: sampling plans and sample preparations.

    PubMed

    Csesztregi, T; Bovens, M; Dujourdy, L; Franc, A; Nagy, J

    2014-08-01

    The findings in this paper are based on the results of our drug homogeneity studies and particle size investigations. Using that information, a general sampling plan (depicted in the form of a flow-chart) was devised that could be applied to the quantitative instrumental analysis of the most common illicit drugs: namely heroin, cocaine, amphetamine, cannabis resin, MDMA tablets and herbal cannabis in 'bud' form (type I). Other more heterogeneous forms of cannabis (type II) were found to require alternative, more traditional sampling methods. A table was constructed which shows the sampling uncertainty expected when a particular number of random increments are taken and combined to form a single primary sample. It also includes a recommended increment size; which is 1 g for powdered drugs and cannabis resin, 1 tablet for MDMA and 1 bud for herbal cannabis in bud form (type I). By referring to that table, individual laboratories can ensure that the sampling uncertainty for a particular drug seizure can be minimised, such that it lies in the same region as their analytical uncertainty for that drug. The table shows that assuming a laboratory wishes to quantitatively analyse a seizure of powdered drug or cannabis resin with a 'typical' heterogeneity, a primary sample of 15×1 g increments is generally appropriate. The appropriate primary sample for MDMA tablets is 20 tablets, while for herbal cannabis (in bud form) 50 buds were found to be appropriate. Our study also showed that, for a suitably homogenised primary sample of the most common powdered drugs, an analytical sample size of between 20 and 35 mg was appropriate and for herbal cannabis the appropriate amount was 200 mg. The need to ensure that the results from duplicate or multiple incremental sampling were compared, to demonstrate whether or not a particular seized material has a 'typical' heterogeneity and that the sampling procedure applied has resulted in a 'correct sample', was highlighted and the setting

  3. Analysis of Picattiny Sample for Trace Explosives

    SciTech Connect

    Klunder, G; Whipple, R; Carman, L; Spackman, P E; Reynolds, J; Alcaraz, A

    2008-05-23

    The sample received from Picatinny Arsenal was analyzed for trace amounts of high explosives (HE). A complete wash of the surface was performed, concentrated, and analyzed using two sensitive analysis techniques that are capable of detecting numerous types of explosives. No explosives were detected with either test.

  4. Exploratory Factor Analysis with Small Sample Sizes

    ERIC Educational Resources Information Center

    de Winter, J. C. F.; Dodou, D.; Wieringa, P. A.

    2009-01-01

    Exploratory factor analysis (EFA) is generally regarded as a technique for large sample sizes ("N"), with N = 50 as a reasonable absolute minimum. This study offers a comprehensive overview of the conditions in which EFA can yield good quality results for "N" below 50. Simulations were carried out to estimate the minimum required "N" for different…

  5. TEGA Sample Delivery and Analysis (Animation)

    NASA Technical Reports Server (NTRS)

    2008-01-01

    [figure removed for brevity, see original site] Click on image for animation

    This animation shows NASA's Phoenix Lander's Robotic Arm scoop delivering a sample to the Thermal and Evolved-Gas Analyzer (TEGA) and how samples are analyzed within the instrument.

    TEGA has eight tiny ovens for measuring constituents in the atmosphere and in the soil, including possible organic constituents and the melting point of ice.

    The scoop drops soil onto a fine mesh screen between TEGA's open doors. Some soil passes through the screen, which vibrates, into the throat of a funnel, where a spinning device called the 'whirligig' aids delivery into one half of a tiny oven. The soil sample is represented here by the white chip. The filled oven half then rotates and mates with the other oven half, closing the complete oven so sample heating can begin. The purple coil in this animation is the spring that moves the oven halves together.

    Heating occurs at successively higher temperatures over several days. The energy required to heat the sample is measured to discover its thermal properties. Gases driven off during sample heating pass through tubing to the mass spectrometer for analysis.

    Note that the exterior doors above the screen never close after sample delivery.

    The Phoenix Mission is led by the University of Arizona, Tucson, on behalf of NASA. Project management of the mission is by NASAaE(TM)s Jet Propulsion Laboratory, Pasadena, Calif. Spacecraft development is by Lockheed Martin Space Systems, Denver.

  6. Animation of TEGA Sample Delivery and Analysis

    NASA Technical Reports Server (NTRS)

    2008-01-01

    [figure removed for brevity, see original site] Click on image to view the animation

    This animation shows NASA's Phoenix Lander's Robotic Arm scoop delivering a sample to the Thermal and Evolved-Gas Analyzer (TEGA) and how samples are analyzed within the instrument.

    TEGA has eight tiny ovens for measuring constituents in the atmosphere and in the soil, including possible organic constituents and the melting point of ice.

    The scoop drops soil onto a fine mesh screen between TEGA's open doors. Some soil passes through the screen, which vibrates, into the throat of a funnel, where a spinning device called the 'whirligig' aids delivery into one half of a tiny oven. The soil sample is represented here by the white chip. The filled oven half then rotates and mates with the other oven half, closing the complete oven so sample heating can begin. The purple coil in this animation is the spring that moves the oven halves together.

    Heating occurs at successively higher temperatures over several days. The energy required to heat the sample is measured to discover its thermal properties. Gases driven off during sample heating pass through tubing to the mass spectrometer for analysis.

    Note that the exterior doors above the screen never close after sample delivery.

    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.

  7. Germanium-76 Sample Analysis: Revision 3

    SciTech Connect

    Kouzes, Richard T.; Zhu, Zihua; Engelhard, Mark H.

    2011-09-19

    The MAJORANA DEMONSTRATOR is a large array of ultra-low background high-purity germanium detectors, enriched in 76Ge, designed to search for zero-neutrino double-beta decay (0{nu}{beta}{beta}). The DEMONSTRATOR will utilize 76Ge from Russia. The first one-gram sample was received from the supplier for analysis on April 24, 2011. The second one-gram sample was received from the supplier for analysis on July 12, 2011. The third sample, which came from the first large shipment of germanium from the vendor, was received from Oak Ridge National Laboratory (ORNL) on September 13, 2011. The Environmental Molecular Sciences facility, a DOE user facility at PNNL, was used to make the required isotopic and chemical purity measurements that are essential to the quality assurance for the MAJORANA DEMONSTRATOR. The results of these analyses are reported here. The isotopic composition of a sample of natural germanium was also measured twice. Differences in the result between these two measurements led to a re-measurement of the second 76Ge sample.

  8. OVERVIEW OF BERYLLIUM SAMPLING AND ANALYSIS

    SciTech Connect

    Brisson, M

    2009-04-01

    Because of its unique properties as a lightweight metal with high tensile strength, beryllium is widely used in applications including cell phones, golf clubs, aerospace, and nuclear weapons. Beryllium is also encountered in industries such as aluminium manufacturing, and in environmental remediation projects. Workplace exposure to beryllium particulates is a growing concern, as exposure to minute quantities of anthropogenic forms of beryllium may lead to sensitization and to chronic beryllium disease, which can be fatal and for which no cure is currently known. Furthermore, there is no known exposure-response relationship with which to establish a 'safe' maximum level of beryllium exposure. As a result, the current trend is toward ever lower occupational exposure limits, which in turn make exposure assessment, both in terms of sampling and analysis, more challenging. The problems are exacerbated by difficulties in sample preparation for refractory forms of beryllium, such as beryllium oxide, and by indications that some beryllium forms may be more toxic than others. This chapter provides an overview of sources and uses of beryllium, health risks, and occupational exposure limits. It also provides a general overview of sampling, analysis, and data evaluation issues that will be explored in greater depth in the remaining chapters. The goal of this book is to provide a comprehensive resource to aid personnel in a wide variety of disciplines in selecting sampling and analysis methods that will facilitate informed decision-making in workplace and environmental settings.

  9. Sampling and Data Analysis for Environmental Microbiology

    SciTech Connect

    Murray, Christopher J.

    2001-06-01

    A brief review of the literature indicates the importance of statistical analysis in applied and environmental microbiology. Sampling designs are particularly important for successful studies, and it is highly recommended that researchers review their sampling design before heading to the laboratory or the field. Most statisticians have numerous stories of scientists who approached them after their study was complete only to have to tell them that the data they gathered could not be used to test the hypothesis they wanted to address. Once the data are gathered, a large and complex body of statistical techniques are available for analysis of the data. Those methods include both numerical and graphical techniques for exploratory characterization of the data. Hypothesis testing and analysis of variance (ANOVA) are techniques that can be used to compare the mean and variance of two or more groups of samples. Regression can be used to examine the relationships between sets of variables and is often used to examine the dependence of microbiological populations on microbiological parameters. Multivariate statistics provides several methods that can be used for interpretation of datasets with a large number of variables and to partition samples into similar groups, a task that is very common in taxonomy, but also has applications in other fields of microbiology. Geostatistics and other techniques have been used to examine the spatial distribution of microorganisms. The objectives of this chapter are to provide a brief survey of some of the statistical techniques that can be used for sample design and data analysis of microbiological data in environmental studies, and to provide some examples of their use from the literature.

  10. Nano-FTIR for Geochemical Sample Analysis

    NASA Astrophysics Data System (ADS)

    Dominguez, G.; McCleod, A.; Gainsforth, Z.; Keilmann, F.; Westphal, A.; Thiemens, M. H.; Basov, D.

    2014-12-01

    Infrared (IR) spectroscopy is considered by many to be the "gold standard" for chemical identification, providing a direct connection between chemical compounds found in the laboratory and those found in natural samples including remote astrophysical environments. However, a well known limitation of using conventional IR spectroscopy is its spatial resolution determined by the wavelength of IR photons. Thus, while other techniques such as XANES and micro-Raman are capable of limited functional group mapping at tens to hundreds of nanometers, their use is limited by accessibility (the need for synchrotron beamlines) or the need for intense irradiation conditions (Raman) that can lead to sample alteration. These limitations and the wealth of information that can be extracted from detailed studies of unique micron-sized samples brought back by recent sample return missions such as NASA's Stardust mission, have motivated the development of a novel infrared mapping technique that is capable of mapping the chemical functional properties of geochemical samples with submicron resolutions. Here we describe our nano-FTIR imaging and analysis technique that allows us to bypass diffraction limited sample imaging in the infrared. Here we show, for the first time, that 1) the combination of an atomic-force microscope (AFM) and laser can be used to obtain the FTIR-equivalent spectra on spatial scales that are much smaller than the wavelength of IR radiation used 2) this technique responds to subtle shifts in cation concentrations as evidenced by changes in the frequencies of phonons at sub-micron scales 3) this technique can be used to identify regions of crystalline and semi-crystalline materials as demonstrated in our analysis of a cometary dust grain Iris. This work has clear implications for interpretations of astronomical observations and adds a new technique for the non-destructive characterization of terrestrial and extraterrestrial samples.

  11. BACTERIOLOGICAL ANALYSIS WITH SAMPLING AND SAMPLE PRESERVATION SPECIFICS

    EPA Science Inventory

    Current federal regulations (40CFR 503) specify that under certain conditions treated municipal biosolids must be analyzed for fecal coliform or salmonellae. The regulations state that representative samples of biosolids must be collected and analyzed using standard methods. Th...

  12. Astrobiology Sample Analysis as a Design Driver

    NASA Technical Reports Server (NTRS)

    Cohen, Marc M.

    2001-01-01

    This effort supports the Astrobiology Objective 8 the Search for LIFE ON MARS PAST AND PRESENT -(Astrobiology Program Office, 1998, p.7). The essential trade analysis is between returning very small samples to the Earth while protecting them versus in situ analysis on Mars. Developing these explicit parameters encompasses design, instrumentation, system integration, human factors and surface operations for both alternatives. This allocation of capability approach incorporates a "humans and machines in the loop" model that recognizes that every exploration system involves both humans and automated systems. The question is where in the loop they occur whether on Earth, in the Mars Base, in the rover or creeping over the Mars surface.

  13. Miniaturization in sample treatment for environmental analysis.

    PubMed

    Ramos, L; Ramos, J J; Brinkman, U A Th

    2005-01-01

    The increasing demand for faster, more cost-effective and environmentally friendly analytical methods is a major incentive to improve the classical procedures used for sample treatment in environmental analysis. In most classical procedures, the use of rapid and powerful instrumental techniques for the final separation and detection of the analytes contrasts with the time-consuming and usually manual methods used for sample preparation, which slows down the total analytical process. The efforts made in this field in the past ten years have led to the adaptation of existing methods and the development of new techniques to save time and chemicals, and improve overall performance. One route has been to develop at-line or on-line and, frequently, automated systems. In these approaches, miniaturization has been a key factor in designing integrated analytical systems to provide higher sample throughput and/or unattended operation. Selected examples of novel developments in the field of miniaturized sample preparation for environmental analysis are used to evaluate the merits of the various techniques on the basis of published data on real-life analyses of trace-level organic pollutants. Perspectives and trends are briefly discussed.

  14. Analysis of particulates on tape lift samples

    NASA Astrophysics Data System (ADS)

    Moision, Robert M.; Chaney, John A.; Panetta, Chris J.; Liu, De-Ling

    2014-09-01

    Particle counts on tape lift samples taken from a hardware surface exceeded threshold requirements in six successive tests despite repeated cleaning of the surface. Subsequent analysis of the particle size distributions of the failed tests revealed that the handling and processing of the tape lift samples may have played a role in the test failures. In order to explore plausible causes for the observed size distribution anomalies, scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), and time-of-flight secondary ion mass spectrometry (ToF-SIMS) were employed to perform chemical analysis on collected particulates. SEM/EDX identified Na and S containing particles on the hardware samples in a size range identified as being responsible for the test failures. ToF-SIMS was employed to further examine the Na and S containing particulates and identified the molecular signature of sodium alkylbenzene sulfonates, a common surfactant used in industrial detergent. The root cause investigation suggests that the tape lift test failures originated from detergent residue left behind on the glass slides used to mount and transport the tape following sampling and not from the hardware surface.

  15. Mars Analogue Field Research and Sample Analysis

    NASA Astrophysics Data System (ADS)

    Foing, Bernard H.

    2016-07-01

    We describe results from the data analysis from a series of field research campaigns (ILEWG EuroMoonMars campaigns 2009 to 2016) in the Utah desert and in other extreme environments (Iceland, Eifel, La Reunion) relevant to habitability and astrobiology in Mars environments, and in order to help in the interpretation of Mars missions measurements from orbit (MEX, MRO) or from the surface (MER, MSL). We discuss results relevant to the scientific study of the habitability factors influenced by the properties of dust, organics, water history and the diagnostics and characterisation of microbial life. We also discuss perspectives for the preparation of future lander and sample return missions. We deployed at Mars Desert Research station, Utah, a suite of instruments and techniques including sample collection, context imaging from remote to local and microscale, drilling, spectrometers and life sensors. We analyzed how geological and geochemical evolution affected local parameters (mineralogy, organics content, environment variations) and the habitability and signature of organics and biota. We find high diversity in the composition of soil samples even when collected in close proximity, the low abundances of detectable PAHs and amino acids and the presence of biota of all three domains of life with significant heterogeneity. An extraordinary variety of putative extremophiles was observed. A dominant factor seems to be soil porosity and lower clay-sized particle content. A protocol was developed for sterile sampling, contamination issues, and the diagnostics of biodiversity via PCR and DGGE analysis in soils and rocks samples. We compare campaign results from 2009-2013 campaigns in Utah and other sites to new measurements concerning: the comparison between remote sensing and in-situ measurements; the study of minerals; the detection of organics and signs of life.

  16. Sampling and analysis of phloem sap.

    PubMed

    Dinant, Sylvie; Kehr, Julia

    2013-01-01

    The transport tubes of the phloem are essential for higher plants. They not only provide the route for the distribution of assimilates produced during photosynthesis from source to sink organs but also (re-) distribute mineral nutrients. Additionally, the phloem is essential for sending information between distant plant organs and steering developmental and defense processes. For example, flowering and tuberization time are controlled by phloem-mobile signals and important defense reactions on the whole plant level, like systemic acquired resistance or systemic gene silencing, are spread through the phloem. In addition, recent results demonstrate that also the allocation of mineral nutrients is coordinated by phloem mobile signaling molecules. However, in many studies the important analysis of phloem sap is neglected, probably because the content of sieve tubes is not easy to access. This chapter will describe the current methods for sampling and analysis of phloem sap in order to encourage researchers to include the analysis of this crucial compartment in their relevant studies.

  17. Characterisation of spilled oil samples: Purpose, sampling, analysis and interpretation

    SciTech Connect

    Butt, J.A.; Duckworth, D.F.; Perry, S.G.

    1986-01-01

    An updated version of Marine Pollution by Oil(l974), this book provides recommendations on the forensic analysis of petroleum derived pollutants fojuind in marine environments. It includes the many new methods developed since the first volume was published.

  18. SALI chemical analysis of provided samples

    NASA Technical Reports Server (NTRS)

    Becker, Christopher H.

    1993-01-01

    SRI has completed the chemical analysis of all the samples supplied by NASA. The final batch of four samples consisted of: one inch diameter MgF2 mirror, control 1200-ID-FL3; one inch diameter neat resin, PMR-15, AO171-IV-55, half exposed and half unexposed; one inch diameter chromic acid anodized, EOIM-3 120-47 aluminum disc; and AO-exposed and unexposed samples of fullerene extract material in powdered form, pressed into In foil for analysis. Chemical analyses of the surfaces were performed by the surface analysis by laser ionization (SALI) method. The analyses emphasize surface contamination or general organic composition. SALI uses nonselective photoionization of sputtered or desorbed atoms and molecules above but close (approximately one mm) to the surface, followed by time-of-flight (TOF) mass spectrometry. In these studies, we used laser-induced desorption by 5-ns pulse-width 355-nm light (10-100 mJ/sq cm) and single-photon ionization (SPI) by coherent 118-nm radiation (at approximately 5 x 10(exp 5) W/sq cm). SPI was chosen primarily for its ability to obtain molecular information, whereas multiphoton ionization (not used in the present studies) is intended primarily for elemental and small molecule information. In addition to these four samples, the Au mirror (EOIM-3 200-11, sample four) was depth profiled again. Argon ion sputtering was used together with photoionization with intense 355-nm radiation (35-ps pulsewidths). Depth profiles are similar to those reported earlier, showing reproducibility. No chromium was found in the sample above noise level; its presence could at most be at the trace level. Somewhat more Ni appears to be present in the Au layer in the unexposed side, indicating thermal diffusion without chemical enhancement. The result of the presence of oxygen is apparently to tie-up/draw out the Ni as an oxide at the surface. The exposed region has a brownish tint appearance to the naked eye.

  19. Microextraction sample preparation techniques in biomedical analysis.

    PubMed

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

    2014-11-01

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

  20. Transuranic waste characterization sampling and analysis plan

    SciTech Connect

    1994-12-31

    Los Alamos National Laboratory (the Laboratory) is located approximately 25 miles northwest of Santa Fe, New Mexico, situated on the Pajarito Plateau. Technical Area 54 (TA-54), one of the Laboratory`s many technical areas, is a radioactive and hazardous waste management and disposal area located within the Laboratory`s boundaries. The purpose of this transuranic waste characterization, sampling, and analysis plan (CSAP) is to provide a methodology for identifying, characterizing, and sampling approximately 25,000 containers of transuranic waste stored at Pads 1, 2, and 4, Dome 48, and the Fiberglass Reinforced Plywood Box Dome at TA-54, Area G, of the Laboratory. Transuranic waste currently stored at Area G was generated primarily from research and development activities, processing and recovery operations, and decontamination and decommissioning projects. This document was created to facilitate compliance with several regulatory requirements and program drivers that are relevant to waste management at the Laboratory, including concerns of the New Mexico Environment Department.

  1. High priority tank sampling and analysis report

    SciTech Connect

    Brown, T.M.

    1998-03-05

    In July 1993, the Defense Nuclear Facilities Safety Board (DNFSB) transmitted Recommendation 93-5 (Conway 1993) to the US Department of Energy (DOE). Recommendation 93-5 noted that there was insufficient tank waste technical information and the pace to obtain it was too slow to ensure that Hanford Site wastes could be safely stored, that associated operations could be conducted safely, and that future disposal data requirements could be met. In May 1996, the DOE issued Revision 1 of the Recommendation 93-5 Implementation Plan (DOE-RL 1996). The Implementation Plan revision presented a modified approach to achieve the original plan`s objectives. The approach concentrated on actions necessary to ensure that wastes can be safely stored, that operations can be safely conducted, and that timely characterization information for the tank waste Disposal Program could be obtained. The Implementation Plan proposed 28 High Priority tanks, which, if sampled and analyzed, were expected to provide information to answer questions regarding safety and disposal issues. The High Priority tank list was originally developed in Section 9.0 of the Tank Waste Characterization Basis (Brown et al. 1995) by integrating the needs of the various safety and disposal programs. The High Priority tank list represents a set of tanks that were expected to provide the highest information return for characterization resources expended. The High Priority tanks were selected for near-term core sampling and were not expected to be the only tanks that would provide meaningful information. Sampling and analysis of non-High Priority tanks also could be used to provide scientific and technical data to confirm assumptions, calibrate models, and measure safety related phenomenological characteristics of the waste. When the sampling and analysis results of the High Priority and other tanks were reviewed, it was expected that a series of questions should be answered allowing key decisions to be made. The first

  2. AFCI Options Study

    SciTech Connect

    R. Wigeland; T. Taiwo; M. Todosow; W. Halsey; J. Gehin

    2009-09-01

    This report describes the background and framework for both organizing the discussion and providing information on the potential for nuclear energy R&D to develop alternative nuclear fuel cycles that would address the issues with the current implementations of nuclear power, including nuclear waste disposal, proliferation risk, safety, security, economics, and sustainability. The disposition of used fuel is the cause of many of the concerns, and the possible approaches to used fuel management identify a number of basic technology areas that need to be considered. The basic science in each of the technology areas is discussed, emphasizing what science is currently available, where scientific knowledge may be insufficient, and especially to identify specific areas where transformational discoveries may allow achievement of performance goals not currently attainable. These discussions lead to the wide range of technical options that have been the basis for past and current research and development on advanced nuclear fuel cycles in the United States. The results of this work are then briefly reviewed to show the extent to which such approaches are capable of addressing the issues with nuclear power, the potential for moving further, and the inherent limitations.

  3. Analysis of Returned Comet Nucleus Samples

    NASA Astrophysics Data System (ADS)

    Chang, Sherwood

    1997-12-01

    This volume contains abstracts that have been accepted by the Program Committee for presentation at the Workshop on Analysis of Returned Comet Nucleus Samples, held in Milpitas, California, January 16-18, 1989. Conveners are Sherwood Chang (NASA Ames Research Center) and Larry Nyquist (NASA Johnson Space Center). Program Committee members are Thomas Ahrens (ex-officio; California Institute of Technology), Lou Allamandola (NASA Ames Research Center), David Blake (NASA Ames Research Center), Donald Brownlee (University of Washington, Seattle), Theodore E. Bunch (NASA Ames Research Center), Humberto Campins (Planetary Science Institute), Jeff Cuzzi (NASA Ames Research Center), Eberhard Griin (Max-Plank-Institut fiir Kemphysik), Martha Hanner (Jet Propulsion Laboratory), Alan Harris (Jet Propulsion Laboratory), John Kerrid-e (University of Califomia, Los Angeles), Yves Langevin (University of Paris), Gerhard Schwehm (ESTEC), and Paul Weissman (Jet Propulsion Laboratory). Logistics and administrative support for the workshop were provided by the Lunar and Planetary Institute Projects Office.

  4. Analysis of Returned Comet Nucleus Samples

    NASA Technical Reports Server (NTRS)

    Chang, Sherwood (Compiler)

    1997-01-01

    This volume contains abstracts that have been accepted by the Program Committee for presentation at the Workshop on Analysis of Returned Comet Nucleus Samples, held in Milpitas, California, January 16-18, 1989. Conveners are Sherwood Chang (NASA Ames Research Center) and Larry Nyquist (NASA Johnson Space Center). Program Committee members are Thomas Ahrens (ex-officio; California Institute of Technology), Lou Allamandola (NASA Ames Research Center), David Blake (NASA Ames Research Center), Donald Brownlee (University of Washington, Seattle), Theodore E. Bunch (NASA Ames Research Center), Humberto Campins (Planetary Science Institute), Jeff Cuzzi (NASA Ames Research Center), Eberhard Griin (Max-Plank-Institut fiir Kemphysik), Martha Hanner (Jet Propulsion Laboratory), Alan Harris (Jet Propulsion Laboratory), John Kerrid-e (University of Califomia, Los Angeles), Yves Langevin (University of Paris), Gerhard Schwehm (ESTEC), and Paul Weissman (Jet Propulsion Laboratory). Logistics and administrative support for the workshop were provided by the Lunar and Planetary Institute Projects Office.

  5. Sample Analysis at Mars Instrument Simulator

    NASA Technical Reports Server (NTRS)

    Benna, Mehdi; Nolan, Tom

    2013-01-01

    The Sample Analysis at Mars Instrument Simulator (SAMSIM) is a numerical model dedicated to plan and validate operations of the Sample Analysis at Mars (SAM) instrument on the surface of Mars. The SAM instrument suite, currently operating on the Mars Science Laboratory (MSL), is an analytical laboratory designed to investigate the chemical and isotopic composition of the atmosphere and volatiles extracted from solid samples. SAMSIM was developed using Matlab and Simulink libraries of MathWorks Inc. to provide MSL mission planners with accurate predictions of the instrument electrical, thermal, mechanical, and fluid responses to scripted commands. This tool is a first example of a multi-purpose, full-scale numerical modeling of a flight instrument with the purpose of supplementing or even eliminating entirely the need for a hardware engineer model during instrument development and operation. SAMSIM simulates the complex interactions that occur between the instrument Command and Data Handling unit (C&DH) and all subsystems during the execution of experiment sequences. A typical SAM experiment takes many hours to complete and involves hundreds of components. During the simulation, the electrical, mechanical, thermal, and gas dynamics states of each hardware component are accurately modeled and propagated within the simulation environment at faster than real time. This allows the simulation, in just a few minutes, of experiment sequences that takes many hours to execute on the real instrument. The SAMSIM model is divided into five distinct but interacting modules: software, mechanical, thermal, gas flow, and electrical modules. The software module simulates the instrument C&DH by executing a customized version of the instrument flight software in a Matlab environment. The inputs and outputs to this synthetic C&DH are mapped to virtual sensors and command lines that mimic in their structure and connectivity the layout of the instrument harnesses. This module executes

  6. DWPF GC FILTER ASSEMBLY SAMPLING AND ANALYSIS

    SciTech Connect

    Bannochie, C.; Imrich, K.

    2009-11-11

    On March 18, 2009 a Defense Waste Processing Facility (DWPF) GC Line Filter Assembly was received at the Savannah River National Laboratory (SRNL). This filter assembly was removed from operation following the completion of Sludge Batch 4 processing in the DWPF. Work on this sample was requested in a Technical Assistance Request. This document reports the pictures, observations, samples collected, and analytical results for the assembly. The assembly arrived at SRNL separated into its three component filters: high efficiency particulate air (HEPA)-1, HEPA-2, and a high efficiency mist evaporator (HEME). Each stage of the assembly's media was sampled and examined visually and by scanning electron microscopy (SEM). Solids built up in the filter housing following the first stage HEME, were dissolved in dilute nitric acid and analyzed by ICP-AES and the undissolved white solids were analyzed by x-ray diffraction (XRD). The vast majority of the material in each of the three stages of the DWPF GC Line Filter Assembly appears to be contaminated with a Hg compound that is {approx}59 wt% Hg on a total solids basis. The Hg species was identified by XRD analysis to contain a mixture of Hg{sub 4}(OH)(NO{sub 3}){sub 3} and Hg{sub 10}(OH){sub 4}(NO{sub 3}){sub 6}. Only in the core sample of the second stage HEPA, did this material appear to be completely covering portions of the filter media, possibly explaining the pressure drops observed by DWPF. The fact that the material migrates through the HEME filter and both HEPA filters, and that it was seen collecting on the outlet side of the HEME filter, would seem to indicate that these filters are not efficient at removing this material. Further SRAT off-gas system modeling should help determine the extent of Hg breakthrough past the Mercury Water Wash Tank (MWWT). The SRAT off-gas system has not been modeled since startup of the facility. Improvements to the efficiency of Hg stripping prior to the ammonia scrubber would seem to be

  7. Preparation of urine samples for proteomic analysis.

    PubMed

    Pieper, Rembert

    2008-01-01

    Reproducible procedures for the preparation of protein samples isolated from human urine are essential for meaningful proteomic analyses. Key applications are the discovery of novel proteins or their modifications in the human urine as well as protein biomarker discovery for diseases and drug treatments. The methodology presented here features experimental steps aimed at limiting protein losses because of organic solvent precipitation, effective separation of proteins from other compounds in the human urine and molecular weight-based enrichment of proteins in two distinct fractions. Urinary proteins are separated from cellular debris in the urine via centrifugation, concentrated with 5-kDa-cutoff membrane concentration devices and separated via size exclusion chromatography into fractions with a higher and a lower molecular weight than 30 kDa, respectively. A successive optional affinity removal step for highly abundant plasma proteins is described. Finally, buffer exchange steps useful for specific downstream proteomic analysis experiments of urinary proteins are presented, such as 2-dimensional gel electrophoresis, differential protein or peptide labeling and digestion with trypsin for LC-MS/MS analysis.

  8. Organically bound tritium analysis in environmental samples

    SciTech Connect

    Baglan, N.; Cossonnet, C.; Fournier, M.; Momoshima, N.; Ansoborlo, E.

    2015-03-15

    Organically bound tritium (OBT) has become of increased interest within the last decade, with a focus on its behaviour and also its analysis, which are important to assess tritium distribution in the environment. In contrast, there are no certified reference materials and no standard analytical method through the international organization related to OBT. In order to resolve this issue, an OBT international working group was created in May 2012. Over 20 labs from around the world participated and submitted their results for the first intercomparison exercise results on potato (Sep 2013). The samples, specially-prepared potatoes, were provided in March 2013 to each participant. Technical information and results from this first exercise are discussed here for all the labs which have realised the five replicates necessary to allow a reliable statistical treatment. The results are encouraging as the increased number of participating labs did not degrade the observed dispersion of the results for a similar activity level. Therefore, the results do not seem to depend on the analytical procedure used. From this work an optimised procedure can start to be developed to deal with OBT analysis and will guide subsequent planned OBT trials by the international group.

  9. 40 CFR 761.292 - Chemical extraction and analysis of individual samples and composite samples.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... individual samples and composite samples. 761.292 Section 761.292 Protection of Environment ENVIRONMENTAL....61(a)(6) § 761.292 Chemical extraction and analysis of individual samples and composite samples. Use... individual and composite samples of PCB remediation waste. Use Method 8082 from SW-846, or a method...

  10. 40 CFR 761.292 - Chemical extraction and analysis of individual samples and composite samples.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... individual samples and composite samples. 761.292 Section 761.292 Protection of Environment ENVIRONMENTAL....61(a)(6) § 761.292 Chemical extraction and analysis of individual samples and composite samples. Use... individual and composite samples of PCB remediation waste. Use Method 8082 from SW-846, or a method...

  11. 40 CFR 761.292 - Chemical extraction and analysis of individual samples and composite samples.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... individual samples and composite samples. 761.292 Section 761.292 Protection of Environment ENVIRONMENTAL....61(a)(6) § 761.292 Chemical extraction and analysis of individual samples and composite samples. Use... individual and composite samples of PCB remediation waste. Use Method 8082 from SW-846, or a method...

  12. Europlanet Research Infrastructure: Planetary Sample Analysis Facilities

    NASA Astrophysics Data System (ADS)

    Cloquet, C.; Mason, N. J.; Davies, G. R.; Marty, B.

    2008-09-01

    EuroPlanet The Europlanet Research Infrastructure consortium funded under FP7 aims to provide the EU Planetary Science community greater access for to research infrastructure. A series of networking and outreach initiatives will be complimented by joint research activities and the formation of three Trans National Access distributed service laboratories (TNA's) to provide a unique and comprehensive set of analogue field sites, laboratory simulation facilities, and extraterrestrial sample analysis tools. Here we report on the infrastructure that comprises the third TNA: Planetary Sample Analysis Facilities. The modular infrastructure represents a major commitment of analytical instrumentation by three institutes and together forms a state-of-the-art analytical facility of unprecedented breadth. These centres perform research in the fields of geochemistry and cosmochemistry, studying fluids and rocks in order to better understand the keys cof the universe. Europlanet Research Infrastructure Facilities: Ion Probe facilities at CRPG and OU The Cameca 1270 Ion microprobe is a CNRS-INSU national facility. About a third of the useful analytical time of the ion probe (about 3 months each year) is allocated to the national community. French scientists have to submit their projects to a national committee for selection. The selected projects are allocated time in the following 6 months twice a year. About 15 to 20 projects are run each year. There are only two such instruments in Europe, with cosmochemistry only performed at CRPG. Different analyses can be performed on a routine basis, such as U-Pb dating on Zircon, Monazite or Pechblende, Li, B, C, O, Si isotopic ratios determination on different matrix, 26Al, 60Fe extinct radioactivity ages, light and trace elements contents . The NanoSIMS 50L - producing element or isotope maps with a spatial resolution down to ≈50nm. This is one of the cornerstone facilities of UKCAN, with 75% of available instrument time funded and

  13. Using Inverse Probability Bootstrap Sampling to Eliminate Sample Induced Bias in Model Based Analysis of Unequal Probability Samples.

    PubMed

    Nahorniak, Matthew; Larsen, David P; Volk, Carol; Jordan, Chris E

    2015-01-01

    In ecology, as in other research fields, efficient sampling for population estimation often drives sample designs toward unequal probability sampling, such as in stratified sampling. Design based statistical analysis tools are appropriate for seamless integration of sample design into the statistical analysis. However, it is also common and necessary, after a sampling design has been implemented, to use datasets to address questions that, in many cases, were not considered during the sampling design phase. Questions may arise requiring the use of model based statistical tools such as multiple regression, quantile regression, or regression tree analysis. However, such model based tools may require, for ensuring unbiased estimation, data from simple random samples, which can be problematic when analyzing data from unequal probability designs. Despite numerous method specific tools available to properly account for sampling design, too often in the analysis of ecological data, sample design is ignored and consequences are not properly considered. We demonstrate here that violation of this assumption can lead to biased parameter estimates in ecological research. In addition, to the set of tools available for researchers to properly account for sampling design in model based analysis, we introduce inverse probability bootstrapping (IPB). Inverse probability bootstrapping is an easily implemented method for obtaining equal probability re-samples from a probability sample, from which unbiased model based estimates can be made. We demonstrate the potential for bias in model-based analyses that ignore sample inclusion probabilities, and the effectiveness of IPB sampling in eliminating this bias, using both simulated and actual ecological data. For illustration, we considered three model based analysis tools--linear regression, quantile regression, and boosted regression tree analysis. In all models, using both simulated and actual ecological data, we found inferences to be

  14. Using Inverse Probability Bootstrap Sampling to Eliminate Sample Induced Bias in Model Based Analysis of Unequal Probability Samples

    PubMed Central

    Nahorniak, Matthew

    2015-01-01

    In ecology, as in other research fields, efficient sampling for population estimation often drives sample designs toward unequal probability sampling, such as in stratified sampling. Design based statistical analysis tools are appropriate for seamless integration of sample design into the statistical analysis. However, it is also common and necessary, after a sampling design has been implemented, to use datasets to address questions that, in many cases, were not considered during the sampling design phase. Questions may arise requiring the use of model based statistical tools such as multiple regression, quantile regression, or regression tree analysis. However, such model based tools may require, for ensuring unbiased estimation, data from simple random samples, which can be problematic when analyzing data from unequal probability designs. Despite numerous method specific tools available to properly account for sampling design, too often in the analysis of ecological data, sample design is ignored and consequences are not properly considered. We demonstrate here that violation of this assumption can lead to biased parameter estimates in ecological research. In addition, to the set of tools available for researchers to properly account for sampling design in model based analysis, we introduce inverse probability bootstrapping (IPB). Inverse probability bootstrapping is an easily implemented method for obtaining equal probability re-samples from a probability sample, from which unbiased model based estimates can be made. We demonstrate the potential for bias in model-based analyses that ignore sample inclusion probabilities, and the effectiveness of IPB sampling in eliminating this bias, using both simulated and actual ecological data. For illustration, we considered three model based analysis tools—linear regression, quantile regression, and boosted regression tree analysis. In all models, using both simulated and actual ecological data, we found inferences to be

  15. Tank 241-TY-103 rotary core sampling and analysis

    SciTech Connect

    Jo, J.

    1995-10-30

    This Sampling and Analysis Plan (SAP) identifies characterization objectives pertaining to sample collection, laboratory analytical evaluation, and reporting requirements for two rotary-mode core samples from tank 241-TY-103

  16. Sampling and analysis plan for canister liquid and gas sampling at 105 KW fuel storage basin

    SciTech Connect

    Trimble, D.J.

    1996-08-09

    This Sampling and Analysis Plan describes the equipment,procedures and techniques for obtaining gas and liquid samples from sealed K West fuel canisters. The analytical procedures and quality assurance requirements for the subsequent laboratory analysis of the samples are also discussed.

  17. Techniques for geothermal liquid sampling and analysis

    SciTech Connect

    Kindle, C.H.; Woodruff, E.M.

    1981-07-01

    A methodology has been developed that is particularly suited to liquid-dominated resources and adaptable to a variety of situations. It is intended to be a base methodology upon which variations can be made to meet specific needs or situations. The approach consists of recording flow conditions at the time of sampling, a specific insertable probe sampling system, a sample stabilization procedure, commercially available laboratory instruments, and data quality check procedures.

  18. Prompt Gamma Ray Analysis of Soil Samples

    SciTech Connect

    Naqvi, A.A.; Khiari, F.Z.; Haseeb, S.M.A.; Hussein, Tanvir; Khateeb-ur-Rehman; Isab, A.H.

    2015-07-01

    Neutron moderation effects were measured in bulk soil samples through prompt gamma ray measurements from water and benzene contaminated soil samples using 14 MeV neutron inelastic scattering. The prompt gamma rays were measured using a cylindrical 76 mm x 76 mm (diameter x height) LaBr{sub 3}:Ce detector. Since neutron moderation effects strongly depend upon hydrogen concentration of the sample, for comparison purposes, moderation effects were studied from samples containing different hydrogen concentrations. The soil samples with different hydrogen concentration were prepared by mixing soil with water as well as benzene in different weight proportions. Then, the effects of increasing water and benzene concentrations on the yields of hydrogen, carbon and silicon prompt gamma rays were measured. Moderation effects are more pronounced in soil samples mixed with water as compared to those from soil samples mixed with benzene. This is due to the fact that benzene contaminated soil samples have about 30% less hydrogen concentration by weight than the water contaminated soil samples. Results of the study will be presented. (authors)

  19. Colling Wipe Samples for VX Analysis

    SciTech Connect

    Koester, C; Hoppes, W G

    2010-02-11

    This standard operating procedure (SOP) provides uniform procedures for the collection of wipe samples of VX residues from surfaces. Personnel may use this procedure to collect and handle wipe samples in the field. Various surfaces, including building materials (wood, metal, tile, vinyl, etc.) and equipment, may be sampled based on this procedure. The purpose of such sampling is to determine whether or not the relevant surfaces are contaminated, to determine the extent of their contamination, to evaluate the effectiveness of decontamination procedures, and to determine the amount of contaminant that might present as a contact hazard.

  20. Space X First Entry Sample Analysis

    NASA Technical Reports Server (NTRS)

    James, John T.

    2012-01-01

    The toxicological assessment of one sample collected on May 26, 2012 and returned to earth on May 31, 2012 was analyzed for pollutants that had offgassed into the Dragon capsule by the time of first entry operations performed by the ISS crew. The components identified in the first-entry sample and their contributions to the total T-value are shown.

  1. 7 CFR 58.245 - Method of sample analysis.

    Code of Federal Regulations, 2013 CFR

    2013-01-01

    ... 7 Agriculture 3 2013-01-01 2013-01-01 false Method of sample analysis. 58.245 Section 58.245... Procedures § 58.245 Method of sample analysis. Samples shall be tested according to the applicable methods of laboratory analysis contained in either DA Instruction 918-RL as issued by the USDA, Agricultural...

  2. 7 CFR 58.812 - Methods of sample analysis.

    Code of Federal Regulations, 2013 CFR

    2013-01-01

    ... 7 Agriculture 3 2013-01-01 2013-01-01 false Methods of sample analysis. 58.812 Section 58.812... Procedures § 58.812 Methods of sample analysis. Samples shall be tested according to the applicable methods of laboratory analysis contained in either DA Instruction 918-RL, as issued by the USDA,...

  3. 7 CFR 58.812 - Methods of sample analysis.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... 7 Agriculture 3 2010-01-01 2010-01-01 false Methods of sample analysis. 58.812 Section 58.812... Procedures § 58.812 Methods of sample analysis. Samples shall be tested according to the applicable methods of laboratory analysis contained in either DA Instruction 918-RL, as issued by the USDA,...

  4. 7 CFR 58.245 - Method of sample analysis.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... 7 Agriculture 3 2010-01-01 2010-01-01 false Method of sample analysis. 58.245 Section 58.245... Procedures § 58.245 Method of sample analysis. Samples shall be tested according to the applicable methods of laboratory analysis contained in either DA Instruction 918-RL as issued by the USDA, Agricultural...

  5. Developments in Sampling and Analysis Instrumentation for Stationary Sources

    ERIC Educational Resources Information Center

    Nader, John S.

    1973-01-01

    Instrumentation for the measurement of pollutant emissions is considered including sample-site selection, sample transport, sample treatment, sample analysis, and data reduction, display, and interpretation. Measurement approaches discussed involve sample extraction from within the stack and electro-optical methods. (BL)

  6. Lab Analysis of Dust Wipe Samples

    EPA Pesticide Factsheets

    Dust wipe samples collected on residential properties near the fenceline of KCBX North and South Terminals in Chicago, which store and handle pet coke, were analyzed for polycyclic aromatic hydrocarbons (PAHs) and trace metals and minerals.

  7. LABORATORY GUIDELINES FOR ANALYSIS OF BIOTERRORISM SAMPLES

    EPA Science Inventory

    With advent of deaths associated with Bacillus anthracis spore contaminated mail, a worldwide need was apparent for increased laboratory capacity to safely analyze bioterrorism samples. The U.S. Department of Health and Human Services has furnished guidelines for microbiological...

  8. WRAP Module 1 sampling and analysis plan

    SciTech Connect

    Mayancsik, B.A.

    1995-03-24

    This document provides the methodology to sample, screen, and analyze waste generated, processed, or otherwise the responsibility of the Waste Receiving and Processing Module 1 facility. This includes Low-Level Waste, Transuranic Waste, Mixed Waste, and Dangerous Waste.

  9. POTW Sludge Sampling and Analysis Guidance Document

    EPA Pesticide Factsheets

    In view of the variability of municipal sludge quality,appropriate procedures must be followed to collect and analyze samples that accurately represent each POTW's sludge quality.This manual was developed to provide that guidance to POTW operators, engin

  10. [Variance estimation considering multistage sampling design in multistage complex sample analysis].

    PubMed

    Li, Yichong; Zhao, Yinjun; Wang, Limin; Zhang, Mei; Zhou, Maigeng

    2016-03-01

    Multistage sampling is a frequently-used method in random sampling survey in public health. Clustering or independence between observations often exists in the sampling, often called complex sample, generated by multistage sampling. Sampling error may be underestimated and the probability of type I error may be increased if the multistage sample design was not taken into consideration in analysis. As variance (error) estimator in complex sample is often complicated, statistical software usually adopt ultimate cluster variance estimate (UCVE) to approximate the estimation, which simply assume that the sample comes from one-stage sampling. However, with increased sampling fraction of primary sampling unit, contribution from subsequent sampling stages is no more trivial, and the ultimate cluster variance estimate may, therefore, lead to invalid variance estimation. This paper summarize a method of variance estimation considering multistage sampling design. The performances are compared with UCVE and the method considering multistage sampling design by simulating random sampling under different sampling schemes using real world data. Simulation showed that as primary sampling unit (PSU) sampling fraction increased, UCVE tended to generate increasingly biased estimation, whereas accurate estimates were obtained by using the method considering multistage sampling design.

  11. COMPOSITE SAMPLING FOR SOIL VOC ANALYSIS

    EPA Science Inventory

    Data published by numerous researchers over the last decade demonstrate that there is a high degree of spatial variability in the measurement of volatile organic compounds (VOCs) in soil at contaminated waste sites. This phenomenon is confounded by the use of a small sample aliqu...

  12. Trace Element Analysis of Biological Samples.

    ERIC Educational Resources Information Center

    Veillon, Claude

    1986-01-01

    Reviews background of atomic absorption spectrometry techniques. Discusses problems encountered and precautions to be taken in determining trace elements in the parts-per-billion concentration range and below. Concentrates on determining chromium in biological samples by graphite furnace atomic absorption. Considers other elements, matrices, and…

  13. LABORATORY GUIDELINES FOR ANALYSIS OF BIOTERRORISM SAMPLES

    EPA Science Inventory

    After the attack on the World Trade Center on September 11, 2002, and the subsequent deaths associated with Bacillus anthracis spore contaminated mail, a worldwide need was apparent for increased laboratory capacity to safely analyze bioterrorism samples. The U.S. Department o...

  14. Analysis of large soil samples for actinides

    DOEpatents

    Maxwell, III; Sherrod L.

    2009-03-24

    A method of analyzing relatively large soil samples for actinides by employing a separation process that includes cerium fluoride precipitation for removing the soil matrix and precipitates plutonium, americium, and curium with cerium and hydrofluoric acid followed by separating these actinides using chromatography cartridges.

  15. UMTRA water sampling and analysis plan, Tuba City, Arizona. Draft

    SciTech Connect

    Not Available

    1993-09-01

    The purpose of this document is to provide background, guidance, and justification for fiscal year (FY) 1994 water sampling activities for the uranium mil tailings site at Tuba City, Arizona. This sampling and analysis plan will form the basis for groundwater sampling and analysis work orders to be implemented in FY94.

  16. 27 CFR 26.192 - Samples and analysis.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 27 Alcohol, Tobacco Products and Firearms 1 2012-04-01 2012-04-01 false Samples and analysis. 26.192 Section 26.192 Alcohol, Tobacco Products and Firearms ALCOHOL AND TOBACCO TAX AND TRADE BUREAU... Samples and analysis. The chemist of the Treasury of Puerto Rico may take samples of the product to...

  17. Ozone data and mission sampling analysis

    NASA Technical Reports Server (NTRS)

    Robbins, J. L.

    1980-01-01

    A methodology was developed to analyze discrete data obtained from the global distribution of ozone. Statistical analysis techniques were applied to describe the distribution of data variance in terms of empirical orthogonal functions and components of spherical harmonic models. The effects of uneven data distribution and missing data were considered. Data fill based on the autocorrelation structure of the data is described. Computer coding of the analysis techniques is included.

  18. UMTRA water sampling and analysis plan, Green River, Utah

    SciTech Connect

    Papusch, R.

    1993-12-01

    The purpose of this water sampling and analysis plan (WSAP) is to provide a basis for groundwater and surface water sampling at the Green River Uranium Mill Tailing Remedial Action (UMTRA) Project site. This WSAP identifies and justifies the sampling locations, analytical parameters, detection limits, and sampling frequency for the monitoring locations.

  19. Waste minimization in environmental sampling and analysis

    SciTech Connect

    Brice, D.A.; Nixon, J. . Fernald Environmental Management Project); Lewis, E.T. )

    1992-01-01

    Environmental investigations of the extent and effect of contamination, and projects to remediate such contamination, are designed to mitigate perceived threats to human health and the environment. During the course of these investigations, excavations, borings, and monitoring wells are constructed: monitoring wells are developed and purged prior to sampling; samples are collected; equipment is decontaminated; constituents extracted and analyzed; and personal protective equipment is used to keep workers safe. All of these activities generate waste. A large portion of this waste may be classified as hazardous based on characteristics or constituent components. Waste minimization is defined as reducing the volume and/or toxicity of waste generated by a process. Waste minimization has proven to be an effective means of cost reduction and improving worker health, safety, and environmental awareness in the industrial workplace through pollution prevention. Building waste minimization goals into a project during the planning phase is both cost effective and consistent with total quality management principles. Application of waste minimization principles should be an integral part of the planning and conduct of environmental investigations. Current regulatory guidance on planning environmental investigations focuses on data quality and risk assessment objectives. Waste minimization should also be a scoping priority, along with meeting worker protection requirements, protection of human health and the environment, and achieving data quality objectives. Waste volume or toxicity can be reduced through the use of smaller sample sizes, less toxic extraction solvents, less hazardous decontamination materials, smaller excavations and borings, smaller diameter monitoring wells, dedicated sampling equipment, well-fitting personal protective equipment, judicious use of screening technologies, and analyzing only for parameters of concern.

  20. Waste minimization in environmental sampling and analysis

    SciTech Connect

    Brice, D.A.; Nixon, J.; Lewis, E.T.

    1992-03-01

    Environmental investigations of the extent and effect of contamination, and projects to remediate such contamination, are designed to mitigate perceived threats to human health and the environment. During the course of these investigations, excavations, borings, and monitoring wells are constructed: monitoring wells are developed and purged prior to sampling; samples are collected; equipment is decontaminated; constituents extracted and analyzed; and personal protective equipment is used to keep workers safe. All of these activities generate waste. A large portion of this waste may be classified as hazardous based on characteristics or constituent components. Waste minimization is defined as reducing the volume and/or toxicity of waste generated by a process. Waste minimization has proven to be an effective means of cost reduction and improving worker health, safety, and environmental awareness in the industrial workplace through pollution prevention. Building waste minimization goals into a project during the planning phase is both cost effective and consistent with total quality management principles. Application of waste minimization principles should be an integral part of the planning and conduct of environmental investigations. Current regulatory guidance on planning environmental investigations focuses on data quality and risk assessment objectives. Waste minimization should also be a scoping priority, along with meeting worker protection requirements, protection of human health and the environment, and achieving data quality objectives. Waste volume or toxicity can be reduced through the use of smaller sample sizes, less toxic extraction solvents, less hazardous decontamination materials, smaller excavations and borings, smaller diameter monitoring wells, dedicated sampling equipment, well-fitting personal protective equipment, judicious use of screening technologies, and analyzing only for parameters of concern.

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

    NASA Technical Reports Server (NTRS)

    Sarrazin, P.; Chipera, S.; Bish, D.; Blake, D.; Feldman, S.; Vaniman, D.; Bryson, C.

    2004-01-01

    Sample preparation and sample handling are among the most critical operations associated with X-ray diffraction (XRD) analysis. These operations require attention in a laboratory environment, but they become a major constraint in the deployment of XRD instruments for robotic planetary exploration. We are developing a novel sample handling system that dramatically relaxes the constraints on sample preparation by allowing characterization of coarse-grained material that would normally be impossible to analyze with conventional powder-XRD techniques.

  2. Exomars 2018 Rover Pasteur Payload Sample Analysis

    NASA Astrophysics Data System (ADS)

    Debus, Andre; Bacher, M.; Ball, A.; Barcos, O.; Bethge, B.; Gaubert, F.; Haldemann, A.; Kminek, G.; Lindner, R.; Pacros, A.; Rohr, T.; Trautner, R.; Vago, J.

    The ExoMars programme is a joint ESA-NASA program having exobiology as one of the key science objectives. It is divided into 2 missions: the first mission is ESA-led with an ESA orbiter and an ESA Entry, Descent and Landing (EDL) demonstrator, launched in 2016 by NASA, and the second mission is NASA-led, launched in 2018 by NASA including an ESA rover and a NASA rover both deployed by a single NASA EDL system. For ESA, the ExoMars programme will demonstrate key flight and in situ enabling technologies in support of the European ambitions for future exploration missions, as outlined in the Aurora Declaration. The ExoMars 2018 ESA Rover will carry a comprehensive and coherent suite of analytical instruments dedicated to exobiology and geology research: the Pasteur Payload (PPL). This payload includes a selection of complementary instruments, having the following goals: to search for signs of past and present life on Mars and to investigate the water/geochemical environment as a function of depth in the shallow subsurface. The ExoMars Rover will travel several kilometres searching for sites warranting further investigation. The Rover includes a drill and a Sample Preparation and Distribution System which will be used to collect and analyse samples from within outcrops and from the subsurface. The Rover systems and instruments, in particular those located inside the Analytical Laboratory Drawer must meet many stringent requirements to be compatible with exobiologic investigations: the samples must be maintained in a cold and uncontaminated environment, requiring sterile and ultraclean preparation of the instruments, to preserve volatile materials and to avoid false positive results. The value of the coordinated observations suggests that a significant return on investment is to be expected from this complex development. We will present the challenges facing the ExoMars PPL, and the plans for sending a robust exobiology laboratory to Mars in 2018.

  3. Asbestos Workshop: Sampling, Analysis, and Risk Assessment

    DTIC Science & Technology

    2012-03-01

    fibrosis (fibrosis of the lining of the cavity holding the lungs) EMDQ March 2012 Chest x - ray showing areas of scarring related to asbestosis. 8...soil) •If the expected number of asbestos structures in a sample is λ, then the probability that there are exactly x asbestos fibers is equal to: •E.g...Estimating Risk for Asbestos Risk = Exposure x Toxicity = [Air] × ET × EF × IUR = f/cm3× hour/hour × day/day × (f/cm3)-1 For asbestos , ED is

  4. Analysis of a Suspected Drug Sample

    ERIC Educational Resources Information Center

    Schurter, Eric J.; Zook-Gerdau, Lois Anne; Szalay, Paul

    2011-01-01

    This general chemistry laboratory uses differences in solubility to separate a mixture of caffeine and aspirin while introducing the instrumental analysis methods of GCMS and FTIR. The drug mixture is separated by partitioning aspirin and caffeine between dichloromethane and aqueous base. TLC and reference standards are used to identify aspirin…

  5. Neutron activation analysis for antimetabolites. [in food samples

    NASA Technical Reports Server (NTRS)

    1973-01-01

    Determination of metal ion contaminants in food samples is studied. A weighed quantity of each sample was digested in a concentrated mixture of nitric, hydrochloric and perchloric acids to affect complete solution of the food products. The samples were diluted with water and the pH adjusted according to the specific analysis performed. The samples were analyzed by neutron activation analysis, polarography, and atomic absorption spectrophotometry. The solid food samples were also analyzed by neutron activation analysis for increased sensitivity and lower levels of detectability. The results are presented in tabular form.

  6. Modified electrokinetic sample injection method in chromatography and electrophoresis analysis

    DOEpatents

    Davidson, J. Courtney; Balch, Joseph W.

    2001-01-01

    A sample injection method for horizontal configured multiple chromatography or electrophoresis units, each containing a number of separation/analysis channels, that enables efficient introduction of analyte samples. This method for loading when taken in conjunction with horizontal microchannels allows much reduced sample volumes and a means of sample stacking to greatly reduce the concentration of the sample. This reduction in the amount of sample can lead to great cost savings in sample preparation, particularly in massively parallel applications such as DNA sequencing. The essence of this method is in preparation of the input of the separation channel, the physical sample introduction, and subsequent removal of excess material. By this method, sample volumes of 100 nanoliter to 2 microliters have been used successfully, compared to the typical 5 microliters of sample required by the prior separation/analysis method.

  7. ENVIRONMENTAL SAMPLING AND ANALYSIS - GETTING IT RIGHT

    SciTech Connect

    CONNELL CW

    2008-01-22

    The Department of Energy's Hanford Site in southeastern Washington State was established in the 1940s as part of the Manhattan Project. Hanford's role was to produce weapons-grade nuclear material for defense, and by 1989, when the Site's mission changed from operations to cleanup, Hanford had produced more than 60 percent of the nation's plutonium. The legacy of Hanford's production years is enormous in terms of nuclear and hazardous waste, especially the 270 billion gallons of contaminated groundwater and the 5 million cubic yards of contaminated soil. Managing the contaminated soil and groundwater are particularly important because the Columbia River, the lifeblood of the northwest and the nation's eighth largest river, bounds the Site. Fluor Hanford's Soil & Groundwater Remediation Project (S&GRP) integrates all of the activities that deal with remediating and monitoring the groundwater across the Site. The S&GRP uses a detailed series of steps to record, track, and verify information. The Sample and Data Management (SDM) Process consists of 10 integrated steps that start with the data quality objectives process that establishes the mechanism for collecting the right information with the right people. The process ends with data quality assessment, which is used to ensure that all quantitative data (e.g., field screening, fixed laboratory) are the right type, and of adequate quality to support the decision-making process. Steps 3 through 10 of the process are production steps and are integrated electronically. The detailed plans, procedures, and systems used day-to-day by the SDM process require a high degree of accuracy and reliability. Tools must be incorporated into the processes that minimize errors. This paper discusses all of the elements of the SDM process in detail.

  8. Real-time Sample Analysis using Sampling Probe and Miniature Mass Spectrometer

    PubMed Central

    Chen, Chien-Hsun; Lin, Ziqing; Tian, Ran; Shi, Riyi; Cooks, R. Graham; Ouyang, Zheng

    2016-01-01

    A miniature mass spectrometry system with a sampling probe has been developed for real-time analysis of chemicals from sample surfaces. The sampling probe is 1.5m in length and is comprised of one channel for introducing the spray and the other channel for transferring the charged species back to the Mini MS. This system provides a solution to the problem of real-time mass spectrometry analysis of a three-dimensional object in the field and is successful with compounds including those in inks, agrochemicals, explosives, and animal tissues. This system can be implemented in the form of a backpack MS with a sampling probe for forensic analysis or in the form of a compact MS with an intra-surgical probe for tissue analysis. PMID:26237577

  9. 40 CFR 86.1340-90 - Exhaust sample analysis.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... sample analysis perform the following sequence: (1) Warm-up and stabilize the analyzers; clean and/or... sample analysis perform the following sequence: (1) Warm-up and stabilize the analyzers; clean and/or... lines, filters, pumps, etc., to stabilize at operating temperature. (3) Optional: Perform a...

  10. 40 CFR 86.1340-90 - Exhaust sample analysis.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... sample analysis perform the following sequence: (1) Warm-up and stabilize the analyzers; clean and/or... sample analysis perform the following sequence: (1) Warm-up and stabilize the analyzers; clean and/or... lines, filters, pumps, etc., to stabilize at operating temperature. (3) Optional: Perform a...

  11. 40 CFR 86.240-94 - Exhaust sample analysis.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 19 2013-07-01 2013-07-01 false Exhaust sample analysis. 86.240-94 Section 86.240-94 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR PROGRAMS...-Duty Passenger Vehicles; Cold Temperature Test Procedures § 86.240-94 Exhaust sample analysis....

  12. 40 CFR 600.112-78 - Exhaust sample analysis.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... FUEL ECONOMY AND CARBON-RELATED EXHAUST EMISSIONS OF MOTOR VEHICLES Fuel Economy Regulations for 1978 and Later Model Year Automobiles-Test Procedures § 600.112-78 Exhaust sample analysis. The exhaust... 40 Protection of Environment 29 2010-07-01 2010-07-01 false Exhaust sample analysis....

  13. 40 CFR 600.112-08 - Exhaust sample analysis.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... FUEL ECONOMY AND CARBON-RELATED EXHAUST EMISSIONS OF MOTOR VEHICLES Fuel Economy Regulations for 1978 and Later Model Year Automobiles-Test Procedures § 600.112-08 Exhaust sample analysis. The exhaust... 40 Protection of Environment 29 2010-07-01 2010-07-01 false Exhaust sample analysis....

  14. Analysis of organic compounds in returned comet nucleus samples

    NASA Technical Reports Server (NTRS)

    Cronin, J. R.

    1989-01-01

    Techniques for analysis of organic compounds in returned comet nucleus samples are described. Interstellar, chondritic and transitional organic components are discussed. Appropriate sampling procedures will be essential to the success of these analyses. It will be necessary to return samples that represent all the various regimes found in the nucleus, e.g., a complete core, volatile components (deep interior), and crustal components (surface minerals, rocks, processed organics such as macromolecular carbon and polymers). Furthermore, sampling, storage, return, and distribution of samples must be done under conditions that preclude contamination of the samples by terrestrial matter.

  15. Analysis of the research sample collections of Uppsala biobank.

    PubMed

    Engelmark, Malin T; Beskow, Anna H

    2014-10-01

    Uppsala Biobank is the joint and only biobank organization of the two principals, Uppsala University and Uppsala University Hospital. Biobanks are required to have updated registries on sample collection composition and management in order to fulfill legal regulations. We report here the results from the first comprehensive and overall analysis of the 131 research sample collections organized in the biobank. The results show that the median of the number of samples in the collections was 700 and that the number of samples varied from less than 500 to over one million. Blood samples, such as whole blood, serum, and plasma, were included in the vast majority, 84.0%, of the research sample collections. Also, as much as 95.5% of the newly collected samples within healthcare included blood samples, which further supports the concept that blood samples have fundamental importance for medical research. Tissue samples were also commonly used and occurred in 39.7% of the research sample collections, often combined with other types of samples. In total, 96.9% of the 131 sample collections included samples collected for healthcare, showing the importance of healthcare as a research infrastructure. Of the collections that had accessed existing samples from healthcare, as much as 96.3% included tissue samples from the Department of Pathology, which shows the importance of pathology samples as a resource for medical research. Analysis of different research areas shows that the most common of known public health diseases are covered. Collections that had generated the most publications, up to over 300, contained a large number of samples collected systematically and repeatedly over many years. More knowledge about existing biobank materials, together with public registries on sample collections, will support research collaborations, improve transparency, and bring us closer to the goals of biobanks, which is to save and prolong human lives and improve health and quality of life.

  16. Theory of sampling: four critical success factors before analysis.

    PubMed

    Wagner, Claas; Esbensen, Kim H

    2015-01-01

    Food and feed materials characterization, risk assessment, and safety evaluations can only be ensured if QC measures are based on valid analytical data, stemming from representative samples. The Theory of Sampling (TOS) is the only comprehensive theoretical framework that fully defines all requirements to ensure sampling correctness and representativity, and to provide the guiding principles for sampling in practice. TOS also defines the concept of material heterogeneity and its impact on the sampling process, including the effects from all potential sampling errors. TOS's primary task is to eliminate bias-generating errors and to minimize sampling variability. Quantitative measures are provided to characterize material heterogeneity, on which an optimal sampling strategy should be based. Four critical success factors preceding analysis to ensure a representative sampling process are presented here.

  17. Construction Site Storm Water Sampling California's New Construction Sampling and Analysis Requirements

    SciTech Connect

    Forrest, C.L.; Mathews, S.

    2002-04-02

    The California State Water Resources Control Board (State Board) originally issued a National Pollutant Discharge System (NPDES) permit for storm water discharges associated with construction activities in 1992. This NPDES permit was issued as a general permit, applicable throughout the state (with certain exceptions). The general construction permit was made site-specific by a discharger-developed Storm Water Pollution Prevention Plan (SWPPP). As with most NPDES construction storm water permits, monitoring requirements were limited to inspections. Sampling and analysis of discharges was not specifically required, but a Regional Water Quality Control Board (Regional Board) could require additional monitoring. In 1999, the State -Board revised and reissued its construction general permit. While the 1999 permit significantly enhanced the erosion and sediment control descriptions and requirements, and expanded the inspection program, sampling and analysis was still not required. Environmental advocacy groups took exception to the absence of sampling requirements and sought relief in court to add sampling and analysis. In 2001, the State Board in response to the court order adopted a resolution requiring sampling and analysis of construction site runoff under two conditions. Turbidity and/or sediment sampling is required when construction site runoff enters water bodies determined to impaired for sediment or turbidity. Sampling for non-visible pollutants is required when construction operations expose materials to storm water. Sampling construction site runoff is relatively new concept for NPDES permits. Only a few permits throughout the country require sampling and analysis for sediment-related pollutants, and California is one of the only permitting entities to require sampling for non-visible pollutants in construction site runoff. The added complexity of sampling runoff requires construction operators and erosion and sediment control professionals to expand their

  18. STATISTICAL ANALYSIS OF TANK 19F FLOOR SAMPLE RESULTS

    SciTech Connect

    Harris, S.

    2010-09-02

    Representative sampling has been completed for characterization of the residual material on the floor of Tank 19F as per the statistical sampling plan developed by Harris and Shine. Samples from eight locations have been obtained from the tank floor and two of the samples were archived as a contingency. Six samples, referred to in this report as the current scrape samples, have been submitted to and analyzed by SRNL. This report contains the statistical analysis of the floor sample analytical results to determine if further data are needed to reduce uncertainty. Included are comparisons with the prior Mantis samples results to determine if they can be pooled with the current scrape samples to estimate the upper 95% confidence limits (UCL95%) for concentration. Statistical analysis revealed that the Mantis and current scrape sample results are not compatible. Therefore, the Mantis sample results were not used to support the quantification of analytes in the residual material. Significant spatial variability among the current scrape sample results was not found. Constituent concentrations were similar between the North and South hemispheres as well as between the inner and outer regions of the tank floor. The current scrape sample results from all six samples fall within their 3-sigma limits. In view of the results from numerous statistical tests, the data were pooled from all six current scrape samples. As such, an adequate sample size was provided for quantification of the residual material on the floor of Tank 19F. The uncertainty is quantified in this report by an UCL95% on each analyte concentration. The uncertainty in analyte concentration was calculated as a function of the number of samples, the average, and the standard deviation of the analytical results. The UCL95% was based entirely on the six current scrape sample results (each averaged across three analytical determinations).

  19. STATISTICAL ANALYSIS OF TANK 18F FLOOR SAMPLE RESULTS

    SciTech Connect

    Harris, S.

    2010-09-02

    Representative sampling has been completed for characterization of the residual material on the floor of Tank 18F as per the statistical sampling plan developed by Shine [1]. Samples from eight locations have been obtained from the tank floor and two of the samples were archived as a contingency. Six samples, referred to in this report as the current scrape samples, have been submitted to and analyzed by SRNL [2]. This report contains the statistical analysis of the floor sample analytical results to determine if further data are needed to reduce uncertainty. Included are comparisons with the prior Mantis samples results [3] to determine if they can be pooled with the current scrape samples to estimate the upper 95% confidence limits (UCL{sub 95%}) for concentration. Statistical analysis revealed that the Mantis and current scrape sample results are not compatible. Therefore, the Mantis sample results were not used to support the quantification of analytes in the residual material. Significant spatial variability among the current sample results was not found. Constituent concentrations were similar between the North and South hemispheres as well as between the inner and outer regions of the tank floor. The current scrape sample results from all six samples fall within their 3-sigma limits. In view of the results from numerous statistical tests, the data were pooled from all six current scrape samples. As such, an adequate sample size was provided for quantification of the residual material on the floor of Tank 18F. The uncertainty is quantified in this report by an upper 95% confidence limit (UCL{sub 95%}) on each analyte concentration. The uncertainty in analyte concentration was calculated as a function of the number of samples, the average, and the standard deviation of the analytical results. The UCL{sub 95%} was based entirely on the six current scrape sample results (each averaged across three analytical determinations).

  20. UMTRA water sampling and analysis plan, Lakeview, Oregon

    SciTech Connect

    Not Available

    1993-09-29

    The purpose of this document is to provide background, guidance, and justification for water sampling activities for the Lakeview, Oregon, Uranium Mill Tailings Remedial Action (UMTRA) processing and disposal sites. This water sampling and analysis plan will form the basis for groundwater sampling and analysis work orders (WSAWO) to be implemented during 1993. Monitoring at the former Lakeview processing site is for characterization purposes and in preparation for the risk assessment, scheduled for the fall of 1993. Compliance monitoring was conducted at the disposal site. Details of the sampling plan are discussed in Section 5.0.

  1. Modular Automated Processing System (MAPS) for analysis of biological samples.

    SciTech Connect

    Gil, Geun-Cheol; Chirica, Gabriela S.; Fruetel, Julia A.; VanderNoot, Victoria A.; Branda, Steven S.; Schoeniger, Joseph S.; Throckmorton, Daniel J.; Brennan, James S.; Renzi, Ronald F.

    2010-10-01

    We have developed a novel modular automated processing system (MAPS) that enables reliable, high-throughput analysis as well as sample-customized processing. This system is comprised of a set of independent modules that carry out individual sample processing functions: cell lysis, protein concentration (based on hydrophobic, ion-exchange and affinity interactions), interferent depletion, buffer exchange, and enzymatic digestion of proteins of interest. Taking advantage of its unique capacity for enclosed processing of intact bioparticulates (viruses, spores) and complex serum samples, we have used MAPS for analysis of BSL1 and BSL2 samples to identify specific protein markers through integration with the portable microChemLab{trademark} and MALDI.

  2. Workshop on Analysis of Returned Comet Nucleus Samples

    NASA Technical Reports Server (NTRS)

    1989-01-01

    This volume contains abstracts that were accepted by the Program Committee for presentation at the workshop on the analysis of returned comet nucleus samples held in Milpitas, California, January 16 to 18, 1989. The abstracts deal with the nature of cometary ices, cryogenic handling and sampling equipment, origin and composition of samples, and spectroscopic, thermal and chemical processing methods of cometary nuclei. Laboratory simulation experimental results on dust samples are reported. Some results obtained from Halley's comet are also included. Microanalytic techniques for examining trace elements of cometary particles, synchrotron x ray fluorescence and instrument neutron activation analysis (INAA), are presented.

  3. Variability and specificity associated with environmental methamphetamine sampling and analysis.

    PubMed

    Van Dyke, Mike V; Serrano, Kate A; Kofford, Shalece; Contreras, John; Martyny, John W

    2011-11-01

    This study was designed to explore the efficacy of the use of wipe sampling to determine methamphetamine contamination associated with the clandestine manufacture of methamphetamine. Three laboratories were utilized to analyze wipe samples to investigate variability in reported methamphetamine concentration among samples spiked with known amounts of methamphetamine. Different sampling media, surfaces, and solvents were also utilized to determine potential differences in measured methamphetamine concentration due to different wipes, wipe solvents, and wipe contaminants. This study examined rate of false positive detection among blank samples and whether interference with common household substances would create a false positive detection of methamphetamine. Variability between the three labs-using liquid chromatography with mass spectrometry or gas chromatography with mass spectrometry for detection of a known concentration of methamphetamine-resulted in percent differences of 3-30%. Results from wipe sample analysis for methamphetamine, using methanol or isopropanol, showed no significant difference in methamphetamine contamination recovery. Dust and paint contamination on methamphetamine wipe samples with known methamphetamine spike amounts did not affect methamphetamine wipe sample recovery. This study confirmed that either methanol or isopropanol is an appropriate solvent for use in methamphetamine wipe sampling. Dust and paint contamination on wipe samples will not interfere with the wipe sample analysis for methamphetamine. False positive detection for methamphetamine was not observed in any of the blank wipe samples submitted for the study. Finally, this study determined that methamphetamine will not be detected in structures that are truly methamphetamine free at current laboratory limits of quantification.

  4. Tank 241AP104 Grab Sampling and Analysis Plan

    SciTech Connect

    TEMPLETON, A.M.

    2000-11-09

    This sampling and analysis plan (SAP) identifies characterization objectives pertaining to sample collection, laboratory analytical evaluation, and reporting requirements for samples obtained from tank 241-AP-104. The purpose of this sampling event is to obtain information about the characteristics of the contents of 241-AP-104 required to provide sample material to the Waste Treatment Contractor. Grab samples will be obtained from riser 001 to provide sufficient material for the chemical analyses and tests required to satisfy these data quality objectives and ICD-23. The 222-S Laboratory will receive samples; composite the samples; perform chemical analyses on composite samples; and provide samples to the Waste Treatment Contractor and the Process Chemistry Laboratory. The Process Chemistry Laboratory at the 222-S Laboratory Complex will perform process tests to evaluate the behavior of the 241-AP-104 waste undergoing the retrieval and treatment scenarios defined in the applicable DQOs. The Waste Treatment Contractor will perform process verification and waste form qualification tests. Requirements for analyses of samples originating in the L & H DQO process tests will be documented in the corresponding test plan (Person 2000) and are not within the scope of this SAP. This report provides the general methodology and procedures to be used in the preparation, retrieval, transport, analysis, and reporting of results from grab samples retrieved from tank 241-AP-104.

  5. PIXE analysis of Nigerian flour and bread samples

    NASA Astrophysics Data System (ADS)

    Olise, Felix S.; Fernandes, Adriana M.; Cristina Chaves, P.; Taborda, Ana; Reis, Miguel A.

    2014-01-01

    The alleged use of potassium bromate (KBrO3) in bread baking led a few authors to report on the chemical methods for the determination of KBrO3 levels in bread. In order to examine the potentials of a non chemical particle induced X-ray emission (PIXE) method for this purpose, six sets of samples, each composed of flour, dough and bread from a production batch were analysed. The samples were obtained from six different bakers of bread at Ile-Ife, Nigeria. The flour samples were air-dried while others were freeze dried at about -16 °C. The samples were homogenised in an agate mortar and then pelletised. Samples were analysed at the CTN standard PIXE setup and standard procedures for thick target samples analysis were followed. In some samples significant concentrations of bromine were found. In the present work we present possible explanations for the presence of this potentially dangerous contaminant in the samples.

  6. Requirements for Minimum Sample Size for Sensitivity and Specificity Analysis

    PubMed Central

    Adnan, Tassha Hilda

    2016-01-01

    Sensitivity and specificity analysis is commonly used for screening and diagnostic tests. The main issue researchers face is to determine the sufficient sample sizes that are related with screening and diagnostic studies. Although the formula for sample size calculation is available but concerning majority of the researchers are not mathematicians or statisticians, hence, sample size calculation might not be easy for them. This review paper provides sample size tables with regards to sensitivity and specificity analysis. These tables were derived from formulation of sensitivity and specificity test using Power Analysis and Sample Size (PASS) software based on desired type I error, power and effect size. The approaches on how to use the tables were also discussed. PMID:27891446

  7. Integration of sample analysis method (SAM) for polychlorinated biphenyls

    SciTech Connect

    Monagle, M.; Johnson, R.C.

    1996-05-01

    A completely integrated Sample Analysis Method (SAM) has been tested as part of the Contaminant Analysis Automation program. The SAM system was tested for polychlorinated biphenyl samples using five Standard Laboratory Modules{trademark}: two Soxtec{trademark} modules, a high volume concentrator module, a generic materials handling module, and the gas chromatographic module. With over 300 samples completed within the first phase of the validation, recovery and precision data were comparable to manual methods. Based on experience derived from the first evaluation of the automated system, efforts are underway to improve sample recoveries and integrate a sample cleanup procedure. In addition, initial work in automating the extraction of semivolatile samples using this system will also be discussed.

  8. Environmental sampling and analysis in support of NTI-3

    SciTech Connect

    McGuire, R.R.; Harrar, J.E.; Haas, J.S.; Eagle, R.J.; Andresen, B.D.

    1991-04-06

    The third National Trail Inspection took place at the Monsanto Chemical Plant in Luling, Louisiana. In order to test the effectiveness of environmental sampling (soil, water and air) in determining the nature of the chemical process in a given production plant and to examine the distance from a process building that samples can effectively be taken, we needed to select some materials that constituted components of process streams. Three materials were selected: 1. isopropyl amine for air monitoring, 2. 4-nitrophenol, one of the precursors in the acetaminophen process, and 3. an intermediate in the production of glyphosate for ROUNDUP that is known simply as glyphosate intermediated. LLNL did not participate in the air sampling nor the analysis for isopropyl amine. This paper discussed the steps in this experiment including sample collection, sample workshop, sample analysis the results and discussion and the conclusion. 3 figs., 6 tabs.

  9. Soil sample preparation using microwave digestion for uranium analysis

    SciTech Connect

    MOHAGHEGHI,AMIR H.; PRESTON,ROSE; AKBARZADEH,MANSOOR; BAKHTIAR,STEVEN

    2000-04-05

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

  10. ALVEOLAR BREATH SAMPLING AND ANALYSIS IN HUMAN EXPOSURE ASSESSMENT STUDIES

    EPA Science Inventory

    Alveolar breath sampling and analysis can be extremely useful in exposure assessment studies involving volatile organic compounds (VOCs). Over recent years scientists from the EPA's National Exposure Research Laboratory have developed and refined an alveolar breath collection ...

  11. Methods for collection and analysis of water samples

    USGS Publications Warehouse

    Rainwater, Frank Hays; Thatcher, Leland Lincoln

    1960-01-01

    This manual contains methods used by the U.S. Geological Survey to collect, preserve, and analyze water samples. Throughout, the emphasis is on obtaining analytical results that accurately describe the chemical composition of the water in situ. Among the topics discussed are selection of sampling sites, frequency of sampling, field equipment, preservatives and fixatives, analytical techniques of water analysis, and instruments. Seventy-seven laboratory and field procedures are given for determining fifty-three water properties.

  12. 40 CFR 92.129 - Exhaust sample analysis.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... “before” span check for the next mode. (d) For sample analysis perform the following sequence: (1) Warm-up... temperature. (3) Optional: Perform a hang-up check for the HFID sampling system: (i) Zero the analyzer using... exceeds the analyzer zero response by 2 percent or more of the HFID full-scale deflection, hang-up...

  13. 40 CFR 92.129 - Exhaust sample analysis.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... “before” span check for the next mode. (d) For sample analysis perform the following sequence: (1) Warm-up... temperature. (3) Optional: Perform a hang-up check for the HFID sampling system: (i) Zero the analyzer using... exceeds the analyzer zero response by 2 percent or more of the HFID full-scale deflection, hang-up...

  14. Analysis of Iron in Lawn Fertilizer: A Sampling Study

    ERIC Educational Resources Information Center

    Jeannot, Michael A.

    2006-01-01

    An experiment is described which uses a real-world sample of lawn fertilizer in a simple exercise to illustrate problems associated with the sampling step of a chemical analysis. A mixed-particle fertilizer containing discrete particles of iron oxide (magnetite, Fe[subscript 3]O[subscript 4]) mixed with other particles provides an excellent…

  15. 40 CFR 265.92 - Sampling and analysis.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... water supply, as specified in appendix III. (2) Parameters establishing ground-water quality: (i... frequencies: (1) Samples collected to establish ground-water quality must be obtained and analyzed for the... FACILITIES Ground-Water Monitoring § 265.92 Sampling and analysis. (a) The owner or operator must obtain...

  16. 40 CFR 265.92 - Sampling and analysis.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... water supply, as specified in appendix III. (2) Parameters establishing ground-water quality: (i... frequencies: (1) Samples collected to establish ground-water quality must be obtained and analyzed for the... FACILITIES Ground-Water Monitoring § 265.92 Sampling and analysis. (a) The owner or operator must obtain...

  17. 40 CFR 265.92 - Sampling and analysis.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... water supply, as specified in appendix III. (2) Parameters establishing ground-water quality: (i... frequencies: (1) Samples collected to establish ground-water quality must be obtained and analyzed for the... FACILITIES Ground-Water Monitoring § 265.92 Sampling and analysis. (a) The owner or operator must obtain...

  18. 40 CFR 265.92 - Sampling and analysis.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... water supply, as specified in appendix III. (2) Parameters establishing ground-water quality: (i... frequencies: (1) Samples collected to establish ground-water quality must be obtained and analyzed for the... FACILITIES Ground-Water Monitoring § 265.92 Sampling and analysis. (a) The owner or operator must obtain...

  19. Sampling and Analysis Instruction for Borehole Sampling at 118-B-1 Burial Ground

    SciTech Connect

    W. S. Thompson

    2007-04-02

    The Washington Closure Hanford (WCH) Field Remediation Project has removed all of the disposed materials and contaminated soil from the 118-B-1 Burial Ground with the exception of tritium-contaminated soil that is believed to extend from the bottom of the present excavation to groundwater and is believed to contribute to tritium contamination observed at down-gradient monitoring Well 199-B8-6. This sampling and analysis instruction (SAI) provides the requirements for sample collection and laboratory analysis for characterization of the vertical distribution of tritium contamination in the vadose zone soil below the 118-B-1 Burial Ground remedial action excavation.

  20. An Integrated Tool for System Analysis of Sample Return Vehicles

    NASA Technical Reports Server (NTRS)

    Samareh, Jamshid A.; Maddock, Robert W.; Winski, Richard G.

    2012-01-01

    The next important step in space exploration is the return of sample materials from extraterrestrial locations to Earth for analysis. Most mission concepts that return sample material to Earth share one common element: an Earth entry vehicle. The analysis and design of entry vehicles is multidisciplinary in nature, requiring the application of mass sizing, flight mechanics, aerodynamics, aerothermodynamics, thermal analysis, structural analysis, and impact analysis tools. Integration of a multidisciplinary problem is a challenging task; the execution process and data transfer among disciplines should be automated and consistent. This paper describes an integrated analysis tool for the design and sizing of an Earth entry vehicle. The current tool includes the following disciplines: mass sizing, flight mechanics, aerodynamics, aerothermodynamics, and impact analysis tools. Python and Java languages are used for integration. Results are presented and compared with the results from previous studies.

  1. Liquid MALDI MS Analysis of Complex Peptide and Proteome Samples.

    PubMed

    Wiangnon, Kanjana; Cramer, Rainer

    2016-09-02

    Matrix-assisted laser desorption/ionization (MALDI) time-of-flight (TOF) mass spectrometry (MS) is well-known to be a powerful technique for the analysis of biological samples. By using glycerol-based liquid support matrices (LSMs) instead of conventional MALDI matrices the power of this technique can be extended further. In this study, we exploited LSMs for the identification of complex samples, that is, the Lactobacillus proteome and a bovine serum albumin (BSA) digest. Liquid and solid MALDI samples were manually and robotically prepared by coupling a nanoflow high-performance liquid chromatography (nanoHPLC) system to an automated MALDI sample spotting device. MS and MS/MS data were successfully acquired at the femtomole level using TOF/TOF as well as Q-TOF instrumentation and used for protein identification searching sequence databases. For the BSA digest analysis, liquid MALDI samples resulted in peptide mass fingerprints, which led to a higher confidence in protein identification compared with solid (crystalline) MALDI samples; however, postsource decay (PSD) MS/MS analysis of both the proteome of Lactobacillus plantarum WCFS1 cells and BSA digest showed that further optimization of the formation and detection of peptide fragment ions is still needed for liquid MALDI samples, as the MS/MS ion search score was lower than that for the solid MALDI samples, reflecting the poorer quality of the liquid MALDI-PSD spectra, which can be attributed to the differences in PSD parameters and their optimization that is currently achievable.

  2. Forensic Comparison of Soil Samples Using Nondestructive Elemental Analysis.

    PubMed

    Uitdehaag, Stefan; Wiarda, Wim; Donders, Timme; Kuiper, Irene

    2016-12-01

    Soil can play an important role in forensic cases in linking suspects or objects to a crime scene by comparing samples from the crime scene with samples derived from items. This study uses an adapted ED-XRF analysis (sieving instead of grinding to prevent destruction of microfossils) to produce elemental composition data of 20 elements. Different data processing techniques and statistical distances were evaluated using data from 50 samples and the log-LR cost (Cllr ). The best performing combination, Canberra distance, relative data, and square root values, is used to construct a discriminative model. Examples of the spatial resolution of the method in crime scenes are shown for three locations, and sampling strategy is discussed. Twelve test cases were analyzed, and results showed that the method is applicable. The study shows how the combination of an analysis technique, a database, and a discriminative model can be used to compare multiple soil samples quickly.

  3. Sample size and power considerations in network meta-analysis

    PubMed Central

    2012-01-01

    Background Network meta-analysis is becoming increasingly popular for establishing comparative effectiveness among multiple interventions for the same disease. Network meta-analysis inherits all methodological challenges of standard pairwise meta-analysis, but with increased complexity due to the multitude of intervention comparisons. One issue that is now widely recognized in pairwise meta-analysis is the issue of sample size and statistical power. This issue, however, has so far only received little attention in network meta-analysis. To date, no approaches have been proposed for evaluating the adequacy of the sample size, and thus power, in a treatment network. Findings In this article, we develop easy-to-use flexible methods for estimating the ‘effective sample size’ in indirect comparison meta-analysis and network meta-analysis. The effective sample size for a particular treatment comparison can be interpreted as the number of patients in a pairwise meta-analysis that would provide the same degree and strength of evidence as that which is provided in the indirect comparison or network meta-analysis. We further develop methods for retrospectively estimating the statistical power for each comparison in a network meta-analysis. We illustrate the performance of the proposed methods for estimating effective sample size and statistical power using data from a network meta-analysis on interventions for smoking cessation including over 100 trials. Conclusion The proposed methods are easy to use and will be of high value to regulatory agencies and decision makers who must assess the strength of the evidence supporting comparative effectiveness estimates. PMID:22992327

  4. ANALYSIS OF ATMOSPHERE DEPOSITION SAMPLES FROM EASTON, PA

    EPA Science Inventory

    The report gives results of an analysis of samples of tenacious atmospheric deposits on exposed surfaces (e.g., automobiles and houses) in an industrial area near Easton, PA. The analysis was made at the request of the State of Pennsylvania. The Pennsylvania Department of Environ...

  5. Development of field portable sampling and analysis systems

    SciTech Connect

    Beals, D.

    2000-06-08

    A rapid field portable sample and analysis system has been demonstrated at the Savannah River Site and the Hanford Site. The portable system can be used when rapid decisions are needed in the field during scoping or remediation activities, or when it is impractical to bring large volumes of water to the lab for analysis.

  6. Hayabusa Recovery, Curation and Preliminary Sample Analysis: Lessons Learned from Recent Sample Return Mission

    NASA Technical Reports Server (NTRS)

    Zolensky, Michael E.

    2011-01-01

    I describe lessons learned from my participation on the Hayabusa Mission, which returned regolith grains from asteroid Itokawa in 2010 [1], comparing this with the recently returned Stardust Spacecraft, which sampled the Jupiter Family comet Wild 2. Spacecraft Recovery Operations: The mission Science and Curation teams must actively participate in planning, testing and implementing spacecraft recovery operations. The crash of the Genesis spacecraft underscored the importance of thinking through multiple contingency scenarios and practicing field recovery for these potential circumstances. Having the contingency supplies on-hand was critical, and at least one full year of planning for Stardust and Hayabusa recovery operations was necessary. Care must be taken to coordinate recovery operations with local organizations and inform relevant government bodies well in advance. Recovery plans for both Stardust and Hayabusa had to be adjusted for unexpectedly wet landing site conditions. Documentation of every step of spacecraft recovery and deintegration was necessary, and collection and analysis of launch and landing site soils was critical. We found the operation of the Woomera Text Range (South Australia) to be excellent in the case of Hayabusa, and in many respects this site is superior to the Utah Test and Training Range (used for Stardust) in the USA. Recovery operations for all recovered spacecraft suffered from the lack of a hermetic seal for the samples. Mission engineers should be pushed to provide hermetic seals for returned samples. Sample Curation Issues: More than two full years were required to prepare curation facilities for Stardust and Hayabusa. Despite this seemingly adequate lead time, major changes to curation procedures were required once the actual state of the returned samples became apparent. Sample databases must be fully implemented before sample return for Stardust we did not adequately think through all of the possible sub sampling and

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

    SciTech Connect

    Udey, R. N.; Corzett, T. H.; Alcaraz, A.

    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.

  8. Protocol for Microplastics Sampling on the Sea Surface and Sample Analysis

    PubMed Central

    Kovač Viršek, Manca; Palatinus, Andreja; Koren, Špela; Peterlin, Monika; Horvat, Petra; Kržan, Andrej

    2016-01-01

    Microplastic pollution in the marine environment is a scientific topic that has received increasing attention over the last decade. The majority of scientific publications address microplastic pollution of the sea surface. The protocol below describes the methodology for sampling, sample preparation, separation and chemical identification of microplastic particles. A manta net fixed on an »A frame« attached to the side of the vessel was used for sampling. Microplastic particles caught in the cod end of the net were separated from samples by visual identification and use of stereomicroscopes. Particles were analyzed for their size using an image analysis program and for their chemical structure using ATR-FTIR and micro FTIR spectroscopy. The described protocol is in line with recommendations for microplastics monitoring published by the Marine Strategy Framework Directive (MSFD) Technical Subgroup on Marine Litter. This written protocol with video guide will support the work of researchers that deal with microplastics monitoring all over the world. PMID:28060297

  9. Protocol for Microplastics Sampling on the Sea Surface and Sample Analysis.

    PubMed

    Kovač Viršek, Manca; Palatinus, Andreja; Koren, Špela; Peterlin, Monika; Horvat, Petra; Kržan, Andrej

    2016-12-16

    Microplastic pollution in the marine environment is a scientific topic that has received increasing attention over the last decade. The majority of scientific publications address microplastic pollution of the sea surface. The protocol below describes the methodology for sampling, sample preparation, separation and chemical identification of microplastic particles. A manta net fixed on an »A frame« attached to the side of the vessel was used for sampling. Microplastic particles caught in the cod end of the net were separated from samples by visual identification and use of stereomicroscopes. Particles were analyzed for their size using an image analysis program and for their chemical structure using ATR-FTIR and micro FTIR spectroscopy. The described protocol is in line with recommendations for microplastics monitoring published by the Marine Strategy Framework Directive (MSFD) Technical Subgroup on Marine Litter. This written protocol with video guide will support the work of researchers that deal with microplastics monitoring all over the world.

  10. Biomass Thermogravimetric Analysis: Uncertainty Determination Methodology and Sampling Maps Generation

    PubMed Central

    Pazó, Jose A.; Granada, Enrique; Saavedra, Ángeles; Eguía, Pablo; Collazo, Joaquín

    2010-01-01

    The objective of this study was to develop a methodology for the determination of the maximum sampling error and confidence intervals of thermal properties obtained from thermogravimetric analysis (TG), including moisture, volatile matter, fixed carbon and ash content. The sampling procedure of the TG analysis was of particular interest and was conducted with care. The results of the present study were compared to those of a prompt analysis, and a correlation between the mean values and maximum sampling errors of the methods were not observed. In general, low and acceptable levels of uncertainty and error were obtained, demonstrating that the properties evaluated by TG analysis were representative of the overall fuel composition. The accurate determination of the thermal properties of biomass with precise confidence intervals is of particular interest in energetic biomass applications. PMID:20717532

  11. Potential applications of environmental sampling and analysis for the IAEA

    SciTech Connect

    Raber, E.

    1993-03-01

    This objective of this paper is to address the usefulness of envirorunental sampling and analysis in support of the IAEA. In particular, whether state-of-the-art analytical methods may provide detection of undeclared nuclear activities. It is important to emphasize that envirorunental sampling offers the IAEA a method of improving the assurance that a particular facility has no ongoing undeclared nuclear activities. It is suggested as a supplement to the existing IAEA safeguards inspections and activities. Enviromental sampling with appropriate analytical techniques can detect unknown activity fairly well, but it is not very reliable for determining how much or when activity has actually occured. Additionally, it is important to point out that the cost of such an envirorunental sampling program needs to be balanced with the confidence provided to detect undeclared nuclear activities. Environmental sampling wig probably not allow the IAEA to reduce or eliminate some of its existing baseline activities. The addition of an environmental sampling and analysis program will entail a cost of its own, and adding such a program may not reduce IAEA total costs. The overall cost of such a program will depend on the level of confidence required, (e.g. number and type of samples and analyses), the Quality Assurance plan to be implemented and the number of sites to be inspected. A more detailed cost analysis is not within the scope of this paper.

  12. Appendix C. Collection of Samples for Chemical Agent Analysis

    SciTech Connect

    Koester, C; Thompson, C; Doerr, T; Scripsick, R

    2005-09-23

    This chapter describes procedures for the collection and analysis of samples of various matrices for the purpose of determining the presence of chemical agents in a civilian setting. This appendix is intended to provide the reader with sufficient information to make informed decisions about the sampling and analysis process and to suggest analytical strategies that might be implemented by the scientists performing sampling and analysis. This appendix is not intended to be used as a standard operating procedure to provide detailed instructions as to how trained scientists should handle samples. Chemical agents can be classified by their physical and chemical properties. Table 1 lists the chemical agents considered by this report. In selecting sampling and analysis methods, we have considered procedures proposed by the Organization for Prohibition of Chemical Weapons (OPCW), the U. S. Environmental Protection Agency (EPA), and peer-reviewed scientific literature. EPA analytical methods are good resources describing issues of quality assurance with respect to chain-of-custody, sample handling, and quality control requirements.

  13. Tritium analysis of urine samples from the general Korean public.

    PubMed

    Yoon, Seokwon; Ha, Wi-Ho; Lee, Seung-Sook

    2013-11-01

    The tritium concentrations of urine samples and the effective dose of the general Korean public were evaluated. To achieve accurate HTO analysis of urine samples, we established the optimal conditions for measuring the HTO content of urine samples. Urine samples from 50 Koreans who do not work at a nuclear facility were analyzed on the basis of the results. The average urine analysis result was 2.8 ±1 .4 Bq/L, and the range was 1.8-5.6 Bq/L. The measured values were lower than those reported for other countries. These results show that environmental factors and lifestyle differences are the main factors affecting the tritium level of the general public.

  14. Nanomaterials for sample pretreatment prior to capillary electrophoretic analysis.

    PubMed

    Adam, Vojtech; Vaculovicova, Marketa

    2017-02-16

    Nanomaterials are, in analytical science, used for a broad range of purposes, covering the area of sample pretreatment as well as separation, detection and identification of target molecules. This review covers the application of nanomaterials for sample pretreatment in capillary electrophoresis. It targets the utilization of nanomaterials for sample purification, preconcentration and/or extraction coupled both off-line and on-line with capillary electrophoretic analysis. Especially due to their large surface area, nanoparticles and nanomaterials are exceptionally helpful in making up for the limited concentration detection limits provided by capillary electrophoresis. This method possesses excellent separation power; however, its sensitivity may be problematic in some cases. Therefore, this review is focused on utilization of nanomaterials as a powerful tool for sample preconcentration, which is so often required prior to capillary electrophoretic analysis.

  15. Principal Component Analysis for Biosignature Detection in Extraterrestrial Samples

    NASA Technical Reports Server (NTRS)

    McDonald, G. D.; Storrie-Lombardi, M. C.

    1998-01-01

    Analysis of extraterrestrial samples for organic signatures of past or present life presents several problems. Chief among these is distinguishing bonafide extraterrestrial organic material from terrestrial contamination, either carried on a spacecraft or present in the terrestrial environment to which the sample is exposed. A related problem is separating biologically derived molecules from those produced by abiotic syntheses in the interstellar medium, on meteorite parent bodies, or in planetary atmospheres and oceans.

  16. Northern Marshall Islands radiological survey: sampling and analysis summary

    SciTech Connect

    Robison, W.L.; Conrado, C.L.; Eagle, R.J.; Stuart, M.L.

    1981-07-23

    A radiological survey was conducted in the Northern Marshall Islands to document reamining external gamma exposures from nuclear tests conducted at Enewetak and Bikini Atolls. An additional program was later included to obtain terrestrial and marine samples for radiological dose assessment for current or potential atoll inhabitants. This report is the first of a series summarizing the results from the terrestrial and marine surveys. The sample collection and processing procedures and the general survey methodology are discussed; a summary of the collected samples and radionuclide analyses is presented. Over 5400 samples were collected from the 12 atolls and 2 islands and prepared for analysis including 3093 soil, 961 vegetation, 153 animal, 965 fish composite samples (average of 30 fish per sample), 101 clam, 50 lagoon water, 15 cistern water, 17 groundwater, and 85 lagoon sediment samples. A complete breakdown by sample type, atoll, and island is given here. The total number of analyses by radionuclide are 8840 for /sup 241/Am, 6569 for /sup 137/Cs, 4535 for /sup 239 +240/Pu, 4431 for /sup 90/Sr, 1146 for /sup 238/Pu, 269 for /sup 241/Pu, and 114 each for /sup 239/Pu and /sup 240/Pu. A complete breakdown by sample category, atoll or island, and radionuclide is also included.

  17. Estimating the Expected Value of Sample Information Using the Probabilistic Sensitivity Analysis Sample

    PubMed Central

    Oakley, Jeremy E.; Brennan, Alan; Breeze, Penny

    2015-01-01

    Health economic decision-analytic models are used to estimate the expected net benefits of competing decision options. The true values of the input parameters of such models are rarely known with certainty, and it is often useful to quantify the value to the decision maker of reducing uncertainty through collecting new data. In the context of a particular decision problem, the value of a proposed research design can be quantified by its expected value of sample information (EVSI). EVSI is commonly estimated via a 2-level Monte Carlo procedure in which plausible data sets are generated in an outer loop, and then, conditional on these, the parameters of the decision model are updated via Bayes rule and sampled in an inner loop. At each iteration of the inner loop, the decision model is evaluated. This is computationally demanding and may be difficult if the posterior distribution of the model parameters conditional on sampled data is hard to sample from. We describe a fast nonparametric regression-based method for estimating per-patient EVSI that requires only the probabilistic sensitivity analysis sample (i.e., the set of samples drawn from the joint distribution of the parameters and the corresponding net benefits). The method avoids the need to sample from the posterior distributions of the parameters and avoids the need to rerun the model. The only requirement is that sample data sets can be generated. The method is applicable with a model of any complexity and with any specification of model parameter distribution. We demonstrate in a case study the superior efficiency of the regression method over the 2-level Monte Carlo method. PMID:25810269

  18. Neutron activation analysis of certified samples by the absolute method

    NASA Astrophysics Data System (ADS)

    Kadem, F.; Belouadah, N.; Idiri, Z.

    2015-07-01

    The nuclear reactions analysis technique is mainly based on the relative method or the use of activation cross sections. In order to validate nuclear data for the calculated cross section evaluated from systematic studies, we used the neutron activation analysis technique (NAA) to determine the various constituent concentrations of certified samples for animal blood, milk and hay. In this analysis, the absolute method is used. The neutron activation technique involves irradiating the sample and subsequently performing a measurement of the activity of the sample. The fundamental equation of the activation connects several physical parameters including the cross section that is essential for the quantitative determination of the different elements composing the sample without resorting to the use of standard sample. Called the absolute method, it allows a measurement as accurate as the relative method. The results obtained by the absolute method showed that the values are as precise as the relative method requiring the use of standard sample for each element to be quantified.

  19. UMTRA project water sampling and analysis plan -- Shiprock, New Mexico

    SciTech Connect

    Not Available

    1994-02-01

    Water sampling and analysis plan (WSAP) is required for each U.S. Department of Energy (DOE) Uranium Mill Tailings Remedial Action (UMTRA) Project site to provide a basis for ground water and surface water sampling at disposal and former processing sites. This WSAP identifies and justifies the sampling locations, analytical parameters, detection limits, and sampling frequency for the monitoring stations at the Navaho Reservation in Shiprock, New Mexico, UMTRA Project site. The purposes of the water sampling at Shiprock for fiscal year (FY) 1994 are to (1) collect water quality data at new monitoring locations in order to build a defensible statistical data base, (2) monitor plume movement on the terrace and floodplain, and (3) monitor the impact of alluvial ground water discharge into the San Juan River. The third activity is important because the community of Shiprock withdraws water from the San Juan River directly across from the contaminated alluvial floodplain below the abandoned uranium mill tailings processing site.

  20. UMTRA project water sampling and analysis plan, Tuba City, Arizona

    SciTech Connect

    1996-02-01

    Planned, routine ground water sampling activities at the U.S. Department of Energy (DOE) Uranium Mill Tailings Remedial Action (UMTRA) Project site in Tuba City, Arizona, are described in the following sections of this water sampling and analysis plan (WSAP). This plan identifies and justifies the sampling locations, analytical parameters, detection limits, and sampling frequency for the stations routinely monitored at the site. The ground water data are used for site characterization and risk assessment. The regulatory basis for routine ground water monitoring at UMTRA Project sites is derived from the U.S. Environmental Protection Agency (EPA) regulations in 40 CFR Part 192 (1994) and the final EPA standards of 1995 (60 FR 2854). Sampling procedures are guided by the UMTRA Project standard operating procedures (SOP) (JEG, n.d.), and the most effective technical approach for the site.

  1. Fluidics platform and method for sample preparation and analysis

    SciTech Connect

    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.

  2. Analysis of Waste Isolation Pilot Plant Samples: Integrated Summary Report

    SciTech Connect

    Britt, Phillip F

    2015-03-01

    Analysis of Waste Isolation Pilot Plant Samples: Integrated Summary Report. Summaries of conclusions, analytical processes, and analytical results. Analysis of samples taken from the Waste Isolation Pilot Plant (WIPP) near Carlsbad, New Mexico in support of the WIPP Technical Assessment Team (TAT) activities to determine to the extent feasible the mechanisms and chemical reactions that may have resulted in the breach of at least one waste drum and release of waste material in WIPP Panel 7 Room 7 on February 14, 2014. This report integrates and summarizes the results contained in three separate reports, described below, and draws conclusions based on those results. Chemical and Radiochemical Analyses of WIPP Samples R-15 C5 SWB and R16 C-4 Lip; PNNL-24003, Pacific Northwest National Laboratory, December 2014 Analysis of Waste Isolation Pilot Plant (WIPP) Underground and MgO Samples by the Savannah River National Laboratory (SRNL); SRNL-STI-2014-00617; Savannah River National Laboratory, December 2014 Report for WIPP UG Sample #3, R15C5 (9/3/14); LLNL-TR-667015; Lawrence Livermore National Laboratory, January 2015 This report is also contained in the Waste Isolation Pilot Plant Technical Assessment Team Report; SRNL-RP-2015-01198; Savannah River National Laboratory, March 17, 2015, as Appendix C: Analysis Integrated Summary Report.

  3. Preparation of ultra small samples for optical and microprobe analysis

    NASA Technical Reports Server (NTRS)

    Inman, C. S.

    1973-01-01

    This paper describes a simple but satisfactory new method for the preparation of tiny, varied and specialized specimens for electron or ion-microprobe analysis developed over the past five years. Microtektites, individual chondrules, single grains, blebs from lunar samples and meteoritic minerals have been prepared by this technique. A description of the preparation of these usually difficult samples from the initial mounting through the various polishing steps to their final polish is presented in detail. The procedures used to prevent any contamination of these specimens by the polishing agents and to prevent cross contamination to the other samples used for geochronology studies are presented.

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

    NASA Astrophysics Data System (ADS)

    Lari, L.; Dudkiewicz, A.

    2014-06-01

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

  5. Analysis report for 241-BY-104 Auger samples

    SciTech Connect

    Beck, M.A.

    1994-11-10

    This report describes the analysis of the surface crust samples taken from single-shell tank (SST) BY-104, suspected of containing ferrocyanide wastes. This sampling and analysis will assist in ascertaining whether there is any hazard due to combustion (burning) or explosion of these solid wastes. These characteristics are important to future efforts to characterize the salt and sludge in this type of waste tank. This report will outline the methodology and detail the results of analyses performed during the characterization of this material. All analyses were performed by Westinghouse Hanford Company at the 222-S laboratory unless stated otherwise.

  6. Formaldehyde monitoring program: development of sampling and analysis procedures

    SciTech Connect

    Matthews, T. G.; Hawthorne, A. R.

    1980-01-01

    This report outlines the scope and goals of the formaldehyde analysis program being carried out in Health and Safety Research Division of the Oak Ridge National Laboratory under contract of the US Consumer Product Safety Commission. The outline of the sampling and analysis techniques under consideration, with reference to a time frame for developmental work and field application, is discussed. The complexity of the different techniques is addressed in instances where technical staff would be requird for accurate operation of the instrumentation.

  7. QA/QC requirements for physical properties sampling and analysis

    SciTech Connect

    Innis, B.E.

    1993-07-21

    This report presents results of an assessment of the available information concerning US Environmental Protection Agency (EPA) quality assurance/quality control (QA/QC) requirements and guidance applicable to sampling, handling, and analyzing physical parameter samples at Comprehensive Environmental Restoration, Compensation, and Liability Act (CERCLA) investigation sites. Geotechnical testing laboratories measure the following physical properties of soil and sediment samples collected during CERCLA remedial investigations (RI) at the Hanford Site: moisture content, grain size by sieve, grain size by hydrometer, specific gravity, bulk density/porosity, saturated hydraulic conductivity, moisture retention, unsaturated hydraulic conductivity, and permeability of rocks by flowing air. Geotechnical testing laboratories also measure the following chemical parameters of soil and sediment samples collected during Hanford Site CERCLA RI: calcium carbonate and saturated column leach testing. Physical parameter data are used for (1) characterization of vadose and saturated zone geology and hydrogeology, (2) selection of monitoring well screen sizes, (3) to support modeling and analysis of the vadose and saturated zones, and (4) for engineering design. The objectives of this report are to determine the QA/QC levels accepted in the EPA Region 10 for the sampling, handling, and analysis of soil samples for physical parameters during CERCLA RI.

  8. Investigation of spectral analysis techniques for randomly sampled velocimetry data

    NASA Technical Reports Server (NTRS)

    Sree, Dave

    1993-01-01

    It is well known that velocimetry (LV) generates individual realization velocity data that are randomly or unevenly sampled in time. Spectral analysis of such data to obtain the turbulence spectra, and hence turbulence scales information, requires special techniques. The 'slotting' technique of Mayo et al, also described by Roberts and Ajmani, and the 'Direct Transform' method of Gaster and Roberts are well known in the LV community. The slotting technique is faster than the direct transform method in computation. There are practical limitations, however, as to how a high frequency and accurate estimate can be made for a given mean sampling rate. These high frequency estimates are important in obtaining the microscale information of turbulence structure. It was found from previous studies that reliable spectral estimates can be made up to about the mean sampling frequency (mean data rate) or less. If the data were evenly samples, the frequency range would be half the sampling frequency (i.e. up to Nyquist frequency); otherwise, aliasing problem would occur. The mean data rate and the sample size (total number of points) basically limit the frequency range. Also, there are large variabilities or errors associated with the high frequency estimates from randomly sampled signals. Roberts and Ajmani proposed certain pre-filtering techniques to reduce these variabilities, but at the cost of low frequency estimates. The prefiltering acts as a high-pass filter. Further, Shapiro and Silverman showed theoretically that, for Poisson sampled signals, it is possible to obtain alias-free spectral estimates far beyond the mean sampling frequency. But the question is, how far? During his tenure under 1993 NASA-ASEE Summer Faculty Fellowship Program, the author investigated from his studies on the spectral analysis techniques for randomly sampled signals that the spectral estimates can be enhanced or improved up to about 4-5 times the mean sampling frequency by using a suitable

  9. 40 CFR 600.112-08 - Exhaust sample analysis.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 31 2013-07-01 2013-07-01 false Exhaust sample analysis. 600.112-08 Section 600.112-08 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) ENERGY POLICY FUEL ECONOMY AND GREENHOUSE GAS EXHAUST EMISSIONS OF MOTOR VEHICLES Fuel Economy and...

  10. 40 CFR 600.112-08 - Exhaust sample analysis.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 31 2012-07-01 2012-07-01 false Exhaust sample analysis. 600.112-08 Section 600.112-08 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) ENERGY POLICY FUEL ECONOMY AND GREENHOUSE GAS EXHAUST EMISSIONS OF MOTOR VEHICLES Fuel Economy and...

  11. 400 area secondary cooling water sampling and analysis plan

    SciTech Connect

    Penn, L.L.

    1996-10-29

    This is a total rewrite of the Sampling and Analysis Plan in response to, and to ensure compliance with, the State Waste Discharge Permit ST 4501 issued on July 31, 1996. This revision describes changes in facility status and implements requirements of the permit.

  12. Rapid Screening of Complex Chemical Samples via Capillary Array Analysis

    SciTech Connect

    D. S. Anex; D. W. Neyer

    1998-11-01

    This report is a summary of the results of a two-year Laboratory-Directed Research and Development (LDRD) project that developed instrumentation and methods for capillary array analysis. During the course of this project, a new capillary array electrochromatography instrument was developed to perform eight simultaneous separations and provide complementary chromatographic information from each column on a single sample.

  13. 40 CFR 600.112-08 - Exhaust sample analysis.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 30 2014-07-01 2014-07-01 false Exhaust sample analysis. 600.112-08 Section 600.112-08 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) ENERGY POLICY FUEL ECONOMY AND GREENHOUSE GAS EXHAUST EMISSIONS OF MOTOR VEHICLES Fuel Economy and...

  14. Analysis of flavonoids in foods and biological samples.

    PubMed

    Gonzalez-Paramas, A M; Santos-Buelga, C; Duenas, M; Gonzalez-Manzano, S

    2011-12-01

    Flavonoids are a major class of plant phenolics that are widely distributed in the human diet and have been related to health promotion. They may occur in their natural sources in free forms (aglycones), as glycosylated or acylated derivatives, or as oligomeric and polymerized structures. This structural diversity affects their physicochemical behaviour and complicates their analysis. Thus, there is not a single standardized procedure that can be recommended for all flavonoid groups and/or type of samples, and the procedures have to be optimized depending on the nature of the sample and the target analytes. Furthermore, when dealing with the analysis of flavonoids biological samples (i.e., human and animal fluids and tissues) some differential aspects have to be taken into account; the nature of the compounds that can be found in those samples may differ from that present in plants and food, and flavonoids and metabolites occur in much lower concentrations, which make their analysis still more challenging. In this review the main techniques for extraction and analysis of flavonoids in foodstuffs and biological fluids are revised, as well as their occurrence in foods and beverages and available databases.

  15. METHODS FOR THE ANALYSIS OF CARPET SAMPLES FOR ASBESTOS

    EPA Science Inventory

    Assessing asbestos fiber contamination in a carpet is complicated by the nature of the carpeting – because of the pile’s rough surface and thickness, samples cannot be collected directly from carpet for analysis by TEM. Two indirect methods are currently used by laboratories when...

  16. Air sampling and analysis in a rubber vulcanization area.

    PubMed

    Rappaport, S M; Fraser, D A

    1977-05-01

    Results of sampling and analysis of air in a rubber vulcanization area are described. Organic compounds were collected on activated charcoal, desorbed with carbon disulfide and analyzed by gas chromatography. Several previously identified substances were quantitated, including styrene, toluene, ethylbenzene, and several oligomers of 1,3-butadiene. Concentrations ranged from 0.007 to 1.1 ppm.

  17. Language Sample Analysis: The Wisconsin Guide. Bulletin 92424.

    ERIC Educational Resources Information Center

    Leadholm, Barbara J.; Miller, Jon F.

    This publication discusses the role of Language Sample Analysis (LSA) in identifying language disorders, providing detail necessary to initiate a focused intervention program, and providing a method for monitoring progress in language intervention. Section 1 provides an overview of the LSA process and types of language disorders, while Section 2…

  18. The Precision Efficacy Analysis for Regression Sample Size Method.

    ERIC Educational Resources Information Center

    Brooks, Gordon P.; Barcikowski, Robert S.

    The general purpose of this study was to examine the efficiency of the Precision Efficacy Analysis for Regression (PEAR) method for choosing appropriate sample sizes in regression studies used for precision. The PEAR method, which is based on the algebraic manipulation of an accepted cross-validity formula, essentially uses an effect size to…

  19. Modern Numerical Methods for Classical Sampled System Analysis-SAMSAN

    NASA Technical Reports Server (NTRS)

    Frisch, H. P.

    1984-01-01

    SAMSAN aids control-system analyst by providing self-consistent set of computer algorithms that support large-order control-system design and evaluation studies, with emphasis placed on sampled system analysis. Program provides set of algorithms readily integrated for solving control-system problems.

  20. Numerical Methods for Classical Sampled-System Analysis

    NASA Technical Reports Server (NTRS)

    Frisch, H. P.; Bauer, F. H.

    1986-01-01

    SAMSAN provides control-system analyst with self-consistent computer algorithms that support large-order control-system design and evaluation studies. Emphasizes sampled-system analysis. SAMSAN reduces burden on analyst by providing set of algorithms well tested and documented and readily integrated for solving control-system problems.

  1. 40 CFR 600.112-08 - Exhaust sample analysis.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... FUEL ECONOMY AND CARBON-RELATED EXHAUST EMISSIONS OF MOTOR VEHICLES Fuel Economy and Carbon-Related Exhaust Emission Regulations for 1978 and Later Model Year Automobiles-Test Procedures § 600.112-08... 40 Protection of Environment 30 2011-07-01 2011-07-01 false Exhaust sample analysis....

  2. 40 CFR 600.112-78 - Exhaust sample analysis.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... FUEL ECONOMY AND CARBON-RELATED EXHAUST EMISSIONS OF MOTOR VEHICLES Fuel Economy and Carbon-Related Exhaust Emission Regulations for 1978 and Later Model Year Automobiles-Test Procedures § 600.112-78... 40 Protection of Environment 30 2011-07-01 2011-07-01 false Exhaust sample analysis....

  3. Entry Dispersion Analysis for the Genesis Sample Return Capsule

    NASA Technical Reports Server (NTRS)

    Desai, Prasun N.; Cheatwood, F. McNeil

    2005-01-01

    Genesis will be the first mission to return samples from beyond the Earth-Moon system. The spacecraft will be inserted into a halo orbit about the L1 (Sun-Earth) libration point where it will remain for two years collecting solar wind particles. Upon Earth return, the sample return capsule, which is passively controlled, will descend under parachute to Utah. The present study describes the analysis of the entry, descent, and landing scenario of the returning sample capsule. The robustness of the entry sequence is assessed through a Monte Carlo dispersion analysis where the impact of off-nominal conditions is ascertained. The dispersion results indicate that the capsule attitude excursions near peak heating and drogue chute deployment are within Genesis mission limits. Additionally, the size of the resulting 3-sigma landing ellipse is 47.8 km in downrange by 15.2 km in crossrange, which is within the Utah Test and Training Range boundaries.

  4. Entry Dispersion Analysis for the Genesis Sample Return Capsule

    NASA Technical Reports Server (NTRS)

    Desai, Prasun N.; Cheatwood, F. McNeil

    1999-01-01

    Genesis will be the first mission to return samples from beyond the Earth-Moon system. The spacecraft will be inserted into a halo orbit about the L1 (Sun- Earth) libration point where it will remain for two years collecting solar wind particles. Upon Earth return, the sample return capsule, which is passively controlled, will descend under parachute to Utah. The present study describes the analysis of the entry, descent, and landing scenario of the returning sample capsule. The robustness of the entry sequence is assessed through a Monte Carlo dispersion analysis where the impact of off-nominal conditions is ascertained. The dispersion results indicate that the capsule attitude excursions near peak heating and drogue chute deployment are within Genesis mission limits. Additionally, the size of the resulting 3-sigma landing ellipse is 47.8 km in downrange by 15.2 km in crossrange, which is within the Utah Test and Training Range boundaries.

  5. Entry Dispersion Analysis for the Genesis Sample Return Capsule

    NASA Technical Reports Server (NTRS)

    Desai, Prasun, N.; Cheatwood, F. McNeil

    1999-01-01

    Genesis will be the first mission to return samples from beyond the Earth-Moon system. The spacecraft will be inserted into a halo orbit about the L1 (Sun- Earth) libration point where it will remain for two years collecting solar wind particles. Upon Earth return, the sample return capsule, which is passively controlled, will descend under parachute to Utah. The present study describes the analysis of the entry, descent, and landing scenario of the returning sample cap- sule. The robustness of the entry sequence is assessed through a Monte Carlo dispersion analysis where the impact of off-nominal conditions is ascertained. The dispersion results indicate that the capsule attitude excursions near peak heating and drogue chute deployment are within Genesis mission limits. Additionally, the size of the resulting 3-sigma landing ellipse is 47.8 km in downrange by 15.2 km in crossrange, which is within the Utah Test and Training Range boundaries.

  6. Power and Sample Size Calculations for Contrast Analysis in ANCOVA.

    PubMed

    Shieh, Gwowen

    2017-01-01

    Analysis of covariance (ANCOVA) is commonly used in behavioral and educational research to reduce the error variance and improve the power of analysis of variance by adjusting the covariate effects. For planning and evaluating randomized ANCOVA designs, a simple sample-size formula has been proposed to account for the variance deflation factor in the comparison of two treatment groups. The objective of this article is to highlight an overlooked and potential problem of the exiting approximation and to provide an alternative and exact solution of power and sample size assessments for testing treatment contrasts. Numerical investigations are conducted to reveal the relative performance of the two procedures as a reliable technique to accommodate the covariate features that make ANCOVA design particularly distinctive. The described approach has important advantages over the current method in general applicability, methodological justification, and overall accuracy. To enhance the practical usefulness, computer algorithms are presented to implement the recommended power calculations and sample-size determinations.

  7. Statistical Analysis of Tank 5 Floor Sample Results

    SciTech Connect

    Shine, E. P.

    2013-01-31

    Sampling has been completed for the characterization of the residual material on the floor of Tank 5 in the F-Area Tank Farm at the Savannah River Site (SRS), near Aiken, SC. The sampling was performed by Savannah River Remediation (SRR) LLC using a stratified random sampling plan with volume-proportional compositing. The plan consisted of partitioning the residual material on the floor of Tank 5 into three non-overlapping strata: two strata enclosed accumulations, and a third stratum consisted of a thin layer of material outside the regions of the two accumulations. Each of three composite samples was constructed from five primary sample locations of residual material on the floor of Tank 5. Three of the primary samples were obtained from the stratum containing the thin layer of material, and one primary sample was obtained from each of the two strata containing an accumulation. This report documents the statistical analyses of the analytical results for the composite samples. The objective of the analysis is to determine the mean concentrations and upper 95% confidence (UCL95) bounds for the mean concentrations for a set of analytes in the tank residuals. The statistical procedures employed in the analyses were consistent with the Environmental Protection Agency (EPA) technical guidance by Singh and others [2010]. Savannah River National Laboratory (SRNL) measured the sample bulk density, nonvolatile beta, gross alpha, and the radionuclide1, elemental, and chemical concentrations three times for each of the composite samples. The analyte concentration data were partitioned into three separate groups for further analysis: analytes with every measurement above their minimum detectable concentrations (MDCs), analytes with no measurements above their MDCs, and analytes with a mixture of some measurement results above and below their MDCs. The means, standard deviations, and UCL95s were computed for the analytes in the two groups that had at least some measurements

  8. STATISTICAL ANALYSIS OF TANK 5 FLOOR SAMPLE RESULTS

    SciTech Connect

    Shine, E.

    2012-03-14

    Sampling has been completed for the characterization of the residual material on the floor of Tank 5 in the F-Area Tank Farm at the Savannah River Site (SRS), near Aiken, SC. The sampling was performed by Savannah River Remediation (SRR) LLC using a stratified random sampling plan with volume-proportional compositing. The plan consisted of partitioning the residual material on the floor of Tank 5 into three non-overlapping strata: two strata enclosed accumulations, and a third stratum consisted of a thin layer of material outside the regions of the two accumulations. Each of three composite samples was constructed from five primary sample locations of residual material on the floor of Tank 5. Three of the primary samples were obtained from the stratum containing the thin layer of material, and one primary sample was obtained from each of the two strata containing an accumulation. This report documents the statistical analyses of the analytical results for the composite samples. The objective of the analysis is to determine the mean concentrations and upper 95% confidence (UCL95) bounds for the mean concentrations for a set of analytes in the tank residuals. The statistical procedures employed in the analyses were consistent with the Environmental Protection Agency (EPA) technical guidance by Singh and others [2010]. Savannah River National Laboratory (SRNL) measured the sample bulk density, nonvolatile beta, gross alpha, radionuclide, inorganic, and anion concentrations three times for each of the composite samples. The analyte concentration data were partitioned into three separate groups for further analysis: analytes with every measurement above their minimum detectable concentrations (MDCs), analytes with no measurements above their MDCs, and analytes with a mixture of some measurement results above and below their MDCs. The means, standard deviations, and UCL95s were computed for the analytes in the two groups that had at least some measurements above their

  9. Statistical Analysis Of Tank 5 Floor Sample Results

    SciTech Connect

    Shine, E. P.

    2012-08-01

    Sampling has been completed for the characterization of the residual material on the floor of Tank 5 in the F-Area Tank Farm at the Savannah River Site (SRS), near Aiken, SC. The sampling was performed by Savannah River Remediation (SRR) LLC using a stratified random sampling plan with volume-proportional compositing. The plan consisted of partitioning the residual material on the floor of Tank 5 into three non-overlapping strata: two strata enclosed accumulations, and a third stratum consisted of a thin layer of material outside the regions of the two accumulations. Each of three composite samples was constructed from five primary sample locations of residual material on the floor of Tank 5. Three of the primary samples were obtained from the stratum containing the thin layer of material, and one primary sample was obtained from each of the two strata containing an accumulation. This report documents the statistical analyses of the analytical results for the composite samples. The objective of the analysis is to determine the mean concentrations and upper 95% confidence (UCL95) bounds for the mean concentrations for a set of analytes in the tank residuals. The statistical procedures employed in the analyses were consistent with the Environmental Protection Agency (EPA) technical guidance by Singh and others [2010]. Savannah River National Laboratory (SRNL) measured the sample bulk density, nonvolatile beta, gross alpha, and the radionuclide, elemental, and chemical concentrations three times for each of the composite samples. The analyte concentration data were partitioned into three separate groups for further analysis: analytes with every measurement above their minimum detectable concentrations (MDCs), analytes with no measurements above their MDCs, and analytes with a mixture of some measurement results above and below their MDCs. The means, standard deviations, and UCL95s were computed for the analytes in the two groups that had at least some measurements

  10. Optimized design and analysis of sparse-sampling FMRI experiments.

    PubMed

    Perrachione, Tyler K; Ghosh, Satrajit S

    2013-01-01

    Sparse-sampling is an important methodological advance in functional magnetic resonance imaging (fMRI), in which silent delays are introduced between MR volume acquisitions, allowing for the presentation of auditory stimuli without contamination by acoustic scanner noise and for overt vocal responses without motion-induced artifacts in the functional time series. As such, the sparse-sampling technique has become a mainstay of principled fMRI research into the cognitive and systems neuroscience of speech, language, hearing, and music. Despite being in use for over a decade, there has been little systematic investigation of the acquisition parameters, experimental design considerations, and statistical analysis approaches that bear on the results and interpretation of sparse-sampling fMRI experiments. In this report, we examined how design and analysis choices related to the duration of repetition time (TR) delay (an acquisition parameter), stimulation rate (an experimental design parameter), and model basis function (an analysis parameter) act independently and interactively to affect the neural activation profiles observed in fMRI. First, we conducted a series of computational simulations to explore the parameter space of sparse design and analysis with respect to these variables; second, we validated the results of these simulations in a series of sparse-sampling fMRI experiments. Overall, these experiments suggest the employment of three methodological approaches that can, in many situations, substantially improve the detection of neurophysiological response in sparse fMRI: (1) Sparse analyses should utilize a physiologically informed model that incorporates hemodynamic response convolution to reduce model error. (2) The design of sparse fMRI experiments should maintain a high rate of stimulus presentation to maximize effect size. (3) TR delays of short to intermediate length can be used between acquisitions of sparse-sampled functional image volumes to increase

  11. Micropyrolyzer for chemical analysis of liquid and solid samples

    DOEpatents

    Mowry, Curtis D.; Morgan, Catherine H.; Manginell, Ronald P.; Frye-Mason, Gregory C.

    2006-07-18

    A micropyrolyzer has applications to pyrolysis, heated chemistry, and thermal desorption from liquid or solid samples. The micropyrolyzer can be fabricated from semiconductor materials and metals using standard integrated circuit technologies. The micropyrolyzer enables very small volume samples of less than 3 microliters and high sample heating rates of greater than 20.degree. C. per millisecond. A portable analyzer for the field analysis of liquid and solid samples can be realized when the micropyrolyzer is combined with a chemical preconcentrator, chemical separator, and chemical detector. Such a portable analyzer can be used in a variety of government and industrial applications, such as non-proliferation monitoring, chemical and biological warfare detection, industrial process control, water and air quality monitoring, and industrial hygiene.

  12. ACCU Core Sampling/Storage Device for VOC Analysis

    SciTech Connect

    Susan S. Sorini; John F. Schabron; Mark M. Sanderson

    2007-04-30

    The Accu Core sampler system consists of alternating cylindrical clear acrylic sections and one-inch cylindrical stainless steel sections arranged in clear shrink wrap. The set of alternating acrylic and stainless steel sections in the shrink wrap are designed to fit in a Geoprobe dual-tube penetrometer for collection of continuous soil cores. The clear acrylic sections can have 1/2-inch access holes for easy soil headspace screening without violating the integrity of the adjacent stainless steel sections. The Accu Core sampler system can be used to store a soil sample collected in the stainless steel section by capping the ends of the section so it becomes a sample storage container. The sampler system can also be used to collect a subsurface soil sample in one of the sections that can be directly extruded from the section into a container for storage during shipment to the laboratory. In addition, the soil in a sampler section can be quickly sub-sampled using a coring tool and extruded into a storage container so the integrity of the soil is not disrupted and the potential for VOC loss during sub-sampling is greatly reduced. A field validation study was conducted to evaluate the performance of the Accu Core sampler to store VOC soil samples during transportation to the laboratory for analysis and to compare the performance of the Accu Core with current sampling and storage techniques, all of which require sub-sampling when the soil sample is brought to the surface. During some of the validation testing, the acrylic sections having access holes for headspace screening were included in the Accu Core sampler configuration and soil in these sections was screened to show the usefulness of the sample screening capability provided by the Accu Core system. This report presents the results of the field validation study as well as recommendations for the Accu Core sampler system.

  13. Design, data analysis and sampling techniques for clinical research.

    PubMed

    Suresh, Karthik; Thomas, Sanjeev V; Suresh, Geetha

    2011-10-01

    Statistical analysis is an essential technique that enables a medical research practitioner to draw meaningful inference from their data analysis. Improper application of study design and data analysis may render insufficient and improper results and conclusion. Converting a medical problem into a statistical hypothesis with appropriate methodological and logical design and then back-translating the statistical results into relevant medical knowledge is a real challenge. This article explains various sampling methods that can be appropriately used in medical research with different scenarios and challenges.

  14. Analysis of illicit drugs by direct ablation of solid samples.

    PubMed

    Bermúdez, Celina; Cabezas, Carlos; Mata, Santiago; Berdakin, Matias; Tejedor, Jesús M; Alonso, José L

    2015-01-01

    Analysis of illicit drugs arises as an important field of work given the high social impacts presented by drugs in the modern society. Direct laser ablation of solid compounds allows their analysis without sampling or preparation procedures. For that purpose, an experimental set-up that combines laser ablation with time-of- flight mass spectrometry has been constructed very recently to perform studies on the mass spectra of such drugs as 3,4-methylenedioxy-N-methylamphetamine, commonly known as MDMA or ecstasy. Analysis of the observed fragmentation pattern in mass spectra may elucidate the ablation-induced photofragmentation phenomena produced, which differ from those previously observed with conventional ionization methods.

  15. Microfluidic devices for DNA sequencing: sample preparation and electrophoretic analysis.

    PubMed

    Paegel, Brian M; Blazej, Robert G; Mathies, Richard A

    2003-02-01

    Modern DNA sequencing 'factories' have revolutionized biology by completing the human genome sequence, but in the race to completion we are left with inefficient, cumbersome, and costly macroscale processes and supporting facilities. During the same period, microfabricated DNA sequencing, sample processing and analysis devices have advanced rapidly toward the goal of a 'sequencing lab-on-a-chip'. Integrated microfluidic processing dramatically reduces analysis time and reagent consumption, and eliminates costly and unreliable macroscale robotics and laboratory apparatus. A microfabricated device for high-throughput DNA sequencing that couples clone isolation, template amplification, Sanger extension, purification, and electrophoretic analysis in a single microfluidic circuit is now attainable.

  16. Plural output optimetric sample cell and analysis system

    NASA Technical Reports Server (NTRS)

    Haley, F. C. (Inventor)

    1971-01-01

    An apparatus suitable for receiving a sample for optimetric analysis includes a sample cell comprising an opaque hollow tube. Several apertures are defined in the wall of the tubing and a lens barrel which extends beyond to opposite surfaces of the wall is supported within at least one of the apertures. A housing is provided with one channel for receiving the sample cell and a series of channels extending from the exterior housing to the sample cell apertures. A filter element is housed in each of these latter channels. These channels slidingly receive an excitation light source for a photodetector cell to permit selective focusing. A sample cell containing at least three apertures in the walls can be mounted for rotation relative to a light source or photoconduction means for simultaneous or alternative optimetric determination of the components of a single sample. The sample cell is fabricated by supporting a lens barrel within the aperture. A molten portion of glass is deposited in the lens barrel and cooled while in a horizontal position to form a lens having an acceptable angle.

  17. Enhanced Sampling and Analysis, Selection of Technology for Testing

    SciTech Connect

    Svoboda, John; Meikrantz, David

    2010-02-01

    The focus of this study includes the investigation of sampling technologies used in industry and their potential application to nuclear fuel processing. The goal is to identify innovative sampling methods using state of the art techniques that could evolve into the next generation sampling and analysis system for metallic elements. This report details the progress made in the first half of FY 2010 and includes a further consideration of the research focus and goals for this year. Our sampling options and focus for the next generation sampling method are presented along with the criteria used for choosing our path forward. We have decided to pursue the option of evaluating the feasibility of microcapillary based chips to remotely collect, transfer, track and supply microliters of sample solutions to analytical equipment in support of aqueous processes for used nuclear fuel cycles. Microchip vendors have been screened and a choice made for the development of a suitable microchip design followed by production of samples for evaluation by ANL, LANL, and INL on an independent basis.

  18. RAPID ANALYSIS OF EMERGENCY URINE AND WATER SAMPLES

    SciTech Connect

    Maxwell, S

    2007-02-26

    There is a need for fast, reliable methods for the determination of actinides and Sr-89/90 analysis on environmental and bioassay samples in response to an emergency radiological incident. The SRS (Savannah River Site) Environmental Bioassay Laboratory participated in the National Institute of Standards and Technology Radiochemistry Intercomparison Program (NRIP-06) and analyzed water and urine samples within 8 hours of receipt. The SRS Environmental Laboratory was the only lab that participated in the program that analyzed these samples for both actinides and Sr-89/90 within the requested 8 hour turnaround time. A new, rapid actinide and strontium 89/90 separation method was used for both urine and water samples. This method uses stacked TEVA Resin{reg_sign}, TRU Resin{reg_sign} and Sr-Resin{reg_sign} cartridges from Eichrom Technologies (Darien, IL, USA) that allows the rapid separation of plutonium (Pu), neptunium (Np), uranium (U), and americium (Am), curium (Cm) and thorium (Th) using a single multi-stage column combined with alpha spectrometry. By using vacuum box cartridge technology and stacked cartridges with rapid flow rates, sample preparation time was minimized. This paper discusses the technology and conditions employed for both water and urine samples and presents the SRS performance data on the NRIP-06 samples.

  19. Analysis of the Tank 6F Final Characterization Samples-2012

    SciTech Connect

    Oji, L. N.; Diprete, D. P.; Coleman, C. J.; Hay, M. S.; Shine, E. P.

    2013-01-31

    The Savannah River National Laboratory (SRNL) was requested by Savannah River Remediation (SRR) to provide sample preparation and analysis of the Tank 6F final characterization samples to determine the residual tank inventory prior to grouting. Fourteen residual Tank 6F solid samples from three areas on the floor of the tank were collected and delivered to SRNL between May and August 2011. These Tank 6F samples were homogenized and combined into three composite samples based on a proportion compositing scheme and the resulting composite samples were analyzed for radiological, chemical and elemental components. Additional measurements performed on the Tank 6F composite samples include bulk density and water leaching of the solids to account for water soluble components. The composite Tank 6F samples were analyzed and the data reported in triplicate. Sufficient quality assurance standards and blanks were utilized to demonstrate adequate characterization of the Tank 6F samples. The main evaluation criteria were target detection limits specified in the technical task request document. While many of the target detection limits were met for the species characterized for Tank 6F some were not met. In a few cases, the relatively high levels of radioactive species of the same element or a chemically similar element precluded the ability to measure some isotopes to low levels. The isotopes whose detection limits were not met in all cases included Sn-126, Sb-126, Sb-126m, Eu-152, Cm- 243 and Cf-249. SRNL, in conjunction with the customer, reviewed all of these cases and determined that the impacts of not meeting the target detection limits were acceptable. Based on the analyses of variance (ANOVA) for the inorganic constituents of Tank 6F, all the inorganic constituents displayed heterogeneity. The inorganic results demonstrated consistent differences across the composite samples: lowest concentrations for Composite Sample 1, intermediate-valued concentrations for Composite

  20. ANALYSIS OF THE TANK 6F FINAL CHARACTERIZATION SAMPLES-2012

    SciTech Connect

    Oji, L.; Diprete, D.; Coleman, C.; Hay, M.; Shine, G.

    2012-06-28

    The Savannah River National Laboratory (SRNL) was requested by Savannah River Remediation (SRR) to provide sample preparation and analysis of the Tank 6F final characterization samples to determine the residual tank inventory prior to grouting. Fourteen residual Tank 6F solid samples from three areas on the floor of the tank were collected and delivered to SRNL between May and August 2011. These Tank 6F samples were homogenized and combined into three composite samples based on a proportion compositing scheme and the resulting composite samples were analyzed for radiological, chemical and elemental components. Additional measurements performed on the Tank 6F composite samples include bulk density and water leaching of the solids to account for water soluble components. The composite Tank 6F samples were analyzed and the data reported in triplicate. Sufficient quality assurance standards and blanks were utilized to demonstrate adequate characterization of the Tank 6F samples. The main evaluation criteria were target detection limits specified in the technical task request document. While many of the target detection limits were met for the species characterized for Tank 6F some were not met. In a few cases, the relatively high levels of radioactive species of the same element or a chemically similar element precluded the ability to measure some isotopes to low levels. The isotopes whose detection limits were not met in all cases included Sn-126, Sb-126, Sb-126m, Eu-152, Cm-243 and Cf-249. SRNL, in conjunction with the customer, reviewed all of these cases and determined that the impacts of not meeting the target detection limits were acceptable. Based on the analyses of variance (ANOVA) for the inorganic constituents of Tank 6F, all the inorganic constituents displayed heterogeneity. The inorganic results demonstrated consistent differences across the composite samples: lowest concentrations for Composite Sample 1, intermediate-valued concentrations for Composite

  1. Analysis Of The Tank 6F Final Characterization Samples-2012

    SciTech Connect

    Oji, L. N.; Diprete, D. P.; Coleman, C. J.; Hay, M. S.; Shine, E. P.

    2012-09-27

    The Savannah River National Laboratory (SRNL) was requested by Savannah River Remediation (SRR) to provide sample preparation and analysis of the Tank 6F final characterization samples to determine the residual tank inventory prior to grouting. Fourteen residual Tank 6F solid samples from three areas on the floor of the tank were collected and delivered to SRNL between May and August 2011. These Tank 6F samples were homogenized and combined into three composite samples based on a proportion compositing scheme and the resulting composite samples were analyzed for radiological, chemical and elemental components. Additional measurements performed on the Tank 6F composite samples include bulk density and water leaching of the solids to account for water soluble components. The composite Tank 6F samples were analyzed and the data reported in triplicate. Sufficient quality assurance standards and blanks were utilized to demonstrate adequate characterization of the Tank 6F samples. The main evaluation criteria were target detection limits specified in the technical task request document. While many of the target detection limits were met for the species characterized for Tank 6F some were not met. In a few cases, the relatively high levels of radioactive species of the same element or a chemically similar element precluded the ability to measure some isotopes to low levels. The isotopes whose detection limits were not met in all cases included Sn-126, Sb-126, Sb-126m, Eu-152, Cm-243 and Cf-249. SRNL, in conjunction with the customer, reviewed all of these cases and determined that the impacts of not meeting the target detection limits were acceptable. Based on the analyses of variance (ANOVA) for the inorganic constituents of Tank 6F, all the inorganic constituents displayed heterogeneity. The inorganic results demonstrated consistent differences across the composite samples: lowest concentrations for Composite Sample 1, intermediate-valued concentrations for Composite

  2. Sampling and Analysis Plan for canister liquid and gas sampling at 105-KW fuel storage basin

    SciTech Connect

    Harris, R.A.; Green, M.A.; Makenas, B.J.; Trimble, D.J.

    1995-03-01

    This Sampling and Analysis Plan (SAP) details the sampling and analyses to be performed on fuel canisters transferred to the Weasel Pit of the 105-KW fuel storage basin. The radionuclide content of the liquid and gas in the canisters must be evaluated to support the shipment of fuel elements to the 300 Area in support of the fuel characterization studies (Abrefah, et al. 1994, Trimble 1995). The following sections provide background information and a description of the facility under investigation, discuss the existing site conditions, present the constituents of concern, outline the purpose and scope of the investigation, outline the data quality objectives (DQO), provide analytical detection limit, precision, and accuracy requirements, and address other quality assurance (QA) issues.

  3. Analysis of the Einstein sample of early-type galaxies

    NASA Technical Reports Server (NTRS)

    Eskridge, Paul B.; Fabbiano, Giuseppina

    1993-01-01

    The EINSTEIN galaxy catalog contains x-ray data for 148 early-type (E and SO) galaxies. A detailed analysis of the global properties of this sample are studied. By comparing the x-ray properties with other tracers of the ISM, as well as with observables related to the stellar dynamics and populations of the sample, we expect to determine more clearly the physical relationships that determine the evolution of early-type galaxies. Previous studies with smaller samples have explored the relationships between x-ray luminosity (L(sub x)) and luminosities in other bands. Using our larger sample and the statistical techniques of survival analysis, a number of these earlier analyses were repeated. For our full sample, a strong statistical correlation is found between L(sub X) and L(sub B) (the probability that the null hypothesis is upheld is P less than 10(exp -4) from a variety of rank correlation tests. Regressions with several algorithms yield consistent results.

  4. Consequences of sequential sampling for meta-analysis.

    PubMed

    Braschi, Lorenzo; Botella, Juan; Suero, Manuel

    2014-12-01

    Sequential stopping rules allow hypotheses to be tested using smaller sample sizes than are possible under conventional methods, while controlling the Type I and II error rates. However, the consequences of using such procedures when combining studies in a meta-analysis have rarely been discussed. For a primary study to be included in a meta-analysis, it must provide an estimate of the effect size, and it must be possible to calculate the variance of this estimate, which is used for weighting the study. It is therefore crucial to know whether the use of sequential stopping rules introduces any bias in the estimate of the effect size and/or modifies the variance of the estimate. In the present research, both aspects were studied for the CLAST rule, as applied to testing the difference between two means from paired samples, in a variety of scenarios of sample size and population effect size. The results show that although the bias is small, but still larger than that for the fixed-sample rule, the variance of the estimate is much higher with the CLAST sequential stopping rule. The implications of these results for the incorporation of such studies into meta-analyses are discussed. It is recommended to incorporate such studies into meta-analyses by taking only the information conveyed in the initial sample. The authors of primary studies employing sequential rules should report that information when publishing their results.

  5. Mercury Source Zone Identification using Soil Vapor Sampling and Analysis

    SciTech Connect

    Watson, David B; Miller, Carrie L; Lester, Brian P; Lowe, Kenneth Alan; Southworth, George R; Bogle, Mary Anna; Liang, Liyuan; Pierce, Eric M

    2014-01-01

    Development and demonstration of reliable measurement techniqes that can detect and help quantify the nature and extent of elemental mercury (Hg(0)) in the subsurface are needed to reduce certainties in the decision making process and increase the effectiveness of remedial actions. We conducted field tests at the Y-12 National Security Complex (NSC) in Oak Ridge, TN, to determine if sampling and analysis of Hg(0) vapors in the shallow subsurface (<0.3 m depth) can be used to as an indicator of the location and extent of Hg(0) releases in the subsurface. We constructed a rigid PVC pushprobe assembly, which was driven into the ground. Soil gas samples were collected through a sealed inner tube of the assembly and analyzed immediately in the field with a Lumex and/or Jerome Hg(0) analyzer. Time-series sampling showed that Hg vapor concentrations were fairly stable over time suggesting that the vapor phase Hg(0) was not being depleted and that sampling results were not dependent on the soil gas purge volume. Hg(0) vapor data collected at over 200 pushprobe locations at 3 different release sites correlated well to areas of known Hg(0) contamination. Vertical profiling of Hg(0) vapor concentrations conducted at 2 locations provided information on the vertical distribution of Hg(0) contamination in the subsurface. We concluded from our studies that soil gas sampling and analysis can be conducted rapidly and inexpensively at a large scale to help identify areas contaminated with Hg(0).

  6. A quarantine protocol for analysis of returned extraterrestrial samples

    NASA Technical Reports Server (NTRS)

    Bagby, J. R.; Sweet, H. C.; Devincenzi, D. L.

    1983-01-01

    A protocol is presented for the analysis at an earth-orbiting quarantine facility of return samples of extraterrestrial material that might contain (nonterrestrial) life forms. The protocol consists of a series of tests designed to determine whether the sample, conceptualized as a 1-kg sample of Martian soil, is free from nonterrestrial biologically active agents and so may safely be sent to a terrestrial containment facility, or it exhibits biological activity requiring further (second-order) testing outside the biosphere. The first-order testing procedure seeks to detect the presence of any replicating organisms or toxic substances through a series of experiments including gas sampling, analysis of radioactivity, stereomicroscopic inspection, chemical analysis, microscopic examination, the search for metabolic products under growth conditions, microbiologicl assays, and the challenge of cultured cells with any agents found or with the extraterrestrial material as is. Detailed plans for the second-order testing would be developed in response to the actual data received from primary testing.

  7. ANALYSIS OF THE TANK 5F FINAL CHARATERIZATION SAMPLES-2011

    SciTech Connect

    Oji, L.; Diprete, D.; Coleman, C.; Hay, M.

    2012-01-20

    The Savannah River National Laboratory (SRNL) was requested by SRR to provide sample preparation and analysis of the Tank 5F final characterization samples to determine the residual tank inventory prior to grouting. Two types of samples were collected and delivered to SRNL: floor samples across the tank and subsurface samples from mounds near risers 1 and 5 of Tank 5F. These samples were taken from Tank 5F between January and March 2011. These samples from individual locations in the tank (nine floor samples and six mound Tank 5F samples) were each homogenized and combined in a given proportion into 3 distinct composite samples to mimic the average composition in the entire tank. These Tank 5F composite samples were analyzed for radiological, chemical and elemental components. Additional measurements performed on the Tank 5F composite samples include bulk density and water leaching of the solids to account for water soluble species. With analyses for certain challenging radionuclides as the exception, all composite Tank 5F samples were analyzed and reported in triplicate. The target detection limits for isotopes analyzed were based on customer desired detection limits as specified in the technical task request documents. SRNL developed new methodologies to meet these target detection limits and provide data for the extensive suite of components. While many of the target detection limits were met for the species characterized for Tank 5F, as specified in the technical task request, some were not met. In a few cases, the relatively high levels of radioactive species of the same element or a chemically similar element precluded the ability to measure some isotopes to low levels. The Technical Task Request allows that while the analyses of these isotopes is needed, meeting the detection limits for these isotopes is a lower priority than meeting detection limits for the other specified isotopes. The isotopes whose detection limits were not met in all cases included the

  8. ANALYSIS OF THE TANK 5F FINAL CHARACTERIZATION SAMPLES-2011

    SciTech Connect

    Oji, L.; Diprete, D.; Coleman, C.; Hay, M.

    2012-08-03

    The Savannah River National Laboratory (SRNL) was requested by SRR to provide sample preparation and analysis of the Tank 5F final characterization samples to determine the residual tank inventory prior to grouting. Two types of samples were collected and delivered to SRNL: floor samples across the tank and subsurface samples from mounds near risers 1 and 5 of Tank 5F. These samples were taken from Tank 5F between January and March 2011. These samples from individual locations in the tank (nine floor samples and six mound Tank 5F samples) were each homogenized and combined in a given proportion into 3 distinct composite samples to mimic the average composition in the entire tank. These Tank 5F composite samples were analyzed for radiological, chemical and elemental components. Additional measurements performed on the Tank 5F composite samples include bulk density and water leaching of the solids to account for water soluble species. With analyses for certain challenging radionuclides as the exception, all composite Tank 5F samples were analyzed and reported in triplicate. The target detection limits for isotopes analyzed were based on customer desired detection limits as specified in the technical task request documents. SRNL developed new methodologies to meet these target detection limits and provide data for the extensive suite of components. While many of the target detection limits were met for the species characterized for Tank 5F, as specified in the technical task request, some were not met. In a few cases, the relatively high levels of radioactive species of the same element or a chemically similar element precluded the ability to measure some isotopes to low levels. The Technical Task Request allows that while the analyses of these isotopes is needed, meeting the detection limits for these isotopes is a lower priority than meeting detection limits for the other specified isotopes. The isotopes whose detection limits were not met in all cases included the

  9. Analysis Of The Tank 5F Final Characterization Samples-2011

    SciTech Connect

    Oji, L. N.; Diprete, D.; Coleman, C. J.; Hay, M. S.

    2012-09-27

    The Savannah River National Laboratory (SRNL) was requested by SRR to provide sample preparation and analysis of the Tank 5F final characterization samples to determine the residual tank inventory prior to grouting. Two types of samples were collected and delivered to SRNL: floor samples across the tank and subsurface samples from mounds near risers 1 and 5 of Tank 5F. These samples were taken from Tank 5F between January and March 2011. These samples from individual locations in the tank (nine floor samples and six mound Tank 5F samples) were each homogenized and combined in a given proportion into 3 distinct composite samples to mimic the average composition in the entire tank. These Tank 5F composite samples were analyzed for radiological, chemical and elemental components. Additional measurements performed on the Tank 5F composite samples include bulk density and water leaching of the solids to account for water soluble species. With analyses for certain challenging radionuclides as the exception, all composite Tank 5F samples were analyzed and reported in triplicate. The target detection limits for isotopes analyzed were based on customer desired detection limits as specified in the technical task request documents. SRNL developed new methodologies to meet these target detection limits and provide data for the extensive suite of components. While many of the target detection limits were met for the species characterized for Tank 5F, as specified in the technical task request, some were not met. In a few cases, the relatively high levels of radioactive species of the same element or a chemically similar element precluded the ability to measure some isotopes to low levels. The Technical Task Request allows that while the analyses of these isotopes is needed, meeting the detection limits for these isotopes is a lower priority than meeting detection limits for the other specified isotopes. The isotopes whose detection limits were not met in all cases included the

  10. Accuracy of remotely sensed data: Sampling and analysis procedures

    NASA Technical Reports Server (NTRS)

    Congalton, R. G.; Oderwald, R. G.; Mead, R. A.

    1982-01-01

    A review and update of the discrete multivariate analysis techniques used for accuracy assessment is given. A listing of the computer program written to implement these techniques is given. New work on evaluating accuracy assessment using Monte Carlo simulation with different sampling schemes is given. The results of matrices from the mapping effort of the San Juan National Forest is given. A method for estimating the sample size requirements for implementing the accuracy assessment procedures is given. A proposed method for determining the reliability of change detection between two maps of the same area produced at different times is given.

  11. Sampling and Analysis Plan - Waste Treatment Plant Seismic Boreholes Project

    SciTech Connect

    Reidel, Steve P.

    2006-05-26

    This sampling and analysis plan (SAP) describes planned data collection activities for four entry boreholes through the sediment overlying the basalt, up to three new deep rotary boreholes through the basalt and sedimentary interbeds, and one corehole through the basalt and sedimentary interbeds at the Waste Treatment Plant (WTP) site. The SAP will be used in concert with the quality assurance plan for the project to guide the procedure development and data collection activities needed to support borehole drilling, geophysical measurements, and sampling. This SAP identifies the American Society of Testing Materials standards, Hanford Site procedures, and other guidance to be followed for data collection activities.

  12. Proteome Analysis of Human Perilymph using an Intraoperative Sampling Method.

    PubMed

    Schmitt, Heike Andrea; Pich, Andreas; Schröder, Anke; Scheper, Verena; Lilli, Giorgio; Reuter, Günter; Lenarz, Thomas

    2017-03-10

    The knowledge about the etiology and pathophysiology of sensorineural hearing loss (SNHL) is still very limited. The project aims at the improvement of understanding different types of SNHL by proteome analysis of human perilymph. Sampling of perilymph has been established during inner ear surgeries (cochlear implant and vestibular schwannoma surgeries) and safety of the sampling method was determined by pure tone audiometry. An in-depth shot-gun proteomics approach was performed to identify cochlear proteins and individual proteome in perilymph of patients. This method enables the identification and quantification of protein composition of perilymph. The proteome of 41 collected perilymph samples with volumes of 1-12 µl was analyzed by data dependent acquisition resulting in overall 878 detected protein groups. At least 203 protein groups were solely identified in perilymph, not in reference samples (serum, cerebrospinal fluid), displaying a specific protein pattern for perilymph. Samples were grouped according to age of patients and type of surgery leading to identification of some proteins specific to particular subgroups. Proteins with different abundances between different sample groups were subjected to classification by gene ontology annotations. The identified proteins might be used to develop tools for non-invasive inner ear diagnostics and to elucidate molecular profiles of SNHL.

  13. A geostatistical and sampling analysis of regraded spoil materials

    SciTech Connect

    Myers, J.C.; Brown, T.H.

    1990-12-31

    Characterization of the pH and acid-base account levels in regraded spoil materials from mining operations is a difficult task due to mixing and the directional nature of product extraction. Geostatistical analysis of regraded spoil materials is currently being studied as the eventual methodology for determining sample grid size and sub-sample number for minesoil monitoring programs in the State of Texas. It is anticipated that geostatistics will soon be utilized for similar reasons at mine sites in other regions. In view of this, it is necessary to develop a position on geostatistics as a method for determining sample intensity necessary to statistically characterize Acid Forming Material (AFM) conditions existing in post-mined soils. A group of six Texas lignite mines has been analyzed using geostatistical methods. Acid-base account and pH values were mapped at four levels in each site. Determinations as to the confidence of the sampling programs were performed for all sites. Recommendations and strategies were developed for future sampling programs. Additional techniques to minimize sub-sample spacing were also developed.

  14. The Sample Analysis at Mars Investigation and Instrument Suite

    NASA Technical Reports Server (NTRS)

    Mahaffy, Paul; Webster, Christopher R.; Conrad, Pamela G.; Arvey, Robert; Bleacher, Lora; Brinckerhoff, William B.; Eigenbrode, Jennifer L.; Chalmers, Robert A.; Dworkin, Jason P.; Errigo, Therese; Farley, Rodger; Feng, Steven; Frazier, Gregory; Glavin, Daniel P.; Harpold, Daniel N.; Jordan, Partick; Kellogg, James; Lewis, Jesse; Martin, David K.; Maurer, John; McAdam, Amy C.; McLennan, Douglas; Pavlov, Alexander A.; Raaen, Eric; Schinman, Oren

    2012-01-01

    The Sample Analysis at Mars (SAM) investigation of the Mars Science Laboratory (MSL) addresses the chemical and isotopic composition of the atmosphere and volatiles extracted from solid samples. The SAM investigation is designed to contribute substantially to the mission goal of quantitatively assessing the habitability of Mars as an essential step in the search for past or present life on Mars. SAM is a 40 kg instrument suite located in the interior of MSL's Curiosity rover. The SAM instruments are a quadrupole mass spectrometer, a tunable laser spectrometer, and a 6-column gas chromatograph all coupled through solid and gas processing systems to provide complementary information on the same samples. The SAM suite is able to measure a suite of light isotopes and to analyze volatiles directly from the atmosphere or thermally released from solid samples. In addition to measurements of simple inorganic compounds and noble gases SAM will conduct a sensitive search for organic compounds with either thermal or chemical extraction from sieved samples delivered by the sample processing system on the Curiosity rover's robotic arm,

  15. The Sample Analysis at Mars Investigation and Instrument Suite

    NASA Technical Reports Server (NTRS)

    Mahaffy, Paul; Webster, Chris R.; Cabane, M.; Conrad, Pamela G.; Coll, Patrice; Atreya, Sushil K.; Arvey, Robert; Barciniak, Michael; Benna, Mehdi; Bleacher, L.; Brinckerhoff, William B.; Eigenbrode, Jennifer L.; Carignan, Daniel; Cascia, Mark; Chalmers, Robert A.; Dworkin, Jason P.; Errigo, Therese; Everson, Paula; Franz, Heather; Farley, Rodger; Feng, Steven; Frazier, Gregory; Freissinet, Caroline; Glavin, Daniel P.; Harpold, Daniel N.

    2012-01-01

    The Sample Analysis at Mars (SAM) investigation of the Mars Science Laboratory(MSL) addresses the chemical and isotopic composition of the atmosphere and volatilesextracted from solid samples. The SAM investigation is designed to contribute substantiallyto the mission goal of quantitatively assessing the habitability of Mars as an essentialstep in the search for past or present life on Mars. SAM is a 40 kg instrument suite locatedin the interior of MSLs Curiosity rover. The SAM instruments are a quadrupole massspectrometer, a tunable laser spectrometer, and a 6-column gas chromatograph all coupledthrough solid and gas processing systems to provide complementary information on thesame samples. The SAM suite is able to measure a suite of light isotopes and to analyzevolatiles directly from the atmosphere or thermally released from solid samples. In additionto measurements of simple inorganic compounds and noble gases SAM will conducta sensitive search for organic compounds with either thermal or chemical extraction fromsieved samples delivered by the sample processing system on the Curiosity rovers roboticarm.

  16. UMTRA project water sampling and analysis plan, Monument Valley, Arizona

    SciTech Connect

    Not Available

    1994-04-01

    The Monument Valley Uranium Mill Tailings Remedial Action (UMTRA) Project site in Cane Valley is a former uranium mill that has undergone surface remediation in the form of tailings and contaminated materials removal. Contaminated materials from the Monument Valley (Arizona) UMTRA Project site have been transported to the Mexican Hat (Utah) UMTRA Project site for consolidation with the Mexican Hat tailings. Tailings removal was completed in February 1994. Three geologic units at the site contain water: the unconsolidated eolian and alluvial deposits (alluvial aquifer), the Shinarump Conglomerate (Shinarump Member), and the De Chelly Sandstone. Water quality analyses indicate the contaminant plume has migrated north of the site and is mainly in the alluvial aquifer. An upward hydraulic gradient in the De Chelly Sandstone provides some protection to that aquifer. This water sampling and analysis plan recommends sampling domestic wells, monitor wells, and surface water in April and September 1994. The purpose of sampling is to continue periodic monitoring for the surface program, evaluate changes to water quality for site characterization, and provide data for the baseline risk assessment. Samples taken in April will be representative of high ground water levels and samples taken in September will be representative of low ground water levels. Filtered and nonfiltered samples will be analyzed for plume indicator parameters and baseline risk assessment parameters.

  17. Conservative Sample Size Determination for Repeated Measures Analysis of Covariance.

    PubMed

    Morgan, Timothy M; Case, L Douglas

    2013-07-05

    In the design of a randomized clinical trial with one pre and multiple post randomized assessments of the outcome variable, one needs to account for the repeated measures in determining the appropriate sample size. Unfortunately, one seldom has a good estimate of the variance of the outcome measure, let alone the correlations among the measurements over time. We show how sample sizes can be calculated by making conservative assumptions regarding the correlations for a variety of covariance structures. The most conservative choice for the correlation depends on the covariance structure and the number of repeated measures. In the absence of good estimates of the correlations, the sample size is often based on a two-sample t-test, making the 'ultra' conservative and unrealistic assumption that there are zero correlations between the baseline and follow-up measures while at the same time assuming there are perfect correlations between the follow-up measures. Compared to the case of taking a single measurement, substantial savings in sample size can be realized by accounting for the repeated measures, even with very conservative assumptions regarding the parameters of the assumed correlation matrix. Assuming compound symmetry, the sample size from the two-sample t-test calculation can be reduced at least 44%, 56%, and 61% for repeated measures analysis of covariance by taking 2, 3, and 4 follow-up measures, respectively. The results offer a rational basis for determining a fairly conservative, yet efficient, sample size for clinical trials with repeated measures and a baseline value.

  18. Efficient Coalescent Simulation and Genealogical Analysis for Large Sample Sizes

    PubMed Central

    Kelleher, Jerome; Etheridge, Alison M; McVean, Gilean

    2016-01-01

    A central challenge in the analysis of genetic variation is to provide realistic genome simulation across millions of samples. Present day coalescent simulations do not scale well, or use approximations that fail to capture important long-range linkage properties. Analysing the results of simulations also presents a substantial challenge, as current methods to store genealogies consume a great deal of space, are slow to parse and do not take advantage of shared structure in correlated trees. We solve these problems by introducing sparse trees and coalescence records as the key units of genealogical analysis. Using these tools, exact simulation of the coalescent with recombination for chromosome-sized regions over hundreds of thousands of samples is possible, and substantially faster than present-day approximate methods. We can also analyse the results orders of magnitude more quickly than with existing methods. PMID:27145223

  19. Proteomic analysis of tissue samples in translational breast cancer research.

    PubMed

    Gromov, Pavel; Moreira, José M A; Gromova, Irina

    2014-06-01

    In the last decade, many proteomic technologies have been applied, with varying success, to the study of tissue samples of breast carcinoma for protein expression profiling in order to discover protein biomarkers/signatures suitable for: characterization and subtyping of tumors; early diagnosis, and both prognosis and prediction of outcome of chemotherapy. The purpose of this review is to critically appraise what has been achieved to date using proteomic technologies and to bring forward novel strategies - based on the analysis of clinically relevant samples - that promise to accelerate the translation of basic discoveries into the daily breast cancer clinical practice. In particular, we address major issues in experimental design by reviewing the strengths and weaknesses of current proteomic strategies in the context of the analysis of human breast tissue specimens.

  20. Landscape Characterization and Representativeness Analysis for Understanding Sampling Network Coverage

    SciTech Connect

    Maddalena, Damian; Hoffman, Forrest; Kumar, Jitendra; Hargrove, William

    2014-08-01

    Sampling networks rarely conform to spatial and temporal ideals, often comprised of network sampling points which are unevenly distributed and located in less than ideal locations due to access constraints, budget limitations, or political conflict. Quantifying the global, regional, and temporal representativeness of these networks by quantifying the coverage of network infrastructure highlights the capabilities and limitations of the data collected, facilitates upscaling and downscaling for modeling purposes, and improves the planning efforts for future infrastructure investment under current conditions and future modeled scenarios. The work presented here utilizes multivariate spatiotemporal clustering analysis and representativeness analysis for quantitative landscape characterization and assessment of the Fluxnet, RAINFOR, and ForestGEO networks. Results include ecoregions that highlight patterns of bioclimatic, topographic, and edaphic variables and quantitative representativeness maps of individual and combined networks.

  1. Informational Analysis for Compressive Sampling in Radar Imaging

    PubMed Central

    Zhang, Jingxiong; Yang, Ke

    2015-01-01

    Compressive sampling or compressed sensing (CS) works on the assumption of the sparsity or compressibility of the underlying signal, relies on the trans-informational capability of the measurement matrix employed and the resultant measurements, operates with optimization-based algorithms for signal reconstruction and is thus able to complete data compression, while acquiring data, leading to sub-Nyquist sampling strategies that promote efficiency in data acquisition, while ensuring certain accuracy criteria. Information theory provides a framework complementary to classic CS theory for analyzing information mechanisms and for determining the necessary number of measurements in a CS environment, such as CS-radar, a radar sensor conceptualized or designed with CS principles and techniques. Despite increasing awareness of information-theoretic perspectives on CS-radar, reported research has been rare. This paper seeks to bridge the gap in the interdisciplinary area of CS, radar and information theory by analyzing information flows in CS-radar from sparse scenes to measurements and determining sub-Nyquist sampling rates necessary for scene reconstruction within certain distortion thresholds, given differing scene sparsity and average per-sample signal-to-noise ratios (SNRs). Simulated studies were performed to complement and validate the information-theoretic analysis. The combined strategy proposed in this paper is valuable for information-theoretic orientated CS-radar system analysis and performance evaluation. PMID:25811226

  2. Contemporary Impact Analysis Methodology for Planetary Sample Return Missions

    NASA Technical Reports Server (NTRS)

    Perino, Scott V.; Bayandor, Javid; Samareh, Jamshid A.; Armand, Sasan C.

    2015-01-01

    Development of an Earth entry vehicle and the methodology created to evaluate the vehicle's impact landing response when returning to Earth is reported. NASA's future Mars Sample Return Mission requires a robust vehicle to return Martian samples back to Earth for analysis. The Earth entry vehicle is a proposed solution to this Mars mission requirement. During Earth reentry, the vehicle slows within the atmosphere and then impacts the ground at its terminal velocity. To protect the Martian samples, a spherical energy absorber called an impact sphere is under development. The impact sphere is composed of hybrid composite and crushable foam elements that endure large plastic deformations during impact and cause a highly nonlinear vehicle response. The developed analysis methodology captures a range of complex structural interactions and much of the failure physics that occurs during impact. Numerical models were created and benchmarked against experimental tests conducted at NASA Langley Research Center. The postimpact structural damage assessment showed close correlation between simulation predictions and experimental results. Acceleration, velocity, displacement, damage modes, and failure mechanisms were all effectively captured. These investigations demonstrate that the Earth entry vehicle has great potential in facilitating future sample return missions.

  3. Sampling and Analysis Plan Waste Treatment Plant Seismic Boreholes Project.

    SciTech Connect

    Brouns, Thomas M.

    2007-07-15

    This sampling and analysis plan (SAP) describes planned data collection activities for four entry boreholes through the sediment overlying the Saddle Mountains Basalt, up to three new deep rotary boreholes through the Saddle Mountains Basalt and sedimentary interbeds, and one corehole through the Saddle Mountains Basalt and sedimentary interbeds at the Waste Treatment Plant (WTP) site. The SAP will be used in concert with the quality assurance plan for the project to guide the procedure development and data collection activities needed to support borehole drilling, geophysical measurements, and sampling. This SAP identifies the American Society of Testing Materials standards, Hanford Site procedures, and other guidance to be followed for data collection activities. Revision 3 incorporates all interim change notices (ICN) that were issued to Revision 2 prior to completion of sampling and analysis activities for the WTP Seismic Boreholes Project. This revision also incorporates changes to the exact number of samples submitted for dynamic testing as directed by the U.S. Army Corps of Engineers. Revision 3 represents the final version of the SAP.

  4. Loop flow analysis of dissolved reactive phosphorus in aqueous samples.

    PubMed

    Ma, Jian; Li, Quanlong; Yuan, Dongxing

    2014-06-01

    The current flow based method for the determination of dissolved reactive phosphorus (DRP) suffers interference from salinity (e.g. index refractive difference) and the incidentally formed bubbles, which can be a problem for optical detection. Here we reported a simple and robust loop flow analysis (LFA) method for accurate measurement of DRP in different aqueous samples. The chemistry is based on the classic phosphomolybdenum blue (PMB) reaction and the PMB formed in a novel cross-shaped flow cell was detected at 700 nm using a miniature spectrophotometer. The effects of reagents on the kinetic formation of PMB were evaluated. The detection limit was 32 nM with an optical pathlength of 1cm and the relative standard deviations for repetitive determinations of 1, 2 and 8 µM phosphate solutions were 1.8% (n=113, without any stoppage during repeating analysis for >7h), 1.0% (n=49) and 0.39% (n=9), respectively. The analysis time was 4 min sample(-1). The effects of salinity and interfering ions (silicate and arsenate) were evaluated and showed no interference under the proposed protocol for DRP analysis. Using the LFA method, different aqueous samples with a salinity range of 0-34 were analyzed and the results showed excellent agreement with the reference method (slope 0.9982±0.0063, R(2)=0.9987, n=34). Recoveries for spiked samples varied from 95.4% to 103.7%. The proposed method showed insignificant interference from salinity, silicate and arsenate, higher reproducibility, easier operation and was free of the bubble problem.

  5. Safety analysis report for packaging (onsite) sample pig transport system

    SciTech Connect

    MCCOY, J.C.

    1999-03-16

    This Safety Analysis Report for Packaging (SARP) provides a technical evaluation of the Sample Pig Transport System as compared to the requirements of the U.S. Department of Energy, Richland Operations Office (RL) Order 5480.1, Change 1, Chapter III. The evaluation concludes that the package is acceptable for the onsite transport of Type B, fissile excepted radioactive materials when used in accordance with this document.

  6. Trace-element analysis of 1000 environmental samples per year using instrumental neutron activation analysis

    NASA Technical Reports Server (NTRS)

    Sheibley, D. W.

    1974-01-01

    The technology and methods developed at the Plum Brook Reactor to analyze 1000 samples per year and report data on as many as 56 elements are described. The manpower for the complete analysis of 20 to 24 samples per week required only 3 to 3.5 hours per sample. The solutions to problems encountered in sample preparation, irradiation, and counting are discussed. The automation of data reduction is described. Typical data on various sample matrices are presented.

  7. Method for preconcentrating a sample for subsequent analysis

    DOEpatents

    Zaromb, Solomon

    1990-01-01

    A system for analysis of trace concentration of contaminants in air includes a portable liquid chromatograph and a preconcentrator for the contaminants to be analyzed. The preconcentrator includes a sample bag having an inlet valve and an outlet valve for collecting an air sample. When the sample is collected the sample bag is connected in series with a sorbing apparatus in a recirculation loop. The sorbing apparatus has an inner gas-permeable container containing a sorbent material and an outer gas-impermeable container. The sample is circulated through the outer container and around the inner container for trapping and preconcentrating the contaminants in the sorbent material. The sorbent material may be a liquid having the same composition as the mobile phase of the chromatograph for direct injection thereinto. Alternatively, the sorbent material may be a porous, solid body, to which mobile phase liquid is added after preconcentration of the contaminants for dissolving the contaminants, the liquid solution then being withdrawn for injection into the chromatograph.

  8. Tank 241-AZ-102 Privatization Push Mode Core Sampling and Analysis Plan

    SciTech Connect

    RASMUSSEN, J.H.

    2000-05-23

    This sampling and analysis plan (SAP) identifies characterization objectives pertaining to sample collection, laboratory analytical evaluation, and reporting requirements for samples obtained from tank 241-AZ-102.

  9. Sampling and analysis of natural gas trace constituents

    SciTech Connect

    Attari, A.; Chao, S.

    1993-09-01

    Major and minor components of natural gas are routinely analyzed by gas chromatography (GC), using a thermal conductivity (TC). The best results obtained by these methods can report no better than 0.01 mole percent of each measured component. Even the extended method of analysis by flame ionization detector (FID) can only improve on the detection limit of hydrocarbons. The gas industry needs better information on all trace constituents of natural gas, whether native or inadvertently added during gas processing that may adversely influence the operation of equipment or the safety of the consumer. The presence of arsenic and mercury in some gas deposits have now been documented in international literature as causing not only human toxicity but also damaging to the field equipment. Yet, no standard methods of sampling and analysis exist to provide this much needed information. In this paper the authors report the results of a three-year program to develop an extensive array of sampling and analysis methods for speciation and measurement of trace constituents of natural gas. A cryogenic sampler operating at near 200 K ({minus}99 F) and at pipeline pressures up to 12.4 {times} 10{sup 6}Pa (1800 psig) has been developed to preconcentrate and recover all trace constituents with boiling points above butanes. Specific analytical methods have been developed for speciating and measurement of many trace components (corresponding to US EPA air toxics) by GC-AED and GC-MS, and for determining various target compounds by other techniques. Moisture, oxygen and sulfur contents are measured on site using dedicated field instruments. Arsenic, mercury and radon are sampled by specific solid sorbents for subsequent laboratory analysis.

  10. Colorimetric Analysis of Ochratoxin A in Beverage Samples.

    PubMed

    Bueno, Diana; Valdez, Luis F; Gutiérrez Salgado, Juan Manuel; Marty, Jean Louis; Muñoz, Roberto

    2016-11-10

    This manuscript describes the use of a portable and low cost fluorescence setup to quantify the concentration of ochratoxin A (OTA) in beverage samples using an in-house developed system and different color models. It is reported that OTA is naturally fluorescent, for that reason an ultraviolet light at 365 nm was used to excite the samples and a Complementary Metal Oxide Semiconductor (CMOS) sensor was used to get a photograph of the OTA under excitation conditions, which is controlled by an executable interface designed in MATLAB. For each concentration of OTA, the coordinates with respect to each model color were obtained and plotted to quantify the mycotoxin present in the sample. It was possible to observe that despite the fact no extraction column was employed, the Red, Green, Blue (RGB) model shows a proportional relation to the evaluated concentrations. Despite the fact more analysis and other methods are required to quantify the OTA concentration, the brightness and a,b for the color-opponent dimensions (L*a*b) and Hue, Saturation, Value (HSV) tests provide results whereby it is possible to identify the concentration of OTA in beverage samples such as beer and wine.

  11. Ultra-trace analysis of platinum in human tissue samples.

    PubMed

    Rudolph, Elisabeth; Hann, Stephan; Stingeder, Gerhard; Reiter, Christian

    2005-08-01

    Background levels of platinum were determined in human autopsy tissues taken from five individuals. The investigated specimens were lung, liver and kidney. Sample preparation involved microwave digestion followed by an open vessel treatment. Inductively-coupled plasma sector field mass spectrometry (ICP-SFMS) was applied in combination with an ultrasonic nebulization/membrane desolvation system for sample introduction. Isotope dilution analysis was employed for accurate quantification of platinum. Excellent procedural detection limits (3 s validation) of 20, 20 and 34 pg g(-1) dry weight were obtained for lung, liver and kidney tissue, respectively. Due to the lack of appropriate biological reference material, road dust (BCR-723) was used for method validation. Platinum levels ranging between 0.03 and 1.42 ng g(-1) were determined in the investigated samples. The platinum concentrations observed in human lung tissue may reflect the increasing atmospheric background levels of platinum originating from car catalysts. The presence of platinum in kidney and liver tissue samples clearly indicates the bioavailability of the element.

  12. Colorimetric Analysis of Ochratoxin A in Beverage Samples

    PubMed Central

    Bueno, Diana; Valdez, Luis F.; Gutiérrez Salgado, Juan Manuel; Marty, Jean Louis; Muñoz, Roberto

    2016-01-01

    This manuscript describes the use of a portable and low cost fluorescence setup to quantify the concentration of ochratoxin A (OTA) in beverage samples using an in-house developed system and different color models. It is reported that OTA is naturally fluorescent, for that reason an ultraviolet light at 365 nm was used to excite the samples and a Complementary Metal Oxide Semiconductor (CMOS) sensor was used to get a photograph of the OTA under excitation conditions, which is controlled by an executable interface designed in MATLAB. For each concentration of OTA, the coordinates with respect to each model color were obtained and plotted to quantify the mycotoxin present in the sample. It was possible to observe that despite the fact no extraction column was employed, the Red, Green, Blue (RGB) model shows a proportional relation to the evaluated concentrations. Despite the fact more analysis and other methods are required to quantify the OTA concentration, the brightness and a,b for the color-opponent dimensions (L*a*b) and Hue, Saturation, Value (HSV) tests provide results whereby it is possible to identify the concentration of OTA in beverage samples such as beer and wine. PMID:27834900

  13. Observations from TEM Analysis of Swift Creek Samples

    NASA Astrophysics Data System (ADS)

    Harris, J. R.

    2012-12-01

    Samples analyzed by transmission electron microscopy (TEM) from suspended sediments in Swift Creek have unique characteristics compared to other naturally occurring asbestos (NOA) sites across the country. Our first introduction to the uniqueness of the Swift Creek site came about when we analyzed soil sediments by polarized light microscopy (PLM) and found relatively low or nonexistent levels of chrysotile asbestos. Upon submission of these samples for TEM analysis, we found that the samples were literally filled with small chrysotile fibers and bundles. We also notice a high number of dark, rounded particles which were not asbestiform. Out of curiosity, we viewed the surface features of one of these particles using scanning electron microscopy to find compacted chrysotile fibers bundled inside these particles. These particles contained the vast majority of chrysotile in the sample. This finding began our approach to provide more advanced TEM/SEM methods for identifying and characterizing complex arrangements of asbestos from NOA sites. We will present some of our experiences and methods for characterizing these types of particles common to NOA sites.

  14. Sampling and analysis plan for the consolidated sludge samples from the canisters and floor of the 105-K East basin

    SciTech Connect

    BAKER, R.B.

    1999-02-18

    This Sampling and Analysis Plan (SAP) provides direction for sampling of fuel canister and floor Sludge from the K East Basin to complete the inventory of samples needed for Sludge treatment process testing. Sample volumes and sources consider recent reviews made by the Sludge treatment subproject. The representative samples will be characterized to the extent needed for the material to be used effectively for testing. Sampling equipment used allows drawing of large volume sludge samples and consolidation of sample material from a number of basin locations into one container. Once filled, the containers will be placed in a cask and transported to Hanford laboratories for recovery and evaluation. Included in the present SAP are the logic for sample location selection, laboratory analysis procedures required, and reporting needed to meet the Data Quality Objectives (DQOs) for this initiative.

  15. Power and sample size in cost-effectiveness analysis.

    PubMed

    Laska, E M; Meisner, M; Siegel, C

    1999-01-01

    For resource allocation under a constrained budget, optimal decision rules for mutually exclusive programs require that the treatment with the highest incremental cost-effectiveness ratio (ICER) below a willingness-to-pay (WTP) criterion be funded. This is equivalent to determining the treatment with the smallest net health cost. The designer of a cost-effectiveness study needs to select a sample size so that the power to reject the null hypothesis, the equality of the net health costs of two treatments, is high. A recently published formula derived under normal distribution theory overstates sample-size requirements. Using net health costs, the authors present simple methods for power analysis based on conventional normal and on nonparametric statistical theory.

  16. 303-K Storage facility sampling and analysis plan

    SciTech Connect

    Adler, J.G.

    1997-07-01

    This document describes the cleanup, sampling, and analysis activities associated with the closure of the 303-K Storage Facility under the Washington Administrative Code (WAC) 173-303-610, ``Dangerous Waste Regulations.`` this document is a supplement to the 303-K Storage Facility Closure Plan (DOE-RL 1995a) (Closure Plan). The objective of these activities is to support clean closure of the 303 K Storage Facility. This document defines the information and activities needed to meet this objective, including: constituents of concern, cleanup performance standards, cleanup activities, sampling locations and methods, field screening locations and methods, field quality control requirements, laboratory analytical methods, and data validation methodology. This document supersedes the Closure Plan if the two conflict

  17. Optimization conditions of samples saponification for tocopherol analysis.

    PubMed

    Souza, Aloisio Henrique Pereira; Gohara, Aline Kirie; Rodrigues, Ângela Claudia; Ströher, Gisely Luzia; Silva, Danielle Cristina; Visentainer, Jesuí Vergílio; Souza, Nilson Evelázio; Matsushita, Makoto

    2014-09-01

    A full factorial design 2(2) (two factors at two levels) with duplicates was performed to investigate the influence of the factors agitation time (2 and 4 h) and the percentage of KOH (60% and 80% w/v) in the saponification of samples for the determination of α, β and γ+δ-tocopherols. The study used samples of peanuts (cultivar armadillo), produced and marketed in Maringá, PR. The factors % KOH and agitation time were significant, and an increase in their values contributed negatively to the responses. The interaction effect was not significant for the response δ-tocopherol, and the contribution of this effect to the other responses was positive, but less than 10%. The ANOVA and response surfaces analysis showed that the most efficient saponification procedure was obtained using a 60% (w/v) solution of KOH and with an agitation time of 2 h.

  18. Robotic Mars Sample Return: Risk Assessment and Analysis Report

    NASA Technical Reports Server (NTRS)

    Lalk, Thomas R.; Spence, Cliff A.

    2003-01-01

    A comparison of the risk associated with two alternative scenarios for a robotic Mars sample return mission was conducted. Two alternative mission scenarios were identified, the Jet Propulsion Lab (JPL) reference Mission and a mission proposed by Johnson Space Center (JSC). The JPL mission was characterized by two landers and an orbiter, and a Mars orbit rendezvous to retrieve the samples. The JSC mission (Direct/SEP) involves a solar electric propulsion (SEP) return to earth followed by a rendezvous with the space shuttle in earth orbit. A qualitative risk assessment to identify and characterize the risks, and a risk analysis to quantify the risks were conducted on these missions. Technical descriptions of the competing scenarios were developed in conjunction with NASA engineers and the sequence of events for each candidate mission was developed. Risk distributions associated with individual and combinations of events were consolidated using event tree analysis in conjunction with Monte Carlo techniques to develop probabilities of mission success for each of the various alternatives. The results were the probability of success of various end states for each candidate scenario. These end states ranged from complete success through various levels of partial success to complete failure. Overall probability of success for the Direct/SEP mission was determined to be 66% for the return of at least one sample and 58% for the JPL mission for the return of at least one sample cache. Values were also determined for intermediate events and end states as well as for the probability of violation of planetary protection. Overall mission planetary protection event probabilities of occurrence were determined to be 0.002% and 1.3% for the Direct/SEP and JPL Reference missions respectively.

  19. WIPP waste characterization program sampling and analysis guidance manual

    SciTech Connect

    Not Available

    1991-01-01

    The Waste Isolation Pilot Plant (WIPP) Waste Characterization Program Sampling and Analysis Guidance Manual (Guidance Manual) provides a unified source of information on the sampling and analytical techniques that enable Department of Energy (DOE) facilities to comply with the requirements established in the current revision of the Quality Assurance Program Plan (QAPP) for the WIPP Experimental-Waste Characterization Program (the Program). This Guidance Manual includes all of the sampling and testing methodologies accepted by the WIPP Project Office (DOE/WPO) for use in implementing the Program requirements specified in the QAPP. This includes methods for characterizing representative samples of transuranic (TRU) wastes at DOE generator sites with respect to the gas generation controlling variables defined in the WIPP bin-scale and alcove test plans, as well as waste container headspace gas sampling and analytical procedures to support waste characterization requirements under the WIPP test program and the Resource Conservation and Recovery Act (RCRA). The procedures in this Guidance Manual are comprehensive and detailed and are designed to provide the necessary guidance for the preparation of site specific procedures. The use of these procedures is intended to provide the necessary sensitivity, specificity, precision, and comparability of analyses and test results. The solutions to achieving specific program objectives will depend upon facility constraints, compliance with DOE Orders and DOE facilities' operating contractor requirements, and the knowledge and experience of the TRU waste handlers and analysts. With some analytical methods, such as gas chromatography/mass spectrometry, the Guidance Manual procedures may be used directly. With other methods, such as nondestructive/destructive characterization, the Guidance Manual provides guidance rather than a step-by-step procedure.

  20. [Analysis of human tissue samples for volatile fire accelerants].

    PubMed

    Treibs, Rudolf

    2014-01-01

    In police investigations of fires, the cause of a fire and the fire debris analysis regarding traces of fire accelerants are important aspects for forensic scientists. Established analytical procedures were recently applied to the remains of fire victims. When examining lung tissue samples, vapors inhaled from volatile ignitable liquids could be identified and differentiated from products of pyrolysis caused by the fire. In addition to the medico-legal results this evidence allowed to draw conclusions as to whether the fire victim was still alive when the fire started.

  1. Sample EP Flow Analysis of Severely Damaged Networks

    SciTech Connect

    Werley, Kenneth Alan; McCown, Andrew William

    2016-10-12

    These are slides for a presentation at the working group meeting of the WESC SREMP Software Product Integration Team on sample EP flow analysis of severely damaged networks. The following topics are covered: ERCOT EP Transmission Model; Zoomed in to Houston and Overlaying StreetAtlas; EMPACT Solve/Dispatch/Shedding Options; QACS BaseCase Power Flow Solution; 3 Substation Contingency; Gen. & Load/100 Optimal Dispatch; Dispatch Results; Shed Load for Low V; Network Damage Summary; Estimated Service Areas (Potential); Estimated Outage Areas (potential).

  2. 241-Z-361 Sludge Characterization Sampling and Analysis Plan

    SciTech Connect

    BANNING, D.L.

    1999-08-05

    This sampling and analysis plan (SAP) identifies the type, quantity, and quality of data needed to support characterization of the sludge that remains in Tank 241-2-361. The procedures described in this SAP are based on the results of the 241-2-361 Sludge Characterization Data Quality Objectives (DQO) (BWHC 1999) process for the tank. The primary objectives of this project are to evaluate the contents of Tank 241-2-361 in order to resolve safety and safeguards issues and to assess alternatives for sludge removal and disposal.

  3. 241-Z-361 Sludge Characterization Sampling and Analysis Plan

    SciTech Connect

    BANNING, D.L.

    1999-07-29

    This sampling and analysis plan (SAP) identifies the type, quantity, and quality of data needed to support characterization of the sludge that remains in Tank 241-2-361. The procedures described in this SAP are based on the results of the 241-2-361 Sludge Characterization Data Quality Objectives (DQO) (BWHC 1999) process for the tank. The primary objectives of this project are to evaluate the contents of Tank 241-2-361 in order to resolve safety and safeguards issues and to assess alternatives for sludge removal and disposal.

  4. Metagenomics - a guide from sampling to data analysis

    PubMed Central

    2012-01-01

    Metagenomics applies a suite of genomic technologies and bioinformatics tools to directly access the genetic content of entire communities of organisms. The field of metagenomics has been responsible for substantial advances in microbial ecology, evolution, and diversity over the past 5 to 10 years, and many research laboratories are actively engaged in it now. With the growing numbers of activities also comes a plethora of methodological knowledge and expertise that should guide future developments in the field. This review summarizes the current opinions in metagenomics, and provides practical guidance and advice on sample processing, sequencing technology, assembly, binning, annotation, experimental design, statistical analysis, data storage, and data sharing. As more metagenomic datasets are generated, the availability of standardized procedures and shared data storage and analysis becomes increasingly important to ensure that output of individual projects can be assessed and compared. PMID:22587947

  5. Nondestructive neutron activation analysis of volcanic samples: Hawaii

    SciTech Connect

    Zoller, W.H.; Finnegan, D.L.; Crowe, B.

    1986-01-01

    Samples of volcanic emissions have been collected between and during eruptions of both Kilauea and Mauna Loa volcanoes during the last three years. Airborne particles have been collected on Teflon filters and acidic gases on base-impregnated cellulose filters. Chemically neutral gas-phase species are collected on charcoal-coated cellulose filters. The primary analytical technique used is nondestructive neutron activation analysis, which has been used to determine the quantities of up to 35 elements on the different filters. The use of neutron activation analysis makes it possible to analyze for a wide range of elements in the different matrices used for the collection and to learn about the distribution between particles and gas phases for each of the elements.

  6. Laminated microfluidic system for small sample protein analysis

    PubMed Central

    Saedinia, Sara; Nastiuk, Kent L.; Krolewski, John J.; Li, G. P.; Bachman, Mark

    2014-01-01

    We describe a technology based on lamination that allows for the production of highly integrated 3D devices suitable for performing a wide variety of microfluidic assays. This approach uses a suite of microfluidic coupons (“microfloupons”) that are intended to be stacked as needed to produce an assay of interest. Microfloupons may be manufactured in paper, plastic, gels, or other materials, in advance, by different manufacturers, then assembled by the assay designer as needed. To demonstrate this approach, we designed, assembled, and characterized a microfloupon device that performs sodium-dodecyl-sulfate polyacrylamide gel electrophoresis on a small sample of protein. This device allowed for the manipulation and transport of small amounts of protein sample, tight injection into a thin polyacrylamide gel, electrophoretic separation of the proteins into bands, and subsequent removal of the gel from the device for imaging and further analysis. The microfloupons are rugged enough to handle and can be easily aligned and laminated, allowing for a variety of different assays to be designed and configured by selecting appropriate microfloupons. This approach provides a convenient way to perform assays that have multiple steps, relieving the need to design highly sophisticated devices that incorporate all functions in a single unit, while still achieving the benefits of small sample size, automation, and high speed operation. PMID:24753728

  7. Analysis and comparison of two Victorian Brown Coal resinite samples

    SciTech Connect

    Anderson, K.B.; Botto, R.E.; Dyrkacz, G.R.; Hayatsu, R.; Winans, R.E. )

    1989-01-01

    Among the organic constituents of coal, the maceral resinite is probably the least complex structurally, due to the relatively simple composition of the original resins. Hence, with careful analysis, it may be possible to construct meaningful and accurate structural descriptions of this maceral. For the purposes of this study, two physically diverse resinite samples were obtained from Victorian Brown Coal (VBC) by hand picking from open cut mine faces. The first sample, which is referred to as resinite'' throughout this text is a hard, brittle, glassy material, yellow/brown in color. The second is a soft, brittle, bone white material, which was found in association with a large gymnosperm log, of undetermined paleobotanical affinity, as sheets between wood'' and bark.'' This material is sometimes referred to as bombicite'' by geologists, and is referred to by this name in this text in the interests of clarity. Petrographically, both samples are classified as resinite. Pyrolysis-high resolution mass spectra were recorded on a Kratos MS-50 mass spectrometer. FTIR spectra were recorded on a Bruker 113 V FTIR spectrometer. CP/MAS {sup 13}C NMR spectra were recorded on a Bruker CPX-100 NMR spectrometer. 7 refs., 3 figs., 1 tab.

  8. Ergonomic and usability analysis on a sample of automobile dashboards.

    PubMed

    Carvalho, Raíssa; Soares, Marcelo

    2012-01-01

    This is a research study based on an analysis which sets out to identify and pinpoint ergonomic and usability problems found in a sample of automobile dashboards. The sample consisted of three dashboards, of three different makes and characterized as being a popular model, an average model and a luxury model. The examination was conducted by observation, with the aid of photography, notes and open interview, questionnaires and performing tasks with users, the bases of which are on the principles laid down by methodologies. From this it was possible to point to the existence of problems such as: complaints about the layout, lighting, colors, available area, difficult access to points of interaction, such as buttons, and the difficult nomenclature of dials. Later, the findings and recommendations presented show the need for a further, deeper study, using more accurate tools, a larger sample of users, and an anthropometric study focused on the dashboard, since reading and understanding it have to be done quickly and accurately, and that more attention be given to the study of automobile dashboards, particularly in the most popular vehicles in order to maintain the standards of usability, and drivers' comfort and safety.

  9. Eigenvector method for umbrella sampling enables error analysis.

    PubMed

    Thiede, Erik H; Van Koten, Brian; Weare, Jonathan; Dinner, Aaron R

    2016-08-28

    Umbrella sampling efficiently yields equilibrium averages that depend on exploring rare states of a model by biasing simulations to windows of coordinate values and then combining the resulting data with physical weighting. Here, we introduce a mathematical framework that casts the step of combining the data as an eigenproblem. The advantage to this approach is that it facilitates error analysis. We discuss how the error scales with the number of windows. Then, we derive a central limit theorem for averages that are obtained from umbrella sampling. The central limit theorem suggests an estimator of the error contributions from individual windows, and we develop a simple and computationally inexpensive procedure for implementing it. We demonstrate this estimator for simulations of the alanine dipeptide and show that it emphasizes low free energy pathways between stable states in comparison to existing approaches for assessing error contributions. Our work suggests the possibility of using the estimator and, more generally, the eigenvector method for umbrella sampling to guide adaptation of the simulation parameters to accelerate convergence.

  10. Entry Dispersion Analysis for the Stardust Comet Sample Return Capsule

    NASA Technical Reports Server (NTRS)

    Desai, Prasun N.; Mitcheltree, Robert A.; Cheatwood, F. McNeil

    1997-01-01

    Stardust will be the first mission to return samples from beyond the Earth-Moon system. The sample return capsule, which is passively controlled during the fastest Earth entry ever, will land by parachute in Utah. The present study analyzes the entry, descent, and landing of the returning sample capsule. The effects of two aerodynamic instabilities are revealed (one in the high altitude free molecular regime and the other in the transonic/subsonic flow regime). These instabilities could lead to unacceptably large excursions in the angle-of-attack near peak heating and main parachute deployment, respectively. To reduce the excursions resulting from the high altitude instability, the entry spin rate of the capsule is increased. To stabilize the excursions from the transonic/subsonic instability, a drogue chute with deployment triggered by an accelerometer and timer is added prior to main parachute deployment. A Monte Carlo dispersion analysis of the modified entry (from which the impact of off-nominal conditions during the entry is ascertained) shows that the capsule attitude excursions near peak heating and drogue chute deployment are within Stardust program limits. Additionally, the size of the resulting 3-sigma landing ellipse is 83.5 km in downrange by 29.2 km in crossrange, which is within the Utah Test and Training Range boundaries.

  11. Analysis of hepatitis C viral dynamics using Latin hypercube sampling

    NASA Astrophysics Data System (ADS)

    Pachpute, Gaurav; Chakrabarty, Siddhartha P.

    2012-12-01

    We consider a mathematical model comprising four coupled ordinary differential equations (ODEs) to study hepatitis C viral dynamics. The model includes the efficacies of a combination therapy of interferon and ribavirin. There are two main objectives of this paper. The first one is to approximate the percentage of cases in which there is a viral clearance in absence of treatment as well as percentage of response to treatment for various efficacy levels. The other is to better understand and identify the parameters that play a key role in the decline of viral load and can be estimated in a clinical setting. A condition for the stability of the uninfected and the infected steady states is presented. A large number of sample points for the model parameters (which are physiologically feasible) are generated using Latin hypercube sampling. An analysis of the simulated values identifies that, approximately 29.85% cases result in clearance of the virus during the early phase of the infection. Results from the χ2 and the Spearman's tests done on the samples, indicate a distinctly different distribution for certain parameters for the cases exhibiting viral clearance under the combination therapy.

  12. Eigenvector method for umbrella sampling enables error analysis

    NASA Astrophysics Data System (ADS)

    Thiede, Erik H.; Van Koten, Brian; Weare, Jonathan; Dinner, Aaron R.

    2016-08-01

    Umbrella sampling efficiently yields equilibrium averages that depend on exploring rare states of a model by biasing simulations to windows of coordinate values and then combining the resulting data with physical weighting. Here, we introduce a mathematical framework that casts the step of combining the data as an eigenproblem. The advantage to this approach is that it facilitates error analysis. We discuss how the error scales with the number of windows. Then, we derive a central limit theorem for averages that are obtained from umbrella sampling. The central limit theorem suggests an estimator of the error contributions from individual windows, and we develop a simple and computationally inexpensive procedure for implementing it. We demonstrate this estimator for simulations of the alanine dipeptide and show that it emphasizes low free energy pathways between stable states in comparison to existing approaches for assessing error contributions. Our work suggests the possibility of using the estimator and, more generally, the eigenvector method for umbrella sampling to guide adaptation of the simulation parameters to accelerate convergence.

  13. Dropouts from nursing education: path analysis of a national sample.

    PubMed

    Munro, B H

    1980-01-01

    Path analysis was used to test a theoretical model of college nursing student dropouts. Multiple regression was used to assess the relative importance of the predictor variables. Students' self-reported reasons for dropping out were studied by contingency and correlational analyses to determine the relationship between these reasons and individual difference variables. Factor analysis was used to develop scales to measure the variables of locus of control, self-esteem, social integration, and institutional commitment. The sample of students was drawn from the National Longitudinal Study of the High School Class of 1972. Included in the sample were students entering two- and four-year nursing programs full-time in the fall of 1972. These two groups of students were found to be significantly different in measures of cognitive ability and in aspirations for further education. Approximately 27 percent of the two-year and 41 percent of the four-year students withdrew from their nursing programs during this study. Reasons for withdrawal most frequently cited by both groups related to losing interest in nursing and becoming interested in other fields of study. Educational aspirations had the strongest direct effect on persistence in nursing for two-year students; for four-year students, academic ability was the most powerful predictor of persistence.

  14. Analysis of Helicobacter pylori genotypes in clinical gastric wash samples.

    PubMed

    Miyamoto, Shuichi; Watanabe, Yoshiyuki; Oikawa, Ritsuko; Ono, Shoko; Mabe, Katsuhiro; Kudo, Takahiko; Yamamoto, Hiroyuki; Itoh, Fumio; Kato, Mototsugu; Sakamoto, Naoya

    2016-08-01

    Helicobacter pylori is a key factor in the development of gastric cancer; indeed, clearance of H. pylori helps prevent gastric cancer. However, the relationship between gastric cancer and the abundance and diversity of H. pylori genotypes in the stomach remains unknown. Here, we present, for the first time, a quantitative analysis of H. pylori genotypes in gastric washes. A method was first developed to assess diversity and abundance by pyrosequencing and analysis of single nucleotide polymorphisms in 23S ribosomal RNA (rRNA), a gene associated with clarithromycin resistance. This method was then validated using arbitrarily mixed plasmids carrying 23S rRNA with single nucleotide polymorphisms. Multiple strains were detected in many of 34 clinical samples, with frequency 24.3 ± 24.2 and 26.3 ± 33.8 % for the A2143G and A2144G strains, respectively. Importantly, results obtained from gastric washes were similar to those obtained from biopsy samples. The method provides opportunities to investigate drug resistance in H. pylori and assess potential biomarkers of gastric cancer risk, and should thus be validated in large-scale clinical trials.

  15. Sampling and Analysis Plan for K Basins Debris

    SciTech Connect

    WESTCOTT, J.L.

    2000-06-21

    This Sampling and Analysis Plan presents the rationale and strategy for sampling and analysis activities to support removal of debris from the K-East and K-West Basins located in the 100K Area at the Hanford Site. This project is focused on characterization to support waste designation for disposal of waste at the Environmental Restoration Disposal Facility (ERDF). This material has previously been dispositioned at the Hanford Low-Level Burial Grounds or Central Waste Complex. The structures that house the basins are classified as radioactive material areas. Therefore, all materials removed from the buildings are presumed to be radioactively contaminated. Because most of the materials that will be addressed under this plan will be removed from the basins, and because of the cost associated with screening materials for release, it is anticipated that all debris will be managed as low-level waste. Materials will be surveyed, however, to estimate radionuclide content for disposal and to determine that the debris is not contaminated with levels of transuranic radionuclides that would designate the debris as transuranic waste.

  16. Transuranic waste characterization sampling and analysis methods manual. Revision 1

    SciTech Connect

    Suermann, J.F.

    1996-04-01

    This Methods Manual provides a unified source of information on the sampling and analytical techniques that enable Department of Energy (DOE) facilities to comply with the requirements established in the current revision of the Transuranic Waste Characterization Quality Assurance Program Plan (QAPP) for the Waste Isolation Pilot Plant (WIPP) Transuranic (TRU) Waste Characterization Program (the Program) and the WIPP Waste Analysis Plan. This Methods Manual includes all of the testing, sampling, and analytical methodologies accepted by DOE for use in implementing the Program requirements specified in the QAPP and the WIPP Waste Analysis Plan. The procedures in this Methods Manual are comprehensive and detailed and are designed to provide the necessary guidance for the preparation of site-specific procedures. With some analytical methods, such as Gas Chromatography/Mass Spectrometry, the Methods Manual procedures may be used directly. With other methods, such as nondestructive characterization, the Methods Manual provides guidance rather than a step-by-step procedure. Sites must meet all of the specified quality control requirements of the applicable procedure. Each DOE site must document the details of the procedures it will use and demonstrate the efficacy of such procedures to the Manager, National TRU Program Waste Characterization, during Waste Characterization and Certification audits.

  17. Analysis of Selected Legacy 85Kr Samples

    SciTech Connect

    Jubin, Robert Thomas; Bruffey, Stephanie H.

    2016-09-02

    Legacy samples composed of 85Kr encapsulated in solid zeolite 5A material and five small metal tubes containing a mixture of the zeolite combined with a glass matrix resulting from hot isostatic pressing have been preserved. The samples were a result of krypton R&D encapsulation efforts in the late 1970s performed at the Idaho Chemical Processing Plant. These samples were shipped to Oak Ridge National Laboratory (ORNL) in mid-FY 2014. Upon receipt the outer shipping package was opened, and the inner package, removed and placed in a radiological hood. The individual capsules were double bagged as they were removed from the inner shipping pig and placed into individual glass sample bottles for further analysis. The five capsules were then x-ray imaged. Capsules 1 and 4 appear intact and to contain an amorphous mass within the capsules. Capsule 2 clearly shows the saw marks on the capsule and a quantity of loose pellet or bead-like material remaining in the capsule. Capsule 3 shows similar bead-like material within the intact capsule. Capsule 5 had been opened at an undetermined time in the past. The end of this capsule appears to have been cut off, and there are additional saw marks on the side of the capsule. X-ray tomography allowed the capsules to be viewed along the three axes. Of most interest was determining whether there was any residual material in the closed end of Capsule 5. The images confirmed the presence of residual material within this capsule. The material appears to be compacted but still retains some of the bead-like morphology. Based on the nondestructive analysis (NDA) results, a proposed path forward was formulated to advance this effort toward the original goals of understanding the effects of extended storage on the waste form and package. Based on the initial NDA and the fact that there are at least two breached samples, it was proposed that exploratory tests be conducted with the breached specimens before opening the three intact

  18. Components for automated microfluidics sample preparation and analysis

    NASA Astrophysics Data System (ADS)

    Archer, M.; Erickson, J. S.; Hilliard, L. R.; Howell, P. B., Jr.; Stenger, D. A.; Ligler, F. S.; Lin, B.

    2008-02-01

    The increasing demand for portable devices to detect and identify pathogens represents an interdisciplinary effort between engineering, materials science, and molecular biology. Automation of both sample preparation and analysis is critical for performing multiplexed analyses on real world samples. This paper selects two possible components for such automated portable analyzers: modified silicon structures for use in the isolation of nucleic acids and a sheath flow system suitable for automated microflow cytometry. Any detection platform that relies on the genetic content (RNA and DNA) present in complex matrices requires careful extraction and isolation of the nucleic acids in order to ensure their integrity throughout the process. This sample pre-treatment step is commonly performed using commercially available solid phases along with various molecular biology techniques that require multiple manual steps and dedicated laboratory space. Regardless of the detection scheme, a major challenge in the integration of total analysis systems is the development of platforms compatible with current isolation techniques that will ensure the same quality of nucleic acids. Silicon is an ideal candidate for solid phase separations since it can be tailored structurally and chemically to mimic the conditions used in the laboratory. For analytical purposes, we have developed passive structures that can be used to fully ensheath one flow stream with another. As opposed to traditional flow focusing methods, our sheath flow profile is truly two dimensional, making it an ideal candidate for integration into a microfluidic flow cytometer. Such a microflow cytometer could be used to measure targets captured on either antibody- or DNA-coated beads.

  19. ANALYSIS OF SAMPLES FROM TANK 6F CHEMICAL CLEANING

    SciTech Connect

    Poirier, M.; Fink, S.

    2010-02-02

    Savannah River Remediation (SRR) is preparing Tank 6F for closure. The first step in preparing the tank for closure is mechanical sludge removal. In mechanical sludge removal, personnel add liquid (e.g., inhibited water or supernate salt solution) to the tank to form a slurry. They mix the liquid and sludge with pumps, and transfer the slurry to another tank for further processing. Mechanical sludge removal effectively removes the bulk of the sludge from a tank, but is not able to remove all of the sludge. In Tank 6F, SRR estimated a sludge heel of 5,984 gallons remained after mechanical sludge removal. To remove this sludge heel, SRR performed chemical cleaning. The chemical cleaning included two oxalic acid strikes, a spray wash, and a water wash. SRR conducted the first oxalic acid strike as follows. Personnel added 110,830 gallons of 8 wt % oxalic acid to Tank 6F and mixed the contents of Tank 6F with two submersible mixer pumps (SMPs) for approximately four days. Following the mixing, they transferred 115,903 gallons of Tank 6F material to Tank 7F. The SMPs were operating when the transfer started and were shut down approximately five hours after the transfer started. SRR collected a sample of the liquid from Tank 6F and submitted it to SRNL for analysis. Mapping of the tank following the transfer indicated that 2,400 gallons of solids remained in the tank. SRR conducted the second oxalic acid strike as follows. Personnel added 28,881 gallons of 8 wt % oxalic acid to Tank 6F. Following the acid addition, they visually inspected the tank and transferred 32,247 gallons of Tank 6F material to Tank 7F. SRR collected a sample of the liquid from Tank 6F and submitted it to SRNL for analysis. Mapping of the tank following the transfer indicated that 3,248 gallons of solids remained in the tank. Following the oxalic acid strikes, SRR performed Spray Washing with oxalic acid to remove waste collected on internal structures, cooling coils, tank top internals, and tank

  20. UMTRA project water sampling and analysis plan, Mexican Hat, Utah

    SciTech Connect

    Not Available

    1994-04-01

    The Mexican Hat, Utah, Uranium Mill Tailings Remedial Action (UMTRA) Project site is a former uranium mill that is undergoing surface remediation in the form of on-site tailings stabilization. Contaminated surface materials from the Monument Valley, Arizona, UMTRA Project site have been transported to the Mexican Hat site and are being consolidated with the Mexican Hat tailings. The scheduled completion of the tailings disposal cell is August 1995. Water is found in two geologic units at the site: the Halgaito Shale Formation and the Honaker Trail Formation. The tailings rest on the Halgaito Shale, and water contained in that unit is a result of milling activities and, to a lesser extent, water released from the tailings from compaction during remedial action construction of the disposal cell. Water in the Halgaito Shale flows through fractures and discharges at seeps along nearby arroyos. Flow from the seeps will diminish as water drains from the unit. Ground water in the lower unit, the Honaker Trail Formation, is protected from contamination by an upward hydraulic gradient. There are no nearby water supply wells because of widespread poor background ground water quality and quantity, and the San Juan River shows no impacts from the site. This water sampling and analysis plan (WSAP) recommends sampling six seeps and one upgradient monitor well compared in the Honaker Trail Formation. Samples will be taken in April 1994 (representative of high group water levels) and September 1994 (representative of low ground water levels). Analyses will be performed on filtered samples for plume indicator parameters.

  1. Fluid sample collection and distribution system. [qualitative analysis of aqueous samples from several points

    NASA Technical Reports Server (NTRS)

    Brooks, R. L. (Inventor)

    1979-01-01

    A multipoint fluid sample collection and distribution system is provided wherein the sample inputs are made through one or more of a number of sampling valves to a progressive cavity pump which is not susceptible to damage by large unfiltered particles. The pump output is through a filter unit that can provide a filtered multipoint sample. An unfiltered multipoint sample is also provided. An effluent sample can be taken and applied to a second progressive cavity pump for pumping to a filter unit that can provide one or more filtered effluent samples. The second pump can also provide an unfiltered effluent sample. Means are provided to periodically back flush each filter unit without shutting off the whole system.

  2. ANALYSIS OF SAMPLES FROM TANK 5F CHEMICAL CLEANING

    SciTech Connect

    Poirier, M.; Fink, S.

    2011-03-07

    The Savannah River Site (SRS) is preparing Tank 5F for closure. The first step in preparing the tank for closure is mechanical sludge removal. Following mechanical sludge removal, SRS performed chemical cleaning with oxalic acid to remove the sludge heel. Personnel are currently assessing the effectiveness of the chemical cleaning. SRS personnel collected liquid samples during chemical cleaning and submitted them to Savannah River National Laboratory (SRNL) for analysis. Following chemical cleaning, they collected a solid sample (also known as 'process sample') and submitted it to SRNL for analysis. The authors analyzed these samples to assess the effectiveness of the chemical cleaning process. The conclusions from this work are: (1) With the exception of iron, the dissolution of sludge components from Tank 5F agreed with results from the actual waste demonstration performed in 2007. The fraction of iron removed from Tank 5F by chemical cleaning was significantly less than the fraction removed in the SRNL demonstrations. The likely cause of this difference is the high pH following the first oxalic acid strike. (2) Most of the sludge mass remaining in the tank is iron and nickel. (3) The remaining sludge contains approximately 26 kg of barium, 37 kg of chromium, and 37 kg of mercury. (4) Most of the radioactivity remaining in the residual material is beta emitters and {sup 90}Sr. (5) The chemical cleaning removed more than {approx} 90% of the uranium isotopes and {sup 137}Cs. (6) The chemical cleaning removed {approx} 70% of the neptunium, {approx} 83% of the {sup 90}Sr, and {approx} 21% of the {sup 60}Co. (7) The chemical cleaning removed less than 10% of the plutonium, americium, and curium isotopes. (8) The chemical cleaning removed more than 90% of the aluminium, calcium, and sodium from the tank. (9) The cleaning operations removed 61% of lithium, 88% of non-radioactive strontium, and 65% of zirconium. The {sup 90}Sr and non-radioactive strontium were measured

  3. Sample Analysis Results for a Benchscale Evaporator Test Using a Hanford Tank 241-AN-102 Sample

    SciTech Connect

    Ferrara, D.M.

    2003-08-25

    This report provides the analytical results of samples taken during the low-activity waste evaporator process demonstration conducted at the Savannah River Technology Center with a 15-liter sample of Hanford tank 241-AN102 pretreated radioactive supernate. The objective of the task was to determine the concentration of various organic, inorganic and radionuclide constituents of potential concern and physical properties of the evaporator feed, concentrate, condensate and off gas for the Hanford River Protection Project. Over 150 samples and blanks were collected and analyzed in accordance with EPA methods. One hundred nineteen target organic analyze concentrations were shown to be less than the minimum quantitative limits in all samples (feed, concentrate, condensate, and off gas samples).Tetrahydrofuran (THF) was present in evaporator samples. THF was the most concentrated volatile compound detected in the off gas. No pesticides or polychlorinated biphenyls (PCBs) were detected in any evaporator sample. Very low levels of some dioxins and furans were reported in the off-gas samples, but are thought to have been due to contamination. Most of the sample collection, sample preparation, and sample analyses provided results with sufficient pedigree to support the rigor associated with regulatory application of these results.

  4. Trends in proteomic analysis of human vitreous humor samples.

    PubMed

    Rocha, Ana S; Santos, Fátima M; Monteiro, João P; Castro-de-Sousa, João P; Queiroz, João A; Tomaz, Cândida T; Passarinha, Luís A

    2014-09-01

    Proteomic analysis of human vitreous humor (VH) may elucidate the pathogenesis of retinal ocular diseases and may provide information for the development of potential therapeutic targets due to its pivotal location near lens and retina. The discovery of whole VH proteome involves a complex analysis of thousands of proteins simultaneously. Therefore, in proteomic studies the protein fractionation is important for reducing sample complexity, facilitating the access to the low-abundant proteins, and recognizing them as biotargets for clinical research. Although several separation methods have been used, gel-based proteomics are the most popular and versatile ones applied for global protein separation. However, chromatographic methods and its combination with other separation techniques are now beginning to be used as promising set-ups for VH protein identification. This review attempts to offer an overview of the techniques currently used with VH, exploring its methodological demands, exposing its advantages, and helping the reader to plan future experiences. Moreover, this review shows the relevance of VH proteomic analysis as a tool for the study of the mechanisms underlying some ocular diseases and for the development of new therapeutic approaches.

  5. Regional climate network analysis from irregularly sampled satellite data

    NASA Astrophysics Data System (ADS)

    Wiedermann, Marc; Sykioti, Olga; Papadimitriou, Constantinos; Balasis, George; Kurths, Jürgen; Donner, Reik V.

    2016-04-01

    With the increasing availability of remote sensing data Earth System Analysis has taken a great step forward. This type of data, however, also harbors a variety of conceptual complications. First, depending on whether the satellite is orbiting on an ascending or descending path systematic biases are induced into the data, and both measurements cannot be evaluated simultaneously without an appropriate preprocessing. Second, remote sensing data are usually not produced with equidistant temporal sampling, but might contain huge gaps and irregular time steps. Third, the time period covered by the data is often too short to perform an appropriate seasonal detrending. Here, we propose a general framework to create homogeneous anomalized time series for a (multivariate) satellite data set by combining time series from ascending and descending satellite paths or even different missions using principal component and singular spectrum analysis. We then exemplarily apply our method to sea surface temperature data obtained from the SMOS satellite mission to study small-scale regional correlative patterns covering different parts of the Aegean Sea. To address the issue of irregular temporal sampling we utilize a kernel weighted version of the linear cross-correlation function to compute lagged correlations between all pairs of grid points in the data set. By binarizing the thus obtained matrices, we obtain a network representation of the system's similarity structure. Ultimately, we use tools from complex network theory to study regional interdependencies in the study area for different time lags of up to forty days. We find that the obtained networks represent well the observed average wind directions and speeds and display interaction structures between small regions in the Aegean Sea, which are in good agreement with earlier observations. In a second step, we extend the study area to the whole Mediterranean and Black Sea and investigate lagged interactions between these two

  6. Organic Contaminants Library for the Sample Analysis at Mars

    NASA Astrophysics Data System (ADS)

    Misra, P.; Garcia-Sanchez, R.; Canham, J.; Mahaffy, P. R.

    2012-12-01

    A library containing mass spectra for Sample Analysis at Mars (SAM) materials has been developed with the purpose of contamination identification and control. Based on analysis of the Gas Chromatography-Mass Spectrometric (GCMS) data through thermal desorption, organic compounds were successfully identified from material samples, such as polymers, paints and adhesives. The library contains the spectra for all the compounds found in each of these analyzed files and is supplemented by a file information spreadsheet, a spreadsheet-formatted library for easy searching, and a Perfluorotributylamine (PFTBA) based normalization protocol to make corrections to SAM data in order to meet the standard set by commercial libraries. An example of the library in use can be seen in Figure 1, where the abundances match closely, the spectral shape is retained, and the library picks up on it with an 88% identification probability. Of course, there are also compounds that have not been identified and are retained as unknowns. The library we have developed, along with its supplemental materials, is useful from both organizational and practical viewpoints. Through them we are able to organize large volumes of GCMS data, while at the same time breaking down the components that each material sample is made of. This approach in turn allows us straightforward and fast access to information that will be critical while performing analysis on the data recorded by the SAM instrumentation. In addition, the normalization protocol dramatically increased the identification probability. In SAM GCMS, PFTBA signals were obfuscated, resulting in library matches far away from PFTBA; by using the normalization protocol we were able to transform it into a 92% probable spectral match for PFTBA. The project has demonstrated conclusively that the library is successful in identifying unknown compounds utilizing both the Automated Mass Spectral Deconvolution & Identification System (AMDIS) and the Ion

  7. Tank 241-Z-361 vapor sampling and analysis plan

    SciTech Connect

    BANNING, D.L.

    1999-02-23

    Tank 241-Z-361 is identified in the Hanford Federal Facility Agreement and Consent Order (commonly referred to as the Tri-Party Agreement), Appendix C, (Ecology et al. 1994) as a unit to be remediated under the authority of the Comprehensive Environmental Response, Compensation, and Liability Act of 1980 (CERCLA). As such, the U.S. Environmental Protection Agency will serve as the lead regulatory agency for remediation of this tank under the CERCLA process. At the time this unit was identified as a CERCLA site under the Tri-Party Agreement, it was placed within the 200-ZP-2 Operable Unit. In 1997, The Tri-parties redefined 200 Area Operable Units into waste groupings (Waste Site Grouping for 200 Areas Soils Investigations [DOE-RL 1992 and 1997]). A waste group contains waste sites that share similarities in geological conditions, function, and types of waste received. Tank 241-Z-361 is identified within the CERCLA Plutonium/Organic-rich Process Condensate/Process Waste Group (DOE-RL 1992). The Plutonium/Organic-rich Process Condensate/Process Waste Group has been prioritized for remediation beginning in the year 2004. Results of Tank 216-Z-361 sampling and analysis described in this Sampling and Analysis Plan (SAP) and in the SAP for sludge sampling (to be developed) will determine whether expedited response actions are required before 2004 because of the hazards associated with tank contents. Should data conclude that remediation of this tank should occur earlier than is planned for the other sites in the waste group, it is likely that removal alternatives will be analyzed in a separate Engineering Evaluation/Cost Analysis (EE/CA). Removal actions would proceed after the U.S. Environmental Protection Agency (EPA) signs an Action Memorandum describing the selected removal alternative for Tank 216-Z-361. If the data conclude that there is no immediate threat to human health and the environment from this tank, remedial actions for the tank will be defined in a

  8. Workshop on Analysis of Returned Comet Nucleus Samples

    NASA Astrophysics Data System (ADS)

    Chang, Sherwood

    This volume contains abstracts that have been accepted by the Program Committee for presentation at the Workshop on Analysis of Returned Comet Nucleus Samples, held in Milpitas, California, January 16-18, 1989. Conveners are Sherwood Chang (NASA Ames Research Center) and Larry Nyquist (NASA Johnson Space Center). Program Committee members are Thomas Ahrens (ex-officio; California Institute of Technology), Lou Allamandola (NASA Ames Research Center), David Blake (NASA Ames Research Center), Donald Brownlee (University of Washington, Seattle), Theodore E. Bunch (NASA Ames Research Center), Humberto Campins (Planetary Science Institute), Jeff Cuzzi (NASA Ames Research Center), Eberhard Griin (Max-Plank-Institut fiir Kemphysik), Martha Hanner (Jet Propulsion Laboratory), Alan Harris (Jet Propulsion Laboratory), John Kerrid-e (University of Califomia, Los Angeles), Yves Langevin (University of Paris), Gerhard Schwehm (ESTEC), and Paul Weissman (Jet Propulsion Laboratory). Logistics and administrative support for the workshop were provided by the Lunar and Planetary Institute Projects Office.

  9. Surrogate matrix: opportunities and challenges for tissue sample analysis.

    PubMed

    Ho, Stacy; Gao, Hong

    2015-09-23

    Often there is limited availability of matching tissue matrix and/or the analyte may occur endogenously in the target tissue. Surrogate matrix provides an option for quantitation of drug, metabolite(s) and biomarker(s) in these circumstances. However, the use of a surrogate matrix also presents challenges. This paper summarizes and discusses the challenges of selecting a proper surrogate, validating the suitability of the surrogate and establishing a surrogate tissue method using the fit-for-purpose approach. This paper also systematically reviews the current practices for evaluating key parameters of a surrogate tissue assay, including sensitivity, specificity, selectivity, interference, precision, accuracy, recovery, matrix effects and stability. Considerations and suggestions are provided for dealing with such challenges during method establishment and tissue sample analysis.

  10. Earth recovery mode analysis for a Martian sample return mission

    NASA Technical Reports Server (NTRS)

    Green, J. P.

    1978-01-01

    The analysis has concerned itself with evaluating alternative methods of recovering a sample module from a trans-earth trajectory originating in the vicinity of Mars. The major modes evaluated are: (1) direct atmospheric entry from trans-earth trajectory; (2) earth orbit insertion by retropropulsion; and (3) atmospheric braking to a capture orbit. In addition, the question of guided vs. unguided entry vehicles was considered, as well as alternative methods of recovery after orbit insertion for modes (2) and (3). A summary of results and conclusions is presented. Analytical results for aerodynamic and propulsive maneuvering vehicles are discussed. System performance requirements and alternatives for inertial systems implementation are also discussed. Orbital recovery operations and further studies required to resolve the recovery mode issue are described.

  11. Hierarchical Bayesian Modeling, Estimation, and Sampling for Multigroup Shape Analysis

    PubMed Central

    Yu, Yen-Yun; Fletcher, P. Thomas; Awate, Suyash P.

    2016-01-01

    This paper proposes a novel method for the analysis of anatomical shapes present in biomedical image data. Motivated by the natural organization of population data into multiple groups, this paper presents a novel hierarchical generative statistical model on shapes. The proposed method represents shapes using pointsets and defines a joint distribution on the population’s (i) shape variables and (ii) object-boundary data. The proposed method solves for optimal (i) point locations, (ii) correspondences, and (iii) model-parameter values as a single optimization problem. The optimization uses expectation maximization relying on a novel Markov-chain Monte-Carlo algorithm for sampling in Kendall shape space. Results on clinical brain images demonstrate advantages over the state of the art. PMID:25320776

  12. ACTINIDE REMOVAL PROCESS SAMPLE ANALYSIS, CHEMICAL MODELING, AND FILTRATION EVALUATION

    SciTech Connect

    Martino, C.; Herman, D.; Pike, J.; Peters, T.

    2014-06-05

    Filtration within the Actinide Removal Process (ARP) currently limits the throughput in interim salt processing at the Savannah River Site. In this process, batches of salt solution with Monosodium Titanate (MST) sorbent are concentrated by crossflow filtration. The filtrate is subsequently processed to remove cesium in the Modular Caustic Side Solvent Extraction Unit (MCU) followed by disposal in saltstone grout. The concentrated MST slurry is washed and sent to the Defense Waste Processing Facility (DWPF) for vitrification. During recent ARP processing, there has been a degradation of filter performance manifested as the inability to maintain high filtrate flux throughout a multi-batch cycle. The objectives of this effort were to characterize the feed streams, to determine if solids (in addition to MST) are precipitating and causing the degraded performance of the filters, and to assess the particle size and rheological data to address potential filtration impacts. Equilibrium modelling with OLI Analyzer{sup TM} and OLI ESP{sup TM} was performed to determine chemical components at risk of precipitation and to simulate the ARP process. The performance of ARP filtration was evaluated to review potential causes of the observed filter behavior. Task activities for this study included extensive physical and chemical analysis of samples from the Late Wash Pump Tank (LWPT) and the Late Wash Hold Tank (LWHT) within ARP as well as samples of the tank farm feed from Tank 49H. The samples from the LWPT and LWHT were obtained from several stages of processing of Salt Batch 6D, Cycle 6, Batch 16.

  13. Preamplification Procedure for the Analysis of Ancient DNA Samples

    PubMed Central

    Del Gaudio, Stefania; Cirillo, Alessandra; Di Bernardo, Giovanni; Galderisi, Umberto; Thanassoulas, Theodoros; Pitsios, Theodoros; Cipollaro, Marilena

    2013-01-01

    In ancient DNA studies the low amount of endogenous DNA represents a limiting factor that often hampers the result achievement. In this study we extracted the DNA from nine human skeletal remains of different ages found in the Byzantine cemetery of Abdera Halkidiki and in the medieval cemetery of St. Spiridion in Rhodes (Greece). Real-time quantitative polymerase chain reaction (qPCR) was used to detect in the extracts the presence of PCR inhibitors and to estimate the DNA content. As mitochondrial DNA was detected in all samples, amplification of nuclear targets, as amelogenin and the polymorphism M470V of the transmembrane conductance regulator gene, yielded positive results in one case only. In an effort to improve amplification success, we applied, for the first time in ancient DNA, a preamplification strategy based on TaqMan PreAmp Master Mix. A comparison between results obtained from nonpreamplified and preamplified samples is reported. Our data, even if preliminary, show that the TaqMan PreAmp procedure may improve the sensitivity of qPCR analysis. PMID:24187523

  14. Preamplification procedure for the analysis of ancient DNA samples.

    PubMed

    Del Gaudio, Stefania; Cirillo, Alessandra; Di Bernardo, Giovanni; Galderisi, Umberto; Thanassoulas, Theodoros; Pitsios, Theodoros; Cipollaro, Marilena

    2013-01-01

    In ancient DNA studies the low amount of endogenous DNA represents a limiting factor that often hampers the result achievement. In this study we extracted the DNA from nine human skeletal remains of different ages found in the Byzantine cemetery of Abdera Halkidiki and in the medieval cemetery of St. Spiridion in Rhodes (Greece). Real-time quantitative polymerase chain reaction (qPCR) was used to detect in the extracts the presence of PCR inhibitors and to estimate the DNA content. As mitochondrial DNA was detected in all samples, amplification of nuclear targets, as amelogenin and the polymorphism M470V of the transmembrane conductance regulator gene, yielded positive results in one case only. In an effort to improve amplification success, we applied, for the first time in ancient DNA, a preamplification strategy based on TaqMan PreAmp Master Mix. A comparison between results obtained from nonpreamplified and preamplified samples is reported. Our data, even if preliminary, show that the TaqMan PreAmp procedure may improve the sensitivity of qPCR analysis.

  15. Analysis of micrometeorological data using a two sample variance

    NASA Astrophysics Data System (ADS)

    Werle, Peter; Falge, Eva

    2010-05-01

    In ecosystem research infrared gas analyzers are increasingly used to measure fluxes of carbon dioxide, water vapour, methane, nitrous oxide and even stable carbon isotopes. As these complex measurement devices under field conditions cannot be considered as absolutely stable, drift characterisation is an issue to distinguish between atmospheric data and sensor drift. In this paper the concept of the two sample variance is utilized in analogy to previous stability investigations to characterize the stationarity of both, spectroscopic measurements of concentration time series and micrometeorological data in the time domain, which is a prerequisite for covariance calculations. As an example, the method is applied to assess the time constant for detrending of time series data and the optimum trace gas flux integration time. The method described here provides information similar to existing characterizations as the ogive analysis, the normalized error variance of the second order moment and the spectral characteristics of turbulence in the inertial subrange. The method is easy to implement and, therefore, well suited to assist as a useful tool for a routine data quality check for both, new practitioners and experts in the field. Werle, P., Time domain characterization of micrometeorological data based on a two sample variance. Agric. Forest Meteorol. (2010), doi:10.1016/j.agrformet.2009.12.007

  16. Environmental sampling and analysis as a safeguards tool

    SciTech Connect

    Perkins, R.W.; Wogman, N.A.; Holdren, G.R.

    1994-03-01

    Environmental sampling and radionuclide analysis of the resulting material can be utilized as a supplemental approach in safeguarding practices and particularly for detection of undeclared nuclear activities. The production of nuclear weapons could be pursued by uranium enrichment processes to produce highly enriched U-235 or by nuclear reactor operations followed by chemical separations to produce Pu-239. The application of either of these processes results in the production of signature materials, some of which will be released to the environs. Results from the operations of the Hanford production facilities are discussed and indicate the type of signatures that may be expected from plutonium production facilities. These include noble gas emissions from the reactors and chemical separations processes, the production of radionuclides in reactor cooling water followed by their subsequent release to the Columbia River, and the release of mildly contaminated process water from the chemical processing facilities. These signature materials are carried by both gaseous and liqid effluents and enter various compartments of the environment. The types of signature materials which are most likely to be accumulated are discussed, together with examples of the quantities which have been released during past separations. There are numerous processes by which natural uranium may be enriched to produce highly enriched U-235. The most definitive signature of such processes is always a modification in uranium isotope ratios, and materials showing either enriched or depleted uranium in gaseous and liquid effluents provide the best indication that uramium enrichment processes are taking place. Therefore, techniques for sampling and analysis of airborne, waterborne, or deposited uranium in environmental matrices provide a means of detecting uranium enrichment which may lead to proliferation products.

  17. 40 CFR 761.292 - Chemical extraction and analysis of individual samples and composite samples.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL ACT POLYCHLORINATED BIPHENYLS (PCBs) MANUFACTURING, PROCESSING, DISTRIBUTION IN COMMERCE, AND USE PROHIBITIONS Sampling To Verify Completion of...

  18. 40 CFR 761.292 - Chemical extraction and analysis of individual samples and composite samples.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL ACT POLYCHLORINATED BIPHENYLS (PCBs) MANUFACTURING, PROCESSING, DISTRIBUTION IN COMMERCE, AND USE PROHIBITIONS Sampling To Verify Completion of...

  19. Plutonium Mobility Studies: 216-Z-9 Trench Sample Analysis Results

    SciTech Connect

    Cantrell, Kirk J.; Geiszler, Keith N.; Arey, Bruce W.

    2008-09-05

    A variety of analyses were conducted on selected sediment samples collected from two wells (299 W15-46 and 299-W15-48) drilled near the 216-Z-9 Trench to elucidate the form and potential for Pu and Am to be mobilized under present conditions and those that could be expected in future remediation scenarios. Analyses included moisture content, determination of the less than sand size fraction (silt plus clay), carbon analysis, SEM/EDS analysis, microwave-assisted acid digestions for total element analysis, and extraction tests using Hanford groundwater as the leachate. Results of the extraction tests were used as input to conduct equilibrium geochemical modeling of the solutions with Geochemist’s Workbench®. Geochemical modeling results for Pu were evaluated in terms of recent conclusions regarding the solubility and redox reactions of Pu by Neck et al. (2007a, 2007b). It was found that the highest concentrations of Pu and Am were associated with sediments of low silt/clay content and occur above silt/clay rich layers within the sediment profile. It was also found that the Pu and Am were relatively enriched in the silt/clay portion of these samples. The fact that the highest concentrations of Pu and Am occurred in sediments with low silt/clay contents suggests that waste solutions had perched on top of the low permeability silt/clay rich layers and interactions with the high silt/clay layers was minimal. SEM/EDS analysis indicated that the Pu and Am in these sediments does not occur as discrete micron size particles, and therefore must occur as mononuclear or polynuclear/ nanoclusters size particles adsorbed throughout the sediment samples. Leaching of these samples with Hanford groundwater indicates that release of Pu and Am from the sediments is correlated most significantly with the acidity of the water and not the initial concentrations of Pu and Am in the sediments. Only extracts that were acidic after contact with the sediments (pH 4.3 to 5.4) contained

  20. K West Basin Sand Filter Backwash Sample Analysis

    SciTech Connect

    Fiskum, Sandra K.; Smoot, Margaret R.; Coffey, Deborah S.; Pool, Karl N.

    2016-03-01

    A sand filter is used to help maintain water clarity at the K West Basin where highly radioactive sludge is stored. Eventually that sand filter will require disposal. The radionuclide content of the solids trapped in the sand filter will affect the selection of the sand filter disposal pathway. The Pacific Northwest National Laboratory (PNNL) was contracted by the K Basin Operations & Plateau Remediation Project (operations contractor CH2M Hill) to analyze the radionuclide content of the solids collected from the backwash of the K West Basin sand filter. The radionuclide composition in the sand filter backwash solids will be used by CH2M Hill to determine if the sand filter media and retained sludge solids will be designated as transuranic waste for disposal purposes or can be processed through less expensive means. On October 19, 2015, K Basin Operations & Plateau Remediation Project staff backwashed the sand filter into the North Load-Out Pit (NLOP) and immediately collected sample slurry from a sampling tube positioned 24 in. above the NLOP floor. The 764 g sand filter backwash slurry sample, KW-105 SFBW-001, was submitted to PNNL for analysis on October 20, 2015. Solids from the slurry sample were consolidated into two samples (i.e., a primary and a duplicate sample) by centrifuging and measured for mass (0.82 g combined – wet centrifuged solids basis) and volume (0.80 mL combined). The solids were a dark brown/orange color, consistent with iron oxide/hydroxide. The solids were dried; the combined dry solids mass was 0.1113 g, corresponding to 0.0146 weight percent (wt%) solids in the original submitted sample slurry. The solids were acid-digested using nitric and hydrochloric acids. Insoluble solids developed upon dilution with 0.5 M HNO3, corresponding to an average 6.5 wt% of the initial dry solids content. The acid digestate and insoluble solids were analyzed separately by gamma spectrometry. Nominally, 7.7% of the 60Co was present

  1. Analysis of Organic Compounds in Mars Analog Samples

    NASA Technical Reports Server (NTRS)

    Mahaffy, P. R.; Brinckerhoff, W. B.; Buch, A.; Cabane, M.; Coll, P.; Demick, J.; Glavin, D. P.

    2004-01-01

    The detailed characterization of organic compounds that might be preserved in rocks, ices, or sedimentary layers on Mars would be a significant step toward resolving the question of the habitability and potential for life on that planet. The fact that the Viking gas chromatograph mass spectrometer (GCMS) did not detect organic compounds should not discourage further investigations since (a) an oxidizing environment in the near surface fines analyzed by Viking is likely to have destroyed many reduced carbon species; (b) there are classes of refractory or partially oxidized species such as carboxylic acids that would not have been detected by the Viking GCMS; and (c) the Viking landing sites are not representative of Mars overall. These factors motivate the development of advanced in situ analytical protocols to carry out a comprehensive survey of organic compounds in martian regolith, ices, and rocks. We combine pyrolysis GCMS for analysis of volatile species, chemical derivatization for transformation of less volatile organics, and laser desorption mass spectrometry (LDMS) for analysis of elements and more refractory, higher-mass organics. To evaluate this approach and enable a comparison with other measurement techniques we analyze organics in Mars simulant samples.

  2. Analysis of the Touch-And-Go Surface Sampling Concept for Comet Sample Return Missions

    NASA Technical Reports Server (NTRS)

    Mandic, Milan; Acikmese, Behcet; Bayard, David S.; Blackmore, Lars

    2012-01-01

    This paper studies the Touch-and-Go (TAG) concept for enabling a spacecraft to take a sample from the surface of a small primitive body, such as an asteroid or comet. The idea behind the TAG concept is to let the spacecraft descend to the surface, make contact with the surface for several seconds, and then ascend to a safe location. Sampling would be accomplished by an end-effector that is active during the few seconds of surface contact. The TAG event is one of the most critical events in a primitive body sample-return mission. The purpose of this study is to evaluate the dynamic behavior of a representative spacecraft during the TAG event, i.e., immediately prior, during, and after surface contact of the sampler. The study evaluates the sample-collection performance of the proposed sampling end-effector, in this case a brushwheel sampler, while acquiring material from the surface during the contact. A main result of the study is a guidance and control (G&C) validation of the overall TAG concept, in addition to specific contributions to demonstrating the effectiveness of using nonlinear clutch mechanisms in the sampling arm joints, and increasing the length of the sampling arms to improve robustness.

  3. Analysis of sampling artifacts on the Granger causality analysis for topology extraction of neuronal dynamics.

    PubMed

    Zhou, Douglas; Zhang, Yaoyu; Xiao, Yanyang; Cai, David

    2014-01-01

    Granger causality (GC) is a powerful method for causal inference for time series. In general, the GC value is computed using discrete time series sampled from continuous-time processes with a certain sampling interval length τ, i.e., the GC value is a function of τ. Using the GC analysis for the topology extraction of the simplest integrate-and-fire neuronal network of two neurons, we discuss behaviors of the GC value as a function of τ, which exhibits (i) oscillations, often vanishing at certain finite sampling interval lengths, (ii) the GC vanishes linearly as one uses finer and finer sampling. We show that these sampling effects can occur in both linear and non-linear dynamics: the GC value may vanish in the presence of true causal influence or become non-zero in the absence of causal influence. Without properly taking this issue into account, GC analysis may produce unreliable conclusions about causal influence when applied to empirical data. These sampling artifacts on the GC value greatly complicate the reliability of causal inference using the GC analysis, in general, and the validity of topology reconstruction for networks, in particular. We use idealized linear models to illustrate possible mechanisms underlying these phenomena and to gain insight into the general spectral structures that give rise to these sampling effects. Finally, we present an approach to circumvent these sampling artifacts to obtain reliable GC values.

  4. Analysis and differentiation of paper samples by capillary electrophoresis and multivariate analysis.

    PubMed

    Fernández de la Ossa, Ma Ángeles; Ortega-Ojeda, Fernando; García-Ruiz, Carmen

    2014-11-01

    This work reports an investigation for the analysis of different paper samples using CE with laser-induced detection. Papers from four different manufactures (white-copy paper) and four different paper sources (white and recycled-copy papers, adhesive yellow paper notes and restaurant serviettes) were pulverized by scratching with a surgical scalpel prior to their derivatization with a fluorescent labeling agent, 8-aminopyrene-1,3,6-trisulfonic acid. Methodological conditions were evaluated, specifically the derivatization conditions with the aim to achieve the best S/N signals and the separation conditions in order to obtain optimum values of sensitivity and reproducibility. The best conditions, in terms of fastest, and easiest sample preparation procedure, minimal sample consumption, as well as the use of the simplest and fastest CE-procedure for obtaining the best analytical parameters, were applied to the analysis of the different paper samples. The registered electropherograms were pretreated (normalized and aligned) and subjected to multivariate analysis (principal component analysis). A successful discrimination among paper samples without entanglements was achieved. To the best of our knowledge, this work presents the first approach to achieve a successful differentiation among visually similar white-copy paper samples produced by different manufactures and paper from different paper sources through their direct analysis by CE-LIF and subsequent comparative study of the complete cellulose electropherogram by chemometric tools.

  5. Analysis of Cervical Supernatant Samples Luminescence Using 355 nm Laser

    NASA Astrophysics Data System (ADS)

    Vaitkuviene, A.; Gegzna, V.; Kurtinaitiene, R.; Stanikunas, R.; Rimiene, J.; Vaitkus, J.

    2010-05-01

    The biomarker discovery for accurate detection and diagnosis of cervical carcinoma and its malignant precursors represents one of the current challenges in clinical medicine. Laser induced autofluorescence spectra in cervical smear content were fitted to predict the cervical epithelium diagnosis as a lab off "optical biopsy" method. Liquid PAP supernatant sediment dried on Quartz plate spectroscopy was performed by 355 nm Nd YAG microlaser STA-1 (Standa, Ltd). For comparison a liquid supernatant spectroscopy was formed by laboratory "Perkin Elmer LS 50B spetrometer at 290, 300, 310 nm excitations. Analysis of spectrum was performed by approximation using the multi-peaks program with Lorentz functions for the liquid samples and with Gaussian functions for the dry samples. Ratio of spectral components area to the area under whole experimental curve (SPP) was calculated. The spectral components were compared by averages of SPP using Mann-Whitney U-test in histology groups. Results. Differentiation of Normal and HSIL/CIN2+ cases in whole supernatant could be performed by stationary laboratory lamp spectroscopy at excitation 290 nm and emission >379 nm with accuracy AUC 0,69, Sens 0,72, Spec 0,65. Differentiation Normal versus HSIL/CIN2+ groups in dried enriched supernatant could be performed by 355 nm microlaser excitation at emission 405-424 nm with accuracy (AUC 0,96, Sens 0,91, Spec 1.00). Diagnostic algorithm could be created for all histology groups differentiation under 355 nm excitation. Microlaser induced "optical biopsy "looks promising method for cervical screening at the point of care.

  6. On-chip analysis of respiratory viruses from nasopharyngeal samples.

    PubMed

    Ritzi-Lehnert, Marion; Himmelreich, Ralf; Attig, Hans; Claussen, Jan; Dahlke, Rainer; Grosshauser, Gerd; Holzer, Eva; Jeziorski, Markus; Schaeffer, Eva; Wende, Andy; Werner, Sabine; Wiborg, Jens Ole; Wick, Isabell; Drese, Klaus Stefan; Rothmann, Thomas

    2011-10-01

    Point-of-care (PoC) testing followed by personalized efficient therapy of infectious diseases may result in a considerable reduction of associated health care costs. Lab-on-a-chip (LoC) systems represent a potentially high efficient class of PoC tools. Here, we present a LoC system for automated pathogen analysis of respiratory viruses from nasopharyngeal specimens. The device prepares total nucleic acids from extracted swab samples using magnetic silica beads. After reverse transcription the co-purified viral RNA is amplified in accordance with the QIAplex multiplex PCR technology. Hybridized to corresponding QIAGEN LiquiChip beads and labelled with streptavidin R-phycoerythrin, the amplified target sequences are finally detected using a QIAGEN LiquiChip200 workstation. All chemicals needed are either stored freeze-dried on the disposable chip or are provided in liquid form in a reagent cartridge for up to 24 runs. Magnetic stir bars for mixing as well as turning valves with metering structures are integrated into the injection-moulded disposable chip. The core of the controlling instrument is a rotating heating bar construction providing fixed temperatures for fast cycling. PCR times of about half an hour (for 30 cycles) could be achieved for 120 μl reactions, making this system the fastest currently available high-volume PCR chip. The functionality of the system was shown by comparing automatically processed nasopharyngeal samples to ones processed manually according to the QIAGEN "ResPlex™ II Panel v2.0" respiratory virus detection kit. A prototype of the present instrument revealed slightly weaker signal intensities with a similar sensitivity in comparison to the commercially available kit and automated nucleic acid preparation devices, even without protocol optimization.

  7. Treaty verification sample analysis program analytical results: UNSCOM 65 samples. Final report, December 1993-January 1994

    SciTech Connect

    Szafraniec, L.L.; Beaudry, W.T.; Bossle, P.C.; Durst, H.D.; Ellzy, M.W.

    1994-07-01

    Nineteen samples from the United Nations Special Commission 65 on Iraq (UNSCOM 65) were analyzed for chemical warfare (CW) related compounds using a variety of highly sophisticated spectroscopic and chromatographic techniques. The samples consisted of six water, six soil, two vegetation, one cloth, one wood, and two mortar shell crosscut sections. No sulfur or nitrogen mustards, Lewsite, or any of their degradation products were detected. No nerve agents were observed, and no tin was detected precluding the presence of stannic chloride, a component of NC, a World War I choking agent. Diethyl phosphoric acid was unambiguously identified in three water samples, and ethyl phosphoric acid was tentatively identified, at very low levels, in one water sample. These phosphoric acids are degradation products of Amiton, many commercially available pesticides, as well as Tabun, and impurities in munitions-grade Tabun. No definitive conclusions concerning the source of these two chemicals could be drawn from the analytical results.

  8. ANALYSIS OF THE SALT FEED TANK CORE SAMPLE

    SciTech Connect

    Reigel, M.; Cheng, W.

    2012-01-26

    The Saltstone Production Facility (SPF) immobilizes and disposes of low-level radioactive and hazardous liquid waste (salt solution) remaining from the processing of radioactive material at the Savannah River Site (SRS). Low-level waste (LLW) streams from processes at SRS are stored in Tank 50 until the LLW can be transferred to the SPF for treatment and disposal. The Salt Feed Tank (SFT) at the Saltstone Production Facility (SPF) holds approximately 6500 gallons of low level waste from Tank 50 as well as drain water returned from the Saltstone Disposal Facility (SDF) vaults. Over the past several years, Saltstone Engineering has noted the accumulation of solids in the SFT. The solids are causing issues with pump performance, agitator performance, density/level monitoring, as well as taking up volume in the tank. The tank has been sounded at the same location multiple times to determine the level of the solids. The readings have been 12, 25 and 15 inches. The SFT is 8.5 feet high and 12 feet in diameter, therefore the solids account for approximately 10 % of the tank volume. Saltstone Engineering has unsuccessfully attempted to obtain scrape samples of the solids for analysis. As a result, Savannah River National Laboratory (SRNL) was tasked with developing a soft core sampler to obtain a sample of the solids and to analyze the core sample to aid in determining a path forward for removing the solids from the SFT. The source of the material in the SFT is the drain water return system where excess liquid from the Saltstone disposal vaults is pumped back to the SFT for reprocessing. It has been shown that fresh grout from the vault enter the drain water system piping. Once these grout solids return to the SFT, they settle in the tank, set up, and can't be reprocessed, causing buildup in the tank over time. The composition of the material indicates that it is potentially toxic for chromium and mercury and the primary radionuclide is cesium-137. Qualitative measurements

  9. Cold Vacuum Drying (CVD) Facility Sampling and Analysis Plan

    SciTech Connect

    IRWIN, J.J.

    2000-09-22

    The Cold Vacuum Drying (CVD) Facility provides the required process systems, supporting equipment, and facilities needed for the conditioning of spent nuclear fuel (SNF) from the Hanford K-Basins prior to storage at the Canister Storage Building (CSB). The process water conditioning (PWC) system collects and treats the selected liquid effluent streams generated by the CVD process. The PWC system uses ion exchange modules (IXMs) and filtration to remove radioactive ions and particulate from CVD effluent streams. Water treated by the PWC is collected in a 5000-gallon storage tank prior to shipment to an on-site facility for additional treatment and disposal. The purpose of this sampling and analysis plan is to document the basis for achieving the following data quality objectives: (1) Measurement of the radionuclide content of the water transferred from the multi-canister overpack (MCO), vacuum purge system (VPS) condensate tank, MCO/Cask annulus and deionized water flushes to the PWC system receiver tanks. (2) Trending the radionuclide inventory of IXMs to assure that they do not exceed the limits prescribed in HNF-2760, Rev. 0-D, ''Safety Analysis Report for Packaging (Onsite) Ion Exchange Modules,'' and HNF-EP-0063 Rev. 5, ''Hanford Site Solid Waste Acceptance Criteria'' for Category 3, non-TRU, low level waste (LLW). (3) Determining the radionuclide content of the PWC system bulk water storage tank to assure that it meets the limits set forth in HNF-3 172, Rev. 0, ''Hanford Site Liquid Waste Acceptance Criteria,'' to permit transfer and disposal at the Effluent Treatment Facility (ETF) located at the 200 East Area.

  10. Sampling analysis for the earth radiation budget satellite system mission

    NASA Technical Reports Server (NTRS)

    Harrison, E. F.; Gibson, G. G.

    1977-01-01

    A study was conducted to identify problems related to sampling the Earth's radiant energy budget and to define a satellite system with sufficient sampling to satisfy science requirements on global, zonal, and regional scales.

  11. SAMSAN- MODERN NUMERICAL METHODS FOR CLASSICAL SAMPLED SYSTEM ANALYSIS

    NASA Technical Reports Server (NTRS)

    Frisch, H. P.

    1994-01-01

    SAMSAN was developed to aid the control system analyst by providing a self consistent set of computer algorithms that support large order control system design and evaluation studies, with an emphasis placed on sampled system analysis. Control system analysts have access to a vast array of published algorithms to solve an equally large spectrum of controls related computational problems. The analyst usually spends considerable time and effort bringing these published algorithms to an integrated operational status and often finds them less general than desired. SAMSAN reduces the burden on the analyst by providing a set of algorithms that have been well tested and documented, and that can be readily integrated for solving control system problems. Algorithm selection for SAMSAN has been biased toward numerical accuracy for large order systems with computational speed and portability being considered important but not paramount. In addition to containing relevant subroutines from EISPAK for eigen-analysis and from LINPAK for the solution of linear systems and related problems, SAMSAN contains the following not so generally available capabilities: 1) Reduction of a real non-symmetric matrix to block diagonal form via a real similarity transformation matrix which is well conditioned with respect to inversion, 2) Solution of the generalized eigenvalue problem with balancing and grading, 3) Computation of all zeros of the determinant of a matrix of polynomials, 4) Matrix exponentiation and the evaluation of integrals involving the matrix exponential, with option to first block diagonalize, 5) Root locus and frequency response for single variable transfer functions in the S, Z, and W domains, 6) Several methods of computing zeros for linear systems, and 7) The ability to generate documentation "on demand". All matrix operations in the SAMSAN algorithms assume non-symmetric matrices with real double precision elements. There is no fixed size limit on any matrix in any

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

    PubMed Central

    Feist, Peter; Hummon, Amanda B.

    2015-01-01

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

  13. Portable system for microbial sample preparation and oligonucleotide microarray analysis.

    SciTech Connect

    Bavykin, S. G.; Akowski, J. P.; Zakhariev, V. M.; Barsky, V. E.; Mirzabekov, A. D.; Perov, A. N.; Biochip Technology Center; Engelhardt Inst. of Molecular Biology

    2001-02-01

    We have developed a three-component system for microbial identification that consists of (i) a universal syringe-operated silica minicolumn for successive DNA and RNA isolation, fractionation, fragmentation, fluorescent labeling, and removal of excess free label and short oligonucleotides; (ii) microarrays of immobilized oligonucleotide probes for 16S rRNA identification; and (iii) a portable battery-powered device for imaging the hybridization of fluorescently labeled RNA fragments with the arrays. The minicolumn combines a guanidine thiocyanate method of nucleic acid isolation with a newly developed hydroxyl radical-based technique for DNA and RNA labeling and fragmentation. DNA and RNA can also be fractionated through differential binding of double- and single-stranded forms of nucleic acids to the silica. The procedure involves sequential washing of the column with different solutions. No vacuum filtration steps, phenol extraction, or centrifugation is required. After hybridization, the overall fluorescence pattern is captured as a digital image or as a Polaroid photo. This three-component system was used to discriminate Escherichia coli, Bacillus subtilis, Bacillus thuringiensis, and human HL60 cells. The procedure is rapid: beginning with whole cells, it takes approximately 25 min to obtain labeled DNA and RNA samples and an additional 25 min to hybridize and acquire the microarray image using a stationary image analysis system or the portable imager.

  14. An integrated sampling and analysis approach for improved biodiversity monitoring

    USGS Publications Warehouse

    DeWan, Amielle A.; Zipkin, Elise

    2010-01-01

    Successful biodiversity conservation requires high quality monitoring data and analyses to ensure scientifically defensible policy, legislation, and management. Although monitoring is a critical component in assessing population status and trends, many governmental and non-governmental organizations struggle to develop and implement effective sampling protocols and statistical analyses because of the magnitude and diversity of species in conservation concern. In this article we describe a practical and sophisticated data collection and analysis framework for developing a comprehensive wildlife monitoring program that includes multi-species inventory techniques and community-level hierarchical modeling. Compared to monitoring many species individually, the multi-species approach allows for improved estimates of individual species occurrences, including rare species, and an increased understanding of the aggregated response of a community to landscape and habitat heterogeneity. We demonstrate the benefits and practicality of this approach to address challenges associated with monitoring in the context of US state agencies that are legislatively required to monitor and protect species in greatest conservation need. We believe this approach will be useful to regional, national, and international organizations interested in assessing the status of both common and rare species.

  15. An Integrated Sampling and Analysis Approach for Improved Biodiversity Monitoring

    NASA Astrophysics Data System (ADS)

    Dewan, Amielle A.; Zipkin, Elise F.

    2010-05-01

    Successful biodiversity conservation requires high quality monitoring data and analyses to ensure scientifically defensible policy, legislation, and management. Although monitoring is a critical component in assessing population status and trends, many governmental and non-governmental organizations struggle to develop and implement effective sampling protocols and statistical analyses because of the magnitude and diversity of species in conservation concern. In this article we describe a practical and sophisticated data collection and analysis framework for developing a comprehensive wildlife monitoring program that includes multi-species inventory techniques and community-level hierarchical modeling. Compared to monitoring many species individually, the multi-species approach allows for improved estimates of individual species occurrences, including rare species, and an increased understanding of the aggregated response of a community to landscape and habitat heterogeneity. We demonstrate the benefits and practicality of this approach to address challenges associated with monitoring in the context of US state agencies that are legislatively required to monitor and protect species in greatest conservation need. We believe this approach will be useful to regional, national, and international organizations interested in assessing the status of both common and rare species.

  16. Prospecting by sampling and analysis of airborne particulates and gases

    DOEpatents

    Sehmel, G.A.

    1984-05-01

    A method is claimed for prospecting by sampling airborne particulates or gases at a ground position and recording wind direction values at the time of sampling. The samples are subsequently analyzed to determine the concentrations of a desired material or the ratios of the desired material to other identifiable materials in the collected samples. By comparing the measured concentrations or ratios to expected background data in the vicinity sampled, one can select recorded wind directions indicative of the upwind position of the land-based source of the desired material.

  17. Compilation of PRF Canyon Floor Pan Sample Analysis Results

    SciTech Connect

    Pool, Karl N.; Minette, Michael J.; Wahl, Jon H.; Greenwood, Lawrence R.; Coffey, Deborah S.; McNamara, Bruce K.; Bryan, Samuel A.; Scheele, Randall D.; Delegard, Calvin H.; Sinkov, Sergey I.; Soderquist, Chuck Z.; Fiskum, Sandra K.; Brown, Garrett N.; Clark, Richard A.

    2016-06-30

    On September 28, 2015, debris collected from the PRF (236-Z) canyon floor, Pan J, was observed to exhibit chemical reaction. The material had been transferred from the floor pan to a collection tray inside the canyon the previous Friday. Work in the canyon was stopped to allow Industrial Hygiene to perform monitoring of the material reaction. Canyon floor debris that had been sealed out was sequestered at the facility, a recovery plan was developed, and drum inspections were initiated to verify no additional reactions had occurred. On October 13, in-process drums containing other Pan J material were inspected and showed some indication of chemical reaction, limited to discoloration and degradation of inner plastic bags. All Pan J material was sealed back into the canyon and returned to collection trays. Based on the high airborne levels in the canyon during physical debris removal, ETGS (Encapsulation Technology Glycerin Solution) was used as a fogging/lock-down agent. On October 15, subject matter experts confirmed a reaction had occurred between nitrates (both Plutonium Nitrate and Aluminum Nitrate Nonahydrate (ANN) are present) in the Pan J material and the ETGS fixative used to lower airborne radioactivity levels during debris removal. Management stopped the use of fogging/lock-down agents containing glycerin on bulk materials, declared a Management Concern, and initiated the Potential Inadequacy in the Safety Analysis determination process. Additional drum inspections and laboratory analysis of both reacted and unreacted material are planned. This report compiles the results of many different sample analyses conducted by the Pacific Northwest National Laboratory on samples collected from the Plutonium Reclamation Facility (PRF) floor pans by the CH2MHill’s Plateau Remediation Company (CHPRC). Revision 1 added Appendix G that reports the results of the Gas Generation Rate and methodology. The scope of analyses requested by CHPRC includes the determination of

  18. Binary Mixtures of Permanganate and Chlorinated Volatile Organic Compounds in Groundwater Samples: Sample Preservation and Analysis

    EPA Science Inventory

    Ground water samples collected at sites where in-situ chemical oxidation (ISCO) has been deployed may contain binary mixtures of ground water contaminants and permanganate (MnO4-), an oxidant injected into the subsurface to destroy the contaminant. Commingling of the oxidant and ...

  19. Analysis of bioethanol samples through Inductively Coupled Plasma Mass Spectrometry with a total sample consumption system

    NASA Astrophysics Data System (ADS)

    Sánchez, Carlos; Lienemann, Charles-Philippe; Todolí, Jose-Luis

    2016-10-01

    Bioethanol real samples have been directly analyzed through ICP-MS by means of the so called High Temperature Torch Integrated Sample Introduction System (hTISIS). Because bioethanol samples may contain water, experiments have been carried out in order to determine the effect of ethanol concentration on the ICP-MS response. The ethanol content studied went from 0 to 50%, because higher alcohol concentrations led to carbon deposits on the ICP-MS interface. The spectrometer default spray chamber (double pass) equipped with a glass concentric pneumatic micronebulizer has been taken as the reference system. Two flow regimes have been evaluated: continuous sample aspiration at 25 μL min- 1 and 5 μL air-segmented sample injection. hTISIS temperature has been shown to be critical, in fact ICP-MS sensitivity increased with this variable up to 100-200 °C depending on the solution tested. Higher chamber temperatures led to either a drop in signal or a plateau. Compared with the reference system, the hTISIS improved the sensitivities by a factor included within the 4 to 8 range while average detection limits were 6 times lower for the latter device. Regarding the influence of the ethanol concentration on sensitivity, it has been observed that an increase in the temperature was not enough to eliminate the interferences. It was also necessary to modify the torch position with respect to the ICP-MS interface to overcome them. This fact was likely due to the different extent of ion plasma radial diffusion encountered as a function of the matrix when working at high chamber temperatures. When the torch was moved 1 mm plasma down axis, ethanolic and aqueous solutions provided statistically equal sensitivities. A preconcentration procedure has been applied in order to validate the methodology. It has been found that, under optimum conditions from the point of view of matrix effects, recoveries for spiked samples were close to 100%. Furthermore, analytical concentrations for real

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

    PubMed Central

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

    2016-01-01

    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. PMID:28248234

  1. Liquid microjunction surface sampling probe fluid dynamics: computational and experimental analysis of coaxial intercapillary positioning effects on sample manipulation.

    PubMed

    Elnaggar, Mariam S; Barbier, Charlotte; Van Berkel, Gary J

    2011-07-01

    A coaxial geometry liquid microjunction surface sampling probe (LMJ-SSP) enables direct extraction of analytes from surfaces for subsequent analysis by techniques like mass spectrometry. Solution dynamics at the probe-to-sample surface interface in the LMJ-SSP has been suspected to influence sampling efficiency and dispersion but has not been rigorously investigated. The effect on flow dynamics and analyte transport to the mass spectrometer caused by coaxial retraction of the inner and outer capillaries from each other and the surface during sampling with a LMJ-SSP was investigated using computational fluid dynamics and experimentation. A transparent LMJ-SSP was constructed to provide the means for visual observation of the dynamics of the surface sampling process. Visual observation, computational fluid dynamics (CFD) analysis, and experimental results revealed that inner capillary axial retraction from the flush position relative to the outer capillary transitioned the probe from a continuous sampling and injection mode through an intermediate regime to sample plug formation mode caused by eddy currents at the sampling end of the probe. The potential for analytical implementation of these newly discovered probe operational modes is discussed.

  2. Liquid Microjunction Surface Sampling Probe Fluid Dynamics: Computational and Experimental Analysis of Coaxial Intercapillary Positioning Effects on Sample Manipulation

    NASA Astrophysics Data System (ADS)

    ElNaggar, Mariam S.; Barbier, Charlotte; Van Berkel, Gary J.

    2011-07-01

    A coaxial geometry liquid microjunction surface sampling probe (LMJ-SSP) enables direct extraction of analytes from surfaces for subsequent analysis by techniques like mass spectrometry. Solution dynamics at the probe-to-sample surface interface in the LMJ-SSP has been suspected to influence sampling efficiency and dispersion but has not been rigorously investigated. The effect on flow dynamics and analyte transport to the mass spectrometer caused by coaxial retraction of the inner and outer capillaries from each other and the surface during sampling with a LMJ-SSP was investigated using computational fluid dynamics and experimentation. A transparent LMJ-SSP was constructed to provide the means for visual observation of the dynamics of the surface sampling process. Visual observation, computational fluid dynamics (CFD) analysis, and experimental results revealed that inner capillary axial retraction from the flush position relative to the outer capillary transitioned the probe from a continuous sampling and injection mode through an intermediate regime to sample plug formation mode caused by eddy currents at the sampling end of the probe. The potential for analytical implementation of these newly discovered probe operational modes is discussed.

  3. Sleep Apnea and Cancer: Analysis of a Nationwide Population Sample

    PubMed Central

    Gozal, David; Ham, Sandra A.; Mokhlesi, Babak

    2016-01-01

    Study Objectives: Epidemiological evidence from relatively small cohorts suggests that obstructive sleep apnea (OSA) is associated with higher cancer incidence and mortality. Here we aimed to determine whether cancer incidence for major cancer types and risk of metastases or mortality from cancer are increased in the presence of OSA. Methods: All OSA diagnoses included in an employee-sponsored health insurance database spanning the years 2003–2012 were identified and 1:1 matched demographically based on age, gender, and state of residence, or alternatively matched by comorbidities. The incidence of 12 types of cancer was assessed. In addition, another cohort of patients with a primary diagnosis of cancer was retrieved, and the risk of metastatic disease or cancer mortality was determined as a function of the presence or absence of OSA. Multivariate Cox proportional hazards regression models were fitted to assess the independent associations between OSA and outcomes of interest. Results: Based on a cohort of ∼5.6 million individuals, the incidence of all cancer diagnoses combined was similar in OSA and retrospectively matched cases. However, the adjusted risk of pancreatic and kidney cancer and melanoma were significantly higher in patients with OSA, while the risk of colorectal, breast, and prostate cancers appeared to be lower. Among individuals with a diagnosis of cancer, the presence of OSA was not associated with an increased risk for metastasis or death. Conclusions: In a large nationally representative health insurance database, OSA appears to increase the risk for only a very selective number of cancer types, and does not appear to be associated with an increased risk of metastatic cancer or cancer-related deaths. Citation: Gozal D, Ham SA, Mokhlesi B. Sleep apnea and cancer: analysis of a nationwide population sample. SLEEP 2016;39(8):1493–1500. PMID:27166241

  4. Analysis of imprecision in incurred sample reanalysis for small molecules.

    PubMed

    Subramaniam, Sriram; Patel, Devvrat; Davit, Barbara M; Conner, Dale P

    2015-01-01

    Over the years, incurred sample (IS) reanalysis (ISR) has become a tool to confirm the reliability of bioanalytical measurements. The recommendation for ISR acceptance criterion for small molecules is at least 67% of ISR samples that have reanalyzed concentrations within 20% of their original concentrations when normalized to their means. To understand the relevance of the ISR acceptance criterion and sample size requirements, simulated ISR studies evaluated the probability of ISR studies passing the acceptance criterion (ISR pass rate) as a function of IS imprecision and sample size. When IS imprecision (percent coefficient of variation: %CV) is low (≤ 10 or 1-10% CV), high ISR pass rate (≥ 99%) is attained with <50 samples. At intermediate IS imprecision (e.g., 12% CV or 7-12% CV range), 80-160 samples are required for a high ISR pass rate. When IS imprecision is at the higher end of the acceptance limit, ISR pass rate decreases significantly, and increasing sample size fails to achieve high ISR pass rate. The effect of systematic bias (e.g., instability, interconversion) on ISR pass rate is strongly dependent on sample size at intermediate IS imprecision. The results provide an understanding of the effect of IS imprecision on ISR pass rates and a framework for selection of ISR sample sizes.

  5. [Drinking water analysis for Legionella. Suggestions for sampling, laboratory analysis and assessment].

    PubMed

    Schaefer, B

    2007-03-01

    Drinking water analysis for Legionella from building installations is done quite frequently. Some questions arise from experience with this analysis. They will be discussed to allow uniform and comparable execution. Application of DIN EN ISO 19458 will lead to changes in the sampling procedure. This may make changes necessary even in current sampling and assessment programs. Concerning laboratory investigation, quality control of membrane filters and media turned out to be crucial. The assessment of quantitative results requires knowledge of the drinking water distribution system and of other facts that may be relevant for hygiene. Therefore, the assessment ought to be conducted by somebody with the respective knowledge.

  6. Guidance for establishment and implementation of a national sample management program in support of EM environmental sampling and analysis activities

    SciTech Connect

    Not Available

    1994-02-18

    The role of the National Sample Management Program (NSMP) proposed by the Department of Energy`s Office of Environmental Management (EM) is to be a resource for EM programs and for local Field Sample Management Programs (FSMPs). It will be a source of information on sample analysis and data collection within the DOE complex. Therefore the NSMP`s primary role is to coordinate and function as a central repository for information collected from the FSMPs. An additional role of the NSMP is to monitor trends in data collected from the FSMPs over time and across sites and laboratories. Tracking these trends will allow identification of potential problems in the sampling and analysis process.

  7. Buckling and dynamic analysis of drill strings for core sampling

    SciTech Connect

    Ziada, H.H., Westinghouse Hanford

    1996-05-15

    This supporting document presents buckling and dynamic stability analyses of the drill strings used for core sampling. The results of the drill string analyses provide limiting operating axial loads and rotational speeds to prevent drill string failure, instability and drill bit overheating during core sampling. The recommended loads and speeds provide controls necessary for Tank Waste Remediation System (TWRS) programmatic field operations.

  8. 40 CFR 86.540-90 - Exhaust sample analysis.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ...) Introduce span gases and set instrument gains. In order to avoid errors, span and calibrate at the same flow rates used to analyze the test sample. Span gases should have concentrations equal to 75 to 100 percent... appropriate, NOX. concentrations of samples. (6) Check zero and span points. If difference is greater than...

  9. 40 CFR 86.540-90 - Exhaust sample analysis.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ...) Introduce span gases and set instrument gains. In order to avoid errors, span and calibrate at the same flow rates used to analyze the test sample. Span gases should have concentrations equal to 75 to 100 percent... appropriate, NOX. concentrations of samples. (6) Check zero and span points. If difference is greater than...

  10. 40 CFR 86.540-90 - Exhaust sample analysis.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ...) Introduce span gases and set instrument gains. In order to avoid errors, span and calibrate at the same flow rates used to analyze the test sample. Span gases should have concentrations equal to 75 to 100 percent... appropriate, NOX. concentrations of samples. (6) Check zero and span points. If difference is greater than...

  11. Analysis of chemical components from plant tissue samples

    NASA Technical Reports Server (NTRS)

    Laseter, J. L.

    1972-01-01

    Information is given on the type and concentration of sterols, free fatty acids, and total fatty acids in plant tissue samples. All samples were analyzed by gas chromatography and then by gas chromatography-mass spectrometry combination. In each case the mass spectral data was accumulated as a computer printout and plot. Typical gas chromatograms are included as well as tables describing test results.

  12. Preliminary Proactive Sample Size Determination for Confirmatory Factor Analysis Models

    ERIC Educational Resources Information Center

    Koran, Jennifer

    2016-01-01

    Proactive preliminary minimum sample size determination can be useful for the early planning stages of a latent variable modeling study to set a realistic scope, long before the model and population are finalized. This study examined existing methods and proposed a new method for proactive preliminary minimum sample size determination.

  13. 40 CFR 86.140-94 - Exhaust sample analysis.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ...) and (2) of this section if required. (4) Check flow rates and pressures. (5) Measure THC, CO, CO2, CH4... accomplished by either of the following methods: (i) Close heated valve in THC sample (see Figures B94-5 or B94... pressure. (ii) Connect zero and span line directly to THC sample probe and introduce gases at a flow...

  14. 40 CFR 86.140-94 - Exhaust sample analysis.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ...) and (2) of this section if required. (4) Check flow rates and pressures. (5) Measure THC, CO, CO2, CH4... accomplished by either of the following methods: (i) Close heated valve in THC sample (see Figures B94-5 or B94... pressure. (ii) Connect zero and span line directly to THC sample probe and introduce gases at a flow...

  15. 40 CFR 86.140-94 - Exhaust sample analysis.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ...) and (2) of this section if required. (4) Check flow rates and pressures. (5) Measure THC, CO, CO2, CH4... accomplished by either of the following methods: (i) Close heated valve in THC sample (see Figures B94-5 or B94... pressure. (ii) Connect zero and span line directly to THC sample probe and introduce gases at a flow...

  16. 40 CFR 86.140-94 - Exhaust sample analysis.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ...) and (2) of this section if required. (4) Check flow rates and pressures. (5) Measure THC, CO, CO2, CH4... accomplished by either of the following methods: (i) Close heated valve in THC sample (see Figures B94-5 or B94... pressure. (ii) Connect zero and span line directly to THC sample probe and introduce gases at a flow...

  17. 40 CFR 86.140-94 - Exhaust sample analysis.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ...) and (2) of this section if required. (4) Check flow rates and pressures. (5) Measure THC, CO, CO2, CH4... accomplished by either of the following methods: (i) Close heated valve in THC sample (see Figures B94-5 or B94... pressure. (ii) Connect zero and span line directly to THC sample probe and introduce gases at a flow...

  18. 28 CFR 28.13 - Analysis and indexing of DNA samples.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 28 Judicial Administration 1 2010-07-01 2010-07-01 false Analysis and indexing of DNA samples. 28.13 Section 28.13 Judicial Administration DEPARTMENT OF JUSTICE DNA IDENTIFICATION SYSTEM DNA Sample Collection, Analysis, and Indexing § 28.13 Analysis and indexing of DNA samples. (a) The Federal Bureau...

  19. 28 CFR 28.13 - Analysis and indexing of DNA samples.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 28 Judicial Administration 1 2014-07-01 2014-07-01 false Analysis and indexing of DNA samples. 28.13 Section 28.13 Judicial Administration DEPARTMENT OF JUSTICE DNA IDENTIFICATION SYSTEM DNA Sample Collection, Analysis, and Indexing § 28.13 Analysis and indexing of DNA samples. (a) The Federal Bureau...

  20. 28 CFR 28.13 - Analysis and indexing of DNA samples.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 28 Judicial Administration 1 2011-07-01 2011-07-01 false Analysis and indexing of DNA samples. 28.13 Section 28.13 Judicial Administration DEPARTMENT OF JUSTICE DNA IDENTIFICATION SYSTEM DNA Sample Collection, Analysis, and Indexing § 28.13 Analysis and indexing of DNA samples. (a) The Federal Bureau...

  1. 28 CFR 28.13 - Analysis and indexing of DNA samples.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 28 Judicial Administration 1 2012-07-01 2012-07-01 false Analysis and indexing of DNA samples. 28.13 Section 28.13 Judicial Administration DEPARTMENT OF JUSTICE DNA IDENTIFICATION SYSTEM DNA Sample Collection, Analysis, and Indexing § 28.13 Analysis and indexing of DNA samples. (a) The Federal Bureau...

  2. 28 CFR 28.13 - Analysis and indexing of DNA samples.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 28 Judicial Administration 1 2013-07-01 2013-07-01 false Analysis and indexing of DNA samples. 28.13 Section 28.13 Judicial Administration DEPARTMENT OF JUSTICE DNA IDENTIFICATION SYSTEM DNA Sample Collection, Analysis, and Indexing § 28.13 Analysis and indexing of DNA samples. (a) The Federal Bureau...

  3. Analysis of uranium concentration in drinking water samples using ICPMS.

    PubMed

    Rani, Asha; Mehra, Rohit; Duggal, Vikas; Balaram, V

    2013-03-01

    Uranium concentration in drinking water samples collected from some areas of Northern Rajasthan has been measured using inductively coupled plasma mass spectrometry. The water samples were taken from hand pumps. The uranium concentration in water samples varies from 2.54-133.0 μg L with a mean value of 38.48 μg L. The uranium concentration in most of the drinking water samples exceeds the safe limit (30 μg L) recommended by the World Health Organization. The annual effective dose associated with drinking water due to uranium concentration is estimated from its annual intake using dosimetric information based on ICRP 72. The resulting value of the annual effective dose from drinking water sources is in the range of 2.11-110.45 μSv. The annual effective dose in one of the samples was found to be greater than WHO-recommended level of 100 μSv y.

  4. Aerogel as a Sample Collector and Sample Mount for Transmission XRD Analysis

    NASA Technical Reports Server (NTRS)

    Bish, D. L.; Vaniman, D. T.; Chipera, S. J.; Yen, A. S.; Jones, S. M.

    2001-01-01

    Silica aerogel can be used for dust collection and in situ X-ray analysis. Aerogels can be less absorbing than Be, and it is feasible to obtain X-ray transmission factors >50% using typical aerogels together with a 100-micrometer Be backing foil. Additional information is contained in the original extended abstract.

  5. High throughput analysis of samples in flowing liquid

    DOEpatents

    Ambrose, W. Patrick; Grace, W. Kevin; Goodwin, Peter M.; Jett, James H.; Orden, Alan Van; Keller, Richard A.

    2001-01-01

    Apparatus and method enable imaging multiple fluorescent sample particles in a single flow channel. A flow channel defines a flow direction for samples in a flow stream and has a viewing plane perpendicular to the flow direction. A laser beam is formed as a ribbon having a width effective to cover the viewing plane. Imaging optics are arranged to view the viewing plane to form an image of the fluorescent sample particles in the flow stream, and a camera records the image formed by the imaging optics.

  6. Tank 38H Saltcake Core and Supernate Sample Analysis

    SciTech Connect

    MARTINO, CHRISTOPHERJ

    2004-07-07

    This report provides details of the characterization of Tank 38H saltcake and supernate samples pulled in September 2003. The core sample HTF-E-03-114 contained approximately 4 inches of saltcake, which was soupy and brown with white chunks, and contained less than 15 mL of cloudy free liquid. The undrained bulk saltcake had a water content of 16.8 percentage weight and a bulk density that was approximately 1.94 g/cm3 at full saturation. The 137Cs activity of the bulk saltcake in sample HTF-E-03-114 was 3.72E+7 pCi/g, which corresponds to 0.3 Ci per gallon of saltcake. The 238Pu activity of the bulk saltcake was 3.62E+6 pCi/g. The filtered free liquid in sample HTF-E-03-114 had a density of 1.430 g/cm3, a 137Cs activity of 0.73 Ci/gal., and a 238Pu activity of 5.78E+3 pCi/mL. The solids filtered from the HTF-E-03-114 free liquid were primarily composed of salts (sodium nitrate and sodium carbonate monohydrate) and sodium aluminosilicates. The Tank 38H supernate samples (HTF-E-03-122 and 123) had a density of 1.45 g/cm3, a 137Cs activity of 0.65 Ci/gal, a 238Pu activity of 2.2E4 pCi/mL, and contained no visible insoluble solids. The viscosity of supernate samples HTF-E-03-122 and 123 was determined at 25 degrees Celsius, 35 degrees Celsius, and 50 degrees Celsius to be 12.1 cP, 8.1 cP, and 5.1 cP, respectively. An exponential correlation for the Tank 38H supernate viscosity was formulated for use over this temperature range. In the undrained saltcake sample, several components, including cesium, nitrite, hydroxide, phosphate, formate, and potassium, were partitioned predominantly into the interstitial liquid. Although the plutonium, uranium, neptunium, and strontium activities in the Tank 38H saltcake core sample are high compared with recent Tank 41H samples, they are low compared with previous saltcake samples from Tank 38H collected in July 2000 and July 2001. The 137Cs of the Tank 38H saltcake sample is comparable with the previous Tank 38H saltcake samples.

  7. Analysis of water in Autonomous Biological Systems (ABS) samples.

    PubMed

    Ishikawa, Y; Kobayashi, K; Seki, K; Mizutani, H; Kawasaki, Y; Koike, J; Ijiri, K; Yamashita, M; Sugiura, K; Poynter, J; MacCallum, T; Anderson, G

    1998-12-01

    Several soluble components, peptidase and amino acids, and carbon isotopic ratio in the water retrieved from flight experiments of Autonomous Biological Systems (ABS) as well as ground control samples are analyzed to interpret the condition, dynamics, material balance of the ABS ecosystems. Organic carbons in flight samples were found to be more abundant compared with the control ones, which suggested the uniform ecosystems in low gravity might easily dissolve more soluble components. The Mir-1997 flight sample showed higher C/N ratio probably because of the dissolution of carbon-rich plant materials.

  8. Analysis report for 241-BY-104 auger samples

    SciTech Connect

    Beck, M.A.; Bechtold, D.B.; Hey, B.E.

    1992-10-26

    This document details the analytical sample results for two auger samples of the tip 15 cm (6 in.) of tank 241-BY-104 salt cake. The thermal response of tank 241-BY-104 auger samples is generally mild. The level of cyanide and iron, and therefore of ferrocyanide is very low. Evidence of inhomogeneity is present for tank 241-By-104 salt cake. Mass and charge balances were less than ideal. The concentrations found for the major constituents, except chromium, are in line with the expectations.

  9. Analysis of volatile organic compounds from illicit cocaine samples

    SciTech Connect

    Robins, W.H.; Wright, B.W.

    1994-07-01

    Detection of illicit cocaine hydrochloride shipments can be improved if there is a greater understanding of the identity and quantity of volatile compounds present. This study provides preliminary data concerning the volatile organic compounds detected in a limited Set of cocaine hydrochloride samples. In all cases, cocaine was one of the major volatile compounds detected. Other tropeines were detected in almost all samples. Low concentrations of compounds that may be residues of processing solvents were observed in some samples. The equilibrium emissivity of. cocaine from cocaine hydrochloride was investigated and a value of 83 parts-per-trillion was determined.

  10. Assessment of homogeneity and minimum sample mass for cadmium analysis in powdered certified reference materials and real rice samples by solid sampling electrothermal vaporization atomic fluorescence spectrometry.

    PubMed

    Mao, Xuefei; Liu, Jixin; Huang, Yatao; Feng, Li; Zhang, Lihua; Tang, Xiaoyan; Zhou, Jian; Qian, Yongzhong; Wang, Min

    2013-01-30

    To optimize analytical quality controls of solid sampling electrothermal vaporization atomic fluorescence spectrometry (SS-ETV-AFS), the homogeneity (H(E)) of rice samples and their minimum sample mass (M) for cadmium analysis were evaluated using three certified reference materials (CRMs) and real rice samples. The effects of different grinding degrees (particle sizes <0.85, <0.25, <0.15, and >1 mm) on H(E) and M of real rice samples were also investigated. The calculated M values of three CRMs by the Pauwels equation were 2.19, 19.76, and 3.79 mg. The well-ground real rice samples (particle size <0.25 mm) demonstrated good homogeneity, and the M values were 3.48-4.27 mg. On the basis of these results, the Cd concentrations measured by the proposed method were compared with the results by microwave digestion graphite furnace atomic absorption spectrometry with a 0.5 g sample mass. There was no significant difference between these two methods, which meant that SS-ETV-AFS could be used to accurately detect Cd in rice with several milligrams of samples instead of the certified value (200 mg) or the recommended mass (200-500 mg) of the methods of the Association of Official Analytical Chemists.

  11. ENVIRONMENTAL SAMPLING AND ANALYSIS IN THE AFTERMATH OF HURRICANE KATRINA

    EPA Science Inventory

    This presentation describes the environmental sampling completed by EPA in southeastern Louisiana after Hurricane Katrina caused major catastrophic damage. Presentation also describes EPA's Environmental Unit activities in Baton Rouge and New Orleans, LA, and Dallas, TX.

  12. SAMPLING AND ANALYSIS OF MERCURY IN CRUDE OIL

    EPA Science Inventory

    Sampling and analytical procedures used to determine total mercury content in crude oils were examined. Three analytical methods were compared with respect to accuracy, precision and detection limit. The combustion method and a commercial extraction method were found adequate to...

  13. Problems in the sampling and analysis of carbon particulate

    NASA Astrophysics Data System (ADS)

    Cadle, Steven H.; Groblicki, Peter J.; Mulawa, Patricia A.

    Several thermal and wet chemical methods of separating organic from elemental carbon in particulate samples were examined. It is concluded that none of them represents an ideal separation procedure and that only a method-dependent operational definition of organic and elemental carbon is possible at this time. The best separation method appears to be a thermal procedure using 350°C air oxidation followed by pyrolysis in He at 950°C. There are also difficulties in sampling since dual filter techniques show that adsorption of organic compounds on various filter media accounted for at least 15 per cent of the total organic carbon collected during ambient sampling in Warren, MI. This adsorption further confuses the results and needs to be studied at other sampling sites.

  14. Metallurgical analysis of skylab M552 and M557 samples

    NASA Technical Reports Server (NTRS)

    Larson, D. J., Jr.

    1978-01-01

    The anomalous microstructures on the basis of phase equilibria, liquid/liquid phase separation, and liquid/solid segregation for the Skylab M557 and M552 flight samples were studied. All of the unknown diffraction spectra have been identified. The previously unknown crystal structure of the Zn3Sb2 phase the M577B Experiment was determined. Previously unreported effects due to the near-absence of the hydrostatic pressure head are documented for the M557C samples.

  15. Analysis of HEU samples from the ULBA Metallurgical Plant

    SciTech Connect

    Gift, E.H.

    1995-05-01

    In early March 1994, eight highly enriched uranium (HEU) samples were collected from materials stored at the Ulba Metallurgical Plant in Oskamen (Ust Kamenogorsk), Kazakhstan. While at the plant site, portions of four samples were dissolved and analyzed by mass spectrograph at the Ulba analytical laboratory by Ulba analysts. Three of these mass spectrograph solutions and the eight HEU samples were subsequently delivered to the Y-12 Plant for complete chemical and isotopic analyses. Chemical forms of the eight samples were uranium metal chips, U0{sub 2} powder, uranium/beryllium oxide powder, and uranium/beryllium alloy rods. All were declared by the Ulba plant to have a uranium assay of {approximately}90 wt % {sup 235}U. The uranium/beryllium powder and alloy samples were also declared to range from about 8 to 28 wt % uranium. The chemical and uranium isotopic analyses done at the Y-12 Plant confirm the Ulba plant declarations. All samples appear to have been enriched using some reprocessed uranium, probably from recovery of uranium from plutonium production reactors. As a result, all samples contain some {sup 236}U and {sup 232}U and have small but measurable quantities of plutonium. This plutonium could be the result of either contamination carried over from the enrichment process or cross-contamination from weapons material. It is not the result of direct reactor exposure. Neither the {sup 232}U nor the plutonium concentrations are sufficiently high to provide a significant industrial health hazard. Both are well within established or proposed acceptance criteria for storage at Y-12. The trace metal analyses showed that, with the exception of beryllium, there are no trace metals in any of these HEU samples that pose a significant health hazard.

  16. Analysis of Darwin Rainfall Data: Implications on Sampling Strategy

    NASA Technical Reports Server (NTRS)

    Rafael, Qihang Li; Bras, Rafael L.; Veneziano, Daniele

    1996-01-01

    Rainfall data collected by radar in the vicinity of Darwin, Australia, have been analyzed in terms of their mean, variance, autocorrelation of area-averaged rain rate, and diurnal variation. It is found that, when compared with the well-studied GATE (Global Atmospheric Research Program Atlantic Tropical Experiment) data, Darwin rainfall has larger coefficient of variation (CV), faster reduction of CV with increasing area size, weaker temporal correlation, and a strong diurnal cycle and intermittence. The coefficient of variation for Darwin rainfall has larger magnitude and exhibits larger spatial variability over the sea portion than over the land portion within the area of radar coverage. Stationary, and nonstationary models have been used to study the sampling errors associated with space-based rainfall measurement. The nonstationary model shows that the sampling error is sensitive to the starting sampling time for some sampling frequencies, due to the diurnal cycle of rain, but not for others. Sampling experiments using data also show such sensitivity. When the errors are averaged over starting time, the results of the experiments and the stationary and nonstationary models match each other very closely. In the small areas for which data are available for I>oth Darwin and GATE, the sampling error is expected to be larger for Darwin due to its larger CV.

  17. Analysis of the amount of tissue sample necessary for mitotic count and Ki-67 index in gastrointestinal stromal tumor sampling.

    PubMed

    Kobara, Hideki; Mori, Hirohito; Rafiq, Kazi; Fujihara, Shintaro; Nishiyama, Noriko; Chiyo, Taiga; Matsunaga, Tae; Ayaki, Maki; Yachida, Tatsuo; Kato, Kiyohito; Kamada, Hideki; Fujita, Koji; Morishita, Asahiro; Oryu, Makoto; Tsutsui, Kunihiko; Iwama, Hisakazu; Kushida, Yoshio; Haba, Reiji; Masaki, Tsutomu

    2015-01-01

    There are no established opinions concerning whether the amount of tissue affects the accuracy of histological analyses in gastrointestinal stromal tumors (GISTs). The aim of the present study was to investigate the appropriate amount of tissue sample needed for mitotic count based on the risk classification of GISTs and the Ki-67 index using the following three methods: endoscopic ultrasound-guided fine-needle aspiration (FNA), a novel sampling method called tunneling bloc biopsy (TBB), and biopsy forceps followed by TBB (Bf). Forty-three samples (12 FNA, 17 TBB and 14 Bf) diagnosed as GISTs by immunohistological analysis were utilized. The major and minor axes and overlay area of one piece of specimen (OPS) from the three sampling methods were measured using digital imaging software and were analyzed comparatively regarding the acquisition of histological data. The mean major and minor axes (mm) and overlay areas (mm2) were in the order of TBB > Bf > FNA. The evaluable rates by mitotic count and Ki-67 were, respectively, 75% (9/12) and 83.3% (10/12) for FNA samples, 100% (17/17) and 100% (17/17) for TBB samples, and 100% (14/14) and 100% (14/14) for Bf samples (P>0.05). Three FNA samples were judged unevaluable due to too small specimens in overall diagnosis including mitotic count and Ki-67, calculating the cut-off value for the overlay area of OPS as 0.17 mm2. Comparing the concordance rates between the pre- and post-operative samples, TBB samples was significantly better than FNA (P<0.05). Conclusively, while the amounts of tissues obtained by TBB and Bf are unnecessary for the histological assessment of mitotic count and Ki-67 index, developments of the FNA method are needed to minimize sample error. Considering the technical aspects, as well as the size of the specimens, could help to guide therapeutic planning and improve diagnostic yield for GI subepithelial tumors.

  18. Modular Sampling and Analysis Techniques for the Real-Time Analysis of Human Breath

    SciTech Connect

    Frank, M; Farquar, G; Adams, K; Bogan, M; Martin, A; Benner, H; Spadaccini, C; Steele, P; Davis, C; Loyola, B; Morgan, J; Sankaran, S

    2007-07-09

    At LLNL and UC Davis, we are developing several techniques for the real-time sampling and analysis of trace gases, aerosols and exhaled breath that could be useful for a modular, integrated system for breath analysis. Those techniques include single-particle bioaerosol mass spectrometry (BAMS) for the analysis of exhaled aerosol particles or droplets as well as breath samplers integrated with gas chromatography mass spectrometry (GC-MS) or MEMS-based differential mobility spectrometry (DMS). We describe these techniques and present recent data obtained from human breath or breath condensate, in particular, addressing the question of how environmental exposure influences the composition of breath.

  19. Prompt Gamma Activation Analysis (PGAA): Technique of choice for nondestructive bulk analysis of returned comet samples

    NASA Technical Reports Server (NTRS)

    Lindstrom, David J.; Lindstrom, Richard M.

    1989-01-01

    Prompt gamma activation analysis (PGAA) is a well-developed analytical technique. The technique involves irradiation of samples in an external neutron beam from a nuclear reactor, with simultaneous counting of gamma rays produced in the sample by neutron capture. Capture of neutrons leads to excited nuclei which decay immediately with the emission of energetic gamma rays to the ground state. PGAA has several advantages over other techniques for the analysis of cometary materials: (1) It is nondestructive; (2) It can be used to determine abundances of a wide variety of elements, including most major and minor elements (Na, Mg, Al, Si, P, K, Ca, Ti, Cr, Mn, Fe, Co, Ni), volatiles (H, C, N, F, Cl, S), and some trace elements (those with high neutron capture cross sections, including B, Cd, Nd, Sm, and Gd); and (3) It is a true bulk analysis technique. Recent developments should improve the technique's sensitivity and accuracy considerably.

  20. ISS Potable Water Sampling and Chemical Analysis Results for 2016

    NASA Technical Reports Server (NTRS)

    Straub, John E., II; Plumlee, Debrah K.; Wallace William T.; Alverson, James T.; Benoit, Mickie J.; Gillispie, Robert L.; Hunter, David; Kuo, Mike; Rutz, Jeffrey A.; Hudson, Edgar K.; Loh, Leslie J.; Gazda, Daniel B.

    2017-01-01

    This paper continues the annual tradition of summarizing at this conference the results of chemical analyses performed on archival potable water samples returned from the International Space Station (ISS). 2016 represented a banner year for life on board the ISS, including the successful conclusion for two crew members of a record one-year mission. Water reclaimed from urine and/or humidity condensate remained the primary source of potable water for the crew members of ISS Expeditions 46-50. The year 2016 was also marked by the end of a long-standing tradition of U.S. sampling and monitoring of Russian Segment potable water sources. Two water samples taken during Expedition 46 in February 2016 and returned on Soyuz 44, represented the final Russian Segment samples to be collected and analyzed by the U.S. side. Although anticipated for 2016, a rise in the total organic carbon (TOC) concentration of the product water from the U.S. water processor assembly due to breakthrough of organic contaminants from the system did not materialize, as evidenced by the onboard TOC analyzer and archive sample results.

  1. Mars Rover Sample Return: A sample collection and analysis strategy for exobiology

    NASA Technical Reports Server (NTRS)

    Sims, M. H.; Fischler, M.; Schwartz, D. E.; Rosenthal, Donald A.; Mancinelli, Rocco L.; Nedell, Susan S.; Gamble, E.; Mckay, Christopher P.

    1989-01-01

    For reasons defined elsewhere it is reasonable to search for biological signatures, both chemical and morphological, of extinct life on Mars. Life on Earth requries the presence of liquid water, therefore, it is important to explore sites on Mars where standing bodies of water may have once existed. Outcrops of layered deposits within the Valles Marineris appear to be ancient lake beds. Because the outcrops are well exposed, relatively shallow core samples would be very informative. The most important biological signature to detect would be organics, microfossils, or larger stromato-like structures, although the presence of cherts, carbonates, clays, and shales would be significant. In spite of the limitations of current robotics and pattern recognition, and the limitations of rover power, computation, Earth communication bandwidth, and time delays, a partial scenario was developed to implement such a scientific investigation. The rover instrumentation and the procedures and decisions and IR spectrometer are described in detail. Preliminary results from a collaborative effort are described, which indicate the rover will be able to autonomously detect stratification, and hence will ease the interpretation burden and lead to greater scientific productivity during the rover's lifetime.

  2. Sourcing Brazilian marijuana by applying IRMS analysis to seized samples.

    PubMed

    Shibuya, Elisa K; Souza Sarkis, Jorge E; Neto, Osvaldo Negrini; Moreira, Marcelo Z; Victoria, Reynaldo L

    2006-06-27

    The stable carbon and nitrogen isotopic ratios were measured in marijuana samples (Cannabis sativa L.) seized by the law enforcement officers in the three Brazilian production sites: Pernambuco and Bahia (the country's Northeast known as Marijuana Polygon), Pará (North or Amazon region) and Mato Grosso do Sul (Midwest). These regions are regarded as different with respect to climate and water availability, factors which impact upon the isotope fractionations of these elements within plants. It was possible to differentiate samples from the dry regions (Marijuana Polygon) from those from Mato Grosso do Sul and Pará, that present heavier rainfall. The results were in agreement with the climatic conditions of the suspected regions of origin and this demonstrates that seized samples can be used to identify the isotopic signatures of marijuana from the main producing regions in Brazil.

  3. Sample size estimation and power analysis for clinical research studies

    PubMed Central

    Suresh, KP; Chandrashekara, S

    2012-01-01

    Determining the optimal sample size for a study assures an adequate power to detect statistical significance. Hence, it is a critical step in the design of a planned research protocol. Using too many participants in a study is expensive and exposes more number of subjects to procedure. Similarly, if study is underpowered, it will be statistically inconclusive and may make the whole protocol a failure. This paper covers the essentials in calculating power and sample size for a variety of applied study designs. Sample size computation for single group mean, survey type of studies, 2 group studies based on means and proportions or rates, correlation studies and for case-control for assessing the categorical outcome are presented in detail. PMID:22870008

  4. Multielement analysis of micro-volume biological samples by ICP-MS with highly efficient sample introduction system.

    PubMed

    Takasaki, Yuka; Inagaki, Kazumi; Sabarudin, Akhmad; Fujii, Shin-Ichiro; Iwahata, Daigo; Takatsu, Akiko; Chiba, Koichi; Umemura, Tomonari

    2011-12-15

    A method for multielement analysis of micro-volume biological sample by inductively coupled plasma mass spectrometry (ICP-MS) with a highly efficient sample introduction system was presented. The sample introduction system was the combination of (1) an inert loop injection unit and (2) a high performance concentric nebulizer (HPCN) coupled with a temperature controllable cyclone chamber. The loop injection unit could introduce 20 μL samples into the carrier liquid flow of 10 μL min(-1) producing a stable signal for 100s without any dilution. The injection loop is continuously washed with 0.1M HNO(3) carrier solution during the measurement, thereby much improving sample throughput. The HPCN is a triple tube concentric nebulizer, which can generate fine aerosols and provide a stable and highly measurement sensitivity in ICP-MS at a liquid flow rate less than 10 μL min(-1). With the combination of the chamber heating at 60°C, the sensitivity obtained with the proposed sample introduction system at the liquid flow rate of 10 μL min(-1) was almost the same as that with a common concentric nebulizer and cyclone chamber system at the liquid flow rate of 1 mL min(-1), though the sample consumption rate of the HPCN was two orders of the magnitude lower than that of the common nebulizer. The validation of the proposed system was performed by analyzing the NIST SRM 1577b Bovine Liver. The observed values for 12 elements such as Na, P, S, K, Ca, Mn, Fe, Co, Cu, Zn, Mo, Cd were in good agreement with their certified values and information value. Satisfactory analytical results for 14 elements such as Na, Mg, P, S, K, Ca, Cr, Mn, Fe, Ni, Cu, Zn, Y, Ba in Escherichia coli sample were also obtained. The proposed sample introduction system was quite effective in the cases when only micro-volume of biological sample is available.

  5. Aerosol Sampling and Analysis for the GEOTRACES Program

    NASA Astrophysics Data System (ADS)

    Landing, W. M.

    2008-12-01

    The GEOTRACES Science Plan emphasizes the importance of atmospheric deposition on the budgets and biogeochemistry of trace elements and isotopes in the world's oceans. With funding from the National Science Foundation, an aerosol and rainfall sampling program is being developed for use on future GEOTRACES cruises. This includes preparation and testing of dual high-volume TISCH 5170-VBL aerosol samplers for inorganic trace elements and isotopes, major ions, organic material, and isotopes of nitrogen and oxygen. A third 5170-VBL aerosol sampler is equipped with a 5-stage Sierra-style slotted impactor to collect size-fractionated aerosols for chemical measurements. The aerosol samplers will be operated using wind speed and wind sector control to avoid contamination from ship's exhaust. Duplicate automated rain samplers have also been developed to collect unfiltered and filtered rain samples. Rainfall will be filtered immediately (during collection) to avoid re-adsorption artifacts. Two intercalibration experiments are planned where aerosol and rainfall subsamples will be distributed to the community for testing and validation of analytical methods. The first experiment is being conducted in early September 2008 on the roof at RSMAS/University of Miami. Results from the GEOTRACES aerosol samplers will be compared to a multi-channel aerosol sampling system (using 47mm PCTE filters), and with ongoing aerosol collections at RSMAS. The second experiment is planned for the atmospheric sampling tower at Bellows AFB (Oahu, HI) in summer 2009. Details of the sampling equipment and sample collection methods will be discussed, along with preliminary results from the first intercalibration experiment. Community input will be solicited for planning the second intercalibration experiment.

  6. Nuclear forensic analysis of a non-traditional actinide sample.

    PubMed

    Doyle, Jamie L; Kuhn, Kevin; Byerly, Benjamin; Colletti, Lisa; Fulwyler, James; Garduno, Katherine; Keller, Russell; Lujan, Elmer; Martinez, Alexander; Myers, Steve; Porterfield, Donivan; Spencer, Khalil; Stanley, Floyd; Townsend, Lisa; Thomas, Mariam; Walker, Laurie; Xu, Ning; Tandon, Lav

    2016-10-01

    Nuclear forensic publications, performance tests, and research and development efforts typically target the bulk global inventory of intentionally safeguarded materials, such as plutonium (Pu) and uranium (U). Other materials, such as neptunium (Np), pose a nuclear security risk as well. Trafficking leading to recovery of an interdicted Np sample is a realistic concern especially for materials originating in countries that reprocesses fuel. Using complementary forensic methods, potential signatures for an unknown Np oxide sample were investigated. Measurement results were assessed against published Np processes to present hypotheses as to the original intended use, method of production, and origin for this Np oxide.

  7. Nuclear forensic analysis of a non-traditional actinide sample

    DOE PAGES

    Doyle, Jamie L.; Kuhn, Kevin John; Byerly, Benjamin; ...

    2016-06-15

    Nuclear forensic publications, performance tests, and research and development efforts typically target the bulk global inventory of intentionally safeguarded materials, such as plutonium (Pu) and uranium (U). Other materials, such as neptunium (Np), pose a nuclear security risk as well. Trafficking leading to recovery of an interdicted Np sample is a realistic concern especially for materials originating in countries that reprocesses fuel. Using complementary forensic methods, potential signatures for an unknown Np oxide sample were investigated. Measurement results were assessed against published Np processes to present hypotheses as to the original intended use, method of production, and origin for thismore » Np oxide.« less

  8. Nuclear forensic analysis of a non-traditional actinide sample

    SciTech Connect

    Doyle, Jamie L.; Kuhn, Kevin John; Byerly, Benjamin; Colletti, Lisa Michelle; Fulwyler, James Brent; Garduno, Katherine; Keller, Russell; Lujan, Elmer J. W.; Martinez, Alexander; Myers, Steve Charles; Porterfield, Donivan R.; Spencer, Khalil J.; Stanley, Floyd E.; Townsend, Lisa Ellen; Thomas, Mariam; Walker, Laurie F.; Xu, Ning; Tandon, Lav

    2016-06-15

    Nuclear forensic publications, performance tests, and research and development efforts typically target the bulk global inventory of intentionally safeguarded materials, such as plutonium (Pu) and uranium (U). Other materials, such as neptunium (Np), pose a nuclear security risk as well. Trafficking leading to recovery of an interdicted Np sample is a realistic concern especially for materials originating in countries that reprocesses fuel. Using complementary forensic methods, potential signatures for an unknown Np oxide sample were investigated. Measurement results were assessed against published Np processes to present hypotheses as to the original intended use, method of production, and origin for this Np oxide.

  9. Current trends and challenges in sample preparation for metallic nanoparticles analysis in daily products and environmental samples: A review

    NASA Astrophysics Data System (ADS)

    De la Calle, Inmaculada; Menta, Mathieu; Séby, Fabienne

    2016-11-01

    Due to the increasing use of nanoparticles (NPs) in consumer products, it becomes necessary to develop different strategies for their detection, identification, characterization and quantification in a wide variety of samples. Since the analysis of NPs in consumer products and environmental samples is particularly troublesome, a detailed description of challenges and limitations is given here. This review mainly focuses on sample preparation procedures applied for the mostly used techniques for metallic and metal oxide NPs characterization in consumer products and most outstanding publications of biological and environmental samples (from 2006 to 2015). We summarize the procedures applied for total metal content, extraction/separation and/or preconcentration of NPs from the matrix, separation of metallic NPs from their ions or from larger particles and NPs' size fractionation. Sample preparation procedures specifically for microscopy are also described. Selected applications in cosmetics, food, other consumer products, biological tissues and environmental samples are presented. Advantages and inconveniences of those procedures are considered. Moreover, selected simplified schemes for NPs sample preparation, as well as usual techniques applied are included. Finally, promising directions for further investigations are discussed.

  10. Methodological Issues of Sample Collection and Analysis of Exhaled Breath

    EPA Science Inventory

    Recommended standardized procedures have been developed for measurement of exhaled lower respiratory nitric oxide (NO) and nasal NO. It would be desirable to develop similar guidelines for the sampling of exhaled breath related to other compounds. For such systemic volatile o...

  11. Experimental Approaches to Microarray Analysis of Tumor Samples

    ERIC Educational Resources Information Center

    Furge, Laura Lowe; Winter, Michael B.; Meyers, Jacob I.; Furge, Kyle A.

    2008-01-01

    Comprehensive measurement of gene expression using high-density nucleic acid arrays (i.e. microarrays) has become an important tool for investigating the molecular differences in clinical and research samples. Consequently, inclusion of discussion in biochemistry, molecular biology, or other appropriate courses of microarray technologies has…

  12. Incorporating Computer-Aided Language Sample Analysis into Clinical Practice

    ERIC Educational Resources Information Center

    Price, Lisa Hammett; Hendricks, Sean; Cook, Colleen

    2010-01-01

    Purpose: During the evaluation of language abilities, the needs of the child are best served when multiple types and sources of data are included in the evaluation process. Current educational policies and practice guidelines further dictate the use of authentic assessment data to inform diagnosis and treatment planning. Language sampling and…

  13. Sampling of vehicle emissions for chemical analysis and biological testing.

    PubMed Central

    Schuetzle, D

    1983-01-01

    Representative dilution tube sampling techniques for particulate and gas phase vehicle emissions are described using Teflon filter media and XAD-2 resin. More than 90% of the total gas (C8-C18) and particulate direct acting Ames assay mutagenicity (TA 98) was found in the particulate phase. The gas and particulate phase material was fractionated by HPLC into nonpolar, moderately polar and highly polar chemical fractions. The moderately polar chemical fraction of the particulates contained more than 50% of the direct acting Ames assay mutagenicity for the total extract. The concentration of oxygenated polynuclear aromatic hydrocarbons (oxy-PAH) and nitrated PAH (nitro-PAH) identified in the moderately polar particulate fractions are given. Nitro-PAH account for most of the direct-acting (TA 98) Ames assay mutagenicity in these moderately polar fractions. Reactions and kinetic expressions for chemical conversion of PAH are presented. Chemical conversion of PAH to nitro-PAH during dilution tube sampling of particulates on Teflon filters and gases on XAD-2 resin is a minor problem (representing 10-20%, on the average, of the 1-nitropyrene found in extracts) at short (46 min) sampling times, at low sampling temperatures (42 degrees C), and in diluted exhaust containing 3 ppm NO2. Particulate emissions collected from dilution tubes on filter media appear to be representative of what is emitted in the environment as based upon a comparison of highway and laboratory studies. PMID:6186484

  14. Reaching a Representative Sample of College Students: A Comparative Analysis

    ERIC Educational Resources Information Center

    Giovenco, Daniel P.; Gundersen, Daniel A.; Delnevo, Cristine D.

    2016-01-01

    Objective: To explore the feasibility of a random-digit dial (RDD) cellular phone survey in order to reach a national and representative sample of college students. Methods: Demographic distributions from the 2011 National Young Adult Health Survey (NYAHS) were benchmarked against enrollment numbers from the Integrated Postsecondary Education…

  15. THE ESTABLISHMENT OF LABORATORY GUIDELINES FOR ANALYSIS OF BIOTERRORISM SAMPLES

    EPA Science Inventory

    After the attack on the World Trade Center on September 11, 2002, and the subsequent deaths associated with Bacillus anthracis spore contaminated mail, a worldwide need was apparent for increased laboratory capacity to safely analyze bioterrorism samples. The U.S. Department of ...

  16. Description and Analysis of Core Samples: The Lunar Experience

    NASA Technical Reports Server (NTRS)

    McKay, David S.; Allton, Judith H.

    1997-01-01

    Although no samples yet have been returned from a comet, extensive experience from sampling another solar system body, the Moon, does exist. While, in overall structure, composition, and physical properties the Moon bears little resemblance to what is expected for a comet, sampling the Moon has provided some basic lessons in how to do things which may be equally applicable to cometary samples. In particular, an extensive series of core samples has been taken on the Moon, and coring is the best way to sample a comet in three dimensions. Data from cores taken at 24 Apollo collection stations and 3 Luna sites have been used to provide insight into the evolution of the lunar regolith. It is now well understood that this regolith is very complex and reflects gardening (stirring of grains by micrometeorites), erosion (from impacts and solar wind sputtering), maturation (exposure on the bare lunar surface to solar winds ions and micrometeorite impacts) and comminution of coarse grains into finer grains, blanket deposition of coarse-grained layers, and other processes. All of these processes have been documented in cores. While a cometary regolith should not be expected to parallel in detail the lunar regolith, it is possible that the upper part of a cometary regolith may include textural, mineralogical, and chemical features which reflect the original accretion of the comet, including a form of gardening. Differences in relative velocities and gravitational attraction no doubt made this accretionary gardening qualitatively much different than the lunar version. Furthermore, at least some comets, depending on their orbits, have been subjected to impacts of the uppermost surface by small projectiles at some time in their history. Consequently, a more recent post-accretional gardening may have occurred. Finally, for comets which approach the sun, large scale erosion may have occurred driven by gas loss. The uppermost material of these comets may reflect some of the features

  17. Phonological process analysis from spontaneous speech: the influence of sample size.

    PubMed

    Crary, M A

    1983-03-01

    Phonological process analysis is becoming a popular technique for the evaluation of unintelligible children and adults. Spontaneous speech sampling procedures have been advocated as a representative sampling base for phonological process analysis; however, little research has been reported detailing the parameters of spontaneous samples in reference to this assessment technique. The purpose of the present study was to evaluate the influence of increasing sample size on phonological process analyses from spontaneous speech. Results clearly indicated that samples of 50 words provided descriptive information similar to samples of 100 words. Additional studies are called for to investigate other variables that might influence the results of spontaneous speech analysis.

  18. GUM Analysis for TIMS Isotopic Ratios in BEP0 Graphite Qualification Samples, Round 2

    SciTech Connect

    Gerlach, David C.; Heasler, Patrick G.; Reid, Bruce D.

    2009-01-01

    In May 2007, one set of three samples from NBL were addressed to Steve Petersen for TIMS analysis, and included BEP0 samples numbered 27008, 30986, and 50846. All cores were trimmed by tooling, and lightly cleaned by CO2 pellet blasting. Small discs were cut from the second set of samples for SIMS analysis, with the remainder of each used for TIMS preparation.

  19. Developing the Noncentrality Parameter for Calculating Group Sample Sizes in Heterogeneous Analysis of Variance

    ERIC Educational Resources Information Center

    Luh, Wei-Ming; Guo, Jiin-Huarng

    2011-01-01

    Sample size determination is an important issue in planning research. In the context of one-way fixed-effect analysis of variance, the conventional sample size formula cannot be applied for the heterogeneous variance cases. This study discusses the sample size requirement for the Welch test in the one-way fixed-effect analysis of variance with…

  20. A confirmatory factor analysis of the WAIS-III in a clinical sample with crossvalidation in the standardization sample.

    PubMed

    Burton, D Bradley; Ryan, Joseph J; Axelrod, Bradley N; Schellenberger, Tony

    2002-05-01

    A maximum likelihood confirmatory factor analysis of the Wechsler Adult Intelligence Scale-III (WAIS-III) was performed by applying LISREL 8 to a clinical sample (n=328). Analyses were designed to determine which of the nine hypothesized oblique factor solutions could best explain intelligence as measured by the WAIS-III in the general clinical sample. Competing latent variable models were identified in previous studies and a priori model modifications were made to test derivations of the nine base models. Results in the clinical sample were crossvalidated by testing all models in the normative sample used in the standardization of the scale. Findings in both the clinical and standardization samples supported a six-factor model including Semantic Memory, Verbal Reasoning, Constructional Praxis, Visual Reasoning, Working Memory, and Processing Speed factors. Our analysis differed from that presented in the WAIS-III manual as we tested more complex models of intelligence in addition to the ones evaluated by the test publishers. As a result, a six-factor model that corresponded to an expanded version of a model based on Horn's Gf-Gc theory was empirically supported as having the best fit to the data. More complex derivations of this model failed to achieve sufficient goodness of fit.

  1. Uniform sampling analysis of a hybrid phase-locked loop with a sample-and-hold phase detector

    NASA Technical Reports Server (NTRS)

    Barab, S.; Mcbride, A. L.

    1975-01-01

    Phase-locked-loop (PLL) bit synchronizers often employ integrate-and-dump type phase detectors that provide phase error information only at discrete points in time. Usually these phase detectors are followed by sample-and-hold circuits to produce a stairstep error voltage as the input to a standard analog circuit loop filter. When the loop is configured in this manner, it is referred to as a hybrid PLL. Sampled-data analysis methods (Z transforms) are used to determine the stability and transient response of this loop.

  2. Raman spectroscopic analysis of real samples: Brazilian bauxite mineralogy.

    PubMed

    Faulstich, Fabiano Richard Leite; Castro, Harlem V; de Oliveira, Luiz Fernando Cappa; Neumann, Reiner

    2011-10-01

    In this investigation, Raman spectroscopy with 1064 and 632.8 nm excitation was used to investigate real mineral samples of bauxite ore from mines of Northern Brazil, together with Raman mapping and X-rays diffraction. The obtained results show clearly that the use of microRaman spectroscopy is a powerful tool for the identification of all the minerals usually found in bauxites: gibbsite, kaolinite, goethite, hematite, anatase and quartz. Bulk samples can also be analysed, and FT-Raman is more adequate due to better signal-to-noise ratio and representativity, although not efficient for kaolinite. The identification of fingerprinting vibrations for all the minerals allows the acquisition of Raman-based chemical maps, potentially powerful tools for process mineralogy applied to bauxite ores.

  3. Continuous water sampling and water analysis in estuaries

    USGS Publications Warehouse

    Schemel, L.E.; Dedini, L.A.

    1982-01-01

    Salinity, temperature, light transmission, oxygen saturation, pH, pCO2, chlorophyll a fluorescence, and the concentrations of nitrate, nitrite, dissolved silica, orthophosphate, and ammonia are continuously measured with a system designed primarily for estuarine studies. Near-surface water (2-m depth) is sampled continuously while the vessel is underway; on station, water to depths of 100 m is sampled with a submersible pump. The system is comprised of commercially available instruments, equipment, and components, and of specialized items designed and fabricated by the authors. Data are read from digital displays, analog strip-chart recorders, and a teletype printout, and can be logged in disc storage for subsequent plotting. Data records made in San Francisco Bay illustrate physical, biological, and chemical estuarine processes, such as mixing and phytoplankton net production. The system resolves large- and small-scale events, which contributes to its reliability and usefulness.

  4. Selenium sampling and analysis in coal combustion systems

    SciTech Connect

    DeVito, M.S.; Carlson, R.J.

    1995-12-31

    The Clean Air Act Amendments of 1990 (CAAA) identified 189 elements and compounds that are classified by the U.S. EPA as hazardous air pollutants (HAPs). Among these are eleven inorganic trace elements found in coal. A provision of the CAAA required EPA to conduct a study of the health and environmental impacts of HAP emissions from electric utility generating units. EPA has completed a number of draft documents in compliance with this mandate. For trace element emission estimates, they have relied on a number of field tests which were conducted by a variety of organizations including the U.S. Department of Energy (DOE). The DOE program utilized the EPA Method 29 sampling train to measure the emissions of trace elements including Se. EPA Method 29 is validated for municipal waste combustor sampling but not for coal-fired combustion sources.

  5. UMTRA Project water sampling and analysis plan, Salt Lake City, Utah. Revision 1

    SciTech Connect

    1995-06-01

    This water sampling and analysis plan describes planned, routine ground water sampling activities at the US Department of Energy Uranium Mill Tailings Remedial Action Project site in Salt Lake City, Utah. This plan identifies and justifies sampling locations, analytical parameters, detection limits, and sampling frequencies for routine monitoring of ground water, sediments, and surface waters at monitoring stations on the site.

  6. UMTRA project water sampling and analysis plan, Grand Junction, Colorado

    SciTech Connect

    Not Available

    1994-07-01

    Surface remedial action will be completed at the Grand Junction processing site during the summer of 1994. Results of 1993 water sampling indicate that ground water flow conditions and ground water quality at the processing site have remained relatively constant with time. Uranium concentrations in ground water continue to exceed the maximum concentration limits, providing the best indication of the extent of contaminated ground water. Evaluation of surface water quality of the Colorado River indicate no impact from uranium processing activities. No compliance monitoring at the Cheney disposal site has been proposed because ground water in the Dakota Sandstone (uppermost aquifer) is classified as limited-use (Class 111) and because the disposal cell is hydrogeologically isolated from the uppermost aquifer. The following water sampling and water level monitoring activities are planned for calendar year 1994: (i) Semiannual (early summer and late fall) sampling of six existing monitor wells at the former Grand Junction processing site. Analytical results from this sampling will be used to continue characterizing hydrogeochemical trends in background ground water quality and in the contaminated ground water area resulting from source term (tailings) removal. (ii) Water level monitoring of approximately three proposed monitor wells projected to be installed in the alluvium at the processing site in September 1994. Data loggers will be installed in these wells, and water levels will be electronically monitored six times a day. These long-term, continuous ground water level data will be collected to better understand the relationship between surface and ground water at the site. Water level and water quality data eventually will be used in future ground water modeling to establish boundary conditions in the vicinity of the Grand Junction processing site. Modeling results will be used to help demonstrate and document the potential remedial alternative of natural flushing.

  7. Surface plasmon resonance biosensing toward real biological sample analysis

    NASA Astrophysics Data System (ADS)

    Cunche, Audrey; Bolduc, Olivier R.; Masson, Jean-Francois

    2009-05-01

    The development of monolayer chemistry based on amino acid and short peptides decreases significantly the nonspecific adsorption from biological samples such as serum. Nonspecific adsorption of proteins onto the surface of biosensors currently limits the applicability of many biosensing techniques in real biological samples. In order to minimize this problem, a methodology to immobilize short peptides on surface plasmon resonance (SPR) biosensors was developed using a short chain alkyl thiol monolayer derived with the selected peptides. The chain length of the alkane thiol linking the amino acid to the gold surface influences the physico-chemical properties of the layer and the amount of nonspecifically adsorbed proteins. Varying the composition of the monolayer with peptides formed from the natural amino acids investigates the physico-chemical properties required to minimize nonspecific adsorption of serum. It was observed from monolayers of single amino acids that the composition of the side chain of the amino acid greatly influences the resistance to nonspecific adsorption, with more polar, ionic and small chains resulting in an improved performance in biological samples. Building peptides of different lengths resulted in a further decrease of the amount of nonspecifically bound proteins from serum. Leaving the terminal carboxylic acid end of the peptide unreacted provides an anchoring point for a molecular receptor in the design of a biosensor. Biosensing will be demonstrated with a model system of β-lactamase.

  8. Extremely isolated galaxies - I. Sample and simulation analysis

    NASA Astrophysics Data System (ADS)

    Spector, O.; Brosch, N.

    2016-02-01

    We have selected a sample of extremely isolated galaxies (EIGs) from the local Universe (z < 0.024), using a simple isolation criterion: having no known neighbours closer than 300 km s-1(3 h-1 Mpc) in the three-dimensional redshift space (α, δ, z). The sample is unique both in its level of isolation and in the fact that it utilizes H I redshifts from the Arecibo Legacy Fast ALFA (ALFALFA) survey. We analysed the EIG sample using cosmological simulations and found that it contains EIGs with normal mass haloes which have evolved gradually with little or no `major events' (major mergers, or major mass-loss events) in the last 3 Gyr. The fraction of EIGs which deviate from this definition (false positives) is 5-10 per cent. For the general population of dark matter haloes, it was further found that the mass accretion (relative to the current halo mass) is affected by the halo environment mainly through strong interactions with its neighbours. As long as a halo does not experience major events, its mass accretion history does not depend significantly on its environment. `Major events' seem to be the main mechanism that creates low-mass subhaloes (Mhalo < 1010 h- 1 M⊙) that host galaxies (with Mg ≲ -14).

  9. The performance analysis based on SAR sample covariance matrix.

    PubMed

    Erten, Esra

    2012-01-01

    Multi-channel systems appear in several fields of application in science. In the Synthetic Aperture Radar (SAR) context, multi-channel systems may refer to different domains, as multi-polarization, multi-interferometric or multi-temporal data, or even a combination of them. Due to the inherent speckle phenomenon present in SAR images, the statistical description of the data is almost mandatory for its utilization. The complex images acquired over natural media present in general zero-mean circular Gaussian characteristics. In this case, second order statistics as the multi-channel covariance matrix fully describe the data. For practical situations however, the covariance matrix has to be estimated using a limited number of samples, and this sample covariance matrix follow the complex Wishart distribution. In this context, the eigendecomposition of the multi-channel covariance matrix has been shown in different areas of high relevance regarding the physical properties of the imaged scene. Specifically, the maximum eigenvalue of the covariance matrix has been frequently used in different applications as target or change detection, estimation of the dominant scattering mechanism in polarimetric data, moving target indication, etc. In this paper, the statistical behavior of the maximum eigenvalue derived from the eigendecomposition of the sample multi-channel covariance matrix in terms of multi-channel SAR images is simplified for SAR community. Validation is performed against simulated data and examples of estimation and detection problems using the analytical expressions are as well given.

  10. Collection, chemical analysis, and evaluation of coal samples in 1975

    USGS Publications Warehouse

    Swanson, Vernon Emanuel; Medlin, J.H.; Hatch, J.R.; Coleman, S.L.; Wood, G.H.; Woodruff, S.D.; Hildebrand, R.T.

    1976-01-01

    During 1975, the U.S. Geological Survey, in cooperation with other Federal and State agencies, university groups, and private companies, continued its program to augment and refine information on the composition of coal in the United States. This report includes all analytical data on 799 channel samples of coal beds from major operating mines and core holes in 28 States, collected mainly by State Geological Surveys under a cooperative program funded largely by the U.S. Energy Research and Development Administration. For each sample, the U.S. Geological Survey has quantitatively determined the amounts of 24 major, minor, and trace elements (including AI, As, Cd, Cu, F, Hg, Mn, Na, Pb, Se, U, and Zn), and has semiquantitatively determined the concentrations of 15 to 20 additional trace elements (including B, Be, Cr, Ge, Mo, Ni, and V). In addition, the U.S. Bureau of Mines has provided proximate and ultimate analyses, and Btu and forms-of-sulfur determinations on 488 of the samples. Statistical summaries of the data are given for all coal samples in the United States, for coal divided by rank (53 anthracite, 509 bituminous coal, 183 subbituminous coal, and 54 lignite samples), and the arithmetic means, ranges, and geometric means and deviations are given for the coal in each of seven different major coal areas in the United States. For example, the average coal in the United States contains 11.3 percent ash, 10.0 percent moisture, 2.0 percent sulfur, and has 11,180 Btu per pound; of the 10 major oxides determined on the 525?C ash, the average SiO2 content is 38 percent, Al2O3 20 percent, and Na2O 0.67 percent; the average Cd content is 7.3 ppm, Pb 114 ppm, and Zn 151 ppm (range 1 ppm to 6.0 percent). As determined on the raw coal, the average Hg content is 0.18 ppm (range <0.01 to 63.0 ppm), the Se content 4.1 ppm (range <0.1 to 150 ppm), and the U content 1.8 ppm (range <0.2 to 42.9 ppm).

  11. Nuclear monitoring by nonradioactive noble gas sampling and analysis

    SciTech Connect

    Fearey, B.L.; Nakhleh, C.W.; Stanbro, W.D.

    1997-10-01

    This is the final report of a two-year, Laboratory Directed Research and Development (LDRD) project at the Los Alamos National Laboratory (LANL). The perceived importance of measuring the xenon and krypton isotopics of nuclear activities has increased substantially in recent years. We have performed a systems analysis and theoretical simulation of the production, atmospheric dispersion, and isotopic abundances of noble-gas fission products, addressing several questions of interest, including: the relative isotopic variation as a function of nuclear fuel composition, reactor operational history, reactor type, distance from stack, and ambient meteorological conditions. Of particular importance in this analysis was the question of back-calculating process parameters of interest given noble-gas isotopic data. An analysis of the effect of measurement uncertainties was also performed. The results of these analyses indicate that this monitoring concept should be experimentally feasible.

  12. Estimating the Expected Value of Sample Information Using the Probabilistic Sensitivity Analysis Sample: A Fast, Nonparametric Regression-Based Method.

    PubMed

    Strong, Mark; Oakley, Jeremy E; Brennan, Alan; Breeze, Penny

    2015-07-01

    Health economic decision-analytic models are used to estimate the expected net benefits of competing decision options. The true values of the input parameters of such models are rarely known with certainty, and it is often useful to quantify the value to the decision maker of reducing uncertainty through collecting new data. In the context of a particular decision problem, the value of a proposed research design can be quantified by its expected value of sample information (EVSI). EVSI is commonly estimated via a 2-level Monte Carlo procedure in which plausible data sets are generated in an outer loop, and then, conditional on these, the parameters of the decision model are updated via Bayes rule and sampled in an inner loop. At each iteration of the inner loop, the decision model is evaluated. This is computationally demanding and may be difficult if the posterior distribution of the model parameters conditional on sampled data is hard to sample from. We describe a fast nonparametric regression-based method for estimating per-patient EVSI that requires only the probabilistic sensitivity analysis sample (i.e., the set of samples drawn from the joint distribution of the parameters and the corresponding net benefits). The method avoids the need to sample from the posterior distributions of the parameters and avoids the need to rerun the model. The only requirement is that sample data sets can be generated. The method is applicable with a model of any complexity and with any specification of model parameter distribution. We demonstrate in a case study the superior efficiency of the regression method over the 2-level Monte Carlo method.

  13. 105-N basin sediment disposition phase-two sampling and analysis plan

    SciTech Connect

    Smith, R. C.

    1997-03-14

    The sampling and analysis plan for Phase 2 of the 105-N Basin sediment disposition task defines the sampling and analytical activities that will be performed to support characterization of the sediment and selection of an appropriate sediment disposal option.

  14. Heater-Integrated Cantilevers for Nano-Samples Thermogravimetric Analysis

    PubMed Central

    Toffoli, Valeria; Carrato, Sergio; Lee, Dongkyu; Jeon, Sangmin; Lazzarino, Marco

    2013-01-01

    The design and characteristics of a micro-system for thermogravimetric analysis (TGA) in which heater, temperature sensor and mass sensor are integrated into a single device are presented. The system consists of a suspended cantilever that incorporates a microfabricated resistor, used as both heater and thermometer. A three-dimensional finite element analysis was used to define the structure parameters. TGA sensors were fabricated by standard microlithographic techniques and tested using milli-Q water and polyurethane microcapsule. The results demonstrated that our approach provides a faster and more sensitive TGA with respect to commercial systems.

  15. Ion-beam analysis of meteoritic and lunar samples

    NASA Technical Reports Server (NTRS)

    Tombrello, T. A.

    1979-01-01

    Charged particle-induced nuclear reactions were used in the following problems: the determination of elemental abundances of boron and fluorine in carbonaceous chondritic meteorites; the identification of products of lunar vulcanism; and the study of solar wind-implanted atoms in lunar materials. The technique was seen as an important supplement to other methods of elemental and isotopic analysis. This was especially true for cases involving light elements at very low concentrations or where high resolution depth distribution information was needed in non-destructive analysis.

  16. Instrumentation for motor-current signature analysis using synchronous sampling

    SciTech Connect

    Castleberry, K.N.

    1996-07-01

    Personnel in the Instrumentation and Controls Division at Oak Ridge National Laboratory, in association with the United States Enrichment Corporation, the U.S. Navy, and various Department of Energy sponsors, have been involved in the development and application of motor-current signature analysis for several years. In that time, innovation in the field has resulted in major improvements in signal processing, analysis, and system performance and capabilities. Recent work has concentrated on industrial implementation of one of the most promising new techniques. This report describes the developed method and the instrumentation package that is being used to investigate and develop potential applications.

  17. 40 CFR 761.314 - Chemical analysis of standard wipe test samples.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 31 2014-07-01 2014-07-01 false Chemical analysis of standard wipe test samples. 761.314 Section 761.314 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY....314 Chemical analysis of standard wipe test samples. Perform the chemical analysis of standard...

  18. UMTRA project water sampling and analysis plan, Durango, Colorado

    SciTech Connect

    Not Available

    1994-01-01

    Surface remedial action has been completed at the Uranium Mill Tailings Remedial Action Project in Durango, Colorado. Contaminated soil and debris have been removed from the former processing site and placed in the Bodo Canyon disposal cell. Ground water at the former uranium mill/tailings site and raffinate pond area has been contaminated by the former milling operations. The ground water at the disposal site was not impacted by the former milling operations at the time of the cell`s construction. Activities for fiscal 1994 involve ground water sampling and site characterization of the disposal site.

  19. Water Sample Analysis With the Integrated Virus Detection System

    DTIC Science & Technology

    2010-06-01

    ultrafiltered to reduce and concentrate the volume from 1 L to 1.2 mL. This ultrafiltration (UF) was accomplished in -60 min. The remaining volume was...collected and analyzed with the IVDS. In general, the samples were concentrated with the tangential flow ( ultrafiltration ) filter system before IVDS...Biological Center: Aberdeen Proving Ground, MD, 1999; UNCLASSIFIED Report (AD-A368 535). 2. Wick, C.H.; McCubbin, P.E. Removing Complex Growth Media from MS2

  20. Determining Sample Sizes for Precise Contrast Analysis with Heterogeneous Variances

    ERIC Educational Resources Information Center

    Jan, Show-Li; Shieh, Gwowen

    2014-01-01

    The analysis of variance (ANOVA) is one of the most frequently used statistical analyses in practical applications. Accordingly, the single and multiple comparison procedures are frequently applied to assess the differences among mean effects. However, the underlying assumption of homogeneous variances may not always be tenable. This study…

  1. Spatial analysis of NDVI readings with difference sampling density

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Advanced remote sensing technologies provide research an innovative way of collecting spatial data for use in precision agriculture. Sensor information and spatial analysis together allow for a complete understanding of the spatial complexity of a field and its crop. The objective of the study was...

  2. Minimum Sample Size Requirements for Mokken Scale Analysis

    ERIC Educational Resources Information Center

    Straat, J. Hendrik; van der Ark, L. Andries; Sijtsma, Klaas

    2014-01-01

    An automated item selection procedure in Mokken scale analysis partitions a set of items into one or more Mokken scales, if the data allow. Two algorithms are available that pursue the same goal of selecting Mokken scales of maximum length: Mokken's original automated item selection procedure (AISP) and a genetic algorithm (GA). Minimum…

  3. Improvements in PIXE analysis of hourly particulate matter samples

    NASA Astrophysics Data System (ADS)

    Calzolai, G.; Lucarelli, F.; Chiari, M.; Nava, S.; Giannoni, M.; Carraresi, L.; Prati, P.; Vecchi, R.

    2015-11-01

    Most air quality studies on particulate matter (PM) are based on 24-h averaged data; however, many PM emissions as well as their atmospheric dilution processes change within a few hours. Samplings of PM with 1-h resolution can be performed by the streaker sampler (PIXE International Corporation), which is designed to separate the fine (aerodynamic diameter less than 2.5 μm) and the coarse (aerodynamic diameter between 2.5 and 10 μm) fractions of PM. These samples are efficiently analyzed by Particle Induced X-ray Emission (PIXE) at the LABEC laboratory of INFN in Florence (Italy), equipped with a 3 MV Tandetron accelerator, thanks to an optimized external-beam set-up, a convenient choice of the beam energy and suitable collecting substrates. A detailed description of the adopted set-up and results from a methodological study on the detection limits for the selection of the optimal beam energy are shown; the outcomes of the research on alternative collecting substrates, which produce a lower background during the measurements, and with lower contaminations, are also discussed.

  4. Organic analysis of lunar samples and the Martian surface.

    PubMed

    Oro, J; Flory, D

    1973-01-01

    In addition to the organogenic elements (H, C, N, O, S, P) which are necessary for the synthesis of organic molecules, the lunar samples from Apollo 11, 12, 14 and 15 contain substantial amounts (approximately equal to 10 to 100 microgram/g) of CO, N2 and CO2, which are released at relatively high temperatures and smaller amounts (approximately equal to 0.1 to 10 microgram/g) of more complex organic compounds (e.g. benzene). Most of these analyses have been performed by mass spectrometry or by combined gas chromatography-mass spectrometry after appropriate volatilization. The release of very small amounts of water has also been observed and is consistent with the findings of goethite (FeO.OH) and with measurements by the suprathermal ion detector. The lunar surface provides one of the less favorable solar system models for the synthesis of organic compounds yet small amounts of these compounds have been detected in the returned samples. It is reasonable to assume that the different physical and developmental features of the planet Mars (increased gravitational field, presence of an atmosphere with CO2, CO and H2O, recent volcanic and tectonic activity, etc.) would favor an increased organic content of the surface of this planet relative to the moon. Therefore the organic molecules present in the Martian soil should be measurable by miniaturized mass spectrometers after fractional distillation or gas chromatographic separation of the volatiles released by moderate heating.

  5. Statistical analysis of archeomagnetic samples of Teotihuacan, Mexico

    NASA Astrophysics Data System (ADS)

    Soler-Arechalde, A. M.

    2012-12-01

    Teotihuacan was the one of the most important metropolis of Mesoamerica during the Classic Period (1 to 600 AC). The city had a continuous growth in different stages that usually concluded with a ritual. Fire was an important element natives would burn entire structures. An example of this is the Quetzalcoatl pyramid in La Ciudadela (350 AC), it was burned and a new structure was built over it, also the Big Fire at 570 AC, that marks its end. These events are suitable to archaeomagnetic dating. The inclusion of ash in the stucco enhances the magnetic signal of detrital type that also allows us to make dating. This increases the number of samples to be processed as well as the number of dates. The samples have been analyzed according to their type: floor, wall, talud and painting and whether or not exposed to fire. Sequences of directions obtained in excavations in strict stratigraphic control will be shown. A sequence of images was used to analyze the improving of Teotihuacan secular variation curve through more than a decade of continuous work at the area.

  6. UMTRA project water sampling and analysis plan, Riverton, Wyoming

    SciTech Connect

    Not Available

    1994-03-01

    Surface remediation was completed at the former uranium mill site in Riverton, Wyoming, in 1990. Residual radioactive materials (contaminated soil and debris) were removed and disposed of at Union Carbide Corporation`s (Umetco) nearby Gas Hills Title 2 facility. Ground water in the surficial and semiconfined aquifers (known collectively as the `uppermost aquifer`) below the former mill and tailings site has been contaminated. No contamination has been detected in the deeper, confined sandstone aquifer. The contaminant plume extends off site to the south and east. The plume is constrained by surface wetlands and small streams to the east and west of the site and by the Little Wind River to the south. Fifteen monitor wells installed in 1993 were sampled to better define the contaminant plume and to provide additional water quality data for the baseline risk assessment. Samples also were collected from domestic wells in response to a request by the Wyoming Department of Environmental Quality in January 1994. No contamination attributable to the former uranium milling operations have ever been detected in any of the domestic wells used for potable supplies.

  7. Quality assurance guidance for field sampling and measurement assessment plates in support of EM environmental sampling and analysis activities

    SciTech Connect

    Not Available

    1994-05-01

    This document is one of several guidance documents developed by the US Department of Energy (DOE) Office of Environmental Restoration and Waste Management (EM). These documents support the EM Analytical Services Program (ASP) and are based on applicable regulatory requirements and DOE Orders. They address requirements in DOE Orders by providing guidance that pertains specifically to environmental restoration and waste management sampling and analysis activities. DOE 5700.6C Quality Assurance (QA) defines policy and requirements to establish QA programs ensuring that risks and environmental impacts are minimized and that safety, reliability, and performance are maximized. This is accomplished through the application of effective management systems commensurate with the risks imposed by the facility and the project. Every organization supporting EM`s environmental sampling and analysis activities must develop and document a QA program. Management of each organization is responsible for appropriate QA program implementation, assessment, and improvement. The collection of credible and cost-effective environmental data is critical to the long-term success of remedial and waste management actions performed at DOE facilities. Only well established and management supported assessment programs within each EM-support organization will enable DOE to demonstrate data quality. The purpose of this series of documents is to offer specific guidance for establishing an effective assessment program for EM`s environmental sampling and analysis (ESA) activities.

  8. A modular approach for automated sample preparation and chemical analysis

    NASA Technical Reports Server (NTRS)

    Clark, Michael L.; Turner, Terry D.; Klingler, Kerry M.; Pacetti, Randolph

    1994-01-01

    Changes in international relations, especially within the past several years, have dramatically affected the programmatic thrusts of the U.S. Department of Energy (DOE). The DOE now is addressing the environmental cleanup required as a result of 50 years of nuclear arms research and production. One major obstacle in the remediation of these areas is the chemical determination of potentially contaminated material using currently acceptable practices. Process bottlenecks and exposure to hazardous conditions pose problems for the DOE. One proposed solution is the application of modular automated chemistry using Standard Laboratory Modules (SLM) to perform Standard Analysis Methods (SAM). The Contaminant Analysis Automation (CAA) Program has developed standards and prototype equipment that will accelerate the development of modular chemistry technology and is transferring this technology to private industry.

  9. Real-time quadrupole mass spectrometer analysis of gas in boreholefluid samples acquired using the U-Tube sampling methodology

    SciTech Connect

    Freifeld, Barry M.; Trautz, Robert C.

    2006-01-11

    Sampling of fluids in deep boreholes is challenging becauseof the necessity to minimize external contamination and maintain sampleintegrity during recovery. The U-tube sampling methodology was developedto collect large volume, multiphase samples at in situ pressures. As apermanent or semi-permanent installation, the U-tube can be used forrapidly acquiring multiple samples or it may be installed for long-termmonitoring applications. The U-tube was first deployed in Liberty County,TX to monitor crosswell CO2 injection as part of the Frio CO2sequestration experiment. Analysis of gases (dissolved or separate phase)was performed in the field using a quadrupole mass spectrometer, whichserved as the basis for determining the arrival of the CO2 plume. Thepresence of oxygen and argon in elevated concentrations, along withreduced methane concentration, indicate sample alteration caused by theintroduction of surface fluids during borehole completion. Despiteproducing the well to eliminate non-native fluids, measurementsdemonstrate that contamination persists until the immiscible CO2injection swept formation fluid into the observationwellbore.

  10. Comparative analysis of toxin detection in biological and enviromental samples

    NASA Astrophysics Data System (ADS)

    Ogert, Robert A.; Burans, James; O'Brien, Tom; Ligler, Frances S.

    1994-03-01

    The basic recognition schemes underlying the principles of standard enzyme-linked immunosorbent assay (ELISA) and radioimmunoassay (RIA) protocols are increasingly being adapted for use with new detection devices. A direct comparison was made using a fiber optic biosensor that employs evanescent wave detection and an ELISA using avidin-biotin. The assays were developed for the detection of Ricinus communis agglutinin II, also known as ricin or RCA60. Detection limits between the two methods were comparable for ricin in phosphate buffered saline (PBS), however results in complex samples differed slightly. In PBS, sensitivity for ricin was 1 ng/ml using the fiber optic device and 500 pg/ml using the ELISA. The fiber optic sensor could not detect ricin directly in urine or serum spiked with 5 ng/ml ricin, however, the ELISA showed detection but at reduced levels to the PBS control.

  11. Accelerated rare event sampling: Refinement and Ising model analysis

    NASA Astrophysics Data System (ADS)

    Yevick, David; Lee, Yong Hwan

    In this paper, a recently introduced accelerated sampling technique [D. Yevick, Int. J. Mod. Phys. C 27, 1650041 (2016)] for constructing transition matrices is further developed and applied to a two-dimensional 32×32 Ising spin system. By permitting backward displacements up to a certain limit for each forward step while evolving the system to first higher and then lower energies within a restricted interval that is steadily displaced toward zero temperature as the computation proceeds, accuracy can be greatly enhanced. Simultaneously, the elements obtained from numerous independent calculations are collected in a single transition matrix. The relative accuracy of this novel method is established through a comparison to a transition matrix procedure based on the Metropolis algorithm in which the temperature is appropriately varied during the calculation and the results interpreted in terms of the distribution of realizations over both energy and magnetization.

  12. Isotopic analysis of eggs: evaluating sample collection and preparation.

    PubMed

    Rock, Luc; Rowe, Sylwia; Czerwiec, Agnieszka; Richmond, Harold

    2013-02-15

    Egg traceability/authenticity is a worldwide concern. Stable isotope techniques have been suggested as a tool to address this issue. To further validate the use of these techniques, a research project was undertaken to evaluate what effect sample collection and preparation have on the measured isotopic composition of egg components. The timing of egg collection, the timing of egg preparation after collection, and the use of pasteurisation were investigated. The C, N, O, and S isotopic compositions of egg components from 7 different production systems were measured. Two sets of eggs were collected (4 months apart). It was found that the 'isotopic fingerprint' of a particular production system was maintained over time, and that it may be possible to trace liquid egg products based on isotopic data from fresh eggs. The findings from this study support the integration of stable isotope techniques in egg traceability/authenticity systems.

  13. Improving Sampling, Analysis, and Data Management for Site Investigation and Cleanup

    EPA Pesticide Factsheets

    The United States Environmental Protection Agency (EPA) supports the adoption of streamlined approaches to sampling, analysis, and data management activities conducted during site assessment, characterization, and cleanup.

  14. Survey of sampling-based methods for uncertainty and sensitivity analysis.

    SciTech Connect

    Johnson, Jay Dean; Helton, Jon Craig; Sallaberry, Cedric J. PhD.; Storlie, Curt B. (Colorado State University, Fort Collins, CO)

    2006-06-01

    Sampling-based methods for uncertainty and sensitivity analysis are reviewed. The following topics are considered: (1) Definition of probability distributions to characterize epistemic uncertainty in analysis inputs, (2) Generation of samples from uncertain analysis inputs, (3) Propagation of sampled inputs through an analysis, (4) Presentation of uncertainty analysis results, and (5) Determination of sensitivity analysis results. Special attention is given to the determination of sensitivity analysis results, with brief descriptions and illustrations given for the following procedures/techniques: examination of scatterplots, correlation analysis, regression analysis, partial correlation analysis, rank transformations, statistical tests for patterns based on gridding, entropy tests for patterns based on gridding, nonparametric regression analysis, squared rank differences/rank correlation coefficient test, two dimensional Kolmogorov-Smirnov test, tests for patterns based on distance measures, top down coefficient of concordance, and variance decomposition.

  15. Spectral analysis for automated exploration and sample acquisition

    NASA Astrophysics Data System (ADS)

    Eberlein, Susan; Yates, Gigi

    1992-05-01

    Future space exploration missions will rely heavily on the use of complex instrument data for determining the geologic, chemical, and elemental character of planetary surfaces. One important instrument is the imaging spectrometer, which collects complete images in multiple discrete wavelengths in the visible and infrared regions of the spectrum. Extensive computational effort is required to extract information from such high-dimensional data. A hierarchical classification scheme allows multispectral data to be analyzed for purposes of mineral classification while limiting the overall computational requirements. The hierarchical classifier exploits the tunability of a new type of imaging spectrometer which is based on an acousto-optic tunable filter. This spectrometer collects a complete image in each wavelength passband without spatial scanning. It may be programmed to scan through a range of wavelengths or to collect only specific bands for data analysis. Spectral classification activities employ artificial neural networks, trained to recognize a number of mineral classes. Analysis of the trained networks has proven useful in determining which subsets of spectral bands should be employed at each step of the hierarchical classifier. The network classifiers are capable of recognizing all mineral types which were included in the training set. In addition, the major components of many mineral mixtures can also be recognized. This capability may prove useful for a system designed to evaluate data in a strange environment where details of the mineral composition are not known in advance.

  16. Spectral analysis for automated exploration and sample acquisition

    NASA Technical Reports Server (NTRS)

    Eberlein, Susan; Yates, Gigi

    1992-01-01

    Future space exploration missions will rely heavily on the use of complex instrument data for determining the geologic, chemical, and elemental character of planetary surfaces. One important instrument is the imaging spectrometer, which collects complete images in multiple discrete wavelengths in the visible and infrared regions of the spectrum. Extensive computational effort is required to extract information from such high-dimensional data. A hierarchical classification scheme allows multispectral data to be analyzed for purposes of mineral classification while limiting the overall computational requirements. The hierarchical classifier exploits the tunability of a new type of imaging spectrometer which is based on an acousto-optic tunable filter. This spectrometer collects a complete image in each wavelength passband without spatial scanning. It may be programmed to scan through a range of wavelengths or to collect only specific bands for data analysis. Spectral classification activities employ artificial neural networks, trained to recognize a number of mineral classes. Analysis of the trained networks has proven useful in determining which subsets of spectral bands should be employed at each step of the hierarchical classifier. The network classifiers are capable of recognizing all mineral types which were included in the training set. In addition, the major components of many mineral mixtures can also be recognized. This capability may prove useful for a system designed to evaluate data in a strange environment where details of the mineral composition are not known in advance.

  17. Collection and analysis of NASA clean room air samples

    NASA Technical Reports Server (NTRS)

    Sheldon, L. S.; Keever, J.

    1985-01-01

    The environment of the HALOE assembly clean room at NASA Langley Research Center is analyzed to determine the background levels of airborne organic compounds. Sampling is accomplished by pumping the clean room air through absorbing cartridges. For volatile organics, cartridges are thermally desorbed and then analyzed by gas chromatography and mass spectrometry, compounds are identified by searching the EPA/NIH data base using an interactive operator INCOS computer search algorithm. For semivolatile organics, cartridges are solvent entracted and concentrated extracts are analyzed by gas chromatography-electron capture detection, compound identification is made by matching gas chromatogram retention times with known standards. The detection limits for the semivolatile organics are; 0.89 ng cu m for dioctylphlhalate (DOP) and 1.6 ng cu m for polychlorinated biphenyls (PCB). The detection limit for volatile organics ranges from 1 to 50 parts per trillion. Only trace quantities of organics are detected, the DOP levels do not exceed 2.5 ng cu m and the PCB levels do not exceed 454 ng cu m.

  18. Analysis of Direct Samples of Early Solar System Aqueous Fluids

    NASA Technical Reports Server (NTRS)

    Zolensky, Michael E.; Bodnar, R J.; Fedele, L.; Yurimoto,H.; Itoh, S.; Fries, M.; Steele, A.

    2012-01-01

    Over the past three decades we have become increasingly aware of the fundamental importance of water, and aqueous alteration, on primitive solar-system bodies. Some carbonaceous and ordinary chondrites have been altered by interactions with liquid water within the first 10 million years after formation of their parent asteroids. Millimeter to centimeter-sized aggregates of purple halite containing aqueous fluid inclusions were found in the matrix of two freshly-fallen brecciated H chondrite falls, Monahans (1998, hereafter simply "Monahans") (H5) and Zag (H3-6) (Zolensky et al., 1999; Whitby et al., 2000; Bogard et al., 2001) In order to understand origin and evolution of the aqueous fluids inside these inclusions we much measure the actual fluid composition, and also learn the O and H isotopic composition of the water. It has taken a decade for laboratory analytical techniques to catch up to these particular nanomole-sized aqueous samples. We have recently been successful in (1) measuring the isotopic composition of H and O in the water in a few fluid inclusions from the Zag and Monahans halite, (2) mineralogical characterization of the solid mineral phases associated with the aqueous fluids within the halite, and (3) the first minor element analyses of the fluid itself. A Cameca ims-1270 equipped with a cryo-sample-stage of Hokkaido University was specially prepared for the O and H isotopic measurements. The cryo-sample-stage (Techno. I. S. Corp.) was cooled down to c.a. -190 C using liquid nitrogen at which the aqueous fluid in inclusions was frozen. We excavated the salt crystal surfaces to expose the frozen fluids using a 15 keV Cs+ beam and measured negative secondary ions. The secondary ions from deep craters of approximately 10 m in depth emitted stably but the intensities changed gradually during measurement cycles because of shifting states of charge compensation, resulting in rather poor reproducibility of multiple measurements of standard fluid

  19. Isolation and analysis of vitamin B12 from plant samples.

    PubMed

    Nakos, M; Pepelanova, I; Beutel, S; Krings, U; Berger, R G; Scheper, T

    2017-02-01

    Based on increased demands of strict vegetarians, an investigation of vitamin B12 content in plant sources, was carried out. The vitamin B12 concentration was determined by RP-HPLC with UV detection, after prior matrix isolation by immunoaffinity chromatography (IAC). Vitamin B12 was extracted in the presence of sodium cyanide, to transform all forms of cobalamin into cyanocobalamin. Diode array detector was used to monitor vitamin B12, after its chromatographic separation under gradient elution with a mobile phase consisting of acetonitrile and trifluoroacetic acid 0.025% (w/v). The method demonstrated excellent linearity with a limit of detection 0.004μg/ml. The method precision was evaluated for plant samples and it was below 0.7% (n=6). Significant amounts of vitamin B12 in plants were detected in Hippophae rhamnoides (37μg/100g dry weight), in Elymus (26μg/100g dry weight) and in Inula helenium (11μg/100g dry weight).

  20. Chain of custody; recommendations for acceptance and analysis of evidentiary geochemical samples

    USGS Publications Warehouse

    Murphy, Christine M.; Briggs, Paul H.; Adrian, Betty M.; Wilson, Steve A.; Hageman, Phil L.; Theodorakos, Pete M.

    1997-01-01

    Personnel from the Analytical Chemistry Services Group (ACSG), Mineral Resource Survey Program, formed a team to determine the policies for acceptance and analysis of geochemical samples. This team contacted law enforcement agencies that handle litigious samples, laboratories that work with samples of special nature, and the Solicitor General, Department of the Interior. Using the knowledge from these agencies as well as the expertise of ACSG personnel, sample control routine procedures, sample control evidentiary procedures, personnel policy governing chain-of-custody samples, and the general polices governing physical security of chain-of custody samples have been enacted.

  1. FAMeS: Fidelity of Analysis of Metagenomic Samples

    DOE Data Explorer

    Metagenomics is a rapidly emerging field of research for studying microbial communities. To evaluate methods currently used to process metagenomic sequences, simulated datasets of varying complexity were constructed by combining sequencing reads randomly selected from 113 isolate genomes. These datasets were designed to model real metagenomes in terms of complexity and phylogenetic composition. Assembly, gene prediction and binning, employing methods commonly used for the analysis of metagenomic datasets at the DOE JGI, were performed. This site provides access to the simulated datasets, and aims to facilitate standardized benchmarking of tools for metagenomic analysis. FAMeS now hosts data coming from a comprehensive study of methodologies used to create OTUs from 16S rRNA targeted studies of microbial communities. Studies of phylogenetic markers at the molecular level have revealed a vast biodiversity of microorganisms living in the sea, land, and even within the human body. Microbial diversity studies of uncharacterized environments typically seek to estimate the richness and diversity of endemic microflora using a 16S rRNA gene sequencing approach. When most of the species in an environment are unknown and cannot be classified through a database search, researchers cluster 16S sequences into operational taxonomic units (OTUs) or phylotypes, thereby providing an estimate of population structure. Using real 16S sequence data, we have performed a critical analysis of OTU clustering methodologies to assess the potential variability in OTU quality. FAMeS provides the sequence data, taxonomic information, multiple sequence alignments, and distance matrices used and described in the core paper, as well as compiled results of more than 700 unique OTU methods. [The above was copied from the FAMeS home page at http://fames.jgi-psf.org/] The core paper behind FAMeS is: Konstantinos Mavromatis, Natalia Ivanova, Kerrie Barry, Harris Shapiro, Eugene Goltsman, Alice C Mc

  2. Accelerated Gibbs Sampling for Infinite Sparse Factor Analysis

    SciTech Connect

    Andrzejewski, D M

    2011-09-12

    The Indian Buffet Process (IBP) gives a probabilistic model of sparse binary matrices with an unbounded number of columns. This construct can be used, for example, to model a fixed numer of observed data points (rows) associated with an unknown number of latent features (columns). Markov Chain Monte Carlo (MCMC) methods are often used for IBP inference, and in this technical note, we provide a detailed review of the derivations of collapsed and accelerated Gibbs samplers for the linear-Gaussian infinite latent feature model. We also discuss and explain update equations for hyperparameter resampling in a 'full Bayesian' treatment and present a novel slice sampler capable of extending the accelerated Gibbs sampler to the case of infinite sparse factor analysis by allowing the use of real-valued latent features.

  3. Quantitative phase analysis of challenging samples using neutron powder diffraction. Sample #4 from the CPD QPA round robin revisited

    DOE PAGES

    Whitfield, Pamela S.

    2016-04-29

    Here, quantitative phase analysis (QPA) using neutron powder diffraction more often than not involves non-ambient studies where no sample preparation is possible. The larger samples and penetration of neutrons versus X-rays makes neutron diffraction less susceptible to inhomogeneity and large grain sizes, but most well-characterized QPA standard samples do not have these characteristics. Sample #4 from the International Union of Crystallography Commission on Powder Diffraction QPA round robin was one such sample. Data were collected using the POWGEN time-of-flight (TOF) neutron powder diffractometer and analysed together with historical data from the C2 diffractometer at Chalk River. The presence of magneticmore » reflections from Fe3O4 (magnetite) in the sample was an additional consideration, and given the frequency at which iron-containing and other magnetic compounds are present during in-operando studies their possible impact on the accuracy of QPA is of interest. Additionally, scattering from thermal diffuse scattering in the high-Qregion (<0.6 Å) accessible with TOF data could impact QPA results during least-squares because of the extreme peak overlaps present in this region. Refinement of POWGEN data was largely insensitive to the modification of longer d-spacing reflections by magnetic contributions, but the constant-wavelength data were adversely impacted if the magnetic structure was not included. A robust refinement weighting was found to be effective in reducing quantification errors using the constant-wavelength neutron data both where intensities from magnetic reflections were ignored and included. Results from the TOF data were very sensitive to inadequate modelling of the high-Q (lowd-spacing) background using simple polynomials.« less

  4. Quantitative phase analysis of challenging samples using neutron powder diffraction. Sample #4 from the CPD QPA round robin revisited

    SciTech Connect

    Whitfield, Pamela S.

    2016-04-29

    Here, quantitative phase analysis (QPA) using neutron powder diffraction more often than not involves non-ambient studies where no sample preparation is possible. The larger samples and penetration of neutrons versus X-rays makes neutron diffraction less susceptible to inhomogeneity and large grain sizes, but most well-characterized QPA standard samples do not have these characteristics. Sample #4 from the International Union of Crystallography Commission on Powder Diffraction QPA round robin was one such sample. Data were collected using the POWGEN time-of-flight (TOF) neutron powder diffractometer and analysed together with historical data from the C2 diffractometer at Chalk River. The presence of magnetic reflections from Fe3O4 (magnetite) in the sample was an additional consideration, and given the frequency at which iron-containing and other magnetic compounds are present during in-operando studies their possible impact on the accuracy of QPA is of interest. Additionally, scattering from thermal diffuse scattering in the high-Qregion (<0.6 Å) accessible with TOF data could impact QPA results during least-squares because of the extreme peak overlaps present in this region. Refinement of POWGEN data was largely insensitive to the modification of longer d-spacing reflections by magnetic contributions, but the constant-wavelength data were adversely impacted if the magnetic structure was not included. A robust refinement weighting was found to be effective in reducing quantification errors using the constant-wavelength neutron data both where intensities from magnetic reflections were ignored and included. Results from the TOF data were very sensitive to inadequate modelling of the high-Q (lowd-spacing) background using simple polynomials.

  5. Analysis of environmental soil samples for aromatic amines

    SciTech Connect

    Pace, C.M.; Donnelly, J.R.; Brumley, W.C.; Sovocool, G.W.

    1995-12-31

    To support a goal of the USEPA Characterization Research Division in Las Vegas, a rapid HPLC/UV of fluorescence method was developed for ppb levels of aromatic amines in soils. Existing methods were either designed for water, or gave poor and variable recoveries in soils. Both fast, reversible reactions and slow, irreversible reactions of these amines are reported to occur with the humic materials in the soil. The method involved sonication of 2 g soil with 1% NH4 OH/CH{sub 3}CN for 2 hours, centrifuging 30 min, adding 3 mL extract to 7 mL 0.01 M NH{sub 4}OAc, filtering, transferring through an acrodisc for HPLC analysis with gradient elution from 70% 0.01M NH{sub 4}OAc, 30% CH{sub 3}CN to 100% CH{sub 3}CN over 17 min; hold 3.5 min. The analytical method provided reproducible recoveries from both sand and humic-containing soils (e.g., 70-99% on {beta}-naphthylamine and 72-96% on 4-nitroaniline, spiked at 1 ppm). The method detection limits ranged from 1 ppb for {beta}-naphthyl-amine to 1 ppm for pyridines. HPLC analysis used ultraviolet, fluorescence and mass spectrometric detectors. Notice: The US Environmental Protection Agency (EPA), through its Office of Research and Development (ORD), partially funded and collaborated in the research described in this abstract for a proposed poster. It does not necessarily reflect the views of the EPA or ORD.

  6. Analysis of RDX and RDX Breakdown Products in Environmental Samples

    SciTech Connect

    Felt, Deborah R.; Larson, Steven L.; Wani, Altaf; Davis, Jeffrey L.

    2003-03-26

    The identification and quantification of explosives and their degradation products in soil and natural waters is helpful in the design of remediation technologies, mobility investigations and performing risk assessments. The objective of this study was to develop a method for the determination of the degradation of nitramine compounds, specifically hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX). The analytical methods developed in this study were based on reversed-phase high performance liquid chromatography (HPLC) using both C-18 and CN bonded silica columns to eliminate common interferences. Contaminant identification was further confirmed by performing spectral analysis of the compounds upon elution. The proposed method yields good separation of RDX from its degradation products and from other common energetic compounds. Method detection limits for the proposed method ranged from 0.01 to 0.03 mg/L. This method satisfies the need for analytical techniques to monitor the formation and subsequent degradation products of toxic and carcinogenic nitrosyl substituted nitramines.

  7. Quantitative analysis of dynamic association in live biological fluorescent samples.

    PubMed

    Ruusuvuori, Pekka; Paavolainen, Lassi; Rutanen, Kalle; Mäki, Anita; Huttunen, Heikki; Marjomäki, Varpu

    2014-01-01

    Determining vesicle localization and association in live microscopy may be challenging due to non-simultaneous imaging of rapidly moving objects with two excitation channels. Besides errors due to movement of objects, imaging may also introduce shifting between the image channels, and traditional colocalization methods cannot handle such situations. Our approach to quantifying the association between tagged proteins is to use an object-based method where the exact match of object locations is not assumed. Point-pattern matching provides a measure of correspondence between two point-sets under various changes between the sets. Thus, it can be used for robust quantitative analysis of vesicle association between image channels. Results for a large set of synthetic images shows that the novel association method based on point-pattern matching demonstrates robust capability to detect association of closely located vesicles in live cell-microscopy where traditional colocalization methods fail to produce results. In addition, the method outperforms compared Iterated Closest Points registration method. Results for fixed and live experimental data shows the association method to perform comparably to traditional methods in colocalization studies for fixed cells and to perform favorably in association studies for live cells.

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

    PubMed

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

    2012-10-07

    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.

  9. Multidimensional System Analysis of Electro-Optic Sensors with Sampled Deterministic Output.

    DTIC Science & Technology

    1987-12-18

    System descriptions of scanning and staring electro - optic sensors with sampled output are developed as follows. Functions representing image...to complete the system descriptions. The results should be useful for designing electro - optic sensor systems and correcting data for instrumental...effects and other experimental conditions. Keywords include: Electro - optic system analysis, Scanning sensors, Staring sensors, Spatial sampling, and Temporal sampling.

  10. Double Shell Tank (DST) Ventilation System Vapor Sampling and Analysis Plan

    SciTech Connect

    SASAKI, L.M.

    2000-06-08

    This sampling and analysis plan (SAP) identifies characterization objectives pertaining to sample collection, laboratory analytical evaluation, and reporting requirements for vapor samples from the primary ventilation systems of the AN, AP, AW, and AY/AZ tank farms. Sampling will be performed in accordance with Data Quality Objectives for Regulatory Requirements for Hazardous and Radioactive Air Emissions Sampling and Analysis (Air DQO) (Mulkey 1999). The sampling will verify if current air emission estimates used in the permit application are correct and provide information for future air permit applications. Vapor samples will be obtained from tank farm ventilation systems, downstream from the tanks and upstream of any filtration. Samples taken in support of the DQO will consist of SUMMA{trademark} canisters, triple sorbent traps (TSTs), sorbent tube trains (STTs), polyurethane foam (PUF) samples. Particulate filter samples and tritium traps will be taken for radiation screening to allow the release of the samples for analysis. The following sections provide the general methodology and procedures to be used in the preparation, retrieval, transport, analysis, and reporting of results from the vapor samples.

  11. A STRINGENT COMPARISON OF SAMPLING AND ANALYSIS METHODS FOR VOCS IN AMBIENT AIR

    EPA Science Inventory

    A carefully designed study was conducted during the summer of 1998 to simultaneously collect samples of ambient air by canisters and compare the analysis results to direct sorbent preconcentration results taken at the time of sample collection. A total of 32 1-h sample sets we...

  12. Development of a novel reaction chamber for ion beam analysis of large samples

    NASA Astrophysics Data System (ADS)

    Kakuee, O. R.; Fathollahi, V.; Agha-Aligol, D.; Farmahini-Farahani, M.; Oliaiy, P.; Lamehi-Rachti, M.

    2008-04-01

    A novel vacuum chamber for ion beam analysis of large-size industrial samples - whose analysis are not feasible in conventional ion beam analysis reaction chambers - has been designed, fabricated and successfully tested. Using the newly developed chamber, both PIXE and RBS analyses could be carried out at the same time and on the same point of the samples. Ion beam analysis using this novel chamber lacks the disadvantages of external beam analysis and benefits the advantages of in-vacuum analysis. This has been achieved by designing a tiny open port in the wall of the reaction chamber to be sealed with a small flat area of sample body where its analysis is of interest. As a case study, two samples of gas turbine blades, a corroded one at highly corrosive environment and a refurbished one after application of certain coatings are analysed using the novel chamber. Experimental results confirm the performance and capability of the reaction chamber.

  13. Large sample neutron activation analysis: a challenge in cultural heritage studies.

    PubMed

    Stamatelatos, Ion E; Tzika, Faidra

    2007-07-01

    Large sample neutron activation analysis compliments and significantly extends the analytical tools available for cultural heritage and authentication studies providing unique applications of non-destructive, multi-element analysis of materials that are too precious to damage for sampling purposes, representative sampling of heterogeneous materials or even analysis of whole objects. In this work, correction factors for neutron self-shielding, gamma-ray attenuation and volume distribution of the activity in large volume samples composed of iron and ceramic material were derived. Moreover, the effect of inhomogeneity on the accuracy of the technique was examined.

  14. Using Language Sample Analysis to Assess Spoken Language Production in Adolescents

    ERIC Educational Resources Information Center

    Miller, Jon F.; Andriacchi, Karen; Nockerts, Ann

    2016-01-01

    Purpose: This tutorial discusses the importance of language sample analysis and how Systematic Analysis of Language Transcripts (SALT) software can be used to simplify the process and effectively assess the spoken language production of adolescents. Method: Over the past 30 years, thousands of language samples have been collected from typical…

  15. 40 CFR 257.23 - Ground-water sampling and analysis requirements.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... and analysis requirements. (a) The ground-water monitoring program must include consistent sampling... 40 Protection of Environment 24 2010-07-01 2010-07-01 false Ground-water sampling and analysis requirements. 257.23 Section 257.23 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED)...

  16. 40 CFR 258.53 - Ground-water sampling and analysis requirements.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ....53 Ground-water sampling and analysis requirements. (a) The ground-water monitoring program must... 40 Protection of Environment 24 2010-07-01 2010-07-01 false Ground-water sampling and analysis requirements. 258.53 Section 258.53 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED)...

  17. Use of Language Sample Analysis by School-Based SLPs: Results of a Nationwide Survey

    ERIC Educational Resources Information Center

    Pavelko, Stacey L.; Owens, Robert E., Jr.; Ireland, Marie; Hahs-Vaughn, Debbie L.

    2016-01-01

    Purpose: This article examines use of language sample analysis (LSA) by school-based speech-language pathologists (SLPs), including characteristics of language samples, methods of transcription and analysis, barriers to LSA use, and factors affecting LSA use, such as American Speech-Language-Hearing Association certification, number of years'…

  18. Preparation and analysis of standardized waste samples for Controlled Ecological Life Support Systems (CELSS)

    NASA Technical Reports Server (NTRS)

    Carden, J. L.; Browner, R.

    1982-01-01

    The preparation and analysis of standardized waste samples for controlled ecological life support systems (CELSS) are considered. Analysis of samples from wet oxidation experiments, the development of ion chromatographic techniques utilizing conventional high pressure liquid chromatography (HPLC) equipment, and an investigation of techniques for interfacing an ion chromatograph (IC) with an inductively coupled plasma optical emission spectrometer (ICPOES) are discussed.

  19. Granger causality analysis with nonuniform sampling and its application to pulse-coupled nonlinear dynamics.

    PubMed

    Zhang, Yaoyu; Xiao, Yanyang; Zhou, Douglas; Cai, David

    2016-04-01

    The Granger causality (GC) analysis is an effective approach to infer causal relations for time series. However, for data obtained by uniform sampling (i.e., with an equal sampling time interval), it is known that GC can yield unreliable causal inference due to aliasing if the sampling rate is not sufficiently high. To solve this unreliability issue, we consider the nonuniform sampling scheme as it can mitigate against aliasing. By developing an unbiased estimation of power spectral density of nonuniformly sampled time series, we establish a framework of spectrum-based nonparametric GC analysis. Applying this framework to a general class of pulse-coupled nonlinear networks and utilizing some particular spectral structure possessed by these nonlinear network data, we demonstrate that, for such nonlinear networks with nonuniformly sampled data, reliable GC inference can be achieved at a low nonuniform mean sampling rate at which the traditional uniform sampling GC may lead to spurious causal inference.

  20. Granger causality analysis with nonuniform sampling and its application to pulse-coupled nonlinear dynamics

    NASA Astrophysics Data System (ADS)

    Zhang, Yaoyu; Xiao, Yanyang; Zhou, Douglas; Cai, David

    2016-04-01

    The Granger causality (GC) analysis is an effective approach to infer causal relations for time series. However, for data obtained by uniform sampling (i.e., with an equal sampling time interval), it is known that GC can yield unreliable causal inference due to aliasing if the sampling rate is not sufficiently high. To solve this unreliability issue, we consider the nonuniform sampling scheme as it can mitigate against aliasing. By developing an unbiased estimation of power spectral density of nonuniformly sampled time series, we establish a framework of spectrum-based nonparametric GC analysis. Applying this framework to a general class of pulse-coupled nonlinear networks and utilizing some particular spectral structure possessed by these nonlinear network data, we demonstrate that, for such nonlinear networks with nonuniformly sampled data, reliable GC inference can be achieved at a low nonuniform mean sampling rate at which the traditional uniform sampling GC may lead to spurious causal inference.

  1. Enabling Continental-Scale Analysis of Vegetation Foliar Traits through Consistent Sampling and Analysis Protocols

    NASA Astrophysics Data System (ADS)

    Petroy, S. B.; Leisso, N.; Hinckley, E. S.; Meier, C. L.; Barnett, D.

    2013-12-01

    The National Ecological Observatory Network (NEON) is a continental-scale ecological observation platform designed to collect and disseminate data that contributes to understanding and forecasting the impacts of climate change, land use change, and invasive species on ecology. NEON will collect in-situ and airborne data over 60 sites across the US, including Alaska, Hawaii, and Puerto Rico. The NEON vegetation sampling protocol currently directs the collection of foliar samples from dominant species at each site; field spectra are collected from the samples that are further analyzed for bulk and isotopic carbon and nitrogen content. Through employment of consistent sampling and analysis strategies, NEON will provide a unique, rich, and varied data collection to support studies of foliar traits within species at specific sites and across/between regions. When combined with the NEON airborne hyperspectral and LiDAR imagery, these data will be key to support validation efforts of existing algorithms for deriving canopy scale nitrogen, carbon and other foliar traits, as well as supporting development of data products that are informed by - and include - the ground data specifically, thereby potentially reducing uncertainties in the observational data products. Presented here are prototype datasets collected at NEON Domain 1 (Harvard Forest, summer 2012) and Domain 17 (San Joaquin Experiment Range, summer 2013). Lessons-learned from the field campaigns are discussed, along with preliminary results from the Harvard Forest campaign, which combine the field and the laboratory data in support of current algorithm validation efforts. Extension of these protocols to future NEON Domain characterization activities is also presented.

  2. Automated transmission line fault analysis using synchronized sampling at two ends

    SciTech Connect

    Kezunovic, M.; Perunicic, B.

    1996-02-01

    This paper introduces a new approach to fault analysis using synchronized sampling. A digital fault recorder with Global Positioning System (GPS) satellite receiver is the source of data for this approach. Fault analysis functions, such as fault detection, classification and location are implemented for a transmission line using synchronized samples from two ends of a line. This technique can be extremely fast, selective and accurate, providing fault analysis performance that can not easily be matched by other known techniques.

  3. Automated transmission line fault analysis using synchronized sampling at two ends

    SciTech Connect

    Kezunovic, M.; Perunicic, B.

    1995-12-31

    This paper introduces a new approach to fault analysis using synchronized sampling. A digital fault recorder with Global Positioning System (GPS) satellite receiver is the source of data for this approach. Fault analysis functions, such as fault detection, classification and location are implemented for a transmission line using synchronized samples from two ends of a line. This technique can be extremely fast, selective and accurate, providing fault analysis performance that can not easily be matched by other known techniques.

  4. Qualitative and quantitative analysis of environmental samples by laser-induced breakdown spectrometry

    NASA Astrophysics Data System (ADS)

    Zorov, N. B.; Popov, A. M.; Zaytsev, S. M.; Labutin, T. A.

    2015-10-01

    The key achievements in the determination of trace amounts of components in environmental samples (soils, ores, natural waters, etc.) by laser-induced breakdown spectrometry are considered. Unique capabilities of this method make it suitable for rapid analysis of metals and alloys, glasses, polymers, objects of cultural heritage, archaeological and various environmental samples. The key advantages of the method that account for its high efficiency are demonstrated, in particular, a small amount of analyzed material, the absence of sample preparation, the possibility of local and remote analysis of either one or several elements. The use of chemometrics in laser-induced breakdown spectrometry for qualitative sample classification is described in detail. Various approaches to improving the figures of merit of quantitative analysis of environmental samples are discussed. The achieved limits of detection for most elements in geochemical samples are critically evaluated. The bibliography includes 302 references.

  5. A stringent comparison of sampling and analysis methods for VOCs in ambient air

    SciTech Connect

    Daughtrey, E.H. Jr.; Oliver, K.D.; Adams, J.R.; Kronmiller, K.G.; Lonneman, W.A.; McClenny, W.A.; Colon, M.

    1999-07-01

    A carefully designed study was conducted during the summer of 1998 to simultaneously collect samples of ambient air by canisters and compare the analysis results to direct sorbent preconcentration results taken at the time of sample collection. A total of 32 1-h sample sets were taken, each composed of a real-time sample analyzed by an autoGC/MS XonTech 930/Varian Saturn 2000 system, and SUMMA and Silco canisters. Hourly total non-methane organic carbon (TNMOC), ozone, and meteorological measurements were also made. Each of the canisters was analyzed on the autoGC/MS system for a target list of 108 VOCs and on a manual cryosampling GC/FID system. Comparisons are made between the collection and analysis methods. Because of the low sample loading (150--250 ppbC TNMOC), these comparisons are a stringent test of sample collection and analysis capabilities.

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

    PubMed

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

    2014-12-01

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

  7. Adsorptive Films in Support of In-field UF6 Destructive Assay Sample Collection and Analysis

    SciTech Connect

    Barrett, Christopher A.; Martinez, Alonzo; McNamara, Bruce K.; Cannon, Bret D.; Anheier, Norman C.

    2014-07-20

    International Atom Energy Agency (IAEA) safeguard verification measures in gaseous centrifuge enrichment plants (GCEPs) rely on environmental sampling, non-destructive assay (NDA), and destructive assay (DA) sampling and analysis to determine uranium enrichment. UF6 bias defect measurements are made by DA sampling and analysis to assure that enrichment is consistent with declarations. DA samples are collected from a limited number of cylinders for high precision, offsite mass spectrometer analysis. Samples are typically drawn from a sampling tap into a UF6 sample bottle, then packaged, sealed, and shipped under IAEA chain of custody to an offsite analytical laboratory. Future DA safeguard measures may require improvements in efficiency and effectiveness as GCEP capacities increase and UF6 shipping regulations become increasingly more restrictive. The Pacific Northwest National Laboratory (PNNL) DA sampler concept and Laser Ablation Absorption Ratio Spectrometry (LAARS) assay method are under development to potentially provide DA safeguard tools that increase inspection effectiveness and reduce sample shipping constraints. The PNNL DA sampler concept uses a handheld sampler to collect DA samples for either onsite LAARS assay or offsite laboratory analysis. The DA sampler design will use a small sampling planchet that is coated with an adsorptive film to collect controlled quantities of UF6 gas directly from a cylinder or process sampling tap. Development efforts are currently underway at PNNL to enhance LAARS assay performance to allow high-precision onsite bias defect measurements. In this paper, we report on the experimental investigation to develop adsorptive films for the PNNL DA sampler concept. These films are intended to efficiently capture UF6 and then stabilize the collected DA sample prior to onsite LAARS or offsite laboratory analysis. Several porous material composite films were investigated, including a film designed to maximize the chemical adsorption

  8. Instrumental nuclear activation analysis (INAA) characterization of environmental air filter samples.

    PubMed

    Alemón, Ernesto; Herrera, Luis; Ortiz, Elba; Longoria, L C Luis C

    2004-06-01

    Nuclear techniques have been used in quantitations of environmental pollutants, and instrumental neutron activation analysis (INAA) has turned out to be particularly useful in the analysis of airborne suspended particles. This work describes the INAA characterization of the particulate material in the environmental samples obtained in a monitoring campaign in Mexico City's Metropolitan Area. As the types of the irradiation facilities and gamma-ray detection system impose some limitations on the possibilities of INAA analysis, the actual experimental conditions at Gamma Spectroscopy Laboratory, where the analysis was performed, had been assessed. The facilities had been found suitable for the analysis of samples from this campaign, in which 22 elements were determined.

  9. Use of Rutherford forward scattering for the elemental analysis of evaporated liquid samples

    SciTech Connect

    Liendo, J. A.; Gonzalez, A. C.; Fletcher, N. R.; Caussyn, D. D.; Myers, S. H.; Gomez, J.; Castelli, C.; Sajo-Bohus, L.

    1999-06-10

    Multielemental analysis of evaporated liquid samples is possible by irradiating the samples with a 16 MeV {sup 7}Li beam and detecting the elastically scattered ions at 28 degree sign . The method is easily applied when Rutherford scattering dominates. To prepare the targets, the liquid sample is deposited on a formvar backing and dried with vacuum. Preliminary results indicate a possible relationship between sample concentration, uniformity and spectrum energy resolution. Details on the spectrum analysis will be given. The method is mainly useful for multielemental quantification in the low mass region from lithium to fluorine where standard techniques such as PIXE and TXRF are useless.

  10. Potentiometric stripping analysis (PSA) for monitoring of antimony in samples of vegetation from a mining area.

    PubMed

    Toro Gordillo, M C; Pinilla Gil, E; Rodríguez González, M A; Murciego Murciego, A; Ostapczuk, P

    2001-06-01

    A potentiometric stripping analysis (PSA) method has been developed and checked for the fast and reliable determination of antimony in vegetation samples of Cistus ladanifer from a mining area in Badajoz, Southwest Spain. The method, modified from previous PSA methods for Sb in environmental samples, is based on dry ashing of the homogenized leaves, dissolution in hydrochloric acid, and PSA analysis on a mercury film plated on to a glassy carbon disk electrode. The influence of experimental variables such as the deposition potential, the deposition time, the signal stability and the calibration parameters, has been investigated. The method has been compared with an independent technique (instrumental neutron activation analysis) by analysis of standards and reference materials and comparison of the results. As a result of automation of the PSA equipment, the proposed method enables unattended analysis of 20 digested samples in a total time of 2 h, thus providing a useful tool for Sb monitoring of a large number of samples.

  11. An Evaluation of the Effects of Variable Sampling on Component, Image, and Factor Analysis.

    ERIC Educational Resources Information Center

    Velicer, Wayne F.; Fava, Joseph L.

    1987-01-01

    Principal component analysis, image component analysis, and maximum likelihood factor analysis were compared to assess the effects of variable sampling. Results with respect to degree of saturation and average number of variables per factor were clear and dramatic. Differential effects on boundary cases and nonconvergence problems were also found.…

  12. Detection and Quantification of Nitrogen Compounds in Martian Solid Samples by the Sample Analysis at Mars (SAM) Instrument Suite

    NASA Technical Reports Server (NTRS)

    Stern, Jennifer C.; Navarro-Gonzalez, Rafael; Freissinet, Caroline; McKay, Christopher P.; Archer, Paul Douglas; Buch, Arnaud; Eigenbrode, Jennifer L.; Franz, Heather; Glavin, Daniel Patrick; Ming, Douglas W/; Steele, Andrew; Szopa, Cyril; Wray, James J.; Conrad, Pamela Gales; Mahaffay, Paul R.

    2013-01-01

    The Sample Analysis at Mars (SAM) instrument suite on the Mars Science Laboratory (MSL) Curiosity Rover detected both reduced and oxidized nitrogen-bearing compounds during the pyrolysis of surface materials from three sites at Gale Crater. Preliminary detections of nitrogen species include NO, HCN, ClCN, CH3CN, and TFMA (trifluoro-Nmethyl-acetamide). On Earth, nitrogen is a crucial bio-element, and nitrogen availability controls productivity in many environments. Nitrogen has also recently been detected in the form of CN in inclusions in the Martian meteorite Tissint, and isotopically heavy nitrogen (delta N-15 approx +100per mille) has been measured during stepped combustion experiments in several SNC meteorites. The detection of nitrogen-bearing compounds in Martian regolith would have important implications for the habitability of ancient Mars. However, confirmation of indigenous Martian nitrogen bearing compounds will require ruling out their formation from the terrestrial derivatization reagents (e.g. N-methyl-N-tert-butyldimethylsilyl-trifluoroacetamide, MTBSTFA and dimethylformamide, DMF) carried for SAM's wet chemistry experiment that contribute to the SAM background. The nitrogen species we detect in the SAM solid sample analyses can also be produced during laboratory pyrolysis experiments where these reagents are heated in the presence of perchlorate, a compound that has also been identified by SAM in Mars solid samples. However, this does not preclude a Martian origin for some of these compounds, which are present in nanomolar concentrations in SAM evolved gas analyses. Analysis of SAM data and laboratory breadboard tests are underway to determine whether nitrogen species are present at higher concentrations than can be accounted for by maximum estimates of nitrogen contribution from MTBSTFA and DMF. In addition, methods are currently being developed to use GC Column 6, (functionally similar to a commercial Q-Bond column), to separate and identify

  13. Analysis of volatile organic compounds in groundwater samples by gas chromatography-mass spectrometry

    SciTech Connect

    Bernhardt, J.

    1995-08-23

    The Savannah River Site contains approximately 1500 monitoring wells from which groundwater samples are collected. Many of these samples are sent off-site for various analyses, including the determination of trace volatile organic compounds (VOCs). This report describes accomplishments that have been made during the past year which will ultimately allow VOC analysis to be performed on-site using gas chromatography-mass spectrometry. Through the use of the on-site approach, it is expected that there will be a substantial cost savings. This approach will also provide split-sample analysis capability which can serve as a quality control measure for off-site analysis.

  14. Economic Analyiss of "Symbiotic" Light Water Reactor/Fast Burner Reactor Fuel Cycles Proposed as Part of the U.S. Advanced Fuel Cycle Initiative (AFCI)

    SciTech Connect

    Williams, Kent Alan; Shropshire, David E.

    2009-01-01

    A spreadsheet-based 'static equilibrium' economic analysis was performed for three nuclear fuel cycle scenarios, each designed for 100 GWe-years of electrical generation annually: (1) a 'once-through' fuel cycle based on 100% LWRs fueled by standard UO2 fuel assemblies with all used fuel destined for geologic repository emplacement, (2) a 'single-tier recycle' scenario involving multiple fast burner reactors (37% of generation) accepting actinides (Pu,Np,Am,Cm) from the reprocessing of used fuel from the uranium-fueled LWR fleet (63% of generation), and (3) a 'two-tier' 'thermal+fast' recycle scenario where co-extracted U,Pu from the reprocessing of used fuel from the uranium-fueled part of the LWR fleet (66% of generation) is recycled once as full-core LWR MOX fuel (8% of generation), with the LWR MOX used fuel being reprocessed and all actinide products from both UO2 and MOX used fuel reprocessing being introduced into the closed fast burner reactor (26% of generation) fuel cycle. The latter two 'closed' fuel cycles, which involve symbiotic use of both thermal and fast reactors, have the advantages of lower natural uranium requirements per kilowatt-hour generated and less geologic repository space per kilowatt-hour as compared to the 'once-through' cycle. The overall fuel cycle cost in terms of $ per megawatt-hr of generation, however, for the closed cycles is 15% (single tier) to 29% (two-tier) higher than for the once-through cycle, based on 'expected values' from an uncertainty analysis using triangular distributions for the unit costs for each required step of the fuel cycle. (The fuel cycle cost does not include the levelized reactor life cycle costs.) Since fuel cycle costs are a relatively small percentage (10 to 20%) of the overall busbar cost (LUEC or 'levelized unit electricity cost') of nuclear power generation, this fuel cycle cost increase should not have a highly deleterious effect on the competitiveness of nuclear power. If the reactor life cycle

  15. Analysis of Tank 35H Samples in Support of Salt Batch Planning

    SciTech Connect

    Hay, M. S.; Coleman, C. J.; Diprete, D. P.

    2015-04-30

    Savannah River Remediation obtained three samples from different heights within Tank 35H. The samples were analyzed by Savannah River National Laboratory to support Salt Batch planning. The results from the analysis indicate the compositions of the three samples show increasing concentrations for most analytes going from HTF-35-15-17 through HTF-35-15-19 corresponding to successively deeper sampling locations. The data indicate some stratification within the tank. The plutonium and Sr-90 concentrations measured in the filtered samples were slightly lower than in the decanted (unfiltered) samples. The difference in the results for the filtered and unfiltered samples likely lies within the expected uncertainty for the measurement, but may indicate that filtration removed a small amount of suspended material from the samples.

  16. Remedial investigation sampling and analysis plan for J-Field, Aberdeen Proving Ground, Maryland. Volume 1: Field Sampling Plan

    SciTech Connect

    Benioff, P.; Biang, R.; Dolak, D.; Dunn, C.; Martino, L.; Patton, T.; Wang, Y.; Yuen, C.

    1995-03-01

    The Environmental Management Division (EMD) of Aberdeen Proving Ground (APG), Maryland, is conducting a remedial investigation and feasibility study (RI/FS) of the J-Field area at APG pursuant to the Comprehensive Environmental Response, Compensation, and Liability Act (CERCLA), as amended. J-Field is within the Edgewood Area of APG in Harford County, Maryland (Figure 1. 1). Since World War II activities in the Edgewood Area have included the development, manufacture, testing, and destruction of chemical agents and munitions. These materials were destroyed at J-Field by open burning and open detonation (OB/OD). Considerable archival information about J-Field exists as a result of efforts by APG staff to characterize the hazards associated with the site. Contamination of J-Field was first detected during an environmental survey of the Edgewood Area conducted in 1977 and 1978 by the US Army Toxic and Hazardous Materials Agency (USATHAMA) (predecessor to the US Army Environmental Center [AEC]). As part of a subsequent USATHAMA -environmental survey, 11 wells were installed and sampled at J-Field. Contamination at J-Field was also detected during a munitions disposal survey conducted by Princeton Aqua Science in 1983. The Princeton Aqua Science investigation involved the installation and sampling of nine wells and the collection and analysis of surficial and deep composite soil samples. In 1986, a Resource Conservation and Recovery Act (RCRA) permit (MD3-21-002-1355) requiring a basewide RCRA Facility Assessment (RFA) and a hydrogeologic assessment of J-Field was issued by the US Environmental Protection Agency (EPA). In 1987, the US Geological Survey (USGS) began a two-phased hydrogeologic assessment in data were collected to model, groundwater flow at J-Field. Soil gas investigations were conducted, several well clusters were installed, a groundwater flow model was developed, and groundwater and surface water monitoring programs were established that continue today.

  17. Sampling and analysis plan for sampling of liquid waste streams generated by 222-S Laboratory Complex operations

    SciTech Connect

    Benally, A.B.

    1997-08-14

    This Sampling and Analysis Plan (SAP) establishes the requirements and guidelines to be used by the Waste Management Federal Services of Hanford, Inc. personnel in characterizing liquid waste generated at the 222-S Laboratory Complex. The characterization process to verify the accuracy of process knowledge used for designation and subsequent management of wastes consists of three steps: to prepare the technical rationale and the appendix in accordance with the steps outlined in this SAP; to implement the SAP by sampling and analyzing the requested waste streams; and to compile the report and evaluate the findings to the objectives of this SAP. This SAP applies to portions of the 222-S Laboratory Complex defined as Generator under the Resource Conservation and Recovery Act (RCRA). Any portion of the 222-S Laboratory Complex that is defined or permitted under RCRA as a treatment, storage, or disposal (TSD) facility is excluded from this document. This SAP applies to the liquid waste generated in the 222-S Laboratory Complex. Because the analytical data obtained will be used to manage waste properly, including waste compatibility and waste designation, this SAP will provide directions for obtaining and maintaining the information as required by WAC173-303.

  18. Stratospheric Sampling and In Situ Atmospheric Chemical Element Analysis During Meteor Showers: A Resource Study

    NASA Technical Reports Server (NTRS)

    Noever, David A.

    2000-01-01

    Resources studies for asteroidal mining evaluation have depended historically on remote sensing analysis for chemical elements. During the November 1998 Leonids meteor shower, a stratospheric balloon and various low-density capture media were used to sample fragments from Comet Tempel-Tuttle debris during a peak Earth crossing. The analysis not only demonstrates how potential sampling strategies may improve the projections for metals or rare elements in astromining, but also benchmarks materials during low temperature (-60 F), high dessication environments as seen during atmospheric exposure. The results indicate high aluminum, magnesium and iron content for various sampled particles recovered, but generalization to the sporadic meteors expected from asteroidal sources will require future improvements in larger sampling volumes before a broad-use strategy for chemical analysis can be described. A repeat of the experimental procedure is planned for the November 1999 Leonids' shower, and various improvements for atmospheric sampling will be discussed.

  19. Sampling and Analysis Plan for Flammable Gases in Inactive Miscellaneous Underground Storage Tanks

    SciTech Connect

    NGUYEN, D.M.

    2000-02-01

    This sampling and analysis plan (SAP) identifies the field measurements for a screening of flammable gases in the vapor space of the inactive miscellaneous underground storage tanks (IMUSTs) currently assigned to the River Protection Project (RPP). If a measurement exceeds 25% of the lower flammability limit (LFL), vapor grab samples will be collected for laboratory analysis. This SAP also specifies the sample collection, laboratory analysis, quality assurance/quality control (QA/QC), and reporting objectives for grab sampling. Technical bases for the sampling objectives are provided in the Tank Safety Screening Data Quality Objectives (Dukelow et al 1995). The screening data will be used to determine if additional data are needed to support closure of a flammable gas unreviewed safety question for these facilities.

  20. Advanced Robotics for Mars Sample Handling and Analysis: On Earth! Now!

    NASA Astrophysics Data System (ADS)

    Rummel, J. D.; Allen, C.

    2011-12-01

    In the long history of studying Mars sample return missions (now in its 5th decade), there have been several constant constraints on the flight systems and the post-mission analyses of the samples. Sample selection, sample packaging, sample environmental conditions, and the transportation problem of getting the sampling system to Mars and the sample back, safely, are puzzles that are still with us. Those problems drive the mass, power, volume, and cost of mission(s) to return samples from the surface and near-surface of Mars, and there is no reason to think that they will go away anytime soon. Accordingly, a Mars sample return mission will stay expensive and technologically challenging. But what of the post-mission analyses on the sample, themselves? The problem of how to conduct a satisfactory analysis of Mars samples, on Earth, also remains. Those analyses are not only a cost driver, but a major factor in overall mission success. How does one examine "clean" Mars samples, and even check them for life or other potential hazards, when the Earth is effectively bathed in living organisms and other potential contaminants? How can the rest of the mission be worthwhile, if the samples returned become tainted after they reach Earth? Studies of the entire Mars sample return mission architecture have consistently called for the development of a sample-receiving facility and its associated biohazard-test protocol, instrumentation, and operations to be included in the earliest phases of the Mars sample return mission (cf., 1). It has also been noted that "considering the stringent contamination control constraints, together with the small size of samples that need to be manipulated, robotic systems may be a good choice as an integral part of the sample handling chain" (2). This paper will discuss the overall application of robotics technology to Mars sample-handling, and to organic and chemical contamination control to protect the samples and the ability to achieve back

  1. Neutron Activation Analysis of Soil Samples from Different Parts of Edirne in Turkey*

    NASA Astrophysics Data System (ADS)

    Zaim, N.; Dogan, C.; Camtakan, Z.

    2016-05-01

    The concentrations of constituent elements were determined in soil samples collected from different parts of the Maritza Basin, Edirne, Turkey. Neutron activation analysis, an extremely accurate technique, and the comparator method (using a standard) were applied for the first time in this region. After preparing the soil samples for neutron activation analysis, they were activated with thermal neutrons in a nuclear reactor, TRIGA-MARK II, at Istanbul Technical University. The activated samples were analyzed using a high-efficiency high-purity germanium detector, and gamma spectrometry was employed to determine the elemental concentration in the samples. Eight elements (chromium, manganese, cobalt, zinc, arsenic, molybdenum, cadmium, and barium) were qualitatively and quantitatively identified in 36 samples. The concentrations of some elements in the soil samples were high compared with values reported in the literature.

  2. Differentiation of fresh and frozen-thawed fish samples using Raman spectroscopy coupled with chemometric analysis.

    PubMed

    Velioğlu, Hasan Murat; Temiz, Havva Tümay; Boyaci, Ismail Hakki

    2015-04-01

    The potential of Raman spectroscopy was investigated in terms of its capability to discriminate the species of the fish samples and determine their freshness according to the number of freezing/thawing cycles they exposed. Species discrimination analysis was carried out on sixty-four fish samples from six different species, namely horse mackerel (Trachurus trachurus), European anchovy (Engraulis encrasicolus), red mullet (Mullus surmuletus), Bluefish (Pomatamus saltatrix), Atlantic salmon (Salmo salar) and flying gurnard (Trigla lucerna). Afterwards, fish samples were exposed to different numbers of freezing/thawing cycles and separated into three batches, namely (i) fresh, (ii) once frozen-thawed (OF) and (iii) twice frozen-thawed (TF) samples, in order to perform the freshness analysis. Raman data collected were used as inputs for chemometric analysis, which enabled us to develop two main PCA models to successfully terminate the studies for both species discrimination and freshness determination analysis.

  3. Sampling and Analysis Plan - Guidance and Template v.4 - General Projects - 04/2014

    EPA Pesticide Factsheets

    This Sampling and Analysis Plan (SAP) guidance and template is intended to assist organizations in documenting the procedural and analytical requirements for one-time, or time-limited, projects involving the collection of water, soil, sediment, or other

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

    NASA Technical Reports Server (NTRS)

    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

  5. Characterization and forensic analysis of soil samples using laser-induced breakdown spectroscopy (LIBS).

    PubMed

    Jantzi, Sarah C; Almirall, José R

    2011-07-01

    A method for the quantitative elemental analysis of surface soil samples using laser-induced breakdown spectroscopy (LIBS) was developed and applied to the analysis of bulk soil samples for discrimination between specimens. The use of a 266 nm laser for LIBS analysis is reported for the first time in forensic soil analysis. Optimization of the LIBS method is discussed, and the results compared favorably to a laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) method previously developed. Precision for both methods was <10% for most elements. LIBS limits of detection were <33 ppm and bias <40% for most elements. In a proof of principle study, the LIBS method successfully discriminated samples from two different sites in Dade County, FL. Analysis of variance, Tukey's post hoc test and Student's t test resulted in 100% discrimination with no type I or type II errors. Principal components analysis (PCA) resulted in clear groupings of the two sites. A correct classification rate of 99.4% was obtained with linear discriminant analysis using leave-one-out validation. Similar results were obtained when the same samples were analyzed by LA-ICP-MS, showing that LIBS can provide similar information to LA-ICP-MS. In a forensic sampling/spatial heterogeneity study, the variation between sites, between sub-plots, between samples and within samples was examined on three similar Dade sites. The closer the sampling locations, the closer the grouping on a PCA plot and the higher the misclassification rate. These results underscore the importance of careful sampling for geographic site characterization.

  6. Report of Sampling and Analysis Results: Swansea Army Housing Units, Swansea, Massachusetts

    DTIC Science & Technology

    1990-08-01

    recommended to determine if the asbestos is becoming airborne and to define what risks, if3 any , are presented by these findings. These studies were...inspection of the floor coverings and the3 removal and replacement of any that become damaged. Other suspect materials identified but not sampled...a dust sample was collected from this vent and analyzed. The air samples were subjected to analysis by TEM to identify and quantify any asbestos

  7. Analysis of core soil and water samples from the Cactus Crater Disposal Site at Enewetak atoll

    SciTech Connect

    Robison, W.L.; Noshkin, V.E.

    1981-02-18

    Core soil samples and water samples were collected from the Cactus Crater Disposal Site at Enewetak for analysis of /sup 137/Cs, /sup 90/Sr, /sup 239 +240/Pu and /sup 241/Am by both gamma spectroscopy and, through a contractor laboratory, by wet chemistry procedures. The samples processing methods, the analytical methods and the analytical quality control are all procedures developed for the continuing Marshall Island radioecology and dose assessment work.

  8. Sampling of Atmospheric Precipitation and Deposits for Analysis of Atmospheric Pollution

    PubMed Central

    Skarżyńska, K.; Polkowska, Ż; Namieśnik, J.

    2006-01-01

    This paper reviews techniques and equipment for collecting precipitation samples from the atmosphere (fog and cloud water) and from atmospheric deposits (dew, hoarfrost, and rime) that are suitable for the evaluation of atmospheric pollution. It discusses the storage and preparation of samples for analysis and also presents bibliographic information on the concentration ranges of inorganic and organic compounds in the precipitation and atmospheric deposit samples. PMID:17671615

  9. TMT One-Stop Shop: From Reliable Sample Preparation to Computational Analysis Platform.

    PubMed

    Mirzaei, Mehdi; Pascovici, Dana; Wu, Jemma X; Chick, Joel; Wu, Yunqi; Cooke, Brett; Haynes, Paul; Molloy, Mark P

    2017-01-01

    In this chapter we describe the workflow we use for labeled quantitative proteomics analysis using tandem mass tags (TMT) starting with the sample preparation and ending with the multivariate analysis of the resulting data. We detail the step-by-step process from sample processing, labeling, fractionation, and data processing using Proteome Discoverer through to data analysis and interpretation in the context of a multi-run experiment. The final analysis and data interpretation rely on an R package we call TMTPrepPro, which are deployed on a local GenePattern server, and used for generating various outputs which are also outlined herein.

  10. Analysis of phosphorus trends and evaluation of sampling designs in the Quinebaug River Basin, Connecticut

    USGS Publications Warehouse

    Todd Trench, Elaine C.

    2004-01-01

    A time-series analysis approach developed by the U.S. Geological Survey was used to analyze trends in total phosphorus and evaluate optimal sampling designs for future trend detection, using long-term data for two water-quality monitoring stations on the Quinebaug River in eastern Connecticut. Trend-analysis results for selected periods of record during 1971?2001 indicate that concentrations of total phosphorus in the Quinebaug River have varied over time, but have decreased significantly since the 1970s and 1980s. Total phosphorus concentrations at both stations increased in the late 1990s and early 2000s, but were still substantially lower than historical levels. Drainage areas for both stations are primarily forested, but water quality at both stations is affected by point discharges from municipal wastewater-treatment facilities. Various designs with sampling frequencies ranging from 4 to 11 samples per year were compared to the trend-detection power of the monthly (12-sample) design to determine the most efficient configuration of months to sample for a given annual sampling frequency. Results from this evaluation indicate that the current (2004) 8-sample schedule for the two Quinebaug stations, with monthly sampling from May to September and bimonthly sampling for the remainder of the year, is not the most efficient 8-sample design for future detection of trends in total phosphorus. Optimal sampling schedules for the two stations differ, but in both cases, trend-detection power generally is greater among 8-sample designs that include monthly sampling in fall and winter. Sampling designs with fewer than 8 samples per year generally provide a low level of probability for detection of trends in total phosphorus. Managers may determine an acceptable level of probability for trend detection within the context of the multiple objectives of the state?s water-quality management program and the scientific understanding of the watersheds in question. Managers may

  11. Goodness of Fit Confirmatory Factor Analysis: The Effects of Sample Size and Model Parsimony.

    ERIC Educational Resources Information Center

    Marsh, Herbert W.; Balla, John

    The influence of sample size (N) and model parsimony on a set of 22 goodness of fit indices was investigated, including those typically used in confirmatory factor analysis and some recently developed indices. For sample data simulated from 2 known population data structures, values for 6 of 22 fit indices were reasonably independent of N and were…

  12. Trace Chlorinated Organics Analysis in Highly Radioactive Samples-Problems and Solutions

    SciTech Connect

    Macek, P.; Hawthorne, L.; Hass, J. R.; Harvan, D.

    2002-02-26

    This paper discusses some of the problems that are associated with the analysis of highly radioactive samples for chlorinated organic compounds at the part per trillion level. To date, both high fission product activity and transuranic activity have been handle successfully. Communication issues, sample handling, transfer between laboratories and analytical challenges are discussed.

  13. Confirmatory Factor Analysis of the Career Factors Inventory on a Community College Sample

    ERIC Educational Resources Information Center

    Simon, Merril A.; Tovar, Esau

    2004-01-01

    A confirmatory factor analysis was conducted using AMOS 4.0 to validate the 21-item Career Factors Inventory on a community college student sample. The multidimensional inventory assesses types and levels of career indecision antecedents. The sample consisted of 512 ethnically diverse freshmen students; 46% were men and 54% were women.…

  14. Analysis of Large Data Logs: An Application of Poisson Sampling on Excite Web Queries.

    ERIC Educational Resources Information Center

    Ozmutlu, H. Cenk; Spink, Amanda; Ozmutlu, Seda

    2002-01-01

    Discusses the need for tools that allow effective analysis of search engine queries to provide a greater understanding of Web users' information seeking behavior and describes a study that developed an effective strategy for selecting samples from large-scale data sets. Reports on Poisson sampling with data logs from the Excite search engine.…

  15. Tank 241-U-106 vapor sampling and analysis tank characterization report

    SciTech Connect

    Huckaby, J.L.

    1995-05-31

    This report presents the details of the Hanford waste tank characterization study for tank 241-U-106. The drivers and objectives of the headspace vapor sampling and analysis were in accordance with procedures that were presented in other reports. The vapor and headspace gas samples were collected to determine the potential risks to tank farm workers due to fugitive emissions from the tank.

  16. Sampling and analysis plan for the former Atomic Energy Commission bus lot property

    SciTech Connect

    Nielson, R.R.

    1998-07-01

    This sampling and analysis plan (SAP) presents the rationale and strategy for the sampling and analysis activities proposed in support of an initial investigation of the former Atomic Energy Commission (AEC) bus lot property currently owned by Battelle Memorial Institute. The purpose of the proposed sampling and analysis activity is to investigate the potential for contamination above established action levels. The SAP will provide defensible data of sufficient quality and quantity to support recommendations of whether any further action within the study area is warranted. To assist in preparing sampling plans and reports, the Washington State Department of Ecology (Ecology) has published Guidance on Sampling and Data Analysis Methods. To specifically address sampling plans for petroleum-contaminated sites, Ecology has also published Guidance for Remediation of Petroleum Contaminated Sites. Both documents were used as guidance in preparing this plan. In 1992, a soil sample was taken within the current study area as part of a project to remove two underground storage tanks (USTs) at Battelle`s Sixth Street Warehouse Petroleum Dispensing Station (Section 1.3). The results showed that the sample contained elevated levels of total petroleum hydrocarbons (TPH) in the heavy distillate range. This current study was initiated in part as a result of that discovery. The following topics are considered: the historical background of the site, current site conditions, previous investigations performed at the site, an evaluation based on the available data, and the contaminants of potential concern (COPC).

  17. Report of Sampling and Analysis Results, Davisville Army Housing Units North Kingstown, Rhode Island

    DTIC Science & Technology

    1990-08-01

    the National Voluntary Laboratory Accreditation Program (NVLAP). The bulk samples were analyzed by Polarized iUght Microscopy (PLM) using the EPA’s...the Laboratory Accreditation package submitted by WESTON under NVLAP. This document includes standard procedures for sample analysis and quality...National Institute of Standards and Technology’s National VoluntaryE Laboratory Accreditation Program for asbestos fiber analysis (Laboratory Code 1254

  18. The Analysis of Cyanide and Its Breakdown Products in Biological Samples

    DTIC Science & Technology

    2010-01-01

    Literature 3. DATES COVERED (From - To) 4. TITLE AND SUBTITLE The Analysis of Cyanide and Its Breakdown Products in Biological Samples 5a. CONTRACT... cyanide , thiocyanate, 2-amino-2-thiazoline-4-carboxylic acid (ATCA), chemical warfare agent, exposure, toxicology, analytical methods 16. SECURITY...ISSN: 1040-8347 print / 1547-6510 online DOI: 10.1080/10408340903535315 The Analysis of Cyanide and its Breakdown Products in Biological Samples Brian A

  19. Analysis of tank 23H samples in support of salt batch planning

    SciTech Connect

    Hay, M. S.; Coleman, C. J.; Diprete, D. P.

    2015-08-14

    Savannah River Remediation obtained three samples from different heights within Tank 23H. The samples were analyzed by Savannah River National Laboratory to support salt batch planning. The results from the analysis indicate the top two samples from the tank appear similar in composition. The lowest sample from the tank contained significantly more solids and a more concentrated salt solution. The filtered supernate from the bottom sample showed ~60% lower Sr-90 and Pu-238 concentrations than the decanted (unfiltered) supernate results which may indicate the presence of some small amount of entrained solid particles in the decanted sample. The mercury concentrations measured in the filtered supernate were fairly low for all three samples ranging from 11.2 to 42.3 mg/L.

  20. UMTRA Project water sampling and analysis plan, Grand Junction, Colorado. Revision 1, Version 6

    SciTech Connect

    1995-09-01

    This water sampling and analysis plan describes the planned, routine ground water sampling activities at the Grand Junction US DOE Uranium Mill Tailings Remedial Action (UMTRA) Project site (GRJ-01) in Grand Junction, Colorado, and at the Cheney Disposal Site (GRJ-03) near Grand Junction. The plan identifies and justifies the sampling locations, analytical parameters, detection limits, and sampling frequencies for the routine monitoring stations at the sites. Regulatory basis is in the US EPA regulations in 40 CFR Part 192 (1994) and EPA ground water quality standards of 1995 (60 FR 2854). This plan summarizes results of past water sampling activities, details water sampling activities planned for the next 2 years, and projects sampling activities for the next 5 years.

  1. Protocol Improvements for Low Concentration DNA-Based Bioaerosol Sampling and Analysis

    PubMed Central

    Ng, Chun Kiat; Miller, Dana; Cao, Bin

    2015-01-01

    Introduction As bioaerosol research attracts increasing attention, there is a need for additional efforts that focus on method development to deal with different environmental samples. Bioaerosol environmental samples typically have very low biomass concentrations in the air, which often leaves researchers with limited options in choosing the downstream analysis steps, especially when culture-independent methods are intended. Objectives This study investigates the impacts of three important factors that can influence the performance of culture-independent DNA-based analysis in dealing with bioaerosol environmental samples engaged in this study. The factors are: 1) enhanced high temperature sonication during DNA extraction; 2) effect of sampling duration on DNA recoverability; and 3) an alternative method for concentrating composite samples. In this study, DNA extracted from samples was analysed using the Qubit fluorometer (for direct total DNA measurement) and quantitative polymerase chain reaction (qPCR). Results and Findings The findings suggest that additional lysis from high temperature sonication is crucial: DNA yields from both high and low biomass samples increased up to 600% when the protocol included 30-min sonication at 65°C. Long air sampling duration on a filter media was shown to have a negative impact on DNA recoverability with up to 98% of DNA lost over a 20-h sampling period. Pooling DNA from separate samples during extraction was proven to be feasible with margins of error below 30%. PMID:26619279

  2. Production of the ideal sample shape for Total Reflection X-ray Fluorescence analysis

    NASA Astrophysics Data System (ADS)

    Horntrich, C.; Kregsamer, P.; Prost, J.; Stadlbauer, F.; Wobrauschek, P.; Streli, C.

    2012-11-01

    Total Reflection X-ray Fluorescence analysis (TXRF) is a well-established analytical method in the semiconductor industry for the analysis of silicon wafer surfaces. For the calibration of the spectrometer typically an external standard is used which is sensitive to quantification errors. In general TXRF is known to allow for linear calibration. For small sample amounts (pg to ng region) the thin film approximation is valid neglecting absorption effects of the exciting and the detected radiation. For higher total amounts of sample the relation between fluorescence intensity and sample amount diverges from linearity (saturation effect). These deviations lead to difficulties in quantification with external standard. Content of the presented work is the production of the ideal TXRF sample shape, which was theoretically determined to be ring shaped. A possibility for the production of samples with ring shape is the use of a nanodispensing system combined with a positioning device. Therewith it is possible to produce ring shaped samples in a controlled way with the ring consisting of individual nanodroplets, so that the wanted diameter of the ring can be chosen. A comparison of the fluorescence intensities emitted by contracted and ring shaped samples shows that the ring shape is not only theoretically the best TXRF shape but also experimentally. It could be proven that for contracted samples the saturation effect occurs at a lower sample mass than for samples with ring shape.

  3. Uncertainty Determination Methodology, Sampling Maps Generation and Trend Studies with Biomass Thermogravimetric Analysis

    PubMed Central

    Pazó, Jose A.; Granada, Enrique; Saavedra, Ángeles; Eguía, Pablo; Collazo, Joaquín

    2010-01-01

    This paper investigates a method for the determination of the maximum sampling error and confidence intervals of thermal properties obtained from thermogravimetric analysis (TG analysis) for several lignocellulosic materials (ground olive stone, almond shell, pine pellets and oak pellets), completing previous work of the same authors. A comparison has been made between results of TG analysis and prompt analysis. Levels of uncertainty and errors were obtained, demonstrating that properties evaluated by TG analysis were representative of the overall fuel composition, and no correlation between prompt and TG analysis exists. Additionally, a study of trends and time correlations is indicated. These results are particularly interesting for biomass energy applications. PMID:21152292

  4. Uncertainty determination methodology, sampling maps generation and trend studies with biomass thermogravimetric analysis.

    PubMed

    Pazó, Jose A; Granada, Enrique; Saavedra, Angeles; Eguía, Pablo; Collazo, Joaquín

    2010-09-28

    This paper investigates a method for the determination of the maximum sampling error and confidence intervals of thermal properties obtained from thermogravimetric analysis (TG analysis) for several lignocellulosic materials (ground olive stone, almond shell, pine pellets and oak pellets), completing previous work of the same authors. A comparison has been made between results of TG analysis and prompt analysis. Levels of uncertainty and errors were obtained, demonstrating that properties evaluated by TG analysis were representative of the overall fuel composition, and no correlation between prompt and TG analysis exists. Additionally, a study of trends and time correlations is indicated. These results are particularly interesting for biomass energy applications.

  5. Sampling and analysis of hexavalent chromium during exposure to chromic acid mist and welding fumes.

    PubMed

    Blomquist, G; Nilsson, C A; Nygren, O

    1983-12-01

    Sampling and analysis of hexavalent chromium during exposure to chromic acid mist and welding fumes. Scand j work environ & health 9 (1983) 489-495. In view of the serious health effects of hexavalent chromium, the problems involved in its sampling and analysis in workroom air have been the subject of much concern. In this paper, the stability problems arising from the reduction of hexavalent to trivalent chromium during sampling, sample storage, and analysis are discussed. Replacement of sulfuric acid by a sodium acetate buffer (pH 4) as a leaching solution prior to analysis with the diphenylcarbazide (DPC) method is suggested and is demonstrated to be necessary in order to avoid reduction. Field samples were taken from two different industrial processes-manual metal arc welding on stainless steel without shield gas and chromium plating. A comparison was made of the DPC method, acidic dissolution with atomic absorption spectrophotometric (AAS) analysis, and the carbonate method. For chromic acid mist, the DPC method and AAS analysis were shown to give the same results. In the analysis of welding fumes, the modified DPC method gave the same results as the laborious and less sensitive carbonate method.

  6. NEW SOIL VOC SAMPLERS: EN CORE AND ACCU CORE SAMPLING/STORAGE DEVICES FOR VOC ANALYSIS

    SciTech Connect

    Susan S. Sorini; John F. Schabron; Joseph F. Rovani Jr

    2006-06-01

    Soil sampling and storage practices for volatile organic analysis must be designed to minimize loss of volatile organic compounds (VOCs) from samples. The En Core{reg_sign} sampler is designed to collect and store soil samples in a manner that minimizes loss of contaminants due to volatilization and/or biodegradation. An ASTM International (ASTM) standard practice, D 6418, Standard Practice for Using the Disposable En Core Sampler for Sampling and Storing Soil for Volatile Organic Analysis, describes use of the En Core sampler to collect and store a soil sample of approximately 5 grams or 25 grams for volatile organic analysis and specifies sample storage in the En Core sampler at 4 {+-} 2 C for up to 48 hours; -7 to -21 C for up to 14 days; or 4 {+-} 2 C for up to 48 hours followed by storage at -7 to -21 C for up to five days. This report discusses activities performed during the past year to promote and continue acceptance of the En Core samplers based on their performance to store soil samples for VOC analysis. The En Core sampler is designed to collect soil samples for VOC analysis at the soil surface. To date, a sampling tool for collecting and storing subsurface soil samples for VOC analysis is not available. Development of a subsurface VOC sampling/storage device was initiated in 1999. This device, which is called the Accu Core{trademark} sampler, is designed so that a soil sample can be collected below the surface using a dual-tube penetrometer and transported to the laboratory for analysis in the same container. Laboratory testing of the current Accu Core design shows that the device holds low-level concentrations of VOCs in soil samples during 48-hour storage at 4 {+-} 2 C and that the device is ready for field evaluation to generate additional performance data. This report discusses a field validation exercise that was attempted in Pennsylvania in 2004 and activities being performed to plan and conduct a field validation study in 2006. A draft ASTM

  7. Polychlorinated biphenyls (PCB) analysis report for solid sample from 219S tank 104

    SciTech Connect

    Ross, G.A.

    1998-03-27

    A sample of solids was obtained from tank 104 of 219S via a peristaltic pump equipped with a stainless steel tube and Norprenel tubing (Phthalate free). The sample obtained in a glass jar with Teflon 2 lid, was analyzed for PCBs as Aroclor mixtures. A soxhlet extraction procedure was used to extract the Aroclors from the sample. Analysis was performed using dual column confirmation gas chromatography/electron capture detection (GC/ECD). The extraction method closely follows SW-846 method 3540C and the analysis follows SW-846 method.

  8. Polychlorinate biphenyls (PCB) analysis report for solid sample for 219S tank 102

    SciTech Connect

    Ross, G.A.

    1997-12-05

    One waste sample was analyzed (with duplicate, matrix spike, and matrix spike duplicate) for PCBs as Aroclor mixtures by the Inorganic/Organic Chemistry Group. A soxhlet extraction procedure was used for extraction of the Aroclors from the sample. Analysis was performed using dual column confirmation gas chromatography/electron capture detection (GC/ECD). Extraction follows closely method 354 C of SW-846, analysis follows SW-846 method 8082. A cross reference of laboratory sample number to the customer identification is given in a table.

  9. Blocking Gibbs sampling for linkage analysis in large pedigrees with many loops.

    PubMed Central

    Jensen, C S; Kong, A

    1999-01-01

    We apply the method of "blocking Gibbs" sampling to a problem of great importance and complexity-linkage analysis. Blocking Gibbs sampling combines exact local computations with Gibbs sampling, in a way that complements the strengths of both. The method is able to handle problems with very high complexity, such as linkage analysis in large pedigrees with many loops, a task that no other known method is able to handle. New developments of the method are outlined, and it is applied to a highly complex linkage problem in a human pedigree. PMID:10441593

  10. Tannin analysis of chestnut bark samples (Castanea sativa Mill.) by HPLC-DAD-MS.

    PubMed

    Comandini, Patrizia; Lerma-García, María Jesús; Simó-Alfonso, Ernesto Francisco; Toschi, Tullia Gallina

    2014-08-15

    In the present investigation, an HPLC-DAD/ESI-MS method for the complete analysis of tannins and other phenolic compounds of different commercial chestnut bark samples was developed. A total of seven compounds (vescalin, castalin, gallic acid, vescalagin, 1-O-galloyl castalagin, castalagin and ellagic acid) were separated and quantified, being 1-O-galloyl castalagin tentatively identified and found for the first time in chestnut bark samples. Thus, this method provided information regarding the composition and quality of chestnut bark samples, which is required since these samples are commercialised due to their biochemical properties as ingredients of food supplements.

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

    PubMed

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

    2017-04-11

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

  12. Isotopic composition analysis and age dating of uranium samples by high resolution gamma ray spectrometry

    NASA Astrophysics Data System (ADS)

    Apostol, A. I.; Pantelica, A.; Sima, O.; Fugaru, V.

    2016-09-01

    Non-destructive methods were applied to determine the isotopic composition and the time elapsed since last chemical purification of nine uranium samples. The applied methods are based on measuring gamma and X radiations of uranium samples by high resolution low energy gamma spectrometric system with planar high purity germanium detector and low background gamma spectrometric system with coaxial high purity germanium detector. The ;Multigroup γ-ray Analysis Method for Uranium; (MGAU) code was used for the precise determination of samples' isotopic composition. The age of the samples was determined from the isotopic ratio 214Bi/234U. This ratio was calculated from the analyzed spectra of each uranium sample, using relative detection efficiency. Special attention is paid to the coincidence summing corrections that have to be taken into account when performing this type of analysis. In addition, an alternative approach for the age determination using full energy peak efficiencies obtained by Monte Carlo simulations with the GESPECOR code is described.

  13. Accelerating analysis for metabolomics, drugs and their metabolites in biological samples using multidimensional gas chromatography.

    PubMed

    Mitrevski, Blagoj S; Kouremenos, Konstantinos A; Marriott, Philip J

    2009-05-01

    Gas chromatography (GC) with mass spectrometry (MS) is one of the great enabling analytical tools available to the chemical and biochemical analyst for the measurement of volatile and semi-volatile compounds. From the analysis result, it is possible to assess progress in chemical reactions, to monitor environmental pollutants in a wide range of soil, water or air samples, to determine if an athlete or horse trainer has contravened doping laws, or if crude oil has migrated through subsurface rock to a reservoir. Each of these scenarios and samples has an associated implementation method for GC-MS. However, few samples and the associated interpretation of data is as complex or important as biochemical sample analysis for trace drugs or metabolites. Improving the analysis in both the GC and MS domains is a continual search for better separation, selectivity and sensitivity. Multidimensional methods are playing important roles in providing quality data to address the needs of analysts.

  14. Determining the effect of storage of cotton and soybean leaf samples for hyperspectral analysis

    Technology Transfer Automated Retrieval System (TEKTRAN)

    This paper studies the effect of storage techniques for transporting collected plant leaves from the field to the laboratory for hyperspectral analysis. The strategy of collecting leaf samples in field for laboratory analysis is often typically used when ground truthing is needed in remote sensing s...

  15. A look-ahead probabilistic contingency analysis framework incorporating smart sampling techniques

    SciTech Connect

    Chen, Yousu; Etingov, Pavel V.; Ren, Huiying; Hou, Zhangshuan; Rice, Mark J.; Makarov, Yuri V.

    2016-07-18

    This paper describes a framework of incorporating smart sampling techniques in a probabilistic look-ahead contingency analysis application. The predictive probabilistic contingency analysis helps to reflect the impact of uncertainties caused by variable generation and load on potential violations of transmission limits.

  16. COMPARISON OF FAST GC/TOFMS WITH METHOD TO-14 FOR ANALYSIS OF AMBIENT AIR SAMPLES

    EPA Science Inventory

    Field studies using portable gas chromatographs (PGC) to analyze volatile organic compounds in ambient air usually include, as reference standard method, the analysis of concurrent, collocated canister samples by EPA Method TO-14. Each laboratory analysis takes about an hour a...

  17. Space science technology: In-situ science. Sample Acquisition, Analysis, and Preservation Project summary

    NASA Technical Reports Server (NTRS)

    Aaron, Kim

    1991-01-01

    The Sample Acquisition, Analysis, and Preservation Project is summarized in outline and graphic form. The objective of the project is to develop component and system level technology to enable the unmanned collection, analysis and preservation of physical, chemical and mineralogical data from the surface of planetary bodies. Technology needs and challenges are identified and specific objectives are described.

  18. Qualitative analysis of seized cocaine samples using desorption electrospray ionization- mass spectrometry (DESI-MS).

    PubMed

    Stojanovska, Natasha; Tahtouh, Mark; Kelly, Tamsin; Beavis, Alison; Fu, Shanlin

    2015-05-01

    Desorption electrospray ionization - mass spectrometry (DESI-MS) is a useful technique for the qualitative analysis of compounds found in seized drug material. In this study, DESI-MS was utilized in the screening analysis of illicit cocaine samples. The technique was also applied to the geographical origin determination of these samples. The limit of detection was determined to be 24.3 µg (or 3.47 µg/mm(2) ) and the analysis time was less than 1 minute per sample. The intra-day and inter-day precision for the detection of cocaine was 11 % and 42 %, respectively; therefore the quantitative data provided by DESI-MS was limited in its use for accurate determination of cocaine concentration in a sample. Using the quadrupole time-of-flight (QTOF) mass spectrometer, the presence of cocaine and impurities detected were confirmed by accurate tandem MS data. The qualitative chemical profiles obtained using DESI-MS were compared to two popular analysis techniques, GC-MS and LC-MS. The effects of a range of adulterants including caffeine, procaine, levamisole, lignocaine, paracetamol, and atropine on the detectability of cocaine were also investigated. It was found that the addition of these adulterants in a cocaine sample did not prevent the detection of the analyte itself (there was slight enhancement in some samples), which was useful in drug detection. The detection of truxillines in the seized samples by DESI-MS aided in the preliminary determination of geographical origin, i.e., Bolivian, Peruvian or Colombian leaf origin. The application of DESI-MS to the qualitative analysis and screening of seized cocaine samples demonstrates the potential and applicability of the technique to the fast chemical profiling of illicit samples.

  19. A round robin approach to the analysis of bisphenol a (BPA) in human blood samples

    PubMed Central

    2014-01-01

    Background Human exposure to bisphenol A (BPA) is ubiquitous, yet there are concerns about whether BPA can be measured in human blood. This Round Robin was designed to address this concern through three goals: 1) to identify collection materials, reagents and detection apparatuses that do not contribute BPA to serum; 2) to identify sensitive and precise methods to accurately measure unconjugated BPA (uBPA) and BPA-glucuronide (BPA-G), a metabolite, in serum; and 3) to evaluate whether inadvertent hydrolysis of BPA-G occurs during sample handling and processing. Methods Four laboratories participated in this Round Robin. Laboratories screened materials to identify BPA contamination in collection and analysis materials. Serum was spiked with concentrations of uBPA and/or BPA-G ranging from 0.09-19.5 (uBPA) and 0.5-32 (BPA-G) ng/mL. Additional samples were preserved unspiked as ‘environmental’ samples. Blinded samples were provided to laboratories that used LC/MSMS to simultaneously quantify uBPA and BPA-G. To determine whether inadvertent hydrolysis of BPA metabolites occurred, samples spiked with only BPA-G were analyzed for the presence of uBPA. Finally, three laboratories compared direct and indirect methods of quantifying BPA-G. Results We identified collection materials and reagents that did not introduce BPA contamination. In the blinded spiked sample analysis, all laboratories were able to distinguish low from high values of uBPA and BPA-G, for the whole spiked sample range and for those samples spiked with the three lowest concentrations (0.5-3.1 ng/ml). By completion of the Round Robin, three laboratories had verified methods for the analysis of uBPA and two verified for the analysis of BPA-G (verification determined by: 4 of 5 samples within 20% of spiked concentrations). In the analysis of BPA-G only spiked samples, all laboratories reported BPA-G was the majority of BPA detected (92.2 – 100%). Finally, laboratories were more likely to be verified

  20. Distance software: design and analysis of distance sampling surveys for estimating population size.

    PubMed

    Thomas, Len; Buckland, Stephen T; Rexstad, Eric A; Laake, Jeff L; Strindberg, Samantha; Hedley, Sharon L; Bishop, Jon Rb; Marques, Tiago A; Burnham, Kenneth P

    2010-02-01

    1.Distance sampling is a widely used technique for estimating the size or density of biological populations. Many distance sampling designs and most analyses use the software Distance.2.We briefly review distance sampling and its assumptions, outline the history, structure and capabilities of Distance, and provide hints on its use.3.Good survey design is a crucial prerequisite for obtaining reliable results. Distance has a survey design engine, with a built-in geographic information system, that allows properties of different proposed designs to be examined via simulation, and survey plans to be generated.4.A first step in analysis of distance sampling data is modelling the probability of detection. Distance contains three increasingly sophisticated analysis engines for this: conventional distance sampling, which models detection probability as a function of distance from the transect and assumes all objects at zero distance are detected; multiple-covariate distance sampling, which allows covariates in addition to distance; and mark-recapture distance sampling, which relaxes the assumption of certain detection at zero distance.5.All three engines allow estimation of density or abundance, stratified if required, with associated measures of precision calculated either analytically or via the bootstrap.6.Advanced analysis topics covered include the use of multipliers to allow analysis of indirect surveys (such as dung or nest surveys), the density surface modelling analysis engine for spatial and habitat modelling, and information about accessing the analysis engines directly from other software.7.Synthesis and applications. Distance sampling is a key method for producing abundance and density estimates in challenging field conditions. The theory underlying the methods continues to expand to cope with realistic estimation situations. In step with theoretical developments, state-of-the-art software that implements these methods is described that makes the methods

  1. Yeast metabolomics: sample preparation for a GC/MS-based analysis.

    PubMed

    Carneiro, Sónia; Pereira, Rui; Rocha, Isabel

    2014-01-01

    Metabolome sample preparation is one of the key factors in metabolomics analyses. The quality of the metabolome data will depend on the suitability of the experimental procedures to the cellular system (e.g., yeast cells) and the analytical performance. Here, we summarize a protocol for metabolome analysis of yeast cells using gas chromatography-mass spectrometry (GC-MS). First, the main phases of a metabolomics analysis are identified: sample preparation, metabolite extraction, and analysis. We also provide an overview on different methods used to quench samples and extract intracellular metabolites from yeast cells. This protocol provides a detailed description of a GC-MS-based analysis of yeast metabolome, in particular for metabolites containing amino and/or carboxyl groups, which represent most of the compounds participating in the central carbon metabolism.

  2. Interface for the rapid analysis of liquid samples by accelerator mass spectrometry

    DOEpatents

    Turteltaub, Kenneth; Ognibene, Ted; Thomas, Avi; Daley, Paul F; Salazar Quintero, Gary A; Bench, Graham

    2014-02-04

    An interface for the analysis of liquid sample having carbon content by an accelerator mass spectrometer including a wire, defects on the wire, a system for moving the wire, a droplet maker for producing droplets of the liquid sample and placing the droplets of the liquid sample on the wire in the defects, a system that converts the carbon content of the droplets of the liquid sample to carbon dioxide gas in a helium stream, and a gas-accepting ion source connected to the accelerator mass spectrometer that receives the carbon dioxide gas of the sample in a helium stream and introduces the carbon dioxide gas of the sample into the accelerator mass spectrometer.

  3. Method validation and uncertainty evaluation of organically bound tritium analysis in environmental sample.

    PubMed

    Huang, Yan-Jun; Zeng, Fan; Zhang, Bing; Chen, Chao-Feng; Qin, Hong-Juan; Wu, Lian-Sheng; Guo, Gui-Yin; Yang, Li-Tao; Shang-Guan, Zhi-Hong

    2014-08-01

    The analytical method for organically bound tritium (OBT) was developed in our laboratory. The optimized operating conditions and parameters were established for sample drying, special combustion, distillation, and measurement on a liquid scintillation spectrometer (LSC). Selected types of OBT samples such as rice, corn, rapeseed, fresh lettuce and pork were analyzed for method validation of recovery rate reproducibility, the minimum detection concentration, and the uncertainty for typical low level environmental sample was evaluated. The combustion water recovery rate of different dried environmental sample was kept at about 80%, the minimum detection concentration of OBT ranged from 0.61 to 0.89 Bq/kg (dry weight), depending on the hydrogen content. It showed that this method is suitable for OBT analysis of environmental sample with stable recovery rate, and the combustion water yield of a sample with weight about 40 g would provide sufficient quantity for measurement on LSC.

  4. Tank 241-SY-101 push mode core sampling and analysis plan

    SciTech Connect

    CONNER, J.M.

    1998-10-09

    This sampling and analysis plan (SAP) identifies characterization objectives pertaining to sample collection, laboratory analytical evaluation, and reporting requirements for push mode core samples from tank 241-SY-101 (SY-101). It is written in accordance with Data Quality Objective to Support Resolution of the Flammable Gas Safety Issue (Bauer 1998), Low Activity Waste Feed Data Quality Objectives (Wiemers and Miller 1997 and DOE 1998), Data Quality Objectives for TWRS Privatization Phase I: Confirm Tank T is an Appropriate Feed Source for Low-Activity Waste Feed Batch X (Certa 1998), and the Tank Safety Screening Data Quality Objective (Dukelow et al. 1995). The Tank Characterization Technical Sampling Basis document (Brown et al. 1998) indicates that these issues apply to tank SY-101 for this sampling event. Brown et al. also identifies high-level waste, regulatory, pretreatment and disposal issues as applicable issues for this tank. However, these issues will not be addressed via this sampling event.

  5. Finite element analysis of seal mechanism using SMA for Mars sample return

    NASA Astrophysics Data System (ADS)

    Bao, Xiaoqi; Younse, Paulo

    2014-04-01

    Returning Martian samples to Earth for extensive analysis is of great interest to planetary science community. Current Mars sample return architecture would require leaving the acquired samples on Mars for several years before being retrieved by subsequent mission. Each sample would be sealed securely to keep its integrity. A reliable seal technique that does not affect the integrity of the samples and uses simple low-mass tool is required. The shape memory alloy (SMA) seal technique is a promising candidate. The performances of several primary designs of SMA seal for sample tubes were analyzed by finite element (FE) modeling. The results of thermal heating characteristics had been reported in a previous presentation this paper focus on the preparation and actuation of SMA plugs, the seal pressure, and the stress and strain induced in the sealing procedure with various designs.

  6. Report of Sampling and Analysis Results, Manhattan Beach Army Housing Units, Brooklyn, New York

    DTIC Science & Technology

    1990-09-01

    are also included in Appendix A.2. All analyses were performed in accordance with protocols set forth in the Laboratory Accreditation package submitted...Voluntaryi Laboratory Accreditation Program for asbestos fiber analysis (Laboratory Code 1254). I BULK SAMPLE ANALYSIS SUMMARY Weston W.O. No. 2104-13-01...accredited by the National Instiute of Standard an0/Techno0ogy s NationaL Voluntary Laboratory Accreditation Program for asbestos fiber analysis

  7. MALDI MS sample preparation by using paraffin wax film: systematic study and application for peptide analysis.

    PubMed

    Wang, Junhua; Chen, Ruibing; Ma, Mingming; Li, Lingjun

    2008-01-15

    Recently developed sample preparation techniques employing hydrophobic sample support have improved the detection sensitivity and mass spectral quality of matrix-assisted laser desorption/ionization mass spectrometry (MALDI MS). These methods concentrate the samples on target by minimizing the sample area via the solvent repellent effect of the target surface. In the current study, we employed the use of paraffin wax film (Parafilm M) for improved MALDI MS analysis of low-abundance peptide mixtures, including neuronal tissue releasate and protein tryptic digests. This thin film was found to strongly repel polar solvents including water, methanol, and acetonitrile, which enabled the application of a wide range of sample preparation protocols that involved the use of various organic solvents. A "nanoliter-volume deposition" technique employing a capillary column has been used to produce tiny ( approximately 400 microm) matrix spots of 2,5-dihydroxybenzoic acid on the film. By systematically optimizing the sample volume, solvent composition, and film treatment, the Parafilm M substrate in combination with the nanoliter-volume matrix deposition method allowed dilute sample to be concentrated on the film for MALDI MS analysis. Peptide mixtures with nanomolar concentrations have been detected by MALDI time-of-flight and MALDI Fourier transform ion cyclotron resonance mass spectrometers. Overall, the use of Parafilm M enabled improved sensitivity and spectral quality for the analysis of complex peptide mixtures.

  8. Multivariate Curve Resolution Applied to Hyperspectral Imaging Analysis of Chocolate Samples.

    PubMed

    Zhang, Xin; de Juan, Anna; Tauler, Romà

    2015-08-01

    This paper shows the application of Raman and infrared hyperspectral imaging combined with multivariate curve resolution (MCR) to the analysis of the constituents of commercial chocolate samples. The combination of different spectral data pretreatment methods allowed decreasing the high fluorescent Raman signal contribution of whey in the investigated chocolate samples. Using equality constraints during MCR analysis, estimations of the pure spectra of the chocolate sample constituents were improved, as well as their relative contributions and their spatial distribution on the analyzed samples. In addition, unknown constituents could be also resolved. White chocolate constituents resolved from Raman hyperspectral image indicate that, at macro scale, sucrose, lactose, fat, and whey constituents were intermixed in particles. Infrared hyperspectral imaging did not suffer from fluorescence and could be applied for white and milk chocolate. As a conclusion of this study, micro-hyperspectral imaging coupled to the MCR method is confirmed to be an appropriate tool for the direct analysis of the constituents of chocolate samples, and by extension, it is proposed for the analysis of other mixture constituents in commercial food samples.

  9. Quantitative solid sample analysis by ArF excimer laser ablation

    NASA Astrophysics Data System (ADS)

    Delmdahl, Ralph; von Oldershausen, Georg

    2005-06-01

    Reproducible and sensitive elemental analysis of solid samples is a crucial task in areas of geology (e.g. microanalysis of fluid inclusions), material sciences, industrial quality control as well as in environmental, forensic and biological studies. To date the most versatile detection method is mass-spectroscopic multi-element analysis. In order to obtain reproducible results, this requires transferring the solid sample into the gas-phase while preserving the sample's stoichiometric composition. Laser Ablation in combination with inductively coupled plasma-mass spectrometry (LA-ICP-MS) is a proven powerful technique to meet the requirements for reliable solid sample analysis. The sample is laser ablated in an air-tight cell and the aerosol is carried by an inert gas to a micro-wave induced plasma where its constituents are atomized and ionized prior to mass analysis. The 193 nm excimer laser ablation, in particular, provides athermal sample ablation with very precise lateral ablation and controlled depth profiling. The high photon energy and beam homogeneity of the 193 nm excimer laser system avoids elemental fractionation and permits clean ablation of even transmissive solid materials such as carbonates, fluorites and pure quartz.

  10. Total reflection X-ray fluorescence as a fast multielemental technique for human placenta sample analysis

    NASA Astrophysics Data System (ADS)

    Marguí, E.; Ricketts, P.; Fletcher, H.; Karydas, A. G.; Migliori, A.; Leani, J. J.; Hidalgo, M.; Queralt, I.; Voutchkov, M.

    2017-04-01

    In the present contribution, benchtop total reflection X-ray fluorescence spectrometry (TXRF) has been evaluated as a cost-effective multielemental analytical technique for human placenta analysis. An easy and rapid sample preparation consisting of suspending 50 mg of sample in 1 mL of a Triton 1% solution in deionized water showed to be the most suitable for this kind of samples. However, for comparison purposes, an acidic microwave acidic digestion procedure was also applied. For both sample treatment methodologies, limits of detection for most elements were in the low mg/kg level. Accurate and precise results were obtained using internal standardization as quantification approach and applying a correction factor to compensate for absorption effects. The correction factor was based on the proportional ratio between the slurry preparation results and those obtained for the analysis of a set of human placenta samples analysed by microwave acidic digestion and ICP-AES analysis. As a study case, the developed TXRF methodology was applied for multielemental analysis (K, Ca, Fe, Cu, Zn, As, Se, Br, Rb and Sr) of several healthy women's placenta samples from two regions in Jamaica.

  11. Quantitative X-ray fluorescence analysis of samples of less than `infinite thickness': Difficulties and possibilities

    NASA Astrophysics Data System (ADS)

    Sitko, Rafał

    2009-11-01

    X-ray fluorescence spectrometry due to its nondestructive nature is widely applied in analysis of single layers and multiple layer films (e.g. semiconductors, electrooptic and solar cell devices, coatings, corrosion and paint layers), individual particles (airborne, fly ash, gunshot residue particles, etc.), art and archeological objects (manuscripts, paintings, icons) and many others. Quantitative analysis of these materials, frequently classified as samples of less than infinite thickness (thin or intermediate-thickness samples), required applying adequate matrix correction methods taking into account complex dependence of analyte fluorescent radiation intensity on full matrix composition and sample thickness. In this article, the matrix correction methods including fundamental parameters, Monte Carlo simulations, influence coefficients algorithms and methods based on X-ray transmission measurements are reviewed. The difficulties in the analysis of single layer and multiple layer films and the accuracy of fundamental parameter methods in simultaneous determination of their thickness and composition are discussed. The quantitative analysis of individual particles and inhomogeneous and/or complex structure materials using fundamental parameter and Monte Carlo simulation methods in micro-beam X-ray fluorescence spectrometry are also reviewed. Some references are devoted to the analysis of light matrix samples, e.g. geological, environmental and biological samples, in which undetectable low-Z elements are present (so-called 'dark matrix') using backscattered fundamental parameter methods. Since the samples of less than infinite thickness are partially transparent for X-ray beams, the transmission measurements present possibilities that are unattainable for bulk samples. Thus, the emission-transmission method and also new instruments allowing measurements of the primary X-ray beam transmitted through the sample together with measurements of X-ray fluorescence

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

    SciTech Connect

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

    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

  13. Representativeness of laboratory sampling procedures for the analysis of trace metals in soil.

    PubMed

    Dubé, Jean-Sébastien; Boudreault, Jean-Philippe; Bost, Régis; Sona, Mirela; Duhaime, François; Éthier, Yannic

    2015-08-01

    This study was conducted to assess the representativeness of laboratory sampling protocols for purposes of trace metal analysis in soil. Five laboratory protocols were compared, including conventional grab sampling, to assess the influence of sectorial splitting, sieving, and grinding on measured trace metal concentrations and their variability. It was concluded that grinding was the most important factor in controlling the variability of trace metal concentrations. Grinding increased the reproducibility of sample mass reduction by rotary sectorial splitting by up to two orders of magnitude. Combined with rotary sectorial splitting, grinding increased the reproducibility of trace metal concentrations by almost three orders of magnitude compared to grab sampling. Moreover, results showed that if grinding is used as part of a mass reduction protocol by sectorial splitting, the effect of sieving on reproducibility became insignificant. Gy's sampling theory and practice was also used to analyze the aforementioned sampling protocols. While the theoretical relative variances calculated for each sampling protocol qualitatively agreed with the experimental variances, their quantitative agreement was very poor. It was assumed that the parameters used in the calculation of theoretical sampling variances may not correctly estimate the constitutional heterogeneity of soils or soil-like materials. Finally, the results have highlighted the pitfalls of grab sampling, namely, the fact that it does not exert control over incorrect sampling errors and that it is strongly affected by distribution heterogeneity.

  14. An optimization based sampling approach for multiple metrics uncertainty analysis using generalized likelihood uncertainty estimation

    NASA Astrophysics Data System (ADS)

    Zhou, Rurui; Li, Yu; Lu, Di; Liu, Haixing; Zhou, Huicheng

    2016-09-01

    This paper investigates the use of an epsilon-dominance non-dominated sorted genetic algorithm II (ɛ-NSGAII) as a sampling approach with an aim to improving sampling efficiency for multiple metrics uncertainty analysis using Generalized Likelihood Uncertainty Estimation (GLUE). The effectiveness of ɛ-NSGAII based sampling is demonstrated compared with Latin hypercube sampling (LHS) through analyzing sampling efficiency, multiple metrics performance, parameter uncertainty and flood forecasting uncertainty with a case study of flood forecasting uncertainty evaluation based on Xinanjiang model (XAJ) for Qing River reservoir, China. Results obtained demonstrate the following advantages of the ɛ-NSGAII based sampling approach in comparison to LHS: (1) The former performs more effective and efficient than LHS, for example the simulation time required to generate 1000 behavioral parameter sets is shorter by 9 times; (2) The Pareto tradeoffs between metrics are demonstrated clearly with the solutions from ɛ-NSGAII based sampling, also their Pareto optimal values are better than those of LHS, which means better forecasting accuracy of ɛ-NSGAII parameter sets; (3) The parameter posterior distributions from ɛ-NSGAII based sampling are concentrated in the appropriate ranges rather than uniform, which accords with their physical significance, also parameter uncertainties are reduced significantly; (4) The forecasted floods are close to the observations as evaluated by three measures: the normalized total flow outside the uncertainty intervals (FOUI), average relative band-width (RB) and average deviation amplitude (D). The flood forecasting uncertainty is also reduced a lot with ɛ-NSGAII based sampling. This study provides a new sampling approach to improve multiple metrics uncertainty analysis under the framework of GLUE, and could be used to reveal the underlying mechanisms of parameter sets under multiple conflicting metrics in the uncertainty analysis process.

  15. Evaluation of soil gas sampling and analysis techniques at a former petrochemical plant site.

    PubMed

    Hers, I; Li, L; Hannam, S

    2004-07-01

    Methods for soil gas sampling and analysis are evaluated as part of a research study on soil vapour intrusion into buildings, conducted at a former petro-chemical plant site ("Chatterton site"). The evaluation process was designed to provide information on reliability and selection of appropriate methods for soil gas sampling and analysis, and was based on a literature review of data and methods, and experiments completed as part of the research study. The broader context of this work is that soil gas characterization is increasingly being used for input into risk assessment of contaminated sites, particularly when evaluating the potential intrusion of soil vapour into buildings. There are only a limited number of research studies and protocols addressing soil gas sampling and analysis. There is significant variability in soil gas probe design and sample collection and analysis methods used by practitioners. The experimental studies conducted to evaluate soil gas methods address the permeation or leakage of gases from Tedlar bags, time-dependent sorption of volatile organic compound (VOC)-vapours onto probe surfaces and sampling devices, and analytical and quality control issues for light gas and VOC analyses. Through this work, common techniques for soil gas collection and analysis are described together with implications for data quality arising from the different methods used. Some of the potential pitfalls that can affect soil gas testing are identified, and recommendations and guidance for improved protocols are provided.

  16. Probabilistic Round Trip Contamination Analysis of a Mars Sample Acquisition and Handling Process Using Markovian Decompositions

    NASA Technical Reports Server (NTRS)

    Hudson, Nicolas; Lin, Ying; Barengoltz, Jack

    2010-01-01

    A method for evaluating the probability of a Viable Earth Microorganism (VEM) contaminating a sample during the sample acquisition and handling (SAH) process of a potential future Mars Sample Return mission is developed. A scenario where multiple core samples would be acquired using a rotary percussive coring tool, deployed from an arm on a MER class rover is analyzed. The analysis is conducted in a structured way by decomposing sample acquisition and handling process into a series of discrete time steps, and breaking the physical system into a set of relevant components. At each discrete time step, two key functions are defined: The probability of a VEM being released from each component, and the transport matrix, which represents the probability of VEM transport from one component to another. By defining the expected the number of VEMs on each component at the start of the sampling process, these decompositions allow the expected number of VEMs on each component at each sampling step to be represented as a Markov chain. This formalism provides a rigorous mathematical framework in which to analyze the probability of a VEM entering the sample chain, as well as making the analysis tractable by breaking the process down into small analyzable steps.

  17. EMP Attachment 1 DOE-SC PNNL Site Sampling and Analysis Plan

    SciTech Connect

    Meier, Kirsten M.

    2011-11-10

    This Sampling and Analysis Plan (SAP) is written for the radiological environmental air surveillance program for the DOE-SC PNNL Site, Richland Washington. It provides the requirements for planning sampling events, and the requirements imposed on the analytical laboratory analyzing the air samples. The actual air sampling process is in procedure EPRP-AIR-029. The rationale for analyte selection, media, and sampling site location has been vetted through the data quality objectives (DQO) process (Barnett et al. 2010). The results from the DQO process have been reviewed and approved by the Washington State Department of Health. The DQO process (Barnett et al. 2010) identified seven specific radionuclides for analysis along with the need for gross alpha and gross beta radiological analyses. The analytes are {sup 241}Am, {sup 243}Am, {sup 244}Cm, {sup 60}Co, {sup 238}Pu, {sup 239}Pu, and {sup 233}U. The report also determined that air samples for particulates are the only sample matrix required for the monitoring program. These samples are collected on 47-mm glass-fiber filters.

  18. DWPF Sample Vial Insert Study-Statistical Analysis of DWPF Mock-Up Test Data

    SciTech Connect

    Harris, S.P.

    1997-09-18

    This report is prepared as part of Technical/QA Task Plan WSRC-RP-97-351 which was issued in response to Technical Task Request HLW/DWPF/TTR-970132 submitted by DWPF. Presented in this report is a statistical analysis of DWPF Mock-up test data for evaluation of two new analytical methods which use insert samples from the existing HydragardTM sampler. The first is a new hydrofluoric acid based method called the Cold Chemical Method (Cold Chem) and the second is a modified fusion method.Either new DWPF analytical method could result in a two to three fold improvement in sample analysis time.Both new methods use the existing HydragardTM sampler to collect a smaller insert sample from the process sampling system. The insert testing methodology applies to the DWPF Slurry Mix Evaporator (SME) and the Melter Feed Tank (MFT) samples.The insert sample is named after the initial trials which placed the container inside the sample (peanut) vials. Samples in small 3 ml containers (Inserts) are analyzed by either the cold chemical method or a modified fusion method. The current analytical method uses a HydragardTM sample station to obtain nearly full 15 ml peanut vials. The samples are prepared by a multi-step process for Inductively Coupled Plasma (ICP) analysis by drying, vitrification, grinding and finally dissolution by either mixed acid or fusion. In contrast, the insert sample is placed directly in the dissolution vessel, thus eliminating the drying, vitrification and grinding operations for the Cold chem method. Although the modified fusion still requires drying and calcine conversion, the process is rapid due to the decreased sample size and that no vitrification step is required.A slurry feed simulant material was acquired from the TNX pilot facility from the test run designated as PX-7.The Mock-up test data were gathered on the basis of a statistical design presented in SRT-SCS-97004 (Rev. 0). Simulant PX-7 samples were taken in the DWPF Analytical Cell Mock

  19. Sample Size Tables for Correlation Analysis with Applications in Partial Correlation and Multiple Regression Analysis

    ERIC Educational Resources Information Center

    Algina, James; Olejnik, Stephen

    2003-01-01

    Tables for selecting sample size in correlation studies are presented. Some of the tables allow selection of sample size so that r (or r[squared], depending on the statistic the researcher plans to interpret) will be within a target interval around the population parameter with probability 0.95. The intervals are [plus or minus] 0.05, [plus or…

  20. Sampling of illicit drugs for quantitative analysis. Part I: heterogeneity study of illicit drugs in Europe.

    PubMed

    Dujourdy, L; Csesztregi, T; Bovens, M; Franc, A; Nagy, J

    2013-09-10

    Sampling of illicit drugs for qualitative and quantitative analysis would normally be considered as routine and comparable tasks in forensic drugs laboratories and previously similar statistical sampling approaches have been applied. However, we believe that two different sampling approaches, based on two different theoretical and statistical backgrounds are more appropriate. Furthermore the application of the qualitative sampling approach can be impractical for quantitative sampling as it could generate many analytical samples from a single seizure. In some countries the purity of the illicit drug in a seizure may affect the criminal sentence and therefore, reliable results for quantitative analysis are crucial. It was decided to investigate a new approach, which although incorporating some statistics also took account of our background knowledge about the composition of the drugs we were analysing. The ultimate goal was to produce recommendations for a practical sampling plan for quantitative analysis. It was found that the two key factors which had a significant effect on obtaining a representative analytical sample from a bulk seizure were the heterogeneity of the drug powder and the particle sizes of its components. This article concentrates on drug heterogeneity. Particle size effects will be addressed in part II of this study. A sampling plan was devised for a range of drug seizure types and asked ENFSI member laboratories to use it when analysing real drug seizures to provide heterogeneity data for the most common illicit drugs (heroin, cocaine, amphetamine, MDMA and cannabis (herbal and resin)). It was found that for routine quantitative drugs analysis, the sampling problems caused by heterogeneity can be solved by using an incremental sampling protocol. Furthermore, the number of increments that need to be taken for a particular drug is dependent on the relative standard deviation (RSD) required by an individual laboratory and the analytical method that