Science.gov

Sample records for in-situ gamma spectrometry

  1. In situ gamma-spectrometry intercomparison exercise in Salzburg, Austria

    NASA Astrophysics Data System (ADS)

    Lettner, H.; Andrasi, A.; Hubmer, A. K.; Lovranich, E.; Steger, F.; Zombori, P.

    1996-02-01

    In situ gamma-spectrometry has become a useful method of assessing the nuclide concentrations of man-made and natural gamma-emitters in the soil. For the quality assurance of the measurements, periodically conducted intercomparison exercises are essential. Therefore exercises were organized in different European countries since 1990, the last one was conducted in Salzburg, Austria in September 1994. The participation of 27 measurement teams from all over Europe emphasizes the importance of the intercomparison. Salzburg was selected because the Province of Salzburg, Austria was among the most heavily contaminated regions outside the former USSR by the Chernobyl fallout. Two different typical sites were selected for the measurements: Site 1 was inside the urban area of Salzburg on intensively used grassland which had not been tilled since the deposition of the fallout. This site is representative for intensively used agricultural regions in the Province of Salzburg. Site 2 was in the mountainous regions of the Hohe Tauern at an elevated altitude of 1600 m, representing the agricultural soil- and contamination conditions of the Alpine regions in the Tauern. The two sites differ significantly in terms of soil characteristics, a crucial parameter for the evaluation of in situ gamma-spectra. The participants used different approaches for the evaluation of the gamma-spectra in terms of considering the depth distribution. In the paper the results from the 24 European teams are presented.

  2. Radioactivity measurements in the aquatic environment using in-situ and laboratory gamma-ray spectrometry.

    PubMed

    Eleftheriou, G; Tsabaris, C; Androulakaki, E G; Patiris, D L; Kokkoris, M; Kalfas, C A; Vlastou, R

    2013-12-01

    The in-situ underwater gamma-ray spectrometry method is validated by inter-comparison with laboratory method. Deployments of the spectrometer KATERINA on a submarine spring and laboratory measurements of water samples with HPGe detector were performed. Efficiency calibrations, Monte Carlo simulations and the Minimum Detectable Activity (MDA) estimations were realized. MDAs varied from 0.19 to 10.4 (lab) and 0.05 to 0.35 (in-situ) Bq/L, while activity concentrations differed from 7% (for radon progenies) up to 10% (for (40)K), between the two methods. PMID:24103707

  3. Application of in-situ gamma spectrometry in the remediation of radioactively contaminated soil

    SciTech Connect

    Sutton, C.; Yesso, J.D.; Danahy, R.J.; Cox, T.

    1999-06-01

    The Fernald Environmental Management Project (FEMP) is a US Department of Energy site that is undergoing total remediation and closure. Most of the remediation effort entails massive excavation of soil for disposal, both offsite and onsite, at an engineered disposal facility. In-situ gamma spectrometry is routinely used to support soil excavation operations to accurately and quickly identify soil areas as being above or below regulatory remediation criteria. Two different in-situ gamma spectrometry systems are used. The first is a sodium iodide (NaI) detector mounted either on a tractor or a jogging stroller, depending on the terrain to be measured. The NaI system allows the collection of a gamma energy spectrum which can be analyzed to identify and quantify radioactive isotopes which are present within the detector`s viewing area. Each energy spectrum is tagged by location coordinates provided by an on-board global positioning system (GPS) to precisely locate elevated contamination areas. The second is a tripod-mounted, high purity germanium detector (HPGe) gamma spectrometry system that is functionally similar to the NaI system. The principal advantage of the HPGe is its superior resolution, which allows much more accurate identification and quantification of radionuclide contaminants in soils. In order to effectively utilize the data quality objective process with these systems, three quality assurance (QA) elements had to be performed.

  4. Fluence Evaluations For Applications of In Situ Gamma-Ray Spectrometry in Non-Flat Terrain

    SciTech Connect

    Miller, Kevin M.

    1999-02-28

    Evaluations of gamma-ray fluence are made for source geometries that depart from the flat ground geometry that is used in standard applications of in situ spectrometry. Geometries considered include uniform source distributions for soil mounds on top of flat terrain, cylindrical wells, and rectangular trenches. The results indicate that scaling the standard fluence values for flat terrain by the ratio of solid angle subtended by the soil to 2π leads to fluence estimates that are accurate to within a few percent. Practical applications of in situ spectrometry in non-flat terrain also appears to be simplified by the fact that the angular correction factor for a typical coaxial detector in these geometries may typically be about the same as that computed for flat ground.

  5. Effect of environmental variables upon in-situ gamma spectrometry data

    SciTech Connect

    Sutton, C.

    1999-06-01

    The Fernald Environmental Management Project (FEMP) is a US Department of Energy site that is undergoing total remediation and closure. Fernald is a former uranium refinery which produced high quality uranium metal. Soil in the Fernald site is pervasively contaminated with uranium and secondarily with thorium and radium isotopes. In-situ gamma spectrometry is routinely utilized in soil excavation operations at Fernald to provide high quality and timely analytical data on radionuclide contaminants in soil. To understand the effect of environmental conditions upon in-situ gamma spectrometry measurements, twice daily measurements were made, weather permitting, with a tripod-mounted high purity germanium detector (HPGe) at a single field location (field quality control station) at the Fernald Environmental Management Project. Such measurements are the field analogue of a laboratory control standard. The basic concept is that measurement variations over an extended period of time at a single location can be related to environmental parameters. Trends, peaks, and troughs in data might be correlative to both long-term and short-term environmental conditions. In this paper environmental variables/ conditions refer to weather related phenomena such as soil moisture, rainfall, atmospheric humidity, and atmospheric temperature.

  6. In situ gamma spectrometry of piping in a CANDU heat transport system -- Application during decontamination

    SciTech Connect

    Husain, A.; Breckenridge, C.E.; Storey, D.

    1995-02-01

    An in situ pipe gamma spectrometry technique was applied to determine the activity within piping during various stages of CANDU reactor decontaminations. Measurements were performed in general radiation fields up to {approximately}500 mR/h and required both the detector and the pipe being scanned to be appropriately shielded from other neighboring piping. Measured counts were interpreted using a pipe source efficiency calibration with due regard to its distance dependence. Cobalt-60 was the dominant radionuclide on the piping before the decontamination. Deposition of {sup 124}Sb occurred on out-core piping surfaces during the decontamination. The spectrometry measurements were supplemented with contact radiation field measurements, which were performed using survey detectors housed within specially designed pipe shields. Radiation fields estimated from measured radionuclide activities were compared with the measured radiation fields. On average, the ratio of measured to estimated fields was {approximately}72%. Reasons for this discrepancy are discussed.

  7. In situ gamma-ray spectrometry in the environment using dose rate spectroscopy

    NASA Astrophysics Data System (ADS)

    Ji, Young-Yong; Kim, Chang-Jong; Chung, Kun Ho; Choi, Hee-Yeoul; Lee, Wanno; Kang, Mun Ja; Park, Sang Tae

    2016-02-01

    In order to expand the application of dose rate spectroscopy to the environment, in situ gamma-ray spectrometry was first conducted at a height of 1 m above the ground to calculate the ambient dose rate and individual dose rate at that height, as well as the radioactivity in the soil layer for the detected gamma nuclides from the dose rate spectroscopy. The reliable results could be obtained by introducing the angular correction factor to correct the G-factor with respect to incident photons distributed in a certain range of angles. The intercomparison results of radioactivity using ISOCS software, an analysis of a sample taken from the soil around a detector, and dose rate spectroscopy had a difference of <20% for 214Pb, 214Bi, 228Ac, 212Bi, 208Tl, and 40K, except for 212Pb with low-energy photons, that is, <300 keV. In addition, the drawback of using dose rate spectroscopy, that is, all gamma rays from a nuclide should be identified to accurately assess the individual dose rate, was overcome by adopting the concept of contribution ratio of the key gamma ray to the individual dose rate of a nuclide, so that it could be accurately calculated by identifying only a key gamma ray from a nuclide.

  8. In situ gamma-ray spectrometry: A tutorial for environmental radiation scientists

    SciTech Connect

    Miller, K.M.; Shebell, P.

    1993-10-01

    This tutorial is intended for those in the environmental field who perform assessments in areas where there is radioactive contamination in the surface soil. Techniques will be introduced for performing on-site quantitative measurements of gamma radiation in the environment using high resolution germanium detectors. A basic understanding of ionizing radiation principles is assumed; however, a detailed knowledge of gamma spectrometry systems is not required. Emphasized is the practical end of operations in the field and the conversion of measured full absorption peak count rates in a collected spectrum to meaningful radiological quantities, such as the concentration of a radionuclide in the soil, activity per unit area, and dose rate in the air. The theory of operation and calibration procedures will be covered in detail to provide the necessary knowledge to adapt the technique to site-specific problems. Example calculations for detector calibration are also provided.

  9. Radiological Mapping of the Alkaline Intrusive Complex of Jombo, South Coastal Kenya by In-Situ Gamma-Ray Spectrometry

    NASA Astrophysics Data System (ADS)

    Kaniu, Ian; Darby, Iain G.; Kalambuka Angeyo, Hudson

    2016-04-01

    Carbonatites and alkaline intrusive complexes are rich in a variety of mineral deposits such as rare earth elements (REEs), including Nb, Zr and Mn. These are often associated with U and Th bearing minerals, including monazite, samarskite and pyrochlore. Mining waste resulting from mineral processing activities can be highly radioactive and therefore poses a risk to human health and environment. The Jombo complex located in Kenya's south coastal region is potentially one of the richest sources of Nb and REEs in the world. It consists of the main intrusion at Jombo hill, three associated satellite intrusions at Mrima, Kiruku and Nguluku hills, and several dykes. The complex is highly heterogeneous with regard to its geological formation as it is characterized by alkaline igneous rocks and carbonatites which also influence its radio-ecological dynamics. In-situ gamma spectrometry offers a low-cost, rapid and spatially representative radioactivity estimate across a range of landscapes compared to conventional radiometric techniques. In this work, a wide ranging radiological survey was conducted in the Jombo complex as follow up on previous studies[1,2], to determine radiation exposure levels and source distributions, and perform radiological risk assessments. The in-situ measurements were carried out using a 2.0 l NaI(Tl) PGIS-2 portable detector from Pico Envirotec Inc integrated with GPS, deployed for ground (back-pack) and vehicular gamma-ray spectrometry. Preliminary results of radiological distribution and mapping will be presented. [1] Patel, J. P. (1991). Discovery and Innovation, 3(3): 31-35. [2] Kebwaro, J. M. et. al. (2011). J. Phys. Sci., 6(13): 3105-3110.

  10. Spatially-Dependent Measurements of Surface and Near-Surface Radioactive Material Using In situ Gamma Ray Spectrometry (ISGRS) For Final Status Surveys

    SciTech Connect

    J. A. Chapman, A. J. Boerner, E. W. Abelquist

    2006-11-15

    In-situ, high-resolution gamma-ray spectrometry (ISGRS) measurements were conducted at the Oak Ridge Institute for Science and Education (ORISE) field laboratory in Oak Ridge, Tennessee. The purpose of these tests was to provide analytical data for assessing how “fit for use” this technology is for detecting discrete particles in soil.

  11. In-situ ground gamma spectrometry — an effective tool for geological mapping (the Male Karpaty Mts., Slovakia)

    NASA Astrophysics Data System (ADS)

    Mojzeš, Andrej; Porubčanová, Barbara

    2016-06-01

    This contribution presents the results of profile in-situ gamma spectrometry measurements that sought to determine the content of natural radionuclides 40K, 238U and 232Th in a near surface horizon of rocks, their weathering cover and soils in the area of the Malé Karpaty Mts. It is widely established that the exploration of radioactivity of bedrocks and cover rocks can be a very effective and useful tool for both geological mapping, for identifying deposits of mineral resources, and even addressing the issues of structural and tectonic geology. This assertion is equally confirmed by the ground gamma spectrometry measurements carried out as part of this case study on larger scales, seeking more detailed geological structure solutions. The results obtained provide a welcome addition to an already existing database, which monitors the content of naturally occurring radionuclides individually for every rock lithotype of the Western Carpathians, by elaborating on the data collected by previous research and by updating this database for any future needs. The presented results confirmed the low to medium radioactivity levels of rocks and soils in the studied area. The highest values were detected in granitoids and metamorfic phyllitic rocks of the Malé Karpaty Mts. core; the lowest values were detected in carbonates, arenaceous sediments and, above all, amphibolite bodies. In this way, the presented results of the interpreted profile (P5) confirm the model of local geological structure as represented on the most up-to-date edition of the geological map of the Male Karpaty Mts. (Polak et al. 2011).

  12. Survey of the {sup 137}Cs contamination in Belgium by in-situ gamma spectrometry, a decade after the Chernobyl accident

    SciTech Connect

    Uyttenhove, J.; Pomme, S.; Hardenman, F.; Culot, J.P.

    1997-10-01

    The residual radiocesium concentration, nearly 10 y after the Chernobyl accident, is measured at different sites on the Belgian territory by means of in-situ gamma-spectrometry. A possible link between the rainfall at the beginning of May 1986 and the actual cesium concentration is investigated. The radiological impact of this contamination, even in the most affected regions in the Ardennes, is very small (<6 {mu}Sv y{sup -1}). 6 refs., 4 figs., 1 tab.

  13. Assay for uranium and determination of disequilibrium by means of in situ high resolution gamma-ray spectrometry

    USGS Publications Warehouse

    Tanner, Allan B.; Moxham, Robert M.; Senftle, F.E.

    1977-01-01

    Two sealed sondes, using germanium gamma-ray detectors cooled by melting propane, have been field tested to depths of 79 m in water-filled boreholes at the Pawnee Uranium Mine in Bee Co., Texas. When, used as total-count devices, the sondes are comparable in logging speed and counting rate with conventional scintillation detectors for locating zones of high radioactivity. When used with a multichannel analyzer, the sondes are detectors with such high resolution that individual lines from the complex spectra of the uranium and thorium series can be distinguished. Gamma rays from each group of the uranium series can be measured in ore zones permitting determination of the state of equilibrium at each measurement point. Series of 10-minute spectra taken at 0.3- to 0.5-m intervals in several holes showed zones where maxima from the uranium group and from the 222Rn group were displaced relative to each other. Apparent excesses of 230Th at some locations suggest that uranium-group concentrations at those locations were severalfold greater some tens of kiloyears, ago. At the current state of development a 10-minute count yields a sensitivity of about 80 ppm U308. Data reduction could in practice be accomplished in about 5 minutes. The result is practically unaffected by disequilibrium or radon contamination. In comparison with core assay, high-resolution spectrometry samples a larger volume; avoids problems due to incomplete core recovery, loss of friable material to drilling fluids, and errors in depth and marking; and permits use of less expensive drilling methods. Because gamma rays from the radionuclides are accumulated simultaneously, it also avoids the problems inherent in trying to correlate logs made in separate runs with different equipment. Continuous-motion delayed-gamma activation by a 163-?g 252Cf neutron source attached to the sonde yielded poor sensitivity. A better neutron-activation method, in which the sonde is moved in steps so as to place the detector

  14. Validation of in situ and laboratory gamma spectrometry measurements for determination of ²²⁶Ra, ⁴⁰K and ¹³⁷Cs in soil.

    PubMed

    Al-Masri, M S; Doubal, A W

    2013-05-01

    In situ and laboratory gamma spectrometry methods for determination of (226)Ra, (40)K and (137)Cs in soil have been validated and compared. Minimum detectable activity, repeatability, and reproducibility were the main validation parameters. Results have shown that soil humidity lower the in situ measurement results in comparison to laboratory measurements. Measurement uncertainties were also estimated and compared for both techniques. Uncertainty due to soil humidity (55%) using the in situ measurement was the main contributor to the total uncertainty, while the uncertainty due to net counting (71%) using the laboratory measurements was the largest contributor to the total uncertainty value. PMID:23455404

  15. Assessment of natural and anthropogenic radioactivity levels in rocks and soils in the environs of Swieradow Zdroj in Sudetes, Poland, by in situ gamma-ray spectrometry.

    PubMed

    Malczewski, D; Teper, L; Dorda, J

    2004-01-01

    The natural radioactivity of 40K, 208Ti, 212Pb, 214Pb, 228Ac, and the fallout of 137Cs in typical rocks and soils of Swieradów Zdrój area (Sudetes Mountains, Poland) were measured in situ using a portable gamma-ray spectrometry workstation. The measurement points were chosen for different regional lithology: within hornfelses of the Szklarska Poreba schist-belt, quartz rocks, gneisses of the Swieradów Zdrój unit, leucogranites, leptinites, mica schists of the Stara Kamienica belt, and finally the zones of the southern and northern contacts of the Stara Kamienica schist-belt with leucogranites and gneisses of the Lesna unit, respectively. 40K activity varied in the range from about 320 Bq kg(-1) (quartz) to 1200 Bq kg(-1) (gneisses). The activity concentrations associated with 228Ac (232Th series) varied in the range from 25 Bq kg(-1) (quartz) to 62 Bq kg(-1) (leucogranites), whereas activity concentration of 226Ra varied in the range from about 31 Bq kg(-1) (hornfelses) to 122 Bq kg(-1) (leucogranites). Relatively low deposits of 137Cs were noted in the investigated area, where the activity concentrations ranged from 4001 (hornfelses) Bq m(-2) to less than 154 Bq m(-2) (leucogranites). PMID:15050357

  16. In situ secondary ion mass spectrometry analysis

    SciTech Connect

    Groenewold, G.S.; Applehans, A.D.; Ingram, J.C.; Delmore, J.E.; Dahl, D.A.

    1993-01-01

    The direct detection of tributyl phosphate (TBP) on rocks using molecular beam surface analysis [MBSA or in situ secondary ion mass spectrometry (SIMS)] is demonstrated. Quantities as low as 250 ng were detected on basalt and sandstone with little or no sample preparation. Detection of TBP on soil has proven to be more problematic and requires further study. Ethylenediaminetetraacetic acid (EDTA) is more difficult to detect because it is very reactive with surfaces of interest. Nevertheless, it is possible to detect EDTA if the acidity of the surface is controlled. The detection of EDTA-metal complexes is currently an open question, but evidence is presented for the detection of ions arising from a EDTA-lead complex. Carboxylic acids (i.e., citric, ascorbic, malic, succinic, malonic, and oxalic) give characteristic SIM spectra, but their detection on sample surfaces awaits evaluation.

  17. Small Scale Assessment of Spatial and Vertical Redistribution of Fukushima Fallouts Radiocaesium in Contaminated Soil Using in-situ HPGe Gamma Ray Spectrometry

    NASA Astrophysics Data System (ADS)

    Patin, J.; Onda, Y.; Yoda, H.; Kato, H.

    2011-12-01

    After Tohoku earthquake on March 11th 2011, the subsequent tsunami and the resulting Fukushima Daiichi Nuclear Power Plant disaster, gamma emitting particles, first release into the atmosphere, were quickly deposited on the soil surface, with potentially harmful level in the surroundings of the nuclear power plant. Thus, the evaluation of soil deposition pattern, depth migration and afterward radionuclides redistribution and export by erosion and hydrological processes is fundamental for contamination assessments and to plan future actions. Our study site is located 37km from Fukushima power plant, inside the evacuated zone. In this study, we used a bounded erosion plot of 22.1m x 5m to assess global export of sediments and 137Cs. This plot, previously cropped with tobacco, is morphologically divided into inter-rill areas separated by rills that formed into former wheel tracks. The bottom of the plot is subject to deposition of sediments. In order to determine and quantify the internal processes responsible of the export of sediment, the depth distribution of 137Cs is estimated using a portable High Purity Germanium (HPGe) detector. Such a portable device, associated to the high radiation levels, allow an acquisition of spatially distributed data within the plot in a reasonable time (1 min/sample). At the same time, depth distribution of 137Cs are measured using the scrapper plate technique, adapted to obtain a fine resolution in the first, highly contaminated, centimeters of soil. Finally, 137Cs depth profiles, associated with in situ and laboratory gamma spectrums acquired with the portable detector, allow for the detector calibration. Although the initial deposit can reasonably be supposed homogeneous at the plot scale, the dataset obtained 3 months later shows high spatial and temporal variability due to erosion processes. Measurements with the portable HPGe detector proved to be useful at this small scale, avoiding the needs of a large number of soil samples

  18. Spatial mapping of soil and radioactivity redistribution at the hillslope scale using in-situ gamma spectrometry, terrestrial laser scanning and RFID tags after the Fukushima nuclear accident fallout.

    NASA Astrophysics Data System (ADS)

    Patin, Jeremy; Onda, Yuichi; Noguchi, Takehiro; Parsons, Anthony

    2013-04-01

    In March 2011, the Fukushima Daiichi Nuclear Power Plant disaster, triggered by the Tohoku earthquake and the consequent tsunami, released a large amount of radionuclides in the environment. To provide a rapid assessment of the soil contamination and its potential redistribution, intensive scientific monitoring has been conducted since July 2011 in our study site, located in the Yamakiya district of Kawamata town, in Fukushima prefecture, Japan, about 37 km from the power plant. In this paper, we summarize and analyze a dataset combining multiple innovative methods deployed inside a 5m x 22m bounded hillslope plot. In addition to runoff volumes and sediments radiocesium concentrations, each major rainfall event was followed by in situ gamma spectrometry measurements. In 2012, to trace the complex behavior of sediments inside the plot, about 300 RFID (Radio-Frequency IDentification) tags representing coarse sediments were scattered and their spatial position was periodically checked using a total station. Finally, several high resolutions Digital Elevation Models were acquired with a terrestrial laser scanner to assess the surface structure and changes. The observed processes at the event scale include interrill and rill erosion, as well as local deposition and remobilization phenomenon. Not only do they directly provide information on the erosion spatio-temporal variability and the associated radionuclides transfers, but combined together they can constitute a solid basis to improve and challenge process-based distributed erosion models.

  19. In situ secondary ion mass spectrometry analysis. 1992 Summary report

    SciTech Connect

    Groenewold, G.S.; Applehans, A.D.; Ingram, J.C.; Delmore, J.E.; Dahl, D.A.

    1993-01-01

    The direct detection of tributyl phosphate (TBP) on rocks using molecular beam surface analysis [MBSA or in situ secondary ion mass spectrometry (SIMS)] is demonstrated. Quantities as low as 250 ng were detected on basalt and sandstone with little or no sample preparation. Detection of TBP on soil has proven to be more problematic and requires further study. Ethylenediaminetetraacetic acid (EDTA) is more difficult to detect because it is very reactive with surfaces of interest. Nevertheless, it is possible to detect EDTA if the acidity of the surface is controlled. The detection of EDTA-metal complexes is currently an open question, but evidence is presented for the detection of ions arising from a EDTA-lead complex. Carboxylic acids (i.e., citric, ascorbic, malic, succinic, malonic, and oxalic) give characteristic SIM spectra, but their detection on sample surfaces awaits evaluation.

  20. Aerogel dust collection for in situ mass spectrometry analysis

    NASA Astrophysics Data System (ADS)

    Jones, S. M.; Anderson, M. S.; Davies, A. G.; Kirby, J. P.; Burchell, M. J.; Cole, M. J.

    2015-02-01

    The current technique for conducting in situ mass spectroscopic analysis of dust around extraterrestrial bodies is to have the dust impact a solid plate and analyze the atoms and molecular fragments resulting from the high speed impact. Due to the fact that the kinetic energy from the impact is converted primarily to thermal energy, much of the organic compounds present in the dust may be significantly altered or destroyed. To avoid this problem, aerogel could be used to capture the dust grains, largely intact, maintaining the integrity of the organic compounds in the interior of the dust grains. To demonstrate that organic molecules, present as minor components of silica particles, would survive hypervelocity capture in aerogel and can then be analyzed with mass spectrometry, several light gas gun impact tests and analyses were conducted. Fine particles containing polycyclic aromatic hydrocarbons (PAHs) were captured in aerogel at 5.5 km s-1. The flow of metastable helium from a Direct Analysis Real Time (DART) source was used to desorb and ionize the organics, which were then analyzed with a mass spectrometer. The PAHs were detected and identified by the DART-MS, demonstrating that this method could be used on future flight instruments.

  1. Airborne Gamma-Spectrometry in Switzerland

    SciTech Connect

    Butterweck, Gernot; Bucher, Benno; Rybach, Ladislaus

    2008-08-07

    Airborne gamma-spectrometry is able to obtain fast radiological information over large areas. The airborne gamma-spectrometry unit deployed in Switzerland by the Swiss National Emergency Operations Centre (NEOC) consists of a Swiss army Super Puma helicopter equipped with four NaI-Detectors with a total volume of 17 liters, associated electronics and a real-time data evaluation and mapping unit developed by the Swiss Federal Institute of Technology (ETH) and the Paul Scherrer Institut (PSI). The operational readiness of the airborne gamma-spectrometry system is validated in annual exercises of one week duration. Data from 2005 and 2006 exercises are represented in maps of {sup 137}Cs activity concentration for two towns located in southern and western Switzerland. An indicator of man-made radioactivity (MMGC ratio) is demonstrated for an area with four different types of nuclear installations. The intercomparison between airborne gamma-spectrometry and ground measurements showed good agreement between both methods.

  2. Factors influencing in situ gamma-ray measurements

    NASA Astrophysics Data System (ADS)

    Loonstra, E. H.; van Egmond, F. M.

    2009-04-01

    Introduction In situ passive gamma-ray sensors are very well suitable for mapping physical soil properties. In order to make a qualitative sound soil map, high quality input parameters for calibration are required. This paper will focus on the factors that affect the output of in situ passive gamma-ray sensors, the primary source, soil, not taken into account. Factors The gamma-ray spectrum contains information of naturally occurring nuclides 40K, 238U and 232Th and man-made nuclides like 137Cs, as well as the total count rate. Factors that influence the concentration of these nuclides and the count rate can be classified in 3 categories. These are sensor design, environmental conditions and operational circumstances. Sensor design The main elements of an in situ gamma-ray sensor that influence the outcome and quality of the output are the crystal and the spectrum analysis method. Material and size of the crystal determine the energy resolution. Though widely used, NaI crystals are not the most efficient capturer of gamma radiation. Alternatives are BGO and CsI. BGO has a low peak resolution, which prohibits use in cases where man-made nuclides are subject of interest. The material is expensive and prone to temperature instability. CsI is robust compared to NaI and BGO. The density of CsI is higher than NaI, yielding better efficiency, especially for smaller crystal sizes. More volume results in higher energy efficiency. The reduction of the measured spectral information into concentration of radionuclides is mostly done using the Windows analysis method. In Windows, the activities of the nuclides are found by summing the intensities of the spectrum found in a certain interval surrounding a peak. A major flaw of the Windows method is the limited amount of spectral information that is incorporated into the analysis. Another weakness is the inherent use of ‘stripping factors' to account for contributions of radiation from nuclide A into the peak of nuclide B. This

  3. Technology information profile: RL321103 -- In situ gamma spectrometer

    SciTech Connect

    Schilk, A.J.

    1993-11-01

    Past operations of uranium production and support facilities at several Department of Energy (DOE) sites have occasionally resulted in the local contamination of some surface and subsurface soils. Such contamination commonly occurs within waste burial sites, cribs, pond bottom sediments, and areas surrounding waste tanks or uranium scrap, ore, tailing, and slag heaps. The thorough cleanup of these sites is a major public concern and a high priority for the DOE, but before any effective remedial protocols can be established, the three-dimensional distributions of the uranium contaminants must be adequately characterized. Unfortunately, traditional means of obtaining soil activities (e.g., grab sampling followed by laboratory analyses) are notoriously cumbersome, expensive, time-consuming, and often non-representative when very large areas are being surveyed. Hence, new technologies must be developed, or existing ones improved, to allow for the cheaper, better, faster (i.e., real-time) and safer characterization of uranium concentrations at these critical sites. The primary objective for this program is to develop, construct, and field/pilot test the in situ gamma spectrometer for the rapid measurement of uranium in surface and shallow subsurface soils at the Fernald site in Ohio.

  4. Uncertainties in gamma-ray spectrometry

    NASA Astrophysics Data System (ADS)

    Lépy, M. C.; Pearce, A.; Sima, O.

    2015-06-01

    High resolution gamma-ray spectrometry is a well-established metrological technique that can be applied to a large number of photon-emitting radionuclides, activity levels and sample shapes and compositions. Three kinds of quantitative information can be derived using this technique: detection efficiency calibration, radionuclide activity and photon emission intensities. In contrast to other radionuclide measurement techniques gamma-ray spectrometry provides unambiguous identification of gamma-ray emitting radionuclides in addition to activity values. This extra information comes at a cost of increased complexity and inherently higher uncertainties when compared with other secondary techniques. The relative combined standard uncertainty associated with any result obtained by gamma-ray spectrometry depends not only on the uncertainties of the main input parameters but also on different correction factors. To reduce the uncertainties, the experimental conditions must be optimized in terms of the signal processing electronics and the physical parameters of the measured sample should be accurately characterized. Measurement results and detailed examination of the associated uncertainties are presented with a specific focus on the efficiency calibration, peak area determination and correction factors. It must be noted that some of the input values used in quantitative analysis calculation can be correlated, which should be taken into account in fitting procedures or calculation of the uncertainties associated with quantitative results. It is shown that relative combined standard uncertainties are rarely lower than 1% in gamma-ray spectrometry measurements.

  5. Neutral beam species measurements using in situ Rutherford backscatter spectrometry

    SciTech Connect

    Kugel, H.W.; Kaita, R.; Gammel, G.; Williams, M.D.

    1984-12-01

    This work describes a new in situ method for measuring the neutral particle fractions in high power deuterium neutral beams, used to heat magnetically confined fusion plasmas. Deuterium beams, of variable energies, pulse lengths, and powers up to 47 keV, 100 msec, 1.6 MW, were Rutherford backscattered at 135/sup 0/ from TiC inner neutral beam armor of the PDX, and detected using an electrostatic analyzer with microchannel plates. Complete energy scans were made every 20 msec and data were obtained simultaneously from five different positions across the beam profile. The neutral particle fractions were measured to be D/sup 0/(E):D/sup 0/(E/2):D/sup 0/(E/3)=53:32:15. The corresponding neutral power fractions were P/sup 0/(E):P/sup 0/(E/2):P/sup 0/(E/3)=72:21:7, and the associated ionic fractions at the output of the ion source were D/sub 1//sup +/(E):D/sub 2//sup +/(E):D/sub 3//sup +/(E)=74:20:6. The measured neutral particle fractions were relatively constant over more than 70% of the beam power distribution. A decrease in the yield of the full energy component in the outer regions of the beam was observed. Other possible experimental configurations and geometries are discussed.

  6. Monitoring genetic and metabolic potential for in situ bioremediation: Mass spectrometry. 1997 annual progress report

    SciTech Connect

    Buchanan, M.V.; Hurst, G.B.; Britt, P.F.; McLuckey, S.A.; Doktycz, M.J.

    1997-09-01

    'A number of US Department of Energy (DOE) sites are contaminated with mixtures of dense non-aqueous phase liquids (DNAPLs) such as carbon tetrachloride, chloroform,. perchloroethylene, and trichloroethylene. At many of these sites, in situ microbial bioremediation is an attractive strategy for cleanup because it has the potential to degrade DNAPLs in situ without producing toxic byproducts. A rapid screening method to determine the broad range metabolic and genetic potential for contaminant degradation would greatly reduce the cost and time involved in assessment for in situ bioremediation as well as for monitoring ongoing bioremediation treatment. In this project, the ORNL Organic Mass Spectrometry (OMS) group is developing mass-spectrometry-based methods to screen for the genetic and metabolic potential for assessment and monitoring of in situ bioremediation of DNAPLs. In close collaboration, Professor Mary Lidstrom''s group at the University of Washington is identifying short DNA sequences related to microbial processes involved in the biodegradation of pollutants. This work will lay the foundation for development of a field-portable mass-spectrometry-based technique for rapid assessment and monitoring of bioremediation processes on site.'

  7. Review of in situ derivatization techniques for enhanced bioanalysis using liquid chromatography with mass spectrometry.

    PubMed

    Baghdady, Yehia Z; Schug, Kevin A

    2016-01-01

    Accurate and specific analysis of target molecules in complex biological matrices remains a significant challenge, especially when ultra-trace detection limits are required. Liquid chromatography with mass spectrometry is often the method of choice for bioanalysis. Conventional sample preparation and clean-up methods prior to the analysis of biological fluids such as liquid-liquid extraction, solid-phase extraction, or protein precipitation are time-consuming, tedious, and can negatively affect target recovery and detection sensitivity. An alternative or complementary strategy is the use of an off-line or on-line in situ derivatization technique. In situ derivatization can be incorporated to directly derivatize target analytes in their native biological matrices, without any prior sample clean-up methods, to substitute or even enhance the extraction and preconcentration efficiency of these traditional sample preparation methods. Designed appropriately, it can reduce the number of sample preparation steps necessary prior to analysis. Moreover, in situ derivatization can be used to enhance the performance of the developed liquid chromatography with mass spectrometry-based bioanalysis methods regarding stability, chromatographic separation, selectivity, and ionization efficiency. This review presents an overview of the commonly used in situ derivatization techniques coupled to liquid chromatography with mass spectrometry-based bioanalysis to guide and to stimulate future research. PMID:26496130

  8. In-situ gamma-analysis support for Phase I, Middlesex cleanup project, Middlesex, New Jersey

    SciTech Connect

    Reiman, R.T.

    1983-07-01

    At the request of the Department of Energy, the Energy Measurements Group of EG and G participated in the Remedial Action program for the former Middlesex Sampling Plant and associated properties at Middlesex, New Jersey from July to November 1980. EG and G provided real time analysis of the radiological character of the soil of each property included in the Phase I cleanup before, during, and after decontamination. The method used for the analysis was in situ gamma spectroscopy employing a high purity germanium detector. This report describes the in situ system and displays the results of the in situ measurements before and after decontamination of the properties surveyed during Phase I.

  9. Advanced capabilities for in situ planetary mass spectrometry

    NASA Astrophysics Data System (ADS)

    Arevalo, R. D., Jr.; Mahaffy, P. R.; Brinckerhoff, W. B.; Getty, S.; Benna, M.; van Amerom, F. H. W.; Danell, R.; Pinnick, V. T.; Li, X.; Grubisic, A.; Cornish, T.; Hovmand, L.

    2015-12-01

    NASA GSFC has delivered highly capable quadrupole mass spectrometers (QMS) for missions to Venus (Pioneer Venus), Jupiter (Galileo), Saturn/Titan (Cassini-Huygens), Mars (MSL and MAVEN), and the Moon (LADEE). Our understanding of the Solar System has been expanded significantly by these exceedingly versatile yet low risk and cost efficient instruments. GSFC has developed more recently a suite of advanced instrument technologies promising enhanced science return while selectively leveraging heritage designs. Relying on a traditional precision QMS, the Analysis of Gas Evolved from Samples (AGES) instrument measures organic inventory, determines exposure age and establishes the absolute timing of deposition/petrogenesis of interrogated samples. The Mars Organic Molecule Analyzer (MOMA) aboard the ExoMars 2018 rover employs a two-dimensional ion trap, built analogously to heritage QMS rod assemblies, which can support dual ionization sources, selective ion enrichment and tandem mass spectrometry (MS/MS). The same miniaturized analyzer serves as the core of the Linear Ion Trap Mass Spectrometer (LITMS) instrument, which offers negative ion detection (switchable polarity) and an extended mass range (>2000 Da). Time-of-flight mass spectrometers (TOF-MS) have been interfaced to a range of laser sources to progress high-sensitivity laser ablation and desorption methods for analysis of inorganic and non-volatile organic compounds, respectively. The L2MS (two-step laser mass spectrometer) enables the desorption of neutrals and/or prompt ionization at IR (1.0 up to 3.1 µm, with an option for tunability) or UV wavelengths (commonly 266 or 355 nm). For the selective ionization of specific classes of organics, such as aromatic hydrocarbons, a second UV laser may be employed to decouple the desorption and ionization steps and limit molecular fragmentation. Mass analyzers with substantially higher resolving powers (up to m/Δm > 100,000), such as the Advanced Resolution Organic

  10. Comparison of in situ and laboratory gamma spectroscopy of natural radionuclides in desert soil.

    PubMed

    Benke, R R; Kearfott, K J

    1997-08-01

    In situ and laboratory gamma spectroscopy were used to characterize natural background levels of radiation in the soil at eight sites around the Yucca Mountain Range. The purpose of this practical field analysis was to determine if published empirical in situ calibration factors would yield accurate quantitative specific activities (Bq kg(-1)) in a desert environment. Corrections were made to the in situ calibration factors to account for the on-axis response of a detector with a thin beryllium end window. The in situ gamma spectroscopy results were compared to laboratory gamma spectroscopy of soil samples gathered from each site. Five natural radionuclides were considered: 40K, 214Pb, 214Bi, 208Tl, and 228Ac. The in situ determined specific activities were consistently within +/-15% of the laboratory soil sample results. A quantitative discussion of the factors contributing to the uncertainty in the in situ and laboratory results is included. Analysis on the specific activity data using statistical hypothesis tests determined that three nuclides, 214Pb, 214Bi, and 228Ac showed a weak site dependence while the other two nuclides, 40K and 208Tl, did not exhibit a site dependence. Differing radiation background levels from site to site along with in situ and laboratory uncertainties in excess of 10% are two factors that account for the weak site dependence. Despite the good correlation between data, it was recommended that the in situ detector be calibrated by a detector-specific Monte Carlo code which would accurately model more complex geometries and source distributions. PMID:9228170

  11. Mass Spectrometry Guided In Situ Proteolysis to Obtain Crystals for X-ray Structure Determination

    SciTech Connect

    Gheyi, Tarun; Rodgers, Logan; Romero, Richard; Sauder, J. Michael; Burley, Stephen K.

    2012-04-30

    A strategy for increasing the efficiency of protein crystallization/structure determination with mass spectrometry has been developed. This approach combines insights from limited proteolysis/mass spectrometry and crystallization via in situ proteolysis. The procedure seeks to identify protease-resistant polypeptide chain segments from purified proteins on the time-scale of crystal formation, and subsequently crystallizing the target protein in the presence of the optimal protease at the right relative concentration. We report our experience with 10 proteins of unknown structure, two of which yielded high-resolution X-ray structures. The advantage of this approach comes from its ability to select only those structure determination candidates that are likely to benefit from application of in situ proteolysis, using conditions most likely to result in formation of a stable proteolytic digestion product suitable for crystallization.

  12. EML Gamma Spectrometry Data Evaluation Program

    SciTech Connect

    Decker, Karin M.

    2001-01-01

    This report presents the results of the analyses for the third EML Gamma Spectrometry Data Evaluation Program (October 1999). This program assists laboratories in providing more accurate gamma spectra analysis results and provides a means for users of gamma data to assess how a laboratory performed on various types of gamma spectrometry analyses. This is accomplished through the use of synthetic gamma spectra. A calibration spectrum, a background spectrum, and three sample spectra are sent to each participant in the spectral file format requested by the laboratory. The calibration spectrum contains nuclides covering the energy range from 59.5 keV to 1836 keV. The participants are told fallout and fission product nuclides could be present. The sample spectra are designed to test the ability of the software and user to properly resolve multiplets and to identify and quantify nuclides in a complicated fission product spectrum. The participants were asked to report values and uncertainties as Becquerel per sample with no decay correction. Thirty-one sets of results were reported from a total of 60 laboratories who received the spectra. Six foreign laboratories participated. The percentage of the results within 1 of the expected value was 68, 33, and 46 for samples 1, 2, and 3, respectively. From all three samples, 18% of the results were more than 3 from the expected value. Eighty-three (12%) values out of a total of 682 expected results were not reported for the three samples. Approximately 30% of these false negatives were due the laboratories not reporting 144Pr in sample 2 which was present at the minimum detectable activity level. There were 53 false positives reported with 25% of these responses due to problems with background subtraction. The results show improvement in the ability of the software or user to resolve peaks separated by 1 keV. Improvement is still needed either in the analysis report produced by the software or in the review of these

  13. Parametric Studies for 233U Gamma Spectrometry

    SciTech Connect

    Scheffing, C.C.; Krichinsky, A.

    2004-01-01

    Quantification of special nuclear material is a necessary aspect to assuring material accountability and is often accomplished using non-destructive gamma spectrometry. For 233U, gamma rays are affected by matrix and packaging attenuation and by a strong Compton continuum from decay products of 232U (inherently found in 233U) that obscure 233U gamma photopeaks. This project, based on current work at the national repository for separated 233U located at Oak Ridge National Laboratory (ORNL), explores the effects of various parameters on the quantification of 233U– including material form and geometry. Using an attenuation correction methodology for calculating the mass of 233U from NDA analysis, a bias of almost 75% less than the actual 233U mass was identified. The source of the bias needs to be understood at a more fundamental level for further use of this quantification method. Therefore, controlled experiments using well characterized packages of 233U were conducted at the repository and are presented in this paper.

  14. Planetary Geochemistry Techniques: Probing In-Situ with Neutron and Gamma Rays (PING) Instrument

    NASA Technical Reports Server (NTRS)

    Parsons, A.; Bodnarik, J.; Burger, D.; Evans, L.; Floyd, S.; Lin, L.; McClanahan, T.; Nankung, M.; Nowicki, S.; Schweitzer, J.; Starr, R.; Trombka, J.

    2011-01-01

    The Probing In situ with Neutrons and Gamma rays (PING) instrument is a promising planetary science application of the active neutron-gamma ray technology so successfully used in oil field well logging and mineral exploration on Earth. The objective of our technology development program at NASA Goddard Space Flight Center's (NASA/GSFC) Astrochemistry Laboratory is to extend the application of neutron interrogation techniques to landed in situ planetary composition measurements by using a 14 MeV Pulsed Neutron Generator (PNG) combined with neutron and gamma ray detectors, to probe the surface and subsurface of planetary bodies without the need to drill. We are thus working to bring the PING instrument to the point where it can be flown on a variety of surface lander or rover missions to the Moon, Mars, Venus, asteroids, comets and the satellites of the outer planets.

  15. Application of PERALS™ alpha spectrometry and gamma spectrometry for analysis and investigation of environmental spills at ISL uranium mining projects.

    PubMed

    Borysenko, A; Ostrowski, A; Bellifemine, D; Palmer, G; Haigh, P; Johnston, A

    2014-03-01

    Radiation protection and environmental monitoring in mining requires effective and reliable radionuclide analysis at all stages of the mine project-prior to mining, during operation and through to remediation and decommissioning. The approach presented in this paper was specially developed for the monitoring of radioactive waste resulting from spills during mining and mineral processing operations and uses a combination of high resolution gamma spectrometry, and PERALS™ alpha spectrometry to identify and reliably quantify the activity of the major members of the U-238 decay chain at activities down to 10 mBq g(-1) by direct radionuclide counting and by assessment of the activity of their decay products. This approach has reduced sample preparation and analysis time while providing effective analysis and quantification of naturally occurring radionuclides in environmental samples. It has been successfully applied to several in situ leach (ISL) mining-related projects involving investigations of process material spill impacts and also to routine environmental monitoring. PMID:24270399

  16. In situ measurements of the sub-surface gamma dose from Chernobyl fallout.

    PubMed

    Timms, D N; Smith, J T; Coe, E; Kudelsky, A V; Yankov, A I

    2005-06-01

    Methods of estimating external radiation exposure of soil-dwelling organisms are currently of much research and regulatory interest. In this paper, we report the first in situ measurements of the sub-surface gamma dose rate for 137Cs contaminated land that quantify variation in dose rate with depth. Two contrasting sites have been investigated. The first site comprised a mineral type soil with a low percentage of organic matter and the second site chosen was in a peat-bog. The different soil compositions afford different 137Cs mobility and this results in variations in the measured gamma dose-rate with soil depth. For each site the paper reports the measured dose rates, the 137Cs activity depth profile, the 137Cs inventory and a description of the soil-characteristics. It is suggested that these data can be used to produce estimates of the sub-surface gamma dose rate in other sites of 137Cs contamination. PMID:15799871

  17. In situ XRF and gamma ray spectrometer for Mars sample return mission

    NASA Technical Reports Server (NTRS)

    Lo, I. Yin; Trombka, Jacob I.; Evans, Larry G.; Squyres, Steven W.

    1988-01-01

    A combined in situ X-ray fluorescence (XRF) and passive gamma ray spectrometer instrument is proposed for the chemical elemental analysis of various Martian surfaces and samples. The combined instrument can be carried on board a rover. The passive gamma ray or the neutron excited gamma ray system would be used to determine the elemental composition of the Martian surface while the rover is in motion. The XRF system would be used to perform analysis either on the Martian surface or on collected samples when the rover is stationary. The latter function is important both in cataloging the collected samples and in the selection of samples to be returned to earth. For both systems, data accumulation time would be on the order of 30 minutes. No sample preparation would be necessary.

  18. EML Gamma Spectrometry Data Evaluation Program

    SciTech Connect

    Decker, Karin M.

    1998-02-28

    This report represents the results of the analyses for the second EML Gamma Spectrometry Data Evaluation Program (August 1997). A calibration spectrum, a background spectrum and three sample spectra were included for each software format as part of the evaluation. The calibration spectrum contained nuclides covering the range from 59.5 keV to 1836 keV. The participants were told fallout and fission product nuclides as well as naturally occurring nuclides could be present. The samples were designed to test the detection and quantification of very low levels of nuclides and the ability of the software and user to properly resolve multiplets. The participants were asked to report values and uncertainties as Becquerel per sample with no decay correction. Twenty-nine sets of results were reported from a total of 70 laboratories who received the spectra. The percentage of the results within 1 F of the expected value was 76, 67, and 55 for samples 1, 2, and 3, respectively. From all three samples, 12% of the results were more than 3 F from the expected value. Sixty-two nuclides out of a total of 580 expected results were not reported for the three samples. Sixty percent of these false negatives were due to nuclides which were present at the minimum detectable activity level. There were 53 false positives reported with 60% of the responses due to problems with background subtraction. The results indicate that the Program is beneficial to the participating laboratories in that it provides them with analysis problems that are difficult to create with spiked samples due to the unavailability of many nuclides and the short half-lives of others. EML will continue its annual distribution, the third is to be held in March 1999.

  19. In situ capture gamma-ray analysis of coal in an oversize borehole

    USGS Publications Warehouse

    Mikesell, J.L.; Dotson, D.W.; Senftle, F.E.; Zych, R.S.; Koger, J.; Goldman, L.

    1983-01-01

    In situ capture gamma-ray analysis in a coal seam using a high resolution gamma-ray spectrometer in a close-fitting borehole has been reported previously. In order to check the accuracy of the method under adverse conditions, similar measurements were made by means of a small-diameter sonde in an oversize borehole in the Pittsburgh seam, Greene County, Pennsylvania. The hole was 5 times the diameter of the sonde, a ratio that substantially increased the contribution of water (hydrogen) to the total spectral count and reduced the size of the sample measured by the detector. The total natural count, the 40K,count, and the intensities of capture gamma rays from Si, Ca, H, and Al were determined as a function of depth above, through, and below the coal seam. From these logs, the depth and width of the coal seam and its partings were determined. Spectra were accumulated in the seam for 1 h periods by using neutron sources of different strengths. From the spectra obtained by means of several 252Cf neutron sources of different sizes, the ultimate elemental analysis and ash content were determined. The results were not as good as those obtained previously in a close-fitting borehole. However, the results did improve with successively larger source-to-detector distances, i.e.,as the count contribution due to hydrogen in the water decreased. It was concluded that in situ borehole analyses should be made in relatively close-fitting boreholes. ?? 1983.

  20. Active Neutron and Gamma-Ray Instrumentation for In Situ Planetary Science Applications

    NASA Technical Reports Server (NTRS)

    Parsons, A.; Bodnarik, J.; Evans, L.; Floyd, A.; Lim, L.; McClanahan, T.; Namkung, M.; Nowicki, S.; Schweitzer, J.; Starr, R.; Trombka, J.

    2011-01-01

    We describe the development of an instrument capable of detailed in situ bulk geochemical analysis of the surface of planets, moons, asteroids, and comets. This instrument technology uses a pulsed neutron generator to excite the solid materials of a planet and measures the resulting neutron and gamma-ray emission with its detector system. These time-resolved neutron and gamma-ray data provide detailed information about the bulk elemental composition, chemical context, and density distribution of the soil within 50 cm of the surface. While active neutron scattering and neutron-induced gamma-ray techniques have been used extensively for terrestrial nuclear well logging applications, our goal is to apply these techniques to surface instruments for use on any solid solar system body. As described, experiments at NASA Goddard Space Flight Center use a prototype neutron-induced gamma-ray instrument and the resulting data presented show the promise of this technique for becoming a versatile, robust, workhorse technology for planetary science, and exploration of any of the solid bodies in the solar system. The detection of neutrons at the surface also provides useful information about the material. This paper focuses on the data provided by the gamma-ray detector.

  1. Matrix-Assisted Laser Desorption Ionization Imaging Mass Spectrometry: In Situ Molecular Mapping

    PubMed Central

    Angel, Peggi M.; Caprioli, Richard M.

    2013-01-01

    Matrix-assisted laser desorption ionization imaging mass spectrometry (IMS) is a relatively new imaging modality that allows mapping of a wide range of biomolecules within a thin tissue section. The technology uses a laser beam to directly desorb and ionize molecules from discrete locations on the tissue that are subsequently recorded in a mass spectrometer. IMS is distinguished by the ability to directly measure molecules in situ ranging from small metabolites to proteins, reporting hundreds to thousands of expression patterns from a single imaging experiment. This article reviews recent advances in IMS technology, applications, and experimental strategies that allow it to significantly aid in the discovery and understanding of molecular processes in biological and clinical samples. PMID:23259809

  2. Laser Time-of-Flight Mass Spectrometry for Future In Situ Planetary Missions

    NASA Technical Reports Server (NTRS)

    Getty, S. A.; Brinckerhoff, W. B.; Cornish, T.; Ecelberger, S. A.; Li, X.; Floyd, M. A. Merrill; Chanover, N.; Uckert, K.; Voelz, D.; Xiao, X.; Tawalbeh, R.; Glenar, D.; Elsila, J. E.; Callahan, M.

    2012-01-01

    Laser desorption/ionization time-of-flight mass spectrometry (LD-TOF-MS) is a versatile, low-complexity instrument class that holds significant promise for future landed in situ planetary missions that emphasize compositional analysis of surface materials. Here we describe a 5kg-class instrument that is capable of detecting and analyzing a variety of analytes directly from rock or ice samples. Through laboratory studies of a suite of representative samples, we show that detection and analysis of key mineral composition, small organics, and particularly, higher molecular weight organics are well suited to this instrument design. A mass range exceeding 100,000 Da has recently been demonstrated. We describe recent efforts in instrument prototype development and future directions that will enhance our analytical capabilities targeting organic mixtures on primitive and icy bodies. We present results on a series of standards, simulated mixtures, and meteoritic samples.

  3. The Probing In-Situ With Neutron and Gamma Rays (PING) Instrument for Planetary Composition Measurements

    NASA Technical Reports Server (NTRS)

    Parsons, A.; Bodnarik, J.; Evans, L.; McClanahan, T.; Namkung, M.; Nowicki, S.; Schweitzer, J.; Starr, R.

    2012-01-01

    The Probing In situ with Neutrons and Gamma rays (PING) instrument (formerly named PNG-GRAND) [I] experiment is an innovative application of the active neutron-gamma ray technology successfully used in oil field well logging and mineral exploration on Earth over many decades. The objective of our active neutron-gamma ray technology program at NASA Goddard Space Flight Center (NASA/GSFC) is to bring PING to the point where it can be flown on a variety of surface lander or rover missions to the Moon, Mars, Venus, asteroids, comets and the satellites of the outer planets and measure their bulk surface and subsurface elemental composition without the need to drill into the surface. Gamma-Ray Spectrometers (GRS) have been incorporated into numerous orbital planetary science missions. While orbital measurements can map a planet, they have low spatial and elemental sensitivity due to the low surface gamma ray emission rates reSUlting from using cosmic rays as an excitation source, PING overcomes this limitation in situ by incorporating a powerful neutron excitation source that permits significantly higher elemental sensitivity elemental composition measurements. PING combines a 14 MeV deuterium-tritium Pulsed Neutron Generator (PNG) with a gamma ray spectrometer and two neutron detectors to produce a landed instrument that can determine the elemental composition of a planet down to 30 - 50 cm below the planet's surface, The penetrating nature of .5 - 10 MeV gamma rays and 14 MeV neutrons allows such sub-surface composition measurements to be made without the need to drill into or otherwise disturb the planetary surface, thus greatly simplifying the lander design, We are cun'ently testing a PING prototype at a unique outdoor neutron instrumentation test facility at NASA/GSFC that provides two large (1.8 m x 1.8 m x ,9 m) granite and basalt test formations placed outdoors in an empty field, Since an independent trace elemental analysis has been performed on both these

  4. Extractive electrospray ionization mass spectrometry toward in situ analysis without sample pretreatment.

    PubMed

    Li, Ming; Hu, Bin; Li, Jianqiang; Chen, Rong; Zhang, Xie; Chen, Huanwen

    2009-09-15

    A homemade novel nanoextractive electrospray ionization (nanoEESI) source has been characterized for in situ mass spectrometric analysis of ambient samples without sample pretreatment. The primary ions generated using a nanospray emitter interact with the neutral sample plume created by manually nebulizing liquid samples, allowing production of the analyte ions in the spatial cross section of the nanoEESI source. The performance of nanoEESI is experimentally investigated by coupling the nanoEESI source to a commercial LTQ mass spectrometer for rapid analysis of various ambient samples using positive/negative ion detection modes. Compounds of interest in actual samples such as aerosol drug preparations, beverages, milk suspensions, farmland water, and groundwater were unambiguously detected using tandem nanoEESI ion trap mass spectrometry. The limit of detection was low picogram per milliliter levels for the compounds tested. Acceptable relative standard deviation (RSD) values (5-10%) were obtained for direct measurement of analytes in complex matrixes, providing linear dynamic signal responses using manual sample introduction. A single sample analysis was completed within 1.2 s. Requiring no sheath gas for either primary ion production or neutral sample introduction, the nanoEESI has advantages including readiness for miniaturization and integration, simple maintenance, easy operation, and low cost. The experimental data demonstrate that the nanoEESI is a promising tool for high-throughput, sensitive, quantitative, in situ analysis of ambient complex samples, showing potential applications for in situ analysis in multiple disciplines including but not limited to pharmaceutical analysis, food quality control, pesticides residue detection, and homeland security. PMID:19673501

  5. MALDI Mass Spectrometry Imaging for Visualizing In Situ Metabolism of Endogenous Metabolites and Dietary Phytochemicals

    PubMed Central

    Fujimura, Yoshinori; Miura, Daisuke

    2014-01-01

    Understanding the spatial distribution of bioactive small molecules is indispensable for elucidating their biological or pharmaceutical roles. Mass spectrometry imaging (MSI) enables determination of the distribution of ionizable molecules present in tissue sections of whole-body or single heterogeneous organ samples by direct ionization and detection. This emerging technique is now widely used for in situ label-free molecular imaging of endogenous or exogenous small molecules. MSI allows the simultaneous visualization of many types of molecules including a parent molecule and its metabolites. Thus, MSI has received much attention as a potential tool for pathological analysis, understanding pharmaceutical mechanisms, and biomarker discovery. On the other hand, several issues regarding the technical limitations of MSI are as of yet still unresolved. In this review, we describe the capabilities of the latest matrix-assisted laser desorption/ionization (MALDI)-MSI technology for visualizing in situ metabolism of endogenous metabolites or dietary phytochemicals (food factors), and also discuss the technical problems and new challenges, including MALDI matrix selection and metabolite identification, that need to be addressed for effective and widespread application of MSI in the diverse fields of biological, biomedical, and nutraceutical (food functionality) research. PMID:24957029

  6. In-situ gamma-PHA measurements to support unconditional release of 235-F chiller units

    SciTech Connect

    Salaymeh, S.R.

    2000-02-17

    The Analytical Development Section of Savannah River Technology Center (SRTC) was requested by the Facility Decommission Division (FDD) to conduct in-situ gamma-ray pulse height analysis measurements to support the unconditional release of 235-F chiller units. The chiller units were used to cool process water in the 235-F facility. The measurements' main goal is to confirm that there is no process-related contaminants present on the chillers. For each of the two F-area clean water chillers, the authors have acquired ten gamma-ray pulse height analysis spectra. This report will discuss the purpose of the measurements, the experimental setup, data acquisition, calculations and results, and a conclusion of the study.

  7. Laser-based mass spectrometry for in situ chemical composition analysis of planetary surfaces

    NASA Astrophysics Data System (ADS)

    Frey, Samira; Neuland, Maike B.; Grimaudo, Valentine; Moreno-García, Pavel; Riedo, Andreas; Tulej, Marek; Broekmann, Peter; Wurz, Peter

    2016-04-01

    Mass spectrometry is an important analytical technique in space research. The chemical composition of planetary surface material is a key scientific question on every space mission to a planet, moon or asteroid. Chemical composition measurements of rocky material on the surface are of great importance to understand the origin and evolution of the planetary body.[1] A miniature laser ablation/ionisation reflectron- type time-of-flight mass spectrometer (instrument name LMS) was designed and built at the University of Bern for planetary research.[2] Despite its small size and light weight, the LMS instrument still maintains the same capabilities as large laboratory systems, which makes it suitable for its application on planetary space missions.[3-5] The high dynamic range of about eight orders of magnitude, high lateral (μm-level) and vertical (sub-nm level) resolution and high detection sensitivity for almost all elements (10 ppb, atomic fraction) make LMS a versatile instrument for various applications. LMS is a suitable instrument for in situ measurements of elemental and isotope composition with high precision and accuracy. Measurements of Pb- isotope abundances can be used for dating of planetary material. Measurements of bio-relevant elements allow searching for past or present life on a planetary surface. The high spatial resolution, both in lateral and vertical direction, is of considerable interest, e.g. for analysis of inhomogeneous, extraterrestrial samples as well as weathering processes of planetary material. References [1] P. Wurz, D. Abplanalp, M. Tulej, M. Iakovleva, V.A. Fernandes, A. Chumikov, and G. Managadze, "Mass Spectrometric Analysis in Planetary Science: Investigation of the Surface and the Atmosphere", Sol. Sys. Res., 2012, 46, 408. [2] U. Rohner, J.A. Whitby, P. Wurz, "A miniature laser ablation time of flight mass spectrometer for in situ planetary exploration" Meas. Sci. Tch., 2003, 14, 2159. [3] M. Tulej, A. Riedo, M.B. Neuland, S

  8. Monitoring Genetic and Metabolic Potential for in situ Bioremediation: Mass Spectrometry

    SciTech Connect

    Buchanan, Michelle V.

    2000-12-31

    A number of DOE sites are contaminated with mixtures of dense non-aqueous phase liquids (DNAPLs) such as carbon tetrachloride, chloroform, perchloroethylene, and trichloroethylene. At many of these sites, in situ microbial bioremediation is an attractive strategy for cleanup, since it has the potential to degrade DNAPLs in situ without the need for pump-and-treat or soil removal procedures, and without producing toxic byproducts. A rapid screening method to determine broad range metabolic and genetic potential for contaminant degradation would greatly reduce the cost and time involved in assessment for in situ bioremediation, as well as for monitoring ongoing bioremediation treatment. The objective of this project was the development of mass-spectrometry-based methods to screen for genetic potential for both assessment and monitoring of in situ bioremediation of DNAPLs. These methods were designed to provide more robust and routine methods for DNA based characterization of th e genetic potential of subsurface microbes for degrading pollutants. Specifically, we sought to (1) Develop gene probes that yield information equivalent to conventional probes, but in a smaller size that is more amenable to mass spectrometric detection, (2) Pursue improvements to matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) methodology in order to allow its more general application to gene probe detection, (3) Increase the throughput of microbial characterization by integrating gene probe preparation, purification, and MALDI-MS analysis. Effective decision-making regarding remediation strategies requires information on the contaminants present and the relevant hydrogeology. However, it also should include information on the relevant bacterial populations present and the biodegradative processes they carry out. For each site at which bioremediation is considered, it is necessary to determine whether sufficient intrinsic degradative capability is present to suggest

  9. Time-resolved Neutron-gamma-ray Data Acquisition for in Situ Subsurface Planetary Geochemistry

    NASA Technical Reports Server (NTRS)

    Bodnarik, Julie G.; Burger, Dan Michael; Burger, A.; Evans, L. G.; Parsons, A. M.; Schweitzer, J. S.; Starr R. D.; Stassun, K. G.

    2013-01-01

    The current gamma-ray/neutron instrumentation development effort at NASA Goddard Space Flight Center aims to extend the use of active pulsed neutron interrogation techniques to probe the subsurface elemental composition of planetary bodies in situ. Previous NASA planetary science missions, that used neutron and/or gamma-ray spectroscopy instruments, have relied on neutrons produced from galactic cosmic rays. One of the distinguishing features of this effort is the inclusion of a high intensity 14.1 MeV pulsed neutron generator synchronized with a custom data acquisition system to time each event relative to the pulse. With usually only one opportunity to collect data, it is difficult to set a priori time-gating windows to obtain the best possible results. Acquiring time-tagged, event-by-event data from nuclear induced reactions provides raw data sets containing channel/energy, and event time for each gamma ray or neutron detected. The resulting data set can be plotted as a function of time or energy using optimized analysis windows after the data are acquired. Time windows can now be chosen to produce energy spectra that yield the most statistically significant and accurate elemental composition results that can be derived from the complete data set. The advantages of post-processing gamma-ray time-tagged event-by-event data in experimental tests using our prototype instrument will be demonstrated.

  10. Time-resolved neutron/gamma-ray data acquisition for in situ subsurface planetary geochemistry

    NASA Astrophysics Data System (ADS)

    Bodnarik, J. G.; Burger, D. M.; Burger, A.; Evans, L. G.; Parsons, A. M.; Schweitzer, J. S.; Starr, R. D.; Stassun, K. G.

    2013-04-01

    The current gamma-ray/neutron instrumentation development effort at NASA Goddard Space Flight Center aims to extend the use of active pulsed neutron interrogation techniques to probe the subsurface elemental composition of planetary bodies in situ. Previous NASA planetary science missions, that used neutron and/or gamma-ray spectroscopy instruments, have relied on neutrons produced from galactic cosmic rays. One of the distinguishing features of this effort is the inclusion of a high intensity 14.1 MeV pulsed neutron generator synchronized with a custom data acquisition system to time each event relative to the pulse. With usually only one opportunity to collect data, it is difficult to set a priori time-gating windows to obtain the best possible results. Acquiring time-tagged, event-by-event data from nuclear induced reactions provides raw data sets containing channel/energy, and event time for each gamma ray or neutron detected. The resulting data set can be plotted as a function of time or energy using optimized analysis windows after the data are acquired. Time windows can now be chosen to produce energy spectra that yield the most statistically significant and accurate elemental composition results that can be derived from the complete data set. The advantages of post-processing gamma-ray time-tagged event-by-event data in experimental tests using our prototype instrument will be demonstrated.

  11. Calibration of a field-portable gamma detector to obtain in situ measurements of the 137Cs inventories of cultivated soils and floodplain sediments.

    PubMed

    He, Q; Walling, D E

    2000-04-01

    Over the past 10 years, a number of studies have exploited the potential for using measurements of fallout 137Cs inventories to document rates and patterns of soil erosion on cultivated land and to estimate rates of overbank sedimentation on river floodplains. Traditional procedures for applying the 137Cs technique involve the collection of soil or sediment cores from a study site and their subsequent transfer to the laboratory for preparation and analysis by gamma spectrometry. Such procedures are time consuming and there may be a considerable delay before the results are available. It is therefore difficult to obtain preliminary results, which could be used to guide the development of an ongoing sampling programme. The use of in situ gamma spectrometry measurements to quantify 137Cs inventories in soils and sediments offers a number of potential advantages over traditional procedures. However, in order to derive a reliable estimate of the 137Cs inventory for a measurement point, it is necessary to take account of the attenuation of 137Cs gamma rays by the soil matrix and information on the depth distribution of 137Cs in the soil or sediment is therefore required. In the present study, empirical relationships between in situ measurements of 137Cs activity and total 137Cs inventories have been established for soils from a cultivated field and for floodplain sediments, based on information on the vertical distribution of 137Cs in the soils and sediments provided by the forward scattering ratio derived from the field measured spectra. These relationships have been used to estimate 137Cs inventories from in situ measurements of 137Cs activity at other locations. PMID:10800723

  12. In-Situ Gamma-PHA Measurements to Support Unconditional Release of NSR Chiller Unit

    SciTech Connect

    Dewberry, R. A.

    2001-03-07

    The Analytical Development Section of Savannah River Technology Center (SRTC) was requested by the Project Engineering and Construction Division (PE and CD) to conduct in-situ gamma-ray pulse height analysis measurements to support the unconditional release of the 221FBL/NSR chiller unit. The chiller unit was used to cool process water in the 221 FBL/NS facility, and it was serviced by its own cooling tower ''closed circuit'' system. This chiller unit had been in service for 18 years and has never been located within an SRS radiological area. The measurements' main goal is to confirm that there is no process-related contaminants present on the chiller and associated piping. To accomplish this, we have acquired 48 gamma-ray pulse height analysis spectra. All acquisitions were made using a portable HPGe detector and EG and G Dart system that contains high voltage power supply and signal processing electronics. A personal computer with Gamma-Vision software was used to control the Dart MCA and provide space to store and manipulate multiple 4096-channel gamma-ray spectra. Our results showed no activity above background. All peaks identified in the spectra are due to naturally-occurring radionuclides. This confirmed that these chillers are free of process-related gamma-emitting radioactive contamination. We estimate the chillers are completely clean of radioactive contamination to the limits of 1 nCi total gamma-ray activity. This report will discuss the purpose of the measurements, the experimental setup, data acquisition, calculations and results, and a conclusion of the study.

  13. MALDI Imaging Mass Spectrometry for In Situ Proteomic Analysis of Preneoplastic Lesions in Pancreatic Cancer

    PubMed Central

    Grüner, Barbara M.; Hahne, Hannes; Mazur, Pawel K.; Trajkovic-Arsic, Marija; Maier, Stefan; Esposito, Irene; Kalideris, Evdokia; Michalski, Christoph W.; Kleeff, Jörg; Rauser, Sandra; Schmid, Roland M.; Küster, Bernhard; Walch, Axel; Siveke, Jens T.

    2012-01-01

    The identification of new biomarkers for preneoplastic pancreatic lesions (PanINs, IPMNs) and early pancreatic ductal adenocarcinoma (PDAC) is crucial due to the diseasés high mortality rate upon late detection. To address this task we used the novel technique of matrix-assisted laser desorption/ionization (MALDI) imaging mass spectrometry (IMS) on genetically engineered mouse models (GEM) of pancreatic cancer. Various GEM were analyzed with MALDI IMS to investigate the peptide/protein-expression pattern of precursor lesions in comparison to normal pancreas and PDAC with cellular resolution. Statistical analysis revealed several discriminative m/z-species between normal and diseased tissue. Intraepithelial neoplasia (PanIN) and intraductal papillary mucinous neoplasm (IPMN) could be distinguished from normal pancreatic tissue and PDAC by 26 significant m/z-species. Among these m/z-species, we identified Albumin and Thymosin-beta 4 by liquid chromatography and tandem mass spectrometry (LC-MS/MS), which were further validated by immunohistochemistry, western blot, quantitative RT-PCR and ELISA in both murine and human tissue. Thymosin-beta 4 was found significantly increased in sera of mice with PanIN lesions. Upregulated PanIN expression of Albumin was accompanied by increased expression of liver-restricted genes suggesting a hepatic transdifferentiation program of preneoplastic cells. In conclusion we show that GEM of endogenous PDAC are a suitable model system for MALDI-IMS and subsequent LC-MS/MS analysis, allowing in situ analysis of small precursor lesions and identification of differentially expressed peptides and proteins. PMID:22761793

  14. Membrane-Extraction Ion Mobility Spectrometry for In-Situ Detection of Chlorinated Hydrocarbons in Water

    SciTech Connect

    Du, Yongzhai; Zhang, Wei; Whitten, William B; Li, Haiyang; Watson, David B; Xu, Jun

    2010-01-01

    Membrane-extraction ion mobility spectrometry (ME-IMS) has been developed for in-situ sampling and analysis of trace chlorinated hydrocarbons in water in a single procedure. The sampling is configured so that aqueous contaminants permeate through a spiral hollow polydimethylsiloxane (PDMS) membrane and are carried away by a vapor flow through the membrane tube. The extracted analyte flows into an atmospheric pressure chemical ionization (APCI) chamber and is analyzed in a home-made IMS analyzer. PDMS membrane is found to effectively extract chlorinated hydrocarbon solvents from liquid phase to vapor. The specialized IMS analyzer has been found to have resolutions of R=33 and 41, respectively, for negative- and positive-modes and is capable of detecting aqueous tetrachloroethylene (PCE) and trichloroethylene (TCE) as low as 80 g/L and 74 g/L in negative ion mode, respectively. The time-dependent characteristics of sampling and detection of TCE are both experimentally and theoretically studied for various concentrations, membrane lengths, and flow rates. These characteristics demonstrate that membrane-extraction IMS is feasible for the continuous monitoring of chlorinated hydrocarbons in water.

  15. In situ characterizing membrane lipid phenotype of breast cancer cells using mass spectrometry profiling.

    PubMed

    He, Manwen; Guo, Shuai; Li, Zhili

    2015-01-01

    Lipid composition in cell membrane is closely associated with cell characteristics. Here, matrix-assisted laser desorption/ionization- Fourier transform ion cyclotron resonance mass spectrometry was employed to in situ determine membrane components of human mammary epithelial cells (MCF-10 A) and six different breast cancer cell lines (i.e., BT-20, MCF-7, SK-BR-3, MDA-MB-231, MDA-MB-157, and MDA-MB-361) without any lipid extraction and separation. Partial least-square discriminant analysis indicated that changes in the levels of these membrane lipids were closely correlated with the types of breast cell lines. Elevated levels of polyunsaturated lipids in MCF-10 A cells relative to six breast cancer cells and in BT-20 cells relative to other breast cancer cell lines were detected. The Western blotting assays indicated that the expression of five lipogenesis-related enzymes (i.e., fatty acid synthase 1(FASN1), stearoyl-CoA desaturase 1 (SCD1), stearoyl-CoA desaturase 5 (SCD5), choline kinase α (CKα), and sphingomyelin synthase 1) was associated with the types of the breast cells, and that the SCD1 level in MCF-7 cells was significantly increased relative to other breast cell lines. Our findings suggest that elevated expression levels of FASN1, SCD1, SCD5, and CKα may closely correlated with enhanced levels of saturated and monounsaturated lipids in breast cancer cell lines. PMID:26061164

  16. In situ Analysis of Organic Compounds on Mars using Chemical Derivatization and Gas Chromatography Mass Spectrometry

    NASA Technical Reports Server (NTRS)

    Glavin, D. P.; Buch, A.; Cabane, M.; Coll, P.; Navarro-Gonzalez, R.; Mahaffy, P. R.

    2005-01-01

    One of the core science objectives of NASA's 2009 Mars Science Laboratory (MSL) mission is to determine the past or present habitability of Mars. The search for key organic compounds relevant to terrestrial life will be an important part of that assessment. We have developed a protocol for the analysis of amino acids and carboxylic acids in Mars analogue materials using gas chromatography mass spectrometry (GCMS). As shown, a variety of carboxylic acids were readily identified in soil collected from the Atacama Desert in Chile at part-per-billion levels by GCMS after extraction and chemical derivatization using the reagent N,N-tert.-butyl (dimethylsilyl) trifluoroacetamide (MTBSTFA). Several derivatized amino acids including glycine and alanine were also detected by GCMS in the Atacama soil at lower concentrations (chromatogram not shown). Lacking derivatization capability, the Viking pyrolysis GCMS instruments could not have detected amino acids and carboxylic acids, since these non-volatile compounds require chemical transformation into volatile species that are stable in a GC column. We are currently optimizing the chemical extraction and derivatization technique for in situ GCMS analysis on Mars. Laboratory results of analyses of Atacama Desert samples and other Mars analogue materials using this protocol will be presented.

  17. New shield for gamma-ray spectrometry

    NASA Technical Reports Server (NTRS)

    Brar, S. S.; Gustafson, P. F.; Nelson, D. M.

    1969-01-01

    Gamma-ray shield that can be evacuated, refilled with a clean gas, and pressurized for exclusion of airborne radioactive contaminants effectively lowers background noise. Under working conditions, repeated evacuation and filling procedures have not adversely affected the sensitivity and resolution of the crystal detector.

  18. Medium-resolution Autonomous in situ Gamma Detection System for Marine and Coastal Waters

    SciTech Connect

    Schwantes, Jon M.; Addleman, Raymond S.; Davidson, Joseph D.; Douglas, Matthew; Meier, David E.; Mullen, O Dennis; Myjak, Mitchell J.; Jones, Mark E.; Woodring, Mitchell L.; Johnson, Bryce; Santschi, Peter H.

    2009-12-01

    We are developing a medium-resolution autonomous in situ gamma detection system for marine and coastal waters. The system is designed to extract and preconcentrate isotopes of interest from natural waters prior to detection in order to eliminate signal attenuation of the gamma rays traveling through water and lower the overall background due to the presence of naturally occurring radioactive isotopes (40K and U/Th series radionuclides). Filtration is used to preconcentrate target isotopes residing on suspended particles, while chemosorption is employed to preferentially extract truly dissolved components from the water column. A variety of commercial and in-house nano-porus chemosorbents have been selected, procured or produced, and tested. Used filter and chemosorbent media are counted autonomously using two LaBr3 detectors in a near 4-pi configuration around the samples. A compact digital pulse processing system developed in-house and capable of running in coincidence mode is used to process the signal from the detectors to a small on-board computer. The entire system is extremely compact (9” dia. x 30” len.) and platform independent, but designed for initial deployment on a research buoy.

  19. Optimising in situ gamma measurements to identify the presence of radioactive particles in land areas.

    PubMed

    Rostron, Peter D; Heathcote, John A; Ramsey, Michael H

    2014-12-01

    High-coverage in situ surveys with gamma detectors are the best means of identifying small hotspots of activity, such as radioactive particles, in land areas. Scanning surveys can produce rapid results, but the probabilities of obtaining false positive or false negative errors are often unknown, and they may not satisfy other criteria such as estimation of mass activity concentrations. An alternative is to use portable gamma-detectors that are set up at a series of locations in a systematic sampling pattern, where any positive measurements are subsequently followed up in order to determine the exact location, extent and nature of the target source. The preliminary survey is typically designed using settings of detector height, measurement spacing and counting time that are based on convenience, rather than using settings that have been calculated to meet requirements. This paper introduces the basis of a repeatable method of setting these parameters at the outset of a survey, for pre-defined probabilities of false positive and false negative errors in locating spatially small radioactive particles in land areas. It is shown that an un-collimated detector is more effective than a collimated detector that might typically be used in the field. PMID:25233216

  20. In situ digestion for the determination of Ca in beverages by tungsten coil atomic emission spectrometry.

    PubMed

    Santos, Luana N; Gonzalez, Mário H; Moura, Monise F; Donati, George L; Nóbrega, Joaquim A

    2012-08-15

    Tungsten coil atomic emission spectrometry (WCAES) is employed for the determination of calcium in juice, mineral and coconut water samples. A sample aliquot of 20 μL is placed directly on the coil and a constant-voltage power source is used to dry and atomize the sample, as well as to promote Ca atomic emission. Analytical signals are resolved and detected using a Czerny-Turner spectrometer and a charge coupled device detector. Some experimental parameters such as coil position related to the spectrometer entrance slit and integration time are critically evaluated. A heating program with relatively constant drying temperatures is used in all measurements. An in situ digestion procedure is used to partially decompose organic matrices and improve WCAES precision and accuracy. By adding an oxidizing mixture to the sample and including a digestion step in the heating cycle, no statistical difference was observed between WCAES and ICP OES results for Ca in juice and coconut water samples. Mineral water samples were simply diluted with 1% vv(-1) HNO(3) before analysis and no significant interference was observed for concomitants such as Na and K. Despite severe positive interference caused by Mg, good agreement was obtained between WCAES and ICP OES results for Ca in several mineral water samples. Limits of detection and quantification obtained were 0.02 and 0.07 mg L(-1), respectively. The method precision, calculated as the relative standard deviation for 10 consecutive measurements of a 2.5 mg L(-1) Ca solution, is 3.8%. PMID:22841081

  1. In Situ Characterizing Membrane Lipid Phenotype of Human Lung Cancer Cell Lines Using Mass Spectrometry Profiling

    PubMed Central

    He, Manwen; Guo, Shuai; Ren, Junling; Li, Zhili

    2016-01-01

    Abnormal lipid metabolisms are closely associated with cancers. In this study, mass spectrometry was employed to in situ investigate the associations of membrane lipid phenotypes of six human lung cancer cell lines (i.e., A549, H1650, H1975 from adenocarcinoma, H157 and H1703 from squamous cell carcinomas, and H460 from a large cell carcinoma) with cancer cell types and finally total 230 lipids were detected. Based these 230 lipids, partial least-square discriminant analysis indicated that fifteen lipids (i.e., PE 18:0_18:1, PI 18:0_20:4, SM 42:2, PE 16:0_20:4, PE 36:2, PC 36:2, SM 34:1, PA 38:3,C18:0, C22:4, PA 34:2, C20:5, C20:2, C18:2, and CerP 36:2) with variable importance in the projection (VIP) value of > 1.0 could be used to differentiate six cancer cell lines with the Predicted Residual Sum of Square (PRESS) score of 0.1974. Positive correlation between polyunsaturated fatty acids (i.e., C20:4, C22:4, C22:5, and C22:6) and polyunsaturated phospholipids (PE 16:0_20:4, PE 38:4, and PI 18:0_20:4) was observed in lung adenocarcinoma cells, especially for H1975 cells. Three adenocarcinoma cell lines (i.e., A549, H1650, and H1975) could be differentiated from other lung cancer cell lines based on the expression of C18:1, C20:1, C20:2, C20:5, and C22:6. PMID:27162539

  2. Determination of tellurium by hydride generation with in situ trapping flame atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Matusiewicz, Henryk; Krawczyk, Magdalena

    2007-03-01

    The analytical performance of coupled hydride generation — integrated atom trap (HG-IAT) atomizer flame atomic absorption spectrometry (FAAS) system was evaluated for determination of Te in reference material (GBW 07302 Stream Sediment), coal fly ash and garlic. Tellurium, using formation of H 2Te vapors, is atomized in air-acetylene flame-heated IAT. A new design HG-IAT-FAAS hyphenated technique that would exceed the operational capabilities of existing arrangements (a water-cooled single silica tube, double-slotted quartz tube or an "integrated trap") was investigated. An improvement in detection limit was achieved compared with using either of the above atom trapping techniques separately. The concentration detection limit, defined as 3 times the blank standard deviation (3 σ), was 0.9 ng mL - 1 for Te. For a 2 min in situ pre-concentration time (sample volume of 2 mL), sensitivity enhancement compared to flame AAS, was 222 fold, using the hydride generation — atom trapping technique. The sensitivity can be further improved by increasing the collection time. The precision, expressed as RSD, was 7.0% ( n = 6) for Te. The designs studied include slotted tube, single silica tube and integrated atom trap-cooled atom traps. The accuracy of the method was verified using a certified reference material (GBW 07302 Stream Sediment) by aqueous standard calibration curves. The measured Te contents of the reference material was in agreement with the information value. The method was successfully applied to the determination of tellurium in coal fly ash and garlic.

  3. In Situ Characterizing Membrane Lipid Phenotype of Human Lung Cancer Cell Lines Using Mass Spectrometry Profiling.

    PubMed

    He, Manwen; Guo, Shuai; Ren, Junling; Li, Zhili

    2016-01-01

    Abnormal lipid metabolisms are closely associated with cancers. In this study, mass spectrometry was employed to in situ investigate the associations of membrane lipid phenotypes of six human lung cancer cell lines (i.e., A549, H1650, H1975 from adenocarcinoma, H157 and H1703 from squamous cell carcinomas, and H460 from a large cell carcinoma) with cancer cell types and finally total 230 lipids were detected. Based these 230 lipids, partial least-square discriminant analysis indicated that fifteen lipids (i.e., PE 18:0_18:1, PI 18:0_20:4, SM 42:2, PE 16:0_20:4, PE 36:2, PC 36:2, SM 34:1, PA 38:3,C18:0, C22:4, PA 34:2, C20:5, C20:2, C18:2, and CerP 36:2) with variable importance in the projection (VIP) value of > 1.0 could be used to differentiate six cancer cell lines with the Predicted Residual Sum of Square (PRESS) score of 0.1974. Positive correlation between polyunsaturated fatty acids (i.e., C20:4, C22:4, C22:5, and C22:6) and polyunsaturated phospholipids (PE 16:0_20:4, PE 38:4, and PI 18:0_20:4) was observed in lung adenocarcinoma cells, especially for H1975 cells. Three adenocarcinoma cell lines (i.e., A549, H1650, and H1975) could be differentiated from other lung cancer cell lines based on the expression of C18:1, C20:1, C20:2, C20:5, and C22:6. PMID:27162539

  4. In situ calibration of a high-resolution gamma-ray borehole sonde for assaying uranium-bearing sandstone deposits

    USGS Publications Warehouse

    Day, J.H., Jr.

    1985-01-01

    A method is presented for assaying radioactive sandstone deposits in situ by using a high-resolution borehole gamma-ray spectrometer. Gamma-ray photopeaks from the same spectrum acquired to analyze a sample are used to characterize gamma-ray attenuation properties, from which a calibration function is determined. Assay results are independent of differences between properties of field samples and those of laboratory or test-hole standards generally used to calibrate a borehole sonde. This assaying technique is also independent of the state of radioactive disequilibrium that usually exists in nature among members of the natural-decay chains. ?? 1985.

  5. Gamma-ray spectrometry of LDEF samples

    SciTech Connect

    Winn, W.G.

    1991-01-01

    A total of 31 samples from the Long Duration Exposure Facility (LDEF), including materials of aluminum, vanadium, and steel trunnions were analyzed by ultra-low-level gamma spectroscopy. The study quantified particle induced activations of (sup 22)Na, {sup 46}Sc, {sup 51}Cr, {sup 54}Mn, {sup 56}Co, {sup 57}Co, {sup 58}Co, and {sup 60}Co. The samples of trunnion sections exhibited increasing activity toward the outer end of the trunnion and decreasing activity toward its radial center. The trunnion sections did not include end pieces, which have been reported to collect noticeable {sup 7}Be on their leading surfaces. No significant {sup 7}Be was detected in the samples analyzed. The Underground Counting Facility at Savannah River Laboratory (SRL) was used in this work. The facility is 50 ft. underground, constructed with low-background shielding materials, and operated as a clean room. The most sensitive analyses were performed with a 90%-efficient HPGe gamma-ray detector, which is enclosed in a purged active/passive shield. Each sample was counted for one to six days in two orientations to yield more representative average activities for the sample. The non-standard geometries of the LDEF samples prompted the development of a novel calibration method, whereby the efficiency about the samples surfaces (measured with point sources) predicted the efficiency for the bulk sample.

  6. A dedicated LIMS for routine gamma-ray spectrometry.

    PubMed

    Bruggeman, M; Verheyen, L; Vidmar, T

    2014-05-01

    We developed a Microsoft(®) Access-based LIMS (Laboratory Information and Management Systems), γ-LIMS, for the management of our gamma-spectrometry laboratory, in which thousands of routine, but high-quality analyses are performed each year. This paper explains the main features of the γ-LIMS and puts special attention on the interfacing methods and solutions for using the Genie™2000 spectrometry software in conjunction with the EFFTRAN package, which serves for efficiency transfer calculations, coincidence summing corrections and a procedure for uncertainty estimation. PMID:24332338

  7. Detection of soil microorganism in situ by combined gas chromatography mass spectrometry

    NASA Technical Reports Server (NTRS)

    Alexander, M.; Duxbury, J. M.; Francis, A. J.; Adamson, J.

    1972-01-01

    Experimental tests were made to determine whether analysis of volatile metabolic products, formed in situ, is a viable procedure for an extraterrestrial life detection system. Laboratory experiments, carried out under anaerobic conditions with addition of carbon source, extended to include a variety of soils and additional substrates. In situ experiments were conducted without amendment using a vacuum sampling system.

  8. Rapid in situ identification of bioactive compounds in plants by in vivo nanospray high-resolution mass spectrometry.

    PubMed

    Chang, Qing; Peng, Yue'e; Dan, Conghui; Shuai, Qin; Hu, Shenghong

    2015-03-25

    A method for the rapid in situ identification of bioactive compounds in fresh plants has been developed using in vivo nanospray coupled to high-resolution mass spectrometry (HR-MS). Using a homemade in vivo nanospray ion source, the plant liquid was drawn out from a target region and ionized in situ. The ionized bioactive compounds were then identified using Q-Orbitrap HR-MS. The accurate mass measurements of these bioactive compounds were performed by full-scan or selected ion monitoring (SIM), and tandem mass spectrometry (MS/MS) was used in the structural elucidation. Without sample pretreatment, 12 bioactive compounds in 7 different plant species were identified, namely, isoalliin in onion; butylphthalide in celery; N-methylpelletierine, pelletierine, and pseudopelletierine in pomegranate; chlorogenic acid in crabapple; solamargine, solasonine, and solasodine in nightshade; aloin and aloe-emodin in aloe; and menthone in mint. This work demonstrates that in vivo nanospray HR-MS is a good method for rapid in situ identification of bioactive compounds in plants. PMID:25749134

  9. Determination of environmental radiation flux and organ doses using in-situ gamma spectroscopy

    NASA Astrophysics Data System (ADS)

    Al-Ghamdi, Abdulrahman S.

    Contamination of buildings represent a unique problem during Decontamination and Decommissioning (D&D) of nuclear facilities. It is necessary to determine the long-lived radionuclides and their respective specific activities in building materials before the right D&D decision can be made. At the same time, radiation risk of workers or potential occupants in the facility must be assessed as part of the D&D process. The goal of this project was to develop a methodology of obtaining gamma radiation flux and organ doses from in-situ gamma spectroscopy. Algorithms were developed to simulate the response functions of the HPGe detector and to convert the spectra into photon fluences. A Monte Carlo code, MCNP4C, was used to simulate HPGe detector response and to develop the conversion algorithm. The simulated spectra obtained for an HPGe detector were converted to flux using the algorithm for various different geometries. The response functions of the detector are presented in this document for the gamma energies from 60 keV to 2.2 MeV. Published fluence-to-dose conversion coefficients were used to calculate organ doses and effective dose equivalent. We then tested the theory at a 100-MeV linear electron accelerator at Rensselaer Polytechnic Institute (RPI). Samples of the activated concrete walls and floor in the target room of the Linac facility as well as some steel samples were taken to quantify the specific activities of the structures. The results show that the most important long-lived radionuclides include 22 Na, 46Sc, 54 Mn, 57Co, 60 Co, 65Zn, 152 Eu and 154Eu, depending on the location and composition of the material. The specific activities at the Linac facility range from 1.15E-01 to 765.31 muCi/Kg. The annual effective dose equivalent was assessed to be 2.44 mSv y-1 (0.244 rem y-1 ), which is about 5% of the Annual EDE limits to workers.

  10. Rapid, in situ detection of cocaine residues based on paper spray ionization coupled with ion mobility spectrometry.

    PubMed

    Li, Ming; Zhang, Jingjing; Jiang, Jie; Zhang, Jing; Gao, Jing; Qiao, Xiaolin

    2014-04-01

    In this paper, a novel approach based on paper spray ionization coupled with ion mobility spectrometry (PSI-IMS) was developed for rapid, in situ detection of cocaine residues in liquid samples and on various surfaces (e.g. glass, marble, skin, wood, fingernails), without tedious sample pretreatment. The obvious advantages of PSI are its low cost, easy operation and simple configuration without using nebulizing gas or discharge gas. Compared with mass spectrometry, ion mobility spectrometry (IMS) takes advantage of its low cost, easy operation, and simple configuration without requiring a vacuum system. Therefore, IMS is a more congruous detection method for PSI in the case of rapid, in situ analysis. For the analysis of cocaine residues in liquid samples, dynamic responses from 5 μg mL(-1) to 200 μg mL(-1) with a linear coefficient (R(2)) of 0.992 were obtained. In this case, the limit of detection (LOD) was calculated to be 2 μg mL(-1) as signal to noise (S/N) was 3 with a relative standard deviation (RSD) of 6.5% for 11 measurements (n = 11). Cocaine residues on various surfaces such as metal, glass, marble, wood, skin, and fingernails were also directly analyzed before wiping the surfaces with a piece of paper. The LOD was calculated to be as low as 5 ng (S/N = 3, RSD = 6.3%, n = 11). This demonstrates the capability of the PSI-IMS method for direct detection of cocaine residues at scenes of cocaine administration. Our results show that PSI-IMS is a simple, sensitive, rapid and economical method for in situ detection of this illicit drug, which could help governments to combat drug abuse. PMID:24563903

  11. In-situ Isotopic Analysis at Nanoscale using Parallel Ion Electron Spectrometry: A Powerful New Paradigm for Correlative Microscopy.

    PubMed

    Yedra, Lluís; Eswara, Santhana; Dowsett, David; Wirtz, Tom

    2016-01-01

    Isotopic analysis is of paramount importance across the entire gamut of scientific research. To advance the frontiers of knowledge, a technique for nanoscale isotopic analysis is indispensable. Secondary Ion Mass Spectrometry (SIMS) is a well-established technique for analyzing isotopes, but its spatial-resolution is fundamentally limited. Transmission Electron Microscopy (TEM) is a well-known method for high-resolution imaging down to the atomic scale. However, isotopic analysis in TEM is not possible. Here, we introduce a powerful new paradigm for in-situ correlative microscopy called the Parallel Ion Electron Spectrometry by synergizing SIMS with TEM. We demonstrate this technique by distinguishing lithium carbonate nanoparticles according to the isotopic label of lithium, viz. (6)Li and (7)Li and imaging them at high-resolution by TEM, adding a new dimension to correlative microscopy. PMID:27350565

  12. In-situ Isotopic Analysis at Nanoscale using Parallel Ion Electron Spectrometry: A Powerful New Paradigm for Correlative Microscopy

    PubMed Central

    Yedra, Lluís; Eswara, Santhana; Dowsett, David; Wirtz, Tom

    2016-01-01

    Isotopic analysis is of paramount importance across the entire gamut of scientific research. To advance the frontiers of knowledge, a technique for nanoscale isotopic analysis is indispensable. Secondary Ion Mass Spectrometry (SIMS) is a well-established technique for analyzing isotopes, but its spatial-resolution is fundamentally limited. Transmission Electron Microscopy (TEM) is a well-known method for high-resolution imaging down to the atomic scale. However, isotopic analysis in TEM is not possible. Here, we introduce a powerful new paradigm for in-situ correlative microscopy called the Parallel Ion Electron Spectrometry by synergizing SIMS with TEM. We demonstrate this technique by distinguishing lithium carbonate nanoparticles according to the isotopic label of lithium, viz. 6Li and 7Li and imaging them at high-resolution by TEM, adding a new dimension to correlative microscopy. PMID:27350565

  13. Ion funnel augmented Mars atmospheric pressure photoionization mass spectrometry for in situ detection of organic molecules.

    PubMed

    Johnson, Paul V; Hodyss, Robert; Beauchamp, J L

    2014-11-01

    Laser desorption is an attractive technique for in situ sampling of organics on Mars given its relative simplicity. We demonstrate that under simulated Martian conditions (~2.5 Torr CO(2)) laser desorption of neutral species (e.g., polycyclic aromatic hydrocarbons), followed by ionization with a simple ultraviolet light source such as a discharge lamp, offers an effective means of sampling organics for detection and identification with a mass spectrometer. An electrodynamic ion funnel is employed to provide efficient ion collection in the ambient Martian environment. This experimental methodology enables in situ sampling of Martian organics with minimal complexity and maximum flexibility. PMID:24986759

  14. Slow elimination of phosphorylated histone {gamma}-H2AX from DNA of terminally differentiated mouse heart cells in situ

    SciTech Connect

    Gavrilov, Boris; Vezhenkova, Irina; Firsanov, Denis; Solovjeva, Liudmila; Svetlova, Maria; Mikhailov, Vyacheslav; Tomilin, Nikolai . E-mail: nvtom@hotmail.com

    2006-09-08

    Phosphorylation of replacement histone H2AX occurs in megabase chromatin domains around double-strand DNA breaks (DSBs) and this modification (called {gamma}-H2AX) may serve as a useful marker of genome damage and repair in terminally differentiated cells. Here using immunohistochemistry we studied kinetics of {gamma}-H2AX formation and elimination in the X-irradiated mouse heart and renal epithelial tissues in situ. Unirradiated tissues have 3-5% {gamma}-H2AX-positive cells and in tissues fixed 1 h after X-irradiation {gamma}-H2AX-positive nuclei are induced in a dose-dependent manner approaching 20-30% after 3 Gy of IR. Analysis of mouse tissues at different times after 3 Gy of IR showed that maximal induction of {gamma}-H2AX in heart is observed 20 min after IR and then is decreased slowly with about half remaining 23 h later. In renal epithelium maximum of the {gamma}-H2AX-positive cells is observed 40 min after IR and then decreases to control values in 23 h. This indicates that there are significant variations between non-proliferating mammalian tissues in the initial H2AX phosphorylation rate as well as in the rate of {gamma}-H2AX elimination after X-irradiation, which should be taken into account in the analysis of radiation responses.

  15. Basic characterization of highly enriched uranium by gamma spectrometry

    NASA Astrophysics Data System (ADS)

    Nguyen, Cong Tam; Zsigrai, József

    2006-05-01

    Gamma-spectrometric methods suitable for the characterization of highly enriched uranium samples encountered in illicit trafficking of nuclear materials are presented. In particular, procedures for determining the 234U, 235U, 238U, 232U and 236U contents and the age of highly enriched uranium are described. Consequently, the total uranium content and isotopic composition can be calculated. For determining the 238U and 232U contents a low-background chamber was used. In addition, age dating of uranium was also performed using low-background spectrometry.

  16. Gamma ray spectrometry of LDEF samples at SRL

    NASA Technical Reports Server (NTRS)

    Winn, Willard G.

    1992-01-01

    A total of 31 samples from the Long Duration Exposure Facility (LDEF), including materials of aluminum, vanadium, and steel trunnions were analyzed by ultra-low-level gamma spectrometry. The study quantified particle induced activations of Na-22, Sc-46, Cr-51, Mn-54, Co-56, Co-57, Co-58, and Co-60. The samples of trunnion sections exhibited increasing activity toward the outer end of the trunnion and decreasing activity toward its radial center. The trunnion sections did not include end pieces, which were reported to collect noticeable Be-7 on their leading surfaces. No significant Be-7 was detected in the samples analyzed.

  17. Gamma ray spectrometry of LDEF samples at SRS

    NASA Technical Reports Server (NTRS)

    Winn, Willard G.

    1991-01-01

    A total of 31 samples from Long Duration Exposure Facility (LDEF), including materials of Al, V, and steel trunnions were analyzed by ultralow level gamma spectrometry. The study quantified particle induced activations of Na-22, Sc-46, Cr-51, Mn-54, Co-56, Co-57, Co-58, and Co-60. The samples of trunnion sections exhibited increasing activity toward the outer end of the trunnion and decreasing activity toward its radial center. The trunnion sections did not include an end piece that collects noticeable Be-7 on its leading surface. No significant Be-7 was detected in the samples analyzed. The most sensitive analyses were performed with a 90 pct. efficient HPGe gamma ray detector, which is enclosed in a purged active/passive active shield.

  18. In Situ Mass Spectrometry Imaging and Ex Vivo Characterization of Renal Crystalline Deposits Induced in Multiple Preclinical Drug Toxicology Studies

    PubMed Central

    Bjurström, Sivert; Goodwin, Richard J. A.; Basmaci, Elisa; Gustafsson, Ingela; Annas, Anita; Hellgren, Dennis; Svanhagen, Alexander; Andrén, Per E.; Lindberg, Johan

    2012-01-01

    Drug toxicity observed in animal studies during drug development accounts for the discontinuation of many drug candidates, with the kidney being a major site of tissue damage. Extensive investigations are often required to reveal the mechanisms underlying such toxicological events and in the case of crystalline deposits the chemical composition can be problematic to determine. In the present study, we have used mass spectrometry imaging combined with a set of advanced analytical techniques to characterize such crystalline deposits in situ. Two potential microsomal prostaglandin E synthase 1 inhibitors, with similar chemical structure, were administered to rats over a seven day period. This resulted in kidney damage with marked tubular degeneration/regeneration and crystal deposits within the tissue that was detected by histopathology. Results from direct tissue section analysis by matrix-assisted laser desorption ionization mass spectrometry imaging were combined with data obtained following manual crystal dissection analyzed by liquid chromatography mass spectrometry and nuclear magnetic resonance spectroscopy. The chemical composition of the crystal deposits was successfully identified as a common metabolite, bisulphonamide, of the two drug candidates. In addition, an un-targeted analysis revealed molecular changes in the kidney that were specifically associated with the area of the tissue defined as pathologically damaged. In the presented study, we show the usefulness of combining mass spectrometry imaging with an array of powerful analytical tools to solve complex toxicological problems occurring during drug development. PMID:23110069

  19. Investigating the Origin and Evolution of Venus with In Situ Mass Spectrometry

    NASA Technical Reports Server (NTRS)

    Trainer, M. G.; Mahaffy, P. R.; Brinckerhoff, W. B.; Johnson, N. M.; Glaze, L. S.

    2015-01-01

    Measurement of noble gas abundances on Venus remain a high priority for planetary science. These studies are only possible through in situ measurement, and can be accomplished by a modern neutral mass spectrometer (NMS) such as that developed at NASA Goddard, based on flight-proven technology. Here we show how the measurement of noble gases can be secured using demonstrated enrichment techniques.

  20. Physiologically active hydrogel (in situ gel) of sparfloxacin and its evaluation for ocular retention using gamma scintigraphy

    PubMed Central

    Gupta, Himanshu; Malik, Aqil; Khar, R. K.; Ali, Asgar; Bhatnagar, Aseem; Mittal, Gaurav

    2015-01-01

    Objective: Due to the structure and physiological barrier of eye, only 1% of instilled dose is available for action on the corneal surface. In this work, we developed and evaluated chitosan (pH sensitive) and gellan gum (ion sensitive) in situ gel of sparfloxacin to improve precorneal residence time. Materials and Methods: A protocol for radiolabeling of sparfloxacin with Tc-99m was optimized to study the ocular retention using gamma scintigraphy technique. Results: The clear formulation was developed. In vitro release showed a sustained and prolonged release compared to plain eye drop solution. Dynamic and static gamma scintigraphy showed better retention than plain eye drops. The ocular tolerance test (hen's egg test-chorioallantoic membrane test and infra-red study) showed that the formulation is nonirritant and can be used as ocular vehicle. Conclusion: Radiolabel protocol for sparfloxacin was successfully developed and evaluated on ocular retention studies of developed in situ gel. The developed in situ gel is non irritant and can go further with clinical evaluation. PMID:26229353

  1. Investigating the Origin and Evolution of Venus with In Situ Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Trainer, M. G.; Mahaffy, P. R.; Brinckerhoff, W. B.; Johnson, N. M.; Glaze, L. S.

    2015-10-01

    Measurement of noble gas abundances on Venus remain a high priority for planetary science [1,2]. These studies are only possible through in situ measurement, and can be accomplished by a modern neutral mass spectrometer (NMS) such as that developed at NASA Goddard, based on flight-proven technology. Here we show how the measurement of noble gases can be secured using demonstrated enrichment techniques.

  2. Touch Spray Mass Spectrometry for In Situ Analysis of Complex Samples

    PubMed Central

    Kerian, Kevin S.; Jarmusch, Alan K.; Cooks, R. Graham

    2014-01-01

    Touch spray, a spray-based ambient in-situ ionization method, uses a small probe, e.g. a teasing needle to pick up sample and the application of voltage and solvent to cause field-induced droplet emission. Compounds extracted from the microsample are incorporated into the sprayed micro droplets. Performance tests include disease state of tissue, microorganism identification, and therapeutic drug quantitation. Chemical derivatization is performed simultaneously with ionization. PMID:24756256

  3. Characterizing spatial and temporal variability of dissolved gases in aquatic environments with in situ mass spectrometry.

    PubMed

    Camilli, Richard; Duryea, Anthony N

    2009-07-01

    The TETHYS mass spectrometer is intended for long-term in situ observation of dissolved gases and volatile organic compounds in aquatic environments. Its design maintains excellent low mass range sensitivity and stability during long-term operations, enabling characterization of low-frequency variability in many trace dissolved gases. Results are presented from laboratory trials and a 300-h in situ trial in a shallow marine embayment in Massachusetts, U.S.A. This time series consists of over 15000 sample measurements and represents the longest continuous record made by an in situ mass spectrometer in an aquatic environment. These measurements possess sufficient sampling density and duration to apply frequency analysis techniques for study of temporal variability in dissolved gases. Results reveal correlations with specific environmental periodicities. Numerical methods are presented for converting mass spectrometer ion peak ratios to absolute-scale dissolved gas concentrations across wide temperature regimes irrespective of ambient pressure, during vertical water column profiles in a hypoxic deep marine basin off the coast of California, U.S.A. Dissolved oxygen concentration values obtained with the TETHYS instrument indicate close correlation with polarographic oxygen sensor data across the entire depth range. These methods and technology enable observation of aquatic environmental chemical distributions and dynamics at appropriate scales of resolution. PMID:19673300

  4. Development of the Probing In-Situ with Neutron and Gamma Rays (PING) Instrument for Planetary Science Applications

    NASA Technical Reports Server (NTRS)

    Parsons, A.; Bodnarik, J.; Burger, D.; Evans, L.; Floyd, S; Lim, L.; McClanahan, T.; Namkung, M.; Nowicki, S.; Schweitzer, J.; Starr, R.; Trombka, J.

    2011-01-01

    The Probing In situ with Neutrons and Gamma rays (PING) instrument is a promising planetary science application of the active neutron-gamma ray technology that has been used successfully in oil field well logging and mineral exploration on Earth for decades. Similar techniques can be very powerful for non-invasive in situ measurements of the subsurface elemental composition on other planets. The objective of our active neutron-gamma ray technology program at NASA Goddard Space Flight Center (NASA/GSFC) is to bring instruments using this technology to the point where they can be flown on a variety of surface lander or rover missions to the Moon, Mars, Venus, asteroids, comets and the satellites of the outer planets. PING combines a 14 MeV deuterium-tritium pulsed neutron generator with a gamma ray spectrometer and two neutron detectors to produce a landed instrument that can determine the elemental composition of a planet down to 30 - 50 cm below the planet's surface. The penetrating nature of.5 - 10 MeV gamma rays and 14 MeV neutrons allows such sub-surface composition measurements to be made without the need to drill into or otherwise disturb the planetary surface, thus greatly simplifying the lander design. We are currently testing a PING prototype at a unique outdoor neutron instrumentation test facility at NASA/GSFC that provides two large (1.8 m x 1.8 m x.9 m) granite and basalt test formations placed outdoors in an empty field. Since an independent trace elemental analysis has been performed on both the Columbia River basalt and Concord Gray granite materials, these samples present two known standards with which to compare PING's experimentally measured elemental composition results. We will present experimental results from PING measurements of both the granite and basalt test formations and show how and why the optimum PING instrument operating parameters differ for studying the two materials.

  5. Matrix assisted laser desorption/ionization-mass spectrometry imaging (MALDI-MSI) for direct visualization of plant metabolites in situ.

    PubMed

    Sturtevant, Drew; Lee, Young-Jin; Chapman, Kent D

    2016-02-01

    Direct visualization of plant tissues by matrix assisted laser desorption ionization-mass spectrometry imaging (MALDI-MSI) has revealed key insights into the localization of metabolites in situ. Recent efforts have determined the spatial distribution of primary and secondary metabolites in plant tissues and cells. Strategies have been applied in many areas of metabolism including isotope flux analyses, plant interactions, and transcriptional regulation of metabolite accumulation. Technological advances have pushed achievable spatial resolution to subcellular levels and increased instrument sensitivity by several orders of magnitude. It is anticipated that MALDI-MSI and other MSI approaches will bring a new level of understanding to metabolomics as scientists will be encouraged to consider spatial heterogeneity of metabolites in descriptions of metabolic pathway regulation. PMID:26613199

  6. Matrix assisted laser desorption/ionization-mass spectrometry imaging (MALDI-MSI) for direct visualization of plant metabolites in situ

    DOE PAGESBeta

    Sturtevant, Drew; Lee, Young -Jin; Chapman, Kent D.

    2015-11-22

    Direct visualization of plant tissues by matrix assisted laser desorption ionization-mass spectrometry imaging (MALDI-MSI) has revealed key insights into the localization of metabolites in situ. Recent efforts have determined the spatial distribution of primary and secondary metabolites in plant tissues and cells. Strategies have been applied in many areas of metabolism including isotope flux analyses, plant interactions, and transcriptional regulation of metabolite accumulation. Technological advances have pushed achievable spatial resolution to subcellular levels and increased instrument sensitivity by several orders of magnitude. Furthermore, it is anticipated that MALDI-MSI and other MSI approaches will bring a new level of understanding tomore » metabolomics as scientists will be encouraged to consider spatial heterogeneity of metabolites in descriptions of metabolic pathway regulation.« less

  7. In situ GaN decomposition analysis by quadrupole mass spectrometry and reflection high-energy electron diffraction

    SciTech Connect

    Fernandez-Garrido, S.; Calleja, E.; Koblmueller, G.; Speck, J. S.

    2008-08-01

    Thermal decomposition of wurtzite (0001)-oriented GaN was analyzed: in vacuum, under active N exposure, and during growth by rf plasma-assisted molecular beam epitaxy. The GaN decomposition rate was determined by measurements of the Ga desorption using in situ quadrupole mass spectrometry, which showed Arrhenius behavior with an apparent activation energy of 3.1 eV. Clear signatures of intensity oscillations during reflection high-energy electron diffraction measurements facilitated complementary evaluation of the decomposition rate and highlighted a layer-by-layer decomposition mode in vacuum. Exposure to active nitrogen, either under vacuum or during growth under N-rich growth conditions, strongly reduced the GaN losses due to GaN decomposition.

  8. In situ analysis of soybeans and nuts by probe electrospray ionization mass spectrometry.

    PubMed

    Petroselli, Gabriela; Mandal, Mridul K; Chen, Lee C; Hiraoka, Kenzo; Nonami, Hiroshi; Erra-Balsells, Rosa

    2015-04-01

    The probe electrospray ionization (PESI) is an ESI-based ionization technique that generates electrospray from the tip of a solid metal needle. In the present work, we describe the PESI mass spectra obtained by in situ measurement of soybeans and several nuts (peanuts, walnuts, cashew nuts, macadamia nuts and almonds) using different solid needles as sampling probes. It was found that PESI-MS is a valuable approach for in situ lipid analysis of these seeds. The phospholipid and triacylglycerol PESI spectra of different nuts and soybean were compared by principal component analysis (PCA). PCA shows significant differences among the data of each family of seeds. Methanolic extracts of nuts and soybean were exposed to air and sunlight for several days. PESI mass spectra were recorded before and after the treatment. Along the aging of the oil (rancidification), the formation of oxidated species with variable number of hydroperoxide groups could be observed in the PESI spectra. The relative intensity of oxidated triacylglycerols signals increased with days of exposition. Monitoring sensitivity of PESI-MS was high. This method provides a fast, simple and sensitive technique for the analysis (detection and characterization) of lipids in seed tissue and degree of oxidation of the oil samples. PMID:26149112

  9. Multiple-reflection time-of-flight mass spectrometry for in situ applications

    NASA Astrophysics Data System (ADS)

    Dickel, T.; Plaß, W. R.; Lang, J.; Ebert, J.; Geissel, H.; Haettner, E.; Jesch, C.; Lippert, W.; Petrick, M.; Scheidenberger, C.; Yavor, M. I.

    2013-12-01

    Multiple-reflection time-of-flight mass spectrometers (MR-TOF-MS) have recently been installed at different low-energy radioactive ion beam facilities. They are used as isobar separators with high ion capacity and as mass spectrometers with high mass resolving power and accuracy for short-lived nuclei. Furthermore, MR-TOF-MS have a huge potential for applications in other fields, such as chemistry, biology, medicine, space science, and homeland security. The development, commissioning and results of an MR-TOF-MS is presented, which serves as proof-of-principle to show that very high mass resolving powers (∼105) can be achieved in a compact device (length ∼30 cm). Based on this work, an MR-TOF-MS for in situ application has been designed. For the first time, this device combines very high mass resolving power (>105), mobility, and an atmospheric pressure inlet in one instrument. It will enable in situ measurements without sample preparation at very high mass accuracy. Envisaged applications of this mobile MR-TOF-MS are discussed.

  10. The Laser Ablation Ion Funnel: Sampling for in situ Mass Spectrometry on Mars

    NASA Technical Reports Server (NTRS)

    Johnson, Paul V.; Hodyss, Robert; Tang, Keqi; Brinckerhoff, William B.; Smith, Richard D.

    2011-01-01

    A considerable investment has been made by NASA and other space agencies to develop instrumentation suitable for in situ analytical investigation of extra terrestrial bodies including various mass spectrometers (time-of-flight, quadrupole ion trap, quadrupole mass filters, etc.). However, the front-end sample handling that is needed to collect and prepare samples for interrogation by such instrumentation remains underdeveloped. Here we describe a novel approach tailored to the exploration of Mars where ions are created in the ambient atmosphere via laser ablation and then efficiently transported into a mass spectrometer for in situ analysis using an electrodynamic ion funnel. This concept would enable elemental and isotopic analysis of geological samples with the analysis of desorbed organic material a possibility as well. Such an instrument would be suitable for inclusion on all potential missions currently being considered such as the Mid-Range Rover, the Astrobiology Field Laboratory, and Mars Sample Return (i.e., as a sample pre-selection triage instrument), among others.

  11. In situ detection of histone variants and modifications in mouse brain using imaging mass spectrometry.

    PubMed

    Lahiri, Shibojyoti; Sun, Na; Solis-Mezarino, Victor; Fedisch, Andreas; Ninkovic, Jovica; Feuchtinger, Annette; Götz, Magdalena; Walch, Axel; Imhof, Axel

    2016-02-01

    Histone posttranslational modifications and histone variants control the epigenetic regulation of gene expression and affect a wide variety of biological processes. A complex pattern of such modifications and variants defines the identity of cells within complex organ systems and can therefore be used to characterize cells at a molecular level. However, their detection and identification in situ has been limited so far due to lack of specificity, selectivity, and availability of antihistone antibodies. Here, we describe a novel MALDI imaging MS based workflow, which enables us to detect and characterize histones by their intact mass and their correlation with cytological properties of the tissue using novel statistical and image analysis tools. The workflow allows us to characterize the in situ distribution of the major histone variants and their modification in the mouse brain. This new analysis tool is particularly useful for the investigation of expression patterns of the linker histone H1 variants for which suitable antibodies are so far not available. PMID:26593131

  12. In-situ suspended aggregate microextraction of gold nanoparticles from water samples and determination by electrothermal atomic absorption spectrometry.

    PubMed

    Choleva, Tatiana G; Kappi, Foteini A; Tsogas, George Z; Vlessidis, Athanasios G; Giokas, Dimosthenis L

    2016-05-01

    This work describes a new method for the extraction and determination of gold nanoparticles in environmental samples by means of in-situ suspended aggregate microextraction and electrothermal atomic absorption spectrometry. The method relies on the in-situ formation of a supramolecular aggregate phase through ion-association between a cationic surfactant and a benzene sulfonic acid derivative. Gold nanoparticles are physically entrapped into the aggregate phase which is separated from the bulk aqueous solution by vacuum filtration on the surface of a cellulose filter in the form of a thin film. The film is removed from the filter surface and is dissociated into an acidified methanolic solution which is used for analysis. Under the optimized experimental conditions, gold nanoparticles can be efficiently extracted from water samples with recovery rates between 81.0-93.3%, precision 5.4-12.0% and detection limits as low as 75femtomolL(-1) using only 20mL of sample volume. The satisfactory analytical features of the method along with the simplicity indicate the efficiency of this new approach to adequately collect and extract gold nanoparticle species from water samples. PMID:26946014

  13. Guide to plutonium isotopic measurements using gamma-ray spectrometry

    SciTech Connect

    Lemming, J.F.; Rakel, D.A.

    1982-08-26

    Purpose of this guide is to assist those responsible for plutonium isotopic measurements in the application of gamma-ray spectrometry. Objectives are to promote an understanding of the measurement process, including its limitations and applicability, by reviewing the general features of a plutonium spectrum and identifying the quantities which must be extracted from the data; to introduce state-of-the-art analysis techniques by reviewing four isotopic analysis packages and identifying their differences; to establish the basis for measurement control and assurance by discussing means of authenticating the performance of a measurement system; and to prepare for some specific problems encountered in plutonium isotopic analyses by providing solutions from the practical experiences of several laboratories. 29 references, 12 figures, 17 tables.

  14. Efficiency Calibration for Environmental Gamma Spectrometry Using GATE.

    PubMed

    Alrefae, Tareq

    2016-06-01

    This work investigated the utility of performing efficiency calibration for environmental gamma spectrometry using the Monte Carlo based, free of charge GATE toolbox. The validity of this approach was tested by comparing output efficiency values of an in-house developed GATE-based program with experimental measurements covering various geometries and primary photon energies. The results of this comparison revealed relative deviations within ±20%, thus validating the employed computational approach. Moreover, the GATE-based method was able to predict quantities that are generally difficult to measure experimentally, such as the number of interactions preceding full energy absorption. These computationally obtained predictions were found to be in agreement with theory. PMID:27115226

  15. Waste Characterization Using Gamma Ray Spectrometry with Automated Efficiency Optimization - 13404

    SciTech Connect

    Bosko, A.; Venkataraman, R.; Bronson, F.L.; Ilie, G.; Russ, W.R.

    2013-07-01

    Gamma ray spectrometry using High Purity Germanium (HPGe) detectors is commonly employed in assaying radioactive waste streams from a variety of sources: nuclear power plants, Department of Energy (DOE) laboratories, medical facilities, decontamination and decommissioning activities etc. The radioactive material is typically packaged in boxes or drums (for e.g. B-25 boxes or 208 liter drums) and assayed to identify and quantify radionuclides. Depending on the origin of the waste stream, the radionuclides could be special nuclear materials (SNM), fission products, or activation products. Efficiency calibration of the measurement geometry is a critical step in the achieving accurate quantification of radionuclide content. Due to the large size of the waste items, it is impractical and expensive to manufacture gamma ray standard sources for performing a measurement based calibration. For well over a decade, mathematical efficiency methods such as those in Canberra's In Situ Object Counting System (ISOCS) have been successfully employed in the efficiency calibration of gamma based waste assay systems. In the traditional ISOCS based calibrations, the user provides input data such as the dimensions of the waste item, the average density and fill height of the matrix, and matrix composition. As in measurement based calibrations, the user typically defines a homogeneous matrix with a uniform distribution of radioactivity. Actual waste containers can be quite nonuniform, however. Such simplifying assumptions in the efficiency calibration could lead to a large Total Measurement Uncertainty (TMU), thus limiting the amount of waste that can be disposed of as intermediate or low activity level waste. To improve the accuracy of radionuclide quantification, and reduce the TMU, Canberra has developed the capability to optimize the efficiency calibration using the ISOCS method. The optimization is based on benchmarking the efficiency shape and magnitude to the data available in the

  16. Two-Step Resonance-Enhanced Desorption Laser Mass Spectrometry for In Situ Analysis of Organic-Rich Environments

    NASA Technical Reports Server (NTRS)

    Getty, S. A.; Grubisic, A.; Uckert, K.; Li, X.; Cornish, T.; Cook, J. E.; Brinckerhoff, W. B.

    2016-01-01

    A wide diversity of planetary surfaces in the solar system represent high priority targets for in situ compositional and contextual analysis as part of future missions. The planned mission portfolio will inform our knowledge of the chemistry at play on Mars, icy moons, comets, and primitive asteroids, which can lead to advances in our understanding of the interplay between inorganic and organic building blocks that led to the evolution of habitable environments on Earth and beyond. In many of these environments, the presence of water or aqueously altered mineralogy is an important indicator of habitable environments that are present or may have been present in the past. As a result, the search for complex organic chemistry that may imply the presence of a feedstock, if not an inventory of biosignatures, is naturally aligned with targeted analyses of water-rich surface materials. Here we describe the two-step laser mass spectrometry (L2MS) analytical technique that has seen broad application in the study of organics in meteoritic samples, now demonstrated to be compatible with an in situ investigation with technique improvements to target high priority planetary environments as part of a future scientific payload. An ultraviolet (UV) pulsed laser is used in previous and current embodiments of laser desorption/ionization mass spectrometry (LDMS) to produce ionized species traceable to the mineral and organic composition of a planetary surface sample. L2MS, an advanced technique in laser mass spectrometry, is selective to the aromatic organic fraction of a complex sample, which can provide additional sensitivity and confidence in the detection of specific compound structures. Use of a compact two-step laser mass spectrometer prototype has been previously reported to provide specificity to key aromatic species, such as PAHs, nucleobases, and certain amino acids. Recent improvements in this technique have focused on the interaction between the mineral matrix and the

  17. Laser Ablation Electrodynamic Ion Funnel for In Situ Mass Spectrometry on Mars

    NASA Technical Reports Server (NTRS)

    Johnson, Paul V.; Hodyss, Robert P.; Tang, Keqi; Smith, Richard D.

    2012-01-01

    A front-end instrument, the laser ablation ion funnel, was developed, which would ionize rock and soil samples in the ambient Martian atmosphere, and efficiently transport the product ions into a mass spectrometer for in situ analysis. Laser ablation creates elemental ions from a solid with a high-power pulse within ambient Mars atmospheric conditions. Ions are captured and focused with an ion funnel into a mass spectrometer for analysis. The electrodynamic ion funnel consists of a series of axially concentric ring-shaped electrodes whose inside diameters (IDs) decrease over the length of the funnel. DC potentials are applied to each electrode, producing a smooth potential slope along the axial direction. Two radio-frequency (RF) AC potentials, equal in amplitude and 180 out of phase, are applied alternately to the ring electrodes. This creates an effective potential barrier along the inner surface of the electrode stack. Ions entering the funnel drift axially under the influence of the DC potential while being restricted radially by the effective potential barrier created by the applied RF. The net result is to effectively focus the ions as they traverse the length of the funnel.

  18. Analysis of Tropical Forest Fire Emissions Using in Situ Gas Chromatography/Mass Spectrometry during Sambba

    NASA Astrophysics Data System (ADS)

    Minaeian, J.; Lewis, A. C.; Edwards, P. M.; Evans, M. J.; Hopkins, J. R.; Lee, J. D.; Purvis, R.

    2014-12-01

    Vertical atmospheric profiles of volatile organic compounds (VOCs) were made over Amazonia using an in situ gas chromatography/mass spectrometer (GC/MS), including isoprene, methacrolein, methyl vinyl ketone and products of biomass burning such as benzene. Measurements were made in the Amazonian (Rondônia and Amazonas) region during September 2012, a period of extensive biomass burning. Data was obtained between 100m and 8500m from the FAAM BAe 146 research aircraft. Isoprene was observed to be constrained overwhelmingly to the boundary layer (height typically ~2500m) with mean boundary layer mixing ratio of ~2 ppbv and a peak of ~5 ppbv at the lowest flight levels of 100 m. First generation isoprene oxidation products, methyl vinyl ketone and methacrolein, were quantified individually rather than as the sum of the pair, which is more commonly found in the literature. Both MACR and MVK were constrained primarily to the boundary layer, however trace quantities could be seen in the free troposphere to a height of 8000 m. Benzene from biomass burning was observed in both boundary layer and free troposphere, with a peak mixing ratio of ~0.8 ppbv at 750 m. This work will present the spatial distribution of isoprene within the boundary as a function of underlying surface type. The vertical profiles of all species are then compared to representative simulations from the GEOS-Chem chemistry transport model and conclusions drawn on the success of the model in representing emissions and oxidation chemistry.

  19. In situ monitoring of powder blending by non-invasive Raman spectrometry with wide area illumination.

    PubMed

    Allan, Pamela; Bellamy, Luke J; Nordon, Alison; Littlejohn, David; Andrews, John; Dallin, Paul

    2013-03-25

    A 785nm diode laser and probe with a 6mm spot size were used to obtain spectra of stationary powders and powders mixing at 50rpm in a high shear convective blender. Two methods of assessing the effect of particle characteristics on the Raman sampling depth for microcrystalline cellulose (Avicel), aspirin or sodium nitrate were compared: (i) the information depth, based on the diminishing Raman signal of TiO(2) in a reference plate as the depth of powder prior to the plate was increased, and (ii) the depth at which a sample became infinitely thick, based on the depth of powder at which the Raman signal of the compound became constant. The particle size, shape, density and/or light absorption capability of the compounds were shown to affect the "information" and "infinitely thick" depths of individual compounds. However, when different sized fractions of aspirin were added to Avicel as the main component, the depth values of aspirin were the same and matched that of the Avicel: 1.7mm for the "information" depth and 3.5mm for the "infinitely thick" depth. This latter value was considered to be the minimum Raman sampling depth when monitoring the addition of aspirin to Avicel in the blender. Mixing profiles for aspirin were obtained non-invasively through the glass wall of the vessel and could be used to assess how the aspirin blended into the main component, identify the end point of the mixing process (which varied with the particle size of the aspirin), and determine the concentration of aspirin in real time. The Raman procedure was compared to two other non-invasive monitoring techniques, near infrared (NIR) spectrometry and broadband acoustic emission spectrometry. The features of the mixing profiles generated by the three techniques were similar for addition of aspirin to Avicel. Although Raman was less sensitive than NIR spectrometry, Raman allowed compound specific mixing profiles to be generated by studying the mixing behaviour of an aspirin

  20. In situ gamma ray measurements of radionuclides at a disused phosphate mine on the West Coast of South Africa.

    PubMed

    Bezuidenhout, Jacques

    2015-12-01

    High levels of uranium and its radioactive progeny like radium is normally associated with phosphate mining. In Situ gamma ray spectroscopy as a survey tool has been successfully applied to assess radionuclide concentrations in various geographical environments. A transportable and robust gamma ray detection system (GISPI) was therefore employed to determine the concentrations of naturally occurring radionuclides at a disused phosphate mine on the West Coast of South Africa. The concentrations of radium, thorium and potassium were measured and plotted. The measurements showed fairly high concentrations with medians of 320 Bq/kg for (226)Ra, 64 Bq/kg for (232)Th and 390 Bq/kg for (40)K. The highest concentrations were however confined to specific areas of the mine. The effective dose due to gamma irradiation for the various areas of the mine was also estimated and the highest estimated level was 0.45 mSv/y. The article finally draws conclusions as to the origins and impact of the radiation. PMID:26254719

  1. Mass spectrometry imaging: an expeditious and powerful technique for fast in situ lignin assessment in Eucalyptus.

    PubMed

    Araújo, Pedro; Ferreira, Mônica Siqueira; de Oliveira, Diogo Noin; Pereira, Luciano; Sawaya, Alexandra Christine Helena Frankland; Catharino, Rodrigo Ramos; Mazzafera, Paulo

    2014-04-01

    Plant biomass has been suggested as an alternative to produce bioethanol. The recalcitrance of plant biomass to convert cellulose into simpler carbohydrates used in the fermentation process is partially due to lignin, but the standard methods used to analyze lignin composition frequently use toxic solvents and are laborious and time-consuming. MS imaging was used to study lignin in Eucalyptus, since this genus is the main source of cellulose in the world. Hand-cut sections of stems of two Eucalyptus species were covered with silica and directly analyzed by matrix-assisted laser sesorption ionization (MALDI)-imaging mass spectrometry (MS). Information available in the literature about soluble lignin subunits and structures were used to trace their distribution in the sections and using a software image a relative quantification could be made. Matrixes routinely used in MALDI-imaging analysis are not satisfactory to analyze plant material and were efficiently substituted by thin layer chromatography (TLC) grade silica. A total of 22 compounds were detected and relatively quantified. It was also possible to establish a proportion between syringyl and guaiacyl monolignols, characteristic for each species. Because of the simple way that samples are prepared, the MALDI-imaging approach presented here can replace, in routine analysis, complex and laborious MS methods in the study of lignin composition. PMID:24451041

  2. High-speed tandem mass spectrometric in situ imaging by nanospray desorption electrospray ionization mass spectrometry.

    PubMed

    Lanekoff, Ingela; Burnum-Johnson, Kristin; Thomas, Mathew; Short, Joshua; Carson, James P; Cha, Jeeyeon; Dey, Sudhansu K; Yang, Pengxiang; Prieto Conaway, Maria C; Laskin, Julia

    2013-10-15

    Nanospray desorption electrospray ionization (nano-DESI) combined with tandem mass spectrometry (MS/MS), high-resolution mass analysis of the fragment ions (m/Δm = 17 500 at m/z 200), and rapid spectral acquisition enabled simultaneous imaging and identification of a large number of metabolites and lipids from 92 selected m/z windows (±1 Da) with a spatial resolution of better than 150 μm. Mouse uterine sections of implantation sites on day 6 of pregnancy were analyzed in the ambient environment without any sample pretreatment. MS/MS imaging was performed by scanning the sample under the nano-DESI probe at 10 μm/s, while higher-energy collision-induced dissociation (HCD) spectra were acquired for a targeted inclusion list of 92 m/z values at a rate of ∼6.3 spectra/s. Molecular ions and their corresponding fragments, separated by high-resolution mass analysis, were assigned on the basis of accurate mass measurement. Using this approach, we were able to identify and image both abundant and low-abundance isobaric and isomeric species within each m/z window. MS/MS analysis enabled efficient separation and identification of isomeric and isobaric phospholipids that are difficult to separate in full-scan mode. Furthermore, we identified several metabolites associated with early pregnancy and obtained the first 2D images of these molecules. PMID:24040919

  3. In Situ Identification of Plant-Invasive Bacteria with MALDI-TOF Mass Spectrometry

    PubMed Central

    Pflüger, Valentin; Saad, Maged; Vogel, Guido; Tonolla, Mauro; Perret, Xavier

    2012-01-01

    Rhizobia form a disparate collection of soil bacteria capable of reducing atmospheric nitrogen in symbiosis with legumes. The study of rhizobial populations in nature involves the collection of large numbers of nodules found on roots or stems of legumes, and the subsequent typing of nodule bacteria. To avoid the time-consuming steps of isolating and cultivating nodule bacteria prior to genotyping, a protocol of strain identification based on the comparison of MALDI-TOF MS spectra was established. In this procedure, plant nodules were considered as natural bioreactors that amplify clonal populations of nitrogen-fixing bacteroids. Following a simple isolation procedure, bacteroids were fingerprinted by analysing biomarker cellular proteins of 3 to 13 kDa using Matrix Assisted Laser Desorption/Ionization Time of Flight (MALDI-TOF) mass spectrometry. In total, bacteroids of more than 1,200 nodules collected from roots of three legumes of the Phaseoleae tribe (cowpea, soybean or siratro) were examined. Plants were inoculated with pure cultures of a slow-growing Bradyrhizobium japonicum strain G49, or either of two closely related and fast-growing Sinorhizobium fredii strains NGR234 and USDA257, or with mixed inoculants. In the fully automatic mode, correct identification of bacteroids was obtained for >97% of the nodules, and reached 100% with a minimal manual input in processing of spectra. These results showed that MALDI-TOF MS is a powerful tool for the identification of intracellular bacteria taken directly from plant tissues. PMID:22615938

  4. High-Speed Tandem Mass Spectrometric in Situ Imaging by Nanospray Desorption Electrospray Ionization Mass Spectrometry

    SciTech Connect

    Lanekoff, Ingela T.; Burnum-Johnson, Kristin E.; Thomas, Mathew; Short, Joshua TL; Carson, James P.; Cha, Jeeyeon; Dey, Sudhansu K.; Yang, Pengxiang; Prieto Conaway, Maria C.; Laskin, Julia

    2013-10-15

    Nanospray desorption electrospray ionization (nano-DESI) combined with tandem mass spectrometry (MS/MS), high-resolution mass analysis (m/m=17,500 at m/z 200), and rapid spectral acquisition enabled simultaneous imaging and identification of more than 300 molecules from 92 selected m/z windows (± 1 Da) with a spatial resolution of better than 150 um. Uterine sections of implantation sites on day 6 of pregnancy were analyzed in the ambient environment without any sample pre-treatment. MS/MS imaging was performed by scanning the sample under the nano-DESI probe at 10 um/s while acquiring higher-energy collision-induced dissociation (HCD) spectra for a targeted inclusion list of 92 m/z values at a rate of ~6.3 spectra/s. Molecular ions and their corresponding fragments, separated using high-resolution mass analysis, were assigned based on accurate mass measurement. Using this approach, we were able to identify and image both abundant and low-abundance isobaric species within each m/z window. MS/MS analysis enabled efficient separation and identification of isobaric sodium and potassium adducts of phospholipids. Furthermore, we identified several metabolites associated with early pregnancy and obtained the first 2D images of these molecules.

  5. In-situ Observations of Gamma-ray Production in Thunderstorms

    NASA Astrophysics Data System (ADS)

    Eack, Kenneth; Aulich, Graydon; Winn, William; Edens, Harald

    2016-04-01

    The majority of the reported observations of energetic radiation from thunderstorms have come from either ground-based or satellite-based measurements. In order to better understand the physical conditions necessary for the production of fast electrons and gamma-rays, measurements are needed near the production regions inside or above the thunderstorm. Three different measurements are of particular interest. First, gamma-rays produced by the quasi-static electric-field may provide details about the physics of runaway electrons that would be difficult to determine from measurements of transient phenomena, such as lightning and terrestrial gamma-ray flashes (TGFs). Second, what process inside the thunderstorm is responsible for TGFs? Recent ground-bsed studies have pointed to the upward negative leader in inter-cloud lightning as a possible source. Finally, the initiation of lightning appears to be a problem in light of the relatively weak (about 10% of the classical breakdown threshold) electric fields observed inside thunderstorms. Since these field strengths are adequate for runaway electrons, they have been proposed as a possible source for the initial breakdown in lightning. In this paper, we will present observations from balloon-borne gamma-ray detectors and electric-field sensors, as well as ground based instruments like the lightning mapping array (LMA) in effort to examine these areas of interest.

  6. Planetary In Situ Sample Analysis with Tandem Two-Step Laser Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Brinckerhoff, W. B.; Getty, S. A.; Cornish, T. J.; Ecelberger, S. A.; Li, X.; Merrill Floyd, M. A.; Arevalo, R.; Elsila, J.; Callahan, M. P.

    2012-12-01

    Future surface missions to comets and outer solar system satellites such as Europa, Enceladus, and Titan will benefit strongly from investigations that can detect a wide range of organics in complex sample mixtures and ices, as well as determine the structure of selected molecules, to provide insight into their origin and evolution. At the same time, such missions are likely to be among the most highly constrained in mass and power resources, particularly those flown within the tightly focused Discovery and New Frontiers programs. Techniques requiring minimal or no sample manipulation or preparation may be needed to reduce complexity. Pulsed laser-based mass spectrometry may satisfy such requirements, with total instrument masses potentially less than 5 kg, particularly where analysis of higher-molecular weight, nonvolatile species is a priority objective. Prototype flight-compatible mass spectrometers under active development in our lab are based on direct ultraviolet Nd:YAG laser desorption and ionization (LDI) of solid samples under high vacuum. Prompt ions from a single few ns-duration laser pulse are accelerated into a compact time-of-flight mass spectrometer (TOF-MS). Both inorganic species including elements and oxides such as M_xO_y (M = Mg, Al, Cl, Ca, Fe; x, y = 1-4) from the mineral matrix as well as organics with molecular weights up to several kDa are readily detected over a range of laser intensities. To improve our ability to distinguish among peaks and patterns in the often-complex LDI spectra obtained from natural samples, we have recently begun systematically testing several critical instrument enhancements. First, by moving the common voltage bias of the ion flight tube and detector to a common negative potential, we are able to switch between positive and negative ion detection modes with only electrostatic switching. Inter-comparison of cation and anion spectra can provide highly diagnostic information on both inorganic (e.g., Na+ and K+ vs. Cl

  7. Active Neutron and Gamma Ray Instrumentation for In Situ Planetary Science Applications

    NASA Technical Reports Server (NTRS)

    Parsons, A.; Bodnarik, J.; Evans, L.; Floyd, S.; Lim, L.; McClanahan, T.; Namkung, M.; Schweitzer, J.; Starr, R.; Trombka, J.

    2010-01-01

    The Pulsed Neutron Generator-Gamma Ray And Neutron Detectors (PNG-GRAND) experiment is an innovative application of the active neutron-gamma ray technology so successfully used in oil field well logging and mineral exploration on Earth. The objective of our active neutron-gamma ray technology program at NASA Goddard Space Flight Center (NASA-GSFC) is to bring the PNG-GRAND instrument to the point where it can be flown on a variety of surface lander or rover missions to the Moon, Mars, Menus, asteroids, comets and the satellites of the outer planets. Gamma-Ray Spectrometers (GRS) have been incorporated into numerous orbital planetary science missions and, especially its the case of the Mars Odyssey GRS, have contributed detailed maps of the elemental composition over the entire surface of Mars. However, orbital gamma ray measurements have low spatial sensitivity (100's of km) due to their low surface emission rates from cosmic rays and subsequent need to be averaged over large surface areas. PNG-GRAND overcomes this impediment by incorporating a powerful neutron excitation source that permits high sensitivity surface and subsurface measurements of bulk elemental compositions. PNG-GRAND combines a pulsed neutron generator (PNG) with gamma ray and neutron detectors to produce a landed instrument to determine subsurface elemental composition without needing to drill into a planet's surface a great advantage in mission design. We are currently testing PNG-GRAND prototypes at a unique outdoor neutron instrumentation test facility recently constructed at NASA/GSFC that consists of a 2 m x 2 in x 1 m granite structure placed outdoors in an empty field. Because an independent trace elemental analysis has been performed on the material, this granite sample is a known standard with which to compare both Monte Carlo simulations and our experimentally measured elemental composition data. We will present data from operating PNG-GRAND in various experimental configurations on a

  8. A Team Approach to the Development of Gamma Ray and x Ray Remote Sensing and in Situ Spectroscopy for Planetary Exploration Missions

    NASA Technical Reports Server (NTRS)

    Trombka, J. I.; Floyd, S.; Ruitberg, A.; Evans, L.; Starr, R.; Metzger, A.; Reedy, R.; Drake, D.; Moss, C.; Edwards, B.

    1993-01-01

    An important part of the investigation of planetary origin and evolution is the determination of the surface composition of planets, comets, and asteroids. Measurements of discrete line X-ray and gamma ray emissions from condensed bodies in space can be used to obtain both qualitative and quantitative elemental composition information. The Planetary Instrumentation Definition and Development Program (PIDDP) X-Ray/Gamma Ray Team has been established to develop remote sensing and in situ technologies for future planetary exploration missions.

  9. In-situ gamma-ray assay of the west cell line in the 235-F plutonium fuel form facility

    SciTech Connect

    Couture, A. H.; Diprete, D.

    2014-09-01

    On August 29th, 2013, scientists from SRNL took a series of in-situ gamma-ray measurements in the maintenance trench beneath Cells 6-9 on the west line of the PuFF facility using an uncollimated, highpurity germanium detector. The detector efficiency was estimated using a combination of MCNP simulations and empirical measurements. Data analysis was performed using three gamma-rays emitted by Pu-238 (99.85 keV, 152.7 keV, and 766.4 keV) providing three independent estimates of the mass of Pu-238 holdup in each of the cells. The weighted mean of these three results was used as the best estimate of Pu-238 holdup in the West Cell Line of PuFF. The results of the assay measurements are found in the table below along with the results from the scoping assay performed in 2006. All uncertainties in this table (as well as the rest of the report) are given as 1σ. The total holdup in the West Cell Line was 2.4 ± 0.7 grams. This result is 0.6 g higher than the previous estimate, a 0.4σ difference.

  10. Use of a Shielded High Resolution Gamma Spectrometry System to Segregate LLW from Contact Handleable ILW Containing Plutonium - 13046

    SciTech Connect

    Lester, Rosemary; Wilkins, Colin; Chard, Patrick; Jaederstroem, Henrik; LeBlanc, Paul; Mowry, Rick; MacDonald, Sanders; Gunn, William

    2013-07-01

    Dounreay Site Restoration Limited (DSRL) have a number of drums of solid waste that may contain Plutonium Contaminated Material. These are currently categorised as Contact Handleable Intermediate Level Waste (CHILW). A significant fraction of these drums potentially contain waste that is in the Low Level Waste (LLW) category. A Canberra Q2 shielded high resolution gamma spectrometry system is being used to quantify the total activity of drums that are potentially in the LLW category in order to segregate those that do contain LLW from CHILW drums and thus to minimise the total volume of waste in the higher category. Am-241 is being used as an indicator of the presence of plutonium in the waste from its strong 59.54 keV gamma-ray; a knowledge of the different waste streams from which the material originates allows a pessimistic waste 'fingerprint' to be used in order to determine an upper limit to the activities of the weak and non-gamma-emitting plutonium and associated radionuclides. This paper describes the main features of the high resolution gamma spectrometry system being used by DSRL to perform the segregation of CHILW and LLW and how it was configured and calibrated using the Canberra In-Situ Object Counting System (ISOCS). It also describes how potential LLW drums are selected for assay and how the system uses the existing waste stream fingerprint information to determine a reliable upper limit for the total activity present in each measured drum. Results from the initial on-site commissioning trials and the first measurements of waste drums using the new monitor are presented. (authors)

  11. Characterization of carbon surface chemistry by combined temperature programmed desorption with in situ X-ray photoelectron spectrometry and temperature programmed desorption with mass spectrometry analysis.

    PubMed

    Brender, Patrice; Gadiou, Roger; Rietsch, Jean-Christophe; Fioux, Philippe; Dentzer, Joseph; Ponche, Arnaud; Vix-Guterl, Cathie

    2012-03-01

    The analysis of the surface chemistry of carbon materials is of prime importance in numerous applications, but it is still a challenge to identify and quantify the surface functional groups which are present on a given carbon. Temperature programmed desorption with mass spectrometry analysis (TPD-MS) and X-ray photoelectron spectroscopy with an in situ heating device (TPD-XPS) were combined in order to improve the characterization of carbon surface chemistry. TPD-MS analysis allowed the quantitative analysis of the released gases as a function of temperature, while the use of a TPD device inside the XPS setup enabled the determination of the functional groups that remain on the surface at the same temperatures. TPD-MS results were then used to add constraints on the deconvolution of the O1s envelope of the XPS spectra. Furthermore, a better knowledge of the evolution of oxygen functional groups with temperature during a thermal treatment could be obtained. Hence, we show here that the combination of these two methods allows to increase the reliability of the analysis of the surface chemistry of carbon materials. PMID:22242697

  12. Gamma irradiation testing of montan wax barrier materials for in-situ waste containment

    SciTech Connect

    Soo, P.; Heiser, J.

    1996-02-01

    A scoping study was carried out to quantify the potential use of a montan wax as a barrier material for subsurface use. If it possesses resistance to chemical and structural change, it could be used in a barrier to minimize the migration of contaminants from their storage or disposal locations. Properties that were evaluated included hardness, melting point, molecular weight, and biodegradation as a function of gamma radiation dose. The main emphasis was to quantify the wax`s long-term ability to withstand radiation-induced mechanical, chemical, and microbial degradation.

  13. Low level measurement of (60)Co by gamma ray spectrometry using γ-γ coincidence.

    PubMed

    Paradis, H; de Vismes Ott, A; Luo, M; Cagnat, X; Piquemal, F; Gurriaran, R

    2016-03-01

    This paper presents the latest development of the laboratory to measure the natural and artificial massic activities in environmental samples. The measurement method of coincident emitters by gamma-gamma coincidence using an anti-Compton device and its digital electronics is described. Results obtained with environmental samples are shown. Despite its low efficiency, this method decreases detection limits of (60)Co for certain samples compared to conventional gamma-ray spectrometry due to its very low background. PMID:26682892

  14. Dislocation motion in {gamma} TiAl by in situ straining experiments in the HVEM

    SciTech Connect

    Messerschmidt, U.; Bartsch, M.; Haeussler, D.; Hattenhauer, R.; Aindow, M.; Jones, I.P.

    1995-08-01

    Micro-tensile specimens of coarse-grained Ti52at%Al crystals have been deformed in situ in a high voltage electron microscope at room temperature. In addition to some twinning, ``simple`` 1/2{l_angle}110] dislocations as well as super dislocations were moving, with the simple dislocations prevailing even if their orientation factor is lower than that of the super dislocations. Both types of dislocations are pinned, probably by small precipitates having a distance along the dislocations of about 100 nm. The precipitates consist most probably of Al{sub 2}O{sub 3}. Under stress, the dislocations bow out between the obstacles. The bowing is stronger for 1/2{l_angle}110] dislocations. An effective stress of about 41 MPa is estimated from their curvature. The kinematic behavior of the dislocations is in accord with precipitation hardening. The dislocations are generated by the double-cross slip mechanism. Their density within the slip bands corresponds to a long-range internal stress of about 40 MPa. These data are consistent with the flow stress of PST crystals in the easy orientation, taken from the literature.

  15. Effect of chromosome size on aberration levels caused by gamma radiation as detected by fluorescence in situ hybridization.

    PubMed

    Pandita, T K; Gregoire, V; Dhingra, K; Hittelman, W N

    1994-01-01

    Fluorescence in situ hybridization (FISH) is a powerful technique for detecting genomic alterations at the chromosome level. To study the effect of chromosome size on aberration formation, we used FISH to detect initial damage in individual prematurely condensed chromosomes (PCC) of gamma-irradiated G0 human cells. A linear dose response for breaks and a nonlinear dose response for exchanges was obtained using a chromosome 1-specific probe. FISH detected more chromosome 1 breaks than expected from DNA based extrapolation of Giemsa stained PCC preparations. The discrepancy in the number of breaks detected by the two techniques raised questions as to whether Giemsa staining and FISH differ in their sensitivities for detecting breaks, or is chromosome 1 uniquely sensitive to gamma-radiation. To address the question of technique sensitivity, we determined total chromosome damage by FISH using a total genomic painting probe; the results obtained from Giemsa-staining and FISH were nearly identical. To determine if chromosome 1 was uniquely sensitive, we selected four different sized chromosomes for paint probes and scored them for gamma-ray induced aberrations. In these studies the number of chromosome breaks per unit DNA increased linearly with an increase in the DNA content of the chromosomes. However, the number of exchanges per unit of DNA did not increase with an increase in chromosome size. This suggests that chromosome size may influence the levels of aberrations observed. Extrapolation from measurements of a single chromosome's damage to the whole genome requires that the relative DNA content of the measured chromosome be considered. PMID:8039428

  16. Deformation and fracture behavior of Ni-Mo-Al(gamma/gamma prime-alpha) in situ composite

    NASA Technical Reports Server (NTRS)

    Sriramamurthy, A. M.; Tewari, S. N.

    1984-01-01

    Tensile properties of a directionally solidified (DS) eutectic alloy of the nominal composition Ni-33 Mo-5.7 Al (weight percent) have been investigated both at room temperature and elevated temperatures. The microstructure-mechanical property relationship has been studied for the alloy both in the as-DS and heat-treated conditions. Changes in the yield strength, the work hardening behavior, and the fracture morphology have been explained in terms of the microstructural changes due to the heat treatment. The yield drops observed have been attributed to the microdebonding due to the possible segregation of impurities at the fiber-matrix interface, and partly to the strain aging. The deformation mechanism has been identified to be the cutting of gamma prime particles.

  17. Automated in situ trace element analysis of silicate materials by laser ablation inductively coupled plasma mass spectrometry.

    PubMed

    Chen, Z; Canil, D; Longerich, H P

    2000-09-01

    This paper describes the automated in situ trace element analysis of solid materials by laser ablation (LA) inductively coupled plasma mass spectrometry (ICP-MS). A compact computer-controlled solid state Nd:YAG Merchantek EO UV laser ablation (LA) system has been coupled with the high sensitivity VG PQII S ICP-MS. A two-directional communication was interfaced in-house between the ICP-MS and the LA via serial RS-232 port. Each LA-ICP-MS analysis at a defined point includes a 60 s pre-ablation delay, a 60 s ablation, and a 90 s flush delay. The execution of each defined time setting by LA was corresponding to the ICP-MS data acquisition allowing samples to be run in automated cycle sequences like solution auto-sampler ICP-MS analysis. Each analytical cycle consists of four standards, one control reference material, and 15 samples, and requires about 70 min. Data produced by Time Resolved Analysis (TRA) from ICP-MS were later reduced off-line by in-house written software. Twenty-two trace elements from four reference materials (NIST SRM 613, and fused glass chips of BCR-2, SY-4, and G-2) were determined by the automated LA-ICP-MS method. NIST SRM 610 or NIST SRM 613 was used as an external calibration standard, and Ca as an internal standard to correct for drift, differences in transport efficiency and sampling yield. Except for Zr and Hf in G-2, relative standard deviations for all other elements are less than 10%. Results compare well with the data reported from literature with average limits of detection from 1 ng x g(-1) to 455 ng x g(-1) and less than 100 ng x g(-1) for most trace elements. PMID:11220835

  18. Determination of uranium in aqueous attenuating samples using gamma-ray spectrometry.

    PubMed

    Agarwal, Chhavi; Kalsi, P C; Mhatre, A; Goswami, A

    2007-12-01

    In the present work, a method for determination of uranium concentration in aqueous solution in standard geometry from attenuating samples has been developed based on modification of the empirical approach of Venkataraman and Croft [2003. Determination of plutonium mass using gamma-ray spectrometry. Nucl. Instrum. Methods Phys. Res. A 505, 527-530]. The method makes use of the multiple gamma (gamma)-rays emitted by 235U and depends on the empirical relation between apparent mass of the sample and gamma-ray energy. It was possible to determine uranium concentration in the range of 12-400mg/ml rapidly by this method without applying transmission corrections. PMID:17768057

  19. Monte carlo simulation of in situ gamma-spectra recorded by NaI (Tl) detector in the marine environment

    NASA Astrophysics Data System (ADS)

    Wang, Yiming; Zhang, Yingying; Wu, Ning; Wu, Bingwei; Liu, Yan; Cao, Xuan; Wang, Qian

    2015-06-01

    To develop a NaI (Tl) detector for in situ radioactivity monitoring in the marine environment and enhance the confidence of the probability of the gamma-spectrum analysis, Monte Carlo simulations using the Monte Carlo N-Particle ( MNCP ) code were performed to provide the response spectra of some interested radionuclides and the background spectra originating from the natural radionuclides in seawater recorded by a NaI (Tl) detector. A newly developed 75 mm × 75 mm NaI (Tl) detector was calibrated using four reference radioactive sources 137Cs, 60Co, 40K and 54Mn in the laboratory before the field measurements in seawater. A simulation model was established for the detector immersed in seawater. The simulated spectra were all broadened with Gaussian pulses to reflect the statistical fluctuations and electrical noise in the real measurement. The simulated spectra show that the single-energy photons into the detector are mostly scattering low-energy photons and the high background in the low energy region mainly originates from the Compton effect of the high energy ?-rays of natural radionuclides in seawater. The simulated background spectrum was compared with the experimental one recorded in field measurement and they seem to be in good agreement. The simulation method and spectra can be used for the accurate analysis of the filed measurement results of low concentration radioactivity in seawater.

  20. Minimum Detectable Activity in gamma spectrometry and its use in low level activity measurements.

    PubMed

    Done, L; Ioan, M-R

    2016-08-01

    In this paper there are described three different algorithms of Minimum Detectable Activity (MDA) calculus, and its use in high resolution gamma spectrometry. In the first part, few introductive theoretical aspects related to the MDA are presented. Further, the theory was applied to real gamma rays spectrometry measurements and the results were compared with the activities reference values. Two different gamma spectrometry systems, both of them using High Purity Germanium (HPGe) detectors, but having different efficiencies, were used. Samples having different geometries and radionuclides content were measured. The measured samples were made by dissolving of some acids containing anthropogenic radionuclides in water, obtaining a density of 1g/cm(3). Choosing this type of matrix was done because of its high homogeneity. PMID:27172893

  1. QUALITY CONTROL FOR ENVIRONMENTAL MEASUREMENTS USING GAMMA-RAY SPECTROMETRY

    EPA Science Inventory

    This report describes the quality control procedures, calibration, collection, analysis, and interpretation of data in measuring the activity of gamma ray-emitting radionuclides in environmental samples. Included in the appendices are basic data for selected gamma ray-emitting ra...

  2. High-pressure xenon detectors for gamma-ray spectrometry

    PubMed

    Dmitrenko; Gratchev; Ulin; Uteshev; Viasik

    2000-03-01

    The main results of long-term research on compressed xenon detector properties conducted at the laboratory of cosmic physics of MEPhI are given along with a description of the latest gamma-ray spectrometers based on this work. It is shown that using xenon as working substance, it is possible to create a gamma-ray spectrometer with high energy resolution. The construction and the main physical, technical and operation performances of xenon gamma-ray spectrometers based on ionization chambers of various configurations are described. For a gamma-ray spectrometer with a cylindrical ionization chamber and shielding grid, an energy resolution of about 14 keV (10 keV intrinsic resolution) for gamma-ray line of 662 keV is obtained. The characteristics of these detectors allow one to apply them in various fields of science and engineering, moreover, their good spectrometric properties provide the opportunity to use them for metrology measurements. PMID:10724434

  3. ADONIS, high count-rate HP-Ge {gamma} spectrometry algorithm: Irradiated fuel assembly measurement

    SciTech Connect

    Pin, P.; Barat, E.; Dautremer, T.; Montagu, T.; Normand, S.

    2011-07-01

    ADONIS is a digital system for gamma-ray spectrometry, developed by CEA. This system achieves high count-rate gamma-ray spectrometry with correct dynamic dead-time correction, up to, at least, more than an incoming count rate of 3.10{sup 6} events per second. An application of such a system at AREVA NC's La Hague plant is the irradiated fuel scanning facility before reprocessing. The ADONIS system is presented, then the measurement set-up and, last, the measurement results with reference measurements. (authors)

  4. The Dortmund Low Background Facility - Low-background gamma ray spectrometry with an artificial overburden.

    PubMed

    Gastrich, Holger; Gößling, Claus; Klingenberg, Reiner; Kröninger, Kevin; Neddermann, Till; Nitsch, Christian; Quante, Thomas; Zuber, Kai

    2016-06-01

    The Dortmund Low Background Facility is an instrument for low-level gamma ray spectrometry with an artificial overburden of ten meters of water equivalent, an inner shielding, featuring a neutron absorber, and an active muon veto. An integral background count rate between 40keV and 2700keV of (2.528±0.004)counts/(kgmin) enables low-background gamma ray spectrometry with sensitivities in the range of some 10mBq/kg within a week of measurement time. PMID:27082973

  5. In situ identification of organic components of ink used in books from the 1900s by atmospheric pressure matrix assisted laser desorption ionization mass spectrometry

    NASA Astrophysics Data System (ADS)

    Giurato, Laura; Candura, Andrea; Grasso, Giuseppe; Spoto, Giuseppe

    2009-11-01

    This paper describes the use of atmospheric pressure/matrix assisted laser desorption ionization-mass spectrometry (AP/MALDI-MS) as a spatially resolved analytical technique for the study of organic components of inks used to print coloured parts of ancient books. The possibility to operate at atmospheric pressure makes MALDI-MS a new in situ micro-destructive diagnostic tool suitable for analysing samples in air, simplifying the investigation of the organic components of artistic and archaeological objects. In this work, several organic dyes and pigments were identified in situ by analysing different coloured areas of books printed in the years 1911 and 1920. The detected colouring materials, which were available since the 1890s, were often identified as a mixture, confirming the typical procedures used in the lithographic printing processes. The matrix deposition and the laser desorption process did not cause visible alteration of the sample surface.

  6. Comparison between in situ and ex situ gamma measurements on land areas within a decommissioning nuclear site: a case study at Dounreay.

    PubMed

    Rostron, Peter D; Heathcote, John A; Ramsey, Michael H

    2014-09-01

    Measurements made in situ with gamma detectors and ex situ measurements of soil samples in a laboratory can have complementary roles in the assessment of radioactively contaminated land on decommissioning nuclear sites. Both in situ and ex situ methods were used to characterize (137)Cs contamination within an area at the Dounreay site in Scotland. The systematic difference (bias) between estimates of the mean activity concentration was found to be non-significant when in situ measurements were interpreted using a linear depth model, based on ex situ measurements made at two different depths. An established method of evaluating the random components of measurement uncertainty was used. The random component of analytical uncertainty in the in situ measurements, made in field conditions, was found to exceed that for the ex situ measurements, made in the controlled conditions of a laboratory. However, contamination by the target radionuclide was found to be heterogeneous over small spatial scales. This resulted in significantly higher levels of random sampling uncertainty in individual ex situ measurements. As in situ measurements are substantially less costly, a greater number of measurements can be made, which potentially reduces the uncertainty on the mean. Providing the depth profile of contaminants can be modelled with confidence, this can enable estimates of mean activity concentration over an averaging area to be made with lower overall uncertainties than are possible using ex situ methods. PMID:24938421

  7. In-situ gamma-ray assay of the east cell line in the 235-F Plutonium fuel form facility

    SciTech Connect

    Diprete, D.

    2015-08-21

    On September 17th -19th , 2013, scientists from SRNL took a series of in-situ gamma-ray measurements in the maintenance trench beneath Cells 1-5 on the east line of the PuFF facility using a well-collimated, high-purity germanium detector. The cell interiors were assayed along with the furnaces and storage coolers that protrude beneath the cells. The detector efficiency was estimated using a combination of MCNP simulations and empirical measurements. Data analysis was performed using three gamma-rays emitted by Pu-238 (99.85 keV, 152.7 keV, and 766.4 keV) providing three independent estimates of the mass of Pu-238 holdup in each of the cells. The weighted mean of these three results was used as the best estimate of Pu-238 holdup in the East Cell Line of PuFF. The results of the assay measurements are found in the table on the following page along with the results from the scoping assay performed in 2006. All uncertainties in this table (as well as the rest of the report) are reported at 1σ. Summing the assay results and treating MDAs as M238Pu= 0 ± MDA, the total holdup in the East Cell Line was 240 ± 40 grams. This result is 100 grams lower than the previous estimate, a 0.55σ difference. The uncertainty in the Pu-238 holdup is also reduced substantially relative to the 2006 scoping assay. However, the current assay results are in agreement with the 2006 scoping assay results due to the large uncertainty associated with the 2006 scoping assays. The current assay results support the conclusion that the 2006 results bound the Pu-238 mass in Cells 1-5. These results should be considered preliminary since additional measurements of the East Cell line are scheduled for 2017 and 2018. Those measurements will provide detailed information about the distribution of Pu-238 in the cells to be used to refine the results of the current assay.

  8. Pulser injection with subsequent removal for gamma-ray spectrometry

    DOEpatents

    Hartwell, Jack K.; Goodwin, Scott G.; Johnson, Larry O.; Killian, E. Wayne

    1990-01-01

    An improved system for gamma-ray spectroscopy characterized by an interface module that controls the injection of electronic pulses as well as separation logic that enables storage of pulser events in a region of the spectrum of a multichannel analyzer distinct from the region reserved for storage of gamma-ray events. The module accomplishes this by tagging pulser events (high or low) injected into the amplification circuitry, adding an offset to the events so identified at the time the events are at the output of the analog to digital converter, and storing such events in the upper portion of the spectrum stored in the multichannel analyzer. The module can be adapted for use with existing gamma-ray spectroscopy equipment to provide for automatic analyses of radioisotopes.

  9. Characterization of coal and charcoal by alpha-particle and gamma-ray spectrometry

    NASA Astrophysics Data System (ADS)

    Carrasco Lourtau, A. M.; Rubio Montero, M. P.; Jurado Vargas, M.

    2015-11-01

    Although coal and charcoal have similar physical and chemical characteristics, there are several crystallographic procedures used to distinguish and characterize them. But if the matrix is crushed, there is no standard procedure to distinguish coal from charcoal. In this work, a procedure to characterize coal and charcoal samples based on the radioactive content is proposed. The first assay is by gamma-ray spectrometry, which allows a part of the radioactive content to be determined rapidly and non-destructively. Then, alpha-particle spectrometry is applied to assay the content of those radionuclides which are difficult to determine precisely by gamma-ray spectrometry. This second technique requires prior chemical purification of the carbon sample in order to separate the corresponding radionuclides of interest.

  10. Latent transforming growth factor beta1 activation in situ: quantitative and functional evidence after low-dose gamma-irradiation

    NASA Technical Reports Server (NTRS)

    Ehrhart, E. J.; Segarini, P.; Tsang, M. L.; Carroll, A. G.; Barcellos-Hoff, M. H.; Chatterjee, A. (Principal Investigator)

    1997-01-01

    reciprocal shift in immunoreactivity as evidence of activation, and implicate TGF-beta as a mediator of tissue response to ionizing radiation. The sensitivity of activation to low radiation doses points to a potential role for TGF-beta in orchestrating tissue response to oxidative stress. As such, radiation may be useful as a probe to delineate the consequences of latent TGF-beta activation in situ.

  11. Gamma ray spectrometry of LDEF samples at SRL

    NASA Astrophysics Data System (ADS)

    Winn, W. G.

    1991-07-01

    A total of 31 samples from the Long Duration Exposure Facility (LDEF), including materials of aluminum, vanadium, and steel trunnions were analyzed by ultra-low-level gamma spectroscopy. The study quantified particle induced activations of Na-22, Sc-46, Cr-51, Mn-54, Co-56, Co-57, Co-58, and Co-60. The samples of trunnion sections exhibited increasing activity toward the outer end of the trunnion and decreasing activity toward its radial center. The trunnion sections did not include end pieces, which have been reported to collect noticeable Be-7 on their leading surfaces. No significant Be-7 was detected in the samples analyzed. The Underground Counting Facility at Savannah River Laboratory (SRL) was used in this work. The facility is 50 ft. underground, constructed with low-background shielding materials, and operated as a clean room. The most sensitive analyses were performed with a 90 percent efficient HPGe gamma-ray detector, which is enclosed in a purged active/passive shield. Each sample was counted for one to six days in two orientations to yield more representative average activities for the sample. The non-standard geometries of the LDEF samples prompted the development of a novel calibration method, whereby the efficiency about the samples surfaces (measured with point sources) predicted the efficiency for the bulk sample.

  12. Advances in room-temperature solid-state gamma-ray spectrometry

    SciTech Connect

    Iwanczyk, J.S.

    1983-01-01

    This article presents a review and analysis of different concepts of gamma-ray spectrometry using room-temperature solid-state detectors. The classical approach involving the use of a charge-sensitive preamplifier and attempting to collect all the ionization charge produced by the gamma ray is analyzed and discussed in terms of the charge transport parameters of the most promising compound semiconductor materials. It is concluded that compound semiconductor detector materials having a large disparity between the ..mu.. tau products for electrons and holes (such as HgI/sub 2/ and CdTe) will have rather poor energy resolution if the classical method of spectrometry requiring full charge collection is employed. 30 references.

  13. In situ γ-ray spectrometry in the marine environment using full spectrum analysis for natural radionuclides.

    PubMed

    Androulakaki, E G; Kokkoris, M; Tsabaris, C; Eleftheriou, G; Patiris, D L; Pappa, F K; Vlastou, R

    2016-08-01

    The Full Spectrum Analysis approach was applied to obtain activity concentration estimations for in situ measurements in the marine environment. The 'standard spectra' were reproduced using the MCNP-CP code. In order to extract the activity concentrations, χ(2) minimization calculations were performed by implementing the MINUIT code. The method was applied to estimate the activity concentrations for measurements in the marine environment in three different test cases. The estimated activity concentrations were in good agreement with the experimentally derived ones within uncertainties. PMID:27213807

  14. Pulsed Bremsstrahlung Interrogation with Photoneutron - Gamma-Ray Spectrometry for Nondestructive Evaluation

    NASA Astrophysics Data System (ADS)

    Jones, James Litton

    A novel photoneutron-based nondestructive evaluation (NDE) technique which does not require a radioactive neutron source is presented. Some unique features of this technique include: 1) pulsed interrogation neutron production within, or very near, an inspected object, 2) spectrum tailoring of the source neutrons, and 3) compatibility with many existing high-energy, commercial x-ray inspection devices. Basic concept feasibility was first established by numerical methods. The pulsed photoneutron inspection technique performs nondestructive elemental analysis using gamma-ray spectrometry. Highly penetrating bremsstrahlung photons are produced by a pulsed electron accelerator capable of producing up to 16-MeV electrons. The photoneutrons are generated by the bremsstrahlung photons interacting with an inspected object and near-by beryllium metal. The interactions of the neutrons within an inspected item result in the emission of elemental characteristic gamma-rays. Spectrometry is performed by analyzing the gamma -rays acquired between accelerator pulses. A unique fast detection and acquisition system, using two 5.08 x 5.08 -cm organic scintillators, acquires gamma-ray emissions within 100 ns of each accelerator pulse. The fast system is capable of processing individual gamma-ray signals at count rates up to 40 MHz between accelerator pulses with a repetition rate up to 1 kHz. The system incorporates a unique x-ray flash recovery method which allows individual gamma-ray detection as soon as 75 ns after the start of each x-ray flash occurring within the detector. Conventional detection and data acquisition systems are used to acquire gamma-ray spectra for the time period between 1000 ns and the next accelerator pulse. Operational tests using a 30-ps pulse width, electron accelerator demonstrated the x-ray flash recovery methodology, gamma-ray detection, and data acquisition. Although, gamma -ray spectrometry performance was limited by x-ray flash -induced gain shifts in

  15. Determination of impurities in (124)I samples by high resolution gamma spectrometry.

    PubMed

    de Almeida, M C M; da Silva, R L; Delgado, J U; Poledna, R; de Araújo, M T F; Laranjeira, A S; de Veras, E; Braghirolli, A M S; dos Santos, G R; Lopes, R T

    2016-03-01

    (124)I is a radionuclide used in the diagnosis of tumors. The National Health Agency requires identification and activity measurement of impurities. Using gamma spectrometry with an efficiency calibrated high-purity germanium detector, impurities (125)I and (126)I in an (1)(24)I production sample were identified. Activity ratios of (125)I and (126)I to (124)I were approximately 0.5% and 98%, respectively. PMID:26653211

  16. The potential of gamma-ray spectrometry as supplementary information for mapping central European soils

    NASA Astrophysics Data System (ADS)

    Schuler, U.; Bock, M.; Baritz, R.; Willer, J.; Pickert, E.; Kardel, K.; Herrmann, L.

    2012-04-01

    Permanently updated soil maps are needed inter alia for the prediction of landslide hazards, flooding and drought effects, land degradation monitoring, and precision farming. Since comprehensive and intensive field mapping is not affordable, alternative mapping approaches are required. A promising tool, with quite unrecognised potential for modern soil science is gamma-ray spectrometry. As the radioelements potassium, thorium and uranium respond differently to soil forming processes, it should be possible to infer from their concentration on weathering status, and after calibration on soil properties and types. This paper aims to investigate the potential of airborne gamma spectrometry for mapping of central European soils and soil properties. The study was conducted for a test site in Southern Saxony, Germany, 140*85 km wide, representing diverse soil landscapes. Seven different petrographic training and validation areas were chosen each. To assess the potential of gamma-ray spectrometry as additional data layer, predictions were carried out (i) with and (ii) without radiometric data. The outputs were compared with independent soil information of the validation areas. Both prediction runs used the following predictors: elevation, slope, curvature, planform curvature, profile curvature, terrain ruggedness index, relative altitude, vertical distance above drainage network, wetness index, and convergence index. As additional predictor parent material derived from a reclassification of the official geological map (1:1M scale) was used. As radiometric properties potassium, thorium and uranium were used. The radiometric raster datasets were generated by universal kriging using relative altitude as covariate. Training and validation datasets were selected from a comprehensive dataset representing more than 14.000 point data. Point data include soil types and substrates, and for more than 800 sites soil profiles with analysed texture, pH, exchangeable cations, nutrients

  17. Cadium-Zinc-Telluride (CZT) Gamma Ray Spectrometry

    SciTech Connect

    William Quam

    2001-09-01

    This report describes CZT crystals and their use in large arrays for generation of gamma ray spectra. Laboratory spectra will be shown together with spectra accumulated by various battery powered portable instruments (see Appendix A). One of these portable instruments was specifically constructed to minimize power consumption and yet provide reasonable isotope identification capability. Detailed data will be presented covering gamma energy resolution, gamma peak shapes, system background, and detector efficiency. Nearly all data were taken with very small crystals of CZT; cubes 5 mm on a side. A few spectra will be presented from cylindrical crystals of about the same size (see Appendix A). The small crystal size leads to low counting rates and extended counting times for reliable isotope identification. We have addressed this problem by using arrays of CZT crystals, initially two crystals and, at present, arrays of eight crystals. Data will be shown relating spectral parameters for these two arrays. System MDA is one way of combining resolution, efficiency, and background that will enable direct comparison of various detector types for individual isotope identification. We have calculated the MDA for an early dual crystal array and the current eight crystal array. Data derived from each array will be presented. In addition, it is possible to extrapolate the MDA methodology to much larger arrays. A 32-crystal array is under construction and extrapolations to 256 and 1024 crystals are considered possible. Estimated MDA values for these larger arrays are also presented. Several 8-crystal arrays have been constructed and versions have been incorporated into portable instruments. Descriptions of these small instruments are given covering physical size, weight, and general configuration. These instruments have been tested for shock and temperature effects and data will be presented on the results of these tests. The MDA concept will also allow extrapolation to large

  18. Desorption mass spectrometry: Revisiting the in-situ calibration technique for mixed group-V alloy MBE growth of ~3.3 μm diode lasers

    NASA Astrophysics Data System (ADS)

    Kaspi, Ron; Lu, Chunte; Yang, Chi; Newell, Timothy C.; Luong, Sanh

    2015-09-01

    We apply the desorption mass spectrometry (DMS) technique and analyze the desorbed Sb species in-situ during MBE growth of mixed As/Sb heterostructures. We demonstrate how DMS is useful in pre-growth calibration of the V/III ratio, the group-III ratio, as well as the Sb-content in quaternary or quinary mixed As/Sb alloys. We also apply DMS to the digital alloy growth method. For demonstration purposes, we start with an un-calibrated MBE system, use the DMS technique to calibrate all of the previously undetermined MBE parameters and grow a ~3.3 μm diode laser heterostructure in only one attempt. The results demonstrate that the DMS technique will allow the MBE to quickly converge toward a set of acceptable growth parameters without the need for ex-situ calibration of alloy composition.

  19. Photosensitized degradation kinetics of trace halogenated contaminants in natural waters using membrane introduction mass spectrometry as an in situ reaction monitor.

    PubMed

    Letourneau, Dane R; Gill, Chris G; Krogh, Erik T

    2015-11-01

    The photochemically mediated dechlorination of polyhalogenated compounds represents a potential decontamination strategy and a relevant environmental process in chemically reducing media. We report the UV irradiation of natural and artificial waters containing natural dissolved organic matter to effect the photo-sensitized degradation of chlorinated organic compounds, including tetrachloromethane, 1,1,1-tricloroethane, perchloroethene, 1,2-dibromo-3-chloropropane and chlorobenzene at trace (ppb) levels in aqueous solution. The degradation kinetics are followed in situ using membrane introduction mass spectrometry. By re-circulating the reaction mixture in a closed loop configuration over a semi-permeable hollow fiber polydimethylsiloxane membrane in a flow cell interface, volatile and semi-volatile compounds are continuously monitored using a quadrupole ion trap mass spectrometer. The time resolved quantitative information provides useful mechanistic insights, including kinetic data. Pseudo first-order rate constants for the degradation of contaminant mixtures in natural waters are reported. PMID:26439106

  20. Matrix assisted laser desorption/ionization-mass spectrometry imaging (MALDI-MSI) for direct visualization of plant metabolites in situ

    SciTech Connect

    Sturtevant, Drew; Lee, Young -Jin; Chapman, Kent D.

    2015-11-22

    Direct visualization of plant tissues by matrix assisted laser desorption ionization-mass spectrometry imaging (MALDI-MSI) has revealed key insights into the localization of metabolites in situ. Recent efforts have determined the spatial distribution of primary and secondary metabolites in plant tissues and cells. Strategies have been applied in many areas of metabolism including isotope flux analyses, plant interactions, and transcriptional regulation of metabolite accumulation. Technological advances have pushed achievable spatial resolution to subcellular levels and increased instrument sensitivity by several orders of magnitude. Furthermore, it is anticipated that MALDI-MSI and other MSI approaches will bring a new level of understanding to metabolomics as scientists will be encouraged to consider spatial heterogeneity of metabolites in descriptions of metabolic pathway regulation.

  1. NMIS With Gamma Spectrometry for Attributes of Pu and HEU, Explosives and Chemical Agents

    SciTech Connect

    Mihalczo, J. T.; Mattingly, J. K.; Mullens, J. A.; Neal, J. S.

    2002-05-10

    The concept for the system described herein is an active/passive Nuclear Materials Identification System{sup 2} (NMIS) that incorporates gamma ray spectrometry{sup 3}. This incorporation of gamma ray spectrometry would add existing capability into this system. This Multiple Attribute System can determine a wide variety of attributes for Pu and highly enriched uranium (HEU) of which a selected subset could be chosen. This system can be built using commercial off the shelf (COTS) components. NMIS systems are at All-Russian Scientific Research Institute of Experimental Physics (VNIIEF) and Russian Federal Nuclear Center Institute of Technical Physics, (VNIITF) and measurements with Pu have been performed at VNIIEF and analyzed successfully for mass and thickness of Pu. NMIS systems are being used successfully for HEU at the Y-12 National Security Complex. The use of active gamma ray spectrometry for high explosive HE and chemical agent detection is a well known activation analysis technique, and it is incorporated here. This report describes the system, explains the attribute determination methods for fissile materials, discusses technical issues to be resolved, discusses additional development needs, presents a schedule for building from COTS components, and assembly with existing components, and discusses implementation issues such as lack of need for facility modification and low radiation exposure.

  2. In situ Measurement of Pore-Water pH in Anoxic Sediments Using Laser Raman Spectrometry

    NASA Astrophysics Data System (ADS)

    Peltzer, E. T.; Luna, M.; Walz, P. M.; Zhang, X.; Brewer, P. G.

    2010-12-01

    Accurate measurement of the geochemical properties of sediment pore waters is of fundamental importance in ocean geochemistry and microbiology. Recent work has shown that the properties of pore waters can be measured rapidly in situ with a novel Raman based insertion probe (Zhang et al., 2010), and that data obtained from anoxic sediments on in situ dissolved methane concentrations are very different (~30x) than from recovered cores due the large scale degassing that occurs during core recovery (Zhang et al., submitted). Degassing of methane must carry with it via Henry’s Law partioning significant quantities of H2S, which is clearly detectable by smell during sample processing, and thus in situ measurement of H2S is also highly desirable. In practice, dissolved H2S is partitioned between the HS- and H2S species as a function of pH with pKa ~7 for the acid dissociation reaction. Since both species are Raman active full determination of the sulfide system is possible if the relative Raman cross sections are known. The diagenetic equations for these reactions are commonly summarized as: 2CH2O + SO4= ↔ 2HCO3- + H2S CH4 + SO4= ↔ HCO3- + HS- + H2O Three of the major components of these equations, CH4, SO4=, and H2S/HS-, are all observable directly by Raman spectroscopy; but the detection of HCO3- presents a challenge due to its low Raman cross section and thus poor sensitivity. We show that pore water pH, which is a good estimator of HCO3- if total CO2 or alkalinity are known, can be measured by observing the H2S / HS- ratio via the equation: pH = pKa + log([HS-]/[H2S]) thereby fully constraining these equations within a single measurement protocol. The Raman peak for HS- is at 2573 cm-1 and for H2S is at 2592 cm-1; thus the peaks are well separated and may easily be deconvoluted from the observed spectrum. We have determined the relative Raman cross sections by a series of laboratory measurements over a range of pH and by using the definition that when pH = p

  3. In situ metathesis ionic liquid formation dispersive liquid-liquid microextraction for copper determination in water samples by electrothermal atomic absorption spectrometry.

    PubMed

    Stanisz, Ewa; Zgoła-Grześkowiak, Agnieszka

    2013-10-15

    In situ synthesis of ionic liquid extractant for dispersive liquid-liquid microextraction (in situ IL DLLME) combined with electrothermal atomic absorption spectrometry (ET AAS) for determination of copper in water samples was developed. Analytical signals were obtained without the back-extraction of copper from the IL phase prior to its determination by AAS. Some essential parameters of the microextraction and detection techniques such as the pH of sample solution, volume of components for in situ synthesis, matrix interferences and main parameters of graphite furnace atomizer have been studied. Under optimal conditions, high extraction efficiency for copper was achieved for the extraction of 0.7 µg L(-1) in 10.0 mL of sample solution employing 8 μL of 1-hexyl-3-methylimidazolium bis[(trifluoromethyl)sulfonyl]imide (HmimNTf2) as the extraction solvent. The detection limit was found as 0.004 µg L(-1) with an enrichment factor of 200. The relative standard deviation (RSD) for seven replicate measurements of 0.7 µg L(-1) in sample solution was 4%. The accuracy of the proposed method was evaluated by analysis of the Certified Reference Materials: NIST SRM 2709 (San Joaquin Soil), NBS SRM 2704 (Buffalo River Sediment), NRCC DOLT-2 (Dogfish Liver) and NIST SRM 1643e (Trace Element in Water). The measured copper contents in the reference materials were in satisfactory agreement with the certified values. The method was successfully applied to analysis of the tap, lake and mineral water samples. PMID:24054576

  4. In situ location and U-Pb dating of small zircon grains in igneous rocks using laser ablation-inductively coupled plasma-quadrupole mass spectrometry

    NASA Astrophysics Data System (ADS)

    Sack, Patrick J.; Berry, Ron F.; Meffre, Sebastien; Falloon, Trevor J.; Gemmell, J. Bruce; Friedman, Richard M.

    2011-05-01

    A new U-Pb zircon dating protocol for small (10-50 μm) zircons has been developed using an automated searching method to locate zircon grains in a polished rock mount. The scanning electron microscope-energy-dispersive X ray spectrum-based automated searching method can routinely find in situ zircon grains larger than 5 μm across. A selection of these grains was ablated using a 10 μm laser spot and analyzed in an inductively coupled plasma-quadrupole mass spectrometer (ICP-QMS). The technique has lower precision (˜6% uncertainty at 95% confidence on individual spot analyses) than typical laser ablation ICP-MS (˜2%), secondary ion mass spectrometry (<1%), and isotope dilution-thermal ionization mass spectrometry (˜0.4%) methods. However, it is accurate and has been used successfully on fine-grained lithologies, including mafic rocks from island arcs, ocean basins, and ophiolites, which have traditionally been considered devoid of dateable zircons. This technique is particularly well suited for medium- to fine-grained mafic volcanic rocks where zircon separation is challenging and can also be used to date rocks where only small amounts of sample are available (clasts, xenoliths, dredge rocks). The most significant problem with dating small in situ zircon grains is Pb loss. In our study, many of the small zircons analyzed have high U contents, and the isotopic compositions of these grains are consistent with Pb loss resulting from internal α radiation damage. This problem is not significant in very young rocks and can be minimized in older rocks by avoiding high-U zircon grains.

  5. The determination of total Se in urine and serum by graphite furnace atomic absorption spectrometry using Ir as permanent modifier and in situ oxidation for complete trimethylselenonium recovery.

    PubMed

    Grinberg, Patricia; Gonçalves, Rodrigo Araújo; de Campos, Reinaldo Calixto

    2005-12-01

    The present work evaluated the use of iridium (Ir) as permanent modifier for the determination of total selenium in urine and serum by graphite furnace atomic absorption spectrometry. Concerning urine, the presence of trimethylselenonium (TMSe(+)) was especially considered. Pyrolysis and atomization temperatures of 1,000 and 2,100 degrees C, respectively, were used. For nondigested urine and serum samples, 0.2% v/v HNO(3) and Triton X-100 were used as diluents, respectively, and the same initial platform Ir treatment was effective for up to 1,100 atomization cycles. Good precision [less than 5% relative standard deviation (RSD)] can be achieved with the proposed method. Low TMSe(+) recovery was observed for nondigested urine samples. Thus, if this species is to be considered in urine analysis, a previous external mineralization step was found to be necessary. Alternatively, an in situ oxidation treatment was developed. Detection limits of 8, 10, and 7 mug l(-1) were obtained after dilution, microwave-assisted digestion, and in situ oxidation procedures, respectively. The accuracy of the method was validated by the analysis of certified reference or commercial quality control materials and spiked samples. PMID:16267645

  6. Evaluation of TASTEX task H: measurement of plutonium isotopic abundances by gamma-ray spectrometry

    SciTech Connect

    Gunnink, R.; Prindle, A.L.; Asakura, Y.; Masui, J.; Ishiguro, N.; Kawasaki, A.; Kataoka, S.

    1981-10-01

    This report describes a computer-based gamma spectrometer system that was developed for measuring isotopic and total plutonium concentrations in nitric acid solutions. The system was installed at the Tokai reprocessing plant where it is undergoing testing and evaluation as part of the Tokai Advanced Safeguards Exercise (TASTEX). Objectives of TASTEX Task H, High-Resolution Gamma Spectrometer for Plutonium Isotopic Analysis, the methods and equipment used, the installation and calibration of the system, and the measurements obtained from several reprocessing campaigns are discussed and described. In general, we find that measurements for gamma spectroscopy agree well with those of mass spectrometry and of other chemical analysis. The system measures both freshly processed plutonium from the product accountability tank and aged plutonium solutions from storage tanks. 14 figures, 15 tables.

  7. Testing of regolith of celestial bolides with active neutron gamma-ray spectrometry

    NASA Astrophysics Data System (ADS)

    Vostrukhin, Andrey; Mitrofanov, Igor; Golovin, Dmitry; Litvak, Maxim; Sanin, Anton

    2015-04-01

    Current space instruments for studying planet's surface include gamma ray spectrometers that detect natural radioactive isotopes as well as gamma-rays induced in subsurface by galactic cosmic rays. When measuring from celestial body's surface, statistics and amount of detected elements can be dramatically increased with active methods, where soil exposed to artificial flux of particles. One good example is the Russian Dynamic Albedo of Neutron (DAN) instrument onboard Martian Science Laboratory mission (Curiosity rover) developed in 2005-2011. It is the first active neutron spectrometer flown to another planet as part of a landed mission to investigate subsurface water distribution and which has now successfully operated for more than two years on the Martian surface. Presentation describes a number of space instruments for different landers and rovers being developed in Russian Space Research Institute for studying Moon and Mars, as well as method of active neutron and gamma spectrometry overview.

  8. Formation of {gamma}-Fe{sub 2}O{sub 3} nanoparticles and vacancy ordering: An in situ X-ray powder diffraction study

    SciTech Connect

    Jorgensen, Jens-Erik Mosegaard, Lene; Thomsen, Line E.; Jensen, Torben R.; Hanson, Jonathan C.

    2007-01-15

    The formation of maghemite, {gamma}-Fe{sub 2}O{sub 3} nanoparticles has been studied by in situ X-ray powder diffraction. The maghemite was formed by thermal decomposition of an amorphous precursor compound made by reacting lauric acid, CH{sub 3}(CH{sub 2}){sub 10}COOH with Fe(NO{sub 3}){sub 3}.9H{sub 2}O. It has been shown that cubic {gamma}-Fe{sub 2}O{sub 3} was formed directly from the amorphous precursor and that vacancy ordering starts about 45 min later at 305 deg. C resulting in a tripled unit cell along the c-axis. The kinetics of grain growth was found to obey a power law with growth exponents n equal to 0.136(6) and 0.103(5) at 305 and 340 deg. C, respectively. Particles with average sizes of 12 and 13 nm were obtained in 86 and 76 min at 305 and 340 deg. C, respectively. The structure of cubic and vacancy ordered phases of {gamma}-Fe{sub 2}O{sub 3} was studied at 305 deg. C by Rietveld refinements. - Graphical abstract: Stack of powder diagrams showing the formation of {gamma}-Fe{sub 2}O{sub 3} nanoparticles and subsequent vacancy ordering at 305 deg. C.

  9. Characterising in situ activation and degradation of hindered amine light stabilisers using liquid extraction surface analysis-mass spectrometry.

    PubMed

    Paine, Martin R L; Barker, Philip J; Blanksby, Stephen J

    2014-01-15

    Changes in the molecular structure of polymer antioxidants such as hindered amine light stabilisers (HALS) is central to their efficacy in retarding polymer degradation and therefore requires careful monitoring during their in-service lifetime. The HALS, bis-(1-octyloxy-2,2,6,6-tetramethyl-4-piperidinyl) sebacate (TIN123) and bis-(1,2,2,6,6-pentamethyl-4-piperidinyl) sebacate (TIN292), were formulated in different polymer systems and then exposed to various curing and ageing treatments to simulate in-service use. Samples of these coatings were then analysed directly using liquid extraction surface analysis (LESA) coupled with a triple quadrupole mass spectrometer. Analysis of TIN123 formulated in a cross-linked polyester revealed that the polymer matrix protected TIN123 from undergoing extensive thermal degradation that would normally occur at 292°C, specifically, changes at the 1- and 4-positions of the piperidine groups. The effect of thermal versus photo-oxidative degradation was also compared for TIN292 formulated in polyacrylate films by monitoring the in situ conversion of N-CH3 substituted piperidines to N-H. The analysis confirmed that UV light was required for the conversion of N-CH3 moieties to N-H - a major pathway in the antioxidant protection of polymers - whereas this conversion was not observed with thermal degradation. The use of tandem mass spectrometric techniques, including precursor-ion scanning, is shown to be highly sensitive and specific for detecting molecular-level changes in HALS compounds and, when coupled with LESA, able to monitor these changes in situ with speed and reproducibility. PMID:24370104

  10. Speciation of inorganic arsenic in drinking water by wavelength-dispersive X-ray fluorescence spectrometry after in situ preconcentration with miniature solid-phase extraction disks.

    PubMed

    Hagiwara, Kenta; Inui, Tetsuo; Koike, Yuya; Aizawa, Mamoru; Nakamura, Toshihiro

    2015-03-01

    A rapid and simple method using wavelength-dispersive X-ray fluorescence (WDXRF) spectrometry after in situ solid-phase extraction (SPE) was developed for the speciation and evaluation of the concentration of inorganic arsenic (As) in drinking water. The method involves the simultaneous collection of As(III) and As(V) using 13 mm ϕ SPE miniature disks. The removal of Pb(2+) from the sample water was first conducted to avoid the overlapping PbLα and AsKα spectra on the XRF spectrum. To this end, a 50 mL aqueous sample (pH 5-9) was passed through an iminodiacetate chelating disk. The filtrate was adjusted to pH 2-3 with HCl, and then ammonium pyrrolidine dithiocarbamate solution was added. The solution was passed through a hydrophilic polytetrafluoroethylene filter placed on a Zr and Ca loaded cation-exchange disk at a flow rate of 12.5 mL min(-1) to separate As(III)-pyrrolidine dithiocarbamate complex and As(V). Each SPE disk was affixed to an acrylic plate using adhesive cellophane tape, and then examined by WDXRF spectrometry. The detection limits of As(III) and As(V) were 0.8 and 0.6 μg L(-1), respectively. The proposed method was successfully applied to screening for As speciation and concentration evaluation in spring water and well water. PMID:25618730

  11. A Case Study Correlating Innovative Gamma Ray Scanning Detection Systems Data to Surface Soil Gamma Spectrometry Results - 13580

    SciTech Connect

    Thompson, Shannon; Rodriguez, Rene; Billock, Paul; Lit, Peter

    2013-07-01

    HydroGeoLogic (HGL), Inc. completed a United States Environmental Protection Agency (USEPA) study to characterize radiological contamination at a site near Canoga Park, California. The characterized area contained 470 acres including the site of a prototype commercial nuclear reactor and other nuclear design, testing, and support operations from the 1950's until 1988 [1]. The site history included radiological releases during operation followed by D and D activities. The characterization was conducted under an accelerated schedule and the results will support the project remediation. The project has a rigorous cleanup to background agenda and does not allow for comparison to risk-based guidelines. To target soil sample locations, multiple lines of evidence were evaluated including a gamma radiation survey, geophysical surveys, historical site assessment, aerial photographs, and former worker interviews. Due to the time since production and decay, the primary gamma emitting radionuclide remaining is cesium-137 (Cs-137). The gamma ray survey covered diverse, rugged terrain using custom designed sodium iodide thallium-activated (NaI(Tl)) scintillation detection systems. The survey goals included attaining 100% ground surface coverage and detecting gamma radiation as sensitively as possible. The effectiveness of innovative gamma ray detection systems was tested by correlating field Cs-137 static count ratios to Cs-137 laboratory gamma spectrometry results. As a case study, the area encompassing the former location of the first nuclear power station in the U. S. was scanned, and second by second global positioning system (GPS)-linked gamma spectral data were evaluated by examining total count rate and nuclide-specific regions of interest. To compensate for Compton scattering from higher energy naturally occurring radionuclides (U-238, Th-232 and their progeny, and K-40), count rate ratios of anthropogenic nuclide-specific regions of interest to the total count rate were

  12. Combined Gamma-Ray Spectrometer and Pulsed Neutron Generator System for In-Situ Planetary Geochemical Analysis

    SciTech Connect

    Starr, R. D.; Evans, L. G.; Parsons, A. M.; Akkurt, Hatice; Floyd, H.; Wraight, P.; Ziegler, W.; Schweitzer, J.

    2007-01-01

    A combined pulsed neutron/gamma-ray system can be used on planetary surfaces to provide valuable geochemical analysis of surface materials to depths of {approx}1 m. We describe experimental results that demonstrate the capabilities of such a system.

  13. Beam-folding ultraviolet-visible Fourier transform spectrometry and underwater cytometry for in situ measurement of marine phytoplankton

    NASA Astrophysics Data System (ADS)

    Wang, Xuzhu

    itself insensitive to these fluctuations. In addition, an attempt on fast-scanning visible IFTS based on the improved beam-folding technique was done. Preliminary experimental results demonstrated the feasibility of the fast-scanning visible IFTS based on the improved beam-folding technique. In part two, an underwater cytometer for in situ measurement of marine phytoplankton using a combining technique of laser-induced fluorescence (LIF) and laser differential Doppler velocimetry (LDDV) was developed. The advancement compared to the previous work done in the laboratory is to realize an in situ underwater measurement system by means of improving the optical design. The experimental results in June and August 2004 in the coastal area of Hong Kong demonstrated that the new cytometer can be used for in situ measurement of marine phytoplankton. The mean concentration detected by this instrument agreed closely with the experimental data measured by the traditional cell counting under a microscope. With an underwater optical sensing unit that does not rely on an electrical power source, the sensing unit can stay submerged underwater for long periods, making a long-term real-time monitoring system possible.

  14. Measurement of gamma radiation levels in soil samples from Thanjavur using gamma-ray spectrometry and estimation of population exposure.

    PubMed

    Senthilkumar, B; Dhavamani, V; Ramkumar, S; Philominathan, P

    2010-01-01

    This study assesses the level of terrestrial gamma radiation and associated dose rates from the naturally occurring radionuclides (232)Th, (238)U and (40)K in 10 soil samples collected from Thanjavur (Tamil Nadu, India) using gamma-ray spectrometry. The activity profile of radionuclides has clearly showed the existence of low level activity in Thanjavur. The geometric mean activity concentrations of (232)Th, (238)U and (40)K is 42.9+/-9.4 Bq.kg(-1), 14.7+/-1.7 Bq.kg(-1) and 149.5+/-3.1 Bq.kg(-1) respectively are derived from all the soil samples studied. The activity concentration of (232)Th, (238)U and (40)K in soil is due to the presence of metamorphic rocks like shale, hornblende-biotite gneiss and quartzofeldspathic gneiss in these areas. Gamma absorbed dose rates in air outdoors were calculated to be in the range between 32 nGy.h(-1) and 59.1 nGy.h(-1) with an arithmetic mean of 43.3 +/-9 nGy.h(-1). This value is lesser than the population weighted world-averaged of 60 nGy.h(-1). Inhabitants of Thanjavur are subjected to external gamma radiation exposure (effective dose) ranging between 39.2 and 72.6 muSv.y(-1) with an arithmetic mean of 53.1+/-11 muSv.y(-1). The values of the external hazard index determined from the soil radioactivity of the study area are less than the recommended safe levels. PMID:20177570

  15. Rapid and simultaneous in situ assessment of aflatoxins and stilbenes using silica plate imprinting mass spectrometry imaging.

    PubMed

    de Oliveira, Diogo N; Ferreira, Mônica S; Catharino, Rodrigo R

    2014-01-01

    A fast and direct combination of techniques for simultaneous mycotoxin and phytoalexin identification in peanut skin and kernel is described. Silica Plate Imprinting Laser Desorption/Ionization Mass Spectrometry Imaging (SPILDI-MSI) is a powerful technique that exhibits great advantages, such as solvent-free and matrix-free characteristics, as well as no sample preparation or separation steps. It also permits accurate identification of mycotoxins and phytoalexins with unique fingerprint profiles in just a few seconds. Results are expressed as chemical images of the 4 identified types of aflatoxins (B1, B2, G1 and G2) and a stilbenoid (resveratrol). Also, SPILDI-MSI allows the comparison between the spatial distribution of aflatoxins and resveratrol found in kernel and skin. This novel application has proven to be useful for instantaneous qualitative assessment of aflatoxins and stilbenoids both in the peanut skin and kernel and offers precise tracking of fungal contamination in nuts and other foodstuffs. PMID:24595464

  16. A technique coupling the analyte electrodeposition followed by in-situ stripping with electrothermal atomic absorption spectrometry for analysis of samples with high NaCl contents

    NASA Astrophysics Data System (ADS)

    Čánský, Zdeněk; Rychlovský, Petr; Petrová, Zuzana; Matousek, J. P.

    2007-03-01

    A technique coupling the analyte electrodeposition followed by in-situ stripping with electrothermal atomic absorption spectrometry has been developed for determination of lead and cadmium in samples with high salt contents. To separate the analyte from the sample matrix, the analyte was in-situ quantitatively electrodeposited on a platinum sampling capillary serving as the cathode (sample volume, 20 μL). The spent electrolyte containing the sample matrix was then withdrawn, the capillary with the analyte deposited was washed with deionized water and the analyte was stripped into a chemically simple electrolyte (5 g/L NH 4H 2PO 4) by reversing the polarity of the electrodeposition circuit. Electrothermal atomization using a suitable optimized temperature program followed. A fully automated manifold was designed for this coupled technique and the appropriate control software was developed. The operating conditions for determination of Pb and Cd in samples with high contents of inorganic salts were optimized, the determination was characterized by principal analytical parameters and its applicability was verified on analyses of urine reference samples. The absolute limits of detection for lead and cadmium (3 σ criterion) in a sample containing 30 g/L NaCl were 8.5 pg and 2.3 pg, respectively (peak absorbance) and the RSD values amounted to 1.6% and 1.9% for lead (at the 40 ng mL - 1 level) and cadmium (at the 4.0 ng mL - 1 level), respectively. These values (and also the measuring sensitivity) are superior to the results attained in conventional electrothermal atomic absorption spectrometric determination of Pb and Cd in pure solutions (5 g/L NH 4H 2PO 4). The sensitivity of the Pb and Cd determination is not affected by the NaCl concentration up to a value of 100 g/L, demonstrating an efficient matrix removal during the electrodeposition step.

  17. In situ emulsification microextraction using a dicationic ionic liquid followed by magnetic assisted physisorption for determination of lead prior to micro-sampling flame atomic absorption spectrometry.

    PubMed

    Shokri, Masood; Beiraghi, Asadollah; Seidi, Shahram

    2015-08-19

    For the first time, a simple and efficient in situ emulsification microextraction method using a dicationic ionic liquid followed by magnetic assisted physisorption was presented to determine trace amounts of lead. In this method, 400 μL of 1.0 mol L(-1) lithium bis (trifluoromethylsulfonyl) imide aqueous solution, Li[NTf2], was added into the sample solution containing 100 μL of 1.0 mol L(-1) 1,3-(propyl-1,3-diyl) bis (3-methylimidazolium) chloride, [pbmim]Cl2, to form a water immiscible ionic liquid, [pbmim][NTf2]2. This new in situ formed dicationic ionic liquid was applied as the acceptor phase to extract the lead-ammonium pyrrolidinedithiocarbamate (Pb-APDC) complexes from the sample solution. Subsequently, 30 mg of Fe3O4 magnetic nanoparticles (MNPs) were added into the sample solution to collect the fine droplets of [pbmim][NTf2]2, physisorptively. Finally, MNPs were eluted by acetonitrile, separated by an external magnetic field and the obtained eluent was subjected to micro-sampling flame atomic absorption spectrometry (FAAS) for further analysis. Comparing with other microextraction methods, no special devices and centrifugation step are required. Parameters influencing the extraction efficiency such as extraction time, pH, concentration of chelating agent, amount of MNPs and coexisting interferences were studied. Under the optimized conditions, this method showed high extraction recovery of 93% with low LOD of 0.7 μg L(-1). Good linearity was obtained in the range of 2.5-150 μg L(-1) with determination coefficient (r(2)) of 0.9921. Relative standard deviation (RSD%) for seven repeated measurements at the concentration of 10 μg L(-1) was 4.1%. Finally, this method was successfully applied for determination of lead in some water and plant samples. PMID:26343434

  18. Radioactivity Levels and Gamma-Ray Dose Rate in Soil Samples from Kohistan (Pakistan) Using Gamma-Ray Spectrometry

    NASA Astrophysics Data System (ADS)

    Hasan, M. Khan; Ismail, M.; K., Khan; Akhter, P.

    2011-01-01

    The analysis of naturally occurring radionuclides (226Ra, 232Th and 40K) and an anthropogenic radionuclide 137Cs is carried out in some soil samples collected from Kohistan district of N.W.F.P. (Pakistan), using gamma-ray spectrometry. The gamma spectrometry is operated using a high purity Germanium (HPGe) detector coupled with a computer based high resolution multi channel analyzer. The specific activity in soil ranges from 24.72 to 78.48Bq·kg-1 for 226Ra, 21.73 to 75.28Bq·kg-1 for 232Th, 7.06 to 14.9Bq·kg-1 for 137Cs and 298.46 to 570.77Bq·kg-1 for 40K with the mean values of 42.11, 43.27, 9.5 and 418.27Bq·kg-1, respectively. The radium equivalent activity in all the soil samples is lower than the safe limit set in the OECD report (370Bq·kg-1). Man-made radionuclide 137Cs is also present in detectable amount in all soil samples. Presence of 137Cs indicates that the samples in this remote area also receive some fallout from nuclear accident in Chernobyl power plant in 1986. The internal and external hazard indices have the mean values of 0.48 and 0.37 respectively. Absorbed dose rates and effective dose equivalents are also determined for the samples. The concentration of radionuclides found in the soil samples during the present study is nominal and does not pose any potential health hazard to the general public.

  19. Development of routines for simultaneous in situ chemical composition and stable Si isotope ratio analysis by femtosecond laser ablation inductively coupled plasma mass spectrometry.

    PubMed

    Frick, Daniel A; Schuessler, Jan A; von Blanckenburg, Friedhelm

    2016-09-28

    Stable metal (e.g. Li, Mg, Ca, Fe, Cu, Zn, and Mo) and metalloid (B, Si, Ge) isotope ratio systems have emerged as geochemical tracers to fingerprint distinct physicochemical reactions. These systems are relevant to many Earth Science questions. The benefit of in situ microscale analysis using laser ablation (LA) over bulk sample analysis is to use the spatial context of different phases in the solid sample to disclose the processes that govern their chemical and isotopic compositions. However, there is a lack of in situ analytical routines to obtain a samples' stable isotope ratio together with its chemical composition. Here, we evaluate two novel analytical routines for the simultaneous determination of the chemical and Si stable isotope composition (δ(30)Si) on the micrometre scale in geological samples. In both routines, multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) is combined with femtosecond-LA, where stable isotope ratios are corrected for mass bias using standard-sample-bracketing with matrix-independent calibration. The first method is based on laser ablation split stream (LASS), where the laser aerosol is split and introduced simultaneously into both the MC-ICP-MS and a quadrupole ICP-MS. The second method is based on optical emission spectroscopy using direct observation of the MC-ICP-MS plasma (LA-MC-ICP-MS|OES). Both methods are evaluated using international geological reference materials. Accurate and precise Si isotope ratios were obtained with an uncertainty typically better than 0.23‰, 2SD, δ(30)Si. With both methods major element concentrations (e.g., Na, Al, Si, Mg, Ca) can be simultaneously determined. However, LASS-ICP-MS is superior over LA-MC-ICP-MS|OES, which is limited by its lower sensitivity. Moreover, LASS-ICP-MS offers trace element analysis down to the μg g(-1)-range for more than 28 elements due to lower limits of detection, and with typical uncertainties better than 15%. For in situ simultaneous

  20. Mechanistic insights into the reduction of carbon dioxide on tin and bismuth electrodes using in situ infrared spectroscopy and differential electrochemical mass spectrometry

    NASA Astrophysics Data System (ADS)

    Baruch, Maor F.

    The factors that govern the electrochemical reduction of CO2 on Sn and Bi electrodes were studied. Chapter 1 discusses the relevant literature, the merits of reducing CO2 electrochemically, the ways in which CO2 reduction systems are characterized, and the outstanding challenges. Chapter 2 describes the design and construction of a differential electrochemical mass spectrometry (DEMS) system that can be used to probe the products of electrochemical reactions in situ and in real time. In Chapter 3, the role of surface oxides and hydroxides in the reduction of CO2 on Sn electrodes is discussed. in situ attenuated total reflectance infrared (ATR-IR) spectroscopy is the main analytical technique by which the system was studied. Peaks that are attributed to a surface-bound Sn carbonate are present under conditions that are suitable for CO2 reduction. A strong correlation between the presence of these peaks and catalytic activity exists with respect to the applied potential, the pH of the electrolyte, and the surface condition of the electrode. X-ray photoelectron spectroscopy (XPS), energy dispersive X-ray spectroscopy (EDX), scanning electron microscopy (SEM) and electrochemical analysis were also used characterize the catalysts. Based on these data, a mechanism for the reduction of CO2 on Sn cathodes is proposed. The roles of morphology and surface oxide presence in the reduction of CO2 on Bi cathodes are discussed in Chapter 4. ATR-IR spectroscopy, XPS, EDX, SEM, cyclic voltammetry, and preparative electrolysis are used to demonstrate that, unlike Sn, Bi electrodes do not possess oxide-dependent catalytic behavior. Instead, it is shown that Bi electrodes are highly sensitive to morphological changes in surface structure, and that surface roughness is detrimental to HCOO-- production from CO2. Finally, it is shown that oxide-derived Bi, formed by the in situ reduction of Bi2O3 nanoparticles at cathodic potentials, can reduce CO2 to HCOO-- at near unit efficiencies at

  1. Nuclear chemistry of returned lunar samples: Nuclide analysis by gamma-ray spectrometry

    NASA Technical Reports Server (NTRS)

    Okelley, G. D.

    1975-01-01

    Primordial and cosmogenic radionuclide concentrations are determined nondestructively by gamma-ray spectrometry in soil and rock samples from the returned Apollo 17 sample collection from Taurus-Littrow and Descartes. Geochemical evidence in support of field geology speculation concerning layering of the subfloor basalt flows is demonstrated along with a possible correlation of magmatic fractionation of K/U as a function of depth. The pattern of radionuclide concentrations observed in these samples is distinct due to proton bombardment by the intense solar flares of August 4-9, 1972. Such radionuclide determinations are used in determining lunar sample orientation and characterizing solar flare activity.

  2. Comparison of LabSOCS and GESPECOR codes used in gamma-ray spectrometry.

    PubMed

    Done, L; Tugulan, L C; Gurau, D; Dragolici, F; Alexandru, C

    2016-03-01

    Two dedicated software packages -LabSOCS and GESPECOR- for efficiency evaluation in gamma-ray spectrometry, were compared for equivalence. The detection efficiency and the coincidence-summing corrections coefficients were calculated for a specific HPGe detector, for different sample parameters and energies typically encountered in environmental radioactivity measurements. The discrepancy between the results obtained with the two codes were acceptable for most of the applications. Furthermore, the deviations between the values of the standard sources/ reference materials activities from the certificate and the values obtained after Monte Carlo simulation were less than 8% for LabSOCS and 9% for GESPECOR. PMID:26625727

  3. Low Background Gamma-Ray Spectrometry in the 'Laboratoire Souterrain de Modane'

    SciTech Connect

    Hubert, Ph.; Hubert, F.

    2007-03-28

    Most of the underground experiments in physics and many studies in geology, biology or environmental sciences face a common requirement with the necessity of using experimental devices with ultra-low background radioactivity. Many developments involving many different techniques have been used in order to be able to measure extremely low levels of radioactivity in materials. This report will focus on low background gamma-ray spectrometry and will describe the work which has been carried out over the last fifteen years in the 'Laboratoire Souterrain de Modane' (LSM)

  4. Design and fabrication of an in situ gamma radioactivity measurement system for marine environment and its calibration with Monte Carlo method.

    PubMed

    Abdollahnejad, Hamed; Vosoughi, Naser; Zare, Mohammad Reza

    2016-08-01

    Simulation, design and fabrication of a sealing enclosure is carried out for a NaI(Tl) 2″×2″ detector, to be used as in situ gamma radioactivity measurement system in marine environment. Effect of sealing enclosure on performance of the system in laboratory and marine environment (distinct tank with 10m(3) volume) were studied using point sources. The marine volumetric efficiency for radiation with 1461keV energy (from (40)K) is measured with KCl volumetric liquid source diluted in distinct tank. The experimental and simulated efficiency values agreed well. Marine volumetric efficiency calibration curve is calculated for 60keV to 1461keV energy with Monte Carlo method. This curve indicates that efficiency increasing rapidly up to 140.5keV but then drops exponentially. PMID:27213808

  5. Evaluation of radiological data of some saturated fatty acids using gamma ray spectrometry

    NASA Astrophysics Data System (ADS)

    Kore, Prashant S.; Pawar, Pravina P.; Palani Selvam, T.

    2016-02-01

    Radiological parameters such as mass attenuation coefficients (μm), total attenuation cross section (σtot), molar extinction coefficient (ε), mass energy absorption coefficient (μen/ρ) and effective electronic cross section (σt, el) of saturated fatty acids, namely butyric acid (C4H8O2), caproic acid (C6H12O2), enanthic acid (C7H14O2), caprylic acid (C8H16O2), pelargonic acid (C9H18O2) and valeric acid (C5H10O2) were measured using NaI(Tl)-based gamma spectrometry. Radioactive sources used in the study are 57Co, 133Ba, 137Cs, 54Mn, 60Co and 22Na. Gamma ray transmission method in a narrow beam good geometry set up was used in the study. The measured data were compared against Win-XCOM-based data. The agreement is within 1%.

  6. Isotopic analysis of uranium in U3O8 by passive gamma-ray spectrometry

    PubMed

    Nir-El

    2000-03-01

    Passive gamma-ray spectrometry was applied to analyze the isotopic composition of uranium in U3O8. Depleted and enriched U3O8 standard reference materials were used to calibrate the system. An independent calibration was performed by standard gamma-ray point sources. U3O8 SRM samples of the 950 series were analyzed. The present results show that the isotopic abundances of 235U in SRMs 950, 950a and 950b are higher by +3.6, +0.9 and +0.9% (relative deviation) than the natural value 0.7200%, while relative precisions were +/-0.4, +/-0.7 and +/-0.3%, respectively. PMID:10724436

  7. GEANT4 calibration of gamma spectrometry efficiency for measurements of airborne radioactivity on filter paper.

    PubMed

    Alrefae, Tareq

    2014-11-01

    A simple method of efficiency calibration for gamma spectrometry was performed. This method, which focused on measuring airborne radioactivity collected on filter paper, was based on Monte Carlo simulations using the toolkit GEANT4. Experimentally, the efficiency values of an HPGe detector were calculated for a multi-gamma disk source. These efficiency values were compared to their counterparts produced by a computer code that simulated experimental conditions. Such comparison revealed biases of 24, 10, 1, 3, 7, and 3% for the radionuclides (photon energies in keV) of Ce (166), Sn (392), Cs (662), Co (1,173), Co (1,333), and Y (1,836), respectively. The output of the simulation code was in acceptable agreement with the experimental findings, thus validating the proposed method. PMID:25271933

  8. Combination of ESI and MALDI mass spectrometry for qualitative, semi-quantitative and in situ analysis of gangliosides in brain

    PubMed Central

    Zhang, Yangyang; Wang, Jun; Liu, Jian’an; Han, Juanjuan; Xiong, Shaoxiang; Yong, Weidong; Zhao, Zhenwen

    2016-01-01

    Gangliosides are a family of complex lipids that are abundant in the brain. There is no doubt the investigations about the distribution of gangliosides in brian and the relationship between gangliosides and Alzheimer’s disease is profound. However, these investigations are full of challenges due to the structural complexity of gangliosides. In this work, the method for efficient extraction and enrichment of gangliosides from brain was established. Moreover, the distribution of gangliosides in brain was obtained by matrix-assisted laser desorption ionization (MALDI) mass spectrometry imaging (MSI). It was found that 3-aminoquinoline (3-AQ) as matrix was well-suited for MALDI MS analysis of gangliosides in negative ion mode. In addition, the pretreatment by ethanol (EtOH) cleaning brain section and the addition of ammonium formate greatly improved the MS signal of gangliosides in the brain section when MALDI MSI analysis was employed. The distribution of ganliosides in cerebral cortex, hippocampus and cerebellum was respectively acquired by electrospray ionization (ESI) MS and MALDI MSI, and the data were compared for reliability evaluation of MALDI MSI. Further, applying MALDI MSI technology, the distribution of gangliosides in amyloid precursor protein transgenic mouse brain was obtained, which may provide a new insight for bioresearch of Alzheimer’s disease (AD). PMID:27142336

  9. Application of membrane inlet mass spectrometry for online and in situ analysis of methane in aquatic environments.

    PubMed

    Schlüter, Michael; Gentz, Torben

    2008-10-01

    A method is presented for the online measurement of methane in aquatic environments by application of membrane inlet mass spectrometry (MIMS). For this purpose, the underwater mass spectrometer Inspectr200-200 was applied. A simple and reliable volumetric calibration technique, based on the mixing of two end member concentrations, was used for the analysis of CH(4) by MIMS. To minimize interferences caused by the high water vapor content, permeating through the membrane inlet system into the vacuum section of the mass spectrometer, a cool-trap was designed. With the application of the cool-trap, the detection limit was lowered from 100 to 16 nmol/L CH(4). This allows for measurements of methane concentrations in surface and bottom waters of coastal areas and lakes. Furthermore, in case of membrane rupture, the cool-trap acts as a security system, avoiding total damage of the mass spectrometer by flushing it with water. The Inspectr200-200 was applied for studies of methane and carbon dioxide concentrations in coastal areas of the Baltic Sea and Lake Constance. The low detection limit and fast response time of the MIMS allowed a detailed investigation of methane concentrations in the vicinity of gas seepages. PMID:18789719

  10. Real time in situ chemical characterization of submicrometer organic particles using direct analysis in real time-mass spectrometry.

    PubMed

    Nah, Theodora; Chan, ManNin; Leone, Stephen R; Wilson, Kevin R

    2013-02-19

    Direct analysis in real time mass spectrometry (DART-MS) is used to analyze the surface chemical composition of nanometer-sized organic aerosol particles in real time at atmospheric pressure. By introducing a stream of particles in between the DART ionization source and the atmospheric pressure inlet of the mass spectrometer, the aerosol is exposed to a thermal flow of helium or nitrogen gas containing some fraction of metastable helium atoms or nitrogen molecules. In this configuration, the molecular constituents of organic particles are desorbed, ionized, and detected with reduced molecular ion fragmentation, allowing for compositional identification. Aerosol particles detected include alkanes, alkenes, acids, esters, alcohols, aldehydes, and amino acids. The ion signal produced by DART-MS scales with the aerosol surface area rather than volume, suggesting that DART-MS is a viable technique to measure the chemical composition of the particle interface. For oleic acid, particle size measurements of the aerosol stream exiting the ionization region suggest that the probing depth depends upon the desorption temperature, and the probing depth is estimated to be on the order of 5 nm for a 185 nm diameter particle at a DART heater temperature of 500 °C with nitrogen as the DART gas. The reaction of ozone with submicrometer oleic acid particles is measured to demonstrate the ability of this technique to identify products and quantify reaction rates in a heterogeneous reaction. PMID:23330910

  11. In-situ monitoring of actinides and rare earth elements by electrothermal hollow cathode discharge spectrometry. Technical progress report

    SciTech Connect

    Lee, S.C.; Edelson, M.C.

    1992-12-01

    This report describes an Electrothermal Hollow Cathode Discharge Spectrometry (ET-HCDS) source being constructed for the analytical determination of actinides and rare earth elements. This work was initiated with the support of the Office of Safeguards and Security; the Buried Waste Integrated Demonstration began funding work in this area in mid-FY1992 and the work is continuing into FY1993 with funds from both sources. Special features of this instrument should permit it to be used for the determination of individual isotopic species, which is important for safeguard`s materials control and accountancy. ET-HCDS can be achieved using compact instrumentation suitable for use in field laboratories. The technique is capable of determining a suite of environmentally-important species, such as the actinides and the heavy metals, in a variety of physical forms (e.g., in solution, as found on air particulates, or in soils). ET-HCDS should be capable of very sensitive analyses and should require very small samples (e.g., microgram). Since ET-HCDS is possible in an air atmosphere (at reduced pressures), it may be useful for the real-time determination of hazardous materials, both radioactive and non radioactive, contained in dusts released during waste retrieval operations; ET-HCDS should also be useful for the rapid and sensitive analysis of metals in soils.

  12. Combination of ESI and MALDI mass spectrometry for qualitative, semi-quantitative and in situ analysis of gangliosides in brain.

    PubMed

    Zhang, Yangyang; Wang, Jun; Liu, Jian'an; Han, Juanjuan; Xiong, Shaoxiang; Yong, Weidong; Zhao, Zhenwen

    2016-01-01

    Gangliosides are a family of complex lipids that are abundant in the brain. There is no doubt the investigations about the distribution of gangliosides in brian and the relationship between gangliosides and Alzheimer's disease is profound. However, these investigations are full of challenges due to the structural complexity of gangliosides. In this work, the method for efficient extraction and enrichment of gangliosides from brain was established. Moreover, the distribution of gangliosides in brain was obtained by matrix-assisted laser desorption ionization (MALDI) mass spectrometry imaging (MSI). It was found that 3-aminoquinoline (3-AQ) as matrix was well-suited for MALDI MS analysis of gangliosides in negative ion mode. In addition, the pretreatment by ethanol (EtOH) cleaning brain section and the addition of ammonium formate greatly improved the MS signal of gangliosides in the brain section when MALDI MSI analysis was employed. The distribution of ganliosides in cerebral cortex, hippocampus and cerebellum was respectively acquired by electrospray ionization (ESI) MS and MALDI MSI, and the data were compared for reliability evaluation of MALDI MSI. Further, applying MALDI MSI technology, the distribution of gangliosides in amyloid precursor protein transgenic mouse brain was obtained, which may provide a new insight for bioresearch of Alzheimer's disease (AD). PMID:27142336

  13. Determination of methylmercury by electrothermal atomic absorption spectrometry using headspace single-drop microextraction with in situ hydride generation

    NASA Astrophysics Data System (ADS)

    Gil, Sandra; Fragueiro, Sandra; Lavilla, Isela; Bendicho, Carlos

    2005-01-01

    A new method is proposed for preconcentration and matrix separation of methylmercury prior to its determination by electrothermal atomic absorption spectrometry (ETAAS). Generation of methylmercury hydride (MeHgH) from a 5-ml solution is carried out in a closed vial and trapped onto an aqueous single drop (3-μl volume) containing Pd(II) or Pt(IV) (50 and 10 mg/l, respectively). The hydrogen evolved in the headspace (HS) after decomposition of sodium tetrahydroborate (III) injected for hydride generation caused the formation of finely dispersed Pd(0) or Pt(0) in the drop, which in turn, were responsible for the sequestration of MeHgH. A preconcentration factor of ca. 40 is achieved with both noble metals used as trapping agents. The limit of detection of methylmercury was 5 and 4 ng/ml (as Hg) with Pd(II) or Pt(IV) as trapping agents, and the precision expressed as relative standard deviation was about 7%. The preconcentration system was fully characterised through optimisation of the following variables: Pd(II) or Pt(IV) concentration in the drop, extraction time, pH of the medium, temperatures of both sample solution and drop, concentration of salt in the sample solution, sodium tetrahydroborate (III) concentration in the drop and stirring rate. The method has been successfully validated against two fish certified reference materials (CRM 464 tuna fish and CRM DORM-2 dogfish muscle) following selective extraction of methylmercury in 2 mol/l HCl medium.

  14. In Situ Analysis of Bacterial Lipopeptide Antibiotics by Matrix-Assisted Laser Desorption/Ionization Mass Spectrometry Imaging.

    PubMed

    Debois, Delphine; Ongena, Marc; Cawoy, Hélène; De Pauw, Edwin

    2016-01-01

    Matrix-assisted laser desorption/ionization mass spectrometry imaging (MALDI MSI) is a technique developed in the late 1990s enabling the two-dimensional mapping of a broad variety of biomolecules present at the surface of a sample. In many applications including pharmaceutical studies or biomarker discovery, the distribution of proteins, lipids or drugs, and metabolites may be visualized within tissue sections. More recently, MALDI MSI has become increasingly applied in microbiology where the versatility of the technique is perfectly suited to monitor the metabolic dynamics of bacterial colonies. The work described here is focused on the application of MALDI MSI to map secondary metabolites produced by Bacilli, especially lipopeptides, produced by bacterial cells during their interaction with their environment (bacteria, fungi, plant roots, etc.). This chapter addresses the advantages and challenges that the implementation of MALDI MSI to microbiological samples entails, including detailed protocols on sample preparation (from both microbiologist and mass spectrometrist points of view), matrix deposition, and data acquisition and interpretation. Lipopeptide images recorded from confrontation plates are also presented. PMID:26831708

  15. Measurement of uranium series radionuclides in rock and groundwater at the Koongarra ore deposit, Australia, by gamma spectrometry

    SciTech Connect

    Yanase, Nobuyuki; Sekine, Keiichi

    1995-12-31

    Gamma spectrometry without any self-absorption correction was developed to measure low energy gamma rays emitted by uranium and actinium series radionuclides in rock samples and groundwater residues collected at the Koongarra ore deposit, Australia. Thin samples were prepared to minimize the self-absorption by uranium in the samples. The present method gave standard deviations of 0.9 to 18% for the measurements of concentrations of uranium and actinium series radionuclides. The concentrations of {sup 238}U, {sup 230}Th and {sup 235}U measured by gamma spectrometry were compared with those by alpha spectrometry that requires a complicated chemical separation procedure. The results obtained by both methods were in fairly good agreement, and it was found that the gamma spectrometry is applicable to rock and groundwater samples having uranium content sup to 8.1% (10{sup 3} B1/g) and 3 Bq/l of {sup 238}U, respectively. The detection limits were calculated to be of the order of 10{sup {minus}2} Bq/g for rock samples and 10{sup {minus}1} Bq/l for groundwater samples. The concentrations of uranium and actinium series radionuclides can be determined precisely in these samples using gamma spectrometry without any self-absorption correction.

  16. Measuring the radium quartet (228Ra, 226Ra, 224Ra, 223Ra) in seawater samples using gamma spectrometry.

    PubMed

    van Beek, P; Souhaut, M; Reyss, J-L

    2010-07-01

    Radium isotopes are widely used in marine studies (eg. to trace water masses, to quantify mixing processes or to study submarine groundwater discharge). While 228Ra and 226Ra are usually measured using gamma spectrometry, short-lived Ra isotopes (224Ra and 223Ra) are usually measured using a Radium Delayed Coincidence Counter (RaDeCC). Here we show that the four radium isotopes can be analyzed using gamma spectrometry. We report 226Ra, 228Ra, 224Ra, 223Ra activities measured using low-background gamma spectrometry in standard samples, in water samples collected in the vicinity of our laboratory (La Palme and Vaccarès lagoons, France) but also in seawater samples collected in the plume of the Amazon river, off French Guyana (AMANDES project). The 223Ra and 224Ra activities determined in these samples using gamma spectrometry were compared to the activities determined using RaDeCC. Activities determined using the two techniques are in good agreement. Uncertainties associated with the 224Ra activities are similar for the two techniques. RaDeCC is more sensitive for the detection of low 223Ra activities. Gamma spectrometry thus constitutes an alternate method for the determination of short-lived Ra isotopes. PMID:20106569

  17. Real Time in Situ Gamma Radiation Measurements of the Plume Evolution from the Full-Scale Radiological Dispersal Device Field Trials.

    PubMed

    Korpach, Ed; Berg, Rodney; Erhardt, Lorne; Lebel, Luke; Liu, Chuanlei

    2016-05-01

    During the Full-Scale Radiological Dispersal Device Field Trials carried out in Suffield in 2012, several suites of detection and sampling equipment were used to measure and characterize the explosive dispersal of the short half-life radioactive tracer Lanthanum-140 ((140)La). The equipment deployed included networks of in situ real-time radiation monitoring detectors providing measurements of different sensitivities and characteristics. A dense array of lower sensitivity detectors was established near field, ranging from 10 to 450 m from the detonation location. A sparser array of more sensitive detectors was established in the far field (150 m to 3.5 km from the detonation location). Each was used to collect and report the dose rate data from the radioactive plume passage with a sample time resolution of 1 s. The two systems went through independent calibrations and were compared and shown to be consistent with each other. The in situ gamma radiation measurements have allowed the movement and evolution of the plume to be described and to identify deposition rates and non-uniformities in the temporal shape of the plume. This knowledge could be applied for emergency planning guidance for the case of release of radioactive material by a radiological dispersive device. PMID:27023030

  18. An analysis of nuclear fuel burnup in the AGR-1 TRISO fuel experiment using gamma spectrometry, mass spectrometry, and computational simulation techniques

    SciTech Connect

    Harp, Jason M.; Demkowicz, Paul A.; Winston, Philip L.; Sterbentz, James W.

    2014-09-03

    AGR 1 was the first in a series of experiments designed to test US TRISO fuel under high temperature gas-cooled reactor irradiation conditions. This experiment was irradiated in the Advanced Test Reactor (ATR) at Idaho National Laboratory (INL) and is currently undergoing post irradiation examination (PIE) at INL and Oak Ridge National Laboratory. One component of the AGR 1 PIE is the experimental evaluation of the burnup of the fuel by two separate techniques. Gamma spectrometry was used to non destructively evaluate the burnup of all 72 of the TRISO fuel compacts that comprised the AGR 1 experiment. Two methods for evaluating burnup by gamma spectrometry were developed, one based on the Cs 137 activity and the other based on the ratio of Cs 134 and Cs 137 activities. Burnup values determined from both methods compared well with the values predicted from simulations. The highest measured burnup was 20.1% FIMA for the direct method and 20.0% FIMA for the ratio method (compared to 19.56% FIMA from simulations). An advantage of the ratio method is that the burnup of the cylindrical fuel compacts can determined in small (2.5 mm) axial increments and an axial burnup profile can be produced. Destructive chemical analysis by inductively coupled mass spectrometry (ICP MS) was then performed on selected compacts that were representative of the expected range of fuel burnups in the experiment to compare with the burnup values determined by gamma spectrometry. The compacts analyzed by mass spectrometry had a burnup range of 19.3% FIMA to 10.7% FIMA. The mass spectrometry evaluation of burnup for the four compacts agreed well with the gamma spectrometry burnup evaluations and the expected burnup from simulation. For all four compacts analyzed by mass spectrometry, the maximum range in the three experimentally determined values and the predicted value was 6% or less. Furthermore, the results confirm the accuracy of the nondestructive burnup evaluation from gamma spectrometry

  19. An analysis of nuclear fuel burnup in the AGR-1 TRISO fuel experiment using gamma spectrometry, mass spectrometry, and computational simulation techniques

    DOE PAGESBeta

    Harp, Jason M.; Demkowicz, Paul A.; Winston, Philip L.; Sterbentz, James W.

    2014-09-03

    AGR 1 was the first in a series of experiments designed to test US TRISO fuel under high temperature gas-cooled reactor irradiation conditions. This experiment was irradiated in the Advanced Test Reactor (ATR) at Idaho National Laboratory (INL) and is currently undergoing post irradiation examination (PIE) at INL and Oak Ridge National Laboratory. One component of the AGR 1 PIE is the experimental evaluation of the burnup of the fuel by two separate techniques. Gamma spectrometry was used to non destructively evaluate the burnup of all 72 of the TRISO fuel compacts that comprised the AGR 1 experiment. Two methodsmore » for evaluating burnup by gamma spectrometry were developed, one based on the Cs 137 activity and the other based on the ratio of Cs 134 and Cs 137 activities. Burnup values determined from both methods compared well with the values predicted from simulations. The highest measured burnup was 20.1% FIMA for the direct method and 20.0% FIMA for the ratio method (compared to 19.56% FIMA from simulations). An advantage of the ratio method is that the burnup of the cylindrical fuel compacts can determined in small (2.5 mm) axial increments and an axial burnup profile can be produced. Destructive chemical analysis by inductively coupled mass spectrometry (ICP MS) was then performed on selected compacts that were representative of the expected range of fuel burnups in the experiment to compare with the burnup values determined by gamma spectrometry. The compacts analyzed by mass spectrometry had a burnup range of 19.3% FIMA to 10.7% FIMA. The mass spectrometry evaluation of burnup for the four compacts agreed well with the gamma spectrometry burnup evaluations and the expected burnup from simulation. For all four compacts analyzed by mass spectrometry, the maximum range in the three experimentally determined values and the predicted value was 6% or less. Furthermore, the results confirm the accuracy of the nondestructive burnup evaluation from gamma

  20. Ionic liquid based in situ solvent formation microextraction coupled to thermal desorption for chlorophenols determination in waters by gas chromatography/mass spectrometry.

    PubMed

    Galán-Cano, Francisco; Lucena, Rafael; Cárdenas, Soledad; Valcárcel, Miguel

    2012-03-16

    A simple and efficient method for the determination of ten chlorophenols (including mono, di, tri, tetra and pentachlorophenols) in water samples is presented. The analytical method is based on a previous derivatization of the target compounds with acetic anhydride, being the derivatized compounds finally isolated/preconcentrated by an in situ solvent formation microextraction. Later on the extractant (an ionic liquid) containing the analytes is recovered by centrifugation and thermally desorbed. The analytes are finally separated and determined by gas chromatography/mass spectrometry. The main variables involved in the extraction and thermal desorption steps have been studied in depth. Once evaluated, the analytical method has been characterized in terms of linearity, sensitivity, precision and accuracy. The limits of detection were in the range from 60 ng L(-1) (4-chlorophenol) to 440 ng L(-1) (pentachlorophenol) while the precision, expressed as relative standard deviation, was in the interval from 4.5% (2,6-dichlorophenol) to 9.9% (3-chlorophenol). In addition, acceptable recovery values were obtained in samples of different nature, including river, tap and reservoir water samples. PMID:22307153

  1. Apparatus for measuring the stopping power of active materials evaporated in situ and characterized by Auger electron spectrometry and Rutherford backscattering

    NASA Astrophysics Data System (ADS)

    Semrad, D.; Bauer, P.; Eder, K.; Obermann, W.

    1986-07-01

    An ultrahigh-vacuum scattering chamber working in the low 10-9-mbar range is described. It is attached to a standard O-ring sealed beam transport system of an electrostatic accelerator. Twelve targets can be prepared in situ, one by one, by evaporating the material onto backings, which are mounted on tiltable target holders on a wheel. Backscattering spectra are obtained from these targets and the stopping cross section is deduced from their widths. A cooled high-resolution surface barrier detector is used for this purpose. The integral concentrations of light impurities in the target are obtained using Rutherford backscattering (RBS), whereas Auger electron spectrometry (AES) together with a sputtering device is used to determine the depth composition. As a test of the assembly we determined the stopping power of aluminum for protons and deuterons, respectively. The results are compared to published tables based upon fits to experiments. The influence of impurities on the result is discussed for an aluminum target prepared under standard evaporation conditions.

  2. Apparatus for measuring the stopping power of active materials evaporated in situ and characterized by Auger electron spectrometry and Rutherford backscattering

    SciTech Connect

    Semrad, D.; Bauer, P.; Eder, K.; Obermann, W.

    1986-07-01

    An ultrahigh-vacuum scattering chamber working in the low 10/sup -9/-mbar range is described. It is attached to a standard O-ring sealed beam transport system of an electrostatic accelerator. Twelve targets can be prepared in situ, one by one, by evaporating the material onto backings, which are mounted on tiltable target holders on a wheel. Backscattering spectra are obtained from these targets and the stopping cross section is deduced from their widths. A cooled high-resolution surface barrier detector is used for this purpose. The integral concentrations of light impurities in the target are obtained using Rutherford backscattering (RBS), whereas Auger electron spectrometry (AES) together with a sputtering device is used to determine the depth composition. As a test of the assembly we determined the stopping power of aluminum for protons and deuterons, respectively. The results are compared to published tables based upon fits to experiments. The influence of impurities on the result is discussed for an aluminum target prepared under standard evaporation conditions.

  3. Sublimation extraction coupled with gas chromatography-mass spectrometry: A new technique for future in situ analyses of purines and pyrimidines on Mars

    NASA Astrophysics Data System (ADS)

    Glavin, D. P.; Cleaves, H. J.; Buch, A.; Schubert, M.; Aubrey, A.; Bada, J. L.; Mahaffy, P. R.

    2006-12-01

    We have developed a sublimation technique coupled with chemical derivatization and gas chromatography mass spectrometry (GC-MS) to detect nucleobases and other volatile organic compounds derived from bacteria in Mars analog materials. To demonstrate this technique, a sample of serpentine inoculated with Escherichia coli ( E. coli) cells was heated to 500 °C for several seconds under Martian ambient pressure. The sublimate was collected on a cold finger, then derivatized and analyzed by GC-MS. We found that adenine, cytosine, thymine and uracil were the most abundant molecules detected in the sublimed E. coli extract by GC-MS. In addition, nucleobases were also detected in sublimed extracts of a deep-sea sediment sample, seawater, and soil collected from the Atacama Desert in Chile after heating the samples under the same conditions. Our results indicate that nucleobases can be easily isolated directly from natural samples using sublimation and then detected by GC-MS after chemical derivatization. The sublimation-based extraction technique is one approach that should be considered for use by future in situ instruments designed to detect organic compounds relevant to life in the Martian regolith.

  4. Rapid determination of alkylphenols in aqueous samples by in situ acetylation and microwave-assisted headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry.

    PubMed

    Wu, Yu-Pei; Wang, Yu-Chen; Ding, Wang-Hsien

    2012-08-01

    A rapid and solvent-free procedure for the determination of 4-tert-octylphenol and 4-nonylphenol isomers in aqueous samples is described. The method involves in-situ acetylation and microwave-assisted headspace solid-phase microextraction prior to their determination using gas chromatography-ion trap mass spectrometry operated in the selected ion storage mode. The dual experimental protocols to evaluate the effects of various derivatization and extraction parameters were investigated and the conditions optimized. Under optimized conditions, 300 μL of acetic anhydride mixed with 1 g of potassium hydrogencarbonate and 2 g of sodium chloride in a 20 mL aqueous sample were efficiently extracted by a 65 μm polydimethylsiloxane-divinylbenzene fiber that was located in the headspace when the system was microwave irradiated at 80 W for 5 min. The limits of quantitation were 5 and 50 ng/L for 4-tert-octylphenol and 4-nonylphenol isomers, respectively. The precision for these analytes, as indicated by relative standard deviations, were less than 8% for both intra- and inter-day analysis. Accuracy, expressed as the mean extraction recovery, was between 74 to 88%. A standard addition method was used to quantitate 4-tert-octylphenol and 4-nonylphenol isomers, and the concentrations ranged from 120 to 930 ng/L in various environmental water samples. PMID:22899640

  5. Radioactivity of a Rock Profile from Rio do Rasto Formation Measured by High Resolution Gamma Spectrometry

    NASA Astrophysics Data System (ADS)

    Bastos, Rodrigo O.; Appoloni, Carlos R.; Pinese, José P. P.

    2011-08-01

    Natural occurring radionuclides are present in different concentrations in sedimentary rocks. Generally, their distribution correlates reasonably with their geo-physicochemical behavior during sediment deposition and rock consolidation. This fact permits to study some geological characteristics of the rocks by analyzing the radionuclide distribution in the rocks, as it might reflect the origin of the sediments, the depositional environment, and more recent events such as weathering and erosion. In this work, rocks from an exposed profile of the Rio do Rasto Formation were collected and analyzed in laboratory by high resolution gamma spectrometry for 226Ra, 232Th and 40K determination. It was employed a standard gamma ray spectrometry electronic chain, with a 66% relative efficiency HPGe detector. The efficiency calibration, as well as its validation, was accomplished with eight International Atomic Energy Agency certified samples. The outcrop exposes layers of sandstone and siltstone and, secondarily, claystone, with varying colors (gray, red and green). The rocks were collected along this profile, each of them was dried in the open air during 48 hours, grounded, sieved through 4 mm mesh and sealed in cylindrical recipients. The 226Ra, 232Th and 40K activity concentrations are presented, their distribution and the possible relations among activities are analyzed. The general pattern of radionuclides distribution respects well the hypotheses on geo-physicochemical behavior of radioactive elements.

  6. Applications of gamma-ray spectrometry in the quantitative nondestructive assay of special nuclear materials

    SciTech Connect

    Sampson, T.E.; Parker, J.L.

    1990-04-16

    Nearly all applications of gamma-ray spectrometry in the quanitative assay of special nuclear materials can be grouped into five general categories. They are as follows: (1) Quanitative passive assay, of which transmission-corrected passive assay methods for measuring isotopic masses/concentrations are an important subset; (2) Enrichment measurements on infinitely thick'' samples for absolute determination of isotopic fractions/concentrations; (3) Measurements of isotopic ratios using relative detection efficiency principles resulting in absolute isotopic distributions without recourse to standards; (4) Absorption-edge densitometry measurements of elemental concentrations; and (5) X-ray fluorescence measurements of elemental concentrations. Careful and correct practice of these techniques can yield measurement accuracies in the range of 0.1% to 1.0% in favorable situations with measurement times generally in the range of 15 minutes to 1 hour. We present examples of these general categories with emphasis on those measurements and techniques exhibiting the best accuracy, as well as those which are not routinely practiced in many other applications of gamma-ray spectrometry. 20 refs., 6 fig.

  7. Development of a method for in situ measurement of denitrification in aquifers using 15N tracer tests and membrane inlet mass spectrometry

    NASA Astrophysics Data System (ADS)

    Eschenbach, W.; Well, R.; Flessa, H.; Walther, W.; Duijnisveld, W. H. M.

    2009-04-01

    In NO3- contaminated aquifers containing reduced compounds like organic carbon or sulfides, denitrification is an intense process. Its characterization is of interest because NO3- consump-tion improves water quality and N2O production can cause emission of this greenhouse gas to the atmosphere. Spatial distribution of NO3- and N2 produced by denitrification in groundwa-ter (excess N2) reflects the NO3- input as well as cumulative denitrification during aquifer pas-sage. Reaction progress (RP) at a given location, i.e. the relative consumption by denitrifica-tion of the NO3- that had been leached to the aquifers, characterizes the stage of the denitrifi-cation process. RP can be derived from the ratio between accumulated gaseous denitrification products and initial NO3- concentrations. The amount and spatial distribution of reduced com-pounds within denitrifying aquifers is not well known. Recent findings from parallel investi-gations on in situ denitrification and reactive compounds suggests that single-well 15N tracer tests might be suitable to characterize the stock of reduced compounds in aquifers (Konrad 2007). The overall objective of our studies is measure the spatial dynamics of denitrification within two sandy aquifers in northern Germany. This includes measurement of the actually occurring denitrification process. Moreover we want to determine the long-term denitrification potential which is governed by the stock of reactive material. Here we present a new approach for in situ-measurement of denitrification at monitoring wells using a combination of 15N-tracer push-pull experiments with in situ analysis of 15N-labled N2 and N2O using membrane inlet mass spectrometry (MIMS). We will present first results from a laboratory test with aquifer mesocosms using the MIMS method. In this test we supplemented aquifer material of two depths (2 and 7 m below surface) of a drinking water catchment in Northwest Germany with K15NO3 solution. After tracer application we

  8. Total Absorption Gamma-ray Spectrometer (TAGS) Intensity Distributions from INL's Gamma-Ray Spectrometry Center

    DOE Data Explorer

    Greenwood, R. E.

    A 252Cf fission-product source and the INL on-line isotope separator were used to supply isotope-separated fission-product nuclides to a total absorption -ray spectrometer. This spectrometer consisted of a large (25.4-cm diameter x 30.5-cm long) NaI(Tl) detector with a 20.3-cm deep axial well in which is placed a 300-mm2 x 1.0-mm Si detector. The spectra from the NaI(Tl) detector are collected both in the singles mode and in coincidence with the B-events detected in the Si detector. Ideally, this detector would sum all the energy of the B- rays in each cascade following the population of daughter level by B- decay, so that the event could be directly associated with a particular daughter level. However, there are losses of energy from attenuation of the rays before they reach the detector, transmission of rays through the detector, escape of secondary photons from Compton scattering, escape of rays through the detector well, internal conversion, etc., and the measured spectra are thus more complicated than the ideal case and the analysis is more complex. Analysis methods have been developed to simulate all of these processes and thus provide a direct measure of the B- intensity distribution as a function of the excitation energy in the daughter nucleus. These data yield more accurate information on the B- distribution than conventional decay-scheme studies for complex decay schemes with large decay energies, because in the latter there are generally many unobserved and observed but unplaced rays. The TAGS data have been analyzed and published [R. E. Greenwood et al., Nucl Instr. and metho. A390(1997)] for 40 fission product-nuclides to determine the B- intensity distributions. [Copied from the TAGS page at http://www.inl.gov/gammaray/spectrometry/tags.shtml]. Those values are listed on this page for quick reference.

  9. Monte Carlo based method for conversion of in-situ gamma ray spectra obtained with a portable Ge detector to an incident photon flux energy distribution.

    PubMed

    Clouvas, A; Xanthos, S; Antonopoulos-Domis, M; Silva, J

    1998-02-01

    A Monte Carlo based method for the conversion of an in-situ gamma-ray spectrum obtained with a portable Ge detector to photon flux energy distribution is proposed. The spectrum is first stripped of the partial absorption and cosmic-ray events leaving only the events corresponding to the full absorption of a gamma ray. Applying to the resulting spectrum the full absorption efficiency curve of the detector determined by calibrated point sources and Monte Carlo simulations, the photon flux energy distribution is deduced. The events corresponding to partial absorption in the detector are determined by Monte Carlo simulations for different incident photon energies and angles using the CERN's GEANT library. Using the detector's characteristics given by the manufacturer as input it is impossible to reproduce experimental spectra obtained with point sources. A transition zone of increasing charge collection efficiency has to be introduced in the simulation geometry, after the inactive Ge layer, in order to obtain good agreement between the simulated and experimental spectra. The functional form of the charge collection efficiency is deduced from a diffusion model. PMID:9450590

  10. Cosmic veto gamma-spectrometry for Comprehensive Nuclear-Test-Ban Treaty samples

    NASA Astrophysics Data System (ADS)

    Burnett, J. L.; Davies, A. V.

    2014-05-01

    The Comprehensive Nuclear-Test-Ban Treaty (CTBT) is supported by a global network of monitoring stations that perform high-resolution gamma-spectrometry on air filter samples for the identification of 85 radionuclides. At the UK CTBT Radionuclide Laboratory (GBL15), a novel cosmic veto gamma-spectrometer has been developed to improve the sensitivity of station measurements, providing a mean background reduction of 80.8% with mean MDA improvements of 45.6%. The CTBT laboratory requirement for a 140Ba MDA is achievable after 1.5 days counting compared to 5-7 days using conventional systems. The system consists of plastic scintillation plates that detect coincident cosmic-ray interactions within an HPGe gamma-spectrometer using the Canberra LynxTM multi-channel analyser. The detector is remotely configurable using a TCP/IP interface and requires no dedicated coincidence electronics. It would be especially useful in preventing false-positives at remote station locations (e.g. Halley, Antarctica) where sample transfer to certified laboratories is logistically difficult. The improved sensitivity has been demonstrated for a CTBT air filter sample collected after the Fukushima incident.

  11. Nondestructive characterization of radioactive waste drums by gamma spectrometry: a Monte Carlo technique for efficiency calibration.

    PubMed

    Tzika, Faidra; Savidou, Anastasia; Stamatelatos, Ion E

    2007-11-01

    A semi-empirical non-destructive technique to assay radioactive waste drums is presented. The technique is based on gamma spectrometry performed using a portable NaI detector and Monte Carlo simulations using the MCNP code in order to derive the gamma ray detector efficiency for the volume source. The derivation of detector efficiency was performed assuming homogeneous distribution of the source activity within the matrix material. Moreover, the MCNP model was used to examine the effect of inhomogeneities in activity distribution, variation of matrix material density, and drum filling height on the accuracy of the technique, and to estimate the measurement bias. The technique was verified by estimating radioactivity levels in 25 drums containing ion exchange resin waste, and comparing the results of the non-destructive method against the analytical results of samples obtained from each drum. Satisfactory agreement between the two assay techniques was observed. The discussed technique represents a cost effective technology that can be used to assay low-activity, low-density waste drums provided the contribution to the gamma ray spectrum can be resolved. PMID:18049246

  12. The 124Sb activity standardization by gamma spectrometry for medical applications

    NASA Astrophysics Data System (ADS)

    de Almeida, M. C. M.; Iwahara, A.; Delgado, J. U.; Poledna, R.; da Silva, R. L.

    2010-07-01

    This work describes a metrological activity determination of 124Sb, which can be used as radiotracer, applying gamma spectrometry methods with hyper pure germanium detector and efficiency curves. This isotope with good activity and high radionuclidic purity is employed in the form of meglumine antimoniate (Glucantime) or sodium stibogluconate (Pentostam) to treat leishmaniasis. 124Sb is also applied in animal organ distribution studies to solve some questions in pharmacology. 124Sb decays by β-emission and it produces several photons (X and gamma rays) with energy varying from 27 to 2700 keV. Efficiency curves to measure point 124Sb solid sources were obtained from a 166mHo standard that is a multi-gamma reference source. These curves depend on radiation energy, sample geometry, photon attenuation, dead time and sample-detector position. Results for activity determination of 124Sb samples using efficiency curves and a high purity coaxial germanium detector were consistent in different counting geometries. Also uncertainties of about 2% ( k=2) were obtained.

  13. First Year PIDDP Report on gamma-ray and x-ray spectroscopy: X-ray remote sensing and in situ spectroscopy for planetary exploration missions and gamma-ray remote sensing and in situ spectroscopy for planetary exploration missions

    NASA Technical Reports Server (NTRS)

    Mahdavi, M.; Giboni, K. L.; Vajda, S.; Schweitzer, J. S.; Truax, J. A.

    1994-01-01

    Detectors that will be used for planetary missions must have their responses calibrated in a reproducible manner. In addition, it is important to characterize a detector system at uneven portions of its life cycle, for example after exposure to different amounts of radiation. A calibration and response characterization facility has been constructed at Schlumberger-Doll Research for all types of gamma- and x-ray detectors that may be used for planetary measurement. This facility is currently being tested. Initial use is expected for the MARS 94 detectors. The facility will then also be available for calibrating other detectors as well as arrays of detectors such as the NEAR detector with its central Nal(TI) crystal surrounded with a large BGO crystal. Cadmium telluride detectors are investigated for applications in space explorations. These detectors show an energy resolution of 5 keV for the 122 keV 57Co line. Earlier reported polarization effects are not observed. The detectors can be used at temperatures up to 100 C, although with reduced energy resolution. The thickness of standard detectors is limited to 2 mm. These detectors become fully efficient at bias voltages above 200 V. Initial results for a 1 cm thick detector show that the quality of the material is inferior to the thinner standard detectors and hole trapping affects the pulse height. A detailed characterization of the detector is in progress. Prototypes of photomultipliers based on a Channel Electron Multiplier (CEM) are being built to study their performance. Such photomultipliers promise better timing characteristics and a higher dynamic range while being more compact and of lower in weight.

  14. Analysis of spectra from portable handheld gamma-ray spectrometry for terrain comparative assessment.

    PubMed

    Dias, Flávio; Lima, Marco; Sanjurjo-Sánchez, Jorge; Alves, Carlos

    2016-04-01

    Geological characteristics can have impacts on societal development by, e.g., geotechnical issues and radiological hazard levels. Due to urban sprawl, there is an increasing need for detailed geological assessment. In this work are analysed data from portable handheld gamma-ray spectra (K, eU and eTh) obtained in granitic and Silurian metaclastic outcrops as well as in an profile, roughly N-S, on soil covered terrains transecting a mapped contact between these rock types (the profile's northern extremity is at locations mapped as granite). Estimations from gamma-ray spectra were studied by univariate and multivariate analyses. K, eU and eTh values were higher on granite in relation to Silurian metaclastic rocks. The northern extremity of the profile showed clearly higher contents of eTh and this contrast was supported by univariate statistical tools (normality plot and Wilk-Shapiro test; boxplots). A ternary plot with the contribution of the elements to gamma-ray absorbed dose showed the separation of granite from Silurian metaclastic rocks with the former being nearer the eTh vertex. The points in the northern extremity of the profile are nearer the eTh vertex than the other points on the profile. These visual suggestions were supported by hierarchical cluster analysis, which was able to differentiate between granite and metaclastic outcrops and separate portions of the profile located on different terrains. Portable gamma-ray spectrometry showed, hence, the potential to distinguish granite and metaclastic terrains at a scale useful for engineering works. These results can also be useful for a first comparative zoning of radiological hazards (which are higher for granite). PMID:26867098

  15. Let them fly or light them up: matrix-assisted laser desorption/ionization time of flight (MALDI-TOF) mass spectrometry and fluorescence in situ hybridization (FISH).

    PubMed

    Schweickert, Birgitta; Moter, Annette; Lefmann, Michael; Göbel, Ulf B

    2004-01-01

    This review focuses on clinical bacteriology and by and large does not cover the detection of fungi, viruses or parasites. It discusses two completely different but complementary approaches that may either supplement or replace classic culture-based bacteriology. The latter view may appear provocative in the light of the actual market penetration of molecular genetic testing in clinical bacteriology. Despite its elegance, high specificity and sensitivity, molecular genetic diagnostics has not yet reached the majority of clinical laboratories. The reasons for this are manifold: Many microbiologists and medical technologists are more familiar with classical microbiological methods than with molecular biology techniques. Culture-based methods still represent the work horse of everyday routine. The number of available FDA-approved molecular genetic tests is limited and external quality control is still under development. Finally, it appears difficult to incorporate genetic testing in the routine laboratory setting due to the limited number of samples received or the lack of appropriate resources. However, financial and time constraints, particularly in hospitals as a consequence of budget cuts and reduced length of stay, lead to a demand for significantly shorter turnaround times that cannot be met by culture-dependent diagnosis. As a consequence, smaller laboratories that do not have the technical and personal equipment required for molecular genetic amplification techniques may adopt alternative methods such as fluorescence in situ hybridization (FISH) that combines easy-to-perform molecular hybridization with microscopy, a technique familiar to every microbiologist. FISH is hence one of the technologies presented here. For large hospital or reference laboratories with a high sample volume requiring massive parallel high-throughput testing we discuss matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF) of nucleic acids, a

  16. In situ gamma ray survey for geological mapping of Kmetasomatized metavolcanics at Bükkszentkereszt, Bükk Mts, Hungary

    NASA Astrophysics Data System (ADS)

    Németh, Norbert; Pethõ, Gábor; Zajzon, Norbert

    2015-09-01

    The Middle-Upper Triassic Bagolyhegy Metarhyolite Formation of the Bükk Mts. (Hungary) hosts silicified bodies with high potassic feldspar content formed by Kmetasomatism. The rocks underwent a multistage deformation history including syn- and postmetamorphic folding and faulting. As the outcrop area is covered by soil and debris with some exposed silicified cliffs only, and potassium content is a characteristic feature of the metasomatized rocks, geological mapping was supported by a spectral gamma ray survey with a scintillation detector of NaI(Tl) crystal. A thunderstorm felling the beech forest made the soil horizon B also accessible in several pits, providing the opportunity to make measurements on the weathered debris instead of the topsoil (horizon A). Measurements in different arrangements were designed to test the effects of measuring time, measuring geometry and soil horizon. Our results show that concentration values obtained on the debris with a 2 min measuring time can be compared with those measured on exposed rock surfaces, producing a more reliable geological map than measurements on the topsoil with randomly variable K depletion. Pit geometry effects can be eliminated by the K/(eU+eTh) ratio. This results in a more realistic K distribution map if neither U nor Th enrichments are present. The survey successfully delineated the unexposed outcrop of K-enriched rocks on the survey area.

  17. An iterative approach for TRIGA fuel burn-up determination using nondestructive gamma-ray spectrometry.

    PubMed

    Wang, T K; Peir, J J

    2000-01-01

    The purpose of this work is to establish a method for evaluating the burn-up values of the rod-type TRIGA spent fuel by using gamma-ray spectrometry of the short-lived fission products 97Zr/97Nb, 132I, and 140La. Fuel irradiation history is not needed in this method. Short-lived fission-product activities were established by reirradiating the spent fuels in a nuclear reactor. Based on the measured activities, 235U burn-up values can be deduced by iterative calculations. The complication caused by 239Pu production and fission is also discussed in detail. The burn-up values obtained by this method are in good agreement with those deduced from the conventional method based on long-lived fission products 137Cs, 134Cs/137Cs ratio and 106Ru/137Cs ratio. PMID:10670930

  18. The use of difference spectra with a filtered rolling average background in mobile gamma spectrometry measurements

    NASA Astrophysics Data System (ADS)

    Cresswell, A. J.; Sanderson, D. C. W.

    2009-08-01

    The use of difference spectra, with a filtering of a rolling average background, as a variation of the more common rainbow plots to aid in the visual identification of radiation anomalies in mobile gamma spectrometry systems is presented. This method requires minimal assumptions about the radiation environment, and is not computationally intensive. Some case studies are presented to illustrate the method. It is shown that difference spectra produced in this manner can improve signal to background, estimate shielding or mass depth using scattered spectral components, and locate point sources. This approach could be a useful addition to the methods available for locating point sources and mapping dispersed activity in real time. Further possible developments of the procedure utilising more intelligent filters and spatial averaging of the background are identified.

  19. Fast-ion energy resolution by one-step reaction gamma-ray spectrometry

    NASA Astrophysics Data System (ADS)

    Salewski, M.; Nocente, M.; Gorini, G.; Jacobsen, A. S.; Kiptily, V. G.; Korsholm, S. B.; Leipold, F.; Madsen, J.; Moseev, D.; Nielsen, S. K.; Rasmussen, J.; Stejner, M.; Tardocchi, M.; Contributors, JET

    2016-04-01

    The spectral broadening of γ-rays from fusion plasmas can be measured in high-resolution gamma-ray spectrometry (GRS). We derive weight functions that determine the observable velocity space and quantify the velocity-space sensitivity of one-step reaction high-resolution GRS measurements in magnetized fusion plasmas. The weight functions suggest that GRS resolves the energies of fast ions directly without the need for tomographic inversion for selected one-step reactions at moderate plasma temperatures. The D(p,γ)3He reaction allows the best direct fast-ion energy resolution. We illustrate our general formalism using reactions with and without intrinsic broadening of the γ-rays for the GRS diagnostic at JET.

  20. Low-level gamma spectrometry using beta coincidence and Compton suppression.

    PubMed

    Grigorescu, E L; De Felice, P; Razdolescu, Anamaria-Cristina; Luca, A

    2004-01-01

    A low-level gamma-ray spectrometry system was developed using a Ge(Li) detector with 6% relative efficiency coupled to a 2pi beta plastic detector for coincidence selection and a massive NaI(Tl) detector for Compton suppression. The integral background count rate for (50-1500)keV was 0.5 s(-1)kg(-1) (Ge), using only beta coincidences. With Compton suppression, a value of 0.25 s(-1)kg(-1) (Ge) was obtained. Spectra with and without Compton suppression were studied for 60Co, 137Cs and 152Eu point sources. Considerations are made concerning the Compton suppression advantages in different situations. PMID:15177343

  1. Elemental compositions and ages of lunar samples by nondestructive gamma-ray spectrometry.

    PubMed

    O'kelley, G D; Eldridge, J S; Schonfeld, E; Bell, P R

    1970-01-30

    A gamma-ray spectrometry system with low background was used to determine the radioactivity of crystalline rocks, breccias, and fine material. Nuclides identified were (40)K, (232)Th, (238)U, (7)Be, (22)Na (26)A1, (44)Ti, (46)Sc, (48)V, (52)Mn, (54)Mn, and (56)Co. Concentrations of K, Th, and U ranged between 480 and 2550, 1.01 and 3.30, and 0.26 and 0.83 parts per million, respectively. Concentrations of thorium and uranium were those of terrestrial basalts, while the potassium concentrations were near values for chondrites. Products of low-energy nuclear reactions showed pronounced concentration gradients at rock surfaces. Concentrations of K and of (22)Na determined here were combined with concentrations of rare gases to estimate gas-retention ages and cosmic-ray exposure ages with ranges of 2200 to 3200 and 34 to 340 million years, respectively, for three rocks. PMID:17781504

  2. A review of the nationwide proficiency test on natural radioactivity measurements by gamma spectrometry.

    PubMed

    Şahin, N K; Yeltepe, E; Yücel, Ü

    2016-03-01

    This study is the review of the first proficiency test on radioactivity measurement organized in Turkey by Sarayköy Nuclear Research and Training Center (SANAEM) of Turkish Atomic Energy Authority (TAEK) in 2013. The objective of the test was to determine (226)Ra, (232)Th and (40)K activity concentrations in natural soil samples using gamma-ray spectrometry. The bulk material consisting of uranium- and thorium-rich soil and sand was milled, mixed thoroughly and sieved. Homogeneity of the final mix was tested with 6 randomly taken samples. 16 proficiency test samples were distributed to 16 participating laboratories. 12 laboratories reported results. The results were evaluated on the accuracy and precision criteria adopted by the IAEA Proficiency Testing Group. The percentage of acceptable scores was 49%. Some recommendations have been provided to the laboratories to improve the quality of their results. It is planned to extend these proficiency tests periodically for various radionuclides in various matrices. PMID:26750585

  3. The Sandwich spectrometer for ultra low-level gamma-ray spectrometry.

    PubMed

    Wieslander, J S Elisabeth; Hult, Mikael; Gasparro, Joël; Marissens, Gerd; Misiaszek, Marcin; Preusse, Werner

    2009-05-01

    The technical details and performance of the newly developed Sandwich spectrometer for ultra low-level gamma-ray spectrometry are presented. The spectrometer, which consists of two HPGe detectors, an active muon shield and a lead/copper shield with a convenient and rapid opening mechanism, is located in an underground laboratory at a depth of 500 m water equivalent. The data is collected in list mode, which enables off-line data analysis to identify muon-induced events and possible Ge detector crosstalk due to Compton scattering. The background count-rate from 40 to 2700 keV normalised to the mass of the Ge crystals is 220 day(-1)kg(-1). PMID:19246202

  4. Summary of gamma spectrometry on local air samples from 1985--1995

    SciTech Connect

    Winn, W.G.

    1997-04-02

    This report summarizes the 1985--1995 results of low-level HPGe gamma spectrometry analysis of high-volume air samples collected at the Aiken Airport, which is about 25 miles north of SRS. The author began analyzing these samples with new calibrations using the newly developed GRABGAM code in 1985. The air sample collections were terminated in 1995, as the facilities at the Aiken Airport were no longer available. Air sample measurements prior to 1985 were conducted with a different analysis system (and by others prior to 1984), and the data were not readily available. The report serves to closeout this phase of local NTS air sample studies, while documenting the capabilities and accomplishments. Hopefully, the information will guide other applications for this technology, both locally and elsewhere.

  5. NMIS with Imaging and Gamma Ray Spectrometry for Pu, HEU, HE and Other Materials

    SciTech Connect

    Mihalczo, John T; Mullens, James Allen

    2012-03-01

    The Nuclear Material Identification System (NMIS) has been under development at ORNL and the National Nuclear Security Administration (NNSA) Y-12 National Security Complex since 1984. In the mid-1990s, what is now the US Department of Energy (DOE) Office of Nuclear Verification (ONV) realized that it was a useful technology for future arms control treaty applications and supported further development of the system. In 2004, fast-neutron imaging was incorporated into the system. In 2007, the ONV decided to develop a fieldable version of the system, designated as FNMIS, for potential use in future treaties. The FNMIS is being developed to be compatible with the eventual incorporation of gamma-ray spectrometry and an information barrier. This report addresses how and what attributes could be determined by the FNMIS system with gamma-ray spectrometry. The NMIS is a time-dependent coincidence system that incorporates tomographic imaging (including mapping of the fission sites) and gamma-ray spectrometry. It utilizes a small, lightweight (30 lb), portable deuterium-tritium (DT) neutron (14.1 MeV) generator (4 x 10{sup 7} neutrons/second) for active interrogation and can also perform passive interrogation. A high-purity germanium (HPGe) gamma-ray detector with multichannel analysis can be utilized in conjunction with the source for active interrogation or passively. The system uses proton recoil scintillators: 32 small 2.5 x 2.5 x 10.2-cm-thick plastic scintillators for imaging and at least two 2 x 2 arrays of 27 x 27 x 10-cm-thick plastic scintillators that detect induced fission radiation. The DT generator contains an alpha detector that time and directionally tags a fan beam of some of the neutrons emitted and subdivides it into pixels. A fast (1 GHz) time correlation processor measures the time-dependent coincidence among all detectors in the system. A computer-controlled scanner moves the small detectors and the source appropriately for scanning a target object for

  6. High sensitivity gamma spectrometry of air samples near SRS during 1985-1995

    SciTech Connect

    Winn, W.G.; Cadieux, J.R.

    1997-07-01

    High sensitivity gamma analysis of off-site air samples near the Savannah River Site (SRS) is achieved by collecting large volume air samples for analysis by ultra-low-level gamma spectrometry. A review of the 1985-1995 measurements has highlighted local and distant releases of man-made radionuclides, along with cosmogenic radionuclides which correlate with both solar and seasonal phenomena. Measurements typically involve 2-day air collection of a 70,000 m{sup 3} sample on a 51 cm x 51 cm cellulose filter using a high-capacity pump. Short-lived radon background activity is allowed to decay a few days, and then the filter is configured into a smaller calibrated volume and counted 1-3 days on a 30 percent-efficient HPGe in the Ultra-Low-Level Counting Facility. Representative detection limits for this method are shown in Table 1, and even lower limits are achievable by counting on the low-background 160 percent-efficient HPGe of the Underground Counting Facility.

  7. Application of gamma-ray spectrometry in a NORM industry for its radiometrical characterization

    NASA Astrophysics Data System (ADS)

    Mantero, J.; Gázquez, M. J.; Hurtado, S.; Bolívar, J. P.; García-Tenorio, R.

    2015-11-01

    Industrial activities involving Naturally Occurring Radioactive Materials (NORM) are found among the most important industrial sectors worldwide as oil/gas facilities, metal production, phosphate Industry, zircon treatment, etc. being really significant the radioactive characterization of the materials involved in their production processes in order to assess the potential radiological risk for workers or natural environment. High resolution gamma spectrometry is a versatile non-destructive radiometric technique that makes simultaneous determination of several radionuclides possible with little sample preparation. However NORM samples cover a wide variety of densities and composition, as opposed to the standards used in gamma efficiency calibration, which are either water-based solutions or standard/reference sources of similar composition. For that reason self-absorption correction effects (especially in the low energy range) must be considered individually in every sample. In this work an experimental and a semi-empirical methodology of self-absorption correction were applied to NORM samples, and the obtained results compared critically, in order to establish the best practice in relation to the circumstances of an individual laboratory. This methodology was applied in samples coming from a TiO2 factory (NORM industry) located in the south-west of Spain where activity concentration of several radionuclides from the Uranium and Thorium series through the production process was measured. These results will be shown in this work.

  8. Efficiency transfer using the GEANT4 code of CERN for HPGe gamma spectrometry.

    PubMed

    Chagren, S; Ben Tekaya, M; Reguigui, N; Gharbi, F

    2016-01-01

    In this work we apply the GEANT4 code of CERN to calculate the peak efficiency in High Pure Germanium (HPGe) gamma spectrometry using three different procedures. The first is a direct calculation. The second corresponds to the usual case of efficiency transfer between two different configurations at constant emission energy assuming a reference point detection configuration and the third, a new procedure, consists on the transfer of the peak efficiency between two detection configurations emitting the gamma ray in different energies assuming a "virtual" reference point detection configuration. No pre-optimization of the detector geometrical characteristics was performed before the transfer to test the ability of the efficiency transfer to reduce the effect of the ignorance on their real magnitude on the quality of the transferred efficiency. The obtained and measured efficiencies were found in good agreement for the two investigated methods of efficiency transfer. The obtained agreement proves that Monte Carlo method and especially the GEANT4 code constitute an efficient tool to obtain accurate detection efficiency values. The second investigated efficiency transfer procedure is useful to calibrate the HPGe gamma detector for any emission energy value for a voluminous source using one point source detection efficiency emitting in a different energy as a reference efficiency. The calculations preformed in this work were applied to the measurement exercise of the EUROMET428 project. A measurement exercise where an evaluation of the full energy peak efficiencies in the energy range 60-2000 keV for a typical coaxial p-type HpGe detector and several types of source configuration: point sources located at various distances from the detector and a cylindrical box containing three matrices was performed. PMID:26623928

  9. Gamma-ray spectrometry of granitic suites of the Paranaguá Terrane, Southern Brazil

    NASA Astrophysics Data System (ADS)

    Weihermann, Jessica Derkacz; Ferreira, Francisco José Fonseca; Cury, Leonardo Fadel; da Silveira, Claudinei Taborda

    2016-09-01

    The Paranaguá Terrane, located in the coastal portion of the states of Santa Catarina, Paraná and São Paulo in Southern Brazil is a crustal segment constituted mainly by an igneous complex, with a variety of granitic rocks inserted into the Serra do Mar ridge. The average altitude is approximately 1200 m above sea level, with peaks of up to 1800 m. Due to the difficulty of accessing the area, a shortage of outcrops and the thick weathering mantle, this terrane is understudied. This research aims to evaluate the gamma-ray spectrometry data of the granitic suites of the Paranaguá Terrane, in correspondence with the geological, petrographical, lithogeochemical, relief and mass movement information available in the literature. Aerogeophysical data were acquired along north-south lines spaced at 500 m, with a mean terrain clearance of 100 m. These data cover potassium (K, %), equivalent in thorium (eTh, ppm) and equivalent in uranium (eU, ppm). After performing a critical analysis of the data, basic (K, eU, eTh) and ternary (R-K/G-eTh/B-eU) maps were generated and then superimposed on the digital elevation model (DEM). The investigation of the radionuclide mobility across the relief and weathering mantle consisted of an analysis of the schematic profiles of elevation related with each radionuclide; a comparison of the K, eU and eTh maps with their 3D correspondents; and the study of mass movements registered in the region. A statistical comparison of lithogeochemical (K, U, Th) and geophysical (K, eU, eTh) data showed consistency in all the granitic suites studied (Morro Inglês, Rio do Poço and Canavieiras-Estrela). Through gamma-ray spectrometry, it was possible to establish relationships between scars (from mass movements) and the gamma-ray responses as well as the radionuclide mobility and the relief and to map the granitic bodies.

  10. Matrix and energy effects during in-situ determination of Cu isotope ratios by ultraviolet-femtosecond laser ablation multicollector inductively coupled plasma mass spectrometry

    NASA Astrophysics Data System (ADS)

    Lazarov, Marina; Horn, Ingo

    2015-09-01

    , carbonates and oxides in situ with a precision of better than 0.1‰ (2SD) without using a matrix-matched standard during laser ablation analyses. Thus, this is a suitable tool to resolve Cu isotopic zoning larger than 0.1‰ in Cu-sulfides, carbonates and oxides.

  11. Profiling of urinary amino-carboxylic metabolites by in-situ heptafluorobutyl chloroformate mediated sample preparation and gas chromatography-mass spectrometry.

    PubMed

    Hušek, Petr; Švagera, Zdeněk; Hanzlíková, Dagmar; Řimnáčová, Lucie; Zahradníčková, Helena; Opekarová, Iva; Šimek, Petr

    2016-04-22

    A novel 1,1,1,2,2,3,3-heptafluorobutyl chloroformate reagent (HFBCF) was examined for in-situ derivatization of amino-carboxylic metabolites in human urine. The arising reaction products exhibit greatly reduced polarity which facilitates combining the derivatization and liquid-liquid microextraction (LLME) from an aqueous urine into an isooctane phase and immediate gas chromatographic-mas spectrometric analysis (GC-MS). The sample preparation protocol is simple, proceeds without an alcohol excess and provides cleaner extracts than other urinary GC-MS based methods. Moreover, thiol metabolites bound in disulfide bonds can be released by reduction with tris(3-hydroxypropyl)phosphine (THP) prior to the developed derivatization and LLME step. In order to evaluate potential of the novel method for GC-MS metabolomics, reaction products of 153 urinary metabolites with HFBCF, particularly those possessing amino and carboxyl groups (56 amino acids and their conjugates, 84 organic acids, 9 biogenic amines, 4 other polar analytes) and two internal standards were investigated in detail by GC-MS and liquid chromatography-mass spectrometry (LC-MS). One hundred and twenty metabolites (78%) yielded a single product, 25 (16%) and 2 metabolites (2-methylcitrate, citrate) generated two and more derivatives. From the examined set, analytically applicable products of 5 metabolites were not detected; the derivatives of 3 metabolites were only suitable for LC-MS analysis. Electron ionization (EI) of the examined analytes contained characteristic, diagnostic ions enabling to distinguish related and isomeric structures. The new method was validated for 132 metabolites using two internal standards in artificial urine and with special attention to potential disease biomarker candidates. The developed sample preparation protocol was finally evaluated by means of a certified organic acid standard mixture in urine and by GC-MS analysis of 100 morning urines obtained from healthy patients (50

  12. On-line interrogation of pebble bed reactor fuel using passive gamma-ray spectrometry

    NASA Astrophysics Data System (ADS)

    Chen, Jianwei

    The Pebble Bed Reactor (PBR) is a helium-cooled, graphite-moderated high temperature nuclear power reactor. In addition to its inherently safe design, a unique feature of this reactor is its multipass fuel cycle in which graphite fuel pebbles (of varying enrichment) are randomly loaded and continuously circulated through the core until they reach their prescribed end-of-life burnup limit (˜80,000--100,000 MWD/MTU). Unlike the situation with conventional light water reactors (LWRs), depending solely on computational methods to perform in-core fuel management will be highly inaccurate. As a result, an on-line measurement approach becomes the only accurate method to assess whether a particular pebble has reached its end-of-life burnup limit. In this work, an investigation was performed to assess the feasibility of passive gamma-ray spectrometry assay as an approach for on-line interrogation of PBR fuel for the simultaneous determination of burnup and enrichment on a pebble-by-pebble basis. Due to the unavailability of irradiated or fresh pebbles, Monte Carlo simulations were used to study the gamma-ray spectra of the PBR fuel at various levels of burnup. A pebble depletion calculation was performed using the ORIGEN code, which yielded the gamma-ray source term that was introduced into the input of an MCNP simulation. The MCNP simulation assumed the use of a high-purity coaxial germanium detector. Due to the lack of one-group high temperature reactor cross sections for ORIGEN, a heterogeneous MCNP model was developed to describe a typical PBR core. Subsequently, the code MONTEBURNS was used to couple the MCNP model and ORIGEN. This approach allowed the development of the burnup-dependent, one-group spectral-averaged PBR cross sections to be used in the ORIGEN pebble depletion calculation. Based on the above studies, a relative approach for performing the measurements was established. The approach is based on using the relative activities of Np-239/I-132 in combination

  13. Development and application of compact denuder sampling techniques with in situ derivatization followed by gas chromatography-mass spectrometry for halogen speciation in volcanic plumes

    NASA Astrophysics Data System (ADS)

    Rüdiger, Julian; Bobrowski, Nicole; Hoffmann, Thorsten

    2015-04-01

    -mass spectrometry gives a limit of detection below 1 ng of bromine. The method was applied on volcanic gas plumes at Mt. Etna and Mt. Stromboli in Italy in July 2014 and on fumarolic gas emissions at Mt. Lastarria in Chile in November 2014. The results show significant amounts of the concerning bromine species (lower ppb range). Comprehensive data evaluation and comparison with results of impinger extraction with NaOH solution as well as chamber experiments are still in progress. References Bobrowski, N. and G. Giuffrida: Bromine monoxide / sulphur dioxide ratios in relation to volcanological observations at Mt. Etna 2006-2009. Solid Earth, 3, 433-445, 2012 Bobrowski, N., R. von Glasow, A. Aiuppa, S. Inguaggiato, I. Louban, O. W. Ibrahim and U. Platt: Reactive halogen chemistry in volcanic plumes. J. Geophys. Res., 112, 2007 Donovan A., V. Tsanev, C. Oppenheimer and M. Edmonds: Reactive halogens (BrO and OClO) detected in the plume of Soufrière Hills Volcano during an eruption hiatus. Geochem. Geophys. Geosyst., 15, 3346-3363, 2014 Huang, R.-J. and T. Hoffmann: A denuder-impinger system with in situ derivatization followed by gas chromatography-mass spectrometry for the determination of gaseous iodine-containing halogen species. Journal of Chromatography A, 1210, 135-141, 2008

  14. In-situ gamma-ray survey of rare-earth tailings dams--A case study in Baotou and Bayan Obo Districts, China.

    PubMed

    Li, Baochuan; Wang, Nanping; Wan, Jianhua; Xiong, Shengqing; Liu, Hongtao; Li, Shijun; Zhao, Rong

    2016-01-01

    An in-situ gamma-ray spectrometer survey with a scintillation detector of NaI(Tl) (Φ75 mm × 75 mm) was carried out in the Baotou and Bayan Obo Districts in order to estimate the levels of natural radionuclides near rare-earth (RE) tailings dams. In the RE tailings dam of Baotou, the mean concentrations of (238)U and (232)Th were 3.0 ± 1.0 mg/kg (range: 1.9-4.6 mg/kg) and 321 ± 31 mg/kg (range: 294-355 mg/kg), respectively. In the Bayan Obo tailings dam, the mean concentrations of (238)U and (232)Th were 5.7 ± 0.5 mg/kg (range: 5.3-6.1 mg/kg) and 276 ± 0.5 mg/kg (range: 275.5-276.3 mg/kg), respectively. The average (232)Th concentrations in the mining areas of the Bayan Obo Mine and the living areas of the Bayan Obo Town were 18.7 ± 7.5 and 26.2 ± 9.1 mg/kg, respectively. The (232)Th concentration recorded in the tailings dams was much higher than the global average (7.44 mg/kg). Our investigation shows that the (232)Th concentration in the tailings in the Baotou dam was 34.6 times greater than that in the local soil (in Guyang County); the average concentrations of (232)Th in the soil in the Baotou District and Bayan Obo Districts were about 1.35 and 2.82 times greater, respectively, than that in the soil in Guyang County. Based on our results, the highest estimated effective dose due to gamma irradiation was 1.15 mSv per year, estimated from the data observed in the Baotou tailings dams. The results of this preliminary study indicate the potential importance of radioactivity in RE tailings dams and that remedial measures may be required. PMID:26555365

  15. Application of low-background gamma-ray spectrometry to monitor radioactivity in the environment and food.

    PubMed

    Khan, A J; Semkow, T M; Beach, S E; Haines, D K; Bradt, C J; Bari, A; Syed, U-F; Torres, M; Marrantino, J; Kitto, M E; Menia, T; Fielman, E

    2014-08-01

    The results are described of an upgrade of the low-background gamma-ray spectrometry laboratory at New York State Department of Health by acquiring sensitivity to low-energy gamma rays. Tuning of the spectrometer and its low-energy response characteristics are described. The spectrometer has been applied to monitor the environment by measuring aerosols and water in New York State contaminated by the 2011 Fukushima accident plume. In addition, the spectrometer has been used to monitor radioactivity in food by performing a study of cesium in Florida milk. PMID:24836905

  16. Gamma-ray spectrometry across the Aalenian-Bajocian boundary in the Lusitanian Basin (Western Portugal)

    NASA Astrophysics Data System (ADS)

    Santos, Marisa; Henriques, Helena; Pena, Rui

    2016-04-01

    supply, which has enabled the faunal recovery, as well as the raise of deep infaunal foraminifers recorded at the latest part of the Discites Biochron. This could be related to the increase of calcareous nannofossil fluxes that coincide with a positive shift in carbon isotope compositions of bulk carbonate in the earliest Bajocian reported by some authors for the Murtinheira and other Iberian sections. In basin analysis of carbonate platforms the integration of major biotic turnovers and gamma-ray spectrometry data can be a useful tool in the improvement of correlation between wells and outcrops. Moreover, they assist in the interpretation of depositional environment and paleoclimatic constrains assigned to a basin.

  17. Assessment of measurement result uncertainty in determination of (210)Pb with the focus on matrix composition effect in gamma-ray spectrometry.

    PubMed

    Iurian, A R; Pitois, A; Kis-Benedek, G; Migliori, A; Padilla-Alvarez, R; Ceccatelli, A

    2016-03-01

    Reference materials were used to assess measurement result uncertainty in determination of (210)Pb by gamma-ray spectrometry, liquid scintillation counting, or indirectly by alpha-particle spectrometry, using its daughter (210)Po in radioactive equilibrium. Combined standard uncertainties of (210)Pb massic activities obtained by liquid scintillation counting are in the range 2-12%, depending on matrices and massic activity values. They are in the range 1-3% for the measurement of its daughter (210)Po using alpha-particle spectrometry. Three approaches (direct computation of counting efficiency and efficiency transfer approaches based on the computation and, respectively, experimental determination of the efficiency transfer factors) were applied for the evaluation of (210)Pb using gamma-ray spectrometry. Combined standard uncertainties of gamma-ray spectrometry results were found in the range 2-17%. The effect of matrix composition on self-attenuation was investigated and a detailed assessment of uncertainty components was performed. PMID:26653212

  18. Gamma-ray spectrometry of ultra low levels of radioactivity within the material screening program for the GERDA experiment.

    PubMed

    Budjás, D; Gangapshev, A M; Gasparro, J; Hampel, W; Heisel, M; Heusser, G; Hult, M; Klimenko, A A; Kuzminov, V V; Laubenstein, M; Maneschg, W; Simgen, H; Smolnikov, A A; Tomei, C; Vasiliev, S I

    2009-05-01

    In present and future experiments in the field of rare events physics a background index of 10(-3) counts/(keV kg a) or better in the region of interest is envisaged. A thorough material screening is mandatory in order to achieve this goal. The results of a systematic study of radioactive trace impurities in selected materials using ultra low-level gamma-ray spectrometry in the framework of the GERDA experiment are reported. PMID:19243966

  19. Detection of /sup 210/Pb in the lungs of smokers by in-vivo gamma spectrometry

    SciTech Connect

    Berger, C.D.; Lane, B.H.

    1982-09-01

    Since mainstream smoke is highly enriched in /sup 210/Pb, alpha radiation from inhaled cigarette smoke particles has been proposed as a cancer-producing agent in cigarette smokers. /sup 210/Po and /sup 210/Pb have been observed in tobacco, cigarette smoke and in the lungs of smokers. Since /sup 210/Pb is highly enriched in mainstream smoke, there have been estimates of yearly excesses of /sup 210/Pb in the lungs of one-pack-a-day smokers of 3 to 10 pCi (0.11 to 0.37 Bq). The ORNL Whole Body Counter was used to verify this estimate by the methodology of high-resolution, in vivo gamma spectrometry. Measurements were made on 113 adult male non-radiation workers who have either smoked at least one pack of cigarettes per day for at least five years, or have never smoked cigarettes. An analysis-of-variance table was generated based on the Pb-ratio for each individual which revealed that there was no statistically significant increase in the amount of /sup 210/Pb in the lungs of smokers over those of non-smokers. Sources of error are also discussed.

  20. X-ray fluorescence and gamma-ray spectrometry combined with multivariate analysis for topographic studies in agricultural soil.

    PubMed

    de Castilhos, Natara D B; Melquiades, Fábio L; Thomaz, Edivaldo L; Bastos, Rodrigo Oliveira

    2014-10-15

    Physical and chemical properties of soils play a major role in the evaluation of different geochemical signature, soil quality, discrimination of land use type, soil provenance and soil degradation. The objectives of the present study are the soil elemental characterization and soil differentiation in topographic sequence and depth, using Energy Dispersive X-Ray Fluorescence (EDXRF) as well as gamma-ray spectrometry data combined with Principal Component Analysis (PCA). The study area is an agricultural region of Boa Vista catchment which is located at Guamiranga municipality, Brazil. PCA analysis was performed with four different data sets: spectral data from EDXRF, spectral data from gamma-ray spectrometry, concentration values from EDXRF measurements and concentration values from gamma-ray spectrometry. All PCAs showed similar results, confirmed by hierarchical cluster analysis, allowing the data grouping into top, bottom and riparian zone samples, i.e. the samples were separated due to its landscape position. The two hillslopes present the same behavior independent of the land use history. There are distinctive and characteristic patterns in the analyzed soil. The methodologies presented are promising and could be used to infer significant information about the region to be studied. PMID:25464179

  1. Using gamma ray spectrometry for fingerprinting sources of estuarine and coastal sediment in Mukawa coast, Hokkaido, northern Japan

    NASA Astrophysics Data System (ADS)

    Mizugaki, S.; Ohtsuka, J.; Murakami, Y.; Ishiya, T.; Hamamoto, S.

    2010-12-01

    To seek the geological tracers of environmental radionuclide for fingerprinting sources of estuarine and coastal sediment, the gamma ray spectrometry was conducted for the soil and sediment samples collected from subcatchments, rivers, estuaries and coast in Mukawa and Sarugawa river watersheds and Mukawa coast, Hokkaido, northern Japan. Gamma ray spectrometry was conducted to determine the activities of environmental radionuclides associated with each soil and sediment samples using HP Ge well-type detector. Gamma ray spectrometry could determine 15 environmental radionuclides, including U-series, Th-series, cesium-137 and potassium-40. Lead-210 excess was also determined by subtracting the activities of Pb-214 from that of Pb-210. The Kruskal-Wallis H test was conducted to assess the ability of each tracer property to discriminate between surface soil samples from the categories divided by subcatchment, geological era and period, suggesting that more than 11 tracer properties were available. Subsequently, the stepwise discriminant function analysis was conducted to identify which combination of tracer properties provides the best composite fingerprint for differentiating source materials on the basis of subcatchment and geology source groups. This analysis suggested that the composite fingerprints of Pb-212, Ac-228 and K-40 can classify the geology into 6 groups based on rock type. Using these tracer properties, the contribution of rock to estuarine and coastal sediment can be evaluated with the multivariate sediment mixing model.

  2. High Throughput In Situ XAFS Screening of Catalysts

    SciTech Connect

    Tsapatsaris, Nikolaos; Beesley, Angela M.; Weiher, Norbert; Tatton, Helen; Schroeder, Sven L. M.; Dent, Andy J.; Mosselmans, Frederick J. W.; Tromp, Moniek; Russu, Sergio; Evans, John; Harvey, Ian; Hayama, Shu

    2007-02-02

    We outline and demonstrate the feasibility of high-throughput (HT) in situ XAFS for synchrotron radiation studies. An XAS data acquisition and control system for the analysis of dynamic materials libraries under control of temperature and gaseous environments has been developed. The system is compatible with the 96-well industry standard and coupled to multi-stream quadrupole mass spectrometry (QMS) analysis of reactor effluents. An automated analytical workflow generates data quickly compared to traditional individual spectrum acquisition and analyses them in quasi-real time using an HT data analysis tool based on IFFEFIT. The system was used for the automated characterization of a library of 91 catalyst precursors containing ternary combinations of Cu, Pt, and Au on {gamma}-Al2O3, and for the in situ characterization of Au catalysts supported on Al2O3 and TiO2.

  3. A NEW METHDOLOGY FOR DETERMINING FISSILE MASS IN INDIVIDUAL ACCOUNTING ITEMS WITH THE USE OF GAMMA-RAY SPECTROMETRY.

    SciTech Connect

    KANE,W.R.; VANIER,P.E.; ZUHOSKI,P.B.; LEMLEY,J.R.

    2000-07-16

    In the safeguards, arms control, and nonproliferation regimes measurements are required which give the quantity of fissile material in an accounting item, e.g., a standard container of plutonium or uranium oxide. Because of the complexity of modeling the absorption of gamma rays in high-Z materials, gamma-ray spectrometry is not customarily used for this purpose. Gamma-ray measurements can be used to determine the fissile mass when two conditions are met: (1) The material is in a standard container, and (2) The material is finely divided, or a solid item with a reproducible shape. The methodology consists of: (A) Measurement of the emitted gamma rays, and (B) Measurement of the transmission through the item of the high-energy gamma rays of Co-60 and Th-228. We have demonstrated that items containing nuclear materials possess a characteristic ''fingerprint'' of gamma rays which depends not only on the nuclear properties, but also on the mass, density, shape, etc.. The material's spectrum confirms its integrity, homogeneity, and volume as well. While there is attenuation of radiation from the interior, the residual radiation confirms the homogeneity of the material throughout the volume. Transmission measurements, where the attenuation depends almost entirely on Compton scattering, determine the material mass. With well-characterized standards, this methodology can provide an accurate measure of the contained fissile material.

  4. Neanderthal skeleton from Tabun: U-series data by gamma-ray spectrometry.

    PubMed

    Schwarcz, H P; Simpson, J J; Stringer, C B

    1998-12-01

    The Neanderthal hominid Tabun C1, found in Israel by Garrod & Bate, was attributed to either layer B or C of their stratigraphic sequence. We have used gamma-ray spectrometry to determine the 230Th/234U and 231Pa/235U ratios of two bones from this skeleton, the mandible and a femur. The ages calculated from these ratios depend on the uranium uptake history of the bones. Assuming a model of early U (EU) uptake the age of the Tabun C1 mandible is 34+/-5 ka. The EU age of the femur is 19+/-2 ka. The femur may have experienced continuous (linear) U uptake which would give an age of 33+/-4 ka, in agreement with the mandible's EU age, but implies marked inhomogeneity in U uptake history at the site. These new age estimates for the skeleton suggest that it was younger than deposits of layer C. This apparent age is less than those of other Neanderthals found in Israel, and distinctly younger than the ages of the Skhul and Qafzeh burials. This suggests that Neanderthals did not necessarily coexist with the earliest modern humans in the region. All of the more complete Neanderthal fossils from Israel are now dated to the cool period of the last glacial cycle, suggesting that Neanderthals may have arrived in this region as a result of the southward expansion of their habitable range. The young age determined for the Tabun skeleton would suggest that Neanderthals survived as late in the Levant as they did in Europe. PMID:9929173

  5. Jarosite as a Storage Mineral for Small Organic Molecules: Investigations of Natural Samples Using an 'In Situ' Laser Desorption Fourier Transform Mass Spectrometry Technique

    NASA Astrophysics Data System (ADS)

    Kotler, J. M.; Hinman, N. W.; Yan, B.; Stoner, D. L.; Scott, J. R.

    2007-03-01

    The use of laser desorption Fourier transform mass spectrometry has revealed the presence of organic matter in several jarosite samples from various locations worldwide including jarosite precipitated in the lab by acidothiobacillus ferroxidans.

  6. In situ derivatization-ultrasound-assisted dispersive liquid-liquid microextraction for the determination of neurotransmitters in Parkinson's rat brain microdialysates by ultra high performance liquid chromatography-tandem mass spectrometry.

    PubMed

    He, Yongrui; Zhao, Xian-En; Zhu, Shuyun; Wei, Na; Sun, Jing; Zhou, Yubi; Liu, Shu; Liu, Zhiqiang; Chen, Guang; Suo, Yourui; You, Jinmao

    2016-08-01

    Simultaneous monitoring of several neurotransmitters (NTs) linked to Parkinson's disease (PD) has important scientific significance for PD related pathology, pharmacology and drug screening. A new simple, fast and sensitive analytical method, based on in situ derivatization-ultrasound-assisted dispersive liquid-liquid microextraction (in situ DUADLLME) in a single step, has been proposed for the quantitative determination of catecholamines and their biosynthesis precursors and metabolites in rat brain microdialysates. The method involved the rapid injection of the mixture of low toxic bromobenzene (extractant) and acetonitrile (dispersant), which containing commercial Lissamine rhodamine B sulfonyl chloride (LRSC) as derivatization reagent, into the aqueous phase of sample and buffer, and the following in situ DUADLLME procedure. After centrifugation, 50μL of the sedimented phase (bromobenzene) was directly injected for ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) detection in multiple reaction monitoring (MRM) mode. This interesting combination brought the advantages of speediness, simpleness, low matrix effects and high sensitivity in an effective way. Parameters of in situ DUADLLME and UHPLC-MS/MS conditions were all optimized in detail. The optimum conditions of in situ DUADLLME were found to be 30μL of microdialysates, 150μL of acetonitrile containing LRSC, 50μL of bromobenzene and 800μL of NaHCO3-Na2CO3 buffer (pH 10.5) for 3.0min at 37°C. Under the optimized conditions, good linearity was observed with LODs (S/N>3) and LOQs (S/N>10) of LRSC derivatized-NTs in the range of 0.002-0.004 and 0.007-0.015 nmol/L, respectively. It also brought good precision (3.2-12.8%, peak area CVs%), accuracy (94.2-108.6%), recovery (94.5-105.5%) and stability (3.8-8.1%, peak area CVs%) results. Moreover, LRSC derivatization significantly improved chromatographic resolution and MS detection sensitivity of NTs when compared with the

  7. A revision factor to the Cutshall self-attenuation correction in (210)Pb gamma-spectrometry measurements.

    PubMed

    Jodłowski, Paweł

    2016-03-01

    The Cutshall transmission method of determination of self-attenuation correction in (210)Pb measurements by gamma-spectrometry gives the results burdened with errors of up to 10%. The author proposes introducing into the Cutshall correction Cs,Cuts an additional revision factor CCs,Cuts to eliminate errors. The proposed formula of the revision factor describes the CCs,Cuts value depending on the experimentally obtained Cs,Cuts correction. Formula holds true in wide ranges of the measurement geometries and linear attenuation coefficients of both the standard and the sample. PMID:26702546

  8. Gamma spectrometry efficiency calibration using Monte Carlo methods to measure radioactivity of 137Cs in food samples.

    PubMed

    Alrefae, T

    2014-12-01

    A simple method of efficiency calibration for gamma spectrometry was performed. This method, which focused on measuring the radioactivity of (137)Cs in food samples, was based on Monte Carlo simulations available in the free-of-charge toolkit GEANT4. Experimentally, the efficiency values of a high-purity germanium detector were calculated for three reference materials representing three different food items. These efficiency values were compared with their counterparts produced by a computer code that simulated experimental conditions. Interestingly, the output of the simulation code was in acceptable agreement with the experimental findings, thus validating the proposed method. PMID:24214912

  9. IN-SITU ASSAY OF TRANSURANIC RADIONUCLIDES IN THE VADOSE ZONE USING HIGH-RESOLUTION SPECTRAL GAMMA LOGGING - A HANFORD CASE STUDY

    SciTech Connect

    ROHAY VJ; HENWOOD P; MCCAIN R

    2009-11-30

    High-resolution spectral gamma logging in steel-cased boreholes is used to detect and quantify transuranic radionuclides in the subsurface. Pu-239, Pu-241, Am-241, and Np-237 are identified based on characteristic decay gammas. Typical minimum detectable levels are on the order of 20 to 40 nCi/g. In intervals of high transuranic concentrations, gamma rays from other sources may complicate analysis and interpretation. Gamma rays detected in the borehole may originate from three sources: decay of the parent transuranic radionuclide or a daughter; alpha interactions; and interactions with neutrons resulting from either spontaneous fission or alpha particle interactions.

  10. A rapid dissolution procedure to aid initial nuclear forensics investigations of chemically refractory compounds and particles prior to gamma spectrometry.

    PubMed

    Reading, David G; Croudace, Ian W; Warwick, Phillip E; Britton, Richard

    2015-11-01

    A rapid and effective preparative procedure has been evaluated for the accurate determination of low-energy (40-200 keV) gamma-emitting radionuclides ((210)Pb, (234)Th, (226)Ra, (235)U) in uranium ores and uranium ore concentrates (UOCs) using high-resolution gamma ray spectrometry. The measurement of low-energy gamma photons is complicated in heterogeneous samples containing high-density mineral phases and in such situations activity concentrations will be underestimated. This is because attenuation corrections, calculated based on sample mean density, do not properly correct where dense grains are dispersed within a less dense matrix (analogous to a nugget effect). The current method overcomes these problems using a lithium tetraborate fusion that readily dissolves all components including high-density, self-attenuating minerals/compounds. This is the ideal method for dissolving complex, non-volatile components in soils, rocks, mineral concentrates, and other materials where density reduction is required. Lithium borate fusion avoids the need for theoretical efficiency corrections or measurement of matrix matched calibration standards. The resulting homogeneous quenched glass produced can be quickly dissolved in nitric acid producing low-density solutions that can be counted by gamma spectrometry. The effectiveness of the technique is demonstrated using uranium-bearing Certified Reference Materials and provides accurate activity concentration determinations compared to the underestimated activity concentrations derived from direct measurements of a bulk sample. The procedure offers an effective solution for initial nuclear forensic studies where complex refractory minerals or matrices exist. It is also significantly faster, safer and simpler than alternative approaches. PMID:26572834

  11. Linkage-Specific in Situ Sialic Acid Derivatization for N-Glycan Mass Spectrometry Imaging of Formalin-Fixed Paraffin-Embedded Tissues.

    PubMed

    Holst, Stephanie; Heijs, Bram; de Haan, Noortje; van Zeijl, René J M; Briaire-de Bruijn, Inge H; van Pelt, Gabi W; Mehta, Anand S; Angel, Peggy M; Mesker, Wilma E; Tollenaar, Rob A; Drake, Richard R; Bovée, Judith V M G; McDonnell, Liam A; Wuhrer, Manfred

    2016-06-01

    Matrix-assisted laser desorption/ionization (MALDI) mass spectrometry imaging is a rapidly evolving field in which mass spectrometry techniques are applied directly on tissues to characterize the spatial distribution of various molecules such as lipids, protein/peptides, and recently also N-glycans. Glycans are involved in many biological processes and several glycan changes have been associated with different kinds of cancer, making them an interesting target group to study. An important analytical challenge for the study of glycans by MALDI mass spectrometry is the labile character of sialic acid groups which are prone to in-source/postsource decay, thereby biasing the recorded glycan profile. We therefore developed a linkage-specific sialic acid derivatization by dimethylamidation and subsequent amidation and transferred this onto formalin-fixed paraffin-embedded (FFPE) tissues for MALDI imaging of N-glycans. Our results show (i) the successful stabilization of sialic acids in a linkage specific manner, thereby not only increasing the detection range, but also adding biological meaning, (ii) that no noticeable lateral diffusion is induced during to sample preparation, (iii) the potential of mass spectrometry imaging to spatially characterize the N-glycan expression within heterogeneous tissues. PMID:27145236

  12. X-ray remote sensing and in-situ spectroscopy for planetary exploration missions and gamma-ray remote sensing and in-situ spectroscopy for planetary exploration missions

    NASA Technical Reports Server (NTRS)

    Mahdavi, M.; Giboni, K. L.; Vajda, S.; Schweitzer, J.

    1994-01-01

    Detectors that will be used for planetary missions must have their responses calibrated in a reproducible manner. A calibration facility is being constructed at Schlumberger-Doll Research for gamma and x ray detectors. With this facility the detector response can be determined in an invariant and reproducible fashion. Initial use of the facility is expected for the MARS94 detectors. Work is continuing to better understand the rare earth oxyorthosilicates and to define their characteristics. This will allow a better use of these scintillators for planetary missions. In a survey of scintillating materials two scintillators were identified as promising candidates besides GSO, LSO, and YSO. These are CdWO4 and CsI(Tl). It will be investigated if a detector with a better overall performance can be assembled with various photon converters. Considerable progress was achieved in photomultiplier design. The length of an 1 inch diameter PMT could be reduced from 4.2 to 2.5 inches without performance degradation. This technology is being employed in the gamma ray detector for the NEAR project. A further weight and size reduction of the detector package can be achieved with miniaturized integrated power supplies.

  13. Multi-scale monitoring of a marine geologic methane source in the Santa Barbara Channel using imaging spectrometry, ARCTAS-CARB in situ sampling and coastal hourly total hydrocarbon measurements

    NASA Astrophysics Data System (ADS)

    Bradley, E. S.; Leifer, I.; Roberts, D.; Dennison, P. E.; Margolis, J.; Moritsch, M.; Diskin, G. S.; Sachse, G. W.

    2009-12-01

    The Coal Oil Point (COP) hydrocarbon seep field off the coast of Santa Barbara, CA is one of the most active and best-studied marine geologic methane sources in the world and contributes to elevated terrestrial methane concentrations downwind. In this study, we investigate the spatiotemporal variability of this local source and the influence of meteorological conditions on transport and concentration. A methane plume emanating from Trilogy Seep was mapped with the Airborne Visible Infrared Imaging Spectrometer at a 7.5 m resolution with a short-wave infrared band ratio technique. This structure agrees with the local wind speed and direction and is orthogonal to the surface currents. ARCTAS-CARB aircraft in situ sampling of lower-troposphere methane is compared to sub-hour total hydrocarbon concentration (THC) measurements from the Santa Barbara Air Pollution Control District (SBAPCD) station located near COP. Hourly SBAPCD THC values from 1980-2008 demonstrate a decrease in seep source strength until the late 1990s, followed by a consistent increase. The occurrence of elevated SBAPCD THC values for onshore wind conditions as well as numerous positive outliers as high as 17 ppm suggests that seep field emissions are both quasi-steady state and transient, direct (bubble) and diffuse (outgassing). As demonstrated for the COP seeps, the combination of imaging spectrometry, aircraft in situ sampling, and ground-based monitoring provides a powerful approach for understanding local methane sources and transport processes.

  14. Dating of sediments from four Swiss prealpine lakes with (210)Pb determined by gamma-spectrometry: progress and problems.

    PubMed

    Putyrskaya, V; Klemt, E; Röllin, S; Astner, M; Sahli, H

    2015-07-01

    In this paper the most important problems in dating lake sediments with unsupported (210)Pb are summarized and the progress in gamma-spectrometry of the unsupported (210)Pb is discussed. The main topics of these studies concern sediment samples preparation for gamma-spectrometry, measurement techniques and data analysis, as well as understanding of accumulation and sedimentation processes in lakes. The vertical distributions of artificial ((137)Cs, (241)Am, (239)Pu) and natural radionuclides ((40)K, (210,214)Pb, (214)Bi) as well as stable trace elements (Fe, Mn, Pb) in sediment cores from four Swiss lakes were used as examples for the interpretation, inter-comparison and validation of depth-age relations established by three (210)Pb-based models (CF-CSR, CRS and SIT). The identification of turbidite layers and the influence of the turbidity flows on the accuracy of sediment dating is demonstrated. Time-dependent mass sedimentation rates in lakes Brienz, Thun, Biel and Lucerne are discussed and compared with published data. PMID:25875007

  15. Particulate-matter distribution and its flow from power plants using infrared spectrometry and thermodynamics for in situ continuous emissions monitoring

    NASA Astrophysics Data System (ADS)

    Shlifshteyn, Alex; Lang, Fred D.; Ayrapetian, Robert

    1996-01-01

    Spectroscopy measurements made through a continuum having suspended particulate matter are addressed. The applications presented permit correction of spectral transmissions as effected by particulate-producing fossil-fuel combustion. The research is especially applicable to large effluent flows from coal-fired power plants, whose effluents are studied with in situ (smokestack) radiometers. Methods involving fast calculation procedures based on measured irradiances in unabsorbed regions of the IR spectrum are presented. The methodology is based on wavelength-dependent extinction of radiation by small particles, considering both elastic scattering and absorbing effects. This extinction leads to an observed skeweness (or shift) of the blackbody spectral shape. Based on such skeweness, the particulate number distribution is determined with Mie theory. In order to simplify, and to speed up the routine for real-time application, a two-step procedure is presented. During preinstallation calibration with Mie theory, sets of integral tables are computed for all possible solution values and stored in computer memory. Based on instantaneous spectral measurements, the appropriate integral tables are retrieved, then used as inputs in a process leading to particulate number distribution. Because all time-consuming calculations associated with Mie theory are performed during preinstallation calibration, the technique is capable of monitoring particulate emission in real time. Furthermore, given resolution of the number distribution in combination with thermodynamic analysis of the system, determination of particulate apparent density and particulate mass flow rate is made. These values have importance for environmental reporting. Comparisons of calculated particulate distributions with in situ measurements are also presented. Confirmatory testing programs conducted at several power plants are discussed.

  16. A broadband gamma-ray spectrometry using novel unfolding algorithms for characterization of laser wakefield-generated betatron radiation

    SciTech Connect

    Jeon, Jong Ho Nakajima, Kazuhisa Pathak, Vishwa Bandhu; Cho, Myung Hoon; Yoo, Byung Ju; Shin, Kang Woo; Kim, Hyung Taek; Sung, Jae Hee; Lee, Seung Ku; Choi, Il Woo; Rhee, Yong Joo; Shin, Jung Hun; Jo, Sung Ha; Hojbota, Calin; Cho, Byeoung Ick; Nam, Chang Hee

    2015-12-15

    We present a high-flux, broadband gamma-ray spectrometry capable of characterizing the betatron radiation spectrum over the photon energy range from 10 keV to 20 MeV with respect to the peak photon energy, spectral bandwidth, and unique discrimination from background radiations, using a differential filtering spectrometer and the unfolding procedure based on the Monte Carlo code GEANT4. These properties are experimentally verified by measuring betatron radiation from a cm-scale laser wakefield accelerator (LWFA) driven by a 1-PW laser, using a differential filtering spectrometer consisting of a 15-filter and image plate stack. The gamma-ray spectra were derived by unfolding the photostimulated luminescence (PSL) values recorded on the image plates, using the spectrometer response matrix modeled with the Monte Carlo code GEANT4. The accuracy of unfolded betatron radiation spectra was assessed by unfolding the test PSL data simulated with GEANT4, showing an ambiguity of less than 20% and clear discrimination from the background radiation with less than 10%. The spectral analysis of betatron radiation from laser wakefield-accelerated electron beams with energies up to 3 GeV revealed radiation spectra characterized by synchrotron radiation with the critical photon energy up to 7 MeV. The gamma-ray spectrometer and unfolding method presented here facilitate an in-depth understanding of betatron radiation from LWFA process and a novel radiation source of high-quality photon beams in the MeV regime.

  17. A prototype of radioactive waste drum monitor by non-destructive assays using gamma spectrometry.

    PubMed

    Thanh, Tran Thien; Trang, Hoang Thi Kieu; Chuong, Huynh Dinh; Nguyen, Vo Hoang; Tran, Le Bao; Tam, Hoang Duc; Tao, Chau Van

    2016-03-01

    In this work, segmented gamma scanning and the gamma emission tomography were used to locate unknown sources in a radioactive waste drum. The simulated detector response function and full energy peak efficiency are compared to corresponding experimental data and show about 5.3% difference for an energy ranging from 81keV to 1332.5keV for point sources. Computation of the corresponding activity is in good agreement with the true values. PMID:26717796

  18. Determination of endogenous brassinosteroids using sequential magnetic solid phase extraction followed by in situ derivatization/desorption method coupled with liquid chromatography-tandem mass spectrometry.

    PubMed

    Ding, Jun; Mao, Li-Jing; Guo, Ning; Yu, Lei; Feng, Yu-Qi

    2016-05-13

    In this study, a sequential magnetic solid phase extraction followed by in situ derivatization/desorption method was proposed for the fast, selective and sensitive determination of brassinosteroids (BRs) in plant tissues. Magnetic sorbent for quick, easy, cheap, effective, rugged and safe method (mQuEChERS) and polymer(4-vinylphenylboronic acid-co-ethylene glycol dimethacrylate) coated Fe3O4@SiO2 (p(4-VPBA-co-EGDMA) coated Fe3O4@SiO2) were prepared and characterized. Using them as sorbents, pigments and hydrophilic interferents were firstly removed from plant extract by mQuEChERS, and then endogenous BRs were selectively enriched by p(4-VPBA-co-EGDMA) coated Fe3O4@SiO2 through boronate affinity interaction. After loading BRs on p(4-VPBA-co-EGDMA) coated Fe3O4@SiO2, instead of directly eluting free BRs, the adsorbed BRs were released by adding 4-(N,N-dimethyamino)phenylboronic acid (4-DMAPBA) solution for in situ derivatizaiton/desorption of BRs based on a transesterification reaction between the boronate moieties of p(4-VPBA-co-EGDMA) coated Fe3O4@SiO2 and 4-DMAPBA, finally the resultant solution was submitted to LC-MS/MS for quantification. The whole procedure of the sequential MSPE could be accomplished within 1h, and the matrix effect to MS signal after the sample pretreatment was estimated to be in the range of 93.0-97.4%. The established method provided broad linear dynamics ranges (1.0-100.0pg/mL) with correlation coefficients (R) >0.9978, substantial sensitivity (limits of detection ranged from 0.27 to 1.29pg/mL), high reproducibility (intra-day and inter-day relative standard deviations (RSDs) less than 14.8%) and satisfactory accuracy (recoveries ranged from 74.0%-116.6%). Furthermore, endogenous BRs were successfully detected in one flower of Brassica napus L. (22.5-542.7pg/g fresh weight) and other plant tissues (13.7-289.8pg/g fresh weight). PMID:27072523

  19. In situ derivatization combined to automated microextraction by packed sorbents for the determination of chlorophenols in soil samples by gas chromatography mass spectrometry.

    PubMed

    González Paredes, Rosa María; García Pinto, Carmelo; Pérez Pavón, José Luis; Moreno Cordero, Bernardo

    2014-09-12

    A method based on the coupling of in situ extraction and derivatization of chlorophenols (CPs) (2-chlorophenol, 4-chloro-3-methylphenol, 2,4-dichlorophenol, and 2,4,6-trichlorophenol) from soils, accomplishing their preconcentration by means of automated microextraction by packed sorbent (MEPS), is proposed. After extraction and acylation of the chlorophenols in aqueous medium, the liquid phase obtained is subjected to the MEPS procedure. The QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) and MEPS techniques were compared and the results confirmed the preconcentration carried out with MEPS. The existence of a matrix effect was checked and the analytical characteristics of the method were determined in a soil sample. The method provided good linearity (from 1 to 12μgkg(-1)), together with good repeatability and reproducibility values (RSD equal to or less than 10%). The limits of detection were in the 0.118-0.894μgkg(-1) range. A certified reference material was applied to validate the proposed methodology. PMID:25113872

  20. Graphene oxide-based dispersive solid-phase extraction combined with in situ derivatization and gas chromatography-mass spectrometry for the determination of acidic pharmaceuticals in water.

    PubMed

    Naing, Nyi Nyi; Li, Sam Fong Yau; Lee, Hian Kee

    2015-12-24

    A fast and low-cost sample preparation method of graphene based dispersive solid-phase extraction combined with gas chromatography-mass spectrometric (GC-MS) analysis, was developed. The procedure involves an initial extraction with water-immiscible organic solvent, followed by a rapid clean-up using amine functionalized reduced graphene oxide as sorbent. Simple and fast one-step in situ derivatization using trimethylphenylammonium hydroxide was subsequently applied on acidic pharmaceuticals serving as model analytes, ibuprofen, gemfibrozil, naproxen, ketoprofen and diclofenac, before GC-MS analysis. Extraction parameters affecting the derivatization and extraction efficiency such as volume of derivatization agent, effect of desorption solvent, effect of pH and effect of ionic strength were investigated. Under the optimum conditions, the method demonstrated good limits of detection ranging from 1 to 16ngL(-1), linearity (from 0.01 to 50 and 0.05 to 50μgL(-1), depending on the analytes) and satisfactory repeatability of extractions (relative standard deviations, below 13%, n=3). PMID:26684593

  1. In Situ Determination of Trace Elements in Fish Otoliths by Laser Ablation Double Focusing Sector Field Inductively Coupled Plasma Mass Spectrometry Using a Solution Standard Addition Calibration Method

    NASA Astrophysics Data System (ADS)

    Chen, Z.; Jones, C. M.

    2002-05-01

    Microchemistry of fish otoliths (fish ear bones) is a very useful tool for monitoring aquatic environments and fish migration. However, determination of the elemental composition in fish otolith by ICP-MS has been limited to either analysis of dissolved sample solution or measurement of limited number of trace elements by laser ablation (LA)- ICP-MS due to low sensitivity, lack of available calibration standards, and complexity of polyatomic molecular interference. In this study, a method was developed for in situ determination of trace elements in fish otoliths by laser ablation double focusing sector field ultra high sensitivity Finnigan Element 2 ICP-MS using a solution standard addition calibration method. Due to the lack of matrix-match solid calibration standards, sixteen trace elements (Na, Mg, P, Cr, Mn, Fe, Ni, Cu, Rb, Sr, Y, Cd, La, Ba, Pb and U) were determined using a solution standard calibration with Ca as an internal standard. Flexibility, easy preparation and stable signals are the advantages of using solution calibration standards. In order to resolve polyatomic molecular interferences, medium resolution (M/delta M > 4000) was used for some elements (Na, Mg, P, Cr, Mn, Fe, Ni, and Cu). Both external calibration and standard addition quantification strategies are compared and discussed. Precision, accuracy, and limits of detection are presented.

  2. Detection of in-situ derivatized peptides in microbial biofilms by laser desorption 7.87 eV postionizaton mass spectrometry.

    SciTech Connect

    Edirisinghe, P. D.; Moore, J. F.; Skinner-Nemec, K. A.; Lindberg, C.; Giometti, C. S.; Veryovkin, I. V.; Hunt, J. E.; Pellin, M. J.; Hanley, L.; Biosciences Division; Univ. of Illinois at Chicago; MassThink

    2007-01-01

    A novel analytical method based on laser desorption postionization mass spectrometry (LDPI-MS) was developed to investigate the competence and sporulation factor-a pentapeptide of amino acid sequence ERGMT-within intact Bacillus subtilis biofilms. Derivatization of the neat ERGMT peptide with quinoline- and anthracene-based tags was separately used to lower the peptide ionization potential and permit direct ionization by 7.87-eV vacuum ultraviolet radiation. The techniques of mass shifting and selective ionization of the derivatized peptide were combined here to permit detection of ERGMT peptide within intact biofilms by LDPI-MS, without any prior extraction or chromatographic separation. Finally, imaging MS specific to the derivatized peptide was demonstrated on an intact biofilm using LDPI-MS. The presence of ERGMT in the biofilms was verified by bulk extraction/LC-MS. However, MALDI imaging MS analyses were unable to detect ERGMT within intact biofilms.

  3. A convenient method for discriminating between natural and depleted uranium by gamma-ray spectrometry.

    PubMed

    Shoji, M; Hamajima, Y; Takatsuka, K; Honoki, H; Nakajima, T; Kondo, T; Nakanishi, T

    2001-08-01

    A convenient method for discriminating between natural and depleted uranium reagent was developed by measuring and analyzing the gamma-ray spectra of some reagents with no standard source. The counting rates (R) of photoelectric peaks of gamma-rays from nuclides with the same radioactivity divided by their emission probability (B) are expressed as a function of gamma-ray energy. The radioactivities of 234Th and 234mPa and 21.72 times that of 235U are equal to the radioactivity of 235U in natural uranium. Therefore, the plot of 21.72-fold R/B for 235U should be on a curve fitted to the points for 234Th and 234mPa in natural uranium. Depleted uranium with a 235U isotopic composition of less than 0.68% could be discriminated from natural uranium in the case of a reagent containing 4.0 g of uranium. PMID:11393763

  4. High resolution gamma-ray spectrometry of culverts containing transuranic waste at the Savannah River Site

    SciTech Connect

    Hofstetter, K.J.; Sigg, R.

    1990-01-01

    A number of concrete culverts used to retrievably store drummed, dry, radioactive waste at the Savannah River Site (SRS), were suspected of containing ambiguous quantities of transuranic (TRU) nuclides. These culverts were assayed in place for Pu-239 content using thermal and fast neutron counting techniques. High resolution gamma-ray spectroscopy on 17 culverts, having neutron emission rates several times higher than expected, showed characteristic gamma-ray signatures of neutron emitters other than Pu-239 (e.g., Pu-238, Pu/Be, or Am/Be neutron sources). This study confirmed the Pu-239 content of the culverts with anomalous neutron rates and established limits on the Pu-239 mass in each of the 17 suspect culverts by in-field, non-intrusive gamma-ray measurements.

  5. High resolution gamma-ray spectrometry of culverts containing transuranic waste at the Savannah River Site

    SciTech Connect

    Hofstetter, K.J.; Sigg, R.

    1990-12-31

    A number of concrete culverts used to retrievably store drummed, dry, radioactive waste at the Savannah River Site (SRS), were suspected of containing ambiguous quantities of transuranic (TRU) nuclides. These culverts were assayed in place for Pu-239 content using thermal and fast neutron counting techniques. High resolution gamma-ray spectroscopy on 17 culverts, having neutron emission rates several times higher than expected, showed characteristic gamma-ray signatures of neutron emitters other than Pu-239 (e.g., Pu-238, Pu/Be, or Am/Be neutron sources). This study confirmed the Pu-239 content of the culverts with anomalous neutron rates and established limits on the Pu-239 mass in each of the 17 suspect culverts by in-field, non-intrusive gamma-ray measurements.

  6. 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.

  7. Mathematical model of gamma-ray spectrometry borehole logging for quantitative analysis

    USGS Publications Warehouse

    Schimschal, Ulrich

    1981-01-01

    A technique for analyzing gamma-ray spectral-logging data has been developed, in which a digital computer is used to calculate the effects of gamma-ray attentuation in a borehole environment. The computer model allows for the calculation of the effects of lithology, porosity, density, and the thickness of a horizontal layer of uniformly distributed radioactive material surrounding a centralized probe in a cylindrical borehole. The computer program also contains parameters for the calculation of the effects of well casing, drilling fluid, probe housing, and losses through the sodium-iodide crystal. Errors associated with the commonly used mathematical assumption of a point detector are eliminated in this model. (USGS)

  8. Calculation of the decision threshold in gamma-ray spectrometry using sum peaks.

    PubMed

    Korun, M; Vodenik, B; Zorko, B

    2016-03-01

    In the presence of radon daughters, gamma rays from (88)Y with energies at 898.0keV or 1836.1keV appear on a high, continuous background or overlap with other peaks. Therefore a calculation of the decision threshold from the sum peak at 2734.1keV represents a useful alternative, because here the continuous background is low. The decision threshold calculated from this peak can attain a value being comparable to the decision threshold calculated from the gamma-ray peak at 898.0keV. PMID:26625726

  9. Dose rate constant of a Cesium-131 interstitial brachytherapy seed measured by thermoluminescent dosimetry and gamma-ray spectrometry

    SciTech Connect

    Chen, Z.; Bongiorni, P.; Nath, R.

    2005-11-15

    The aim of this work was to conduct an independent determination of the dose rate constant of the newly introduced Model CS-1 {sup 131}Cs seed. A total of eight {sup 131}Cs seeds were obtained from the seed manufacturer. The air-kerma strength of each seed was measured by the manufacturer whose calibration is traceable to the air-kerma strength standard established for the {sup 131}Cs seeds at the National Institute of Standards and Technology (1{sigma} uncertainty <1%). The dose rate constant of each seed was measured by two independent methods: One based on the actual photon energy spectrum emitted by the seed using gamma-ray spectrometry and the other based on the dose-rate measured by thermoluminescent dosimeter (TLD) in a Solid Water{sup TM} phantom. The dose rate constant in water determined by the gamma-ray spectrometry technique and by the TLD dosimetry are 1.066{+-}0.064 cGyh{sup -1}U{sup -1} and 1.058{+-}0.106 cGyh{sup -1}U{sup -1}, respectively, showing excellent agreement with each other. These values, however, are approximately 15% greater than a previously reported value of 0.915 cGyh{sup -1}U{sup -1} [Med. Phys. 31, 1529-1538 (2004)]. Although low-energy fluorescent x rays at 16.6 and 18.7 keV, originating from niobium present in the seed construction, were measured in the energy spectrum of the {sup 131}Cs seeds, their yields were not sufficient to lower the dose rate constant to the value of 0.915 cGyh{sup -1}U{sup -1}. Additional determinations of the dose rate constant may be needed to establish an AAPM recommended consensus value for routine clinical use of the {sup 131}Cs seed.

  10. In situ submicron organic aerosol characterization at a boreal forest research station during HUMPPA-COPEC 2010 using soft and hard ionization mass spectrometry

    NASA Astrophysics Data System (ADS)

    Vogel, A. L.; Äijälä, M.; Corrigan, A. L.; Junninen, H.; Ehn, M.; Petäjä, T.; Worsnop, D. R.; Kulmala, M.; Russell, L. M.; Williams, J.; Hoffmann, T.

    2013-11-01

    The chemical composition of submicron aerosol during the comprehensive field campaign HUMPPA-COPEC 2010 at Hyytiälä, Finland, is presented. The focus lies on online measurements of organic acids, which were achieved by using atmospheric pressure chemical ionization (APCI) ion trap mass spectrometry (IT-MS). These measurements were accompanied by aerosol mass spectrometry (AMS) measurements and Fourier transform infrared spectroscopy (FTIR) of filter samples, all showing a high degree of correlation. The soft ionization mass spectrometer alternated between gas-phase measurements solely and measuring the sum of gas and particle phase. The AMS measurements of C, H and O elemental composition show that the aerosol during the campaign was highly oxidized, which appears reasonable due to high and prolonged radiation during the boreal summer measurement period as well as the long transport times of some of the aerosol. In order to contrast ambient and laboratory aerosol, an average organic acid pattern, measured by APCI-IT-MS during the campaign, was compared to terpene ozonolysis products in a laboratory reaction chamber. Identification of single organic acid species remains a major challenge due to the complexity of the boreal forest aerosol. Unambiguous online species identification was attempted by the combinatorial approach of identifying unique fragments in the MS2 mode of standards, and then comparing these results with MS2 field spectra. During the campaign, unique fragments of limonene-derived organic acids (limonic acid and ketolimononic acid) and of the biomass burning tracer vanillic acid were detected. Other specific fragments (neutral loss of 28 Da) in the MS2 suggest the occurrence of semialdehydes. Furthermore, an approach to determine the average molecular weight of the aerosol is presented. The campaign average organic molecular weight was determined to be 300 g mol-1. However, a plume of aged biomass burning aerosol, arriving at Hyytiälä from Russia