Science.gov

Sample records for acid precipitation samples

  1. Acidic precipitation

    SciTech Connect

    Martin, H.C.

    1987-01-01

    At the International Symposium on Acidic Precipitation, over 400 papers were presented, and nearly 200 of them are included here. They provide an overview of the present state of the art of acid rain research. The Conference focused on atmospheric science (monitoring, source-receptor relationships), aquatic effects (marine eutrophication, lake acidification, impacts on plant and fish populations), and terrestrial effects (forest decline, soil acidification, etc.).

  2. Acid Precipitation

    ERIC Educational Resources Information Center

    Likens, Gene E.

    1976-01-01

    Discusses the fact that the acidity of rain and snow falling on parts of the U.S. and Europe has been rising. The reasons are still not entirely clear and the consequences have yet to be well evaluated. (MLH)

  3. Acid precipitation in southeastern Wyoming

    SciTech Connect

    Ahern, J.; Baird, C.

    1983-09-01

    Snowfall, snowpack, and rainfall samples were collected in Laramie, Wyoming and in the Snowy Range west of Laramie from March to June 1981 to determine the occurrence and sources of acid precipitation in southeast Wyoming. Electrodes measured different pH values in the samples; however, fast-response electrodes yielded higher and apparently more accurate pH measurements. The pH values in the Laramie precipitation and snowpack were typically greater than 5.0, but all the Snowy Range snowpack pH values were less than 5.0. The lower pH values in the Snowy Range snowpack were caused by higher concentrations of the acid-forming nitrate and lower concentrations of the neutralizing calcium. Two organic species, formate and acetate, were detected in the Laramie samples, but had no significant influence on the acidity of the samples. 33 references, 3 figures, 17 tables.

  4. Chemical Data for Precipitate Samples

    USGS Publications Warehouse

    Foster, Andrea L.; Koski, Randolph A.

    2008-01-01

    During studies of sulfide oxidation in coastal areas of Prince William Sound in 2005, precipitate samples were collected from onshore and intertidal locations near the Ellamar, Threeman, and Beatson mine sites (chapter A, fig. 1; table 7). The precipitates include jarosite and amorphous Fe oxyhydroxide from Ellamar, amorphous Fe oxyhydroxide from Threeman, and amorphous Fe oxyhydroxide, ferrihydrite, and schwertmannite from Beatson. Precipitates occurring in the form of loose, flocculant coatings were harvested using a syringe and concentrated in the field by repetitive decanting. Thicker accumulations were either scraped gently from rocks using a stainless steel spatula or were scooped directly into receptacles (polyethylene jars or plastic heavy-duty zippered bags). Most precipitate samples contain small amounts of sedimentary detritus. With three jarosite-bearing samples from Ellamar, an attempt was made to separate the precipitate from the heavy-mineral fraction of the sediment. In this procedure, the sample was stirred in a graduated cylinder containing deionized water. The jarosite-rich suspension was decanted onto analytical filter paper and air dried before analysis. Eleven precipitate samples from the three mine sites were analyzed in laboratories of the U.S. Geological Survey (USGS) in Denver, Colorado (table 8). Major and trace elements were determined by inductively coupled plasma-mass spectrometry following multiacid (HCl-HNO3-HClO4-HF) digestion (Briggs and Meier, 2002), except for mercury, which was analyzed by cold-vapor atomic absorption spectroscopy (Brown and others, 2002a). X-ray diffraction (XRD) analyses were performed on powdered samples (<200 mesh) by S. Sutley of the USGS. Additional details regarding sample preparation and detection limits are found in Taggert (2002). Discussions of the precipitate chemistry and associated microbial communities are presented in Koski and others (2008) and Foster and others (2008), respectively.

  5. Universal sample preparation method integrating trichloroacetic acid/acetone precipitation with phenol extraction for crop proteomic analysis.

    PubMed

    Wu, Xiaolin; Xiong, Erhui; Wang, Wei; Scali, Monica; Cresti, Mauro

    2014-02-01

    Crop plants contain large amounts of secondary compounds that interfere with protein extraction and gel-based proteomic analysis. Thus, a protein extraction protocol that can be easily applied to various crop materials with minimal optimization is essential. Here we describe a universal protocol for total protein extraction involving trichloroacetic acid (TCA)/acetone precipitation followed by SDS and phenol extraction. Through SDS extraction, the proteins precipitated by the TCA/acetone treatment can be fully resolubilized and then further purified by phenol extraction. This protocol combines TCA/acetone precipitation, which aggressively removes nonprotein compounds, and phenol extraction, which selectively dissolves proteins, resulting in effective purification of proteins from crop tissues. This protocol can also produce high-quality protein preparations from various recalcitrant tissues, and therefore it has a wide range of applications in crop proteomic analysis. Designed to run on a small scale, this protocol can be completed within 5 h.

  6. Editorial: Acid precipitation

    SciTech Connect

    1995-09-01

    This editorial focuses on acid rain and the history of public and governmental response to acid rain. Comments on a book by Gwineth Howell `Acid Rain and Acid Waters` are included. The editor feels that Howells has provide a service to the environmental scientific community, with a textbook useful to a range of people, as well as a call for decision makers to learn from the acid rain issue and use it as a model for more sweeping global environmental issues. A balance is needed among several parameters such as level of evidence, probability that the evidence will lead to a specific direction and the cost to the global community. 1 tab.

  7. Acid Precipitation: Causes and Consequences.

    ERIC Educational Resources Information Center

    Babich, Harvey; And Others

    1980-01-01

    This article is the first of three articles in a series on the acid rain problem in recent years. Discussed are the causes of acid precipitation and its consequences for the abiotic and biotic components of the terrestrial and aquatic ecosystems, and for man-made materials. (Author/SA)

  8. Low-molecular-weight organic acids in the Tibetan Plateau: Results from one-year of precipitation samples at the SET station

    NASA Astrophysics Data System (ADS)

    Liu, Bin; Kang, Shichang; Sun, Jimin; Wan, Xin; Wang, Yongjie; Gao, Shaopeng; Cong, Zhiyuan

    2014-04-01

    Background atmospheric organic acids: formic (F), acetic (A), oxalic (O), and methanesulfonic (MSA, abbreviated to M) acids in the southern Tibetan Plateau (TP), were determined in one-year of precipitation measurements at a remote alpine station. These organic acids were dominated by oxalic (volume-weighted mean of 0.51 μmol l-1)/formic acid (0.38 μmol l-1), followed by acetic acid (0.20 μmol l-1) and MSA (0.10 μmol l-1). Their levels were comparable with those from other remote sites, while they were lower than those found in populated areas. The South Asian monsoon is responsible for the seasonal variation of organic acid concentration: a relative abundance of MSA and lower concentrations of other organic acids (by the dilution effect) in the monsoon season, while opposite in the non-monsoon season. Diverse sources were identified by principal component analysis combined with the corresponding tracers. These were anthropogenic disturbances (which explain 41% of the variance), marine emission (24%), and biogenic emission (16%). Moreover, the variances of F/A, M/(F + A), and O/(F + A) in monsoonal versus non-monsoonal samples, were involved with the changes of sources. Furthermore, these chemical indexes suggest that active photochemistry over the TP was significant for the production of organic acids and consequently enhanced the ratios of M/(F + A) and O/(F + A) in monsoonal rainfalls. The elevated organic compounds within the ascending tropical moisture imply potential significances for the secondary formation of organic acids in the high-altitude and the changes of the Asian monsoon.

  9. Acid precipitation; an annotated bibliography

    USGS Publications Warehouse

    Wiltshire, Denise A.; Evans, Margaret L.

    1984-01-01

    This collection of 1660 bibliographies references on the causes and environmental effects of acidic atmospheric deposition was compiled from computerized literature searches of earth-science and chemistry data bases. Categories of information are (1) atmospheric chemistry (gases and aerosols), (2) precipitation chemistry, (3) transport and deposition (wet and dry), (4) aquatic environments (biological and hydrological), (5) terrestrial environments, (6) effects on materials and structures, (7) air and precipitation monitoring and data collection, and (8) modeling studies. References date from the late 1800 's through December 1981. The bibliography includes short summaries of most documents. Omitted are unpublished manuscripts, publications in press, master 's theses and doctoral dissertations, newspaper articles, and book reviews. Coauthors and subject indexes are included. (USGS)

  10. Acid Precipitation and the Forest Ecosystem

    ERIC Educational Resources Information Center

    Dochinger, Leon S.; Seliga, Thomas A.

    1975-01-01

    The First International Symposium on Acid Precipitation and the Forest Ecosystem dealt with the potential magnitude of the global effects of acid precipitation on aquatic ecosystems, forest soils, and forest vegetation. The problem is discussed in the light of atmospheric chemistry, transport, and precipitation. (Author/BT)

  11. Effects of acid precipitation on Daphnia magna

    SciTech Connect

    Parent, S.; Cheetham, R.D.

    1980-08-01

    Pollutants derived from fossil fuel combustion and precipitated from the atmosphere have substantially increased in the past decades. These materials, precipitated in such industrialized areas as southeastern Canada, have caused considerable alterations in aquatic ecosystems. Precipitation over most of the eastern United States is presently 10 to 500 times more acidic than is natural. Most affected aquatic ecosystems contain oligotrophic waters in regions of thin poorly buffered soils. Zooplankton are an important link in food chains of aquatic ecosystems and their disappearance or decline could drastically affect trophic relationships. Declines in zooplankton density in response to acid precipitation have been reported and short term survival of Daphnia pulex between pH 4.3 and 10.4; however, its potential for reproduction was limited to a fairly narrow range. Anderson (1944) noted the advantages of using daphnia as test organisms, and concluded that Daphnia magna was representative of other abundant zooplankton in sensitivity to toxic substances.

  12. Biologically produced acid precipitable polymeric lignin

    DOEpatents

    Crawford, Don L.; Pometto, III, Anthony L.

    1984-01-01

    A water soluble, acid precipitable polymeric degraded lignin (APPL), having a molecular weight of at least 12,000 daltons, and comprising, by percentage of total weight, at least three times the number of phenolic hydroxyl groups and carboxylic acid groups present in native lignin. The APPL may be modified by chemical oxidation and reduction to increase its phenolic hydroxyl content and reduce the number of its antioxidant inhibitory side chains, thereby improving antioxidant properties.

  13. NAPAP (National Acid Precipitation Assessment Program) results on acid rain

    SciTech Connect

    Not Available

    1990-06-01

    The National Acid Precipitation Assessment Program (NAPAP) was mandated by Congress in 1980 to study the effects of acid rain. The results of 10 years of research on the effect of acid deposition and ozone on forests, particularly high elevation spruce and fir, southern pines, eastern hardwoods and western conifers, will be published this year.

  14. Acid precipitation at 3 sites in the Klang Valley, Malaysia

    SciTech Connect

    Philip, E.; Yap, S.K.; Azimi, S.

    1996-12-31

    A study which examined spatial variation, dust and chemical composition factors associated with precipitation pH in the Klang Valley had been conducted. Precipitation samples were collected on a monthly basis at 3 different locations during the periods of 1993-1995. These long term sites were situated at varying distance from the industrial zone of the Klang Valley. Data were collected on a monthly basis and where possible after every rainfall. This included the field pH, electrical conductivity (EC) and analysis of chemical components. To date, the general pH trend at these stations is decreasing towards the acid range. The site furthest from the industrial zone had the highest pH values while site closest to the industrial zone had the lowest pH. There appeared to be a correlation between the precipitation pH and electrical conductivity (EC), the EC readings increased with increased acidity. Variations in precipitation pH was closely associated with the changes in sulfate concentration. The pH of precipitation is determined not only by the anions, but also by the concentration of cations in the atmosphere which neutralized the acidity by forming salts. The main cause for the decrease in the pH values is the significant increase of acidic components and decrease of soil-oriented components (Mg and Ca) in the rain water.

  15. Acid precipitation. (Latest citations from the Compendex database). Published Search

    SciTech Connect

    Not Available

    1993-06-01

    The bibliography contains citations concerning the causes, effects, sources, and controls of acid precipitation and acidification. Techniques and technology for measurement and analysis of acid precipitation are considered. (Contains 250 citations and includes a subject term index and title list.)

  16. Acid precipitation. (Latest citations from Pollution Abstracts database). Published Search

    SciTech Connect

    Not Available

    1993-09-01

    The bibliography contains citations concerning the research of acid precipitation, and the resultant acidification of land and water. Topics include composition, causes, effects, sources, measurements, and controls of acid precipitation. Worldwide geographical distribution of acid precipitation and acidification are covered. (Contains 250 citations and includes a subject term index and title list.)

  17. Acid precipitation. (Latest citations from Pollution abstracts). Published Search

    SciTech Connect

    Not Available

    1994-03-01

    The bibliography contains citations concerning the research of acid precipitation, and the resultant acidification of land and water. Topics include composition, causes, effects, sources, measurements, and controls of acid precipitation. Worldwide geographical distribution of acid precipitation and acidification are covered. (Contains 250 citations and includes a subject term index and title list.)

  18. Direct impact aerosol sampling by electrostatic precipitation

    SciTech Connect

    Braden, Jason D.; Harter, Andrew G.; Stinson, Brad J.; Sullivan, Nicholas M.

    2016-02-02

    The present disclosure provides apparatuses for collecting aerosol samples by ionizing an air sample at different degrees. An air flow is generated through a cavity in which at least one corona wire is disposed and electrically charged to form a corona therearound. At least one grounded sample collection plate is provided downstream of the at least one corona wire so that aerosol ions generated within the corona are deposited on the at least one grounded sample collection plate. A plurality of aerosol samples ionized to different degrees can be generated. The at least one corona wire may be perpendicular to the direction of the flow, or may be parallel to the direction of the flow. The apparatus can include a serial connection of a plurality of stages such that each stage is capable of generating at least one aerosol sample, and the air flow passes through the plurality of stages serially.

  19. Sampling problems: The small scale structure of precipitation

    NASA Technical Reports Server (NTRS)

    Crane, R. K.

    1981-01-01

    The quantitative measurement of precipitation characteristics for any area on the surface of the Earth is not an easy task. Precipitation is rather variable in both space and time, and the distribution of surface rainfall data given location typically is substantially skewed. There are a number of precipitation process at work in the atmosphere, and few of them are well understood. The formal theory on sampling and estimating precipitation appears considerably deficient. Little systematic attention is given to nonsampling errors that always arise in utilizing any measurement system. Although the precipitation measurement problem is an old one, it continues to be one that is in need of systematic and careful attention. A brief history of the presently competing measurement technologies should aid us in understanding the problem inherent in this measurement task.

  20. Sampling of the Diurnal Cycle of Precipitation using TRMM

    NASA Technical Reports Server (NTRS)

    Negri, Andrew J.; Bell, Thomas L.; Xu, Li-Ming; Starr, David OC. (Technical Monitor)

    2001-01-01

    We examine the temporal sampling of tropical regions using observations from the Tropical Rainfall Measuring Mission (TRMM) Microwave Imager (TMI) and Precipitation Radar (PR). We conclude that PR estimates at any one hour, even using three years of data, are inadequate to describe the diurnal cycle of precipitation over regions smaller than 12 degrees, due to high spatial variability in sampling. We show that the optimum period of accumulation is four hours. Diurnal signatures display half as much sampling error when averaged over four hours of local time. A similar pattern of sampling variability is found in the TMI data, despite the TMI's wider swath and increased sampling. These results are verified using an orbital model. The sensitivity of the sampling to satellite altitude is presented, as well as sampling patterns at the new TRMM altitude of 402.5 km.

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

    USGS Publications Warehouse

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

    1985-01-01

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

  2. Acid Precipitation Awareness Curriculum Materials in the Life Sciences.

    ERIC Educational Resources Information Center

    Stubbs, Harriett S.

    1983-01-01

    Provides an outline of course content for acid precipitation and two acid rain activities (introduction to pH and effects of acid rain on an organism). Information for obtaining 20 additional activities as well as an information packet containing booklets, pamphlets, and articles are also provided. (JN)

  3. Acid Precipitation in the Pacific Northwest.

    ERIC Educational Resources Information Center

    Baldwin, John; Kozak, David

    1988-01-01

    Discusses the causes, sources, and problems associated with acid deposition in the Pacific Northwest. Includes a learning activity about acid rain, "Deadly Skies," which was adapted from the Project WILD Aquatic Supplement. (TW)

  4. Use of ion chromatography for analysis of MAP3S precipitation samples

    SciTech Connect

    Rothert, J.

    1980-07-01

    The Multistate Atmospheric Power Production Pollution Study/Regional Acidity of Industrial Emissions, MAP3S/RAINE program includes measurement and modeling of fossil-fuel effluent concentrations in precipitation and air in the northeastern United States. To determine precipitation concentrations of sulfur and nitrogen oxides as well as PO/sub 4//sup 3 -/, Cl/sup -/, Na/sup +/, K/sup +/, NH/sub 4//sup +/, Ca/sup 2 +/, Mg/sup 2 +/, pH, and conductivity, an eight-1 site precipitation network in rural eastern United States has been established. Two Dionex Model 10 ion chromatographs are being used to analyze the precipitation samples. This paper describes the use and operation of these instruments. (ACR)

  5. Effects of acid precipitation on crops

    SciTech Connect

    Lee, J.J.

    1981-01-01

    The effects of acid rain on crop yield have been studied using field-grown and potted plants. Results have shown that the chemicals in acid rain can affect crop growth and yield at ambient concentrations. For many crops, the dose-response curve probably has at least one peak and crossover point from stimulatory to inhibitory response may depend on other environmental factors. Plant parts often are affected differently, suggesting that acid rain can change the allocation of energy within plants. Available experimental results are not transferable to agricultural situations. The characteristics of acid rain which have the greatest influence on crop yield have not been determined. Interactions between acid rain and other environmental factors have scarcely been studied. Before a believable assessment of the economic impact of acid rain on crops can be done, the mechanisms of response have to be studied and the predictive capability enhanced and validated.

  6. Acid Precipitation: Scientific Progress and Public Awareness.

    ERIC Educational Resources Information Center

    Cowling, Ellis B.

    1983-01-01

    Describes certain perspectives on scientific research and on the public debates about acid deposition and its effects. Although primary attention is given to European/North American research, the ideas developed are relevant in any world region sensitive to acid deposition resulting from intense industrialization. (Author/JN)

  7. Acid precipitation. (Latest citations from the Aerospace database). Published Search

    SciTech Connect

    Not Available

    1993-12-01

    The bibliography contains citations concerning the measurement and analysis of acid rain and acidification of areas by precipitation. Both global and regionalized areas of acid rain effects are examined. Control techniques applicable to the sources and causes are discussed. (Contains a minimum of 187 citations and includes a subject term index and title list.)

  8. Effects of acidic precipitation on field crops

    SciTech Connect

    Evans, L.S.; Hendrey, G.R.; Lewin, K.F.; Gmur, N.F.

    1982-02-01

    The effects of acid rain on yields of field-grown soybeans has been investigated. Plants exposed to simulated rainfalls of pH 4.1, 3,3 and 2.7 had decreased seed yields of 10.6, 16.8 and 23.9% below yields of plants exposed to simulated rainfalls of pH 5.6. (ACR)

  9. Acid precipitation chemistry in an urban plume

    SciTech Connect

    Saxena, P.; Arcado, T.D.; Marler, B.L.; Altshuler, S.L. )

    1987-01-01

    In this paper the authors present the results of an ongoing study performed by the Pacific Gas and Electric Company (PGandE) to: investigate the formation, transport and deposition of acidic species in the urban plume from the San Francisco Bay Area (SFBA) and assess the role of two gas-fired electric generation facilities located on the eastern boundary of the SFBA. They present a brief summary of their study area's climate. The network used in this study and our experimental methods are also described. An analysis of wet deposition data collected by our network is presented along with a discussion of the major findings, to date, of our study.

  10. Precipitation of sodium acid urate from electrolyte solutions

    NASA Astrophysics Data System (ADS)

    Füredi-Milhofer, Helga; Babić-Ivaniĉić, Vesna; Milat, Ognjen; Brown, Walter E.; Gregory, Thomas M.

    1987-07-01

    The precipitation of soduim urate from solutions containing uric acid, soduim hydroxide, hydrochloric acid, sodium chloride and water was investigated at constant pH (7.5±0.1) and temperature (308 K). Precipitates were observed by lights and electron microscopy and characterized by electron and X-ray diffraction. The results are presented in the form of "precipitation" and "chemical potential" diagrams, the latter giving the soduim-to-urate molar ratios of the precipitates. Two types of precipitation boundaries were observed, both of which had indicated soduim-to-urate moral ratios of 1:1. The ion activity product, (Na +)(HU -), associated with boundary I was AP I=(4.8±1.1)×10 -5 and with boundary II was with boundary II was AP II=(6.5±0.4)×10 -4. The supersaturation, S, at boundary II was S=AP II/ Ksp=12.3, in which Ksp is the solubility product of soduim acid urate monohydrate. The latter precipitated as well-formed crystals at supersaturations of 12.3 and above. The ion activity product associated with boundary I is approximately equal to the solubility product of soduim acid urate monohydrate. Small amounts of several morphologically different sodium urate crystals formed in the range of supersaturations (1≤ S≤12.3). Crystals formed in this range may include the monohydrate of sodium acid urate and possibly a higher hydrate. The findings have relevance to pathological renal stone formation and gouty arthritis.

  11. Coupling Meteorology, Metal Concentrations, and Pb Isotopes for Source Attribution in Archived Precipitation Samples

    EPA Science Inventory

    A technique that couples lead (Pb) isotopes and multi-element concentrations with meteorological analysis was used to assess source contributions to precipitation samples at the Bondville, Illinois USA National Trends Network (NTN) site. Precipitation samples collected over a 16 ...

  12. Compositions and method for controlling precipitation when acidizing sour wells

    SciTech Connect

    Dill, W.R.; Walker, M.L.

    1989-12-19

    This patent describes an acidizing composition for treating a sour well. It comprises: a base acid solution having an initial ph below 1.9; an iron sequestering agent to combine with iron present in the solution comprising at least one compound selected from the group consisting of aminopolycarboxylic acids, hydroxycarboxylic acids, cyclic polyethers and derivatives of the acids and ethers present in an amount of from about 0.25 to about 5 percent by weight of the acid solution; and a sulfide modifier to combine with sulfides present in the solution comprising at least one member selected from the group consisting of an aldehyde, acetal, hemiacetal and any other compound capable of forming an aldehyde in solution, present in an amount of from about 1 to about 4 percent by weight of the acid solution, whereby precipitation of ferric hydroxide, ferrous sulfide and elemental sulfur is inhibited as acid spending occurs.

  13. Acidic precipitation: considerations for an air-quality standard

    SciTech Connect

    Evans, L.S.; Hendrey, G.R.; Stensland, G.J.; Johnson, D.W.; Francis, A.J.

    1980-01-01

    Acidic precipitation, wet or frozen deposition with a hydrogen ion concentration greatern than 2.5 ..mu..eq l/sup -1/ is a significant air pollution problem in the United States. The chief anions accounting for the hydrogen ions in rainfall are nitrate and sulfate. Agricultural systems are more likely to derive net nutritional benefits from increasing inputs of acidic rain than are forest systems when soils alone are considered. Agricultural soils may benefit because of the high N and S requirements of agricultural plants. Detrimental effects to forest soils may result if atmospheric H/sup +/ inputs significantly add to or exceed H/sup +/ production by soils. Acidification of fresh waters of southern Scandinavia, southwestern Scotland, southeastern Canada, and northeastern United States is caused by acid deposition. Areas of these regions in which this acidification occurs have in common, highly acidic precipitation with volume weighted mean annual H/sup +/ concentrations of 25 ..mu..eq l/sup -1/ or higher and slow weathering granitic or precambrian bedrock with thin soils deficient in minerals which would provide buffer capacity. Biological effects of acidification of fresh waters are detectable below pH 6.0. As lake and stream pH levels decrease below pH. 6.0, many species of plants, invertebrates, and vertebrates are progressively eliminated. Generally, fisheries are impacted below pH 5.0 and are completely destroyed below pH 4.8. There are few studies that document effects of acidic precipitation on terrestrial vegetation to establish an air quality standard. It must be demonstrated that current levels of precipitation acidity alone significantly injure terrestrial vegetation. In terms of documented damanges, current research indicates that establishing a standard for precipitation for the volume weighted annual H/sup +/ concentration at 25 ..mu..eq l/sup -1/ may protect the most sensitive areas from permanent lake acidification.

  14. Glycation inhibits trichloroacetic acid (TCA)-induced whey protein precipitation

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Four different WPI saccharide conjugates were successfully prepared to test whether glycation could inhibit WPI precipitation induced by trichloroacetic acid (TCA). Conjugates molecular weights after glycation were analyzed with SDS-PAGE. No significant secondary structure change due to glycation wa...

  15. Teacher's Resource Guide on Acidic Precipitation with Laboratory Activities.

    ERIC Educational Resources Information Center

    Barrow, Lloyd H.

    The purpose of this teacher's resource guide is to help science teachers incorporate the topic of acidic precipitation into their curricula. A survey of recent junior high school science textbooks found a maximum of one paragraph devoted to the subject; in addition, none of these books had any related laboratory activities. It was on the basis of…

  16. Acidic precipitation, Vol. 2: Biological and ecological effects

    SciTech Connect

    Adriano, D.C.; Johnson, A.H.

    1989-01-01

    Acidic precipitation has its origin in emissions to the atmosphere of numerous compounds from both natural and man-made sources. The chapters in this volume cover a wide array of topics on the biological and ecological effects of acidic precipitation. A chapter on soil productivity emphasizes changes in biological and chemical characters of forest soils impacted by acidic deposition. Additional chapters discuss specific effects on soil microorganisms, trees, and crops. The importance of aluminum in this environmental issue is highlighted by a discussion on the mobility and phytotoxicity of this element in acidic soils. This chapter puts into perspective the biology of Al stressed plants. Two major chapters discuss the effect of acidic precipitation on forest ecosystems; one emphasizing North America, and the other Europe. Effects of soil acidification on key soil processes, including litter decomposition and depletion of essential plant nutrients in the soil profile are emphasized. Finally, three major chapters comprehensively cover limnological ecosystems and their response to acidic perturbation. These chapters discuss the response of stream and lake communities, both floral and faunal, to water acidification, including reduced biodiversity in these systems. Ten chapters have been processed separately for inclusion in the appropriate data bases.

  17. HF acid blends based on formation conditions eliminate precipitation problems

    SciTech Connect

    Gdanski, R.; Shuchart, C.

    1997-03-01

    Formulating HCl-HF acid blends based on the mineralogy and temperature of a formation can increase the success of hydrofluoric acid (HF) treatments. Sodium and potassium in the structures of formation minerals can cause precipitation and matrix plugging problems during acidizing. Slight modifications of the acid blend used in the treatment can help eliminate fluosilicate precipitation. Researchers recently conducted tests to determine how acid blends react in different formations under varying temperatures. The results of the tests indicate that the minimum HCl:HF ratio in an acid blend is 6-to-1, and the optimum ratio is 9-to-1. Regular mud acid (12% HCl-3% HF) has been used successfully for years to enhance production in sandstone formations. By the 1980s, operators began to vary the concentration of HF and HCl acids to solve excessive sanding problems in sandstone. The paper discusses treatment problems, formation characteristics, alumino-silicate scaling, research results, brine compatibility, optimum treatment, and acid volume guidelines.

  18. Reconciling Empirical Carbonate Clumped Isotope Calibrations: A Comparison of Calcite Precipitation and Acid Digestion Methods

    NASA Astrophysics Data System (ADS)

    Kelson, J.; Huntington, K. W.; Schauer, A. J.; Saenger, C.; Lechler, A. R.

    2015-12-01

    An accurate empirical calibration is necessary to confidently apply the carbonate clumped isotope (Δ47) thermometer. Previous synthetic carbonate calibrations disagree in temperature sensitivity, with one group of calibrations displaying a shallow Δ47-temperature slope (e.g., Dennis & Schrag, GCA, 2010), and the other a steep slope (e.g., Zaarur et al., EPSL, 2013). These calibrations differ in both the method of mineral precipitation and the temperature of the phosphoric acid used to digest carbonates for analysis, making it difficult to isolate the cause of the discrepancy. Here, we precipitate synthetic carbonates at temperatures of 6-80ºC using 4 different precipitation methods, and analyze the samples using both 90 and 25°C acid digestion. Precipitation experiments varied the use of salts (NaHCO3 and CaCl2) vs. dissolved CaCO3 as a starting solution, the use of carbonic anhydrase to promote isotopic equilibrium among dissolved inorganic carbon species in solution, and the method by which CO2 degasses to force carbonate precipitation. Carbonates precipitated by using salts and allowing CO2 to passively degas produce a shallow calibration slope that we hypothesize to approach isotopic equilibrium. Precipitation methods that bubble CO2 into solution then degas that CO2 (either passively or actively by bubbling N2) produce carbonates with consistently lower Δ47 and higher δ18O values for a given growth temperature. We infer that these carbonates grew in disequilibrium during rapid CO2 degassing. Varying acid digestion temperature does not change the results; acid fractionation factor is not correlated with grain size, Δ47, or d47 values. No precipitation method produces a steep calibration slope. Our large sample set of >60 carbonates lend confidence to a shallow slope calibration, and inform interpretations of Δ47 and δ18O values of natural carbonates that grow under conditions of isotopic disequilibrium.

  19. Acid precipitation: things one can do - the Tug Hill Commission approach

    SciTech Connect

    Beevers, D.J.

    1982-01-01

    Acid precipitation is an international problem requiring more knowledge of its causes and effects, increased public awareness, and national policies to address it. New York's Temporary Tug Hill State Commission, with limited budget, small staff, and only regional jurisdiction, has sought to learn and provide information about acid precipitation and to impact public policy. The area receives a large quantity of highly acidic precipitation. For example, the average lab pH for 22 samples taken at Bennett Bridge between June and December 1980 (the only data available) was 4.09. Some red spruce and red maple die-back may be linked to acid precipitation. The Commission has implemented a variety of activities in response, including use of students to survey acid precipitation, policy statements, research projects on water quality and forest impacts, and design and implementation of a public opinion survey that may lead to additional public awareness, legislative action, and research. Most of these are relatively low-cost activities that similar agencies or other groups could participate in or initiate. 9 references, 3 figures.

  20. Baseline acidity of precipitation at the South Pole during the last two millennia

    NASA Astrophysics Data System (ADS)

    Cragin, J. H.; Giovinetto, M. B.; Gow, A. J.

    Measurements of meltwater pH from annual layers of South Pole firn and ice samples ranging in age from 40 to 2000 years B.P. show that precipitation at this remote site has a higher natural acidity than that expected from atmospheric equilibrium with CO2. The average pH of deaerated (CO2-free) samples was 5.64 ± 0.08, while air-equilibrated samples averaged 5.37 ± 0.08, a pH that is about a factor of two more acidic than the expected background pH of 5.65. The observed “excess” acidity can be accounted for by SO42- and NO3- levels in the samples originating from non-anthropogenic H2SO4 and HNO3. Because of the presence of these naturally occurring acids in South Pole precipitation, a pH of 5.4 is considered a more representative baseline reference pH for acid precipitation studies.

  1. Composition and hygroscopicity of aerosol particles at Mt. Lu in South China: Implications for acid precipitation

    NASA Astrophysics Data System (ADS)

    Li, Weijun; Chi, Jianwei; Shi, Zongbo; Wang, Xinfeng; Chen, Bin; Wang, Yan; Li, Tao; Chen, Jianmin; Zhang, Daizhou; Wang, Zifa; Shi, Chune; Liu, Liangke; Wang, Wenxing

    2014-09-01

    Physicochemical properties of aerosol particles were studied at Mt. Lu, an elevated site (115°59‧E, 29°35‧N, 1165 m) within the acid precipitation area. Northeast winds transport copious amounts of air pollutants and water vapor from the Yangtze River Delta into this acid precipitation area. NH4+ and SO42- are the dominant ions in PM2.5 and determine aerosol acidity. Individual particle analysis shows abundant S-rich and metals (i.e. Fe-, Zn-, Mn-, and Pb-rich) particles. Unlike aerosol particles in North China and urban areas, there are little soot and mineral particles at Mt. Lu. Lack of mineral particles contributed to the higher acidity in precipitation in the research area. Nano-sized spherical metal particles were observed to be embedded in 37% of S-rich particles. These metal particles were likely originated from heavy industries and fired-power plants. Hygroscopic experiments show that most particles start to deliquesce at 73-76% but organic coating lowers the particle deliquescence relative humidity (DRH) to 63-73%. The DRHs of these aerosol particles are clearly smaller than that of pure ammonium sulfate particles which is 80%. Since RH in ambient air was relatively high, ranging from 65% to 85% during our study period, most particles at our sampling site were in liquid phase. Our results suggest that liquid phase reactions in aerosol particles may contribute to SO2 to sulfuric acid conversion in the acid precipitation area.

  2. Impact of effects of acid precipitation on toxicity of metals.

    PubMed Central

    Nordberg, G F; Goyer, R A; Clarkson, T W

    1985-01-01

    Acid precipitation may increase human exposure to several potentially toxic metals by increasing metal concentrations in major pathways to man, particularly food and water, and in some instances by enhancing the conversion of metal species to more toxic forms. Human exposures to methylmercury are almost entirely by way of consumption of fish and seafood. In some countries, intakes by this route may approach the levels that can give rise to adverse health effects for population groups with a high consumption of these food items. A possible increase in methylmercury concentrations in fish from lakes affected by acid precipitation may thus be of concern to selected population groups. Human exposures to lead reach levels that are near those associated with adverse health effects in certain sensitive segments of the general population in several countries. The possibility exists that increased exposures to lead may be caused by acid precipitation through a mobilization of lead from soils into crops. A route of exposure to lead that may possibly be influenced by acid precipitation is an increased deterioration of surface materials containing lead and a subsequent ingestion by small children. A similar situation with regard to uptake from food exists for cadmium (at least in some countries). Human metal exposures via drinking water may be increased by acid precipitation. Decreasing pH increases corrosiveness of water enhancing the mobilization of metal salts from soil; metallic compounds may be mobilized from minerals, which may eventually reach drinking water. Also, the dissolution of metals (Pb, Cd, Cu) from piping systems for drinking water by soft acidic waters of high corrosivity may increase metal concentrations in drinking water. Exposures have occasionally reached concentrations which are in the range where adverse health effects may be expected in otherwise healthy persons. Dissolution from piping systems can be prevented by neutralizing the water before

  3. Ten-year study on acid precipitation nears conclusion

    SciTech Connect

    Olem, H. )

    1990-04-01

    Results from the National Acid Precipitation Assessment Program (NAPAP) are discussed. Final results are contained in 26 state of the science reports. Seven of the reports provide information on acid rain and aquatic ecosystems. They describe the current state of acidic surface waters, watershed processes affecting surface water chemistry, historical evidence for surface water acidification, methods for forecasting future changes, and the response of acidic surface water to liming. Six areas of the country were found to be of special interest: southwest Adirondacks, New England, forested areas of the mid-Atlantic highlands, the Atlantic coastal plain, the northern Florida highlands, parts of northeastern Wisconsin and the Upper Peninsula of Michigan. Environmental effects, mitigation efforts and possible legislation are briefly discussed.

  4. Natural acidity of waters in podzolized soils and potential impacts from acid precipitation

    SciTech Connect

    Stednick, J.D.; Johnson, D.W.

    1982-01-01

    Nutrient movements through sites in southeast Alaska and Washington were documented to determine net changes in chemical composition of precipitation water as it passed through a forest soil and became stream-flow. These sites were not subject to acid precipitation (rainfall pH 5.8 to 7.2), yet soil water was acidified to 4.2 by natural organic acid-forming processes in the podzol soils. Organic acids precipitated in the subsoils, allowing a pH increase. Streamwater pH ranged from 6.5 to 7.2 indicating a natural buffering capacity that may exceed any additional acid input from acid rain. Precipitation composition was dominated by calcium, magnesium, sodium, and chloride due to the proximity of the ocean at the southeast Alaska site. Anionic constituents of the precipitation were dominated by bicarbonate at the Washington site. Soil podzolization processes concurrently increased solution color and iron concentrations in the litter and surface horizons leachates. The anion flux through the soil profile was dominated by chloride and sulfate at the southeast Alaska site, whereas at the Washington site anion flux appeared to be dominated by organic acids. Electroneutrality calculations indicated a cation deficit for the southeast Alaska site.

  5. Natural acidity of waters in podzolized soils and potential impacts from acid precipitation

    SciTech Connect

    Stednick, J.D.; Johnson, D.W.

    1982-01-01

    Nutrient movements through sites in southeast Alaska and Washington were documented to determine net changes in chemical composition of precipitation water as it passed through a forest soil and became stream flow. These sites were not subject to acid precipitation (rainfall pH 5.8 to 7.2), yet soil water was acidified to 4.2 by natural organic acid forming processes in the podzol soils. Organic acids precipitated in the subsoils, allowing a pH increase. Stream water pH ranged from 6.5 to 7.2 indicating a natural buffering capacity that may exceed any additional acid input from acid rain. Precipitation composition was dominated by magnesium, sodium, and chloride due to the proximity of the ocean at the southeast Alaska site. Anionic constituents of the precipitation were dominated by bicarbonate at the Washington site. Soil podzolization processes concurrently increased solution color and iron concentrations in the litter and surface horizons leachates. The anion flux through the soil profile was dominated by chloride and sulfate at the southwast Alaska site, whereas at the Washington site anion flux appeared to be dominated by organic acids. Electroneutrality calculations indicated a cation deficit for the southeast Alaska site. 10 references, 2 tables.

  6. Precipitation of biomimetic fluorhydroxyapatite/polyacrylic acid nanostructures

    NASA Astrophysics Data System (ADS)

    Roche, Kevin J.; Stanton, Kenneth T.

    2015-01-01

    Ordered structures of fluorhydroxyapatite (FHA) nanoparticles that resemble the nanostructure of natural human enamel have been prepared. Wet precipitation in the presence of polyacrylic acid (PAA) was used, and the particle morphology was altered by varying several reaction conditions. High molecular weight PAA increased particle length from around 54 nm to several hundred nanometres, while maintaining particle width at 15 nm. PAA concentration and the order of mixing the reactants also influenced crystal morphology. Optimum conditions produced dense, aligned bundles of highly elongated nanorods, which are very similar to the hierarchical nanostructure of human tooth enamel.

  7. Amino acid analyses of Apollo 14 samples.

    NASA Technical Reports Server (NTRS)

    Gehrke, C. W.; Zumwalt, R. W.; Kuo, K.; Aue, W. A.; Stalling, D. L.; Kvenvolden, K. A.; Ponnamperuma, C.

    1972-01-01

    Detection limits were between 300 pg and 1 ng for different amino acids, in an analysis by gas-liquid chromatography of water extracts from Apollo 14 lunar fines in which amino acids were converted to their N-trifluoro-acetyl-n-butyl esters. Initial analyses of water and HCl extracts of sample 14240 and 14298 samples showed no amino acids above background levels.

  8. Comparison of daily and weekly precipitation sampling efficiencies using automatic collectors

    USGS Publications Warehouse

    Schroder, L.J.; Linthurst, R.A.; Ellson, J.E.; Vozzo, S.F.

    1985-01-01

    Precipitation samples were collected for approximately 90 daily and 50 weekly sampling periods at Finley Farm, near Raleigh, North Carolina from August 1981 through October 1982. Ten wet-deposition samplers (AEROCHEM METRICS MODEL 301) were used; 4 samplers were operated for daily sampling, and 6 samplers were operated for weekly-sampling periods. This design was used to determine if: (1) collection efficiences of precipitation are affected by small distances between the Universal (Belfort) precipitation gage and collector; (2) measurable evaporation loss occurs and (3) pH and specific conductance of precipitation vary significantly within small distances. Average collection efficiencies were 97% for weekly sampling periods compared with the rain gage. Collection efficiencies were examined by seasons and precipitation volume. Neither factor significantly affected collection efficiency. No evaporation loss was found by comparing daily sampling to weekly sampling at the collection site, which was classified as a subtropical climate. Correlation coefficients for pH and specific conductance of daily samples and weekly samples ranged from 0.83 to 0.99.Precipitation samples were collected for approximately 90 daily and 50 weekly sampling periods at Finley farm, near Raleigh, North Carolina from August 1981 through October 1982. Ten wet-deposition samplers were used; 4 samplers were operated for daily sampling, and 6 samplers were operated for weekly-sampling periods. This design was used to determine if: (1) collection efficiencies of precipitation are affected by small distances between the University (Belfort) precipitation gage and collector; (2) measurable evaporation loss occurs and (3) pH and specific conductance of precipitation vary significantly within small distances.

  9. Sampling of Atmospheric Precipitation and Deposits for Analysis of Atmospheric Pollution

    PubMed Central

    Skarżyńska, K.; Polkowska, Ż; Namieśnik, J.

    2006-01-01

    This paper reviews techniques and equipment for collecting precipitation samples from the atmosphere (fog and cloud water) and from atmospheric deposits (dew, hoarfrost, and rime) that are suitable for the evaluation of atmospheric pollution. It discusses the storage and preparation of samples for analysis and also presents bibliographic information on the concentration ranges of inorganic and organic compounds in the precipitation and atmospheric deposit samples. PMID:17671615

  10. Purification of IgG from serum with caprylic acid and ammonium sulphate precipitation is not superior to ammonium sulphate precipitation alone.

    PubMed

    Mohanty, J G; Elazhary, Y

    1989-01-01

    Immunoglobulin G (IgG) from bovine serum raised against Aeromonas Salmonicida was purified by ammonium sulphate precipitation (ASP) or caprylic acid treatment followed by ammonium sulphate precipitation (CAAS). Purity of IgG samples prepared by both methods were examined by High Performance Gel Permeation Chromatography, electrophoresis and antibody activity assay. Results suggest that IgG prepared by ASP is better than that obtained by CAAS method in terms of the yield of the IgG monomers and the recovery of the antibody activity.

  11. Impact of acid precipitation on recreation and tourism in Ontario: an overview

    SciTech Connect

    Not Available

    1984-01-01

    The impacts of acid precipitation on fishing opportunities, waterfowl and moose hunting, water contact activities, and the perception of the environment in Ontario are analyzed. Economic effects and future research needs are also estimated and discussed. These questions have been examined by identifying the likely links between acidic precipitation and recreation and tourism, by developing estimates of the importance of aquatic-based recreation and tourism, by describing the current and estimated future effects of acid precipitation. 101 references, 9 figures, 19 tables.

  12. Isotope fractionation during precipitation of methamphetamine HCl and discrimination of seized forensic samples.

    PubMed

    David, Gabrielle E; Coxon, Anne; Frew, Russell D; Hayman, Alan R

    2010-07-15

    Methamphetamine is a widely abused illicit drug. Increasingly, studies have focused on stable isotope analysis by isotope ratio mass spectrometry (IRMS) to link samples of methamphetamine synthesized together or from the same source of precursor. For this reason, it is important to understand potential sources of isotope fractionation that could cause variability in forensic data sets. In this study, methamphetamine free base samples were synthesized from (-)-ephedrine HCl using the HI/red phosphorus synthetic route and then precipitated as HCl salts by bubbling with HCl gas. The entire sample did not precipitate when first bubbled with gas, and multiple precipitation steps were required. Fractions of precipitate were individually analyzed for delta(13)C, delta(15)N and delta(2)H by IRMS. Both delta(15)N and delta(2)H were found to become more negative, with the heavy isotopes depleted, in successive fractions of precipitate. Homogenizing the precipitate fractions together could eliminate this fractionation. However, in a clandestine situation this fractionation could lead to greater than expected delta(15)N and delta(2)H variability between illicit samples of methamphetamine HCl that have been synthesized from the same sample of ephedrine. This needs to be taken into account when interpreting forensic IRMS data. We also present an analysis of four separate seized case lots of methamphetamine HCl, taking into account the possible sources of fractionation and available intelligence information.

  13. Colloidal precipitates related to Acid Mine Drainage: bacterial diversity and micro fungi-heavy metal interactions

    NASA Astrophysics Data System (ADS)

    Lucchetti, G.; Carbone, C.; Consani, S.; Zotti, M.; Di Piazza, S.; Pozzolini, M.; Giovine, M.

    2015-12-01

    In Acid Mine Drainage (AMD) settings colloidal precipitates control the mobility of Potential Toxic Elements (PTEs). Mineral-contaminant relationships (i.e. adsorption, ion-exchange, desorption) are rarely pure abiotic processes. Microbes, mainly bacteria and microfungi, can catalyze several reactions modifying the element speciation, as well as the bioavailability of inorganic pollutants. Soil, sediments, and waters heavily polluted with PTEs through AMD processes are a potential reservoir of extremophile bacteria and fungi exploitable for biotechnological purposes. Two different AMD related colloids, an ochraceous precipitate (deposited in weakly acidic conditions, composed by nanocrystalline goethite) and a greenish-blue precipitate (deposited at near-neutral pH, composed by allophane + woodwardite) were sampled. The aims of this work were to a) characterize the mycobiota present in these colloidal minerals by evaluating the presence of alive fungal propagules and extracting bacteria DNA; b) verify the fungal strains tolerance, and bioaccumulation capability on greenish-blue and ZnSO4 enriched media; c) evaluate potential impact of bacteria in the system geochemistry. The preliminary results show an interesting and selected mycobiota able to survive under unfavourable environmental conditions. A significant number of fungal strains were isolated in pure culture. Among them, species belonging to Penicillium and Trichoderma genera were tested on both greenish-blue and ZnSO4 enriched media. The results show a significant tolerance and bioaccumulation capability to some PTEs. The same colloidal precipitates were processed to extract bacteria DNA by using a specific procedure developed for sediments. The results give a good yield of nucleic acids and a positive PCR amplification of 16S rDNA accomplished the first step for future metagenomic analyses.

  14. Relationship between acid precipitation and three-dimensional transport associated with synoptic-scale cyclones

    SciTech Connect

    Haagenson, P.L.; Lazrus, A.L.; Kuo, Y.H.; Caldwell, G.A.

    1985-09-01

    Field data collected during APEX (Acid Precipitation Experiment) are used in combination with an isentropic trajectory model to analyze the relationship between acid precipitation and three-dimensional transport associated with cyclonic storms. Data are presented which indicate that high acidity in precipitation is often associated with slow transport speed and elevated SO2 concentrations in the dry air feeding into the precipitating regions. Conversely, low acidity is usually related to rapid transit, descending motion, and transport above the atmospheric boundary layer. The results also show that precipitation in the cold sector of a cyclone (in advance of the surface warm front) is often more acidic than that in other sectors of the storm. Four case studies are included to detail some of these meteorological effects. 19 references.

  15. Research for amino acids in lunar samples.

    NASA Technical Reports Server (NTRS)

    Gehrke, C. W.; Zumwalt, R. W.; Kuo, K.; Rash, J. J.; Aue , W. A.; Stalling, D. L.; Kvenvolden, K. A.; Ponnamperuma, C.

    1972-01-01

    The study was primarily directed toward the examination of Apollo 14 lunar fines for indigenous amino acids or materials which could be converted to amino acids on hydrolysis with 6 N hydrochloric acid. Initial experiments were conducted to confirm the integrity of the derivatization reactions and reagents, and to optimize the gas-liquid chromatographic (GLC) instrumental and chromatographic system for the separation and flame ionization detection of the amino acid derivatives. In studies on the recovery of amino acids added to lunar fines, low recoveries were obtained when 10 ng of each amino acid were added to 50 mg of virgin fines, but the subsequent addition of 50 ng of each to the previously extracted sample resulted in much higher recoveries.

  16. Occurrence of acid precipitation on the West Coast of the United States

    SciTech Connect

    Powers, C.F.; Rambo, D.L.

    1981-01-01

    Compilation of published and unpublished data shows acid precipitation to be more widespread in the Pacific coastal states than is generally recognized. Although information is scattered and discontinuous, precipitation is definitely acidic in the Los Angeles Basin and north-central California and in the Puget Sound region in Washington. Acid-rain occurrences were observed in western and eastern Oregon, but data are inadequate for regional generalization. New stations currently being established in Washington and Oregon, largely in response to the recently renewed activity of Mount St. Helens, will greatly facilitate assessment of precipitation acidity in the Northwest.

  17. Caprylic acid precipitation method for impurity reduction: an alternative to conventional chromatography for monoclonal antibody purification.

    PubMed

    Brodsky, Yan; Zhang, Cheng; Yigzaw, Yinges; Vedantham, Ganesh

    2012-10-01

    We report the use of caprylic acid based impurity precipitation as (1) an alternative method to polishing chromatography techniques commonly used for monoclonal antibody purification and (2) an impurity reduction step prior to harvesting the bioreactor. This impurity reduction method was tested with protein A purified antibodies and with cell culture fluid. First, the operational parameters influencing precipitation of host cell proteins and high molecular weight aggregate in protein A pools were investigated. When used as a polishing step, the primary factor affecting purification and yield was determined to be pH. Caprylic acid precipitation was comparable to polishing IEX chromatography in reducing host cell protein and aggregate levels. A virus reduction study showed complete clearance of a model retrovirus during caprylic acid precipitation of protein A purified antibody. Caprylic acid mediated impurity precipitation in cell culture showed that the impurity clearance was generally insensitive to pH and caprylic acid concentration whereas yield was a function of caprylic acid concentration. Protein A purification of caprylic acid precipitated cell culture fluid generated less turbid product pool with reduced levels of host cell proteins and high molecular weight aggregate. The results of this study show caprylic acid precipitation to be an effective purification method that can be incorporated into a production facility with minimal cost as it utilizes existing tanks and process flow. Eliminating flow through chromatography polishing step can provide process intensification by avoiding the process tank volume constraints for high titer processes.

  18. Chemical characteristics and sources of organic acids in precipitation at a semi-urban site in Southwest China

    NASA Astrophysics Data System (ADS)

    Zhang, Y. L.; Lee, X. Q.; Cao, F.

    2011-01-01

    In order to investigate the chemical characteristics and sources of organic acids in precipitation in Southwest China, 105 rainwater samples were collected at a semi-urban site in Anshun from June 2007 to June 2008. Organic acids and major anions were analyzed along with pH and electrical conductivity. The pH values varied from 3.57 to 7.09 for all the rainfall events sampled, with an average of 4.67 which was typical acidic value. Formic, acetic and oxalic acids were found to be the predominant carboxylic acids and their volume weighted average (VWA) concentrations were 8.77, 6.93 and 2.84 μmol l -1, respectively. These organic acids were estimated to account for 8.1% to the total free acidity (TFA) in precipitation. The concentrations of the majority organic acids at studied site had a clear seasonal pattern, reaching higher levels during the non-growing season than those in growing season, which was attributed to dilution effect of heavy rainfall during the growing season. The seasonal variation of wet deposition flux of these organic acids confirmed higher source strength of biogenic emissions from vegetation during the growing season. Formic-to-acetic acids ratio (F/A), an indicator of primary versus secondary sources of these organic acids, suggested that primary sources from vehicular emission, biomass burning, soil and vegetation emissions were dominant sources. In addition, the lowest concentrations of organic acids were found under type S, when air masses originated from the marine (South China Sea) during Southern Asian Monsoon period. And the highest concentrations were observed in precipitation events from Northeast China (type NE), prevailing mostly during winter with the lowest rainfall.

  19. Coupling meteorology, metal concentrations, and Pb isotopes for source attribution in archived precipitation samples.

    PubMed

    Graney, Joseph R; Landis, Matthew S

    2013-03-15

    A technique that couples lead (Pb) isotopes and multi-element concentrations with meteorological analysis was used to assess source contributions to precipitation samples at the Bondville, Illinois USA National Trends Network (NTN) site. Precipitation samples collected over a 16month period (July 1994-October 1995) at Bondville were parsed into six unique meteorological flow regimes using a minimum variance clustering technique on back trajectory endpoints. Pb isotope ratios and multi-element concentrations were measured using high resolution inductively coupled plasma-sector field mass spectrometry (ICP-SFMS) on the archived precipitation samples. Bondville is located in central Illinois, ~250km downwind from smelters in southeast Missouri. The Mississippi Valley Type ore deposits in Missouri provided a unique multi-element and Pb isotope fingerprint for smelter emissions which could be contrasted to industrial emissions from the Chicago and Indianapolis urban areas (~125km north and east, of Bondville respectively) and regional emissions from electric utility facilities. Differences in Pb isotopes and element concentrations in precipitation corresponded to flow regime. Industrial sources from urban areas, and thorogenic Pb from coal use, could be differentiated from smelter emissions from Missouri by coupling Pb isotopes with variations in element ratios and relative mass factors. Using a three endmember mixing model based on Pb isotope ratio differences, industrial processes in urban airsheds contributed 56±19%, smelters in southeast Missouri 26±13%, and coal combustion 18±7%, of the Pb in precipitation collected in Bondville in the mid-1990s.

  20. National Acid Precipitation Assessment Program: Acidic deposition: An inventory of non-Federal research, monitoring, and assessment information

    SciTech Connect

    Herrick, C.N.

    1990-01-01

    The Acid Precipitation Act of 1990 (Title VII of the Energy Security Act of 1980, P.L. 96-294) established the Interagency Task Force on Acid Precipitation to develop and implement the National Acid Precipitation Assessment Program (NAPAP). The information included in the document was provided to NAPAP's Task Group Leaders and State-of-Science and State-of-Technology authors in July 1989. The early release was intended to assure that the authors would be aware of the information at an early phase in the assessment production process.

  1. Preserving the distribution of inorganic arsenic species in groundwater and acid mine drainage samples

    USGS Publications Warehouse

    Bednar, A.J.; Garbarino, J.R.; Ranville, J.F.; Wildeman, T.R.

    2002-01-01

    The distribution of inorganic arsenic species must be preserved in the field to eliminate changes caused by metal oxyhydroxide precipitation, photochemical oxidation, and redox reactions. Arsenic species sorb to iron and manganese oxyhydroxide precipitates, and arsenite can be oxidized to arsenate by photolytically produced free radicals in many sample matrices. Several preservatives were evaluated to minimize metal oxyhydroxide precipitation, such as inorganic acids and ethylenediaminetetraacetic acid (EDTA). EDTA was found to work best for all sample matrices tested. Storing samples in opaque polyethylene bottles eliminated the effects of photochemical reactions. The preservation technique was tested on 71 groundwater and six acid mine drainage samples. Concentrations in groundwater samples reached 720 ??g-As/L for arsenite and 1080 ??g-As/L for arsenate, and acid mine drainage samples reached 13 000 ??g-As/L for arsenite and 3700 ??g-As/L for arsenate. The arsenic species distribution in the samples ranged from 0 to 90% arsenite. The stability of the preservation technique was established by comparing laboratory arsenic speciation results for samples preserved in the field to results for subsamples speciated onsite. Statistical analyses indicated that the difference between arsenite and arsenate concentrations for samples preserved with EDTA in opaque bottles and field speciation results were analytically insignificant. The percentage change in arsenite:arsenate ratios for a preserved acid mine drainage sample and groundwater sample during a 3-month period was -5 and +3%, respectively.

  2. DICARBOXYLIC ACID CONCENTRATION TRENDS AND SAMPLING ARTIFACTS

    EPA Science Inventory

    Dicarboxylic acids associated with airborne particulate matter were measured during a summer period in Philadelphia that included multiple air pollution episodes. Samples were collected for two ten hour periods each day using a high volume sampler with two quartz fiber filters in...

  3. Carbonate precipitation under bulk acidic conditions as a potential biosignature for searching life on Mars

    NASA Astrophysics Data System (ADS)

    Fernández-Remolar, David C.; Preston, Louisa J.; Sánchez-Román, Mónica; Izawa, Matthew R. M.; Huang, L.; Southam, Gordon; Banerjee, Neil R.; Osinski, Gordon R.; Flemming, Roberta; Gómez-Ortíz, David; Prieto Ballesteros, Olga; Rodríguez, Nuria; Amils, Ricardo; Darby Dyar, M.

    2012-10-01

    Recent observations of carbonate minerals in ancient Martian rocks have been interpreted as evidence for the former presence of circumneutral solutions optimal for carbonate precipitation. Sampling from surface and subsurface regions of the low-pH system of Río Tinto has shown, unexpectedly, that carbonates can form under diverse macroscopic physicochemical conditions ranging from very low to neutral pH (1.5-7.0). A multi-technique approach demonstrates that carbonate minerals are closely associated with microbial activity. Carbonates occur in the form of micron-size carbonate precipitates under bacterial biofilms, mineralization of subsurface colonies, and possible biogenic microstructures including globules, platelets and dumbbell morphologies. We propose that carbonate precipitation in the low-pH environment of Río Tinto is a process enabled by microbially-mediated neutralization driven by the reduction of ferric iron coupled to the oxidation of biomolecules in microbially-maintained circumneutral oases, where the local pH (at the scale of cells or cell colonies) can be much different than in the macroscopic environment. Acidic conditions were likely predominant in vast regions of Mars over the last four billion years of planetary evolution. Ancient Martian microbial life inhabiting low-pH environments could have precipitated carbonates similar to those observed at Río Tinto. Preservation of carbonates at Río Tinto over geologically significant timescales suggests that similarly-formed carbonate minerals could also be preserved on Mars. Such carbonates could soon be observed by the Mars Science Laboratory, and by future missions to the red planet.

  4. Acid-Base and Precipitation Equilibria in Wine

    ERIC Educational Resources Information Center

    Palma, Miguel; Barroso, Carmelo G.

    2004-01-01

    Experiments are performed to establish the changes of pH during the precipitation of potassium hydrogen tartrate, with its unfavorable impact on the stability of wine. Students, thus, obtain a clearer understanding of the interplay between a variety of chemical equilibria within a single medium.

  5. Cloud microphysical properties of convective clouds sampled during the Convective Precipitation Experiment (COPE) experiment.

    NASA Astrophysics Data System (ADS)

    Jackson, R.; French, J.; Leon, D.; Plummer, D. M.; Lasher-Trapp, S.; Blyth, A. M.

    2015-12-01

    The COnvective Precipitation Experiment (COPE), occurring in the southwest UK during Summer 2013, was motivated to improve quantitative precipitation forecasting, in part, with the aim to increase understanding of the warm and cold precipitation processes that can produce heavy convective rainfall in the southwest UK. In particular, we examine the creation of graupel embryos, the Hallett-Mossop process, and the effect of entrainment on these processes. To characterize the evolution of cloud microphysical properties of maturing thunderstorms, the University of Wyoming King Air sampled the tops of fresh turrets between -15 and 0. Data sampled by the Cloud Droplet Probe, Cloud Imaging grayscale Probe (CIP-Grey) and 2D Precipitation Probe during four missions are examined. Here we characterize the variability of the cloud liquid and ice particle size distributions and liquid water contents (LWC) inside updraft cores, as a function of temperature, T, and vertical velocity, w. On one of the days, the number concentration of particles with maximum dimension D > 300 μm, N>300, was less than 1 L-1, with very few ice hydrometeors observed. However, on the other missions, N>300 ranged from 1 L-1 to 250 L-1. The CIP-Grey detected liquid drops at T > -5 and a mixture of graupel and rimed columns at T < -5 for these missions, consistent with the warm rain process providing the frozen drops necessary to form graupel embryos that initiate secondary production. In general, LWC relative to adiabatic decreased from 0.75 to 0.2 with height and was lowest when N>300 > 1 L-1, consistent with precipitation growth by collision-coalescence and accretion. Finally, ice precipitation was primarily present at w < 7 m s-1 and greatest when w < 3 m s-1, suggesting that w influences the number of ice particles generated in the updraft cores sampled during COPE-MED.

  6. Selective removal of keratan sulfate in chondroitin sulfate samples by sequential precipitation with ethanol.

    PubMed

    Galeotti, Fabio; Maccari, Francesca; Volpi, Nicola

    2014-03-01

    Keratan sulfate (KS) is present as a contaminant in chondroitin sulfate (CS) mainly extracted from shark cartilage. We report a selective removal procedure of KS in CS samples by means of sequential precipitation with ethanol. Purified shark CS containing approximately 10% to 15% KS was subjected to a precipitation procedure in the presence of increasing percentages of saturated ethanol. In contrast to other solvents, 1.0 volume of ethanol was able to selectively purify CS, with a purity of approximately 100%, from KS. The current selective and simple procedure appears to be a reliable industrial preparation of CS devoid of large amounts of the residual KS.

  7. Determination of trifluoroacetic acid in 1996--1997 precipitation and surface waters in California and Nevada

    SciTech Connect

    Wujcik, C.E.; Cahill, T.M.; Seiber, J.N.

    1999-05-15

    The atmospheric degradation of three chlorofluorocarbon (CFC) replacement compounds, namely HFC-134a, HCFC-123, and HCFC-124, results in the formation of trifluoroacetic acid (TFA). Concentrations of TFA were determined in precipitation and surface water samples collected in California and Nevada during 1996--1997. Terminal lake systems were found to have concentrations 4--13 times higher than their calculated yearly inputs, providing evidence for accumulation. The results support dry deposition as the primary contributor of TFA to surface waters in arid and semiarid environments. Precipitation samples obtained from three different locations contained 20.7--1530 ng/L with significantly higher concentrations in fogwater over rainwater. Elevated levels of TFA were observed for rainwater collected in Nevada over those collected in California, indicating continual uptake and concentration as clouds move from a semiarid to arid climate. Thus several mechanisms exist, including evaporative concentration, vapor-liquid phase partitioning, lowered washout volumes of atmospheric deposition water, and dry deposition, which may lead to elevated concentrations of TFA in atmospheric and surface waters above levels expected from usual rainfall washout.

  8. Compositions and method for controlling precipitation when acidizing sour wells

    SciTech Connect

    Dill, W.R.; Walker, M.L.

    1990-08-21

    This patent describes a method of treating a sour well penetrating a subterranean formation. It comprises: introducing into the well a treating fluid comprising an acid solution having a pH below 1.9, an iron sequestering agent comprising at least one compound selected from the group consisting of aminopolycarboxylic acids, hydroxycarboxylic acids, cyclic polyethers and derivatives of the acids and ethers, present in an amount of from about 0.25 to about 5 percent by weight of the acid solution, and a sulfide modifier comprising at least one compound selected from the group consisting of an aldehyde, acetal, hemiacetal and any other compound capable of forming aldehydes in the acid solution, present in an amount of from about 0.25 to about 5 percent of the acid solution; and treating the subterranean formation with the treating fluid.

  9. [Low molecular weight carboxylic acids in precipitation during the rainy season in the rural area of Anshun, West Guizhou Province].

    PubMed

    Zhang, Yan-Lin; Lee, Xin-Qing; Huang, Dai-Kuan; Huang, Rong-Sheng; Jiang, Wei

    2009-03-15

    40 rainwater samples were collected at Anshun from June 2007 to October 2007 and analysed in terms of pH values, electrical conductivity, major inorganic anions and soluble low molecular weight carboxylic acids. The results showed that pH of individual precipitation events ranged from 3.57-7.09 and the volume weight mean pH value was 4.57. The most abundant carboxylic acids were acetic (volume weight mean concentration 6.75 micromol x L(-1)) and formic (4.61 micromol x L(-1)) followed by oxalic (2.05 micromol x L(-1)). The concentration levels for these three species during summer especially June and July were comparatively high; it implied that organic acids in Anshun may came primarily from emissions from growing vegetations or products of the photochemical reactions of unsaturated hydrocarbons. Carboxylic acids were estimated to account for 32.2% to the free acidity in precipitation. The contribution was higher than in Guiyang rainwater, which indicated contamination by industry in Guiyang was more than in Anshun. The remarkable correlation(p = 0.01) between formic acid and acetic acid suggest that they have similar sources or similar intensity but different sources. And the remarkable correlation (p = 0.01) between and formic acid and oxalic acid showed that the precursors of oxalic acid and formic acid had similar sources. During this period, the overall wet deposition of carboxylic acids were 2.10 mmol/m2. And it appeared mainly in the summer, during which both concentration and contribution to free acidity were also relatively high. Consequently, it was necessary to control emission of organic acids in the summer to reduce frequence of acid rain in Anshun.

  10. Organic toxicants in air and precipitation samples from the Lake Michigan area

    SciTech Connect

    Harlin, K.S.; Sweet, C.W.; Gatz, D.F.

    1995-12-31

    Measurements of PCBs, organochlorine insecticides, PAHs, and atrazine were made in air and precipitation samples collected at regionally-representative locations near Lake Michigan from 1992-1995. The purpose of these measurements was to provide information needed to estimate the atmospheric deposition of organic toxicants to Lake Michigan. Twenty-four hour samples of airborne particles and vapor were collected at 12-day intervals on quartz fiber filters and XAD-2 resin vapor traps using modified high volume sampleers. Twenty-eight day precipitation samples were collected using wet-only samplers with stainless steel sampling surfaces and heated enclosure containing an XAD-2 resin adsorption column. Samples were Soxhlet extracted for 24 hours with hexane:acetone (1:1), and concentrated by rotary evaporation. Interferences were removed and the samples separated into analyte groups by silica gel chromatography. Four fractions were collected for GC-ECD and GC-Ion Trap MS analyses. Ten pesticides, 101 PCB congeners, 18 PAHs, and atrazine were measured in all samples. Quality assurance was maintained by including field duplicate samples, field blanks, alboratory matrix spikes, laboratory matrix blanks, and laboratory surrogate spikes in the sampling/analytical protocols. Preliminary results from urban and remote sites show geographical variations in the concentrations of some toxicants due to contributions from local sources. For all sites the total PCB levels are higher in the vapor phase than the particulate phase and show strong seasonal variations. Seasonal variations were also observed for several pesticides.

  11. An In Situ Method for Sizing Insoluble Residues in Precipitation and Other Aqueous Samples.

    PubMed

    Axson, Jessica L; Creamean, Jessie M; Bondy, Amy L; Capracotta, Sonja S; Warner, Katy Y; Ault, Andrew P

    2015-01-01

    Particles are frequently incorporated into clouds or precipitation, influencing climate by acting as cloud condensation or ice nuclei, taking up coatings during cloud processing, and removing species through wet deposition. Many of these particles, particularly ice nuclei, can remain suspended within cloud droplets/crystals as insoluble residues. While previous studies have measured the soluble or bulk mass of species within clouds and precipitation, no studies to date have determined the number concentration and size distribution of insoluble residues in precipitation or cloud water using in situ methods. Herein, for the first time we demonstrate that Nanoparticle Tracking Analysis (NTA) is a powerful in situ method for determining the total number concentration, number size distribution, and surface area distribution of insoluble residues in precipitation, both of rain and melted snow. The method uses 500 μL or less of liquid sample and does not require sample modification. Number concentrations for the insoluble residues in aqueous precipitation samples ranged from 2.0-3.0(±0.3)×10(8) particles cm(-3), while surface area ranged from 1.8(±0.7)-3.2(±1.0)×10(7) μm(2) cm(-3). Number size distributions peaked between 133-150 nm, with both single and multi-modal character, while surface area distributions peaked between 173-270 nm. Comparison with electron microscopy of particles up to 10 μm show that, by number, > 97% residues are <1 μm in diameter, the upper limit of the NTA. The range of concentration and distribution properties indicates that insoluble residue properties vary with ambient aerosol concentrations, cloud microphysics, and meteorological dynamics. NTA has great potential for studying the role that insoluble residues play in critical atmospheric processes.

  12. An In Situ Method for Sizing Insoluble Residues in Precipitation and Other Aqueous Samples

    PubMed Central

    Axson, Jessica L.; Creamean, Jessie M.; Bondy, Amy L.; Capracotta, Sonja S.; Warner, Katy Y.; Ault, Andrew P.

    2015-01-01

    Particles are frequently incorporated into clouds or precipitation, influencing climate by acting as cloud condensation or ice nuclei, taking up coatings during cloud processing, and removing species through wet deposition. Many of these particles, particularly ice nuclei, can remain suspended within cloud droplets/crystals as insoluble residues. While previous studies have measured the soluble or bulk mass of species within clouds and precipitation, no studies to date have determined the number concentration and size distribution of insoluble residues in precipitation or cloud water using in situ methods. Herein, for the first time we demonstrate that Nanoparticle Tracking Analysis (NTA) is a powerful in situ method for determining the total number concentration, number size distribution, and surface area distribution of insoluble residues in precipitation, both of rain and melted snow. The method uses 500 μL or less of liquid sample and does not require sample modification. Number concentrations for the insoluble residues in aqueous precipitation samples ranged from 2.0–3.0(±0.3)×108 particles cm−3, while surface area ranged from 1.8(±0.7)–3.2(±1.0)×107 μm2 cm−3. Number size distributions peaked between 133–150 nm, with both single and multi-modal character, while surface area distributions peaked between 173–270 nm. Comparison with electron microscopy of particles up to 10 μm show that, by number, > 97% residues are <1 μm in diameter, the upper limit of the NTA. The range of concentration and distribution properties indicates that insoluble residue properties vary with ambient aerosol concentrations, cloud microphysics, and meteorological dynamics. NTA has great potential for studying the role that insoluble residues play in critical atmospheric processes. PMID:25705069

  13. Baseline Acidity of Ancient Precipitation from the South Pole,

    DTIC Science & Technology

    1984-06-01

    post-depositional diffusion of ait ferences ( Langway et al. 1975). The first three through the firn was contributing significantly to the measured...C.C. Langway , the Canadian high Arctic. Nature, 295: 137-140. Jr. (1975) Chemistry of 700 years of precipitation Kolthoff, i.M., E.B.Sandell...sis. London: Macmillian Company, p. 55. port 341. ADA 014970. Kuivinen, K.C., B.R. Koci, G.W. Holdsworth Cragin, J.H., M.M. Herron, C.C. Langway , Jr

  14. Considerations of an air-quality standard to protect terrestrial vegetation from acidic precipitation

    SciTech Connect

    Evans, L.S.

    1981-01-01

    Studies on the effects of acidic precipitation which is here defined as wet or frozen deposition with a hydrogen ion concentration greater than 2.5 ..mu..eq 1/sup -1/, are reviewed. At the present time there is an inadequate amount of information that shows decreases in crop growth except for one field study. Most studies with plants (crops and forests) are inadequate for standard setting because they are not conducted in the field with adequate randomization of plots coupled with rigorous statistical analyses. Although visible injury to foliage has been documented in a variety of greenhouse studies, no experimental evidence demonstrates loss of field crop value or reduction in plant productivity due to visible foliar injury. Acidic precipitation can contribute nutrients to vegetation and could also influence leaching rates of nutrients from vegetation. Although these processes occur, there are no data that show changes in nutrient levels in foliage that relate to crop or natural ecosystem productivity. Experimental results show that fertilization of ferns is inhibited by current levels of acidic precipitation in the northeastern United States. However, the overall impacts of inhibited fertilization on perpetuation of the species or ecosystem productivity have not been evaluated. Simulated acidic precipitation has been shown to effect plant pathogens in greenhouse and field experiments. Simulated acidic precipitation inhibited pathogen activities under some circumstances and promoted pathogen activities under other circumstances. No conclusion can be drawn about the effects of current levels of precipitation acidity on plant pathogen-host interactions. From these data it must be concluded that research on the effects of acidic precipitation on terrestrial vegetation is too meager to draw any conclusions with regard to an air quality standard.

  15. Acid Precipitation Learning Materials: Science, Environmental and Social Studies, Grades 6-12.

    ERIC Educational Resources Information Center

    Hessler, Edward W.

    The major environmental problem of acid precipition is addressed through a series of activities contained in this guide for teachers of grades 6 through 12. Exercises are provided to help students learn science inquiry skills, facts, and concepts while focusing on the acid rain situation. Activities are organized by content areas. These include:…

  16. [Study on solid dispersion of precipitated calcium carbonate-based oleanolic acid].

    PubMed

    Yan, Hong-mei; Zhang, Zhen-hai; Jia, Xiao-bin; Jiang, Yan-rong; Sun, E

    2015-05-01

    Oleanolic acid-precipitated calcium carbonate solid dispersion was prepared by using solvent evaporation method. The microscopic structure and physicochemical properties of solid dispersion were analyzed using differential scanning calorimetry and scanning electron microscopy (SEM). And its in vitro release also was investigated. The properties of the precipitated calcium carbonate was studied which was as a carrier of oleanolic acid solid dispersion. Differential scanning calorimetry analysis suggested that oleanolic acid may be present in solid dispersion as amorphous substance. The in vitro release determination results of oleanolic acid-precipitated calcium carbonate (1: 5) solid dispersion showed accumulated dissolution rate of.oleanolic acid was up to 90% at 45 min. Accelerating experiment showed that content and in vitro dissolution of oleanolic acid solid dispersion did not change after storing over 6 months. The results indicated that in vitro dissolution of oleanolic acid was improved greatly by the solid dispersion with precipitated calcium carbonate as a carrier. The solid dispersion is a stabilizing system which has actual applied value.

  17. Selective precipitation of ribonucleic acid from a mixture of total cellular nucleic acids extracted from cultured mammalian cells

    PubMed Central

    Harrison, P. R.

    1971-01-01

    A simple and reproducible method is described for precipitating RNA selectively from total mammalian-cell nucleic acids extracted by the phenol–sodium dodecyl sulphate procedure at pH8.0. Under specified conditions bulk RNA is precipitated almost quantitatively whereas bulk DNA remains in solution. Minor components of RNA (detected by pulse-labelling and chromatography on methylated albumin–kieselguhr) and rapidly labelled components of DNA containing single-stranded regions are also precipitated. The usefulness of the method is discussed in the context of isolating separately both RNA and DNA from cultured cells that are difficult to obtain in quantity. PMID:5165620

  18. A fully automated plasma protein precipitation sample preparation method for LC-MS/MS bioanalysis.

    PubMed

    Ma, Ji; Shi, Jianxia; Le, Hoa; Cho, Robert; Huang, Judy Chi-jou; Miao, Shichang; Wong, Bradley K

    2008-02-01

    This report describes the development and validation of a robust robotic system that fully integrates all peripheral devices needed for the automated preparation of plasma samples by protein precipitation. The liquid handling system consisted of a Tecan Freedom EVO 200 liquid handling platform equipped with an 8-channel liquid handling arm, two robotic plate-handling arms, and two plate shakers. Important additional components integrated into the platform were a robotic temperature-controlled centrifuge, a plate sealer, and a plate seal piercing station. These enabled unattended operation starting from a stock solution of the test compound, a set of test plasma samples and associated reagents. The stock solution of the test compound was used to prepare plasma calibration and quality control samples. Once calibration and quality control samples were prepared, precipitation of plasma proteins was achieved by addition of three volumes of acetonitrile. Integration of the peripheral devices allowed automated sequential completion of the centrifugation, plate sealing, piercing and supernatant transferral steps. The method produced a sealed, injection-ready 96-well plate of plasma extracts. Accuracy and precision of the automated system were satisfactory for the intended use: intra-day and the inter-day precision were excellent (C.V.<5%), while the intra-day and inter-day accuracies were acceptable (relative error<8%). The flexibility of the platform was sufficient to accommodate pharmacokinetic studies of different numbers of animals and time points. To the best of our knowledge, this represents the first complete automation of the protein precipitation method for plasma sample analysis.

  19. CHARACTERIZATION OF A PRECIPITATE REACTOR FEED TANK (PRFT) SAMPLE FROM THE DEFENSE WASTE PROCESSING FACILITY (DWPF)

    SciTech Connect

    Crawford, C.; Bannochie, C.

    2014-05-12

    A sample of from the Defense Waste Processing Facility (DWPF) Precipitate Reactor Feed Tank (PRFT) was pulled and sent to the Savannah River National Laboratory (SRNL) in June of 2013. The PRFT in DWPF receives Actinide Removal Process (ARP)/ Monosodium Titanate (MST) material from the 512-S Facility via the 511-S Facility. This 2.2 L sample was to be used in small-scale DWPF chemical process cell testing in the Shielded Cells Facility of SRNL. A 1L sub-sample portion was characterized to determine the physical properties such as weight percent solids, density, particle size distribution and crystalline phase identification. Further chemical analysis of the PRFT filtrate and dissolved slurry included metals and anions as well as carbon and base analysis. This technical report describes the characterization and analysis of the PRFT sample from DWPF. At SRNL, the 2.2 L PRFT sample was composited from eleven separate samples received from DWPF. The visible solids were observed to be relatively quick settling which allowed for the rinsing of the original shipping vials with PRFT supernate on the same day as compositing. Most analyses were performed in triplicate except for particle size distribution (PSD), X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and thermogravimetric analysis (TGA). PRFT slurry samples were dissolved using a mixed HNO3/HF acid for subsequent Inductively Coupled Plasma Atomic Emission Spectroscopy (ICPAES) and Inductively Coupled Plasma Mass Spectroscopy (ICP-MS) analyses performed by SRNL Analytical Development (AD). Per the task request for this work, analysis of the PRFT slurry and filtrate for metals, anions, carbon and base were primarily performed to support the planned chemical process cell testing and to provide additional component concentrations in addition to the limited data available from DWPF. Analysis of the insoluble solids portion of the PRFT slurry was aimed at detailed characterization of these solids (TGA, PSD

  20. Selenium speciation in acidic environmental samples: application to acid rain-soil interaction at Mount Etna volcano.

    PubMed

    Floor, Geerke H; Iglesías, Mònica; Román-Ross, Gabriela; Corvini, Philippe F X; Lenz, Markus

    2011-09-01

    Speciation plays a crucial role in elemental mobility. However, trace level selenium (Se) speciation analyses in aqueous samples from acidic environments are hampered due to adsorption of the analytes (i.e. selenate, selenite) on precipitates. Such solid phases can form during pH adaptation up till now necessary for chromatographic separation. Thermodynamic calculations in this study predicted that a pH<4 is needed to prevent precipitation of Al and Fe phases. Therefore, a speciation method with a low pH eluent that matches the natural sample pH of acid rain-soil interaction samples from Etna volcano was developed. With a mobile phase containing 20mM ammonium citrate at pH 3, selenate and selenite could be separated in different acidic media (spiked water, rain, soil leachates) in <10 min with a LOQ of 0.2 μg L(-1) using (78)Se for detection. Applying this speciation analysis to study acid rain-soil interaction using synthetic rain based on H(2)SO(4) and soil samples collected at the flanks of Etna volcano demonstrated the dominance of selenate over selenite in leachates from samples collected close to the volcanic craters. This suggests that competitive behavior with sulfate present in acid rain might be a key factor in Se mobilization. The developed speciation method can significantly contribute to understand Se cycling in acidic, Al/Fe rich environments.

  1. Evaluation of sampling errors of precipitation from spaceborne and ground sensors

    NASA Technical Reports Server (NTRS)

    Graves, Charles E.; Valdes, Juan B.; Shen, Samuel S. P.; North, Gerald R.

    1993-01-01

    The spatial and temporal characteristics of rainfall over Oklahoma and Kansas are analyzed using the raingage data collected during the Preliminary Regional Experiment for STORM-Central (PRE-STORM). The spectra obtained are compared with those obtained from the oceanic precipitation in the GARP and with that obtained from analyzing raingage records in east Texas. In addition, the spectra are used to evaluate the sampling errors that are due to the spatial gaps in measurements. It was found that the temporal spectra from PRE-STORM had a spectral shape similar to that obtained in GARP, except that the tail of the PRE-STORM spectra has a lower slope than in GARP spectra, suggesting that the largest difference between tropical oceanic rainfall and convective land precipitation is at the highest frequencies.

  2. Bias correction of EU-ENSEMBLES precipitation data with focus on the effect of sample size

    NASA Astrophysics Data System (ADS)

    Reiter, Philipp; Gutjahr, Oliver; Schefczyk, Lukas; Heinemann, Günther; Casper, Markus C.

    2015-04-01

    The precipitation output of climate models often shows a bias when compared to observed data, so that a bias correction is necessary before using it as climate forcing in impact modeling. We expect the performance of the bias correction to strongly depend on the sample size used for its calibration. This raises the question: how long does a time series need to be to achieve a sufficient bias correction? We carry out experiments using 40 years of daily precipitation data from 10 regional climate models (RCM) of the EU-ENSEMBLES project, splitting them into a 30 year calibration period and a 10 year validation period. The RCM data are bias corrected using decreasing sample sizes out of the calibration period. By applying skill scores we quantify the critical sample size ncrit, at which the quality of the bias correction becomes statistically worse compared to the correction based on 30 years. In order to analyze whether the effect of the sample size depends on the chosen correction method and the calibration period, we applied four variations of the quantile matching (QM) approach and 3 different calibration/validation periods in this study. The results show that the spread of ncrit is large, ranging from 28 years to approximately 10 years. This indicates that even a small decrease in sample size for the calibration can result in a statistical significant degradation of the bias correction. Corrections with sample sizes smaller than 10 years always perform significantly worse than the 'best fit' with 30 years. The chosen QM approach influences ncrit in dependence of its degrees of freedom: the higher the degrees of freedom the larger ncrit. We also found that the choice of the calibration period affects the ncrit values. In conclusion we recommend to use time series as long as possible for bias correction of precipitation data. However, there is a large transition zone of the critical sample size where shorter time series can perform sufficiently well, depending on

  3. Reuse of washing effluent containing oxalic acid by a combined precipitation-acidification process.

    PubMed

    Lim, Mihee; Kim, Myoung-Jin

    2013-01-01

    This study aims at evaluating the reuse feasibility of effluent produced by the soil washing of mine tailings with oxalic acid. Alkaline chemicals such as NaOH, Ca(OH)(2), and Na(2)CO(3) are used for the precipitation of arsenic and heavy metals in the effluent containing oxalic acid. All of the target contaminants are removed with very high efficiency (up to 100%) at high pH. The precipitation using NaOH at pH 9 is determined to be the most cost-effective method for the removal of arsenic as well as heavy metals in the effluent. The effluent decontaminated by NaOH is consecutively reused for the soil washing of raw mine tailings, resulting in considerable efficiency. Furthermore, even more arsenic and heavy metals are extracted from raw mine tailings by acidifying the decontaminated effluent under the alkaline condition, compared with direct reuse of the decontaminated effluent. Here, the oxalic acid, which is a weak complex-forming ligand as well as a weak acid, has noticeable effects on both soil washing and effluent treatment by precipitation. It extracts efficiently the contaminants from the mine tailings without adverse change of soil and also makes possible the precipitation of the contaminants in the effluent unlike strong chelating reagent. Reuse of the washing effluent containing oxalic acid would make the existing soil washing process more environment-friendly and cost-effective.

  4. Chemical Data for Rock, Sediment, Biological, Precipitate, and Water Samples from Abandoned Copper Mines in Prince William Sound, Alaska

    USGS Publications Warehouse

    Koski, Randolph A.; Munk, LeeAnn

    2007-01-01

    In the early 20th century, approximately 6 million metric tons of copper ore were mined from numerous deposits located along the shorelines of fjords and islands in Prince William Sound, Alaska. At the Beatson, Ellamar, and Threeman mine sites (fig. 1), rocks containing Fe, Cu, Zn, and Pb sulfide minerals are exposed to chemical weathering in abandoned mine workings and remnant waste piles that extend into the littoral zone. Field investigations in 2003 and 2005 as well as analytical data for rock, sediment, precipitate, water, and biological samples reveal that the oxidation of sulfides at these sites is resulting in the generation of acid mine drainage and the transport of metals into the marine environment (Koski and others, 2008; Stillings and others, 2008). At the Ellamar and Threeman sites, plumes of acidic and metal-enriched water are flowing through beach gravels into the shallow offshore environment. Interstitial water samples collected from beach sediment at Ellamar have low pH levels (to ~3) and high concentrations of metals including iron, copper, zinc, cobalt, lead, and mercury. The abundant precipitation of the iron sulfate mineral jarosite in the Ellamar gravels also signifies a low-pH environment. At the Beatson mine site (the largest copper mine in the region) seeps containing iron-rich microbial precipitates drain into the intertidal zone below mine dumps (Foster and others, 2008). A stream flowing down to the shoreline from underground mine workings at Beatson has near-neutral pH, but elevated levels of zinc, copper, and lead (Stillings and others, 2008). Offshore sediment samples at Beatson are enriched in these metals. Preliminary chemical data for tissue from marine mussels collected near the Ellamar, Threeman, and Beatson sites reveal elevated levels of copper, zinc, and lead compared to tissue in mussels from other locations in Prince William Sound (Koski and others, 2008). Three papers presenting results of this ongoing investigation of

  5. Chemical Data for Rock, Sediment, Biological, Precipitate, and Water Samples from Abandoned Copper Mines in Prince William Sound, Alaska

    USGS Publications Warehouse

    Koski, Randolph A.; Munk, LeeAnn

    2007-01-01

    Introduction In the early 20th century, approximately 6 million metric tons of copper ore were mined from numerous deposits located along the shorelines of fjords and islands in Prince William Sound, Alaska. At the Beatson, Ellamar, and Threeman mine sites (fig. 1), rocks containing Fe, Cu, Zn, and Pb sulfide minerals are exposed to chemical weathering in abandoned mine workings and remnant waste piles that extend into the littoral zone. Field investigations in 2003 and 2005 as well as analytical data for rock, sediment, precipitate, water, and biological samples reveal that the oxidation of sulfides at these sites is resulting in the generation of acid mine drainage and the transport of metals into the marine environment (Koski and others, 2008; Stillings and others, 2008). At the Ellamar and Threeman sites, plumes of acidic and metal-enriched water are flowing through beach gravels into the shallow offshore environment. Interstitial water samples collected from beach sediment at Ellamar have low pH levels (to ~3) and high concentrations of metals including iron, copper, zinc, cobalt, lead, and mercury. The abundant precipitation of the iron sulfate mineral jarosite in the Ellamar gravels also signifies a low-pH environment. At the Beatson mine site (the largest copper mine in the region) seeps containing iron-rich microbial precipitates drain into the intertidal zone below mine dumps (Foster and others, 2008). A stream flowing down to the shoreline from underground mine workings at Beatson has near-neutral pH, but elevated levels of zinc, copper, and lead (Stillings and others, 2008). Offshore sediment samples at Beatson are enriched in these metals. Preliminary chemical data for tissue from marine mussels collected near the Ellamar, Threeman, and Beatson sites reveal elevated levels of copper, zinc, and lead compared to tissue in mussels from other locations in Prince William Sound (Koski and others, 2008). Three papers presenting results of this ongoing

  6. Stable isotope analysis of precipitation samples obtained via crowdsourcing reveals the spatiotemporal evolution of Superstorm Sandy.

    PubMed

    Good, Stephen P; Mallia, Derek V; Lin, John C; Bowen, Gabriel J

    2014-01-01

    Extra-tropical cyclones, such as 2012 Superstorm Sandy, pose a significant climatic threat to the northeastern United Sates, yet prediction of hydrologic and thermodynamic processes within such systems is complicated by their interaction with mid-latitude water patterns as they move poleward. Fortunately, the evolution of these systems is also recorded in the stable isotope ratios of storm-associated precipitation and water vapor, and isotopic analysis provides constraints on difficult-to-observe cyclone dynamics. During Superstorm Sandy, a unique crowdsourced approach enabled 685 precipitation samples to be obtained for oxygen and hydrogen isotopic analysis, constituting the largest isotopic sampling of a synoptic-scale system to date. Isotopically, these waters span an enormous range of values (> 21‰ for δ(18)O, > 160‰ for δ(2)H) and exhibit strong spatiotemporal structure. Low isotope ratios occurred predominantly in the west and south quadrants of the storm, indicating robust isotopic distillation that tracked the intensity of the storm's warm core. Elevated values of deuterium-excess (> 25‰) were found primarily in the New England region after Sandy made landfall. Isotope mass balance calculations and Lagrangian back-trajectory analysis suggest that these samples reflect the moistening of dry continental air entrained from a mid-latitude trough. These results demonstrate the power of rapid-response isotope monitoring to elucidate the structure and dynamics of water cycling within synoptic-scale systems and improve our understanding of storm evolution, hydroclimatological impacts, and paleo-storm proxies.

  7. Cloning and characterization of four novel coral acid-rich proteins that precipitate carbonates in vitro.

    PubMed

    Mass, Tali; Drake, Jeana L; Haramaty, Liti; Kim, J Dongun; Zelzion, Ehud; Bhattacharya, Debashish; Falkowski, Paul G

    2013-06-17

    Biomineralization is a widely dispersed and highly regulated but poorly understood process by which organisms precipitate minerals from a wide variety of elements [1]. For many years, it has been hypothesized that the biological precipitation of carbonates is catalyzed by and organized on an extracellular organic matrix containing a suite of proteins, lipids, and polysaccharides [2, 3]. The structures of these molecules, their evolutionary history, and the biophysical mechanisms responsible for calcification remain enigmatic. Despite the recognition that mineralized tissues contain proteins that are unusually rich in aspartic and glutamic acids [4-6], the role of these proteins in biomineralization remains elusive [5, 6]. Here we report, for the first time, the identification, cloning, amino acid sequence, and characterization of four highly acidic proteins, derived from expression of genes obtained from the common stony coral, Stylophora pistillata. Each of these four proteins can spontaneously catalyze the precipitation of calcium carbonate in vitro. Our results demonstrate that coral acid-rich proteins (CARPs) not only bind Ca(2+) stoichiometrically but also precipitate aragonite in vitro in seawater at pH 8.2 and 7.6, via an electrostatic interaction with protons on bicarbonate anions. Phylogenetic analysis suggests that at least one of the CARPs arose from a gene fusion. Similar, highly acidic proteins appear to have evolved several times independently in metazoans through convergence. Based purely on thermodynamic grounds, the predicted change in surface ocean pH in the next decades would appear to have minimal effect on the capacity of these acid-rich proteins to precipitate carbonates.

  8. IMPROVEMENT UPON THE CARRIER PRECIPITATION OF PLUTONIUM IONS FROM NITRIC ACID SOLUTIONS

    DOEpatents

    James, R.A.; Thompson, S.G.

    1958-12-23

    A process is reported for improving the removal of plutonlum by carrier precipitation by the addition of nitrite ions to a nitrlc acid solutlon of neutronirradiated unanium so as to destroy any hydrazine that may be present in the solution since the hydrazine tends to complex the tetravalent plutonium and prevents removal by the carrier precipltate, such as bismuth phospbate.

  9. The Contribution Of Sampling Errors In Satellite Precipitation Estimates To High Flood Uncertainty In Subtropical South America

    NASA Astrophysics Data System (ADS)

    Demaria, E. M.; Valdes, J. B.; Nijssen, B.; Rodriguez, D.; Su, F.

    2009-12-01

    Satellite precipitation estimates are becoming increasingly available at temporal and spatial scales of interest for hydrological applications. Unfortunately precipitation estimated from global satellites is prone to errors hailing from different sources. The impact of sampling errors on the hydrological cycle of a large-size basin was assessed with a macroscale hydrological model. Synthetic precipitation fields were generated in a Monte Carlo fashion by perturbing observed precipitation fields with sampling errors. Three sampling intervals were chosen to generate the precipitation fields: one-hour, three-hours which is the canonical Global Precipitation Mission (GPM) sampling interval, and six-hours. The Variable Infiltration Capacity (VIC) model was used to assess the impact of sampling errors on hydrological fluxes and states in the Iguazu basin in South America for the period 1982-2005. The propagation of sampling errors through the hydrological cycle was evaluated for high flow events that have the 2% chance of being exceeded in any given time. Results show that observed event volumes are underestimated for small volumes for the three and six-hours sampling intervals but for the one-hour sampling interval the difference is almost negligible.The timing of the hydrograph is not affected by uncertainty existent in satellite-derived precipitation when it propagates through the hydrological cycle. Results of two non-parametric tests: the Kruskal-Wallis test on the mean ranks of the population and the Ansari-Bradley test on the equality of the variances indicate that sampling errors do no affect the occurrence of high flows since their probability distribution is not affected. The applicability of these results is limited to a humid climate. However the Iguazu basin is representative of several basins located in subtropical regions around the world, many of which are under-instrumented catchments, where satellite precipitation might be one of the few available data

  10. Organic acids in precipitation in the Basque country (North of Spain)

    NASA Astrophysics Data System (ADS)

    Durana, N.; Casado, H.; García, C.; Ezcurra, A.; Lacaux, J. P.; Encinas, D.

    This paper discusses the results of the measurement of organic anions in precipitation collected since July 1989 in Olaeta, a rural village in the Basque Country (North of Spain). In order to gain a deeper knowledge of the characteristics and acids responsible for the free acidity observed in precipitation, a study was started within the EPOCA programme (Estudios en el Pirineo Occidental de la Contaminación Acida), for measuring organic anions: formiate, acetate and propionate. These results show that it was possible to observe organic anions in nearly every event, with a 5% contribution to the anionic total, and with an appreciable seasonal variation in concentration. The maximum contribution of organic acids to free acidity (H +) is 6% in rain events with pH≤5.0. There is significant correlation between acetic acid and inorganic ions of marine origin Cl -, Na + and Mg 2+ which might indicate the importance which the air masses of marine origin are going to have in the concentration of this acid. There is also significant correlation between formic acid and SO 42- and H + ions which might indicate the relatively importance contribution of formic acid to free acidity.

  11. Optimal Concentration of 2,2,2-Trichloroacetic Acid for Protein Precipitation Based on Response Surface Methodology

    PubMed Central

    Ngo, Albert N; Ezoulin, Miezan JM; Youm, Ibrahima; Youan, Bi-Botti C

    2014-01-01

    For low protein concentrations containing biological samples (in proteomics) and for non proteinaceous compound assays (in bioanalysis), there is a critical need for a simple, fast, and cost-effective protein enrichment or precipitation method. However, 2,2,2-trichloroacetic acid (TCA) is traditionally used for protein precipitation at ineffective concentrations for very low protein containing samples. It is hypothesized that response surface methodology, can be used to systematically identify the optimal TCA concentration for protein precipitation in a wider concentration range. To test this hypothesis, a central composite design is used to assess the effects of two factors (X1 = volume of aqueous solution of protein, and X2 = volume of TCA solution 6.1N) on the optical absorbance of the supernatant (Y1), and the percentage of protein precipitated (Y2). Using either bovine serum albumin (BSA) as a model protein or human urine (with 20 ppm protein content), 4% w/v (a saddle point) is the optimal concentration of the TCA solution for protein precipitation that is visualized by SDS-PAGE analysis. At this optimal concentration, the Y2-values range from 76.26 to 92.67% w/w for 0.016 to 2 mg/mL of BSA solution. It is also useful for protein enrichment and xenobiotic analysis in protein-free supernatant as applied to tenofovir (a model HIV microbicide). In these conditions, the limit of detection and limit of quantitation of tenofovir are respectively 0.0014 mg/mL and 0.0042 mg/mL. This optimal concentration of TCA provides optimal condition for protein purification and analysis of any xenobiotic compound like tenofovir. PMID:25750762

  12. Acid precipitation and drinking water quality in the eastern United States. Final report, November 1981-January 1984

    SciTech Connect

    Taylor, F.; Taylor, J.A.; Symons, G.E.; Collins, J.J.; Schock, M.R.

    1984-01-01

    Research was conducted to provide accurate modern and historical data on drinking water quality and the possible effect of acid precipitation on water samples. Samples of source raw and finished water were collected from more than 300 surface and groundwater supplies in the New England States, New York, New Jersey, Pennsylvania, West Virginia, Virginia, and North Carolina. The samples were analyzed at EPA laboratories. Historical records were obtained dating back to 1886. Acid rain may dissolve harmful elements from soils and from water supply distribution systems. Because soils can alter the character of acid rain through buffering, causal relationships are difficult to identify. A helpful approach to this problem is the use of indices of water supply sensitiviy and corrosiveness. With these indices, drinking water standards, and reliable chemical data, an assessment of water supply characteristics has been accomplished. Though solution products of acid rain in the water supply sources studied do not exceed EPA Primary Drinking Water Regulations, a large number of tests for aluminum showed levels that could be of concern to kidney dialysis patients. Because of the present water quality conditions (low alkalinity and pH) at numerous water sources, future acid deposition could be expected to have a detrimental effect on water quality. 42 references, 15 figures, 42 tables.

  13. Effects of acid precipitation on reproduction in alpine plant species. [Erythronium grandiflorum; Aquilegia caerulea

    SciTech Connect

    McKenna, M.A.; Hille-Salgueiro, M.; Musselman, R.C. Dept. of Agriculture, Fort Collins, CO )

    1990-01-01

    A series of experiments were designed to determine the impact of acid rain on plant reproductive processes, a critical component of a species life history. Research was carried out in herbaceous alpine communities at the USDA (United States Department of Agriculture) Forest Service Glacier Lakes Ecosystem Experiments Site in the Snowy Mts. of Wyoming. A range of species were surveyed to monitor the sensitivity of pollen to acidification during germination and growth, and all species demonstrated reduced in vitro pollen germination in acidified media. Field pollinations were carried out in Erythronium grandiflorum and Aquilegia caerulea to determine the reproductive success of plants exposed to simulated ambient precipitation (pH 5.6) or simulated acid precipitation (pH 3.6) prior to pollination. In Erythronium, no differences were observed in seed set and seed weight of fruits resulting from the two pollination treatments. In Aquilegia, fruits resulting from the acid spray treatment produced fewer seeds and lighter seeds.

  14. Dissolved, particulate and acid-leachable trace metal concentrations in North Atlantic precipitation collected on the Global Change Expedition

    SciTech Connect

    Lim, B.; Jickells, T.D. )

    1990-12-01

    Atmospheric inputs of trace metals into surface waters are an important pathway for the oceanic biogeochemical cycling of many trace constituents. Rainwater samples from six precipitation events were collected on board ship during legs 3 and 4 of the Global Change Expedition over the North Atlantic Ocean and analyzed for dissolved, particulate (Al and Pb), and acid-leachable trace metals (Al, Fe, Mn, Cd, Cu, Pb, Zn). Acid-leachable concentrations of the elements were similar to reported values from the North Atlantic and Pacific Oceans which were measured using comparable acidification procedures. Concentrations of dissolved and particulate Al and Pb were determined in rain events acid-leachable and total trace metal concentrations suggest that the acid-leachable fraction of metals can significantly underestimate total concentrations of crustal elements in rain. The solubilities of Al and Pb in precipitation were variable and mean solubilities of the elements were 13% and 45%, respectively. Recycled sea salt components were less than 14% for Al, Fe, Mn, Pb, Cd, Cu, and Zn, indicating that the net trace metal flux is from the atmosphere to the oceans. Deep sea particle fluxes for these metals through the western tropical North Atlantic exceed atmospheric deposition fluxes by a factor of 18 to 41. 57 refs., 2 figs., 12 tabs.

  15. A sampling method for improving the representation of spatially varying precipitation and soil moisture using the Simple Biosphere Model

    NASA Astrophysics Data System (ADS)

    Medina, Isaac D.; Denning, A. Scott; Baker, Ian T.; Ramirez, Jorge A.; Randall, David A.

    2014-03-01

    spatially varying precipitation for current grid length scales used in General Circulation Models (GCMs) is a continuing challenge. Furthermore, to fully capture the hydrologic effects of nonuniform precipitation, a representation of soil moisture heterogeneity and distribution of spatially varying precipitation must exist within the same framework. For this study, the explicit and sampling methods of Sellers et al. (2007) are tested off-line using the Simple Biosphere Model (SiB3) in an arid, semiarid, and wet site, and are numerically compared to the bulk method, which is currently used in GCMs. To carry out the numerical experiments, an arbitrary grid area was defined by (1) a single instance of SiB3 (bulk method), (2) 100 instances of SiB3 (explicit method), and (3) less than 100 instances of SiB3 (sampling method). Precipitation was randomly distributed over fractions of the grid area for the explicit and sampling methods, while the standard SiB3 exponential distribution relating precipitation intensity to the grid area wet fraction was used in the bulk method. Comparing the sampling and bulk method to the explicit method indicates that 10 instances of SiB3 in the sampling method better captures the spatial variability in soil moisture and grid area flux calculations produced by the explicit method, and deals realistically with spatially varying precipitation at little additional computational cost to the bulk method.

  16. Acid deposition in Maryland: Implications of the results of the National Acid Precipitation Assessment Program

    SciTech Connect

    DeMuro, J.; Bowmann, M.; Ross, J.; Blundell, C.; Price, R.

    1991-07-01

    Acid deposition, commonly referred to as 'acid rain,' is a major global environmental concern. Acid deposition has reportedly resulted in damage to aquatic, terrestrial, and physical resources and has potentially adverse effects on human health. A component of the Maryland acid deposition program is the preparation of an annual report that summarizes yearly activities and costs of ongoing acid deposition research and monitoring programs.

  17. Temporal trends in the acidity of precipitation and surface waters of New York

    USGS Publications Warehouse

    Peters, Norman E.; Schroeder, Roy A.; Troutman, David E.

    1982-01-01

    Statistical analyses of precipitation data from a nine-station monitoring network indicate little change in pH from 1965-78 within New York State as a whole but suggest that pH of bulk precipitation has decreased in the western part of the State by approximately 0.2 pH units since 1965 and increased in the eastern part by a similar amount. This trend is equivalent to an annual change in hydrogen-ion concentration of 0.2 microequivalents per liter. An average annual increase in precipitation quantity of 2 to 3 percent since 1965 has resulted in an increased acid load in the western and central parts of the State. During 1965-78, sulfate concentration in precipitation decreased an average of 1-4 percent annually. In general, no trend in nitrate was detected. Calculated trends in hydrogen-ion concentration do not correlate with measured trends of sulfate and nitrate, which suggests variable neutralization of hydrogen ion, possibly by particles from dry deposition. Neutralization has produced an increase of about 0.3 pH units in nonurban areas and 0.7 pH units in urban areas. Statistical analyses of chemical data from several streams throughout New York suggest that sulfate concentrations decreased an average of 1 to 4 percent per year. This decrease is comparable to the sulfate decrease in precipitation during the same period. In most areas of the State, chemical contributions from urbanization and farming, as well as the neutralizing effect of carbonate soils, conceal whatever effects acid precipitation may have on pH of streams.

  18. Fractionation of equine antivenom using caprylic acid precipitation in combination with cationic ion-exchange chromatography.

    PubMed

    Raweerith, Rutai; Ratanabanangkoon, Kavi

    2003-11-01

    A combined process of caprylic acid (CA) precipitation and ion-exchange chromatography on SP-Sepharose was studied as a means to fractionate pepsin-digested horse antivenom F(ab')(2) antibody. In the CA precipitation, the optimal concentration for fractionation of F(ab')(2) from pepsin-digested horse plasma was 2%, in which 89.61% of F(ab')(2) antibody activity was recovered in the supernatant with 1.5-fold purification. A significant amount of pepsin was not precipitated and remained active under these conditions. An analytical cation exchanger Protein-Pak SP 8HR HPLC column was tested to establish optimal conditions for the effective separation of IgG, albumin, pepsin and CA from the F(ab')(2) product. From these results, the supernatant from CA precipitation of pepsin-digested plasma was subjected to a SP-Sepharose column chromatography using a linear salt gradient. With stepwise elution, a peak containing F(ab')(2) antibody could be obtained by elution with 0.25 M NaCl. The total recovery of antibody was 65.56% with 2.91-fold purification, which was higher than that achieved by ammonium sulfate precipitation. This process simultaneously and effectively removed residual pepsin, high molecular weight aggregates and CA in the final F(ab')(2) product, and should be suitable for large-scale fractionation of therapeutic equine antivenoms.

  19. Biomediated Precipitation of Calcium Carbonate and Sulfur in a Faintly Acidic Hot Spring

    NASA Astrophysics Data System (ADS)

    Jiang, L.; Peng, X.; Qiao, H.

    2014-12-01

    A faintly acidic hot spring named "female Tower" (T=73.5 ℃, pH=6.64 ) is located in the Jifei Geothermal Field,Yunnan province, Southwest China. The precipitates in the hot spring are composed of large amounts of calcite and sulfur, as reveals by XRD analysis. Scanning electron microscopy (SEM) analysis show the microbial mats are formed of various coccoid, rod and filamentous microbes. Transmission electron microscopy (TEM) analysis show that intracellular sulfur granules are commonly associated with these microbes. Energy dispersive X-ray spectrometer (EDS) analysis shows that the surface of microbes are mainly composed of Ca, C, O and S. A culture-independent molecular phylogenetic analysis demonstrates the majority of bacteria in the spring are sulfur-oxidizing bacteria. In the spring water, H2S concentration was up to 60 ppm, while SO42- concentration was only about 10 ppm. We suggest that H2S might be utilized by sulfur-oxidizing bacteria in this hot spring water, leading to the formation of sulfur granules intracellularly and extracellularly. In the meantime, this reaction increases the pH in ambient environments, which fosters the precipitation of calcium carbonate precipitation in the microbial mats. This study suggests that the sulfur-oxidizing bacteria could play an important role in calcium carbonate precipitation in faintly acidic hot spring environments.

  20. Precipitation-chemistry measurements from the California Acid Deposition Monitoring Program, 1985-1990

    USGS Publications Warehouse

    Blanchard, Charles L.; Tonnessen, Kathy A.

    1993-01-01

    The configuration of the California Acid Deposition Monitoring Program (CADMP) precipitation network is described and quality assurance results summarized. Comparison of CADMP and the National Acid Deposition Program/National Trends Network (NADP/NTN) data at four parallel sites indicated that mean depth-weighted differences were less than 3 μeq ℓ−1 for all ions, being statistically significant for ammonium, sulfate and hydrogen ion. These apparently small differences were 15–30% of the mean concentrations of ammonium, sulfate and hydrogen ion. Mean depth-weighted concentrations and mass deposition rates for the period 1985–1990 are summarized; the latter were highest either where concentrations or precipitation depths were relatively high.

  1. Leaching of metals from steel samples in peracetic acid

    NASA Astrophysics Data System (ADS)

    Yabutani, Tomoki; Nakamura, Takamasa; Takayabagi, Toshio

    2015-03-01

    In this paper, leaching behavior of metallic species from steel samples in peracetic acid was investigated. We compared the leaching efficiency between peracetic acid and acetic acid to estimate the role of peroxo functional group for the leaching. As a result, peracetic acid enhanced the leaching ability of metallic species from the high speed steel and the alloy steel samples. MoO3, Mo, MO2C, W, WO3, VC and MnO2 were effectively leached by peracetic acid, while the stainless steel had a high resistance against corrosion by peracetic acid.

  2. Silica precipitation in acidic solutions: mechanism, pH effect, and salt effect.

    PubMed

    Gorrepati, Elizabeth A; Wongthahan, Pattanapong; Raha, Sasanka; Fogler, H Scott

    2010-07-06

    This study is the first to show that silica precipitation under very acidic conditions ([HCl] = 2-8 M) proceeds through two distinct steps. First, the monomeric form of silica is quickly depleted from solution as it polymerizes to form primary particles approximately 5 nm in diameter. Second, the primary particles formed then flocculate. A modified Smoluchowski equation that incorporates a geometric population balance accurately describes the exponential growth of silica flocs. Variation of the HCl concentration between 2 and 8 M further showed that polymerization to form primary particles and subsequent particle flocculation become exponentially faster with increasing acid concentration. The effect of salt was also studied by adding 1 M chloride salts to the solutions; it was found that salts accelerated both particle formation and growth rates in the order: AlCl(3) > CaCl(2) > MgCl(2) > NaCl > CsCl > no salt. It was also found that ionic strength, over cation identity, determines silica polymerization and particle flocculation rates. This research reveals that precipitation of silica products from acid dissolution of minerals can be studied apart from the mineral dissolution process. Thus, silica product precipitation from mineral acidization follows a two-step process--formation of 5 nm primary particles followed by particle flocculation--which becomes exponentially faster with increasing HCl concentration and with salts accelerating the process in the above order. This result has implications for any study of acid dissolution of aluminosilicate or silicate material. In particular, the findings are applicable to the process of acidizing oil-containing rock formations, a common practice of the petroleum industry where silica dissolution products encounter a low-pH, salty environment within the oil well.

  3. Distribution and Origin of Amino Acids in Lunar Regolith Samples

    NASA Technical Reports Server (NTRS)

    Elsila, J. E.; Callahan, M. P.; Glavin, D. P.; Dworkin, J. P.; McLain, H. L.; Noble, S. K.; Gibson, E. K., Jr.

    2015-01-01

    The existence of organic compounds on the lunar surface has been a question of interest from the Apollo era to the present. Investigations of amino acids immediately after collection of lunar samples yielded inconclusive identifications, in part due to analytical limitations including insensitivity to certain compounds, an inability to separate enantiomers, and lack of compound-specific isotopic measurements. It was not possible to determine if the detected amino acids were indigenous to the lunar samples or the result of terrestrial contamination. Recently, we presented initial data from the analysis of amino acid abundances in 12 lunar regolith samples and discussed those results in the context of four potential amino acid sources [5]. Here, we expand on our previous work, focusing on amino acid abundances and distributions in seven regolith samples and presenting the first compound-specific carbon isotopic ratios measured for amino acids in a lunar sample.

  4. Influence of phosphate and silica on U(VI) precipitation from acidic and neutralized wastewaters

    SciTech Connect

    Kanematsu, Masakazu; Perdrial, Nicolas; Um, Wooyong; Chorover, Jon; O'Day, Peggy A.

    2014-06-03

    Uranium speciation and physical-chemical characteristics were studied in solids precipitated from synthetic acidic to circumneutral wastewaters in the presence and absence of dissolved silica and phosphate to examine thermodynamic and kinetic controls on phase formation. Composition of synthetic wastewater was based on disposal sites 216-U-8 and 216-U-12 Cribs at the Hanford site (WA, USA). In the absence of dissolved silica or phosphate, crystalline or amorphous uranyl oxide hydrates, either compreignacite or meta-schoepite, precipitated at pH 5 or 7 after 30 d of reaction, in agreement with thermodynamic calculations. In the presence of 1 mM dissolved silica representative of groundwater concentrations, amorphous phases dominated by compreignacite precipitated rapidly at pH 5 or 7 as a metastable phase and formation of poorly-crystalline boltwoodite, the thermodynamically stable uranyl silicate phase, was slow. In the presence of phosphate (3 mM), meta-ankoleite initially precipitated as the primary phase at pH 3, 5, or 7 regardless of the presence of 1 mM dissolved silica. Analysis of precipitates by U LIII-edge EXAFS indicated that “autunite-type” sheets of meta-ankoleite transformed to “phosphuranylite-type” sheets after 30 d of reaction, probably due to Ca substitution in the structure. Low solubility of uranyl phosphate phases limits dissolved U(VI) concentrations but differences in particle size, crystallinity, and precipitate composition vary with pH and base cation concentration, which will influence the thermodynamic and kinetic stability of these phases.

  5. Effect of precipitation, geographical location and biosynthesis on New Zealand milk powder bulk and fatty acids D/H ratios

    NASA Astrophysics Data System (ADS)

    Frew, R.; Emad Ehtesham, R.; Van Hale, R.; Hayman, A.; Baisden, T.

    2012-04-01

    D/H ratio measurements provide useful information for the investigation of biogeochemical influences on natural and agricultural produce, particularly with application to food traceability and authentication. Numerous studies have shown that variation of a product's D/H ratio is influenced by both environmental factors and biological processes. This study investigates the D/H ratio of New Zealand milk powder and individual fatty acids, and causal determinants of isotopic variation. One of the key environmental factors is precipitation, and the D/H ratio "isoscaping" of NZ has been undertaken. New Zealand provides a unique geography for these kinds of study in terms of proximity to the ocean and natural geographical variability from sea level to elevations as high as 3700 m. Milk powder samples were collected from different geographical regions from milk processing units, which were supplied by producers in the immediate region. H/D ratios of bulk milk powder and of individual fatty acids were determined. Initial comparison of the precipitation and milk powder bulk D/H data show a very good differentiation from north to southernmost parts of New Zealand and a relation between rain and milk bulk D/H abundance ratio. Almost 98% of milk FAs are in the form of triglycerides that have been extracted and hydrolysed to free FAs. Free FAs were esterified and analyzed with GC-IRMS. Individual FAs show variation in D/H ratio, and all values are depleted relative to the precipitation data. The difference in D/H ratio amongst individual FAs reflects the geographical environment and biological processes i.e. micro-organisms activity in the rumen of the cow. Short chain FAs (less than 8 carbons), particularly C4 (Butyric acid), appear to be key determinants. The variation in the data can be rationalized using statistical multivariate analysis.

  6. Relationship between acidity and ionic composition of wet precipitation: A two years study at an urban site, Thessaloniki, Greece

    NASA Astrophysics Data System (ADS)

    Anatolaki, Ch.; Tsitouridou, R.

    2009-03-01

    Wet precipitation samples were collected in the city center of Thessaloniki, northern Greece, for two years with different rainfall amount (April 2002-March 2004). All samples were analyzed for major anions and cations (Cl -, NO 3-, SO 42-, NH 4+, Na +, K +, Ca 2+ and Mg 2+). HCO 3- concentrations were calculated through pH measurements. Arithmetic mean pH values of 6.06 and 6.57 were found for the two periods. 10.5% of the first year rain events (April 2002-March 2003) and 2.5% of the second (April 2003-March 2004) exhibited pH ≤ 4.5. The quite typical, for Mediterranean areas, trend Ca 2+ > SO 42- > NH 4+ > Cl - > NO 3- was observed in the majority of the samples. The study of the relationship between the ionic concentrations and the precipitation amount gave information about the scavenging mechanism of ions (below or in-cloud). 67% of the rain acidity was found to be due to sulfuric acid and the rest 33% to nitric acid. The calculation of Neutralization Factors (NF) and the application of Multiple Linear Regression Analysis (MLR), showed the higher Ca 2+ contribution to the neutralization process. The impact of maritime sources was extracted from the SSF of Cl - and Mg 2+, while the anthropogenic origin of SO 42- was supported by the high NSSF (~ 98%). The local calcareous soil dust and possible long-range transport are the main sources of Ca 2+ in the area. A case study by using trajectory analysis to predict a long-range transport of pollutants from Etnean volcano, Italy, to the study area, is described.

  7. Particle size tailoring of ursolic acid nanosuspensions for improved anticancer activity by controlled antisolvent precipitation.

    PubMed

    Wang, Yancai; Song, Ju; Chow, Shing Fung; Chow, Albert H L; Zheng, Ying

    2015-10-15

    The present study was aimed at tailoring the particle size of ursolic acid (UA) nanosuspension for improved anticancer activity. UA nanosuspensions were prepared by antisolvent precipitation using a four-stream multi-inlet vortex mixer (MIVM) under defined conditions of varying solvent composition, drug feeding concentration or stream flow rate. The resulting products were characterized for particle size and polydispersity. Two of the UA nanosuspensions with mean particle sizes of 100 and 300 nm were further assessed for their in-vitro activity against MCF-7 breast cancer cells using fluorescence microscopy with 4',6-diamidino-2-phenylindole (DAPI) staining, as well as flow cytometry with propidium (PI) staining and with double staining by fluorescein isothiocyanate. It was revealed that the solvent composition, drug feeding concentration and stream flow rate were critical parameters for particle size control of the UA nanosuspensions generated with the MIVM. Specifically, decreasing the UA feeding concentration or increasing the stream flow rate or ethanol content resulted in a reduction of particle size. Excellent reproducibility for nanosuspension production was demonstrated for the 100 and 300 nm UA preparations with a deviation of not more than 5% in particle size from the mean value of three independent batches. Fluorescence microscopy and flow cytometry revealed that these two different sized UA nanosuspensions, particularly the 300 nm sample, exhibited a higher anti-proliferation activity against the MCF-7 cells and afforded a larger population of these cells in both early and late apoptotic phases. In conclusion, MIVM is a robust and pragmatic tool for tailoring the particle size of the UA nanosuspension. Particle size appears to be a critical determinant of the anticancer activity of the UA nanoparticles.

  8. The Origin of Amino Acids in Lunar Regolith Samples

    NASA Technical Reports Server (NTRS)

    Cook, Jamie E.; Callahan, Michael P.; Dworkin, Jason P.; Glavin, Daniel P.; McLain, Hannah L.; Noble, Sarah K.; Gibson, Everett K., Jr.

    2016-01-01

    We analyzed the amino acid content of seven lunar regolith samples returned by the Apollo 16 and Apollo 17 missions and stored under NASA curation since collection using ultrahigh-performance liquid chromatography with fluorescence detection and time-of-flight mass spectrometry. Consistent with results from initial analyses shortly after collection in the 1970s, we observed amino acids at low concentrations in all of the curated samples, ranging from 0.2 parts-per-billion (ppb) to 42.7 ppb in hot-water extracts and 14.5 ppb to 651.1 ppb in 6M HCl acid-vapor-hydrolyzed, hot-water extracts. Amino acids identified in the Apollo soil extracts include glycine, D- and L-alanine, D- and L-aspartic acid, D- and L-glutamic acid, D- and L-serine, L-threonine, and L-valine, all of which had previously been detected in lunar samples, as well as several compounds not previously identified in lunar regoliths: -aminoisobutyric acid (AIB), D-and L-amino-n-butyric acid (-ABA), DL-amino-n-butyric acid, -amino-n-butyric acid, -alanine, and -amino-n-caproic acid. We observed an excess of the L enantiomer in most of the detected proteinogenic amino acids, but racemic alanine and racemic -ABA were present in some samples.

  9. Influence of Aldrich humic acid and metal precipitates on survivorship of mayflies (Atalophlebia spp.) to acid mine drainage.

    PubMed

    Holland, Aleicia; Duivenvoorden, Leo J; Kinnear, Susan H W

    2014-03-01

    Humic substances (HS) have been shown to decrease the toxicity of environmental stressors, but knowledge of their ability to influence the toxicity of multiple stressors such as metal mixtures and low pH associated with acid mine drainage (AMD) is still limited. The present study investigated the ability of HS to decrease toxicity of AMD to mayflies (Atalophlebia spp.). The AMD was collected from the Mount Morgan (Mount Morgan, Queensland, Australia) open pit. Mayflies were exposed to concentrations of AMD at 0%, 1%, 2%, 3%, and 4% in the presence of 0 mg/L, 10 mg/L, and 20 mg/L Aldrich humic acid (AHA). A U-shaped response was noted in all AHA treatments, with higher rates of mortality recorded in the 2% and 3% dilutions compared with 4%. This result was linked with increased precipitates in the lower concentrations. A follow-up trial showed significantly higher concentrations of precipitates in the 2% and 3% AMD dilutions in the 0 mg/L AHA treatment and higher precipitates in the 2% AMD, 10 mg/L and 20 mg/L AHA, treatments. Humic substances were shown to significantly increase survival of mayflies exposed to AMD by up to 50% in the 20 mg/L AHA treatment. Humic substances may have led to increased survival after AMD exposure through its ability to influence animal physiology and complex heavy metals. These results are valuable in understanding the ability of HS to influence the toxicity of multiple stressors.

  10. Biomediated Precipitation of Calcium Carbonate in a Slightly Acidic Hot Spring

    NASA Astrophysics Data System (ADS)

    Jiang, L.

    2015-12-01

    A slightly acidic hot spring named "Female Tower" (T=73.5 °C, pH=6.64) is located in the Jifei Geothermal Field, Yunnan Province, Southwest China. The precipitates in the hot spring are composed of large amounts of calcite, aragonite, and sulfur. Scanning electron microscopy (SEM) analyses revealed that the microbial mats were formed of various coccoid, rod-shaped, and filamentous microbes. Transmission electron microscopy (TEM) showed that the intracellular sulfur granules were commonly associated with these microbes. A culture-independent molecular phylogenetic analysis demonstrated that the majority of the bacteria in the spring were sulfur-oxidizing bacteria. In the spring water, H2S concentration was up to 60 ppm, while SO42- concentration was only about 10 ppm. We speculated that H2S might be utilized by sulfur-oxidizing bacteria in this hot spring water, leading to the intracellular formation of sulfur granules. In the meantime, this reaction increased the pH in the micron-scale microdomains, which fostered the precipitation of calcium carbonate in the microbial mats. The results of this study indicated that the sulfur-oxidizing bacteria could play an important role in calcium carbonate precipitation in slightly acidic hot spring environments.

  11. Mathematical model and computer simulation on moving precipitate boundary electrophoresis for offline sample pre- concentration of heavy metal ion.

    PubMed

    Chang, Jiang; Zhang, Jie; Wang, Hou-Yu; Fan, Liu-Yin; Fan, Yin-Ping; Li, Shan; Cao, Cheng-Xi

    2013-01-15

    In this paper, a mathematical model and computer simulator were developed for offline sample pretreatment of heavy metal ion based on moving precipitate boundary (MPB) electrophoresis. The simulation indicates that (i) the program can easily accomplish numerical computations, such as the velocities of MPB and elution boundary (EB), and enrichment factor (EF) etc; (ii) the simulator can vividly imitate the dynamics of MPB, EB, precipitate zone, and precipitate-elution; and (iii) the software may simply optimized experimental conditions via the influence factors (e.g., voltage, hydroxyl, hydrogen and metal ions) on the EF. As a proof of concept, copper ion and its precipitate with definite blue color were, respectively chosen as mode heavy metal ion and alkaline precipitate for the relevant experiments of MPB-based sample preconcentration of heavy metal ion in large tube. All of the experimental results manifest the validity of developed mathematical model and the relevant simulation results. The model and simulator advanced herein are of clear significance to the optimization of experimental conditions and understanding of offline MPB- based sample condensation of heavy metal ion.

  12. Study on dicarboxylic acids in aerosol samples with capillary electrophoresis.

    PubMed

    Adler, Heidi; Sirén, Heli

    2014-01-01

    The research was performed to study the simultaneous detection of a homologous series of α , ω -dicarboxylic acids (C2-C10), oxalic, malonic, succinic, glutaric, adipic, pimelic, suberic, azelaic, and sebacic acids, with capillary electrophoresis using indirect UV detection. Good separation efficiency in 2,6-pyridinedicarboxylic acid as background electrolyte modified with myristyl trimethyl ammonium bromide was obtained. The dicarboxylic acids were ionised and separated within five minutes. For the study, authentic samples were collected onto dry cellulose membrane filters of a cascade impactor (12 stages) from outdoor spring aerosols in an urban area. Hot water and ultrasonication extraction methods were used to isolate the acids from membrane filters. Due to the low concentrations of acids in the aerosols, the extracts were concentrated with solid-phase extraction (SPE) before determination. The enrichment of the carboxylic acids was between 86 and 134% with sample pretreatment followed by 100-time increase by preparation of the sample to 50  μ L. Inaccuracy was optimised for all the sample processing steps. The aerosols contained dicarboxylic acids C2-C10. Then, mostly they contained C2, C5, and C10. Only one sample contained succinic acid. In the study, the concentrations of the acids in aerosols were lower than 10 ng/m(3).

  13. Bioprocess monitoring: minimizing sample matrix effects for total protein quantification with bicinchoninic acid assay.

    PubMed

    Reichelt, Wieland N; Waldschitz, Daniel; Herwig, Christoph; Neutsch, Lukas

    2016-09-01

    Determining total protein content is a routine operation in many laboratories. Despite substantial work on assay optimization interferences, the widely used bicinchoninic acid (BCA) assay remains widely recognized for its robustness. Especially in the field of bioprocess engineering the inaccuracy caused by interfering substances remains hardly predictable and not well understood. Since the introduction of the assay, sample pre-treatment by trichloroacetic acid (TCA) precipitation has been indicated as necessary and sufficient to minimize interferences. However, the sample matrix in cultivation media is not only highly complex but also dynamically changing over process time in terms of qualitative and quantitative composition. A significant misestimation of the total protein concentration of bioprocess samples is often observed when following standard work-up schemes such as TCA precipitation, indicating that this step alone is not an adequate means to avoid measurement bias. Here, we propose a modification of the BCA assay, which is less influenced by sample complexity. The dynamically changing sample matrix composition of bioprocessing samples impairs the conventional approach of compensating for interfering substances via a static offset. Hence, we evaluated the use of a correction factor based on an internal spike measurement for the respective samples. Using protein spikes, the accuracy of the BCA protein quantification could be improved fivefold, taking the BCA protein quantification to a level of accuracy comparable to other, more expensive methods. This will allow reducing expensive iterations in bioprocess development to due inaccurate total protein analytics.

  14. Preparation of All-Trans Retinoic Acid nanosuspensions using a modified precipitation method.

    PubMed

    Zhang, X; Xia, Q; Gu, N

    2006-08-01

    All-Trans Retinoic Acid (ATRA) nanosuspensions were prepared with a modified precipitation method. The ATRA solution in acetone was injected into pure water by an air compressor under the action of ultrasonication. Photon correlation spectroscopy results showed that the mean particle size of ATRA nanoparticles in nanosuspensions reduced from 337 nm to 155 nm as the injection velocity increased and the polydispersity index was 0.45-0.50. The morphology of ATRA nanoparticles varied with the different concentration of ATRA solution in acetone. ATRA nanoparticles showed an amorphous state and stable in 6 months. It could be concluded that this modified precipitation method could produce stable and controllable ATRA nanosuspension to a certain extent, thus benefit for higher saturation solubility.

  15. Factors affecting the rate of hydrolysis of phenylboronic acid in lab-scale precipitate reactor studies

    SciTech Connect

    Bannochie, C.J.; Marek, J.C.; Eibling, R.E.; Baich, M.A.

    1992-01-01

    Removing aromatic carbon from an aqueous slurry of cesium-137 and other alkali tetraphenylborates by acid hydrolysis will be an important step in preparing high-level radioactive waste for vitrification at the Savannah River Site's Defense Waste Processing Facility (DWPF). Kinetic data obtained in bench-scale precipitate hydrolysis reactors suggest changes in operating parameters to improve product quality in the future plant-scale radioactive operation. The rate-determining step is the removal of the fourth phenyl group, i.e. hydrolysis of phenylboronic acid. Efforts to maximize this rate have established the importance of several factors in the system, including the ratio of copper(II) catalyst to formic acid, the presence of nitrite ion, reactions of diphenylmercury, and the purge gas employed in the system.

  16. Factors affecting the rate of hydrolysis of phenylboronic acid in lab-scale precipitate reactor studies

    SciTech Connect

    Bannochie, C.J.; Marek, J.C.; Eibling, R.E.; Baich, M.A.

    1992-10-01

    Removing aromatic carbon from an aqueous slurry of cesium-137 and other alkali tetraphenylborates by acid hydrolysis will be an important step in preparing high-level radioactive waste for vitrification at the Savannah River Site`s Defense Waste Processing Facility (DWPF). Kinetic data obtained in bench-scale precipitate hydrolysis reactors suggest changes in operating parameters to improve product quality in the future plant-scale radioactive operation. The rate-determining step is the removal of the fourth phenyl group, i.e. hydrolysis of phenylboronic acid. Efforts to maximize this rate have established the importance of several factors in the system, including the ratio of copper(II) catalyst to formic acid, the presence of nitrite ion, reactions of diphenylmercury, and the purge gas employed in the system.

  17. Recovery of molybdenum, nickel and cobalt by precipitation from the acidic leachate of a mineral sludge.

    PubMed

    Vemic, M; Bordas, F; Comte, S; Guibaud, G; Lens, P N L; van Hullebusch, E D

    2016-09-01

    The objective of this study was to investigate the recovery potential of molybdenum (Mo), nickel (Ni) and cobalt (Co) from synthetic and real acidic leachate of a mineral sludge from a metal recycling plant by sulfide precipitation. The operational parameters (metal sulfide (M/S) ratio 0.1-1, agitation speed 0-100 rpm, contact time 15-120 min and pH 1-5) were optimized in batch conditions on synthetic metal leachate (0.5 M HNO3, Mo = 101.6 mg L(-1), Ni = 70.8 mg L(-1), Co = 27.1 mg L(-1)) with a 0.1 M Na2S solution. Additionally, recovery of the target metals was theoretically simulated with a chemical equilibrium model (Visual MINTEQ 3.0). The optimized Na2S precipitation of metals from the synthetic leachate resulted in the potential selective recovery of Mo at pH 1 (98% by modeling, 95% experimental), after simultaneous precipitation of Ni and Co as sulfide at pH 4 (100% by modeling, 98% experimental). Metal precipitation from the real leachate (18 M H2SO4, Mo = 10,160 mg L(-1), Ni = 7,080 mg L(-1), Co = 2,710 mg L(-1)) was performed with 1 M Na2S, and resulted in a maximal Mo recovery at pH 2 (50%), while maximal recoveries of Ni and Co were observed at pH 4 (56% and 60%, respectively). Real leachate gave a lower metals recovery efficiency compared with synthetic leachate, which can be attributed to changes in the pH, nature of leachant, co-precipitation of Zn and competition for S(2-) ions.

  18. Polybrominated diphenyl ethers and alternative flame retardants in air and precipitation samples from the northern Lake Victoria region, East Africa.

    PubMed

    Arinaitwe, Kenneth; Muir, Derek C G; Kiremire, Bernard T; Fellin, Phil; Li, Henrik; Teixeira, Camilla

    2014-01-01

    High volume air and precipitation samples were collected close to the shore of Lake Victoria at Entebbe, Uganda, between October 2008 and July 2010 inclusive. Polybrominated diphenyl ethers (PBDEs) and alternative flame retardants (AFRs) were analyzed by GC-MS. BDEs 47, 99, and 209 were the predominant PBDEs with mean concentrations (in air) of 9.84, 4.38, 8.27 pg m(-3) and mean fluxes in precipitation of 3.40, 6.23, and 7.82 ng m(-2) sample(-1), respectively. 1,2-bis(2,4,6-tribromophenoxy)ethane (BTBPE), and hexabromocyclododecane (HBCDD), anti- and syn-Dechlorane plus were detected at levels comparable with those of PBDEs. Both PBDEs and AFRs in air generally increased from 2008 to 2010. Elevated PBDE concentrations in air were associated with slow moving low altitude air masses from the region immediately adjacent to the lake, while low concentrations were mostly associated with fast moving westerly and southwesterly air masses. Analysis of the octa- and nona-BDE profiles suggested photolysis and pyrolytic debromination of BDE-209 in the air samples. The highly halogenated and most abundant PBDEs and AFRs in air also predominated in precipitation samples. This is the first study to report flame retardants in high volume air samples and precipitation in Equatorial Africa.

  19. Synthesis of WO{sub 3} nanoparticles by citric acid-assisted precipitation and evaluation of their photocatalytic properties

    SciTech Connect

    Sánchez-Martínez, D.; Martínez-de la Cruz, A.; López-Cuéllar, E.

    2013-02-15

    Graphical abstract: Display Omitted Highlights: ► WO{sub 3} nanoparticles were synthesized by a simple citric acid-assisted precipitation. ► WO{sub 3} photocatalyst was able to the partial mineralization of rhB, IC and MO. ► WO{sub 3} can be considered as a photocatalyst active under visible light irradiation. -- Abstract: WO{sub 3} nanoparticles were synthesized by citric acid-assisted precipitation method using a 1:1.5 molar ratio of ammonium paratungstate hydrate (H{sub 42}N{sub 10}O{sub 42}W{sub 12}·xH{sub 2}O):citric acid (C{sub 6}H{sub 8}O{sub 7}). The formation of monoclinic crystal structure of WO{sub 3} at different temperatures was confirmed by X-ray powder diffraction (XRD). The characterization of the samples synthesized was complemented by transmission electron microscopy (TEM), Brunauer–Emmitt–Teller surface area (BET) and diffuse reflectance spectroscopy (DRS). According to the thermal treatment followed during the synthesis of WO{sub 3}, the morphology of the nanoparticles formed was characterized by rectangular and ovoid shapes. The photocatalytic activity of WO{sub 3} obtained under different experimental conditions was evaluated in the degradation of rhodamine B (rhB), indigo carmine (IC), methyl orange (MO), and Congo red (CR) in aqueous solution under UV and UV–vis radiation. The highest photocatalytic activity was observed in the sample obtained by thermal treatment at 700 °C. In general, the sequence of degradation of the organic dyes was: indigo carmine (IC) > rhodamine B (rhB) > methyl orange (MO) > Congo red (CR). The mineralization degree of organic dyes by WO{sub 3} photocatalysts was determined by total organic carbon analysis (TOC) reaching percentages of mineralization of 82% (rhB), 85% (IC), 28% (MO), and 7% (CR) for 96 h of lamp irradiation.

  20. Contribution of natural and anthropogenic emissions to acid precipitation formation in the Mexico City Metropolitan Area

    SciTech Connect

    Garcia, L.; Barrera, G.; Castellanos, L.; Moreno, D.

    1996-12-31

    The emissions of precursor compounds that contribute significantly the formation of acid precipitation in urban areas are associated with the burning of fossils fuels from mobile, area and point sources. In Mexico City, these include services, institutions and residences aggregated as area sources, as well as industrial point sources, including smelting, refinement of petroleum and power generation. In addition, dusts from soil erosion and lack of vegetation in the urban landscape contribute to modification of natural rain water. It is common knowledge that acid precipitation characterizes a large variety of compounds, as much related to precursor emissions as to prevailing environmental factors. This study attempts to establish the contribution of natural and anthropogenic emissions and meteorological conditions during the rainy season by analysis of spatial and temporal distributions, as of different ions in solution with rain water, as well as the modeling of wind patterns, as represented by using the arc/info software. This study`s results also show the geographic areas impacted by the acid rain phenomenon and the acidification rates in the Mexico City Metropolitan Area during the past 3 years.

  1. Precipitation of heavy metals from acid mine drainage and their geochemical modeling

    NASA Astrophysics Data System (ADS)

    Petrilakova, Aneta; Balintova, Magdalena; Holub, Marian

    2014-06-01

    Geochemical modeling plays an increasingly vital role in a number of areas of geoscience, ranging from groundwater and surface water hydrology to environmental preservation and remediation. Geochemical modeling is also used to model the interaction processes at the water - sediment interface in acid mine drainage (AMD). AMD contains high concentrations of sulfate and dissolved metals and it is a serious environmental problem in eastern Slovakia. The paper is focused on comparing the results of laboratory precipitation of metal ions from AMD (the Smolnik creek, Slovakia) with the results obtained by geochemical modeling software Visual Minteq 3.0.

  2. Seasonal factors controlling mineral precipitation in the acid mine drainage at Donghae coal mine, Korea.

    PubMed

    Kim, J J; Kim, S J

    2004-06-05

    Monitoring over a 12 month period in the Sanae creek flow in acid mine drainage, Donghae coal mine area, demonstrates that the concentrations of dissolved metals and sulphate are highest during autumn when water flow in the creek is at its lowest. The highest pH values of the stream were measured in April and May, whereas the lowest pH was recorded in October. The Fe concentration of stream water rapidly decreased downstream due to the precipitation of Fe oxyhydroxide and/or oxyhydroxysulfate phases in the stream. Mineral precipitates in the creek in the Donghae mine area show various colours such as brownish yellow (Munsell colour 9.5 YR hues), reddish brown (Munsell colour 3.5 YR hues) and white depending on seasons and distance from the pollution source in the creek. Such phenomena are attributed to the variation in pH and chemical composition of stream water caused by seasonal factors. The measured pH ranges in stream water of the brownish yellow, white and reddish brown precipitates are pH 3.2-4.5, 4.5-6.0 and 5.3-6.9, respectively.

  3. Histone-dependent IgG conservation in octanoic acid precipitation and its mechanism.

    PubMed

    Chen, Quan; Toh, Phyllicia; Sun, Yue; Latiff, Sarah Maria Abdul; Hoi, Aina; Xian, Mo; Zhang, Haibo; Nian, Rui; Zhang, Wei; Gagnon, Pete

    2016-12-01

    Octanoic acid (OA) precipitation has long been used in protein purification. Recently, we reported a new cell culture clarification method for immunoglobulin G (IgG) purification, employing an advance elimination of chromatin heteroaggregates with a hybrid OA-solid phase system. This treatment reduced DNA more than 3 logs, histone below the detection limit (LOD), and non-histone host cell proteins (nh-HCP) by 90 % while conserving more than 90 % of the IgG monomer. In this study, we further investigated the conservation of IgG monomer and antibody light chain (LC) to the addition of OA/OA-solid phase complex, with or without histone and DNA in different combinations. The results showed that highly basic histone protein was the prime target in OA/OA-solid phase precipitation system for IgG purification, and the selective conservation of IgG monomer in this system was histone dependent. Our findings partially support the idea that OA works by sticking to electropositive hydrophobic domains on proteins, reducing their solubility, and causing them to agglomerate into large particles that precipitate from solution. Our findings also provide a new perspective for IgG purification and emphasize the necessity to re-examine the roles of various host contaminants in IgG purification.

  4. Comparison of Four Strong Acids on the Precipitation Potential of Gypsum in Brines During Distillation of Pretreated, Augmented Urine

    NASA Technical Reports Server (NTRS)

    Muirhead, Dean

    2011-01-01

    Two batches of nominally pretreated and augmented urine were prepared with the baseline pretreatment formulation of sulfuric acid and chromium trioxide. The urine was augmented with inorganic salts and organic compounds in order to simulate a urinary ionic concentrations representing the upper 95 percentile on orbit. Three strong mineral acids: phosphoric, hydrochloric, and nitric acid, were substituted for the sulfuric acid for comparison to the baseline sulfuric acid pretreatment formulation. Three concentrations of oxidizer in the pretreatment formulation were also tested. Pretreated urine was distilled to 85% water recovery to determine the effect of each acid and its conjugate base on the precipitation of minerals during distillation. The brines were analyzed for calcium and sulfate ion, total, volatile, and fixed suspended solids. Test results verified that substitution of phosphoric, hydrochloric, or nitric acids for sulfuric acid would prevent the precipitation of gypsum up to 85% recovery from pretreated urine representing the upper 95 percentile calcium concentration on orbit.

  5. Biogenic precipitation of manganese oxides and enrichment of heavy metals at acidic soil pH

    NASA Astrophysics Data System (ADS)

    Mayanna, Sathish; Peacock, Caroline L.; Schäffner, Franziska; Grawunder, Anja; Merten, Dirk; Kothe, Erika; Büchel, Georg

    2014-05-01

    The precipitation of biogenic Mn oxides at acidic pH is rarely reported and poorly understood, compared to biogenic Mn oxide precipitation at near neutral conditions. Here we identified and investigated the precipitation of biogenic Mn oxides in acidic soil, and studied their role in the retention of heavy metals, at the former uranium mining site of Ronneburg, Germany. The site is characterized by acidic pH, low carbon content and high heavy metal loads including rare earth elements. Specifically, the Mn oxides were present in layers identified by detailed soil profiling and within these layers pH varied from 4.7 to 5.1, Eh varied from 640 to 660 mV and there were enriched total metal contents for Ba, Ni, Co, Cd and Zn in addition to high Mn levels. Using electron microprobe analysis, synchrotron X-ray diffraction and X-ray absorption spectroscopy, we identified poorly crystalline birnessite (δ-MnO2) as the dominant Mn oxide in the Mn layers, present as coatings covering and cementing quartz grains. With geochemical modelling we found that the environmental conditions at the site were not favourable for chemical oxidation of Mn(II), and thus we performed 16S rDNA sequencing to isolate the bacterial strains present in the Mn layers. Bacterial phyla present in the Mn layers belonged to Firmicutes, Actinobacteria and Proteobacteria, and from these phyla we isolated six strains of Mn(II) oxidizing bacteria and confirmed their ability to oxidise Mn(II) in the laboratory. The biogenic Mn oxide layers act as a sink for metals and the bioavailability of these metals was much lower in the Mn layers than in adjacent layers, reflecting their preferential sorption to the biogenic Mn oxide. In this presentation we will report our findings, concluding that the formation of natural biogenic poorly crystalline birnessite can occur at acidic pH, resulting in the formation of a biogeochemical barrier which, in turn, can control the mobility and bioavailability of heavy metals in

  6. Microscopic evaluation of trace metals in cloud droplets in an acid precipitation region.

    PubMed

    Li, Weijun; Wang, Yan; Collett, Jeffrey L; Chen, Jianmin; Zhang, Xiaoye; Wang, Zifa; Wang, Wenxing

    2013-05-07

    Mass concentrations of soluble trace metals and size, number, and mixing properties of nanometal particles in clouds determine their toxicity to ecosystems. Cloud water was found to be acidic, with a pH of 3.52, at Mt. Lu (elevation 1,165 m) in an acid precipitation region in South China. A combination of Inductively Coupled Plasma Mass Spectrometry (ICPMS) and Transmission Electron Microscopy (TEM) for the first time demonstrates that the soluble metal concentrations and solid metal particle number are surprisingly high in acid clouds at Mt. Lu, where daily concentrations of SO2, NO2, and PM10 are 18 μg m(-3), 7 μg m(-3), and 22 μg m(-3). The soluble metals in cloudwater with the highest concentrations were zinc (Zn, 200 μg L(-1)), iron (Fe, 88 μg L(-1)), and lead (Pb, 77 μg L(-1)). TEM reveals that 76% of cloud residues include metal particles that range from 50 nm to 1 μm diameter with a median diameter of 250 nm. Four major metal-associated particle types are Pb-rich (35%), fly ash (27%), Fe-rich (23%), and Zn-rich (15%). Elemental mapping shows that minor soluble metals are distributed within sulfates of cloud residues. Emissions of fine metal particles from large, nonferrous industries and coal-fired power plants with tall stacks were transported upward to this high elevation. Our results suggest that the abundant trace metals in clouds aggravate the impacts of acid clouds or associated precipitation on the ecosystem and human health.

  7. Evaluation of simulated acid precipitation effects on forest microcosms. Final report

    SciTech Connect

    Kelly, J.M.; Strickland, R.C.; Weatherford, F.P.; Noggle, J.C.

    1984-04-01

    Microcosms were treated for a 30-month period with simulated precipitation acidified to four pH levels (5.7, 4.5, 4.0, and 3.5) to evaluate the impact of acid precipitation on foliar leaching, plant nutrient content, soil leaching, soil nutrient content, and litter decomposition. Direct effects of acid precipitation on diameter growth, bud break, leaf senescence, chlorophyll content, stomatal size, stomatal density, photosynthesis, respiration, transpiration, and cuticle erosion were evaluated on tulip poplar, white oak, and Virginia pine seedlings growing as mixed stands in the microcosms. None of the plant physiological or morphological parameters evaluated responded in a statistically significant manner as a result of treatment. A significant treatment canopy interaction was observed in the form of a 60 percent increase in calcium input in throughfall in response to the pH 3.5 treatment. Foliar nutrient content did not change in response to treatment nor did field measurements of decomposer activity. Soil analysis indicated a significantly lower concentration of exchangeable calcium and magnesium in the top 3.5 cm of the mineral soil in association with the pH 3.5 treatment. Soil leachate concentrations exhibited significant increases at both the 25 and 50 cm depths. However, at the 100 cm depth no significant response in concentration or elemental loss from the system was observed. Laboratory respiration measurements indicated a small, but statistically significant reduction in decomposer activity in the lower litter (02) horizon. This reduction was masked in the field measurements of decomposer activity due to the relatively small contribution of the 02 to total soil respiration. 38 references, 12 figures, 18 tables.

  8. Effectiveness of coagulation and acid precipitation processes for the pre-treatment of diluted black liquor.

    PubMed

    Garg, Anurag; Mishra, I M; Chand, S

    2010-08-15

    The effectiveness of coagulation (using aluminium-based chemicals and ferrous sulfate) and acid precipitation (using H(2)SO(4)) processes for the pre-treatment of diluted black liquor obtained from a pulp and paper mill is reported. Commercial alum was found to be the most economical among all the aluminium and ferrous salts used as a coagulant. A maximum removal of chemical oxygen demand (COD) (ca. 63%) and colour reduction (ca. 90%) from the wastewater (COD = 7000 mg l(-1)) at pH 5.0 was obtained with alum. During the acid precipitation process, at pH < 5.0, significant COD reductions (up to 64%) were observed. Solid residue obtained from the alum treatment at a temperature of 95 degrees C showed much better (3 times) settling rate than that for the residue obtained after treatment with the same coagulant at a temperature of 25 degrees C. The settling curves had three parts, namely, hindered, transition and compression zones. Tory plots were used to determine the critical height of suspension-supernatant interface that is used in the design of a clarifier-thickener unit. High heating values and large biomass fraction of the solid residues can encourage the fuel users to use this waste derived sludge as a potential renewable energy source.

  9. Technical and economical assessment of formic acid to recycle phosphorus from pig slurry by a combined acidification-precipitation process.

    PubMed

    Daumer, M-L; Picard, S; Saint-Cast, P; Dabert, P

    2010-08-15

    Dissolution by acidification followed by a liquid/solid separation and precipitation of phosphorus from the liquid phase is one possibility to recycle phosphorus from livestock effluents. To avoid increase of effluent salinity by using mineral acids in the recycling process, the efficiency of two organic acids, formic and acetic acid, in dissolving the mineral phosphorus from piggery wastewater was compared. The amount of formic acid needed to dissolve the phosphorus was reduced three fold, compared to acetic acid. The amount of magnesium oxide needed for further precipitation was decreased by two with formic acid. Neither the carbon load nor the effluent salinity was significantly increased by using formic acid. An economical comparison was performed for the chemical recycling process (mineral fertilizer) vs. centrifugation (organic fertilizer) considering the centrifugation and the mineral fertilizers sold in the market. After optimisation of the process, the product could be economically competitive with mineral fertilizer as superphosphate in less than 10 years.

  10. The origin of amino acids in lunar regolith samples

    NASA Astrophysics Data System (ADS)

    Elsila, Jamie E.; Callahan, Michael P.; Dworkin, Jason P.; Glavin, Daniel P.; McLain, Hannah L.; Noble, Sarah K.; Gibson, Everett K.

    2016-01-01

    We analyzed the amino acid content of seven lunar regolith samples returned by the Apollo 16 and Apollo 17 missions and stored under NASA curation since collection using ultrahigh-performance liquid chromatography with fluorescence detection and time-of-flight mass spectrometry. Consistent with results from initial analyses shortly after collection in the 1970s, we observed amino acids at low concentrations in all of the curated samples, ranging from 0.2 parts-per-billion (ppb) to 42.7 ppb in hot-water extracts and 14.5-651.1 ppb in 6 M HCl acid-vapor-hydrolyzed, hot-water extracts. Amino acids identified in the Apollo soil extracts include glycine, D- and L-alanine, D- and L-aspartic acid, D- and L-glutamic acid, D- and L-serine, L-threonine, and L-valine, all of which had previously been detected in lunar samples, as well as several compounds not previously identified in lunar regoliths: α-aminoisobutyric acid (AIB), D- and L-β-amino-n-butyric acid (β-ABA), DL-α-amino-n-butyric acid, γ-amino-n-butyric acid, β-alanine, and ε-amino-n-caproic acid. We observed an excess of the L enantiomer in most of the detected proteinogenic amino acids, but racemic alanine and racemic β-ABA were present in some samples. We also examined seven samples from Apollo 15, 16, and 17 that had been previously allocated to a non-curation laboratory, as well as two samples of terrestrial dunite from studies of lunar module engine exhaust that had been stored in the same laboratory. The amino acid content of these samples suggested that contamination had occurred during non-curatorial storage. We measured the compound-specific carbon isotopic ratios of glycine, β-alanine, and L-alanine in Apollo regolith sample 70011 and found values of -21‰ to -33‰. These values are consistent with those seen in terrestrial biology and, together with the enantiomeric compositions of the proteinogenic amino acids, suggest that terrestrial biological contamination is a primary source of the

  11. Improvement of (31)P NMR spectral resolution by 8-hydroxyquinoline precipitation of paramagnetic Fe and Mn in environmental samples.

    PubMed

    Ding, Shiming; Xu, Di; Li, Bin; Fan, Chengxin; Zhang, Chaosheng

    2010-04-01

    Solution (31)P nuclear magnetic resonance (NMR) spectroscopy is currently the main method for the characterization of phosphorus (P) forms in environment samples. However, identification and quantification of P compounds may be hampered by poor resolution of spectra caused by paramagnetic Fe and Mn. In this study, a novel technique was developed to improve spectral resolution by removing paramagnetic Fe and Mn from alkaline extracts via 8-hydroxyquinoline (8-HOQ) precipitation. Batch experiments showed that both Fe and Mn were effectively removed by the precipitation at pH 9.0, with the removal efficiencies of 83-91% for Fe and 67-78% for Mn from the extracts of five different environmental samples, while little effect was found on concentration of total P. The (31)P NMR analysis of a model P solution showed that addition of 8-HOQ and its precipitation with metal ions did not alter P forms. Further analyses of the five extracts with (31)P NMR spectroscopy demonstrated that the 8-HOQ precipitation was an ideal method compared with the present postextraction techniques, such as bicarbonate dithionate (BD), EDTA and Chelex-100 treatments, by improving spectral resolution to a large extent with no detrimental effects on P forms.

  12. Multi-Element Preconcentration/Separation of Some Metal Ions in Environmental Samples by Using Co-precipitation.

    PubMed

    Soylak, Mustafa; Aydin, Ayse; Kizil, Nebiye

    2016-01-01

    A preconcentration/separation system for cadmium(II), nickel(II), copper(II), lead(II), iron(II), cobalt(II), and manganese(II) ions has been established prior to their atomic absorption spectrometric determinations. The procedure is based on the co-precipitation of these ions by the aid of a praseodymium hydroxide (Pr(OH)3) precipitate. The precipitate was dissolved in 0.5 mL of concentrated HNO3, and made up to 10.0 mL with water. The analytes were determined by a flame atomic absorption spectrometer. The effects of analytical parameters including pH, amounts of praseodymium as carrier element, sample volume, etc. on the recoveries of heavy metals were investigated. The effects of matrix ions were also examined. The limits of detection for analyte ions were found in the range between 0.7-5.2 μg/L. The validation of this present procedure was verified by the analysis of certified reference materials, TMDA-54.4 (fortified water) and NIST 1570a (spinach leaves). The proposed co-precipitation procedure was applied for the determination of cadmium(II), nickel(II), copper(II), lead(II), iron(II), cobalt(II), and manganese(II) ions in various environmental water samples.

  13. National Acid Precipitation Assessment Program Report to Congress: An Integrated Assessment

    SciTech Connect

    Uhart, M.; et al,

    2005-08-01

    Under Title IX of the 1990 Clean Air Act Amendments, Congress reauthorized the National Acid Precipitation Assessment Program (NAPAP) to continue coordinating acid rain research and monitoring, as it had done during the previous decade, and to provide Congress with periodic reports. In particular, Congress asked NAPAP to assess all available data and information to answer two questions: (1) What are the costs, benefits, and effectiveness of Title IV? This question addresses the costs and economic impacts of complying with the Acid Rain Program as well as benefit analyses associated with the various human health and welfare effects, including reduced visibility, damages to materials and cultural resources, and effects on ecosystems. (2) What reductions in deposition rates are needed to prevent adverse ecological effects? This complex questions addresses ecological systems and the deposition levels at which they experience harmful effects. The results of the assessment of the effects of Title IV and of the relationship between acid deposition rates and ecological effects were to be reported to Congress quadrennially, beginning with the 1996 report to Congress. The objective of this Report is to address the two main questions posed by Congress and fully communicate the results of the assessment to decision-makers. Given the primary audience, most of this report is not written as a technical document, although information supporting the conclusions is provided along with references.

  14. Precipitation of Metallic Cations by the Acidic Exopolysaccharides from Bradyrhizobium japonicum and Bradyrhizobium (Chamaecytisus) Strain BGA-1

    PubMed Central

    Corzo, J.; León-Barrios, M.; Hernando-Rico, V.; Gutierrez-Navarro, A. M.

    1994-01-01

    The interaction between the acidic exopolysaccharides produced by two Bradyrhizobium strains and several metal cations has been studied. Aqueous solutions in the millimolar range of Fe3+ but not of Fe2+ precipitated the exopolysaccharides from Bradyrhizobium (Chamaecytisus) strain BGA-1 and, to a lesser extent, Bradyrhizobium japonicum USDA 110. The precipitation was pH dependent, with a maximum around pH 3. The precipitate was redissolved by changing the pH and by Fe3+ reduction or chelation. Deacetylation of B. japonicum polysaccharide increased its precipitation by Fe3+. At pH near neutrality, the polysaccharide from Bradyrhizobium (Chamaecytisus) strain BGA-1 stabilized Fe3+ solutions, despite the insolubility of Fe(OH)3. Aluminum precipitated Bradyrhizobium (Chamaecytisus) polysaccharide but not the polysaccharide produced by B. japonicum. The precipitation showed a maximum at about pH 4.8, and the precipitate was redissolved after Al3+ chelation with EDTA. Precipitation was inhibited by increases in the ionic strength over 10 mM. Bradyrhizobium (Chamaecytisus) polysaccharide was also precipitated by Th4+, Sn2+, Mn2+, and Co2+. The presence of Fe3+ increased the exopolysaccharide precipitation by aluminum. No precipitation, gelation, or increase in turbidity of polysaccharide solutions occurred when K+, Na+, Ca2+, Mg2+, Cu2+, Cd2+, Pb2+, Zn2+, Hg2+, or U6+ was added at several pH values. The results suggest that the precipitation is based on the interaction between carboxylate groups from different polysaccharide chains and the partially hydrolyzed aquoions of Fe3+, Al3+, Th4+, and Sn2+. PMID:16349466

  15. Performance of a pilot-scale wet electrostatic precipitator for the control of sulfuric acid mist.

    PubMed

    Huang, Jiayu; Wang, Hongmei; Shi, Yingjie; Zhang, Fan; Dang, Xiaoqing; Zhang, Hui; Shu, Yun; Deng, Shuang; Liu, Yu

    2016-10-01

    The use of a wet electrostatic precipitator (WESP) is often regarded as a viable option to reduce sulfuric acid mist emitted from the wet flue gas desulfurization (WFGD) tower in coal-fired power plants. In this study, a pilot-scale wet electrostatic precipitator equipped with a wall-cooled collection electrode is investigated for the control of sulfuric acid mist from a simulated WFGD system. The results show that due to partial charging effect, the removal efficiency of sulfuric acid aerosol decreases when the aerosol size decreases to several tens of nanometers. Moreover, due to the plasma-induced effect, a large number of ultrafine sulfuric acid aerosols below 50 nm formed at a voltage higher than 24 kV inside the WESP. The percentages of submicron-sized aerosols significantly increase together with the voltage. To minimize the adverse plasma-induced effect, a WESP should be operated at a high gas velocity with an optimum high voltage. Even at a high flue gas velocity of 2.3 m s(-1), the mass concentration and the total number concentration of uncaptured sulfuric acid aerosols at the WESP outlet are as low as ca. 0.6 mg m(-3) and ca. 10(4) 1 cm(-3) at 28 kV, respectively. The corresponding removal efficiencies were respectively higher than 99.4 and 99.9 % and are very similar to that at 1.1 and 1.6 m s(-1). Moreover, the condensation-induced aerosol growth enhances the removal of sulfuric acid mist inside a WESP and enables a low emission concentration of ca. 0.65 mg m(-3) with a corresponding removal efficiency superior to 99.4 % even at a low voltage of 21 kV, and of ca. 0.35 mg m(-3) with a corresponding removal efficiency superior to 99.6 % at a higher voltage level of 26 kV.

  16. Concentration of infectious hematopoietic necrosis virus from water samples by tangential flow filtration and polyethylene glycol precipitation

    USGS Publications Warehouse

    Batts, W.N.; Winton, J.R.

    1989-01-01

    Infectious hematopoietic necrosis virus (IHNV) was concentrated from water samples by polyethylene glycol (PEG) precipitation, tangential flow filtration (TFF), and by a combination of TFF followed by PEG precipitation of the retentate. Used alone, PEG increased virus titers more than 200-fold, and the efficiency of recovery was as great as 100%. Used alone, TFF concentrated IHNV more than 20-fold, and average recovery was 70%. When the two techniques were combined, 10-L water samples were reduced to about 300 mL by TFF and the virus was precipitated with PEG into a 1 to 2 g pellet; total recovery was as great as 100%. The combined techniques were used to isolate IHNV from water samples taken from a river containing adult sockeye salmon (Oncorhynchus nerka) and from a hatchery pond containing adult spring chinook salmon (O. tshawytscha). The combination of these methods was effective in concentrating and detecting IHNV from water containing only three infectious particles per 10-L sample.

  17. Application of dissolvable layered double hydroxides as sorbent in dispersive solid-phase extraction and extraction by co-precipitation for the determination of aromatic acid anions.

    PubMed

    Tang, Sheng; Lee, Hian Kee

    2013-08-06

    Three types of magnesium-aluminum layered double hydroxides were synthesized and employed as solid-phase extraction (SPE) sorbents to extract several aromatic acids (protocatechuic acid, mandelic acid, phthalic acid, benzoic acid, and salicylic acid) from aqueous samples. An interesting feature of these sorbents is that they dissolve when the pH of the solution is lower than 4. Thus, the analyte elution step, as needed in conventional sorbent-based extraction, was obviated by dissolving the sorbent in acid after extraction and separation from the sample solution. The extract was then directly injected into a high-performance liquid chromatography-ultraviolet detection system for analysis. In the key adsorption process, both dispersive SPE and co-precipitation extraction with the sorbents were conducted and experimental parameters such as pH, temperature, and extraction time were optimized. The results showed that both extraction methods provided low limits of detection (0.03-1.47 μg/L) and good linearity (r(2) > 0.9903). The optimized extraction conditions were applied to human urine and sports drink samples. This new and interesting extraction approach was demonstrated to be a fast and efficient procedure for the extraction of organic anions from aqueous samples.

  18. Preparation and characterization of micronized ellagic acid using antisolvent precipitation for oral delivery.

    PubMed

    Li, Yong; Zhao, Xiuhua; Zu, Yuangang; Zhang, Yin; Ge, Yunlong; Zhong, Chen; Wu, Weiwei

    2015-01-01

    In this work, poorly water soluble phytochemical ellagic acid (EA) was micronized to increase its solubility and thereby the bioavailability during antisolvent precipitation process using N-methyl pyrrolidone (NMP) as solvent and deionized water as antisolvent. The micronized EA (m-EA) freeze-dried powder was prepared by the subsequent lyophilization process. The effects of various experimental parameters on the mean particle size (MPS) of m-EA suspension (m-EAS) in the antisolvent precipitation process were investigated. MPS and production efficiency were taken into account comprehensively to obtain the optimum conditions of antisolvent precipitation. Under the optimum conditions, m-EA freeze-dried powder with a MPS of 429.2 ± 7.6 nm was obtained. The physico-chemical properties of m-EA freeze-dried powder were detected by scanning electron microscope (SEM), Fourier transform infrared spectroscopy (FTIR), liquid chromatography-tandem mass spectrometry (LC-MS/MS), X-ray diffraction (XRD), differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). The results indicated m-EA kept the same chemical structure with raw EA, but the crystallinity was greatly reduced. Furthermore, a comparison of the 50% inhibition concentration (IC50) values revealed that m-EA was more effective than raw EA in scavenging 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical. Meanwhile, m-EA also showed higher reducing power. Moreover, the residual amount of NMP was lower than the International Conference on Harmonization limit (530 ppm) for solvents. The dissolution rate of m-EA was approximately 2 times of raw EA. Moreover, the solubility of m-EA was about 6.5 times of raw EA. Meanwhile, the bioavailability of m-EA increased about 2 times compared with raw EA via oral administration.

  19. Microwave acid digestion and preconcentration neutron activation analysis of biological and diet samples for iodine.

    PubMed

    Rao, R R; Chatt, A

    1991-07-01

    A simple preconcentration neutron activation analysis (PNAA) method has been developed for the determination of low levels of iodine in biological and nutritional materials. The method involves dissolution of the samples by microwave digestion in the presence of acids in closed Teflon bombs and preconcentration of total iodine, after reduction to iodide with hydrazine sulfate, by coprecipitation with bismuth sulfide. The effects of different factors such as acidity, time for complete precipitation, and concentrations of bismuth, sulfide, and diverse ions on the quantitative recovery of iodide have been studied. The absolute detection limit of the PNAA method is 5 ng of iodine. Precision of measurement, expressed in terms of relative standard deviation, is about 5% at 100 ppb and 10% at 20 ppb levels of iodine. The PNAA method has been applied to several biological reference materials and total diet samples.

  20. Selective removal of phosphate for analysis of organic acids in complex samples.

    PubMed

    Deshmukh, Sandeep; Frolov, Andrej; Marcillo, Andrea; Birkemeyer, Claudia

    2015-04-03

    Accurate quantitation of compounds in samples of biological origin is often hampered by matrix interferences one of which occurs in GC-MS analysis from the presence of highly abundant phosphate. Consequently, high concentrations of phosphate need to be removed before sample analysis. Within this context, we screened 17 anion exchange solid-phase extraction (SPE) materials for selective phosphate removal using different protocols to meet the challenge of simultaneous recovery of six common organic acids in aqueous samples prior to derivatization for GC-MS analysis. Up to 75% recovery was achieved for the most organic acids, only the low pKa tartaric and citric acids were badly recovered. Compared to the traditional approach of phosphate removal by precipitation, SPE had a broader compatibility with common detection methods and performed more selectively among the organic acids under investigation. Based on the results of this study, it is recommended that phosphate removal strategies during the analysis of biologically relevant small molecular weight organic acids consider the respective pKa of the anticipated analytes and the detection method of choice.

  1. Purification of human immunoglobulins by sequential precipitation with caprylic acid and ammonium sulphate.

    PubMed

    Perosa, F; Carbone, R; Ferrone, S; Dammacco, F

    1990-03-27

    We have tested the usefulness of sequential precipitation with caprylic acid and ammonium sulfate to purify human monoclonal and polyclonal immunoglobulins from sera of 11 patients with monoclonal gammapathy (4 IgG kappa, 2 IgG lambda, 2 IgM kappa, 1 IgA kappa, 2 IgA lambda), four patients with autoimmune diseases and four healthy donors. In terms of purity and activity of Ig as well as execution time and cost, this two-step non-chromatographic procedure is highly efficient for the purification of IgG, IgA and IgM, thus offering several advantages over other methods of purification. Therefore, this procedure may have useful application in the preparation of human Ig for structural studies and therapeutic purposes.

  2. Determination of Cremophor EL in plasma after sample preparation with solid phase extraction and plasma protein precipitation.

    PubMed

    Meyer, T H; Böhler, J; Frahm, A W

    2001-01-01

    The non-ionic emulsifier Cremophor EL can be quantified using a special potentiometric titration technique with barium chloride activation and precipitation with sodium tetraphenylborate. The end point of the titration is indicated by an ionsensitive coated wire electrode which responds to an excess of tetraphenylborate ions. Sample preparation is necessary to quantify the excipient in plasma of patients receiving ciclosporin formulations with Cremophor EL (Sandimmun), since plasma proteins cause disturbances of the titration. Solid phase extraction was tested with various sorbent materials. Although some of the sorbents yielded good extraction rates of Cremophor EL from aqueous solutions, the extraction rates from plasma were significantly lower. Therefore, plasma protein precipitation with acetonitrile has been examined as an alternative to SPE and has been proved the superior method. Using the precipitation technique, a recovery rate of above 90% was achieved. Furthermore, the limit of detection from plasma was found to be 30 microg, in analogy to the determination from aqueous solutions. The combination of the plasma protein precipitation with the potentiometric titration allows quantitation and thus pharmakokinetic investigations of Cremophor EL in patients treated with Sandimmun after kidney-transplantation.

  3. Selective precipitation of potassium in seawater samples for improving the sensitivity of plain γ-ray spectrometry

    SciTech Connect

    Ferrante, Marco De Angelis, Francesco; Nisi, Stefano Laubenstein, Matthias

    2015-08-17

    An analytical method is presented to reduce the amount of {sup 40}K in sea water samples, in order to lower its interference in γ-ray analysis below 1.4 MeV due to the Compton continuum. Sodium tetraphenylborate was used to successfully precipitate {sup 40}K in the samples. A custom procedure for precipitation of potassium was developed and it was evaluated for its selectivity, reproducibility and efficiency, using conventional analytical techniques such as atomic absorption spectrophotometry and inductively coupled plasma mass spectrometry (ICP-MS). This work has shown that the selective precipitation of potassium with sodium tetraphenylborate has led to a decrease of detection limit of radio nuclides such as {sup 238}U, {sup 226}Ra, {sup 228}Ra, {sup 137}Cs, {sup 134}Cs, {sup 133}I, {sup 134}I, {sup 60}Co in γ-analysis. In particular, the detection limit for nuclides with emissions in the energy window energy below 1400 keV is improved by almost one order of magnitude.

  4. A study of the source-receptor relationships influencing the acidity of precipitation collected at a rural site in France

    NASA Astrophysics Data System (ADS)

    Charron, Aurélie; Plaisance, Hervé; Sauvage, Stéphane; Coddeville, Patrice; Galloo, Jean-Claude; Guillermo, René

    In order to examine the qualitative and quantitative source-receptor relationships responsible for acid rains at a background site in France, a receptor-oriented model was applied to the precipitation data collected from 1992 to 1995. Origins of acidic and alkaline species in precipitations have been investigated. The methodology combines precipitation chemical data with air parcel backward trajectories to establish concentration field maps of likely contributing sources. Highest acidities and concentrations of sulfate and nitrate in precipitation were associated with transport from the high emission areas of central Europe. Alkaline events were associated with air masses originating from Mediterranean basin or northern Africa. The quantitative relationships between the maps of potential sources and the European emissions of SO 2 and NO x were examined performing a correlation analysis. Good correlations were found between computed concentrations of acidic species and emissions of SO 2 and NO x. Substantial seasonal variations of acidic species were revealed. The highest concentrations occurred during the warm season. These seasonal variations are the effect of change of meteorological conditions and of the strength atmospheric processes according to the season.

  5. Environmental, mineralogical, and genetic characterization of ochreous and white precipitates from acid mine drainages in Taebaeg, Korea.

    PubMed

    Kim, Jeong Tin; Kim, Soo Jin

    2003-05-15

    X-ray diffraction, energy-dispersive X-ray fluorescence, thermal analysis, scanning electron microscopy, inductively coupled plasma emission spectroscopy, and ion chromatography were used for the environmental, mineralogical, and genetic characterization of brownish yellow, reddish brown, and white precipitates from acid mine drainage in Taebaeg, Korea. Ferrihydrite+goethite, schwertmannite, and Al-sulfate were precipitated under different chemical environments on the stream bottom of acid mine drainages. The brownish yellow precipitates (Munsell color 9.5YR hues) consist mainly of schwertmannite with traces of quartz, illite, pyrophyllite, goethite, lepidocrocite, and gypsum. The reddish brown precipitates (Munsell color 3.5YR hues) consist mainly of ferrihydrite with small amount of goethite. The white precipitates consist mainly of poorly crystalline Al-sulfate with small amounts of quartz, gypsum, and calcite. Thermal decomposition due to dehydration of ferrihydrite and schwertmannite takes place at approximately 120 degrees C and 140 degrees C, respectively. Al-sulfate converts to gamma-alumina at 850 degrees C. SEM study shows that the spheroid and rod-shaped precipitates characteristic of Gallionella consist of iron hydroxide with varying chemical compositions.

  6. Determination of Mycophenolic Acid in Plasma Samples Using the Terbium-Sensitized Luminescence Method

    NASA Astrophysics Data System (ADS)

    Shayanfar, A.; Ghavimi, H.; Zolali, E.; Jouyban, A.

    2015-09-01

    The objectives of this work were to provide an analytical method, for the quantitative determination of the mycophenolic acid (MFA) in plasma samples and its application to quantification of the MFA in rat plasma after oral administration. In order to remove the fluorescence interferences of the plasma, the samples were precipitated by acetonitrile in 1:8 ratio and then a few parameters were optimized and the fluorescence intensity measured at 545 nm using an excitation wavelength of 347 nm. Under the optimized concentration, the method provided a linear range between 1.0 and 10.0 mg/l with a correlation coefficient of 0.998. MFA was detected and the validation was performed according to the FDA guidelines. Linearity, accuracy, precision, and selectivity of the developed method were suitable for th determination of the MFA in plasma samples. The proposed analytical approach was applied to determine the MFA concentration in a rat plasma-time profile study.

  7. A simple procedure for preparing chitin oligomers through acetone precipitation after hydrolysis in concentrated hydrochloric acid.

    PubMed

    Kazami, Nao; Sakaguchi, Masayoshi; Mizutani, Daisuke; Masuda, Tatsuhiko; Wakita, Satoshi; Oyama, Fumitaka; Kawakita, Masao; Sugahara, Yasusato

    2015-11-05

    Chitin oligomers are of interest because of their numerous biologically relevant properties. To prepare chitin oligomers containing 4-6 GlcNAc units [(GlcNAc)4-6], α- and β-chitin were hydrolyzed with concentrated hydrochloric acid at 40 °C. The reactant was mixed with acetone to recover the acetone-insoluble material, and (GlcNAc)4-6 was efficiently recovered after subsequent water extraction. Composition analysis using gel permeation chromatography and MALDI-TOF mass spectrometry indicated that (GlcNAc)4-6 could be isolated from the acetone-insoluble material with recoveries of approximately 17% and 21% from the starting α-chitin and β-chitin, respectively. The acetone precipitation method is highly useful for recovering chitin oligomers from the acid hydrolysate of chitin. The changes in the molecular size and higher-order structure of chitin during the course of hydrolysis were also analyzed, and a model that explains the process of oligomer accumulation is proposed.

  8. Weathering processes and pickeringite formation in a sulfidic schist: a consideration in acid precipitation neutralization studies

    SciTech Connect

    Parnell, R.A. Jr.

    1983-01-01

    Extremely low abrasion pH values (2.8-3.3) characterize the weathering products of the Partridge Formation, a Middle-Ordovician metamorphosed, black, sulfidic shale. The local occurrence is observed of two sulfates that are rare in the Northeast: pickeringite and jarosite. X-ray diffraction studies of the weathering residues and the sulfate efflorescences have also identified dioctahedral and trioctahedral illite, kaolinite, vermiculite, and an 11-12 Angstrom phase, thought to be a type of randomly-interstratified biotite-vermiculite. From the mineralogical studies, qualitative weathering processes for the schist are formulated. A probable mechanism for the intense chemical weathering of the schist appears to be oxidation of iron sulfides to form iron oxide-hydroxides, sulfates, and sulfuric acid. This natural weathering process is proposed as an analog to anthropogenic low pH rock weathering resulting from acid precipitation. In the Northeast, natural weathering rates, may, in places, significantly affect the water chemistry and mineralogy used to quantify total (natural plus anthropogenic) weathering and leaching rates. 27 references, 4 figures.

  9. Sample pretreatment for the capillary electrophoretic determination of organic acids in chromium(III) plating baths.

    PubMed

    Taraba, Lukáš; Křížek, Tomáš; Kubíčková, Anna; Coufal, Pavel

    2015-12-01

    This work deals with the development and optimization of the sample pretreatment and consequent electrophoretic analysis of two modern plating baths containing chromium(III) and either citric acid or oxalic acid. Some model mixtures containing known amounts of components of industrial baths have been prepared to simulate simplified bath matrices. Prior to analysis, a sample pretreatment consisting of the addition of some agents that could release acid from the stable chromium complex was tested. Determination of organic anions was accomplished by indirect UV detection. The best results were achieved by precipitation of chromium(III) hydroxide. The content of oxalate and citrate in real samples was calculated as 96.5% (SD 2.3%) and 97.3% (SD 0.8%), respectively, of the declared amount. Very good robustness of the method and satisfactory repeatability of migration time and peak area were obtained. This simple inexpensive method is suitable for routine determination of citric and oxalic acid in chromium(III)-based plating baths.

  10. Aquatic hazard assessment of a commercial sample of naphthenic acids.

    PubMed

    Swigert, James P; Lee, Carol; Wong, Diana C L; White, Russell; Scarlett, Alan G; West, Charles E; Rowland, Steven J

    2015-04-01

    This paper presents chemical composition and aquatic toxicity characteristics of a commercial sample of naphthenic acids (NAs). Naphthenic acids are derived from the refining of petroleum middle distillates and can contribute to refinery effluent toxicity. NAs are also present in oil sands process-affected water (OSPW), but differences in the NAs compositions from these sources precludes using a common aquatic toxicity dataset to represent the aquatic hazards of NAs from both origins. Our chemical characterization of a commercial sample of NAs showed it to contain in order of abundance, 1-ring>2-ring>acyclic>3-ring acids (∼84%). Also present were monoaromatic acids (7%) and non-acids (9%, polyaromatic hydrocarbons and sulfur heterocyclic compounds). While the acyclic acids were only the third most abundant group, the five most abundant individual compounds were identified as C(10-14) n-acids (n-decanoic acid to n-tetradecanoic acid). Aquatic toxicity testing of fish (Pimephales promelas), invertebrate (Daphnia magna), algae (Pseudokirchneriella subcapitata), and bacteria (Vibrio fischeri) showed P. promelas to be the most sensitive species with 96-h LL50=9.0 mg L(-1) (LC50=5.6 mg L(-1)). Acute EL50 values for the other species ranged 24-46 mg L(-1) (EC50 values ranged 20-30 mg L(-1)). Biomimetic extraction via solid-phase-microextraction (BE-SPME) suggested a nonpolar narcosis mode of toxic action for D. magna, P. subcapitata, and V. fischeri. The BE analysis under-predicted fish toxicity, which indicates that a specific mode of action, besides narcosis, may be a factor for fishes.

  11. [Characterization and analysis of direction extraction and precipitation of cerium loading organic phase by oxalic acid solution].

    PubMed

    Mei, Yan; Xia, Chuan; Chen, Xiao-Li; Sun, He; Nie, Zuo-Ren

    2011-11-01

    In the condition of sodium hydroxide saponification, the test results using direction extraction and precipitation of cerium from P507 loading organic phase by oxalic acid solution were studied. Infared (IR) spectrum, X-ray diffraction (XRD), transmission electron microscope (TEM) and thermogravimetry (TG-DSC) were used to study and characterize organic cerium precipitates and the final calcined products. The results showed that organic cerium precipitates and final calcined products were spheric organic cerium coordination and spheric cube CeO2 crystal, respectively, showing their morphologies were successive. IR made out that the structures of organic cerium precipitates and final calcined products were different. TG-DSC indicated that the final calcined products weightlessness was 3.5% and chemical composing was CeO2 x 1/3H2O.

  12. Effects of nitrate and water on the oxygen isotopic analysis of barium sulfate precipitated from water samples.

    PubMed

    Hannon, Janet E; Böhlke, John Karl; Mroczkowski, Stanley J

    2008-12-01

    BaSO(4) precipitated from mixed salt solutions by common techniques for SO(4) (2-) isotopic analysis may contain quantities of H(2)O and NO(3) (-) that introduce errors in O isotope measurements. Experiments with synthetic solutions indicate that delta(18)O values of CO produced by decomposition of precipitated BaSO(4) in a carbon reactor may be either too low or too high, depending on the relative concentrations of SO(4) (2-) and NO(3) (-) and the delta(18)O values of the H(2)O, NO(3) (-), and SO(4) (2-). Typical delta(18)O errors are of the order of 0.5 to 1 per thousand in many sample types, and can be larger in samples containing atmospheric NO(3) (-), which can cause similar errors in delta(17)O and Delta(17)O. These errors can be reduced by (1) ion chromatographic separation of SO(4) (2-) from NO(3) (-), (2) increasing the salinity of the solutions before precipitating BaSO(4) to minimize incorporation of H(2)O, (3) heating BaSO(4) under vacuum to remove H(2)O, (4) preparing isotopic reference materials as aqueous samples to mimic the conditions of the samples, and (5) adjusting measured delta(18)O values based on amounts and isotopic compositions of coexisting H(2)O and NO(3) (-). These procedures are demonstrated for SO(4) (2-) isotopic reference materials, synthetic solutions with isotopically known reagents, atmospheric deposition from Shenandoah National Park, Virginia, USA, and sulfate salt deposits from the Atacama Desert, Chile, and Mojave Desert, California, USA. These results have implications for the calibration and use of O isotope data in studies of SO(4) (2-) sources and reaction mechanisms.

  13. Effects of nitrate and water on the oxygen isotopic analysis of barium sulfate precipitated from water samples

    USGS Publications Warehouse

    Hannon, J.E.; Böhlke, J.K.; Mroczkowski, S.J.

    2008-01-01

    BaSO4 precipitated from mixed salt solutions by common techniques for SO42- isotopic analysis may contain quantities of H2O and NO3- that introduce errors in O isotope measurements. Experiments with synthetic solutions indicate that ??18O values of CO produced by decomposition of precipitated BaSO4 in a carbon reactor may be either too low or too high, depending on the relative concentrations of SO42- and NO3- and the ??18O values of the H2O, NO3-, and SO42-. Typical ??18O errors are of the order of 0.5 to 1??? in many sample types, and can be larger in samples containing atmospheric NO 3-, which can cause similar errors in ?? 17O and ??17O. These errors can be reduced by (1) ion chromatographic separation of SO42- from NO 3-, (2) increasing the salinity of the solutions before precipitating BaSO4 to minimize incorporation of H2O, (3) heating BaSO4 under vacuum to remove H2O, (4) preparing isotopic reference materials as aqueous samples to mimic the conditions of the samples, and (5) adjusting measured ??18O values based on amounts and isotopic compositions of coexisting H2O and NO 3-. These procedures are demonstrated for SO 42- isotopic reference materials, synthetic solutions with isotopically known reagents, atmospheric deposition from Shenandoah National Park, Virginia, USA, and sulfate salt deposits from the Atacama Desert, Chile, and Mojave Desert, California, USA. These results have implications for the calibration and use of O isotope data in studies of SO42- sources and reaction mechanisms.

  14. Integrated Lake-Watershed Acidification Study (ILWAS): contributions to the international conference on the ecological impact of acid precipitation

    SciTech Connect

    Not Available

    1981-05-01

    The Integrated Lake-Watershed Acidification Study (ILWAS) was initiated to study and detail lake acidification processes for three lake watershed basins in the Adirondack Park region of New York. The three basins (Woods, Sagamore, and Panther), receive similar amounts of acid deposition yet observable pH values for the lakes are very dissimilar indicating unequal acid neutralizing capacities among the watersheds. This volume contains a compilation of seven papers. Relevant topics include: a characterization of the geology, hydrology, limnology and vegetation of the three study sites, an analysis of acid precipitation quality and quantity, the effects of vegetative canopy, the effects of snowmelt, the effects of winter lake stratification, comparison of heavy metal transport, examination of acidic sources other than direct precipitation, assessment of lake acidification during spring thaw and integration of all acidification components with a mathematical model.

  15. Sampling the oxidative weathering products and the potentially acidic permafrost on Mars

    NASA Technical Reports Server (NTRS)

    Burns, Roger G.

    1988-01-01

    Large areas of Mars' surface are covered by oxidative weathering products containing ferric and sulfate ions having analogies to terrestrial gossans derived from sulfide mineralization associated with iron-rich basalts. Chemical weathering of such massive and disseminated pyrrhotite-pentlandite assemblages and host basaltic rocks in the Martian environment could have produced metastable gossaniferous phases (limonite containing poorly crystalline hydrated ferric sulfates and oxyhydroxides, clay silicates and opal). Underlying groundwater, now permafrost on Mars, may still be acidic due to incomplete buffering reactions by wall-rock alteration of unfractured host rock. Such acidic solutions stabilize temperature-sensitive complex ions and sols which flocculate to colloidal precipitates at elevated temperatures. Sampling procedures of Martian regolith will need to be designed bearing in mind that the frozen permafrost may be corrosive and be stabilizing unique complex ions and sols of Fe, Al, Mg, Ni and other minor elements.

  16. Determination of malic acid and other C4 dicarboxylic acids in atmospheric aerosol samples.

    PubMed

    Röhrl, Andreas; Lammel, Gerhard

    2002-03-01

    An ion chromatographic method was developed which is able to separate five unsubstituted and hydroxy C4 dicarboxylic acids, succinic, malic, tartaric, maleic and fumaric acid, besides the other unsubstituted C2-C5 dicarboxylic acids, oxalic, malonic and glutaric acids, as well as inorganic ions in samples extracted from atmospheric particulate matter. By the application of this method it was found for both rural and urban sites and for various types of air masses that in the summer-time malic acid is the most prominent C4 diacid (64 ng m(-3) by average), exceeding succinic acid concentration (28 ng m(-3) by average) considerably. In winter-time considerably less, a factor of 4-15, C4 acids occurred and succinic acid was more concentrated than malic acid. Tartaric, fumaric and maleic acids were less concentrated (5.1, 5.0 and 4.5 ng m(-3) by average, respectively). Tartaric acid was observed for the first time in ambient air. The results indicate that in particular anthropogenic sources are important for the precursors of succinic, maleic and fumaric acids. Biogenic sources seem to influence the occurrence of malic acid significantly.

  17. [Formation and environmental implications of iron-enriched precipitates derived from natural neutralization of acid mine drainage].

    PubMed

    Zhou, Yue-Fei; Xie, Yue; Zhou, Li-Xiang

    2010-06-01

    Acid mine drainage (AMD) and its natural neutralizing products in Wangjiatan iron mine were collected and analyzed by using spectroscopic and electron microanalytic methods. The results show that after natural neutralization of AMD by surface water of the stream, acidity and electric conductivity of AMD are both decreased. While for dissolved elements, no other element is obviously decreased except for Fe3+, SO4(2-), and Ca2+. For precipitates formed by natural neutralization, Fe is enriched and ferrihydrite is the main iron mineral, with little amount of goethite and fibroferrite contained in downstream precipitates. To ferrihydrite, 2-line and 6-line ferrihydrite are the main mineral type in upstream and downstream precipitates, respectively. Furthermore, for all precipitates, two layers are observed. In outer layer 2-line ferrihydrite is the main mineral, while in inner layer 6-line ferrihydrite and goethite are the main minerals. Ferrihydrite dominated precipitates are favorable in immobilizing toxic and hazardous elements. Furthermore, it is demonstrated that pH and the concentration of SO4(2-) are decisive factors for ferrihydrite formation. The ferrihydrite translocation and its attenuation for toxic elements are, to a great extent, affected by hydrodynamics in neutralization zone.

  18. An assessment of the isotopic (2H/18O) integrity of water samples collected and stored by unattended precipitation totalizers

    NASA Astrophysics Data System (ADS)

    Terzer, Stefan; Wassenaar, Leonard I.; Douence, Cedric; Araguas-Araguas, Luis

    2016-04-01

    The IAEA-WMO Global Network of Isotopes in Precipitation (GNIP) provides worldwide δ18O and δ2H data for numerous hydrological and climatological studies. The traditional GNIP sample collection method relies on weather station operators to accumulate precipitation obtained from manual rain gauges. Over the past decades, widespread weather station automatization resulted in the increased use of unattended precipitation totalizers that accumulate and store the rainwater in the field for up to one month. Several low-tech measures were adopted to prevent in situ secondary evaporative isotopic enrichment (SEE) of totalized water samples (i.e. disequilibrium isotopic fractionation after precipitation is stored in the collection device). These include: (a) adding a 0.5-1 cm floating layer of paraffin oil to the totalizer bottle, (b) using an intake tube leading from the collection funnel and submerged to the bottom of the totalizer bottle, or (c) placing a table tennis ball in the funnel aiming to reduce evaporation of the collected water from the receiving bottle to the atmosphere. We assessed the isotopic integrity of stored rainwater samples for three totalizers under controlled settings: each aforementioned totalizer was filled with a 100 or 500 mL of isotopically known water and installed in the field with the intake funnels sheltered to prevent rainwater collection. Potential evapotranspiration (PET) was obtained from on-site meteorological recordings. Stored evaporative loss from each totalizer was evaluated on a monthly basis; gravimetrically and by analysing δ18O and δ2H of the stored water, for a period of 6 months and a cumulative PET of ˜500 mm. The gravimetric and isotope results revealed that for smaller water volumes (100 ml, corresponding to ca. 5 mm of monthly precipitation), negligible isotope enrichment (δ18O) was observed in the paraffin-oil based totalizer, whereas unacceptable evaporative isotope effects were observed for the ball

  19. Comparison of Four Strong Acids on the Precipitation Potential of Gypsum in Brines During Distillation of Pretreated, Augmented Urine

    NASA Technical Reports Server (NTRS)

    Muirhead, Dean; Carrier, Christopher

    2012-01-01

    In this study, three different mineral acids were substituted for sulfuric acid (H2SO4) in the urine stabilizer solution to eliminate the excess of sulfate ions in pretreated urine and assess the impact on maximum water recovery to avoid precipitation of minerals during distillation. The study evaluated replacing 98% sulfuric acid with 85% phosphoric acid (H3PO4), 37% hydrochloric acid (HCl), or 70% nitric acid (HNO3). The effect of lowering the oxidizer concentration in the pretreatment formulation also was studied. This paper summarizes the test results, defines candidate formulations for further study, and specifies the injection masses required to stabilize urine and minimize the risk of mineral precipitation during distillation. In the first test with a brine ersatz acidified with different acids, the solubility of calcium in gypsum saturated solutions was measured. The solubility of gypsum was doubled in the brines acidified with the alternative acids compared to sulfuric acid. In a second series of tests, the alternative acid pretreatment concentrations were effective at preventing precipitation of gypsum and other minerals up to 85% water recovery from 95th-percentile pretreated, augmented urine. Based on test results, phosphoric acid is recommended as the safest alternative to sulfuric acid. It also is recommended that the injected mass concentration of chromium trioxide solution be reduced by 75% to minimize liquid resupply mass by about 50%, reduce toxicity of brines, and reduce the concentration of organic acids in distillate. The new stabilizer solution formulations and required doses to stabilize urine and prevent precipitation of minerals up to 85% water recovery are given. The formulations in this study were tested on a limited number of artificially augmented urine batches collected from employees at the Johnson Space Center (JSC). This study successfully demonstrated that the desired physical and chemical stability of pretreated urine and brines

  20. Geological and hydrochemical sensitivity of the eastern United States to acid precipitation

    SciTech Connect

    Hendrey, G.R.; Galloway, J.N.; Norton, S.A.; Schofield, C.L.; Shaffer, P.W.; Burns, D.A.

    1980-03-01

    A new analysis of bedrock geology maps of the eastern US constitutes a simple model for predicting areas which might be impacted by acid precipitation and it allows much greater resolution for detecting sensitivity than has previously been available for the region. Map accuracy has been verified by examining current alkalinities and pH's of waters in several test states, including Maine, New Hampshire, New York, Virginia and North Carolina. In regions predicted to be highly sensitive, alkalinities in upstream sites were generally low. Many areas of the eastern US are pinpointed in which some of the surface waters, especially upstream reaches, may be sensitive to acidification. Pre-1970 data were compared to post-1975 data, revealing marked declines in both alkalinity and pH of sensitive waters of two states tested, North Carolina, where pH and alkalinity have decreased in 80% of 38 streams and New Hampshire, where pH in 90% of 49 streams and lakes has decreased since 1949. These sites are predicted to be sensitive by the geological map on the basis of their earlier alkalinity values. The map is to be improved by the addition of a soils component.

  1. Selective recovery of soil-borne metal contaminants through integrated solubilization by biogenic sulfuric acid and precipitation by biogenic sulfide.

    PubMed

    Fang, Di; Zhang, Ruichang; Liu, Xue; Zhou, Lixiang

    2012-06-15

    A hybrid process combining solubilization via sulfuric acid produced by sulfur-oxidizing bacteria with precipitation via sulfide produced by sulfate-reducing bacteria was investigated to isolate soil-borne metal contaminants as purified metal-sulfides. The highly efficient two-step acidification process involved bioproduction of sulfuric acid in a culture medium containing 30% (v/v) of sludge filtrate (SF). Soil was added to the culture after maximum acid production. Solubilization efficiencies of 95% for Zn, 76% for Cu and 97% for Cd were achieved after 16 days. At pH 1.9, 3.0 and 4.0, 99% of Cu(2+), 96% of Cd(3+) and 93% of Zn(2+), respectively, were precipitated from the soil leachate by sulfide transported from sulfidogenic bioreactor via N(2) sparging, resulting in final effluent metal contents at the ppb-level. The introduction of SF did not affect the precipitation kinetics and purity of the recovered precipitates. Ultimately, 75% of Cu and 86% of Zn were recovered from the soil as pure CuS and ZnS (confirmed by SEM-EDS and XRD). These results demonstrate the potential of the integrated method for the selective production of valuable metals from metal contamination in soils.

  2. Effects of Race and Precipitating Event on Suicide versus Nonsuicide Death Classification in a College Sample

    ERIC Educational Resources Information Center

    Walker, Rheeda L.; Flowers, Kelci C.

    2011-01-01

    Race group differences in suicide death classification in a sample of 109 Black and White university students were examined. Participants were randomly assigned to read three vignettes for which the vignette subjects' race (only) varied. The vignettes each described a circumstance (terminal illness, academic failure, or relationship difficulties)…

  3. Historic volcanism, European dry fogs, and greenland Acid precipitation, 1500 B.C. To a.d. 1500.

    PubMed

    Stothers, R B; Rampino, M R

    1983-10-28

    Historic dry fogs in Europe, acid precipitation in Greenland, and major explosive volcanic eruptions correlate well with each other between 1500 B.C. and A.D. 1500. European (Mediterranean and Icelandic) volcanic eruptions appear to be the source of at least five of the nine largest acidity signals found in Greenland ice for this period. Between 152 B.C. and A.D. 43, eruptions of sulfur-rich Mount Etna probably supplied about 15 percent of the smaller acidity signals.

  4. Nucleic Acid Sample Preparation using Spontaneous Biphasic Plug Flow

    PubMed Central

    Thomas, Peter C.; Strotman, Lindsay N.; Theberge, Ashleigh B.; Berthier, Erwin; O’Connell, Rachel; Loeb, Jennifer M.; Berry, Scott M.; Beebe, David J.

    2013-01-01

    Nucleic acid (NA) extraction and purification has become a common technique in both research and clinical laboratories. Current methods require repetitive wash steps with a pipette that is laborious and time consuming making it inefficient for clinical settings. We present here a simple technique that relies on spontaneous biphasic plug flow inside a capillary to achieve sample preparation. By filling the sample with oil, aqueous contaminants were displaced from the captured NA without pipetting wash buffers or use of external force and equipment. mRNA from mammalian cell culture was purified and PCR amplification showed similar threshold cycle values as those obtained from a commercially available kit. HIV viral like particles were spiked into serum and a 5-fold increase in viral RNA extraction yield was achieved compared to the conventional wash method. In addition, viral RNA was successfully purified from human whole blood, and a limit of detection of approximately 14 copies of RNA extracted per sample. The results demonstrate the utility of the current technique for nucleic acid purification for clinical purposes, and the overall approach provides a potential method to implement nucleic acid testing in low resource settings. PMID:23941230

  5. Nucleic acid sample preparation using spontaneous biphasic plug flow.

    PubMed

    Thomas, Peter C; Strotman, Lindsay N; Theberge, Ashleigh B; Berthier, Erwin; O'Connell, Rachel; Loeb, Jennifer M; Berry, Scott M; Beebe, David J

    2013-09-17

    Nucleic acid (NA) extraction and purification has become a common technique in both research and clinical laboratories. Current methods require repetitive wash steps with a pipet that are laborious and time-consuming, making the procedure inefficient for clinical settings. We present here a simple technique that relies on spontaneous biphasic plug flow inside a capillary to achieve sample preparation. By filling the sample with oil, aqueous contaminants were displaced from the captured NA without pipetting wash buffers or use of external force and equipment. mRNA from mammalian cell culture was purified, and polymerase chain reaction (PCR) amplification showed similar threshold cycle values as those obtained from a commercially available kit. Human immunodeficiency virus (HIV) viral-like particles were spiked into serum and a 5-fold increase in viral RNA extraction yield was achieved compared to the conventional wash method. In addition, viral RNA was successfully purified from human whole blood, and a limit of detection of approximately 14 copies of RNA extracted per sample was determined. The results demonstrate the utility of the current technique for nucleic acid purification for clinical purposes, and the overall approach provides a potential method to implement nucleic acid testing in low-resource settings.

  6. Survival of Listeria innocua in rainbow trout protein recovered by isoelectric solubilization and precipitation with acetic and citric acids.

    PubMed

    Otto, R A; Paker, I; Bane, L; Beamer, S; Jaczynski, J; Matak, K E

    2011-08-01

    During mechanical fish processing, a substantial amount of protein is discarded as by-products. Isoelectric solubilization and precipitation (ISP) is a process that uses extreme pH shifts to solubilize and precipitate protein from by-products to recover previously discarded protein. Typically, strong acids are used for pH reduction, but these acids do not have a pasteurization effect (6 log reduction) on bacterial load; therefore, organic acids were used during ISP processing to test the impact on Listeria innocua concentrations. Headed and gutted rainbow trout (Oncorhynchus mykiss) were inoculated with L. innocua, homogenized, and brought to the target pH with granular citric acid (pH 2.0 and 2.5) or glacial acetic acid (pH 3.0 and 3.5). Proteins were solubilized for 10 min at 4°C, and insoluble components (e.g., skin and insoluble protein) were removed by centrifugation. The remaining solution was pH shifted to the protein isoelectric point (pH 5.5) with sodium hydroxide, and precipitated protein was separated from the water. Microbial cells for each component (proteins, insolubles, and water) were enumerated on modified Oxford agar (MOX) and tryptic soy agar with 6% yeast extract (TSAYE). The sums of the surviving cells from each component were compared with the initial inoculum levels. No significant differences were observed between results obtained from TSAYE and from MOX (P > 0.05). Significant reductions in microbial populations were detected, regardless of pH or acid type (P < 0.05). The greatest reduction was at pH 3.0 with glacial acetic acid, resulting in a mean reduction of 6.41 log CFU/g in the recovered protein and 5.88 log CFU/g in the combined components. These results demonstrate the antimicrobial potential of organic acids in ISP processing.

  7. Increased amplification success from forensic samples with locked nucleic acids.

    PubMed

    Ballantyne, Kaye N; van Oorschot, Roland A H; Mitchell, R John

    2011-08-01

    Inadequate sample quantities and qualities can commonly result in poor DNA amplification success rates for forensic case samples. In some instances, modifying the PCR protocol or components may assist profiling by overcoming inhibition, or reducing the threshold required for successful amplification and detection. Incorporation of locked nucleic acids (LNAs) into PCR primers has previously been shown to increase amplification success for a range of non-forensic sample types and applications. To investigate their use in a forensic context, the PCR primers for four commonly used STR loci have been redesigned to include LNA bases. The modified LNA primers provided significantly increased amplification success when compared to standard DNA primers, with both high-quality buccal samples and simulated forensic casework samples. Peak heights increased by as much as 5.75× for the singleplex amplifications. When incorporated into multiplexes, the LNA primers continued to outperform standard DNA primers, with increased ease of optimisation, and increased amplification success. The use of LNAs in PCR primers can greatly assist the profiling of a range of samples, and increase success rates from challenging forensic samples.

  8. Determination of cadmium in grains by isotope dilution ICP-MS and coprecipitation using sample constituents as carrier precipitants.

    PubMed

    Inagaki, Kazumi; Narukawa, Tomohiro; Yarita, Takashi; Takatsu, Akiko; Okamoto, Kensaku; Chiba, Koichi

    2007-10-01

    A coprecipitation method using sample constituents as carrier precipitants was developed that can remove molybdenum, which interferes with the determination of cadmium in grain samples via isotope dilution inductively coupled plasma mass spectrometry (ID-ICPMS). Samples were digested with HNO3, HF, and HClO4, and then purified 6 M sodium hydroxide solution was added to generate colloidal hydrolysis compounds, mainly magnesium hydroxide. Cadmium can be effectively separated from molybdenum because the cadmium forms hydroxides and adsorbs onto and/or is occluded in the colloid, while the molybdenum does not form hydroxides or adsorb onto the hydrolysis colloid. The colloid was separated by centrifugation and then dissolved with 0.2 M HNO3 solution to recover the cadmium. The recovery of Cd achieved using the coprecipitation was >97%, and the removal efficiency of Mo was approximately 99.9%. An extremely low procedural blank (below the detection limit of ICPMS) was achieved by purifying the 6 M sodium hydroxide solution via Mg coprecipitation using Mg(NO3)2 solution. The proposed method was applied to two certified reference materials (NIST SRM 1567a wheat flour and SRM 1568a rice flour) and CCQM-P64 soybean powder. Good analytical results with small uncertainties were obtained for all samples. This method is simple and reliable for the determination of Cd in grain samples by ID-ICPMS.

  9. Effects of race and precipitating event on suicide versus nonsuicide death classification in a college sample.

    PubMed

    Walker, Rheeda L; Flowers, Kelci C

    2011-02-01

    Race group differences in suicide death classification in a sample of 109 Black and White university students were examined. Participants were randomly assigned to read three vignettes for which the vignette subjects' race (only) varied. The vignettes each described a circumstance (terminal illness, academic failure, or relationship difficulties) that preceded the vignette subject's ambiguously premature death. Participants were asked to describe "what happened." Black participants were significantly less likely than White participants to attribute a vignette target's death to suicide and also less likely to report that suicide is acceptable. Implications for future research and prevention efforts are discussed.

  10. Soluble species in the Arctic summer troposphere: Acidic gases, aerosols, and precipitation

    NASA Astrophysics Data System (ADS)

    Talbot, R. W.; Vijgen, A. S.; Harriss, R. C.

    1992-10-01

    with mid-latitude source regions was previously believed to be minimal. Stratospheric inputs may also be important as a source of Arctic tropospheric SO42-. On several occasions we sampled directly within plumes or highly contaminated air masses representing various anthropogenic sources. The composition of these pollution sources suggested that they were important in determining the large-scale distribution of acidic gases and aerosol species in the Arctic summer troposphere. Outside the plumes the anthropogenic influences are chemically diffuse and variable, making it very difficult to quantitatively ascertain the magnitude of the effects. Present-day "background" air during summertime in the North American Arctic and sub-Arctic mid-troposphere appears to have the following average composition (parts per trillion by volume): HCOOH (70), CH3COOH (70), HNO3 (40), NO3- (10), SO42- (25), and NH4+ (55). These concentrations which were observed on only a few isolated days can be compared to the grand average (Arctic and sub-Arctic) mid-tropospheric levels during July-August 1988: HCOOH (166 ± 81), CH3COOH (215 ± 90), HNO3 (48 ± 29), NO3- (22 ± 17), SO42- (61 ± 30), and NH4+ (68 ± 30). A "first-look" comparison of the large-scale mid-tropospheric composition in a remote area of the northern hemisphere with that over a remote region of the southern hemisphere, the Amazon Basin, suggests no identifiable difference in the levels of NH4+ but possibly twofold and fivefold enhancement of NO3- and SO42- in "background" air for North America.

  11. WACCM-D—Improved modeling of nitric acid and active chlorine during energetic particle precipitation

    NASA Astrophysics Data System (ADS)

    Andersson, M. E.; Verronen, P. T.; Marsh, D. R.; Päivärinta, S.-M.; Plane, J. M. C.

    2016-09-01

    Observations have shown that a number of neutral minor species are affected by energetic particle precipitation (EPP) and ion chemistry (IC) in the polar regions. However, to date the complexity of the ion chemistry below the mesopause (i.e., in the D region ionosphere) has restricted global models to simplified EEP/IC parameterizations which are unable to reproduce some important effects, e.g., the increase of mesospheric nitric acid (HNO3). Here we use WACCM-D, a variant of the Whole Atmosphere Community Climate Model which includes a selected set of D region ion chemistry designed to produce the observed effects of EPP/IC. We evaluate the performance of EPP/IC modeling by comparing WACCM-D results for the January 2005 solar proton event (SPE) to those from the standard WACCM and Aura/Microwave Limb Sounder (MLS) and SCISAT/Atmospheric Chemistry Experiment-Fourier Transform Spectrometer (ACE-FTS) observations. The results indicate that WACCM-D improves the modeling of HNO3, HCl, ClO, OH, and NOx during the SPE. Northern Hemispheric HNO3 from WACCM-D shows an increase by 2 orders of magnitude at 40-70 km compared to WACCM, reaching 2.6 ppbv, in agreement with the observations. For HCl and ClO, the improvement is most pronounced in the Southern Hemisphere at 40-50 km where WACCM-D predicts a decrease of HCl and increase of ClO by 1.6% and 10%, respectively, similar to MLS data. Compared to WACCM, WACCM-D produces 25-50% less OH and 30-130% more NOx at 70-85 km which leads to better agreement with the observations. Although not addressed here, longer-term NOx impact of ion chemistry could be important for polar stratospheric ozone and middle atmospheric dynamics.

  12. Potential effects of clean coal technologies on acid precipitation, greenhouse gases, and solid waste disposal

    SciTech Connect

    Blasing, T.J.; Miller, R.L.; McCold, L.N.

    1993-11-01

    The US Department of Energy`s (DOE`s) Clean Coal Technology Demonstration Program (CCTDP) was initially funded by Congress to demonstrate more efficient, economically feasible, and environmentally acceptable coal technologies. Although the environmental focus at first was on sulfur dioxide (SO{sub 2}) and nitrogen oxides (NO{sub x}) because their relationship to acid precipitation, the CCTDP may also lead to reductions in carbon dioxide (CO{sub 2}) emissions and in the volume of solid waste produced, compared with conventional technologies. The environmental effects of clean coal technologies (CCTs) depend upon which (if any) specific technologies eventually achieve high acceptance in the marketplace. In general, the repowering technologies and a small group of retrofit technologies show the most promise for reducing C0{sub 2} emissions and solid waste. These technologies also compare favorably with other CCTs in terms of SO{sub 2} and NO{sub x} reductions. The upper bound for CO{sup 2} reductions in the year 2010 is only enough to reduce global ``greenhouse`` warming potential by about 1%. However, CO{sub 2} emissions come from such variety of sources around the globe that no single technological innovation or national policy change could realistically be expected to reduce these emissions by more than a few percent. Particular CCTs can lead to either increases or decreases in the amount of solid waste produced. However, even if decreases are not achieved, much of the solid waste from clean coal technologies would be dry and therefore easier to dispose of than scrubber sludge.

  13. STRONTIUM PRECIPITATION

    DOEpatents

    McKenzie, T.R.

    1960-09-13

    A process is given for improving the precipitation of strontium from an aqueous phosphoric-acid-containing solution with nickel or cobalt ferrocyanide by simultaneously precipitating strontium or calcium phosphate. This is accomplished by adding to the ferrocyanide-containing solution calcium or strontium nitrate in a quantity to yield a concentration of from 0.004 to 0.03 and adjusting the pH of the solution to a value of above 8.

  14. Precipitation and Surface-Runoff Sampling in the Arid Regions - New Lysimeter Techniques

    NASA Astrophysics Data System (ADS)

    Al-Qudah, O. M.; Walton, J. C.; Woocay, A.

    2009-12-01

    In order to measure the chemical characteristics of runoff water which has entered the sediments beneath ephemeral streams, Surface Runoff Samplers (SRS's) were designed. SRS represent a modification to the lysimeter. SRS's were designed to provide a stronger collection surface, more efficient connections for sample collection and to measure particularly the first flush of runoff. In addition, Infiltration characteristics, which are predominantly influenced by soil properties, were considered in the SRS design. Advantages of SRS design are: easy to assemble, requires minimum maintenance once installed, and total cost is relatively low. The limitations include: manual pumping is required and SRS must be checked on a regular schedule and pumped when full (depending on rain frequency and intensity). The design and emplacement of 56 SRS’s at 28 separate locations in the main arroyos around the Amargosa Desert region is explained and provides a look at initial data collection. It is our belief that long term data collection of this type will help us to better understand processes controlling groundwater recharge and thus the sustainable yield of groundwater in Nye County.

  15. Speciation and precipitation of heavy metals in high-metal and high-acid mine waters from the Iberian Pyrite Belt (Portugal).

    PubMed

    Durães, Nuno; Bobos, Iuliu; da Silva, Eduardo Ferreira

    2017-02-01

    Acid mine waters (AMW) collected during high- and low-flow water conditions from the Lousal, Aljustrel, and São Domingos mining areas (Iberian Pyrite Belt) were physicochemically analyzed. Speciation calculation using PHREEQC code confirms the predominance of Me(n+) and Me-SO4 species in AMW samples. Higher concentration of sulfate species (Me-SO4) than free ion species (Me(n+), i.e., Al, Fe, and Pb) were found, whereas opposite behavior is verified for Mg, Cu, and Zn. A high mobility of Zn than Cu and Pb was identified. The sulfate species distribution shows that Fe(3+)-SO4(2-), SO4(2-), HSO4(-), Al-SO4, MgSO4(0), and CaSO4(0) are the dominant species, in agreement with the simple and mixed metal sulfates and oxy-hydroxysulphates precipitated from AMW. The saturation indices (SI) of melanterite and epsomite show a positive correlation with Cu and Zn concentrations in AMW, which are frequently retained in simple metal sulfates. Lead is well correlated with jarosite and alunite (at least in very acid conditions) than with simple metal sulfates. The Pb for K substitution in jarosite occurs as increasing Pb concentration in solution. Lead mobility is also controlled by anglesite precipitation (a fairly insoluble sulfate), where a positive correlation was ascertained when the SI approaches equilibrium. The zeta potential of AMW decreased as pH increased due to colloidal particles aggregation, where water species change from SO4(2-) to OH(-) species during acid to alkaline conditions, respectively. The AMW samples were supersaturated in schwertmannite and goethite, confirmed by the Me(n+)-SO4, Me(n+)-Fe-O-OH, or Me(n+)-S-O-Fe-O complexes identified by attenuated total reflectance infrared spectroscopy (ATR-IR). The ATR-IR spectrum of an AMW sample with pH 3.5 (sample L1) shows well-defined vibration plans attributed to SO4 tetrahedron bonded with Fe-(oxy)hydroxides and the Me(n+) sorbed by either SO4 or Fe-(oxy)hydroxides. For samples with lower pH values (pH ~ 2

  16. Stepwise ethanolic precipitation of sugar beet pectins from the acidic extract.

    PubMed

    Guo, Xiaoming; Meng, Hecheng; Zhu, Siming; Tang, Qiang; Pan, Runquan; Yu, Shujuan

    2016-01-20

    A stepwise ethanol-precipitation (SEP) procedure was developed for the purification of sugar beet pectins (SBP) from a pectin-containing aqueous extract. Five fractions of different chemical and molecular characteristics were produced by stepwise elevating the alcohol concentration of the precipitation medium from 50% to 80% v/v. Comparison of chemical and macromolecular features between the obtained fractions indirectly suggested that the ability of pectin to solubilize in the ethanol-water binary mixture depended greatly on the polymer structure. Fractions rich in neutral sugars were precipitated at relatively high ethanol concentrations, probably due to the enhanced interactions generated between pectin side chains and solvent molecules. Furthermore, the obtained fractions displayed different surface activities. Results obtained in this work indicate that the SEP procedure is more selective with respect to pectin structural features and surface properties than the one-step ethanolic precipitation.

  17. Advances in biotreatment of acid mine drainage and biorecovery of metals: 1. Metal precipitation for recovery and recycle.

    PubMed

    Tabak, Henry H; Scharp, Richard; Burckle, John; Kawahara, Fred K; Govind, Rakesh

    2003-12-01

    Acid mine drainage (AMD), an acidic metal-bearing wastewater, poses a severe pollution problem attributed to post mining activities. The metals usually encountered in AMD and considered of concern for risk assessment are arsenic, cadmium, iron, lead, manganese, zinc, copper and sulfate. The pollution generated by abandoned mining activities in the area of Butte, Montana has resulted in the designation of the Silver Bow Creek-Butte Area as the largest Superfund (National Priorities List) site in the U.S. This paper reports the results of bench-scale studies conducted to develop a resource recovery based remediation process for the clean up of the Berkeley Pit. The process utilizes selective, sequential precipitation (SSP) of metals as hydroxides and sulfides, such as copper, zinc, aluminum, iron and manganese, from the Berkeley Pit AMD for their removal from the water in a form suitable for additional processing into marketable precipitates and pigments. The metal biorecovery and recycle process is based on complete separation of the biological sulfate reduction step and the metal precipitation step. Hydrogen sulfide produced in the SRB bioreactor systems is used in the precipitation step to form insoluble metal sulfides. The average metal recoveries using the SSP process were as follows: aluminum (as hydroxide) 99.8%, cadmium (as sulfide) 99.7%, cobalt (as sulfide) 99.1% copper (as sulfide) 99.8%, ferrous iron (sulfide) 97.1%, manganese (as sulfide) 87.4%, nickel (as sulfide) 47.8%, and zinc (as sulfide) 100%. The average precipitate purity for metals, copper sulfide, ferric hydroxide, zinc sulfide, aluminum hydroxide and manganese sulfide were: 92.4, 81.5, 97.8, 95.6, 92.1 and 75.0%, respectively. The final produced water contained only calcium and magnesium and both sulfate and sulfide concentrations were below usable water limits. Water quality of this agriculturally usable water met the EPA's gold standard criterion.

  18. Synthesis by precipitation polymerization of molecularly imprinted polymer for the selective extraction of diclofenac from water samples.

    PubMed

    Dai, Chao-meng; Zhou, Xue-fei; Zhang, Ya-lei; Liu, Shu-guang; Zhang, Juan

    2011-12-30

    A molecularly imprinted polymer (MIP) was synthesized by precipitation polymerization using diclofenac (DFC) as a template, 2-vinylpyridine (2-VP) as functional monomer, ethylene glycol dimethacrylate (EGDMA) as cross-linker, and toluene as porogen. The MIP showed outstanding affinity toward DFC in aqueous solution with a binding site capacity (Q(max)) of 324.8 mg/g (1.09 mmol/g) and was used as solid-phase extraction (SPE) material for the quantitative enrichment of DFC in environmental water samples and off-line coupled to a reversed-phase HPLC/DAD. Various parameters including washing solvent, elution solvent and breakthrough volume affecting the extraction efficiency of the polymers have been evaluated to achieve the selective preconcentration of DFC from water samples and to reduce non-specific interactions. Recoveries of DFC extracted from tap water, river water and wastewater samples were higher than 95%, and no significant DFC recovery difference was obtained among the different water matrix. The stability of MIP was tested by consecutive percolation of water sample, and it was shown that the performance of the MIP did not vary even after 30 adsorption and desorption cycles. Furthermore, the MISPE was used for the analysis of DFC in river water and wastewater samples and revealed DFC concentrations of 0.69±0.002 μg/L (n=3) and 0.31±0.004μg/L (n=3), respectively. The results were in good agreement with corresponding LC-MS/MS data.

  19. Pyridine-2,6-bis(thiocarboxylic acid) produced by Pseudomonas stutzeri KC reduces and precipitates selenium and tellurium oxyanions.

    PubMed

    Zawadzka, Anna M; Crawford, Ronald L; Paszczynski, Andrzej J

    2006-05-01

    The siderophore of Pseudomonas stutzeri KC, pyridine-2,6-bis(thiocarboxylic acid) (pdtc), is shown to detoxify selenium and tellurium oxyanions in bacterial cultures. A mechanism for pdtc's detoxification of tellurite and selenite is proposed. The mechanism is based upon determination using mass spectrometry and energy-dispersive X-ray spectrometry of the chemical structures of compounds formed during initial reactions of tellurite and selenite with pdtc. Selenite and tellurite are reduced by pdtc or its hydrolysis product H(2)S, forming zero-valent pdtc selenides and pdtc tellurides that precipitate from solution. These insoluble compounds then hydrolyze, releasing nanometer-sized particles of elemental selenium or tellurium. Electron microscopy studies showed both extracellular precipitation and internal deposition of these metalloids by bacterial cells. The precipitates formed with synthetic pdtc were similar to those formed in pdtc-producing cultures of P. stutzeri KC. Culture filtrates of P. stutzeri KC containing pdtc were also active in removing selenite and precipitating elemental selenium and tellurium. The pdtc-producing wild-type strain KC conferred higher tolerance against selenite and tellurite toxicity than a pdtc-negative mutant strain, CTN1. These observations support the hypothesis that pdtc not only functions as a siderophore but also is involved in an initial line of defense against toxicity from various metals and metalloids.

  20. Effects of airborne particulate matter on the acidity of precipitation in central Missouri

    SciTech Connect

    Applin, K.R.

    1985-01-01

    The pH of rainfall in central Missouri was monitored at four sites during the fall of 1983. Several pH values were well above 5.6, the theoretical pH of pure water in equilibrium with ambient levels of CO/sub 2/. Most of the higher pH's were measured on rainfall of short duration or rainfall collected during the first few hours of extended rainfall events. Furthermore, the rainfall associated with storm events lasting several days exhibited a trend of decreasing pH with time approaching values as low as 4.0 during the late stages of rainfall. Precipitation pH values above 5.6 apparently reflect neutralization reactions between wet precipitation and various components of airborne dust, especially clays and carbonates. During extended rainfalls, the neutralization effects gradually diminish as suspended dust is washed from the atmosphere yielding more accurate values of the wet precipitation pH. The results of this study suggest that airborne particulate matter generated from the dust bowl region of the US may affect the chemistry of precipitation in areas hundreds of kilometers downwind. Using date available in the literature, a direct relationship between precipitation pH and accumulated dustfall was found for data taken along a transect which represents the path of major storms crossing the US, i.e., from the south-central to northeastern regions.

  1. Chiral speciation of selenoamino acids in biological samples.

    PubMed

    Chen, Beibei; He, Man; Zhong, Cheng; Hu, Bin

    2014-10-10

    In this paper, the "state of the art" of chiral speciation of selenoamino acids (SeAAs) in biological samples is critically reviewed. The significance and the features of such studies are highlighted. A special focus lies on chiral speciation of SeAAs by hyphenation techniques in which a chiral separation method (such as gas chromatography (GC), high performance liquid chromatography (HPLC) and capillary electrophoresis (CE)) is on-line coupled with an elemental specific detector, especially inductively coupled plasma mass spectrometry (ICP-MS). The advances in the development and application of hyphenation techniques in chiral speciation of SeAAs in biological samples are summarized and a perspective for future developments including sophisticated and innovative applications is discussed. Overall, HPLC-ICP-MS is more applicable than GC/CE-ICP-MS for chiral speciation of SeAAs. In the future, more novel chiral HPLC methods with high enantio-resolution, low cost and robustness, and their more applications in real biological samples analysis are expected.

  2. Adsorption and co-precipitation behavior of arsenate, chromate, selenate and boric acid with synthetic allophane-like materials.

    PubMed

    Opiso, Einstine; Sato, Tsutomu; Yoneda, Tetsuro

    2009-10-15

    Pollution caused by boric acid and toxic anions such as As(V), Cr(VI) and Se(VI) is hazardous to human health and environment. The sorption characteristics of these environmentally significant ionic species on allophane-like nanoparticles were investigated in order to determine whether allophane can reduce their mobility in the subsurface environment at circum-neutral pH condition. Solutions containing 100 or 150 mmol of AlCl(3)x6H(2)O were mixed to 100 mmol of Na(4)SiO(4) and the pH were adjusted to 6.4+/-0.3. The mineral suspensions were shaken for 1h and incubated at 80 degrees C for 5 days. Appropriate amounts of As, B, Cr and Se solutions were added separately during and after allophane precipitation. The results showed that As(V) and boric acid can be irreversibly fixed during co-precipitation in addition to surface adsorption. However, Cr(VI) and Se(VI) retention during and after allophane precipitation is mainly controlled by surface adsorption. The structurally fixed As(V) and boric acid were more resistant to release than those bound on the surface. The sorption characteristics of oxyanions and boric acid were also influenced by the final Si/Al molar ratio of allophane in which Al-rich allophane tend to have higher uptake capacity. The overall results of this study have demonstrated the role of allophane-like nanoparticles and the effect of its Si/Al ratio on As, B, Cr and Se transport processes in the subsurface environment.

  3. Perfluoroalkyl acids in aqueous samples from Germany and Kenya.

    PubMed

    Shafique, Umer; Schulze, Stefanie; Slawik, Christian; Böhme, Alexander; Paschke, Albrecht; Schüürmann, Gerrit

    2016-06-22

    Continuous monitoring of chemicals in the environment is important to control their fate and to protect human health, flora, and fauna. Perfluoroalkyl acids (PFAAs) have been detected frequently in different environmental compartments during the last 15 years and have drawn much attention because of their environmental persistence, omnipresence, and bioaccumulation potential. Water is an important source of their transport. In the present study, distributions of PFAAs in river water, wastewater treatment plant (WWTP) effluent, and tap water from eastern part of Germany and western part of Kenya were investigated. Eleven perfluorocarboxylic acids (PFCAs) and five perfluorosulfonic acids (PFSAs) were analyzed using liquid chromatography/tandem mass spectrometry. Sum of mean concentrations of eight PFAAs detected in drinking tap water from Leipzig was 11.5 ng L(-1), dominated by perfluorooctanoic acid (PFOA, 6.2 ng L(-1)). Sums of mean riverine concentrations of PFAAs detected in Pleiße/White Elster, Saale, and Elbe (Germany) were 24.8, 54.3, and 26.8 ng L(-1), respectively. Annual flux of PFAAs from River Saale was estimated to be 164 ± 23 kg a(-1). The effluent of WWTP in Halle was found to contain four times higher levels of PFAAs than river water and was dominated by perfluorobutane sulfonate (PFBS) with 32 times higher concentration than the riverine level. It advocates that WWTPs are the point source of contaminating water bodies with PFAAs, and short-chain PFAAs are substituting long-chain homologues. Sums of mean riverine concentrations of PFAAs in Sosiani (Kenya) in samples from sparsely populated and densely populated areas were 58.8 and 109.4 ng L(-1), respectively, indicating that population directly affected the emissions of PFAAs to surface waters. The discussion includes thorough review and comparison of recently published literature reporting occurrence of PFAAs in aqueous matrices. Graphical abstract Perfluoroalkyl acids in aqueous

  4. Quantifying foliar responses of white ash to ozone and simulated acid precipitation: An assessment proposal for forest exposure studies. Forest Service research paper. (Final)

    SciTech Connect

    Dochinger, L.S.; Jensen, K.F.

    1990-04-01

    Seedlings populations represent an important linkage for assessing the effect of air pollution on forests. The study examines the foliar responses of white ash seedlings to ozone and acid precipitation as a means of identifying atmospheric deposition effects on forests.

  5. Searching for Amino Acids in Meteorites and Comet Samples

    NASA Technical Reports Server (NTRS)

    Cook, Jamie Elsila

    2010-01-01

    Chemistry plays an important role in the interdisciplinary field of astrobiology, which strives to understand the origin, distribution, and evolution of life throughout the universe. Chemical techniques are used to search for and characterize the basic ingredients for life, from the elements through simple molecules and up to the more complex compounds that may serve as the ingredients for life. The Astrobiology Analytical Laboratory at NASA Goddard uses state-of-the-art laboratory analytical instrumentation in unconventional ways to examine extraterrestrial materials and tackle some of the big questions in astrobiology. This talk will discuss some of the instrumentation and techniques used for these unique samples, as well as some of our most interesting results. The talk will present two areas of particular interest in our laboratory: (1) the search for chiral excesses in meteoritic amino acids, which may help to explain the origin of homochirality in life on Earth; and (2) the detection of amino acids and amines in material returned by NASA's Stardust mission, which rendevouzed with a cornet and brought back cometary particles to the Earth.

  6. LC-MS/MS analysis of Δ9-tetrahydrocannabinolic acid A in serum after protein precipitation using an in-house synthesized deuterated internal standard.

    PubMed

    Wohlfarth, Ariane; Roth, Nadine; Auwärter, Volker

    2012-06-01

    An assay based on liquid chromatography/tandem mass spectrometry is presented for the fast, precise and sensitive quantitation of Δ9-tetrahydrocannabinolic acid A (THCA) in serum. THCA is the biogenetic precursor of Δ9-tetrahydrocannabinol in cannabis and has aroused interest in the pharmacological and forensic field especially as a potential marker for recent cannabis use. After addition of deuterated THCA, synthesized from D(3)-THC as starting material, and protein precipitation, the analytes were separated using gradient elution on a Luna C18 column (150 × 2.0 mm × 5 µm) with 0.1% formic acid and acetonitrile/0.1% formic acid. Data acquisition was performed on a triple quadrupole linear ion trap mass spectrometer in multiple reaction monitoring mode with negative electrospray ionization. After optimization, the following sample preparation procedure was used: 200 μL serum was spiked with internal standard solution and methanol and then precipitated 'in fractions' with 500 μL ice-cold acetonitrile. After storage and centrifugation, the supernatant was evaporated and the residue redissolved in mobile phase. The assay was fully validated according to international guidelines including, for the first time, the assessment of matrix effects and stability experiments. Limit of detection was 0.1 ng/mL, and limit of quantification was 1.0 ng/mL. The method was found to be selective and proved to be linear over a range of 1.0 to 100 ng/mL using a 1/x weighted calibration model with regression coefficients >0.9996. Accuracy and precision data were within the required limits (RSD ≤ 8.6%, bias: 2.4 to 11.4%), extractive yield was greater than 84%. The analytes were stable in serum samples after three freeze/thaw cycles and storage at -20 °C for one month.

  7. Electron micrographic study of precipitates formed by interaction of silicic acid and alkaline phosphatase: contribution to a study of silica urolithiasis in cattle.

    PubMed

    Bailey, C B; Cheng, K J; Costerton, J W

    1982-12-01

    Association of alkaline phosphatase with silicic acid in precipitates formed in dilute solution was studied as a model for the nonspecific reaction between silicic acid and protein. Precipitates contained 68-83% of the silicic acid and 52-83% of the enzyme in the original mixture and were in the form of aggregates of roundish particles 150-800 nm in diameter. Enzyme protein formed a tightly bound layer on the surface of particles formed in solutions of freshly prepared silicic acid. The similarity between the ultrastructural features of precipitates from solutions of silicic acid and of internal portions of siliceous urinary calculi from cattle suggests that deposition of silica during development of such calculi is due, at least in part, to the interaction of protein with silicic acid in urine.

  8. Determination of paclitaxel in hyaluronic acid polymeric micelles in rat blood by protein precipitation-micelle breaking method: application to a pharmacokinetic study.

    PubMed

    Liu, Yanhua; Sun, Jin; Lian, He; Li, Xin; Cao, Wen; Bai, Liming; Wang, Yongjun; He, Zhonggui

    2013-09-15

    An efficient dissociation of paclitaxel (PTX) from the home-made hyaluronic acid-octadecyl (HA-C18) polymeric micelles formulation in rat blood could not be achieved using previously published PTX analytical methods. So, we intended to develop the micelle-breaking method to determine paclitaxel encapsulated in the HA-C18 polymeric micelles in blood. The pretreatment method of blood samples adopted a simple one-step protein precipitation-micelle breaking process with methanol as micelle-breaking and protein precipitant solvents for complete extraction of PTX from HA-C18 micelles in blood. The micelle breaking efficiency of methanol was as high as 97.7%. Separation was carried out by gradient elution on an Acquity UPLC BEH C18 column with a mobile phase consisting of water (containing 0.1% formic acid) and acetonitrile. A total single run time was as short as 3.0min. Detection was performed by triple-quadrupole mass spectrometry with positive electrospray ionization as source ionization in multiple-reaction monitoring mode at m/z 854.3→286.2 for PTX and m/z 808.5→527.3 for the internal standard, docetaxel. The method demonstrated good linearity at the concentrations ranging from 20 to 10,000ng/mL. The intra- and inter-day relative standard deviations were less than 9.9%. The mean extraction recoveries of PTX and IS were 94.7% and 87.5%, respectively. In summary, the methanol protein precipitation-micelle breaking method could extract PTX completely from the polymeric micelles. Finally, the method was successfully applied to a pharmacokinetic study of the home-made PTX-loaded HA-C18 polymeric micelles and Taxol solution after intravenous administration in rats.

  9. Precipitation of jarosite-type double salts from spent acid solutions from a chemical coal cleaning process

    SciTech Connect

    Norton, G.

    1990-09-21

    The precipitation of jarosite compounds to remove Na, K, Fe, and SO{sub 4}{sup 2{minus}} impurities from spent acid solutions from a chemical coal cleaning process was studied. Simple heating of model solutions containing Fe{sub 2}(SO{sub 4}){sub 3}, Na{sub 2}SO{sub 4}, and K{sub 2}SO{sub 4} caused jarosite (KFe{sub 3}(SO{sub 4}){sub 2}(OH){sub 6}) to form preferentially to natrojarosite (NaFe{sub 3}(SO{sub 4}){sub 2}(OH){sub 6}). Virtually all of the K, about 90% of the Fe, and about 30% of the SO{sub 4}{sup 2{minus}} could be precipitated from those solutions at 95{degree}C, while little or no Na was removed. However, simple heating of model solutions containing only Fe{sub 2}(SO{sub 4}){sub 3} and Na{sub 2}SO{sub 4} up to 95{degree}C for {le}12 hours produced low yields of jarosite compounds, and the Fe concentration in the solution had to be increased to avoid the formation of undesirable Fe compounds. Precipitate yields could be increased dramatically in model solutions of Na{sub 2}SO{sub 4}/Fe{sub 2}(SO{sub 4}){sub 3} containing excess Fe by using either CaCO{sub 3}, Ca(OH){sub 2}, or ZnO to neutralize H{sub 2}SO{sub 4} released during hydrolysis of the Fe{sub 2}(SO{sub 4}){sub 3} and during the precipitation reactions. Results obtained from the studies with model solutions were applied to spent acids produced during laboratory countercurrent washing of coal which had been leached with a molten NaOH/KOH mixture. Results indicated that jarosite compounds can be precipitated effectively from spent acid solutions by heating for 6 hours at 80{degree}C while maintaining a pH of about 1.5 using CaCO{sub 3}.

  10. Understanding barite and gypsum precipitation in upland acid-sulfate soils: An example from a Lufkin Series toposequence, south-central Texas, USA

    NASA Astrophysics Data System (ADS)

    Jennings, Debra S.; Driese, Steven G.

    2014-01-01

    Although low-temperature barite precipitation has been previously documented in soils and paleosols, pedogenic barite precipitation remains poorly understood. This study characterizes the micromorphology, elemental trends, and stable isotope geochemistry of sulfates in a barite-bearing soil (Lufkin Series) toposequence using optical microscopy, XRD, ICP-MS, and stable S and O isotope data. Synthesized data indicate that fluctuating redox processes and microbial activity resulting from epiaquatic and evaporative conditions lead to the precipitation of sulfates in the Lufkin soils. Stable sulfur and oxygen isotopes indicate that the primary source of sulfur is the partial dissolution of jarosite during microbial sulfate reduction. Barium-rich parent material provides adequate barium for barite precipitation. Barium is mobilized and concentrated in Btg horizons ~ 100-160 cm below the surface. The presence of humic acids in profiles lower on the landscape prevents barite precipitation and drives the precipitation of gypsum between saturated, anoxic conditions (November to May) and drier, more oxic conditions (May to November). Barite precipitation is a slow, punctuated process. Micromorphological data reveal that barite precipitates first along evacuated macropores and then in the adjacent matrix. In general, optimal conditions for pedogenic barite precipitation in upland wetland acid-sulfate soils are: 1) warm soil temperature that supports active sulfur-reducing and sulfur oxidizing microbes; 2) distinct wet/dry seasons that allow alternating redox conditions; 3) low-gradient landscape; 4) parent material that contains barium- and sulfur-rich constituents; and 5) a long-lived, stable landscape.

  11. Measurement of fexofenadine concentration in micro-sample human plasma by a rapid and sensitive LC-MS/MS employing protein precipitation: application to a clinical pharmacokinetic study.

    PubMed

    Guo, Daqing; Zou, Jianjun; Zhu, Yubing; Lou, Sheng; Fan, Hongwei; Qin, Qun

    2010-03-01

    A simple, rapid and sensitive liquid chromatography/positive ion electro-spray tandem mass spectrometry method (LC-MS/MS) was developed and validated for the quantification of fexofenadine with 100 microL human plasma employing glipizide as internal standard (IS). Protein precipitation was used in the sample preparation procedure. Chromatographic separation was achieved on a reversed-phase C(18 )column (5 microm, 100 x 2.1 mm) with methanol : buffer (containing 10 mmol/L ammonium acetate and 0.1% formic acid; 70 : 30, v/v) as mobile phase. The total chromatographic runtime was approximately 3.0 min with retention time for fexofenadine and IS at approximately 1.9 and 2.1 min, respectively. Detection of fexofenadine and IS was achieved by LC-MS/MS in positive ion mode using 502.1 --> 466.2 and 446.0 --> 321.1 transitions, respectively. The method was proved to be accurate and precise at linearity range of 1-600 ng/mL with a correlation coefficient (r) of > or =0.9976. The validated method was applied to a pharmacokinetic study in human volunteers following oral administration of 60 or 120 mg fexofenadine formulations, successfully.

  12. Amino acid preservation in saline halite core samples: Analogs for Martian dry evaporitic regions

    NASA Astrophysics Data System (ADS)

    Bada, J.; Aubrey, A.; Lowenstein, T.; Timofeeff, M.

    2008-12-01

    Recent data returned from several Mars spacecraft show substantial evidence for mineral precipitation from bodies of liquid water. Evaporitic minerals such as gypsum, kieserite and poly-hydrated magnesium sulfates have been detected remotely by orbiting spacecraft [1], jarosite has been detected in situ by the MER Opportunity [2], and chlorides are highly abundant upon the surface of Mars [3], often in correlation with siliclastic deposits [4]. Terrestrial environments can provide analogs for these systems identified on the Martian surface, and in-depth characterization of the terrestrial systems can provide valuable insights into processes that may have occurred on Mars during the late Noachian/early Hesperian. This is especially true in ancient playa or evaporative basin environments where deep core sampling offers a method of observing the geochemical diagenetic changes with time within a constrained environment. Deep coring can provide samples upwards of 200 ka within hundreds of meters of core [5]. The analysis of these sections can allow for the determination of preservation of various biosignatures from extinct microbial communities as well as their in situ diagenetic rates. Amino acids are powerful biomarkers that can be used to estimate biomass [6] and determine ages of extinct microbial communities [7]. Preliminary data for a core sample collected from Saline Valley, CA, shows the effect of time on amino acid biosignatures. The core has been dated by U-series: 35 feet, 20.9 ± 1.1 ka; 127 feet, 61.1 ±2.8 ka; 204 feet, 73.9 ±4.8 ka; and 310 feet, 150.3 ± 7.8 ka. The abundance of amino acids is observed to decrease drastically over the first 20 ka and then stabilize, although the overall composition changes. Acidic amino acids along with alanine and valine are the dominant amino acids. The enantiomeric (D/L) ratios generally increase with age because of in situ racemization, although the enantiomeric ratios for alanine and glutamic acid show a decrease

  13. The ecological effect of acid conditions and precipitation of hydrous metal oxides in a Rocky Mountain stream

    USGS Publications Warehouse

    McKnight, Diane M.; Feder, G.L.

    1984-01-01

    Periphyton and benthic invertebrates assemblages were studied at the confluence of two Rocky Mountain streams, Deer Creek and the Snake River near Montezuma, Colorado. Upstream from the confluence the Snake River is acidic and enriched in dissolved trace metals, while Deer Creek is a typical Rocky Mountain stream. In the Snake River, downstream from the confluence, the pH increases and hydrous metal oxides precipitate and cover the streambed. The algal and benthic invertebrate communities in the upstream reaches of the Snake River and in Deer Creek were very different. A liverwort, Scapania undulata var. undulata, was abundant in the Snake River, and although periphyton were very sparse, there were as many benthic invertebrates as in Deer Creek. Downstream from the confleunce, the precipitation of hydrous metal oxides greatly decreased the abundance of periphyton and benthic invertebrates. This study shows that in streams metal precipitates covering the streambed may have a more deleterious effect on stream communities than high metal-ion activities. ?? 1984 Dr. W. Junk Publishers.

  14. Accumulated analyses of amino acid precursors in returned lunar samples

    NASA Technical Reports Server (NTRS)

    Fox, S. W.; Harada, K.; Hare, P. E.

    1973-01-01

    Six amino acids (glycine, alanine, aspartic acid, glutamic acid, serine, and threonine) obtained by hydrolysis of extracts have been quantitatively determined in ten collections of fines from five Apollo missions. Although the amounts found, 7-45 ng/g, are small, the lunar amino acid/carbon ratios are comparable to those of the carbonaceous chondrites, Murchison and Murray, as analyzed by the same procedures. Since both the ratios of amino acid to carbon, and the four or five most common types of proteinous amino acid found, are comparable for the two extraterrestrial sources despite different cosmophysical histories of the moon and meteorites, common cosmochemical processes are suggested.

  15. The Consistency of Isotopologues of Ambient Atmospheric Nitric Acid in Passively Collected Samples

    NASA Astrophysics Data System (ADS)

    Bell, M. D.; Sickman, J. O.; Bytnerowicz, A.; Padgett, P.; Allen, E. B.

    2012-12-01

    Anthropogenic sources of nitrogen oxides have previously been shown to have distinctive isotopic signatures of oxygen and nitrogen. Nylon filters are currently used in passive sampling arrays to measure ambient atmospheric nitric acid concentrations and estimate deposition rates. This experiment measured the ability of nylon filters to consistently collect isotopologues of atmospheric nitric acid in the same ratios as they are present in the atmosphere. Samplers were deployed in continuous stirred tank reactors (CSTR) and at field sites across a nitrogen deposition gradient in Southern California. Filters were exposed over a four week period with individual filters being subjected to 1-4 week exposure times. Extracted nitric acid were measured for δ18O and δ15N ratios and compared for consistency based on length of exposure and amount of HNO3 collected. Filters within the CSTRs collected HNO3 at a consistent rate in both high and low concentration chambers. After two weeks of exposure, the mean δ18O values were within 0.5‰ of the δ18O of the source HNO3 solution. The mean of all weekly exposures were within 0.5‰ of the δ15N of the source solution, but after three weeks, the mean δ15N of adsorbed HNO3 was within 0.2‰. As the length of the exposure increased, the variability of measured delta values decreased for both elements. The field samplers collected HNO3 consistent with previously measured values along a deposition gradient. The mean δ18O at high deposition sites was 52.2‰ compared to 35.7‰ at the low deposition sites. Mean δ15N values were similar at all sites across the deposition gradient. Due to precipitation events occurring during the exposure period, the δ15N and δ18O of nitric acid were highly variable at all field sites. At single sites, changes in δ15N and δ18O were negatively correlated, consistent with two-sourcing mixing dynamics, but the slope of the regressions differed between high and low deposition sites. Anthropogenic

  16. Washout/rainout contribution in wet deposition estimated by 0.5 mm precipitation sampling/analysis

    NASA Astrophysics Data System (ADS)

    Aikawa, Masahide; Hiraki, Takatoshi

    A precipitation dataset collected on a 0.5 mm precipitation basis was studied. The parameters analyzed in this study were the pH (i.e., H + concentration), electric conductivity (EC), and SO42- and NO3- concentrations. The NO3- concentration clearly decayed with an increase of the precipitation amount, while a larger variation was observed in the SO42- concentration even when the precipitation amount increased. Assuming that the decaying NO3- concentration (0.70 μg ml -1) was the result of the rainout process, the estimates were: annual total deposition, 3252 mg m -2 yr -1; rainout process, 1092 mg m -2 yr -1; and rainout/total, 34%. The estimates for SO42- were: annual total deposition, 4687 mg m -2 yr -1; rainout process, 2096 mg m -2 yr -1; and rainout/total, 45%.

  17. The Debate over Acid Precipitation--Opposing Views--Status of Research.

    DTIC Science & Technology

    1981-09-11

    effects of acid deposition on terrestrial ecosystems. This contrasts with the general agreement among scientists that oxides of sulfur and nitro - gen...Altsnuller and G.A. McBean, Co-chairman, Nov. 148U, p. 1I. 2/Peter E. Coffee , "Long-Range Transport of Acidic Pollutants to New York," in Proceedings of

  18. Investigation of differences between field and laboratory pH measurements of national atmospheric deposition program/national trends network precipitation samples

    USGS Publications Warehouse

    Latysh, N.; Gordon, J.

    2004-01-01

    A study was undertaken to investigate differences between laboratory and field pH measurements for precipitation samples collected from 135 weekly precipitation-monitoring sites in the National Trends Network from 12/30/1986 to 12/28/1999. Differences in pH between field and laboratory measurements occurred for 96% of samples collected during this time period. Differences between the two measurements were evaluated for precipitation samples collected before and after January 1994, when modifications to sample-handling protocol and elimination of the contaminating bucket o-ring used in sample shipment occurred. Median hydrogen-ion and pH differences between field and laboratory measurements declined from 3.9 ??eq L-1 or 0.10 pH units before the 1994 protocol change to 1.4 ??eq L-1 or 0.04 pH units after the 1994 protocol change. Hydrogen-ion differences between field and laboratory measurements had a high correlation with the sample pH determined in the field. The largest pH differences between the two measurements occurred for high-pH samples (>5.6), typical of precipitation collected in Western United States; however low- pH samples (<5.0) displayed the highest variability in hydrogen-ion differences between field and laboratory analyses. Properly screened field pH measurements are a useful alternative to laboratory pH values for trend analysis, particularly before 1994 when laboratory pH values were influenced by sample-collection equipment.

  19. Molecularly imprinted polymer for chlorogenic acid by modified precipitation polymerization and its application to extraction of chlorogenic acid from Eucommia ulmodies leaves.

    PubMed

    Miura, Chitose; Li, Hui; Matsunaga, Hisami; Haginaka, Jun

    2015-10-10

    Molecularly imprinted polymers (MIPs) for chlorogenic acid (CGA) were prepared by modified precipitation polymerization using methacrylic acid as a functional monomer, divinylbenzene as a crosslinker and methanol or dimethylsulfoxide as a co-solvent. The prepared MIPs were microspheres with a narrow particle size distribution. Binding experiments and Scatchard analyses revealed that two classes of binding sites, high and low affinity sites, were formed on the MIP. The retention and molecular-recognition properties of the prepared MIP were evaluated using a mixture of water and acetonitrile as a mobile phase in hydrophilic interaction chromatography. With an increase of acetonitrile content, the retention factor of CGA was increased on the MIP. In addition to shape recognition, hydrophilic interactions seem to work for the recognition of CGA on the MIP. The MIP had a specific molecular-recognition ability for CGA, while other related compounds, such as caffeic acid, gallic acid, protocatechuic acid and vanillic acid, could not be recognized by the MIP. Furthermore, the MIP for CGA was successfully applied for extraction of CGA in the leaves of Eucommia ulmodies.

  20. Precipitation polymerization in acetic acid: study of the solvent effect on the morphology of poly(divinylbenzene).

    PubMed

    Yan, Qing; Zhao, Tongyang; Bai, Yaowen; Zhang, Fen; Yang, Wantai

    2009-03-12

    This paper reports on two important results regarding the precipitation polymerization of poly(divinylbenzene) (PDVB) in acetic acid (HAc). (1) Acetic acid is a novel kind of solvent worthy of investigation because it is amphipathic and innoxious. Thus, two kinds of model solvents, methyl ethyl ketone (MEK) and n-heptane, were selected to investigate the solvent effect on the particle morphology of PDVB-55 during precipitation polymerization in acetic acid. Monodisperse PDVB-55 microspheres were obtained with an MEK content of 30 vol % and a DVB loading of 2 vol %. Odd-shaped particles were found to almost disappear when MEK was added. For MEK contents up to 90 vol %, space-filling macrogels consisting of small particles with diameters of around 10 nm were obtained. More homocoagulated particles were produced when n-heptane was added, for which concentrations up to 50 vol % gave rise to cauliflower-like particles. Thus, in the acetic acid system, microspheres, pumpkin-like particles, macrogels, and coagulum could be successfully obtained. (2) The preparation of nonpolar PDVB-55 particles could be more predictable. For the first time-based on the regulation of former studies--the regularity of the dispersive term (delta(d)) on the particle morphology for a PDVB precipitation polymerization system was reported. The three-dimensional Hansen solubility parameters were utilized to perfect the regularity of the Hildebrand solubility parameter. Microspheres or particles were formed in the range of moderate delta values for both parameters, i.e., delta = 20.2-24.3 MPa1/2 or delta = 16 MPa1/2. What was even more important, delta(d) was found to be around 15.4 MPa1/2, and delta(h) should be below 13.5 MPa1/2. Cyclohexane, cyclohexanone, n-butyl acetate, and 1,4-dioxane were used to verify this regularity, and positive results were obtained. Stable, uniform, and well-separated PDVB-55 microspheres and particles were produced as a result of interaction forces between oligomers

  1. Soluble species in the Arctic summer troposphere - Acidic gases, aerosols, and precipitation

    NASA Technical Reports Server (NTRS)

    Talbot, R. W.; Vijgen, A. S.; Harriss, R. C.

    1992-01-01

    The large-scale spatial distribution from 0.15-to 6 km altitude in the North American Arctic troposphere of several soluble acidic gases and major aerosol species during the summertime is reported. The distribution is found to be compositionally consistent on a large spatial scale. The summertime troposphere is an acidic environment, with HCOOH and CH3COOH the principal acidic gases while acidic sulfate aerosols dominate the particulate phase. There appears to be a surface source of NH3 over the pack ice which may originate from decay of dead marine organisms on the ice surface, evolution from surface ocean waters in open ice leads, or release from rotting sea ice. At low altitude over the pack ice this NH34 appears to partially neutralize aerosol acidity. Over sub-Arctic tundra in southeastern Alaska, inputs of marine biogenic sulfur from the Bering Sea appear to be an important source of boundary layer aerosol SO4(2-). The rainwater acidity over the tundra is typical of remote regions.

  2. Soluble species in the Arctic summer troposphere - acidic gases, aerosols, and precipitation

    SciTech Connect

    Talbot, R.W.; Vijgen, A.S.; Harriss, R.C. Old Dominion Univ., Norfolk, VA )

    1992-10-01

    The large-scale spatial distribution from 0.15-to 6 km altitude in the North American Arctic troposphere of several soluble acidic gases and major aerosol species during the summertime is reported. The distribution is found to be compositionally consistent on a large spatial scale. The summertime troposphere is an acidic environment, with HCOOH and CH3COOH the principal acidic gases while acidic sulfate aerosols dominate the particulate phase. There appears to be a surface source of NH3 over the pack ice which may originate from decay of dead marine organisms on the ice surface, evolution from surface ocean waters in open ice leads, or release from rotting sea ice. At low altitude over the pack ice this NH34 appears to partially neutralize aerosol acidity. Over sub-Arctic tundra in southeastern Alaska, inputs of marine biogenic sulfur from the Bering Sea appear to be an important source of boundary layer aerosol SO4(2-). The rainwater acidity over the tundra is typical of remote regions. 61 refs.

  3. Generation of dose-response relationships to assess the effects of acidity in precipitation on growth and productivity of vegetation

    SciTech Connect

    Evans, L.S.

    1981-01-01

    Experiments were performed with several plant species in natural environments as well in a greenhouse and/or tissue culture facilities to establish dose-response functions of plant responses to simulated acidic rain in order to determine environmental risk assessments to ambient levels of acidic rain. Response functions of foliar injury, biomass of leaves and seed of soybean and pinto beans, root yields of radishes and garden beets, and reproduction of bracken fern are considered. The dose-response function of soybean seed yields with the hydrogen ion concentration of simulated acidic rainfalls was expressed by the equation y = 21.06-1.01 log x where y = seed yield in grams per plant and x = the hydrogen concentration if ..mu..eq l/sup -1/. The correlation coefficient of this relationship was -0.90. A similar dose-response function was generated for percent fertilization of ferns in a forest understory. When percent fertilization is plotted on logarithmic scale with hydrogen ion concentration of the simulated rain solution, the Y intercept is 51.18, slope -0.041 with a correlation coefficient of -0.98. Other dose-response functions were generated that assist in a general knowledge as to which plant species and which physiological processes are most impacted by acidic precipitation. Some responses did not produce convenient dose-response relationships. In such cases the responses may be altered by other environmental factors or there may be no differences among treatment means.

  4. SPECIAL SESSION: (H21) on Global Precipitation Mission for Hydrology and Hydrometeorology. Sampling-Error Considerations for GPM-Era Rainfall Products

    NASA Technical Reports Server (NTRS)

    Bell, Thomas L.; Lau, William K. M. (Technical Monitor)

    2002-01-01

    The proposed Global Precipitation Mission (GPM) builds on the success of the Tropical Rainfall Measuring Mission (TRMM), offering a constellation of microwave-sensor-equipped smaller satellites in addition to a larger, multiply-instrumented "mother" satellite that will include an improved precipitation radar system to which the precipitation estimates of the smaller satellites can be tuned. Coverage by the satellites will be nearly global rather than being confined as TRMM was to lower latitudes. It is hoped that the satellite constellation can provide observations at most places on the earth at least once every three hours, though practical considerations may force some compromises. The GPM system offers the possibility of providing precipitation maps with much better time resolution than the monthly averages around which TRMM was planned, and therefore opens up new possibilities for hydrology and data assimilation into models. In this talk, methods that were developed for estimating sampling error in the rainfall averages that TRMM is providing will be used to estimate sampling error levels for GPM-era configurations. Possible impacts on GPM products of compromises in the sampling frequency will be discussed.

  5. Field enhancement sample stacking for analysis of organic acids in traditional Chinese medicine by capillary electrophoresis.

    PubMed

    Zhu, Qianqian; Xu, Xueqin; Huang, Yuanyuan; Xu, Liangjun; Chen, Guonan

    2012-07-13

    A technique known as field enhancement sample stacking (FESS) and capillary electrophoresis (CE) separation has been developed to analyze and detect organic acids in the three traditional Chinese medicines (such as Portulaca oleracea L., Crataegus pinnatifida and Aloe vera L.). In FESS, a reverse electrode polarity-stacking mode (REPSM) was applied as on-line preconcentration strategy. Under the optimized condition, the baseline separation of eight organic acids (linolenic acid, lauric acid, p-coumaric acid, ascorbic acid, benzoic acid, caffeic acid, succinic acid and fumaric acid) could be achieved within 20 min. Validation parameters of this method (such as detection limits, linearity and precision) were also evaluated. The detection limits ranged from 0.4 to 60 ng/mL. The results indicated that the proposed method was effective for the separation of mixtures of organic acids. Satisfactory recoveries were also obtained in the analysis of these organic acids in the above traditional Chinese medicine samples.

  6. Stereochemistry of amino acids in surface samples of a marine sediment

    USGS Publications Warehouse

    Pollock, G.E.; Kvenvolden, K.A.

    1978-01-01

    In two surface samples of marine sediment, the percentages of d-alanine and d-aspartic acid are significantly higher than the other d-amino acids and are similar to the range found in soils. The percentage of d-glutamic acid is also higher than the other amino acids but less than d-alanine and d-aspartic acid. These d-amino acids may come mainly from bacteria. ?? 1978.

  7. Stereochemistry of amino acids in surface samples of a marine sediment

    NASA Technical Reports Server (NTRS)

    Pollock, G. E.; Kvenvolden, K. A.

    1978-01-01

    In two surface samples of marine sediment, the percentages of D-alanine and D-aspartic acid are significantly higher than the other D-amino acids and are similar to the range found in soils. The percentage of D-glutamic acid is also higher than the other amino acids but less than D-alanine and D-aspartic acid. These D-amino acids may come mainly from bacteria.

  8. Enhanced Resolution of Chiral Amino Acids with Capillary Electrophoresis for Biosignature Detection in Extraterrestrial Samples.

    PubMed

    Creamer, Jessica S; Mora, Maria F; Willis, Peter A

    2017-01-17

    Amino acids are fundamental building blocks of terrestrial life as well as ubiquitous byproducts of abiotic reactions. In order to distinguish between amino acids formed by abiotic versus biotic processes it is possible to use chemical distributions to identify patterns unique to life. This article describes two capillary electrophoresis methods capable of resolving 17 amino acids found in high abundance in both biotic and abiotic samples (seven enantiomer pairs d/l-Ala, -Asp, -Glu, -His, -Leu, -Ser, -Val and the three achiral amino acids Gly, β-Ala, and GABA). To resolve the 13 neutral amino acids one method utilizes a background electrolyte containing γ-cyclodextrin and sodium taurocholate micelles. The acidic amino acid enantiomers were resolved with γ-cyclodextrin alone. These methods allow detection limits down to 5 nM for the neutral amino acids and 500 nM for acidic amino acids and were used to analyze samples collected from Mono Lake with minimal sample preparation.

  9. Use of NADP archive samples to determine the isotope composition of precipitation: characterizing the meteoric input function for use in ground water studies.

    PubMed

    Harvey, F E

    2001-01-01

    Stable oxygen and hydrogen isotopes have been used in ground water studies to investigate recharge, mixing, ground water/surface water interaction, advective-diffusive transport, paleohydrogeologic interactions and to estimate ground water ages. Such studies require that the isotopic composition of precipitation be known, as precipitation is a major input to ground water and surface water systems. As oxygen-18 and deuterium data for precipitation are lacking across much of the United States, there is need to establish additional local meteoric water lines as isotope input functions across the region, as well as to develop better understanding of the isotopic climate linkages that control oxygen and hydrogen isotope ratios in precipitation. In the absence of long-term monitoring stations, one possible solution to this problem is to determine the delta 18O and delta 2H values of precipitation using archive samples collected at monitoring stations managed by the National Atmospheric Deposition Program (NADP). This study describes and interprets the seasonal delta 18O and delta 2H composition of archived precipitation samples collected in eastern Nebraska near the town of Mead during the years 1992-1994. Values for delta 18O range from -23.6 to -0.7@1000. Values for delta 2H range from -172 to 0@1000. Yearly arithmetic mean delta 18O and delta 2H values for the Mead station are -8.1@1000 and -53@1000, respectively. Weighted yearly means for delta 18O and delta 2H were -7.4@1000 and -48@1000, respectively. Mead values show a strong isotopic enrichment between winter and summer precipitation, and a strong delta 18O-T correlation (r2 = 0.91) for mean monthly values of about 0.5@1000 per degree Celsius. The local meteoric water line for the Mead site is delta 2H = 7.40 delta 18O + 7.32. Deuterium excess values suggest that most of the moisture across the region is derived primarily from a Gulf of Mexico source. The results of this study demonstrate that in the absence of

  10. Effects of calcium phosphate precipitation method on acid resistance to apatite powder and bovine tooth.

    PubMed

    Suge, Toshiyuki; Kawasaki, Akiko; Ishikawa, Kunio; Matsuo, Takashi; Ebisu, Shigeyuki

    2008-07-01

    The aims of this study were to evaluate the effects of CPP method on the crystallinity of apatite powder and on the acid resistance of bovine enamel. Crystallinity degrees of apatite powder before and after CPP treatment were measured by powder X-ray diffraction analysis. Polished bovine enamel specimens treated with CPP method or NaF were immersed in a lactic acid solution for up to five days. The demineralized depth of enamel was measured with a surface roughness analyzer. XRD peaks became sharper after the CPP treatment, indicating an increased crystallinity of the apatite powder. The demineralized depth of bovine enamel treated with CPP method was shallower than that of enamel treated with NaF. Results of this study revealed that the CPP method increased the crystallinity of apatite powder and the acid resistance of enamel. Therefore, the CPP method would be useful not only for treating dentin hypersensitivity, but also for the prevention of dental caries.

  11. Acid precipitation effects on algal productivity and biomass in Adirondack Lakes. Final completion report

    SciTech Connect

    Hendrey, G.R.

    1982-12-01

    Relationships between phytoplankton communities and lake acidity in three Adirondack Mountain Lakes were studied at Woods Lake, Sagamore Lake (pH ca. 5.5), and Panther Lake (pH ca. 7.0). Numbers of phytoplankton species observed were Woods 45, Sagamore 55, and Panther 85, conforming to observations at many other sites that species numbers decrease with increasing acidity. The smaller plankton are relatively more important in the more acid lakes, Woods > Sagamore > Panther. This pattern could be determined by nutrient availability (lake acidification is suspected of leading to decreased availability of phosphorus). The amount of 14C-labelled dissolved photosynthate (14C-DOM), as a percent of total productivity, is ordered Woods > Sagamore > Panther.

  12. Determination of deoxycholic acid pool size and input rate using (24-/sup 13/C)deoxycholic acid and serum sampling

    SciTech Connect

    Stellard, F.; Paumgartner, G.; van Berge Henegouwen, G.P.; van der Werf, S.D.

    1986-11-01

    We have developed an isotope dilution method for determination of deoxycholic acid pool size and input rate which employs oral administration of 50 mg of (24-/sup 13/C)deoxycholic acid and serum sampling. The method has been validated by classical isotope dilution technique using (24-/sup 14/C)deoxycholic acid and bile sampling in five patients with colonic adenomas. Excellent agreement between pool sizes and input rates determined with /sup 13/C/12C isotope ratio measurements in serum and /sup 14/C measurements in bile was obtained when isotope ratios were measured in the conjugated fraction of deoxycholic acid in serum. We conclude that pool size and input rate of deoxycholic acid can accurately be determined by blood sampling after oral administration of (24-/sup 13/C)deoxycholic acid, therewith eliminating the use of radioactive tracers and the need for bile sampling.

  13. A global assessment of precipitation chemistry and deposition of sulfur, nitrogen, sea salt, base cations, organic acids, acidity and pH, and phosphorus

    NASA Astrophysics Data System (ADS)

    Vet, Robert; Artz, Richard S.; Carou, Silvina

    2014-08-01

    Investigating and assessing the chemical composition of precipitation and atmospheric deposition is essential to understanding how atmospheric pollutants contribute to contemporary environmental concerns including ecosystem acidification and eutrophication, loss of biodiversity, air pollution and global climate change. Evidence of the link between atmospheric deposition and these environmental issues is well established. The state of scientific understanding of this link is that present levels of atmospheric deposition of sulfur and nitrogen adversely affect terrestrial and aquatic ecosystems, putting forest sustainability and aquatic biodiversity at risk. Nitrogen and phosphorus loadings are linked to impacts on the diversity of terrestrial and aquatic vegetation through biological cycling, and atmospheric deposition plays a major role in the emission-transport-conversion-loss cycle of chemicals in the atmosphere as well as the formation of particulate matter and ozone in the troposphere. Evidence also shows that atmospheric constituents are changing the earth's climate through direct and indirect atmospheric processes. This Special Issue, comprising a single article titled "A global assessment of precipitation chemistry and deposition of sulfur, nitrogen, sea salt, base cations, organic acids, acidity and pH, and phosphorus", presents a recent comprehensive review of precipitation chemistry and atmospheric deposition at global and regional scales. The information in the Special Issue, including all supporting data sets and maps, is anticipated to be of great value not only to the atmospheric deposition community but also to other science communities including those that study ecosystem impacts, human health effects, nutrient processing, climate change, global and hemispheric modeling and biogeochemical cycling. Understanding and quantifying pollutant loss from the atmosphere is, and will remain, an important component of each of these scientific fields as they

  14. Metal and acidity fluxes controlled by precipitation/dissolution cycles of sulfate salts in an anthropogenic mine aquifer

    NASA Astrophysics Data System (ADS)

    Cánovas, C. R.; Macías, F.; Pérez-López, R.

    2016-05-01

    Underground mine drainages are extremely difficult to study due to the lack of information about the flow path and source proximity in relation to the outflow adit. Geochemical processes controlling metals and acidity fluxes in a complex anthropogenic mine aquifer in SW Spain during the dry and rainy season were investigated by geochemical and statistical tools. High concentrations of acidity, sulfate, metals and metalloids (e.g. Fe, Cu, Zn, As, Cd, Ni, Co) were observed due to intense sulfide oxidation processes. The high residence time inside the anthropogenic aquifer, around 40 days, caused the release of significant quantities of metals linked to host rocks (e.g. Al, Ca, Ge, Li, Mg, REE). The most outstanding characteristic of the acid mine drainage (AMD) outflows is the existence of higher Fe/SO4 molar ratios than those theoretical of pyrite (0.50) during most of the monitored period, due to a fire which occurred in 1949 and remained active for decades. Permanent and temporal retention mechanisms of acidity and metals were observed in the galleries. Once released from sulfide oxidation, Pb and As are sorbed on Fe oxyhydroxysulfate or precipitated as low solubility minerals (i.e. anglesite) inside the galleries. The precipitation of evaporitic sulfate salts during the dry season and the subsequent re-dissolution after rainfall control the fluxes of acidity and main metals (i.e. Fe, Mg, Al) from this anthropogenic aquifer. Some elements, such as Cd, Cu, Ni, REE and Zn, are retained in highly soluble sulfate salts while other elements, such as Ge, Pb and Sc, have a lower response to washout processes due to its incorporation in less soluble sulfate salts. In this way, metal concentration during the washout processes would be controlled by the proportion and solubility of each type of evaporitic sulfate salt stored during the dry season. The recovery of metals of economic interest contained in the AMD could help to self-finance the remediation of these waters in

  15. Acid precipitation effects on algal productivity and biomass in Adirondack Mountain lakes

    SciTech Connect

    Hendrey, G.R.

    1982-12-01

    Relationships between phytoplankton communities and lake acidity in three Adirondack Mountain lakes were studied at Woods Lake (pH ca. 4.9), Sagamore Lake (pH ca. 5.5), and Panther Lake (pH ca. 7.0). Species numbers decrease with increasing acidity. Patterns of increasing biomass and productivity in Woods Lake may be atypical of similar oligotrophic lakes in that they develop rather slowly to maxima six weeks after ice-out, instead of occurring very close to ice-out. Contributions of netplankton, nannoplankton and ultraplankton to productivity per m/sup 2/ show that the smaller plankton are relatively more important in the more acid lakes. This pattern could be determined by nutrient availability (lake acidification is suspected of leading to decreased availability of phosphorus). This was consistent with a hypothesis that microbial heterotrophic activity is reduced with increasing acidity, but the smaller phytoplankton may be more leaky at low pH. 11 references, 2 tables.

  16. Potential for acid precipitation damage to lakes of the Sierra Nevada, California

    SciTech Connect

    Harte, J.; Holdren, J.; Tonnesson, K.

    1983-04-01

    One of the areas of California potentially sensitive to acidic deposition is the Sierra Nevada, located along the eastern boundary. A report on sensitive areas in North America identifies the Sierra as a region characterized by poorly buffered soils and granite based lakes. The subalpine and alpine lakes in this region share many of the characteristics of lakes adversely affected by acid deposition in other parts of the US and the world. For this investigation selected subalpine lakes of the western slope of the Sierra were chosen for study, to establish baseline water quality which would allow for the identification of chemical and biological changes due to acidic deposition. It was then attempted to simulate the ecosystem stress of increased acidic deposition, particularly in the form of snowmelt, on these systems by performing microcosm experiments in the laboratory. These experiments were particularly concerned with recording changes in concentrations of micronutrients which might be leached from lake sediments with increasing acidification. This phenomenon is particularly important to study in the light of finds on the importance of aluminum leaching in the northeast which was led to toxic effects of biota in Adirondack lakes. 10 references, 3 figures, 1 table.

  17. Aquatic Activities for Middle School Children. A Focus on the Effects of Acid Precipitation.

    ERIC Educational Resources Information Center

    Minnesota Univ., Minneapolis. Minnesota Sea Grant Program.

    Basic water-related concepts and underlying principles of acid rain are described in this curriculum in a manner that young children can understand. The curriculum consists of activities presented in four units: Background Unit, Earth Science Unit, Life Science Unit, and Extension Unit. The first three units consist of several modules, each module…

  18. On the abiotic formation of amino acids. I - HCN as a precursor of amino acids detected in extracts of lunar samples. II - Formation of HCN and amino acids from simulated mixtures of gases released from lunar samples

    NASA Technical Reports Server (NTRS)

    Yuasa, S.; Flory, D.; Basile, B.; Oro, J.

    1984-01-01

    Two studies on the abiotic formation of amino acids are presented. The first study demonstrates the role of hydrogen cyanide as a precursor of amino acids detected in extracts of lunar samples. The formation of several amino acids, including glycine, alanine, aspartic acid, and glutamic acid, under conditions similar to those used for the analysis of lunar samples is demonstrated. The second study investigates the formation of hydrogen cyanide as well as amino acids from lunar-sample gas mixtures under electrical discharge conditions. These results extend the possibility of synthesis of amino acids to planetary bodies with primordial atmospheres less reducing than a mixture of methane, ammonia, hydrogen and water.

  19. Acetylation dictates the morphology of nanophase biosilica precipitated by a 14-amino acid leucine-lysine peptide.

    PubMed

    Lutz, Helmut; Jaeger, Vance; Bonn, Mischa; Pfaendtner, Jim; Weidner, Tobias

    2017-02-01

    N-terminal acetylation is a commonly used modification technique for synthetic peptides, mostly applied for reasons of enhanced stability, and in many cases regarded as inconsequential. In engineered biosilification - the controlled deposition of silica for nanotechnology applications by designed peptides - charged groups often play a deciding role. Here we report that changing the charge by acetylation of a 14-amino acid leucine-lysine (LK) peptide dramatically changes the morphology of precipitated biosilica; acetylated LK peptides produce nano-spheres, whereas nano-wires are precipitated by the same peptide in a non-acetylated form. By using interface-specific vibrational spectroscopy and coarse-grained molecular simulations, we show that this change in morphology is not the result of modified peptide-silica interactions, but rather caused by the stabilization of the hydrophobic core of peptide aggregates created by the removal of a peptide charge upon acetylation. These results should raise awareness of the potential impact of N-terminal modifications in peptide applications. Copyright © 2016 European Peptide Society and John Wiley & Sons, Ltd.

  20. Production and characterization of poly(3-hydroxybutyrate) generated by Alcaligenes latus using lactose and whey after acid protein precipitation process.

    PubMed

    Berwig, Karina Hammel; Baldasso, Camila; Dettmer, Aline

    2016-10-01

    Whey after acid protein precipitation was used as substrate for PHB production in orbital shaker using Alcaligenes latus. Statistical analysis determined the most appropriate hydroxide for pH neutralization of whey after protein precipitation among NH4OH, KOH and NaOH 10%w/v. The results were compared to those of commercial lactose. A scale-up test in a 4L bioreactor was done at 35°C, 750rpm, 7L/min air flow, and 6.5 pH. The PHB was characterized through Fourier Transform Infrared Spectroscopy, thermogravimetry and differential scanning calorimetry. NH4OH provided the best results for productivity (p), 0.11g/L.h, and for polymer yield, (YP/S), 1.08g/g. The bioreactor experiment resulted in lower p and YP/S. PHB showed maximum degradation temperature (291°C), melting temperature (169°C), and chemical properties similar to those of standard PHB. The use of whey as a substrate for PHB production did not affect significantly the final product quality.

  1. SAMPLING ARTIFACT ESTIMATES FOR ALKANES, HOPANES, AND ALIPHATIC CARBOXYLIC ACIDS

    EPA Science Inventory

    Sampling artifacts for molecular markers from organic speciation of particulate matter were investigated by analyzing forty-one samples collected in Philadelphia as a part of the Northeast Oxidant and Particulate Study (NEOPS). Samples were collected using a high volume sampler ...

  2. Targeted toxicological screening for acidic, neutral and basic substances in postmortem and antemortem whole blood using simple protein precipitation and UPLC-HR-TOF-MS.

    PubMed

    Telving, Rasmus; Hasselstrøm, Jørgen Bo; Andreasen, Mette Findal

    2016-09-01

    A broad targeted screening method based on broadband collision-induced dissociation (bbCID) ultra-performance liquid chromatography high-resolution time-of-flight mass spectrometry (UPLC-HR-TOF-MS) was developed and evaluated for toxicological screening of whole blood samples. The acidic, neutral and basic substances covered by the method were identified in postmortem and antemortem whole blood samples from forensic autopsy cases, clinical forensic cases and driving under the influence of drugs (DUID) cases by a reverse target database search. The screening method covered 467 substances. Validation was performed on spiked whole blood samples and authentic postmortem and antemortem whole blood samples. For most of the basic drugs, the established cut-off limits were very low, ranging from 0.25ng/g to 50ng/g. The established cut-off limits for most neutral and acidic drugs, were in the range from 50ng/g to 500ng/g. Sample preparation was performed using simple protein precipitation of 300μL of whole blood with acetonitrile and methanol. Ten microliters of the reconstituted extract were injected and separated within a 13.5min UPLC gradient reverse-phase run. Positive electrospray ionization (ESI) was used to generate the ions in the m/z range of 50-1000. Fragment ions were generated by bbCID. Identification was based on retention time, accurate mass, fragment ion(s) and isotopic pattern. A very sensitive broad toxicological screening method using positive electrospray ionization UPLC-HR-TOF-MS was achieved in one injection. This method covered basic substances, substances traditionally analyzed in negative ESI (e.g., salicylic acid), small highly polar substances such as beta- and gamma-hydroxybutyric acid (BHB and GHB, respectively) and highly non-polar substances such as amiodarone. The new method was shown to combine high sensitivity with a very broad scope that has not previously been reported in toxicological whole blood screening when using only one injection.

  3. Use of nitric acid in sample pretreatment for determination of trace elements in various biological samples by ETAAS.

    PubMed

    Scancar, J; Milacic, R; Falnoga, I; Cemazar, M; Bukovec, P

    2000-07-01

    Trace elements in liquid biological samples may be determined by direct electrothermal atomic absorption spectrometry (ETAAS). In our previous work it was found that samples containing proteins or DNA may leak out of the graphite tube before the drying step, despite the addition of various modifiers. In order to keep the sample to the graphite tube, samples were diluted before analysis 1 + 1 with 32% v/v nitric acid, or 5 microl of 32% v/v nitric acid was added to the graphite tube before ETAAS determination. Applying the proposed procedure, the concentrations of lead in eluted fractions after gel chromatographic separation of human cerebellar nucleus dentatus supernatant and platinum in isolated DNA samples were determined. The use of nitric acid in sample pretreatment prevent sample leakage out of the graphite tube, provided for even drying and considerably reduced nonspecific absorption in lead determination. The repeatability of measurements was better than + 6%. The accuracy of the procedure was checked by spiking samples. The recoveries for both elements lay between 93--104%. Nitric acid was found to be a better modifier than TRITON X-100.

  4. Ammonia emission factors for the NAPAP (National Acid Precipitation Assessment Program) emission inventory. Final report, January 1985-December 1986

    SciTech Connect

    Misenheimer, D.C.; Warn, T.E.; Zelmanowitz, S.

    1987-01-01

    The report provides information on certain sources of ammonia emissions to the atmosphere for use in the National Acid Precipitation Assessment Program (NAPAP) emission inventories. Major anthropogenic sources of ammonia emissions to the atmosphere are identified, and emission factors for these sources are presented based on a review of the most recent data available. The emission factors developed are used to estimate nationwide emissions for base year 1980 and are compared to ammonia emission factors used in other emission inventories. Major anthropogenic source categories covered are cropland spreading of livestock wastes, beef cattle feedlots, fertilizer manufacture and use, fuel combustion, ammonia synthesis, petroleum refineries, and coke manufacture. Approximately 840,000 tons of ammonia is estimated to have been emitted in the U.S. in 1980; over 64% of which is estimated to have been from livestock wastes.

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

    SciTech Connect

    Cary, Robert E.

    2015-12-08

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

  6. A computer simulation of ecosystem processes in forests for application to air pollution, acid precipitation and global change

    SciTech Connect

    Kercher, J.R. ); Anderson, P.D. . Dept. of Forestry and Resource Management)

    1992-07-17

    We have developed a simulation model, TREE, of the effects of gaseous air pollutants and acid precipitation on the forest ecosystem processes of tree productivity and growth. This model is based on an existing general model of forest ecosystem processes developed for regional application (FOREST-BGC) combined with an existing model of plant productivity and transpiration (BACROS). The former model uses daily and annual time-steps; BACROS uses hourly time-steps and computes gaseous pollutant (ozone) uptake. In FOREST-BGC, we model the effects of ozone by reducing productivity based on the cumulative uptake for each leaf age-class. The model computations convert this reduction in productivity to a reduction in growth. This version of the model restricts consideration of acid precipitation to possible effects on productivity due to foliar exposure. Basic model performance has been studied for ponderosa pine exposed to ozone at the USFS Chico Tree Improvement Center The model simulates observed phenomena such as draw down of soil water during summer months. For ozone levels for the Chico Field Site for the 1990 season, maximum daily ozone uptake occurred in August with peak of 2.2 {times} 10{sup {minus}5} kg m{sup {minus}2} d{sup 1}. Cumulative annual ozone uptake for current year needles was 3.2 {times} 10{sup {minus}2} kg m{sup {minus}2} producing a 12.6% reduction in productivity for current year needles and a 13.3% reduction in chlorophyll and effective leaf area. Total transpiration was 0.95 m. The model is now being used to develop a terrestrial ecosystem submodel for a global scale Earth System Model (ESM) that integrates interacting atmospheric, oceanic, and land system components. Algorithms from the forest model will support feedback calculation of the effect of forests on atmospheric physics and chemistry as well as calculate effects of climate- and C0{sub 2}-change on forest productivity.

  7. Validation of a NIR quantification method for the determination of chlorogenic acid in Lonicera japonica solution in ethanol precipitation process.

    PubMed

    Wu, Zhisheng; Xu, Bing; Du, Min; Sui, Chenglin; Shi, Xinyuan; Qiao, Yanjiang

    2012-03-25

    The feasibility of near-infrared spectroscopy (NIRS) for chlorogenic acid content analysis in ethanol precipitation process of water extract of Lonicera japonica was verified in this work. A calibration and validation set was designed for the conception and evaluation of the method adequacy. An experimental protocol was then followed, involving two different NIR instruments for data acquisition. On the basis of this protocol, the model was developed based on partial least squares regression (PLS) and the determination coefficient (R(2)(cal) and R(2)(val)), standard error of calibration and prediction (SEC and SEP) were 0.9962, 0.9955, 111.1 μg/mL and 107.1 μg/mL for Holographic Grating NIR instrument, and 0.9984, 0.9971, 53.6 μg/mL and 83.3 μg/mL for Fourier Transform NIR instrument. However, such above criteria did not clearly demonstrate the model's prediction error over each analyzed content range. Consequently, a novel approach based on accuracy profile which allowed the acquisition of the lower limit of quantification (LLOQ) was used to validate the robustness and accuracy of PLS model. The resulting accuracy profile showed that PLS model was able to determine chlorogenic acid content by two NIR systems, whose LLOQ was about 1550 μg/mL. It was concluded that the two NIR systems were suitable for use as Process Analytical Technology (PAT) to understand ethanol precipitation process of water extract of Lonicera japonica.

  8. Red spruce germination and growth in soil-mediated regeneration microcosms under acid precipitation

    SciTech Connect

    Ho, M.

    1992-01-01

    In the past three decades, atmospheric pollution has caused substantial problems for the environment as well as for many biological processes. The objective of this study focuses on red spruce (Picea ruben Sarg.) regeneration potential and chemical change within the soil-water-plant continuum following simulated acid rain treatments. Inceptisols from three forests at 1735, 1920, and 2015 m at Mt. Mitchell, North Carolina had lower pH, bulk density, and higher organic matter, and base cations as altitude increased. Red spruce seeds were collected from two nearby standing trees at the 1735 m site. A strip-split-split plot experiment was constructed using soils from the two lower elevations, which support natural red spruce stands. Besides a control (pH 5.6, NO[sub 3]:SO[sub 4] ratio 0.10), eight treatments corresponding to two pHs (3.5 and 4.2) with four NO[sub 3]:SO[sub 4] ratios (0.20, 0.33, 0.40, and 0.67) each were used. Seedling emergence and growth, chemistry of soil. Soil leachate, and plant tissue were analyzed to test soil differences and treatment effects of acidity, nitrate, and sulfate. Temporal patterns of germination respond more to soil than to rain chemistry, but significant interactions were found. Besides higher survival, faster germinating seedlings in the 1735 m soil also produced more complex root system and more biomass. Lower root-to-shoot ratios at more acidic treatments suggest a negative effect of acidity on root growth. Canonical discriminant analysis revealed that factors controlling overall soil chemistry were dominated by soil origin, then by rain pH.

  9. National Acid Precipitation Assessment Program Report to Congress: An Integrated Assessment

    DTIC Science & Technology

    2005-01-01

    qualitative indicators to assess the effectiveness of the cap and trade approach to reduce emissions, improve air quality and reduce acid deposition while...report indicates that nitrogen deposition has declined in some areas with resulting benefits. Overall a 40% reduction in NOx emissions from power...acidification.The report, however, also indicates that emission reductions beyond Title IV alone are not sufficient to allow sensitive forests and aquatic systems

  10. Production and functional evaluation of a protein concentrate from giant squid (Dosidicus gigas) by acid dissolution and isoelectric precipitation.

    PubMed

    Cortés-Ruiz, Juan A; Pacheco-Aguilar, Ramón; Elena Lugo-Sánchez, M; Gisela Carvallo-Ruiz, M; García-Sánchez, Guillermina

    2008-09-15

    A protein concentrate from giant squid (Dosidicus gigas) was produced under acidic conditions and its functional-technological capability evaluated in terms of its gel-forming ability, water holding capacity and colour attributes. Technological functionality of the concentrate was compared with that of squid muscle and a neutral concentrate. Protein-protein aggregates insoluble at high ionic strength (I=0.5M), were detected in the acidic concentrate as result of processing with no preclusion of its gel-forming ability during the sol-to-gel thermal transition. Even though washing under acidic condition promoted autolysis of the myosin heavy chain, the acidic concentrate displayed an outstanding ability to gel giving samples with a gel strength of 455 and 1160gcm at 75% and 90% compression respectively, and an AA folding test grade indicative of high gel strength, elasticity, and cohesiveness. The process proved to be a good alternative for obtaining a functional protein concentrate from giant squid muscle.

  11. Capillary Electrophoresis Analysis of Organic Amines and Amino Acids in Saline and Acidic Samples Using the Mars Organic Analyzer

    NASA Astrophysics Data System (ADS)

    Stockton, Amanda M.; Chiesl, Thomas N.; Lowenstein, Tim K.; Amashukeli, Xenia; Grunthaner, Frank; Mathies, Richard A.

    2009-11-01

    The Mars Organic Analyzer (MOA) has enabled the sensitive detection of amino acid and amine biomarkers in laboratory standards and in a variety of field sample tests. However, the MOA is challenged when samples are extremely acidic and saline or contain polyvalent cations. Here, we have optimized the MOA analysis, sample labeling, and sample dilution buffers to handle such challenging samples more robustly. Higher ionic strength buffer systems with pKa values near pH 9 were developed to provide better buffering capacity and salt tolerance. The addition of ethylaminediaminetetraacetic acid (EDTA) ameliorates the negative effects of multivalent cations. The optimized protocol utilizes a 75 mM borate buffer (pH 9.5) for Pacific Blue labeling of amines and amino acids. After labeling, 50 mM (final concentration) EDTA is added to samples containing divalent cations to ameliorate their effects. This optimized protocol was used to successfully analyze amino acids in a saturated brine sample from Saline Valley, California, and a subcritical water extract of a highly acidic sample from the Río Tinto, Spain. This work expands the analytical capabilities of the MOA and increases its sensitivity and robustness for samples from extraterrestrial environments that may exhibit pH and salt extremes as well as metal ions.

  12. Capillary electrophoresis analysis of organic amines and amino acids in saline and acidic samples using the Mars organic analyzer.

    PubMed

    Stockton, Amanda M; Chiesl, Thomas N; Lowenstein, Tim K; Amashukeli, Xenia; Grunthaner, Frank; Mathies, Richard A

    2009-11-01

    The Mars Organic Analyzer (MOA) has enabled the sensitive detection of amino acid and amine biomarkers in laboratory standards and in a variety of field sample tests. However, the MOA is challenged when samples are extremely acidic and saline or contain polyvalent cations. Here, we have optimized the MOA analysis, sample labeling, and sample dilution buffers to handle such challenging samples more robustly. Higher ionic strength buffer systems with pK(a) values near pH 9 were developed to provide better buffering capacity and salt tolerance. The addition of ethylaminediaminetetraacetic acid (EDTA) ameliorates the negative effects of multivalent cations. The optimized protocol utilizes a 75 mM borate buffer (pH 9.5) for Pacific Blue labeling of amines and amino acids. After labeling, 50 mM (final concentration) EDTA is added to samples containing divalent cations to ameliorate their effects. This optimized protocol was used to successfully analyze amino acids in a saturated brine sample from Saline Valley, California, and a subcritical water extract of a highly acidic sample from the Río Tinto, Spain. This work expands the analytical capabilities of the MOA and increases its sensitivity and robustness for samples from extraterrestrial environments that may exhibit pH and salt extremes as well as metal ions.

  13. Acidity, nutrients, and minerals in atmospheric precipitation over Florida: deposition patterns, mechanisms and ecological effects

    SciTech Connect

    Brezonik, P.L.; Hendry, C.D. Jr.; Edgerton, E.S.; Schulze, R.L.; Crisman, T.L.

    1983-06-01

    A monitoring network of 21 bulk and 4 wet/dry collectors located throughout Florida measured spatial and temporal trends during a one-year period from May 1978 to April 1979. The project summary notes that statewide deposition rates of nitrogen and phosphorus were below the loading rates associated with eutrophication, although nutrient concentrations were higher during the summer. Overall, pH appears to have relatively small effects (in the range 4.7-6.8) on community structure in soft-water Florida lakes. More dramatic effects could occur under more acidic conditions in the future. 4 references, 5 figures, 1 table.

  14. Universal nucleic acids sample preparation method for cells, spores and their mixture

    DOEpatents

    Bavykin, Sergei [Darien, IL

    2011-01-18

    The present invention relates to a method for extracting nucleic acids from biological samples. More specifically the invention relates to a universal method for extracting nucleic acids from unidentified biological samples. An advantage of the presently invented method is its ability to effectively and efficiently extract nucleic acids from a variety of different cell types including but not limited to prokaryotic or eukaryotic cells and/or recalcitrant organisms (i.e. spores). Unlike prior art methods which are focused on extracting nucleic acids from vegetative cell or spores, the present invention effectively extracts nucleic acids from spores, multiple cell types or mixtures thereof using a single method. Important that the invented method has demonstrated an ability to extract nucleic acids from spores and vegetative bacterial cells with similar levels effectiveness. The invented method employs a multi-step protocol which erodes the cell structure of the biological sample, isolates, labels, fragments nucleic acids and purifies labeled samples from the excess of dye.

  15. Nickel recovery from spent Raneynickel catalyst through dilute sulfuric acid leaching and soda ash precipitation.

    PubMed

    Lee, Jin Young; Rao, S Venkateswara; Kumar, B Nagaphani; Kang, Dong Jun; Reddy, B Ramachandra

    2010-04-15

    Pharmaceutical industry makes extensive use of Raneynickel catalyst for various organic drug intermediates/end products. Spent catalysts contain environmentally critical and economically valuable metals. In the present study, a simple hydrometallurgical process using dilute sulfuric acid leaching was described for the recovery of nickel from spent Raneynickel catalyst. Recovery of nickel varied with acid concentration and time, whereas temperature had negligible effect. Increase of S/L ratio to 30% (w/v) showed marginal effect on nickel (90%) recovery, whereas Al recovery decreased drastically to approximately 20%. Under the optimum conditions of leaching viz: 12 vol.% H(2)SO(4), 30 degrees C, 20% solid to liquid (S/L) ratio and 120 min reaction time, it was possible to recover 98.6% Ni along with 39.2% Al. Leach liquor [pH 0.7] containing 85.0 g/L Ni and 3.25 g/L Al was adjusted to pH 5.4 with 30 wt.% alkali for quantitative aluminum removal. Nickel loss was about 2% during this Al removal step. Nickel from the purified leach liquor was recovered as nickel carbonate by adding required amount of Na(2)CO(3). The purity of NiCO(3) product was found to be 100% with a Ni content of 48.6%. Na(2)SO(4) was recovered as a by-product with a purity of 99%. Complete process is presented.

  16. Evaluation of phosphate pebble as a precipitant for acid mine drainage treatment

    SciTech Connect

    Choi, J.C.; West, T.R.

    1995-12-01

    Laboratory testing was performed to evaluate the effectiveness of phosphate pebbles from Florida in the treatment of acid mine drainage under aerobic conditions. Using different flow rates, results show that phosphate pebbles effectively removed ferric iron up to 1,200 mg/l, aluminum up to 800 mg/l and sulfate up to 8,600 mg/l in three weeks. In addition, the pH increased to values as high as 3.2 in the effluent water from a pH of the influent water ranging from 2.1 to 2.2. Removal of ferric iron, aluminum, and sulfate as well as pH increases were inversely proportional to flow rates, ranging from 1.17 {times} 10{sup {minus}4} to 1.05 {times} 10{sup {minus}3} liters per minute per kg of phosphate pebble. Apparently this method can be applied to reduce acid mine drainage from old coal refuse piles, even those containing high concentration of ferric iron and aluminum ions.

  17. Effect of acidic precipitation on amphibian breeding in temporary ponds in Pennsylvania. [Rana sylvatica; Ambystoma jeffersonianum

    SciTech Connect

    Freda, J.; Dunson, W.A.

    1985-11-01

    This study assessed the impacts of acid deposition on amphibians breeding in temporary ponds in Pennsylvania by investigating the lowest pH's at which embryos could hatch, the physiological effects of low pH on amphibian larvae, pond chemistry and the influence of rainfall on pond pH, and the effect of pond pH on embryonic survival and local distribution of Ambystoma jeffersonianum and Rana sylvatica. At very low pH's, embryos stopped development soon after exposure. At higher but still lethal pH's, embryos became curled and failed to hatch. Embryos of Ambystoma were able to hatch even though they were curled, but R. sylvatica became trapped and died. Acute exposure to low pH's depressed sodium influx and accelerated sodium efflux, with a net loss of 50% of body sodium resulting in death. Increasing the external calcium concentration extended survival time by slowing the loss of sodium. Chronic exposure to low pH's resulted in reduction in body sodium, but to a lesser degree. R sylvatica tadpoles from a low pH pond had lower body sodium than tadpoles from a nearby high pH pond. Tadpoles from both ponds placed in a low pH pond underwent higher sodium efflux than when placed in the high pH pond. In studying the effect of low environmental pH, A. jeffersonianum was intolerant of low pH and was absent from most acidic ponds. R. sylvatica was tolerant and was found in ponds with the lowest pH. 73 refs., 14 figs., 21 tabs.

  18. Convenient and rapid determination of cimetidine in human plasma using perchloric acid-mediated plasma protein precipitation and high-performance liquid chromatography.

    PubMed

    Jantratid, Ekarat; Prakongpan, Sompol; Foley, Joe P; Dressman, Jennifer B

    2007-09-01

    This study demonstrates the analysis of cimetidine in human plasma with HPLC using a simplified sample preparation by protein precipitation with perchloric acid. Plasma cimetidine concentration was determined by plotting peak height ratio of cimetidine to ranitidine (internal standard, IS) against cimetidine concentrations in plasma. The cimetidine and ranitidine peaks were completely separated and no interference from plasma was observed. The lower limit of quantification (LLOQ) of the method was established at 0.1 microg/mL with a precision of 4.3% and a relative error of 1.9%. The average analytical recovery was >90% over the range of cimetidine concentrations (0.1-15.0 microg/mL). The linearity of calibration curve was excellent (r(2) > 0.999). The within- and between-day precision and accuracy, expressed as the coefficients of variation and relative error, were found to be less than 5%. Compared with previously reported methods, the analytical technique for cimetidine determination in human plasma presented here demonstrates comparable accuracy and precision, an acceptable analysis time, shorter and simpler sample preparation, and a reduced need for complicated equipment. The method presented here is simple and rapid, and the precision and sensitivity are appropriate for the determination of cimetidine in plasma in pharmacokinetic studies.

  19. Jarosite Precipitation from Acidic Saline Waters in Kachchh, Gujarat, India: an Appropriate Martian Analogue?

    NASA Astrophysics Data System (ADS)

    Mitra, S.; Gupta, S.; Bhattacharya, S.; Banerjee, S.; Chauhan, P.; Parthasarathy, G.

    2014-12-01

    The origin of jarosite [KFe3(SO4)2(OH)6] on the Martian surface has been an intriguing problem since the Mars Exploration Rover 'Opportunity' first revealed its presence at the Meridiani Planum on Mars. To explain its origin, several terrestrial analogue sites have been studied in different geographical zones. Although several models have been suggested, there is a consensus that only the prevalence of acidic and oxidizing aqueous environmental conditions are conducive to form jarosite. In the Kachchh region of Gujarat, western India, jarosite has been recently discovered from gorges dissecting the Paleocene Matanumadh Formation sediments, that overlie basalts of the Deccan Volcanic Province. This formation comprises pebble conglomerates, carbonaceous shales and purple sandstones capped by a laterite on top. Jarosite, in association with gypsum and goethite, has been detected through FTIR and VNIR spectrometry in almost all litho-units of the succession, albeit in different modes and concentrations. The occurrence of jarosite within black shale in other parts of the world, has been attributed to the oxidation of pyrites within the shale layers. However, in shales of the Matanumadh Formation, jarosite is restricted to fractures that cut across the bedding, while the overlying purple sandstone unit only preserves jarosite in shale clasts within the sandstone. Since the sandstone overlies the black shale layer, downward percolation of sulfate-bearing water from the oxidation of pyrite within the shale layer cannot explain jarosite formation in this unit. In addition, no jarosite is observed below or within pyrite-rich lignite bearing sections in other parts of Kachchh. Alternative suggestions, that jarosite developed in the immediate aftermath of Deccan volcanism as surface waters were rendered acidic by interaction with the final phase of volcanic effusives, are also unlikely as on-going studies suggest that jarosite is not restricted to the Matanumadh Formation. The

  20. Limestone characterization to model damage from acidic precipitation: Effect of pore structure on mass transfer

    USGS Publications Warehouse

    Leith, S.D.; Reddy, M.M.; Irez, W.F.; Heymans, M.J.

    1996-01-01

    The pore structure of Salem limestone is investigated, and conclusions regarding the effect of the pore geometry on modeling moisture and contaminant transport are discussed based on thin section petrography, scanning electron microscopy, mercury intrusion porosimetry, and nitrogen adsorption analyses. These investigations are compared to and shown to compliment permeability and capillary pressure measurements for this common building stone. Salem limestone exhibits a bimodal pore size distribution in which the larger pores provide routes for convective mass transfer of contaminants into the material and the smaller pores lead to high surface area adsorption and reaction sites. Relative permeability and capillary pressure measurements of the air/water system indicate that Salem limestone exhibits high capillarity end low effective permeability to water. Based on stone characterization, aqueous diffusion and convection are believed to be the primary transport mechanisms for pollutants in this stone. The extent of contaminant accumulation in the stone depends on the mechanism of partitioning between the aqueous and solid phases. The described characterization techniques and modeling approach can be applied to many systems of interest such as acidic damage to limestone, mass transfer of contaminants in concrete and other porous building materials, and modeling pollutant transport in subsurface moisture zones.

  1. Chemical composition of softwater Florida lakes and their sensitivity to acid precipitation

    SciTech Connect

    Hendry, C.D.; Brezonik, P.L.

    1984-02-01

    Based on alkalinity data for 596 lakes, 31 percent of Florida's 7300 lakes have < 100 ..mu..eq/L alkalinity and are sensitive to acid deposition. More than two-thirds of the lakes in 12 northern Florida counties fit this criterion. Increasing aluminum and decreasing nutrient and chlorophyll a concentrations were observed with decreasing pH in a survey of 20 softwater lakes. Maximum measured aluminum values (100-150 ..mu..g/L) are below levels associated with fish toxicity. Factor analysis showed that lake chemistry was related to three principal factors, representing three major processes: watershed weathering, acidification, and nutrient inputs. An acidification index defined as the difference between excess SO/sub 4//sup 2 -/ and excess (Ca/sup 2 +/ + Mg/sup 2 +/) accounted for 74 percent of the variance in lake pH. Comparison of historical (late 1950s) and present data for pH, alkalinity, and excess SO/sub 4//sup 2 -/ indicated loss of alkalinity (> 25 ..mu..eq/L) and increases in excess SO/sub 4//sup 2 -/ (16-34 ..mu..eq/L) in several softwater lakes.

  2. Digital microfluidic hub for automated nucleic acid sample preparation.

    SciTech Connect

    He, Jim; Bartsch, Michael S.; Patel, Kamlesh D.; Kittlaus, Eric A.; Remillared, Erin M.; Pezzola, Genevieve L.; Renzi, Ronald F.; Kim, Hanyoup

    2010-07-01

    We have designed, fabricated, and characterized a digital microfluidic (DMF) platform to function as a central hub for interfacing multiple lab-on-a-chip sample processing modules towards automating the preparation of clinically-derived DNA samples for ultrahigh throughput sequencing (UHTS). The platform enables plug-and-play installation of a two-plate DMF device with consistent spacing, offers flexible connectivity for transferring samples between modules, and uses an intuitive programmable interface to control droplet/electrode actuations. Additionally, the hub platform uses transparent indium-tin oxide (ITO) electrodes to allow complete top and bottom optical access to the droplets on the DMF array, providing additional flexibility for various detection schemes.

  3. Using column lysimetry to evaluate acid-precipitation effects. Forest Service research paper

    SciTech Connect

    Harris, A.R.; Stone, D.M.

    1990-01-01

    The paper describes the experimental design and approach used to solve problems encountered with soil column collection, instrumentation, materials and methods, and maintenance of natural soil temperatures. Some preliminary results are presented. Also, basic data on the soil and vegetation of the sampled sites are included to form a database for use by forest soil scientists and land managers. The specific objective of the study was to determine the sensitivity of soils with low base-saturation to increased anion loadings and the susceptibility of these soil solutions to pH depression and negative alkalinities. A secondary objective was to determine whether reduced sulfate deposition will reverse the acidification processes and return soil water alkalinities from negative to positive.

  4. On the range of future Sahel precipitation projections and the selection of a sub-sample of CMIP5 models for impact studies

    NASA Astrophysics Data System (ADS)

    Monerie, Paul-Arthur; Sanchez-Gomez, Emilia; Boé, Julien

    2016-06-01

    The future evolution of the West African Monsoon is studied by analyzing 32 CMIP5 models under the rcp8.5 emission scenario. A hierarchical clustering method based on the simulated pattern of precipitation changes is used to classify the models. Four groups, which do not agree on the simple sign of future Sahel precipitation change, are obtained. We find that the inter-group differences are mainly associated with the large spread in (1) temperature increase over the Sahara and North Atlantic and in (2) the strengthening of low and mid-level winds. A wetter Sahel is associated with a strong increase in temperature over the Sahara (>6 °C), a northward shift of the monsoon system and a weakening of the African Easterly jet. A dryer Sahel is associated with subsidence anomalies, a strengthening of the 600 hPa wind speed, and a weaker warming over the Northern Hemisphere. Moreover, the western (central) Sahel is projected to become dryer (wetter) during the first months (last months) of the rainy season in a majority of models. We propose several methods to select a sub-sample of models that captures both the ensemble mean pattern and/or the spread of precipitation changes from the full ensemble. This methodology is useful in all the situations for which it is not possible to deal with a large ensemble of models, and in particular most impact studies. We show that no relationship exists between the climatological mean biases in precipitation and temperature and the future changes in the monsoon intensity. This indicates that the mean bias is therefore not a reliable metric for the model selection. For this reason, we propose several methodologies, based on the projected precipitation changes: The "diversity" method, which consists in the selection of one model from each group is the most appropriate to capture the spread in precipitation change. The "pattern selection" method, which consists in the selection of models in a single group allows to select models for the

  5. Heterogeneous degradation of precipitated hexamine from wastewater by catalytic function of silicotungstic acid in the presence of H2O2 and H2O2/Fe2+.

    PubMed

    Taghdiri, Mehdi; Saadatjou, Naghi; Zamani, Navid; Farrokhi, Reyhaneh

    2013-02-15

    The industrial wastewater produced by hexamine plants is considered as a major environmental polluting factor due to resistance to biodegradation. So the treatment of such wastewater is required. In this work, the removal of hexamine from wastewater and its degradation have been studied. Hexamine was precipitated through formation of an insoluble and stable compound with silicotungstic acid. The oxidative heterogeneous degradation of precipitated hexamine was carried out with hydrogen peroxide (H(2)O(2)) aqueous solution and H(2)O(2)/Fe(2+) under the catalysis of silicotungstic acid. The operating conditions including amount of precipitate, hydrogen peroxide and ferrous ion dosage, temperature, time and pH were optimized by evaluating the removal of total organic carbon from system. A total organic carbon conversion higher than 70% was achieved in the presence of H(2)O(2)/Fe(2+). The experimental results showed that hexamine can be effectively degraded with H(2)O(2) and H(2)O(2)/Fe(2+) under the catalysis of silicotungstic acid. It was interesting that the solution of dissolved precipitate with H(2)O(2) can re-react with hexamine after the removal of excess hydrogen peroxide. This observation indicates the catalysis role of silicotungstic acid in the degradation of hexamine. A kinetic analysis based on total organic carbon reduction was carried out. The two steps mechanism was proposed for the degradation of hexamine.

  6. Determination of cadmium in tobacco smoke by electrothermal atomic absorption spectroscopy with electrostatic precipitation of samples on the graphite tube atomizer

    NASA Astrophysics Data System (ADS)

    Altman, E. L.; Panichev, N. A.

    2003-05-01

    The determination of Cd in ambient air, associated with tobacco smoke, has been carried out by electrostatic precipitation of Cd directly in a graphite tube, which was subsequently used as an atomizer in electrothermal atomization atomic absorption spectroscopy (ET-AAS). It is shown that graphite tube permanently modified with Ir allows carrying out pyrolysis of collected samples at 1000^circC, leading to minimization of the blank. The combination of electrostatic precipitation of Cd from ambient air into the graphite tube with high efficiency of Cd determination by ET-AAS allows to trace Cd in ambient air for 25 min after the smoking a cigarette. The limit of detection (LOD) of Cd determination was found to be 0.2 ng m^{-3} The results of investigations confirm the danger of passive smoking due to the presence of Cd in smoking areas.

  7. Archive of Samples for Long-Term Preservation of RNA and Other Nucleic Acids

    DTIC Science & Technology

    2016-05-15

    nucleic acids W81XWH-12-C-0030 Sb. GRANT NUMBER Sc. PROGRAM ELEMENT NUMBER 6. AUTHOR(S) Sd. PROJECT NUMBER Gerald Dodson Se. TASK NUMBER Sf. WORK...the development of a scalable all ambient temperature biological sample workflow preserving nucleic acids for molecular analysis. This ambient...achieved the final Phase II milestone of processing 500 samples n a week. 1S. SUBJECT TERMS Nucleic Acid Preservation , Cost Reduction , Ambient

  8. Natural abiotic formation of oxalic acid in soils: results from aromatic model compounds and soil samples.

    PubMed

    Studenroth, Sabine; Huber, Stefan G; Kotte, Karsten; Schöler, Heinz F

    2013-02-05

    Oxalic acid is the smallest dicarboxylic acid and plays an important role in soil processes (e.g., mineral weathering and metal detoxification in plants). We have first proven its abiotic formation in soils and investigated natural abiotic degradation processes based on the oxidation of soil organic matter, enhanced by Fe(3+) and H(2)O(2) as hydroxyl radical suppliers. Experiments with the model compound catechol and further hydroxylated benzenes were performed to examine a common degradation pathway and to presume a general formation mechanism of oxalic acid. Two soil samples were tested for the release of oxalic acid and the potential effects of various soil parameters on oxalic acid formation. Additionally, the soil samples were treated with different soil sterilization methods to prove the oxalic acid formation under abiotic soil conditions. Different series of model experiments were conducted to determine a range of factors including Fe(3+), H(2)O(2), reaction time, pH, and chloride concentration on oxalic acid formation. Under certain conditions, catechol is degraded up to 65.6% to oxalic acid referring to carbon. In serial experiments with two soil samples, oxalic acid was produced, and the obtained results are suggestive of an abiotic degradation process. In conclusion, Fenton-like conditions with low Fe(3+) concentrations and an excess of H(2)O(2) as well as acidic conditions were required for an optimal oxalic acid formation. The presence of chloride reduced oxalic acid formation.

  9. Correlating Mineralogy and Amino Acid Contents of Milligram-Scale Murchison Carbonaceous Chondrite Samples

    NASA Technical Reports Server (NTRS)

    Burton, Aaron, S.; Berger, Eve L.; Locke, Darren R.; Elsila, Jamie E.; Glavin, Daniel P.; Dworkin, Jason P.

    2015-01-01

    Amino acids, the building blocks of proteins, have been found to be indigenous in most of the carbonaceous chondrite groups. The abundances of amino acids, as well as their structural, enantiomeric and isotopic compositions differ significantly among meteorites of different groups and petrologic types. This suggests that there is a link between parent-body conditions, mineralogy and the synthesis and preservation of amino acids (and likely other organic molecules). However, elucidating specific causes for the observed differences in amino acid composition has proven extremely challenging because samples analyzed for amino acids are typically much larger ((is) approximately 100 mg powders) than the scale at which meteorite heterogeneity is observed (sub mm-scale differences, (is) approximately 1-mg or smaller samples). Thus, the effects of differences in mineralogy on amino acid abundances could not be easily discerned. Recent advances in the sensitivity of instrumentation have made possible the analysis of smaller samples for amino acids, enabling a new approach to investigate the link between mineralogical con-text and amino acid compositions/abundances in meteorites. Through coordinated mineral separation, mineral characterization and highly sensitive amino acid analyses, we have performed preliminary investigations into the relationship between meteorite mineralogy and amino acid composition. By linking amino acid data to mineralogy, we have started to identify amino acid-bearing mineral phases in different carbonaceous meteorites. The methodology and results of analyses performed on the Murchison meteorite are presented here.

  10. A perspective of stepwise utilisation of Bayer red mud: Step two--Extracting and recovering Ti from Ti-enriched tailing with acid leaching and precipitate flotation.

    PubMed

    Huang, Yanfang; Chai, Wencui; Han, Guihong; Wang, Wenjuan; Yang, Shuzhen; Liu, Jiongtian

    2016-04-15

    The extraction and recovery of Ti from Ti-enriched tailing with acid leaching and precipitate flotation, as one of the critical steps, was proposed for the stepwise utilization of red mud. The factors influencing acid leaching and precipitate flotation were examined by factorial design. The leaching thermodynamics, kinetics of Ti(4+), Al(3+) and Fe(3+), and the mechanism of selectively Fe(3+) removal using [Hbet][Tf2N] as precipitating reagent were discussed. The extracting of Ti(4+), Al(3+) and Fe(3+) in concentrated H2SO4 is controlled by diffusion reactions, depending mainly upon leaching time and temperature. The maximum extracting efficiency of Ti(4+) is approximately 92.3%, whereas Al(3+) and Fe(3+) leaching are respectively 75.8% and 84.2%. [Hbet][Tf2N], as a precipitating reagent, operates through a coordination mechanism in flotation. The pH value is the key factor influencing the flotation recovery of Ti(4+), whereas the dosage of precipitating reagent is that for Al(3+) recovery. The maximum flotation recovery of Ti(4+) is 92.7%, whereas the maximum Al(3+) recovery is 93.5%. The total recovery rate for extracting and recovering titanium is 85.5%. The liquor with Ti(4+) of 15.5g/L, Al(3+) of 30.4g/L and Fe(3+) of 0.48g/L was obtained for the following hydrolysis step in the integrated process for red mud utilisation.

  11. Strategies for automated sample preparation, nucleic acid purification, and concentration of low-target-number nucleic acids in environmental and food processing samples

    NASA Astrophysics Data System (ADS)

    Bruckner-Lea, Cynthia J.; Holman, David A.; Schuck, Beatrice L.; Brockman, Fred J.; Chandler, Darrell P.

    1999-01-01

    The purpose of this work is to develop a rapid, automated system for nucleic acid purification and concentration from environmental and food processing samples. Our current approach involves off-line filtration and cell lysis (ballistic disintegration) functions in appropriate buffers followed by automated nucleic acid capture and purification on renewable affinity matrix microcolumns. Physical cell lysis and renewable affinity microcolumns eliminate the need for toxic organic solvents, enzyme digestions or other time- consuming sample manipulations. Within the renewable affinity microcolumn, we have examined nucleic acid capture and purification efficiency with various microbead matrices (glass, polymer, paramagnetic), surface derivitization (sequence-specific capture oligonucleotides or peptide nucleic acids), and DNA target size and concentration under variable solution conditions and temperatures. Results will be presented comparing automated system performance relative to benchtop procedures for both clean (pure DNA from a laboratory culture) and environmental (soil extract) samples, including results which demonstrate 8 minute purification and elution of low-copy nucleic acid targets from a crude soil extract in a form suitable for PCR or microarray-based detectors. Future research will involve the development of improved affinity reagents and complete system integration, including upstream cell concentration and cell lysis functions and downstream, gene-based detectors. Results of this research will ultimately lead to improved processes and instrumentation for on-line, automated monitors for pathogenic micro-organisms in food, water, air, and soil samples.

  12. Molecularly imprinted microspheres and nanoparticles prepared using precipitation polymerisation method for selective extraction of gallic acid from Emblica officinalis.

    PubMed

    Pardeshi, Sushma; Dhodapkar, Rita; Kumar, Anupama

    2014-03-01

    This paper reports the preparation of gallic acid (GA) molecularly imprinted polymers (MIPs) by the precipitation polymerisation and highlights the effect of porogen on particle size and specific molecular recognition properties. MIP, M-100 prepared in the porogen acetonitrile and MIP, M-75 prepared in a mixture of acetonitrile-toluene (75:25 v/v), resulted in the formation of microspheres with approximately 4μm particle size and surface area of 96.73m(2)g(-1) and nanoparticles (0.8-1000nm) and a surface area of 345.9m(2)g(-1), respectively. The Langmuir-Freundlich isotherm study revealed that M-75 has comparatively higher number of binding sites which are homogenous and has higher affinity for GA. The MIPs selectively recognised GA in presence of its structural analogues. Pure GA with percent recovery of 75 (±1.6) and 83.4 (±2.2) was obtained from the aqueous extract of Emblica officinalis by M-100 and M-75, respectively and hot water at 60°C served as the eluting solvent.

  13. Zirconium(IV) tungstate nanoparticles prepared through chemical co-precipitation method and its function as solid acid catalyst

    NASA Astrophysics Data System (ADS)

    Sadanandan, Manoj; Bhaskaran, Beena

    2014-08-01

    In this paper, we report the synthesis of zirconium(IV) tungstate nanoparticles, a new and efficient catalyst for the oxidation of benzyl alcohol and esterification of acetic acid with various alcohols. The nanoparticle catalyst was prepared using the room temperature chemical co-precipitation method. The catalyst was characterized with thermogravimetric and differential thermal analysis, elemental analysis, X-ray diffraction analysis (XRD), fourier transform infrared spectroscopy (FT-IR), high-resolution transmission electron microscopy (HRTEM), atomic force microscopy (AFM) and the Brunauer-Emmett-Teller (BET) surface area. The crystallite size was found to be ~20 nm as revealed by XRD, HRTEM and AFM. The Na+ exchange capacity was found to be 2.76 meq g-1 and the surface area of the compound measured using BET method was found to be 250-265 m2 g-1. The high value of ion exchange capacity indicates the presence of surface hydroxyl groups. The prepared nanoparticles have proven to be excellent catalysts for both oxidation and ester synthesis under mild reaction conditions. The mechanism of the catalytic reaction was studied as well.

  14. The effects of acid precipitation runoff episodes on reservoir and tapwater quality in an Appalachian Mountain water supply.

    PubMed Central

    Sharpe, W E; DeWalle, D R

    1990-01-01

    The aluminum concentration and Ryznar Index increased and the pH decreased in a small Appalachian water supply reservoir following acid precipitation runoff episodes. Concomitant increases in tapwater aluminum and decreases in tapwater pH were also observed at two homes in the water distribution system. Lead concentrations in the tapwater of one home frequently exceeded recommended levels, although spatial and temporal variation in tapwater copper and lead concentrations was considerable. Since source water and reservoir water copper and lead concentrations were much lower, the increased copper and lead concentrations in tapwater were attributed to corrosion of household plumbing. Tapwater copper concentration correlated well with tapwater pH and tapwater temperature. Asbestos fibers were not detected in tapwater. The asbestos-cement pipe in the water distribution system was protected by a spontaneous metallic coating that inhibited fiber release from the pipe. Several simultaneous reactions were hypothesized to be taking place in the distribution system that involved corrosion of metallic components and coating of asbestos-cement pipe components in part with corrosion products and in part by cations of watershed origin. Greater water quality changes might be expected in areas of higher atmospheric deposition. Images FIGURE 5. FIGURE 6. PMID:2088742

  15. Response of surface water chemistry to reduced levels of acid precipitation: Comparison of trends in two regions of New York, USA

    USGS Publications Warehouse

    Burns, Douglas A.; McHale, M.R.; Driscoll, C.T.; Roy, K.M.

    2006-01-01

    In light of recent reductions in sulphur (S) and nitrogen (N) emissions mandated by Title IV of the Clean Air Act Amendments of 1990, temporal trends and trend coherence in precipitation (1984-2001 and 1992-2001) and surface water chemistry (1992-2001) were determined in two of the most acid-sensitive regions of North America, i.e. the Catskill and Adirondack Mountains of New York. Precipitation chemistry data from six sites located near these regions showed decreasing sulphate (SO42-), nitrate (NO3-), and base cation (CB) concentrations and increasing pH during 1984-2001, but few significant trends during 1992-2001. Data from five Catskill streams and 12 Adirondack lakes showed decreasing trends in SO42- concentrations at all sites, and decreasing trends in NO3-, CB, and H+ concentrations and increasing trends in dissolved organic carbon at most sites. In contrast, acid-neutralizing capacity (ANC increased significantly at only about half the Adirondack lakes and in one of the Catskill streams. Flow correction prior to trend analysis did not change any trend directions and had little effect on SO42- trends, but it caused several significant non-flow-corrected trends in NO3- and ANC to become non-significant, suggesting that trend results for flow-sensitive constituents are affected by flow-related climate variation. SO42- concentrations showed high temporal coherence in precipitation, surface waters, and in precipitation-surface water comparisons, reflecting a strong link between S emissions, precipitation SO42- concentrations, and the processes that affect S cycling within these regions. NO3- and H+ concentrations and ANC generally showed weak coherence, especially in surface waters and in precipitation-surface water comparisons, indicating that variation in local-scale processes driven by factors such as climate are affecting trends in acid-base chemistry in these two regions. Copyright ?? 2005 John Wiley & Sons, Ltd.

  16. A Simple Protein Precipitation-based Simultaneous Quantification of Lovastatin and Its Active Metabolite Lovastatin Acid in Human Plasma by Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry using Polarity Switching.

    PubMed

    Wujian, Ju; Kuan-Wei, Peng; Sihyung, Yang; Huijing, Sun; Mario, Sampson; Zhuo, Wang Michael

    2015-05-01

    Lovastatin is an anti-cholesterol lactone drug indicated for the treatment of hyperlipidemia and to reduce the risk of coronary heart disease. It is converted to the β-hydroxy acid form (lovastatin acid) in vivo, which is the major pharmacologically active metabolite. Here, we describe the development and validation of an ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)-based method utilizing polarity switching for the simultaneous quantification of lovastatin and lovastatin acid in human plasma. Simple protein precipitation extraction and direct injection of the extracted samples without drying/reconstitution showed good recoveries of both analytes (~70%). The developed method exhibited satisfactory intra-day and inter-day accuracy and precision. The interconversion between lovastatin and lovastatin acid during sample preparation and storage was minimal (< 1.9%). The lower limits of quantification were 0.5 and 0.2 nM (or 0.2 and 0.084 ng/mL) for lovastatin and lovastatin acid, respectively, using only 50 μL of plasma during extraction. The validated method was successfully applied to analyze plasma samples obtained from a healthy human subject who enrolled in a clinical drug interaction study involving lovastatin.

  17. Nucleic acid isolation from ecological samples--fungal associations, mycorrhizae.

    PubMed

    Koide, Roger T

    2005-01-01

    Mycorrhizal fungi are among the most common symbioses found in terrestrial ecosystems, both natural and managed. They are important for many reasons, but most notably because of their positive effects on plant growth, which are mediated by their uptake of nutrients from the soil and transport of these to the roots. Moreover, many edible fungi are mycorrhizal. The study of mycorrhizal fungi has been hampered by the inability to identify species and individuals in the soil. This has been greatly aided by DNA-based methods, which first require the extraction of DNA. Herein, I discuss some general concerns that must be considered when extracting and purifying DNA from ecological samples and offer specific methods for soil, mycorrhizal roots, and fruiting bodies. These methods are rapid, safe, effective, relatively inexpensive, and convenient because they are based on commercially available kits.

  18. Purifying Nucleic Acids from Samples of Extremely Low Biomass

    NASA Technical Reports Server (NTRS)

    La Duc, Myron; Osman, Shariff; Venkateswaran, Kasthuri

    2008-01-01

    A new method is able to circumvent the bias to which one commercial DNA extraction method falls prey with regard to the lysing of certain types of microbial cells, resulting in a truncated spectrum of microbial diversity. By prefacing the protocol with glass-bead-beating agitation (mechanically lysing a much more encompassing array of cell types and spores), the resulting microbial diversity detection is greatly enhanced. In preliminary studies, a commercially available automated DNA extraction method is effective at delivering total DNA yield, but only the non-hardy members of the bacterial bisque were represented in clone libraries, suggesting that this method was ineffective at lysing the hardier cell types. To circumvent such a bias in cells, yet another extraction method was devised. In this technique, samples are first subjected to a stringent bead-beating step, and then are processed via standard protocols. Prior to being loaded into extraction vials, samples are placed in micro-centrifuge bead tubes containing 50 micro-L of commercially produced lysis solution. After inverting several times, tubes are agitated at maximum speed for two minutes. Following agitation, tubes are centrifuged at 10,000 x g for one minute. At this time, the aqueous volumes are removed from the bead tubes and are loaded into extraction vials to be further processed via extraction regime. The new method couples two independent methodologies in such as way as to yield the highest concentration of PCR-amplifiable DNA with consistent and reproducible results and with the most accurate and encompassing report of species richness.

  19. Selective Precipitation of Thorium lodate from a Tartaric Acid-Hydrogen Peroxide Medium Application to Rapid Spectrophotometric Determination of Thorium in Silicate Rocks and in Ores

    USGS Publications Warehouse

    Grimaldi, F.S.

    1957-01-01

    This paper presents a selective iodate separation of thorium from nitric acid medium containing d-tartaric acid and hydrogen peroxide. The catalytic decomposition of hydrogen peroxide is prevented by the use of 8quinolinol. A few micrograms of thorium are separated sufficiently clean from 30 mg. of such oxides as cerium, zirconium, titanium, niobium, tantalum, scandium, or iron with one iodate precipitation to allow an accurate determination of thorium with the thoronmesotartaric acid spectrophotometric method. The method is successful for the determination of 0.001% or more of thorium dioxide in silicate rocks and for 0.01% or more in black sand, monazite, thorite, thorianite, eschynite, euxenite, and zircon.

  20. Polymerase chain reaction system using magnetic beads for analyzing a sample that includes nucleic acid

    DOEpatents

    Nasarabadi, Shanavaz [Livermore, CA

    2011-01-11

    A polymerase chain reaction system for analyzing a sample containing nucleic acid includes providing magnetic beads; providing a flow channel having a polymerase chain reaction chamber, a pre polymerase chain reaction magnet position adjacent the polymerase chain reaction chamber, and a post pre polymerase magnet position adjacent the polymerase chain reaction chamber. The nucleic acid is bound to the magnetic beads. The magnetic beads with the nucleic acid flow to the pre polymerase chain reaction magnet position in the flow channel. The magnetic beads and the nucleic acid are washed with ethanol. The nucleic acid in the polymerase chain reaction chamber is amplified. The magnetic beads and the nucleic acid are separated into a waste stream containing the magnetic beads and a post polymerase chain reaction mix containing the nucleic acid. The reaction mix containing the nucleic acid flows to an analysis unit in the channel for analysis.

  1. Citric acid traps to replace sulphuric acid in the ammonia diffusion of dilute water samples for 15N analysis.

    PubMed

    Schleppi, Patrick; Bucher-Wallin, Inga; Saurer, Matthias; Jäggi, Maya; Landolt, Werner

    2006-01-01

    The analysis of 15N in aqueous samples requires the concentration of dissolved nitrogen (N) into a small volume that can be analysed by mass spectrometry. This is conveniently achieved by the NH3 diffusion technique, where NH4+ is captured on small acidified filters enclosed in PTFE. NO3- can be analysed the same way by reducing it to NH4+ with Devarda's alloy. H2SO4 is commonly used for the acidification of the filters. During combustion, however, this acid leads to the production of SO2 and elemental sulphur, which both have detrimental effects on the mass spectrometer. We propose here to replace H2SO4 with citric acid because it is combusted completely to CO2 and H2O in the elemental analyser before entering the mass spectrometer. Citric acid was found to give comparable results in terms of N recovery and 15N values, both for NH4+ and for NO3- samples. Blank samples revealed that N contamination was slightly lower using citric instead of sulphuric acid as acidifier of the glass filters. NH4+ samples first concentrated over cation-exchange columns were strongly acidic and several methods were tested to raise the pH for the subsequent diffusion. These samples gave incomplete N recoveries, but this problem was independent of the acid used on the filters and of the final pH of the sample. Complete recovery was achieved only by increasing the volume of the eluate from the columns. Citric acid can thus generally be recommended instead of H2SO4 for ammonia diffusion.

  2. The search for and identification of amino acids, nucleobases and nucleosides in samples returned from Mars

    NASA Technical Reports Server (NTRS)

    Gehrke, Charles W.; Ponnamperuma, Cyril; Kuo, Kenneth C.; Stalling, David L.; Zumwalt, Robert W.

    1989-01-01

    An investigation of the returned Mars samples for biologically important organic compounds, with emphasis on amino acid, the puring and pyrimidine bases, and nucleosides is proposed. These studies would be conducted on subsurface samples obtained by drilling past the surface oxidizing layer with emphasis on samples containing the larges quantities of organic carbon as determined by the rover gas chromatographic mass spectrometer (GCMS). Extraction of these molecules from the returned samples will be performed using the hydrothermal extraction technique described by Cheng and Ponnamperuma. More rigorous extraction methods will be developed and evaluated. For analysis of the extract for free amino acids or amino acids present in a bound or peptidic form, aliquots will be analyzed by capillary GCMS both before and after hydrolysis with 6N hydrochloric acid. Establishment of the presence of amino acids would then lead to the next logical step which would be the use of chiral stationary gas chromatography phases to determine the enatiomeic composition of the amino acids present, and thus potentially establish their biotic or abiotic origin. Confirmational analyses for amino acids would include ion-exchange and reversed-phase liquid chromatographic analysis. For analyses of the returned Mars samples for nucleobases and nucleosides, affinity and reversed-phase liquid chromatography would be utilized. This technology coupled with scanning UV detection for identification, presents a powerful tool for nucleobase and nucleoside analysis. Mass spectrometric analysis of these compounds would confirm their presence in samples returned form Mars.

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

    PubMed

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

    2008-02-01

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

  4. PRECIPITATION OF PROTACTINIUM

    DOEpatents

    Moore, R.L.

    1958-07-15

    An lmprovement in the separation of protactinium from aqueous nitric acid solutions is described. 1t covers the use of lead dioxide and tin dioxide as carrier precipitates for the protactinium. In carrying out the process, divalent lead or divalent tin is addcd to the solution and oxidized, causing formation of a carrier precipitate of lead dioxide or stannic oxide, respectively.

  5. Methods for point-of-care detection of nucleic acid in a sample

    DOEpatents

    Bearinger, Jane P.; Dugan, Lawrence C.

    2015-12-29

    Provided herein are methods and apparatus for detecting a target nucleic acid in a sample and related methods and apparatus for diagnosing a condition in an individual. The condition is associated with presence of nucleic acid produced by certain pathogens in the individual.

  6. Apparatus for point-of-care detection of nucleic acid in a sample

    DOEpatents

    Bearinger, Jane P.; Dugan, Lawrence C.

    2016-04-19

    Provided herein are methods and apparatus for detecting a target nucleic acid in a sample and related methods and apparatus for diagnosing a condition in an individual. The condition is associated with presence of nucleic acid produced by certain pathogens in the individual.

  7. The precipitation of indium at elevated pH in a stream influenced by acid mine drainage.

    PubMed

    White, Sarah Jane O; Hussain, Fatima A; Hemond, Harold F; Sacco, Sarah A; Shine, James P; Runkel, Robert L; Walton-Day, Katherine; Kimball, Briant A

    2017-01-01

    Indium is an increasingly important metal in semiconductors and electronics and has uses in important energy technologies such as photovoltaic cells and light-emitting diodes (LEDs). One significant flux of indium to the environment is from lead, zinc, copper, and tin mining and smelting, but little is known about its aqueous behavior after it is mobilized. In this study, we use Mineral Creek, a headwater stream in southwestern Colorado severely affected by heavy metal contamination as a result of acid mine drainage, as a natural laboratory to study the aqueous behavior of indium. At the existing pH of ~3, indium concentrations are 6-29μg/L (10,000× those found in natural rivers), and are completely filterable through a 0.45μm filter. During a pH modification experiment, the pH of the system was raised to >8, and >99% of the indium became associated with the suspended solid phase (i.e. does not pass through a 0.45μm filter). To determine the mechanism of removal of indium from the filterable and likely primarily dissolved phase, we conducted laboratory experiments to determine an upper bound for a sorption constant to iron oxides, and used this, along with other published thermodynamic constants, to model the partitioning of indium in Mineral Creek. Modeling results suggest that the removal of indium from the filterable phase is consistent with precipitation of indium hydroxide from a dissolved phase. This work demonstrates that nonferrous mining processes can be a significant source of indium to the environment, and provides critical information about the aqueous behavior of indium.

  8. The precipitation of indium at elevated pH in a stream influenced by acid mine drainage

    USGS Publications Warehouse

    White, Sarah Jane O.; Hussain, Fatima A.; Hemond, Harold F.; Sacco, Sarah A.; Shine, James P.; Runkel, Robert L.; Walton-Day, Katherine; Kimball, Briant A.

    2017-01-01

    Indium is an increasingly important metal in semiconductors and electronics and has uses in important energy technologies such as photovoltaic cells and light-emitting diodes (LEDs). One significant flux of indium to the environment is from lead, zinc, copper, and tin mining and smelting, but little is known about its aqueous behavior after it is mobilized. In this study, we use Mineral Creek, a headwater stream in southwestern Colorado severely affected by heavy metal contamination as a result of acid mine drainage, as a natural laboratory to study the aqueous behavior of indium. At the existing pH of ~ 3, indium concentrations are 6–29 μg/L (10,000 × those found in natural rivers), and are completely filterable through a 0.45 μm filter. During a pH modification experiment, the pH of the system was raised to > 8, and > 99% of the indium became associated with the suspended solid phase (i.e. does not pass through a 0.45 μm filter). To determine the mechanism of removal of indium from the filterable and likely primarily dissolved phase, we conducted laboratory experiments to determine an upper bound for a sorption constant to iron oxides, and used this, along with other published thermodynamic constants, to model the partitioning of indium in Mineral Creek. Modeling results suggest that the removal of indium from the filterable phase is consistent with precipitation of indium hydroxide from a dissolved phase. This work demonstrates that nonferrous mining processes can be a significant source of indium to the environment, and provides critical information about the aqueous behavior of indium.

  9. Synthetic Precipitation Leaching Procedure (SPLP) leachate chemistry data for solid mine-waste composite samples from southwestern New Mexico, and Leadville, Colorado

    USGS Publications Warehouse

    Hageman, Philip L.; Briggs, Paul H.; Desborough, George A.; Lamothe, Paul J.; Theodorakos, Peter M.

    2000-01-01

    This report details chemistry data derived from leaching of mine-waste composite samples using a modification of E.P.A. Method 1312, Synthetic Precipitation Leaching Procedure (SPLP). In 1998, members of the U.S. Geological Survey Mine Waste Characterization Project collected four mine-waste composite samples from mining districts in southwestern New Mexico (CAR and PET) and near Leadville, Colorado (TUC and MII). Resulting leachate pH values for the four composites ranged from 5.45 to 8.84 and ranked in the following order: CAR < TUC < MII < PET. Specific conductivity values ranged from 85 uS/cm to 847 uS/cm in the following order: PET < MII < CAR < TUC. Geochemical data generated from this investigation reveal that leachate from the CAR composite contains the highest concentrations of Pb, Zn, Ni, Mn, Cu, Cd, and Al

  10. Chemical trends in background air quality and the ionic composition of precipitation for the period 1980-2004 from samples collected at Valentia Observatory, Co. Kerry, Ireland.

    PubMed

    Bashir, Wasim; McGovern, Frank; O'Brien, Phillip; Ryan, Margaret; Burke, Liam; Paull, Brett

    2008-06-01

    A major Irish study, based upon more than 8000 samples collected over the measurement period of 22 years, for sulfur dioxide (SO2-S), sulfate (SO4-S) and nitrogen dioxide (NO2-N) concentrations (microg m(-3)) within air, and the ionic composition of precipitation samples based on sodium (Na+), potassium (K+), magnesium (Mg2+), calcium (Ca2+), chloride (Cl-), sulfate (SO4-S), non-sea salt sulfate (nssSO4-S), ammonium (NH4-N), and nitrate (NO3-N) weighted mean concentrations (mg l(-1)), has been completed. For the air samples, the sulfur dioxide and sulfate concentrations decreased over the sampling period (1980-2004) by 75% and 45%, respectively, whereas no significant trend was observed for nitrogen dioxide. The highest concentrations for sulfur dioxide, sulfate and nitrogen dioxide were associated with wind originating from the easterly and northeasterly directions i.e. those influenced by Irish and European sources. The lowest concentrations were associated with the westerly directions i.e. for air masses originating in the North Atlantic region. This was further verified with the use of backward (back) trajectory analysis, which allowed tracing the movement of air parcels using the European Centre for Medium range Weather Forecasting (ECMWF) ERA-40 re-analysis data. High non-sea salt sulfate levels were being associated with air masses originating from Europe (easterlies) with lower levels from the Atlantic (westerlies). With the precipitation data, analysis of the non-sea salt sulfate concentrations showed a decrease by 47% since the measurements commenced.

  11. Preparation and adsorption properties of molecularly imprinted polymer via RAFT precipitation polymerization for selective removal of aristolochic acid I.

    PubMed

    Xiao, Yonghua; Xiao, Rong; Tang, Jian; Zhu, Qiankun; Li, Xiaoming; Xiong, Yan; Wu, Xuewen

    2017-01-01

    The molecularly imprinted polymers (MIP) were prepared via aqueous RAFT precipitation polymerization, with aristolochic acid I (AAI) as the template molecule, AA as the functional monomer, EGDMA as the cross-linker, AIBN as the chain initiator, CTP as the chain transfer agent and 80% (g/g) DMF-aqueous solution as the porogen. The differential UV-vis spectra revealed that a cooperative hydrogen-bonding complex between AAI and AA might be formed at the molar ratio of 1:3 in prepolymerized system. The synthesized MIPs were characterized by FTIR spectra, solid UV-visible absorption spectra, nitrogen adsorption-desorption isotherms and scanning electron microscope, which proved that the MIPs and NIPs have the similar chemical structures and the adding of AAI could affect the size and morphology of the microspheres. UV-visible absorption spectra and High-performance liquid chromatography (HPLC) was used to investigate the adsorption and recognition properties of the MIPs. The Scatchard isotherm model described that the binding sites independently acted. The Langmuir isotherm model suggested an excellent imprinting effect owing to the presence of a large number of specific binding sites on the MIP. The Freundlich model indicated that the AAI could be readily absorbed by MIP. Selective absorption of the template molecule was demonstrated in presence of its analogous compounds, benzoic acid and nitrobenzene. The recycling experiments implied that the MIP could be reused to further selective recognition and separation to AAI for six times at least. MIP was developed for removal of AAI from the Aristolochia manshuriensis extraction. The results indicated that 25mg of MIP could remove the AAI below the HPLC detection limits (6.47ngmL(-1)) from 5.0mL of the extraction (CAAI=0.0018mgmL(-1)) with the recovery of AAI to 91.50% (n=3, SD=4.24%). Therefore, it is clearly revealed that the MIP can be a useful tool to remove toxic compounds from natural products.

  12. Carbon Isotopic Measurements of Amino Acids in Stardust-Returned Samples

    NASA Technical Reports Server (NTRS)

    Elsila, Jamie

    2009-01-01

    NASA's Stardust spacecraft returned to Earth samples from comet 81P/Wild 2 in January 2006. Preliminary examinations revealed the presence of a suite of organic compounds including several amines and amino acids, but the origin of these compounds could not be identified. Here, we present the carbon isotopic ratios of glycine and e-aminocaproic acid (EACA), the two most abundant amino acids, in Stardust-returned foil samples measured by gas chromatography-combustion-isotope ratio mass spectrometry coupled with quadrupole mass spectrometry (GC-CAMS/IRMS).

  13. Carbon Isotopic Ratios of Amino Acids in Stardust-Returned Samples

    NASA Technical Reports Server (NTRS)

    Elsila, Jamie E.; Glavin, Daniel P.; Dworkin, Jason P.

    2009-01-01

    NASA's Stardust spacecraft returned to Earth samples from comet 81P/Wild 2 in January 2006. Preliminary examinations revealed the presence of a suite of organic compounds including several amines and amino acids, but the origin of these compounds could not be identified. Here. we present the carbon isotopic ratios of glycine and E-aminocaproic acid (EACH), the two most abundant amino acids observed, in Stardust-returned foil samples measured by gas chromatography-combustion-isotope ratio crass spectrometry coupled with quadrupole mass spectrometry (GC-QMS/IRMS).

  14. Bioavailability of zinc to rats from defatted soy flour, acid-precipitated soy concentrate and neutralized soy concentrate as determined by intrinsic and extrinsic labeling techniques

    SciTech Connect

    Ketelsen, S.M.; Stuart, M.A.; Weaver, C.M.; Forbes, R.M.; Erdman, J.W. Jr.

    1984-03-01

    The bioavailability of 65Zn from intrinsically and extrinsically labeled soy flour, acid-precipitated soy concentrate and neutralized soy concentrate was evaluated in rats. Weanling rats were fed marginally zinc-deficient diets, providing 8 ppm zinc from one of these three soy products, for 7 days. The rats then received a radioactively labeled test meal, identical in composition to the previous diet except that the soy product was either intrinsically or extrinsically labeled with 65Zn. After the test meal the rats were again fed diets the same as those consumed prior to the test meal. Whole-body retention of 65Zn at 24 hours and 12 days as well as 65Zn retained in tibias of rats given meals containing neutralized concentrate-based meals was significantly lower than for rats given meals containing the soy flour or acid-precipitated concentrate. In addition, retention of 65Zn from the extrinsically labeled acid-precipitated concentrate-based meal was significantly higher than from the same product intrinsically labeled. These findings confirm the results of previous feeding studies from which it was suggested that neutralization of soy protein concentrates reduces zinc bioavailability to the rat. In addition, the results are taken to suggest that experimental conditions may influence the validity of the extrinsic labeling technique for zinc.

  15. Effects of acidic precipitation on the water quality of streams in the Laurel Hill area, Somerset County, Pennsylvania, 1983-86

    USGS Publications Warehouse

    Barker, J.L.; Witt, E. C.

    1990-01-01

    Five headwater streams in the Laurel Hill area in southwestern Pennsylvania were investigated from September 1983 through February 1986 to determine possible effects of acidic precipitation on water quality. Precipitation in the Laurel Hill area is among the most acidic in the Nation, with a mean volume-weighted pH of 4.06. Sulfate is the dominant acid-forming anion, averaging 3.6 milligrams per liter or about 50 kilograms per hectare in wet deposition alone. Nitrate averages about 2 milligrams per liter or 7 kilograms per hectare in the study area. Stream chemistry in the five streams is quite variable and apparently is influenced to a large degree by the bedrock geology and by small amounts of alkaline material in watershed soils. Three of the five streams with no or little acid-neutralizing capacity presently are devoid of fish because of low pH and elevated aluminum concentrations. Aluminum concentrations increase in the other two streams during rainfall and snowmelt despite comparatively higher base flow and acid-neutralizing capacities. Comparison of the chemistry of streamflow during 14 storm events at South Fork Bens Creek and North Fork Bens Creek reveals similar chemical responses when discharge suddenly increases. Concentrations of dissolved metals and sulfate increased during stormflow and snowmelt runoff, whereas concentrations of base cations, silica, and chloride decreased. Nitrate concentrations were not affected by rainfall runoff by tended to increase with snowmelt runoff.

  16. Synthesis of aqueous suspensions of magnetic nanoparticles with the co-precipitation of iron ions in the presence of aspartic acid

    NASA Astrophysics Data System (ADS)

    Pušnik, Klementina; Goršak, Tanja; Drofenik, Miha; Makovec, Darko

    2016-09-01

    There is increasing demand for the production of large quantities of aqueous suspensions of magnetic iron-oxide nanoparticles. Amino acids are one possible type of inexpensive, nontoxic, and biocompatible molecules that can be used as the surfactants for the preparation of stable suspensions. This preparation can be conducted in a simple, one-step process based on the co-precipitation of Fe3+/Fe2+ ions in the presence of the amino acid. However, the presence of this amino acid changes the mechanism of the magnetic nanoparticles' formation. In this investigation we analyzed the influence of aspartic amino acid (Asp) on the formation of magnetic iron-oxide nanoparticles during the co-precipitation. The process of the nanoparticles' formation was followed using a combination of TEM, x-ray diffractometry, magnetic measurements, in-situ FT-IR spectroscopy, and chemical analysis, and compared with the formation of nanoparticles without the Asp. The Asp forms a coordination complex with the Fe3+ ions, which impedes the formation of the intermediate iron oxyhydroxide phase and suppresses the growth of the final magnetic iron-oxide nanoparticles. Slower reaction kinetics can lead to the formation of nonmagnetic secondary phases. The aspartic-acid-absorbed nanoparticles can be dispersed to form relatively concentrated aqueous suspensions displaying a good colloidal stability at an increased pH.

  17. Tank 12H Acidic Chemical Cleaning Sample Analysis And Material Balance

    SciTech Connect

    Martino, C. J.; Reboul, S. H.; Wiersma, B. J.; Coleman, C. J.

    2013-11-08

    A process of Bulk Oxalic Acid (BOA) chemical cleaning was performed for Tank 12H during June and July of 2013 to remove all or a portion of the approximately 4400 gallon sludge heel. Three strikes of oxalic acid (nominally 4 wt% or 2 wt%) were used at 55°C and tank volumes of 96- to 140-thousand gallons. This report details the sample analysis of a scrape sample taken prior to BOA cleaning and dip samples taken during BOA cleaning. It also documents a rudimentary material balance for the Tank 12H cleaning results.

  18. Simple protein precipitation extraction technique followed by validated chromatographic method for linezolid analysis in real human plasma samples to study its pharmacokinetics.

    PubMed

    Mohammed, Samah A; Eissa, Maya S; Ahmed, Hytham M

    2017-02-01

    Fast and sensitive HPLC method was developed, optimized and validated for quantification of linezolid (LNZ) in human plasma using guaifenesin as an internal standard (IS). Analyte and IS were extracted from plasma by simple protein precipitation extraction technique using methanol as the precipitating solvent. The pretreated samples were injected in a mobile phase formed of acetonitrile:water:methanol (20:70:10v/v/v) in an isocratic mode at a flow rate of 1.5mL/min with UV detection at 251nm. Separation was done using Aglient ODS C18. The method showed linearity in the range of 0.75-50μg/mL with correlation coefficients equals to 0.9991. Precision and accuracy were in conformity with the criteria normally accepted in bio-analytical method validation. The RSDs for intra- and inter-day assays were <3.56 and 4.63%, respectively. The intra- and inter-day accuracies were 94.67-98.28% and 91.25-96.18%, respectively. The mean absolute recoveries ranged from 92.56±1.78 to 95.24±2.84. According to stability results, LNZ was stable in human plasma during the storage and analysis. LNZ a pharmacokinetic behavior was studied by applying the proposed analytical method.

  19. Filtration of a Hanford Site Tank 241-AN-102 Waste Sample with Alternate Sr/TRU Precipitation Conditions at Bench and Pilot Scales

    SciTech Connect

    ZAMECNIK, JR

    2004-05-27

    In support of the design of the Hanford Waste Treatment Plant, the Savannah River Technology Center has conducted crossflow ultrafiltration tests on the bench scale with both a radioactive sample and simulants and at pilot scale with simulants. The waste tested was from Tank 241-AN-102, which underwent isotopic dilution with strontium nitrate to reduce the soluble (superscript 90)Sr concentration, and sodium permanganate precipitation to remove selected transuranic species. Experimental work validated the use of a simulant by comparison of bench scale simulant filtration data with radioactive filtration test data. Tests on a pilot scale were also conducted and showed that the filtration flux in the pilot unit was consistently lower than in the bench scale unit. An alternative precipitation method resulted in less filterable slurries. Several possible explanations for the differences in flux were proposed, including differences in particle size distribution and slurry viscosity (th e term viscosity will be used, although consistency is more correct for non-Newtonian fluids). The experimental data was also fit to an empirical model and several filtration models. The trends in the data generally followed the predictions of the filtration models. Differences in flux between the bench and pilot scales could not be accounted for by the calculated difference in the average wall shear stress.

  20. Caprylic acid-induced impurity precipitation from protein A capture column elution pool to enable a two-chromatography-step process for monoclonal antibody purification.

    PubMed

    Zheng, Ji; Wang, Lu; Twarowska, Barbara; Laino, Sarah; Sparks, Colleen; Smith, Timothy; Russell, Reb; Wang, Michelle

    2015-01-01

    This article presents the use of caprylic acid (CA) to precipitate impurities from the protein A capture column elution pool for the purification of monoclonal antibodies (mAbs) with the objective of developing a two chromatography step antibody purification process. A CA-induced impurity precipitation in the protein A column elution pool was evaluated as an alternative method to polishing chromatography techniques for use in the purification of mAbs. Parameters including pH, CA concentrations, mixing time, mAb concentrations, buffer systems, and incubation temperatures were evaluated on their impacts on the impurity removal, high-molecular weight (HMW) formation and precipitation step yield. Both pH and CA concentration, but not mAb concentrations and buffer systems, are key parameters that can affect host-cell proteins (HCPs) clearance, HMW species, and yield. CA precipitation removes HCPs and some HMW species to the acceptable levels under the optimal conditions. The CA precipitation process is robust at 15-25°C. For all five mAbs tested in this study, the optimal CA concentration range is 0.5-1.0%, while the pH range is from 5.0 to 6.0. A purification process using two chromatography steps (protein A capture column and ion exchange polishing column) in combination with CA-based impurity precipitation step can be used as a robust downstream process for mAb molecules with a broad range of isoelectric points. Residual CA can be effectively removed by the subsequent polishing cation exchange chromatography.

  1. Amino acid analysis in micrograms of meteorite sample by nanoliquid chromatography-high-resolution mass spectrometry.

    PubMed

    Callahan, Michael P; Martin, Mildred G; Burton, Aaron S; Glavin, Daniel P; Dworkin, Jason P

    2014-03-07

    Amino acids and their enantiomers in a 360 microgram sample of Murchison meteorite were unambiguously identified and quantified using chemical derivatization and nanoliquid chromatography coupled to nanoelectrospray ionization high resolution orbitrap mass spectrometry techniques. The distribution and abundance of amino acids were similar to past studies of Murchison meteorite but the samples used here were three orders of magnitude lower. The analytical method was also highly sensitive, and some amino acid reference standards were successfully detected at a level of ∼200 attomoles (on column). These results may open up the possibility for investigating other less studied, sample-limited extraterrestrial samples (e.g., micrometeorites, interplanetary dust particles, and cometary particles) for biologically-relevant organic molecules.

  2. Multiple stable isotope characterization as a forensic tool to distinguish acid scavenger samples

    SciTech Connect

    Moran, James J.; Kreuzer, Helen W.; Carman, April J.; Wahl, Jon H.; Duckworth, Douglas C.

    2012-01-01

    Acid scavengers are frequently used as stabilizer compounds in a variety of applications. When used to stabilize volatile compounds such as nerve agents, the lower volatility and higher stability of acid scavengers make them more persistent in a post-event forensic setting. We are employing compound-specific stable isotope analysis of the carbon, nitrogen, and hydrogen components of three acid scavenging compounds (N,N-diethylaniline, tributylamine, and triethylamine) as a tool for distinguishing between different samples of the stabilizers. Combined analysis of three stable isotopes in these samples improves the technique’s resolving potential, enhancing sample matching capabilities. The compound specific methods developed here can be applied to instances where these compounds are not pure, such as when mixed with an agent or when found as a residue at an event site. Effective sample matching can be crucial for linking compounds at multiple event sites or linking a supply inventory to an event.

  3. Sample to answer: a fully integrated nucleic acid identification system for bacteria monitoring

    NASA Astrophysics Data System (ADS)

    Kim, Jungkyu; Elsnab, John; Johnson, Michael; Gale, Bruce K.

    2010-02-01

    A fully integrated microfluidic system was developed and incorporates an EC-MWCNT (electrochemical multiwalled carbon nanotube) sensor for the detection of bacteria. Sample metering, reagent metering and delivery was implemented with microvalves and pumps embedded inside the microfluidic system. The nucleic acid extraction was performed using microchannels controlled using automated platforms and a disposable microfluidic silica cartridge. The target samples were flowed and hybridized with probe ssDNA (single strand DNA) across the MWCNT-EC sensor (built on a silicon chip), which was embedded in a microfluidic cell. The 9-pad sensor was scanned before and after hybridization to measure the quantity of RNA (Ribonucleic acid) bound to the array surface. A rapid and accurate sample-in answer-out nucleic acid system was realized with automated volume metering, microfluidic sample preparation, and integrated nano-biosensors.

  4. Applicability Comparison of Methods for Acid Generation Assessment of Rock Samples

    NASA Astrophysics Data System (ADS)

    Oh, Chamteut; Ji, Sangwoo; Yim, Giljae; Cheong, Youngwook

    2014-05-01

    Minerals including various forms of sulfur could generate AMD (Acid Mine Drainage) or ARD (Acid Rock Drainage), which can have serious effects on the ecosystem and even on human when exposed to air and/or water. To minimize the hazards by acid drainage, it is necessary to assess in advance the acid generation possibility of rocks and estimate the amount of acid generation. Because of its relatively simple and effective experiment procedure, the method of combining the results of ABA (Acid Base Accounting) and NAG (Net Acid Generation) tests have been commonly used in determining acid drainage conditions. The simplicity and effectiveness of the above method however, are derived from massive assumptions of simplified chemical reactions and this often leads to results of classifying the samples as UC (Uncertain) which would then require additional experimental or field data to reclassify them properly. This paper therefore, attempts to find the reasons that cause samples to be classified as UC and suggest new series of experiments where samples can be reclassified appropriately. Study precedents on evaluating potential acid generation and neutralization capacity were reviewed and as a result three individual experiments were selected in the light of applicability and compatibility of minimizing unnecessary influence among other experiments. The proposed experiments include sulfur speciation, ABCC (Acid Buffering Characteristic Curve), and Modified NAG which are all improved versions of existing experiments of Total S, ANC (Acid Neutralizing Capacity), and NAG respectively. To assure the applicability of the experiments, 36 samples from 19 sites with diverse geologies, field properties, and weathering conditions were collected. The samples were then subject to existing experiments and as a result, 14 samples which either were classified as UC or could be used as a comparison group had been selected. Afterwards, the selected samples were used to conduct the suggested

  5. Photocatalytic removal of 2,4-dichlorophenoxyacetic acid herbicide on copper oxide/titanium dioxide prepared by co-precipitation method

    NASA Astrophysics Data System (ADS)

    Lee, Shu Chin; Hasan, Norhasnita; Lintang, Hendrik O.; Shamsuddin, Mustaffa; Yuliati, Leny

    2016-02-01

    In this work, suppression of the charge recombination on the titanium dioxide (TiO2) was reported by the addition of copper oxide (CuO), which led to a higher activity of TiO2 for removal of 2,4-dichlorophenoxyacetic acid (2,4-D) herbicide. A series of CuO/TiO2 with CuO loadings of 0.1-1 wt% was prepared through a co-precipitation method. X-ray diffraction patterns revealed that the presence of CuO could not be detected as the low loading amount of CuO might have good dispersion on the surface of TiO2. Diffuse reflectance UV-visible spectra suggested that low loading amount of CuO did not influence the optical property of TiO2. Fluorescence spectroscopy revealed that TiO2 possessed a dominant emission peak of 407 nm at an excitation wavelength of 218 nm. The increasing loading amount of CuO decreased the emission intensity of TiO2, suggesting the successful reduction of charge recombination. After irradiation under UV light for 1 h, CuO(0.1 wt%)/TiO2 gave the highest percentage removal of the herbicide among the samples. The optimum loading amount of CuOmight improve the charge separation and reduce the electron-hole recombination on TiO2 without blocking the active sites, thus leading to the improved photocatalytic activity. This work showed that CuO/TiO2 is a potential photocatalyst for environmental remediation.

  6. Determination of methylphenidate and ritalinic acid in blood, plasma and oral fluid from adolescents and adults using protein precipitation and liquid chromatography tandem mass spectrometry--a method applied on clinical and forensic investigations.

    PubMed

    Josefsson, Martin; Rydberg, Irene

    2011-07-15

    A validated, accurate and sensitive LC-MS/MS method for determination of racemic methylphenidate and its metabolite ritalinic acid has been developed. The analytes were quantified by tandem mass spectrometry operating in positive electrospray ionization mode with multiple reaction monitoring. Blood, plasma and oral fluid samples of 100μl were prepared by simple precipitation with 200μl of an aqueous solution of zinc sulphate in methanol. Corresponding deuterated internal standards were used for quantification. Calibrations for methylphenidate and ritalinic acid were linear within the selected range of 0.2-30ng/ml and 10-1500ng/ml in blood or plasma and in the range of 1-500ng/ml and 0.25-125ng/ml in oral fluid, respectively. The method was successfully applied for the analysis of samples from patients treated with methylphenidate in the dose range of 36-72mg/day and some representative ante mortem and post mortem samples from clinical and forensic toxicological investigations. A three to fourfold higher concentration of methylphenidate was found in oral fluid compared with blood while for ritalinic acid the concentrations were about 25-fold lower in oral fluid.

  7. Formation of an artifact of diclofenac during acidic extraction of environmental water samples.

    PubMed

    Reddersen, K; Heberer, Th

    2003-09-05

    Solid-phase extraction at an acidic pH is used as a common sample preparation method for analyzing residues of the analgesic drug diclofenac (2-[(2,6-dichlorophenyl)amino] benzeneacetic acid) in environmental water samples. This paper describes the matrix-dependent formation of an artifact of diclofenac during sample preparation resulting in an up to 40% underestimation of diclofenac concentrations especially in matrix-prone samples such as sewage effluents or surface water. The artifact most likely being formed during acidification of the sample was unequivocally identified as 1-(2,6-dichlorophenyl)indolin-2-one by capillary gas chromatography-mass spectrometry. To avoid an underestimation of the analytical results quantification of both diclofenac and its artifact is recommended.

  8. Determination of herbicides paraquat, glyphosate, and aminomethylphosphonic acid in marijuana samples by capillary electrophoresis.

    PubMed

    Lanaro, Rafael; Costa, José L; Cazenave, Silvia O S; Zanolli-Filho, Luiz A; Tavares, Marina F M; Chasin, Alice A M

    2015-01-01

    In this work, two methods were developed to determine herbicides paraquat, glyphosate, and aminomethylphosphonic acid (AMPA) in marijuana samples by capillary electrophoresis. For paraquat analysis, sample was extracted with aqueous acetic acid solution and analyzed by capillary zone electrophoresis with direct UV detection. The running electrolyte was 50 mmol/L phosphate buffer (pH 2.50). For glyphosate and AMPA, indirect UV/VIS detection was used, as these substances do not present chromophoric groups. Samples were extracted with 5 mmol/L hydrochloric acid. The running electrolyte was 10 mmol/L gallic acid, 6 mmol/L TRIS, and 0.1 mmol/L CTAB (pH = 4.7). The methods presented good linearity, precision, accuracy, and recovery. Paraquat was detected in 12 samples (n = 130), ranging from 0.01 to 25.1 mg/g. Three samples were positive for glyphosate (0.15-0.75 mg/g), and one sample presented AMPA as well. Experimental studies are suggested to evaluate the risks of these concentrations to marijuana user.

  9. Modeling Precipitation and Sorption of Al, U and Co-contaminants during Titration of Acidic Sediments in Recirculation Flow-Through Experiments

    SciTech Connect

    Tang, Guoping; Luo, Wensui; Brooks, Scott C; Watson, David B; Gu, Baohua

    2013-01-01

    We conducted batch and recirculating column titration tests with contaminated acidic sediments with controlled CO2 in the headspace, and extended the geochemical model by Gu et al. (2003, GCA) to better understand and quantify the reactions governing trace metal fate in the subsurface. The sediment titration curve showed slow pH increase due to strong buffering by Al precipitation and CO2 uptake. Assuming precipitation of basaluminite at low saturation index (SI=-4), and decreasing cation exchange selectivity coefficient (kNa\\Al=0.3), the predictions are close to the observed pH and Al; and the model explains 1) the observed Ca, Mg, and Mn concentration decrease by cation exchange with sorbed Al, and 2) the decrease of U by surface complexation with Fe hydroxides at low pH, and precipitation as liebigite (Ca2UO2(CO3)3:10H2O) at pH>5.5. Without further adjustment geochemical parameters, the model describes reasonably well previous sediment and column titration tests without CO2 in the headspace, as well as the new large column test. The apparent inhibition of U and Ni decrease in the large column can be explained by formation of aqueous carbonate complexes and/or competition with carbonate for surface sites. These results indicated that ignoring labile solid phase Al would underestimate base requirement in titration of acidic aquifers.

  10. High concentrations of furan fatty acids in organic butter samples from the German market.

    PubMed

    Wendlinger, Christine; Vetter, Walter

    2014-08-27

    Furan fatty acids (F-acids) are valuable antioxidants containing a furan moiety in the central part of the molecule. They occur in the lipids of different foodstuffs and plants, with grass being the main source for their presence in milk fat and butter. Because cows from organic farming receive higher portions of grass-based feed, it was tested whether organic butter samples (n = 26) contain more F-acids than conventional ones (n = 25) in Germany. For this purpose, samples were melted, and the lipid phase was separated and transesterified into methyl esters, which were enriched using silver ion chromatography and analyzed by GC-EI/MS in the selected ion monitoring (SIM) mode. Levels of F-acids in butter were higher in summer than in winter, and in both seasons, organic samples contained significantly higher levels of F-acids than conventional ones (one-way ANOVA: p < 0.001). Furthermore, the daily intake of F-acids via milk fat and other foodstuffs was calculated.

  11. Preparation of porous carboxymethyl chitosan grafted poly (acrylic acid) superabsorbent by solvent precipitation and its application as a hemostatic wound dressing.

    PubMed

    Chen, Yu; Zhang, Yong; Wang, Fengju; Meng, Weiwei; Yang, Xinlin; Li, Peng; Jiang, Jianxin; Tan, Huimin; Zheng, Yongfa

    2016-06-01

    The volume phase transition of a hydrogel initiated by shrinking may result in complex patterns on its surface. Based on this unique property of hydrogel, we have developed a novel solvent precipitation method to prepare a kind of novel superabsorbent polymers with excellent hemostatic properties. A porous carboxymethyl chitosan grafted poly (acrylic acid) (CMCTS-g-PAA) superabsorbent polymer was prepared by precipitating CMCTS-g-PAA hydrogel with ethanol. Its potential application in hemostatic wound dressing was investigated. The results indicate that the modified superabsorbent polymer is non-cytotoxic. It showed a high swelling capacity and better hemostatic performance in the treatments of hemorrhage model of ear artery, arteria cruralis and spleen of the New Zealand white rabbit than the unmodified polymer and other commonly used clinic wound dressings. The hemostatic mechanism of the porous CMCTS-g-PAA polymer was also discussed.

  12. Acidification of soil-water in low base-saturated sand soils of the superior uplands under acid and normal precipitation.

    PubMed

    Harris, A R

    1989-04-01

    Lakes and streams are acidified by direct precipitation and water channeled through nearby soils, but water in low base-saturation soils can produce highly acidic percolate after prolonged contact and subsequent degassing in surface waters. Theories advanced by Reuss (1983), Reuss and Johnson (1985), and Seip and Rustad (1984) suggest that soils with less than 15% base saturation are susceptible to soil-water pH depression of up to 0.4 unit, which is sufficient to cause negative alkalinity in soil solutions. High concentrations of mobile anions (notably sulfate) are responsible for the negative alkalinity and these solutions on CO2 degassing in surface waters can retain acidities equivalent to a pH value of 5.0 or less. This mechanism purports to explain why some lakes acidify when they are surrounded by acid soils and cation leaching is not required.Ambient precipitation set to pH 5.4 and pH 4.2 was applied to columns of low base-saturated, sand, soils, starting in 1985. The columns (15 cm diameter and 150 cm long) were collected from soils with base saturations falling into one of three groups (0-10, 10-20, and 20-40%) from national forests in the Superior Uplands area (includes Boundary Waters Canoe Area, Rainbow Lakes, Sylvania, Moquah Barrens, and other Wilderness and Natural areas). The soils were Haplorthods and Udipsamments mainly from outwash plains.The soil columns were instrumented and reburied around a subterranean structure used to collect leachate water and to maintain natural temperature, air, and light conditions. Three humus treatments were applied to soil column (none, northern hardwood, and jack pine) to measure the effect of natural acidification compared to acidification by acid precipitation. The cores were treated with precipitation buffered to pH 5.4 to simulate natural rain and pH 4.2 to simulate acid rain.Columns were treated in 1985 and 1986 with approximately 200 cm of buffered precipitation each year over the frost-free season. Data is

  13. Sampling and analysis of hexavalent chromium during exposure to chromic acid mist and welding fumes.

    PubMed

    Blomquist, G; Nilsson, C A; Nygren, O

    1983-12-01

    Sampling and analysis of hexavalent chromium during exposure to chromic acid mist and welding fumes. Scand j work environ & health 9 (1983) 489-495. In view of the serious health effects of hexavalent chromium, the problems involved in its sampling and analysis in workroom air have been the subject of much concern. In this paper, the stability problems arising from the reduction of hexavalent to trivalent chromium during sampling, sample storage, and analysis are discussed. Replacement of sulfuric acid by a sodium acetate buffer (pH 4) as a leaching solution prior to analysis with the diphenylcarbazide (DPC) method is suggested and is demonstrated to be necessary in order to avoid reduction. Field samples were taken from two different industrial processes-manual metal arc welding on stainless steel without shield gas and chromium plating. A comparison was made of the DPC method, acidic dissolution with atomic absorption spectrophotometric (AAS) analysis, and the carbonate method. For chromic acid mist, the DPC method and AAS analysis were shown to give the same results. In the analysis of welding fumes, the modified DPC method gave the same results as the laborious and less sensitive carbonate method.

  14. [Chemical characteristics of atmospheric precipitation in Shenzhen].

    PubMed

    Niu, Yu-wen; He, Ling-yan; Hu, Min

    2008-04-01

    The precipitation chemical components are good indicators of the air pollution. With rapid economic developing, air quality has greatly changed in Shenzhen. To investigate Chemical feature of precipitation and atmospheric pollution characteristics in Shenzhen, two-year precipitation samples in Shenzhen were collected and analyzed. Based on the dataset, chemical characteristics of rainwater in Shenzhen were discussed. Results show that the concentration of the sum of anions and rations in Shenzhen rainwater was lower compared to northern cities like Beijing, whereas the acidification of rainwater was very serious in Shenzhen. Volume-weighted mean pH values of rainwater were 4.48 and 4.68 respectively, and 88% and 91% of rain events were acidic in 2004 and 2005, respectively. The contribution of SO4(2-) to Shenzhen rainwater acidity was smaller than that in northern cities and NO3- and Cl- played an important part to acidification of Shenzhen precipitation. The contribution of Cl- and Na+ to rainwater chemical components was higher, indicating the significant marine influence on Shenzhen precipitation. The secondary components like SO4(2-), NO3- and NH4+ contributed significantly to total ions of rainwater and they accounted for more than 40% of total ions in 2004 and 2005, which indicated the severe secondary pollution in Shenzhen. There was the obvious difference in origins for different rainwater components. Cl-, K+ and Na+ were mainly from marine contribution while SO4(2-), NO3-, Ca2+ and Mg2+ were mainly from non-sea salt fraction. Formic acid, acetic acid and oxalic acid were most abundant low-molecular weight organic acids and the sum of their concentrations accounted for 94% and 99% of total organic acids determined in 2004 and 2005, respectively.

  15. Synthesis and evaluation of uniformly sized nalidixic acid-imprinted nanospheres based on precipitation polymerization method for analytical and biomedical applications.

    PubMed

    Abouzarzadeh, Atefeh; Forouzani, Mehdi; Jahanshahi, Mohsen; Bahramifar, Nader

    2012-07-01

    For the first time in this work, uniform molecularly imprinted polymer (MIP) nanoparticles were prepared using nalidixic acid as a template. The MIP nanoparticles were successfully synthesized by precipitation polymerization applying methacrylic acid (MAA) as a functional monomer and trimethylolpropane trimethacrylate (TRIM) as a cross-linking monomer at different mole ratios. The morphology, binding, recognition, selectivity, and in vitro release behaviors of obtained particles were studied. The produced polymers were characterized by Fourier transform infrared spectroscopy and differential scanning calorimetric. Furthermore, their morphology was analyzed accurately by scanning electron microscopy, photon correlation spectroscopy, and Brunauer-Emmett-Teller analysis. The nanospheres and microspheres with mean diameter values of 94 nm, 256 nm, and 1.2 µm were obtained using nalidixic acid-MAA-TRIM various mole ratios. Among the MIPs, the product with nalidixic acid-MAA-TRIM mole ratio of 1:12:12 established nanospheres with the lowest polydispersity index (0.003), an average pore diameter (12 nm), and the highest specific surface area (280 m(2) g(-1)) and selectivity factor (10.4). Results from binding experiments demonstrated that the imprinted nanospheres with a 94-nm mean diameter and a binding capacity of 28 mg of nalidixic acid per gram of polymer had higher specific affinity to nalidixic acid in contrast with the other imprinted nanospheres, microspheres, and nonimprinted particles. However, the binding performance of imprinted nanospheres in human serum was estimated using high-performance liquid chromatography analysis (binding approximately 98% of nalidixic acid). In addition, release experiments proved to be successful in the controlled release of nalidixic acid during a long period. The 20% of loaded nalidixic acid was released from the imprinted nanospheres within the first 20 h, whereas the remaining 80% was released in the after 120 h. The nalidixic

  16. Gas chromatographic/mass spectrometric determination of lysergic acid diethylamide (LSD) in serum samples.

    PubMed

    Musshoff, F; Daldrup, T

    1997-08-04

    A sensitive method for the detection and quantification of lysergic acid diethylamide (LSD) in serum samples is described. After liquid-liquid extraction the trimethylsilyl derivative of LSD is detected by gas chromatography-mass spectrometry. Experiments with spiked samples resulted in a recovery of 76%, the coefficient of variation was 9.3%. Excellent linearity was obtained over the range 0.1-10 ng ml-1. Additionally experiments demonstrating the light sensitivity of LSD are presented together with casuistics.

  17. Stable Isotope Analyses of Phosphate Oxygen From Micro-samples of Biological Apatite: A new Routine Procedure for Silverphosphate Micro-precipitation and the Removal of Organic Contamination

    NASA Astrophysics Data System (ADS)

    Wiedemann-Bidlack, F. B.; Colman, A. S.; Fogel, M. L.

    2003-12-01

    Oxygen isotope analyses in bone and teeth of living and fossil animals are widely used for testing hypotheses about variability of diet and habitat. For the analysis of environmental or dietary changes in the past, tooth enamel has become the preferred study material, because its mineral content is higher than bone and dentine, and the relatively large size of the carbonato-apatite crystals of enamel make it more stable against post mortem diagenetic alteration than dentine or bone. Intra-tooth sampling of dental enamel is increasingly used for the investigation of seasonal climate variability, taking advantage of both the high correlation between an animal's drinking water and the δ 18O in its mineralized tissues and the incremental growth pattern of tooth enamel. The different oxygen-containing ions of bioapatite (phosphate, carbonate, and hydroxyl group) incorporate into the mineral lattice at different rates during enamel mineralization, and differ in their susceptibility against post mortem diagenetic alteration. In addition, it is difficult to account for the different reaction chemistries of phosphate, carbonate, and hydroxyl group using isotope analysis techniques that include all oxygen contained in the enamel (e.g., laser ablation). These problems can be addressed analyzing phosphate oxygen only. However, two major factors limit the potential of δ 18O analyses in dental enamel: A) the starting sample size for isotope analyzes often precludes the use of small teeth or the intra-tooth sampling of a given tooth; B) Small amounts of biogenic organic material in tooth enamel (less than 1% by wt) can reduce the precision and lead to anomalous analytical results in δ 18O measurements on Ag3PO4 produced from tooth enamel. A new procedure was developed for the pre-treatment and δ 18O analysis of phosphate from small samples (500 μ g) of tooth enamel containing organic matter. Ag3PO{4} was precipitated quantitatively for analysis of δ 18Ophosphate using a

  18. Acid digestion of geological and environmental samples using open-vessel focused microwave digestion.

    PubMed

    Taylor, Vivien F; Toms, Andrew; Longerich, Henry P

    2002-01-01

    The application of open vessel focused microwave acid digestion is described for the preparation of geological and environmental samples for analysis using inductively coupled plasma-mass spectrometry (ICP-MS). The method is compared to conventional closed-vessel high pressure methods which are limited in the use of HF to break down silicates. Open-vessel acid digestion more conveniently enables the use of HF to remove Si from geological and plant samples as volatile SiF4, as well as evaporation-to-dryness and sequential acid addition during the procedure. Rock reference materials (G-2 granite, MRG-1 gabbros, SY-2 syenite, JA-1 andesite, and JB-2 and SRM-688 basalts) and plant reference materials (BCR and IAEA lichens, peach leaves, apple leaves, Durham wheat flour, and pine needles) were digested with results comparable to conventional hotplate digestion. The microwave digestion method gave poor results for granitic samples containing refractory minerals, however fusion was the preferred method of preparation for these samples. Sample preparation time was reduced from several days, using conventional hotplate digestion method, to one hour per sample using our microwave method.

  19. Acetic Acid Detection Threshold in Synthetic Wine Samples of a Portable Electronic Nose

    PubMed Central

    Macías, Miguel Macías; Manso, Antonio García; Orellana, Carlos Javier García; Velasco, Horacio Manuel González; Caballero, Ramón Gallardo; Chamizo, Juan Carlos Peguero

    2013-01-01

    Wine quality is related to its intrinsic visual, taste, or aroma characteristics and is reflected in the price paid for that wine. One of the most important wine faults is the excessive concentration of acetic acid which can cause a wine to take on vinegar aromas and reduce its varietal character. Thereby it is very important for the wine industry to have methods, like electronic noses, for real-time monitoring the excessive concentration of acetic acid in wines. However, aroma characterization of alcoholic beverages with sensor array electronic noses is a difficult challenge due to the masking effect of ethanol. In this work, in order to detect the presence of acetic acid in synthetic wine samples (aqueous ethanol solution at 10% v/v) we use a detection unit which consists of a commercial electronic nose and a HSS32 auto sampler, in combination with a neural network classifier (MLP). To find the characteristic vector representative of the sample that we want to classify, first we select the sensors, and the section of the sensors response curves, where the probability of detecting the presence of acetic acid will be higher, and then we apply Principal Component Analysis (PCA) such that each sensor response curve is represented by the coefficients of its first principal components. Results show that the PEN3 electronic nose is able to detect and discriminate wine samples doped with acetic acid in concentrations equal or greater than 2 g/L. PMID:23262483

  20. Acetic acid detection threshold in synthetic wine samples of a portable electronic nose.

    PubMed

    Macías, Miguel Macías; Manso, Antonio García; Orellana, Carlos Javier García; Velasco, Horacio Manuel González; Caballero, Ramón Gallardo; Chamizo, Juan Carlos Peguero

    2012-12-24

    Wine quality is related to its intrinsic visual, taste, or aroma characteristics and is reflected in the price paid for that wine. One of the most important wine faults is the excessive concentration of acetic acid which can cause a wine to take on vinegar aromas and reduce its varietal character. Thereby it is very important for the wine industry to have methods, like electronic noses, for real-time monitoring the excessive concentration of acetic acid in wines. However, aroma characterization of alcoholic beverages with sensor array electronic noses is a difficult challenge due to the masking effect of ethanol. In this work, in order to detect the presence of acetic acid in synthetic wine samples (aqueous ethanol solution at 10% v/v) we use a detection unit which consists of a commercial electronic nose and a HSS32 auto sampler, in combination with a neural network classifier (MLP). To find the characteristic vector representative of the sample that we want to classify, first we select the sensors, and the section of the sensors response curves, where the probability of detecting the presence of acetic acid will be higher, and then we apply Principal Component Analysis (PCA) such that each sensor response curve is represented by the coefficients of its first principal components. Results show that the PEN3 electronic nose is able to detect and discriminate wine samples doped with acetic acid in concentrations equal or greater than 2 g/L.

  1. DEVELOPMENTS IN THE SUPERCRITICAL FLUID EXTRACTION OF CHLOROPHENOXY ACID HERBICIDES FROM SOIL SAMPLES

    EPA Science Inventory

    Extraction of chlorophenoxy acid herbicides from soil samples with supercritical carbon dioxide as extractant and tetrabutylammonium hydroxide and methyl iodide as derivatization agents was investigated. The extraction was carried out at 400 atm and 80 C for 15 min static, follow...

  2. Direct analysis for urinary protein with biuret reagent, with use of urine ultrafiltrate blanking: comparison with a manual biuret method involving trichloroacetic acid precipitation.

    PubMed

    Eckfeldt, J H; Kershaw, M J; Dahl, I I

    1984-03-01

    We describe a method for measuring urinary protein with a centrifugal analyzer. Biuret reagent is used, and blanking with an ultrafiltrate of urine eliminates interferences from the nonprotein, biuret-positive chromogens in urine. We compare results by this new method with those by a manual method in which trichloroacetic acid precipitation and biuret reagent are used. The new method shows good precision and excellent correlation (r = 0.997) with the manual method. The ease and convenience of this assay should make this a useful method for the routine clinical laboratory.

  3. The effect of using citric or acetic acid on survival of Listeria monocytogenes during fish protein recovery by isoelectric solubilization and precipitation process.

    PubMed

    Otto, R A; Beamer, S; Jaczynski, J; Matak, K E

    2011-10-01

    Isoelectric solubilization and precipitation (ISP) is a protein recovery process effective at reducing Listeria innocua, a nonpathogenic bacterium typically used as a surrogate for L. monocytogenes in recovered trout protein. The response of L. monocytogenes to ISP processing was determined and compared to the response of L. innocua. Headed and gutted rainbow trout were inoculated with L. monocytogenes (10.16 log CFU/g), homogenized, and pH-adjusted with granular citric acid (pH 2.0 and 2.5) or glacial acetic acid (pH 3.0 and 3.5). Proteins were solubilized and centrifugation was used to remove insoluble components (skin, insoluble protein, so on). The supernatant was returned to the protein isoelectric point (pH 5.5) with NaOH and centrifuged to remove precipitated protein. Microbial load was enumerated on both growth and selective media; recovery was not significantly different (P > 0.05). Surviving cells from each component (protein, insoluble, and water) were compared to initial inoculum numbers. Significant reductions were detected at all pH (P < 0.05). The greatest reductions were at pH 3.0 with acetic acid, with a mean log reduction of 3.03 in the combined components, and a 3.53 log reduction in the protein portion. Data were compared to results from a previous study using L. innocua. Significant differences (P < 0.05) in recovery were found between the 2 species at pH 2.0 and 3.0 with greater recovery of L. monocytogenes, regardless of processing pH or acid type. These results demonstrate the variability in resistance between species and indicate that L. innocua is not an appropriate surrogate for L. monocytogenes for ISP processing with organic acids.

  4. Analysis of large soil samples for actinides

    DOEpatents

    Maxwell, III; Sherrod L.

    2009-03-24

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

  5. Compound-Specific Isotope Analysis of Amino Acids for Stardust-Returned Samples

    NASA Technical Reports Server (NTRS)

    Cook, Jamie; Elsila, Jamie E.; Stern J. C.; Glavin, D. P.; Dworkin, J. P.

    2008-01-01

    Significant portions of the early Earth's prebiotic organic inventory , including amino acids, could have been delivered to the Earth's sur face by comets and their fragments. Analysis of comets via spectrosc opic observations has identified many organic molecules, including me thane, ethane, arnmonia, cyanic acid, formaldehyde, formamide, acetal ehyde, acetonitrile, and methanol. Reactions between these identifie d molecules could allow the formation of more complex organics such a s amino acids. Isotopic analysis could reveal whether an extraterrest rial signature is present in the Stardust-exposed amines and amino ac ids. Although bulk isotopic analysis would be dominated by the EACA contaminant's terrestrial signature, compoundspecific isotope analysi s (CSIA) could determine the signature of each of the other individua l amines. Here, we report on progress made towards CSIA of the amino acids glycine and EACA in Stardustreturned samples.

  6. Flavonoids and Phenolic Acids in Methanolic Extracts, Infusions and Tinctures from Commercial Samples of Lemon Balm.

    PubMed

    Arceusz, Agnieszka; Wesolowski, Marek; Ulewicz-Magulska, Beata

    2015-06-01

    The aim of this study was to quantify the levels of flavonoids (rutin, myricetin, quercetin, kaempferol) and phenolic acids (gallic, p-coumaric, rosmarinic, syringic, caffeic, chlorogenic, ellagic, ferulic) in lemon balm (Melissa officinalis L.) commonly used as a culinary, aromatic and medicinal herb. A rapid and reliable HPLC procedure was developed to determine the phenolic compounds in methanolic extracts, infusions and tinctures prepared from lemon balm. Except for myricetin and quercetin, as well as ellagic, gallic and rosmarinic acids, higher levels of the analytes under study were determined in the methanolic extracts (up to 22 mg/g of dry weight, DW), than in infusions (up to 5 mg/g DW). Tinctures were the poorest in flavonoids and phenolic acids (below 550 μg/g DW), except for ellagic and rosmarinic acids, which were quantified in tinctures at higher levels (mg/g DW). To sum up, the flavonoids were extracted more effectively in the infusions and tinctures than the phenolic acids. Statistically significant correlations were found between phenolic acids, possibly owing to similar biochemical pathways of the compounds. The hierarchical cluster and principal component analyses have also shown that the samples of lemon balm could be differentiated based on the levels of flavonoids and phenolic acids.

  7. Accurate analysis of taurine, anserine, carnosine and free amino acids in a cattle muscle biopsy sample.

    PubMed

    Imanari, Mai; Higuchi, Mikito; Shiba, Nobuya; Watanabe, Akira

    2010-06-01

    We have established an analysis method for some free amino acids (FAAs), as well as taurine (Tau), anserine (Ans) and carnosine (Car), in a fresh biopsy sample from cattle muscle. A series of model biopsy samples, corresponding to the mixtures of lean meat, fat and connective tissue, was prepared and showed high correlation coefficients between the compound concentration and the 3-methylhistidine (3-MeHis) content derived from hydrolysis of the biopsy sample (r = 0.74-0.95, P < 0.01). Interference from blood contamination could not be neglected, because the concentration of some FAAs in blood was comparable to that in muscle. However, it was possible to control the contamination of Tau, Ans, Car, glutamic acid, glutamine, asparatic acid and alanine to less than 5.0% when the blood contamination was controlled to less than 23%.These results suggest the necessity of measuring 3-MeHis as an index of lean meat and hemoglobin as an index of blood contamination when compounds in muscle biopsy samples are evaluated. We have carried out a series of these analyses using one biopsy sample and reveal differences in Tau, Ans, Car and some FAAs in beef muscle after different feeding regimes.

  8. Sample pretreatment and nucleic acid-based detection for fast diagnosis utilizing microfluidic systems.

    PubMed

    Wang, Jung-Hao; Wang, Chih-Hung; Lee, Gwo-Bin

    2012-06-01

    Recently, micro-electro-mechanical-systems (MEMS) technology and micromachining techniques have enabled miniaturization of biomedical devices and systems. Not only do these techniques facilitate the development of miniaturized instrumentation for biomedical analysis, but they also open a new era for integration of microdevices for performing accurate and sensitive diagnostic assays. A so-called "micro-total-analysis-system", which integrates sample pretreatment, transport, reaction, and detection on a small chip in an automatic format, can be realized by combining functional microfluidic components manufactured by specific MEMS technologies. Among the promising applications using microfluidic technologies, nucleic acid-based detection has shown considerable potential recently. For instance, micro-polymerase chain reaction chips for rapid DNA amplification have attracted considerable interest. In addition, microfluidic devices for rapid sample pretreatment prior to nucleic acid-based detection have also achieved significant progress in the recent years. In this review paper, microfluidic systems for sample preparation, nucleic acid amplification and detection for fast diagnosis will be reviewed. These microfluidic devices and systems have several advantages over their large-scale counterparts, including lower sample/reagent consumption, lower power consumption, compact size, faster analysis, and lower per unit cost. The development of these microfluidic devices and systems may provide a revolutionary platform technology for fast sample pretreatment and accurate, sensitive diagnosis.

  9. Extraction, separation, and intramolecular carbon isotope characterization of athabasca oil sands acids in environmental samples.

    PubMed

    Ahad, Jason M E; Pakdel, Hooshang; Savard, Martine M; Simard, Marie-Christine; Smirnoff, Anna

    2012-12-04

    Here we report a novel approach to extract, isolate, and characterize high molecular weight organic acids found in the Athabasca oil sands region using preparative capillary gas chromatography (PCGC) followed by thermal conversion/elemental analysis-isotope ratio mass spectrometry (TC/EA-IRMS). A number of different "naphthenic acids" surrogate standards were analyzed as were samples from the bitumen-rich unprocessed McMurray Formation, oil sands process water, groundwater from monitoring wells, and surface water from the Athabasca River. The intramolecular carbon isotope signature generated by online pyrolysis (δ(13)C(pyr)) showed little variation (±0.6‰) within any given sample across a large range of mass fractions separated by PCGC. Oil sand, tailings ponds, and deep McMurray Formation groundwater were significantly heavier (up to ∼9‰) compared to surface water and shallow groundwater samples, demonstrating the potential use of this technique in source apportionment studies.

  10. Comparative study of the stability of saxitoxin and neosaxitoxin in acidic solutions and lyophilized samples.

    PubMed

    Alfonso, A; Louzao, M C; Vieytes, M R; Botana, L M

    1994-12-01

    Paralytic shellfish poison (PSP) has historically been a problem for the shellfish industry. In order to prevent the marketing of contaminated seafood products, governments have implemented monitoring programs where standards of toxins are necessary. The stability of these standard toxins is very important. In this paper we analysed the stability of saxitoxin (STX) and neosaxitoxin in acidic solution and lyophilized samples. Individual toxins were determined in each sample using a high-performance liquid chromatographic procedure employing post-column oxidation of the toxins to form fluorescent derivatives. Our results demonstrate that STX is very stable in solution samples and could be adopted as a reference standard. This toxin can be kept in dilute acidic solutions for 18 months without loss of potency. However, neosaxitoxin is unstable, possibly due to transformation to other toxins.

  11. URANIUM PRECIPITATION PROCESS

    DOEpatents

    Thunaes, A.; Brown, E.A.; Smith, H.W.; Simard, R.

    1957-12-01

    A method for the recovery of uranium from sulfuric acid solutions is described. In the present process, sulfuric acid is added to the uranium bearing solution to bring the pH to between 1 and 1.8, preferably to about 1.4, and aluminum metal is then used as a reducing agent to convert hexavalent uranium to the tetravalent state. As the reaction proceeds, the pH rises amd a selective precipitation of uranium occurs resulting in a high grade precipitate. This process is an improvement over the process using metallic iron, in that metallic aluminum reacts less readily than metallic iron with sulfuric acid, thus avoiding consumption of the reducing agent and a raising of the pH without accomplishing the desired reduction of the hexavalent uranium in the solution. Another disadvantage to the use of iron is that positive ferric ions will precipitate with negative phosphate and arsenate ions at the pH range employed.

  12. Preserving ground water samples with hydrochloric acid does not result in the formation of chloroform

    USGS Publications Warehouse

    Squillace, Paul J.; Pankow, James F.; Barbash, Jack E.; Price, Curtis V.; Zogorski, John S.

    1999-01-01

    Water samples collected for the determination of volatile organic compounds (VOCs) are often preserved with hydrochloric acid (HCl) to inhibit the biotransformation of the analytes of interest until the chemical analyses can he performed. However, it is theoretically possible that residual free chlorine in the HCl can react with dissolved organic carbon (DOC) to form chloroform via the haloform reaction. Analyses of 1501 ground water samples preserved with HCl from the U.S. Geological Survey's National Water-Quality Assessment Program indicate that chloroform was the most commonly detected VOC among 60 VOCs monitored. The DOC concentrations were not significantly larger in samples with detectable chloroform than in those with no delectable chloroform, nor was there any correlation between the concentrations of chloroform and DOC. Furthermore, chloroform was detected more frequently in shallow ground water in urban areas (28.5% of the wells sampled) than in agricultural areas (1.6% of the wells sampled), which indicates that its detection was more related to urban land-use activities than to sample acidification. These data provide strong evidence that acidification with HCl does not lead to the production of significant amounts of chloroform in ground water samples. To verify these results, an acidification study was designed to measure the concentrations of all trihalomethanes (THMs) that can form as a result of HCl preservation in ground water samples and to determine if ascorbic acid (C6H8O6) could inhibit this reaction if it did occur. This study showed that no THMs were formed as a result of HCl acidification, and that ascorbic acid had no discernible effect on the concentrations of THMs measured.

  13. Characterization on the precipitate sample of cetyltrimethylammonium bromide adsorbed onto nanocube CaCO3 particles from aqueous-ammonia-rich solution

    NASA Astrophysics Data System (ADS)

    Virtudazo, Raymond V. Rivera; Fuji, Masayoshi; Takai, Chika; Shirai, Takashi

    2012-12-01

    Physicochemical analysis on the precipitate samples of the cationic cetyltrimethylammonium bromide (CTAB) adsorbed onto nanocube CaCO3 particles (NcCP) in aqueous ammonia rich (NH4 +) solution was initially examined. The amount of CTAB added to the (<100 nm) NcCP ranging from 0.04 to 88.5 mM was prepared under room temperature aqueous alkaline condition and characterized by thermogravimetry/differential thermogravimetric analysis (TGA/DTA), Raman spectroscopy (RS), scanning electron microscopy, transmission electron microscopy (TEM), gas chromatograph combined with mass spectrometer analysis (GC-MS), and powder X-ray diffraction pattern. RS, GC-MS, and TGA/DTA analyses indicate that only layer of CTAB molecules were present on the surface of the NcCP. Moreover, this thin sheet layer was morphologically observed by the TEM image (particularly at 88 mM concentration of CTAB). In general, adsorption of CTAB molecules onto NcCP under aqueous alkaline medium had no effect on the cubic crystal structure and particle morphology. The present study confirms the adsorption mechanism of cationic surfactant onto NcCP colloids model and contributes to the better understanding of the possible structural arrangement of the sorbed surfactant molecules onto the NcCP-aqueous alkaline interface by simple characterization method. This investigation is expected to create new, low-cost route to produce promising nanopowders and conversion to hollow particles with multi-component porous surface shell wall.

  14. Effects of ascorbic acid on sperm motility, viability, acrosome reaction and DNA integrity in teratozoospermic samples

    PubMed Central

    Fanaei, Hamed; Khayat, Samira; Halvaei, Iman; Ramezani, Vahid; Azizi, Yaser; Kasaeian, Amir; Mardaneh, Jalal; Parvizi, Mohammad Reza; Akrami, Maryam

    2014-01-01

    Background: Oxidative stress in teratozoospermic semen samples caused poor assisted reproductive techniques (ART) outcomes. Among antioxidants, ascorbic acid is a naturally occurring free radical scavenger and as such its presence assists various other mechanisms in decreasing numerous disruptive free radical processes. Objective: The main goal of this study was to evaluate potential protective effects of ascorbic acid supplementation during in vitro culture of teratozoospermic specimens. Materials and Methods: Teratozoospermic semen samples that collected from 15 volunteers were processed, centrifuged and incubated at 37oC until sperm swimmed-up. Supernatant was divided into four groups and incubated at 37oC for one hour under different experimental conditions: Control, 10 µm A23187, 600µm ascorbic acid and 10 µm A23187+600 µm ascorbic acid. After incubation sperm motility, viability, acrosome reaction, DNA damage and malondialdehyde levels were evaluated. Results: Our results indicated that after one hour incubation, ascorbic acid significantly reduced malondialdehyde level in ascorbic acid group (1.4±0.11 nmol/ml) compared to control group (1.58±0.13 nmol/ml) (p<0.001). At the end of incubation, progressive motility and viability in ascorbic acid group (64.5±8.8% and 80.3±6.4%, respectively) were significantly (p<0.05 and p<0.001, respectively) higher than the control group (54.5±6.8% and 70.9±7.3%, respectively). A23187 significantly (p<0.0001) increased acrosome reaction in A23187 group (37.3±5.6%) compared to control group (8.5±3.2%) and this effect of A23187 attenuated by ascorbic acid in ascorbic acid+A23187 group (17.2±4.4%). DNA fragmentation in ascorbic acid group (20±4.1%) was significantly (p<0.001) lower than controls (28.9±4.6%). Conclusion: In vitro ascorbic acid supplementation during teratozoospermic semen processing for ART could protect teratozoospermic specimens against oxidative stress, and it could improve ART outcome. PMID

  15. Simultaneous Determination of Trigonelline, Caffeine, Chlorogenic Acid and Their Related Compounds in Instant Coffee Samples by HPLC Using an Acidic Mobile Phase Containing Octanesulfonate.

    PubMed

    Arai, Kana; Terashima, Hiroyuki; Aizawa, Sen-ichi; Taga, Atsushi; Yamamoto, Atsushi; Tsutsumiuchi, Kaname; Kodama, Shuji

    2015-01-01

    In order to analyze trigonelline, caffeine, chlorogenic acid, and their related compounds simultaneously, an HPLC method using an InertSustain C18 column and a mobile phase containing octanesulfonate as an ion-pairing reagent under an acidic condition was developed. The optimum mobile phase conditions were determined to be 0.1% phosphoric acid, 4 mM octanesulfonate, and 15% methanol at 35°C. Using the proposed method, trigonelline, nicotinic acid, caffeine, theophylline, chlorogenic acid, and caffeic acid in ten instant coffee samples were analyzed. These analytes except for theophylline were detected in all samples. An increase in the caffeine content in instant coffee samples tended to decrease in both trigonelline and chlorogenic acid contents, and the trigonelline content was found to be correlated well with the chlorogenic acid content (R(2) = 0.887).

  16. ADVANCES IN BIOTREATMENT OF ACID MINE DRAINAGE AND BIORECOVERY OF METALS: 1. METAL PRECIPITATION FOR RECOVERY AND RECYCLE

    EPA Science Inventory

    Acid-mine drainage (AMD) is a severe pollution problem attributed to past mining activities. AMD is an acidic, metal-bearing wastewater generated by the oxidation of metal sulfides to sulfates by Thiobacillus bacteria in both active and abandoned mining operations. The wastewater...

  17. Solar-thermal complex sample processing for nucleic acid based diagnostics in limited resource settings

    PubMed Central

    Gumus, Abdurrahman; Ahsan, Syed; Dogan, Belgin; Jiang, Li; Snodgrass, Ryan; Gardner, Andrea; Lu, Zhengda; Simpson, Kenneth; Erickson, David

    2016-01-01

    The use of point-of-care (POC) devices in limited resource settings where access to commonly used infrastructure, such as water and electricity, can be restricted represents simultaneously one of the best application fits for POC systems as well as one of the most challenging places to deploy them. Of the many challenges involved in these systems, the preparation and processing of complex samples like stool, vomit, and biopsies are particularly difficult due to the high number and varied nature of mechanical and chemical interferents present in the sample. Previously we have demonstrated the ability to use solar-thermal energy to perform PCR based nucleic acid amplifications. In this work demonstrate how the technique, using similar infrastructure, can also be used to perform solar-thermal based sample processing system for extracting and isolating Vibrio Cholerae nucleic acids from fecal samples. The use of opto-thermal energy enables the use of sunlight to drive thermal lysing reactions in large volumes without the need for external electrical power. Using the system demonstrate the ability to reach a 95°C threshold in less than 5 minutes and maintain a stable sample temperature of +/− 2°C following the ramp up. The system is demonstrated to provide linear results between 104 and 108 CFU/mL when the released nucleic acids were quantified via traditional means. Additionally, we couple the sample processing unit with our previously demonstrated solar-thermal PCR and tablet based detection system to demonstrate very low power sample-in-answer-out detection. PMID:27231636

  18. Solar-thermal complex sample processing for nucleic acid based diagnostics in limited resource settings.

    PubMed

    Gumus, Abdurrahman; Ahsan, Syed; Dogan, Belgin; Jiang, Li; Snodgrass, Ryan; Gardner, Andrea; Lu, Zhengda; Simpson, Kenneth; Erickson, David

    2016-05-01

    The use of point-of-care (POC) devices in limited resource settings where access to commonly used infrastructure, such as water and electricity, can be restricted represents simultaneously one of the best application fits for POC systems as well as one of the most challenging places to deploy them. Of the many challenges involved in these systems, the preparation and processing of complex samples like stool, vomit, and biopsies are particularly difficult due to the high number and varied nature of mechanical and chemical interferents present in the sample. Previously we have demonstrated the ability to use solar-thermal energy to perform PCR based nucleic acid amplifications. In this work demonstrate how the technique, using similar infrastructure, can also be used to perform solar-thermal based sample processing system for extracting and isolating Vibrio Cholerae nucleic acids from fecal samples. The use of opto-thermal energy enables the use of sunlight to drive thermal lysing reactions in large volumes without the need for external electrical power. Using the system demonstrate the ability to reach a 95°C threshold in less than 5 minutes and maintain a stable sample temperature of +/- 2°C following the ramp up. The system is demonstrated to provide linear results between 10(4) and 10(8) CFU/mL when the released nucleic acids were quantified via traditional means. Additionally, we couple the sample processing unit with our previously demonstrated solar-thermal PCR and tablet based detection system to demonstrate very low power sample-in-answer-out detection.

  19. Realistic sampling of amino acid geometries for a multipolar polarizable force field.

    PubMed

    Hughes, Timothy J; Cardamone, Salvatore; Popelier, Paul L A

    2015-09-15

    The Quantum Chemical Topological Force Field (QCTFF) uses the machine learning method kriging to map atomic multipole moments to the coordinates of all atoms in the molecular system. It is important that kriging operates on relevant and realistic training sets of molecular geometries. Therefore, we sampled single amino acid geometries directly from protein crystal structures stored in the Protein Databank (PDB). This sampling enhances the conformational realism (in terms of dihedral angles) of the training geometries. However, these geometries can be fraught with inaccurate bond lengths and valence angles due to artefacts of the refinement process of the X-ray diffraction patterns, combined with experimentally invisible hydrogen atoms. This is why we developed a hybrid PDB/nonstationary normal modes (NM) sampling approach called PDB/NM. This method is superior over standard NM sampling, which captures only geometries optimized from the stationary points of single amino acids in the gas phase. Indeed, PDB/NM combines the sampling of relevant dihedral angles with chemically correct local geometries. Geometries sampled using PDB/NM were used to build kriging models for alanine and lysine, and their prediction accuracy was compared to models built from geometries sampled from three other sampling approaches. Bond length variation, as opposed to variation in dihedral angles, puts pressure on prediction accuracy, potentially lowering it. Hence, the larger coverage of dihedral angles of the PDB/NM method does not deteriorate the predictive accuracy of kriging models, compared to the NM sampling around local energetic minima used so far in the development of QCTFF.

  20. Realistic sampling of amino acid geometries for a multipolar polarizable force field

    PubMed Central

    Hughes, Timothy J.; Cardamone, Salvatore

    2015-01-01

    The Quantum Chemical Topological Force Field (QCTFF) uses the machine learning method kriging to map atomic multipole moments to the coordinates of all atoms in the molecular system. It is important that kriging operates on relevant and realistic training sets of molecular geometries. Therefore, we sampled single amino acid geometries directly from protein crystal structures stored in the Protein Databank (PDB). This sampling enhances the conformational realism (in terms of dihedral angles) of the training geometries. However, these geometries can be fraught with inaccurate bond lengths and valence angles due to artefacts of the refinement process of the X‐ray diffraction patterns, combined with experimentally invisible hydrogen atoms. This is why we developed a hybrid PDB/nonstationary normal modes (NM) sampling approach called PDB/NM. This method is superior over standard NM sampling, which captures only geometries optimized from the stationary points of single amino acids in the gas phase. Indeed, PDB/NM combines the sampling of relevant dihedral angles with chemically correct local geometries. Geometries sampled using PDB/NM were used to build kriging models for alanine and lysine, and their prediction accuracy was compared to models built from geometries sampled from three other sampling approaches. Bond length variation, as opposed to variation in dihedral angles, puts pressure on prediction accuracy, potentially lowering it. Hence, the larger coverage of dihedral angles of the PDB/NM method does not deteriorate the predictive accuracy of kriging models, compared to the NM sampling around local energetic minima used so far in the development of QCTFF. © 2015 The Authors. Journal of Computational Chemistry Published by Wiley Periodicals, Inc. PMID:26235784

  1. Analysis of chiral amino acids in cerebrospinal fluid samples linked to different stages of Alzheimer disease.

    PubMed

    Samakashvili, Shorena; Ibáñez, Clara; Simó, Carolina; Gil-Bea, Francisco J; Winblad, Bengt; Cedazo-Mínguez, Angel; Cifuentes, Alejandro

    2011-10-01

    Chiral micellar electrokinetic chromatography with laser-induced fluorescence detection (chiral-MEKC-LIF) was used to investigate D- and L-amino acid contents in cerebrospinal fluid (CSF) samples related to different Alzheimer disease (AD) stages. CSF samples were taken from (i) control subjects (S1 pool), (ii) subjects showing a mild cognitive impairment who remained stable (S2 pool), (iii) subjects showing an mild cognitive impairment that progressed to AD (S3 pool) and (iv) subjects diagnosed with AD (S4 pool). The optimized procedure only needed 10 μL of CSF and it included sample cleaning, derivatization with FITC and chiral-MEKC-LIF separation. Eighteen standard amino acids were baseline separated with efficiencies up to 703,000 plates/m, high sensitivity (LODs in the nM range) and good resolution (values ranging from 2.6 to 9.5). Using this method, L-Arg, L-Leu, L-Gln, γ-aminobutyric acid, L-Ser, D-Ser, L-Ala, Gly, L-Lys, L-Glu and L-Asp were detected in all the CSF samples. S3 and S4 samples (i.e. AD subjects) showed significant lower amounts of L-Arg L-Lys, L-Glu and L-Asp compared to the non-AD S1 and S2 samples, showing in the S4 group the lowest amounts of L-Arg L-Lys, L-Glu and L-Asp. Moreover, γ-aminobutyric acid was significantly higher in AD subjects with the highest amount also found for S4. No significant differences were observed for the rest of amino acids including D-Ser. Based on the obtained chiral-MEKC-LIF data, it was possible to correctly classify all the samples into the four groups. These results demonstrate that the use of enantioselective procedures as the one developed in this work can provide some new light on the investigations of AD, including the discovery of new biomarkers related to different stages of AD.

  2. Ascorbic Acid Determination in Commercial Fruit Juice Samples by Cyclic Voltammetry

    PubMed Central

    Pisoschi, Aurelia Magdalena; Danet, Andrei Florin; Kalinowski, Slawomir

    2008-01-01

    A method was developed for assessing ascorbic acid concentration in commercial fruit juice by cyclic voltammetry. The anodic oxidation peak for ascorbic acid occurs at about 490 mV on a Pt disc working electrode (versus SCE). The influence of the potential sweep speed on the peak height was studied. The obtained calibration graph shows a linear dependence between peak height and ascorbic acid concentration in the domain (0.1–10 mmol·L−1). The equation of the calibration graph was y = 6.391x + 0.1903 (where y represents the value of intensity measured for the anodic peak height, expressed as μA and x the analyte concentration, as mmol·L−1, r2 = 0.9995, r.s.d. = 1.14%, n = 10, Cascorbic acid = 2 mmol·L−1). The developed method was applied to ascorbic acid assessment in fruit juice. The ascorbic acid content determined ranged from 0.83 to 1.67 mmol·L−1 for orange juice, from 0.58 to 1.93 mmol·L−1 for lemon juice, and from 0.46 to 1.84 mmol·L−1 for grapefruit juice. Different ascorbic acid concentrations (from standard solutions) were added to the analysed samples, the degree of recovery being comprised between 94.35% and 104%. Ascorbic acid determination results obtained by cyclic voltammetry were compared with those obtained by the volumetric method with dichlorophenol indophenol. The results obtained by the two methods were in good agreement. PMID:19343183

  3. The First Observation of Domoic Acid in Plankton Net Samples from the Sea of Marmara, Turkey.

    PubMed

    Dursun, Fuat; Yurdun, Türkan; Ünlü, Selma

    2016-01-01

    This study reports the first evidence of domoic acid (DA), an algal neurotoxin produced by the genus Pseudo-nitzschia, from plankton net samples collected in the Sea of Marmara in December, 2010 and February, 2011. DA concentrations of plankton net samples were analyzed by high-performance liquid chromatography (HPLC), using the fluorenylmethoxycarbonyl fluorescence derivatization technique (detection limit 0.2 ng DA). The biotoxin concentrations in samples from coastal waters varied between 0.96 and 5.25 µg DA/mL. We also investigated possible correlations between physicochemical parameters and DA concentration. The DA levels appear to be correlated negatively with silica and nitrite concentrations for both sampling periods. These data may be used to evaluate the probability of finding similar conditions in coastal waters of the Sea of Marmara in order to determine the potential risks to local aquaculture and fisheries.

  4. Voltammetric Determination of Ferulic Acid Using Polypyrrole-Multiwalled Carbon Nanotubes Modified Electrode with Sample Application

    PubMed Central

    Abdel-Hamid, Refat; Newair, Emad F.

    2015-01-01

    A polypyrrole-multiwalled carbon nanotubes modified glassy carbon electrode-based sensor was devised for determination of ferulic acid (FA). The fabricated sensor was prepared electrochemically using cyclic voltammetry (CV) and characterized using CV and scanning electron microscope (SEM). The electrode shows an excellent electrochemical catalytic activity towards FA oxidation. Under optimal conditions, the anodic peak current correlates linearly to the FA concentration throughout the range of 3.32 × 10−6 to 2.59 × 10−5 M with a detection limit of 1.17 × 10−6 M (S/N = 3). The prepared sensor is highly selective towards ferulic acid without the interference of ascorbic acid. The sensor applicability was tested for total content determination of FA in a commercial popcorn sample and showed a robust functionality.

  5. Automated sampling system for the analysis of amino acids using microfluidic capillary electrophoresis.

    PubMed

    Xu, Zhang-Run; Lan, Yue; Fan, Xiao-Feng; Li, Qi

    2009-04-30

    An improved automated continuous sample introduction system for microfluidic capillary electrophoresis (CE) is described. A sample plate was designed into gear-shaped and was fixed onto the shaft of a step motor. Twenty slotted reservoirs for containing samples and working electrolytes were fabricated on the "gear tooth" of the plate. A single 7.5-cm long Teflon AF-coated silica capillary serves as separation channel, sampling probe, as well as liquid-core waveguide (LCW) for light transmission. Platinum layer deposited on the capillary tip serves as the electrode. Automated continuous sample introduction was achieved by scanning the capillary tip through the slots of reservoirs. The sample was introduced into capillary and separated immediately in the capillary with only about 2-nL gross sample consumption. The laser-induced fluorescence (LIF) method with LCW technique was used for detecting fluorescein isothiocyanate (FITC)-labeled amino acids. With electric-field strength of 320 V/cm for injection and separation, and 1.0-s sample injection time, a mixture of FITC-labeled arginine and leucine was separated with a throughput of 60/h and a carryover of 2.7%.

  6. Development and application of a method for analyzing trifluoroacetic acid in environmental samples

    SciTech Connect

    Zehavi, D.; Seiber, J.N.; Wujcik, C.

    1995-12-01

    Trifluoroacetic acid (TFA) is a stable end-product from the oxidative degradation of halocarbon refrigerants proposed for replacement of chlorofluorocarbons. The potential accumulation of TFA in the environment is of concern as halocarbons such as HCFC-123 (CCl{sub 2}HCF{sub 3}), HCFC-124 (CClHFCF{sub 3}) and HFC-134a (CF{sub 3}CFH{sub 2}) become more widely used. We developed a method for analyzing TFA in air, atmospheric water, and surface water, based upon (1) methylation of TFA with dimethylsulfate in sulfuric acid and (2) head-space gas chromatographic determination of TFA as its methyl ester using electron capture or mass selective detection. TFA levels at 50 ppt or less may be detected in water subjected to evaporative concentration, and at 1 ng/m{sup 3} or less in air sampled through a glycerine-bicarbonate denuder. Results from analyses of samples from Nevada and California will be presented.

  7. Effects of acid precipitation on forest soils and watershed biogeochemistry in New England. A technical progress report

    SciTech Connect

    Cronan, C.S.

    1984-05-01

    The research described was initiated to address the need for improved understanding of the mechanistic linkages between forest growth and acidic depositing. A long-term whole-system investigation of forest responses to acidic deposition has been initiated. Nutrient depletion and availability in forest soils, plant nutrient status, trace metal cycling and toxicity, plant disease resistance, and overall plant productivity is emphasized. 48 references, 4 figures, 7 tables.

  8. Acid precipitation: Effects on fresh water ecosystems. (Latest citations from the Life Sciences Collection database). Published Search

    SciTech Connect

    Not Available

    1993-05-01

    The bibliography contains citations concerning the effects of acidification on fresh water ecosystems. Algae and diatom distribution, survival and reproduction rates of specific fish species under acid lake conditions, and tolerance to stress caused by acidic conditions in fresh water ecosystems are studied. Effects of water pH on trace metal toxicity to fresh water organisms are briefly considered. Control and reduction of acidification are excluded from this bibliography. (Contains 250 citations and includes a subject term index and title list.)

  9. Comparison of acid leachate and fusion methods to determine plutonium and americium in environmental samples

    SciTech Connect

    Smith, L.L.; Markun, F.; TenKate, T.

    1992-06-01

    The Analytical Chemistry Laboratory at Argonne National Laboratory performs radiochemical analyses for a wide variety of sites within the Department of Energy complex. Since the chemical history of the samples may vary drastically from site to site, the effectiveness of any analytical technique may also vary. This study compares a potassium fluoride-pyrosulfate fusion technique with an acid leachate method. Both normal and high-fired soils and vegetation samples were analyzed for both americium and plutonium. Results show both methods work well, except for plutonium in high-fired soils. Here the fusion method provides higher accuracy.

  10. The use of variable temperature and magic-angle sample spinning in studies of fulvic acids

    USGS Publications Warehouse

    Earl, W.L.; Wershaw, R. L.; Thorn, K.A.

    1987-01-01

    Intensity distortions and poor signal to noise in the cross-polarization magic-angle sample spinning NMR of fulvic acids were investigated and attributed to molecular mobility in these ostensibly "solid" materials. We have shown that inefficiencies in cross polarization can be overcome by lowering the sample temperature to about -60??C. These difficulties can be generalized to many other synthetic and natural products. The use of variable temperature and cross-polarization intensity as a function of contact time can yield valuable qualitative information which can aid in the characterization of many materials. ?? 1987.

  11. In vitro assessment of potential intestinal absorption of some phenolic families and carboxylic acids from commercial instant coffee samples.

    PubMed

    López-Froilán, R; Ramírez-Moreno, E; Podio, N S; Pérez-Rodríguez, M L; Cámara, M; Baroni, M V; Wunderlin, D A; Sánchez-Mata, M C

    2016-06-15

    Coffee is one of the most consumed beverages in the world, being a source of bioactive compounds as well as flavors. Hydroxycinnamic acids, flavonols, and carboxylic acids have been studied in the samples of instant coffee commercialized in Spain. The studies about contents of food components should be complemented with either in vitro or in vivo bioaccessibility studies to know the amount of food components effectively available for functions in the human body. In this sense, a widely used in vitro model has been applied to assess the potential intestinal absorption of phenolic compounds and organic acids. The contents of hydroxycinnamic acids and flavonols were higher in instant regular coffee samples than in the decaffeinated ones. Bioaccessible phenolic compounds in most analyzed samples account for 20-25% of hydroxycinnamic acids and 17-26% of flavonols. This could mean that a great part of them can remain in the gut, acting as potential in situ antioxidants. Quinic, acetic, pyroglutamic, citric and fumaric acids were identified in commercial instant coffee samples. Succinic acid was found in the coffee blend containing chicory. All carboxylic acids showed a very high bioaccessibility. Particularly, acetic acid and quinic acid were found in higher contents in the samples treated with the in vitro simulation of gastrointestinal processes, compared to the original ones, which can be explained by their cleavage from chlorogenic acid during digestion. This is considered as a positive effect, since quinic acid is considered as an antioxidant inducer.

  12. APols-aided protein precipitation: a rapid method for concentrating proteins for proteomic analysis.

    PubMed

    Ning, Zhibin; Hawley, Brett; Seebun, Deeptee; Figeys, Daniel

    2014-10-01

    Amphipols (APols) are a newly designed and milder class of detergent. They have been used primarily in protein structure analysis for membrane protein trapping and stabilization. We have recently demonstrated that APols can be used as an alternative detergent for proteome extraction and digestion, to achieve a "One-stop" single-tube workflow for proteomics. In this workflow, APols are removed by precipitation after protein digestion without depleting the digested peptides. Here, we took further advantage of this precipitation characteristic of APols to concentrate proteins from diluted samples. In contrast with tryptic peptides, a decrease in pH leads to the unbiased co-precipitation of APols with proteins, including globular hydrophilic proteins. We demonstrated that this precipitation is a combined effect of acid precipitation and the APols' protein interactions. Also, we have been able to demonstrate that APols-aided protein precipitation works well on diluted samples, such as secretome sample, and provides a rapid method for protein concentration.

  13. First LC/MS determination of cyanazine amide, cyanazine acid, and cyanazine in groundwater samples

    USGS Publications Warehouse

    Ferrer, Imma; Thurman, E.M.; Barceló, Damià

    2000-01-01

    Cyanazine and two of its major metabolites, cyanazine amide and cyanazine acid, were measured at trace levels in groundwater using liquid chromatography/atmospheric pressure chemical ionization/mass spectrometry (LC/APCI/MS). Solid-phase extraction was carried out by passing 20 mL of groundwater sample through a cartridge containing a polymeric phase (PLRP-s), with recoveries ranging from 99 to 108% (n = 5). Using LC/MS detection in positive ion mode, useful structural information was obtained by increasing the fragmentor voltage, thus permitting the unequivocal identification of these compounds in groundwater samples with low sample volumes. The fragmentation of the amide, carboxylic acid, and cyano group was observed for both metabolites and cyanazine, respectively, leading to a diagnostic ion at m/z 214. Method detection limits were in the range of 0.002−0.005 μg/L for the three compounds. Finally, the newly developed method was evaluated for the analysis of groundwater samples from New York containing the compounds under study and presents evidence that the metabolites, cyanazine acid, and cyanazine amide may leach to groundwater and serve as sources for deisopropylatrazine. The combination of on-line SPE and LC/APCI/MS represents an important advance in environmental analysis of herbicide metabolites in groundwater since it demonstrates that trace amounts of polar metabolites may be determined rapidly. Furthermore, the presence of both cyanazine amide and cyanazine acid indicate that another degradation product, deisopropylatrazine, may be occurring at depth because of the subsequent degradation of cyanazine.

  14. Vanilmandelic acid and homovanillic acid levels in patients with neural crest tumor: 24-hour urine collection versus random sample.

    PubMed

    Gregianin, L J; McGill, A C; Pinheiro, C M; Brunetto, A L

    1997-01-01

    Neuroblastoma is the most common solid tumor in childhood and is the most frequent neural crest tumor (NCT). More than 90% of the patients excrete high levels of vanilmandelic acid (VMA) and homovanillic acid (HVA) in the urine. Original biochemical methods for measuring these two metabolites of catecholamines employed a collection of urine for 24 hours to avoid errors related to circadian cycle variations. More recently, attempts have been made to replace the 24-hour collections by random samples (RSs). This has practical advantages particularly for young children. The objective of this study is to assess whether urinary VMA related to urinary creatinine levels can be determined reliably by the method of Pisano et al. from RSs in patients with NCT. The determination of the consumption of VMA in urine stored for prolonged periods of time was also studied. We found a good correlation between the values of metabolites of catecholamines in RSs compared with 24-hour urine collections. There was consumption of VMA in urine samples after storage. We conclude that determination of VMA in RSs of urine by Pisano's method may identify NCT production of catecholamines and that the consumption of these catecholamines is an important factor to consider in the interpretation of values obtained with stored urine specimens.

  15. Evaluation of sampling methods for measuring exposure to volatile inorganic acids in workplace air. Part 1: sampling hydrochloric acid (HCl) and nitric acid (HNO₃) from a test gas atmosphere.

    PubMed

    Howe, Alan; Musgrove, Darren; Breuer, Dietmar; Gusbeth, Krista; Moritz, Andreas; Demange, Martine; Oury, Véronique; Rousset, Davy; Dorotte, Michel

    2011-08-01

    Historically, workplace exposure to the volatile inorganic acids hydrochloric acid (HCl) and nitric acid (HNO(3)) has been determined mostly by collection on silica gel sorbent tubes and analysis of the corresponding anions by ion chromatography (IC). However, HCl and HNO(3) can be present in workplace air in the form of mist as well as vapor, so it is important to sample the inhalable fraction of airborne particles. As sorbent tubes exhibit a low sampling efficiency for inhalable particles, a more suitable method was required. This is the first of two articles on "Evaluation of Sampling Methods for Measuring Exposure to Volatile Inorganic Acids in Workplace Air" and describes collaborative sampling exercises carried out to evaluate an alternative method for sampling HCl and HNO(3) using sodium carbonate-impregnated filters. The second article describes sampling capacity and breakthrough tests. The method was found to perform well and a quartz fiber filter impregnated with 500 μL of 1 M Na(2)CO(3) (10% (m/v) Na(2)CO(3)) was found to have sufficient sampling capacity for use in workplace air measurement. A pre-filter is required to remove particulate chlorides and nitrates that when present would otherwise result in a positive interference. A GSP sampler fitted with a plastic cone, a closed face cassette, or a plastic IOM sampler were all found to be suitable for mounting the pre-filter and sampling filter(s), but care has to be taken with the IOM sampler to ensure that the sampler is tightly closed to avoid leaks. HCl and HNO(3) can react with co-sampled particulate matter on the pre-filter, e.g., zinc oxide, leading to low results, and stronger acids can react with particulate chlorides and nitrates removed by the pre-filter to liberate HCl and HNO(3), which are subsequently collected on the sampling filter, leading to high results. However, although there is this potential for both positive and negative interferences in the measurement, these are unavoidable

  16. Precipitation Recycling

    NASA Technical Reports Server (NTRS)

    Eltahir, Elfatih A. B.; Bras, Rafael L.

    1996-01-01

    The water cycle regulates and reflects natural variability in climate at the regional and global scales. Large-scale human activities that involve changes in land cover, such as tropical deforestation, are likely to modify climate through changes in the water cycle. In order to understand, and hopefully be able to predict, the extent of these potential global and regional changes, we need first to understand how the water cycle works. In the past, most of the research in hydrology focused on the land branch of the water cycle, with little attention given to the atmospheric branch. The study of precipitation recycling which is defined as the contribution of local evaporation to local precipitation, aims at understanding hydrologic processes in the atmospheric branch of the water cycle. Simply stated, any study on precipitation recycling is about how the atmospheric branch of the water cycle works, namely, what happens to water vapor molecules after they evaporate from the surface, and where will they precipitate?

  17. Demonstration of the efficiency and robustness of an acid leaching process to remove metals from various CCA-treated wood samples.

    PubMed

    Coudert, Lucie; Blais, Jean-François; Mercier, Guy; Cooper, Paul; Janin, Amélie; Gastonguay, Louis

    2014-01-01

    In recent years, an efficient and economically attractive leaching process has been developed to remove metals from copper-based treated wood wastes. This study explored the applicability of this leaching process using chromated copper arsenate (CCA) treated wood samples with different initial metal loading and elapsed time between wood preservation treatment and remediation. The sulfuric acid leaching process resulted in the solubilization of more than 87% of the As, 70% of the Cr, and 76% of the Cu from CCA-chips and in the solubilization of more than 96% of the As, 78% of the Cr and 91% of the Cu from CCA-sawdust. The results showed that the performance of this leaching process might be influenced by the initial metal loading of the treated wood wastes and the elapsed time between preservation treatment and remediation. The effluents generated during the leaching steps were treated by precipitation-coagulation to satisfy the regulations for effluent discharge in municipal sewers. Precipitation using ferric chloride and sodium hydroxide was highly efficient, removing more than 99% of the As, Cr, and Cu. It appears that this leaching process can be successfully applied to remove metals from different CCA-treated wood samples and then from the effluents.

  18. Analysis of carbonic acid in water samples by ion-exclusion chromatography with pure water as eluent.

    PubMed

    Fan, Hui; Ding, Mingyu; Tanaka, Kazuhiko; Hu, Wenzhi

    2005-02-01

    A simple, sensitive and rapid ion-exclusion chromatographic method for the simultaneous separation of carbonic acid and short chain organic acids (formic acid, acetic acid, and propionic acid) has been developed. A weakly acidic cation exchange resin column TSKgel OApak-A was used for the separation; pure water, owing to its lower background conductance, was employed as eluent in order to obtain high detection sensitivity. A good separation of these weak acids was achieved in 16 min. The linear range of the peak area calibration curve for carbonic acid was from 3.0 mg/L to 500 mg/L. The conductivity detection limit calculated at S/N = 3 was 0.084 mg/L for carbonic acid. The method developed in this work was successfully applied to the determination of carbonic acid in several environmental water samples without any pretreatment.

  19. Quantitative validation of different protein precipitation methods in proteome analysis of blood platelets.

    PubMed

    Zellner, Maria; Winkler, Wolfgang; Hayden, Hubert; Diestinger, Michael; Eliasen, Maja; Gesslbauer, Bernd; Miller, Ingrid; Chang, Martina; Kungl, Andreas; Roth, Erich; Oehler, Rudolf

    2005-06-01

    For the preparation of proteins for proteome analysis, precipitation is frequently used to concentrate proteins and to remove interfering compounds. Various methods for protein precipitation are applied, which rely on different chemical principles. This study compares the changes in the protein composition of human blood platelet extracts after precipitation with ethanol (EtOH) or trichloroacetic acid (TCA). Both methods yielded the same amount of proteins from the platelet preparations. However, the EtOH-precipitated samples had to be dialyzed because of the considerable salt content. To characterize single platelet proteins, samples were analyzed by two-dimensional fluorescence differential gel electrophoresis. More than 90% of all the spots were equally present in the EtOH- and TCA-precipitated samples. However, both precipitation methods showed a smaller correlation with nonprecipitated samples (EtOH 74.9%, TCA 79.2%). Several proteins were either reduced or relatively enriched in the precipitated samples. The proteins varied randomly in molecular weight and isoelectric point. This study shows that protein precipitation leads to specific changes in the protein composition of proteomics samples. This depends more on the specific structure of the protein than on the precipitating agent used in the experiment.

  20. Highly sensitive disposable nucleic acid biosensors for direct bioelectronic detection in raw biological samples

    PubMed Central

    Kuralay, Filiz; Campuzano, Susana; Haake, David A.; Wang, Joseph

    2015-01-01

    The development of rapid, low-cost and reliable diagnostic methods is crucial for the identification and treatment of many diseases. Screen-printed gold electrodes (Au/SPEs), coated with a ternary monolayer interface, involving hexanedithiol (HDT), a specific thiolated capture probe (SHCP), and 6-mercapto-1 hexanol (MCH) (SHCP/HDT/MCH) are shown here to offer direct and sensitive detection of nucleic acid hybridization events in untreated raw biological samples (serum, urine and crude bacterial lysate solutions). The composition of the ternary monolayer was modified and tailored to the surface of the Au/SPE. The resulting SHCP/HDT/MCH monolayer has demonstrated to be extremely useful for enhancing the performance of disposable nucleic acid sensors based on screen-printed electrodes. Compared to common SHCP/MCH binary interfaces, the new ternary self-assembled monolayer (SAM) resulted in a 10-fold improvement in the signal (S)-to-noise (N) ratio (S/N) for 1 nM target DNA. The SHCP/HDT/MCH-modified Au/SPEs allowed the direct quantification of the target DNA down to 25 pM (0.25 fmol) and 100 pM (1 fmol) in undiluted/untreated serum and urine samples, respectively, and of 16S rRNA Escherichia coli (E. coli) corresponding to 3000 CFU μL−1 in raw cell lysate samples. The new SAM-coated screen-printed electrodes also displayed favorable non-fouling properties after a 24 h exposure to raw human serum and urine samples, offering great promise as cost-effective nucleic acid sensors for a wide range of decentralized genetic tests. PMID:21807191

  1. Fluorometric Quantification of Polyphosphate in Environmental Plankton Samples: Extraction Protocols, Matrix Effects, and Nucleic Acid Interference

    PubMed Central

    Martin, Patrick

    2013-01-01

    Polyphosphate (polyP) is a ubiquitous biochemical with many cellular functions and comprises an important environmental phosphorus pool. However, methodological challenges have hampered routine quantification of polyP in environmental samples. We tested 15 protocols to extract inorganic polyphosphate from natural marine samples and cultured cyanobacteria for fluorometric quantification with 4′,6-diamidino-2-phenylindole (DAPI) without prior purification. A combination of brief boiling and digestion with proteinase K was superior to all other protocols, including other enzymatic digestions and neutral or alkaline leaches. However, three successive extractions were required to extract all polyP. Standard addition revealed matrix effects that differed between sample types, causing polyP to be over- or underestimated by up to 50% in the samples tested here. Although previous studies judged that the presence of DNA would not complicate fluorometric quantification of polyP with DAPI, we show that RNA can cause significant interference at the wavelengths used to measure polyP. Importantly, treating samples with DNase and RNase before proteinase K digestion reduced fluorescence by up to 57%. We measured particulate polyP along a North Pacific coastal-to-open ocean transect and show that particulate polyP concentrations increased toward the open ocean. While our final method is optimized for marine particulate matter, different environmental sample types may need to be assessed for matrix effects, extraction efficiency, and nucleic acid interference. PMID:23104409

  2. DISSOLUTION OF LANTHANUM FLUORIDE PRECIPITATES

    DOEpatents

    Fries, B.A.

    1959-11-10

    A plutonium separatory ore concentration procedure involving the use of a fluoride type of carrier is presented. An improvement is given in the derivation step in the process for plutonium recovery by carrier precipitation of plutonium values from solution with a lanthanum fluoride carrier precipitate and subsequent derivation from the resulting plutonium bearing carrier precipitate of an aqueous acidic plutonium-containing solution. The carrier precipitate is contacted with a concentrated aqueous solution of potassium carbonate to effect dissolution therein of at least a part of the precipitate, including the plutonium values. Any remaining precipitate is separated from the resulting solution and dissolves in an aqueous solution containing at least 20% by weight of potassium carbonate. The reacting solutions are combined, and an alkali metal hydroxide added to a concentration of at least 2N to precipitate lanthanum hydroxide concomitantly carrying plutonium values.

  3. Acid precipitation and food quality: Inhibition of growth and survival in black ducks and mallards by dietary aluminum, calcium and phosphorus

    USGS Publications Warehouse

    Robbins, C.S.

    1990-01-01

    In areas impacted by acid precipitation, water chemistry of acidic ponds and streams often changes, resulting in increased mobilization of aluminum and decreased concentration of calcium carbonate. Aluminum binds with phosphorus and inhibits its uptake by organisms. Thus, invertebrate food organisms used by waterfowl may have inadequate Ca and P or elevated Al for normal growth and development. Acid rain and its effects may be one of the factors negatively impacting American black ducks (Anas rubripes) in eastern North America. One-day old mallards (A. platyrhynchos) and black ducks were placed on one of three Ca:P regimens: low:low (LL), normal:normal (NN), and low:high (LH) with each regimen divided further into three or four Al levels for 10 weeks. Forty-five % of the black ducks died on nine different diets whereas only 28% of the mallards died on three different diets. Mortality was significantly related to diet in both species. Growth rates for body weight, culmens, wings, and tarsi of both species on control diets exceeded those on many treatment diets but the differences were less apparent for mallards than for black ducks. Differences among treatments were due to both Ca:P and Al levels.

  4. Inhibition of stromelysin-1 by caffeic acid derivatives from a propolis sample from Algeria.

    PubMed

    Segueni, Narimane; Magid, Abdulmagid Alabdul; Decarme, Martine; Rhouati, Salah; Lahouel, Mesbah; Antonicelli, Frank; Lavaud, Catherine; Hornebeck, William

    2011-07-01

    Stromelysin-1 (matrix metalloproteinase-3: MMP-3) occupies a central position in collagenolytic and elastolytic cascades, leading to cutaneous intrinsic and extrinsic aging. We screened extracts of a propolis sample from Algeria with the aim to isolate compounds able to selectively inhibit this enzyme. A butanolic extract (B (3)) of the investigated propolis sample was found to potently inhibit MMP-3 activity (IC (50) = 0.15 ± 0.03 µg/mL), with no or only weak activity on other MMPs. This fraction also inhibited plasmin amidolytic activity (IC (50) = 0.05 µg/mL) and impeded plasmin-mediated proMMP-3 activation. B (3) was fractionated by HPLC, and one compound, characterized by NMR and mass spectroscopy and not previously identified in propolis, i.e., (+)-chicoric acid, displayed potent IN VITRO MMP-3 inhibitory activity (IC (50) = 6.3 × 10 (-7) M). In addition, both caffeic acid and (+)-chicoric acid methyl ester present in fraction B (3) significantly inhibited UVA-mediated MMP-3 upregulation by fibroblasts.

  5. Analysis of underivatized amino acids in geological samples using ion-pairing liquid chromatography and electrospray tandem mass spectrometry.

    PubMed

    Liu, De-Ling; Beegle, Luther W; Kanik, Isik

    2008-04-01

    The capability of detecting biomarkers, such as amino acids, in chemically complex field samples is essential to establishing the knowledge required to search for chemical signatures of life in future planetary explorations. However, due to the complexities of in situ investigations, it is important to establish a new analytical scheme that utilizes a minimal amount of sample preparation. This paper reports the feasibility of a novel and sensitive technique, which has been established to quantitate amino acids in terrestrial crust samples directly without derivatization using volatile ion-pairing liquid chromatography and tandem mass spectrometry equipped with an electrospray ionization source. Adequate separation of 20 underivatized amino acids was achieved on a C(18) capillary column within 26 min with nonafluoropentanoic acid (NFPA) as ion-pairing reagent. Each amino acid was identified from its retention time as well as from its characteristic parent-to-daughter ion transition. Using tandem mass spectrometry as a detection technique allows co-elution of some amino acids, as it is more specific than traditional spectrophotometric methods. In the present study, terrestrial samples collected from 3 different locations were analyzed for their water-extractable free amino acid contents, following the removal of metal and organic interferences via ion exchange procedures. This is the first time that amino acids in geological samples were directly determined quantitatively without complicated derivatization steps. Depending on the amino acid, the detection limits varied from 0.02 to 5.7 pmol with the use of a 1 microl sample injection loop.

  6. Effects of organic and inorganic acids on phosphorus release from municipal sludge.

    PubMed

    Pakdil, N B; Filibeli, A

    2007-01-01

    This paper reports on the effects of inorganic acids (sulphuric acid, hydrochloric acid, nitric acid) and organic acids (citric acid, oxalic acids) for phosphorus recovery from sludge and struvite precipitation results. It was observed that both inorganic acid and organic acids were effective at phosphorus release. The studies on precipitation of released phosphorus from sludge as magnesium ammonium phosphate (struvite) were also done using nitric and oxalic acids. Phosphorus and heavy metals of leachate were analyzed before and after precipitation. It was observed that heavy metal concentrations in the extracted samples decrease after precipitation. Precipitation was accomplished by using extract derived with nitric acid; however, in oxalic acid applications, it was not achieved. When the chemical constituents of the dried material were examined oxygen, sodium and nitrogen were found to be the major elements.

  7. Final Report Nucleic Acid System - PCR, Multiplex Assays and Sample Preparation Project

    SciTech Connect

    Koopman, R.P.; Langlois, R.G.; Nasarabadi, S.; Benett, W.J.; Richards, J.B.; Hadley, D.R.; Miles, R.R.; Brown, S.B.; Stratton, P.L.; Milanovich, F.P.

    2001-04-20

    The objective of this project was to reduce to practice the detection and identification of biological warfare pathogens by the nucleic acid recognition technique of PCR (polymerase chain reaction). This entailed not only building operationally functional instrumentation but also developing the chemical assays for detection of priority pathogens. This project had two principal deliverables: (1) design, construct, test and deliver a 24 chamber, multiplex capable suitcase sized PCR instrument, and (2) develop and reduce to practice a multiplex assay for the detection of PCR product by flow cytometry. In addition, significant resources were allocated to test and evaluation of the Hand-held Advanced Nucleic Acid Analyzer (HANAA). This project helps provide the signature and intelligence gathering community the ability to perform, on-site or remote, rapid analysis of environmental or like samples for the presence of a suite of biological warfare pathogens.

  8. CONCENTRATION OF Pu USING AN IODATE PRECIPITATE

    DOEpatents

    Fries, B.A.

    1960-02-23

    A method is given for separating plutonium from lanthanum in a lanthanum fluoride carrier precipitation process for the recovery of plutonium values from an aqueous solution. The carrier precipitation process includes the steps of forming a lanthanum fluoride precipi- . tate, thereby carrying plutonium out of solution, metathesizing the fluoride precipitate to a hydroxide precipitate, and then dissolving the hydroxide precipitate in nitric acid. In accordance with the invention, the nitric acid solution, which contains plutonium and lanthanum, is made 0.05 to 0.15 molar in potassium iodate. thereby precipitating plutonium as plutonous iodate and the plutonous iodate is separated from the lanthanum- containing supernatant solution.

  9. Precipitation chemistry in central Amazonia

    NASA Technical Reports Server (NTRS)

    Andreae, M. O.; Talbot, R. W.; Berresheim, H.; Beecher, K. M.

    1990-01-01

    Rain samples from three sites in central Amazonia were collected over a period of 6 weeks during the 1987 wet season and analyzed for ionic species and dissolved organic carbon. A continuous record of precipitation chemistry and amount was obtained at two of these sites, which were free from local or regional pollution, for a time period of over 1 month. The volume-weighted mean concentrations of most species were found to be about a factor of 5 lower during the wet season compared with previous results from the dry season. Only sodium, potassium, and chloride showed similar concentrations in both seasons. When the seasonal difference in rainfall amount is taken into consideration, the deposition fluxes are only slightly lower for most species during the wet season than during the dry season, again with the exception of chloride, potassium, and sodium. Sodium and chloride are present in the same ratio as in sea salt; rapid advection of air masses of marine origin to the central Amazon Basin during the wet season may be responsible for the observed higher deposition flux of these species. Statistical analysis suggests that sulfate is, to a large extent, of marine (sea salt and biogenic) origin, but that long-range transport of combustion-derived aerosols also makes a significant contribution to sulfate and nitrate levels in Amazonian rain. Organic acid concentrations in rain were responsible for a large fraction of the observed precipitation acidity; their concentration was strongly influenced by gas/liquid interactions.

  10. Determination of uranium isotopes in environmental samples by anion exchange in sulfuric and hydrochloric acid media.

    PubMed

    Popov, L

    2016-09-01

    Method for determination of uranium isotopes in various environmental samples is presented. The major advantages of the method are the low cost of the analysis, high radiochemical yields and good decontamination factors from the matrix elements, natural and man-made radionuclides. The separation and purification of uranium is attained by adsorption with strong base anion exchange resin in sulfuric and hydrochloric acid media. Uranium is electrodeposited on a stainless steel disk and measured by alpha spectrometry. The analytical method has been applied for the determination of concentrations of uranium isotopes in mineral, spring and tap waters from Bulgaria. The analytical quality was checked by analyzing reference materials.

  11. Acid-Sulfate Alteration at Gusev Crater and Across Mars: High-SiO2 Residues and Ferric Sulfate Precipitates

    NASA Technical Reports Server (NTRS)

    Morris, R. V.; Catalano, J. G.; Klingelhoefer, G.; Schroeder, C.; Gellert, R.; Clark, B. C.; Ming, D. W.; Yen, A. S.; Arvidson, R. E.; Cohen, B. A.; Fleischer, I.; McCoy, T. J.; Mittlefehldt, D. W.; Squyres, S. W.

    2017-01-01

    The Mars Exploration Rover Spirit ended its mission in Gusev crater on sol 2210 after it had become stuck in a deposit of fined-grained and sulfate rich soil with dust covered solar panels unfavorably pointed toward the sun. Final analysis of remaining data from Spirit's Moessbauer spectrometer (Fe redox and mineralogy) for sols 1529 through 2071 is now complete. We focus here on chemical (APXS) and MB data for targets having high-SiO2 or high-SO3 and process link the targets through mixing and geochemical modelling to an acid-sulfate system centered at Home Plate, which is considered to be a hydrovolcanic complex.

  12. Trace elements in atmospheric precipitation at Northern Jordan measured by ICP-MS: acidity and possible sources

    NASA Astrophysics Data System (ADS)

    Al-Momani, I. F.

    Rainwater samples were collected in a rural region in Northern Jordan using 24-h sampling periods from December 1998 to April 2000. All samples were analyzed for major ions (Na +, K +, Ca 2+, H +, Mg 2+, NH 4+, Cl -, NO 3- and SO 42-) and trace metals (Pb, Cd, Zn, Cu, Al, Fe, Mn, Mo, Ni, Sb and V). The majority of the rain samples collected had pH values higher than 5.6. The average pH was 6.4±0.9. High values of pH were attributed to the neutralization by natural alkaline local dusts which contain large fractions of calcite. The annual average SO 42--to-NO 3- ratio is 1.8, which is close to that observed in more polluted regions. Concentrations of measured species were lower than those reported for other rural sites worldwide. Elements of anthropogenic origins (Zn, Pb, As, Sb, Ag and Cd) were highly enriched with respect to crustal composition. Factor analysis permitted the identification of four source groups, namely crustal dust, sea-salt spray, road traffic and combustion and secondary aerosol formation processes.

  13. Comparison of manual and automated nucleic acid extraction from whole-blood samples.

    PubMed

    Riemann, Kathrin; Adamzik, Michael; Frauenrath, Stefan; Egensperger, Rupert; Schmid, Kurt W; Brockmeyer, Norbert H; Siffert, Winfried

    2007-01-01

    Nucleic acid extraction and purification from whole blood is a routine application in many laboratories. Automation of this procedure promises standardized sample treatment, a low error rate, and avoidance of contamination. The performance of the BioRobot M48 (Qiagen) and the manual QIAmp DNA Blood Mini Kit (Qiagen) was compared for the extraction of DNA from whole blood. The concentration and purity of the extracted DNAs were determined by spectrophotometry. Analytical sensitivity was assessed by common PCR and genotyping techniques. The quantity and quality of the generated DNAs were slightly higher using the manual extraction method. The results of downstream applications were comparable to each other. Amplification of high-molecular-weight PCR fragments, genotyping by restriction digest, and pyrosequencing were successful for all samples. No cross-contamination could be detected. While automated DNA extraction requires significantly less hands-on time, it is slightly more expensive than the manual extraction method.

  14. BEDAM Binding Free Energy Predictions for the SAMPL4 Octa-Acid Host Challenge

    PubMed Central

    Gallicchio, Emilio; Chen, Haoyuan; Chen, He; Fitzgerald, Michael; Gao, Yang; He, Peng; Kalyanikar, Malathi; Kao, Chuan; Lu, Beidi; Niu, Yijie; Pethe, Manasi; Zhu, Jie; Levy, Ronald M.

    2015-01-01

    The Binding Energy Distribution Analysis Method (BEDAM) protocol has been employed as part of the SAMPL4 blind challenge to predict the binding free energies of a set of octa-acid host-guest complexes. The resulting predictions were consistently judged as some of the most accurate predictions in this category of the SAMPL4 challenge in terms of quantitative accuracy and statistical correlation relative to the experimental values, which were not known at the time the predictions were made. The work has been conducted as part of a hands-on graduate class laboratory session. Collectively the students, aided by automated setup and analysis tools, performed the bulk of the calculations and the numerical and structural analysis. The success of the experiment confirms the reliability of the BEDAM methodology and it shows that physics-based atomistic binding free energy estimation models, when properly streamlined and automated, can be successfully employed by non-specialists. PMID:25726024

  15. Isomers/enantiomers of perfluorocarboxylic acids: Method development and detection in environmental samples.

    PubMed

    Naile, Jonathan E; Garrison, A Wayne; Avants, Jimmy K; Washington, John W

    2016-02-01

    Perfluoroalkyl substances are globally distributed in both urban and remote settings, and routinely are detected in wildlife, humans, and the environment. One of the most prominent and routinely detected perfluoroalkyl substances is perfluorooctanoic acid (PFOA), which has been shown to be toxic to both humans and animals. PFOA exists as both linear and branched isomers; some of the branched isomers are chiral. A novel GC-NCI-MS method was developed to allow for isomer/enantiomer separation, which was achieved using two columns working in tandem; a 30-m DB-5MS column and a 30-m BGB-172 Analytik column. Samples were derivatized with diazomethane to form methyl esters of the PFOA isomers. In standards, at least eight PFOA isomers were detected, of which at least four were enantiomers of chiral isomers; one chiral isomer (P3) was sufficiently separated to allow for enantiomer-fraction calculations. Soil, sediment and plant samples from contaminated locations in Alabama and Georgia were analyzed. P3 was observed in most of these environmental samples, and was non-racemic in at least one sediment, suggesting the possibility of chirally selective generation from precursors or enantioselective sorption. In addition, the ratio of P3/linear PFOA was inversely related to distance from source, which we suggest might reflect a higher sorption affinity for the P3 over the linear isomer. This method focuses on PFOA, but preliminary results suggest that it should be broadly applicable to other chiral and achiral perfluorocarboxylic acids (PFCAs); e.g., we detected several other homologous PFCA isomers in our PFCA standards and some environmental samples.

  16. Comparison of high-performance liquid chromatography with radioimmunoassay for the determination of domoic acid in biological samples.

    PubMed

    Lawrence, J F; Cleroux, C; Truelove, J F

    1994-02-18

    A reversed-phase liquid chromatographic method employing UV absorption detection at 242 nm was compared to a radioimmunoassay technique for the determination of the marine toxin, domoic acid, in several types of seafood and biological samples. Agreement between the two methods for spiked samples of mussels and rat serum was very good over a range of concentrations of 0.15-7.3 micrograms/g domoic acid. Also, a very good correlation was observed between the two methods for naturally incurred residues of domoic acid in razor clams, anchovies and crab meat over a concentration range of 0.6-43 micrograms/g domoic acid.

  17. Acid precipitation studies in Colorado and Wyoming: interim report of surveys of montane amphibians and water chemistry

    USGS Publications Warehouse

    Corn, Paul Stephen; Stolzenburg, William; Bury, R. Bruce

    1989-01-01

    Acid deposition may be detrimental or stressful to native populations of wildlife. Because many species of amphibians breed in shallow ponds created by spring rains or melting snow, they may be particularly vulnerable to the effects of acidification. From 1986 to 1988, we surveyed 105 locations in the central Rocky Mountains where amphibians had been recorded previously, and we found that two species of amphibians had experiences major losses. We found the northern leopard frog (Rana pipiens) at only 4 of 33 (12%) historically known localities, and the boreal toad (Bufo boreas) was present at 10 of 59 (17%) known localities. Three other species have not suffered region-wide declines. Tiger salamanders (Ambystoma tigrinum) and wood frogs (Rana sylvatica) were present at 45% and 69% of known localities respectively, and were observed at several localities were they had not been recorded previously. Chorus frogs (Pseudacris triseriata) suffered a catastrophic decline in population size in one population monitored since 1961, but regionally, this species was observed in 36 of 56 (64%) known localities and in another 19 localities where there were no previous records. Complete water chemistry was recorded for 41 localities, and pH was measured at 110 sites in total. Acid neutralizing capacity, pH, specific conductivity, and cation concentrations were negatively correlated with elevation. However, in mountain ponds and lakes, pH was rarely less than 6.0 during the amphibian breeding season. We tested the tolerance of embryos of the four species of frogs to low pH. The LC50 pH was 4.8 for chorus frogs, 4.4-4.7 for leopard frogs, 4.4-4.5 for boreal toads, and 4.2-4.3 for wood frogs. Survival of wood frog embryos declined when exposed to aluminum concentrations of 100 µg/L or greater, but boreal toad embryos survived exposure to aluminum concentrations of 400 µg/L. Acid deposition does not appear to be a major factor in the decline of leopard frogs and boreal toads

  18. Determination of ethyl glucuronide and fatty acid ethyl esters in hair samples.

    PubMed

    Oppolzer, David; Barroso, Mário; Passarinha, Luís; Gallardo, Eugenia

    2017-04-01

    Hair testing for alcohol biomarkers is an important tool for monitoring alcohol consumption. We propose two methods for assessing alcohol exposure through combined analysis of ethyl glucuronide (EtG) and fatty acid ethyl esters (FAEEs) species (ethyl myristate, palmitate, stearate and oleate) in hair (30 mg). EtG was analysed by liquid chromatography-tandem mass spectrometry, while FAEEs were analysed by gas chromatography-tandem mass spectrometry using electron impact ionization. Both methods were validated according to internationally accepted guidelines. Linearity was proven between 3 and 500 pg/mg for EtG and 30-5000 pg/mg for FAEEs, and the limits of quantification were 3 pg/mg for EtG and 30 pg/mg for each of the four FAEEs. Precision and accuracy were considered adequate, processed EtG samples were found to be stable for up to 96 h left in the injector and processed FAEEs samples for up to 24 h. Matrix effects were not significant. Both methods were applied to the analysis of 15 authentic samples, using the cut-off values proposed by the Society of Hair Testing for interpretation. The results agreed well with the self-reported alcohol consumption in most cases, and demonstrated the suitability of the methods to be applied in routine analysis of alcohol biomarkers, allowing monitoring consumption using low sample amounts.

  19. A Simple Purification of Indole-3-Acetic Acid and Abscisic Acid for GC-SIM-MS Analysis by Microfiltration of Aqueous Samples through Nylon

    PubMed Central

    Dunlap, James R.; Guinn, Gene

    1989-01-01

    A simple procedure was developed for the partial purification of plant tissue samples to be analyzed simultaneously for indole-3-acetic acid (IAA) and abscisic acid (ABA). The procedure relies on removal of contaminants by filtration through nylon and partitioning into dichloromethane. This procedure successfully purified both IAA and ABA from muskmelon, cotton, and broccoli tissue. Twenty individual samples can be purified and methylated in 8 h for analysis of free IAA and ABA with gas chromatography-selected ion monitoring-mass spectrometry. The use of microfiltration of aqueous samples through nylon offers new opportunities for improving the efficiency of existing sample purification procedures. PMID:16666735

  20. Growth response of four species of Eastern hardwood tree seedlings exposed to ozone, acidic precipitation, and sulfur dioxide. [Prunus serotina, Acer rubrum, Quercus rubra, Liriodendron tulipifera

    SciTech Connect

    Davis, D.D. Skelly, J.M. )

    1992-03-01

    In 1987 a study was conducted in controlled environment chambers to determine the foliar sensitivity of tree seedlings of eight species to ozone and acidic precipitation, and to determine the influence of leaf position on symptom severity. Jensen and Dochinger conducted concurrent similar studies in Continuously Stirred Tank Reactor (CSTR) chambers with ten species of forest trees. Based on the results of these initial studies, four species representing a range in foliar sensitivity to ozone were chosen: black cherry (Prunus serotina Ehrh.), red maple (Acer rubrum L.), northern red oak (Quercus rubra L.) and yellow-poplar (Liriodendron tulipifera L.). These species were also chosen because of their ecological and/or commercial importance in Pennsylvania. Seedlings were exposed in growth chambers simulated acid rain. In addition acute exposures to sulfur dioxide were conducted in a regime based on unpublished monitoring data collected near coal-fired power plants. The objective of this study was to determine if the pollutant treatments influenced the growth and productivity of seedlings of these four species. This information will help researchers and foresters understand the role of air pollution in productivity of eastern forests.

  1. The determination of haloacetic acids in real world samples using IC-ESI-MS-MS.

    PubMed

    Slingsby, Rosanne; Saini, Charanjit; Pohl, Christopher

    2009-08-01

    This paper presents the determination of nine haloacetic acids (HAAs) in high ionic strength, treated effluent waters using an ion chromatography-electrospray ionization-tandem mass spectrometry (IC-ESI-MS-MS) method with internal standards and discussions of each of the method parameters. Data is also provided for these same samples using USEPA Method 552.2. The sample matrices contain up to 170 mg/L chloride and 243 mg/L sulfate. Matrix ions are separated from the analytes using a high capacity anion exchange analytical column and diverted to a waste stream during each analysis to avoid signal suppression and contamination of the detector. No derivatization, offline matrix elimination, or preconcentration is used. Four isotopically-labeled HAAs are used for quantification, and detection limits are in the range of 400-1000 microg/L with R(2) of at least 0.997 over two orders of magnitude for all analytes in matrix. A trichloroacetic acid (TCAA) internal standard with the label on the alpha carbon is found to be more stable than the TCAA-1-(13)C. Amounts found using IC-MS-MS are 65-130% of amounts found using Method 552.2 for all analytes in the real world treated effluent waters. Detection limits for all nine analytes in matrix are in the range of 100-700 ng/L.

  2. Selective local lysis and sampling of live cells for nucleic acid analysis using a microfluidic probe

    PubMed Central

    Kashyap, Aditya; Autebert, Julien; Delamarche, Emmanuel; Kaigala, Govind V.

    2016-01-01

    Heterogeneity is inherent to biology, thus it is imperative to realize methods capable of obtaining spatially-resolved genomic and transcriptomic profiles of heterogeneous biological samples. Here, we present a new method for local lysis of live adherent cells for nucleic acid analyses. This method addresses bottlenecks in current approaches, such as dilution of analytes, one-sample-one-test, and incompatibility to adherent cells. We make use of a scanning probe technology - a microfluidic probe - and implement hierarchical hydrodynamic flow confinement (hHFC) to localize multiple biochemicals on a biological substrate in a non-contact, non-destructive manner. hHFC enables rapid recovery of nucleic acids by coupling cell lysis and lysate collection. We locally lysed ~300 cells with chemical systems adapted for DNA or RNA and obtained lysates of ~70 cells/μL for DNA analysis and ~15 cells/μL for mRNA analysis. The lysates were introduced into PCR-based workflows for genomic and transcriptomic analysis. This strategy further enabled selective local lysis of subpopulations in a co-culture of MCF7 and MDA-MB-231 cells, validated by characteristic E-cadherin gene expression in individually extracted cell types. The developed strategy can be applied to study cell-cell, cell-matrix interactions locally, with implications in understanding growth, progression and drug response of a tumor. PMID:27411740

  3. Precipitation Matters

    ERIC Educational Resources Information Center

    McDuffie, Thomas

    2007-01-01

    Although weather, including its role in the water cycle, is included in most elementary science programs, any further examination of raindrops and snowflakes is rare. Together rain and snow make up most of the precipitation that replenishes Earth's life-sustaining fresh water supply. When viewed individually, raindrops and snowflakes are quite…

  4. Linking autotrophic activity in environmental samples with specific bacterial taxa by detection of 13C-labelled fatty acids.

    PubMed

    Knief, Claudia; Altendorf, Karlheinz; Lipski, André

    2003-11-01

    A method for the detection of physiologically active autotrophic bacteria in complex microbial communities was developed based on labelling with the stable isotope 13C. Labelling of autotrophic nitrifying, sulphur-oxidizing and iron-oxidizing populations was performed in situ by incubation with NaH[13C]O3. Incorporated label into fatty acid methyl esters (FAMEs) was detected and quantified using gas chromatography-mass spectrometry in single ion monitoring mode. Before the analyses of different environmental samples, the protocol was evaluated in pure culture experiments. In different environmental samples a selective labelling of fatty acids demonstrated which microbial taxa were responsible for the respective chemolithoautotrophic activity. The most strongly labelled fatty acids of a sample from a sulphide treating biofilter from an animal rendering plant were cis-7-hexadecenoic acid (16:1 cis7) and 11-methyl hexadecanoic acid (16:0 11methyl), which are as-yet not known for any sulphide-oxidizing autotroph. The fatty acid labelling pattern of an experimental biotrickling filter sample supplied with dimethyl disulphide clearly indicated the presence and activity of sulphide-oxidizing bacteria of the genus Thiobacillus. For a third environmental sample from an acid mining lake sediment, the assignment of autotrophic activity to bacteria of the genus Leptospirillum but not to Acidithiobacillus could be made by this method, as the fatty acid patterns of these bacteria show clear differences.

  5. A high-performance direct transmethylation method for total fatty acids assessment in biological and foodstuff samples.

    PubMed

    Castro-Gómez, Pilar; Fontecha, Javier; Rodríguez-Alcalá, Luis M

    2014-10-01

    Isolation is the main bottleneck in the analysis of fatty acids in biological samples and foods. In the last few decades some methods described direct derivatization procedures bypassing these steps. They involve the utilization of methanolic HCL or BF3 as catalysts, but several evidences from previous works suggest these reagents are unstable, lead to the formation of artifacts and alter the distribution of specific compounds as hydroxy fatty acids or CLA. However, the main issue is that they are excellent esterification reagents but poor in transterification, being not suitable for the analysis of all lipid classes and leading to erroneous composition quantitations. The present research work is a comprehensive comparison of six general methylation protocols using base, acid or base/acid catalysts plus a proposed method in the analysis of total fatty acids in lipid standards mixtures, foodstuff and biological samples. The addition of aprotic solvents to the reaction mixture to avoid alterations was also tested. Results confirmed that procedures solely involving acid catalyst resulted in incomplete derivatizations and alteration of the fatty acid profile, partially corrected by addition of the aprotic solvent. The proposed method combining sodium methoxyde and sulfuric acid showed absence of alteration of the FAME profile and the best values for response factors (short chain fatty acids to PUFA), accuracy in the determination of total cholesterol and derivatization performance, thus showing a high reliability in the determination of the total fatty acid composition in biological samples and foods.

  6. Surfactant-aided precipitation/on-pellet-digestion (SOD) procedure provides robust and rapid sample preparation for reproducible, accurate and sensitive LC/MS quantification of therapeutic protein in plasma and tissues.

    PubMed

    An, Bo; Zhang, Ming; Johnson, Robert W; Qu, Jun

    2015-04-07

    For targeted protein quantification by liquid chromatography mass spectrometry (LC/MS), an optimal approach for efficient, robust and hi-throughput sample preparation is critical, but often remains elusive. Here we describe a straightforward surfactant-aided-precipitation/on-pellet-digestion (SOD) strategy that provides effective sample cleanup and enables high and constant peptide yields in various matrices, allowing reproducible, accurate and sensitive protein quantification. This strategy was developed using quantification of monocolnocal antibody in tissues and plasma as the model system. Surfactant treatment before precipitation substantially increased peptide recovery and reproducibility from plasma/tissue, likely because surfactant permits extensive denaturation/reduction/alkylation of proteins and inactivation of endogenous protease inhibitors, and facilitates removal of matrix components. The subsequent precipitation procedure effectively eliminates the surfactant and nonprotein matrix components, and the thorough denaturation by both surfactant and precipitation enabled very rapid on-pellet-digestion (45 min at 37 °C) with high peptide recovery. The performance of SOD was systematically compared against in-solution-digestion, in-gel-digestion and filter-aided-sample-preparation (FASP) in plasma/tissues, and then examined in a full pharmacokinetic study in rats. SOD achieved the best peptide recovery (∼21.0-700% higher than the other three methods across various matrices), reproducibility (3.75-10.9%) and sensitivity (28-30 ng/g across plasma and tissue matrices), and its performance was independent of matrix types. Finally, in validation and pharmacokinetic studies in rats, SOD outperformed other methods and provided highly accurate and precise quantification in all plasma samples without using stable isotope labeled (SIL)-protein internal standard (I.S.). In summary, the SOD method has proven to be highly robust, efficient and rapid, making it readily

  7. Developmental and anatomical changes in leaves of yellow birch and red kidney bean exposed to simulated acid precipitation

    SciTech Connect

    Paparozzi, E.T.; Tukey, H.B. Jr.

    1983-01-01

    Leaves of Betula alleghaniensis Britt. (yellow birch) and Phaseolus vulgaris L cv. Red Kidney (bean) were examined microscopically during development and after exposure to simulated rain of pH 5.5, 4.3, 3.2, and 2.8. Yellow birch leaves attained maximal leaf area, midvein length, and cuticle thickness at 21 days. Trichomes were either long, unicellular, or multicellular with caplike head and stalk. Epicuticular wax was a bumpy and amorphous layer. The 2nd trifoliolate leaf of red kidney bean attained maximal leaf area, midvein length, and cuticle thickness when the 3rd trifoliolate leaf was expanding. Trichomes present were long, with a unicellular head and a multicellular base; long, unicellular, and terminally hooked; and small and multicellular. Epicuticular wax was present as small irregular flakes. After 2 days of pH 2.8 and 4 days of pH 3.2 simulated acid rain, round yellow and small tan lesions appeared on birch and bean leaves, respectively. Most injury occurred on or between small veins. Most trichome types were uninjured. Lesions formed as a result of collapsed epidermal and highly plasmolyzed palisade cells. The cuticle was still present over injured epidermal cells and epicuticular waxes were unchanged. There was not statistical difference in mean cuticle thickness due to pH of simulated rain. 25 references, 10 figures, 4 tables.

  8. Chemical alteration of limestone and marble samples exposed to acid rain and weathering in the eastern United States, 1984--1988

    SciTech Connect

    Reimann, K.J.

    1991-06-01

    In a long-term program that began in 1984, limestone and marble briquettes have been exposed to both anthropogenic acid deposition and natural weathering of four field sites in the eastern United States. Similar tests began at an Ohio site in 1986. Effects of exposure on the briquettes and other materials at the sites are evaluated periodically by several federal agencies cooperating in the National Acid Precipitation Assessment Program (NAPAP). A primary contribution of Argonne National Laboratory to the NAPAP has been chemical analysis to determine changes in the samples caused by exposure to the environment. Wet chemical analysis was used to detect sulfates, nitrates, fluorides, chlorides, and a series of metal cations in sequential layers of stone removed from the briquettes after field exposure. Results from the first four years of the program indicate that rinsing by rain keeps skyward-facing stone relatively clean of reaction products, especially sulfate, the most abundant product. On groundward-facing samples, sulfate concentrations increased linearly with exposure time, and values were proportional to atmospheric SO{sub 2} concentrations at the site. Sulfate concentrations in groundward samples were much higher in limestone than in marble, because of the greater porosity of the limestone. A steep sulfate gradient was seen in both sample types from the surface to the interior. On skyward surfaces, material losses per rain event due to complete dissolution of accumulated sulfates were approximately equal to concentrations measured in runoff. Preexposed limestone samples had sulfate accumulations deep in their interiors, while fresh, unexposed limestone did not. No substantial changes in cation accumulations wee detected in either limestone or marble.

  9. IDENTIFICATION OF DIMETHYLTHIOARSINIC ACID BY ICP-MS AND IC-ESI-MS/MS IN RICE SAMPLES

    EPA Science Inventory

    Recently, sulfur analogs of well known arsenicals have been identified in biological and dietary matrices. In this presentation, the detection and identification of dimethylthioarsinic acid (DMTA) will be reported in rice samples after an enzymatic extraction. The enzymatic ext...

  10. Co-precipitation of asiatic acid and poly( l-lactide) using rapid expansion of subcritical solutions into liquid solvents

    NASA Astrophysics Data System (ADS)

    Sane, Amporn; Limtrakul, Jumras

    2011-09-01

    Poly( l-lactide) (PLLA) nanoparticles loaded with asiatic acid (AA) were successfully produced by rapid expansion of a subcritical solution into an aqueous receiving solution containing a dispersing agent. A mixture of carbon dioxide (CO2) and ethanol (EtOH) with a weight ratio of 1:1 was used as the solvent for AA and PLLA. Two surfactants, Pluronic F127 and sodium dodecyl sulfate were employed. The former was found to be more effective for stabilizing AA-loaded PLLA nanoparticles, as a rapid expansion into a 0.1 wt% Pluronic F127 solution produced a stable nanosuspension consisting mainly of well-dispersed, individual nanoparticles. The effects of rapid expansion-processing conditions—AA to PLLA weight ratio and pre-expansion temperature (Tpre)—on the size and morphology of composite nanoparticles, and the loading capacity and entrapment efficiency of AA in PLLA nanoparticles, were systematically investigated. It was found that AA-loaded PLLA nanoparticles with a size range of 30-100 nm were consistently fabricated by rapid expansion at Tpre of 70-100 °C and AA to PLLA weight ratios of 1:2 and 1:4, and with a constant pre-expansion pressure of 330 bar. The Tpre and AA to PLLA weight ratio had no significant effects on the size of the nanoparticles. The AA to PLLA weight ratio is a controlling parameter for both the loading capacity and the entrapment efficiency of AA in PLLA nanoparticles. The loading capacity and entrapment efficiency increased from 8-11 to 16-21 wt%, and 38-57 to 50-62 wt%, respectively, when the AA to PLLA weight ratio changed from 1:4 to 1:2. However, increasing the Tpre from 70 to 100 °C decreased both the loading capacity and entrapment efficiency of AA in PLLA nanoparticles by 20-30%.

  11. Effects of acidic deposition on the erosion of carbonate stone - experimental results from the U.S. National Acid Precipitation Assessment Program (NAPAP)

    USGS Publications Warehouse

    Baedecker, P.A.; Reddy, M.M.; Reimann, K.J.; Sciammarella, C.A.

    1992-01-01

    One of the goals of NAPAP-sponsored research on the effects of acidic deposition on carbonate stone has been to quantify the incremental effects of wet and dry deposition of hydrogen ion, sulfur dioxide and nitrogen oxides on stone erosion. Test briquettes and slabs of freshly quarried Indiana limestone and Vermont marble have been exposed to ambient environmental conditions in a long-term exposure program. Physical measurements of the recession of test stones exposed to ambient conditions at an angle of 30?? to horizontal at the five NAPAP materials exposure sites range from ~15 to ~30?? ??m yr-1 for marble, and from ~25 to ~45 ??m yr -1 for limestone, and are approximately double the recession estimates based on the observed calcium content of run-off solutions from test slabs. The difference between the physical and chemical recession measurements is attributed to the loss of mineral grains from the stone surfaces that are not measured in the run-off experiments. The erosion due to grain loss does not appear to be influenced by rainfall acidity, however, preliminary evidence suggests that grain loss may be influenced by dry deposition of sulfur dioxide between rainfall events. Chemical analyses of the run-off solutions and associated rainfall blanks suggest that ~30% of erosion by dissolution can be attributed to the wet deposition of hydrogen ion and the dry deposition of sulfur dioxide and nitric acid between rain events. The remaining ~70% of erosion by dissolution is accounted for by the solubility of carbonate stone in rain that is in equilibrium with atmospheric carbon dioxide ('clean rain'). These results are for marble and limestone slabs exposed at an angle of 30?? from horizontal. The relative contribution of sulfur dioxide to chemical erosion is significantly enhanced for stone slabs having an inclination of 60?? or 85??. The dry deposition of alkaline particulate material has a mitigating effect at the two urban field exposure sites at Washington, DC

  12. Precipitation chemistry and occurrence of acid rain over the oil-producing Niger Delta region of Nigeria.

    PubMed

    Nduka, John K C; Orisakwe, Orish Ebere

    2010-04-01

    This study investigated the nitrate, sulfate, total dissolved solid (TDS), electrical conductivity, total hardness (TH), and bicarbonates of rainwater samples collected from Warri and Port Harcourt between April-June, July-August, and September-October of 2005 and 2006 to depict onset of rainy season, mid-rainy season, and end of rainy season for the two major crude oil-producing cities of the Niger Delta region of Nigeria (although Port Harcourt is also noted for non-oil manufacturing industries). The same was done in Awka, a non-oil producing city in the hinterland of southeastern Nigeria. In each of the cities, rain samples were collected from three points in a triangular equilibrium using a clean plastic basin fastened to a table 2 m above ground level and 115 m away from tall buildings and trees. The parameters were determined after filtering, using their respective standard methods. Averages of 1.50, 1.81, 1.13 and 2.14, 1.50, 1.86 mg/l of nitrate for April-June, July-August, and September-October were recorded for Warri in 2005 and 2006, respectively. While 15.21, 3.23, 22.31 and 20.89, 9.96, and 14.27mg/l were recorded in Port Harcourt. Sulfate levels for Warri and Port Harcourt for the same periods are follows: 1.38, 1.88, 1.06, 1.50, 1.43, 1.50 and 2.64, 1.15, 5.88, 4.73, 1.90, 1.55 mg/l, respectively. Nitrate levels were higher than sulfate. Other parameters include TDS (5.44, 4.79, 3.30 and 7.63, 3.69, 2.56 mg/l for Warri in 2005 and 2006; 12.57, 2.07, 25.214 and 28.87, 6.73, 7.80 mg/l for Port Harcourt for the same periods). Other parameters also varied in that order for the 2 years in same cities. Crude oil exploration and gas flaring in the Niger Delta, and multiplicity of cottage industries in Awka, impacted on the inorganic ion pollution of the rainwater. This may have public health implications in the region.

  13. Minimization of sample requirement for delta18O in benzoic acid.

    PubMed

    Hagopian, William M; Jahren, A Hope

    2010-09-15

    The measurement of the oxygen stable isotope content in organic compounds has applications in many fields, ranging from paleoclimate reconstruction to forensics. Conventional High-Temperature Conversion (HTC) techniques require >20 microg of O for a single delta(18)O measurement. Here we describe a system that converts the CO produced by HTC into CO(2) via reduction within a Ni-furnace. This CO(2) is then concentrated cryogenically, and 'focused' into the isotope ratio mass spectrometry (IRMS) source using a low-flow He carrier gas (6-8 mL/min). We report analyses of benzoic acid (C(7)H(6)O(2)) reference materials that yielded precise delta(18)O measurement down to 1.3 microg of O, suggesting that our system could be used to decrease sample requirement for delta(18)O by more than an order of magnitude.

  14. Update and revisions for Open-File Report 98-624, synthetic precipitation leaching procedure (SPLP) leachate chemistry data for solid mine-waste composite samples from the Silverton and Leadville districts in Colorado

    USGS Publications Warehouse

    Hageman, Philip L.; Desborough, George A.; Lamothe, Paul J.; Theodorakos, Peter M.

    2000-01-01

    This report supersedes, revises, and updates information and data previously released in Open-File Report 98-624 (Montour and others, 1998). Data for this report were derived from leaching of mine-waste composite samples using a modification of E.P. A. Method 1312, Synthetic Precipitation Leaching Procedure (SPLP). In 1997, members of the U.S. Geological Survey Mine Waste Characterization Project collected four mine-waste composite samples from mining districts near Silverton, Colorado (MAY and YUK), and near Leadville, Colorado (VEN and SUN). This report presents analytical results from these sites.

  15. Enhanced Sampling and Overfitting Analyses in Structural Refinement of Nucleic Acids into Electron Microscopy Maps

    PubMed Central

    Vashisth, Harish; Skiniotis, Georgios; Brooks, Charles L.

    2013-01-01

    Flexible-fitting computational algorithms are often useful to interpret low resolution maps of many macromolecular complexes generated by electron microscopy (EM) imaging. One such atomistic simulation technique is molecular dynamics flexible fitting (MDFF), which has been widely applied to generate structural models of large ribonucleoprotein assemblies such as the ribosome. We have previously shown that MDFF simulations of globular proteins are sensitive to the resolution of the target EM map, and the strength of restraints used to preserve the secondary structure elements during fitting (Vashisth et al. Structure 2012, 20, 1453–1462). In this work, we aim to systematically examine the quality of structural models of various nucleic acids obtained via MDFF by varying the map resolution and the strength of structural restraints. We also demonstrate how an enhanced conformational sampling technique for proteins, temperatureaccelerated molecular dynamics (TAMD), can be combined with MDFF for the structural refinement of nucleic acids in EMmaps. Finally, we also demonstrate application of TAMD-assisted MDFF (TAMDFF) on a RNA/protein complex and suggest that TAMDFF is a viable strategy for enhanced conformational fitting in target maps of ribonucleoprotein complexes. PMID:23506287

  16. Absolute binding free energies for octa-acids and guests in SAMPL5

    NASA Astrophysics Data System (ADS)

    Tofoleanu, Florentina; Lee, Juyong; Pickard, Frank C., IV; König, Gerhard; Huang, Jing; Baek, Minkyung; Seok, Chaok; Brooks, Bernard R.

    2017-01-01

    As part of the SAMPL5 blind prediction challenge, we calculate the absolute binding free energies of six guest molecules to an octa-acid (OAH) and to a methylated octa-acid (OAMe). We use the double decoupling method via thermodynamic integration (TI) or Hamiltonian replica exchange in connection with the Bennett acceptance ratio (HREM-BAR). We produce the binding poses either through manual docking or by using GalaxyDock-HG, a docking software developed specifically for this study. The root mean square deviations for our most accurate predictions are 1.4 kcal mol-1 for OAH with TI and 1.9 kcal mol-1 for OAMe with HREM-BAR. Our best results for OAMe were obtained for systems with ionic concentrations corresponding to the ionic strength of the experimental solution. The most problematic system contains a halogenated guest. Our attempt to model the σ-hole of the bromine using a constrained off-site point charge, does not improve results. We use results from molecular dynamics simulations to argue that the distinct binding affinities of this guest to OAH and OAMe are due to a difference in the flexibility of the host. We believe that the results of this extensive analysis of host-guest complexes will help improve the protocol used in predicting binding affinities for larger systems, such as protein-substrate compounds.

  17. The Global Precipitation Mission

    NASA Technical Reports Server (NTRS)

    Braun, Scott; Kummerow, Christian

    2000-01-01

    The Global Precipitation Mission (GPM), expected to begin around 2006, is a follow-up to the Tropical Rainfall Measuring Mission (TRMM). Unlike TRMM, which primarily samples the tropics, GPM will sample both the tropics and mid-latitudes. The primary, or core, satellite will be a single, enhanced TRMM satellite that can quantify the 3-D spatial distributions of precipitation and its associated latent heat release. The core satellite will be complemented by a constellation of very small and inexpensive drones with passive microwave instruments that will sample the rainfall with sufficient frequency to be not only of climate interest, but also have local, short-term impacts by providing global rainfall coverage at approx. 3 h intervals. The data is expected to have substantial impact upon quantitative precipitation estimation/forecasting and data assimilation into global and mesoscale numerical models. Based upon previous studies of rainfall data assimilation, GPM is expected to lead to significant improvements in forecasts of extratropical and tropical cyclones. For example, GPM rainfall data can provide improved initialization of frontal systems over the Pacific and Atlantic Oceans. The purpose of this talk is to provide information about GPM to the USWRP (U.S. Weather Research Program) community and to discuss impacts on quantitative precipitation estimation/forecasting and data assimilation.

  18. Denuder/filter sampling of organic acids and organosulfates at urban and boreal forest sites: Gas/particle distribution and possible sampling artifacts

    NASA Astrophysics Data System (ADS)

    Kristensen, Kasper; Bilde, Merete; Aalto, Pasi P.; Petäjä, Tuukka; Glasius, Marianne

    2016-04-01

    Carboxylic acids and organosulfates comprise an important fraction of atmospheric secondary organic aerosols formed from both anthropogenic and biogenic precursors. The partitioning of these compounds between the gas and particle phase is still unclear and further research is warranted to better understand the abundance and effect of organic acids and organosulfates on the formation and properties of atmospheric aerosols. This work compares atmospheric aerosols collected at an urban and a boreal forest site using two side-by-side sampling systems; a high volume sampler (HVS) and a low volume (LVS) denuder/filter sampling system allowing for separate collection of gas- and particle-phase organics. All particle filters and denuder samples were collected at H.C. Andersen Boulevard (HCAB), Copenhagen, Denmark in the summer of 2010, and at the remote boreal forest site at Hyytiälä forestry field station in Finland in the summer of 2012. The chemical composition of gas- and particle-phase secondary organic aerosol was investigated by ultra-high performance liquid chromatography/electrospray ionization quadrupole time-of-flight mass spectrometry (UPLC/ESI-Q-TOFMS), with a focus on carboxylic acids and organosulfates. Results show gas-phase concentrations higher than those observed in the particle phase by a factor of 5-6 in HCAB 2010 and 50-80 in Hyytiälä 2012. Although abundant in the particle phase, no organosulfates were detected in the gas phase at either site. Through a comparison of samples collected by the HVS and the LVS denuder/filter sampling system we evaluate the potential artifacts associated with sampling of atmospheric aerosols. Such comparison shows that particle phase concentrations of semi-volatile organic acids obtained from the filters collected by HVS are more than two times higher than concentrations obtained from filters collected using LVS denuder/filter system. In most cases, higher concentrations of organosulfates are observed in particles

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

    PubMed

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

    2016-01-01

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

  20. New amperometric biosensors based on diamond paste for the assay of L- and D-pipecolic acids in serum samples.

    PubMed

    Stefan, Raluca-Ioana; Nejem, R'afat Mahmoud; van Staden, Jacobus F; Aboul-Enein, Hassan Y

    2004-05-01

    Monocrystalline natural diamond, L-amino acid oxidase (L-AAOD), D-amino acid oxidase (D-AAOD), and paraffin oil were used for the design of the modified diamond paste. The technique used for the direct voltammetric assay was differential pulse voltammetry (DPV) with applied potential pulse amplitude of 25 mV vs. Ag/AgCl. Using the new amperometric biosensors L-pipecolic acid (L-PA) and D-pipecolic acid (D-PA) were determined reliably from serum samples at 700 and 200 mV vs. Ag/AgCl, respectively, with low limits of detection.

  1. Simple and rapid determination of ferulic acid levels in food and cosmetic samples using paper-based platforms.

    PubMed

    Tee-ngam, Prinjaporn; Nunant, Namthip; Rattanarat, Poomrat; Siangproh, Weena; Chailapakul, Orawon

    2013-09-26

    Ferulic acid is an important phenolic antioxidant found in or added to diet supplements, beverages, and cosmetic creams. Two designs of paper-based platforms for the fast, simple and inexpensive evaluation of ferulic acid contents in food and pharmaceutical cosmetics were evaluated. The first, a paper-based electrochemical device, was developed for ferulic acid detection in uncomplicated matrix samples and was created by the photolithographic method. The second, a paper-based colorimetric device was preceded by thin layer chromatography (TLC) for the separation and detection of ferulic acid in complex samples using a silica plate stationary phase and an 85:15:1 (v/v/v) chloroform: methanol: formic acid mobile phase. After separation, ferulic acid containing section of the TLC plate was attached onto the patterned paper containing the colorimetric reagent and eluted with ethanol. The resulting color change was photographed and quantitatively converted to intensity. Under the optimal conditions, the limit of detection of ferulic acid was found to be 1 ppm and 7 ppm (S/N = 3) for first and second designs, respectively, with good agreement with the standard HPLC-UV detection method. Therefore, these methods can be used for the simple, rapid, inexpensive and sensitive quantification of ferulic acid in a variety of samples.

  2. Thiomonas sp. CB2 is able to degrade urea and promote toxic metal precipitation in acid mine drainage waters supplemented with urea

    PubMed Central

    Farasin, Julien; Andres, Jérémy; Casiot, Corinne; Barbe, Valérie; Faerber, Jacques; Halter, David; Heintz, Dimitri; Koechler, Sandrine; Lièvremont, Didier; Lugan, Raphael; Marchal, Marie; Plewniak, Frédéric; Seby, Fabienne; Bertin, Philippe N.; Arsène-Ploetze, Florence

    2015-01-01

    The acid mine drainage (AMD) in Carnoulès (France) is characterized by the presence of toxic metals such as arsenic. Several bacterial strains belonging to the Thiomonas genus, which were isolated from this AMD, are able to withstand these conditions. Their genomes carry several genomic islands (GEIs), which are known to be potentially advantageous in some particular ecological niches. This study focused on the role of the “urea island” present in the Thiomonas CB2 strain, which carry the genes involved in urea degradation processes. First, genomic comparisons showed that the genome of Thiomonas sp. CB2, which is able to degrade urea, contains a urea genomic island which is incomplete in the genome of other strains showing no urease activity. The urease activity of Thiomonas sp. CB2 enabled this bacterium to maintain a neutral pH in cell cultures in vitro and prevented the occurrence of cell death during the growth of the bacterium in a chemically defined medium. In AMD water supplemented with urea, the degradation of urea promotes iron, aluminum and arsenic precipitation. Our data show that ureC was expressed in situ, which suggests that the ability to degrade urea may be expressed in some Thiomonas strains in AMD, and that this urease activity may contribute to their survival in contaminated environments. PMID:26441922

  3. Acid precipitation and food quality: Effects of dietary Al, Ca and P on bone and liver characteristics in American black ducks and mallards

    USGS Publications Warehouse

    Sparling, D.W.

    1991-01-01

    American black ducks (Anas rubripes) and mallards (A. platyrhynchos) were fed diets varying in concentrations of aluminum (Al). calcium (Ca), and phosphorus (P) for 10 weeks to identify toxic effects of Al under conditions representative of areas with acid precipitation. Femur and liver tissues were analyzed for Al. Ca, and P concentrations and structural characteristics. At two weeks of age, both species demonstrated pronounced differences in femur Al and P concentrations and femur mass from dietary Al and interaction between Ca:P regimen and Al:Low Ca:Low P enhanced Al storage and decreased P and mass in femurs. Femur Ca was lowest in the Low Ca:Low P regimen but was not affected by dietary Al. At 10 weeks, femur and liver Al continued to vary with dietary Al. Elevated Al and reduced Ca lowered modulus of elasticity. Femur P increased with elevated dietary P in black ducks. Elevated dietary P negated some of the effects of dietary A! on femur mass in black ducks. Reduced Ca concentrations weakened bones of both species and lowered both Ca and P. An array of clinical signs including lameness, discoloration of the upper mandible, complete and greenstick fractures, and death were responses to elevated Al and Ca:P regimen. Black ducks seemed to display these signs over a wider range of diets than mallards. Diets of 1,000 mg/kg Al had toxic effects on both species, particularly when combined with diets low in Ca and P.

  4. The search for an identification of amino acids, nucleobases and nucleosides in samples returned from Mars

    NASA Technical Reports Server (NTRS)

    Gehrke, Charles W.; Ponnamperuma, Cyril; Kuo, Kenneth C.; Stalling, David L.; Zumwalt, Robert W.

    1988-01-01

    The Mars Sample Return mission will provide us with a unique source of material from our solar system; material which could advance our knowledge of the processes of chemical evolution. As has been pointed out, Mars geological investigations based on the Viking datasets have shown that primordial Mars was in many biologically important ways similar to the primordial Earth; the presence of surface liquid water, moderate surface temperatures, and atmosphere of carbon dioxide and nitrogen, and high geothermal heat flow. Indeed, it would seem that conditions on Earth and Mars were fundamentally similar during the first one billion years or so. As has been pointed out, Mars may well contain the best preserved record of the events that transpired on the early planets. Examination of that early record will involve searching for many things, from microfossils to isotopic abundance data. We propose an investigation of the returned Mars samples for biologically important organic compounds, with emphases on amino acids, the purine and pyrimidine bases, and nucleosides.

  5. Nitrate and Nitrite Determination in Gunshot Residue Samples by Capillary Electrophoresis in Acidic Run Buffer().

    PubMed

    Erol, Özge Ö; Erdoğan, Behice Y; Onar, Atiye N

    2017-03-01

    Simultaneous determination of nitrate and nitrite in gunshot residue has been conducted by capillary electrophoresis using an acidic run buffer (pH 3.5). In previously developed capillary electrophoretic methods, alkaline pH separation buffers were used where nitrite and nitrate possess similar electrophoretic mobility. In this study, the electroosmotic flow has been reversed by using low pH running buffer without any additives. As a result of reversing the electroosmotic flow, very fast analysis has been actualized, well-defined and separated ion peaks emerge in less than 4 min. Besides, the limit of detection was improved by employing large volume sample stacking. Limit of detection values were 6.7 and 4.3 μM for nitrate and nitrite, respectively. In traditional procedure, mechanical agitation is employed for extraction, while in this work the extraction efficiency of ultrasound mixing for 30 min was found sufficient. The proposed method was successfully applied to authentic gunshot residue samples.

  6. Centrifugal precipitation chromatography.

    PubMed

    Ito, Yoichiro; Qi, Lin

    2010-01-15

    Centrifugal precipitation chromatography separates analytes according their solubility in ammonium sulfate (AS) solution and other precipitants. The separation column is made from a pair of long spiral channels partitioned with a semipermeable membrane. In a typical separation, concentrated ammonium sulfate is eluted through one channel while water is eluted through the other channel in the opposite direction. This countercurrent process forms an exponential AS concentration gradient through the water channel. Consequently, protein samples injected into the water channel is subjected to a steadily increasing AS concentration and at the critical AS concentration they are precipitated and deposited in the channel bed by the centrifugal force. Then the chromatographic separation is started by gradually reducing the AS concentration in the AS channel which lowers the AS gradient concentration in the water channel. This results in dissolution of deposited proteins which are again precipitated at an advanced critical point as they move through the channel. Consequently, proteins repeat precipitation and dissolution through a long channel and finally eluted out from the column in the order of their solubility in the AS solution. The present method has been successfully applied to a number of analytes including human serum proteins, recombinant ketosteroid isomerase, carotenoid cleavage enzymes, plasmid DNA, polysaccharide, polymerized pigments, PEG-protein conjugates, etc. The method is capable to single out the target species of proteins by affinity ligand or immunoaffinity separation.

  7. Extraction and Separation of Vitisin D, Ampelopsin B and cis-Vitisin A from Iris lactea Pall. var. chinensis (Fisch.) Koidz by Alkaline Extraction-Acid Precipitation and High-Speed Counter-Current Chromatography.

    PubMed

    Lv, Huanhuan; Zhou, Wenna; Wang, Xiaoyan; Wang, Zhenhua; Suo, Yourui; Wang, Honglun

    2016-01-01

    Naturally occurring oligostilbenes are receiving more attention because they exhibit several beneficial effects for health, including hepatoprotective, antitumor, anti-adipogenic, antioxidant, antiaging, anti-inflammatory, anti-microbial, antiviral, immunosuppressive and neuroprotective activities. Thus, they could be of some potentially therapeutic values for several diseases. In this study, we adopted the alkaline extraction-acid precipitation (AEAP) method for extraction of oligostilbenes from the seed kernel of Iris lactea Then, the high-speed counter-current chromatography (HSCCC) was used for preparative isolation and purification of oligostilbenes from the AEAP extracts. Finally, three oligostilbenes, namely vitisin D (73 mg), ampelopsin B (25 mg) and cis-vitisin A (16 mg), were successfully fractionated by HSCCC with a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (2:5:3:6, v/v/v/v) from 300 mg of the AEAP extracts in ∼ 190 min. The purities of the three isolated oligostilbenes were all over 95.0% as analyzed by high performance liquid chromatography. They all were isolated from I. lacteal for the first time.The method of AEAP for the preparation of the oligostilbene-enriched crude sample was simple, and the HSCCC technique for the isolation and purification of oligostilbenes was efficient.

  8. Acid rains over semi-urban atmosphere at eastern Himalaya and near coast of Bay of Bengal and alkaline rains over typical urban atmosphere in India: A study on precipitation chemistry during monsoon, 2013

    NASA Astrophysics Data System (ADS)

    Roy, Arindam; Chatterjee, Abhijit; Sarkar, Chirantan; Ghosh, Sanjay; Raha, Sibaji

    A study has been made on precipitation chemistry over three different atmosphere in India. Rain samples were collected during the entire period of monsoon (June-October) in the year of 2013 over Kolkata (22.6 (°) N, 89.4 (°) E), a mega city with typical urban atmosphere; Falta (22.3 (°) N, 88.1 (°) E), a rural atmosphere near eastern coast of Bay of Bengal and Darjeeling (27.01 (°) N, 88.15 (°) E), a high altitude (2200 m asl)hill station over eastern Himalaya in India. The major focus of the study is to investigate the composition of various types of aerosol ionic components scavenged and its effect on the acidity and how it differs between these three distinctly different atmospheres. The results showed that the sea-salt components were higher in Falta (140 mueqv/lit) followed by Kolkata (120 mueqv/lit) and minimum in Darjeeling (30 mueqv/lit). Over all the stations, Na (+) and Cl (-) showed strong correlations indicating common marine source. The marine air masses originated from Bay of Bengal (BoB) were found to significantly enrich sea-salt particles over Falta, the nearest station from BoB and having least effect on Darjeeling, the farthest station from BoB. Dust and anthropogenic aerosols particles were significantly higher over Kolkata compared to other two stations. Dust particles were found to scavenge more in the initial phase of monsoon and it gradually decreased as the monsoon progressed. The average pH of rain water over Kolkata was 6.0 indicating alkaline in nature. pH over Falta was 5.2 indicating slightly acidic in nature and the most important fact is that pH over Darjeeling was 4.6 indicating highly acidic in nature. It was found that Ca (2+) , Mg (2+) and NH _{4} (+) neutralized the acidity of rain water over all the stations with the maximum neutralizing factor for Ca (2+) . However, NH _{4} (+) played important role over Darjeeling in neutralizing rain water acidity. The major reason for high acidity of rain water was not due to high

  9. A poly(3-acetylthiophene) modified glassy carbon electrode for selective voltammetric measurement of uric acid in urine sample.

    PubMed

    Aslanoglu, Mehmet; Kutluay, Aysegul; Abbasoglu, Sultan; Karabulut, Serpil

    2008-03-01

    A reliable and reproducible method for the determination of uric acid in urine samples has been developed. The method is based on the modification of a glassy carbon electrode by 3-acetylthiophene using cyclic voltammetry. The poly(3-acetylthiophene) modified glassy carbon electrode showed an excellent electrocatalytic effect towards the oxidation of uric acid in 0.1 m phosphate buffer solution (PBS) at pH 7.2. Compared with a bare glassy carbon electrode (GCE), an obvious shift of the oxidation peak potential in the cathodic direction and a marked enhancement of the anodic current response for uric acid were observed. The poly(3-acetylthiophene)/GCE was used for the determination of uric acid using square wave voltammetry. The peak current increased linearly with the concentration of uric acid in the range of 1.25 x 10(-5)-1.75 x 10(-4) M. The detection limit was 5.27 x 10(-7) M by square wave voltammetry. The poly(3-acetylthiophene)/GCE was also effective to determine uric acid and ascorbic acid in a mixture and resolved the overlapping anodic peaks of these two species into two well-defined voltammetric peaks in cyclic voltammetry at 0.030 V and 0.320 V (vs. Ag/AgCl) for ascorbic acid and uric acid, respectively. The modified electrode exhibited stable and sensitive current responses toward uric acid and ascorbic acid. The method has successfully been applied for determination of uric acid in urine samples.

  10. Characterization of citrus pectin samples extracted under different conditions: influence of acid type and pH of extraction

    PubMed Central

    Kaya, Merve; Sousa, António G.; Crépeau, Marie-Jeanne; Sørensen, Susanne O.; Ralet, Marie-Christine

    2014-01-01

    Background and Aims Pectin is a complex macromolecule, the fine structure of which is influenced by many factors. It is used as a gelling, thickening and emulsifying agent in a wide range of applications, from food to pharmaceutical products. Current industrial pectin extraction processes are based on fruit peel, a waste product from the juicing industry, in which thousands of tons of citrus are processed worldwide every year. This study examines how pectin components vary in relation to the plant source (orange, lemon, lime, grapefruit) and considers the influence of extraction conditions on the chemical and macromolecular characteristics of pectin samples. Methods Citrus peel (orange, lemon, lime and grapefruit) from a commercial supplier was used as raw material. Pectin samples were obtained on a bulk plant scale (kilograms; harsh nitric acid, mild nitric acid and harsh oxalic acid extraction) and on a laboratory scale (grams; mild oxalic acid extraction). Pectin composition (acidic and neutral sugars) and physicochemical properties (molar mass and intrinsic viscosity) were determined. Key Results Oxalic acid extraction allowed the recovery of pectin samples of high molecular weight. Mild oxalic acid-extracted pectins were rich in long homogalacturonan stretches and contained rhamnogalacturonan I stretches with conserved side chains. Nitric acid-extracted pectins exhibited lower molecular weights and contained rhamnogalacturonan I stretches encompassing few and/or short side chains. Grapefruit pectin was found to have short side chains compared with orange, lime and lemon. Orange and grapefruit pectin samples were both particularly rich in rhamnogalacturonan I backbones. Conclusions Structural, and hence macromolecular, variations within the different citrus pectin samples were mainly related to their rhamnogalacturonan I contents and integrity, and, to a lesser extent, to the length of their homogalacturonan domains. PMID:25081519

  11. Synthesis of 2-Mercaptonicotinic Acid-Capped CdSe Quantum Dots and its Application to Spectrofluorometric Determination of Cr(VI) in Water Samples.

    PubMed

    Hosseini, Mohammad Saeid; Khorashahi, Somayeh; Hosseini, Navid

    2016-05-01

    The CdSe quantum dots (QDs) capped with 2-mercaptonicotinic acid (H2MN) were prepared through a controllable process at 80 °C. The prepared QDs were characterized by XRD, TEM, IR, UV-Vis and fluorescence (FL) techniques. It was found that the QDs were nearly mono-disperse with the diameters in the range of 8-10 nm. These QDs are capable to exhibit strong FL even in concentrated acidic media. They exhibit an enhanced fluorescence in the presence of Cr(VI), which was used for the determination of Cr(VI) in water samples. The linear range was found to be 1 × 10(-7)-6.0 × 10(-6) M with the RSD and DL of 0.92 % and 5 × 10(-8) M, respectively. Except that Ca(2+) and Fe(3+) which can be eliminated through a simple precipitation process, the other co-existent ions present in natural water were not interfered. The recoveries obtained for the added amounts of Cr(VI) were in the range of 96.9-103.2 %, which denote on application of the method, satisfactorily.

  12. Polycyclic aromatic hydrocarbons and amino acids in meteorites and ice samples from LaPaz Icefield, Antarctica

    NASA Astrophysics Data System (ADS)

    Botta, O.; Martins, Z.; Emmenegger, C.; Dworkin, J. P.; Glavin, D. P.; Harvey, R. P.; Zenobi, R.; Bada, J. L.; Ehrenfreund, P.

    2008-11-01

    We have analyzed ice samples and meteorites from the LaPaz region of Antarctica to investigate the composition of polycyclic aromatic hydrocarbons (PAHs) and amino acids with the goal to understand whether or not there is a compositional relationship between the two reservoirs. Four LL5 ordinary chondrites (OCs) and one CK carbonaceous chondrite were collected as part of the 2003/2004 ANSMET season. Ice samples collected from directly underneath the meteorites were extracted. In addition, exhaust particles from the snowmobiles used during the expedition were collected to investigate possible contributions from this source. The meteorite samples, the particulate matter and solid-state extracts of the ice samples and the exhaust filters were subjected to two-step laser mass spectrometry (L2MS) to investigate the PAH composition. For amino acids analysis, the meteorites were extracted with water and acid hydrolyzed, and the extracts were analyzed with offline OPA/NAC derivatization combined with liquid chromatography with UV fluorescence detection and time of flight mass spectrometry (LC-FD/ToF-MS). PAHs in the particulate matter of the ice were found to be qualitatively similar to the meteorite samples, indicating that micron-sized grains of the meteorite may be embedded in the ice samples. The concentration levels of dissolved PAHs in all the ice samples were found to be below the detection limit of the L2MS. The PAH composition of the snowmobile exhaust is significantly different to the one in particulate matter, making it an unlikely source of contamination for Antarctic meteorites. The amino acids glycine, β-alanine and γ-amino-n-butyric acid that were detected at concentrations of 3 to 19 parts per billion (ppb) are probably indigenous to the Antarctic meteorites. Some of the LaPaz ice samples were also found to contain amino acids at concentration levels of 1 to 33 parts per trillion (ppt), in particular α-aminoisobutyric acid (AIB), an abundant non

  13. Validation of Internal Controls for Extraction and Amplification of Nucleic Acids from Enteric Viruses in Water Samples ▿ †

    PubMed Central

    Hata, Akihiko; Katayama, Hiroyuki; Kitajima, Masaaki; Visvanathan, Chettiyappan; Nol, Chea; Furumai, Hiroaki

    2011-01-01

    Inhibitors that reduce viral nucleic acid extraction efficiency and interfere with cDNA synthesis and/or polymerase activity affect the molecular detection of viruses in aquatic environments. To overcome these significant problems, we developed a methodology for assessing nucleic acid yields and DNA amplification efficiencies for environmental water samples. This involved adding particles of adenovirus type 5 and murine norovirus and newly developed primer-sharing controls, which are amplified with the same primer pairs and result in the same amplicon sizes as the targets, to these samples. We found that nucleic acid loss during the extraction process, rather than reverse transcription-PCR (RT-PCR) inhibition, more significantly attributed to underestimation of the presence of viral genomes in the environmental water samples tested in this study. Our success rate for satisfactorily amplifying viral RNAs and DNAs by RT-PCR was higher than that for obtaining adequate nucleic acid preparations. We found that inhibitory properties were greatest when we used larger sample volumes. A magnetic silica bead-based RNA extraction method effectively removed inhibitors that interfere with viral nucleic acid extraction and RT-PCR. To our knowledge, this is the first study to assess the inhibitory properties of environmental water samples by using both control virus particles and primer-sharing controls. PMID:21602369

  14. Determination of the mode of occurrence of As, Cr, and Hg in three Chinese coal samples by sequential acid leaching

    SciTech Connect

    Wang, B.; Li, W.; Wang, G.; Chen, H.; Li, B.

    2007-07-01

    Sequential acid leaching was used to leach minerals and the trace elements they contain. One-step leaching uses concentrated nitric acid as solvent, while three-step leaching uses 5M hydrochloric acid, concentrated hydrofluoric acid, and concentrated hydrochloric acid as solvents. The sequential acid leaching by three-and one-step leach was also examined. The results showed that one-step leaching could leach over 80% of arsenic from coal samples, and also could leach mercury to a certain degree. During one-step leaching, little chromium is removed, but it is available to leach by three-step leaching; and during the sequential acid leaching by three and one-step leaching, almost 98% ash is leached. The result of acid leaching could also give detailed information on mode of occurrence of As, Cr, and Hg, which could be classified into: silicate association, pyrite association, organic association, and carbonates and sulfates association. Over half of chromium in the three coals is associated with organic matters and the rest is associated with silicates. The mode of occurrence of arsenic and mercury is mainly associated with different mineral matters depending on the coal samples studied.

  15. Effects of packaging and storage conditions on the quality of amoxicillin-clavulanic acid – an analysis of Cambodian samples

    PubMed Central

    2013-01-01

    Background The use of substandard and degraded medicines is a major public health problem in developing countries such as Cambodia. A collaborative study was conducted to evaluate the quality of amoxicillin–clavulanic acid preparations under tropical conditions in a developing country. Methods Amoxicillin-clavulanic acid tablets were obtained from outlets in Cambodia. Packaging condition, printed information, and other sources of information were examined. The samples were tested for quantity, content uniformity, and dissolution. Authenticity was verified with manufacturers and regulatory authorities. Results A total of 59 samples were collected from 48 medicine outlets. Most (93.2%) of the samples were of foreign origin. Using predetermined acceptance criteria, 12 samples (20.3%) were non-compliant. Eight (13.6%), 10 (16.9%), and 20 (33.9%) samples failed quantity, content uniformity, and dissolution tests, respectively. Samples that violated our observational acceptance criteria were significantly more likely to fail the quality tests (Fisher’s exact test, p < 0.05). Conclusions Improper packaging and storage conditions may reduce the quality of amoxicillin–clavulanic acid preparations at community pharmacies. Strict quality control measures are urgently needed to maintain the quality of amoxicillin–clavulanic acid in tropical countries. PMID:23773420

  16. Application of self-organising maps towards segmentation of soybean samples by determination of amino acids concentration.

    PubMed

    Silva, Lívia Ramazzoti Chanan; Angilelli, Karina Gomes; Cremasco, Hágata; Romagnoli, Érica Signori; Galão, Olívio Fernandes; Borsato, Dionisio; Moraes, Larissa Alexandra Cardoso; Mandarino, José Marcos Gontijo

    2016-09-01

    Soybeans are widely used both for human nutrition and animal feed, since they are an important source of protein, and they also provide components such as phytosterols, isoflavones, and amino acids. In this study, were determined the concentrations of the amino acids lysine, histidine, arginine, asparagine, glutamic acid, glycine, alanine, valine, isoleucine, leucine, tyrosine, phenylalanine present in 14 samples of conventional soybeans and 6 transgenic, cultivated in two cities of the state of Paraná, Londrina and Ponta Grossa. The results were tabulated and presented to a self-organising map for segmentation according planting regions and conventional or transgenic varieties. A network with 7000 training epochs and a 10 × 10 topology was used, and it proved appropriate in the segmentation of the samples using the data analysed. The weight maps provided by the network, showed that all the amino acids were important in targeting the samples, especially isoleucine. Three clusters were formed, one with only Ponta Grossa samples (including transgenic (PGT) and common (PGC)), a second group with Londrina transgenic (LT) samples and the third with Londrina common (LC) samples.

  17. Sequential injection titration method using second-order signals: determination of acidity in plant oils and biodiesel samples.

    PubMed

    del Río, Vanessa; Larrechi, M Soledad; Callao, M Pilar

    2010-06-15

    A new concept of flow titration is proposed and demonstrated for the determination of total acidity in plant oils and biodiesel. We use sequential injection analysis (SIA) with a diode array spectrophotometric detector linked to chemometric tools such as multivariate curve resolution-alternating least squares (MCR-ALS). This system is based on the evolution of the basic specie of an acid-base indicator, alizarine, when it comes into contact with a sample that contains free fatty acids. The gradual pH change in the reactor coil due to diffusion and reaction phenomenona allows the sequential appearance of both species of the indicator in the detector coil, recording a data matrix for each sample. The SIA-MCR-ALS method helps to reduce the amounts of sample, the reagents and the time consumed. Each determination consumes 0.413ml of sample, 0.250ml of indicator and 3ml of carrier (ethanol) and generates 3.333ml of waste. The frequency of the analysis is high (12 samples h(-1) including all steps, i.e., cleaning, preparing and analysing). The utilized reagents are of common use in the laboratory and it is not necessary to use the reagents of perfect known concentration. The method was applied to determine acidity in plant oil and biodiesel samples. Results obtained by the proposed method compare well with those obtained by the official European Community method that is time consuming and uses large amounts of organic solvents.

  18. Chemical characteristics of precipitation at metropolitan Newark in the US East Coast

    NASA Astrophysics Data System (ADS)

    Song, Fei; Gao, Yuan

    To investigate the chemical characteristics of precipitation in the polluted coastal atmosphere, a total of 46 event-based precipitation samples were collected using a wet-only automatic precipitation collector from September 2006 to October 2007 at metropolitan Newark, New Jersey in the US East Coast. Samples were analyzed by ion chromatography for the concentrations of major inorganic ions (Cl -, NO 3-, SO 42-, F -, NH 4+, Ca 2+, Mg 2+, Na +, K +) and organic acid species (CH 3COO -, HCOO -, CH 2(COO) 22-, C 2O 42-). Selected trace metals (Sb, Pb, Al, V, Fe, Cr, Co, Ni, Cu, Zn, Cd) in samples were determined by ICPMS. Mass concentration results show that SO 42- was the most dominant anion accounting for 51% of the total anions, controlling the acidity of the precipitation. NH 4+ accounted for 48.6% of the total cations, dominating the precipitation neutralization. CH 3COO - and HCOO - were the two dominant water-soluble organic acid species, accounting for 42% and 40% of the total organic acids analyzed, respectively. Al, Zn and Fe were the three major trace metals in precipitation, accounting for 34%, 27%, and 25% of the total mass of metals analyzed. The pH values in precipitation ranged from 4.4 to 4.9, indicating an acidic nature. Enrichment Factor (EF) Analysis showed that Na +, Cl -, Mg 2+ and K + in the precipitation were primarily of marine origin, while most of the Fe, Co and Al were from crust sources. Pb, V, Cr, Ni were moderately enriched with EFs ranging 43-410, while Zn, Sb, Cu, Cd and F - were highly enriched with EFs > 700, indicating significant anthropogenic influences. Factor analysis suggests 6 major sources contributing to the observed composition of precipitation at this location: (1) nitrogen-enriched soil, (2) secondary pollution processes, (3) marine sources, (4) incinerations, (5) oil combustions, and (6) malonate-vanadium enriched sources. To further explore the source-precipitation event relationships and seasonality, cluster analysis

  19. Quantitative enantioseparation of amino acids by comprehensive two-dimensional gas chromatography applied to non-terrestrial samples.

    PubMed

    Myrgorodska, Iuliia; Meinert, Cornelia; Martins, Zita; le Sergeant d'Hendecourt, Louis; Meierhenrich, Uwe J

    2016-02-12

    This work presents an improved analytical procedure for the resolution and quantification of amino acid enantiomers by multidimensional gas chromatography. The procedure contains a derivatization step, by which amino acids were transformed into N(O,S)-ethoxycarbonylheptafluorobutyl esters. It was optimized for the resolution of non-proteinogenic amino acids in the matrix of complex non-terrestrial samples. The procedure has proven to be highly sensitive and shows a wide linearity range with 0.005-3 pmol detection limits for quantitative determinations. The developed procedure was tested on a sample of the Murchison meteorite, for which obtained chromatograms show excellent peak resolution, minimal co-elution and peak overlap. We conclude that comprehensive two dimensional chromatography, in combination with the optimized derivatization method is a highly suitable technique for the analysis of samples with very limited quantities and containing potentially prebiotic molecules, such as interstellar ice analogs and meteorites.

  20. Nickel-aluminum layered double hydroxide as a nanosorbent for selective solid-phase extraction and spectrofluorometric determination of salicylic acid in pharmaceutical and biological samples.

    PubMed

    Abdolmohammad-Zadeh, H; Kohansal, S; Sadeghi, G H

    2011-04-15

    The nickel-aluminum layered double hydroxide (Ni-Al LDH) was synthesized by a simple co-precipitation method and used as a solid-phase extraction (SPE) sorbent for separation and pre-concentration of trace levels of salicylic acid (SA) from aqueous solutions. Extraction of analyte is based on the adsorption of salicylate ions on the Ni-Al (NO(3)(-)) LDH and/or their exchanging with LDH interlayer NO(3)(-) ions. The retained analyte on the LDH was stripped by 3 mol L(-1) NaOH solution and its concentration was subsequently determined spectrofluorometrically at λ(em)=400 nm with excitation at λ(ex)=270 nm. Various parameters affecting the extraction efficiency of SA on the Ni-Al (NO(3)(-)) LDH, such as pH, amount of nano-sorbent, sample loading flow rate, elution conditions, sample volume and matrix effects were investigated. In the optimum experimental conditions, the limit of detection (3s) and enrichment factor were 0.12 μg L(-1) and 40, respectively. The relative standard deviation (RSD) for six replicate determinations of 10 μg L(-1) SA was 2.3%. The calibration graph using the pre-concentration system was linear in the range of 0.3-45 μg L(-1) with a correlation coefficient of 0.9985. The optimized method was successfully applied to the determination of SA in blood serum, willow leaf and aspirin tablet.

  1. Selective recovery of dissolved Fe, Al, Cu, and Zn in acid mine drainage based on modeling to predict precipitation pH.

    PubMed

    Park, Sang-Min; Yoo, Jong-Chan; Ji, Sang-Woo; Yang, Jung-Seok; Baek, Kitae

    2015-02-01

    Mining activities have caused serious environmental problems including acid mine drainage (AMD), the dispersion of mine tailings and dust, and extensive mine waste. In particular, AMD contaminates soil and water downstream of mines and generally contains mainly valuable metals such as Cu, Zn, and Ni as well as Fe and Al. In this study, we investigated the selective recovery of Fe, Al, Cu, Zn, and Ni from AMD. First, the speciation of Fe, Al, Cu, Zn, and Ni as a function of the equilibrium solution pH was simulated by Visual MINTEQ. Based on the simulation results, the predicted pHs for the selective precipitation of Fe, Al, Cu, and Zn/Ni were determined. And recovery yield of metals using simulation is over 99 %. Experiments using artificial AMD based on the simulation results confirmed the selective recovery of Fe, Al, Cu, and Zn/Ni, and the recovery yields of Fe/Al/Cu/Zn and Fe/Al/Cu/Ni mixtures using Na2CO3 were 99.6/86.8/71.9/77.0 % and 99.2/85.7/73.3/86.1 %, respectively. After then, the simulation results were applied to an actual AMD for the selective recovery of metals, and the recovery yields of Fe, Al, Cu, and Zn using NaOH were 97.2, 74.9, 66.9, and 89.7 %, respectively. Based on the results, it was concluded that selective recovery of dissolved metals from AMD is possible by adjusting the solution pH using NaOH or Na2CO3 as neutralizing agents.

  2. Evaluation of commercial kits for the extraction and purification of viral nucleic acids from environmental and fecal samples.

    PubMed

    Iker, Brandon C; Bright, Kelly R; Pepper, Ian L; Gerba, Charles P; Kitajima, Masaaki

    2013-07-01

    The extraction and purification of nucleic acids is a critical step in the molecular detection of enteric viruses from environmental or fecal samples. In the present study, the performance of three commercially available kits was assessed: the MO BIO PowerViral Environmental DNA/RNA Isolation kit, the Qiagen QIAamp Viral RNA Mini kit, and the Zymo ZR Virus DNA/RNA Extraction kit. Viral particles of adenovirus 2 (AdV), murine norovirus (MNV), and poliovirus type 1 (PV1) were spiked in molecular grade water and three different types of sample matrices (i.e., biosolids, feces, and surface water concentrates), extracted with the kits, and the yields of the nucleic acids were determined by quantitative PCR (qPCR). The MO BIO kit performed the best with the biosolids, which were considered to contain the highest level of inhibitors and provided the most consistent detection of spiked virus from all of the samples. A qPCR inhibition test using an internal control plasmid DNA and a nucleic acid purity test using an absorbance at 230 nm for the nucleic acid extracts demonstrated that the MO BIO kit was able to remove qPCR inhibitors more effectively than the Qiagen and Zymo kits. These results suggest that the MO BIO kit is appropriate for the extraction and purification of viral nucleic acids from environmental and clinical samples that contain high levels of inhibitors.

  3. Akaganéite (β-FeOOH) precipitation in inland acid sulfate soils of south-western New South Wales (NSW), Australia

    NASA Astrophysics Data System (ADS)

    Bibi, Irshad; Singh, Balwant; Silvester, Ewen

    2011-11-01

    The prevalence of sulphidic sediments in inland wetlands has been only recently recognized in many parts of the world, including Australia. The exposure of sulphidic sediments in these wetlands due to natural and human induced drying events has resulted in the oxidation of iron sulfide minerals, the formation of secondary iron minerals characteristic of acid sulfate soils and the release of highly acidic solutions. The objective of this study was to determine the mineralogy and morphology of sediments collected from the oxidized surface horizon (0-5 cm) of an inland acid sulfate soil located in south-western New South Wales (NSW), Australia. Random powder X-ray diffraction (XRD), transmission electron microscopy (TEM) and scanning transmission electron microscopy combined with energy dispersive X-ray spectroscopy (STEM-EDS) techniques were used to characterize the minerals present in these sediments. Akaganéite was identified as the major mineral phase in the sediments; K-jarosite was also determined in small amounts in some sediments. The XRD patterns of sequentially washed (E-pure® water-0.01 M HCl-0.01 M EDTA) sediment samples showed all akaganéite peaks; the Rietveld refinement of these patterns also revealed a predominance of akaganéite. The chemical analyses of the original and washed sediments using STEM-EDS clearly showed the presence of akaganéite as a pure mineral phase with an average Fe/Cl mole ratio of 6.7 and a structural formula of Fe 8O 8(OH) 6.8(Cl) 1.2. These findings show that the extreme saline-acidic solutions (pH ˜ 2, EC = 216 dS/m) at the Bottle Bend lagoon provide ideal conditions for the crystallization of this rarely forming mineral.

  4. [Densitometric method for parallel measurement of rosmarinic and caffeic acids in plant samples].

    PubMed

    Janicsák, G; Máthé, I

    1998-09-01

    In the last few years, the role of free radicals in the promotion of cell aging and tumour growth has focused attention on phenolic compounds. Rosmarinic acid (RA) and caffeic acid (CA), as major components of tannins, commonly occur together in many species of the Lamiaceae. A TLC-densitometric method was introduced for the parallel determination of RA and CA. Experiments were performed to establish the optimal measurement parameters related to the excitation wavelength, colour stability, linearity of the calibration curves, sensitivity and reproducibility. In the wavelength range 290-330 nm, it was found that the emission peak areas exhibit a maximum at 325 nm. Therefore, the densitometric evaluations of these tannins were made at 325 nm. The two compounds behaved very similarly as regards colour stability. The changes during the 3 hours of observation were not strong, as reflected by coefficients of variation of 8.20% for RA and 5.40% for CA. The calibration plots demonstrating the relation between the spotted amount and the measured peak area were found to include 2 intersecting linear sections, in the intervals 0-0.40 microgram and 0.40-1.20 micrograms for RA and 0-0.08 microgram and 0.08-0.30 microgram for CA. The correlation coefficients ranging between 0.991 and 0.998. The lower limits of detection were 1 ng for RA and 0.1 ng for CA. The reproducibility proved to be very good: the 10 times repeated densitometric estimation of the same spot yielded a coefficient of variation of 0.34% for RA and 0.36 for CA. The application of TLC permits utilization of the fluorescence of both phenols, often without the need for prior purification. This fluorescence measurement makes the detection extremely sensitive. The densitometric quantification allows the routine analysis of many samples in a short time with reasonable accuracy. The practical application of the elaborated method will be demonstrated on the leaves of 5 Salvia species. The results are shown in table I.

  5. Single-step enantioselective amino acid flux analysis by capillary electrophoresis using on-line sample preconcentration with chemical derivatization.

    PubMed

    Ptolemy, Adam S; Tran, Lara; Britz-McKibbin, Philip

    2006-07-15

    Capillary electrophoresis (CE) represents a versatile platform for integrating sample pretreatment with chemical analysis because of its ability to tune analyte electromigration and band dispersion properties in discontinuous electrolyte systems. In this article, a single-step method that combines on-line sample preconcentration with in-capillary chemical derivatization is developed for rapid, sensitive, and enantioselective analysis of micromolar levels of amino acids that lack intrinsic chromophores by CE with UV detection. Time-resolved electrophoretic studies revealed two distinct stages of amino acid band narrowing within the original long sample injection plug occurring both prior to and after in-capillary labeling via zone passing by ortho-phthalaldehyde/N-acetyl l-cysteine (OPA/NAC). This technique enabled direct analysis of d-amino acids in a 95% enantiomeric excess mixture with sub-micromolar detection limits and minimal sample handling, where the capillary functions as a preconcentrator, microreactor, and chiral selector. On-line sample preconcentration with chemical derivatization CE (SPCD-CE) was applied to study the enantioselective amino acid flux in Escherichia coli bacteria cultures, which demonstrated a unique l-Ala efflux into the extracellular medium. New strategies for high-throughput analyses of low-abundance metabolites are important for understanding fundamental physiological processes in bacteria required for screening the efficacy of new classes of antibiotics as well as altered metabolism in genetically modified mutant strains.

  6. Catalytic kinetic spectrophotometry for the determination of trace amount of oxalic acid in biological samples with oxalic acid-rhodamine B-potassium dichromate system

    NASA Astrophysics Data System (ADS)

    Zhai, Qing-Zhou; Zhang, Xiao-Xia; Liu, Qing-Zhou

    2006-09-01

    A new catalytic kinetic spectrophotometric method was proposed for determining trace oxalic acid based on the catalytic effect of oxalate on the oxidation of potassium dichromate with rhodamin B in 0.10 M of sulfuric acid. Good linearity is obtained over the concentration range 0.40-6.0 μg/mL of oxalic acid. After the reactions of the catalytic and non-catalytic systems were terminated by using 2.00 mL of 4 M sodium hydroxide solution, they can be stable for 3 h at room temperature. The apparent activation energy of the catalytic reaction is 12.44 kJ/mol. The effect of 50 coexisting substances was observed. The method was used to determine trace oxalic acid in tea, spinach and urine samples with satisfactory results.

  7. Catalytic kinetic spectrophotometry for the determination of trace amount of oxalic acid in biological samples with oxalic acid-rhodamine B-potassium dichromate system.

    PubMed

    Zhai, Qing-Zhou; Zhang, Xiao-Xia; Liu, Qing-Zhou

    2006-09-01

    A new catalytic kinetic spectrophotometric method was proposed for determining trace oxalic acid based on the catalytic effect of oxalate on the oxidation of potassium dichromate with rhodamin B in 0.10 M of sulfuric acid. Good linearity is obtained over the concentration range 0.40-6.0 microg/mL of oxalic acid. After the reactions of the catalytic and non-catalytic systems were terminated by using 2.00 mL of 4 M sodium hydroxide solution, they can be stable for 3 h at room temperature. The apparent activation energy of the catalytic reaction is 12.44 kJ/mol. The effect of 50 coexisting substances was observed. The method was used to determine trace oxalic acid in tea, spinach and urine samples with satisfactory results.

  8. Method and Apparatus for Automated Isolation of Nucleic Acids from Small Cell Samples

    NASA Technical Reports Server (NTRS)

    Sundaram, Shivshankar; Prabhakarpandian, Balabhaskar; Pant, Kapil; Wang, Yi

    2014-01-01

    RNA isolation is a ubiquitous need, driven by current emphasis on microarrays and miniaturization. With commercial systems requiring 100,000 to 1,000,000 cells for successful isolation, there is a growing need for a small-footprint, easy-to-use device that can harvest nucleic acids from much smaller cell samples (1,000 to 10,000 cells). The process of extraction of RNA from cell cultures is a complex, multi-step one, and requires timed, asynchronous operations with multiple reagents/buffers. An added complexity is the fragility of RNA (subject to degradation) and its reactivity to surface. A novel, microfluidics-based, integrated cartridge has been developed that can fully automate the complex process of RNA isolation (lyse, capture, and elute RNA) from small cell culture samples. On-cartridge cell lysis is achieved using either reagents or high-strength electric fields made possible by the miniaturized format. Traditionally, silica-based, porous-membrane formats have been used for RNA capture, requiring slow perfusion for effective capture. In this design, high efficiency capture/elution are achieved using a microsphere-based "microfluidized" format. Electrokinetic phenomena are harnessed to actively mix microspheres with the cell lysate and capture/elution buffer, providing important advantages in extraction efficiency, processing time, and operational flexibility. Successful RNA isolation was demonstrated using both suspension (HL-60) and adherent (BHK-21) cells. Novel features associated with this development are twofold. First, novel designs that execute needed processes with improved speed and efficiency were developed. These primarily encompass electric-field-driven lysis of cells. The configurations include electrode-containing constructs, or an "electrode-less" chip design, which is easy to fabricate and mitigates fouling at the electrode surface; and the "fluidized" extraction format based on electrokinetically assisted mixing and contacting of microbeads

  9. Measurement of naphthenic acids in the receiving waters around an offshore oil platform by passive sampling.

    PubMed

    Harman, Christopher; Langford, Katherine; Sundt, Rolf C; Brooks, Steven

    2014-09-01

    Polar organic chemical integrative samplers (POCIS) were deployed in the vicinity of an offshore oil installation and analyzed for naphthenic acids (NAs). The POCIS accumulated a range of mono- to tetracyclic NAs, with different degrees of alkylation, with monocyclic acids being the most abundant. Currently, POCIS or similar polar samplers may be the only way to measure exposure to NAs from offshore discharges in situ. In addition, they may be a valuable tool for monitoring similar organic acids in general.

  10. MAP3S/RAINE precipitation chemistry network: quality control

    SciTech Connect

    Not Available

    1980-10-01

    The participants of the precipitation chemistry network of the Multi-State Atmospheric Power Production Pollution Study/Regional Acidity of Industrial Emissions (MAP3S/RAINE) have developed procedures for maintenance of high quality output from the network operation. The documented procedures-most of which were in place before the network began sampling in 1976-include those for site selection and verification, field equipment, laboratory and data handling, and external laboratory quality testing.

  11. Voltammetric iodometric titration of ascorbic acid with dead-stop end-point detection in fresh vegetables and fruit samples.

    PubMed

    Verdini, R A; Lagier, C M

    2000-07-01

    The present work describes a method for determining ascorbic acid, which combines iodometry with a voltammetric technique to detect the end point of the titration. In addition, the validity of the method applied to natural vegetable or fruit samples was assessed. The results were compared with those obtained by an accurate method such as HPLC using UV detection. Similar values of ascorbic acid for different natural samples were obtained by means of this approach (p > 0.05). The limit of quantification was 0.1 mg. This technique presents the advantage of other electroanalytical methods such as avoiding filtration or ultracentrifugation steps, with the additional benefit of using the platinum electrodes, which are routinely used in the laboratory. These facts allow a rapid and efficient quantification of ascorbic acid with very low cost of reagents and equipment.

  12. Optimization of the treatment of wheat samples for the determination of phytic acid by HPLC with refractive index detection.

    PubMed

    Amaro, Rosa; Murillo, Miguel; González, Zurima; Escalona, Andrés; Hernández, Luís

    2009-01-01

    The treatment of wheat samples was optimized before the determination of phytic acid by high-performance liquid chromatography with refractive index detection. Drying by lyophilization and oven drying were studied; drying by lyophilization gave better results, confirming that this step is critical in preventing significant loss of analyte. In the extraction step, washing of the residue and collection of this water before retention of the phytates in the NH2 Sep-Pak cartridge were important. The retention of phytates in the NH2 Sep-Pak cartridge and elimination of the HCI did not produce significant loss (P = 0.05) in the phytic acid content of the sample. Recoveries of phytic acid averaged 91%, which is a substantial improvement with respect to values reported by others using this methodology.

  13. Characterization of the first core sample of neutralized current acid waste from double-shell tank 101-AZ

    SciTech Connect

    Peterson, M E; Scheele, R D; Tingey, J M

    1989-09-01

    In FY 1989, Westinghouse Hanford Company (WHC) successfully obtained four core samples (totaling seven segments) of neutralized current acid waste (NCAW) from double-shell tanks (DSTs) 101-AZ and 102-AZ. A segment was a 19-in.-long and 1-in.-diameter cylindrical sample of waste. A core sample consisted of enough 19-in.-long segments to obtain the waste of interest. Three core samples were obtained from DST 101-AZ and one core sample from DST 102-AZ. Two DST 101-AZ core samples consisted of two segments per core, and the third core sample consisted of only one segment. The third core consisted of the solids from the bottom of the tank and was used to determine the relative abrasiveness of this NCAW. The DST 102-AZ core sample consisted of two segments. The core samples were transported to the Pacific Northwest Laboratory (PNL), where the waste was extruded from its sampler and extensively characterized. A characterization plan was followed that simulated the processing of the NCAW samples through retrieval, pretreatment and vitrification process steps. Physical, rheological, chemical and radiochemical properties were measured throughout the process steps. The characterization of the first core sample from DST 101-AZ was completed, and the results are provided in this report. The results for the other core characterizations will be reported in future reports. 3 refs., 13 figs., 10 tabs.

  14. Use of a polystyrene-divinylbenzene-based weakly acidic cation-exchange resin column and propionic acid as an eluent in ion-exclusion/adsorption chromatography of aliphatic carboxylic acids and ethanol in food samples.

    PubMed

    Mori, Masanobu; Hironaga, Takahiro; Kajiwara, Hiroe; Nakatani, Nobutake; Kozaki, Daisuke; Itabashi, Hideyuki; Tanaka, Kazuhiko

    2011-01-01

    We developed an ion-exclusion/adsorption chromatography (IEAC) method employing a polystyrene-divinylbenzene-based weakly acidic cation-exchange resin (PS-WCX) column with propionic acid as the eluent for the simultaneous determination of multivalent aliphatic carboxylic acids and ethanol in food samples. The PS-WCX column well resolved mono-, di-, and trivalent carboxylic acids in the acidic eluent. Propionic acid as the eluent gave a higher signal-to-noise ratio, and enabled sensitive conductimetric detection of analyte acids. We found the optimal separation condition to be the combination of a PS-WCX column and 20-mM propionic acid. Practical applicability of the developed method was confirmed by using a short precolumn with a strongly acidic cation-exchange resin in the H(+)-form connected before the separation column; this was to remove cations from food samples by converting them to hydrogen ions. Consequently, common carboxylic acids and ethanol in beer, wine, and soy sauce were successfully separated by the developed method.

  15. Comparison of GC-MS and FTIR methods for quantifying naphthenic acids in water samples.

    PubMed

    Scott, Angela C; Young, Rozlyn F; Fedorak, Phillip M

    2008-11-01

    The extraction of bitumen from the oil sands in Canada releases toxic naphthenic acids into the process-affected waters. The development of an ideal analytical method for quantifying naphthenic acids (general formula C(n)H(2n+Z)O(2)) has been impeded by the complexity of these mixtures and the challenges of differentiating naphthenic acids from other naturally-occurring organic acids. The oil sands industry standard FTIR method was compared with a newly-developed GC-MS method. Naphthenic acids concentrations were measured in extracts of surface and ground waters from locations within the vicinity of and away from the oil sands deposits and in extracts of process-affected waters. In all but one case, FTIR measurements of naphthenic acids concentrations were greater than those determined by GC-MS. The detection limit of the GC-MS method was 0.01 mg L(-1) compared to 1 mg L(-1) for the FTIR method. The results indicated that the GC-MS method is more selective for naphthenic acids, and that the FTIR method overestimates their concentrations.

  16. DISSOLUTION OF PLUTONIUM CONTAINING CARRIER PRECIPITATE BY CARBONATE METATHESIS AND SEPARATION OF SULFIDE IMPURITIES THEREFROM BY SULFIDE PRECIPITATION

    DOEpatents

    Duffield, R.B.

    1959-07-14

    A process is described for recovering plutonium from foreign products wherein a carrier precipitate of lanthanum fluoride containing plutonium is obtained and includes the steps of dissolving the carrier precipitate in an alkali metal carbonate solution, adding a soluble sulfide, separating the sulfide precipitate, adding an alkali metal hydroxide, separating the resulting precipitate, washing, and dissolving in a strong acid.

  17. The research of the contamination levels present in samples of precipitation and surface waters collected from the catchment area Fuglebekken (Hornsund, Svalbard Archipelago)

    NASA Astrophysics Data System (ADS)

    Ruman, Marek; Szopińska, Małgorzata; Kozak, Katarzyna; Lehmann, Sara; Polkowska, Żaneta

    2014-10-01

    Persistent organic pollutants (POPs) are contaminants that may appear in polar regions. In present work surface water was collected from the main stream water in the Fuglebekken basin. The precipitationsamples was collected from the near area by Polish Polar Station in Hornsund. The present investigationreveals the results of the analysis of these samples for their total phenols, formaldehyde, TOC, PAHs and PCBs content. The presence in the basin (thousands of kilometers distant from industrial centers) of those compounds is testimony to the fact that these compounds are transported over vast distances with air masses and deposited in regions devoid of any human impact.

  18. Isomers/enantiomers of perfluorocarboxylic acids: Method development and detection in environmental samples

    EPA Science Inventory

    Perfluoroalkyl substances are globally distributed in both urban and remote settings, and routinely are detected in wildlife, humans, and the environment. One of the most prominent and routinely detected perfluoroalkyl substances is perfluorooctanoic acid (PFOA), which has been s...

  19. One-pot synthesis of quantum dot-labeled hydrophilic molecularly imprinted polymer nanoparticles for direct optosensing of folic acid in real, undiluted biological samples.

    PubMed

    Yang, Yaqiong; Wang, Zhengzheng; Niu, Hui; Zhang, Huiqi

    2016-12-15

    A facile and efficient one-pot approach for the synthesis of quantum dot (QD)-labeled hydrophilic molecularly imprinted polymer (MIP) nanoparticles for direct optosensing of folic acid (FA) in the undiluted bovine and porcine serums is described. Hydrophilic macromolecular chain transfer agent-mediated reversible addition-fragmentation chain transfer (RAFT) precipitation polymerization was used to implement the molecular imprinting of FA in the presence of CdTe quantum dots (QDs). The resulting FA-imprinted polymer nanoparticles with surface-grafted hydrophilic poly(glyceryl monomethacrylate) brushes and QDs labeling not only showed outstanding specific molecular recognition toward FA in biological samples, but also exhibited good photostability, rapid binding kinetics, and obvious template binding-induced fluorescence quenching. These characteristics make them a useful fluorescent chemosensor for directly and selectively optosensing FA in the undiluted bovine and porcine serums, with its limit of detection being 0.025μM and average recoveries ranging from 98% to 102%, even in the presence of several interfering compounds. This advanced fluorescent MIP chemosensor is highly promising for rapid quantification of FA in such applications as clinical diagnostics and food analysis.

  20. Dual-column cation-exchange chromatographic method for beta-aminoisobutyric acid and beta-alanine in biological samples.

    PubMed

    Kuo, K C; Cole, T F; Gehrke, C W; Waalkes, T P; Borek, E

    1978-08-01

    A rapid, automated chromatographic method has been developed for the quantitation of the nucleic acid catabolites beta-aminoisobutyric acid and beta-alanine in urine, serum, and other physiological fluids. The analyses were performed on a modified Beckman 121M amino acid analyzer with dual ion-exchange columns and the use of a single sodium citrate buffer (pH 4.38, 0.20 mol/liter). By carefully matching the elution pattern for the two ion-exchange columns and alternating use of these columns, analyses are completed every 40 min. The chromatography, regeneration, and equilibration of the two columns are precisely programmed, thus the detector sees only the elution of beta-aminoisobutyric acid and beta-alanine alternately from each column. Long-term precision and analytical recovery for the two metabolites in urine were 1.9 and 102%, and 3.3 and 101%, respectively. Their normal physiological values were determined in human serum and urine. Their excretion in the urine was also studied as a function of collection time, to validate a more convenient, less costly method of sampling. This study shows that randomly collected samples are acceptable when the concentration of the two metabolites are expressed in terms of creatinine excretion. In addition, the distribution of the free and conjugated forms of the two metabolites in urine and serum was studied. A preparative method was also developed for the quantitative isolation of beta-amino-isobutyric acid from urine samples. The alternating dual-column technique may be applied to any ion-exchange chromatographic method where many analyses must be performed. This method is currently used in our laboratories for measuring these beta-amino acids in urine and serum of patients with various types of cancers.

  1. Non-precipitating cumulus cloud study

    SciTech Connect

    Alkezweeny, A.J.

    1984-10-01

    This document describes the field experiment that was conducted in Kentucky during the period from July 20 to August 24, 1983. The objectives were to determine the vertical transport of acidic pollutants by cumulus convection and formation of acidic substances in non-precipitating clouds. The study is a research component of Task Group C (Atmospheric Processes) of the National Acid Precipitation Assessment Program. To examine the vertical transport, an SF/sub 6/ tracer was released from one aircraft, sampled by another aircraft, and sampled on the ground. The results show that pollutants from the boundary layer are lifted to the cloud layer. From there, they are intermittently transported both to the ground and to higher elevations, possibly in the vertical updrafts of towering cumulus clouds. A series of instrumented aircraft flights around the clouds were conducted to study the formation of acidic aerosols. The concentrations of SO/sub 2/, SO/sub 4/, NO/sub 3/, NH/sub 4/, NH/sub 3/, HNO/sub 3/ and trace metals were measured by filter techniques. Furthermore, NO/sub x/, O/sub 3/, light scattering, and basic meteorological parameters were measured in real-time. Detailed chemical composition of aerosols and NH/sub 3/ was also measured on the ground. Preliminary results show that the molar ratio of SO/sub 2//SO/sub 2/ + SO/sub 4/) at cloud tops is higher than at cloud bases. This indicates that sulfate aerosols were formed in the clouds. The NH/sub 3/ concentration shows higher values at nighttime than daytime and decreases sharply with increasing altitude. 3 references.

  2. Pulsed electromembrane extraction for analysis of derivatized amino acids: A powerful technique for determination of animal source of gelatin samples.

    PubMed

    Rezazadeh, Maryam; Yamini, Yadollah; Seidi, Shahram; Aghaei, Ali

    2015-05-01

    Differentiation of animal sources of gelatin is required for many reasons such as some anxieties about bovine spongiform encephalopathy or a ban on consuming porcine gelatin in some religions. In the present work, an efficient method is introduced for determination of animal origin of gelatin samples. The basis of this procedure is the application of pulsed electric field for extraction, preconcentration, and analysis of derivatized amino acids in gelatin. To this end, after derivatization of amino acids of interest by means of o-phthalaldehyde (OPA) for enhancing their ultraviolet (UV) absorbance as well as increasing their lipophilicities, a 137V electric field was applied for 20min with 10min(-1) frequency to make the analytes migrate through a 200µm organic liquid membrane into an aqueous acceptor phase. Finally, the acceptor phase was analyzed by HPLC-UV. The proposed technique offered a high efficiency for analysis of amino acids, regarding 43% and 79% as extraction recoveries and 25ng mL(-1) and 50ng mL(-1) as limits of detection (LODs) for asparagine and glutamine, respectively. Therefore, due to sample cleanup ability of the proposed method and obtained preconcentration factors (29 and 53 for asparagine and glutamine, respectively), it could be carried out for differentiation of animal origins of gelatin samples, even if only small amounts of samples are available or in complicated media of foodstuffs and medicament.

  3. Plasma proteome coverage is increased by unique peptide recovery from sodium deoxycholate precipitate.

    PubMed

    Serra, Aida; Zhu, Hongbin; Gallart-Palau, Xavier; Park, Jung Eun; Ho, Hee Haw; Tam, James P; Sze, Siu Kwan

    2016-03-01

    The ionic detergent sodium deoxycholate (SDC) is compatible with in-solution tryptic digestion and LC-MS/MS-based shotgun proteomics by virtue of being easy to separate from the peptide products via precipitation in acidic buffers. However, it remains unclear whether unique human peptides co-precipitate with SDC during acid treatment of complex biological samples. In this study, we demonstrate for the first time that a large quantity of unique peptides in human blood plasma can be co-precipitated with SDC using an optimized sample preparation method prior to shotgun proteomic analysis. We show that the plasma peptides co-precipitated with SDC can be successfully recovered using a sequential re-solubilization and precipitation procedure, and that this approach is particularly efficient at the extraction of long peptides. Recovery of peptides from the SDC pellet dramatically increased overall proteome coverage (>60 %), thereby improving the identification of low-abundance proteins and enhancing the identification of protein components of membrane-bound organelles. In addition, when we analyzed the physiochemical properties of the co-precipitated peptides, we observed that SDC-based sample preparation improved the identification of mildly hydrophilic/hydrophobic proteins that would otherwise be lost upon discarding the pellet. These data demonstrate that the optimized SDC protocol is superior to sodium dodecyl sulfate (SDS)/urea treatment for identifying plasma biomarkers by shotgun proteomics.

  4. Quantitative and discriminative analysis of nucleic acid samples using luminometric nonspecific nanoparticle methods

    NASA Astrophysics Data System (ADS)

    Pihlasalo, S.; Mariani, L.; Härmä, H.

    2016-03-01

    Homogeneous simple assays utilizing luminescence quenching and time-resolved luminescence resonance energy transfer (TR-LRET) were developed for the quantification of nucleic acids without sequence information. Nucleic acids prevent the adsorption of a protein to europium nanoparticles which is detected as a luminescence quenching of europium nanoparticles with a soluble quencher or as a decrease of TR-LRET from europium nanoparticles to the acceptor dye. Contrary to the existing methods based on fluorescent dye binding to nucleic acids, equal sensitivities for both single- (ssDNA) and double-stranded DNA (dsDNA) were measured and a detection limit of 60 pg was calculated for the quenching assay. The average coefficient of variation was 5% for the quenching assay and 8% for the TR-LRET assay. The TR-LRET assay was also combined with a nucleic acid dye selective to dsDNA in a single tube assay to measure the total concentration of DNA and the ratio of ssDNA and dsDNA in the mixture. To our knowledge, such a multiplexed assay is not accomplished with commercially available assays.Homogeneous simple assays utilizing luminescence quenching and time-resolved luminescence resonance energy transfer (TR-LRET) were developed for the quantification of nucleic acids without sequence information. Nucleic acids prevent the adsorption of a protein to europium nanoparticles which is detected as a luminescence quenching of europium nanoparticles with a soluble quencher or as a decrease of TR-LRET from europium nanoparticles to the acceptor dye. Contrary to the existing methods based on fluorescent dye binding to nucleic acids, equal sensitivities for both single- (ssDNA) and double-stranded DNA (dsDNA) were measured and a detection limit of 60 pg was calculated for the quenching assay. The average coefficient of variation was 5% for the quenching assay and 8% for the TR-LRET assay. The TR-LRET assay was also combined with a nucleic acid dye selective to dsDNA in a single tube

  5. The effect of sample hydration on 13C CPMAS NMR spectra of fulvic acids

    USGS Publications Warehouse

    Hatcher, P.G.; Wilson, M.A.

    1991-01-01

    Three fulvic acids, two of which have been well studied by a number of other groups (Armadale and Suwannee river fulvic acids) have been examined by high resolution solid-state 13C-NMR techniques to delineate the effect of absorbed water. Two main effects of absorbed water were observed: (1) changes in spin lattice relaxation times in the rotating frame and cross polarization times and (2) total loss of signal so that some fulvic acid is effectively in solution. These results suggest that discrepancies in the literature concerning observed relative signal intensities from different structural groups are due to absorbed water and emphasize the necessity for proper precautionary drying before spectroscopic analysis. ?? 1991.

  6. Aluminum colloid formation and its effect on co-precipitation of zinc during acid rock drainage remediation with clinoptilolite in a slurry bubble column

    NASA Astrophysics Data System (ADS)

    Xu, W.; Li, L. Y.; Grace, J. R.

    2012-04-01

    Zinc and other metal ions were adsorbed in a laboratory slurry bubble column (SBC) by natural clinoptilolite sorbent particles. During the remediation process, significant white precipitates were sometimes observed. Both zinc and aluminum were detected in the colloidal mixtures. It is shown that Al leached from clinoptilolite during the agitation, contributing to the precipitate. As a result of the Al leaching and increase of pH during the remediation process, the formation of an Al colloid and zinc adsorption onto it could significantly improve ARD remediation, given the high adsorption capacity of the colloid. Sorption of cations increased with increasing colloid formation. Various conditions were tested to investigate their impact on (a) dealumination of clinoptilolite; (b) Al hydrolysis/colloid formation; and (c) adsorption onto the colloidal mixture. The test results indicate that dealumination contributes to the excess aluminum in the aqueous phase and to precipitates. The excess dealumination varies with pH and agitation time. Al hydrolysis occurs with increasing pH due to the neutralization effect of clinoptilolite. A significant proportion of zinc adsorbed onto the collectible aluminum precipitates.

  7. HYDROLYSIS OF MTBE IN GROUND WATER SAMPLES PRESERVED WITIH HYDROCHLORIC ACID

    EPA Science Inventory

    Conventional sampling and analytical protocols have poor sensitivity for fuel oxygenates that are alcohols, such as TBA. Because alcohols tend to stay with the water samples, they are not efficiently transferred to the gas chromatograph for separation and analysis. A common tec...

  8. Seasonal and rainfall-type variations in inorganic ions and dicarboxylic acids and acidity of wet deposition samples collected from subtropical East Asia

    NASA Astrophysics Data System (ADS)

    Tsai, Ying I.; Hsieh, Li-Ying; Kuo, Su-Ching; Chen, Chien-Lung; Wu, Pei-Ling

    2011-07-01

    Rainfall samples were collected over a period of 3 years and 8 months in subtropical East Asia. They are categorized into different rainfall types and analyzed to assess the ionic composition and its effect on the acidity of wet deposition in southern Taiwan. Only 4% of samples had a pH of <5.0, indicating that the study area is not impacted significantly by acid rain. The volume-weighted mean (VWM) pH by rainfall type was Spring Rain 5.74, Typhoon Rain 5.56, Summer Rain 5.46, Typhoon Outer Circulation (TOC) Rain 5.45, Plum Rain 5.32 and Autumn-Winter Rain 5.29. Dilution effects were important to the equivalent ionic concentration of different rainfall types. HCO 3-, SO 42- and Cl - were detected as major anions whereas NH 4+, Na + and Ca 2+ were major cations. CO 2-derived HCO 3- was the major ionic species in all but Typhoon Rain and Spring Rain, in which the major species were Na + and Cl - and Ca 2+, respectively. Excluding HCO 3-, the major species were NH 4+, Na + and Ca 2+ in Plum Rain, the secondary photochemical products SO 42-, NO 3- and NH 4+ in TOC Rain and Summer Rain, and Na + and Ca 2+ in Autumn-Winter Rain. Calculation of arithmetic means showed that dicarboxylic acids contributed between 0.25% and 0.53% of the total ionic concentration and of these, oxalic acid contributed the least (81.3% of the dicarboxylic acid) to TOC Rain and the most (96.1% of the dicarboxylic acid) to Spring Rain, suggestive of long-range transport in the latter. Differences in wet deposition composition were shown to be a result of differences in local emissions and long-range transport (hence of prevailing wind direction) during the period of rainfall and of the frequency and volume of rain that typifies each rainfall type. Principal component analysis (PCA) further revealed that traffic-related and industrial organic and inorganic pollutants, their secondary photochemical products, sea salts, and dust are important contributors to wet deposition. Moreover, the ratio of

  9. Use of sequential sampling of amphipod abundance to classify the biotic integrity of acid-sensitive lakes

    NASA Astrophysics Data System (ADS)

    France, Robert

    1992-03-01

    A sequential sampling program using previously published zoobenthos data is described for ubiquitous, cost-effective biomonitoring of the effects of lake acidification. Spring densities of the littoral amphipod Hyalella azteca are quantitatively sorted into five abundance catagories. An essential step in the a priori definition of decision criteria is the stratification of proportional densities per unit macrophyte biomass in relation to aqueous total phosphorus concentrations. Density rankings were related to lake acidity and to detailed lake-specific information on patterns of Hyalella life history and acid tolerance. Incorporation of Hyalella abundance as a potential metric for the assessment of the biological integrity of acid-sensitive waters is recommended. The temporal integration of transient changes in spring meltwater chemistry is an important rationale for the development of such biomonitoring procedures.

  10. Preservation of nucleic acids and tissue morphology in paraffin-embedded clinical samples: comparison of five molecular fixatives.

    PubMed

    Staff, Synnöve; Kujala, Paula; Karhu, Ritva; Rökman, Annika; Ilvesaro, Joanna; Kares, Saara; Isola, Jorma

    2013-09-01

    Formalin fixation preserves tissue morphology at the expense of macromolecule integrity. Freshly frozen samples are the golden standard for DNA and RNA analyses but require laborious deep-freezing and frozen sectioning for morphological studies. Alternative tissue stabilisation methods are therefore needed. We analysed the preservation of nucleic acids, immunohistochemical staining properties and tissue morphology in paraffin-embedded clinical tissue samples fixed with Z7, RCL2, PAXgene, Allprotect and RNAlater. Formalin-fixed and deep-frozen samples were used as controls. Immunohistochemical analyses showed good preservation of antigenicity in all except Allprotect and RNAlater-fixed samples. RNA quality, based on RNA integrity number value by Bioanalyzer, was comparable with freshly frozen samples only in PAXgene-fixed samples. According to quantitative reverse transcription-polymerase chain reaction (qRT-PCR) analyses, RNA from PAXgene samples yielded results similar to freshly frozen samples. No difference between fixatives was seen in DNA analyses (PCR and real-time PCR). In conclusion, PAXgene seems to be superior to other molecular fixatives and formaldehyde.

  11. Rapid and sensitive determination of ethylenediaminetetraacetic acid and diethylenetriaminepentaacetic acid in water samples by ion-pair reversed-phase liquid chromatography--electrospray tandem mass spectrometry.

    PubMed

    Quintana, José Benito; Reemtsma, Thorsten

    2007-03-23

    A new method is presented for the quantitative determination of ethylenediaminetetraacetic acid (EDTA) and diethylenetriaminepentaacetic acid (DTPA) from aqueous samples without an enrichment step. It consist of the formation of the Fe(III) complexes of EDTA and DTPA, liquid-chromatography with a volatile ion-pairing agent and determination by electrospray ionization-tandem mass spectrometry (ESI-MS/MS). Limits of quantification (LOQ) of 1.0 and 0.6 microgL(-1) for EDTA and DTPA were obtained, allowing the direct injection of most aqueous environmental samples without any preceding enrichment. With a more recent mass spectrometer, the LOQ could be further decreased by almost one order of magnitude. Parallel analysis of real samples by a standardized method employing enrichment, derivatization and GC-MS analysis yielded comparable results. The method was applied to the determination of both complexing agents in several wastewater, surface water and drinking water samples, showing that EDTA is an omnipresent contaminant in partially closed water cycles.

  12. An integrated paper-based sample-to-answer biosensor for nucleic acid testing at the point of care.

    PubMed

    Choi, Jane Ru; Hu, Jie; Tang, Ruihua; Gong, Yan; Feng, Shangsheng; Ren, Hui; Wen, Ting; Li, XiuJun; Wan Abas, Wan Abu Bakar; Pingguan-Murphy, Belinda; Xu, Feng

    2016-02-07

    With advances in point-of-care testing (POCT), lateral flow assays (LFAs) have been explored for nucleic acid detection. However, biological samples generally contain complex compositions and low amounts of target nucleic acids, and currently require laborious off-chip nucleic acid extraction and amplification processes (e.g., tube-based extraction and polymerase chain reaction (PCR)) prior to detection. To the best of our knowledge, even though the integration of DNA extraction and amplification into a paper-based biosensor has been reported, a combination of LFA with the aforementioned steps for simple colorimetric readout has not yet been demonstrated. Here, we demonstrate for the first time an integrated paper-based biosensor incorporating nucleic acid extraction, amplification and visual detection or quantification using a smartphone. A handheld battery-powered heating device was specially developed for nucleic acid amplification in POC settings, which is coupled with this simple assay for rapid target detection. The biosensor can successfully detect Escherichia coli (as a model analyte) in spiked drinking water, milk, blood, and spinach with a detection limit of as low as 10-1000 CFU mL(-1), and Streptococcus pneumonia in clinical blood samples, highlighting its potential use in medical diagnostics, food safety analysis and environmental monitoring. As compared to the lengthy conventional assay, which requires more than 5 hours for the entire sample-to-answer process, it takes about 1 hour for our integrated biosensor. The integrated biosensor holds great potential for detection of various target analytes for wide applications in the near future.

  13. Quantification of 4'-geranyloxyferulic acid (GOFA) in honey samples of different origin by validated RP-HPLC-UV method.

    PubMed

    Genovese, Salvatore; Taddeo, Vito Alessandro; Fiorito, Serena; Epifano, Francesco

    2016-01-05

    Natural honey has been employed as a nutraceutical agent with benefits and therapeutic promises for humans for many centuries. It has been largely used as food and medicine by all generations, traditions, and civilizations, both ancient and modern. Several chemicals having beneficial effects for human health have been reported as components of natural honey and these include sugars, organic acids, aminoacids, minerals, and vitamins. Also some important phytochemicals have been described and these comprise tannins, flavonoids, terpenes, saponins, and alkaloids. In this note it is described the successful application of a RP HPLC-UV-vis method for the separation and quantification of 4'-geranyloxyferulic acid (GOFA) in four honey samples of different origin. Concentration values showed a great variation between the four samples tested, being chestnut honey the one richest in GOFA (7.87 mg/g). The findings described herein represent the first example reported in the literature of the characterization of an oxyprenylated phenylpropanoid in honey.

  14. Folic acid absorption determined by a single stool sample test--a double-isotope technique. The folic acid absorption capacity in children

    SciTech Connect

    Hjelt, K. )

    1989-10-01

    The fractional folic acid absorption (FAFol) was determined in 66 patients with various gastrointestinal diseases by a double-isotope technique, employing a single stool sample test (SSST) as well as a complete stool collection. The age of the patients ranged from 2.5 months to 16.8 years (mean 6.3 years). The test dose was administered orally and consisted of 50 micrograms of (3H)folic acid (monoglutamate) (approximately 20 muCi), carmine powder, and 2 mg 51CrCl3 (approximately 1.25 muCi) as the unabsorbable tracer. The whole-body radiation given to a 1-year-old child averaged 4.8 mrad only. The stool and napkin contents were collected and homogenized by the addition of 300 ml chromium sulfuric acid. A 300-ml sample of the homogenized stool and napkin contents, as well as 300 ml chromium sulfuric acid (75% vol/vol) containing the standards, were counted for the content of 51Cr in a broad-based well counter. The quantity of (3H)folic acid was determined by liquid scintillation, after duplicate distillation. Estimated by SSST, the FAFol, which employs the stool with the highest content of 51Cr corresponding to the most carmine-colored stool, correlated closely with the FAFol based on complete stool collection (r = 0.96, n = 39, p less than 0.0001). The reproducibility of FAFol determined by SSST was assessed from repeated tests in 18 patients. For a mean of 81%, the SD was 4.6%, which corresponded to a coefficient of variation of 5.7%.

  15. Determination of amines as pentafluoropropionic acid anhydride derivatives in biological samples using liquid chromatography and tandem mass spectrometry.

    PubMed

    Marand, Asa; Karlsson, Daniel; Dalene, Marianne; Skarping, Gunnar

    2004-06-01

    Determination of amines in biological samples as markers of exposure to the amines or the corresponding isocyanates is an important tool for industrial exposure assessment. In this study, a liquid chromatography and tandem mass spectrometry (LC-MS/MS) method for determination of amines in biological samples as perfluorofatty amides derivatives is presented. The method enables determination of diamines such as methylene diamine (MDA), toluene diamine (TDA), naphthalene diamine (NDA), hexamethylene diamine (HDA), isophorone diamine (IPDA), methylenedi(cyclohexylamine)(HMDA) and 4,4'-methylene-(2-chloroaniline)(MOCA) in human urine and plasma. The work-up procedure included hydrolysis of the biological samples with 3 M H(2)SO(4) at 100 degrees C for 16 h and extraction of the amines into toluene, where derivatisation of the amines with perfluorofatty acid anhydride was performed. Following removal of excess reagent and the acid formed and an exchange of solvent, the derivatives were analysed using gradient elution with an acetonitrile/water mobile phase composition and electrospray ionisation (ESI) with multiple reaction monitoring (MRM) of [M - H](-)-->[M - H - 120](-) or [119](-). Several perfluorofatty acid anhydrides were evaluated as derivatisation reagents, but the LC chromatographic properties of the pentafluoropropionic acid anhydride (PFPA) derivatives were favourable. Quantification of amine-PFPA derivatives was performed using deuterium labelled amine-PFPA derivatives as internals standards with good precision and linearity in the investigated range of 0-20 ng ml(-1) urine. The instrumental detection limits for the amine-PFPA derivatives were 0.2-3 fmol for MRM of [M - H](-)-->[119](-) and 0.3-8 fmol for [M - H](-)-->[M - H - 120](-). In 10 urine and 6 plasma samples from workers exposed to isocyanates, determination of TDA and MDA as PFPA derivatives was performed using LC-MS/MS and a reference GC-MS method. No significant difference between the two

  16. Four-way calibration applied to the simultaneous determination of folic acid and methotrexate in urine samples.

    PubMed

    Muñoz de la Peña, A; Durán Merás, I; Jiménez Girón, A

    2006-08-01

    First-, second- and third-order calibration methods were investigated for the simultaneous determination of folic acid and methotrexate. The interest in the determination of these compounds is related to the fact that methotrexate inhibits the body's absorption of folic acid and prolonged treatment with methotrexate may lead to folic acid deficiency, and to the use of folic acid to cope with toxic side effects of methotrexate. Both analytes were converted into highly fluorescent compounds by oxidation with potassium permanganate, and the kinetics of the reaction was continuously monitored by recording the kinetics curves of fluorescence emission, the evolution with time of the emission spectra and the excitation-emission matrices (EEMs) of the samples at different reaction times. Direct determination of mixtures of both drugs in urine was accomplished on the basis of the evolution of the kinetics of EEMs by fluorescence measurements and four-way parallel-factor analysis (PARAFAC) or multiway partial least squares (N-PLS) chemometric calibration. The core consistency diagnostic (CORCONDIA) was employed to determine the correct number of factors in PARAFAC and the procedure converged to a choice of three factors, attributed to folic acid, methotrexate and to the sum of fluorescent species present in the urine.

  17. Quantification of fatty acids as methyl esters and phospholipids in cheese samples after separation of triacylglycerides and phospholipids.

    PubMed

    Hauff, Simone; Vetter, Walter

    2009-03-23

    Determination of the individual fatty acid composition of neutral- and phospholipids as well as the phospholipid content of dairy food and other foodstuffs are important tasks in life sciences. For these purposes, a method was developed for the separation of lipids (standards of triolein and diacylphosphatidylcholines as well as three cheese samples) by solid-phase extraction using a self-packed column filled with partly deactivated silica. Non-halogenated solvents were used for the elution of the lipid classes. Cyclohexane/ethyl acetate (1:1, v/v) served for the elution of neutral lipids, while polar lipids were eluted with three solvents (ethyl acetate/methanol, methanol, and methanol/water) into one fraction. The separated lipid fractions were transesterified and the individual fatty acids were quantified by using gas chromatography coupled to electron ionization mass spectrometry (GC/EI-MS) in the selected ion monitoring (SIM) mode. The recovery rate for standard phosphatidylcholines was approximately 90% and cross-contamination from neutral lipids was negligible. The method was applied to cheese samples. Quantitative amounts of individual fatty acids in the phospholipid fraction were <0.002-0.29% of total lipids from camembert, <0.002-0.12% of total lipids from mozzarella, and <0.002-0.18% of total lipids in a goat cream cheese. Differences in the fatty acid pattern of neutral and polar lipids were detected. The quantity of the fatty acids determined in the phospholipid fraction was divided by the factor 0.7 in order to convert the fatty acid content into the phospholipid content of the cheese samples. This factor is based on the contribution of 16:0 to dipalmitoylphosphatidylcholine (DPPC). The resulting DPPC equivalents (DPPC(eq)) were found to be representative for the average contribution of fatty acids to all classes of phospholipids in dairy products. Using this approach, the phospholipid content of lipids from mozzarella, camembert, and goat cream

  18. PRECIPITATION OF PLUTONOUS PEROXIDE

    DOEpatents

    Barrick, J.G.; Manion, J.P.

    1961-08-15

    A precipitation process for recovering plutonium values contained in an aqueous solution is described. In the process for precipitating plutonium as plutonous peroxide, hydroxylamine or hydrazine is added to the plutoniumcontaining solution prior to the addition of peroxide to precipitate plutonium. The addition of hydroxylamine or hydrazine increases the amount of plutonium precipitated as plutonous peroxide. (AEC)

  19. Free and combined amino acids in size-segregated atmospheric aerosol samples

    NASA Astrophysics Data System (ADS)

    Di Filippo, Patrizia; Pomata, Donatella; Riccardi, Carmela; Buiarelli, Francesca; Gallo, Valentina; Quaranta, Alessandro

    2014-12-01

    Concentrations of free and combined amino acids in an urban atmosphere and their distributions in size-segregated particles were investigated in the cold and warm seasons. In particular this article provides the first investigation of protein bioaerosol concentrations in ultrafine fraction (PM0.1) of particulate matter. In addition the present work provides amino acid and total proteinaceous material concentrations in NIST SRM 1649b, useful as reference values. The reference material was also used to build matrix matched calibration curves. Free amino acid total content in winter and summer PM0.1 was respectively 48.0 and 94.4 ng m-3, representing about 0.7 and 7.4% by weight of urban particulate matter in the two seasons. Total airborne protein and peptide concentrations in the same ultrafine fractions were 93.6 and 449.9 ng m-3 respectively in winter and in summer, representing 7.5 and 35.4% w/w of PM0.1, and demonstrating an exceptionally high percentage in summer ultrafine fraction. The significant potential adverse health effects of ultrafine particulate matter include allergies mainly caused by protein particles and we assumed that in summer 162 ng h-1 of proteinaceous material, by means of ultrafine particles, can penetrate from the lungs into the bloodstream.

  20. Degradation of vanillic acid and production of guaiacol by microorganisms isolated from cork samples.

    PubMed

    Alvarez-Rodríguez, María Luisa; Belloch, Carmela; Villa, Mercedes; Uruburu, Federico; Larriba, Germán; Coque, Juan José R

    2003-03-14

    The presence of guaiacol in cork stoppers is responsible for some cases of cork taint causing unpleasant alterations to wine. We have performed a characterization of the cork-associated microbiota by isolating 55 different microorganisms: eight yeast, 14 filamentous fungi or molds, 13 actinomycetes and 20 non-filamentous bacteria. A screening for degradation of vanillic acid and guaiacol production showed that none of the filamentous fungi could achieve any of these processes. By contrast, five of the eight yeast strains isolated were able to degrade vanillic acid, although it was not converted to guaiacol. Guaiacol production was only detected in four bacterial strains: one isolate of Bacillus subtilis and three actinomycetes, Streptomyces sp. A3, Streptomyces sp. A5 and Streptomyces sp. A13, were able to accumulate this compound in both liquid media and cultures over cork. These results suggest that guaiacol-mediated cork taint should be attributed to the degradative action of vanillic acid by bacterial strains growing on cork.

  1. Sulfate removal from waste chemicals by precipitation.

    PubMed

    Benatti, Cláudia Telles; Tavares, Célia Regina Granhen; Lenzi, Ervim

    2009-01-01

    Chemical oxidation using Fenton's reagent has proven to be a viable alternative to the oxidative destruction of organic pollutants in mixed waste chemicals, but the sulfate concentration in the treated liquor was still above the acceptable limits for effluent discharge. In this paper, the feasibility of sulfate removal from complex laboratory wastewaters using barium and calcium precipitation was investigated. The process was applied to different wastewater cases (two composite samples generated in different periods) in order to study the effect of the wastewater composition on the sulfate precipitation. The experiments were performed with raw and oxidized wastewater samples, and carried out according to the following steps: (1) evaluate the pH effect upon sulfate precipitation on raw wastewaters at pH range of 2-8; (2) conduct sulfate precipitation experiments on raw and oxidized wastewaters; and (3) characterize the precipitate yielded. At a concentration of 80 g L(-1), barium precipitation achieved a sulfate removal up to 61.4% while calcium precipitation provided over 99% sulfate removal in raw and oxidized wastewaters and for both samples. Calcium precipitation was chosen to be performed after Fenton's oxidation; hence this process configuration favors the production of higher quality precipitates. The results showed that, when dried at 105 degrees C, the precipitate is composed of hemidrate and anhydrous calcium sulfate ( approximately 99.8%) and trace metals ( approximately 0.2%: Fe, Cr, Mn, Co, Ag, Mg, K, Na), what makes it suitable for reuse in innumerous processes.

  2. Hydrocarbonates in precipitation of Moscow

    NASA Astrophysics Data System (ADS)

    Larin, Igor; Eremina, Iren; Aloyan, Artash; Arutunan, Vardan; Chubarova, Natalia; Yermakov, Alexandr

    2016-04-01

    According to monitoring of the atmospheric precipitation of Moscow a number of episodes is revealed, the content of hydrocarbonates in which repeatedly surpasses equilibrium level. Facts of their registration are linked to complex structure of precipitation which is caused by a different chemical composition of condensation nucleus. As a result on the underlying surface two groups of drops with acidity of the different nature are transferred. The acidity of the first, "metal" group of droplets, is determined by a carbonate equilibrium with atmospheric CO2 and with dissolved carbonates of alkali and alkaline earth metals. The acidity of the second, "ammonium" group droplets, is characterized by the balance between an ammonia absorbed from the air and atmospheric acids. Regulation of acidity of the deposits measured in a course of monitoring, occurs for this reason not only in the air, but also in the condensate receiver. A mixing "metal" and "ammonium" groups precipitation accompanied by only a partial transfer of hydrocarbonates in the dissolved CO2. The process is braked as a result of a practical stop of exit of CO2 into the atmosphere because of a mass transfer deceleration. In turn it leads to excess of equilibrium level of hydrocarbonates in the receiver. Estimates show that the acidity of "ammonia" component of precipitation should be much higher than the reported monitoring data. In other words, real acidity of rain drops can essentially exceed that is measured by standard procedures of monitoring of deposits, that it is necessary to take into consideration at calculations of so-called critical levels of acid loading on people and environment. In other words, the actual acidity of raindrops could greatly exceed that is measured by the standard procedures for monitoring rainfall, which should be taken into account when calculating the so-called critical levels of acid loads on people and the environment. It follows that the true level of hazard of acid rain

  3. Dissolved organic nitrogen in precipitation at two contrasting sites in Korea: Urban versus Rural

    NASA Astrophysics Data System (ADS)

    Yan, G.; Kim, G.

    2013-12-01

    It has been recognized that organic nitrogen is a significant and ubiquitous constituent of total fixed nitrogen in the atmosphere (contributing approx. 30% on average). Despite the growing number of studies being conducted on atmospheric organic nitrogen worldwide, virtually nothing is known about its distribution and characteristics in Korea. In this work, dissolved organic nitrogen (DON) was investigated in precipitation samples collected over a one-year period at two representative sites in Korea with contrasting environmental settings: Seoul (urban terrestrial, 2012-2013) and Uljin (background coastal, 2011-2012). The concentrations of DON in precipitation ranged from 0 to 72 μM (average of 11 μM) for Seoul, and from 0 to 145 μM (average of 30 μM) for Uljin, respectively. The fraction of total dissolved nitrogen (inorganic plus organic) composed by DON was found to be much higher in Uljin (28%) than that in Seoul (12%), which might indicate the significant contribution by natural sources to atmospheric DON. In addition, amino acids which are one of the most important components of atmospheric DON were also analyzed in our precipitation samples. The total concentrations (free plus combined) of 13 individual amino acids were determined by using high performance liquid chromatography after acidic liquid hydrolysis. The compositions of the amino acids pool showed considerable variations from sample to sample, suggesting the contributions from diverse sources and/or varying degradation states of the amino acids in our samples. Moreover, the D-amino acids (enantiomeric isomer) were found to be ubiquitous, with highest D/L ratios of 0.5, 0.5, 0.7, and 0.8 for aspartic acid, glutamic acid, serine, and alanine, respectively. The noteworthy presence of D-amino acids reveals the significant contributions to DON in our samples from bacterial biomass. Overall, our results fill the knowledge gap in distributions of atmospheric DON and contribute to the understanding of

  4. Can the use of deactivated glass fibre filters eliminate sorption artefacts associated with active air sampling of perfluorooctanoic acid?

    PubMed

    Johansson, Jana H; Berger, Urs; Cousins, Ian T

    2017-05-01

    Experimental work was undertaken to test whether gaseous perfluorooctanoic acid (PFOA) sorbs to glass fibre filters (GFFs) during air sampling, causing an incorrect measure of the gas-particle equilibrium distribution. Furthermore, tests were performed to investigate whether deactivation by siliconisation prevents sorption of gaseous PFOA to filter materials. An apparatus was constructed to closely simulate a high-volume air sampler, although with additional features allowing introduction of gaseous test compounds into an air stream stripped from particles. The set-up enabled investigation of the sorption of gaseous test compounds to filter media, eliminating any contribution from particles. Experiments were performed under ambient outdoor air conditions at environmentally relevant analyte concentrations. The results demonstrate that gaseous PFOA sorbs to GFFs, but that breakthrough of gaseous PFOA on the GFFs occurs at trace-level loadings. This indicates that during high volume air sampling, filters do not quantitatively capture all the PFOA in the sampled air. Experiments with siliconised GFFs showed that this filter pre-treatment reduced the sorption of gaseous PFOA, but that sorption still occurred at environmentally relevant air concentrations. We conclude that deactivation of GFFs does not allow for the separation of gaseous and particle bound perfluorinated carboxylic acids (PFCAs) during active air sampling. Consequently, the well-recognised theory that PFCAs do not prevail as gaseous species in the atmosphere may be based on biased measurements. Caution should be taken to ensure that this artefact will not bias the conclusions of future field studies.

  5. Protein concentration by precipitation with pyrogallol red prior to electrophoresis.

    PubMed

    Marshall, T; Abbott, N J; Fox, P; Williams, K M

    1995-01-01

    The pyrogallol red protein assay (Clinical Chemistry 1986, 32, 1551-1554) is based upon formation of a blue protein-dye complex in the presence of molybdate under acidic conditions. However, centrifugation of the assay mixture results in loss of color yield and precipitation of the protein-dye complex which can be recovered and resolubilized to achieve protein concentration prior to sodium dodecyl sulfate-polyacrylamide gel electrophoresis. The method has been evaluated relative to trichloroacetic acid (TCA) precipitation for recovery and electrophoresis of commercial protein and peptide molecular weight markers. Precipitation with pyrogallol red-molybdate (PRM) gives better and more uniform recovery of both proteins and peptides as compared to TCA. The lower limit of PRM precipitation is similar to TCA and corresponds to 1 microgram protein per mL assay mixture. This is equivalent to 100 microL of 10 micrograms/mL protein using the standard protein assay or 1 microgram/mL protein using a modified assay incorporating a fivefold concentrate of the dye reagent. Application of the method is demonstrated by concentration of urinary proteins. The method is simple and economic and useful for conserving trace amounts of precious sample as it allows recovery of protein for electrophoresis following protein assay.

  6. Mechanisms by which acid precipitation produces embryonic death in aquatic vertebrates. Technical completion report, 1 May 1977-31 December 1980

    SciTech Connect

    Pough, F.H.

    1981-03-01

    Fourteen species of amphibians show a general similarity in their tolerance of acid media during embryonic development. More than 85% mortality is produced by pHs of 3.7 to 3.9 and more than 50% mortality occurs at pHs of 4.0 or less. Similar values have been reported for fishes. The sensitivity of amphibian embryos to acidity is greater in late stages of their development than it is during the initial cleavage of the embryos. The teratogenic effects of acidity appear to be the result of damage to the superficial tissues of the embryo. A similar response occurs in fish embryos. Because of the similarity of sensitivity and response to acidity of fishes and amphibians, the latter animals are suitable experimental models for investigations of the details of acid resistance. Controlled breedings of African clawed frogs (Xenopus laevis) indicated that the offspring of some pairs of parents were more resistant to acidity than those of other pairs. Wild populations of spotted salamanders (Ambystoma maculatum) breeding in some ponds in the Ithaca, New York, region have probably been exposed to increasingly acid conditions for the past three decades (10 or more generations). In the most acid ponds more than 70% of the embryos die before hatching. Despite the intensity and duration of this selection, it was not possible to demonstrate any difference in sensitivity to acidity between eggs collected from acidic and neutral breeding sites.

  7. Oxalic-acid leaching of rock, soil, and stream-sediment samples as an anomaly-accentuated technique

    USGS Publications Warehouse

    Alminas, Henry V.; Mosier, Elwin L.

    1976-01-01

    In many instances total-rock and sieved-soil and stream-sediment samples lack the sensitivity and contrast required for reconnaissance exploration and necessary in the search for blind ore deposits. Heavy-mineral concentrates incorporate the required sensitivity and contrast but are overly expensive for two reasons: time-consuming sample preparation is required to obtain them, and they cannot be easily derived from all bulk-sample types. Trace-metal-content comparisons of the oxalic-acid-leachable portions with heavy-mineral concentrates show that the leachates are equal to the heavy-mineral concentrates in sensitivity and contrast. Simplicity of preparation and the resultant cost savings are additional advantages of this proposed method.

  8. Two-stage sample-to-answer system based on nucleic acid amplification approach for detection of malaria parasites.

    PubMed

    Liu, Qing; Nam, Jeonghun; Kim, Sangho; Lim, Chwee Teck; Park, Mi Kyoung; Shin, Yong

    2016-08-15

    Rapid, early, and accurate diagnosis of malaria is essential for effective disease management and surveillance, and can reduce morbidity and mortality associated with the disease. Although significant advances have been achieved for the diagnosis of malaria, these technologies are still far from ideal, being time consuming, complex and poorly sensitive as well as requiring separate assays for sample processing and detection. Therefore, the development of a fast and sensitive method that can integrate sample processing with detection of malarial infection is desirable. Here, we report a two-stage sample-to-answer system based on nucleic acid amplification approach for detection of malaria parasites. It combines the Dimethyl adipimidate (DMA)/Thin film Sample processing (DTS) technique as a first stage and the Mach-Zehnder Interferometer-Isothermal solid-phase DNA Amplification (MZI-IDA) sensing technique as a second stage. The system can extract DNA from malarial parasites using DTS technique in a closed system, not only reducing sample loss and contamination, but also facilitating the multiplexed malarial DNA detection using the fast and accurate MZI-IDA technique. Here, we demonstrated that this system can deliver results within 60min (including sample processing, amplification and detection) with high sensitivity (<1 parasite μL(-1)) in a label-free and real-time manner. The developed system would be of great potential for better diagnosis of malaria in low-resource settings.

  9. Precipitation of a poorly soluble model drug during in vitro lipolysis: characterization and dissolution of the precipitate.

    PubMed

    Sassene, Philip J; Knopp, Matthias M; Hesselkilde, Janne Z; Koradia, Vishal; Larsen, Anne; Rades, Thomas; Müllertz, Anette

    2010-12-01

    Precipitation of cinnarizine during in vitro lipolysis of a self-microemulsifying drug delivery system (SMEDDS) was characterized to gain a better understanding of the mechanisms behind the precipitation. During in vitro lipolysis of the SMEDDS with or without cinnarizine, samples were taken at several timepoints and ultracentrifuged. Cinnarizine content in the pellet increased from 4% to 59% during lipolysis. The precipitation of cinnarizine during in vitro lipolysis correlated well with the degree of lipid digestion, determined by sodium hydroxide addition. The pellet from the endpoint of lipolysis was isolated and subjected to dissolution in biorelevant media. Dissolution rate of cinnarizine from pellets containing precipitated cinnarizine was initially 10-fold higher than dissolution from blank pellet spiked with crystalline cinnarizine, reaching more than 50% drug dissolved in the first minute. Pellets were further characterized by X-ray powder diffraction (XRPD) and polarized light microscopy (PLM). Both methods indicated the presence of liquid crystalline phases of calcium fatty acid soaps, but no presence of crystalline cinnarizine in the pellet. Overall, dissolution studies along with XRPD and PLM analysis indicate that cinnarizine precipitating during in vitro lipolysis of this SMEDDS is not crystalline, suggesting an either amorphous form or a molecular dispersion.

  10. Omega 3 and omega 6 fatty acids intake and dietary sources in a representative sample of Spanish adults.

    PubMed

    González-Rodríguez, Liliana G; Aparicio, Aránzazu; López-Sobaler, Ana M; Ortega, Rosa M

    2013-01-01

    The present study analyzes the intake of omega 3 (n-3 PUFAs) and omega 6 (n-6 PUFAs) and dietary sources in a representative sample of Spanish adults. For this purpose 418 adults (18 - 60 y), from 15 Spanish provinces were studied. The intake of energy and nutrients [specifically, the n-3 polyunsaturated fatty acids (PUFAs,) α-linolenic acid (ALA), eicosapentaenoic acid (EPA), docosahexaenoic acid (DHA); and the n-6 PUFA, linoleic acid (LA)] was determined using a 24-hour recall questionnaire for two days. The Multiple Source Method (MSM) was used to estimate participants’ usual fatty acid intake. The total n-3 PUFAs intake was 1.8 ± 0.60 g/day (ALA: 1.3 ± 0.32, EPA: 0.16 ± 0.14, and DHA: 0.33 ± 0.21 g/day) and n-6 PUFA intake was 11.0 ± 2.7 g/day (LA: 10.8 ± 2.7 g/day). A high proportion of participants did not meet their nutrient intake goals for total n-3 PUFAs (84.7 %), ALA (45.0 %), and EPA plus DHA (62.9 %). The main food sources for ALA were oil, dairy products, and meat; for EPA fish; for DHA, fish, eggs, and meat; and for LA, oils, meat, and cereals. Therefore, an increase in the intake of foods rich in n-3 PUFAs or the use of supplements with n-3 PUFAs might help to improve the n-3 PUFA intake.

  11. Influence of UV Light on Phenolic Acid Content of Broccoli Samples (Brassica oleracea)

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Influence of environmental factors (such as rainfall, pests, soil, irrigation levels, and fertilization) on the phenolic composition of fruits and vegetables is well documented in the literature. We have evaluated the significance of ultraviolet light on the phenolic composition of broccoli samples....

  12. HYDROLYSIS OF MTBE TO TBA IN GROUND WATER SAMPLES WITH HYDROCHLORIC ACID

    EPA Science Inventory

    Conventional sampling and analytical protocols have poor sensitivity for fuel oxygenates that are alcohols, such as tert-butyl alcohol (TBA). Because alcohols are miscible or highly soluble in water, alcohols are not efficiently transferred to the gas chromatograph for analysis....

  13. Comparison of hot hydroxylamine hydrochloride and oxalic acid leaching of stream sediment and coated rock samples as anomaly enhancement techniques

    USGS Publications Warehouse

    Filipek, L.H.; Chao, T.T.; Theobald, P.K.

    1982-01-01

    A hot hydroxylamine hydrochloride (H-Hxl) extraction in 25% acetic acid is compared with the commonly used oxalic acid extraction as a method of anomaly enhancement for Cu and Zn in samples from two very different metal deposits and climatic environments. Results obtained on minus-80-mesh stream sediments from an area near the Magruder massive sulfide deposit in Lincoln County, Georgia, where the climate is humid subtropical, indicate that H-Hxl enhances the anomaly for Cu by a factor of 2 and for Zn by a factor of 1.5, compared to the oxalic method. Analyses of Fe oxide-coated rock samples from outcrops overlying the North Silver Bell porphyry copper deposit near Tucson, Arizona, where the climate is semi-arid to arid, indicate that both techniques effectively outline the zones of hydrothermal alteration. The H-Hxl extraction can also perform well in high-carbonate or high-clay environments, where other workers have suggested that oxalic acid is not very effective. Therefore, the H-Hxl method is recommended for general exploration use. ?? 1982.

  14. Conformational analysis of short polar side-chain amino-acids through umbrella sampling and DFT calculations.

    PubMed

    Ramos, Javier; Cruz, Victor L

    2016-11-01

    Molecular and quantum mechanics calculations were carried out in a series of tripeptides (GXG, where X = D, N and C) as models of the unfolded states of proteins. The selected central amino acids, especially aspartic acid (D) and asparagine (N) are known to present significant average conformations in partially allowed areas of the Ramachandran plot, which have been suggested to be important in unfolded protein regions. In this report, we present the calculation of the propensity values through an umbrella sampling procedure in combination with the calculation of the NMR J-coupling constants obtained by a DFT model. The experimental NMR observations can be reasonably explained in terms of a conformational distribution where PPII and β basins sum up propensities above 0.9. The conformational analysis of the side chain dihedral angle (χ1), along with the computation of (3)J(H(α)H(β)), revealed a preference for the g - and g + rotamers. These may be connected with the presence of intermolecular H-bonding and carbonyl-carbonyl interactions sampled in the PPII and β basins. Taking into account all those results, it can be established that these residues show a similar behavior to other amino acids in short peptides regarding backbone φ,ψ dihedral angle distribution, in agreement with some experimental analysis of capped dipeptides.

  15. An analytical method for the measurement of trace level acidic and basic AMC using liquid-free sample traps

    NASA Astrophysics Data System (ADS)

    Moulton, Tyler M.; Zaloga, Emily C.; Chase, Katherine M.; Lobert, Jürgen M.

    2014-04-01

    The measurement of parts-per-trillion (ppt) level acidic and basic airborne molecular contamination (AMC) is essential for process protection and yield control in semiconductor photo-lithography and adjacent applications. Real-time monitoring solutions are highly desired, as they provide instantaneous and continuous measurement. However, even the most advanced monitors cannot achieve detection limits in the low parts-per-trillion (ppt) range and many restrictions apply for the detection of acidic AMC. High cost of ownership is another disadvantage. Discontinuous sampling with sample traps is capable of achieving ppt-level measurement, but the currently accepted methods use sample traps filled with de-ionized water (impingers) to capture soluble acidic and basic AMC. Several inherent disadvantages of these methods result in inconsistent data and increased detection limits. Some proprietary solid state solutions have been reported, but involve complex preparation, have high background signals and require 24-72 hour sample duration, or they are protected trade secrets that are not available as an industry standard. To eliminate these disadvantages, we developed a liquid-free sample trap that allows parts-per-quadrillion level (ppq) measurement of acidic and basic AMC within one work shift, typically a 4-6 hour sample period. The traps can easily be manufactured and prepared in small lab operations, are sealed and protected from the outside and operator handling in the field, have months of shelf life and show high capture efficiencies while minimizing reactions and artifacts. Capacity results for the liquid-free base trap using ammonia (NH3) as a test gas yielded more than 200 ppb-h at 100% capture efficiency without any moisture (simulating sampling of CDA or N2) and 350 ppb-h at 40% RH. The capacity results for sulfur dioxide (SO2) were highly dependent on moisture content of the sample gas and yielded 5 ppb-h at 90% capture efficiency and 0% RH, but increased

  16. Improved consistency in DNPH-mediated pyruvic acid analysis of onion juice by modifying the sample processing order.

    PubMed

    Yoo, Kil Sun; Lee, Eun Jin; Patil, Bhimanagouda S

    2011-01-01

    Onion pungency is commonly measured on absorbency of the wine pink color that results from adding NaOH to the heated mixture of dinitrophenylhydrazine (DNPH) and onion juice. However, significant variation exists among several modifications of the original Schwimmer and Weston (SW) method. We observed differences in pyruvic acid concentrations of 20%-30% between our automated method and a batch method with manual absorbency readings. To determine the source of the differences, we examined the heating time and waiting time of the sample-DNPH mixtures and found no differences. The differences were caused by differential color degradation between the pyruvic acid standards and onion juice samples. These differences could be minimized by reading the absorbency within 1 min of NaOH addition. Using this information, we devised the one-by-one method to control the reading time at 30 s. We compared 5 different analysis methods of 40 onion samples representing 4 onion colors. The automated, high-performance liquid chromatography, and SW methods had similar results, with only about a 5% difference. However, the batch method resulted in differences of approximately 24% as compared to the automated method. The one-by-one method produced very comparable results, within 5%, to the automated method. By modifying the procedure to ensure a uniform and fast reading time, we increased the consistency between the pungency analysis methods. Therefore, fast and uniform absorbency reading time is essential for an accurate measurement of pungency in undiluted onion juice.

  17. Routine sample preparation and HPLC analysis for ascorbic acid (vitamin C) determination in wheat plants and Arabidopsis leaf tissues.

    PubMed

    Szalai, Gabriella; Janda, T; Pál, Magda

    2014-06-01

    Plants have developed various mechanisms to protect themselves against oxidative stress. One of the most important non-enzymatic antioxidants is ascorbic acid. There is thus a need for a rapid, sensitive method for the analysis of the reduced and oxidised forms of ascorbic acid in crop plants. In this paper a simple, economic, selective, precise and stable HPLC method is presented for the detection of ascorbate in plant tissue. The sensitivity, the short retention time and the simple isocratic elution mean that the method is suitable for the routine quantification of ascorbate in a high daily sample number. The method has been found to be better than previously reported methods, because of the use of an economical, readily available mobile phase, UV detection and the lack of complicated extraction procedures. The method has been tested on Arabidopsis plants with different ascorbate levels and on wheat plants during Cd stress.

  18. Electrochemical determination of hydrochlorothiazide and folic acid in real samples using a modified graphene oxide sheet paste electrode.

    PubMed

    Beitollahi, Hadi; Hamzavi, Mozhdeh; Torkzadeh-Mahani, Masoud

    2015-01-01

    A new ferrocene-derivative compound, 2-chlorobenzoyl ferrocene, was synthesized and used to construct a modified graphene oxide sheet paste electrode. The electrooxidation of hydrochlorothiazide at the surface of the modified electrode was studied. Under optimized conditions, the square wave voltammetric (SWV) peak current of hydrochlorothiazide increased linearly with hydrochlorothiazide concentration in the range of 5.0 × 10(-8) to 2.0 × 10(-4) M and a detection limit of 20.0 nM was obtained for hydrochlorothiazide. The diffusion coefficient and kinetic parameters (such as electron transfer coefficient and the heterogeneous rate constant) for hydrochlorothiazide oxidation were also determined. The prepared modified electrode exhibits a very good resolution between the voltammetric peaks of hydrochlorothiazide and folic acid which makes it suitable for the detection of hydrochlorothiazide in the presence of folic acid in real samples.

  19. Relation of precipitation quality to storm type, and deposition of dissolved chemical constituents from precipitation in Massachusetts, 1983-85

    USGS Publications Warehouse

    Gay, F.B.; Melching, C.S.

    1995-01-01

    Precipitation samples were collected for 83 storms at a rural inland site in Princeton, Mass., and 73 storms at a rural coastal site in Truro, Mass., to examine the quality of precipitation from storms and relate quality to three storm types (oceanic cyclone, continental cyclone, and cold front). At the inland site, Princeton, ranked-means of precipitation depth, storm duration, specific conductance, and concentrations and loads of hydrogen, sulfate, aluminum, bromide, and copper ions were affected by storm type. At the coastal site, Truro, ranked means of precipitation depth, storm duration, and concentrations and loads of calcium, chloride, magnesium, potassium, and sodium ions were affected by storm type. Precipitation chemistry at the coastal site was 85 percent oceanic in orgin, whereas precipitation 72 kilometers inland was 60 percent hydrogen, nitrate, and sulfate ions, reflecting fossil-fuel combustion. Concentrations and loads for specific conductance and 9 chemical constituents on an annual and seasonal basis were determined from National Atmospheric Deposition Program data for spring 1983 through winter 1985 at Quabbin (rural, inland), Waltham (suburban, inland) and Truro (rural, coastal), Massachusetts. Concentrations of magnesium, potassium, sodium, and chloride concentrations were highest at the coast and much lower inland, with very little difference between Waltham and Quabbin. Loads of ammonium, nitrate, sulfate, and hydrogen are highest at Quabbin and are about equal at Waltham and Truro. About twice as much nitrate and hydrogen and about 35 percent more sulfate is deposited at Quabbin than at Waltham or Truro; this pattern indicates that the interior of Massachusetts receives more acidic precipitation than do the eastern or the coastal areas of Massachusetts.

  20. Rheological characterization of acid pectin samples in the absence and presence of monovalent ions.

    PubMed

    Ström, Anna; Schuster, Erich; Goh, Suk Meng

    2014-11-26

    Pectins are traditionally divided into two groups, high methoxy and low methoxy. The groupings determine the charge of the pectin and the gelation mechanism. However, not as yet extensively studied is the impact on gelation of the distribution of the charges as characterized by an absolute degree of blockiness (DBabs). The aim of this study was to characterize rheologically the acid gelation of a pectin with a high DBabs and a degree of methyl esterification of ∼ 37%, in the absence and presence of monovalent ions. The results obtained suggest that a pectin with a blocky charge distribution at pH conditions close to or below the pKa exhibits weak gel-like properties at intermediate frequencies, despite the absence of a permanent network structure. The addition of monovalent ions changed the rheological behavior to resemble that of a strong gel whose properties depended on the type and concentration of the ions.

  1. Perfluoroalkyl acids and their precursors in indoor air sampled in children's bedrooms.

    PubMed

    Winkens, Kerstin; Koponen, Jani; Schuster, Jasmin; Shoeib, Mahiba; Vestergren, Robin; Berger, Urs; Karvonen, Anne M; Pekkanen, Juha; Kiviranta, Hannu; Cousins, Ian T

    2017-03-01

    The contamination levels and patterns of perfluoroalkyl acids (PFAAs) and their precursors in indoor air of children's bedrooms in Finland, Northern Europe, were investigated. Our study is among the most comprehensive indoor air monitoring studies (n = 57) and to our knowledge the first one to analyse air in children's bedrooms for PFASs (17 PFAAs and 9 precursors, including two acrylates, 6:2 FTAC and 6:2 FTMAC). The most frequently detected compound was 8:2 fluorotelomer alcohol (8:2 FTOH) with the highest median concentration (3570 pg/m(3)). FTOH concentrations were generally similar to previous studies, indicating that in 2014/2015 the impact of the industrial transition had been minor on FTOH levels in indoor air. However, in contrast to earlier studies (with one exception), median concentrations of 6:2 FTOH were higher than 10:2 FTOH. The C8 PFAAs are still the most abundant acids, even though they have now been phased out by major manufacturers. The mean concentrations of FOSE/As, especially MeFOSE (89.9 pg/m(3)), were at least an order of magnitude lower compared to previous studies. Collectively the comparison of FTOHs, PFAAs and FOSE/FOSAs with previous studies indicates that indoor air levels of PFASs display a time lag to changes in production of several years. This is the first indoor air study investigating 6:2 FTMAC, which was frequently detected (58%) and displayed some of the highest maximum concentrations (13 000 pg/m(3)). There were several statistically significant correlations between particular house and room characteristics and PFAS concentrations, most interestingly higher EtFOSE air concentrations in rooms with plastic floors compared to wood or laminate.

  2. Electrocatalytic simultaneous determination of ascorbic acid, uric acid and L-Cysteine in real samples using quercetin silver nanoparticles-graphene nanosheets modified glassy carbon electrode

    NASA Astrophysics Data System (ADS)

    Zare, Hamid R.; Jahangiri-Dehaghani, Fahime; Shekari, Zahra; Benvidi, Ali

    2016-07-01

    By immobilizing of quercetin at the surface of a glassy carbon electrode modified with silver nanoparticles and graphene nanosheets (Q-AgNPs-GNs-GCE) a new sensor has been fabricated. The cyclic voltammogram of Q-AgNPs-GNs-GCE shows a stable redox couple with surface confined characteristics. Q-AgNPs-GNs-GCE demonstrated a high catalytic activity for L-Cysteine (L-Cys) oxidation. Results indicated that L-Cys peak potential at Q-AgNPs-GNs-GCE shifted to less positive values compared to GNs-GCE or AgNPs-GCE. Also, the kinetic parameters such as the electron transfer coefficient,, and the heterogeneous electron transfer rate constant, k‧, for the oxidation of L-Cys at the Q-AgNPs-GNs-GCE surface were estimated. In differential pulse voltammetric determination, the detection limit of L-Cys was obtained 0.28 μM, and the calibration plots were linear within two ranges of 0.9-12.4 μM and 12.4-538.5 μM of L-Cys. Also, the proposed modified electrode is used for the simultaneous determinations of ascorbic acid (AA), uric acid (UA), and L-Cys. Finally, this study has demonstrated the practical analytical utility of the sensor for determination of AA in vitamin C tablet, L-Cys in a milk sample and UA in a human urine sample.

  3. Spectrophotometric determination of copper(II) in pharmaceutical, biological and water samples by 4-(2'-benzothiazolylazo)-salicylic acid

    NASA Astrophysics Data System (ADS)

    Hashem, E. Y.; Seleim, M. M.; El-Zohry, A. M.

    2011-09-01

    A highly sensitive method is proposed to determine copper(II) ions by forming a stable complex through their interaction with 4-(2'-benzothiazolylazo)-salicylic acid (BTAS) at room temperature and pH of about 5.0. The complex gave a maximum absorption at λ = 485 nm with a molar absorptivity coefficient of 2.35·104 l/(mol·cm). The linear range for the copper determination is 0.63-5.04 mg/l. The method can be applied to determine copper ions in different biological specimens like some drugs and water samples.

  4. DNA recognition by peptide nucleic acid-modified PCFs: from models to real samples

    NASA Astrophysics Data System (ADS)

    Selleri, S.; Coscelli, E.; Poli, F.; Passaro, D.; Cucinotta, A.; Lantano, C.; Corradini, R.; Marchelli, R.

    2010-04-01

    The increased concern, emerged in the last few years, on food products safety has stimulated the research on new techniques for traceability of raw food materials. DNA analysis is one of the most powerful tools for the certification of food quality, and it is presently performed through the polymerase chain reaction technique. Photonic crystal fibers, due to the presence of an array of air holes running along their length, can be exploited for performing DNA recognition by derivatizing hole surfaces and checking hybridization of complementary nucledotide chains in the sample. In this paper the application of a suspended core photonic crystal fiber in the recognition of DNA sequences is discussed. The fiber is characterized in terms of electromagnetic properties by means of a full-vector modal solver based on the finite element method. Then, the performances of the fiber in the recognition of mall synthetic oligonucleotides are discussed, together with a test of the possibility to extend this recognition to samples of DNA of applicative interest, such as olive leaves.

  5. Precipitation Climate Data Records

    NASA Astrophysics Data System (ADS)

    Nelson, B. R.; Prat, O.; Vasquez, L.

    2015-12-01

    Five precipitation CDRs are now or soon will be transitioned to NOAA's CDR program. These include the PERSIANN data set, which is a 30-year record of daily adjusted global precipitation based on retrievals from satellite microwave data using artificial neural networks. The AMSU-A/B/Hydrobundle is an 11-year record of precipitable water, cloud water, ice water, and other variables. CMORPH (the NOAA Climate Prediction Center Morphing Technique) is a 17-year record of daily and sub-daily adjusted global precipitation measured from passive microwave and infrared data at high spatial and temporal resolution. GPCP (the Global Precipitation Climatology Project) is an approximately 30-year record of monthly and pentad adjusted global precipitation and a 17-year record of daily adjusted global precipitation. The NEXRAD Reanalysis is a 10-year record of high resolution NEXRAD radar based adjusted CONUS-wide hourly and daily precipitation. This study provides an assessment of the existing and transitioned long term precipitation CDRs and includes the verification of the five precipitation CDRs using various methods including comparison with in-situ data sets and trend analysis. As all of the precipitation related CDRs are transitioned, long term analyses can be performed. Comparisons at varying scales (hourly, daily and longer) of the precipitation CDRs with in-situ data sets are provided as well as a first look at what could be an ensemble long term precipitation data record.

  6. Ethanol contamination leads to Fatty acid ethyl esters in hair samples.

    PubMed

    De Giovanni, Nadia; Donadio, Giuseppe; Chiarotti, Marcello

    2008-03-01

    The diagnosis of alcoholism is a topical subject of discussion; in fact, many studies have been published on the determination of biochemical markers useful to this target. Fatty acid ethyl esters (FAEE) are minor metabolites of ethanol, and their usefulness has been demonstrated by their detection in hair using a headspace solid-phase microextraction-gas chromatographic-mass spectrometric technique. Environmental contamination in the analysis of drugs of abuse is a well-known focus of discussion between scientists. In the same way, interference from the surroundings could be hypothesized in FAEE detection. To assess the influence of ethanol contamination, an in vitro experiment was performed, leaving hair in an atmosphere saturated with ethanol vapors for 15 days. The spontaneous production of FAEE was demonstrated by analyzing hair day by day. In fact, we observed a constant increase of ethyl myristate, palmitate, and stearate that reached very high concentrations at the end of the investigation. Although the experiment was managed in a stressed way and could not represent real life, its purpose was to focus the attention of researchers on the problem of hair contamination that can occur, for example, with ethanol-containing cosmetics. Therefore, care in interpretation must be taken into account, especially with such a volatile molecule.

  7. Label-free imaging of fatty acid content within yeast samples

    NASA Astrophysics Data System (ADS)

    Garrett, N.; Moger, J.

    2013-02-01

    Fungi have been found to be an underlying cause of 70% of all plant and animal extinctions caused by infectious diseases. Fungal infections are a growing problem affecting global health, food production and ecosystems. Lipid metabolism is a promising target for antifungal drugs and since effective treatment of fungal infections requires a better understanding of the effects of antifungal agents at the cellular level, new techniques are needed to investigate this problem. Recent advances in nonlinear microscopy allow chemically-specific contrast to be obtained non-invasively from intrinsic chemical bonds within live samples using advanced spectroscopy techniques probing Raman-active resonances. We present preliminary data using Stimulated Raman Scattering (SRS) microscopy as a means to visualise lipid droplets within individual living fungi by probing Raman resonances of the CH stretching region between 2825cm-1 and 3030cm-1.

  8. Acid precipitation: effects on fresh-water ecosystems. January 1978-September 1988 (Citations from the Life Sciences Collection data base). Report for January 1978-September 1988

    SciTech Connect

    Not Available

    1988-10-01

    This bibliography contains citations concerning the effects of acidification of fresh-water ecosystems. Algae and diatom distribution, survival, and reproduction rates of specific fish species under acid-lake conditions, and tolerance to stress caused by acidic conditions in fresh water ecosystems are studied. Effects of water ph on trace metal toxicity to fresh water organisms is briefly considered. Control and reduction of acidification is excluded from this bibliography. (Contains 290 citations fully indexed and including a title list.)

  9. Auroral helium precipitation.

    NASA Technical Reports Server (NTRS)

    Axford, W. I.; Chivers, H. J. A.; Eberhardt, P.; Geiss, J.; Buehler, F.

    1972-01-01

    Application of the metal foil sampling technique, which has been used to measure helium, neon, and argon fluxes in the solar wind, to the problem of measuring the fluxes of these gases in the auroral primary radiation. Aluminum and platinum foils have been flown into two bright auroras and have been recovered. The foils have been analyzed for helium and neon isotopes with a mass spectrometer; so far only He4 has been detected. In the first flight the precipitating flux of He4 with particle energies above about 1 keV was approximately 1,000,000 per sq cm per sec, and the backscattered flux was smaller by about a factor of 10. In the second flight the aurora was less bright, and the He4 fluxes were lower by a factor of about 2. A rough analysis suggests that the mean energy of the incident particles was greater than 3 keV.

  10. Rapid determination of total polyphenolic content in tea samples based on caffeic acid voltammetric behaviour on a disposable graphite electrode.

    PubMed

    David, Iulia Gabriela; Bizgan, Ana-Maria Cristina; Popa, Dana Elena; Buleandra, Mihaela; Moldovan, Zenovia; Badea, Irinel Adriana; Tekiner, Tuğçe Ayça; Basaga, Huveyda; Ciucu, Anton A

    2015-04-15

    The present paper describes the voltammetric behaviour and the quantitative determination of caffeic acid (CA) on a disposable pencil graphite electrode (PGE). The anodic peak current of CA recorded by differential pulse voltammetry (DPV) varies linearly with CA concentration in the range 1×10(-7)-3×10(-3) M. The detection and quantification limits were 8.83×10(-8) M and 2.94×10(-7) M caffeic acid, respectively. The mean recoveries of CA from Turkish green, white and black teas were 98.30%, 99.57% and 91.46%. For these three tea types the corresponding total polyphenolic contents (TPCs) evaluated by DPV on PGE were 35.81, 34.59 and 31.21 mg caffeic acid equivalent/g tea, respectively. These TPC values were in good accordance with those obtained by the Folin-Ciocalteu method. The developed DPV on PGE method constitutes a simple and inexpensive tool for the rapid assessment of TPC of tea samples.

  11. A Fully Integrated Paperfluidic Molecular Diagnostic Chip for the Extraction, Amplification, and Detection of Nucleic Acids from Clinical Samples

    PubMed Central

    Rodriguez, Natalia M.; Wong, Winnie S.; Liu, Lena; Dewar, Rajan; Klapperich, Catherine M.

    2016-01-01

    Paper diagnostics have successfully been employed to detect the presence of antigens or small molecules in clinical samples through immunoassays; however, the detection of many disease targets relies on the much higher sensitivity and specificity achieved via nucleic acid amplification tests (NAAT). The steps involved in NAAT have recently begun to be explored in paper matrices, and our group, among others, has reported on paper-based extraction, amplification, and detection of DNA and RNA targets. Here, we integrate these paper-based NAAT steps onto a single paperfluidic chip in a modular, foldable system that allows for fully integrated fluidic handling from sample to result. We showcase the functionality of the chip by combining nucleic acid isolation, isothermal amplification, and lateral flow detection of human papillomavirus (HPV) 16 DNA directly from crude cervical specimens in under 1 hour for rapid, early detection of cervical cancer. The chip is made entirely of paper and adhesive sheets, making it low-cost, portable, and disposable, and offering the potential for a point-of-care molecular diagnostic platform even in remote and resource-limited settings. PMID:26785636

  12. Flow-Injection Determination of Thiabendazole Fungicide in Water Samples Using a Diperiodatocuprate(III)-Sulfuric Acid-Chemiluminescence System.

    PubMed

    Asghar, Mohammad; Yaqoob, Mohammad; Munawar, Nusrat; Nabi, Abdul

    2016-01-01

    Chemiluminescence (CL) with a flow-injection method is reported for the determination of thiabendazole (TBZ) fungicide based on its enhancement effect on diperiodatocuprate(III) (DPC)-sulfuric acid-CL system. The calibration graph was linear in the concentration range of 1 - 2000 μg L(-1) (R(2) = 0.9999, n = 8) with a limit of detection (S/N = 3) of 0.3 μg L(-1). The injection throughput was 160 h(-1) with relative standard deviations (RSD, n = 4) of 1.1 - 2.9% in the concentration range studied. The experimental variables e.g., reagents concentrations, flow rates, sample volume, and PMT voltage were optimized, and the potential interferences were investigated individually. The method was successfully applied to the determination of TBZ in water samples showing good agreement and recovery in the range of 92 ± 2.2 - 108 ± 3% (n = 3) using dispersive liquid-liquid micro-extraction (DLLME). The possible CL reaction mechanism for DPC-sulfuric acid-TBZ is also discussed.

  13. Application of a nanostructured platform and imprinted sol-gel film for determination of chlorogenic acid in food samples.

    PubMed

    Ribeiro, Carla M; Miguel, Eliane M; Silva, Jonadab Dos S; Silva, Cristian B da; Goulart, Marília O F; Kubota, Lauro T; Gonzaga, Fabiano B; Santos, Wilney J R; Lima, Phabyanno R

    2016-08-15

    Chlorogenic acid (CGA) is a polyphenol derivative that widely exists in higher plants like fruits, vegetables, black teas, and some traditional Chinese medicines. In this work, we have proposed a sensitive and selective electrochemical sensor for detection of CGA. The sensor was based on a glassy carbon electrode (GCE) modified with a functional platform by grafting vinyltrimethoxysilane (VTMS) in multi-walled carbon nanotubes (MWCNTs) and covered by a molecularly imprinted siloxane (MIS) film prepared using the sol-gel process. The VTMS was grafted onto the surface of the MWCNTs via in situ free radical polymerization. The MIS was obtained from the acid-catalyzed hydrolysis/condensation of a solution consisting of tetraethoxysilane (TEOS), phenyltriethoxysilane (PTEOS), (3-aminopropyl)trimethoxysilane (APTMS), and CGA as a template molecule. The modification procedure was evaluated by differential pulse voltammetry (DPV) and scanning electron microscopy (SEM). Under optimized operational conditions, a linear response was obtained covering a concentration ranging from 0.08μmolL(-1) to 500μmolL(-1) with a detection limit (LOD) of 0.032μmolL(-1). The proposed sensor was applied to CGA determination in coffee, tomato, and apple samples with recoveries ranging from 99.3% to 108.6%, showing a promising potential application in food samples. Additionally, the imprinted sensor showed a significantly higher affinity for target CGA than the non-imprinted siloxane (NIS) sensor.

  14. Retrospective bioindication of stratospheric ozone and ultraviolet radiation using hydroxycinnamic acid derivatives of herbarium samples of an aquatic liverwort.

    PubMed

    Otero, Saúl; Núñez-Olivera, Encarnación; Martínez-Abaigar, Javier; Tomás, Rafael; Huttunen, Satu

    2009-01-01

    We analyzed bulk UV absorbance of methanolic extracts and levels of five UV-absorbing compounds (hydroxycinnamic acid derivatives) in 135 herbarium samples of the liverwort Jungermannia exsertifolia subsp. cordifolia from northern Europe. Samples had been collected in 1850-2006 (96% in June-August). Both UV absorbance and compound levels were correlated positively with collection year. p-Coumaroylmalic acid (C1) was the only compound showing a significant (and negative) correlation with stratospheric ozone and UV irradiance in the period that real data of these variables existed. Stratospheric ozone reconstruction (1850-2006) based on C1 showed higher values in June than in July and August, which coincides with the normal monthly variation of ozone. Combining all the data, there was no long-term temporal trend from 1850 to 2006. Reconstructed UV showed higher values in June-July than in August, but again no temporal trend was detected in 1918-2006 using the joint data. This agrees with previous UV reconstructions.

  15. Correlations of beta-aminoisobutyric acid in 8 hour and 24 hour urinary samples determined by dual column gas chromatography.

    PubMed

    Sjölin, K E; Nyholm, K K

    1980-05-01

    The correlations of beta-aminoisobutyric acid values in 8 hour and 24 hour urinary samples from 23 healthy persons were determined. beta-AIB in the 8 hour urinary samples was measured by gas chromatography and the 24 hour excretion was calculated from the results of three 8 hour determinations. Simultaneous determinations of urinary creatinine were performed by Jaffe's reaction. Based on the 8 hour values of urinary beta-AIB the results demonstrated a constant excretion of beta-aminoisobutyric acid within the 24 hour periods in both low and high excretors. The precision in distinguishing low and high 24 hour excretors of beta-AIB by using 8 hour values was 91%. If 8 hour values of beta-AIB were related to creatinine the same precision for this calculated ratio was 96.5%. However, for high excretors of beta-AIB, failures were 24.5% by using the 8 hour excretion of beta-AIB as indicator, but only 6.5% by using the ratio.

  16. Immunoaffinity centrifugal precipitation chromatography.

    PubMed

    Qi, Lin; Ito, Yoichiro

    2007-06-01

    Purification of proteins based on immunoaffinity has been performed using a solid support coated with antibody against the target proteins. The method requires immobilizing the antibody onto the solid support using protein A or G, and has a risk of adsorptive loss of target proteins onto the solid support. Centrifugal precipitation chromatography has been successfully used to purify enzymes, such as ketosteroid isomerase and hyaluronidase without the use of solid support. The purpose of this study is to demonstrate that immunoaffinity centrifugal precipitation chromatography is capable of isolating an antigen by exploiting antigen-antibody binding. The separation was initiated by filling both channels with 40% saturated ammonium sulfate (AS) of pH 4-4.5 followed by loading 20 microl of human plasma (National Institutes of Health blood bank) mixed with 2 mg of rabbit anti-HSA (human serum protein) antibody (Sigma). Then, the sample channel was eluted with water at 0.03 ml/min and AS channel with 40% AS solution of pH 4-4.5 at 1 ml/min until all non-binding components were eluted. Then, the releasing reagent (50% AS solution containing 0.5 M glycine and 10% ammonium hydroxide at pH 10) was introduced through the AS channel to release the target protein (HSA). The retained antibody was recovered by eluting the sample channel with water at 1 ml/min. A hollow fiber membrane device at the outlet (MicroKros, Spectrum, New Brunswick, NJ, USA) was provided on-line dialysis of the eluent before fractions were collected, so that the fractions could be analyzed by SDS-PAGE (sodium dodecyl sulfate - polyacrylamide gel electrophoresis) without further dialysis. The current method does not require immobilizing the antibody onto a matrix, which is used by the conventional immunoaffinity chromatography. This method ensures full recovery of the antigen and antibody, and it may be applied to purification of other proteins.

  17. Global Precipitation Measurement (GPM) Mission Development Status

    NASA Technical Reports Server (NTRS)

    Azarbarzin, Ardeshir Art

    2011-01-01

    Mission Objective: (1) Improve scientific understanding of the global water cycle and fresh water availability (2) Improve the accuracy of precipitation forecasts (3) Provide frequent and complete sampling of the Earth s precipitation Mission Description (Class B, Category I): (1) Constellation of spacecraft provide global precipitation measurement coverage (2) NASA/JAXA Core spacecraft: Provides a microwave radiometer (GMI) and dual-frequency precipitation radar (DPR) to cross-calibrate entire constellation (3) 65 deg inclination, 400 km altitude (4) Launch July 2013 on HII-A (5) 3 year mission (5 year propellant) (6) Partner constellation spacecraft.

  18. As, Cd, Cr, Ni and Pb pressurized liquid extraction with acetic acid from marine sediment and soil samples

    NASA Astrophysics Data System (ADS)

    Moreda-Piñeiro, Jorge; Alonso-Rodríguez, Elia; López-Mahía, Purificación; Muniategui-Lorenzo, Soledad; Prada-Rodríguez, Darío; Moreda-Piñeiro, Antonio; Bermejo-Barrera, Adela; Bermejo-Barrera, Pilar

    2006-12-01

    Rapid leaching procedures by Pressurized Liquid Extraction (PLE) have been developed for As, Cd, Cr, Ni and Pb leaching from environmental matrices (marine sediment and soil samples). The Pressurized Liquid Extraction is completed after 16 min. The released elements by acetic acid Pressurized Liquid Extraction have been evaluated by inductively coupled plasma-optical emission spectrometry. The optimum multi-element leaching conditions when using 5.0 ml stainless steel extraction cells, were: acetic acid concentration 8.0 M, extraction temperature 100 °C, pressure 1500 psi, static time 5 min, flush solvent 60%, two extraction steps and 0.50 g of diatomaceous earth as dispersing agent (diatomaceous earth mass/sample mass ratio of 2). Results have showed that high acetic acid concentrations and high extraction temperatures increase the metal leaching efficiency. Limits of detection (between 0.12 and 0.5 μg g - 1 ) and repeatability of the over-all procedure (around 6.0%) were assessed. Finally, accuracy was studied by analyzing PACS-2 (marine sediment), GBW-07409 (soil), IRANT-12-1-07 (cambisol soil) and IRANT-12-1-08 (luvisol soil) certified reference materials (CRMs). These certified reference materials offer certified concentrations ranges between 2.9 and 26.2 μg g - 1 for As, from 0.068 to 2.85 μg g - 1 for Cd, between 26.4 and 90.7 μg g - 1 for Cr, from 9.3 to 40.0 μg g - 1 for Ni and between 16.3 and 183.0 μg g - 1 for Pb. Recoveries after analysis were between 95.7 and 105.1% for As, 96.2% for Cd, 95.2 and 100.6% for Cr, 95.7 and 103% for Ni and 94.2 and 105.5% for Pb.