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Sample records for complex samples determination

  1. Cyclopentanone thiosemicarbazone, a new complexing agent for copper determination in biological samples by adsorptive stripping voltammetry.

    Science.gov (United States)

    Mahajan, Rakesh Kumar; Walia, T P S; Sumanjit; Lobana, T S

    2006-03-01

    A selective and sensitive stripping voltammetric method for the determination of trace amounts of copper(II) with cyclopentanone thiosemicarbazone (CPTSC) is presented. The method is based on the adsorptive accumulation of the resulting copper-CPTSC complex on a hanging mercury drop electrode, followed by the stripping voltammetric measurements at the reduction current of the adsorbed complex at -0.37 V vs. Ag/AgCl. The optimal conditions for the stripping analysis of copper include pH 9.3, deposition time of 120 s, and a deposition potential of -0.1 V (vs. Ag/AgCl). The peak current is linearly proportional to the copper concentration over a range 3.14 x 10(-9) M to 1.57 x 10(-6) M with a limit of detection of 1.57 x 10(-9) M. The technique has been applied to the determination of copper in biological samples, like urine and whole blood.

  2. Selective determination of total vanadium in water samples by cloud point extraction of its ternary complex

    Energy Technology Data Exchange (ETDEWEB)

    Filik, Hayati [Istanbul University, Faculty of Engineering, Department of Chemistry, Avcilar, 34320 Istanbul (Turkey)], E-mail: filik@istanbul.edu.tr; Yanaz, Zeynep; Apak, Resat [Istanbul University, Faculty of Engineering, Department of Chemistry, Avcilar, 34320 Istanbul (Turkey)

    2008-07-14

    A highly sensitive micelle-mediated extraction methodology for the preconcentration of trace levels of vanadium as a prior step to its determination by flame atomic absorption spectrometry (FAAS) has been developed. Vanadium was complexed with 1-(2-pyridylazo)-2-naphthol (PAN) and hydrogen peroxide in acidic medium (0.2 mol L{sup -1} phosphoric acid) using Triton X-100 as surfactant and quantitatively extracted into a small volume of the surfactant-rich phase after centrifugation. The color reaction of vanadium ions with hydrogen peroxide and PAN in phosphoric acid medium is highly selective. The chemical variables affecting cloud point extraction (CPE) were evaluated and optimized. The R.S.D. for 5 replicate determinations at the 20 {mu}g L{sup -1} V level was 3.6%. The calibration graph using the preconcentration system for vanadium was linear with a correlation coefficient of 0.99 at levels near the detection limits up to at least 0.6 {mu}g L{sup -1}. The method has good sensitivity and selectivity and was applied to the determination of trace amounts of vanadium in water samples with satisfactory result. The proposed method is a rare application of CPE-atomic spectrometry to vanadium assay, and is superior to most other similar methods, because its useful pH range is in the moderately acidic range achieved with phosphoric acid. At this pH, many potential interferents are not chelated with PAN, and iron(III) as the major interferent is bound in a stable phosphate complex.

  3. Eigenvalue Tests and Distributions for Small Sample Order Determination for Complex Wishart Matrices

    Science.gov (United States)

    1994-08-13

    zonal polynomials", Journal of Multivariate Analysis 14 336-347 (1984). [160] Serge Lang , Complex Analysis, 2 nd Edition, Springer-Verlag (1985). [161...independent if for any polynomial function _ aifigji = 0 with complex coefficients aij, we must have a0j = 0 for all i, j. This definition was taken from Lang

  4. Determination of organophosphorus pesticides in water samples by using a new sensitive luminescent probe of Eu (III) complex

    Energy Technology Data Exchange (ETDEWEB)

    Azab, Hassan A., E-mail: azab2@yahoo.com; Anwar, Z.M.; Rizk, M.A.; Khairy, Gasser M.; El-Asfoury, M.H.

    2015-01-15

    This work describes the application of fluorescence for investigating the interactions of Eu(III)-TAN-1,10 phenanthroline (where TAN=4,4,4-Trifluoro-1-(2-naphthyl)-1,3-butanedione) with pesticides Chlorpyrifos, Malathion, Endosulfan, Heptachlor. The complex was synthesized and characterized by elemental analysis, FTIR, x-ray spectroscopy, solid fluorescence and thermal analysis. The results indicated that the composition of this complex is [Eu(TAN){sub 2}(Phen)(H{sub 2}O){sub 2}]Cl. The luminescence properties of the complex in different solvents and at different pH values have been investigated. The results show that the complex exhibits more efficient luminescence at pH=7.5. The interactions of Eu-complex with different pesticides (Chlorpyrifos, Malathion, Endosulfan, and Heptachlor) in aqueous medium have been investigated by fluorescence measurements. The luminescence intensity of the probe is quenched by Malathion and enhanced by (Endosulfan, Heptachlor, and Chlorpyrifos). Direct methods for the determination of the pesticides under investigation have been developed using the luminescence variations of the probe in solution. The detection limits are 0.47, 1.02, 0.66, 0.64 µmol/L for Chlorpyrifos, Endosulfan, Heptachlor, and Malathion, respectively. The binding constants and thermodynamic parameters of the pesticides with probe were evaluated. The emission quantum yield (QY=0.71) of Eu(III)-complex was determined using tris (2,2'-bipyridyl) dichlororuthenium(II) hexahydrate. A thermodynamic analysis showed that the reaction is spontaneous with negative ΔG. Effect of some relevant interferents on the detection of pesticides has been investigated. The new method was applied to the determination of the pesticides in different types of water samples (tap, river, and waste water). - Highlights: • A new luminescent probe of Eu (III) complex has been developed for sensing some organophosphorus pesticides. • Four guest pesticides Chlorpyrifos, Malathion

  5. Simple and fast HPLC method for simultaneous determination of retinol, tocopherols, coenzyme Q(10) and carotenoids in complex samples.

    Science.gov (United States)

    Gleize, Béatrice; Steib, Marlène; André, Marc; Reboul, Emmanuelle

    2012-10-15

    The effects of fat-soluble vitamins (such as vitamins A and E) and lipid microconstituents (such as carotenoids) on human health are now well established. However, high-performance liquid chromatography (HPLC) methods able to detect these molecules in simultaneous runs are often difficult to set up. We report here a 35-min reversed-phase HPLC method using a single C30 column kept at 35°C with a gradient system of methanol, methyl-tert-butyl ether and water at a flow-rate of 1 mL/min. This method resolves 11 carotenoids, retinol, α- and γ-tocopherol from complex matrixes such as food samples, human plasma and human adipose tissue within 35 min. The method is also able to separate coenzyme Q(10). The intra-day and inter-day coefficients of variation are suitable for routine clinical and scientific applications for the determination of lipid micronutrients from various sample types.

  6. Rapid Isolation and Determination of Flavones in Biological Samples Using Zinc Complexation Coupled with High-Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Chenghe Sun

    2016-08-01

    Full Text Available Chlorophyll-type contaminants are commonly encountered in the isolation and determination of flavones of plant aerial plant parts. Heme is also a difficult background substance in whole blood analysis. Both chlorophyll and heme are porphyrin type compounds. In this study, a rapid method for isolating flavones with 5-hydroxyl or ortho-hydroxyl groups from biological samples was developed based on the different solubilities of porphyrin-metal and flavone-metal complexes. It is important that other background substances, e.g., proteins and lipids, are also removed from flavones without an additional processing. The recoveries of scutellarin, baicalin, baicalein, wogonoside and wogonin, which are the primary constituents of Scutellaria baicalensis (skullcaps were 99.65% ± 1.02%, 98.98% ± 0.73%, 99.65% ± 0.03%, 97.59% ± 0.09% and 95.19% ± 0.47%, respectively. As a sample pretreatment procedure, this method was coupled to high-performance liquid chromatography (HPLC with good separation, sensitivity and linearity and was applied to determine the flavone content in different aerial parts of S. baicalensis and in dried blood spot samples.

  7. Determination of aluminium in groundwater samples by GF-AAS, ICP-AES, ICP-MS and modelling of inorganic aluminium complexes.

    Science.gov (United States)

    Frankowski, Marcin; Zioła-Frankowska, Anetta; Kurzyca, Iwona; Novotný, Karel; Vaculovič, Tomas; Kanický, Viktor; Siepak, Marcin; Siepak, Jerzy

    2011-11-01

    The paper presents the results of aluminium determinations in ground water samples of the Miocene aquifer from the area of the city of Poznań (Poland). The determined aluminium content amounted from aluminium determinations were performed using three analytical techniques: graphite furnace atomic absorption spectrometry (GF-AAS), inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS). The results of aluminium determinations in groundwater samples for particular analytical techniques were compared. The results were used to identify the ascent of ground water from the Mesozoic aquifer to the Miocene aquifer in the area of the fault graben. Using the Mineql+ program, the modelling of the occurrence of aluminium and the following aluminium complexes: hydroxy, with fluorides and sulphates was performed. The paper presents the results of aluminium determinations in ground water using different analytical techniques as well as the chemical modelling in the Mineql+ program, which was performed for the first time and which enabled the identification of aluminium complexes in the investigated samples. The study confirms the occurrence of aluminium hydroxy complexes and aluminium fluoride complexes in the analysed groundwater samples. Despite the dominance of sulphates and organic matter in the sample, major participation of the complexes with these ligands was not stated based on the modelling.

  8. Determination of uranium and thorium in complex samples using chromatographic separation, ICP-MS and spectrophotometric detection.

    Science.gov (United States)

    Rozmarić, Martina; Ivsić, Astrid Gojmerac; Grahek, Zeljko

    2009-11-15

    The paper describes a research of possible application of UTEVA and TRU resins and anion exchanger AMBERLITE CG-400 in nitrate form for the isolation of uranium and thorium from natural samples. The results of determination of distribution coefficient have shown that uranium and thorium bind on TRU and UTEVA resins from the solutions of nitric and hydrochloric acids, and binding strength increases proportionally to increase the concentration of acids. Uranium and thorium bind rather strongly to TRU resin from the nitric acid in concentration ranging from 0.5 to 5 mol L(-1), while large quantities of other ions present in the sample do not influence on the binding strength. Due to the difference in binding strength in HCl and HNO(3) respectively, uranium and thorium can be easily separated from each other on the columns filled with TRU resin. Furthermore, thorium binds to anion exchanger in nitrate form from alcohol solutions of nitric acid very strongly, while uranium does not, so they can be easily separated. Based on these results, we have created the procedures of preconcentration and separation of uranium and thorium from the soil, drinking water and seawater samples by using TRU and UTEVA resins and strong base anion exchangers in nitrate form. In one of the procedures, uranium and thorium bind directly from the samples of drinking water and seawater on the column filled with TRU resin from 0.5 mol L(-1) HNO(3) in a water sample. After binding, thorium is separated from uranium with 0.5 mol L(-1) HCl, and uranium is eluted with deionised water. By applying the described procedure, it is possible to achieve the concentration factor of over 1000 for the column filled with 1g of resin and splashed with 2L of the sample. Spectrophotometric determination with Arsenazo III, with this concentration factor results in detection limits below 1 microg L(-1) for uranium and thorium. In the second procedure, uranium and thorium are isolated from the soil samples with TRU

  9. Spectrophotometric determination of Mercury (II by simultaneous micelle mediated extraction through ternary complex formation in water samples

    Directory of Open Access Journals (Sweden)

    Farzin Nekouei

    2014-06-01

    Full Text Available In this study, a micelle mediated extraction procedure for preconcentration of trace quantities of Hg(II as a prior step to its simultaneous spectrophotometric determination has been developed. The method is based on a ternary ion-association of Hg(II, Xylidyl Blue (XB and cationic surfactant (CTAB. Major factors affecting the efficiency of the method has been studied. The limit of detection (LOD under optimum conditions based on 3Sb was 4.65 ng mL-1. The proposed method has been applied for determination of trace amount of mercury in water samples with satisfactory results.

  10. Polymeric membrane sensors based on Cd(II) Schiff base complexes for selective iodide determination in environmental and medicinal samples.

    Science.gov (United States)

    Singh, Ashok Kumar; Mehtab, Sameena

    2008-01-15

    The two cadmium chelates of schiff bases, N,N'-bis(salicylidene)-1,4-diaminobutane, (Cd-S(1)) and N,N'-bis(salicylidene)-3,4-diaminotoluene (Cd-S(2)), have been synthesized and explored as ionophores for preparing PVC-based membrane sensors selective to iodide(I) ion. Potentiometric investigations indicate high affinity of these receptors for iodide ion. Polyvinyl chloride (PVC)-based membranes of Cd-S(1) and Cd-S(2) using as hexadecyltrimethylammonium bromide (HTAB) cation discriminator and o-nitrophenyloctyl ether (o-NPOE), dibutylphthalate (DBP), acetophenone (AP) and tributylphosphate (TBP) as plasticizing solvent mediators were prepared and investigated as iodide-selective sensors. The best performance was shown by the membrane of composition (w/w) of (Cd-S(1)) (7%):PVC (31%):DBP (60%):HTAB (2%). The sensor works well over a wide concentration range 5.3x10(-7) to 1.0x10(-2)M with Nernstian compliance (59.2mVdecade(-1) of activity) within pH range 2.5-9.0 with a response time of 11s and showed good selectivity for iodide ion over a number of anions. The sensor exhibits adequate life (3 months) with good reproducibility (S.D.+/-0.24mV) and could be used successfully for the determination of iodide content in environmental water samples and mouth wash samples.

  11. Spectrophotometric determination of platinum(IV) in alloys, complexes, environmental, and pharmaceutical samples using 4-[N,N-(diethyl)amino] benzaldehyde thiosemicarbazone.

    Science.gov (United States)

    Naik, P Parameshwara; Karthikeyan, J; Shetty, A Nityananda

    2010-12-01

    4-[N,N-(Diethyl)amino] benzaldehyde thiosemicarbazone (DEABT) is proposed as an analytical reagent for the spectrophotometric determination of platinum(IV). The DEABT forms 1:2 yellow complex with Pt(IV), which is sparingly soluble in water and completely soluble in water-ethanol-DMF medium. The Pt(IV)-DEABT complex shows maximum absorbance at 405 nm. Beer's law is valid up to 7.80 μg cm(-3), and optimum concentration range for the determination of platinum(IV) is 0.48-7.02 μg cm(-3). The molar absorptivity and Sandell's sensitivity of the method are found to be 1.755 × 10(4) dm(3) mol(-1) cm(-1) and 0.0012 μg cm(-2), respectively. The relative error and coefficient of variation (n=6) for the method does not exceed ± 0.43% and 0.35%, respectively. Since the method tolerates a number of metal ions commonly associated with platinum, it can be employed for the determination of platinum in environmental samples, pharmaceutical samples, alloys, catalysts, and complexes. The method is rapid as the Pt(IV)-DEABT complex is soluble in water-ethanol-DMF medium and not requiring any time consuming extraction method for the complex.

  12. Spectrophotometric determination of copper in environmental samples by solid-liquid extraction of its 9, 10-phenanthrenequinone monoximate complex into molten naphthalene

    Energy Technology Data Exchange (ETDEWEB)

    Wasey, A.; Puri, B.K.; Katyal, M.; Satake, M.

    1986-01-01

    A fairly selective and sensitive spectrophotometric method has been developed for determination of copper after extraction of its 9, 10-phenanthrenequinone monoximate complex into molten naphthalene in the pH range of 6.1-8.4. At room temperature, the solid naphthalene containing the metal complex is separated by filtration, dissolved in dimethylformamide (DMF) and the absorbance measured at 470 nm against the reagent blank. Beer's law is obeyed in the concentration range, 0.0-9.6 micrograms of copper in 10ml of DMF. The molar absorptivity and sensitivity are 6.30 X 10(4) 1 mol-1 cm-1 and 0.001 micrograms cm-2, respectively. The interference of various ions has been studied and the method has been applied for the determination of copper in various standard reference materials, beers, wines, human hair and environmental samples.

  13. Determination of uranium, iron, copper, and nickel from ore samples by MEKC using N,N'-ethylene bis(salicylaldimine) as complexing reagent.

    Science.gov (United States)

    Mirza, Muhammed Aslam; Khuhawar, Muhammad Yar; Arain, Rafee

    2008-02-01

    An analytical procedure has been developed for the separation of dioxouranium(VI), iron(III), copper(II), nickel(II), cobalt(II), cobalt(III), palladium(II), and thorium(IV) by MEKC using N,N'-ethylene bis(salicylaldimine) (H(2)SA(2)en) as a complexing reagent with total runtime ore samples indicating its presence within 103-1789 microg/g with RSD within 0.79-1.87%. Likewise copper, nickel, and iron in their combined matrix were also simultaneously determined with RSD 0.4-1.6% (n = 6).

  14. Determination of Some Trace Metals in Environmental Samples by Flame AAS Following Solid Phase Extraction with Amberlite XAD-2000 Resin after Complexing with 8-Hydroxyquinoline

    Institute of Scientific and Technical Information of China (English)

    DURAN Celal; SENTURK H.Basri; GUNDOGDU Ali; BULUT V.Numan; EICi Latif; SOYLAK Mustafa; TUFEKCI,Mehmet; UYGUR Yaprak

    2007-01-01

    A procedure for preconcentration of Mn(Ⅱ), Fe(Ⅱ), Co(Ⅱ), Cu(Ⅱ), Cd(Ⅱ), Zn(Ⅱ), Pb(Ⅱ) and Ni(Ⅱ) based on retention of their complexes with 8-hydroxyquinoline (HQ) on Amberlite XAD-2000 resin in a column was proposed for the analysis of environmental samples by flame AAS. Various parameters such as pH, eluent type, volume,concentration, flow rate and volume of sample solution, and matrix interference effect on the retention of the metal ions were investigated. The optimum pHs for the retention of metal complexes in question were about 6 except for Mn2+ for whose value is 8. The loading capacity of the adsorbent for these metals and their recoveries from the resin under the optimum conditions were in the range 6.82-9.26 mg·g-1 and 95%-101%, respectively. The enrichment factor was calculated as 100 and the limit of detection was in the range 0.3-2.2 μg·L 1 (n=20, blank+3s). The proposed enrichment method was applied to tap water, stream water and vegetable samples. The validation of the procedure was carried out by analysis of certified reference material and standard addition. The analytes were determined with a relative standard deviation lower than 6% in all samples.

  15. Sample size determination and power

    CERN Document Server

    Ryan, Thomas P, Jr

    2013-01-01

    THOMAS P. RYAN, PhD, teaches online advanced statistics courses for Northwestern University and The Institute for Statistics Education in sample size determination, design of experiments, engineering statistics, and regression analysis.

  16. Spectrophotometeric determination of trace amounts of Al3+ ion in water samples after cloud point extraction using quinizarin as a complexing agent.

    Science.gov (United States)

    Shokrollahi, Ardeshir; Aghaei, Roghayeh

    2014-02-01

    In this study, cloud point extraction was used for the preconcentration of Al(3+) ion after the complex formation with 1,4-dihydroxy-9,10-anthraquinone (Quinizarin [QUIN]), and subsequent analysis by spectrophotometeric method, using Triton X-114 as surfactant. The optimal extraction and reaction conditions were studied (i.e., pH = 5.5, 0.1 mM QUIN, Triton X-114 = 0.1% (w/v)), and the analytical characteristics of the method (e.g., limit of detection, linear range, preconcentration, and enrichment factors) were obtained. Linearity was obeyed in the range of 3.33-166.67 ng ml(-1) of Al(3+) ion. The detection limit of the method was 2.09 ng ml(-1) for Al(3+) ion. The interference effect of some anions and cations was also tested. The method was applied to determine Al(3+) ion in water samples.

  17. Evaluation of a synergetic effect between Rh as permanent chemical modifier and acetylacetone as complexing agent in Sc determination in sediment slurry samples by ETAAS

    Energy Technology Data Exchange (ETDEWEB)

    Flores, Araceli Veronica [Departamento de Quimica Analitica, Instituto de Quimica, Universidade Estadual de Campinas, P.O. Box 6154, 13084 971 Campinas, Sao Paulo (Brazil); Perez, Carlos Alberto [Laboratorio Nacional de Luz Sincrotron, P.O. Box 6192, 13084 971 Campinas, Sao Paulo (Brazil); Arruda, Marco Aurelio Zezzi [Departamento de Quimica Analitica, Instituto de Quimica, Universidade Estadual de Campinas, P.O. Box 6154, 13084 971 Campinas, Sao Paulo (Brazil)]. E-mail: zezzi@iqm.unicamp.br

    2005-02-14

    In the present work, scandium was determined in sediment slurry samples (from three different rivers) by electrothermal atomic absorption spectrometry (ETAAS). Slurries were prepared by weighting 100 mg of dry sediment samples ({<=}53 {mu}m particle sizes) and adding 6 ml of HCl:HNO{sub 3}:HF (3:1:2, v/v). Accurate results were only possible due to the synergetic effect between Rh as permanent chemical modifier and acetylacetone (Acac) as complexing agent. The same platform was used for 400 heating cycles. The performance of the chemical modification was evaluated by using scanning electron microscopy (SEM), synchrotron radiation X-ray fluorescence (SRXRF) and some figures of merit (precision and detectability). The best analytical conditions were attained using 1500 and 2550 deg. C as pyrolysis and atomization temperatures. The scandium content in the liquid phase of the slurries ranged from 61 to 73%, thus indicating, in this study, that both liquid and solid phases play an important role in slurry analyses. An amount of 5.0-20.0 {mu}g l{sup -1} Sc linear range as well as LOD and LOQ of 0.19 and 0.62 {mu}g l{sup -1}, respectively, were obtained under these conditions. The accuracy was checked by using microwave-assisted decomposition, and the results compared to those obtained with the proposed methodology (slurry analysis). By checking both sets of the results, there is no statistical difference at the 95% confidence levels.

  18. Enantioselective column coupled electrophoresis employing large bore capillaries hyphenated with tandem mass spectrometry for ultra-trace determination of chiral compounds in complex real samples.

    Science.gov (United States)

    Piešťanský, Juraj; Maráková, Katarína; Kovaľ, Marián; Havránek, Emil; Mikuš, Peter

    2015-12-01

    A new multidimensional analytical approach for the ultra-trace determination of target chiral compounds in unpretreated complex real samples was developed in this work. The proposed analytical system provided high orthogonality due to on-line combination of three different methods (separation mechanisms), i.e. (1) isotachophoresis (ITP), (2) chiral capillary zone electrophoresis (chiral CZE), and (3) triple quadrupole mass spectrometry (QqQ MS). The ITP step, performed in a large bore capillary (800 μm), was utilized for the effective sample pretreatment (preconcentration and matrix clean-up) in a large injection volume (1-10 μL) enabling to obtain as low as ca. 80 pg/mL limits of detection for the target enantiomers in urine matrices. In the chiral CZE step, the different chiral selectors (neutral, ionizable, and permanently charged cyclodextrins) and buffer systems were tested in terms of enantioselectivity and influence on the MS detection response. The performance parameters of the optimized ITP - chiral CZE-QqQ MS method were evaluated according to the FDA guidance for bioanalytical method validation. Successful validation and application (enantioselective monitoring of renally eliminated pheniramine and its metabolite in human urine) highlighted great potential of this chiral approach in advanced enantioselective biomedical applications.

  19. Sampling and Representation Complexity of Revenue Maximization

    OpenAIRE

    Dughmi, Shaddin; Han, Li; Nisan, Noam

    2014-01-01

    We consider (approximate) revenue maximization in auctions where the distribution on input valuations is given via "black box" access to samples from the distribution. We observe that the number of samples required -- the sample complexity -- is tightly related to the representation complexity of an approximately revenue-maximizing auction. Our main results are upper bounds and an exponential lower bound on these complexities.

  20. Mixture model analysis of complex samples

    NARCIS (Netherlands)

    Wedel, M; ter Hofstede, F; Steenkamp, JBEM

    1998-01-01

    We investigate the effects of a complex sampling design on the estimation of mixture models. An approximate or pseudo likelihood approach is proposed to obtain consistent estimates of class-specific parameters when the sample arises from such a complex design. The effects of ignoring the sample desi

  1. Tangential-flow ultrafiltration: a versatile methodology for determination of complexation parameters in refractory organic matter from Brazilian water and soil samples.

    Science.gov (United States)

    Romão, L P C; Castro, G R; Rosa, A H; Rocha, J C; Padilha, P M; Silva, H C

    2003-04-01

    In this work the copper(II) complexation parameters of aquatic organic matter, aquatic and soil humic substances from Brazilian were determined using a new versatile approach based on a single-stage tangential-flow ultrafiltration (TF-UF) technique (cut-off 1 kDa) and sensitive atomic spectrometry methods. The results regarding the copper(II) complexation capacity and conditional stability constants obtained for humic materials were compared with those obtained using direct potentiometry with a copper-ion-selective electrode. The analytical procedure based on ultrafiltration is a good alternative to determine the complexation parameters in natural organic material from aquatic and soil systems. This approach presents additional advantages such as better sensibility, applicability for multi-element capability, and its possible to be used under natural conditions when compared with the traditional ion-selective electrode.

  2. Biostatistics Series Module 5: Determining Sample Size.

    Science.gov (United States)

    Hazra, Avijit; Gogtay, Nithya

    2016-01-01

    principles are long known, historically, sample size determination has been difficult, because of relatively complex mathematical considerations and numerous different formulas. However, of late, there has been remarkable improvement in the availability, capability, and user-friendliness of power and sample size determination software. Many can execute routines for determination of sample size and power for a wide variety of research designs and statistical tests. With the drudgery of mathematical calculation gone, researchers must now concentrate on determining appropriate sample size and achieving these targets, so that study conclusions can be accepted as meaningful.

  3. Accuracy assessment with complex sampling designs

    Science.gov (United States)

    Raymond L. Czaplewski

    2010-01-01

    A reliable accuracy assessment of remotely sensed geospatial data requires a sufficiently large probability sample of expensive reference data. Complex sampling designs reduce cost or increase precision, especially with regional, continental and global projects. The General Restriction (GR) Estimator and the Recursive Restriction (RR) Estimator separate a complex...

  4. Determination of Trace Amounts of Gold in Environmental Samples by Adsorptive Stripping Voltammetry of Its Complex with Rhodamine Using Osc-Pls

    Directory of Open Access Journals (Sweden)

    A. Akrami

    2012-11-01

    Full Text Available The multivariate calibration method was applied for the determination of trace amounts of gold based on a hanging mercury drop electrode (HMDE in the presence of rhodanine, followed by reduction of adsorbed gold by voltammetric scan using differential pulse modulation The optimum experimental conditions are: rhodanine concentration of 0.20 mg mL-1, pH 5.0, accumulation potential of -600 mV versus Ag/AgCl, accumulation time of 100 sec, scan rate of 30 mV s-1 and pulse height of 100 mV. The calibration matrix for partial least squares (PLS regression was designed with 9 samples. Orthogonal signal correction (OSC is a preprocessing technique used for removing the information unrelated to the target variables based on constrained principal component analysis. OSC is a suitable preprocessing method for PLS calibration without loss of prediction capacity using electrochemical method. The RMSEP for gold determination with PLS and OSC-PLS were 8.51 and 1.94, respectively. This procedure allows the determination of gold in synthetic and real samples with good reliability of the determination

  5. Gibbs sampling of complex-valued distributions

    Science.gov (United States)

    Salcedo, L. L.

    2016-10-01

    A new technique is explored for the Monte Carlo sampling of complex-valued distributions. The method is based on a heat bath approach where the conditional probability is replaced by a positive representation of it on the complex plane. Efficient ways to construct such representations are also introduced. The performance of the algorithm is tested on small and large lattices with a λ ϕ4 theory with quadratic nearest-neighbor complex coupling. The method works for moderate complex couplings, reproducing reweighting and complex Langevin results and fulfilling various Schwinger-Dyson relations.

  6. A novel solid fluorescence method for the fast determination of quercetin in biological samples based on the quercetin-Al(III) complex imprinted polymer

    Science.gov (United States)

    Hu, Yufei; Feng, Ting; Li, Gongke

    2014-01-01

    In this work, a novel solid fluorescence method was proposed and applied to the fast determination of quercetin in urine and onion skin samples by using metal coordination imprinted polymer membrane, which was regarded as a recognition element. The quercetin-Al(III) imprinted polymer was immobilized in the microporous polypropylene fiber membrane via consecutive in situ polymerization. The CIP membrane had the porous, loose and layer upon layer structure. The CIP membrane was characterized by electron microscope photographs, infrared spectra, thermogravimetric analysis and solvent-resistant investigation. The extraction conditions including extraction solvent, extraction time, desorption solvent were optimized. Compared with MIP and NIP membrane, CIP membrane had been proved to be peculiar selective for quercetin even in presence of the structurally similar compounds such as kaempferol, rutin, naringenin and alpinetin. The CIP membrane was characteristic of high selectivity, stable and sensitive response to quercetin in polar environment. Under the optimum condition, there was a linear relationship between the state fluorescent response and the concentration of quercetin. The linear calibration range was over 0.02 mg L-1-0.80 mg L-1 with a detection limit of 5 μg L-1. The method was characteristic of flexible and good repeatability with relative standard deviation (RSD) of 4.1%. The proposed method was also successfully applied for the determination of quercetin in urine and onion skin samples without complicated pretreatment. The recoveries were 84.0-112.4% and RSDs varied from 1.5% to 6.8%. The results obtained by the proposed method agreed well with those obtained by HPLC method.

  7. Separation and Analysis of Complex Samples

    Institute of Scientific and Technical Information of China (English)

    2011-01-01

    @@ Founded on the basis of the CAS Key Lab of Separation Sciences for Analytical Chemistry, this group has been conducting research into separation and analysis of complex samples for five years.Thanks to their hard work, a number of achievements were scored in the following fields: highly selective and highly efficient separation and analysis of complex samples, high through-put analysis and highly sensitive detection.Besides, the group also made many efforts on the development and application of new technologies and as a result, a total of 13 innovative patents were or are being commercialized.Now, facing great demands for separation and analysis of complex samples in other areas such as lite sciences and environmental sciences, this group will further extend their research directions.

  8. Sampling of Complex Networks: A Datamining Approach

    Science.gov (United States)

    Loecher, Markus; Dohrmann, Jakob; Bauer, Gernot

    2007-03-01

    Efficient and accurate sampling of big complex networks is still an unsolved problem. As the degree distribution is one of the most commonly used attributes to characterize a network, there have been many attempts in recent papers to derive the original degree distribution from the data obtained during a traceroute- like sampling process. This talk describes a strategy for predicting the original degree of a node using the data obtained from a network by traceroute-like sampling making use of datamining techniques. Only local quantities (the sampled degree k, the redundancy of node detection r, the time of the first discovery of a node t and the distance to the sampling source d) are used as input for the datamining models. Global properties like the betweenness centrality are ignored. These local quantities are examined theoretically and in simulations to increase their value for the predictions. The accuracy of the models is discussed as a function of the number of sources used in the sampling process and the underlying topology of the network. The purpose of this work is to introduce the techniques of the relatively young field of datamining to the discussion on network sampling.

  9. Simultaneous determination of Mn2+ and Fe3+ as 4,4'[(4-cholorophenyl)methylene] bis(3-methyl-1-phenyl-1H-pyrazol-5-ol) complexes in some foods, vegetable and water samples by artificial neural networks.

    Science.gov (United States)

    Abbasi-Tarighat, Maryam; Shahbazi, Elahe; Niknam, Khodabakhsh

    2013-06-01

    A simple and sensitive spectrophotometric method to the simultaneous determination of Mn(2+) and Fe(3+) in foods, vegetable and water sample with the aid of artificial neural networks (ANNs) is described. It relies on the complexation of analytes with recently synthesised bis pyrazol base ligand as 4,4'[(4-cholorophenyl)methylene] bis(3-methyl-1-phenyl-1H-pyrazol-5-ol)(CMBPP). The analytical data show that the ratio of ligand to metal in metal complexes is 1:1 and 1:2 for Fe(3+) and Mn(2+), respectively. It was found that the complexation reactions are completed at pH 6.7 and 5 min after mixing. The results showed that Mn(2+) and Fe(3+) could be determined simultaneously in the range of 0.20-7.5 and 0.30-9.0 mgl(-1), respectively. The analytical characteristics of the method such as the detection limit and the relative standard error predictions were calculated. The data obtained from synthetic mixtures of the metal ions were processed by radial basis function networks (RBFNs) and feed forward neural networks (FFNNs). The optimal conditions of the neural networks were obtained by adjusting various parameters by trial-and-error. Under the working conditions, the proposed methods were successfully applied to the simultaneous determination of elements in different water, tablet, rice, tea leaves, tomato, cabbage and lettuce samples.

  10. DEVELOPMENT AND APPLICATION OF IMMUNOAFFINITY COLUMN CHROMATOGRAPHY AS A CLEANUP METHOD FOR THE DETERMINATION OF ATRAZINE IN COMPLEX ENVIRONMENTAL SAMPLE MEDIA

    Science.gov (United States)

    A rabbit antibody immunoaffinity (IA) column procedure was evaluated as a cleanup method for the determination of atrazine in soil, sediment, and food. Four IA columns were prepared by immobilizing a polyclonal rabbit anti-atrazine antibody solution to HiTrap Sepharose columns. A...

  11. Electrochemical determination of an antitumour platinum(IV complex: trans-[PtCl2(OH2(dimethylamine(isopro­pylamine]. Application to biological samples

    Directory of Open Access Journals (Sweden)

    PEDRO HERNÁNDEZ

    2013-04-01

    Full Text Available A differential pulse voltammetry (DPV method has been applied for the first time for determination of trans-Pt[Cl2(OH2(dimethylamine(isopropylamine]. To this end, all chemical and instrumental variables affecting the determination of trans-Pt[Cl2(OH2(dimethylamine(isopropylamine] were optimized. From studies of the mechanisms governing the electrochemical response of trans-Pt[Cl2(OH2(dimethylamine(isopropylamine], it was concluded that it is an electrochemically irreversible system with a reduc­tion under diffusion control, with a reduction potential of -425 mV. Under optimal conditions, the variation in the analytical signal (Ip with trans-Pt[Cl2(OH2(dimethylamine(isopropylamine] concentration is linear in the 0.8 µg mL-1 to 20 µg mL-1 range, with an LOD of 97 ng mL-1 and a LOQ of 323 ng mL-1, RSD = 1.58 % and Er = 0.83 %. The optimized method was applied to the determination of trans-Pt[Cl2(OH2(di-methylamine(isopropylamine] in biological fluids, human urine and synthetic urine

  12. RAPID DETERMINATION OF RADIOSTRONTIUM IN SEAWATER SAMPLES

    Energy Technology Data Exchange (ETDEWEB)

    Maxwell, S.

    2013-01-16

    A new method for the determination of radiostrontium in seawater samples has been developed at the Savannah River National Laboratory (SRNL) that allows rapid preconcentration and separation of strontium and yttrium isotopes in seawater samples for measurement. The new SRNL method employs a novel and effective pre-concentration step that utilizes a blend of calcium phosphate with iron hydroxide to collect both strontium and yttrium rapidly from the seawater matrix with enhanced chemical yields. The pre-concentration steps, in combination with rapid Sr Resin and DGA Resin cartridge separation options using vacuum box technology, allow seawater samples up to 10 liters to be analyzed. The total {sup 89}Sr + {sup 90}Sr activity may be determined by gas flow proportional counting and recounted after ingrowth of {sup 90}Y to differentiate {sup 89}Sr from {sup 90}Sr. Gas flow proportional counting provides a lower method detection limit than liquid scintillation or Cerenkov counting and allows simultaneous counting of samples. Simultaneous counting allows for longer count times and lower method detection limits without handling very large aliquots of seawater. Seawater samples up to 6 liters may be analyzed using Sr Resin for {sup 89}Sr and {sup 90}Sr with a Minimum Detectable Activity (MDA) of 1-10 mBq/L, depending on count times. Seawater samples up to 10 liters may be analyzed for {sup 90}Sr using a DGA Resin method via collection and purification of {sup 90}Y only. If {sup 89}Sr and other fission products are present, then {sup 91}Y (beta energy 1.55 MeV, 58.5 day half-life) is also likely to be present. {sup 91}Y interferes with attempts to collect {sup 90}Y directly from the seawater sample without initial purification of Sr isotopes first and {sup 90}Y ingrowth. The DGA Resin option can be used to determine {sup 90}Sr, and if {sup 91}Y is also present, an ingrowth option with using DGA Resin again to collect {sup 90}Y can be performed. An MDA for {sup 90}Sr of <1 m

  13. Code Samples Used for Complexity and Control

    Science.gov (United States)

    Ivancevic, Vladimir G.; Reid, Darryn J.

    2015-11-01

    The following sections are included: * MathematicaⓇ Code * Generic Chaotic Simulator * Vector Differential Operators * NLS Explorer * 2C++ Code * C++ Lambda Functions for Real Calculus * Accelerometer Data Processor * Simple Predictor-Corrector Integrator * Solving the BVP with the Shooting Method * Linear Hyperbolic PDE Solver * Linear Elliptic PDE Solver * Method of Lines for a Set of the NLS Equations * C# Code * Iterative Equation Solver * Simulated Annealing: A Function Minimum * Simple Nonlinear Dynamics * Nonlinear Pendulum Simulator * Lagrangian Dynamics Simulator * Complex-Valued Crowd Attractor Dynamics * Freeform Fortran Code * Lorenz Attractor Simulator * Complex Lorenz Attractor * Simple SGE Soliton * Complex Signal Presentation * Gaussian Wave Packet * Hermitian Matrices * Euclidean L2-Norm * Vector/Matrix Operations * Plain C-Code: Levenberg-Marquardt Optimizer * Free Basic Code: 2D Crowd Dynamics with 3000 Agents

  14. Complex Sample Data Recommendations and Troubleshooting

    Science.gov (United States)

    Hahs-Vaughn, Debbie L.; McWayne, Christine M.; Bulotsky-Shearer, Rebecca J.; Wen, Xiaoli; Faria, Ann-Marie

    2011-01-01

    Complex survey data, as highlighted in this issue of "Evaluation Review", provide a wealth of opportunities for answering methodological and/or applied research questions. However, the analytic issues of nonindependence and unequal selection probability must be addressed when analyzing this type of data. Thus, to ensure that research questions are…

  15. Analyzing Complex Reaction Mechanisms Using Path Sampling.

    Science.gov (United States)

    van Erp, Titus S; Moqadam, Mahmoud; Riccardi, Enrico; Lervik, Anders

    2016-11-08

    We introduce an approach to analyze collective variables (CVs) regarding their predictive power for a reaction. The method is based on already available path sampling data produced by, for instance, transition interface sampling or forward flux sampling, which are path sampling methods used for efficient computation of reaction rates. By a search in CV space, a measure of predictiveness can be optimized and, in addition, the number of CVs can be reduced using projection operations which keep this measure invariant. The approach allows testing hypotheses on the reaction mechanism but could, in principle, also be used to construct the phase-space committor surfaces without the need of additional trajectory sampling. The procedure is illustrated for a one-dimensional double-well potential, a theoretical model for an ion-transfer reaction in which the solvent structure can lower the barrier, and an ab initio molecular dynamics study of water auto-ionization. The analysis technique enhances the quantitative interpretation of path sampling data which can provide clues on how chemical reactions can be steered in desired directions.

  16. Evaluation of the capabilities of atmospheric pressure chemical ionization source coupled to tandem mass spectrometry for the determination of dioxin-like polychlorobiphenyls in complex-matrix food samples.

    Science.gov (United States)

    Portolés, T; Sales, C; Abalos, M; Sauló, J; Abad, E

    2016-09-21

    The use of the novel atmospheric pressure chemical ionization (APCI) source for gas chromatography (GC) coupled to triple quadrupole using tandem mass spectrometry (MS/MS) and its potential for the simultaneous determination of the 12 dioxin-like polychlorobiphenyls (DL-PCBs) in complex food and feed matrices has been evaluated. In first place, ionization and fragmentation behavior of DL-PCBs on the APCI source under charge transfer conditions has been studied followed by their fragmentation in the collision cell. Linearity, repeatability and sensitivity have been studied obtaining instrumental limits of detection and quantification of 0.0025 and 0.005 pg μL(-1) (2.5 and 5 fg on column) respectively for every DL-PCB. Finally, application to real samples has been carried out and DL-PCB congeners (PCB 77, 81, 105, 114, 118, 123, 126, 156, 157, 167, 169, 189) have been detected in the different samples in the range of 0.40-10000 pg g(-1). GC-(APCI)MS/MS has been proved as a suitable alternative to the traditionally accepted confirmation method based on the use of high resolution mass spectrometry and other triple quadrupole tandem mass spectrometry techniques operating with electron ionization. The development of MS/MS methodologies for the analysis of dioxins and DL-PCBs is nowadays particularly important, since this technique was included as a confirmatory method in the present European Union regulations that establish the requirements for the determination of these compounds in food and feed matrices.

  17. Field-Flow Fractionation Analysis of Complex Biological Samples

    Directory of Open Access Journals (Sweden)

    Mijić, I.

    2014-03-01

    Full Text Available Normal analytical methods have difficulties when analysing complex samples containing particles of different size. In the 1960s, a new analytical technique was developed, which was able to overcome those difficulties. This new, Field-Flow Fractionation (FFF technique has been primarily used in the separation of large particles such as macromolecules and colloids. The development and improvement of the FFF technique led to the coupling of the technique with other specific and sensitive analytical methods which resulted in the FFF technique becoming very useful in isolation, separation and analysis of various complex samples, such as powders, emulsions, colloids, geological sediments, biopolymers, complex proteins, polysaccharides, synthetic polymers, and many others. The separation field in the FFF technique is a thin, empty flow chamber called a channel. The structure of the ribbonlike channel with view of the parabolic flow can be seen in Fig. 1. Separation is achieved by the interaction of sample components with an externally generated field, which is applied perpendicularly to the direction of the mobile flow inside the channel. Sample components, which differ in molar mass, size or other properties are pushed by the applied perpendicular field into different velocity regions within the parabolic flow profile of the mobile phase across the channel. The flow has different velocity depending on the position within the channel; the velocity at the walls is zero and it increases towards the centre of the channel. Samples are carried downstream through the channel at different velocities and exit the channel after different retention times. The relative distribution of samples in the parabolic flow determines the separation characteristics. Different operating modes have different types of distributions. The most frequently used mechanisms of FFF separation are listed in Fig. 2. Based on the characteristics of analysed particles and applied outer

  18. Synchronous derivative fluorimetric determination of boron in Uranium fuel samples

    Energy Technology Data Exchange (ETDEWEB)

    Verma, Poonam, E-mail: poonamv@barc.gov.in [Radioanalytical Chemistry Division, Bhabha Atomic Research Centre, Mumbai 400085 (India); Kumar, Shiny S.; Sawant, R.M.; Tomar, B.S. [Radioanalytical Chemistry Division, Bhabha Atomic Research Centre, Mumbai 400085 (India); Ramakumar, K.L. [Radiochemistry and Isotope Group, Bhabha Atomic Research Centre, Mumbai 400085 (India)

    2014-09-15

    We report a sensitive and selective method for determination of boron in uranium samples by spectrofluorimetry in synchronous derivative mode. This method is based on the complexation of non-fluorescent boron with fluorescent chromotropic acid to form fluorescent boron–chromotrope complex. The spectrum of native fluorescence of chromotropic acid seriously overlaps with that of the complex and hence, synchronous derivative mode was employed in which physical separation of excess ligand and complex is not necessary. With the optimized experimental and instrumental conditions, limit of detection obtained is 2 ng mL{sup −1}. The linear concentration range is 5–100 ng mL{sup −1} with regression coefficient better than 0.997. The precision is better than 5% at 10 ng mL{sup −1} level and 3% at 50 ng mL{sup −1} level (n=9). Fluorescence quenching by residual matrix elements in the final sample solution is corrected by slope-ratio method. The method is validated with reference materials and successfully applied to the uranium nuclear fuels with the accuracy of ±10%. The proposed method reduces sample size requirement; thereby reducing load of uranium recovery from analytical waste in case of enriched uranium based samples. - Highlights: • Selectivity and sensitivity increases in synchronous derivative mode. • Sample size reduction that reduces load of enriched uranium recovery. • Eliminates need of physical separation of excess ligand and complex. • Quenching by residual matrix elements corrected by the slope-ratio method. • Important contribution to quality control of fuel materials in nuclear technology.

  19. The Sample Complexity of Search over Multiple Populations

    OpenAIRE

    Malloy, Matthew L.; Tang, Gongguo; Nowak, Robert D.

    2012-01-01

    This paper studies the sample complexity of searching over multiple populations. We consider a large number of populations, each corresponding to either distribution P0 or P1. The goal of the search problem studied here is to find one population corresponding to distribution P1 with as few samples as possible. The main contribution is to quantify the number of samples needed to correctly find one such population. We consider two general approaches: non-adaptive sampling methods, which sample ...

  20. Sample handling strategies for the determination of persistent trace organic contaminants from biota samples.

    Science.gov (United States)

    Fidalgo-Used, Natalia; Blanco-González, Elisa; Sanz-Medel, Alfredo

    2007-05-02

    Even after emergence of most advanced instrumental techniques for the final separation, detection, identification and determination of analytes, sample handling continues to play a basic role in environmental analysis of complex matrices. In fact, sample preparation steps are often the bottleneck for combined time and efficiency in many overall analytical procedures. Thus, it is not surprising that, in the last two decades, a lot of effort has been devoted to the development of faster, safer, and more environment friendly techniques for sample extraction and extract clean up, prior to actual instrumental analysis. This article focuses on the state of the art in sample preparation of environmental solid biological samples dedicated to persistent organic pollutants (POPs) analysis. Extraction techniques such as Soxhlet extraction, sonication-assisted extraction, supercritical fluid extraction (SFE), microwave-assisted extraction (MAE), pressurised liquid extraction (PLE) and matrix solid-phase dispersion (MSPD) are reviewed and their most recent applications to the determination of POPs in biota samples are provided. Additionally, classical as well as promising novel extraction/clean-up techniques such as solid phase microextraction (SPME) are also summarized. Finally, emerging trends in sample preparation able to integrate analytes extraction and their adequate clean-up are presented.

  1. Tight Sample Complexity of Large-Margin Learning

    CERN Document Server

    Sabato, Sivan; Tishby, Naftali

    2010-01-01

    We obtain a tight distribution-specific characterization of the sample complexity of large-margin classification with L_2 regularization: We introduce the \\gamma-adapted-dimension, which is a simple function of the spectrum of a distribution's covariance matrix, and show distribution-specific upper and lower bounds on the sample complexity, both governed by the \\gamma-adapted-dimension of the source distribution. We conclude that this new quantity tightly characterizes the true sample complexity of large-margin classification. The bounds hold for a rich family of sub-Gaussian distributions.

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

    Science.gov (United States)

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

    2016-03-01

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

  3. Determination of copper in powdered chocolate samples by slurry-sampling flame atomic-absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Walter N.L. dos; Silva, Erik G.P. da; Fernandes, Marcelo S.; Araujo, Rennan G.O.; Costa, Anto' ' enio C.S.; Ferreira, Sergio L.C. [Nucleo de Excelencia em Quimica Analitica da Bahia, Universidade Federal da Bahia, Instituto de Quimica, Salvador, Bahia (Brazil); Vale, M.G.R. [Instituto de Quimica, Universidade Federal da Bahia do Rio Grande do Sul, Porto Alegre, Rio Grande do Sul (Brazil)

    2005-06-01

    Chocolate is a complex sample with a high content of organic compounds and its analysis generally involves digestion procedures that might include the risk of losses and/or contamination. The determination of copper in chocolate is important because copper compounds are extensively used as fungicides in the farming of cocoa. In this paper, a slurry-sampling flame atomic-absorption spectrometric method is proposed for determination of copper in powdered chocolate samples. Optimization was carried out using univariate methodology involving the variables nature and concentration of the acid solution for slurry preparation, sonication time, and sample mass. The recommended conditions include a sample mass of 0.2 g, 2.0 mol L{sup -1} hydrochloric acid solution, and a sonication time of 15 min. The calibration curve was prepared using aqueous copper standards in 2.0 mol L{sup -1} hydrochloric acid. This method allowed determination of copper in chocolate with a detection limit of 0.4 {mu}g g{sup -1} and precision, expressed as relative standard deviation (RSD), of 2.5% (n=10) for a copper content of approximately 30 {mu}g g{sup -1}, using a chocolate mass of 0.2 g. The accuracy was confirmed by analyzing the certified reference materials NIST SRM 1568a rice flour and NIES CRM 10-b rice flour. The proposed method was used for determination of copper in three powdered chocolate samples, the copper content of which varied between 26.6 and 31.5 {mu}g g{sup -1}. The results showed no significant differences with those obtained after complete digestion, using a t-test for comparison. (orig.)

  4. Evaluating quantitative measures of grammatical complexity in spontaneous speech samples.

    Science.gov (United States)

    Blake, J; Quartaro, G; Onorati, S

    1993-02-01

    The validity of MLU and a measure of syntactic complexity were tested against LARSP on spontaneous speech samples from 87 children, ranging in age from 1;6 to 4;9. Change in some LARSP clausal measures was found across MLU stages up to MLU 4.5. For the measure of syntactic complexity, no such ceiling was found for the clausal connectivity score in LARSP or for average clausal complexity in LARSP. Neither MLU nor the measure of syntactic complexity indexed LARSP phrasal complexity. It is concluded that MLU is a valid measure of clausal complexity up to 4.5 and that our measure of syntactic complexity is more valid at more advanced stages.

  5. Performance of Random Effects Model Estimators under Complex Sampling Designs

    Science.gov (United States)

    Jia, Yue; Stokes, Lynne; Harris, Ian; Wang, Yan

    2011-01-01

    In this article, we consider estimation of parameters of random effects models from samples collected via complex multistage designs. Incorporation of sampling weights is one way to reduce estimation bias due to unequal probabilities of selection. Several weighting methods have been proposed in the literature for estimating the parameters of…

  6. Determination of Cd in biological samples by flame AAS following on-line preconcentration by complexation with O,O-diethyldithiophosphate and solid phase extraction with Amberlite XAD-4.

    Science.gov (United States)

    Santos, Eder José Dos; Herrmann, Amanda Beatriz; Ribeiro, Anderson Schwingel; Curtius, Adilson José

    2005-01-30

    A method for the on-line preconcentration of Cd based on its complex formation with the ammonium salt of O,O-diethylditiophosphate (DDTP) and using the Amberlite XAD-4 resin as a solid support in a column is proposed. Cadmium was detected by flame atomic absorption spectrometry. Different conditions, such as complexing agent concentration, preconcentration time, solutions flow rates and nature and concentration of the eluent were optimized. Different detection limits (LODs) could be established by using different preconcentration times, between 30s and 5min, with corresponding LODs from 5 to 1mugL(-1), respectively. The method was validated by analyzing five biological certified samples. The relative standard deviation was usually around 3%, indicating a very good precision. The found concentrations values are in agreement with the certified ones, according to the t-test, for a confidence level of 95%. Enriched seawaters were also analyzed, and the recoveries were between 93 and 108%. The FI method is very simple and probably can be coupled to other measuring analytical techniques.

  7. Using light scattering to determine the stoichiometry of protein complexes.

    Science.gov (United States)

    Mogridge, Jeremy

    2015-01-01

    The stoichiometry of a protein complex can be calculated from an accurate measurement of the complex's molecular weight. Multiangle laser light scattering in combination with size exclusion chromatography and interferometric refractometry provides a powerful means for determining the molecular weights of proteins and protein complexes. In contrast to conventional size exclusion chromatography and analytical centrifugation, measurements do not rely on the use of molecular weight standards and are not affected by the shape of the proteins. The technique is based on the direct relationship between the amount of light scattered by a protein in solution, and the product of its concentration and molecular weight. A typical experimental configuration includes a size exclusion column to fractionate the sample, a light scattering detector to measure scattered light, and an interferometric refractometer to measure protein concentration. The determination of the molecular weight of an anthrax toxin complex will be used to illustrate how multiangle laser light scattering can be used to determine the stoichiometry of protein complexes.

  8. Structural elucidation of low abundant metabolites in complex sample matrices

    NARCIS (Netherlands)

    Hooft, van der J.J.J.; Vos, de R.C.H.; Ridder, L.O.; Vervoort, J.; Bino, R.J.

    2013-01-01

    Identification of metabolites is a major challenge in biological studies and relies in principle on mass spectrometry (MS) and nuclear magnetic resonance (NMR) methods. The increased sensitivity and stability of both NMR and MS systems have made dereplication of complex biological samples feasible.

  9. Quantitative imaging of complex samples by spiral phase contrast microscopy.

    Science.gov (United States)

    Bernet, Stefan; Jesacher, Alexander; Fürhapter, Severin; Maurer, Christian; Ritsch-Marte, Monika

    2006-05-01

    Recently a spatial spiral phase filter in a Fourier plane of a microscopic imaging setup has been demonstrated to produce edge enhancement and relief-like shadow formation of amplitude and phase samples. Here we demonstrate that a sequence of at least 3 spatially filtered images, which are recorded with different rotational orientations of the spiral phase plate, can be used to obtain a quantitative reconstruction of both, amplitude and phase information of a complex microscopic sample, i.e. an object consisting of mixed absorptive and refractive components. The method is demonstrated using a calibrated phase sample, and an epithelial cheek cell.

  10. Synthetic Multiple-Imputation Procedure for Multistage Complex Samples

    Directory of Open Access Journals (Sweden)

    Zhou Hanzhi

    2016-03-01

    Full Text Available Multiple imputation (MI is commonly used when item-level missing data are present. However, MI requires that survey design information be built into the imputation models. For multistage stratified clustered designs, this requires dummy variables to represent strata as well as primary sampling units (PSUs nested within each stratum in the imputation model. Such a modeling strategy is not only operationally burdensome but also inferentially inefficient when there are many strata in the sample design. Complexity only increases when sampling weights need to be modeled. This article develops a generalpurpose analytic strategy for population inference from complex sample designs with item-level missingness. In a simulation study, the proposed procedures demonstrate efficient estimation and good coverage properties. We also consider an application to accommodate missing body mass index (BMI data in the analysis of BMI percentiles using National Health and Nutrition Examination Survey (NHANES III data. We argue that the proposed methods offer an easy-to-implement solution to problems that are not well-handled by current MI techniques. Note that, while the proposed method borrows from the MI framework to develop its inferential methods, it is not designed as an alternative strategy to release multiply imputed datasets for complex sample design data, but rather as an analytic strategy in and of itself.

  11. Voltammetric Determination of Ni and Co in Water Samples

    Science.gov (United States)

    Herrera-Melian, Jose Alberto; Dona-Rodriguez, Jose Miguel; Hernandez-Brito, Joaquin; Perez Pena, Jesus

    1997-12-01

    Stripping voltammetry has attracted considerable attention for the determination of trace and ultratrace metals. This is mainly due to its high sensitivity and low cost of instrumentation. In adsorptive stripping voltammetry an organometallic complex is formed by the addition of a suitable ligand to the sample. The complex is adsorbed onto the Hg-drop by the application of the proper adsorption potential (more positive than E1/2) and solution stirring. After an adsorption period a cathodic (negative going) potential scan is applied and the metal concentration is calculated by the standard addition method. Nickel is found in natural waters at nM levels and is closely related with phosphates and silicates. Cobalt is a component of vitamin B12 and occurs in natural waters at concentration about 0.1 nM. We propose the voltammetric analysis of these elements by adsorptive stripping voltammetry as an introductory laboratory experiment for advanced chemistry or for chemical or environmental engineering students. The experiment has been proven to be very suitable for the laboratory part of the instrumental analysis course at the University of Las Palmas de Gran Canaria (Spain). In general, about 70% of the students have obtained good agreement (less than 10% of difference) between their results and the expected ones. Two hours is enough for the overall instrumental performance and the preparation of Ni and Co standards.

  12. Approaches to sample size determination for multivariate data

    NARCIS (Netherlands)

    Saccenti, Edoardo; Timmerman, Marieke E.

    2016-01-01

    Sample size determination is a fundamental step in the design of experiments. Methods for sample size determination are abundant for univariate analysis methods, but scarce in the multivariate case. Omics data are multivariate in nature and are commonly investigated using multivariate statistical

  13. Optical properties of the Eu(III)-La(III)-complex-doped polyolefine film and rod samples

    Science.gov (United States)

    Pogreb, Roman; Popov, Oleg; Lirtsman, Vlad; Pyshkin, Oleg; Kazachkov, Alexander; Musin, Albina; Finkelshtein, Binyamin; Shmukler, Yuri; Davidov, Dan; Bormashenko, Edward

    2005-04-01

    The work is devoted to luminescent properties of trivalent lanthanide complexes dispersed in thermoplastic host matrices. Polyethylene-based film and polypropylene-based rod both doped with these complexes were manufactured using an extrusion technique. Two kinds of dopants were used: Eu(III)-thenoyltrifluoroacetone-1,10-phenanthroline complex (Eu(III)) and Eu(III)-La(III)-1,10-phenanthroline complex (Eu(III)-La(III)). Comparison was made between these samples regarding absorption, excitation, emission and a lifetime of luminescence. Dependence of emission intensity on the excitation energy was determined. Emission spectra of the films were studied at room and helium temperatures. Optical properties of Eu(III) samples are different from Eu(III)-La(III) samples. Significant difference in spectra of these two types of samples may be attributed to the La(III) action.

  14. Sampling informative/complex a priori probability distributions using Gibbs sampling assisted by sequential simulation

    DEFF Research Database (Denmark)

    Hansen, Thomas Mejer; Mosegaard, Klaus; Cordua, Knud Skou

    2010-01-01

    Markov chain Monte Carlo methods such as the Gibbs sampler and the Metropolis algorithm can be used to sample the solutions to non-linear inverse problems. In principle these methods allow incorporation of arbitrarily complex a priori information, but current methods allow only relatively simple...... this algorithm with the Metropolis algorithm to obtain an efficient method for sampling posterior probability densities for nonlinear inverse problems....

  15. Spectrophotometric determination of molybdenum by extraction of its thiosulphate complex.

    Science.gov (United States)

    Yatirajam, V; Ram, J

    1974-12-01

    A simple and rapid spectrophotometric determination of molybdenum is described. The molybdenum thiosulphate complex is extracted into isoamyl alcohol from 1.0-1.5M hydrochloric acid containing 36-40 mg of Na(2)S(2)O(3).5H(2)O per ml. The absorbance at lambda(max) = 475 nm obeys Beer's law over the range 0-32 microg of Mo per ml of solvent phase. Up to 5 mg/ml of Ti(IV), V(V), Cr(VI), Fe(III), Co(II), Ni(II), U(VI), W(VI), Sb(III), 1 mg/ml of Cu(II), Sn(II), Bi(V) and 10 microg/ml of Pt(IV) and Pd(II) do not interfere. Large amounts of complexing agents interfere. The method has been applied to analysis of synthetic and industrial samples.

  16. Sample size determination in clinical trials with multiple endpoints

    CERN Document Server

    Sozu, Takashi; Hamasaki, Toshimitsu; Evans, Scott R

    2015-01-01

    This book integrates recent methodological developments for calculating the sample size and power in trials with more than one endpoint considered as multiple primary or co-primary, offering an important reference work for statisticians working in this area. The determination of sample size and the evaluation of power are fundamental and critical elements in the design of clinical trials. If the sample size is too small, important effects may go unnoticed; if the sample size is too large, it represents a waste of resources and unethically puts more participants at risk than necessary. Recently many clinical trials have been designed with more than one endpoint considered as multiple primary or co-primary, creating a need for new approaches to the design and analysis of these clinical trials. The book focuses on the evaluation of power and sample size determination when comparing the effects of two interventions in superiority clinical trials with multiple endpoints. Methods for sample size calculation in clin...

  17. Textile-based sampling for potentiometric determination of ions.

    Science.gov (United States)

    Lisak, Grzegorz; Arnebrant, Thomas; Ruzgas, Tautgirdas; Bobacka, Johan

    2015-06-02

    Potentiometric sensing utilizing textile-based micro-volume sampling was applied and evaluated for the determination of clinically (Na(+), K(+), Cl(-)) and environmentally (Cd(2+), Pb(2+) and pH) relevant analytes. In this technological design, calibration solutions and samples were absorbed into textiles while the potentiometric cells (ion-selective electrodes and reference electrode) were pressed against the textile. Once the liquid, by wicking action, reached the place where the potentiometric cell was pressed onto the textile, hence closing the electric circuit, the potentiometric response was obtained. Cotton, polyamide, polyester and their blends with elastane were applied for micro-volume sampling. The textiles were found to influence the determination of pH in environmental samples with pH close to neutral and Pb(2+) at low analyte concentrations. On the other hand, textile-based micro-volume sampling was successfully applied in measurements of Na(+) using solid-contact sodium-selective electrodes utilizing all the investigated textiles for sampling. It was found that in order to extend the application of textile-based sampling toward environmental analysis of ions it will be necessary to tailor the physio-chemical properties of the textile materials. In general, textile-based sampling opens new possibilities for direct chemical analysis of small-volume samples and provide a simple and low-cost method to screen various textiles for their effects on samples to identify which textiles are the most suitable for on-body sensing.

  18. Real-time potentiometric detection of bacteria in complex samples.

    Science.gov (United States)

    Zelada-Guillén, Gustavo A; Bhosale, Suryakant V; Riu, Jordi; Rius, F Xavier

    2010-11-15

    Detecting and identifying pathogen bacteria is essential to ensure quality at all stages of the food chain and to diagnose and control microbial infections. Traditional detection methods, including those based on cell culturing, are tedious and time-consuming, and their further application in real samples generally implies more complex pretreatment steps. Even though state-of-the-art techniques for detecting microorganisms enable the quantification of very low concentrations of bacteria, to date it has been difficult to obtain successful results in real samples in a simple, reliable, and rapid manner. In this Article, we demonstrate that the label-free detection and identification of living bacteria in real samples can be carried out in a couple of minutes and in a direct, simple, and selective way at concentration levels as low as 6 colony forming units/mL (CFU) in complex matrices such as milk or 26 CFU/mL in apple juice where the pretreatment step of samples is extremely easy. We chose Escherichia coli ( E. coli ) CECT 675 cells as a model organism as a nonpathogenic surrogate for pathogenic E. coli O157:H7 to test the effectiveness of a potentiometric aptamer-based biosensor. This biosensor uses single-walled carbon nanotubes (SWCNT) as excellent ion-to-electron transducers and covalently immobilized aptamers as biorecognition elements. The selective aptamer-target interaction significantly changes the electrical potential, thus allowing for both interspecies and interstrain selectivity and enabling the direct detection of the target. This technique is therefore a powerful tool for the immediate identification and detection of microorganisms. We demonstrate the highly selective detection of living bacteria with an immediate linear response of up to 10(4) CFU/mL. The biosensor can be easily built and used, is regenerated without difficulty, and can be used at least five times with no loss in the minimum amount of detected bacteria.

  19. Factors determining nestedness in complex networks

    CERN Document Server

    Johnson, Samuel; Munoz, Miguel A

    2013-01-01

    Understanding the causes and effects of network structural features is a key task in deciphering complex systems. In this context, the property of network nestedness has aroused a fair amount of interest as regards ecological networks. Indeed, Bastolla et al. introduced a simple measure of network nestedness which opened the door to analytical understanding, allowing them to conclude that biodiversity is strongly enhanced in highly nested mutualistic networks. Here, we suggest a slightly refined version of such a measure and go on to study how it is influenced by the most basic structural properties of networks, such as degree distribution and degree-degree correlations (i.e. assortativity). We find that heterogeneity in the degree has a very strong influence on nestedness. Once such an influence has been discounted, we find that nestedness is strongly correlated with disassortativity and hence, as random (neutral) networks have been recently found to be naturally disassortative, they tend to be naturally nes...

  20. Rapid determination of 226Ra in environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Maxwell, Sherrod L.; Culligan, Brian K.

    2012-02-04

    A new rapid method for the determination of {sup 228}Ra in natural water samples has been developed at the SRNL/EBL (Savannah River National Lab/ Environmental Bioassay Laboratory) that can be used for emergency response or routine samples. While gamma spectrometry can be employed with sufficient detection limits to determine {sup 228}Ra in solid samples (via {sup 228}Ac) , radiochemical methods that employ gas flow proportional counting techniques typically provide lower MDA (Minimal Detectable Activity) levels for the determination of {sup 228}Ra in water samples. Most radiochemical methods for {sup 228}Ra collect and purify {sup 228}Ra and allow for {sup 228}Ac daughter ingrowth for ~36 hours. In this new SRNL/EBL approach, {sup 228}Ac is collected and purified from the water sample without waiting to eliminate this delay. The sample preparation requires only about 4 hours so that {sup 228}Ra assay results on water samples can be achieved in < 6 hours. The method uses a rapid calcium carbonate precipitation enhanced with a small amount of phosphate added to enhance chemical yields (typically >90%), followed by rapid cation exchange removal of calcium. Lead, bismuth, uranium, thorium and protactinium isotopes are also removed by the cation exchange separation. {sup 228}Ac is eluted from the cation resin directly onto a DGA Resin cartridge attached to the bottom of the cation column to purify {sup 228}Ac. DGA Resin also removes lead and bismuth isotopes, along with Sr isotopes and {sup 90}Y. La is used to determine {sup 228}Ac chemical yield via ICP-MS, but {sup 133}Ba can also be used instead if ICP-MS assay is not available. Unlike some older methods, no lead or strontium holdback carriers or continual readjustment of sample pH is required.

  1. Determining the vibrations between sensor and sample in SQUID microscopy

    Science.gov (United States)

    Schiessl, Daniel; Kirtley, John R.; Paulius, Lisa; Rosenberg, Aaron J.; Palmstrom, Johanna C.; Ullah, Rahim R.; Holland, Connor M.; Fung, Y.-K.-K.; Ketchen, Mark B.; Gibson, Gerald W.; Moler, Kathryn A.

    2016-12-01

    Vibrations can cause noise in scanning probe microscopies. Relative vibrations between the scanning sensor and the sample are important but can be more difficult to determine than absolute vibrations or vibrations relative to the laboratory. We measure the noise spectral density in a scanning SQUID microscope as a function of position near a localized source of magnetic field and show that we can determine the spectra of all three components of the relative sensor-sample vibrations. This method is a powerful tool for diagnosing vibrational noise in scanning microscopies.

  2. Generic parallel Wang-Landau sampling for complex systems

    Science.gov (United States)

    Li, Ying Wai; Vogel, Thomas; Landau, David P.; Wüst, Thomas

    2013-03-01

    We introduce a parallel realization for Wang-Landau sampling in Monte Carlo simulations based on a replica-exchange framework. The key idea is to split the entire energy range of the system under consideration into several smaller, overlapping sub intervals. The survey of configurational phase space can then be distributed over multiple processors, with exchanges of random walkers taking place in the overlapping energy windows. To demonstrate the robustness and advantages of this parallel scheme for the simulations of complex systems, we have applied it to protein adsorption problems using the HP lattice protein model[1]. The method gives significant speed-up and achieves strong scaling on small computer architectures like multi-core processors, with a possible improvement in accuracy. We believe that it could be potentially beneficial for large-scale petaflop machines.

  3. Factors Determining Nestedness in Complex Networks

    Science.gov (United States)

    Jonhson, Samuel; Domínguez-García, Virginia; Muñoz, Miguel A.

    2013-01-01

    Understanding the causes and effects of network structural features is a key task in deciphering complex systems. In this context, the property of network nestedness has aroused a fair amount of interest as regards ecological networks. Indeed, Bastolla et al. introduced a simple measure of network nestedness which opened the door to analytical understanding, allowing them to conclude that biodiversity is strongly enhanced in highly nested mutualistic networks. Here, we suggest a slightly refined version of such a measure of nestedness and study how it is influenced by the most basic structural properties of networks, such as degree distribution and degree-degree correlations (i.e. assortativity). We find that most of the empirically found nestedness stems from heterogeneity in the degree distribution. Once such an influence has been discounted – as a second factor – we find that nestedness is strongly correlated with disassortativity and hence – as random networks have been recently found to be naturally disassortative – they also tend to be naturally nested just as the result of chance. PMID:24069264

  4. Determination of ziram in vegetable samples by square wave voltammetry

    Institute of Scientific and Technical Information of China (English)

    Ping Qiu; Yong Nian Ni

    2008-01-01

    The electrochemical behaviour and electrode reaction mechanism of ziram (zinc-dimethyl dithiocarbamate) on a hanging mercury drop electrode were investigated in Britton-Robinson (B-R) buffer by using cyclic and square wave voltammetry (SWV).Based on these studies a voltammetric method for determination of ziram was developed and applied to determine the ziram in synthetic and spiked vegetable samples,satisfactory results were obtained in both eases.

  5. Chemometric and Statistical Analyses of ToF-SIMS Spectra of Increasingly Complex Biological Samples

    Energy Technology Data Exchange (ETDEWEB)

    Berman, E S; Wu, L; Fortson, S L; Nelson, D O; Kulp, K S; Wu, K J

    2007-10-24

    Characterizing and classifying molecular variation within biological samples is critical for determining fundamental mechanisms of biological processes that will lead to new insights including improved disease understanding. Towards these ends, time-of-flight secondary ion mass spectrometry (ToF-SIMS) was used to examine increasingly complex samples of biological relevance, including monosaccharide isomers, pure proteins, complex protein mixtures, and mouse embryo tissues. The complex mass spectral data sets produced were analyzed using five common statistical and chemometric multivariate analysis techniques: principal component analysis (PCA), linear discriminant analysis (LDA), partial least squares discriminant analysis (PLSDA), soft independent modeling of class analogy (SIMCA), and decision tree analysis by recursive partitioning. PCA was found to be a valuable first step in multivariate analysis, providing insight both into the relative groupings of samples and into the molecular basis for those groupings. For the monosaccharides, pure proteins and protein mixture samples, all of LDA, PLSDA, and SIMCA were found to produce excellent classification given a sufficient number of compound variables calculated. For the mouse embryo tissues, however, SIMCA did not produce as accurate a classification. The decision tree analysis was found to be the least successful for all the data sets, providing neither as accurate a classification nor chemical insight for any of the tested samples. Based on these results we conclude that as the complexity of the sample increases, so must the sophistication of the multivariate technique used to classify the samples. PCA is a preferred first step for understanding ToF-SIMS data that can be followed by either LDA or PLSDA for effective classification analysis. This study demonstrates the strength of ToF-SIMS combined with multivariate statistical and chemometric techniques to classify increasingly complex biological samples

  6. RAPID DETERMINATION OF RA-226 IN ENVIRONMENTAL SAMPLES

    Energy Technology Data Exchange (ETDEWEB)

    Maxwell, S.

    2012-01-03

    A new rapid method for the determination of {sup 226}Ra in environmental samples has been developed at the Savannah River Site Environmental Lab (Aiken, SC, USA) that can be used for emergency response or routine sample analyses. The need for rapid analyses in the event of a Radiological Dispersive Device or Improvised Nuclear Device event is well-known. In addition, the recent accident at Fukushima Nuclear Power Plant in March, 2011 reinforces the need to have rapid analyses for radionuclides in environmental samples in the event of a nuclear accident. {sup 226}Ra (T1/2 = 1,620 years) is one of the most toxic of the long-lived alpha-emitters present in the environment due to its long life and its tendency to concentrate in bones, which increases the internal radiation dose of individuals. The new method to determine {sup 226}Ra in environmental samples utilizes a rapid sodium hydroxide fusion method for solid samples, calcium carbonate precipitation to preconcentrate Ra, and rapid column separation steps to remove interferences. The column separation process uses cation exchange resin to remove large amounts of calcium, Sr Resin to remove barium and Ln Resin as a final purification step to remove {sup 225}Ac and potential interferences. The purified {sup 226}Ra sample test sources are prepared using barium sulfate microprecipitation in the presence of isopropanol for counting by alpha spectrometry. The method showed good chemical recoveries and effective removal of interferences. The determination of {sup 226}Ra in environmental samples can be performed in less than 16 h for vegetation, concrete, brick, soil, and air filter samples with excellent quality for emergency or routine analyses. The sample preparation work takes less than 6 h. {sup 225}Ra (T1/2 = 14.9 day) tracer is used and the {sup 225}Ra progeny {sup 217}At is used to determine chemical yield via alpha spectrometry. The rapid fusion technique is a rugged sample digestion method that ensures that any

  7. Classifier-Guided Sampling for Complex Energy System Optimization

    Energy Technology Data Exchange (ETDEWEB)

    Backlund, Peter B. [Sandia National Laboratories (SNL-NM), Albuquerque, NM (United States); Eddy, John P. [Sandia National Laboratories (SNL-NM), Albuquerque, NM (United States)

    2015-09-01

    This report documents the results of a Laboratory Directed Research and Development (LDRD) effort enti tled "Classifier - Guided Sampling for Complex Energy System Optimization" that was conducted during FY 2014 and FY 2015. The goal of this proj ect was to develop, implement, and test major improvements to the classifier - guided sampling (CGS) algorithm. CGS is type of evolutionary algorithm for perform ing search and optimization over a set of discrete design variables in the face of one or more objective functions. E xisting evolutionary algorithms, such as genetic algorithms , may require a large number of o bjecti ve function evaluations to identify optimal or near - optimal solutions . Reducing the number of evaluations can result in significant time savings, especially if the objective function is computationally expensive. CGS reduce s the evaluation count by us ing a Bayesian network classifier to filter out non - promising candidate designs , prior to evaluation, based on their posterior probabilit ies . In this project, b oth the single - objective and multi - objective version s of the CGS are developed and tested on a set of benchm ark problems. As a domain - specific case study, CGS is used to design a microgrid for use in islanded mode during an extended bulk power grid outage.

  8. Power Analysis and Sample Size Determination in Metabolic Phenotyping.

    Science.gov (United States)

    Blaise, Benjamin J; Correia, Gonçalo; Tin, Adrienne; Young, J Hunter; Vergnaud, Anne-Claire; Lewis, Matthew; Pearce, Jake T M; Elliott, Paul; Nicholson, Jeremy K; Holmes, Elaine; Ebbels, Timothy M D

    2016-05-17

    Estimation of statistical power and sample size is a key aspect of experimental design. However, in metabolic phenotyping, there is currently no accepted approach for these tasks, in large part due to the unknown nature of the expected effect. In such hypothesis free science, neither the number or class of important analytes nor the effect size are known a priori. We introduce a new approach, based on multivariate simulation, which deals effectively with the highly correlated structure and high-dimensionality of metabolic phenotyping data. First, a large data set is simulated based on the characteristics of a pilot study investigating a given biomedical issue. An effect of a given size, corresponding either to a discrete (classification) or continuous (regression) outcome is then added. Different sample sizes are modeled by randomly selecting data sets of various sizes from the simulated data. We investigate different methods for effect detection, including univariate and multivariate techniques. Our framework allows us to investigate the complex relationship between sample size, power, and effect size for real multivariate data sets. For instance, we demonstrate for an example pilot data set that certain features achieve a power of 0.8 for a sample size of 20 samples or that a cross-validated predictivity QY(2) of 0.8 is reached with an effect size of 0.2 and 200 samples. We exemplify the approach for both nuclear magnetic resonance and liquid chromatography-mass spectrometry data from humans and the model organism C. elegans.

  9. Crystallization and Structure Determination of Superantigens and Immune Receptor Complexes.

    Science.gov (United States)

    Rödström, Karin E J; Lindkvist-Petersson, Karin

    2016-01-01

    Structure determination of superantigens and the complexes they form with immune receptors have over the years provided insight in their modes of action. This technique requires growing large and highly ordered crystals of the superantigen or receptor-superantigen complex, followed by exposure to X-ray radiation and data collection. Here, we describe methods for crystallizing superantigens and superantigen-receptor complexes using the vapor diffusion technique, how the crystals may be optimized, and lastly data collection and structure determination.

  10. Experimental determination of size distributions: analyzing proper sample sizes

    Science.gov (United States)

    Buffo, A.; Alopaeus, V.

    2016-04-01

    The measurement of various particle size distributions is a crucial aspect for many applications in the process industry. Size distribution is often related to the final product quality, as in crystallization or polymerization. In other cases it is related to the correct evaluation of heat and mass transfer, as well as reaction rates, depending on the interfacial area between the different phases or to the assessment of yield stresses of polycrystalline metals/alloys samples. The experimental determination of such distributions often involves laborious sampling procedures and the statistical significance of the outcome is rarely investigated. In this work, we propose a novel rigorous tool, based on inferential statistics, to determine the number of samples needed to obtain reliable measurements of size distribution, according to specific requirements defined a priori. Such methodology can be adopted regardless of the measurement technique used.

  11. Determination of technetium-99 in environmental samples: A review

    DEFF Research Database (Denmark)

    Shi, Keliang; Hou, Xiaolin; Roos, Per

    2012-01-01

    Due to the lack of a stable technetium isotope, and the high mobility and long half-life, 99Tc is considered to be one of the most important radionuclides in safety assessment of environmental radioactivity as well as nuclear waste management. 99Tc is also an important tracer for oceanographic...... research due to the high technetium solubility in seawater as TcO4−. A number of analytical methods, using chemical separation combined with radiometric and mass spectrometric measurement techniques, have been developed over the past decades for determination of 99Tc in different environmental samples....... This article summarizes and compares recently reported chemical separation procedures and measurement methods for determination of 99Tc. Due to the extremely low concentration of 99Tc in environmental samples, the sample preparation, pre-concentration, chemical separation and purification for removal...

  12. Method of determining an electrical property of a test sample

    DEFF Research Database (Denmark)

    2010-01-01

    A method of obtaining an electrical property of a test sample, comprising a non-conductive area and a conductive or semi-conductive test area, byperforming multiple measurements using a multi-point probe. The method comprising the steps of providing a magnetic field having field lines passing...... each tip, selecting one tip to be a current source positioned between conductive tips being used for determining a voltage in the test sample, performing a first measurement, moving the probe and performing a second measurement, calculating on the basis of the first and second measurement...... perpendicularly through the test area, bringing the probe into a first position on the test area, the conductive tips of the probe being in contact with the test area, determining a position for each tip relative to the boundary between the non- conductive area and the test area, determining distances between...

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

    Science.gov (United States)

    Morgan, Timothy M; Case, L Douglas

    2013-07-05

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

  14. Cheap in situ voltammetric copper determination from freshwater samples

    Directory of Open Access Journals (Sweden)

    David I. G.

    2013-04-01

    Full Text Available Detection of low concentrations of heavy metals in environmental samples is of particular interest because most of them represent persistent, highly toxic pollutants. Cu2+ detection in environmental samples is important because it is typical heavy metal, being an essential element for human beings but at higher concentrations it can create health risks. Due to the accumulation steps involved, anodic stripping voltammetry (ASV is one of the most sensitive techniques used for the detection of low concentrations of metal ions form different environmental samples. In order to minimize sample loss during sample collection, storage and transportation it is of particular interest to perform in situ rapid and reliable routine analysis. In the present paper we describe the use of a simple, disposable pencil graphite electrode (PGE for the determination of Cu from river water samples by mercury film anodic stripping voltammetry. The investigated water samples were collected during a period of 3 years (2009-2011, from six sampling points situated along the lower part of the Prut River (Romania. ASV measurements were performed in the presence of Hg2+ in 0.1 M HNO3 at a carbon pencil graphite working electrode. Standard addition method was applied for the quantification of Cu2+. The Cu2+ content of the most river water samples analysed exceeded 2 ⎧g/L (MEWM, 2006, the maximum admitted concentration for surface waters, and these could be due to the anthropogenic activities in the region (e.g. the largest steel factory in Romania is located in the vicinity of the sampling area. Samples show an additional importance as the region is included in a protected area, Lower Prut Floodplain Natural Park, and trace elements transfer along the aquatic food chain has been previously documented (Matache et. al, 2012. The results obtained by ASV on PGE agreed well with those obtained by inductively coupled plasma atomic emission spectrometry (ICP-AES using the Romanian

  15. Determination of critical micelle concentration with the rotating sample system.

    Science.gov (United States)

    Kao, Linus T; Shetty, Gautam N; Gratzl, Miklós

    2008-12-01

    A novel experimental approach using the rotating sample system (RSS) is proposed here for the determination of the critical micelle concentration (CMC) of surfactants. The RSS has been conceived in our laboratory as a convection platform for physicochemical studies and analyses in microliter-sized sample drops. The scheme allows for vigorous rotation of the drop despite its small size through efficient air-liquid mechanical coupling. Thus, changes in surface properties of aqueous samples result in corresponding modulation of the hydrodynamic performance of the RSS, which can be utilized to investigate interfacial phenomena. In this work, we demonstrate that the RSS can be used to study the effects of surfactants on the surface and in the bulk of very small samples with hydrodynamic electrochemistry. Potassium ferrocyanide is employed here with cyclic voltammetry to probe the air-water interface of solutions containing Triton X-100. The CMC of this surfactant determined using this approach is 140 ppm, which agrees well with reported values obtained with conventional methods in much larger samples. The results also demonstrate that besides the CMC, variations in bulk rheological properties can also be investigated in very small specimens using the RSS with a simple method.

  16. DETERMINATION OF RADIUM AND RADON CONCENTRATIONS IN SOME ROCK SAMPLES

    OpenAIRE

    BAYKARA, Oktay

    2006-01-01

    The concentrations of radium (226Ra), radon (222Rn) and radon exhalation rate in nine rock samples have been determined using solid-state nuclear track detectors (CR-39). The measured maximum values of radium, radon and radon exhalation rate in rock samples were found to be 24.62 Bq/kg, 4911.32 Bq/m3 and 4,86 Bqm-2h-1, respectively. Linear correlation was observed among radon concentration, radon exhalation and radium concentration. The linear correlation coefficient between radium content an...

  17. Chemometrics-assisted spectrophotometric method for simultaneous determination of Pb2+ and Cu2+ ions in different foodstuffs, soil and water samples using 2-benzylspiro [isoindoline-1,5‧-oxazolidine]-2‧,3,4‧-trione using continuous wavelet transformation and partial least squares - Calculation of pKf of complexes with rank annihilation factor analysis

    Science.gov (United States)

    Abbasi Tarighat, Maryam; Nabavi, Masoume; Mohammadizadeh, Mohammad Reza

    2015-06-01

    A new multi-component analysis method based on zero-crossing point-continuous wavelet transformation (CWT) was developed for simultaneous spectrophotometric determination of Cu2+ and Pb2+ ions based on the complex formation with 2-benzyl espiro[isoindoline-1,5oxasolidine]-2,3,4 trione (BSIIOT). The absorption spectra were evaluated with respect to synthetic ligand concentration, time of complexation and pH. Therefore according the absorbance values, 0.015 mmol L-1 BSIIOT, 10 min after mixing and pH 8.0 were used as optimum values. The complex formation between BSIIOT ligand and the cations Cu2+ and Pb2+ by application of rank annihilation factor analysis (RAFA) were investigated. Daubechies-4 (db4), discrete Meyer (dmey), Morlet (morl) and Symlet-8 (sym8) continuous wavelet transforms for signal treatments were found to be suitable among the wavelet families. The applicability of new synthetic ligand and selected mother wavelets were used for the simultaneous determination of strongly overlapped spectra of species without using any pre-chemical treatment. Therefore, CWT signals together with zero crossing technique were directly applied to the overlapping absorption spectra of Cu2+ and Pb2+. The calibration graphs for estimation of Pb2+ and Cu 2+were obtained by measuring the CWT amplitudes at zero crossing points for Cu2+ and Pb2+ at the wavelet domain, respectively. The proposed method was validated by simultaneous determination of Cu2+ and Pb2+ ions in red beans, walnut, rice, tea and soil samples. The obtained results of samples with proposed method have been compared with those predicted by partial least squares (PLS) and flame atomic absorption spectrophotometry (FAAS).

  18. Using the modified sample entropy to detect determinism

    Energy Technology Data Exchange (ETDEWEB)

    Xie Hongbo, E-mail: xiehb@sjtu.or [Department of Health Technology and Informatics, The Hong Kong Polytechnic University, Hung Hom, Kowloon (Hong Kong); Department of Biomedical Engineering, Jiangsu University, Zhenjiang (China); Guo Jingyi [Department of Health Technology and Informatics, Hong Kong Polytechnic University, Hung Hom, Kowloon (Hong Kong); Zheng Yongping, E-mail: ypzheng@ieee.or [Department of Health Technology and Informatics, Hong Kong Polytechnic University, Hung Hom, Kowloon (Hong Kong); Reseach Institute of Innovative Products and Technologies, Hong Kong Polytechnic University (Hong Kong)

    2010-08-23

    A modified sample entropy (mSampEn), based on the nonlinear continuous and convex function, has been proposed and proven to be superior to the standard sample entropy (SampEn) in several aspects. In this Letter, we empirically investigate the ability of the mSampEn statistic combined with surrogate data method to detect determinism. The effects of the datasets length and noise on the proposed method to differentiate between deterministic and stochastic dynamics are tested on several benchmark time series. The noise performance of the mSampEn statistic is also compared with the singular value decomposition (SVD) and symplectic geometry spectrum (SGS) based methods. The results indicate that the mSampEn statistic is a robust index for detecting determinism in short and noisy time series.

  19. Instantaneous GNSS attitude determination: A Monte Carlo sampling approach

    Science.gov (United States)

    Sun, Xiucong; Han, Chao; Chen, Pei

    2017-04-01

    A novel instantaneous GNSS ambiguity resolution approach which makes use of only single-frequency carrier phase measurements for ultra-short baseline attitude determination is proposed. The Monte Carlo sampling method is employed to obtain the probability density function of ambiguities from a quaternion-based GNSS-attitude model and the LAMBDA method strengthened with a screening mechanism is then utilized to fix the integer values. Experimental results show that 100% success rate could be achieved for ultra-short baselines.

  20. Spectrophotometric Determination of Fenpropathrin in its Formulations and Water Samples

    OpenAIRE

    B. Krishna Priya; Subrahmanyam, P.; Dakshayani, K.; P. Chiranjeevi

    2007-01-01

    Novel spectrophotometric methods were developed for the determination of fenpropathrin in insecticidal formulations and water samples. The methods were based on the hydrolysis of fenpropathrin with ethanolic KOH to form 3-phenoxy benzaldehyde. The resultant aldehyde group was condensed with anthranilic acid in presence of basic medium to form yellowish red color product having λmax of 485 nm or condensed with 2-chloro phenyl hydrazine to form pink color product having λmax of 557 nm. The colo...

  1. Microbiosensors for determination of glucose in the blood sample

    Institute of Scientific and Technical Information of China (English)

    金鹏; 谭久彬; 孙凯

    2002-01-01

    Describes the general design of Microbiosensors for determination of glucose in blood sample for medical purpose as an important branch of medical analysis instrument discusses the fabrication of microbiosensors. By the technology of microfabrication, self-assembled monolayers (SAMs) and enzyme immobilization, stresses their properties, such as improvement in system efficiency, shorter analysis time reduction of reagent waste and reduction of device sizes, which makes them suitable for bed-side monitor of emergency patients.

  2. Determination of chloride in geological samples by ion chromatography

    Science.gov (United States)

    Wilson, S.A.; Gent, C.A.

    1983-01-01

    Samples of silicate rocks are prepared by sodium carbonate fusion and then treated by ion chromatography. The method was tested for geological standards with chloride concentration between 0.003 and 3%. Observed chloride concentrations comparedd favorably with literature values. The relative standard deviation and detection limit for the method were 8% and 7 ppm, respectively. Up to 30 determination per 24-hour period were possible. ?? 1983.

  3. RAPID DETERMINATION OF {sup 210} PO IN WATER SAMPLES

    Energy Technology Data Exchange (ETDEWEB)

    Maxwell, S.

    2013-05-22

    A new rapid method for the determination of {sup 210}Po in water samples has been developed at the Savannah River National Laboratory (SRNL) that can be used for emergency response or routine water analyses. If a radiological dispersive device (RDD) event or a radiological attack associated with drinking water supplies occurs, there will be an urgent need for rapid analyses of water samples, including drinking water, ground water and other water effluents. Current analytical methods for the assay of {sup 210}Po in water samples have typically involved spontaneous auto-deposition of {sup 210}Po onto silver or other metal disks followed by counting by alpha spectrometry. The auto-deposition times range from 90 minutes to 24 hours or more, at times with yields that may be less than desirable. If sample interferences are present, decreased yields and degraded alpha spectrums can occur due to unpredictable thickening in the deposited layer. Separation methods have focused on the use of Sr Resin, often in combination with 210Pb analysis. A new rapid method for {sup 210}Po in water samples has been developed at the Savannah River National Laboratory (SRNL) that utilizes a rapid calcium phosphate co-precipitation method, separation using DGA Resin (N,N,N,N-tetraoctyldiglycolamide extractant-coated resin, Eichrom Technologies or Triskem-International), followed by rapid microprecipitation of {sup 210}Po using bismuth phosphate for counting by alpha spectrometry. This new method can be performed quickly with excellent removal of interferences, high chemical yields and very good alpha peak resolution, eliminating any potential problems with the alpha source preparation for emergency or routine samples. A rapid sequential separation method to separate {sup 210} Po and actinide isotopes was also developed. This new approach, rapid separation with DGA Resin plus microprecipitation for alpha source preparation, is a significant advance in radiochemistry for the rapid

  4. Extractive Spectrophotometric determination of Dimethoate in Environmental Samples with Azure-B

    Directory of Open Access Journals (Sweden)

    K. M. Reddy

    2005-01-01

    Full Text Available A new simple and selective spectrophotometric method is developed for the determination of dimethoate by using Azure-B is described. The method was based on the alkaline hydrolysis of dimethoate in presence of sodium ethoxide to form sodium dimethyl dithiophosphate (Na-DMDTP. The Na-DMDTP was formed as an ion-pair complex with cationic dye, azure-B. The ion-pair complex was extracted into chloroform. The color of the organic layer was measured at 535 nm. The method was applied to the determination of dimethoate residues in water, grain and soil samples.

  5. On-capillary sample cleanup method for the electrophoretic determination of carbohydrates in juice samples.

    Science.gov (United States)

    Morales-Cid, Gabriel; Simonet, Bartolomé M; Cárdenas, Soledad; Valcárcel, Miguel

    2007-05-01

    On many occasions, sample treatment is a critical step in electrophoretic analysis. As an alternative to batch procedures, in this work, a new strategy is presented with a view to develop an on-capillary sample cleanup method. This strategy is based on the partial filling of the capillary with carboxylated single-walled carbon nanotube (c-SWNT). The nanoparticles retain interferences from the matrix allowing the determination and quantification of carbohydrates (viz glucose, maltose and fructose). The precision of the method for the analysis of real samples ranged from 5.3 to 6.4%. The proposed method was compared with a method based on a batch filtration of the juice sample through diatomaceous earth and further electrophoretic determination. This method was also validated in this work. The RSD for this other method ranged from 5.1 to 6%. The results obtained by both methods were statistically comparable demonstrating the accuracy of the proposed methods and their effectiveness. Electrophoretic separation of carbohydrates was achieved using 200 mM borate solution as a buffer at pH 9.5 and applying 15 kV. During separation, the capillary temperature was kept constant at 40 degrees C. For the on-capillary cleanup method, a solution containing 50 mg/L of c-SWNTs prepared in 300 mM borate solution at pH 9.5 was introduced for 60 s into the capillary just before sample introduction. For the electrophoretic analysis of samples cleaned in batch with diatomaceous earth, it is also recommended to introduce into the capillary, just before the sample, a 300 mM borate solution as it enhances the sensitivity and electrophoretic resolution.

  6. Isotope determination of sulfur by mass spectrometry in soil samples

    Directory of Open Access Journals (Sweden)

    Alexssandra Luiza Rodrigues Molina Rossete

    2012-12-01

    Full Text Available Sulphur plays an essential role in plants and is one of the main nutrients in several metabolic processes. It has four stable isotopes (32S, 33S, 34S, and 36S with a natural abundance of 95.00, 0.76, 4.22, and 0.014 in atom %, respectively. A method for isotopic determination of S by isotope-ratio mass spectrometry (IRMS in soil samples is proposed. The procedure involves the oxidation of organic S to sulphate (S-SO4(2-, which was determined by dry combustion with alkaline oxidizing agents. The total S-SO4(2- concentration was determined by turbidimetry and the results showed that the conversion process was adequate. To produce gaseous SO2 gas, BaSO4 was thermally decomposed in a vacuum system at 900 ºC in the presence of NaPO3. The isotope determination of S (atom % 34S atoms was carried out by isotope ratio mass spectrometry (IRMS. In this work, the labeled material (K2(34SO4 was used to validate the method of isotopic determination of S; the results were precise and accurate, showing the viability of the proposed method.

  7. Expert system for determination of fumonisins in corn samples

    Directory of Open Access Journals (Sweden)

    Abramović Biljana F.

    2005-01-01

    Full Text Available An expert system (ES to solve the problem of choosing an optimal procedure for the determination of fumonisins in corn samples was developed, having in mind that these toxins most frequently contaminate this particular cereal. In constructing the ES use was made of the deterministic approach starting from the assumption that the experts in the field have a profound knowledge about the problem in question. The ES knowledge base contains the solutions that have been published in the pertinent literature, as well as some solutions and recommendations, which we have developed and introduced. On the basis of this information, as well as on the basis of the demanded method detection limit, available equipment, chemicals, as well as the time the experimenter has at his disposal for the determination, the ES proposes a procedure for solving the given analytical problem, starting from sampling, preparation of all the necessary solutions, the appropriate apparatus, probe preparation, the mode of determining results, calculation of the results, and provides a survey of all the relevant literature references. The base of ES is a shell, which can work under a variety of Microsoft Windows operating systems. In the development of ES and its adaptation for users who are not familiar with computer techniques, different tools, which operate with Microsoft Windows operating systems, as well as the tools within Microsoft Office are used.

  8. Forensic study of sex determination using PCR on teeth samples.

    Directory of Open Access Journals (Sweden)

    Murakami H

    2000-02-01

    Full Text Available In this study, sex determination using polymerase chain reaction (PCR on tooth material was evaluated from the viewpoint of forensic medicine. The sensitivity of PCR for detection of the Y chromosome-specific alphoid repeat sequence and the X chromosome-specific alphoid repeat sequence was 0.5 pg of genomic DNA. Sex could be determined by PCR of DNA extracted from the pulp of 16 freshly extracted permanent teeth and dentine including the surface of the pulp cavity of 6 freshly extracted milk teeth. Sex could be determined using the pulp in all 20 teeth (10 male and 10 female preserved at room temperature for 22 years. For the pulp of teeth stored in sea water, the sex could be determined in all 8 teeth immersed for 1 week and in 5 of 6 teeth immersed for 4 weeks. In the remaining 1 tooth, in which sex determination based on the pulp failed, the sex could be determined correctly when DNA extracted from the tooth hard tissue was examined. For teeth stored in soil, the sex could be determined accurately in all 8 teeth buried for 1 week, 7 of 8 teeth buried for 4 weeks, and in all 6 teeth buried for 8 weeks. When teeth were heated for 30 min, sex determination from the pulp was possible in all teeth heated to 100, 150, and 200 degrees C, and even in some teeth heated to 250 degrees C. When this method was applied to actual forensic cases, the sex of a mummified body estimated to have been discovered half a year to 1 year after death could be determined readily by examination of the dental pulp. In the skeletons of 2 bodies placed under water for approximately 1 year and approximately 11 years and 7 months, pulp tissues had been dissolved and lost, but sex determination was possible using DNA extracted from hard dental tissues. These results indicate that this method is useful in forensic practices for sex determination based on teeth samples.

  9. Determining the Bayesian optimal sampling strategy in a hierarchical system.

    Energy Technology Data Exchange (ETDEWEB)

    Grace, Matthew D.; Ringland, James T.; Boggs, Paul T.; Pebay, Philippe Pierre

    2010-09-01

    Consider a classic hierarchy tree as a basic model of a 'system-of-systems' network, where each node represents a component system (which may itself consist of a set of sub-systems). For this general composite system, we present a technique for computing the optimal testing strategy, which is based on Bayesian decision analysis. In previous work, we developed a Bayesian approach for computing the distribution of the reliability of a system-of-systems structure that uses test data and prior information. This allows for the determination of both an estimate of the reliability and a quantification of confidence in the estimate. Improving the accuracy of the reliability estimate and increasing the corresponding confidence require the collection of additional data. However, testing all possible sub-systems may not be cost-effective, feasible, or even necessary to achieve an improvement in the reliability estimate. To address this sampling issue, we formulate a Bayesian methodology that systematically determines the optimal sampling strategy under specified constraints and costs that will maximally improve the reliability estimate of the composite system, e.g., by reducing the variance of the reliability distribution. This methodology involves calculating the 'Bayes risk of a decision rule' for each available sampling strategy, where risk quantifies the relative effect that each sampling strategy could have on the reliability estimate. A general numerical algorithm is developed and tested using an example multicomponent system. The results show that the procedure scales linearly with the number of components available for testing.

  10. A general method to determine sampling windows for nonlinear mixed effects models with an application to population pharmacokinetic studies.

    Science.gov (United States)

    Foo, Lee Kien; McGree, James; Duffull, Stephen

    2012-01-01

    Optimal design methods have been proposed to determine the best sampling times when sparse blood sampling is required in clinical pharmacokinetic studies. However, the optimal blood sampling time points may not be feasible in clinical practice. Sampling windows, a time interval for blood sample collection, have been proposed to provide flexibility in blood sampling times while preserving efficient parameter estimation. Because of the complexity of the population pharmacokinetic models, which are generally nonlinear mixed effects models, there is no analytical solution available to determine sampling windows. We propose a method for determination of sampling windows based on MCMC sampling techniques. The proposed method attains a stationary distribution rapidly and provides time-sensitive windows around the optimal design points. The proposed method is applicable to determine sampling windows for any nonlinear mixed effects model although our work focuses on an application to population pharmacokinetic models. Copyright © 2012 John Wiley & Sons, Ltd.

  11. Biosensor for determination of glucose in real samples of beverages

    Directory of Open Access Journals (Sweden)

    Flavio Marques Lopes

    2012-03-01

    Full Text Available A biosensor was developed for spectrophotometric determination of glucose concentrations in real samples of orange juice energetic drinks, and sport drinks. The biosensor consisted of glucose oxidase (GOD and horseradish peroxidase (HRP immobilized onto polyaniline activated with glutaraldehyde (PANIG. Immobilization parameters were optimized for GOD, and maximum immobilization yield was 16% when 5.0 mg of PANIG and 8.9 U prepared in 0.1 mol.L-1 sodium phosphate buffer (pH 7.0 reacted for 60 minutes at 4 °C with gentle stirring. The linear operational range for glucose determination using optimized operational parameters was between 0.05 and 6.0 mg.mL-1 with a very good reproducibility of response. The results obtained in the biosensor were compared with those obtained using free enzymes (commercial kits and then validated through statistical analysis using the Tukey test (95% confidence interval.

  12. Direct rapid determination of traces of sulfide in environment samples

    Institute of Scientific and Technical Information of China (English)

    郭方遒; 黄兰芳; 梁逸曾

    2002-01-01

    An improved ethylene blue method for determination of sulfide is developed. It has been adapted to a direct determination of sulfide by both common spectrophotometric method and total differential spectrophotometric method. In common spectrophotometric method, the calibration curve is A=1.69ρ+0.006 and the correlation coefficient is 0.9994.The apparent molar absorptivity is 5.42×104 L*mol-1*cm-1 and calibration curve is liner when ρ is in the range of 0-0.9 mg*L-1. In total differential spectrophotometric method, the calibration curve is A=9.25ρ+0.004 and the correlation coefficient is 0.9996. The apparent molar absorptivity is 2.96×105 L*mol-1*cm-1and calibration curve is liner when ρ is in the range of 0-0.10 mg*L-1. The sensitivity of this method is increased significantly compared with the former ethylene blue method. The speed of reaction is also faster than the former one. The limit of detection is found to be 1.0 ng*mL-1 by both common spectrophotometric method and total differential spectrophotometric method. Ten replicate analyses of a sample solution containing 100 ng*mL-1sulfide give a relative standard deviation of 1.8%. The effects of various cations and anions on the determination of sulfide are studied and procedures for removal of interference is described. The method is used for the determination of sulfide in environment samples with satisfactory results.

  13. Calibration of the complex matrix effects on the sampling of polycyclic aromatic hydrocarbons in milk samples using solid phase microextraction.

    Science.gov (United States)

    Lin, Wei; Wei, Songbo; Jiang, Ruifen; Zhu, Fang; Ouyang, Gangfeng

    2016-08-24

    Solid phase microextraction (SPME), a simple, fast and promising sampling technique, has been widely used for complex sample analysis. However, complex matrices could modify the absorption property of coatings as well as the uptake kinetics of analytes, eventually biasing the quantification results. In the current study, we demonstrated the feasibility of a developed calibration method for the analysis of polycyclic aromatic hydrocarbons (PAHs) in complex milk samples. Effects of the complex matrices on the SPME sampling process and the sampling conditions were investigated. Results showed that short exposure time (pre-equilibrium SPME, PE-SPME) could increase the lifetime of coatings, and the complex matrices in milk samples could significantly influence the sampling kinetics of SPME. In addition, the optimized sampling time, temperature and dilution factor for PAHs were 10 min, 85 °C and 20, respectively. The obtained LODs and LOQs of all the PAHs were 0.1-0.8 ng/mL and 1.4-4.7 ng/mL, respectively. Furthermore, the accuracy of the proposed PE-SPME method for milk sampling was validated by the recoveries of the studied compounds in two concentration levels, which ranged from 75% to 110% for all the compounds. Finally, the proposed method was applied to the screening of PAHs in milk samples.

  14. Miniaturized sample preparation method for determination of amphetamines in urine.

    Science.gov (United States)

    Nishida, Manami; Namera, Akira; Yashiki, Mikio; Kimura, Kojiro

    2004-07-16

    A simple and miniaturized sample preparation method for determination of amphetamines in urine was developed using on-column derivatization and gas chromatography-mass spectrometry (GC-MS). Urine was directly applied to the extraction column that was pre-packed with Extrelut and sodium carbonate. Amphetamine (AP) and methamphetamine (MA) in urine were adsorbed on the surface of Extrelut. AP and MA were then converted to a free base and derivatized to N-propoxycarbonyl derivatives using propylchloroformate on the column. Pentadeuterated MA was used as an internal standard. The recoveries of AP and MA from urine were 100 and 102%, respectively. The calibration curves showed linearity in the range of 0.50-50 microg/mL for AP and MA in urine. When urine samples containing two different concentrations (0.50 and 5.0 microg/mL) of AP and MA were determined, the intra-day and inter-day coefficients of variation were 1.4-7.7%. This method was applied to 14 medico-legal cases of MA intoxication. The results were compared and a good agreement was obtained with a HPLC method.

  15. Analytical methodologies for the determination of benzodiazepines in biological samples.

    Science.gov (United States)

    Persona, Karolina; Madej, Katarzyna; Knihnicki, Paweł; Piekoszewski, Wojciech

    2015-09-10

    Benzodiazepine drugs belong to important and most widely used medicaments. They demonstrate such therapeutic properties as anxiolytic, sedative, somnifacient, anticonvulsant, diastolic and muscle relaxant effects. However, despite the fact that benzodiazepines possess high therapeutic index and are considered to be relatively safe, their use can be dangerous when: (1) co-administered with alcohol, (2) co-administered with other medicaments like sedatives, antidepressants, neuroleptics or morphine like substances, (3) driving under their influence, (4) using benzodiazepines non-therapeutically as drugs of abuse or in drug-facilitated crimes. For these reasons benzodiazepines are still studied and determined in a variety of biological materials. In this article, sample preparation techniques which have been applied in analysis of benzodiazepine drugs in biological samples have been reviewed and presented. The next part of the article is focused on a review of analytical methods which have been employed for pharmacological, toxicological or forensic study of this group of drugs in the biological matrices. The review was preceded by a description of the physicochemical properties of the selected benzodiazepines and two, very often coexisting in the same analyzed samples, sedative-hypnotic drugs.

  16. Fast identification of microplastics in complex environmental samples by a thermal degradation method.

    Science.gov (United States)

    Dümichen, Erik; Eisentraut, Paul; Bannick, Claus Gerhard; Barthel, Anne-Kathrin; Senz, Rainer; Braun, Ulrike

    2017-05-01

    In order to determine the relevance of microplastic particles in various environmental media, comprehensive investigations are needed. However, no analytical method exists for fast identification and quantification. At present, optical spectroscopy methods like IR and RAMAN imaging are used. Due to their time consuming procedures and uncertain extrapolation, reliable monitoring is difficult. For analyzing polymers Py-GC-MS is a standard method. However, due to a limited sample amount of about 0.5 mg it is not suited for analysis of complex sample mixtures like environmental samples. Therefore, we developed a new thermoanalytical method as a first step for identifying microplastics in environmental samples. A sample amount of about 20 mg, which assures the homogeneity of the sample, is subjected to complete thermal decomposition. The specific degradation products of the respective polymer are adsorbed on a solid-phase adsorber and subsequently analyzed by thermal desorption gas chromatography mass spectrometry. For certain identification, the specific degradation products for the respective polymer were selected first. Afterwards real environmental samples from the aquatic (three different rivers) and the terrestrial (bio gas plant) systems were screened for microplastics. Mainly polypropylene (PP), polyethylene (PE) and polystyrene (PS) were identified for the samples from the bio gas plant and PE and PS from the rivers. However, this was only the first step and quantification measurements will follow.

  17. Membrane optode for mercury(II) determination in aqueous samples

    Energy Technology Data Exchange (ETDEWEB)

    Kalyan, Y. [Department of Environmental Sciences, S.V. University, Tirupati 517502 (India); Pandey, A.K.; Bhagat, P.R.; Acharya, R.; Natarajan, V. [Radiochemistry Division, Bhabha Atomic Research Centre, Mumbai 400085 (India); Naidu, G.R.K. [Department of Environmental Sciences, S.V. University, Tirupati 517502 (India); Reddy, A.V.R., E-mail: avreddy@barc.gov.in [Radiochemistry Division, Bhabha Atomic Research Centre, Mumbai 400085 (India)

    2009-07-15

    A color changeable optode for Hg(II) was prepared by the immobilization of a dye 4-(2-pyridylazo)resorcinol (PAR) and a liquid ion-exchanger trioctylmethylammonium chloride (Aliquat-336) in the tri-(2-ethylhexyl) phosphate plasticized cellulose triacetate matrix. Hg(II) and CH{sub 3}Hg{sup +} from aqueous samples could be quantitatively preconcentrated in this transparent optode producing a distinct color change ({lambda}{sub max} = 520 nm) within 5 min equilibration time in bicarbonate aqueous medium or 30 min in natural water. Whereas optode sample without Aliquat-336 did not change its color corresponding to Hg-PAR complex on equilibrium with the same aqueous solution containing Hg(II) ions. The uptake of Hg(II) was found to be pH dependant with a maximum (>90%) at a pH 7.5. The uptake of ions like Cu(II), Fe(II), Zn(II) and Pb(II) was negligible in the optode where as the uptake of Cd(II) and Zn(II) ions was 10-15% at pH 7.5. The optode developed in the present work was studied for its analytical application for Hg(II) in the aqueous samples by spectrophotometry, radiotracer ({sup 203}Hg), Energy Dispersive X-ray Fluorescence (EDXRF) analyses and Instrumental Neutron Activation Analysis (INAA). The minimum amount of Hg(II) required to produce detectable response by spectrophotometry, INAA and EDXRF were found to be 5.5, 1 and 12 {mu}g, respectively. This optode showed a linear increase in the absorbance at {lambda}{sub max} = 520 nm over a concentration range of 0.22-1.32 {mu}g/mL of Hg(II) ions in aqueous solution for 5 min. The preconcentration of Hg(II) from large volume of aqueous solution was used to extend the lower limit of concentration range that can be quantified by the spectrophotometry of optode. It was observed that preconcentration of 11 {mu}g Hg(II) in 100 mL (0.11 {mu}g/mL) in aqueous samples gives a distinct color change and absorbance above 3{sigma} of the blank absorbance. The optode developed in the present work was found to be reusable.

  18. Determination of cell electroporation in small-volume samples.

    Science.gov (United States)

    Saulis, Gintautas; Praneviciŭte, Rita

    2007-01-01

    Expose of cells to electric field pulses increases the cell membrane permeability. Intracellular potassium ions leak out of the cells through aqueous pores created in the membrane. This release is used here for the determination of the fraction of electroporated cells. To determine cell membrane electroporation in small-volume samples (40-50 miacrol), mini both potassium ion-selective and reference electrodes, with tip diameters of 1-1.5 mm and minimum immersion depths of 1 mm, were utilized. The obtained calibration graph was linear within the concentration range 0.2-100 mM. The slope was 50-51 and 53-56 mV per concentration order at 10-11 and 19-21 degrees C, respectively. Detection limit of the electrode was determined to be 0.05-0.08 mM, however, it was possible to work down to concentrations in the range of 0.01 mM. Experiments have been carried out on human erythrocytes exposed to a square-wave electric pulse with the duration of 0.1-2 ms. The extracellular potassium concentrations were in the range between 0.04-0.08 mM (intact cells) and 3-5 mM (100% electroporation). The obtained dependences of the fraction of electroporated cells on the pulse intensity were of a sigmoid shape. The dependence of the pulse amplitude required to electroporate 50% of cells on the pulse duration, obtained from the release of intracellular potassium ions, coincided with the one determined from the extent of hemolysis after 24 h-incubation at low temperature.

  19. Aluminum complexation by catechol as determined by ultraviolet spectrophotometry

    Energy Technology Data Exchange (ETDEWEB)

    Sikora, F.J.; McBride, M.B.

    1989-03-01

    Methods of ultraviolet (UV) spectrophotometry were used to determine the stoichiometry and association constant for the Al-catechol complex from pH 3.8 to 4.6. Job's method of continuous variation indicated the Al-catechol complex had a 1:1 stoichiometry in the pH range studied. Aluminum titrations of catechol and pH titrations of catechol plus Al resulted in a shift in the UV spectra due to the formation of an Al-catechol complex absorbing UV radiation uniquely different than that of free catechol. General equations were developed for the determination of association constants assuming an organic and Al-organic complex absorb UV radiation. Aluminum titrations with constant catechol concentration yielded a log k/sub 0.1//sup c/ of 16.22 for a 1:1 Al-catechol complex. Calculated absorbance as a function of pH agree dwell with experimental pH titrations of solutions containing catechol plus Al. The fact that Al can be complexed by catechol at low pH indicates the o-hydroxy group provides a potential source for Al complexation in soil and surface waters.

  20. Determination of As, Mo, V, W in environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Ferri, T.; Sangiorgio, P.; Valentini, M. [Rome Univ. La Sapienza, Rome (Italy). Dipt. di Chmica; Morabito, R. [ENEA Centro Ricerche Casaccia, Rome (Italy). Dipt. Ambiente

    1999-10-01

    The paper describes the combined use of a preconcentration method using resin and ICP-AES (inductively coupled plasma atomic emission spectrometry) for determining As, Mo, V and W simultaneously in polluted waters and has been applied to five geological reference samples kindly supplied by USGS (united States Geological Survey). The method, whose reliability has been checked on standard reference materials by NIST (National Institute of Standards and Technology), is easy to apply and also characterized by good precision. [Italian] Il lavoro descrive l'uso combinato di una resina chelante come mezzo di preconcentrazione e l'ICP-AES (inductively coupled plasma atomic emission spectrometry) come mezzo di quantizzazione per determinare simultaneamente As, Mo, V, W nelle acque. Il metodo, che e' stato provato su materiale certificato dal NIST (National Institute of Standards and Technology), si e' dimostrato di facile impiego e caratterizzato da buona precisione.

  1. Determination of trihalomethanes in water samples: A review

    Energy Technology Data Exchange (ETDEWEB)

    Perez Pavon, Jose Luis [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias Quimicas, Universidad de Salamanca, 37008 Salamanca (Spain)], E-mail: jlpp@usal.es; Herrero Martin, Sara; Garcia Pinto, Carmelo; Moreno Cordero, Bernardo [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias Quimicas, Universidad de Salamanca, 37008 Salamanca (Spain)

    2008-11-23

    This article reviews the most recent literature addressing the analytical methods applied for trihalomethanes (THMs) determination in water samples. This analysis is usually performed with gas chromatography (GC) combined with a preconcentration step. The detectors most widely used in this type of analyses are mass spectrometers (MS) and electron capture detectors (ECD). Here, we review the analytical characteristics, the time required for analysis, and the simplicity of the optimised methods. The main difference between these methods lies in the sample pretreatment step; therefore, special emphasis is placed on this aspect. The techniques covered are direct aqueous injection (DAI), liquid-liquid extraction (LLE), headspace (HS), and membrane-based techniques. We also review the main chromatographic columns employed and consider novel aspects of chromatographic analysis, such as the use of fast gas chromatography (FGC). Concerning the detection step, besides the common techniques, the use of uncommon detectors such as fluorescence detector, pulsed discharge photoionization detector (PDPID), dry electrolytic conductivity detector (DELCD), atomic emission detector (AED) and inductively coupled plasma-mass spectrometry (ICP-MS) for this type of analysis is described.

  2. Methods for determining pesticides and polychlorinated biphenyls in food samples--problems and challenges.

    Science.gov (United States)

    Beyer, Angelika; Biziuk, Marek

    2008-11-01

    Determination of residual amounts of pesticides and polychlorinated biphenyls (PCBs) in food samples requires the use of specific techniques regarding sample preparation as well as instrumental analysis which should be characterized by a very low detection limit. A problem associated with the use of pesticides and PCBs is the need for controlling their residues in the environment, particularly in food, as these chemicals show a propensity to accumulate. The analysis of food samples for the presence of pesticides and PCBs brings on many difficulties because of the specificity of sample preparation consisting of multistep purification procedures of samples that contain trace amounts of an analyte. Concentration determinations of pollutants that easily dissolve in complex matrices, particularly in the presence of a large apportionment of interfering substances, pose a big challenge. Therefore, the basic step in food analysis for the presence of pesticides and PCBs is sample preparation which mainly consists of analyte enrichment and the removal of interfering substances. But all steps of the analytical procedure that include sample collection and preparation, extraction of analytes from matrix, extract purification, and final determination, are very significant; their precision and correct application have a decisive effect on the final result.

  3. Extractive spectrophotometric determination of Cobalt(II) in synthetic and pharmaceutical samples using Cyanex 923.

    Science.gov (United States)

    Reddy, B Ramachandra; Radhika, P; Kumar, J Rajesh; Priya, D Neela; Rajgopal, K

    2004-02-01

    Cyanex 923 has been proposed as a sensitive analytical reagent for the direct extractive spectrophotometric determination of cobalt(II). Cobalt(II) forms a blue-colored complex with Cyanex 923 in the organic phase. The maximum absorbance of the complex is measured at 635 nm. Beer's law was obeyed in the range 58.9 - 589.0 microg of cobalt. The molar absorptivitiy and Sandell's sensitivity of the complex was calculated to be 6.79 x 10920 l mol(-1) cm(-1) and 0.088 microg cm(-2), respectively. The nature of the extracted species was found to be Co(SCN)2 x 2S. An excellent linearity with a correlation coefficient value of 0.999 was obtained for the Co(II)-Cyanex 923 complex. Stability and regeneration of the reagent (Cyanex 923) for reuse is the main advantage of the present method. The method was successfully applied to the determination of cobalt in synthetic mixtures and pharmaceutical samples was found to give values close to the actual ones. Standard alloy samples, such as high-speed tool BCS 484 and 485, have been tested for the determination of cobalt for the purpose of validating the present method. The results of the proposed method are comparable with atomic absorption spectrometry and were found to be in good agreement.

  4. Extractive Spectrophotometric Determination of Fluconazole by Ion-pair Complex Formation with Bromocresol Green

    Institute of Scientific and Technical Information of China (English)

    JALALI,Fahimeh; RAJABI,Mohammad J.

    2007-01-01

    An extraction-spectrophotometric method for the determination of trace amounts of fluconazole was described.Fluconazole was effectively extracted as a 1 : 1 ion-pair complex with bromocresole green (BCG) at pH 3.0 into chloroform, followed by spectrophotometric determination at 420 nm. Beer's law was obeyed over the range of 4-procedure was applied to the determination of fluconazole in pharmaceutical preparations as well as its recovery from a blood serum sample.

  5. Application of a Dual-Arm Robot in Complex Sample Preparation and Measurement Processes.

    Science.gov (United States)

    Fleischer, Heidi; Drews, Robert Ralf; Janson, Jessica; Chinna Patlolla, Bharath Reddy; Chu, Xianghua; Klos, Michael; Thurow, Kerstin

    2016-10-01

    Automation systems with applied robotics have already been established in industrial applications for many years. In the field of life sciences, a comparable high level of automation can be found in the areas of bioscreening and high-throughput screening. Strong deficits still exist in the development of flexible and universal fully automated systems in the field of analytical measurement. Reasons are the heterogeneous processes with complex structures, which include sample preparation and transport, analytical measurements using complex sensor systems, and suitable data analysis and evaluation. Furthermore, the use of nonstandard sample vessels with various shapes and volumes results in an increased complexity. The direct use of existing automation solutions from bioscreening applications is not possible. A flexible automation system for sample preparation, analysis, and data evaluation is presented in this article. It is applied for the determination of cholesterol in biliary endoprosthesis using gas chromatography-mass spectrometry (GC-MS). A dual-arm robot performs both transport and active manipulation tasks to ensure human-like operation. This general robotic concept also enables the use of manual laboratory devices and equipment and is thus suitable in areas with a high standardization grade.

  6. Determination of complex microcalorimeter parameters with impedance measurements

    Energy Technology Data Exchange (ETDEWEB)

    Saab, T. [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States)]. E-mail: tsaab@phys.ufl.edu; Bandler, S.R. [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Chervenak, J. [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Figueroa-Feliciano, E. [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Finkbeiner, F. [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Iyomoto, N. [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Kelley, R.L. [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Kilbourne, C.A. [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Lindeman, M.A. [University of Wisconsin, Madison, WI 53706 (United States); Porter, F.S. [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States); Sadleir, J. [NASA Goddard Space Flight Center, Greenbelt, MD 20771 (United States)

    2006-04-15

    The proper understanding and modeling of a microcalorimeter's response requires accurate knowledge of a handful of parameters, such as C, G, {alpha}. While a few of these parameters are directly determined from the IV characteristics, some others, notoriously the heat capacity (C) and {alpha}, appear in degenerate combinations in most measurable quantities. The consideration of a complex microcalorimeter leads to an added ambiguity in the determination of the parameters. In general, the dependence of the microcalorimeter's complex impedance on these various parameters varies with frequency. This dependence allows us to determine individual parameters by fitting the prediction of the microcalorimeter model to impedance data. In this paper we describe efforts at characterizing the Goddard X-ray microcalorimeters. With the parameters determined by this method, we compare the pulse shape and noise spectra predictions to data taken with the same devices.

  7. Lanthanide complexes as luminogenic probes to measure sulfide levels in industrial samples.

    Science.gov (United States)

    Thorson, Megan K; Ung, Phuc; Leaver, Franklin M; Corbin, Teresa S; Tuck, Kellie L; Graham, Bim; Barrios, Amy M

    2015-10-08

    A series of lanthanide-based, azide-appended complexes were investigated as hydrogen sulfide-sensitive probes. Europium complex 1 and Tb complex 3 both displayed a sulfide-dependent increase in luminescence, while Tb complex 2 displayed a decrease in luminescence upon exposure to NaHS. The utility of the complexes for monitoring sulfide levels in industrial oil and water samples was investigated. Complex 3 provided a sensitive measure of sulfide levels in petrochemical water samples (detection limit ∼ 250 nM), while complex 1 was capable of monitoring μM levels of sulfide in partially refined crude oil.

  8. Adsorptive stripping voltammetric determination of trace amounts of lead in environmental water samples with complicated matrix

    Directory of Open Access Journals (Sweden)

    Grabarczyk M.

    2013-04-01

    Full Text Available A sensitive, simple and fast adsorptive stripping voltammetric procedure for trace determination of lead in environmental water samples has been developed. The method is based on adsorptive accumulation of the Pb(II-cupferron complex onto a hanging mercury drop electrode, followed by the reduction of the adsorbed species by a voltammetric scan using differential pulse modulation. The interference from surface active substances was eliminated by adsorption of interferents onto an Amberlite XAD-16 resin. Optimumconditions for removing the surfactants by mixing the analysed sample with resin were evaluated. The accuracy of the method was tested by analyzing certified reference material (SPS-WW1 Waste Water.

  9. ICDF Complex Waste Profile and Verification Sample Guidance

    Energy Technology Data Exchange (ETDEWEB)

    W. M. Heileson

    2006-10-01

    This guidance document will assist waste generators who characterize waste streams destined for disposal at the Idaho Comprehensive Environmental Response, Compensation, and Liability Act (CERCLA) Disposal Facility (ICDF) Complex. The purpose of this document is to develop a conservative but appropriate way to (1) characterize waste for entry into the ICDF; (2) ensure compliance with the waste acceptance criteria; and (3) facilitate disposal at the ICDF landfill or evaporation pond. In addition, this document will establish the waste verification process used by ICDF personnel to ensure that untreated waste meets applicable ICDF acceptance limits

  10. Handling complex effects in slurry-sampling-electrothermal atomic absorption spectrometry by multivariate calibration

    Energy Technology Data Exchange (ETDEWEB)

    Felipe-Sotelo, M. [Dept. Analytical Chemistry. University of A Coruna, Campus da Zapateira s/n, E-15071 A Coruna (Spain); Cal-Prieto, M.J. [Dept. Analytical Chemistry. University of A Coruna, Campus da Zapateira s/n, E-15071 A Coruna (Spain); Gomez-Carracedo, M.P. [Dept. Analytical Chemistry. University of A Coruna, Campus da Zapateira s/n, E-15071 A Coruna (Spain); Andrade, J.M. [Dept. Analytical Chemistry. University of A Coruna, Campus da Zapateira s/n, E-15071 A Coruna (Spain)]. E-mail: andrade@udc.es; Carlosena, A. [Dept. Analytical Chemistry. University of A Coruna, Campus da Zapateira s/n, E-15071 A Coruna (Spain); Prada, D. [Dept. Analytical Chemistry. University of A Coruna, Campus da Zapateira s/n, E-15071 A Coruna (Spain)

    2006-07-07

    Analysis of solid samples by slurry-sampling-electrothermal atomic absorption spectrometry (SS-ETAAS) can imply spectral and chemical interferences caused by the large amount of concomitants introduced into the graphite furnace. Sometimes they cannot be solved using stabilized temperature platform furnace (STPF) conditions or typical approaches (previous sample ashing, use of chemical modifiers, etc.), which are time consuming and quite expensive. A new approach to handle interferences using multivariate calibrations (partial least squares, PLS, and artificial neural networks, ANN) is presented and exemplified with a real problem consisting on determining Sb in several solid matrices (soils, sediments and coal fly ash) as slurries by ETAAS. Experimental designs were implemented at different levels of Sb to develop the calibration matrix and assess which concomitants (seven ions were considered) modified the atomic signal mostly. They were Na{sup +} and Ca{sup 2+} and they induced simultaneous displacement, depletion (enhancement) and broadening of the atomic peak. Here it is shown that these complex effects can be handled in a reliable, fast and cost-effective way to predict the concentration of Sb in slurry samples of several solid matrices. The method was validated predicting the concentrations of five certified reference materials (CRMs) and studying its robustness to current ETAAS problems. It is also shown that linear PLS can handle eventual non-linearities and that its results are comparable to more complex (non-linear) models, as those from ANNs.

  11. A neutron activation analysis procedure for the determination of uranium, thorium and potassium in geologic samples

    Science.gov (United States)

    Aruscavage, P. J.; Millard, H.T.

    1972-01-01

    A neutron activation analysis procedure was developed for the determination of uranium, thorium and potassium in basic and ultrabasic rocks. The three elements are determined in the same 0.5-g sample following a 30-min irradiation in a thermal neutron flux of 2??1012 n??cm-2??sec-1. Following radiochemical separation, the nuclides239U (T=23.5 m),233Th (T=22.2 m) and42K (T=12.36 h) are measured by ??-counting. A computer program is used to resolve the decay curves which are complex owing to contamination and the growth of daughter activities. The method was used to determine uranium, throium and potassium in the U. S. Geological Survey standard rocks DTS-1, PCC-1 and BCR-1. For 0.5-g samples the limits of detection for uranium, throium and potassium are 0.7, 1.0 and 10 ppb, respectively. ?? 1972 Akade??miai Kiado??.

  12. Approach of Complex Networks for the Determination of Brain Death

    Science.gov (United States)

    Sun, Wei-Gang; Cao, Jian-Ting; Wang, Ru-Bin

    2011-06-01

    In clinical practice, brain death is the irreversible end of all brain activity. Compared to current statistical methods for the determination of brain death, we focus on the approach of complex networks for real-world electroencephalography in its determination. Brain functional networks constructed by correlation analysis are derived, and statistical network quantities used for distinguishing the patients in coma or brain death state, such as average strength, clustering coefficient and average path length, are calculated. Numerical results show that the values of network quantities of patients in coma state are larger than those of patients in brain death state. Our findings might provide valuable insights on the determination of brain death.

  13. Generalized molybdenum oxide surface chemical state XPS determination via informed amorphous sample model

    Energy Technology Data Exchange (ETDEWEB)

    Baltrusaitis, Jonas, E-mail: job314@lehigh.edu [Department of Chemical Engineering, Lehigh University, B336 Iacocca Hall, 111 Research Drive, Bethlehem, PA 18015 (United States); PhotoCatalytic Synthesis group, MESA+ Institute for Nanotechnology, Faculty of Science and Technology, University of Twente, Meander 229, P.O. Box 217, 7500 AE Enschede (Netherlands); Mendoza-Sanchez, Beatriz [CRANN, Chemistry School, Trinity College Dublin, Dublin (Ireland); Fernandez, Vincent [Institut des Matériaux Jean Rouxel, 2 rue de la Houssinière, BP 32229, F-44322 Nantes Cedex 3 (France); Veenstra, Rick [PhotoCatalytic Synthesis group, MESA+ Institute for Nanotechnology, Faculty of Science and Technology, University of Twente, Meander 229, P.O. Box 217, 7500 AE Enschede (Netherlands); Dukstiene, Nijole [Department of Physical and Inorganic Chemistry, Kaunas University of Technology, Radvilenu pl. 19, LT-50254 Kaunas (Lithuania); Roberts, Adam [Kratos Analytical Ltd, Trafford Wharf Road, Wharfside, Manchester, M17 1GP (United Kingdom); Fairley, Neal [Casa Software Ltd, Bay House, 5 Grosvenor Terrace, Teignmouth, Devon TQ14 8NE (United Kingdom)

    2015-01-30

    Highlights: • We analyzed and modeled spectral envelopes of complex molybdenum oxides. • Molybdenum oxide films of varying valence and crystallinity were synthesized. • MoO{sub 3} and MoO{sub 2} line shapes from experimental data were created. • Informed amorphous sample model (IASM) developed. • Amorphous molybdenum oxide XPS envelopes were interpreted. - Abstract: Accurate elemental oxidation state determination for the outer surface of a complex material is of crucial importance in many science and engineering disciplines, including chemistry, fundamental and applied surface science, catalysis, semiconductors and many others. X-ray photoelectron spectroscopy (XPS) is the primary tool used for this purpose. The spectral data obtained, however, is often very complex and can be subject to incorrect interpretation. Unlike traditional XPS spectra fitting procedures using purely synthetic spectral components, here we develop and present an XPS data processing method based on vector analysis that allows creating XPS spectral components by incorporating key information, obtained experimentally. XPS spectral data, obtained from series of molybdenum oxide samples with varying oxidation states and degree of crystallinity, were processed using this method and the corresponding oxidation states present, as well as their relative distribution was elucidated. It was shown that monitoring the evolution of the chemistry and crystal structure of a molybdenum oxide sample due to an invasive X-ray probe could be used to infer solutions to complex spectral envelopes.

  14. Beyond inequality: Acknowledging the complexity of social determinants of health.

    Science.gov (United States)

    Eckersley, Richard

    2015-12-01

    The impact of inequality on health is gaining more attention as public and political concern grows over increasing inequality. The income inequality hypothesis, which holds that inequality is detrimental to overall population health, is especially pertinent. However the emphasis on inequality can be challenged on both empirical and theoretical grounds. Empirically, the evidence is contradictory and contested; theoretically, it is inconsistent with our understanding of human societies as complex systems. Research and discussion, both scientific and political, need to reflect better this complexity, and give greater recognition to other social determinants of health.

  15. Extruded dielectric sample tubes of complex cross section for EPR signal enhancement of aqueous samples

    Science.gov (United States)

    Sidabras, Jason W.; Mett, Richard R.; Hyde, James S.

    2017-04-01

    This paper builds on the work of Mett and Hyde (2003) and Sidabras et al. (2005) where multiple flat aqueous sample cells placed perpendicular to electric fields in microwave cavities were used to reduce the RF losses and increase the EPR signal. In this work, we present three novel sample holders for loop-gap resonators (LGRs) and cylindrical cavity geometries. Two sample holders have been commissioned and built by polytetrafluoroethylene (PTFE) extrusion techniques: a 1 mm O.D. capillary with a septum down the middle, named DoubleDee, and a 3.5 mm O.D. star shaped sample holder, named AquaStar. Simulations and experimental results at X-band show that the EPR signal intensity increases by factors of 1.43 and 3.87 in the DoubleDee and AquaStar respectively, over the current TPX 0.9 mm O.D. sample tube in a two-loop-one-gap LGR. Finally, combining the insight gained from the constructed sample holders and finite-element solutions, a third multi-lumen sample holder for a cylindrical TE011 cavity is optimized, named AquaSun, where simulations show an EPR signal intensity increase by a factor of 8.2 over a standard 1 mm capillary.

  16. Reducing sample complexity of polyclonal human autoantibodies by chromatofocusing.

    Science.gov (United States)

    Hagemann, Sascha; Faude, Alexander; Rabenstein, Monika; Balzer-Geldsetzer, Monika; Nölker, Carmen; Bacher, Michael; Dodel, Richard

    2010-08-15

    Chromatofocusing was performed in order to separate a polyclonal antigen-specific mixture of human immunoglobulins (IgGs) that would then allow for further analyses of as few different IgGs as possible. Because polyclonal IgGs only differ by amino acid sequence and possible post-translational modifications but not by molecular weight, we chose chromatofocusing for protein separation by different isoelectric points. We isolated antigen-specific IgGs from commercially available intravenous immunoglobulins (IVIG) using a combination of affinity- and size exclusion-chromatography and in order to reduce the complexity of the starting material IVIG was then replaced by single-donor plasmapheresis material. Using two-dimensional gel electrophoresis (2-DE), we observed a clear decrease in the number of different light and heavy chains in the chromatofocusing peak as compared to the starting material. In parallel, we monitored slight problems with the selected peak in isoelectric focusing as the first dimension of 2-DE, displayed in by the less proper focusing of the spots. When we tested whether IgGs were binding to their specific antigen after chromatofocusing, we were able to show that they were still in native conformation. In conclusion, we showed that chromatofocusing can be used as a first step in the analysis of mixtures of very similar proteins, e.g. polyclonal IgG preparations, in order to minimize the amount of different proteins in separated fractions in a reproducible way. Copyright 2010 Elsevier B.V. All rights reserved.

  17. Approach of Complex Networks for the Determination of Brain Death

    Institute of Scientific and Technical Information of China (English)

    SUN Wei-Gang; CAO Jian-Ting; WANG Ru-Bin

    2011-01-01

    In clinical practice, brain death is the irreversible end of all brain activity. Compared to current statistical methods for the determination of brain death, we focus on the approach of complex networks for real-world electroencephalography in its determination. Brain functional networks constructed by correlation analysis are derived, and statistical network quantities used for distinguishing the patients in coma or brain death state, such as average strength, clustering coefficient and average path length, are calculated. Numerical results show that the values of network quantities of patients in coma state are larger than those of patients in brain death state. Our Sndings might provide valuable insights on the determination of brain death.%@@ In clinical practice, brain death is the irreversible end of all brain activity.Compared to current statistical methods for the determination of brain death, we focus on the approach of complex networks for real-world electroencephalography in its determination.Brain functional networks constructed by correlation analysis axe derived, and statistical network quantities used for distinguishing the patients in coma or brain death state, such as average strength, clustering coefficient and average path length, are calculated.Numerical results show that the values of network quantities of patients in coma state are larger than those of patients in brain death state.Our findings might provide valuable insights on the determination of brain death.

  18. Determination of apparent sampling thickness of sea surface microlayer

    Science.gov (United States)

    Li, Jun; Ding, Hai-Bing; Wu, Zhi-Jian; Zhang, Zheng-Bin; Liu, Lian-Sheng

    1998-06-01

    In situ and laboratory studies of sea—surface microlayer sampling methods using glass plate, rotating drum, screen and funnel samplers were conducted. For glass plate and rotating drum samplers, surface microlayer samples of different thickness were collected by controlling their withdrawal rate and rotating rate. The relationships between pH, surface tension, the concentration of dissolved trace metals Cu and Pb, phosphate, particulate matters and sampling thickness were carefully investigated. It was shown that physicochemical and biological properties change obviously at the sampling thickness of about 50 μm, which is consistent with the mean thickness of the boundary film in the models of gas exchange across the sea surface. It is proposed that the apparent sampling thickness of the surface microlayer should be less than 40 μm. The factors affecting the sampling thickness are discussed, and the feasibility and applicable conditions for different sampling methods are evaluated.

  19. An extension of the Wilcoxon Rank-Sum test for complex sample survey data

    OpenAIRE

    Natarajan, Sundar; Lipsitz, Stuart R.; FITZMAURICE, GARRETT M.; SINHA, DEBAJYOTI; Ibrahim, Joseph G.; Haas, Jennifer; Gellad, Walid

    2012-01-01

    In complex survey sampling, a fraction of a finite population is sampled. Often, the survey is conducted so that each subject in the population has a different probability of being selected into the sample. Further, many complex surveys involve stratification and clustering. For generalizability of the sample to the finite population, these features of the design are usually incorporated in the analysis. While the Wilcoxon rank sum test is commonly used to compare an ordinal variable in bivar...

  20. Potentiometric detection in UPLC as an easy alternative to determine cocaine in biological samples.

    Science.gov (United States)

    Daems, Devin; van Nuijs, Alexander L N; Covaci, Adrian; Hamidi-Asl, Ezat; Van Camp, Guy; Nagels, Luc J

    2015-07-01

    The analytical methods which are often used for the determination of cocaine in complex biological matrices are a prescreening immunoassay and confirmation by chromatography combined with mass spectrometry. We suggest an ultra-high-pressure liquid chromatography combined with a potentiometric detector, as a fast and practical method to detect and quantify cocaine in biological samples. An adsorption/desorption model was used to investigate the usefulness of the potentiometric detector to determine cocaine in complex matrices. Detection limits of 6.3 ng mL(-1) were obtained in plasma and urine, which is below the maximum residue limit (MRL) of 25 ng mL(-1). A set of seven plasma samples and 10 urine samples were classified identically by both methods as exceeding the MRL or being inferior to it. The results obtained with the UPLC/potentiometric detection method were compared with the results obtained with the UPLC/MS method for samples spiked with varying cocaine concentrations. The intraclass correlation coefficient was 0.997 for serum (n =7) and 0.977 for urine (n =8). As liquid chromatography is an established technique, and as potentiometry is very simple and cost-effective in terms of equipment, we believe that this method is potentially easy, inexpensive, fast and reliable.

  1. Genetic Association Analysis under Complex Survey Sampling: The Hispanic Community Health Study/Study of Latinos

    Science.gov (United States)

    Lin, Dan-Yu; Tao, Ran; Kalsbeek, William D.; Zeng, Donglin; Gonzalez, Franklyn; Fernández-Rhodes, Lindsay; Graff, Mariaelisa; Koch, Gary G.; North, Kari E.; Heiss, Gerardo

    2014-01-01

    The cohort design allows investigators to explore the genetic basis of a variety of diseases and traits in a single study while avoiding major weaknesses of the case-control design. Most cohort studies employ multistage cluster sampling with unequal probabilities to conveniently select participants with desired characteristics, and participants from different clusters might be genetically related. Analysis that ignores the complex sampling design can yield biased estimation of the genetic association and inflation of the type I error. Herein, we develop weighted estimators that reflect unequal selection probabilities and differential nonresponse rates, and we derive variance estimators that properly account for the sampling design and the potential relatedness of participants in different sampling units. We compare, both analytically and numerically, the performance of the proposed weighted estimators with unweighted estimators that disregard the sampling design. We demonstrate the usefulness of the proposed methods through analysis of MetaboChip data in the Hispanic Community Health Study/Study of Latinos, which is the largest health study of the Hispanic/Latino population in the United States aimed at identifying risk factors for various diseases and determining the role of genes and environment in the occurrence of diseases. We provide guidelines on the use of weighted and unweighted estimators, as well as the relevant software. PMID:25480034

  2. Approximate determination of efficiency for activity measurements of cylindrical samples

    Energy Technology Data Exchange (ETDEWEB)

    Helbig, W. [Nuclear Engineering and Analytics Rossendorf, Inc. (VKTA), Dresden (Germany); Bothe, M. [Nuclear Engineering and Analytics Rossendorf, Inc. (VKTA), Dresden (Germany)

    1997-03-01

    Some calibration samples are necessary with the same geometrical parameters but of different materials, containing known activities A homogeniously distributed. Their densities are measured, their mass absorption coefficients may be unknown. These calibration samples are positioned in the counting geometry, for instance directly on the detector. The efficiency function {epsilon}(E) for each sample is gained by measuring the gamma spectra and evaluating all usable gamma energy peaks. From these {epsilon}(E) the common valid {epsilon}{sub geom}(E) will be deduced. For this purpose the functions {epsilon}{sub mu}(E) for these samples have to be established. (orig.)

  3. Comparison of Methods for Soil Sampling and Carbon Content Determination

    Directory of Open Access Journals (Sweden)

    Željka Zgorelec

    2011-03-01

    Full Text Available In this paper methods for sampling and analysis of total carbon in soil were compared. Soil sampling was done by sampling scheme according to agricultural soil monitoring recommendations. Soil samples were collected as single (four individual probe patterns and composite soil samples (16 individual probe patterns from agriculture soil. In soil samples mass ratio of total soil carbon was analyzed by dry combustion method (according to Dumas; HRN ISO 10694:2004 in Analytical Laboratory of Department of General Agronomy, Faculty of Agriculture University of Zagreb (FAZ and by oxidation method with chromium sulfuric acid (modified HRN ISO 14235:2004 in Analytical laboratory of Croatian Center for Agriculture, Food and Rural Affairs, Department of Soil and Land Conservation (ZZT. The observed data showed very strong correlation (r = 0.8943; n = 42 between two studied methods of analysis. Very strong correlation was also noted between different sampling procedures for single and composite samples in both laboratories, and coefficients of correlation were 0.9697 and 0.9950 (n = 8, respectively.

  4. Determination of sample size in genome-scale RNAi screens.

    Science.gov (United States)

    Zhang, Xiaohua Douglas; Heyse, Joseph F

    2009-04-01

    For genome-scale RNAi research, it is critical to investigate sample size required for the achievement of reasonably low false negative rate (FNR) and false positive rate. The analysis in this article reveals that current design of sample size contributes to the occurrence of low signal-to-noise ratio in genome-scale RNAi projects. The analysis suggests that (i) an arrangement of 16 wells per plate is acceptable and an arrangement of 20-24 wells per plate is preferable for a negative control to be used for hit selection in a primary screen without replicates; (ii) in a confirmatory screen or a primary screen with replicates, a sample size of 3 is not large enough, and there is a large reduction in FNRs when sample size increases from 3 to 4. To search a tradeoff between benefit and cost, any sample size between 4 and 11 is a reasonable choice. If the main focus is the selection of siRNAs with strong effects, a sample size of 4 or 5 is a good choice. If we want to have enough power to detect siRNAs with moderate effects, sample size needs to be 8, 9, 10 or 11. These discoveries about sample size bring insight to the design of a genome-scale RNAi screen experiment.

  5. Determination of polycyclic aromatic hydrocarbons in limpet samples

    Energy Technology Data Exchange (ETDEWEB)

    Rodriguez Delgado, M.A.; Corbella Tena, R.; Garcia Montelongo, F.J. [La Laguna Univ. (Spain). Dept. of Analytical Chemistry

    1999-08-01

    An HPLC method with UV and programmed fluorescence detection has been optimized and used to evaluate the levels of contamination of PAHs in lightly contaminated biota samples. A specific stationary phase was used that offers high selectivity for PAH separation. The proposed method was applied to limpet samples from Fuerteventura (Canary Island) with good results. (orig.)

  6. Sample-to-answer acoustic detection of DNA in complex samples.

    Science.gov (United States)

    Papadakis, George; Palladino, Pasquale; Chronaki, Dimitra; Tsortos, Achilleas; Gizeli, Electra

    2017-07-13

    The present study demonstrates the sensitive and label-free acoustic detection of dsDNA amplicons produced from whole Salmonella Thyphimurium cells without employing any DNA extraction and/or purification step, in the presence of the lysed bacterial cells and in a hybridization-free assay. A sample-to-answer assay is also shown during DNA detection directly in milk.

  7. Influences of Rate, Length, and Complexity on Speech Disfluency in a Single-Speech Sample in Preschool Children Who Stutter

    Science.gov (United States)

    Sawyer, Jean; Chon, HeeCheong; Ambrose, Nicoline G.

    2008-01-01

    The purpose of the present study was (1) to determine whether speech rate, utterance length, and grammatical complexity (number of clauses and clausal constituents per utterance) influenced stuttering-like disfluencies as children became more disfluent at the end of a 1200-syllable speech sample [Sawyer, J., & Yairi, E. (2006). "The effect of…

  8. [Ambient and enclosed space air sampling for determination of contaminants].

    Science.gov (United States)

    Dorogova, V B

    2010-01-01

    The paper touches upon the issues how to correctly and maximally take single and average daily samples of ambient, residential and public building, and enclosed space air for further tests for the content of hazardous substances. The paper is debated.

  9. Randomization-Based Inference about Latent Variables from Complex Samples: The Case of Two-Stage Sampling

    Science.gov (United States)

    Li, Tiandong

    2012-01-01

    In large-scale assessments, such as the National Assessment of Educational Progress (NAEP), plausible values based on Multiple Imputations (MI) have been used to estimate population characteristics for latent constructs under complex sample designs. Mislevy (1991) derived a closed-form analytic solution for a fixed-effect model in creating…

  10. Evaluation of Gravimetric Tar Determination in Particle Samples

    DEFF Research Database (Denmark)

    Hindsgaul, Claus; Henriksen, Ulrik B.; Bentzen, Jens Dall

    2000-01-01

    A comparison of tar determination of particles from a down-draft gasifier using soxhlet extractions (with anisole, dichloromethane and acetone) and pyrolysis of the particles.......A comparison of tar determination of particles from a down-draft gasifier using soxhlet extractions (with anisole, dichloromethane and acetone) and pyrolysis of the particles....

  11. Use of passive sampling devices to determine soil contaminant concentrations

    Energy Technology Data Exchange (ETDEWEB)

    Johnson, K.A. [Clemson Univ., Pendleton, SC (United States)]|[Washington State Univ., Richland, WA (United States); Hooper, M.J. [Clemson Univ., Pendleton, SC (United States); Weisskopf, C.P. [Washington State Univ., Richland, WA (United States)

    1996-12-31

    The effective remediation of contaminated sites requires accurate identification of chemical distributions. A rapid sampling method using passive sampling devices (PSDs) can provide a thorough site assessment. We have been pursuing their application in terrestrial systems and have found that they increase the ease and speed of analysis, decrease solvent usage and overall cost, and minimize the transport of contaminated soils. Time and cost savings allow a higher sampling frequency than is generally the case using traditional methods. PSDs have been used in the field in soils of varying physical properties and have been successful in estimating soil concentrations ranging from 1 {mu}g/kg (parts per billion) to greater than 200 mg/kg (parts per million). They were also helpful in identifying hot spots within the sites. Passive sampling devices show extreme promise as an analytical tool to rapidly characterize contaminant distributions in soil. There are substantial time and cost savings in laboratory personnel and supplies. By selectively excluding common interferences that require sample cleanup, PSDs can be retrieved from the field and processed rapidly (one technician can process approximately 90 PSDs in an 8-h work day). The results of our studies indicate that PSDs can be used to accurately estimate soil contaminant concentrations and provide lower detection limits. Further, time and cost savings will allow a more thorough and detailed characterization of contaminant distributions. 13 refs., 4 figs., 2 tabs.

  12. Usefulness of ytterbium(III) as analytical reagent for total sulfite determination in white wine samples.

    Science.gov (United States)

    Rodríguez-Díaz, Rafael Carlos; Aguilar-Caballos, Maria Paz; Gómez-Hens, Agustina

    2004-12-29

    Ytterbium(III) is used as reagent for the determination of sulfite by measuring the formation of the Yb(III)-sulfite complex through the variation of the light scattering intensity with time. The low solubility of this complex causes an efficient dispersion of the radiation at 490 nm, which is measured at 980 nm. Each kinetic datum is automatically obtained in only 0.5 s by stopped-flow mixing technique. The application of the initial rate method using a long emission wavelength minimizes the potential interference of fluorescent background signals from the sample matrix. The dynamic range of the calibration graph is 1-250 microg/mL, and the calculated detection limit is 0.35 microg/mL. The precision, expressed as relative standard deviation, is wine samples, which requires only the sample dilution and the use of two aliquots to improve selectivity. However, the matrix effect found for red wines precludes the application of the method to the direct analysis of these samples. Analytical recoveries ranged from 96.0 to 106.7%. The results obtained with the proposed method agreed with those provided by the p-rosaniline method. Unlike this method, in which toxic reagents are required, the use of ytterbium(III) as analytical reagent shows the advantage of its low acute toxic rating.

  13. Improved FIA-ABTS method for antioxidant capacity determination in different biological samples.

    Science.gov (United States)

    Bompadre, Stefano; Leone, Luciana; Politi, Alessia; Battino, Maurizio

    2004-08-01

    In order to evaluate the actual antioxidant features of foods, beverages and also plasma from patients, a number of assays have been developed in the last few years to determine the so called total antioxidant activity (TAA), intended as the cumulative capacity of a biological sample to scavenge free radicals. Most of the assays partially failed in obtaining a good reproducibility when using plasma because it is composed of a large number of substances, some of which are present at very high concentrations and possess masking features. For these reasons we have improved the widely known ABTS method by means of a FIA system where both temperature and dispersion of sample and reagent were strictly controlled. We found that temperature may be a critical aspect in the measurement of plasma TAA whilst its influence may be less important in the assay of non-complex biological samples. We demonstrated that also the reaction time may be critical, depending on the nature of the substance employed. Data confirmed the high TAA of a methylsalicylate-containing mouthrinse as well as the negligible TAA offered by the chlorhexidine containing one. White wines (Verdicchio) also displayed interesting TAA values. The improved method was useful to screen rapidly, without dilution, with very limited handling of the sample and with high repeatability the TAA of plasma in addition to chemical products, beverages and non-complex biological mixtures.

  14. A quantitative method for determining the robustness of complex networks

    Science.gov (United States)

    Qin, Jun; Wu, Hongrun; Tong, Xiaonian; Zheng, Bojin

    2013-06-01

    Most current studies estimate the invulnerability of complex networks using a qualitative method that analyzes the decay rate of network performance. This method results in confusion over the invulnerability of various types of complex networks. By normalizing network performance and defining a baseline, this paper defines the invulnerability index as the integral of the normalized network performance curve minus the baseline. This quantitative method seeks to measure network invulnerability under both edge and node attacks and provides a definition on the distinguishment of the robustness and fragility of networks. To demonstrate the proposed method, three small-world networks were selected as test beds. The simulation results indicate that the proposed invulnerability index can effectively and accurately quantify network resilience and can deal with both the node and edge attacks. The index can provide a valuable reference for determining network invulnerability in future research.

  15. Determination of gadolinium-based MRI contrast agents in biological and environmental samples: A review

    Energy Technology Data Exchange (ETDEWEB)

    Telgmann, Lena [University of Münster, Institute of Inorganic and Analytical Chemistry, Münster (Germany); Sperling, Michael [University of Münster, Institute of Inorganic and Analytical Chemistry, Münster (Germany); European Virtual Institute for Speciation Analysis (EVISA), Münster (Germany); Karst, Uwe, E-mail: uk@uni-muenster.de [University of Münster, Institute of Inorganic and Analytical Chemistry, Münster (Germany)

    2013-02-18

    Highlights: ► All major methods for the analysis of Gd-based MRI contrast agents are discussed. ► Biological and environmental samples are covered. ► Pharmacokinetics and species transformation can be investigated. ► The figures of merit as limit of detection and analysis time are described. -- Abstract: The development of analytical methods and strategies to determine gadolinium and its complexes in biological and environmental matrices is evaluated in this review. Gadolinium (Gd) chelates are employed as contrast agents for magnetic resonance imaging (MRI) since the 1980s. In general they were considered as safe and well-tolerated, when in 2006, the disease nephrogenic systemic fibrosis (NSF) was connected to the administration of MRI contrast agents based on Gd. Pathogenesis and etiology of NSF are yet unclear and called for the development of several analytical methods to obtain elucidation in this field. Determination of Gd complex stability in vitro and in vivo, as well as the quantification of Gd in body fluids like blood and urine was carried out. Separation of the Gd chelates was achieved with high performance liquid chromatography (HPLC) and capillary electrophoresis (CE). For detection, various methods were employed, including UV–vis absorbance and fluorescence spectroscopy, electrospray ionization mass spectrometry (ESI-MS) and inductively coupled plasma mass spectrometry (ICP-MS). A second challenge for analysts was the discovery of high concentrations of anthropogenic Gd in surface waters draining populated areas. The source could soon be determined to be the increasing administration of Gd complexes during MRI examinations. Identification and quantification of the contrast agents was carried out in various surface and groundwater samples to determine the behavior and fate of the Gd chelates in the environment. The improvement of limits of detection (LOD) and limits of quantification (LOQ) was and still is the goal of past and ongoing

  16. 40 CFR 761.257 - Determining the regulatory status of sampled pipe.

    Science.gov (United States)

    2010-07-01

    ... sampled pipe. 761.257 Section 761.257 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED... Samples § 761.257 Determining the regulatory status of sampled pipe. (a) For purposes of removal for disposal of a pipe segment that has been sampled, the sample results for that segment determines its PCB...

  17. Profiling of Protein N-Termini and Their Modifications in Complex Samples.

    Science.gov (United States)

    Demir, Fatih; Niedermaier, Stefan; Kizhakkedathu, Jayachandran N; Huesgen, Pitter F

    2017-01-01

    Protein N termini are a unique window to the functional state of the proteome, revealing translation initiation sites, co-translation truncation and modification, posttranslational maturation, and further proteolytic processing into different proteoforms with distinct functions. As a direct readout of proteolytic activity, protein N termini further reveal proteolytic regulation of diverse biological processes and provide a route to determine specific substrates and hence the physiological functions for any protease of interest. Here, we describe our current protocol of the successful Terminal Amine Isotope Labeling of Substrates (TAILS) technique, which enriches protein N-terminal peptides from complex proteome samples by negative selection. Genome-encoded N termini, protease-generated neo-N termini, and endogenously modified N termini are all enriched simultaneously. Subsequent mass spectrometric analysis therefore profiles all protein N termini and their modifications present in a complex sample in a single experiment. We further provide a detailed protocol for the TAILS-compatible proteome preparation from plant material and discuss specific considerations for N terminome data analysis and annotation.

  18. Enhanced conformational sampling to visualize a free-energy landscape of protein complex formation.

    Science.gov (United States)

    Iida, Shinji; Nakamura, Haruki; Higo, Junichi

    2016-06-15

    We introduce various, recently developed, generalized ensemble methods, which are useful to sample various molecular configurations emerging in the process of protein-protein or protein-ligand binding. The methods introduced here are those that have been or will be applied to biomolecular binding, where the biomolecules are treated as flexible molecules expressed by an all-atom model in an explicit solvent. Sampling produces an ensemble of conformations (snapshots) that are thermodynamically probable at room temperature. Then, projection of those conformations to an abstract low-dimensional space generates a free-energy landscape. As an example, we show a landscape of homo-dimer formation of an endothelin-1-like molecule computed using a generalized ensemble method. The lowest free-energy cluster at room temperature coincided precisely with the experimentally determined complex structure. Two minor clusters were also found in the landscape, which were largely different from the native complex form. Although those clusters were isolated at room temperature, with rising temperature a pathway emerged linking the lowest and second-lowest free-energy clusters, and a further temperature increment connected all the clusters. This exemplifies that the generalized ensemble method is a powerful tool for computing the free-energy landscape, by which one can discuss the thermodynamic stability of clusters and the temperature dependence of the cluster networks.

  19. determination of lead at nanogram level in water samples by ...

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    concentration of Pb(II) in the range of 0.04–1.8 μg/mL for the system with a low ... storage battery, drainage from lead ore mines, paints, munitions, and ... Water samples were immediately filtered through cellulose nitrate (0.45 μm pore size, 47.

  20. Complex refractive indices of Saharan dust samples at visible and near UV wavelengths: a laboratory study

    Directory of Open Access Journals (Sweden)

    R. Wagner

    2011-07-01

    Full Text Available We have retrieved the wavelength-dependent imaginary parts of the complex refractive index for five different Saharan dust aerosol particles of variable mineralogical composition at wavelengths between 305 and 955 nm. The dust particles were generated by re-dispersing soil samples into a laboratory aerosol chamber, typically yielding particle sizes with mean diameters ranging from 0.3 to 0.4 μm and maximum diameters from 2 to 4 μm. The extinction and absorption coefficients as well as the number size distribution of the dust particles were simultaneously measured by various established techniques. An inversion scheme based on a spheroidal dust model was employed to deduce the refractive indices. The retrieved imaginary parts of the complex refractive index were in the range from 0.003 to 0.005, 0.005 to 0.011, and 0.016 to 0.050 at the wavelengths 955, 505, and 305 nm. The hematite content of the dust particles was determined by electron-microscopical single particle analysis. Hematite volume fractions in the range from 1.1 to 2.7 % were found for the different dusts, a range typical for atmospheric mineral dust. We have performed a sensitivity study to assess how accurately the retrieved imaginary refractive indices could be reproduced by calculations with mixing rule approximations using the experimentally determined hematite contents as input.

  1. Characterizing the Sample Complexity of Large-Margin Learning With Second-Order Statistics

    CERN Document Server

    Sabato, Sivan; Tishby, Naftali

    2012-01-01

    We obtain a tight distribution-specific characterization of the sample complexity of large-margin classification with L_2 regularization: We introduce the margin-adapted dimension, which is a simple function of the second order statistics of the data distribution, and show distribution-specific upper and lower bounds on the sample complexity, both governed by the margin-adapted dimension of the data distribution. The upper bounds are universal, and the lower bounds hold for a rich family of sub-Gaussian distributions. We conclude that this new quantity tightly characterizes the true sample complexity of large-margin classification.

  2. Spectroscopic infrared ellipsometry to determine the structure of layered samples

    Energy Technology Data Exchange (ETDEWEB)

    Korte, Ernst-Heiner; Hinrichs, Karsten; Roeseler, Arnulf

    2002-10-15

    This contribution outlines investigations in our laboratory in the course of developing spectroscopic infrared ellipsometry into an analytical tool for structure elucidation of a given solid sample with one single experimental technique. The term 'structure' is meant here to comprise the layer or stack geometry of a sample along with the thicknesses, as well as the optical properties of the individual layers. The latter ones--expressed as optical constants--serve as a basis to characterize the layer material, from the identity of the compound to specific molecular interactions and order. There are no general restrictions as to the physical properties of the materials; the individual layers or films should advantageously be thin enough to transmit infrared radiation at least within spectral windows. The sensitivity of infrared ellipsometry to films as thin as a few nanometers or less is illustrated by experimental examples.

  3. Forensic study of sex determination using PCR on teeth samples.

    OpenAIRE

    Murakami H; Yamamoto Y; Yoshitome K; Ono T; Okamoto O; Shigeta Y; Doi Y; Miyaishi S; Ishizu H

    2000-01-01

    In this study, sex determination using polymerase chain reaction (PCR) on tooth material was evaluated from the viewpoint of forensic medicine. The sensitivity of PCR for detection of the Y chromosome-specific alphoid repeat sequence and the X chromosome-specific alphoid repeat sequence was 0.5 pg of genomic DNA. Sex could be determined by PCR of DNA extracted from the pulp of 16 freshly extracted permanent teeth and dentine including the surface of the pulp cavity of 6 freshly extracted milk...

  4. CLUSTER SAMPLING FOR DETERMINATION OF IMMUNIZATION COVERAGE: A LIMITATION

    Directory of Open Access Journals (Sweden)

    K. Nasseri

    1989-08-01

    Full Text Available Evidence provided from studies in Iran points to a possible bias in application of the standard EPI cluster sampling procedure, When carried out in populations with highly variant birth rates, tends to over-represent the low birth rate, i.e. higher socio-economic, strata, and if the entity under study shows significant socio-economic gradient, then the estimates arrived at by this method might be highly biased. Some alternatives have been mentioned.

  5. Determination of estrogenic potential in waste water without sample extraction.

    Science.gov (United States)

    Avberšek, Miha; Žegura, Bojana; Filipič, Metka; Uranjek-Ževart, Nataša; Heath, Ester

    2013-09-15

    This study describes the modification of the ER-Calux assay for testing water samples without sample extraction (NE-(ER-Calux) assay). The results are compared to those obtained with ER-Calux assay and a theoretical estrogenic potential obtained by GC-MSD. For spiked tap and waste water samples there was no statistical difference between estrogenic potentials obtained by the three methods. Application of NE-(ER-Calux) to "real" influent and effluents from municipal waste water treatment plants and receiving surface waters found that the NE-(ER-Calux) assay gave higher values compared to ER-Calux assay and GC-MSD. This is explained by the presence of water soluble endocrine agonists that are usually removed during extraction. Intraday dynamics of the estrogenic potential of a WWTP influent and effluent revealed an increase in the estrogenic potential of the influent from 12.9 ng(EEQ)/L in the morning to a peak value of 40.0 ng(EEQ)/L in the afternoon. The estrogenic potential of the effluent was

  6. Membrane preconcentration of iron in seawater samples and on-site determination in spectrophotometry

    Institute of Scientific and Technical Information of China (English)

    PENG Yuanzhen; YUAN Dongxing; HUANG Yongming; JIANG Tao; LIU Baomin

    2012-01-01

    A novel method for on-site determination of trace iron was developed using membrane preconcentration and spectrophotometric detection.Fe(Ⅱ)-ferrozine complex was reacted with cetyltrimethylammonium bromide (CTAB) to form a Fe(Ⅱ)-ferrozine-CTAB paired compound,which was collected on a membrane by filtration under vacuum.The membrane was immersed in 2 mL of ethanol-nitric acid and the absorbance of the solution measured for quantitative analysis.Various factors affecting the iron collection and determination were investigated.With different sample preconcentration volumes,the range of determination was broadened to 0.5-120 μg/L.The detection limit of this method reached 0.19 μg/L and the recoveries were between 97.2 and 109% when the concentration enrichment was about 45.The relative standard deviation (n =7) was 1.9% for samples containing 10 μg/L Fe.Twelve seawater samples were analyzed on-site using the proposed method,and two were also analyzed in inductively coupled plasma mass spectrometry.No significant difference was shown between the two methods by the Student's t-test.The method has also been used on-site for iron enrichment experiments with phytoplankton and concluded to be simple,accurate and inexpensive.

  7. Generalized molybdenum oxide surface chemical state XPS determination via informed amorphous sample model

    Science.gov (United States)

    Baltrusaitis, Jonas; Mendoza-Sanchez, Beatriz; Fernandez, Vincent; Veenstra, Rick; Dukstiene, Nijole; Roberts, Adam; Fairley, Neal

    2015-01-01

    Accurate elemental oxidation state determination for the outer surface of a complex material is of crucial importance in many science and engineering disciplines, including chemistry, fundamental and applied surface science, catalysis, semiconductors and many others. X-ray photoelectron spectroscopy (XPS) is the primary tool used for this purpose. The spectral data obtained, however, is often very complex and can be subject to incorrect interpretation. Unlike traditional XPS spectra fitting procedures using purely synthetic spectral components, here we develop and present an XPS data processing method based on vector analysis that allows creating XPS spectral components by incorporating key information, obtained experimentally. XPS spectral data, obtained from series of molybdenum oxide samples with varying oxidation states and degree of crystallinity, were processed using this method and the corresponding oxidation states present, as well as their relative distribution was elucidated. It was shown that monitoring the evolution of the chemistry and crystal structure of a molybdenum oxide sample due to an invasive X-ray probe could be used to infer solutions to complex spectral envelopes.

  8. Spectrophotometric determination of copper(II) in pharmaceutical, biological and water samples by 4-(2'-benzothiazolylazo)-salicylic acid

    Science.gov (United States)

    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.

  9. Bio-sample preparation and gas chromatographic determination of benzodiazepines--a review.

    Science.gov (United States)

    Uddin, Mohammad Nasir; Samanidou, Victoria F; Papadoyannis, Ioannis N

    2013-08-01

    Benzodiazepines have become commonly prescribed medicines worldwide in the therapy of anxiety, sleep disorders and convulsive attacks because they are relatively safe, with mild side effects. The availability of rapid, sensitive and selective analytical methods is essential for the determination of these drugs in clinical and forensic cases. Benzodiazepines are usually present at trace levels (μg/mL or ng/mL) in a complex biological matrix, and the potentially interfering compounds need to be removed before analysis. Therefore, a sample preparation technique is often mandatory, both to extract the drugs of interest from the matrices and to increase their concentration. An extended and comprehensive review is presented herein, focusing on bio-sample preparation (pretreatment, extraction and derivatization) and gas chromatographic methods applied for the quantification of 1,4-benzodiazepines.

  10. Application of experimental design on determination of aluminum content in saline samples by adsorptive cathodic stripping voltammetry

    OpenAIRE

    YILMAZ, Sinan; Öztürk, Betül; ÖZDEMİR, Durmuş

    2013-01-01

    Adsorptive cathodic stripping voltammetric determination of aluminum at ng mL-1 levels in salt samples based on the metal complexation with Calcon (1-(2-hydroxynaphthylazo)-2 naphthol-4-sulfonic acid) and the subsequent adsorptive deposition onto a hanging mercury drop electrode was studied. Central composite design was used as a design method. Several chemical and instrumental parameters (pH, ligand concentration, deposition time, deposition potential, and complexing time) were invo...

  11. Detection of Bacillus anthracis DNA in complex soil and air samples using next-generation sequencing.

    Directory of Open Access Journals (Sweden)

    Nicholas A Be

    Full Text Available Bacillus anthracis is the potentially lethal etiologic agent of anthrax disease, and is a significant concern in the realm of biodefense. One of the cornerstones of an effective biodefense strategy is the ability to detect infectious agents with a high degree of sensitivity and specificity in the context of a complex sample background. The nature of the B. anthracis genome, however, renders specific detection difficult, due to close homology with B. cereus and B. thuringiensis. We therefore elected to determine the efficacy of next-generation sequencing analysis and microarrays for detection of B. anthracis in an environmental background. We applied next-generation sequencing to titrated genome copy numbers of B. anthracis in the presence of background nucleic acid extracted from aerosol and soil samples. We found next-generation sequencing to be capable of detecting as few as 10 genomic equivalents of B. anthracis DNA per nanogram of background nucleic acid. Detection was accomplished by mapping reads to either a defined subset of reference genomes or to the full GenBank database. Moreover, sequence data obtained from B. anthracis could be reliably distinguished from sequence data mapping to either B. cereus or B. thuringiensis. We also demonstrated the efficacy of a microbial census microarray in detecting B. anthracis in the same samples, representing a cost-effective and high-throughput approach, complementary to next-generation sequencing. Our results, in combination with the capacity of sequencing for providing insights into the genomic characteristics of complex and novel organisms, suggest that these platforms should be considered important components of a biosurveillance strategy.

  12. Liquid Chromatographic Method for Determination of Nisoldipine from Pharmaceutical Samples

    Directory of Open Access Journals (Sweden)

    Amit Gupta

    2010-01-01

    Full Text Available A simple and specific high performance thin layer chromatographic method was developed and validated for the determination of nisoldipine from tablet dosage form. The method was carried out at 320 nm after extraction of drug in methanol. The method uses aluminum plates pre-coated with silica gel 60F-254 as stationary phase and cyclohexane-ethyl acetate-toluene (3:3:4, v/v/v as mobile phase. Linearity was established over a range of 400-2400 ng per zone. Both peak area ratio and peak height ratio showed acceptable correlation coefficient i.e. more than 0.99. However we used peak area for validation purpose. Intra-day and inter-day precision was determined and found to have less than 6.0 % RSD.

  13. Methods for determination of polybrominated diphenyl ethers in environmental samples--review.

    Science.gov (United States)

    Fulara, Izabela; Czaplicka, Marianna

    2012-08-01

    Polybrominated diphenyl ethers (PBDEs) are a group of persistent organic pollutants. They are used as flame retardants in plastics, paints, varnishes and textile materials. PBDEs pose great risk to the environment because of their high persistence and ability to get into the environment easily due to the lack of chemical bonds with the matrix of materials, to which they are added. Global research studies confirmed the occurrence of those compounds in the majority of elements of water and land environment. Analysis of PBDEs in environmental samples is one of the specific analytical methods of criteria that comprise low detection limits and high selectivity. The analysis of PBDEs in environmental samples is one of the specific analytical methods, in which the main criteria are low detection limits and high selectivity. In this article, a literature review of methods for environmental sample preparation and analysis of the PBDE content was presented. The article discusses the potential of modern extraction techniques such as: solid-phase microextraction, single-drop microextraction, dispersive liquid-liquid microextraction, microwave-assisted extraction, cloud point extraction, hollow fibre-liquid phase microextraction and others for the separation of PBDEs from environmental samples with a complex matrix. Among the methods for qualitative and quantitative determination of PBDEs, a particular focus was put on gas chromatography/mass spectrometry with various injection techniques and different types of sample ionisation.

  14. [Isolation of Sporothrix pallida complex in clinical and environmental samples from Chile].

    Science.gov (United States)

    Cruz Choappa, Rodrigo M; Vieille Oyarzo, Peggy I; Carvajal Silva, Laura C

    2014-01-01

    The isolation of S. pallida complex from medical samples and home garden soil of a patient in Chile is here in reported. Fungi of the Sporothrix schenckii complex can cause various infections. In Chile, the medical and environmental isolates of these this complex are rare. The aim of this study was to identify an unusual agent in a case of onychomycosis and to detect its presence in the patient's home garden. For this purpose, clinical samples were obtained by scraping the patient's subungueal first right toe nail as well as by taking soil samples from different areas of her home garden. Species identification was performed by morphophysiology and one of the strains isolated from the patient's toe nail was sent to CBS for molecular confirmation (14.062). S. pallida complex was identified both from the patient's toe nail and samples taken from her home garden.

  15. Challenging genosensors in food samples: The case of gluten determination in highly processed samples.

    Science.gov (United States)

    Martín-Fernández, Begoña; de-los-Santos-Álvarez, Noemí; Martín-Clemente, Juan Pedro; Lobo-Castañón, María Jesús; López-Ruiz, Beatriz

    2016-01-01

    Electrochemical genosensors have undergone an enormous development in the last decades, but only very few have achieved a quantification of target content in highly processed food samples. The detection of allergens, and particularly gluten, is challenging because legislation establishes a threshold of 20 ppm for labeling as gluten-free but most genosensors expresses the results in DNA concentration or DNA copies. This paper describes the first attempt to correlate the genosensor response and the wheat content in real samples, even in the case of highly processed food samples. A sandwich-based format, comprising a capture probe immobilized onto the screen-printed gold electrode, and a signaling probe functionalized with fluorescein isothiocyanate (FITC), both hybridizing with the target was used. The hybridization event was electrochemically monitored by adding an anti-FITC peroxidase (antiFITC-HRP) and its substrate, tetramethylbenzidine. Binary model mixtures, as a reference material, and real samples have been analyzed. DNA from food was extracted and a fragment encoding the immunodominant peptide of α2-gliadin amplified by a tailored PCR. The sensor was able to selectively detect toxic cereals for celiac patients, such as different varieties of wheat, barley, rye and oats, from non-toxic plants. As low as 0.001% (10 mg/kg) of wheat flour in an inert matrix was reliably detected, which directly compete with the current method of choice for DNA detection, the real-time PCR. A good correlation with the official immunoassay was found in highly processed food samples.

  16. Selective spectrofluorimetric determination of zinc in biological samples by Flow Injection Analysis (FIA)

    Energy Technology Data Exchange (ETDEWEB)

    Fernandez, P.; Perez Conde, C.; Gutierrez, A.; Camara, C. (Universidad Complutense, Madrid (Spain). Dept. de Quimica Analitica)

    1992-03-01

    The automatization of a spectrofluorimetric method for the determination of zinc at trace level is described. It is based on the formation of the fluorescent complex Zn(II)-5,7-dibromo-8-quinolinol (Zn(II)-DBQ) followed by extraction into diethylether using flow injection analysis. The optimum fluorescent emission is reached in hexamethylenetetramine (H{sub 2}MTA{sup +}/HMTA) buffer pH 6.0. A membrane phase separator was used. The calibration graph is linear up to 1.5 {mu}g/ml of Zn(II). The proposed method (detection limit 3 ng/ml) is very selective and has been successfully applied to determine Zn(II) in biological samples, tap waters and various food items. (orig.).

  17. Image analysis of pubic bone for sex determination in a computed tomography sample.

    Science.gov (United States)

    López-Alcaraz, Manuel; Garamendi González, Pedro Manuel; Alemán Aguilera, Inmaculada; Botella López, Miguel

    2013-11-01

    Radiology has demonstrated great utility for sex determination, but most studies are based in metrical and morphological methods in order to perform an identification profile. It is presented an easy image analysis-based method aimed to demonstrate the relationship between the bony tissue ultrastructure and sex by using several grey level histogram variables obtained from computed tomography images using sagittal sections of the pubic symphysis surface and the body of the pubis. The CT sample consisted of 169 hospital DICOM archives of known sex and age. The multivariate binary logistic regression models calculated showed reliabilities for sex determination between 87.4 and 95.8 %, with a high intra and inter-observer agreement. The suggested method is not only considered useful to perform an identification profile during Virtopsy, but even for application in further studies in order to attach a quantitative correlation for tissue ultrastructure characteristics without complex and expensive methods beyond image analysis.

  18. Cloud point extraction, preconcentration and simultaneous spectrophotometric determination of nickel and cobalt in water samples

    Science.gov (United States)

    Safavi, A.; Abdollahi, H.; Hormozi Nezhad, M. R.; Kamali, R.

    2004-10-01

    Cloud point extraction has been used for the preconcentration and simultaneous spectrophotometric determination of nickel and cobalt after the formation of a complex with 2-amino-cyclopentene-1-dithiocarboxylic acid (ACDA), and latter analysis by spectrophotometer using Triton X-114 as surfactant. The parameters affecting the separation phase and detection process were optimized. Under the optimum experimental conditions (i.e. pH=5, 0.07 mM ACDA, Triton X-114 = 0.25% (w/v)), calibration graphs were linear in the range of 20-500 and 20-200 μg l -1 with detection limits of 10 and 7.5 μg l -1 for Ni and Co, respectively. The method was applied to the determination of Ni and Co in natural and waste water samples with satisfactory results.

  19. Spectrophotometric determination of lead after preconcentration of its diphenylthiocarbazone complex on an Amberlite XAD-1180 column

    Science.gov (United States)

    Rajesh, N.; Manikandan, S.

    2008-09-01

    A simple methodology has been developed for the solid phase extraction of lead based on the adsorption of its diphenylthiocarbazone complex on an Amberlite XAD-1180 column. The effect of various parameters such as eluting agents, stability of the column, sample volume, interfering ions, etc. were studied in detail. The adsorbed complex could be eluted using acetone and the concentration of lead was determined using visible spectrophotometry at a wavelength maximum of 486 nm. A detection limit of 3.5 μg L -1 could be achieved and the validity of the proposed method was checked in spiked tap water, well water and industrial wastewater samples. The relative standard deviation of the method was found to be 3.0%. The highest preconcentration factor attainable for quantitative recovery (>95%) of lead was 25 for a 250 mL sample volume.

  20. Bounds on the sample complexity for private learning and private data release

    Energy Technology Data Exchange (ETDEWEB)

    Kasiviswanathan, Shiva [Los Alamos National Laboratory; Beime, Amos [BEN-GURION UNIV.; Nissim, Kobbi [BEN-GURION UNIV.

    2009-01-01

    Learning is a task that generalizes many of the analyses that are applied to collections of data, and in particular, collections of sensitive individual information. Hence, it is natural to ask what can be learned while preserving individual privacy. [Kasiviswanathan, Lee, Nissim, Raskhodnikova, and Smith; FOCS 2008] initiated such a discussion. They formalized the notion of private learning, as a combination of PAC learning and differential privacy, and investigated what concept classes can be learned privately. Somewhat surprisingly, they showed that, ignoring time complexity, every PAC learning task could be performed privately with polynomially many samples, and in many natural cases this could even be done in polynomial time. While these results seem to equate non-private and private learning, there is still a significant gap: the sample complexity of (non-private) PAC learning is crisply characterized in terms of the VC-dimension of the concept class, whereas this relationship is lost in the constructions of private learners, which exhibit, generally, a higher sample complexity. Looking into this gap, we examine several private learning tasks and give tight bounds on their sample complexity. In particular, we show strong separations between sample complexities of proper and improper private learners (such separation does not exist for non-private learners), and between sample complexities of efficient and inefficient proper private learners. Our results show that VC-dimension is not the right measure for characterizing the sample complexity of proper private learning. We also examine the task of private data release (as initiated by [Blum, Ligett, and Roth; STOC 2008]), and give new lower bounds on the sample complexity. Our results show that the logarithmic dependence on size of the instance space is essential for private data release.

  1. Sequential determination of lead and cobalt in tap water and foods samples by fluorescence.

    Science.gov (United States)

    Talio, María Carolina; Alesso, Magdalena; Acosta, María Gimena; Acosta, Mariano; Fernández, Liliana P

    2014-09-01

    In this work, a new procedure was developed for the separation and preconcentration of lead(II) and cobalt(II) in several water and foods samples. Complexes of metal ions with 8-hydroxyquinolein (8-HQ) were formed in aqueous solution. The proposed methodology is based on the preconcentration/separation of Pb(II) by solid-phase extraction using paper filter, followed by spectrofluorimetric determination of both metals, on the solid support and the filtered aqueous solution, respectively. The solid surface fluorescence determination was carried out at λem=455 nm (λex=385 nm) for Pb(II)-8-HQ complex and the fluorescence of Co(II)-8-HQ was determined in aqueous solution using λem=355 nm (λex=225 nm). The calibration graphs are linear in the range 0.14-8.03×10(4) μg L(-1) and 7.3×10(-2)-4.12×10(3) μg L(-1), for Pb(II) and Co(II), respectively, with a detection limit of 4.3×10(-2) and 2.19×10(-2) μg L(-1) (S/N=3). The developed methodology showed good sensitivity and adequate selectivity and it was successfully applied to the determination of trace amounts of lead and cobalt in tap waters belonging of different regions of Argentina and foods samples (milk powder, express coffee, cocoa powder) with satisfactory results. The new methodology was validated by electrothermal atomic absorption spectroscopy with adequate agreement. The proposed methodology represents a novel application of fluorescence to Pb(II) and Co(II) quantification with sensitivity and accuracy similar to atomic spectroscopies.

  2. A practical approach for near infrared spectral quantitative analysis of complex samples using partial least squares modeling

    Institute of Scientific and Technical Information of China (English)

    2009-01-01

    The number of latent variables (LVs) or the factor number is a key parameter in PLS modeling to obtain a correct prediction. Although lots of work have been done on this issue, it is still a difficult task to determine a suitable LV number in practical uses. A method named independent factor diagnostics (IFD) is proposed for investigation of the contribution of each LV to the predicted results on the basis of discussion about the determination of LV number in PLS modeling for near infrared (NIR) spectra of complex samples. The NIR spectra of three data sets of complex samples, including a public data set and two tobacco lamina ones, are investigated. It is shown that several high order LVs constitute main contributions to the predicted results, albeit the contribution of the low order LVs should not be neglected in the PLS models. Therefore, in practical uses of PLS for analysis of complex samples, it may be better to use a slightly large LV number for NIR spectral analysis of complex samples.

  3. A practical approach for near infrared spectral quantitative analysis of complex samples using partial least squares modeling

    Institute of Scientific and Technical Information of China (English)

    LIU ZhiChao; MA Xiang; WEN YaDong; WANG Yi; CAI WenSheng; SHAO XueGuang

    2009-01-01

    The number of latent variables (LVs) or the factor number is a key parameter in PLS modeling to obtain a correct prediction.Although lots of work have been done on this issue,it is still a difficult task to determine a suitable LV number in practical uses.A method named independent factor diagnostics (IFD) is proposed for investigation of the contribution of each LV to the predicted results on the basis of discussion about the determination of LV number in PLS modeling for near infrared (NIR) spectra of complex samples.The NIR spectra of three data sets of complex samples,including a public data set and two tobacco lamina ones,are investigated.It is shown that several high order LVs constitute main contributions to the predicted results,albeit the contribution of the low order LVs should not be neglected in the PLS models.Therefore,in practical uses of PLS for analysis of complex samples,it may be better to use a slightly large LV number for NIR spectral analysis of complex samples.

  4. Development of a full automation solid phase microextraction method for investigating the partition coefficient of organic pollutant in complex sample.

    Science.gov (United States)

    Jiang, Ruifen; Lin, Wei; Wen, Sijia; Zhu, Fang; Luan, Tiangang; Ouyang, Gangfeng

    2015-08-07

    A fully automated solid phase microextraction (SPME) depletion method was developed to study the partition coefficient of organic compound between complex matrix and water sample. The SPME depletion process was conducted by pre-loading the fiber with a specific amount of organic compounds from a proposed standard gas generation vial, and then desorbing the fiber into the targeted samples. Based on the proposed method, the partition coefficients (Kmatrix) of 4 polyaromatic hydrocarbons (PAHs) between humic acid (HA)/hydroxypropyl-β-cyclodextrin (β-HPCD) and aqueous sample were determined. The results showed that the logKmatrix of 4 PAHs with HA and β-HPCD ranged from 3.19 to 4.08, and 2.45 to 3.15, respectively. In addition, the logKmatrix values decreased about 0.12-0.27 log units for different PAHs for every 10°C increase in temperature. The effect of temperature on the partition coefficient followed van't Hoff plot, and the partition coefficient at any temperature can be predicted based on the plot. Furthermore, the proposed method was applied for the real biological fluid analysis. The partition coefficients of 6 PAHs between the complex matrices in the fetal bovine serum and water were determined, and compared to ones obtained from SPME extraction method. The result demonstrated that the proposed method can be applied to determine the sorption coefficients of hydrophobic compounds between complex matrix and water in a variety of samples.

  5. Microextraction Techniques Used in the Procedures for Determining Organomercury and Organotin Compounds in Environmental Samples

    Directory of Open Access Journals (Sweden)

    Małgorzata Rutkowska

    2014-06-01

    Full Text Available Due to human activities, the concentrations of organometallic compounds in all parts of the environment have increased in recent decades. The toxicity and some biochemical properties of mercury and tin present in the environment depend on the concentration and chemical form of these two elements. The ever-increasing demand for determining compounds at very low concentration levels in samples with complex matrices requires the elimination of interfering substances, the reduction of the final extract volume, and analyte enrichment in order to employ a detection technique, which is characterised by high sensitivity at low limits of quantification. On the other hand, in accordance with current trends, the analytical procedures should aim at the miniaturisation and simplification of the sample preparation step. In the near future, more importance will be given to the fulfilment of the requirements of Green Chemistry and Green Analytical Chemistry in order to reduce the intensity of anthropogenic activities related to analytical laboratories. In this case, one can consider the use of solvent-free/solvent-less techniques for sample preparation and microextraction techniques, because the use of the latter leads to lowering the quantity of reagents used (including solvents due to the reduction of the scale of analysis. This paper presents an overview of microextraction techniques (SPME and LPME used in the procedures for determining different chemical forms of mercury and tin.

  6. Analytical methods for the endocrine disruptor compounds determination in environmental water samples.

    Science.gov (United States)

    Locatelli, Marcello; Sciascia, Francesco; Cifelli, Roberta; Malatesta, Luciano; Bruni, Pantaleone; Croce, Fausto

    2016-02-19

    The potential risk of exposure to different xenobiotics, which can modulate the endocrine system and represent a treat for the wellness of an increasing number of people, has recently drawn the attention of international environmental and health agencies. Several agents, characterized by structural diversity, may interfer with the normal endocrine functions that regulate cell growth, homeostasis and development. Substances such as pesticides, herbicides, plasticizers, metals, etc. having endocrine activity (EDCs) are used in agriculture and industry and are also used as drugs for humans and animals. A difficulty in the analytical determination of these substances is the complexity of the matrix in which they are present. In fact, the samples most frequently analyzed consist of groundwater and surface water, including influent and effluent of wastewater treatment plants and drinking water. In this review, several sample pretreatment protocols, assays and different instrumental techniques recently used in the EDCs determination have been considered. This review concludes with a paragraph in which the most recent hyphenated-instrument techniques are treated, highlighting their sensitivity and selectivity for the analyses of environmental water samples.

  7. Direct experimental determination of spectral densities of molecular complexes

    Energy Technology Data Exchange (ETDEWEB)

    Pachón, Leonardo A. [Grupo de Física Atómica y Molecular, Instituto de Física, Facultad de Ciencias Exactas y Naturales, Universidad de Antioquia UdeA, Calle 70 No. 52-21, Medellín (Colombia); Chemical Physics Theory Group, Department of Chemistry and Center for Quantum Information and Quantum Control, University of Toronto, Toronto, Ontario M5S 3H6 (Canada); Brumer, Paul [Chemical Physics Theory Group, Department of Chemistry and Center for Quantum Information and Quantum Control, University of Toronto, Toronto, Ontario M5S 3H6 (Canada)

    2014-11-07

    Determining the spectral density of a molecular system immersed in a proteomic scaffold and in contact to a solvent is a fundamental challenge in the coarse-grained description of, e.g., electron and energy transfer dynamics. Once the spectral density is characterized, all the time scales are captured and no artificial separation between fast and slow processes need to be invoked. Based on the fluorescence Stokes shift function, we utilize a simple and robust strategy to extract the spectral density of a number of molecular complexes from available experimental data. Specifically, we show that experimental data for dye molecules in several solvents, amino acid proteins in water, and some photochemical systems (e.g., rhodopsin and green fluorescence proteins), are well described by a three-parameter family of sub-Ohmic spectral densities that are characterized by a fast initial Gaussian-like decay followed by a slow algebraic-like decay rate at long times.

  8. Direct Experimental Determination of Spectral Densities of Molecular Complexes

    CERN Document Server

    Pachon, Leonardo A

    2014-01-01

    Determining the spectral density of a molecular system immersed in a proteomic scaffold and in contact to a solvent is a fundamental challenge in the coarse-grained description of, e.g., electron and energy transfer dynamics. Once the spectral density is characterized, all the time scales are captured and no artificial separation between fast and slow processes need be invoked. Based on the fluorescence Stokes shift function, we utilize a simple and robust strategy to extract the spectral density of a number of molecular complexes from available experimental data. Specifically, we show that experimental data for dye molecules in several solvents, amino acid proteins in water, and some photochemical systems (e.g., rhodopsin and green fluorescence proteins), are well described by a three-parameter family of sub-Ohmic spectral densities that are characterized by a fast initial Gaussian-like decay followed by a slow algebraic-like decay rate at long times.

  9. Clustering determines the dynamics of complex contagions in multiplex networks

    CERN Document Server

    Zhuang, Yong; Yağan, Osman

    2016-01-01

    We present the mathematical analysis of generalized complex contagions in clustered multiplex networks for susceptible-infected-recovered (SIR)-like dynamics. The model is intended to understand diffusion of influence, or any other spreading process implying a threshold dynamics, in setups of interconnected networks with significant clustering. The contagion is assumed to be general enough to account for a content-dependent linear threshold model, where each link type has a different weight (for spreading influence) that may depend on the content (e.g., product, rumor, political view) that is being spread. Using the generating functions formalism, we determine the conditions, probability, and expected size of the emergent global cascades. This analysis provides a generalization of previous approaches and is specially useful in problems related to spreading and percolation. The results present non trivial dependencies between the clustering coefficient of the networks and its average degree. In particular, sev...

  10. Complexity and determining dangerous levels of climate impacts

    Science.gov (United States)

    Huntingford, Chris

    2014-01-01

    A recent paper (Garten et al 2013 Environ. Res. Lett. 8 034032) finds very different global warming thresholds of concern between water scarcity and ecosystem changes. This may at first appear surprising, as each process is controlled to some extent by functioning of the land surface. Hence this analysis reflects the fundamentally different character of what constitutes water scarcity among people, compared to water stress for ecosystems. Garten et al (2013 Environ. Res. Lett. 8 034032) find both responses to warming are highly nonlinear, but in opposite senses. Water scarcity could affect multiple millions of people for even low levels of warming, but that number would almost stabilise should warming continue. In contrast, ecosystem changes become massively more responsive to climate change at higher warming levels. This re-iterates how complex the Earth system is, making it difficult to determine what constitutes overall single thresholds of climate change society may choose to consider avoiding. However, it is argued here that such targets are still much needed, providing a focal point for discussion, and complexity should not be used as an excuse to prevent setting them.

  11. Clustering determines the dynamics of complex contagions in multiplex networks

    Science.gov (United States)

    Zhuang, Yong; Arenas, Alex; Yaǧan, Osman

    2017-01-01

    We present the mathematical analysis of generalized complex contagions in a class of clustered multiplex networks. The model is intended to understand spread of influence, or any other spreading process implying a threshold dynamics, in setups of interconnected networks with significant clustering. The contagion is assumed to be general enough to account for a content-dependent linear threshold model, where each link type has a different weight (for spreading influence) that may depend on the content (e.g., product, rumor, political view) that is being spread. Using the generating functions formalism, we determine the conditions, probability, and expected size of the emergent global cascades. This analysis provides a generalization of previous approaches and is especially useful in problems related to spreading and percolation. The results present nontrivial dependencies between the clustering coefficient of the networks and its average degree. In particular, several phase transitions are shown to occur depending on these descriptors. Generally speaking, our findings reveal that increasing clustering decreases the probability of having global cascades and their size, however, this tendency changes with the average degree. There exists a certain average degree from which on clustering favors the probability and size of the contagion. By comparing the dynamics of complex contagions over multiplex networks and their monoplex projections, we demonstrate that ignoring link types and aggregating network layers may lead to inaccurate conclusions about contagion dynamics, particularly when the correlation of degrees between layers is high.

  12. Report on sampling and analysis of ambient air at the central waste complex

    Energy Technology Data Exchange (ETDEWEB)

    Stauffer, M., Fluor Daniel Hanford

    1997-02-13

    Over 160 ambient indoor air samples were collected from warehouses at the Central Waste Complex used for the storage of low- level radioactive and mixed wastes. These grab (SUMMA) samples were analyzed by gas chromatography-mass spectrometry using a modified EPA TO-14 procedure. The data from this survey suggest that several buildings had elevated concentrations of volatile organic compounds.

  13. Reducing the Computational Complexity of Reconstruction in Compressed Sensing Nonuniform Sampling

    DEFF Research Database (Denmark)

    Grigoryan, Ruben; Jensen, Tobias Lindstrøm; Arildsen, Thomas

    2013-01-01

    This paper proposes a method that reduces the computational complexity of signal reconstruction in single-channel nonuniform sampling while acquiring frequency sparse multi-band signals. Generally, this compressed sensing based signal acquisition allows a decrease in the sampling rate of frequency...

  14. Lanthanide complexes as luminogenic probes to measure sulfide levels in industrial samples

    Energy Technology Data Exchange (ETDEWEB)

    Thorson, Megan K. [Department of Medicinal Chemistry, University of Utah College of Pharmacy, Salt Lake City, UT 84108 (United States); Ung, Phuc [Monash Institute of Pharmaceutical Sciences, Monash University, Victoria 3052 (Australia); Leaver, Franklin M. [Water & Energy Systems Technology, Inc., Kaysville, UT 84037 (United States); Corbin, Teresa S. [Quality Services Laboratory, Tesoro Refining and Marketing, Salt Lake City, UT 84103 (United States); Tuck, Kellie L., E-mail: kellie.tuck@monash.edu [School of Chemistry, Monash University, Victoria 3800 (Australia); Graham, Bim, E-mail: bim.graham@monash.edu [Monash Institute of Pharmaceutical Sciences, Monash University, Victoria 3052 (Australia); Barrios, Amy M., E-mail: amy.barrios@utah.edu [Department of Medicinal Chemistry, University of Utah College of Pharmacy, Salt Lake City, UT 84108 (United States)

    2015-10-08

    A series of lanthanide-based, azide-appended complexes were investigated as hydrogen sulfide-sensitive probes. Europium complex 1 and Tb complex 3 both displayed a sulfide-dependent increase in luminescence, while Tb complex 2 displayed a decrease in luminescence upon exposure to NaHS. The utility of the complexes for monitoring sulfide levels in industrial oil and water samples was investigated. Complex 3 provided a sensitive measure of sulfide levels in petrochemical water samples (detection limit ∼ 250 nM), while complex 1 was capable of monitoring μM levels of sulfide in partially refined crude oil. - Highlights: • Lanthanide–azide based sulfide sensors were synthesized and characterized. • The probes have excitation and emission profiles compatible with sulfide-contaminated samples from the petrochemical industry. • A terbium-based probe was used to measure the sulfide concentration in oil refinery wastewater. • A europium-based probe had compatibility with partially refined crude oil samples.

  15. Determination of Optimal Double Sampling Plan using Genetic Algorithm

    Directory of Open Access Journals (Sweden)

    Sampath Sundaram

    2012-03-01

    Full Text Available Normal 0 false false false EN-US X-NONE X-NONE MicrosoftInternetExplorer4 Designing double sampling plan requires identification of sample sizes and acceptance numbers. In this paper a genetic algorithm has been designed for the selection of optimal acceptance numbers and sample sizes for the specified producer’s risk and consumer’s risk. Implementation of the algorithm has been illustrated numerically for different choices of quantities involved in a double sampling plan   

  1. A novel slurry sampling analysis of lead in different water samples by electrothermal atomic absorption spectrometry after coprecipitated with cobalt/pyrrolidine dithiocarbamate complex

    Energy Technology Data Exchange (ETDEWEB)

    Baysal, A. [Istanbul Technical University, Faculty of Science and Letters, Department of Chemistry, 34469 Maslak, Istanbul (Turkey); Akman, S. [Istanbul Technical University, Faculty of Science and Letters, Department of Chemistry, 34469 Maslak, Istanbul (Turkey)], E-mail: akmans@itu.edu.tr; Calisir, F. [Istanbul Technical University, Faculty of Science and Letters, Department of Chemistry, 34469 Maslak, Istanbul (Turkey)

    2008-10-30

    A preconcentration/separation technique based on the coprecipitation of lead with cobalt/pyrrolidine dithiocarbamate complex (Co(PDC){sub 2}) and subsequently its direct slurry sampling determination by electrothermal atomic absorption spectrometry (AAS) was described. For this purpose, at first, lead was coprecipitated with cobalt/pyrrolidine dithiocarbamate complex formed using ammonium pyrrolidine dithiocarbamate (APDC) as a chelating agent and cobalt as a carrier element. The supernatant was then separated and the slurry of the precipitate prepared in Triton X-100 was directly analyzed by electrothermal atomic absorption spectrometry with respect to lead concentration. The effects of experimental conditions on coprecipitation of lead with gathering precipitate as well as homogeneity and stability of the slurry were investigated. After the optimization of experimental parameters, a 100-fold enrichment of the analyte with quantitative recovery (>90%) and high precision (<10% R.S.D.) were obtained. By using the proposed technique, the lead concentrations in heavy matrices of Certified Sea-water and wastewater samples could be practically and rapidly determined in the range of 95% confidence level. The detection limit of the described method for lead using sample-matching blanks was 1.5 ng/L (3{sigma}, N = 10)

  2. The complex Langevin analysis of spontaneous symmetry breaking induced by complex fermion determinant

    CERN Document Server

    Ito, Yuta

    2016-01-01

    In many interesting physical systems, the determinant which appears from integrating out fermions becomes complex, and its phase plays a crucial role in the determination of the vacuum. An example of this is QCD at low temperature and high density, where various exotic fermion condensates are conjectured to form. Another example is the Euclidean version of the type IIB matrix model for 10d superstring theory, where spontaneous breaking of the SO(10) rotational symmetry down to SO(4) is expected to occur. When one applies the complex Langevin method to these systems, one encounters the singular-drift problem associated with the appearance of nearly zero eigenvalues of the Dirac operator. Here we propose to avoid this problem by deforming the action with a fermion bilinear term. The results for the original system are obtained by extrapolations with respect to the deformation parameter. We demonstrate the power of this approach by applying it to a simple matrix model, in which spontaneous symmetry breaking from...

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

    Directory of Open Access Journals (Sweden)

    Sharon L. Goddard

    2014-11-01

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

  4. A novel spectrophotometric determination of trace copper based on charge transfer complex

    Science.gov (United States)

    Di, Junwei; Wu, Ying; Ma, Yun

    2005-03-01

    A new type of colored complex, the charge transfer complex, was used to develop the spectrophotometric determination of copper. The method was based on the formation of a colored product, the charge transfer complex of copper substituted tungstophosphate with 3,3',5,5'-tetramethybenzidine (TMB), which was stabilized and sensitized by the addition of polyvinyl alcohol (PVA) in aqueous solution. The structure of copper substituted tungstophosphate was Keggin-type according to the results of infrared (IR) spectra. The optimum reaction conditions and other important analytic parameters had been investigated. Beer's law was obeyed in the copper(II) concentration range of 0.003-0.1 μg mL -1, and the molar absorptivity at 660 nm is 2.54×10 5 L mol -1 cm -1. The proposed method was simple, selective, and sensitive. It was applied to the analytic samples with satisfactory results.

  5. Determination of metals in air samples using X-Ray fluorescence associated the APDC preconcentration technique

    Energy Technology Data Exchange (ETDEWEB)

    Nardes, Raysa C.; Santos, Ramon S.; Sanches, Francis A.C.R.A.; Gama Filho, Hamilton S.; Oliveira, Davi F.; Anjos, Marcelino J., E-mail: rc.nardes@gmail.com, E-mail: ramonziosp@yahoo.com.br, E-mail: francissanches@gmail.com, E-mail: hamiltongamafilho@hotmail.com, E-mail: davi.oliveira@uerj.br, E-mail: marcelin@uerj.br [Universidade do Estado do Rio de Janeiro (UERJ), Rio de Janeiro, RJ (Brazil). Instituto de Fisica. Departamento de Fisica Aplicada e Termodinamica

    2015-07-01

    Air pollution has become one of the leading quality degradation factors of life for people in large urban centers. Studies indicate that the suspended particulate matter in the atmosphere is directly associated with risks to public health, in addition, it can cause damage to fauna, flora and public / cultural patrimonies. The inhalable particulate materials can cause the emergence and / or worsening of chronic diseases related to respiratory system and other diseases, such as reduced physical strength. In this study, we propose a new method to measure the concentration of total suspended particulate matter (TSP) in the air using an impinger as an air cleaning apparatus, preconcentration with APDC and Total Reflection X-ray Fluorescence technique (TXRF) to analyze the heavy metals present in the air. The samples were collected from five random points in the city of Rio de Janeiro/Brazil. Analyses of TXRF were performed at the Brazilian Synchrotron Light Laboratory (LNLS). The technique proved viable because it was able to detect five important metallic elements to environmental studies: Cr, Fe, Ni, Cu and Zn. This technique presented substantial efficiency in determining the elementary concentration of air pollutants, in addition to low cost. It can be concluded that the metals analysis technique in air samples using an impinger as sample collection instrument associated with a complexing agent (APDC) was viable because it is a low-cost technique, moreover, it was possible the detection of five important metal elements in environmental studies associated with industrial emissions and urban traffic. (author)

  6. Design and performance of a complex-coupled DFB laser with sampled grating

    Institute of Scientific and Technical Information of China (English)

    王桓; 朱洪亮; 贾凌慧; 陈向飞; 王圩

    2009-01-01

    A complex-coupled DFB laser with sampled grating has been designed and fabricated. The method uses the + 1 st order reflection of the sampled grating for laser single-mode operation. The typical threshold current of the sampled grating based DFB laser is 25 mA, and the optical output is about 10 mW at the injected current of 100 mA. The lasing wavelength of the device is 1.5385μm, which is the +1 st order wavelength of the sampled grating.

  7. [Determination of residual aluminium Ion in Huoxiang Zhengqi pellets by GFAAS with EDTA complexation extraction].

    Science.gov (United States)

    Wang, Xue-Na; Ran, Cong-Cong; Li, Qing-Lian; Du, Chao-Hui; Jiang, Ye

    2015-06-01

    To establish an EDTA complexation extraction pretreatment combining with GFAAS method for the determination of residual aluminium ion in Huoxiang zhengqi pellets without digestive treatment, systematical investigation was made on sample preparation, and EDTA was used for the complexation extraction of residual aluminium ion in samples. The pH, concentration and volume of extraction solution, the temperature and time of microwave extraction, and graphite furnace temperature program were investigated. The results were compared with the microwave digestion. It was showed that, 0.1 g of sample weight was added in 20 mL 0.05 mol x L(-1) EDTA solution (pH 3.5), followed by heating at 150 degrees C for 10 min in the microwave extraction device. The determination of GFAAS was performed at optimized detection wavelength (257.4 nm) as well as graphite furnace temperature program, the detection limits and quantification limits were 2.37 μg x L(-1) and 7.89 μg x L(-1), respectively. The precision (RSD) was less than 2.3%. The average recovery was 96.9% -101%. The present method is easy, rapid and accurate for the determination of residual aluminium ion in Huoxiang zhengqi pellets.

  8. Development of a sample preparation procedure for the simultaneous determination of Np and Pu in clay samples

    Energy Technology Data Exchange (ETDEWEB)

    Renz, Tobias; Quinto, Francesca; Lagos, Markus; Plaschke, Markus; Bauer, Andreas; Geckeis, Horst [INE, KIT, Eggenstein-Leopoldshafen (Germany); Taubald, Heinrich [Eberhard Karls Universitaet, Tuebingen (Germany)

    2015-07-01

    Neptunium (Np) and plutonium (Pu) are two key radionuclides for the long-term disposal of nuclear waste. Within this context Opalinus Clay formations are considered as a potential location for disposal of high-level radioactive waste. In the framework of experiments studying the diffusion behavior and retention of actinides under repository conditions, the present work focuses on the development of an analytical-chemical procedure for the determination of Np and Pu in clay (or clay-rich soil) samples. The procedure aims at the simultaneous determination of Np and Pu at femto- to attogram levels with AMS. Fields of application are the investigation of global fallout actinides in environmental clay-rich samples or the diffusion behavior of actinides in compacted clay liners used as technical barriers in nuclear waste repositories. Clay samples are spiked with certified standards of Pu-242 and Np-237. The analytical method, including a) leaching of the spiked clay samples, b) redox adjustments of Np and Pu, c) chromatographic separation of Np and Pu from the sample matrix and d) measurement of the actinides with Sector Field (SF)-ICP-MS will be presented. The suitability of a Pu isotope as non-isotopic tracer for determination of Np-237 is evaluated by determining the chemical yield using SF-ICP-MS.

  9. Determination of total sulfur in food samples by solid sampling high-resolution continuum source graphite furnace molecular absorption spectrometry.

    Science.gov (United States)

    Ozbek, Nil; Akman, Suleyman

    2013-05-22

    The determination of sulfur in food samples via the rotational molecular absorption of carbon monosulfide (CS) was performed using a solid sampling high-resolution continuum source electrothermal atomic absorption spectrophotometer (SS-HR-CS-ETAAS). In the presence of plenty of carbon in the graphite furnace as well as in food samples, CS was formed in the gas phase without the addition of any molecule forming element externally. The effects of the wavelength selected to detect CS, graphite furnace program, amount of sample, coating of the graphite tube and platform with Ir, and the use of a Pd modifier on the accuracy, precision, and sensitivity were investigated and optimized. Sulfur was determined in an iridium-coated graphite tube/platform at 258.056 nm by applying a pyrolysis temperature of 1000 °C and a molecule forming temperature of 2400 °C. The calibration curve prepared from Na2S was linear between 0.01 μg (LOQ) and 10 μg of S. The accuracy of the method was tested by analyzing certified reference spinach and milk powder samples by applying a linear calibration technique prepared from aqueous standard. The results were in good agreement with certified values. The limit of detection and characteristic mass of the method were 3.5 and 8.1 ng of S, respectively. By applying the optimized parameters, the concentrations of S in onion and garlic samples were determined.

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

    Science.gov (United States)

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

    2012-10-07

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

  11. A simple method for determining water content in organic solvents based on cobalt(II) complexes

    Institute of Scientific and Technical Information of China (English)

    Lin Zhou; Xiao Hua Liu; Hai Xin Bai; Hong Juan Wang

    2011-01-01

    A method to determine water content in organic solvents was developed based on the color change of cobalt(II) nitrate in different solvents. The color-change mechanism and optimal conditions for determining the water content were investigated. The results showed that there was a good linear relationships between the absorbance of cobalt(II) complexes in organic solvents and water contents with y in 0.9989~0.9994. This method has the advantages of low cost, good reproducibility, good sensitivity, simple in operation, fast in detection, friendly to the environment and no limitation on linear range for determining water content. It was used to determine water in samples with a satisfactory recovery in 97.81%~101.24%.

  12. A note on sample complexity of learning binary output neural networks under fixed input distributions

    CERN Document Server

    Pestov, Vladimir

    2010-01-01

    We show that the learning sample complexity of a sigmoidal neural network constructed by Sontag (1992) required to achieve a given misclassification error under a fixed purely atomic distribution can grow arbitrarily fast: for any prescribed rate of growth there is an input distribution having this rate as the sample complexity, and the bound is asymptotically tight. The rate can be superexponential, a non-recursive function, etc. We further observe that Sontag's ANN is not Glivenko-Cantelli under any input distribution having a non-atomic part.

  13. Quantitative method of determining beryllium or a compound thereof in a sample

    Science.gov (United States)

    McCleskey, T. Mark; Ehler, Deborah S.; John, Kevin D.; Burrell, Anthony K.; Collis, Gavin E.; Minogue, Edel M.; Warner, Benjamin P.

    2010-08-24

    A method of determining beryllium or a beryllium compound thereof in a sample, includes providing a sample suspected of comprising beryllium or a compound thereof, extracting beryllium or a compound thereof from the sample by dissolving in a solution, adding a fluorescent indicator to the solution to thereby bind any beryllium or a compound thereof to the fluorescent indicator, and determining the presence or amount of any beryllium or a compound thereof in the sample by measuring fluorescence.

  14. Quantitative method of determining beryllium or a compound thereof in a sample

    Energy Technology Data Exchange (ETDEWEB)

    McCleskey, T. Mark (Los Alamos, NM); Ehler, Deborah S. (Los Alamos, NM); John, Kevin D. (Santa Fe, NM); Burrell, Anthony K. (Los Alamos, NM); Collis, Gavin E. (Los Alamos, NM); Minogue, Edel M. (Los Alamos, NM); Warner, Benjamin P. (Los Alamos, NM)

    2010-08-24

    A method of determining beryllium or a beryllium compound thereof in a sample, includes providing a sample suspected of comprising beryllium or a compound thereof, extracting beryllium or a compound thereof from the sample by dissolving in a solution, adding a fluorescent indicator to the solution to thereby bind any beryllium or a compound thereof to the fluorescent indicator, and determining the presence or amount of any beryllium or a compound thereof in the sample by measuring fluorescence.

  15. Quantitative method of determining beryllium or a compound thereof in a sample

    Energy Technology Data Exchange (ETDEWEB)

    McCleskey, T. Mark; Ehler, Deborah S.; John, Kevin D.; Burrell, Anthony K.; Collis, Gavin E.; Minogue, Edel M.; Warner, Benjamin P.

    2006-10-31

    A method of determining beryllium or a beryllium compound thereof in a sample, includes providing a sample suspected of comprising beryllium or a compound thereof, extracting beryllium or a compound thereof from the sample by dissolving in a solution, adding a fluorescent indicator to the solution to thereby bind any beryllium or a compound thereof to the fluorescent indicator, and determining the presence or amount of any beryllium or a compound thereof in the sample by measuring fluorescence.

  16. SIPPI: A Matlab toolbox for sampling the solution to inverse problems with complex prior information

    DEFF Research Database (Denmark)

    Hansen, Thomas Mejer; Cordua, Knud Skou; Caroline Looms, Majken

    2013-01-01

    for solving such probabilistically formulated inverse problems by sampling the a posteriori probability density function. In order to describe the a priori probability density function, we consider both simple Gaussian models and more complex (and realistic) a priori models based on higher order statistics....... These a priori models can be used with both linear and non-linear inverse problems. For linear inverse Gaussian problems we make use of least-squares and kriging-based methods to describe the a posteriori probability density function directly. For general non-linear (i.e. non-Gaussian) inverse problems, we make...... use of the extended Metropolis algorithm to sample the a posteriori probability density function. Together with the extended Metropolis algorithm, we use sequential Gibbs sampling that allow computationally efficient sampling of complex a priori models. The toolbox can be applied to any inverse...

  17. A novel chemiluminescence method for the determination of ergometrine maleate in serum sample without chemiluminescence reagent.

    Science.gov (United States)

    Hu, Yufei; Zhang, Zhujun; Li, Gongke

    2010-04-15

    In this paper, a novel flow injection-chemiluminescence (FI-CL) method was proposed for the determination of ergometrine maleate in serum. The new CL reaction was based on the direct oxidation of ergometrine maleate by the complex of metal chelate diperiodatocuprate(III) (K(5)[Cu(HIO(6))(2)]) in an alkaline medium. The CL intensity was enhanced in the presence of ascorbic acid. Hereby under the optimum conditions, ergometrine maleate was determined over the range of 4.0 x 10(-9) gm L(-1) to 4.0 x 10(-7) gm L(-1) with a limit of detection (3 sigma) of 1.1 x 10(-9) gm L(-1). The relative standard deviation (R.S.D.) was 2.1% for 8.0 x 10(-9) gm L(-1) ergometrine maleate (n=7). The sensitive method was successfully applied to the direct determination of ergometrine maleate (ng mL(-1)) in pharmaceutical injection and serum samples. The mechanism of the reactions was also discussed.

  18. Identification and assembly of genomes and genetic elements in complex metagenomic samples without using reference genomes

    DEFF Research Database (Denmark)

    Nielsen, Henrik Bjørn; Almeida, Mathieu; Juncker, Agnieszka

    2014-01-01

    , such as particular bacterial strains or viruses, remains a largely unsolved problem. Here we present a method, based on binning co-abundant genes across a series of metagenomic samples, that enables comprehensive discovery of new microbial organisms, viruses and co-inherited genetic entities and aids assembly...... affiliations between MGS and hundreds of viruses or genetic entities. Our method provides the means for comprehensive profiling of the diversity within complex metagenomic samples....

  19. Study of complex matrix effect on solid phase microextraction for biological sample analysis.

    Science.gov (United States)

    Jiang, Ruifen; Xu, Jianqiao; Zhu, Fang; Luan, Tiangang; Zeng, Feng; Shen, Yong; Ouyang, Gangfeng

    2015-09-11

    Solid phase microextraction (SPME) has become a useful tool for in vivo monitoring the behavior of environmental organic pollutants in biological species due to its simplicity, relatively non-invasive, and cost-effective manner. However, the complex matrices in biological samples could significantly influence the extraction kinetic, and bias the quantification result. In this study, we investigated the effect of complex matrix on the extraction kinetic of SPME for biological sample analysis. Two sample matrices, phosphate-buffered saline (PBS) with bovine serum albumin (BSA) and agarose gel with BSA were used to simulate the biological fluid and tissue. Results showed that the addition of BSA significantly enhanced the mass transfer of organic compounds onto SPME fiber in both PBS buffer and gel sample. Enhancement factors ranging from 1.3 to 27, and 2.0 to 80 were found for all selected polyaromatic hydrocarbons (PAHs) in PBS buffer and agarose gel with BSA concentration of 0.1-5%, respectively. Then, an improved theoretical model was applied to quantify the observed enhancement effect, and the result showed that the predicted sampling time constant agreed well with the experimental one in complex matrix. Furthermore, a simplified equation was proposed for the real biological sample analysis.

  20. Can Soil Penetration Resistance and Bulk Density Be Determined in a Single Undisturbed Sample?

    Directory of Open Access Journals (Sweden)

    Carolina Fernandes

    2015-06-01

    Full Text Available Soil quality indicators such as penetration resistance (PR and bulk density (BD are traditionally determined in a single undisturbed soil sample. The aim of this study was to assess the effect of PR measurements of undisturbed samples on the determination of BD in the same sample of two soils differing in clay contents. To this end, samples were collected from the 0.00-0.10 and 0.10-0.20 m layers of two soils of clayey and very clayey texture. Volumetric rings were used to collect a total of 120 undisturbed soil samples from each soil layer that were divided into two subsets containing 60 units each. One sample set, designated “perforated samples”, was used to determine PR and BD in the same undisturbed sample; the other, named “intact samples”, was used to determine BD only. Bulk density values for perforated and intact samples were compared by analysis of variance, using a completely randomized experimental design. Means were compared by the t-test at 5 %. The BD values for the clayey soil were similar in perforated and intact samples from the two layers. However, BD of the very clayey soil was lower in the perforated than in the intact samples at both depths. Therefore, PR and BD in clayey soils can be accurately determined in the same undisturbed sample whereas in very clayey soils, different samples are required for this purpose.

  1. Analysis of complex samples using a portable multi-wavelength light emitting diode (LED) fluorescence spectrometer

    Science.gov (United States)

    Spectroscopic analysis of chemically complex samples often requires an increase n the dimensionality of the measured response surface. This often involves the measurement of emitted light intensities as functions of both wavelengths of excitation and emission resulting in the generation of an excita...

  2. Alignment-Free Phylogenetic Reconstruction: Sample Complexity via a Branching Process Analysis

    CERN Document Server

    Daskalakis, Constantinos

    2011-01-01

    We present an efficient phylogenetic reconstruction algorithm, allowing insertions and deletions, which provably achieves a sequence-length requirement (or sample complexity) growing polynomially in the number of taxa. Our algorithm is distance-based, that is, it relies on pairwise sequence comparisons. More importantly, our approach largely bypasses the difficult problem of multiple sequence alignment.

  3. Statistical analysis of relative labeled mass spectrometry data from complex samples using ANOVA

    Science.gov (United States)

    Oberg, Ann L.; Mahoney, Douglas W.; Eckel-Passow, Jeanette E.; Malone, Christopher J.; Wolfinger, Russell D.; Hill, Elizabeth G.; Cooper, Leslie T.; Onuma, Oyere K.; Spiro, Craig; Therneau, Terry M.; Bergen, H. Robert

    2008-01-01

    Statistical tools enable unified analysis of data from multiple global proteomic experiments, producing unbiased estimates of normalization terms despite the missing data problem inherent in these studies. The modeling approach, implementation and useful visualization tools are demonstrated via case study of complex biological samples assessed using the iTRAQ™ relative labeling protocol. PMID:18173221

  4. Detection of mutant protein in complex biological samples: Glucocerebrosidase mutations in Gaucher’s disease

    NARCIS (Netherlands)

    Bleijlevens, B.; van Breemen, M.J.; Donker-Koopman, W.E.; de Koster, C.G.; Aerts, J.M.F.G.

    2008-01-01

    We report a sensitive method to detect point mutations in proteins from complex samples. The method is based on surface-enhanced laser desorption/ionization time-of-flight (SELDI-ToF) MS but can be extended to other MS platforms. The target protein in this study is the lysosomal enzyme glucocerebros

  5. Preconcentration of Arsenic in Water Samples Using the Composition-Induced Phase Separation Method and Determination by ETAAS

    Directory of Open Access Journals (Sweden)

    Güçoğlu M.

    2013-04-01

    Full Text Available A new phase transition microextraction method was developed for determination of trace amount of arsenic ions in water samples in this work. The method is based on the critical point of miscibility of solvents. In this method the mixed solution of sample and organic solvent is initially homogeneous but is separated into two phases by adding a secondary solvent (modifier. In acidic medium As(V was complexed with ammonium molybdate, this complex was quantitatively extracted to the mixture of organic solvent (acetonitrile/methyl isobutyl ketone before ETAAS determination. Total inorganic arsenic (III, V was extracted similarly after oxidation of As(III to As(V with nitric acid. Concentration of As(III was calculated by difference in the concentration between total arsenic and As(V. Optimization of the experimental conditions and instrumental parameters was investigated in detail. A detection limit of 0.05 μgL−1 with enrichment factor of 85 was achieved for only 5 mL of sample. The analytical curve was linear in the concentration range of 0.25-4.00 μgL−1. Relative standard deviation (RSD for 10 replicate determinations of 2.0 μgL−1 of As(V was 4,1%. The method was successfully applied to preconcentration and determination of arsenic in real water samples.

  6. Determination of thorium(IV with rifampicin in synthetic mixture and soil samples by spectrophotometry

    Directory of Open Access Journals (Sweden)

    Lutfullah

    2016-11-01

    Full Text Available A validated spectrophotometric method has been described for the determination of thorium(IV in synthetic mixture and soil samples. The method is based on the complexation of thorium(IV with rifampicin at room temperature which absorbs maximally at 525 nm. Beer's law is obeyed in the concentration range 1.16–23.2 μg mL−1 with apparent molar absorptivity and Sandell's sensitivity of 8.23 × 103 L mol−1 cm−1 and 0.0232 μg/cm2/0.001 absorbance unit, respectively. The influence of variables was investigated and optimized. Interference due to other metal ions was studied and the tolerance limit was achieved. The proposed method was applied to the analysis of thorium(IV in a synthetic mixture containing various other metal ions and in soil samples. The results of analyses of the proposed method were statistically compared with the reference method showing acceptable recovery and precision.

  7. Cloud point extraction and flame atomic absorption spectrometric determination of cadmium and nickel in drinking and wastewater samples.

    Science.gov (United States)

    Naeemullah; Kazi, Tasneem G; Shah, Faheem; Afridi, Hassan I; Baig, Jameel Ahmed; Soomro, Abdul Sattar

    2013-01-01

    A simple method for the preconcentration of cadmium (Cd) and nickel (Ni) in drinking and wastewater samples was developed. Cloud point extraction has been used for the preconcentration of both metals, after formation of complexes with 8-hydroxyquinoline (8-HQ) and extraction with the surfactant octylphenoxypolyethoxyethanol (Triton X-114). Dilution of the surfactant-rich phase with acidified ethanol was performed after phase separation, and the Cd and Ni contents were measured by flame atomic absorption spectrometry. The experimental variables, such as pH, amounts of reagents (8-HQ and Triton X-114), temperature, incubation time, and sample volume, were optimized. After optimization of the complexation and extraction conditions, enhancement factors of 80 and 61, with LOD values of 0.22 and 0.52 microg/L, were obtained for Cd and Ni, respectively. The proposed method was applied satisfactorily for the determination of both elements in drinking and wastewater samples.

  8. New Laboratory Technique to Determine Thermal Conductivity of Complex Regolith Simulants Under High Vacuum

    Science.gov (United States)

    Ryan, A. J.; Christensen, P. R.

    2016-12-01

    Laboratory measurements have been necessary to interpret thermal data of planetary surfaces for decades. We present a novel radiometric laboratory method to determine temperature-dependent thermal conductivity of complex regolith simulants under high vacuum and across a wide range of temperatures. Here, we present our laboratory method, strategy, and initial results. This method relies on radiometric temperature measurements instead of contact measurements, eliminating the need to disturb the sample with thermal probes. We intend to determine the conductivity of grains that are up to 2 cm in diameter and to parameterize the effects of angularity, sorting, layering, composition, and cementation. These results will support the efforts of the OSIRIS-REx team in selecting a site on asteroid Bennu that is safe and meets grain size requirements for sampling. Our system consists of a cryostat vacuum chamber with an internal liquid nitrogen dewar. A granular sample is contained in a cylindrical cup that is 4 cm in diameter and 1 to 6 cm deep. The surface of the sample is exposed to vacuum and is surrounded by a black liquid nitrogen cold shroud. Once the system has equilibrated at 80 K, the base of the sample cup is rapidly heated to 450 K. An infrared camera observes the sample from above to monitor its temperature change over time. We have built a time-dependent finite element model of the experiment in COMSOL Multiphysics. Boundary temperature conditions and all known material properties (including surface emissivities) are included to replicate the experiment as closely as possible. The Optimization module in COMSOL is specifically designed for parameter estimation. Sample thermal conductivity is assumed to be a quadratic or cubic polynomial function of temperature. We thus use gradient-based optimization methods in COMSOL to vary the polynomial coefficients in an effort to reduce the least squares error between the measured and modeled sample surface temperature.

  9. Assessment of methods to recover DNA from bacteria, fungi and archaea in complex environmental samples.

    Science.gov (United States)

    Guillén-Navarro, Karina; Herrera-López, David; López-Chávez, Mariana Y; Cancino-Gómez, Máximo; Reyes-Reyes, Ana L

    2015-11-01

    DNA extraction from environmental samples is a critical step for metagenomic analysis to study microbial communities, including those considered uncultivable. Nevertheless, obtaining good quality DNA in sufficient quantities for downstream methodologies is not always possible, and it depends on the complexity and stability of each ecosystem, which could be more problematic for samples from tropical regions because those ecosystems are less stable and more complex. Three laboratory methods for the extraction of nucleic acids from samples representing unstable (decaying coffee pulp and mangrove sediments) and relatively stable (compost and soil) environments were tested. The results were compared with those obtained using two commercial DNA extraction kits. The quality of the extracted DNA was evaluated by PCR amplification to verify the recovery of bacterial, archaeal, and fungal genetic material. The laboratory method that gave the best results used a lysis procedure combining physical, chemical, and enzymatic steps.

  10. Immersed single-drop microextraction-electrothermal vaporization atomic absorption spectroscopy for the trace determination of mercury in water samples.

    Science.gov (United States)

    Bagheri, Habib; Naderi, Mehrnoush

    2009-06-15

    A new method based on single-drop microextraction (SDME) combined with electrothermal vaporization atomic absorption spectroscopy (ETV-AAS) was developed for the trace determination of mercury in water samples. A microdrop of m-xylene was applied as the extraction solvent. After extraction, the microdrop was introduced, directly, into a graphite furnace of AAS. Some important extraction parameters such as type of solvent, volume of solvent, sample stirring, ionic strength, sample pH, chelating agent concentration, sample temperature, and extraction time were investigated and optimized. The highest possible microdrop volume of 10 microL, a sampling temperature of 27 degrees C, and use of m-xylene containing dithizone, as complexing agent, are major parameters led to achieve a high enrichment factor of 970. Under the optimized conditions, the detection limit of the method was 0.01 microg L(-1) and the relative standard deviation was 6.1% (n=7). The proposed method has been successfully applied to the determination of Hg in two river water samples. The effects of interfering species such as Pt, Pd, Cu, Au, and Bi, having the tendency to form complexes with dithizone, at two concentration levels of 100 and 1000 microg L(-1) were also studied.

  11. Determining the topology of stable protein-DNA complexes.

    Science.gov (United States)

    Darcy, Isabel K; Vazquez, Mariel

    2013-04-01

    Difference topology is an experimental technique that can be used to unveil the topological structure adopted by two or more DNA segments in a stable protein-DNA complex. Difference topology has also been used to detect intermediates in a reaction pathway and to investigate the role of DNA supercoiling. In the present article, we review difference topology as applied to the Mu transpososome. The tools discussed can be applied to any stable nucleoprotein complex.

  12. Sample Size Determination for Regression Models Using Monte Carlo Methods in R

    Science.gov (United States)

    Beaujean, A. Alexander

    2014-01-01

    A common question asked by researchers using regression models is, What sample size is needed for my study? While there are formulae to estimate sample sizes, their assumptions are often not met in the collected data. A more realistic approach to sample size determination requires more information such as the model of interest, strength of the…

  13. Rapid detection of Mycobacterium tuberculosis complex in sputum Samples using PURE TB-LAMP assay.

    Science.gov (United States)

    N'guessan, K; Horo, K; Coulibaly, I; Adegbele, J; Kouame-Adjei, N; Seck-Angu, H; Guei, A; Kouakou, J; Dosso, M

    2016-12-01

    Lack of rapid and accurate diagnostic testing is a critical obstacle to global tuberculosis (TB) control. Sensitivity of sputum smear microscopy (SSM) is not optimal; however, it remains the most prevalent tool for TB confirmation in poor countries. As a part of passive case finding of TB detection, this study was conducted to determine the clinical performance of PURE TB-LAMP assay using liquid culture medium as the gold standard. Centre Antituberculeux de Yopougon is one of the 17 intermediate Tuberculosis centers in Côte d'Ivoire. A standardized questionnaire was submitted to patients with signs and symptoms consistent with tuberculosis by a trained caregiver. After obtaining signed consent forms, sputum samples were collected according to National TB Control Programme guidelines (spot-morning). SSM after Ziehl-Neelsen staining and TB-LAMP assay were blindly performed on the first sample. Samples transported to Institut Pasteur de Côte d'Ivoire were decontaminated according to the N-acetyl-L-Cystein method. In Mycobacteria Growth Indicator Tube (MGIT), 500mL of pellets were inoculated and incubated in the MGIT 960 system. MPT64 antigen was detected in positive cultures. Of the 500 patients enrolled, 469 (232men and 239 women) patients were included. The mean ages of men and women were 36.9 (15-86) and 37.3 (15-37.3) years, respectively. There were 56 (12.2%) HIV-infected patients, including 14 women. Clinical isolates of M. tuberculosis complex were detected for 157 (33.5%) patients. Compared with culturing, the overall sensitivity and specificity of SSM were 86% (95% confidence interval [CI]=81-91) and 96% (95% CI=94-98), respectively. The overall sensitivity and specificity for TB-LAMP was 92% (95% CI=0.88-0.96) and 94% (95% CI=0.91-0.97), respectively. Positive likelihood ratios for TB-LAMP and SSM were 15.3 and 21.5, respectively, and negative likelihood ratios for TB-LAMP and SSM were 0.09 and 0.15, respectively. Among the 469 patients, active

  14. Determination of rhodium in metallic alloy and water samples using cloud point extraction coupled with spectrophotometric technique.

    Science.gov (United States)

    Kassem, Mohammed A; Amin, Alaa S

    2015-02-01

    A new method to estimate rhodium in different samples at trace levels had been developed. Rhodium was complexed with 5-(4'-nitro-2',6'-dichlorophenylazo)-6-hydroxypyrimidine-2,4-dione (NDPHPD) as a complexing agent in an aqueous medium and concentrated by using Triton X-114 as a surfactant. The investigated rhodium complex was preconcentrated with cloud point extraction process using the nonionic surfactant Triton X-114 to extract rhodium complex from aqueous solutions at pH 4.75. After the phase separation at 50°C, the surfactant-rich phase was heated again at 100°C to remove water after decantation and the remaining phase was dissolved using 0.5mL of acetonitrile. Under optimum conditions, the calibration curve was linear for the concentration range of 0.5-75ngmL(-1) and the detection limit was 0.15ngmL(-1) of the original solution. The enhancement factor of 500 was achieved for 250mL samples containing the analyte and relative standard deviations were ⩽1.50%. The method was found to be highly selective, fairly sensitive, simple, rapid and economical and safely applied for rhodium determination in different complex materials such as synthetic mixture of alloys and environmental water samples.

  15. Determination of rhodium in metallic alloy and water samples using cloud point extraction coupled with spectrophotometric technique

    Science.gov (United States)

    Kassem, Mohammed A.; Amin, Alaa S.

    2015-02-01

    A new method to estimate rhodium in different samples at trace levels had been developed. Rhodium was complexed with 5-(4‧-nitro-2‧,6‧-dichlorophenylazo)-6-hydroxypyrimidine-2,4-dione (NDPHPD) as a complexing agent in an aqueous medium and concentrated by using Triton X-114 as a surfactant. The investigated rhodium complex was preconcentrated with cloud point extraction process using the nonionic surfactant Triton X-114 to extract rhodium complex from aqueous solutions at pH 4.75. After the phase separation at 50 °C, the surfactant-rich phase was heated again at 100 °C to remove water after decantation and the remaining phase was dissolved using 0.5 mL of acetonitrile. Under optimum conditions, the calibration curve was linear for the concentration range of 0.5-75 ng mL-1 and the detection limit was 0.15 ng mL-1 of the original solution. The enhancement factor of 500 was achieved for 250 mL samples containing the analyte and relative standard deviations were ⩽1.50%. The method was found to be highly selective, fairly sensitive, simple, rapid and economical and safely applied for rhodium determination in different complex materials such as synthetic mixture of alloys and environmental water samples.

  16. Determination of Fluoride in Various Samples and Some Infusions Using a Fluoride Selective Electrode

    OpenAIRE

    TOKALIOĞLU, Şerife; Kartal, Şenol; ŞAHİN, Uğur

    2004-01-01

    The determination of fluoride in some environmental samples was performed using a fluoride ion-selective electrode. Fluoride concentrations were determined in drinking waters (from different provinces, districts and villages in Turkey), fruit juices, bottled water samples, toothpastes and tooth powders, liquors of Turkish coffee, coffee, linden, rose hip, and various brand tea infusions, and dust samples collected from the Erciyes University campus car park. The average fluoride conc...

  17. Determination of total mercury for marine environmental monitoring studies by solid sampling continuum source high resolution atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mandjukov, Petko; Orani, Anna Maria; Han, Eunmi; Vassileva, Emilia, E-mail: e.vasileva-veleva@iaea.org

    2015-01-01

    The most critical step in almost all commonly used analytical procedures for Hg determination is the sample preparation due to its extreme volatility. One of the possible solutions of this problem is the application of methods for direct analysis of solid samples. The possibilities for solid sampling high resolution continuum source atomic absorption spectrometry (HR CS AAS) determination of total mercury in various marine environmental samples e.g. sediments and biota are object of the present study. The instrumental parameters were optimized in order to obtain reproducible and interference free analytical signal. A calibration technique based on the use of solid standard certified reference materials similar to the nature of the analyzed sample was developed and applied to various CRMs and real samples. This technique allows simple and reliable evaluation of the uncertainty of the result and the metrological characteristics of the method. A validation approach in line with the requirements of ISO 17025 standard and Eurachem guidelines was followed. With this in mind, selectivity, working range (0.06 to 25 ng for biota and 0.025 to 4 ng for sediment samples, expressed as total Hg) linearity (confirmed by Student's t-test), bias (1.6–4.3%), repeatability (4–9%), reproducibility (9–11%), and absolute limit of detection (0.025 ng for sediment, 0.096 ng for marine biota) were systematically assessed using solid CRMs. The relative expanded uncertainty was estimated at 15% for sediment sample and 8.5% for marine biota sample (k = 2). Demonstration of traceability of measurement results is also presented. The potential of the proposed analytical procedure, based on solid sampling HR CS AAS technique was demonstrated by direct analysis of sea sediments form the Caribbean region and various CRMs. Overall, the use of solid sampling HR CS AAS permits obtaining significant advantages for the determination of this complex analyte in marine samples, such as

  18. Using machine learning tools to model complex toxic interactions with limited sampling regimes.

    Science.gov (United States)

    Bertin, Matthew J; Moeller, Peter; Guillette, Louis J; Chapman, Robert W

    2013-03-19

    A major impediment to understanding the impact of environmental stress, including toxins and other pollutants, on organisms, is that organisms are rarely challenged by one or a few stressors in natural systems. Thus, linking laboratory experiments that are limited by practical considerations to a few stressors and a few levels of these stressors to real world conditions is constrained. In addition, while the existence of complex interactions among stressors can be identified by current statistical methods, these methods do not provide a means to construct mathematical models of these interactions. In this paper, we offer a two-step process by which complex interactions of stressors on biological systems can be modeled in an experimental design that is within the limits of practicality. We begin with the notion that environment conditions circumscribe an n-dimensional hyperspace within which biological processes or end points are embedded. We then randomly sample this hyperspace to establish experimental conditions that span the range of the relevant parameters and conduct the experiment(s) based upon these selected conditions. Models of the complex interactions of the parameters are then extracted using machine learning tools, specifically artificial neural networks. This approach can rapidly generate highly accurate models of biological responses to complex interactions among environmentally relevant toxins, identify critical subspaces where nonlinear responses exist, and provide an expedient means of designing traditional experiments to test the impact of complex mixtures on biological responses. Further, this can be accomplished with an astonishingly small sample size.

  19. Determination of iodine and iodine compounds in marine samples by ICPMS and HPLC-ICPMS

    DEFF Research Database (Denmark)

    Hansen, Maiken Sødergreen; Lewandowski, Daniel Jacob; Rasmussen, Rie Romme

    2014-01-01

    for determining the different iodine species. For determining the total iodine concentration in marine samples five different extraction methods were compared. The most efficient and precise method was then used for determining the total concentration of iodine in seaweed and fish samples using inductively...... (HPLC) coupled to ICPMS. These studies may be a stepping stone for further studies that can clarify the cycle and implications of iodine species in relation to the use of marine food items as iodine sources....

  20. The mitochondrial contact site complex, a determinant of mitochondrial architecture

    Science.gov (United States)

    Harner, Max; Körner, Christian; Walther, Dirk; Mokranjac, Dejana; Kaesmacher, Johannes; Welsch, Ulrich; Griffith, Janice; Mann, Matthias; Reggiori, Fulvio; Neupert, Walter

    2011-01-01

    Mitochondria are organelles with a complex architecture. They are bounded by an envelope consisting of the outer membrane and the inner boundary membrane (IBM). Narrow crista junctions (CJs) link the IBM to the cristae. OMs and IBMs are firmly connected by contact sites (CS). The molecular nature of the CS remained unknown. Using quantitative high-resolution mass spectrometry we identified a novel complex, the mitochondrial contact site (MICOS) complex, formed by a set of mitochondrial membrane proteins that is essential for the formation of CS. MICOS is preferentially located at the CJs. Upon loss of one of the MICOS subunits, CJs disappear completely or are impaired, showing that CJs require the presence of CS to form a superstructure that links the IBM to the cristae. Loss of MICOS subunits results in loss of respiratory competence and altered inheritance of mitochondrial DNA. PMID:22009199

  1. Determination of ferrous iron in rock and mineral samples by three volumetric methods

    OpenAIRE

    Saikkonen, R.J.; Rautiainen, I.A.

    1993-01-01

    Ferrous iron was determined by three volumetric methods in 13 in-house reference rock samples and in 31 international geological reference samples. The methods used were Amonette & Scott' s oxidimetric method, Wilson's oxidimetric method and Pratt's method. The results for FeO by these volumetric methods in 13 in-house rock samples were compared to the results obtained in other analytical laboratories in Finland. The results for FeO in the international samples were compared with published da...

  2. Preconcentration and determination of heavy metals in water, sediment and biological samples

    OpenAIRE

    Shirkhanloo Hamid; Mousavi Zavvar Hassan; Rouhollahi Ahmad

    2011-01-01

    In this study, a simple, sensitive and accurate column preconcentration method was developed for the determination of Cd, Cu and Pb ions in river water, urine and sediment samples by flame atomic absorption spectrometry. The procedure is based on the retention of the analytes on a mixed cellulose ester membrane (MCEM) column from buffered sample solutions and then their elution from the column with nitric acid. Several parameters, such as pH of the sample solution, volume of the sample ...

  3. Statistical power to detect genetic (covariance of complex traits using SNP data in unrelated samples.

    Directory of Open Access Journals (Sweden)

    Peter M Visscher

    2014-04-01

    Full Text Available We have recently developed analysis methods (GREML to estimate the genetic variance of a complex trait/disease and the genetic correlation between two complex traits/diseases using genome-wide single nucleotide polymorphism (SNP data in unrelated individuals. Here we use analytical derivations and simulations to quantify the sampling variance of the estimate of the proportion of phenotypic variance captured by all SNPs for quantitative traits and case-control studies. We also derive the approximate sampling variance of the estimate of a genetic correlation in a bivariate analysis, when two complex traits are either measured on the same or different individuals. We show that the sampling variance is inversely proportional to the number of pairwise contrasts in the analysis and to the variance in SNP-derived genetic relationships. For bivariate analysis, the sampling variance of the genetic correlation additionally depends on the harmonic mean of the proportion of variance explained by the SNPs for the two traits and the genetic correlation between the traits, and depends on the phenotypic correlation when the traits are measured on the same individuals. We provide an online tool for calculating the power of detecting genetic (covariation using genome-wide SNP data. The new theory and online tool will be helpful to plan experimental designs to estimate the missing heritability that has not yet been fully revealed through genome-wide association studies, and to estimate the genetic overlap between complex traits (diseases in particular when the traits (diseases are not measured on the same samples.

  4. Spectrofluorimetric quantification of bilirubin using yttrium-norfloxacin complex as a fluorescence probe in serum samples

    Energy Technology Data Exchange (ETDEWEB)

    Kamruzzaman, Mohammad; Alam, Al-Mahmnur [Department of Chemistry, Kyungpook National University, Daegu 702-701 (Korea, Republic of); Hak Lee, Sang, E-mail: shlee@knu.ac.kr [Department of Chemistry, Kyungpook National University, Daegu 702-701 (Korea, Republic of); Ho Kim, Young, E-mail: youngkim@knu.ac.kr [Research Institute of Advanced Energy Technology, Kyungpook National University, Daegu 702-701 (Korea, Republic of); Kim, Gyu-Man [School of Mechanical Engineering, Kyungpook National University, Daegu 702-701 (Korea, Republic of); Hyub Oh, Sang [Center for Gas Analysis, Korea Research Institute of Standards and Science, Daejeon 305-600 (Korea, Republic of)

    2012-11-15

    A simple and sensitive spectrofluorimetric method was developed to determine trace amounts of bilirubin (BR) using yttrium (Y{sup 3+})-norfloxacin (NFLX) complex as a fluorescence (FL) probe. NFLX can form a stable binary complex with Y{sup 3+} and markedly enhances the weak FL signal of the NFLX. The FL intensity of the Y{sup 3+}-NFLX complex decreased significantly in the presence of BR in a buffer solution at pH=7.2. Under optimal conditions, the FL intensity decreased according to the BR concentration and showed a good linear relationship in the range of 0.03-2.3 {mu}g mL{sup -1} of BR with a correlation coefficient of 0.9988. The limit of detection for the determination of BR was 2.8 ng mL{sup -1} with a relative standard deviation (RSD) of 1.55% for five replicate determination of 0.05 {mu}g mL{sup -1} BR. The presented method offers higher sensitivity with simple instrumentation and was applied successfully in detecting BR at low concentrations. Highlights: Black-Right-Pointing-Pointer Weak FL signal of NFLX was enhanced at 419 nm by forming binary complex with Y{sup 3+}. Black-Right-Pointing-Pointer The FL intensity of Y{sup 3+}-NFLX complex was quenched markedly in the presence of ATP. Black-Right-Pointing-Pointer NFLX can transfer energy to Y{sup 3+} and BR and form the Y{sup 3+}-NFLX-ATP ternary complex. Black-Right-Pointing-Pointer The reduced FL intensity of the system was correlated with the concentration of BR. Black-Right-Pointing-Pointer The method is applied to determine BR at low concentration (2.8 ng mL{sup -1}) in serum.

  5. nES GEMMA Analysis of Lectins and Their Interactions with Glycoproteins - Separation, Detection, and Sampling of Noncovalent Biospecific Complexes

    Science.gov (United States)

    Engel, Nicole Y.; Weiss, Victor U.; Marchetti-Deschmann, Martina; Allmaier, Günter

    2017-01-01

    In order to better understand biological events, lectin-glycoprotein interactions are of interest. The possibility to gather more information than the mere positive or negative response for interactions brought mass spectrometry into the center of many research fields. The presented work shows the potential of a nano-electrospray gas-phase electrophoretic mobility molecular analyzer (nES GEMMA) to detect weak, noncovalent, biospecific interactions besides still unbound glycoproteins and unreacted lectins without prior liquid phase separation. First results for Sambucus nigra agglutinin, concanavalin A, and wheat germ agglutinin and their retained noncovalent interactions with glycoproteins in the gas phase are presented. Electrophoretic mobility diameters (EMDs) were obtained by nES GEMMA for all interaction partners correlating very well with molecular masses determined by matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) of the individual molecules. Moreover, EMDs measured for the lectin-glycoprotein complexes were in good accordance with theoretically calculated mass values. Special focus was laid on complex formation for different lectin concentrations and binding specificities to evaluate the method with respect to results obtained in the liquid phase. The latter was addressed by capillary electrophoresis on-a-chip (CE-on-a-chip). Of exceptional interest was the fact that the formed complexes could be sampled according to their size onto nitrocellulose membranes after gas-phase separation. Subsequent immunological investigation further proved that the collected complex actually retained its native structure throughout nES GEMMA analysis and sampling.

  6. Indirect spectrophotometric determination of arbutin, whitening agent through oxidation by periodate and complexation with ferric chloride

    Science.gov (United States)

    Barsoom, B. N.; Abdelsamad, A. M. E.; Adib, N. M.

    2006-07-01

    A simple and accurate spectrophotometric method for the determination of arbutin (glycosylated hydroquinone) is described. It is based on the oxidation of arbutin by periodate in presence of iodate. Excess periodate causes liberation of iodine at pH 8.0. The unreacted periodate is determined by measurement of the liberated iodine spectrophotometrically in the wavelength range (300-500 nm). A calibration curve was constructed for more accurate results and the correlation coefficient of linear regression analysis was -0.9778. The precision of this method was better than 6.17% R.S.D. ( n = 3). Regression analysis of Bear-Lambert plot shows good correlation in the concentration range 25-125 ug/ml. The identification limit was determined to be 25 ug/ml a detailed study of the reaction conditions was carried out, including effect of changing pH, time, temperature and volume of periodate. Analyzing pure and authentic samples containing arbutin tested the validity of the proposed method which has an average percent recovery of 100.86%. An alternative method is also proposed which involves a complexation reaction between arbutin and ferric chloride solution. The produced complex which is yellowish-green in color was determined spectophotometrically.

  7. Demonstrating an Order-of-Magnitude Sampling Enhancement in Molecular Dynamics Simulations of Complex Protein Systems.

    Science.gov (United States)

    Pan, Albert C; Weinreich, Thomas M; Piana, Stefano; Shaw, David E

    2016-03-01

    Molecular dynamics (MD) simulations can describe protein motions in atomic detail, but transitions between protein conformational states sometimes take place on time scales that are infeasible or very expensive to reach by direct simulation. Enhanced sampling methods, the aim of which is to increase the sampling efficiency of MD simulations, have thus been extensively employed. The effectiveness of such methods when applied to complex biological systems like proteins, however, has been difficult to establish because even enhanced sampling simulations of such systems do not typically reach time scales at which convergence is extensive enough to reliably quantify sampling efficiency. Here, we obtain sufficiently converged simulations of three proteins to evaluate the performance of simulated tempering, a member of a widely used class of enhanced sampling methods that use elevated temperature to accelerate sampling. Simulated tempering simulations with individual lengths of up to 100 μs were compared to (previously published) conventional MD simulations with individual lengths of up to 1 ms. With two proteins, BPTI and ubiquitin, we evaluated the efficiency of sampling of conformational states near the native state, and for the third, the villin headpiece, we examined the rate of folding and unfolding. Our comparisons demonstrate that simulated tempering can consistently achieve a substantial sampling speedup of an order of magnitude or more relative to conventional MD.

  8. Identifying Determinants for Neurobehavioral Morbidity in Tuberous Sclerosis Complex

    NARCIS (Netherlands)

    A.M. van Eeghen (Agnies)

    2013-01-01

    markdownabstract__Abstract__ Tuberous Sclerosis Complex (TSC) is a multisystem disorder characterized by the growth of hamartomas in multiple organ systems. The syndrome was described as early as 1835 by Rayer, and later by von Recklinghousen. In 1880, Bourneville described the syndrome in three pa

  9. Characterization and classification of complex PAH samples using GC-qMS and GC-TOFMS.

    Science.gov (United States)

    Bergknut, Magnus; Frech, Kristina; Andersson, Patrik L; Haglund, Peter; Tysklind, Mats

    2006-12-01

    The aim of this study was to compare the polycyclic aromatic hydrocarbon (PAH) contents in a number of complex samples, including soil samples from industrial sites, anti-skid sand, urban dust and ash samples from municipal solid waste incinerators. The samples were characterized by routine analysis of PAHs (gas chromatography-quadrupole mass spectrometry) and gas chromatography-time of flight mass spectrometry (GC-TOFMS). Classification of the samples by principal component analysis (PCA) according to their composition of PAHs revealed that samples associated with traffic and the municipal incinerator formed homogeneous clusters, while the PAH-contaminated soils clustered in separate groups. Using spectral data to resolve co-eluting chromatographic peaks, 962 peaks could be identified in the GC-TOFMS analysis of a pooled sample and 123-527 peaks in the individual samples. Many of the studied extracts included a unique set of chemicals, indicating that they had a much more diverse contamination profile than their PAH contents suggested. Compared to routine analysis, GC-TOFMS provided more detailed information about each sample and in this study a large number of alkylated PAHs were found to be associated with the corresponding unsubstituted PAHs. The possibility to filter peaks according to different criteria (e.g. to include only peaks that were detected in the analysis of another sample) was explored and used to identify unique as well as common compounds within samples. This procedure could prove to be valuable for obtaining relevant chemical data for use in conjunction with results from various biological test systems.

  10. Separation and characterization of nanoparticles in complex food and environmental samples by field-flow fractionation

    DEFF Research Database (Denmark)

    Kammer, Frank von der; Legros, Samuel; Hofmann, Thilo

    2011-01-01

    The thorough analysis of natural nanoparticles (NPs) and engineered NPs involves the sequence of detection, identification, quantification and, if possible, detailed characterization. In a complex or heterogeneous sample, each step of this sequence is an individual challenge, and, given suitable...... has been applied for separation of various types of NP (e.g., organic macromolecules, and carbonaceous or inorganic NPs) in different types of media (e.g., natural waters, soil extracts or food samples).FFF can be coupled to different types of detectors that offer additional information...

  11. Determination of thorium and uranium contents in soil samples using SSNTD's passive method

    Indian Academy of Sciences (India)

    T A Salama; U Seddik; T M Dsoky; A Ahmed Morsy; R El-Asser

    2006-08-01

    Thorium-to-uranium ratios have been determined in different soil samples using CR-39 and LR-115-II solid-state nuclear track detectors (SSNTDs). A calibration method based on determination of SSNTD registration sensitivity ratio for -particles of thorium and uranium series has been developed. Thorium and uranium contents of the standard soil samples have been determined and compared with its known values. There is a good agreement between the results of this method and the values of standard samples. The method is simple, inexpensive, non-destructive and has a wide range of applications in environment, building materials and petroleum fields.

  12. Sorptive extraction with in-sample acetylation for gas chromatography-mass spectrometry determination of ethylphenol species in wine samples.

    Science.gov (United States)

    Carpinteiro, I; Abuín, B; Rodríguez, I; Ramil, M; Cela, R

    2010-11-12

    An inexpensive and effective sample preparation procedure for the determination of three ethylphenolic off-flavours (4-ethylphenol, 4-ethylguaiacol and 4-ethylcathecol) in wine samples is presented. Analytes were in situ acetylated and concentrated using a disposable silicone sorbent (DSS) exposed to the diluted sample. After that, the analytes were recovered with ethyl acetate and determined by gas chromatography with mass spectrometry. The influence of different parameters (volume of acetic anhydride, basic catalyst, ionic strength, sorbent format, sampling mode and extraction time) on the efficiency of derivatization and extraction steps is discussed. Under optimized conditions, 2 mL of wine were diluted with 15 mL of an aqueous solution of potassium bicarbonate (5%, m/v) in a 22 mL vessel, containing 2 g of sodium chloride. The volume of acetic anhydride and the extraction time were set at 90 μL and 2 h, and the extraction was carried out at room temperature (20±2°C). Analytes were concentrated using a silicone disc (5 mm diameter × 0.5 mm thickness) and further desorbed with 0.2 mL of ethyl acetate. The achieved limits of quantification (LOQs), defined as the concentration of each compound providing a signal 10 times higher than the baseline noise, stayed between 5 and 15 ng mL(-1). The method provided a linear response range of up to 5000 ng mL(-1) and relative recoveries from 91% to 116%. The 4-ethylphenol off-flavour was detected in most red wine samples at concentrations of up to 2700 ng mL(-1). Copyright © 2010 Elsevier B.V. All rights reserved.

  13. Mutually exclusive CBC-containing complexes determine RNA fate

    DEFF Research Database (Denmark)

    Giacometti, Simone; Benbahouche, Nour El Houda; Domanski, Michal

    2016-01-01

    The cap-binding complex (CBC) stimulates processing reactions of capped RNAs, including their splicing, 3'end formation, degradation and nuclear transport. CBC effects are particular for individual RNA families, but how such selectivity is achieved remains elusive. Here, we map in vivo RNA binding...... specificities of CBC partners: PHAX, which functions in pre-sn(o)RNAs transport; ZC3H18, which associates with the nuclear exosome targeting (NEXT) complex to trigger RNA degradation and ARS2, which stimulates 3' end-formation/transcription termination of several transcript types. Surprisingly, these proteins...... all bind capped RNAs without strong preferences for given families or individual transcripts. Despite this, PHAX and ZC3H18 compete for CBC-binding, which is functionally relevant, since depletion of one factor sensitizes RNAs to the presence of the other. This suggests that interactions of factors...

  14. Electrostatics determine vibrational frequency shifts in hydrogen bonded complexes.

    Science.gov (United States)

    Dey, Arghya; Mondal, Sohidul Islam; Sen, Saumik; Ghosh, Debashree; Patwari, G Naresh

    2014-12-14

    The red-shifts in the acetylenic C-H stretching vibration of C-H∙∙∙X (X = O, N) hydrogen-bonded complexes increase with an increase in the basicity of the Lewis base. Analysis of various components of stabilization energy suggests that the observed red-shifts are correlated with the electrostatic component of the stabilization energy, while the dispersion modulates the stabilization energy.

  15. Assessing usual dietary intake in complex sample design surveys: the National Dietary Survey

    Directory of Open Access Journals (Sweden)

    Flávia dos Santos Barbosa

    2013-02-01

    Full Text Available The National Cancer Institute (NCI method allows the distributions of usual intake of nutrients and foods to be estimated. This method can be used in complex surveys. However, the user must perform additional calculations, such as balanced repeated replication (BRR, in order to obtain standard errors and confidence intervals for the percentiles and mean from the distribution of usual intake. The objective is to highlight adaptations of the NCI method using data from the National Dietary Survey. The application of the NCI method was exemplified analyzing the total energy (kcal and fruit (g intake, comparing estimations of mean and standard deviation that were based on the complex design of the Brazilian survey with those assuming simple random sample. Although means point estimates were similar, estimates of standard error using the complex design increased by up to 60% compared to simple random sample. Thus, for valid estimates of food and energy intake for the population, all of the sampling characteristics of the surveys should be taken into account because when these characteristics are neglected, statistical analysis may produce underestimated standard errors that would compromise the results and the conclusions of the survey.

  16. Optimized and validated spectrophotometric method for the determination of uranium(VI) via complexation with meloxicam

    Energy Technology Data Exchange (ETDEWEB)

    Lutfullah [Department of Chemistry, Aligarh Muslim University, Aligarh 202002, Uttar Pradesh (India)], E-mail: lutfullah786@gmail.com; Alam, Mohd Noor; Rahman, Nafisur; Azmi, Syed Najmul Hejaz [Department of Chemistry, Aligarh Muslim University, Aligarh 202002, Uttar Pradesh (India)

    2008-06-30

    An optimized and validated spectrophotometric method has been developed for the determination of uranyl ion in the presence of other metal ions. The method is based on the chelation of uranyl ion with meloxicam via {beta}-diketone moiety to produce a yellow colored complex, which absorbs maximally at 398 nm. Beer's law is obeyed in the concentration range of 5-60 {mu}g/mL with apparent molar absorptivity and Sandell's sensitivity of 5.02 x 10{sup 4} L/mol/cm and 0.1 {mu}g/cm{sup 2}/0.001 absorbance unit, respectively. The method has been successfully applied for the determination of uranyl ion in synthetic mixture and soil samples. Results of analysis were statistically compared with those obtained by Currah's spectrophotometric method showing acceptable recovery and precision.

  17. Determination of the freezing point in cow milk samples preserved with azidiol

    Directory of Open Access Journals (Sweden)

    Nataša Pintić-Pukec

    2011-12-01

    Full Text Available The study involved determination of the freezing point of cow milk by a reference (thermistor cryoscopy and an instrumental (infrared spectrometry method. The aim of the study was to evaluate the possibility of milk freezing point determination in milk samples preserved with azidiol by using a reference and an instrumental method of analysis. Five hundred cow milk samples were analysed during three research periods. Samples were taken at milk collection points in north-western Croatia. Samples preserved with azidiol (0.3 mL azidiol/40 mL; 0.011 g sodium azide/40 mL and without preservatives (control samples were analysed. The freezing point of milk was determined in duplicate. Average freezing point results of azidiol preserved samples were lower compared to control samples. A statistically significant difference between the means of the results obtained for azidiol preserved and control samples was determined (P<0.05; P<0.01 in all research periods. The results revealed a significant influence of the preservative azidiol on milk freezing point determination regardless of the method of analysis applied, which could lead to wrong interpretation of the results.

  18. SMALL SAMPLE SIZE IN 2X2 CROSS OVER DESIGNS: CONDITIONS OF DETERMINATION

    Directory of Open Access Journals (Sweden)

    B SOLEYMANI

    2001-09-01

    Full Text Available Introduction. Determination of small sample size in some clinical trials is a matter of importance. In cross-over studies which are one types of clinical trials, the matter is more significant. In this article, the conditions in which determination of small sample size in cross-over studies are possible were considered, and the effect of deviation from normality on the matter has been shown. Methods. The present study has been done on such 2x2 cross-over studies that variable of interest is quantitative one and is measurable by ratio or interval scale. The method of consideration is based on use of variable and sample mean"s distributions, central limit theorem, method of sample size determination in two groups, and cumulant or moment generating function. Results. In normal variables or transferable to normal variables, there is no restricting factors other than significant level and power of the test for determination of sample size, but in the case of non-normal variables, it should be determined such large that guarantee the normality of sample mean"s distribution. Discussion. In such cross over studies that because of existence of theoretical base, few samples can be computed, one should not do it without taking applied worth of results into consideration. While determining sample size, in addition to variance, it is necessary to consider distribution of variable, particularly through its skewness and kurtosis coefficients. the more deviation from normality, the more need of samples. Since in medical studies most of the continuous variables are closed to normal distribution, a few number of samples often seems to be adequate for convergence of sample mean to normal distribution.

  19. Determination of uranium and thorium by neutron activation analysis applied to fossil samples dating

    Energy Technology Data Exchange (ETDEWEB)

    Ticianelli, Regina B.; Figueiredo, Ana Maria Graciano; Zahn, Guilherme S. [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Kinoshita, Angela; Baffa, Oswaldo [Universidade de Sao Paulo (FFCRLP/USP), Ribeirao Preto, SP (Brazil). Faculdade de Filosofia, Ciencias e Letras de Ribeirao Preto. Dept. de Fisica

    2011-07-01

    Electron Spin Resonance (ESR) dating is based on the fact that ionizing radiation can create stable free radicals in insulating materials, like tooth enamel and bones. The concentration of these radicals - determined by ESR - is a function of the dose deposed in the sample along the years. The accumulated dose of radiation, called Archaeological Dose, is produced by the exposition to environmental radiation provided by U, Th, K and cosmic rays. If the environmental dose rate in the site where the fossil sample is found is known, it is possible to convert this dose into the age of the sample. The annual dose rate coming from the radioactive elements present in the soil and in the sample itself can be calculated by determining the U, Th and K concentration. Therefore, the determination of the dose rate depends on the concentration of these main radioactive elements. Neutron Activation Analysis has the sensitivity and the accuracy necessary to determine U, Th and K with this objective. Depending on the composition of the sample, the determination of U and Th can be improved irradiating the sample inside a Cd capsule, reducing the thermal neutron incidence on the sample and, therefore, diminishing the activation of possible interfering nuclides. In this study the optimal irradiation and counting conditions were established for U and Th determination in fossil teeth and soil. (author)

  20. The Search Engine for Multi-Proteoform Complexes: An Online Tool for the Identification and Stoichiometry Determination of Protein Complexes.

    Science.gov (United States)

    Skinner, Owen S; Schachner, Luis F; Kelleher, Neil L

    2016-12-08

    Recent advances in top-down mass spectrometry using native electrospray now enable the analysis of intact protein complexes with relatively small sample amounts in an untargeted mode. Here, we describe how to characterize both homo- and heteropolymeric complexes with high molecular specificity using input data produced by tandem mass spectrometry of whole protein assemblies. The tool described is a "search engine for multi-proteoform complexes," (SEMPC) and is available for free online. The output is a list of candidate multi-proteoform complexes and scoring metrics, which are used to define a distinct set of one or more unique protein subunits, their overall stoichiometry in the intact complex, and their pre- and post-translational modifications. Thus, we present an approach for the identification and characterization of intact protein complexes from native mass spectrometry data. © 2016 by John Wiley & Sons, Inc.

  1. Near-infrared diffuse reflectance spectroscopy with sample spots and chemometrics for fast determination of bovine serum albumin in micro-volume samples

    Institute of Scientific and Technical Information of China (English)

    Cai-Jing Cui; Wen-Sheng Cai; Xue-Guang Shao

    2013-01-01

    Near-infrared diffuse reflectance spectroscopy (NIRDRS) has attracted more and more attention in analyzing the components in samples with complex matrices.However,to apply this technique to micro-analysis,there are still some obstacles to overcome such as the low sensitivity and spectral overlapping associated with this approach.A method for fast determination of bovine serum albumin (BSA) in micro-volume samples was studied using NIRDRS with sample spots and chemometric techniques.10 μL of sample spotted on a filter paper substrate was used for the spectral measurements.Quantitative analysis was obtained by partial least squares (PLS) regression with signal processing and variable selection.The results show that the correlation coefficient (R) between the predicted and the reference concentration is 0.9897 and the recoveries are in the range of 87.4%-114.4% for the validation samples in the concentration range of 0.61-8.10 mg/mL.These results suggest that the method has the potential to quickly measure proteins in micro-volume solutions.

  2. Efficient sample clean-up and online preconcentration for sensitive determination of melamine in milk samples by capillary electrophoresis with contactless conductivity detection.

    Science.gov (United States)

    Ji, Yan-ling; Chen, Xiao-wei; Zhang, Zhu-bao; Li, Jing; Xie, Tian-yao

    2014-10-01

    Based on an efficient sample clean-up and field-amplified sample injection online preconcentration technique in capillary electrophoresis with contactless conductivity detection, a new analytical method for the sensitive determination of melamine in milk samples was established. In order to remove the complex matrix interference, which resulted in a serious problem during field-amplified sample injection, liquid-liquid extraction was utilized. As a result, liquid-liquid extraction provides excellent sample clean-up efficiency when ethyl acetate was used as organic extraction by adjusting the pH of the sample solution to 9.5. Both inorganic salts and biological macromolecules are effectively removed by liquid-liquid extraction. The sample clean-up procedure, capillary electrophoresis separation parameters and field-amplified sample injection conditions are discussed in detail. The capillary electrophoresis separation was achieved within 5 min under the following conditions: an uncoated fused-silica capillary, 12 mM HAc + 10 mM NaAc (pH = 4.6) as running buffer, separation voltage of +13 kV, electrokinetic injection of +12 kV × 10 s. Preliminary validation of the method performance with spiked melamine provided recoveries >90%, with limits of detection and quantification of 0.015 and 0.050 mg/kg, respectively. The relative standard deviations of intra- and inter-day were below 6%. This newly developed method is sensitive and cost effective, therefore, suitable for screening of melamine contamination in milk products.

  3. Cloud point extraction-atomic absorption spectrometry for pre-concentration and determination of cadmium in cigarette samples.

    Science.gov (United States)

    Tavallali, Hossein; Boustani, Fazlollah; Yazdandoust, Mozhdeh; Aalaei, Mehdi; Tabandeh, Mahboobeh

    2013-05-01

    A new complexing agent, 2-((2-((1H-benzo[d]imidazole-2yl)methoxy)phenoxy)methyl)-1H-benzo[d]imidazole (BIMPI), was used in cloud point extraction and applied for selective pre-concentration of trace amounts of cadmium in cigarette samples. Cadmium was complexed with BIMPI in a buffer solution (pH = 10) using Triton X-114 as surfactant and quantitatively extracted into a small volume of the surfactant-rich phase after centrifugation. Under optimized conditions (pH = 10.0, 0.8 × 10(-4) mol L(-1) BIMPI and 0.08 % (w/v) Triton X-114), calibration graph was linear in the range of 34.0-1,670.0 μg L(-1). The proposed method was applied to the determination of Cd in various cigarette (tobacco) samples which gave satisfactory results.

  4. An error criterion for determining sampling rates in closed-loop control systems

    Science.gov (United States)

    Brecher, S. M.

    1972-01-01

    The determination of an error criterion which will give a sampling rate for adequate performance of linear, time-invariant closed-loop, discrete-data control systems was studied. The proper modelling of the closed-loop control system for characterization of the error behavior, and the determination of an absolute error definition for performance of the two commonly used holding devices are discussed. The definition of an adequate relative error criterion as a function of the sampling rate and the parameters characterizing the system is established along with the determination of sampling rates. The validity of the expressions for the sampling interval was confirmed by computer simulations. Their application solves the problem of making a first choice in the selection of sampling rates.

  5. Development of a Cloud-Point Extraction Method for Cobalt Determination in Natural Water Samples

    Directory of Open Access Journals (Sweden)

    Mohammad Reza Jamali

    2013-01-01

    Full Text Available A new, simple, and versatile cloud-point extraction (CPE methodology has been developed for the separation and preconcentration of cobalt. The cobalt ions in the initial aqueous solution were complexed with 4-Benzylpiperidinedithiocarbamate, and Triton X-114 was added as surfactant. Dilution of the surfactant-rich phase with acidified ethanol was performed after phase separation, and the cobalt content was measured by flame atomic absorption spectrometry. The main factors affecting CPE procedure, such as pH, concentration of ligand, amount of Triton X-114, equilibrium temperature, and incubation time were investigated and optimized. Under the optimal conditions, the limit of detection (LOD for cobalt was 0.5 μg L-1, with sensitivity enhancement factor (EF of 67. Calibration curve was linear in the range of 2–150 μg L-1, and relative standard deviation was 3.2% (c=100 μg L-1; n=10. The proposed method was applied to the determination of trace cobalt in real water samples with satisfactory analytical results.

  6. Determinants of favourable opinions about euthanasia in a sample of French physicians

    National Research Council Canada - National Science Library

    Dany, Lionel; Baumstarck, Karine; Dudoit, Eric; Duffaud, Florence; Auquier, Pascal; Salas, Sébastien

    2015-01-01

    .... The objective of this study in a sample of French physicians was to establish the potential determinants of a favourable opinion about euthanasia in general and when faced with a specific situation...

  7. Determination of the effective atomic number of thick samples of unknown composition using scattering studies

    Science.gov (United States)

    Sankarshan, B. M.; Athrey, C. D.; Umesh, T. K.

    2017-06-01

    The effective atomic number ( Z_eff is a quantity which gives the fraction of the total number of electrons in a composite material participating in the photon-atom interaction. The effective atomic number has been determined for the materials of known composition by using different methods. However, no method has been reported so far to determine Z_eff for thick samples of unknown composition. In view of this, we have evolved a simple method to determine the effective atomic number, which uses the scattering intensity ratios measured at two scattering angles, in which a sample of known Z_eff or Z is taken as a reference sample. The values of Z_eff obtained by this method agree with those obtained from the Auto-Zeff software within the stated errors. This method could be helpful in determining the effective atomic number of samples of unknown composition.

  8. Microwave-assisted extraction and ultrasonic slurry sampling procedures for cobalt determination in geological samples by electrothermal atomic absorption spectroscopy.

    Science.gov (United States)

    Felipe-Sotelo, M; Carlosena, A; Fernández, E; López-Mahía, P; Muniategui, S; Prada, D

    2004-06-17

    Slurry sampling is compared to microwave-assisted acid digestion for cobalt determination in soil/sediment samples by electrothermal atomic absorption spectrometry (ETAAS). Furnace temperature programs and appropriate amounts of three chemical modifiers were optimised in order to get the highest signals and good separations between the atomic and background signals. Using nitric acid (0.5% (v/v)) as liquid medium, no chemical modifier was needed. The detection limit, based on integrated absorbance, was 0.04mugg(-1) for digests and slurries. Within-batch precision and analytical recoveries were satisfactory for both procedures. Accuracy was tested by analysing a reference soil and a sediment from IRMM. The methods were further compared employing a set of roadside soils and estuarine sediments. As no significant differences (95% confidence) were found, practical analytical properties were suggested in order to select one of them.

  9. Total nitrogen determination of various sample types: a comparison of the Hach, Kjeltec, and Kjeldahl methods.

    Science.gov (United States)

    Watkins, K L; Veum, T L; Krause, G F

    1987-01-01

    Conventional Kjeldahl analysis with modifications, Kjeltec analysis with block digestion and semiautomated distillation, and the Hach method for determining nitrogen (N) were compared using a wide range of samples. Twenty different sample types were ground and mixed. Each sample type was divided into 5 subsamples which were analyzed for N by each of the 3 methods. In each sample type, differences (P less than 0.05) were detected among the 3 N determination methods in 5 of the 20 N sources analyzed. The mean N content over all 20 samples was higher with Kjeldahl analysis (P less than 0.05) than with Kjeltec, while Hach analysis produced intermediate results. Results also indicated that the Hach procedure had the greatest ability to detect differences in N content among sample types, being more sensitive than either other method (P less than 0.05).

  10. Determination of ultra trace arsenic species in water samples by hydride generation atomic absorption spectrometry after cloud point extraction

    Energy Technology Data Exchange (ETDEWEB)

    Ulusoy, Halil Ibrahim, E-mail: hiulusoy@yahoo.com [University of Cumhuriyet, Faculty of Science, Department of Chemistry, TR-58140, Sivas (Turkey); Akcay, Mehmet; Ulusoy, Songuel; Guerkan, Ramazan [University of Cumhuriyet, Faculty of Science, Department of Chemistry, TR-58140, Sivas (Turkey)

    2011-10-10

    Graphical abstract: The possible complex formation mechanism for ultra-trace As determination. Highlights: {yields} CPE/HGAAS system for arsenic determination and speciation in real samples has been applied first time until now. {yields} The proposed method has the lowest detection limit when compared with those of similar CPE studies present in literature. {yields} The linear range of the method is highly wide and suitable for its application to real samples. - Abstract: Cloud point extraction (CPE) methodology has successfully been employed for the preconcentration of ultra-trace arsenic species in aqueous samples prior to hydride generation atomic absorption spectrometry (HGAAS). As(III) has formed an ion-pairing complex with Pyronine B in presence of sodium dodecyl sulfate (SDS) at pH 10.0 and extracted into the non-ionic surfactant, polyethylene glycol tert-octylphenyl ether (Triton X-114). After phase separation, the surfactant-rich phase was diluted with 2 mL of 1 M HCl and 0.5 mL of 3.0% (w/v) Antifoam A. Under the optimized conditions, a preconcentration factor of 60 and a detection limit of 0.008 {mu}g L{sup -1} with a correlation coefficient of 0.9918 was obtained with a calibration curve in the range of 0.03-4.00 {mu}g L{sup -1}. The proposed preconcentration procedure was successfully applied to the determination of As(III) ions in certified standard water samples (TMDA-53.3 and NIST 1643e, a low level fortified standard for trace elements) and some real samples including natural drinking water and tap water samples.

  11. Determination of natural uranium, thorium and radium isotopes in water and soil samples by alpha spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Hao, Le Cong; Tao, Chau Van; Thong, Luong Van; Linh, Duong Mong [University of Science Ho Chi Minh City (Viet Nam). Faculty of Physics and Engineering Physics; Dong, Nguyen Van [University of Science Ho Chi Minh City (Viet Nam). Faculty of Chemistry

    2011-08-15

    In this study, a simple procedure for the determination of natural uranium, thorium and radium isotopes in water and soil samples by alpha spectroscopy is described. This procedure allows a sequential extraction polonium, uranium, thorium and radium radionuclides from the same sample in two to three days. It was tested and validated with the analysis of certified reference materials from the IAEA. (orig.)

  12. On the determination of the position of extrema of sampled correlators

    NARCIS (Netherlands)

    Moddemeijer, R.

    1991-01-01

    The problem of determination of the position of the extremum of a continuous correlator function from its samples, if the spectrum of the correlator is not bandlimited, is discussed. Searching for the position of the extremum by fitting a parabola through three samples around that extremum leads to

  13. Determination of platinum, palladium, and lead in biological samples by atomic absorption spectrophotometry.

    Science.gov (United States)

    Tillery, J B; Johnson, D E

    1975-01-01

    A flameless atomic absorption method for the coextraction of platinum and palladium from biological and environmental samples by high molecular weight amine (HMWA) is given. Also, methods for lead determination in biological samples by use of extraction flameless analysis and direct aspiration-flame analysis are reported. A study of lead contamination of Vacutainer tubes is given. PMID:1227857

  14. 40 CFR 761.358 - Determining the PCB concentration of samples of waste.

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Determining the PCB concentration of samples of waste. 761.358 Section 761.358 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY... concentration of samples of waste. Use either Method 3500B/3540C or Method 3500B/3550B from EPA's SW-846, Test...

  15. Radiochemical separation of actinides for their determination in environmental samples and waste products

    Energy Technology Data Exchange (ETDEWEB)

    Gleisberg, B. [Nuclear Engineering and Analytics Rossendorf, Inc. (VKTA), Dresden (Germany)

    1997-03-01

    The determination of low level activities of actinides in environmental samples and waste products makes high demands on radiochemical separation methods. Artificial and natural actinides were analyzed in samples form the surrounding areas of NPP and of uranium mines, incorporation samples, solutions containing radioactive fuel, solutions and solids resutling from the process, and in wastes. The activities are measured by {alpha}-spectrometry and {gamma}-spectrometry. (DG)

  16. Determination of specific activity of 230Th in uranium ore samples

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    A new method suitable for determining specific activity of 230Th in uranium ore samples is built. The method is characterized by adding the 230Th/ 232Th standard dilution agent with lower activity ratio (Its 230Th/ 232Th activity ratio and 230Th have been known) to the samples and using isotopic dilution analysis. The method can be applied to analyses of 230Th specific activity in various 230Th/ 232Th activity ratio samples. The precision can also be improved.

  17. Fluorimetric Determination of Carbamate Pesticides in Host-Guest Complexes

    Directory of Open Access Journals (Sweden)

    Alicia Viviana Veglia

    2000-03-01

    Full Text Available From the effect of β-cyclodextrin and hydroxypropyl-β-cyclodextrin on the UVvisible and fluorescence spectra of carbaryl and carbofuran, the values of association constants were determined. The ratio of the fluorescence quantum yields for the bound and free substrates indicated an enhanced fluorimetric method of detection.

  18. Noun combination in interlanguage typology effects in complex determiner phrases

    CERN Document Server

    Bongartz, Christiane

    2002-01-01

    This study examines effects of L1 typology on the interlanguage of L2 learners of English. Czech learners use phrasal constructs (the song about love) significantly more often than Chinese learners, who prefer noun+noun compounds (the love song). Determiner properties and the process of noun incorporation systematically relate both options.

  19. Floatation-spectrophotometric Determination of Thorium, Using Complex Formation with Eriochrome Cyanine R.

    Science.gov (United States)

    Shiri, Sabah; Delpisheh, Ali; Haeri, Ali; Poornajaf, Abdolhossein; Khezeli, Tahereh; Badkiu, Nadie

    2011-01-23

    A novel and sensitive floatation-spectrophotometric method is presented for determination of trace amounts of thorium in water samples. The method is based on the ion-associated formation between thorium, Eriochrome cyanine R and Brij-35 at pH = 4 media. The complex was floated in the interface of the aqueous phase and n-hexane by vigorous shaking. After removing the aqueous phase the floated particles were dissolved in methanol and the absorbance was measured at 607 nm. The influence of different important parameters such as Eriochrome cyanine R and surfactants concentration, pH, volume of n-hexane, standing time and interfering ions were evaluated. Under optimized conditions the calibration graph was linear in the range of 6-230 ng mL(-1) of thorium with a correlation coefficient of 0.9985. The limit of detections (LOD), based on signal to noise ratio (S/N) of 3 was 1.7 ng mL(-1). The relative standard deviations for determination of 150 and 30 ng ml(-1) of thorium were 3.26 and 4.41%, respectively (n = 10). The method showed a good linearity, recoveries, as well as some advantages such as sensitivity, simplicity, affordability and a high feasibility. The method was successfully applied to determine thorium in different water and urine samples.

  20. Lifetime heterogeneity of DNA-bound dppz complexes originates from distinct intercalation geometries determined by complex-complex interactions.

    Science.gov (United States)

    Andersson, Johanna; Fornander, Louise H; Abrahamsson, Maria; Tuite, Eimer; Nordell, Pär; Lincoln, Per

    2013-01-18

    Despite the extensive interest in structurally explaining the photophysics of DNA-bound [Ru(phen)(2)dppz](2+) and [Ru(bpy)(2)dppz](2+), the origin of the two distinct emission lifetimes of the pure enantiomers when intercalated into DNA has remained elusive. In this report, we have combined a photophysical characterization with a detailed isothermal titration calorimetry study to investigate the binding of the pure Δ and Λ enantiomers of both complexes with [poly(dAdT)](2). We find that a binding model with two different binding geometries, proposed to be symmetric and canted intercalation from the minor groove, as recently reported in high-resolution X-ray structures, is required to appropriately explain the data. By assigning the long emission lifetime to the canted binding geometry, we can simultaneously fit both calorimetric data and the binding-density-dependent changes in the relative abundance of the two emission lifetimes using the same binding model. We find that all complex-complex interactions are slightly unfavorable for Δ-[Ru(bpy)(2)dppz](2+), whereas interactions involving a complex canted away from a neighbor are favorable for the other three complexes. We also conclude that Δ-[Ru(bpy)(2)dppz](2+) preferably binds isolated, Δ-[Ru(phen)(2)dppz](2+) preferably binds as duplets of canted complexes, and that all complexes are reluctant to form longer consecutive sequences than triplets. We propose that this is due to an interplay of repulsive complex-complex and attractive complex-DNA interactions modulated by allosteric DNA conformation changes that are largely affected by the nature of the ancillary ligands.

  1. Solid phase extraction and spectrophotometric determination of mercury by adsorption of its diphenylthiocarbazone complex on an alumina column.

    Science.gov (United States)

    Rajesh, N; Gurulakshmanan, G

    2008-02-01

    A simple method has been developed for the preconcentration of mercury based on the adsorption of its diphenylthiocarbazone complex on a neutral alumina column. The influence of acidity, eluting agents, stability of the column, sample volume and interfering ions has been investigated in detail. The adsorbed complex could be eluted using environmentally benign polyethylene glycol (PEG 400) and the concentration of mercury was determined by visible spectrophotometry at a wavelength maximum of 520nm. A detection limit of 4microgL(-1) could be achieved and the developed procedure was successfully applied for the determination of mercury in spiked water samples and city waste incineration ash (CRM176). The preconcentration factor attainable for quantitative recovery (>95%) of mercury(II) was 100 for a 1000mL sample volume.

  2. Determination of the neutron activation profile of core drill samples by gamma-ray spectrometry.

    Science.gov (United States)

    Gurau, D; Boden, S; Sima, O; Stanga, D

    2017-08-04

    This paper provides guidance for determining the neutron activation profile of core drill samples taken from the biological shield of nuclear reactors using gamma spectrometry measurements. Thus, it provides guidance for selecting a model of the right form to fit data and using least squares methods for model fitting. The activity profiles of two core samples taken from the biological shield of a nuclear reactor were determined. The effective activation depth and the total activity of core samples along with their uncertainties were computed by Monte Carlo simulation. Copyright © 2017 Elsevier Ltd. All rights reserved.

  3. A study on determination of potentially hazardous plutonium isotopes in environmental samples.

    Science.gov (United States)

    Strumińska-Parulska, Dagmara I

    2013-01-01

    Due to the lack of stable plutonium isotopes, and the high mobility as well as long half-life, plutonium is considered one of the most important radioelement in safety assessment of environmental radioactivity and nuclear waste management. A number of analytical methods have been developed over the past decades for determination of plutonium in environmental samples. The article discusses different analytical techniques and presents the results of plutonium isotopes determination by alpha spectrometry and accelerator mass spectrometry in environmental samples. The concentrations of plutonium isotopes in analyzed samples indicates its measurement is of great importance for environmental and safety assessment, especially in contaminated areas.

  4. Evaluating Complex Mixtures in the Zebrafish Embryo by Reconstituting Field Water Samples: A Metal Pollution Case Study

    Directory of Open Access Journals (Sweden)

    Ellen D. G. Michiels

    2017-03-01

    Full Text Available Accurately assessing the toxicity of complex, environmentally relevant mixtures remains an important challenge in ecotoxicology. The goal was to identify biological effects after exposure to environmental water samples and to determine whether the observed effects could be explained by the waterborne metal mixture found in the samples. Zebrafish embryos were exposed to water samples of five different sites originating from two Flemish (Mol and Olen, Belgium metal contaminated streams: “Scheppelijke Nete” (SN and “Kneutersloop” (K, and a ditch (D, which is the contamination source of SN. Trace metal concentrations, and Na, K, Mg and Ca concentrations were measured using ICP-MS and were used to reconstitute site-specific water samples. We assessed whether the effects that were observed after exposure to environmental samples could be explained by metal mixture toxicity under standardized laboratory conditions. Exposure to “D” or “reconstituted D” water caused 100% mortality. SN and reconstituted SN water caused similar effects on hatching, swim bladder inflation, growth and swimming activity. A canonical discriminant analysis confirmed a high similarity between both exposure scenarios, indicating that the observed toxicity was indeed primarily caused by metals. The applied workflow could be a valuable approach to evaluate mixture toxicity that limits time and costs while maintaining biological relevance.

  5. Evaluating Complex Mixtures in the Zebrafish Embryo by Reconstituting Field Water Samples: A Metal Pollution Case Study

    Science.gov (United States)

    Michiels, Ellen D. G.; Vergauwen, Lucia; Hagenaars, An; Fransen, Erik; Dongen, Stefan Van; Van Cruchten, Steven J.; Bervoets, Lieven; Knapen, Dries

    2017-01-01

    Accurately assessing the toxicity of complex, environmentally relevant mixtures remains an important challenge in ecotoxicology. The goal was to identify biological effects after exposure to environmental water samples and to determine whether the observed effects could be explained by the waterborne metal mixture found in the samples. Zebrafish embryos were exposed to water samples of five different sites originating from two Flemish (Mol and Olen, Belgium) metal contaminated streams: “Scheppelijke Nete” (SN) and “Kneutersloop” (K), and a ditch (D), which is the contamination source of SN. Trace metal concentrations, and Na, K, Mg and Ca concentrations were measured using ICP-MS and were used to reconstitute site-specific water samples. We assessed whether the effects that were observed after exposure to environmental samples could be explained by metal mixture toxicity under standardized laboratory conditions. Exposure to “D” or “reconstituted D” water caused 100% mortality. SN and reconstituted SN water caused similar effects on hatching, swim bladder inflation, growth and swimming activity. A canonical discriminant analysis confirmed a high similarity between both exposure scenarios, indicating that the observed toxicity was indeed primarily caused by metals. The applied workflow could be a valuable approach to evaluate mixture toxicity that limits time and costs while maintaining biological relevance. PMID:28257097

  6. Rapid determination of lead and cadmium in sewage sludge samples using electrothermal atomic absorption spectrometry with slurry sample introduction

    Energy Technology Data Exchange (ETDEWEB)

    Lopez-Garcia, I.; Vinas, P.; Arroyo-Cortez, J.; Hernandez-Cordoba, M. [Dept. of Analytical Chem., Univ. of Murcia (Spain)

    2000-08-01

    Lead and cadmium concentrations in sewage sludge samples are determined by suspending the ground samples in a solution containing 10% (v/v) concentrated hydrofluoric acid, 1% (v/v) concentrated nitric acid, 0.5% (m/v) dihydrogen ammonium phosphate and 0.1% (m/v) sodium hexametaphosphate. Aliquots of 20 {mu}L of these suspensions (4 mg/mL) are diluted to 1000 {mu}L with the same solution and then injected into the electrothermal atomizer. The drying stage is performed by programming a 400 C temperature, a ramp time of 20 s and a hold time of 15 s on the power supply of the atomizer. No ashing step is used. Platform atomization is carried out at 1600 and 1800 C for Pb and Cd, respectively. Calibration is performed using aqueous standards in the 5-75 and 0.2- 5 {mu}g/L Pb and Cd ranges, respectively. Results obtained for three certified reference materials and four samples demonstrate the reliability of the procedures described. (orig.)

  7. Quantitative determination of minerals in Nevada Test Site samples by x-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Pawloski, G.A.

    1983-07-01

    The external standard intensity ratio technique has been developed into a routine procedure for quantitatively determining mineralogic compositions of Nevada Test Site (NTS) samples by x-ray diffraction. This technique used ratios of x-ray intensity peaks from the same run which eliminates many possible errors. Constants have been determined for each of thirteen minerals commonly found in NTS samples - quartz, montmorillonite, illite, clinoptilolite, cristobalite, feldspars, calcite, dolomite, hornblende, kaolinite, muscovite, biotite, and amorphous glass. Ratios of the highest intensity peak of each mineral to be quantified in the sample and the highest intensity peak of quartz are used to calculate sample composition. The technique has been tested on samples with three to eleven components representative of geologic environments at NTS, and is accurate to 7.0 wt % of the total sample. The minimum amount of each of these minerals detectable by x-ray diffraction has also been determined. QUANTS is a computer code that calculates mineral contents and produces a report sheet. Constants for minerals in NTS samples other than those listed above can easily be determined, and added to QUANTS at any time.

  8. 210Pb and 210Po determination in environmental samples using liquid scintillation counting and alpha spectrometry

    Science.gov (United States)

    Pérez Sánchez, D.; Martin Sánchez, A.; Jurado Vargas, M.

    2003-01-01

    A simple radiochemical procedure has been developed to determine 210Pb and 210Po in environmental samples from the same matrix. Sediment samples are decomposed by leaching with mineral acids or by microwave digestion, while water samples are pre-concentrated. One part of the resulting solution, spiked with 209Po, is used for 210Po determination by spontaneous deposition onto nickel disks (α-spectrometry). The other part is assayed for 210Pb, separating the Pb either by anion-exchange (sediment samples), or by solvent extraction (water samples). The 210Pb source is finally prepared by precipitation as oxalate and the chemical recovery determined by gravimetry. The 210Pb activity concentration is determined by liquid scintillation. A standard sediment sample supplied by IAEA and spiked water samples were analysed to check the procedure. The 210Pb and 210Po measurements agreed well with the certifications, deviations being less than 10%. The mean recoveries for Pb and Po were (70±12)% and (77±8%) for sediments, and (70±10)% and (81±7)% for waters, respectively.

  9. Sample size determination for logistic regression on a logit-normal distribution.

    Science.gov (United States)

    Kim, Seongho; Heath, Elisabeth; Heilbrun, Lance

    2017-06-01

    Although the sample size for simple logistic regression can be readily determined using currently available methods, the sample size calculation for multiple logistic regression requires some additional information, such as the coefficient of determination ([Formula: see text]) of a covariate of interest with other covariates, which is often unavailable in practice. The response variable of logistic regression follows a logit-normal distribution which can be generated from a logistic transformation of a normal distribution. Using this property of logistic regression, we propose new methods of determining the sample size for simple and multiple logistic regressions using a normal transformation of outcome measures. Simulation studies and a motivating example show several advantages of the proposed methods over the existing methods: (i) no need for [Formula: see text] for multiple logistic regression, (ii) available interim or group-sequential designs, and (iii) much smaller required sample size.

  10. Calibration of Ge gamma-ray spectrometers for complex sample geometries and matrices

    Energy Technology Data Exchange (ETDEWEB)

    Semkow, T.M., E-mail: thomas.semkow@health.ny.gov [Wadsworth Center, New York State Department of Health, Empire State Plaza, Albany, NY 12201 (United States); Department of Environmental Health Sciences, School of Public Health, University at Albany, State University of New York, Rensselaer, NY 12144 (United States); Bradt, C.J.; Beach, S.E.; Haines, D.K.; Khan, A.J.; Bari, A.; Torres, M.A.; Marrantino, J.C.; Syed, U.-F. [Wadsworth Center, New York State Department of Health, Empire State Plaza, Albany, NY 12201 (United States); Kitto, M.E. [Wadsworth Center, New York State Department of Health, Empire State Plaza, Albany, NY 12201 (United States); Department of Environmental Health Sciences, School of Public Health, University at Albany, State University of New York, Rensselaer, NY 12144 (United States); Hoffman, T.J. [Wadsworth Center, New York State Department of Health, Empire State Plaza, Albany, NY 12201 (United States); Curtis, P. [Kiltel Systems, Inc., Clyde Hill, WA 98004 (United States)

    2015-11-01

    A comprehensive study of the efficiency calibration and calibration verification of Ge gamma-ray spectrometers was performed using semi-empirical, computational Monte-Carlo (MC), and transfer methods. The aim of this study was to evaluate the accuracy of the quantification of gamma-emitting radionuclides in complex matrices normally encountered in environmental and food samples. A wide range of gamma energies from 59.5 to 1836.0 keV and geometries from a 10-mL jar to 1.4-L Marinelli beaker were studied on four Ge spectrometers with the relative efficiencies between 102% and 140%. Density and coincidence summing corrections were applied. Innovative techniques were developed for the preparation of artificial complex matrices from materials such as acidified water, polystyrene, ethanol, sugar, and sand, resulting in the densities ranging from 0.3655 to 2.164 g cm{sup −3}. They were spiked with gamma activity traceable to international standards and used for calibration verifications. A quantitative method of tuning MC calculations to experiment was developed based on a multidimensional chi-square paraboloid. - Highlights: • Preparation and spiking of traceable complex matrices in extended geometries. • Calibration of Ge gamma spectrometers for complex matrices. • Verification of gamma calibrations. • Comparison of semi-empirical, computational Monte Carlo, and transfer methods of Ge calibration. • Tuning of Monte Carlo calculations using a multidimensional paraboloid.

  11. Determination of trace inorganic mercury species in water samples by cloud point extraction and UV-vis spectrophotometry.

    Science.gov (United States)

    Ulusoy, Halil Ibrahim

    2014-01-01

    A new micelle-mediated extraction method was developed for preconcentration of ultratrace Hg(II) ions prior to spectrophotometric determination. 2-(2'-Thiazolylazo)-p-cresol (TAC) and Ponpe 7.5 were used as the chelating agent and nonionic surfactant, respectively. Hg(II) ions form a hydrophobic complex with TAC in a micelle medium. The main factors affecting cloud point extraction efficiency, such as pH of the medium, concentrations of TAC and Ponpe 7.5, and equilibration temperature and time, were investigated in detail. An overall preconcentration factor of 33.3 was obtained upon preconcentration of a 50 mL sample. The LOD obtained under the optimal conditions was 0.86 microg/L, and the RSD for five replicate measurements of 100 microg/L Hg(II) was 3.12%. The method was successfully applied to the determination of Hg in environmental water samples.

  12. Predicting the coexistence of an endometrial adenocarcinoma in the presence of atypical complex hyperplasia: immunohistochemical analysis of endometrial samples

    NARCIS (Netherlands)

    Robbe, E.J.; Kuijk, S.M. van; Boed, E.M. de; Smits, L.J.; Wurff, A.A. van der; Kruitwagen, R.F.P.M.; Pijnenborg, J.M.A.

    2012-01-01

    OBJECTIVE: This study aimed to determine whether immunohistochemical markers in complex atypical endometrial hyperplasia could predict the presence of a concurrent endometrial carcinoma. METHODS: Endometrial biopsies of 39 patients with complex atypical hyperplasia were selected retrospectively betw

  13. Preconcentration and determination of heavy metals in water, sediment and biological samples

    Directory of Open Access Journals (Sweden)

    Shirkhanloo Hamid

    2011-01-01

    Full Text Available In this study, a simple, sensitive and accurate column preconcentration method was developed for the determination of Cd, Cu and Pb ions in river water, urine and sediment samples by flame atomic absorption spectrometry. The procedure is based on the retention of the analytes on a mixed cellulose ester membrane (MCEM column from buffered sample solutions and then their elution from the column with nitric acid. Several parameters, such as pH of the sample solution, volume of the sample and eluent and flow rates of the sample were evaluated. The effects of diverse ions on the preconcentration were also investigated. The recoveries were >95 %. The developed method was applied to the determination of trace metal ions in river water, urine and sediment samples, with satisfactory results. The 3δ detection limits for Cu, Pb and Cd were found to be 2, 3 and 0.2 μg dm−3, respectively. The presented procedure was successfully applied for determination of the copper, lead and cadmium contents in real samples, i.e., river water and biological samples.

  14. Complex and novel determinants of empathy change in medical students

    Directory of Open Access Journals (Sweden)

    Gerald Sng Gui Ren

    2016-03-01

    Full Text Available Purpose: Physician empathy is a core attribute in medical professionals, giving better patient outcomes. Medical school is an opportune time for building empathetic foundations. This study explores empathy change and focuses on contributory factors. Methods: We conducted a cross-sectional study involving 881 students (63% from Years 1 to 5 in a Singaporean medical school using the Jefferson Scale of Physician Empathy-Student version (JSPE-S and a questionnaire investigating the relationship between reported and novel personal-social empathy determinants. Results: Empathy declined significantly between preclinical and clinical years. Female and medical specialty interest respondents had higher scores than their counterparts. Despite strong internal consistency, factor analysis suggested that the JSPE model is not a perfect fit. Year 1 students had highest Perspective Taking scores and Year 2 students had highest Compassionate Care scores. High workload and inappropriate learning environments were the most relevant stressors. Time spent with family, arts, and community service correlated with higher empathy scores, whilst time spent with significant others and individual leisure correlated with lower scores. Thematic analysis revealed that the most common self-reported determinants were exposure to activity (community service or socialisation, personal and family-related event as well as environment (high work-load. Conclusion: While the empathy construct in multicultural Singapore is congruent with a Western model, important differences remain. A more subtle understanding of the heterogeneity of the medical student experience is important. A greater breadth of determinants of empathy, such as engagement in arts-related activities should be considered.

  15. sup 2 sup 1 sup 0 Pb determination by gamma spectrometry in voluminal samples (cylindrical geometry)

    CERN Document Server

    San Miguel, E G; Bolivar, J P; Garcia-Tenorio, R; Martin, J E

    2002-01-01

    In this paper a simple method for the direct analysis of sup 2 sup 1 sup 0 Pb (T sub 1 sub / sub 2 =22.3 years) by gamma-ray spectrometry in sediment samples with coaxial Ge detectors is outlined. This method, developed for a cylindrical sample geometry, accounts for variable sample heights and provides a fundamental advantage: individual self-absorption corrections can easily be determined knowing the apparent densities of the samples. The results obtained with the proposed method are in good agreement with those given by other techniques.

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

    DEFF Research Database (Denmark)

    Qiao, Jixin

    and optimization for rapid determination of plutonium in environmental samples using SIextraction chromatography prior to inductively coupled plasma mass spectrometry (Paper III); (3) Development of an SI-chromatographic method for simultaneous determination of plutonium and neptunium in environmental samples...... (Paper IV); (4) Investigation of the suitability and applicability of 242Pu as a tracer for rapid neptunium determination using anion exchange chromatography in an SI-network coupled with inductively coupled plasma mass spectrometry (Paper V); (5) Exploration of macro-porous anion exchange chromatography......This thesis presents improved analytical methods for rapid and automated determination of plutonium and neptunium in environmental samples using sequential injection (SI) based chromatography and inductively coupled plasma mass spectrometry (ICP-MS). The progress of methodology development...

  17. Complexity quantification of cardiac variability time series using improved sample entropy (I-SampEn).

    Science.gov (United States)

    Marwaha, Puneeta; Sunkaria, Ramesh Kumar

    2016-09-01

    The sample entropy (SampEn) has been widely used to quantify the complexity of RR-interval time series. It is a fact that higher complexity, and hence, entropy is associated with the RR-interval time series of healthy subjects. But, SampEn suffers from the disadvantage that it assigns higher entropy to the randomized surrogate time series as well as to certain pathological time series, which is a misleading observation. This wrong estimation of the complexity of a time series may be due to the fact that the existing SampEn technique updates the threshold value as a function of long-term standard deviation (SD) of a time series. However, time series of certain pathologies exhibits substantial variability in beat-to-beat fluctuations. So the SD of the first order difference (short term SD) of the time series should be considered while updating threshold value, to account for period-to-period variations inherited in a time series. In the present work, improved sample entropy (I-SampEn), a new methodology has been proposed in which threshold value is updated by considering the period-to-period variations of a time series. The I-SampEn technique results in assigning higher entropy value to age-matched healthy subjects than patients suffering atrial fibrillation (AF) and diabetes mellitus (DM). Our results are in agreement with the theory of reduction in complexity of RR-interval time series in patients suffering from chronic cardiovascular and non-cardiovascular diseases.

  18. A sequential injection system for the spectrophotometric determination of calcium, magnesium and alkalinity in water samples.

    Science.gov (United States)

    Mesquita, Raquel B R; Rangel, António O S S

    2004-08-01

    A sequential injection methodology for the spectrophotometric determination of calcium, magnesium and alkalinity in water samples is proposed. A single manifold is used for the determination of the three analytes, and the same protocol sequence allows the sequential determination of calcium and magnesium (the sum corresponds to the water hardness). The determination of both metals is based on their reaction with cresolphtalein complexone; mutual interference is minimized by using 8-hydroxyquinoline for the determination of calcium and ethylene glycol-bis(beta-aminoethyl ether)-N,N,N',N'-tetraacetic acid (EGTA) for the determination of magnesium. Alkalinity determination is based on a reaction with acetic acid, and corresponding color change of Bromcresol Green. Working ranges of 0.5 - 5 mg dm(-3) for Ca, 0.5 - 10 mg dm(-3) for Mg, and 10 - 100 mg HCO3- dm(-3), for alkalinity have been achieved. The results for water samples were comparable to those of the reference methods and to a certified reference water sample. RSDs lower than 5% were obtained, a low reagent consumption and a reduced volume of effluent have been accomplished. The determination rate for calcium and magnesium is 80 h(-1), corresponding to 40 h(-1) per element, while 65 determinations of alkalinity per hour could be carried out.

  19. Cloud-point extraction, preconcentration and spectrophotometric determination of trace quantities of copper in food, water and biological samples.

    Science.gov (United States)

    Gouda, Ayman A; Amin, Alaa S

    2014-01-01

    A new, simple and sensitive cloud point extraction procedure was presented for the preconcentration and determination of copper(II) ion in food, water and biological samples. The analyte was complexed with a new synthesized reagent, 2-amino-4-(m-tolylazo)pyridine-3-ol (ATAP) as a new complexing agent and Triton X-114 as the surfactant. After centrifugation, dilution of the surfactant-rich phase with 0.4 mL of ethanol acidified with 1.0M HNO3 was performed after phase separation, and the copper contents were measured by spectrophotometry at λmax 608 nm. The influence of analytical parameters including concentration of complexing agent, Triton X-114, pH, equilibration temperature and time, centrifuge rate and time were optimized. The analytical characteristics of the method (e.g. linear range, molar absorptivity, Sandell sensitivity, optimum Ringbom concentration ranges limits of detection and quantification, preconcentration factor, and improvement factors) were obtained. Linearity was obeyed in the range of 4.0-115 ng mL(-1) of Cu(II) ion. The detection and quantification limits of the method were 1.20 and 3.94 ng mL(-1) of Cu(II) ion, respectively. The interference effect of some anions and cations was also tested. The method was applied for determination of copper in food, water and biological samples.

  20. Me-BTABr reagent in cloud point extraction for spectrometric determination of copper in water samples

    OpenAIRE

    Lemos,Valfredo A; Santos, Juracir S.; Baliza,Patrícia X.

    2006-01-01

    A new preconcentration method using cloud point approach is proposed for copper determination. The reagent 2-[2´-(6-methyl-benzothiazolylazo)]-4-bromophenol (Me-BTABr) was used as a complexing agent and Triton X-114 was added as a surfactant. After phase separation, dilution of the surfactant-rich phase with acidified methanol was performed, and the copper content was measured by flame atomic absorption spectrometry. The proposed procedure allowed the determination of copper with detect...

  1. Universality in the bulk of the spectrum for complex sample covariance matrices

    CERN Document Server

    Péché, S

    2009-01-01

    We consider complex sample covariance matrices $M_N=\\frac{1}{N}YY^*$ where $Y$ is a $N \\times p$ random matrix with i.i.d. entries $Y_{ij}, 1\\leq i\\leq N, 1\\leq j \\leq p$ with distribution $F$. Under some regularity and decay assumption on $F$, we prove universality of some local eigenvalue statistics in the bulk of the spectrum in the limit where $N\\to \\infty$ and $\\lim_{N \\to \\infty}p/N =\\gamma$ for any real number $\\gamma \\in (0, \\infty)$.

  2. Correlation of mRNA and protein in complex biological samples.

    Science.gov (United States)

    Maier, Tobias; Güell, Marc; Serrano, Luis

    2009-12-17

    The correlation between mRNA and protein abundances in the cell has been reported to be notoriously poor. Recent technological advances in the quantitative analysis of mRNA and protein species in complex samples allow the detailed analysis of this pathway at the center of biological systems. We give an overview of available methods for the identification and quantification of free and ribosome-bound mRNA, protein abundances and individual protein turnover rates. We review available literature on the correlation of mRNA and protein abundances and discuss biological and technical parameters influencing the correlation of these central biological molecules.

  3. Unraveling the Beautiful Complexity of Simple Lattice Model Polymers and Proteins Using Wang-Landau Sampling

    Science.gov (United States)

    Wüst, T.; Li, Y. W.; Landau, D. P.

    2011-08-01

    We describe a class of "bare bones" models of homopolymers which undergo coil-globule collapse and proteins which fold into their native states in free space or into denatured states when captured by an attractive substrate as the temperature is lowered. We then show how, with the use of a properly chosen trial move set, Wang-Landau Monte Carlo sampling can be used to study the rough free energy landscape and ground (native) states of these intriguingly simple systems and thus elucidate their thermodynamic complexity.

  4. Antioxidant study of quercetin and their metal complex and determination of stability constant by spectrophotometry method.

    Science.gov (United States)

    Ravichandran, R; Rajendran, M; Devapiriam, D

    2014-03-01

    Quercetin found chelate cadmium ions, scavenge free radicals produced by cadmium. Hence new complex, quercetin with cadmium was synthesised, and the synthesised complex structures were determined by UV-vis spectrophotometry, infrared spectroscopy, thermogravimetry and differential thermal analysis techniques (UV-vis, IR, TGA and DTA). The equilibrium stability constants of quercetin-cadmium complex were determined by Job's method. The determined stability constant value of quercetin-cadminum complex at pH 4.4 is 2.27×10(6) and at pH 7.4 is 7.80×10(6). It was found that the quercetin and cadmium ion form 1:1 complex in both pH 4.4 and pH 7.4. The structure of the compounds was elucidated on the basis of obtained results. Furthermore, the antioxidant activity of the free quercetin and quercetin-cadmium complexes were determined by DPPH and ABTS assays.

  5. Simultaneous Determination of Vitamin B Complex Using Wavelet Neural Network

    Institute of Scientific and Technical Information of China (English)

    YIN,Chun-Sheng(印春生); YIN,Chun-Sheng; GUO,Wei-Min(郭卫民); GUO,Wei-Min; LIU,Shu-Shen(刘树深); LIU,Shu-Shen; SHEN,Yang(沈阳); SHEN,Yang; Zhong-Xiao(潘忠孝); PAN,Zhong-Xiao; WANG,Lian-Sheng(王连生); WANG,Lian-Sheng

    2001-01-01

    A simultaneous determination of four conponents of B-groupvitamin, using a novel wavelet-based neural network (WNN), combined with correlation coefficient and standard deviation approach for wavelength selection, was reported in this work. Eleven representative wavelength points were selected from each o inginal UV spectrun, based on correlation coefficients and standard deviations of the observed data. A family of wavelet basic functions built from Morlet wavelet was adopted to improve the transfer quality of output data and solve the problems of training difficultly involved in neural networks, Tne predicted results, with fitting correlation coefficients (R = 0.9998-0.9999) and rooted mean squares errors (RMS =0.0578-0.1478), are satisfactory.

  6. Jackknife Estimation of Sampling Variance of Ratio Estimators in Complex Samples: Bias and the Coefficient of Variation. Research Report. ETS RR-06-19

    Science.gov (United States)

    Oranje, Andreas

    2006-01-01

    A multitude of methods has been proposed to estimate the sampling variance of ratio estimates in complex samples (Wolter, 1985). Hansen and Tepping (1985) studied some of those variance estimators and found that a high coefficient of variation (CV) of the denominator of a ratio estimate is indicative of a biased estimate of the standard error of a…

  7. Amelogenin Gene - The Pioneer in Gender Determination from Forensic Dental Samples

    Science.gov (United States)

    Bhosale, Satish; Singh, Rajeshwar; Gubrellay, Priyanka; Patil, Jitendra; Sehdev, Bhumika; Bhagat, Sachin; Bansal, Tajinder

    2017-01-01

    Introduction In the event of any mass fatality incident, DNA analysis plays a vital role in disaster victim identification. Teeth are one of the most resistant structures in the human body that resist decomposition hence making them prime choice for extracting DNA for identification of individuals. Polymerase Chain Reaction (PCR) analysis that target regions of Amelogenin gene have become the method of choice for sex determination of biological samples. Aim Determining the sex of a given DNA sample from either dental pulp or dentin of tooth and help in identification of missing persons and disaster victims. Materials and Methods In our study 50 teeth samples were studied and they were subjected to various environmental conditions along with freshly extracted teeth taken as control for duration of one month and three months. Pulpal tissue was retrieved from the teeth specimens by access opening of root canals and for incinerated samples, the specimens were crushed. From the DNA that was extracted from the dental pulp sample Amelogenin gene locus was used for sex determination by amplifying a segment of X-Y homologous gene locus through PCR analysis. Results ANOVA test and t-test proved to be statistically significant and 100% retrieval rate was observed in samples. Conclusion Pulpal tissue along with degenerating odontoblastic processes yield sufficient amount of DNA for gender determination when subjected to various forensic conditions with maximum accuracy. PMID:28384982

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

    Science.gov (United States)

    Stastna, Miroslava; Slais, Karel

    2010-01-01

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

  9. Fourier Method for an Over-Determined Elliptic System with Several Complex Variables

    Institute of Scientific and Technical Information of China (English)

    Dao Qing DAI

    2006-01-01

    Two boundary value problems are investigated for an over-determined elliptic system with several complex variables in polydisc. Necessary and sufficient conditions for the existence of finitely many linearly independent solutions and finitely many solvability conditions are derived. Moreover,the boundary value problem for any number of complex variables is treated in a unified way and the essential difference between the case of one complex variable and that of several complex variables is revealed.

  10. Combining Passive Sampling with Toxicological Characterization of Complex Mixtures of Pollutants from the Aquatic Environment.

    Science.gov (United States)

    Jahnke, Annika; Witt, Gesine; Schäfer, Sabine; Haase, Nora; Escher, Beate I

    2016-08-04

    The combination of polymer-based passive sampling to collect complex environmental mixtures of pollutants, the transfer of these mixtures into bioassays, and their related toxicological characterization is still in its infancy. However, this approach has considerable potential to improve environmental hazard and risk assessment for two reasons. First, the passive sampler collects a broad range of chemicals representing the fraction of compounds available for diffusion and (bio)uptake, excluding a large part of the matrix; thus, extensive sample cleanup which could discriminate certain compounds can be avoided. Second, the toxicological characterization of samples using bioassays is complementary to chemical (target) analysis within environmental monitoring because it captures all chemicals exerting the same mode of toxic action and acting jointly in mixtures, thus providing a comprehensive picture of their overall combined effects. The scientific literature describes a range of examples from the water phase where passive sampling is usually carried out in the kinetic uptake regime for most chemicals although some may already have reached equilibrium. The composition of the chemical mixture changes from the water phase to the passive sampling material because of kinetic effects and polymer/water partition coefficients which depend on the chemicals' hydrophobicity. In contrast, only a few applications in sediment and biota have been described, but amongst these some pioneering studies have demonstrated the feasibility and potential of this combined approach. This chapter gives an overview of what has been carried out in this research area, focusing on opportunities and challenges, and points out desirable future developments with a focus on the importance of choosing a suitable combination of sampling and dosing to transfer (or re-establish) the environmental mixture into the bioassay.

  11. Determining cardiac vagal threshold from short term heart rate complexity

    Directory of Open Access Journals (Sweden)

    Hamdan Rami Abou

    2016-09-01

    Full Text Available Evaluating individual aerobic exercise capacity is fundamental in sports and exercise medicine but associated with organizational and instrumental effort. Here, we extract an index related to common performance markers, the aerobic and anaerobic thresholds enabling the estimation of exercise capacity from a conventional sports watch supporting beatwise heart rate tracking. Therefore, cardiac vagal threshold (CVT was determined in 19 male subjects performing an incremental maximum exercise test. CVT varied around the anaerobic threshold AnT with mean deviation of 7.9 ± 17.7 W. A high correspondence of the two thresholds was indicated by Bland-Altman plots with limits of agreement −27.5 W and 43.4 W. Additionally, CVT was strongly correlated AnT (rp = 0.86, p < 0.001 and reproduced this marker well (rc = 0.81. We conclude, that cardiac vagal threshold derived from compression entropy time course can be useful to assess physical fitness in an uncomplicated way.

  12. Colorimetric determination of sildenafil citrate (Viagra) through ion-associate complex formation.

    Science.gov (United States)

    Amin, Alaa S; Moustafa, Moustafa E; El-Dosoky, Reham

    2009-01-01

    A simple, quick, accurate, and sensitive colorimetric method is described for the determination of sildenafil citrate (SLD). The method is based on the reaction of SLD with Congo Red, Sudan II, and Gentian Violet in buffered aqueous solutions at pH 2.5, 6.5, and 11.0, respectively, to give highly colored soluble ion-associate complex species; the colored products are quantitated colorimetrically at 523, 554, and 569 nm, respectively. The various experimental conditions were optimized. The stoichiometric ratio was found to be 1:1 for all ion associates; the calculated logarithmic stability constants were 8.51, 7.79, and 5.58, respectively. Beer's law was obeyed over the concentration range of 0.2-7.0 microg/mL, whereas the Ringbom optimum concentration range was 0.4-6.5 microg/mL. Values for molar absorptivity, Sandell sensitivity, and detection and quantification limits were also calculated. The proposed method was successfully applied to the determination of SLD in Viagra tablets and in serum samples by using the technique of standard additions with mean accuracy values of 100.06 +/- 1.14, 99.87 +/- 0.70, and 99.86 +/- 0.97% for Viagra tablets and 99.88 +/- 0.60, 99.90 +/- 0.90, and 100.24 +/- 0.80% for serum samples, respectively.

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

    Energy Technology Data Exchange (ETDEWEB)

    Qiao, J.

    2011-03-15

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

  14. The accuracy of parameters determined with the core-sampling method application to Voronoi tessellations

    CERN Document Server

    Doroshkevich, A G; Madsen, S; Doroshkevich, Andrei G.; Gottloeber, Stefan; Madsen, Soeren

    1996-01-01

    The large-scale matter distribution represents a complex network of structure elements such as voids, clusters, filaments, and sheets. This network is spanned by a point distribution. The global properties of the point process can be measured by different statistical methods, which, however, do not describe directly the structure elements. The morphology of structure elements is an important property of the point distribution. Here we apply the core-sampling method to various Voronoi tessellations. Using the core-sampling method we identify one- and two-dimensional structure elements (filaments and sheets) in these Voronoi tessellations and reconstruct their mean separation along random straight lines. We compare the results of the core-sampling method with the a priori known structure elements of the Voronoi tessellations under consideration and find good agreement between the expected and found structure parameters, even in the presence of substantial noise. We conclude that the core-sampling method is a po...

  15. A new ion-selective electrode based on aluminium tungstate for Fe(III) determination in rock sample, pharmaceutical sample and water sample

    Indian Academy of Sciences (India)

    Mu Naushad

    2008-12-01

    An inorganic cation exchanger, aluminum tungstate (AT), has been synthesized by adding 0.1 M sodium tungstate gradually into 0.1 M aluminium nitrate at pH 1.2 with continuous stirring. The ion exchange capacity for Na+ ion and distribution coefficients of various metal ions was determined on the column of aluminium tungstate. The distribution studies of various metal ions showed the selectivity of Fe(III) ions by this cation exchange material. So, a Fe(III) ion-selective membrane electrode was prepared by using this cation exchange material as an electroactive material. The effect of plasticizers viz. dibutyl phthalate (DBP), dioctylphthalate (DOP), di-(butyl) butyl phosphate (DBBP) and tris-(2-ethylhexylphosphate) (TEHP), has also been studied on the performance of membrane sensor. It was observed that the membrane containing the composition AT: PVC: DBP in the ratio 2 : 20 : 15 displayed a useful analytical response with excellent reproducibility, low detection limit, wide working pH range (1–3.5), quick response time (15 s) and applicability over a wide concentration range of Fe(III) ions from 1 × 10-7 M to 1 × 10-1 M with a slope of 20 ± 1 mV per decade. The selectivity coefficients were determined by the mixed solution method and revealed that the electrode was selective for Fe(III) ions in the presence of interfering ions. The electrode was used for atleast 5 months without any considerable divergence in response characteristics. The constructed sensor was used as indicator electrode in the potentiometric titration of Fe(III) ions against EDTA and Fe(III) determination in rock sample, pharmaceutical sample and water sample. The results are found to be in good agreement with those obtained by using conventional methods.

  16. Sampling

    CERN Document Server

    Thompson, Steven K

    2012-01-01

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

  17. Sensitive spectrophotometric determination of Co(II) using dispersive liquid-liquid micro-extraction method in soil samples.

    Science.gov (United States)

    Hasanpour, Foroozan; Hadadzadeh, Hassan; Taei, Masoumeh; Nekouei, Mohsen; Mozafari, Elmira

    2016-05-01

    Analytical performance of conventional spectrophotometer was developed by coupling of effective dispersive liquid-liquid micro-extraction method with spectrophotometric determination for ultra-trace determination of cobalt. The method was based on the formation of Co(II)-alpha-benzoin oxime complex and its extraction using a dispersive liquid-liquid micro-extraction technique. During the present work, several important variables such as pH, ligand concentration, amount and type of dispersive, and extracting solvent were optimized. It was found that the crucial factor for the Co(II)-alpha benzoin oxime complex formation is the pH of the alkaline alcoholic medium. Under the optimized condition, the calibration graph was linear in the ranges of 1.0-110 μg L(-1) with the detection limit (S/N = 3) of 0.5 μg L(-1). The preconcentration operation of 25 mL of sample gave enhancement factor of 75. The proposed method was applied for determination of Co(II) in soil samples.

  18. Optimal adaptive group sequential design with flexible timing of sample size determination.

    Science.gov (United States)

    Cui, Lu; Zhang, Lanju; Yang, Bo

    2017-04-26

    Flexible sample size designs, including group sequential and sample size re-estimation designs, have been used as alternatives to fixed sample size designs to achieve more robust statistical power and better trial efficiency. In this work, a new representation of sample size re-estimation design suggested by Cui et al. [5,6] is introduced as an adaptive group sequential design with flexible timing of sample size determination. This generalized adaptive group sequential design allows one time sample size determination either before the start of or in the mid-course of a clinical study. The new approach leads to possible design optimization on an expanded space of design parameters. Its equivalence to sample size re-estimation design proposed by Cui et al. provides further insight on re-estimation design and helps to address common confusions and misunderstanding. Issues in designing flexible sample size trial, including design objective, performance evaluation and implementation are touched upon with an example to illustrate. Copyright © 2017. Published by Elsevier Inc.

  19. [The quality control of preanalytical variations for the determination of lead in samples of human origin].

    Science.gov (United States)

    Zhong, Kun; Wang, Wei; He, Falin; Wang, Zhiguo

    2015-02-01

    The aims of this article was to provide the quality control requirements of preanalytical variation for the determination of lead in samples of human origin, reduce the influence of preanalytical variation on the test results. According to the Clinical and Laboratory Standards Institute documents, control of preanalytical variation in trace element determinations, analytical procedures for the determination of lead in blood and urine and other references and guidelines, the methods of quality control of lead determination had been made, including: the factors needed to be considered before collection, preservation, transportation and other preanalytical factors, the abilities and considerations of laboratory staff, etc.

  20. Direct infusion-SIM as fast and robust method for absolute protein quantification in complex samples

    Directory of Open Access Journals (Sweden)

    Christina Looße

    2015-06-01

    Full Text Available Relative and absolute quantification of proteins in biological and clinical samples are common approaches in proteomics. Until now, targeted protein quantification is mainly performed using a combination of HPLC-based peptide separation and selected reaction monitoring on triple quadrupole mass spectrometers. Here, we show for the first time the potential of absolute quantification using a direct infusion strategy combined with single ion monitoring (SIM on a Q Exactive mass spectrometer. By using complex membrane fractions of Escherichia coli, we absolutely quantified the recombinant expressed heterologous human cytochrome P450 monooxygenase 3A4 (CYP3A4 comparing direct infusion-SIM with conventional HPLC-SIM. Direct-infusion SIM revealed only 14.7% (±4.1 (s.e.m. deviation on average, compared to HPLC-SIM and a decreased processing and analysis time of 4.5 min (that could be further decreased to 30 s for a single sample in contrast to 65 min by the LC–MS method. Summarized, our simplified workflow using direct infusion-SIM provides a fast and robust method for quantification of proteins in complex protein mixtures.

  1. A combined complex electrical impedance and acoustic emission study in limestone samples under uniaxial loading

    Science.gov (United States)

    Saltas, V.; Fitilis, I.; Vallianatos, F.

    2014-12-01

    In the present work, complex electrical impedance measurements in the frequency range of 10 mHz to 1 MHz were carried out in conjunction with acoustic emission monitoring in limestone samples subjected to linear and stepped-like uniaxial loading, up to ultimate failure. Cole-Cole plots of the complex impedance during the stepped loading of limestone have been used to discriminate the contributions of grains interior, grain boundaries and electrode polarization effects to the overall electrical behavior. The latter is well-described with an equivalent-circuit model which comprises components of constant phase elements and resistances in parallel connection. Electrical conductivity increases upon uniaxial loading giving rise to negative values of effective activation volume. This is a strong experimental evidence for the generation of transient electric signals recorded prior to seismic events and may be attributed to charge transfer (proton conduction) due to cracks generation and propagation as a result of the applied stress. The time-series of ac-conductivity at two distinct frequencies (10 kHz, 200 kHz) during linear loading of limestone samples exhibits a strong correlation with the acoustic emission activity obeying the same general self-similar law for critical phenomena that has been reported for the energy release before materials fracture.

  2. Uranium isotopes determination in urine samples using alpha spectrometry and ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Rosa, Mychelle M.L.; Maihara, Vera A. [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Tine, Fernanda D.; Santos, Sandra M.C.; Bonifacio, Rodrigo L.; Taddei, Maria HelenaT. [Comissao Nacional de Energia Nuclear (LAPOC/CNEN-MG), Pocos de Caldas, MG (Brazil). Laboratorio de Pocos de Caldas

    2015-07-01

    The action of determining the concentration of uranium isotopes in biological samples, 'in vitro' bioassay, is an indirect method for evaluating the incorporation and quantification of these radionuclides internally deposited. When incorporated, these radionuclides tend to be disposed through excretion, with urine being the main source of data because it can be easily collected and analyzed. The most widely used methods for determination of uranium isotopes ({sup 234}U, {sup 235}U and {sup 238}U) are Alpha Spectrometry and ICP-MS. This work presents a comparative study for the determination of uranium isotopes using these two methodologies in real samples from occupationally exposed workers. In order to validate the methodology, a sample of the intercomparison exercise organized by PROCORAD (Association pour la Promotion du Controle de Qualite des Analyses de Biologie Medicale em Radiotoxicologie) was used, and the results were statistically compared applying the Student's t-test. (author)

  3. Determination of ammonium in a buddingtonite sample by ion-chromatography

    Science.gov (United States)

    Klock, P.R.; Lamothe, P.J.

    1986-01-01

    An ion-chromatographic method for the direct determination of ammonium, potassium, and sodium in geologic materials is described. Samples are decomposed with a mixture of hydrofluoric and hydrochloric acids in a sealed polycarbonate bottle heated in a microwave oven. The ion-chromatograph separates the cations and determines them by conductivity measurement. The ammonium concentrations thus determined have been verified by use of an ammonia-specific electrode. A total of 32 analyses of ammonium salts by both techniques showed an average error of -4%, with a relative standard deviation (RSD) of 6%. The ammonium concentrations found in a buddingtonite sample had an RSD of 2.2% and their mean agreed with that obtained by the Kjeldahl method. By use of the prescribed dilution of the sample, detection limits of 0.1% can be achieved for all three cations. ?? 1986.

  4. [Sample pretreatment for the measurement of phthalate esters in complex matrices].

    Science.gov (United States)

    Liang, Jing; Zhuang, Wan'e; Lin, Fang; Yao, Wensong

    2014-11-01

    Sample pretreatment methods for the measurement of phthalate esters (PAEs) by gas chromatography-mass spectrometry (GC-MS) in various complex matrices, including sediment, soil, suspended particle matter, urban surface dust, Sinonovacula Constricta, cosmet- ic, leather, plastic and coastal/estuarine seawater, were proposed. The pretreatment which was appropriate for GC-MS detection was focused on the investigation and optimization of oper- ating parameters for the extraction and purification, such as the extraction solvent, the eluant and the adsorbent of solid phase extraction. The results of the study of pretreatment for various complex matrices showed that methylene chloride was the best solvent for the ultrasonic extraction when solid-liquid extraction was used; silica gel was the economical and practical adsorbent for solid-phase extraction for purification; C18 was the most commonly adsorbent for preconcentration of PAE in coastal/estuarine seawater sample; the mixed solution of n-hexane and ethyl acetate with a certain proportion was the suitable SPE eluent. Under the optimized conditions, the spiked recoveries were above 58% and the relative standard deviations (RSDs) were less than 10.5% (n = 6). The detection limits (DL, 3σ) were in the range of 0.3 μg/kg (dibutyl phthalate)--5.2 μg/kg ( diisononyl phthalate) for sediment, and 6 ng/L (dipropyl phthalate)--67 ng/L (diisodecyl phthalate) for costal/estuarine seawater. The pretreatment meth- od for various complex matrices is prominent for the measurement of the 16 PAEs with GC-MS.

  5. Distribution, virulence attributes and antifungal susceptibility patterns of Candida parapsilosis complex strains isolated from clinical samples.

    Science.gov (United States)

    Tosun, Ilknur; Akyuz, Zeynep; Guler, Nejla Cebeci; Gulmez, Dolunay; Bayramoglu, Gulcin; Kaklikkaya, Nese; Arikan-Akdagli, Sevtap; Aydin, Faruk

    2013-07-01

    It was recently proposed that Candida parapsilosis represents a complex composed of three closely related species, i.e., C. parapsilosis sensu stricto, C. orthopsilosis, and C. metapsilosis. The aim of this study was to describe the distribution of C. parapsilosis complex isolates among clinical samples. We also evaluated antifungal susceptibility profiles, in vitro presence of lipase and secreted aspartyl proteinase, as well as their ability to grow in total parenteral nutrition (TPN) solution, and biofilm production. A total of 413 non-C. albicans Candida isolates were obtained from various clinical samples between 2010 and 2011 in a Turkish Tertiary Care Hospital. Of them, 42 were identified as members of the C. parapsilosis complex. Among these, 38 (90.5%) were C. parapsilosis sensu stricto, 3 (7.1%) C. metapsilosis, and 1 (2.4%) C. orthopsilosis. All isolates recovered from blood were found to be C. parapsilosis sensu stricto and C. metapsilosis. In phenotypic tests, all 42 isolates grew in TPN solution and, although 26.2% of C. parapsilosis sensu stricto-isolates were capable of forming biofilms in vitro, neither C. orthopsilosis nor C. metapsilosis isolates were able to do so. Acid proteinase activity was detected in 31% of isolates and lipase activity in 33%. All isolates were sensitive to voriconazole, caspofungin, and anidulafungin, with only a single C. parapsilosis sensu stricto isolate showing dose-dependent susceptible to fluconazole. While the number of C. metapsilosis and C. orthopsilosis isolates remained low, there were no significant differences in antifungal MIC as compared to C. parapsilosis sensu stricto.

  6. Semiquantitative determination of polychlorinated biphenyls in tissue samples by thin layer chromatography

    Science.gov (United States)

    Mulhern, B.M.; Cromartie, E.; Reichel, W.L.; Belisle, A.A.

    1971-01-01

    A method is described for the analysis of polychlorinated biphenyl (PCB) compounds in tissue samples. Cleanup by hexane-aceto-nitrile partitioning and Florisil column chromatography are performed on samples before oxidative treatment to convert DDE to DCBP. PCB components are then determined semi-quantitatively by TLC. No prior separation of PCB from chlorinated pesticides is required. The lower limit of sensitivity is 0.2 ?g.

  7. Determination of metal content in atmospheric dust samples using different vessel and filter materials

    Energy Technology Data Exchange (ETDEWEB)

    Meyer, G.; Wentrup, G.J.

    1989-02-01

    In this paper materials like glassfibre and quartzglass filters were analysed with respect to their application for the analysis of metal contents in atmospheric dust samples. Furthermore different vessel materials, resistant to fluoric acid, have been tested too. In summary the most important fact for the determination of metal content in atmospheric dust samples - prior condition the chosen analysis method is suitable and sensitive enough - is the quality of the used materials. These materials are to be chosen thoroughly to the conditions required.

  8. Determination of phosphorus in small amounts of protein samples by ICP-MS.

    Science.gov (United States)

    Becker, J Sabine; Boulyga, Sergei F; Pickhardt, Carola; Becker, J; Buddrus, Stefan; Przybylski, Michael

    2003-02-01

    Inductively coupled plasma mass spectrometry (ICP-MS) is used for phosphorus determination in protein samples. A small amount of solid protein sample (down to 1 micro g) or digest (1-10 micro L) protein solution was denatured in nitric acid and hydrogen peroxide by closed-microvessel microwave digestion. Phosphorus determination was performed with an optimized analytical method using a double-focusing sector field inductively coupled plasma mass spectrometer (ICP-SFMS) and quadrupole-based ICP-MS (ICP-QMS). For quality control of phosphorus determination a certified reference material (CRM), single cell proteins (BCR 273) with a high phosphorus content of 26.8+/-0.4 mg g(-1), was analyzed. For studies on phosphorus determination in proteins while reducing the sample amount as low as possible the homogeneity of CRM BCR 273 was investigated. Relative standard deviation and measurement accuracy in ICP-QMS was within 2%, 3.5%, 11% and 12% when using CRM BCR 273 sample weights of 40 mg, 5 mg, 1 mg and 0.3 mg, respectively. The lowest possible sample weight for an accurate phosphorus analysis in protein samples by ICP-MS is discussed. The analytical method developed was applied for the analysis of homogeneous protein samples in very low amounts [1-100 micro g of solid protein sample, e.g. beta-casein or down to 1 micro L of protein or digest in solution (e.g., tau protein)]. A further reduction of the diluted protein solution volume was achieved by the application of flow injection in ICP-SFMS, which is discussed with reference to real protein digests after protein separation using 2D gel electrophoresis.The detection limits for phosphorus in biological samples were determined by ICP-SFMS down to the ng g(-1) level. The present work discusses the figure of merit for the determination of phosphorus in a small amount of protein sample with ICP-SFMS in comparison to ICP-QMS.

  9. Contactless conductometric determination of methanol and ethanol in samples containing water after their electrophoretic desalination.

    Science.gov (United States)

    Tůma, Petr; Opekar, František

    2015-08-01

    Determination of the contents of methanol and ethanol in aqueous solutions was performed by measuring the permittivity of solutions using a contactless conductivity detector (C(4) D) normally used for detection in capillary electrophoresis. The detection cell is a section of a fused silica capillary with an internal diameter of 50 μm with a pair of conductivity electrodes on the external walls. The C(4) D response to samples of methanol/water and ethanol/water mixtures is linear in the concentration interval of approx. 40-100% v/v alcohol content. In the analysis of technical samples of methanol and ethanol, the determination is disturbed by the presence of even trace amounts of salts. This interference can be effectively eliminated by integrated electrophoretic desalination of the sample by the application of a direct current electric voltage with a magnitude of 10 kV to the capillary with the injected sample zone. Under these conditions, the ions migrate out of the sample zone and the detector response is controlled purely by the permittivity of the solvent/water zone. Desalinating is effective for NaCl contents in the range from 0 to 5 mmol/L NaCl. The effectiveness of the desalinating process has been verified on MeOH/water samples and in determination of the ethanol content in distilled beverages normally available in the retail network.

  10. Selective cloud point extraction and graphite furnace atomic absorption spectrometric determination of molybdenum (VI) ion in seawater samples

    Energy Technology Data Exchange (ETDEWEB)

    Filik, Hayati, E-mail: filik@istanbul.edu.tr [Istanbul University, Faculty of Engineering, Department of Chemistry, Avcilar, 34320 Istanbul (Turkey); Cengel, Tayfun; Apak, Resat [Istanbul University, Faculty of Engineering, Department of Chemistry, Avcilar, 34320 Istanbul (Turkey)

    2009-09-30

    A cloud point extraction process using the nonionic surfactant Triton X-114 to extract molybdenum from aqueous solutions was investigated. The method is based on the complexation reaction of Mo(VI) with 1,2,5,8-tetrahydroxyanthracene-9,10-dione (quinalizarine: QA) and micelle-mediated extraction of the complex. The enriched analyte in the surfactant-rich phase was determined by graphite furnace atomic absorption spectrometry (GFAAS). The optimal extraction and reaction conditions (e.g. pH, reagent and surfactant concentrations, temperature, incubation and centrifugation times) were evaluated and optimized. Under the optimized experimental conditions, the limit of detection (LOD) for Mo(VI) was 7.0 ng L{sup -1} with an preconcentration factor of {approx}25 when 10 mL of sample solution was preconcentrated to 0.4 mL. The proposed method (with extraction) showed linear calibration within the range 0.03-0.6 {mu}g L{sup -1}. The relative standard deviation (RSD) was found to be 3.7% (C{sub Mo(VI)} = 0.05 {mu}g L{sup -1}, n = 5) for pure standard solutions, whereas RSD for the recoveries from real samples ranged between 2 and 8% (mean RSD = 3.9%). The method was applied to the determination of Mo(VI) in seawater and tap water samples with a recovery for the spiked samples in the range of 98-103%. The interference effect of some cations and anions was also studied. In the presence of foreign ions, no significant interference was observed. In order to verify the accuracy of the method, a certified reference water sample was analysed and the results obtained were in good agreement with the certified values.

  11. Determination of cadmium and lead in human biological samples by spectrometric techniques: a review.

    Science.gov (United States)

    Lemos, Valfredo Azevedo; de Carvalho, Anaildes Lago

    2010-12-01

    The analysis of human biological samples, such as blood, urine, nails, and hair, is generally used for the verification of human exposure to toxic metals. In this review, various spectrometric methods for the determination of cadmium and lead in biological samples are discussed and compared. Several spectrometric techniques are presented and discussed with respect to various characteristics such as sensitivity, selectivity, and cost. Special attention is drawn to the procedures for digestion prior to the determination of cadmium and lead in hair, nails, blood, and urine.

  12. Spectrophotometric determination of Sudan Blue II in environmental samples after dispersive liquid-liquid microextraction

    Directory of Open Access Journals (Sweden)

    Yunus Emre Unsal

    2014-01-01

    Full Text Available A dispersive liquid-liquid microextraction procedure coupled to spectrophotometry is described for the determination of the trace levels of Sudan Blue II. Analytical parameters, such as pH, volume of extraction solvent (carbon tetrachloride, volume of dispersant (ethanol, volume of sample, and extraction time, were optimized. Matrix effects were also investigated. Preconcentration factor was found to be 200. Detection limit and relative standard deviation (RSD were 0.55 µg L-1 and 3.9%, respectively. The procedure was successfully used for the determination of trace levels of Sudan Blue II in food, ink, antifreeze, and industrial waste-water samples.

  13. Optimizing the triple-axis spectrometer PANDA at the MLZ for small samples and complex sample environment conditions

    Science.gov (United States)

    Utschick, C.; Skoulatos, M.; Schneidewind, A.; Böni, P.

    2016-11-01

    The cold-neutron triple-axis spectrometer PANDA at the neutron source FRM II has been serving an international user community studying condensed matter physics problems. We report on a new setup, improving the signal-to-noise ratio for small samples and pressure cell setups. Analytical and numerical Monte Carlo methods are used for the optimization of elliptic and parabolic focusing guides. They are placed between the monochromator and sample positions, and the flux at the sample is compared to the one achieved by standard monochromator focusing techniques. A 25 times smaller spot size is achieved, associated with a factor of 2 increased intensity, within the same divergence limits, ± 2 ° . This optional neutron focusing guide shall establish a top-class spectrometer for studying novel exotic properties of matter in combination with more stringent sample environment conditions such as extreme pressures associated with small sample sizes.

  14. The determination of the content of gold and silver in geological samples

    Directory of Open Access Journals (Sweden)

    B. NESIC

    2001-01-01

    Full Text Available A method has been elaborated for the determination of the content of gold and silver in geological samples by atomic absorption spectrophotometry (AAS in combination with the fire assay method. The weight of sample used for analysis was 10 g. Sulphur present as sulphide, which is an undesirable element in smelting, was removed by the addition of iron to the charge. The sample was smelted with fluxes and lead oxide to replace the silver and gold by lead and to transfer non-precious elements to slag. Lead was separated from precious metals by cupellation. The separated silver and gold alloy was dissolved with aqua regia with addition of hydrochloric acid in excess. Silver and gold were determined from the same solution. For determination of the silver content, the AAS method with an air-acetylene flame was used. Gold was determined in a graphite furnace with the addition of a matrix modifier in an argon current, at an atomization temperature of t = 2200°C. The lower determination limit for silver was 0.05 g/t and for gold 0.005 g/t. The results of the analysis for silver and gold obtained with the proposed method showed good agreement with the results of the analysis of the same samples with the fire assay method.

  15. A NONPARAMETRIC PROCEDURE OF THE SAMPLE SIZE DETERMINATION FOR SURVIVAL RATE TEST

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    Objective This paper proposes a nonparametric procedure of the sample size determination for survival rate test. Methods Using the classical asymptotic normal procedure yields the required homogenetic effective sample size and using the inverse operation with the prespecified value of the survival function of censoring times yields the required sample size. Results It is matched with the rate test for censored data, does not involve survival distributions, and reduces to its classical counterpart when there is no censoring. The observed power of the test coincides with the prescribed power under usual clinical conditions. Conclusion It can be used for planning survival studies of chronic diseases.

  16. Determination of heavy metals in domestic, commercial and industrial soot samples

    Energy Technology Data Exchange (ETDEWEB)

    Iqbal, Yousaf; Sohail, Syed Muhammad; Ahmad, Imtiaz [Peshawar Univ., Khyber Pakhtoonkhwa (Pakistan). Inst. of Chemical Sciences; Saeed, Khalid [Peshawar Univ., Khyber Pakhtoonkhwa (Pakistan). Inst. of Chemical Sciences; Malakand Univ., Khyber Pakhtoonkhwa (Pakistan). Dept. of Chemistry

    2012-07-15

    The heavy metals such as manganese (Mn), cadmium (Cd), zinc (Zn), chromium (Cr), lead (Pb), nickel (Ni), copper (Cu) and iron (Fe) were determined in domestic, commercial and industrial soot samples via atomic absorption spectrophotometer. The vehicle soot samples showed highest concentration of investigated heavy metals as compared to other soot samples. It was also found that the concentration of Fe was high in the soot samples (range 5.75-1105 mg/Kg) followed by Cu (70-990 mg/Kg) while the concentration of Ni was lower (range 0.5-3 mg/Kg). It was also found that the concentration of Mn and Fe was decreased as decreased the size of the soot samples while the concentration of other investigated heavy metals increased as decreased the size fraction. (orig.)

  17. DEVELOPMENT OF UV-VISIBLE SPECTROPHOTOMETRIC METHOD FOR DETERMINATION OF DASATINIB IN PHARMACEUTICAL FORMULATION AND BIOLOGICAL SAMPLES

    Directory of Open Access Journals (Sweden)

    B. Ramachandra

    2015-02-01

    Full Text Available A simple, economical, accurate, precise and reproducible UV-Visible spectrophotometric method for the routine estimation of dasatinib has been developed. The method is based on the formation of a bluish green colored complex by dasatinib in presence of MBTH reagent. The developed colored complex showed λmax at 630 nm. Beer’s law in the concentration range of 10 to 60 μg/ ml. Results of analysis were authenticated statistically as well as by recovery studies, which gave mean recovery between 99 to 100%. The method was successful in determining dasatinib in pharmaceutical formulation and biological samples, with an average recovery between 99 to 100 % respectively. The proposed method could find application to product development scientists in ongoing research; as well provide an additional tool for routine analysis of dasatinib.

  18. Determination of Boron Trifluoride in Boron Trifluoride Complex by Fluoride Ion Selective Electrode

    Institute of Scientific and Technical Information of China (English)

    郎五可; 张卫江; 唐银; 徐姣; 张雷

    2016-01-01

    A method was proposed to determine boron trifluoride in boron trifluoride complex using fluoride ion selective electrode(ISE). Hydroxide was chosen to mask aluminum for the determination of 0.01—0.1 mol/L of fluoride. The simulation indicated that the permissible aluminum masked at a certain pH value was limited and hardly related to F-concentration and boric acid. It is better to control pH value below 11.5 and the aluminum con-centration within 0.025 mol/L to minimize the interference of hydroxide to the fluoride ISE. The decomposition conditions of boron trifluoride by aluminum chloride were investigated. It is found that the F-detection ratio will approach 1.0 if the Al/F molar ratio is 0.3—0.7 and aluminum concentration is no more than 0.02 mol/L when heated at 80℃ for 10 min. In one word, hydroxide is quite fit to mask aluminum for samples which contain high content of fluoride and aluminum and the BF3 content can be successfully determined by this method.

  19. Determination of hydroxylated polycyclic aromatic hydrocarbons by HPLC-photoionization tandem mass spectrometry in wood smoke particles and soil samples.

    Science.gov (United States)

    Avagyan, Rozanna; Nyström, Robin; Boman, Christoffer; Westerholm, Roger

    2015-06-01

    A simple and fast method for analysis of hydroxylated polycyclic aromatic hydrocarbons using pressurized liquid extraction and high performance liquid chromatography utilizing photoionization tandem mass spectrometry was developed. Simultaneous separation and determination of nine hydroxylated polycyclic aromatic hydrocarbons and two hydroxy biphenyls could be performed in negative mode with a run time of 12 min, including equilibration in 5 min. The calibration curves were in two concentration ranges; 1-50 ng/mL and 0.01-50 μg/mL, with coefficients of correlation R (2) > 0.997. The limits of detection and method quantification limits were in the range of 9-56 pg and 5-38 ng/g, respectively. A two-level full factorial experimental design was used for screening of conditions with the highest impact on the extraction. The extraction procedure was automated and suitable for a large number of samples. The extraction recoveries ranged from 70 to 102 % and the matrix effects were between 92 and 104 %. The overall method was demonstrated on wood smoke particles and soil samples with good analytical performance, and five OH-PAHs were determined in the concentration range of 0.19-210 μg/g. As far as we know, hydroxylated polycyclic aromatic hydrocarbons were determined in wood smoke and soil samples using photoionization mass spectrometry for the first time in this present study. Accordingly, this study shows that high performance liquid chromatography photoionization tandem mass spectrometry can be a good option for the determination of hydroxylated polycyclic aromatic hydrocarbons in complex environmental samples. Graphical Abstract The method developed in this study was used to determine hydroxylated polycyclic aromatic hydrocarbons in wood smoke and soil.

  20. Determination of rare-earth elements in Luna 16 regolith sample by chemical spectral method

    Science.gov (United States)

    Stroganova, N. S.; Ryabukhin, V. A.; Laktinova, N. V.; Ageyeva, L. V.; Galkina, I. P.; Gatinskaya, N. G.; Yermakov, A. N.; Karyakin, A. V.

    1974-01-01

    An analysis was made of regolith from layer A of the Luna 16 sample for rare earth elements, by a chemical spectral method. Chemical and ion exchange concentrations were used to determine the content of 12 elements and Y at the level 0.001 to 0.0001 percent with 10 to 15 percent reproducibility of the emission determination. Results within the limits of reproducibility agree with data obtained by mass spectra, activation, and X-ray fluorescent methods.

  1. Mycobacterium tuberculosis complex detected by modified fluorescent in situ hybridization in lymph nodes of clinical samples.

    Science.gov (United States)

    Rodriguez-Nuñez, Juan; Avelar, Francisco J; Marquez, Francisco; Rivas-Santiago, Bruno; Quiñones, Cesar; Guerrero-Barrera, Alma L

    2012-01-12

    Lymph node tuberculosis (TB) is the leading cause of extrapulmonary tuberculosis and is the most frequently identified type in Aguascalientes, Mexico. Conventional diagnosis has serious limitations for rapid detection of extrapulmonary tuberculosis in clinical samples. Here PCR and modified FISH have been tested as complementary diagnosis methods for extrapulmonary tuberculosis. The specific insertion sequence IS6110 for Mycobacterium tuberculosis complex was used to perform PCR and build DNA and PNA FISH probes (20bp). PCR and modified DNA and PNA FISH assays were performed to evaluate 41 lymph node paraffin-embedded tissue samples, in comparison with the histopathology diagnosis, which was considered the gold standard (22 positive and 19 negative). In comparison with histopathology diagnosis PCR showed 62.5 % sensitivity and 77.8 % specificity (χ(2) = 4.583 p 0.05). Ziehl Neelsen stain was positive in only four cases of 22 lymph node samples positive to histopathology.  In contrast, PCR and modified DNA FISH were positive in 20 cases of the same group. The negative cases were coincident in all tests. PCR and DNA FISH showed a significant increase in the number of cases detected and also showed higher sensitivity and specificity compared with data reported by traditional methodology. In developing countries, these techniques could help to complement the early diagnosis and timely treatment of extrapulmonary tuberculosis.

  2. Comparison of label-free quantification methods for the determination of protein complexes subunits stoichiometry

    Directory of Open Access Journals (Sweden)

    Bertrand Fabre

    2014-09-01

    Full Text Available Protein complexes are the main molecular machines that support all major cellular pathways and their in-depth characterization are essential to understand their functions. Determining the stoichiometry of the different subunits of a protein complex still remains challenging. Recently, many label-free quantitative proteomic approaches have been developed to study the composition of protein complexes. It is therefore of great interest to evaluate these different methods in a stoichiometry oriented objective. Here we compare the ability of four absolute quantitative label-free methods currently used in proteomic studies to determine the stoichiometry of a well-characterized protein complex, the 26S proteasome.

  3. Utility of solid phase spectrophotometry for the modified determination of trace amounts of cadmium in food samples.

    Science.gov (United States)

    Amin, Alaa S; Gouda, Ayman A

    2012-05-01

    A modified selective, highly sensitive and accurate procedure for the determination of trace amounts of cadmium which reacts with 1-(2-benzothiazolylazo)-2-hydroxy-3-naphthoic acid (BTAHNA) to give a deep violet complex with high molar absorptivity (7.05×10(6)Lmol(-1) cm(-1), 3.92×10(7)Lmol(-1)cm(-1), 1.78×10(8)Lmol(-1)cm(-1), and 4.10×10(8)Lmol(-1)cm(-1)), fixed on a Dowex 1-X8 type anion-exchange resin for 10mL, 100mL, 500mL, and 1000mL, respectively. Calibration is linear over the range 0.2-3.5μgL(-1) with RSD of ⩽1.14% (n=10). The detection and quantification limits were calculated. Increasing the sample volume can enhance the sensitivity. The method has been successfully applied for the determination of Cd(II) in food samples, water samples and some salts samples without interfering effect of various cations and anions.

  4. EDXRF applied to the chemical element determination of small invertebrate samples

    Energy Technology Data Exchange (ETDEWEB)

    Magalhaes, Marcelo L.R.; Santos, Mariana L.O.; Cantinha, Rebeca S.; Souza, Thomas Marques de; Franca, Elvis J. de, E-mail: marcelo_rlm@hotmail.com, E-mail: marianasantos_ufpe@hotmail.com, E-mail: rebecanuclear@gmail.com, E-mail: thomasmarques@live.com.pt, E-mail: ejfranca@cnen.gov.br [Centro Regional de Ciencias Nucleares do Nordeste (CRCN-NE/CNEN-PE), Recife, PE (Brazil)

    2015-07-01

    Energy Dispersion X-Ray Fluorescence - EDXRF is a fast analytical technique of easy operation, however demanding reliable analytical curves due to the intrinsic matrix dependence and interference during the analysis. By using biological materials of diverse matrices, multielemental analytical protocols can be implemented and a group of chemical elements could be determined in diverse biological matrices depending on the chemical element concentration. Particularly for invertebrates, EDXRF presents some advantages associated to the possibility of the analysis of small size samples, in which a collimator can be used that directing the incidence of X-rays to a small surface of the analyzed samples. In this work, EDXRF was applied to determine Cl, Fe, P, S and Zn in invertebrate samples using the collimator of 3 mm and 10 mm. For the assessment of the analytical protocol, the SRM 2976 Trace Elements in Mollusk produced and SRM 8415 Whole Egg Powder by the National Institute of Standards and Technology - NIST were also analyzed. After sampling by using pitfall traps, invertebrate were lyophilized, milled and transferred to polyethylene vials covered by XRF polyethylene. Analyses were performed at atmosphere lower than 30 Pa, varying voltage and electric current according to the chemical element to be analyzed. For comparison, Zn in the invertebrate material was also quantified by graphite furnace atomic absorption spectrometry after acid treatment (mixture of nitric acid and hydrogen peroxide) of samples have. Compared to the collimator of 10 mm, the SRM 2976 and SRM 8415 results obtained by the 3 mm collimator agreed well at the 95% confidence level since the E{sub n} Number were in the range of -1 and 1. Results from GFAAS were in accordance to the EDXRF values for composite samples. Therefore, determination of some chemical elements by EDXRF can be recommended for very small invertebrate samples (lower than 100 mg) with advantage of preserving the samples. (author)

  5. Using Isotope Ratio Infrared Spectrometer to determine δ13C and δ18O of carbonate samples

    Science.gov (United States)

    Smajgl, Danijela; Stöbener, Nils; Mandic, Magda

    2017-04-01

    The isotopic composition of calcifying organisms is a key tool for reconstruction past seawater temperature and water chemistry. Therefore stable carbon and oxygen isotopes (δ13C and δ18O) in carbonates have been widely used for reconstruction of paleoenvironments. Precise and accurate determination of isotopic composition of carbon (13C) and oxygen (18O) from carbonate sample with proper referencing and data evaluation algorithm presents a challenge for scientists. Mass spectrometry was the only widely used technique for this kind of analysis, but recent advances make laser based spectroscopy a viable alternative. The Thermo Scientific Delta Ray Isotope Ratio Infrared Spectrometer (IRIS) analyzer with the Universal Reference Interface (URI) Connect is one of those alternatives and with TELEDYNE Cetac ASX-7100 autosampler extends the traditional offerings with a system of high precision and throughput of samples. To establish precision and accuracy of measurements and also to develop optimal sample preparation method for measurements with Delta Ray IRIS and URI Connect, IAEA reference materials were used. Preparation is similar to a Gas Bench II method. Carbonate material is added into the vials, flushed with CO2 free synthetic air and acidified with few droplets of 104% H3PO4. Sample amount used for analysis can be as low as 200 μg. Samples are measured after acidification and equilibration time of one hour at 70°C. The CO2 gas generated by reaction is flushed into the variable volume inside the URI Connect through the Nafion based built-in water trap. For this step, carrier gas (CO2 free air) is used to flush the gas from the vial into the variable volume with a maximum volume of 100 ml. A small amount of the sample is then used for automatic concentration determination present in the variable volume. The Thermo Scientific Qtegra Software automatically adjusts any additional dilution of the sample to achieve the desired concentration (usually 400 ppm) in the

  6. Sensitive determination of cadmium in water samples by room temperature ionic liquid-based preconcentration and electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Martinis, Estefania M. [Laboratory of Environmental Research and Services of Mendoza (LISAMEN), (CCT - CONICET - Mendoza), Av. Ruiz Leal S/N Parque General San Martin, C.C. 131, M 5502 IRA Mendoza (Argentina); Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET) (Argentina); Olsina, Roberto A. [Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET) (Argentina); Departamento de Quimica Analitica, Facultad de Quimica, Bioquimica y Farmacia, Universidad Nacional de San Luis (Argentina); Altamirano, Jorgelina C. [Laboratory of Environmental Research and Services of Mendoza (LISAMEN), (CCT - CONICET - Mendoza), Av. Ruiz Leal S/N Parque General San Martin, C.C. 131, M 5502 IRA Mendoza (Argentina); Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET) (Argentina); Instituto de Ciencias Basicas, Universidad Nacional de Cuyo, Mendoza (Argentina); Wuilloud, Rodolfo G. [Laboratory of Environmental Research and Services of Mendoza (LISAMEN), (CCT - CONICET - Mendoza), Av. Ruiz Leal S/N Parque General San Martin, C.C. 131, M 5502 IRA Mendoza (Argentina); Consejo Nacional de Investigaciones Cientificas y Tecnicas (CONICET) (Argentina); Instituto de Ciencias Basicas, Universidad Nacional de Cuyo, Mendoza (Argentina)], E-mail: rwuilloud@mendoza-conicet.gov.ar

    2008-10-17

    A sensitive preconcentration methodology for Cd determination at trace levels in water samples was developed in this work. 1-Butyl-3-methylimidazolium hexafluorophosphate ([C{sub 4}MIM][PF{sub 6}]) room temperature ionic liquid (RTIL) was successfully used for Cd preconcentration, as cadmium-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol complex [Cd-5-Br-PADAP]. Subsequently, Cd was back-extracted from the RTIL phase with 500 {mu}L of 0.5 mol L{sup -1} nitric acid and determined by electrothermal atomic absorption spectrometry (ETAAS). A preconcentration factor of 40 was achieved with 20 mL of sample. The limit of detection (LOD) obtained under optimum conditions was 3 ng L{sup -1} and the relative standard deviation (R.S.D.) for 10 replicates at 1 {mu}g L{sup -1} Cd{sup 2+} concentration level was 3.5%, calculated at peak heights. The calibration graph was linear from concentration levels near the detection limits up to at least 5 {mu}g L{sup -1}. A correlation coefficient of 0.9997 was achieved. Validation of the methodology was performed by standard addition method and analysis of certified reference material (CRM). The method was successfully applied to the determination of Cd in river and tap water samples.

  7. Recent Advances in the Determination of Pesticides in Environmental Samples by Capillary Electrophoresis

    Directory of Open Access Journals (Sweden)

    Po-Ling Chang

    2016-04-01

    Full Text Available Nowadays, owing to the increasing population and the attempts to satisfy its needs, pesticides are widely applied to control the quantity and quality of agricultural products. However, the presence of pesticide residues and their metabolites in environmental samples is hazardous to the health of humans and all other living organisms. Thus, monitoring these compounds is extremely important to ensure that only permitted levels of pesticide are consumed. To this end, fast, reliable, and environmentally friendly methods that can accurately analyze dilute, complex samples containing both parent substances and their metabolites are required. Focusing primarily on research published since 2010, this review summarizes the use of various sample pretreatment techniques to extract pesticides from various matrices, combined with on-line preconcentration strategies for sensitivity improvement, and subsequent capillary electrophoresis analysis.

  8. Micro-column solid phase extraction to determine uranium and thorium in environmental samples.

    Science.gov (United States)

    Tsai, Tsuey-Lin; Lin, Chun-Chih; Chu, Tieh-Chi

    2008-08-01

    Extraction chromatographic separation techniques based on U/TEVA and TEVA resins were utilized to separate uranium and thorium isotopes in complex matrices from environmental samples. This approach has the advantages of ease of quantitative analysis, small sample size, an absence of mixed waste solvents, complete separation of U/Th isotopes, acceptable chemical yields and good energy resolution in the alpha spectrum. The procedure for analyzing alpha-emitting isotopes of uranium and thorium in geothermal water from Peito, Taiwan, is illustrated in detail. It involves sample pre-concentration, filtration and separation by highly selective extraction chromatographic resins, followed by electroplating and alpha-spectroscopy. The analytical results show a chemical recovery exceeding 55% for U and 65% for Th, respectively, under optimized conditions. The efficient and cost-effective use of recyclable columns makes the analytical methods simple, accurate, rapid, reliable and robust.

  9. A FEM-based method to determine the complex material properties of piezoelectric disks.

    Science.gov (United States)

    Pérez, N; Carbonari, R C; Andrade, M A B; Buiochi, F; Adamowski, J C

    2014-08-01

    Numerical simulations allow modeling piezoelectric devices and ultrasonic transducers. However, the accuracy in the results is limited by the precise knowledge of the elastic, dielectric and piezoelectric properties of the piezoelectric material. To introduce the energy losses, these properties can be represented by complex numbers, where the real part of the model essentially determines the resonance frequencies and the imaginary part determines the amplitude of each resonant mode. In this work, a method based on the Finite Element Method (FEM) is modified to obtain the imaginary material properties of piezoelectric disks. The material properties are determined from the electrical impedance curve of the disk, which is measured by an impedance analyzer. The method consists in obtaining the material properties that minimize the error between experimental and numerical impedance curves over a wide range of frequencies. The proposed methodology starts with a sensitivity analysis of each parameter, determining the influence of each parameter over a set of resonant modes. Sensitivity results are used to implement a preliminary algorithm approaching the solution in order to avoid the search to be trapped into a local minimum. The method is applied to determine the material properties of a Pz27 disk sample from Ferroperm. The obtained properties are used to calculate the electrical impedance curve of the disk with a Finite Element algorithm, which is compared with the experimental electrical impedance curve. Additionally, the results were validated by comparing the numerical displacement profile with the displacements measured by a laser Doppler vibrometer. The comparison between the numerical and experimental results shows excellent agreement for both electrical impedance curve and for the displacement profile over the disk surface. The agreement between numerical and experimental displacement profiles shows that, although only the electrical impedance curve is

  10. Determination of trace elements in paints by direct sampling graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bentlin, Fabrina R.S. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, UFRGS, 91501-970 Porto Alegre, RS (Brazil); Pozebon, Dirce [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, UFRGS, 91501-970 Porto Alegre, RS (Brazil)], E-mail: dircepoz@iq.ufrgs.br; Mello, Paola A.; Flores, Erico M.M. [Departamento de Quimica, Universidade Federal de Santa Maria, UFSM, 97105-900 Santa Maria, RS (Brazil)

    2007-10-17

    A direct sampling graphite furnace atomic absorption spectrometric (DS-GFAAS) method for the determination of Cd, Pb, Cr, Ni, Co and Cu in paints has been developed. Serigraphy, acrylic and tattoo paints were analysed. Approaches like pyrolysis and atomization temperatures, modifiers and sample mass introduced in the atomizer were studied. Quantification was performed using calibration curves measured with aqueous standard solutions pipetted onto the platform. The sample mass introduced in the graphite tube ranged from 0.02 to 8.0 mg. Palladium was used as modifier for Cd, Pb and Cu, while Mg(NO{sub 3}){sub 2} was used for Co. For Ni determination, the graphite platform was covered with carbon powder. The characteristic masses of Cd, Pb, Cr, Ni, Co and Cu were 1.4, 22.5, 7.9, 11.0, 9.6 and 12.5 pg, while the limits of detection were 0.0004, 0.001, 0.03, 0.22, 0.11 and 0.05 {mu}g g{sup -1} of Cd, Pb, Cr, Ni, Co and Cu, respectively. The accuracy was determined by comparison of the results with those obtained by inductively coupled plasma mass spectrometry (ICP-MS) and graphite furnace atomic absorption spectrometry (GFAAS), using liquid sampling of digests. For matrix characterization, major and minor elements (Al, Mg, Ba, Ca, Cr, Cu, Pb, Sr, Ti and Mg) were determined by inductively coupled plasma optical emission spectrometry (ICP OES)

  11. DETERMINATION OF CHLOROPHENOLS, NITROPHENOLS, AND METHYLPHENOLS IN GROUND-WATER SAMPLES USING HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

    Science.gov (United States)

    A high performance liquid chromatography (HPLC) method was developed to quantitatively determine phenolic compounds and their isomers in aqueous samples. The HPLC method can analyze a mixture of 15 contaminants in the same analytical run with an analysis time of 25 minutes. The...

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

    Directory of Open Access Journals (Sweden)

    Rodrigo Fernando dos Santos Salazar

    2011-02-01

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

  13. Automatic system for the determination of metals by anodic stripping potentiometry in non-deaerated samples

    OpenAIRE

    1990-01-01

    An automatic system for the determination of Zn, Cd, Pb and Cu by anodic stripping potentiometry using the oxygen dissolved in the sample as oxidant is reported. The system relies on the use of a PC-compatible computer for instrumental control and data acquisition and processing.

  14. Reliable determination of 237Np in environmental solid samples using 242Pu as a potential tracer

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Roos, Per;

    2011-01-01

    onto various AG 1-type anion exchangers; suitability of 242Pu as a tracer for 237Np determination in environmental solid samples; and long-term chemical stability of tetravalent Np. Experimental results revealed that the degree of resin cross-linking has a significant influence on the separation...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-03-15

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

  16. Sample Size Determination: A Comparison of Attribute, Continuous Variable, and Cell Size Methods.

    Science.gov (United States)

    Clark, Philip M.

    1984-01-01

    Describes three methods of sample size determination, each having its use in investigation of social science problems: Attribute method; Continuous Variable method; Galtung's Cell Size method. Statistical generalization, benefits of cell size method (ease of use, trivariate analysis and trichotyomized variables), and choice of method are…

  17. [Determination of high content of tin in geochemical samples by solid emission spectrometry].

    Science.gov (United States)

    Yao, Jian-Zhen; Hao, Zhi-Hong; Tang, Rui-Ling; Li, Xiao-Jing; Li, Wen-Ge; Zhang, Qin

    2013-11-01

    A method for the determination of high content of tin in geochemical samples by solid emission spectrometry was presented. The dedicated high content tin spectrum standard series was developed. K2S2O7, NaF, Al2O3 and carbon powder were used as buffers and Ge was used as internal standard, and the ratio of sample/matrix/buffer is 1 : 1 : 2. A weak sensitive line (Sn 242. 170 0 nm) was used as the analytical line. The technologies of vertical electrodes, AC arc overlap spectrograph, interception of the exposure, quantitative computer translation spectrum and background correction were used. The determination range is 100-22 350 microg x g(-1), the detection limit is 16.64 microg x g(-1), and the precision is (RSD, n = 12) 4.11%-6.46%. The accuracy of the method has been verified by determination of high content of tin in national geochemical standard samples and the results are in agreement with certified value. The method can be used for measurement directly without dilution of high content of tin in geochemical samples, and it greatly improved the detection upper limit for the determination of tin with solid emission spectroscopy and has certain practical value.

  18. Determinants of salivary evening alpha-amylase in a large sample free of psychopathology

    NARCIS (Netherlands)

    Veen, Gerthe; Giltay, Erik J.; Vreeburg, Sophie A.; Licht, Carmilla M. M.; Cobbaert, Christa M.; Zitman, Frans G.; Penninx, Brenda W. J. H.

    2012-01-01

    Objective: Recently, salivary alpha-amylase (sAA) has been proposed as a suitable index for sympathetic activity and dysregulation of the autonomic nervous system (ANS). Although determinants of sAA have been described, they have not been studied within the same study with a large sample size withou

  19. Determination of trace elements in paints by direct sampling graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Bentlin, Fabrina R S; Pozebon, Dirce; Mello, Paola A; Flores, Erico M M

    2007-10-17

    A direct sampling graphite furnace atomic absorption spectrometric (DS-GFAAS) method for the determination of Cd, Pb, Cr, Ni, Co and Cu in paints has been developed. Serigraphy, acrylic and tattoo paints were analysed. Approaches like pyrolysis and atomization temperatures, modifiers and sample mass introduced in the atomizer were studied. Quantification was performed using calibration curves measured with aqueous standard solutions pipetted onto the platform. The sample mass introduced in the graphite tube ranged from 0.02 to 8.0 mg. Palladium was used as modifier for Cd, Pb and Cu, while Mg(NO3)2 was used for Co. For Ni determination, the graphite platform was covered with carbon powder. The characteristic masses of Cd, Pb, Cr, Ni, Co and Cu were 1.4, 22.5, 7.9, 11.0, 9.6 and 12.5 pg, while the limits of detection were 0.0004, 0.001, 0.03, 0.22, 0.11 and 0.05 microg g(-1) of Cd, Pb, Cr, Ni, Co and Cu, respectively. The accuracy was determined by comparison of the results with those obtained by inductively coupled plasma mass spectrometry (ICP-MS) and graphite furnace atomic absorption spectrometry (GFAAS), using liquid sampling of digests. For matrix characterization, major and minor elements (Al, Mg, Ba, Ca, Cr, Cu, Pb, Sr, Ti and Mg) were determined by inductively coupled plasma optical emission spectrometry (ICP OES).

  20. Determinants of salivary evening alpha-amylase in a large sample free of psychopathology

    NARCIS (Netherlands)

    Veen, Gerthe; Giltay, Erik J.; Vreeburg, Sophie A.; Licht, Carmilla M. M.; Cobbaert, Christa M.; Zitman, Frans G.; Penninx, Brenda W. J. H.

    Objective: Recently, salivary alpha-amylase (sAA) has been proposed as a suitable index for sympathetic activity and dysregulation of the autonomic nervous system (ANS). Although determinants of sAA have been described, they have not been studied within the same study with a large sample size

  1. Spectrophotometric Determination of Total Sulfite in White Wine Samples Using Crude Extracts from Flowers

    Science.gov (United States)

    Flora Barbosa Soares, Márlon Herbert; Ramos, Luiz Antonio; Tadeu Gomes Cavalheiro, Éder

    2002-09-01

    A didactic spectrophotometric method for determining the sulfite content in white wine samples is proposed. It is based upon a discoloring reaction between flower anthocyanins and the sulfite in basic media. Students' results obtained from iodometric data agreed well with results obtained by the proposed procedure. The use of natural dyes attracted students' interest, enhancing the learning process.

  2. A bioinformatics approach for determining sample identity from different lanes of high-throughput sequencing data.

    Directory of Open Access Journals (Sweden)

    Rachel L Goldfeder

    Full Text Available The ability to generate whole genome data is rapidly becoming commoditized. For example, a mammalian sized genome (∼3Gb can now be sequenced using approximately ten lanes on an Illumina HiSeq 2000. Since lanes from different runs are often combined, verifying that each lane in a genome's build is from the same sample is an important quality control. We sought to address this issue in a post hoc bioinformatic manner, instead of using upstream sample or "barcode" modifications. We rely on the inherent small differences between any two individuals to show that genotype concordance rates can be effectively used to test if any two lanes of HiSeq 2000 data are from the same sample. As proof of principle, we use recent data from three different human samples generated on this platform. We show that the distributions of concordance rates are non-overlapping when comparing lanes from the same sample versus lanes from different samples. Our method proves to be robust even when different numbers of reads are analyzed. Finally, we provide a straightforward method for determining the gender of any given sample. Our results suggest that examining the concordance of detected genotypes from lanes purported to be from the same sample is a relatively simple approach for confirming that combined lanes of data are of the same identity and quality.

  3. A bioinformatics approach for determining sample identity from different lanes of high-throughput sequencing data.

    Science.gov (United States)

    Goldfeder, Rachel L; Parker, Stephen C J; Ajay, Subramanian S; Ozel Abaan, Hatice; Margulies, Elliott H

    2011-01-01

    The ability to generate whole genome data is rapidly becoming commoditized. For example, a mammalian sized genome (∼3Gb) can now be sequenced using approximately ten lanes on an Illumina HiSeq 2000. Since lanes from different runs are often combined, verifying that each lane in a genome's build is from the same sample is an important quality control. We sought to address this issue in a post hoc bioinformatic manner, instead of using upstream sample or "barcode" modifications. We rely on the inherent small differences between any two individuals to show that genotype concordance rates can be effectively used to test if any two lanes of HiSeq 2000 data are from the same sample. As proof of principle, we use recent data from three different human samples generated on this platform. We show that the distributions of concordance rates are non-overlapping when comparing lanes from the same sample versus lanes from different samples. Our method proves to be robust even when different numbers of reads are analyzed. Finally, we provide a straightforward method for determining the gender of any given sample. Our results suggest that examining the concordance of detected genotypes from lanes purported to be from the same sample is a relatively simple approach for confirming that combined lanes of data are of the same identity and quality.

  4. Determination of heavy metals in solid emission and immission samples using atomic absorption spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Fara, M.; Novak, F. [EGU Prague, PLC, Bichovice, Prague (Czechoslovakia)

    1995-12-01

    Both flame and electrothermal methods of atomic absorption spectroscopy (AAS) have been applied to the determination of Al, As, Be, Ca, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, TI, Se, V and Zn in emission and emission (deposition) samples decomposed in open PTFE test-tubes by individual fuming-off hydrofluoric, perchloroic and nitric acid. An alternative hydride technique was also used for As and Se determination and Hg was determined using a self-contained AAS analyzer. A graphite platform proved good to overcome non-spectral interferences in AAS-ETA. Methods developed were verified by reference materials (inc. NBS 1633a).

  5. An analytical protocol for the determination of total mercury concentrations in solid peat samples.

    Science.gov (United States)

    Roos-Barraclough, F; Givelet, N; Martinez-Cortizas, A; Goodsite, M E; Biester, H; Shotyk, W

    2002-06-20

    Traditional peat sample preparation methods such as drying at high temperatures and milling may be unsuitable for Hg concentration determination in peats due to the possible presence of volatile Hg species, which could be lost during drying. Here, the effects of sample preparation and natural variation on measured Hg concentrations are investigated. Slight increases in mercury concentrations were observed in samples dried at room temperature and at 30 degrees C (6.7 and 2.48 ng kg(-1) h(-1), respectively), and slight decreases were observed in samples dried at 60, 90 and 105 degrees C (2.36, 3.12 and 8.52 ng kg(-1) h(-1), respectively). Fertilising the peat slightly increased Hg loss (3.08 ng kg(-1) h(-1) in NPK-fertilised peat compared to 0.28 ng kg(-1) h(-1) in unfertilised peat, when averaged over all temperatures used). Homogenising samples by grinding in a machine also caused a loss of Hg. A comparison of two Hg profiles from an Arctic peat core, measured in frozen samples and in air-dried samples, revealed that no Hg losses occurred upon air-drying. A comparison of Hg concentrations in several plant species that make up peat, showed that some species (Pinus mugo, Sphagnum recurvum and Pseudevernia furfuracea) are particularly efficient Hg retainers. The disproportionally high Hg concentrations in these species can cause considerable variation in Hg concentrations within a peat slice. The variation of water content (1.6% throughout 17-cm core, 0.97% in a 10 x 10 cm slice), bulk density (40% throughout 17-cm core, 15.6% in a 10 x 10 cm slice) and Hg concentration (20% in a 10 x 10 cm slice) in ombrotrophic peat were quantified in order to determine their relative importance as sources of analytical error. Experiments were carried out to determine a suitable peat analysis program using the Leco AMA 254, capable of determining mercury concentrations in solid samples. Finally, an analytical protocol for the determination of Hg concentrations in solid peat samples

  6. SAMPLE SIZE DETERMINATION IN NON-RADOMIZED SURVIVAL STUDIES WITH NON-CENSORED AND CENSORED DATA

    Directory of Open Access Journals (Sweden)

    S FAGHIHZADEH

    2003-06-01

    Full Text Available Introduction: In survival analysis, determination of sufficient sample size to achieve suitable statistical power is important .In both parametric and non-parametric methods of classic statistics, randomn selection of samples is a basic condition. practically, in most clinical trials and health surveys randomn allocation is impossible. Fixed - effect multiple linear regression analysis covers this need and this feature could be extended to survival regression analysis. This paper is the result of sample size determination in non-randomnized surval analysis with censored and non -censored data. Methods: In non-randomnized survival studies, linear regression with fixed -effect variable could be used. In fact such a regression is conditional expectation of dependent variable, conditioned on independent variable. Likelihood fuction with exponential hazard constructed by considering binary variable for allocation of each subject to one of two comparing groups, stating the variance of coefficient of fixed - effect independent variable by determination coefficient , sample size determination formulas are obtained with both censored and non-cencored data. So estimation of sample size is not based on the relation of a single independent variable but it could be attain the required power for a test adjusted for effect of the other explanatory covariates. Since the asymptotic distribution of the likelihood estimator of parameter is normal, we obtained the variance of the regression coefficient estimator formula then by stating the variance of regression coefficient of fixed-effect variable, by determination coefficient we derived formulas for determination of sample size in both censored and non-censored data. Results: In no-randomnized survival analysis ,to compare hazard rates of two groups without censored data, we obtained an estimation of determination coefficient ,risk ratio and proportion of membership to each group and their variances from

  7. Electrochemical behavior and determination of major phenolic antioxidants in selected coffee samples.

    Science.gov (United States)

    Oliveira-Neto, Jerônimo Raimundo; Rezende, Stefani Garcia; de Fátima Reis, Carolina; Benjamin, Stephen Rathinaraj; Rocha, Matheus Lavorenti; de Souza Gil, Eric

    2016-01-01

    The redox behavior of commercial roasted coffee products were evaluated by electroanalysis, whereas high performance liquid chromatography (HPLC) was used for determination of cinnamic acid markers, the total phenolic content (TPC) was achieved by Folin-Ciocalteu assay, and the traditional DPPH (1-diphenyl-2-picrylhydrazyl) method for antioxidant power determination. In turn, an optimized electrochemical index was proposed to estimate the antioxidant power of different samples and it was found a great correlation between all methods. The voltammetric profile of all coffee samples was quite similar, presenting the same number of peaks at the same potential values. Minor differences on current levels were in agreement with the total phenolic and major markers content, as well as, to the antioxidant power. Therefore, the electrochemical methods showed to be practical, low cost and very useful to evaluate the antioxidant properties of coffee samples, which is a relevant quality parameter of this widely consumed beverage.

  8. Determination of metals in composite diet samples by inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Melnyk, Lisa Jo; Morgan, Jeffrey N; Fernando, Reshan; Pellizzari, Edo D; Akinbo, Olujide

    2003-01-01

    A study was conducted to evaluate the applicability of inductively coupled plasma-mass spectrometry (ICP-MS) techniques for determination of metals in composite diets. Aluminum, cadmium, chromium, copper, lead, manganese, nickel, vanadium, and zinc were determined by this method. Atmospheric pressure microwave digestion was used to solubilize analytes in homogenized composite diet samples, and this procedure was followed by ICP-MS analysis. Recovery of certified elements from standard reference materials ranged from 92 to 119% with relative standard deviations (RSDs) of 0.4-1.9%. Recovery of elements from fortified composite diet samples ranged from 75 to 129% with RSDs of 0-11.3%. Limits of detection ranged from 1 to 1700 ng/g; high values were due to significant amounts of certain elements naturally present in composite diets. Results of this study demonstrate that low-resolution quadrupole-based ICP-MS provides precise and accurate measurements of the elements tested in composite diet samples.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2013-01-15

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

  10. A spectrophotometric flow injection system for streptomycin determination in veterinary samples

    Science.gov (United States)

    Frugeri, Pedro Marcos; Lago, Ayla Campos do; Wisniewski, Célio; Luccas, Pedro Orival

    2014-01-01

    In this work a spectrophotometric flow injection analysis system for streptomycin determination in veterinary samples, is being proposed. The method is based on streptomycin alkaline hydrolysis that forms guanidine, followed by the reaction with Fe(II). The colored product has absorption peak at 520 nm. To evaluate and optimize the system parameters, chemometrics tools, such as factorial design, Pareto chart and Doelhert design, were used. The veterinary samples are diluted in water and introduced in the FIA system, therefore no sample preparation is required. The optimized system presented: linear range of 60 up to 1000 mg L-1, limit of detection of 18 mg L-1 and sampling rate of 36 readings per hour. The precision was checked and the CV for veterinary sample readings were always less than 6.5%. The accuracy was studied by comparison with chromatographic method, thus, five samples of pharmaceutical veterinary were determined by HPLC and by the proposed method, and the results are in agreement (t-test, p = 0.05).

  11. [Determination of Trace Germanium in Plant Samples by Dry Ashing-Atomic Fluorescence Spectrometry].

    Science.gov (United States)

    Chen, Hai-jie; Yu, Zhao-shui; Bai, Jin-feng; Li, Qing-xia; Liu, Ya-xuan; Bo, Wei; Zhang, Qin

    2015-04-01

    To reduce the limit of detection (LOD) and allow the accurate determination of Ge, a dry ashing method was performed to enrich the Ge in plant samples. A method for the determination.of trace Ge in plant samples by HG-AFS was established. Study of the effect of temperature on the ashing of plant samples showed that no volatile loss of Ge occurred even at 900 °C. Additional experiments indicated that a 4 h burning process at 600 °C would be sufficient to fully ash the plant samples. Various digestion methods (involving nitric acid, hydrofluoric acid, and sulfuric acid digestion methods) for ashed samples were investigated. High-temperature ashing with large sample weights was used, which could reduce the reagent doses and the method's LOD effectively and simultaneously, the precision of the method was improved. The method's LOD was 0.27 ng · g(-1), and the relative standard deviation was 3.99%-6.81%. Verified with national biological reference materials (grade I), the proposed method was accurate and reliable.

  12. Highly selective ionic liquid-based microextraction method for sensitive trace cobalt determination in environmental and biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Berton, Paula [Analytical Chemistry Research and Development Group (QUIANID), (LISAMEN - CCT - CONICET - Mendoza), Av. Ruiz Leal S/N Parque General San Martin, M 5502 IRA Mendoza (Argentina); Wuilloud, Rodolfo G., E-mail: rwuilloud@mendoza-conicet.gov.ar [Analytical Chemistry Research and Development Group (QUIANID), (LISAMEN - CCT - CONICET - Mendoza), Av. Ruiz Leal S/N Parque General San Martin, M 5502 IRA Mendoza (Argentina); Instituto de Ciencias Basicas, Universidad Nacional de Cuyo, Mendoza (Argentina)

    2010-03-10

    A simple and rapid dispersive liquid-liquid microextraction procedure based on an ionic liquid (IL-DLLME) was developed for selective determination of cobalt (Co) with electrothermal atomic absorption spectrometry (ETAAS) detection. Cobalt was initially complexed with 1-nitroso-2-naphtol (1N2N) reagent at pH 4.0. The IL-DLLME procedure was then performed by using a few microliters of the room temperature ionic liquid (RTIL) 1-hexyl-3-methylimidazolium hexafluorophosphate [C{sub 6}mim][PF{sub 6}] as extractant while methanol was the dispersant solvent. After microextraction procedure, the Co-enriched RTIL phase was solubilized in methanol and directly injected into the graphite furnace. The effect of several variables on Co-1N2N complex formation, extraction with the dispersed RTIL phase, and analyte detection with ETAAS, was carefully studied in this work. An enrichment factor of 120 was obtained with only 6 mL of sample solution and under optimal experimental conditions. The resultant limit of detection (LOD) was 3.8 ng L{sup -1}, while the relative standard deviation (RSD) was 3.4% (at 1 {mu}g L{sup -1} Co level and n = 10), calculated from the peak height of absorbance signals. The accuracy of the proposed methodology was tested by analysis of a certified reference material. The method was successfully applied for the determination of Co in environmental and biological samples.

  13. Generalized window factor analysis for selective analysis of the target component in real samples with complex matrices.

    Science.gov (United States)

    Li, Pao; Cai, Wensheng; Shao, Xueguang

    2015-08-14

    In chromatographic analysis of multicomponent real samples, peak overlapping, high level of noise and background are frequently encountered, making the qualitative and quantitative analysis difficult or even impossible. In this work, an algorithm named as generalized window factor analysis (GWFA) was proposed for quantitative analysis of the target components in the samples with complex matrices by gas chromatography-mass spectrometry (GC-MS). The theory and calculation of GWFA are just similar with the conventional window factor analysis (WFA), but the "window" is defined as the selected channels (mass-to-charge ratios) in the mass spectral dimension of the data matrix, instead of a continuous region in chromatographic dimension along the retention time. Therefore, the generalized window for a target component can be easily determined with the help of the mass spectrum. Then, the calculated mass spectrum can be obtained with the window and quantitative determination can be achieved with the help of the standard. Both simulated and experimental data were investigated with the proposed method. Whether or not a peak shift occurs during the test, accurate results were obtained from the overlapping GC-MS signals with high level of noise and background.

  14. Determination of noble metals in biological samples by electrothermal vaporization inductively coupled plasma mass spectrometry, following cloud point extraction

    Science.gov (United States)

    Andreia Mesquita da Silva, Márcia; Lúcia Azzolin Frescura, Vera; José Curtius, Adilson

    2001-10-01

    A simple separation procedure for noble metals based on cloud point extraction is proposed. The analyte ions in aqueous acidic solution, obtained by the acid digestion of the samples, were complexed with O, O-diethyl-dithiophosphate and Triton X-114 was added as a non-ionic surfactant. By increasing the temperature up to the cloud point, a phase separation occurs, resulting in an aqueous phase and a surfactant-rich phase containing most of the analytes that were complexed. The metals in the surfactant-rich phase were determined by electrothermal vaporization inductively coupled plasma mass spectrometry. The extraction conditions as well as the instrumental parameters were optimized. Enrichment factors ranging from 7 (Rh) to 60 (Pt) and limits of detection from 0.6 (Pt) to 3.0 ng l -1 (Rh) were obtained in the digested samples. The extraction was not efficient for Ir. Among the reference materials analyzed in this work, only one (SRM 2670, urine) presented recommended values for Au and Pt. Due to the non-availability of adequate CRMs, accuracy was assessed by spiking known analyte amounts to the acid digests. Recoveries close to 100% were observed for all the studied elements but Ru. Poor agreement between found and recommended values was observed for non-digested urine sample, probably due to the carrier effect of co-extracted residual matrix components. However, good agreement was reached after urine acid mineralization.

  15. Determination of diniconazole in agricultural samples by sol-gel immunoaffinity extraction procedure coupled with HPLC and ELISA.

    Directory of Open Access Journals (Sweden)

    Zhenjiang Liu

    Full Text Available BACKGROUND: In the European Union (EU, the use of diniconazole-M is no longer authorized. However, residues of diniconazole-M occur in various plant commodities. METHODOLOGY/PRINCIPAL FINDINGS: A selective and simple analytical method for the trace level determination of diniconazole in soil, fruit, vegetables and water samples was developed based on immunoaffinity extraction followed by Enzyme-linked immunosorbent assay (ELISA and the high-performance liquid chromatography (HPLC analysis. The ELISA was based on monoclonal antibodies highly specific to diniconazole and was a fast, cost-effective, and selective screening method for the detection of diniconazole. The results of the ELISA correlated well with gas chromatography (GC results, with the correlation coefficient of 0.9879 (n = 19. A simple gel permeation chromato- graphy clean-up method was developed to purify extracts from matrices containing high amounts of fat and natural pigments, without the need for a large dilution of the sample. The immunoaffinity column (IAC capacity was 0.180 mg g(-1. The columns could be re-used approximately 20 times with no significant alteration in capacity. The recoveries from complex samples were in the range of 89.2% to 96.1% with a relative standard deviation (RSD of 0.770%-6.11% by ELISA. The results were in good agreement with those obtained by HPLC method. CONCLUSION/SIGNIFICANCE: The IAC extraction procedure coupled with HPLC and ELISA analysis could be also used as alternative effective analytical methods for the determination of diniconazole concentrations in complex samples.

  16. A new Gibbs sampling based algorithm for Bayesian model updating with incomplete complex modal data

    Science.gov (United States)

    Cheung, Sai Hung; Bansal, Sahil

    2017-08-01

    Model updating using measured system dynamic response has a wide range of applications in system response evaluation and control, health monitoring, or reliability and risk assessment. In this paper, we are interested in model updating of a linear dynamic system with non-classical damping based on incomplete modal data including modal frequencies, damping ratios and partial complex mode shapes of some of the dominant modes. In the proposed algorithm, the identification model is based on a linear structural model where the mass and stiffness matrix are represented as a linear sum of contribution of the corresponding mass and stiffness matrices from the individual prescribed substructures, and the damping matrix is represented as a sum of individual substructures in the case of viscous damping, in terms of mass and stiffness matrices in the case of Rayleigh damping or a combination of the former. To quantify the uncertainties and plausibility of the model parameters, a Bayesian approach is developed. A new Gibbs-sampling based algorithm is proposed that allows for an efficient update of the probability distribution of the model parameters. In addition to the model parameters, the probability distribution of complete mode shapes is also updated. Convergence issues and numerical issues arising in the case of high-dimensionality of the problem are addressed and solutions to tackle these problems are proposed. The effectiveness and efficiency of the proposed method are illustrated by numerical examples with complex modes.

  17. Determination of trace lead in biological and water samples with dispersive liquid-liquid microextraction preconcentration.

    Science.gov (United States)

    Liang, Pei; Sang, Hongbo

    2008-09-01

    A new method for the determination of trace lead was developed by dispersive liquid-liquid microextraction preconcentration and graphite furnace atomic absorption spectrometry. In the proposed approach, 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP) was used as a chelating agent, and carbon tetrachloride and ethanol were selected as extraction and dispersive solvents. Some factors influencing the extraction efficiency of lead and its subsequent determination, including extraction and dispersive solvent type and volume, pH of sample solution, concentration of the chelating agent, and extraction time, were studied and optimized. Under the optimum conditions, the enrichment factor of this method for lead was reached at 78. The detection limit for lead was 39 ng L(-1) (3 sigma), and the relative standard deviation (RSD) was 3.2% (n=7, c=10 ng mL(-1)). The method was successfully applied to the determination of trace amounts of lead in human urine and water samples.

  18. Determination of covalently bound hypusine and deoxyhypusine to protein using submilligram of protein samples by HPLC.

    Science.gov (United States)

    Beppu, T; Shirahata, A; Samejima, K

    1996-01-01

    A sensitive and reliable method for the determination of hypusine and deoxyhypusine in eIF-5A protein, an initiation factor of protein synthesis, was developed. An advantage of this method is the use of N epsilon-(5-aminopentyl)lysine, an analogue of deoxyhypusine, as an internal standard. The application made it possible to determine hypusine in less than a mg of protein samples from cultured HTC cells and rat organs. After acid hydrolysis of protein samples to which had been added the internal standard, the hydrolysates were fractionated by carboxymethyl cellulose column chromatography. Also, diamine fractions containing a few pmol of hypusine and deoxyhypusine were successfully analyzed by a reversed phase HPLC with a fluorescence detection of o-phthalaldehyde. The method was applied for the determination of hypusine and deoxyhypusine in drug-treated HTC cells and normal rat organs. The results from HTC cells were discussed based on the known effects of each drug on hypusine biosynthesis.

  19. On-line sample treatment and FT-IR determination of doxylamine succinate in pharmaceuticals.

    Science.gov (United States)

    Ventura-Gayete, Josep F; de la Guardia, Miguel; Garrigues, Salvador

    2006-12-15

    A low solvent consumption method for Fourier transform infrared spectroscopy (FT-IR) determination of doxylamine succinate in pharmaceuticals has been developed. The analyte was continuous and selectively extracted with a 13% (v/v) ethanol:chloroform solvent mixture, recirculating the solvent through the sample and monitoring the process by FT-IR. Doxylamine succinate was determined by on-line standard addition measuring the peak area in the regions 1730-1710 and 1485-1462cm(-1) corrected with a two-point baseline established between 2000 and 1800cm(-1). This new method implies low volumes of chloroformic solvent mixture, only 2.6mL per sample, in front of classical batch FT-IR methods, improving analytical efficiency and reducing waste generation. The on-line extraction and standard addition determination of doxylamine succinate allowed a throughput of 10h(-1).

  20. Simultaneous preconcentration of Co(II), Ni(II), Cu(II), and Cd(II) from environmental samples on Amberlite XAD-2000 column and determination by FAAS

    Energy Technology Data Exchange (ETDEWEB)

    Duran, Celal [Department of Chemistry, Faculty of Arts and Sciences, Karadeniz Technical University, 61080 Trabzon (Turkey)], E-mail: cduran@ktu.edu.tr; Senturk, Hasan Basri [Department of Chemistry, Faculty of Arts and Sciences, Karadeniz Technical University, 61080 Trabzon (Turkey); Elci, Latif [Department of Chemistry, Faculty of Arts and Sciences, Pamukkale University, 20020 Denizli (Turkey); Soylak, Mustafa [Department of Chemistry, Faculty of Arts and Sciences, Erciyes University, 38039 Kayseri (Turkey); Tufekci, Mehmet [Department of Chemistry, Faculty of Arts and Sciences, Karadeniz Technical University, 61080 Trabzon (Turkey)

    2009-02-15

    A new method for the preconcentration of some trace metals (Co, Ni, Cu, and Cd) as complexed with ammonium pyrrolidynedithiocarbamate (APDC) was developed using a mini-column filled with Amberlite XAD-2000 resin. Metal contents were determined by flame atomic absorption spectrometry (FAAS) after the metal complexes accumulated on the resin were eluted with 1 M HNO{sub 3} in acetone. The effects of the analytical parameters such as sample pH, quantity of complexing agent, eluent type, resin quantity, sample volume, sample flow rate, and matrix ions were investigated on the recovery of the metals from aqueous solutions. The relative standard deviation (R.S.D.) of the method was <6%. The validation of the method was confirmed using two certified reference materials (CRM TMDW-500 Drinking Water and CRM SA-C Sandy Soil C). The method was successfully applied to some stream waters and mushroom samples from Eastern Black Sea Region (Trabzon city) of Turkey.

  1. Simultaneous preconcentration of Co(II), Ni(II), Cu(II), and Cd(II) from environmental samples on Amberlite XAD-2000 column and determination by FAAS.

    Science.gov (United States)

    Duran, Celal; Senturk, Hasan Basri; Elci, Latif; Soylak, Mustafa; Tufekci, Mehmet

    2009-02-15

    A new method for the preconcentration of some trace metals (Co, Ni, Cu, and Cd) as complexed with ammonium pyrrolidynedithiocarbamate (APDC) was developed using a mini-column filled with Amberlite XAD-2000 resin. Metal contents were determined by flame atomic absorption spectrometry (FAAS) after the metal complexes accumulated on the resin were eluted with 1M HNO(3) in acetone. The effects of the analytical parameters such as sample pH, quantity of complexing agent, eluent type, resin quantity, sample volume, sample flow rate, and matrix ions were investigated on the recovery of the metals from aqueous solutions. The relative standard deviation (R.S.D.) of the method was <6%. The validation of the method was confirmed using two certified reference materials (CRM TMDW-500 Drinking Water and CRM SA-C Sandy Soil C). The method was successfully applied to some stream waters and mushroom samples from Eastern Black Sea Region (Trabzon city) of Turkey.

  2. Determination of Different Metals in Steel Waste Samples Using laser Induced Breakdown Spectroscopy

    Directory of Open Access Journals (Sweden)

    A. H. Bakry

    2007-12-01

    Full Text Available Elemental analysis of waste samples collected from steel products manufacturing plant (SPS located at industrial city of Jeddah, Saudi-Arabia has been carried out using Laser Induced Breakdown Spectroscopy (LIBS. The 1064 nm laser radiations from a Nd:YAG laser at an irradiance of 7.6  1010 W cm –2 were used. Atomic emission spectra of the elements present in the waste samples were recorded in the 200 – 620 nm region. Elements such as Fe, W, Ti, Al, Mg, Ca, S, Mn, and Na were detected in these samples. Quantitative determination of the elemental concentration was obtained for these metals against certified standard samples. Parametric dependences of LIBS signal intensity on incident laser energy and time delay between the laser pulse and data acquisition system were also carried out.

  3. Determination of polyaromatic hydrocarbons in domestic, commercial and industrial soot samples

    Energy Technology Data Exchange (ETDEWEB)

    Iqbal, Yousaf; Sohail, Syed Muhammad; Ahmad, Imtiaz [Peshawar Univ., Khyber Pakhtunkhawa (Pakistan). Inst. of Chemical Sciences; Saeed, Khalid [Malakand Univ., Khyber Pakhtunkhawa (Pakistan). Dept. of Chemistry

    2013-05-15

    Polycyclic aromatic hydrocarbons (PAHs) were determined in domestic, commercial and industrial soot samples via HPLC. The study showed that benzo[a]pyrene (bap) was not present in most of the samples. The highest quantity of BaP was found in Pakistan Particle Board where its concentration was 259.12 mg/kg. The high quantity of other PAHs such as chrysene (CHR), anthracene (ANT), fluorene (FL), naphthalene (NAP), phenanthrene (PHE), acenaphthylene (ACP) and flouranthene (FTH) were found in tandoor, kabab karayi, tabakhee, brick kiln and motor car soot samples. The low concentration of most of the PAH compounds in most of the samples might be due to their photooxidative, biological and microbial degradation. (orig.)

  4. Determination of Cu, Zn, and Se in microvolumes of liquid biological samples

    Science.gov (United States)

    Shaban, H. A.; Shaltout, A. A.; Abdou, M.; Al Ashker, E. A.; Elgohary, M.

    2011-01-01

    Cu, Zn, and Se were successfully determined in a few microliters (<100 μl) of biological samples using discrete injection atomic absorption spectrometry. Different factors were investigated in order to obtain a biological sample volume which is valid for analysis. Among them are the effect of microsampling volume variations (starting from 40 to 200 μl), nebulization efficiency, detection limits, precision, and finally the calibration and sensitivity of the proposed method. It was found that 60 μl of the biological sample was adequate for the quantitative analysis with reasonable precision. The advantages of the proposed method are not only rapidity, simplicity, sensitivity, and good precision, but also, contrary to conventional flame atomic absorption spectrometry, the capability of analyzing microvolumes of samples.

  5. Determination of single photon ionization cross sections for quantitative analysis of complex organic mixtures.

    Science.gov (United States)

    Adam, Thomas; Zimmermann, Ralf

    2007-11-01

    Soft single photon ionization (SPI)-time-of-flight mass spectrometry (TOFMS) is well suited for fast and comprehensive analysis of complex organic gas mixtures, which has been demonstrated in various applications. This work describes a calibration scheme for SPI, which enables quantification of a large number of compounds by only calibrating one compound of choice, in this case benzene. Photoionization cross sections of 22 substances were determined and related to the yield of benzene. These substances included six alkanes (pentane, hexane, heptane, octane, nonane, decane), three alkenes (propene, butane, pentene), two alkynes (propyne, butyne), two dienes (butadiene, isoprene), five monoaromatic species (benzene, toluene, xylene, styrene, monochlorobenzene) and NO. The cross sections of organic compounds differ by about one order of magnitude but the photoionization properties of compounds belonging to one compound class are rather similar. Therefore, the scheme can also be used for an approximate quantification of compound classes. This is demonstrated by a fast characterization and pattern recognition of two gasoline samples with different origins (Germany and South Africa) and a diesel sample (Germany). The on-line capability of the technique and the scheme is demonstrated by quantitatively monitoring and comparing the cold engine start of four vehicles: a gasoline passenger car, a diesel van, a motorbike and a two-stroke scooter.

  6. Determination of humic substances in natural waters by cathodic stripping voltammetry of their complexes with iron.

    Science.gov (United States)

    Laglera, Luis M; Battaglia, Gianluca; van den Berg, Constant M G

    2007-09-05

    A new voltammetric method is presented for the measurement of humic substances (HS) in natural waters. The method is based on catalytic cathodic stripping voltammetry (CSV) and makes use of adsorptive properties of iron-HS complexes on the mercury drop electrode at natural pH. A fulvic acid standard (IHSS) was used to confirm the voltammetric response (peak potential and sensitivity) for the HS for natural water samples. Optimized conditions included the linear-sweep mode, deposition at -0.1 V, pH buffered at 8 and a scan rate of 50 mV s(-1). At a deposition time of 240 s in the presence of 10 nM iron and 30 mM bromate, the detection limit was 5 microg L(-1) HS in seawater, which could be lowered further by an increase in the bromate concentration, or in the adsorption time. The method was used to determine HS in the Irish Sea which were found to occur at levels between 60 and 600 microg L(-1). The new method is sufficiently sensitive to detect the low HS content in oceanic samples and has implications to the study of iron speciation.

  7. Cadmium and lead determination by ICPMS: Method optimization and application in carabao milk samples

    Directory of Open Access Journals (Sweden)

    Riza A. Magbitang

    2012-06-01

    Full Text Available A method utilizing inductively coupled plasma mass spectrometry (ICPMS as the element-selective detector with microwave-assisted nitric acid digestion as the sample pre-treatment technique was developed for the simultaneous determination of cadmium (Cd and lead (Pb in milk samples. The estimated detection limits were 0.09ìg kg-1 and 0.33ìg kg-1 for Cd and Pb, respectively. The method was linear in the concentration range 0.01 to 500ìg kg-1with correlation coefficients of 0.999 for both analytes.The method was validated using certified reference material BCR 150 and the determined values for Cd and Pb were 18.24 ± 0.18 ìg kg-1 and 807.57 ± 7.07ìg kg-1, respectively. Further validation using another certified reference material, NIST 1643e, resulted in determined concentrations of 6.48 ± 0.10 ìg L-1 for Cd and 21.96 ± 0.87 ìg L-1 for Pb. These determined values agree well with the certified values in the reference materials.The method was applied to processed and raw carabao milk samples collected in Nueva Ecija, Philippines.The Cd levels determined in the samples were in the range 0.11 ± 0.07 to 5.17 ± 0.13 ìg kg-1 for the processed milk samples, and 0.11 ± 0.07 to 0.45 ± 0.09 ìg kg-1 for the raw milk samples. The concentrations of Pb were in the range 0.49 ± 0.21 to 5.82 ± 0.17 ìg kg-1 for the processed milk samples, and 0.72 ± 0.18 to 6.79 ± 0.20 ìg kg-1 for the raw milk samples.

  8. Core size determination and structural characterization of intravenous iron complexes by cryogenic transmission electron microscopy.

    Science.gov (United States)

    Wu, Yong; Petrochenko, Peter; Chen, Lynn; Wong, Sook Yee; Absar, Mohammad; Choi, Stephanie; Zheng, Jiwen

    2016-05-30

    Understanding physicochemical properties of intravenous (IV) iron drug products is essential to ensure the manufacturing process is consistent and streamlined. The history of physicochemical characterization of IV iron complex formulations stretches over several decades, with disparities in iron core size and particle morphology as the major source of debate. One of the main reasons for this controversy is room temperature sample preparation artifacts, which affect accurate determination of size, shape and agglomeration/aggregation of nanoscale iron particles. The present study is first to report the ultra-fine iron core structures of four IV iron complex formulations, sodium ferric gluconate, iron sucrose, low molecular weight iron dextran and ferumoxytol, using a cryogenic transmission electron microscopy (cryo-TEM) preservation technique, as opposed to the conventional room temperature (RT-TEM) technique. Our results show that room temperature preparation causes nanoparticle aggregation and deformation, while cryo-TEM preserves IV iron colloidal suspension in their native frozen-hydrated and undiluted state. In contrast to the current consensus in literature, all four IV iron colloids exhibit a similar morphology of their iron oxide cores with a spherical shape, narrow size distribution and an average size of 2nm. Moreover, out of the four tested formulations, ferumoxytol exhibits a cluster-like community of several iron carbohydrate particles which likely accounts for its large hydrodynamic size of 25nm, measured with dynamic light scattering. Our findings outline a suitable method for identifying colloidal nanoparticle core size in the native state, which is increasingly important for manufacturing and design control of complex drug formulations, such as IV iron drug products.

  9. A comprehensive approach to the determination of two benzimidazoles in environmental samples.

    Science.gov (United States)

    Wagil, Marta; Maszkowska, Joanna; Białk-Bielińska, Anna; Stepnowski, Piotr; Kumirska, Jolanta

    2015-01-01

    Among the various pharmaceuticals regarded as emerging pollutants, benzimidazoles--represented by flubendazole and fenbendazole--are of particular concern because of their large-scale use in veterinary medicine and their health effects on aquatic organisms. For this reason, it is essential to have reliable analytical methods which can be used to simultaneously monitor their appearance in environmental matrices such as water, sediment and tissue samples. To date, however, such methods relating to these three matrices have not been available. In this paper we present a comprehensive approach to the determination of both drugs in the mentioned above matrices using liquid chromatography-ion trap mass spectrometry (LC-MS/MS). Special attention was paid to the sample preparation step. The optimal extraction methods were further validated by experiments with spiked water, sediment and fish tissue samples. Matrix effects were established. The following absolute recoveries of flubendazole and fenbendazole were achieved: 96.2% and 95.4% from waters, 103.4% and 98.3% from sediments, and 98.3% and 97.6% from fish tissue samples, respectively. Validation of the LC-MS/MS methods enable flubendazole and fenbendazole to be determined with method detection limits: 1.6 ng L(-1) and 1.7 ng L(-1) in water samples; 0.3 ng g(-1) for both compounds in sediment samples, and 3.3 ng g(-1) and 3.5 ng g(-1) in tissue samples, respectively. The proposed methods were successfully used for analysing selected pharmaceuticals in real samples collected in northern Poland. There is first data on the concentration in the environment of the target compounds in Poland.

  10. Recent Mapping and Sampling on Chukchi Borderland and the Alpha/Mendeleev Ridge Complex

    Science.gov (United States)

    Mayer, L. A.; Brumley, K.; Andronikov, A.; Chayes, D. N.; Armstrong, A. A.; Calder, B.; Hall, J. K.; Clyde, W. C.; Bothner, W. A.; Gardner, J. V.

    2008-12-01

    Since 2003, four cruises on the icebreaker USCG HEALY have collected high-resolution multibeam sonar mapping data in the Amerasia Basin in support of a potential submission by the U.S. for an extended continental shelf as defined under the United Nations Convention on Law of the Sea Article 76. The latest of these cruises (HEALY0805), completed in early Sept.of 2008, extended this mapping to the southern portions of the Alpha/Mendeleev Ridge complex, and supplemented the mapping with seven dredge stations, providing rare, direct sampling of both regions. While sparse in comparison to complete-coverage multibeam sonar surveys (due to the difficulties associated with operating in ice-covered waters), the new multibeam sonar data still provide an unprecedented new view of the tectonic, sedimentary, glacial and fluid- flow related processes in the Arctic Ocean. The Chukchi Borderland is characterized by shallow plateaus that often show evidence of interaction with icebergs and glaciers (scours and grooves) at depths as great as 900 m, as well as the presence of numerous gas/fluid expulsion features (pockmarks and acoustic wipe-out zones). The topographic highs associated with the Borderland are often bounded by very steep scarps including the eastern edge of Northwind Ridge (the Northwind Escarpment) which is a 600 km long NNE trending feature with an average slope of 10-15 degrees. Similar steep-sided ridges, separated by deep linear valleys also appear in mapped areas of the Alpha/Mendeleev Ridge complex. Some of these features have slopes as great at 60 degrees and thus are excellent targets for dredging. Our dredging of these slopes has returned a wide array of volcanic and sedimentary rock types, many of which appear to be representative of outcrops (rather than ice rafted material). A preliminary shipboard examination of these samples (they were just collected this morning - 3 September 2008 - a few days before the abstract is due) shows them to include mudstone

  11. A fast algorithm for determining the linear complexity of a binary sequence with period 2npm

    Institute of Scientific and Technical Information of China (English)

    魏仕民; 肖国镇; 陈钟

    2001-01-01

    An efficient algorithm for determining the linear complexity and the minimal polynomial of a binary sequence with period 2npm is proposed and proved, where 2 is a primitive root modulo p2. The new algorithm generalizes the algorithm for computing the linear complexity of a binary sequence with period 2 n and the algorithm for computing the linear complexity of a binary sequence with period pn,where 2 is a primitive root modulo p2.

  12. Letter Report: Stable Hydrogen and Oxygen Isotope Analysis of B-Complex Perched Water Samples

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Brady D. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Moran, James J. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Nims, Megan K. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Saunders, Danielle L. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

    2017-04-13

    Fine-grained sediments associated with the Cold Creek Unit at Hanford have caused the formation of a perched water aquifer in the deep vadose zone at the B Complex area, which includes waste sites in the 200-DV-1 Operable Unit and the single-shell tank farms in Waste Management Area B-BX-BY. High levels of contaminants, such as uranium, technetium-99, and nitrate, make this aquifer a continuing source of contamination for the groundwater located a few meters below the perched zone. Analysis of deuterium (2H) and 18-oxygen (18O) of nine perched water samples from three different wells was performed. Samples represent time points from hydraulic tests performed on the perched aquifer using the three wells. The isotope analyses showed that the perched water had δ2H and δ18O ratios consistent with the regional meteoric water line, indicating that local precipitation events at the Hanford site likely account for recharge of the perched water aquifer. Data from the isotope analysis can be used along with pumping and recovery data to help understand the perched water dynamics related to aquifer size and hydraulic control of the aquifer in the future.

  13. Simulated Annealing-Extended Sampling for Multicomponent Decomposition of Spectral Data of DNA Complexed with Peptide

    Science.gov (United States)

    Kang, Jiyoung; Yamasaki, Kazuhiko; Sano, Kuniaki; Tsutsui, Ken; Tsutsui, Kimiko M.; Tateno, Masaru

    2017-01-01

    Theoretical analyses of multivariate data have become increasingly important in various scientific disciplines. The multivariate curve resolution alternating least-squares (MCR-ALS) method is an integrated and systematic tool to decompose such various types of spectral data to several pure spectra, corresponding to distinct species. However, in the present study, the MCR-ALS calculation provided only unreasonable solutions, when used to process the circular dichroism spectra of double-stranded DNA (228 bp) in the complex with a DNA-binding peptide under various concentrations. To resolve this problem, we developed an algorithm by including a simulated annealing (SA) protocol (the SA-MCR-ALS method), to facilitate the expansion of the sampling space. The analysis successfully decomposed the aforementioned data into three reasonable pure spectra. Thus, our SA-MCR-ALS scheme provides a useful tool for effective extended sampling, to investigate the substantial and detailed properties of various forms of multivariate data with significant difficulties in the degrees of freedom.

  14. Performance limitations of label-free sensors in molecular diagnosis using complex samples

    Science.gov (United States)

    Varma, Manoj

    2016-03-01

    Label-free biosensors promised a paradigm involving direct detection of biomarkers from complex samples such as serum without requiring multistep sample processing typical of labelled methods such as ELISA or immunofluorescence assays. Label-free sensors have witnessed decades of development with a veritable zoo of techniques available today exploiting a multitude of physical effects. It is appropriate now to critically assess whether label-free technologies have succeeded in delivering their promise with respect to diagnostic applications, particularly, ambitious goals such as early cancer detection using serum biomarkers, which require low limits of detection (LoD). Comparison of nearly 120 limits of detection (LoD) values reported by labelled and label-free sensing approaches over a wide range of detection techniques and target molecules in serum revealed that labeled techniques achieve 2-3 orders of magnitude better LoDs. Data from experiments where labelled and label-free assays were performed simultaneously using the same assay parameters also confirm that the LoD achieved by labelled techniques is 2 to 3 orders of magnitude better than that by label-free techniques. Furthermore, label-free techniques required significant signal amplification, for e.g. using nanoparticle conjugated secondary antibodies, to achieve LoDs comparable to labelled methods substantially deviating from the original "direct detection" paradigm. This finding has important implications on the practical limits of applying label-free detection methods for molecular diagnosis.

  15. Iterative Monte Carlo with bead-adapted sampling for complex-time correlation functions

    Science.gov (United States)

    Jadhao, Vikram; Makri, Nancy

    2010-03-01

    In a recent communication [V. Jadhao and N. Makri, J. Chem. Phys. 129, 161102 (2008)], we introduced an iterative Monte Carlo (IMC) path integral methodology for calculating complex-time correlation functions. This method constitutes a stepwise evaluation of the path integral on a grid selected by a Monte Carlo procedure, circumventing the exponential growth of statistical error with increasing propagation time, while realizing the advantageous scaling of importance sampling in the grid selection and integral evaluation. In the present paper, we present an improved formulation of IMC, which is based on a bead-adapted sampling procedure; thus leading to grid point distributions that closely resemble the absolute value of the integrand at each iteration. We show that the statistical error of IMC does not grow upon repeated iteration, in sharp contrast to the performance of the conventional path integral approach which leads to exponential increase in statistical uncertainty. Numerical results on systems with up to 13 degrees of freedom and propagation up to 30 times the "thermal" time ℏβ /2 illustrate these features.

  16. Development of active and diffusive sampling methods for determination of 3-methoxybutyl acetate in workplace air.

    Science.gov (United States)

    Takeuchi, Akito; Takigawa, Tomoko; Kawasumi, Yaeko; Yasugi, Tomojiro; Endo, Yoko; Wang, Da-Hong; Takaki, Jiro; Sakurai, Haruhiko; Ogino, Keiki

    2007-11-01

    Monitoring of the workplace concentration of 3-methoxybutyl acetate (MBA), which is used in printer's ink and thinner for screen-printing and as an organic solvent to dissolve various resins, is important for health reasons. An active and a diffusive sampling method, using a gas chromatograph equipped with a flame ionization detector, were developed for the determination of MBA in workplace air. For the active sampling method using an activated charcoal tube, the overall desorption efficiency was 101%, the overall recovery was 104%, and the recovery after 8 days of storage in a refrigerator was more than 90%. For the diffusive sampling method using the 3M 3500 organic vapor monitor, the MBA sampling rate was 19.89 cm(3) min(-1). The linear range was from 0.01 to 96.00 microg ml(-1), with a correlation coefficient of 0.999, and the detection limits of the active and diffusive samplers were 0.04 and 0.07 microg sample(-1), respectively. The geometric mean of stationary sampling and personal sampling in a screen-printing factory were 12.61 and 16.52 ppm, respectively, indicating that both methods can be used to measure MBA in workplace air.

  17. Dimensions and determinants of judgements of colour samples and a simulated interior space by architects and non-architects.

    Science.gov (United States)

    Hogg, J; Goodman, S; Porter, T; Mikellides, B; Preddy, D E

    1979-05-01

    Architects and non-architects made Semantic Differential ratings of colour samples (chips) and a simulated interior space (a model). In analyses of the total samples' ratings (architects and non-architects) of (a) colour chips and (b) models, and individual sample analyses, (c) architects' chip judgements, (d) architects' model judgements, (e) non-architects' chip judgements, and (f) non-architects' model judgements, five factors occurred, though not necessarily all in any one analysis. These were: (i) dynamism; (ii) spatial quality; (iii) emotional tone; (iv) evaluation; (v) complexity. Linear correlations between parameters of the Munsell Color System and the above factors in the various analyses were calculated, while parallel analyses were carried out employing a graphical technique described by Sivik (1974a) involving isosemantic maps. In all analyses, linear correlations between the colour parameters and judgements were found for the dynamism factor, spatial quality factor, and emotional tone factor. They were associated respectively with chroma, value, and hue. Inspection of the isosemantic maps indicated subsidiary effects of the non-dominant dimensions of a non-linear sort, though the maps also exhibited the linear relations. Linear correlations were low or non-existent for the evaluation and complexity factors, and the complex nature of their determinants was clear from the isosemantic maps. The dterminants of judgements were similar for architects and non-architects, with the exception of evaluative judgements for the models in which markedly different determinants were noted. Comparability of the present findings with other studies carried out in a variety of countries over a 20 year period was high for dynamism, spatial quality, and emotional tone, and it is suggested that there may be something inherent in the response to colour in relation to such judgements. Recent physiological work is discussed, and its limitations in terms of colours sampled and

  18. Determination of the Formation Constant of the Inclusion Complex from a Naphthoquinone

    Directory of Open Access Journals (Sweden)

    María M. de Bertorello

    2000-03-01

    Full Text Available Inclusion complexation of 1 with HP-β-CD or HP-β-CD:PVP K30 in aqueous solution was spectroscopically studied and the formation constant for a 1:1 complex was determined from these measurements.

  19. Liquid chromatographic determination of quinolones in water and human urine samples after microextraction by packed sorbent.

    Science.gov (United States)

    Rani, Susheela; Kumar, Ashwini; Malik, Ashok Kumar; Singh, Baldev

    2012-01-01

    A method for the simultaneous determination of quinolones in water and urine samples by microextraction in a sorbent-packed syringe (MEPS) with LC is described. MEPS is a new miniaturized SPE technique that can be used with chromatographic instruments without any modifications. In MEPS, approximately 1 mg of the solid packing material is inserted into a syringe (100-250 microL) as a plug. Sample preparation takes place on the packed bed. The new method is promising, easy to use, economical, and rapid. The determination of quinolones in groundwater and urine was performed using MEPS as a sample preparation method with LC-UV determination. Four quinolone antibiotics--enrofloxacin, enoxacin, danofloxacin, and nalidixic acid--in groundwater and urine samples were used as analytes. The extraction recovery was found to be between 64.9 and 98.9%. The results showed high correlation coefficients (R2 > 0.992) for all of the analytes within the calibration range. The LOQ was between 0.091 and 0.315 ng/mL.

  20. Potentiometric Determination of Chloride and Cyanide Ions in Nanoliter Samples with Capillary Indicating Electrodes

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    The samples of 25 nL of chloride and cyanide were determined with a kind of glass capillary indicating electrodes by potentiometry. Silver was deposited by the silver-mirror reaction on the inner surface of the glass capillary with a volume of 25 nL. The AgCl film and the AgI film were formed by the treatment of the capillary with a FeCl3 solution and further with a KI solution. The samples were collected automatically into the capillary by the capillary ascension. The procedure in the measurement was merely to place a reference electrode and a capillary indicating electrode vertically on a strip filter paper containing a 0.1 mol/L NaNO3 solution. The various i.d. of the capillary electrodes were used to determine samples ranging from 25 nL to dozens of microliters. The ranges of the linear response to chloride and cyanide were 3.2×10-4-2.2×10-1 mol/L and 1.0×10-5-1.0×10-1 mol/L with an average slope of 55.2 and 52-62 mV/decade, respectively. The samples with various concentrations of chloride and cyanide were determined, and the relative standard deviations were less than 7%.

  1. Determination of total magnesium in biological samples using electrothermal atomic absorption spectrometry

    Science.gov (United States)

    Hulanicki, Adam; Godlewska, Beata; Brzóska, Malgorzata

    1995-11-01

    Magnesium content is an important diagnostic parameter in medicine. It is recognized that its determination in one compartment is not sufficient for reliable information about the magnesium status in the body. In addition to the common procedures of magnesium determination in blood by flame atomic absorption spectrometry, the procedure of electrothermal atomization has also been developed and applied to the analysis of blood fractions, mononuclear cells and isolated nuclei of liver cells. Electrothermal atomization is preferred in cases where the sample size is limited and the magnesium content low. The total errors are in the order of 3-4%. Various techniques of sample pretreatment have been tested and direct dilution with 0.05 mol l -1 nitric acid was optimal when the samples were not mineralized. The calibration graph based on standards containing albumin was found to give the best results, as the form of magnesium in the samples may influence the ashing and atomization processes. Good agreement was obtained for determination of magnesium in standard serum. The results are compared with those obtained by the standard flame atomization technique.

  2. Determination of lead in rice grains by solid sampling HR-CS GFAAS.

    Science.gov (United States)

    Gunduz, Sema; Akman, Suleyman

    2013-12-01

    A study was performed for the determination of lead in rice grains directly by solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GFAAS) without digesting sample. The effects of sample amount, pyrolysis/atomization temperatures on the determination of lead in rice were investigated and optimized using a certificated rice flour. The lead concentrations were determined applying 800 °C of pyrolysis and 1800 °C of atomization temperatures without modifier. LOD (N=10, 3σ) and characteristic mass were 2.3 μg kg(-1) and 8.1 pg, respectively. The certified lead value of a rice flour CRM was found in its uncertainity limits. The lead contents of various rice samples obtained from markets in Turkey were between 0.009 and 0.162 mg kg(-1) which are in acceptable range. The average lead concentrations in various rice grains taken from the same package were significantly different from each other.

  3. Method of separate determination of high-ohmic sample resistance and contact resistance

    Directory of Open Access Journals (Sweden)

    Vadim A. Golubiatnikov

    2015-09-01

    Full Text Available A method of separate determination of two-pole sample volume resistance and contact resistance is suggested. The method is applicable to high-ohmic semiconductor samples: semi-insulating gallium arsenide, detector cadmium-zinc telluride (CZT, etc. The method is based on near-contact region illumination by monochromatic radiation of variable intensity from light emitting diodes with quantum energies exceeding the band gap of the material. It is necessary to obtain sample photo-current dependence upon light emitting diode current and to find the linear portion of this dependence. Extrapolation of this linear portion to the Y-axis gives the cut-off current. As the bias voltage is known, it is easy to calculate sample volume resistance. Then, using dark current value, one can determine the total contact resistance. The method was tested for n-type semi-insulating GaAs. The contact resistance value was shown to be approximately equal to the sample volume resistance. Thus, the influence of contacts must be taken into account when electrophysical data are analyzed.

  4. Development of a radioimmunoassay for the determination of buprenorphine in biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Debrabandere, L.; Boven, M. Van; Daenens, P. (Louvain Univ. (Belgium))

    1993-02-01

    The development of a specific and sensitive radioimmunoassay for the detection of buprenorphine in urine samples is described. With minor adjustments, the assay was also applied to the analysis for buprenorphine in plasma samples. The 2-diazobenzoic acid derivative of buprenorphine has been prepared as a hapten. The immunization of rabbits with the hapten-bovine serum albumin conjugate resulted in the production of antibodies, which cross-reacted with N-dealkylbuprenophine up to about the 90% level. The antibodies showed very low cross-reactivities with the 3-O-glucuronides and with the structural analogue etorphine. The assay was mainly used to prescreen for buprenorphine in urine samples of persons suspected of Temgesic misuse and to determine buprenorphine in plasma samples. A linear calibration graph for buprenorphine was obtained after logit-log regression. The spiking recovery study showed a linear regression. Intra-and inter-assay relative standard deviations were < 4.35 and < 6.36%, respectively. A comparison study of the high-performance liquid chromatographic determination (X) to the radioimmunoassay (Y) resulted in the following regression equation for the urine samples: Y = 1.44 + 1.64 X (n = 32; r 0.910) and Y = 0.007 + 1.58 X (n = 10; r = 0.930) for plasma specimens. The minimum detectable dose of the immunoassay was calculated to be 10 pg ml[sup -1] (Student's t-distribution, p 0.01, degrees of freedom = 8). (Author).

  5. Solid phase extraction and determination of carbamate pesticides in water samples by reverse-phase HPLC

    Energy Technology Data Exchange (ETDEWEB)

    Moreno-Tovar, J.; Santos-Delgado, M.J. [Departamento de Quimica Analitica, Facultad de ciencias Quimicas, Universidad Complutense de Madrid (Spain)

    1995-12-31

    Solid phase extraction. SPE. using C{sub 1}8 bonded silica cartridges for trace amounts determination of carbaryl, propoxur, thiram, propham and methiocarb in water samples was studied and the breakthrough volume of the cartridges was established. The high enrichment factor and large injection volume admissible in the isocratic reverse-phase HPLC system allows pesticides determination with UV detection at 22o nm even at a concentration lower than 0.05 mug/L. Purified tap natural and underground water samples were spiked with carbamate pesticides in the concentration range 0.16-16.0 mug/L. Large volumes of samples (up to 2L) were passed through available C{sub 1}8, cartridges and eluted with acetonitrile. The preconcentrated samples were analyzed by HPLC using a Spherisorb ODS column with a 42.58 acetonitrile-water mobile phase. From replicate samples, recovery for the pesticides ranged from 79.0 to 103.7% except for thiran which is not retained. Tehe relative standard deviation (n=4 at 0.16 to 1.61 mug/L concetration level) range from 1.1 to 6.8%. (Author) 14 refs.

  6. Determination of rhodamine B in soft drink, waste water and lipstick samples after solid phase extraction.

    Science.gov (United States)

    Soylak, Mustafa; Unsal, Yunus Emre; Yilmaz, Erkan; Tuzen, Mustafa

    2011-08-01

    A new solid phase extraction method is described for sensitive and selective determination of trace levels of rhodamine B in soft drink, food and industrial waste water samples. The method is based on the adsorption of rhodamine B on the Sepabeads SP 70 resin and its elution with 5 mL of acetonitrile in a mini chromatographic column. Rhodamine B was determined by using UV visible spectrophotometry at 556 nm. The effects of different parameters such as pH, amount of rhodamine B, flow rates of sample and eluent solutions, resin amount, and sample volume were investigated. The influences of some alkali, alkali earth and transition metals on the recoveries of rhodamine B were investigated. The preconcentration factor was found 40. The detection limit based on three times the standard deviation of the reagent blank for rhodamine B was 3.14 μg L⁻¹. The relative standard deviations of the procedure were found as 5% in 1×10⁻⁵ mol L⁻¹ rhodamine B. The presented procedure was successfully applied to real samples including soft drink, food and industrial waste water and lipstick samples. Copyright © 2011 Elsevier Ltd. All rights reserved.

  7. Microwave-assisted extraction and mild saponification for determination of organochlorine pesticides in oyster samples.

    Science.gov (United States)

    Carro, N; García, I; Ignacio, M-C; Llompart, M; Yebra, M-C; Mouteira, A

    2002-10-01

    A sample-preparation procedure (extraction and saponification) using microwave energy is proposed for determination of organochlorine pesticides in oyster samples. A Plackett-Burman factorial design has been used to optimize the microwave-assisted extraction and mild saponification on a freeze dried sample spiked with a mixture of aldrin, endrin, dieldrin, heptachlor, heptachorepoxide, isodrin, transnonachlor, p, p'-DDE, and p, p'-DDD. Six variables: solvent volume, extraction time, extraction temperature, amount of acetone (%) in the extractant solvent, amount of sample, and volume of NaOH solution were considered in the optimization process. The results show that the amount of sample is statistically significant for dieldrin, aldrin, p, p'-DDE, heptachlor, and transnonachlor and solvent volume for dieldrin, aldrin, and p, p'-DDE. The volume of NaOH solution is statistically significant for aldrin and p, p'-DDE only. Extraction temperature and extraction time seem to be the main factors determining the efficiency of extraction process for isodrin and p, p'-DDE, respectively. The optimized procedure was compared with conventional Soxhlet extraction.

  8. An approximate approach to sample size determination in bioequivalence testing with multiple pharmacokinetic responses.

    Science.gov (United States)

    Tsai, Chen-An; Huang, Chih-Yang; Liu, Jen-Pei

    2014-08-30

    The approval of generic drugs requires the evidence of average bioequivalence (ABE) on both the area under the concentration-time curve and the peak concentration Cmax . The bioequivalence (BE) hypothesis can be decomposed into the non-inferiority (NI) and non-superiority (NS) hypothesis. Most of regulatory agencies employ the two one-sided tests (TOST) procedure to test ABE between two formulations. As it is based on the intersection-union principle, the TOST procedure is conservative in terms of the type I error rate. However, the type II error rate is the sum of the type II error rates with respect to each null hypothesis of NI and NS hypotheses. When the difference in population means between two treatments is not 0, no close-form solution for the sample size for the BE hypothesis is available. Current methods provide the sample sizes with either insufficient power or unnecessarily excessive power. We suggest an approximate method for sample size determination, which can also provide the type II rate for each of NI and NS hypotheses. In addition, the proposed method is flexible to allow extension from one pharmacokinetic (PK) response to determination of the sample size required for multiple PK responses. We report the results of a numerical study. An R code is provided to calculate the sample size for BE testing based on the proposed methods.

  9. Determination of acrolein, ethanol, volatile acidity, and copper in different samples of sugarcane spirits

    Directory of Open Access Journals (Sweden)

    José Masson

    2012-09-01

    Full Text Available Seventy-one samples of sugarcane spirits from small and average size stills produced in the northern and southern Minas Gerais (Brazil were analyzed for acrolein using HPLC (High Performance Liquid Chromatography. Ethanol and copper concentrations and volatile acidity were also determined according to methods established by the Ministry of Agriculture, Livestock and Supply (MAPA. A total of 9.85% of the samples tested showed levels of acrolein above the legal limits, while the copper concentrations of 21.00% of the samples and the volatile acidity of 8.85% of the samples were higher than the limits established by the Brazilian legislation. The concentration of acrolein varied from 0 to 21.97 mg.100 mL-1 of ethanol. However, no significant difference at 5% of significance was observed between the samples produced in the northern and southern Minas Gerais. The method used for determination of acrolein in sugarcane spirits involved the formation of a derivative with 2,4-dinitrophenylhydrazine (2,4-DNPH and subsequent analysis by HPLC.

  10. System to determine present elements in oily samples; Sistema para determinar elementos presentes en muestras oleosas

    Energy Technology Data Exchange (ETDEWEB)

    Mendoza G, Y

    2004-11-01

    In the Chemistry Department of the National Institute of Nuclear Investigations of Mexico, dedicated to analyze samples of oleaginous material and of another origin, to determine the elements of the periodic table present in the samples, through the Neutron activation analysis technique (NAA). This technique has been developed to determine majority elements in any solid, aqueous, industrial and environmental sample, which consists basically on to irradiate a sample with neutrons coming from the TRIGA Mark III reactor and to carry out the analysis to obtain those gamma spectra that it emits, for finally to process the information, the quantification of the analysis it is carried out in a manual way, which requires to carry out a great quantity of calculations. The main objective of this project is the development of a software that allows to carry out the quantitative analysis of the NAA for the multielemental determination of samples in an automatic way. To fulfill the objective of this project it has been divided in four chapters: In the first chapter it is shortly presented the history on radioactivity and basic concepts that will allow us penetrate better to this work. In the second chapter the NAA is explained which is used in the sample analysis, the description of the process to be carried out, its are mentioned the characteristics of the used devices and an example of the process is illustrated. In the third chapter it is described the development of the algorithm and the selection of the programming language. The fourth chapter it is shown the structure of the system, the general form of operation, the execution of processes and the obtention of results. Later on the launched results are presented in the development of the present project. (Author)

  11. Practical approach to determine sample size for building logistic prediction models using high-throughput data.

    Science.gov (United States)

    Son, Dae-Soon; Lee, DongHyuk; Lee, Kyusang; Jung, Sin-Ho; Ahn, Taejin; Lee, Eunjin; Sohn, Insuk; Chung, Jongsuk; Park, Woongyang; Huh, Nam; Lee, Jae Won

    2015-02-01

    An empirical method of sample size determination for building prediction models was proposed recently. Permutation method which is used in this procedure is a commonly used method to address the problem of overfitting during cross-validation while evaluating the performance of prediction models constructed from microarray data. But major drawback of such methods which include bootstrapping and full permutations is prohibitively high cost of computation required for calculating the sample size. In this paper, we propose that a single representative null distribution can be used instead of a full permutation by using both simulated and real data sets. During simulation, we have used a dataset with zero effect size and confirmed that the empirical type I error approaches to 0.05. Hence this method can be confidently applied to reduce overfitting problem during cross-validation. We have observed that pilot data set generated by random sampling from real data could be successfully used for sample size determination. We present our results using an experiment that was repeated for 300 times while producing results comparable to that of full permutation method. Since we eliminate full permutation, sample size estimation time is not a function of pilot data size. In our experiment we have observed that this process takes around 30min. With the increasing number of clinical studies, developing efficient sample size determination methods for building prediction models is critical. But empirical methods using bootstrap and permutation usually involve high computing costs. In this study, we propose a method that can reduce required computing time drastically by using representative null distribution of permutations. We use data from pilot experiments to apply this method for designing clinical studies efficiently for high throughput data.

  12. New developments in the extraction and determination of parabens in cosmetics and environmental samples. A review

    Energy Technology Data Exchange (ETDEWEB)

    Ocaña-González, Juan Antonio; Villar-Navarro, Mercedes [Department of Analytical Chemistry, Faculty of Chemistry, Universidad de Sevilla, c/Prof. García González, s/n. 41012 Seville (Spain); Ramos-Payán, María [Department of Analytical Chemistry, Faculty of Chemistry, Universidad de Sevilla, c/Prof. García González, s/n. 41012 Seville (Spain); Department of Analytical Chemistry, Lineberguer Cancer Center, The University of North Carolina at Chapel Hill, NC (United States); Fernández-Torres, Rut [Department of Analytical Chemistry, Faculty of Chemistry, Universidad de Sevilla, c/Prof. García González, s/n. 41012 Seville (Spain); Research Centre of Health and Environment (CYSMA), University of Huelva (Spain); Bello-López, Miguel Angel, E-mail: mabello@us.es [Department of Analytical Chemistry, Faculty of Chemistry, Universidad de Sevilla, c/Prof. García González, s/n. 41012 Seville (Spain)

    2015-02-09

    Highlights: • The analysis of parabens in cosmetics and environmental samples is reviewed. • Literature in this field from 1980 to 2003 is briefly discussed. • Determination and extraction methods in the last decade are discussed in-depth. - Abstract: Parabens are a family of synthetic esters of p-hydroxibenzoic acid widely used as preservatives in cosmetics and health-care products, among other daily-use commodities. Recently, their potential endocrine disrupting effects have raised concerns about their safety and their potential effects as emerging pollutants, leading to the regulation of the presence of parabens in commercial products by national and trans-national organizations. Also, this has led to an interest in developing sensible and reliable methods for their determination in environmental samples, cosmetics and health-care products. This paper is a comprehensive up-to-date review of the literature concerning the determination of parabens in environmental samples and cosmetic and health-care products. A brief revision of the literature concerning the traditional determination of parabens (1980–2003) is included, followed by an in-depth revision of the recent developments in both measurement and extraction methods for parabens in the last years (2003–2013). Finally, possible future perspectives in this field are proposed.

  13. The interaction of taurine-salicylaldehyde Schiff base copper(II) complex with DNA and the determination of DNA using the complex as a fluorescence probe

    Science.gov (United States)

    Zhang, Xiaoyan; Wang, Yong; Zhang, Qianru; Yang, Zhousheng

    2010-09-01

    The interaction of taurine-salicylaldehyde Schiff base copper(II) (Cu(TSSB) 22+) complex with DNA was explored by using UV-vis, fluorescence spectrophotometry, and voltammetry. In pH 7.4 Tris-HCl buffer solution, the binding constant of the Cu(TSSB) 22+ complex interaction with DNA was 3.49 × 10 4 L mol -1. Moreover, due to the fluorescence enhancing of Cu(TSSB) 22+ complex in the presence of DNA, a method for determination of DNA with Cu(TSSB) 22+ complex as a fluorescence probe was developed. The fluorescence spectra indicated that the maximum excitation and emission wavelength were 389 nm and 512 nm, respectively. Under optimal conditions, the calibration graphs are linear over the range of 0.03-9.03 μg mL -1 for calf thymus DNA (CT-DNA), 0.10-36 μg mL -1 for yeast DNA and 0.01-10.01 μg mL -1 for salmon DNA (SM-DNA), respectively. The corresponding detection limits are 7 ng mL -1 for CT-DNA, 3 ng mL -1 for yeast DNA and 3 ng mL -1 for SM-DNA. Using this method, DNA in synthetic samples was determined with satisfactory results.

  14. Determining mutant spectra of three RNA viral samples using ultra-deep sequencing

    Energy Technology Data Exchange (ETDEWEB)

    Chen, H

    2012-06-06

    RNA viruses have extremely high mutation rates that enable the virus to adapt to new host environments and even jump from one species to another. As part of a viral transmission study, three viral samples collected from naturally infected animals were sequenced using Illumina paired-end technology at ultra-deep coverage. In order to determine the mutant spectra within the viral quasispecies, it is critical to understand the sequencing error rates and control for false positive calls of viral variants (point mutantations). I will estimate the sequencing error rate from two control sequences and characterize the mutant spectra in the natural samples with this error rate.

  15. XRF Determination of 17 Trace Elements in Geological Samples Using an Extended Compton Scattering Correction Procedure

    Institute of Scientific and Technical Information of China (English)

    丰梁垣; 鲍惠兰; 等

    1990-01-01

    This work is intended to explore a fast and effective apoproach to the determination of various trace elements in geological samples throuth improvement and simplification of the method developed by Reynolds (1963,1967),Absorption correction was made for the Fe content to eliminate the effect caused by inconsistency in mass absorption coefficients among the samples.A computer-aid regression analysis was performed on a number of standards of various compositions,which resulted in a set of calibration equations for directly converting X-ray intensities to concentrations.An analytical error of 10-30% was involved in the analyses of most elements.

  16. The Prevalence and Determinants of Breastfeeding Initiation and Duration in a Sample of Women in Ireland

    OpenAIRE

    Tarrant, Roslyn; Younger, Katherine; Sheridan-Pereira, Margaret; White, Martin; Kearney, John

    2010-01-01

    Objective: To assess breast-feeding initiation and prevalence from birth to 6 months in a sample of mothers in Dublin, and to determine the factors associated with breast-feeding initiation and ‘any’ breast-feeding at 6 weeks in a sample of Irish-national mothers. Design: This prospective cross-sectional study involved the recruitment of women during the antenatal period, with subsequent follow-up of mothers who delivered healthy, term singleton infants, at 6 weeks and 6 months postpartum. Se...

  17. Determination of burial dose in incompletely bleached fluvial samples using single grains of quartz

    DEFF Research Database (Denmark)

    Thomsen, Kristina Jørkov; Murray, A.S.; Bøtter-Jensen, Lars

    2007-01-01

    We determine the burial dose in three known-age incompletely bleached fluvial samples using single grains of quartz. Estimation of burial dose in incompletely bleached samples requires that the characteristics of the well-bleached part of the distribution are known in order to distinguish between...... well-bleached and poorly bleached grains. It is especially important to investigate if the uncertainties assigned to individual estimates of dose adequately describe the observed variability in well-bleached dose distributions. We investigate this by quantifying the overdispersion in laboratory...

  18. Mercury speciation and total trace element determination of low-biomass biological samples.

    Science.gov (United States)

    Taylor, Vivien F; Jackson, Brian P; Chen, Celia Y

    2008-12-01

    Current approaches to mercury speciation and total trace element analysis require separate extraction/digestions of the sample. Ecologically important aquatic organisms--notably primary consumers such as zooplankton, polychaetes and amphipods--usually yield very low biomass for analysis, even with significant compositing of multiple organisms. Individual organisms in the lower aquatic food chains (mussels, snails, oysters, silversides, killifish) can also have very low sample mass, and analysis of whole single organisms is important to metal uptake studies. A method for the determination of both methyl Hg and total heavy metal concentrations (Zn, As, Se, Cd, Hg, Pb) in a single, low-mass sample of aquatic organisms was developed. Samples (2 to 50 mg) were spiked with enriched with (201)MeHg and (199)Hg, then leached in 4 M HNO(3) at 55 degrees C for extraction of MeHg. After 16 h, an aliquot (0.05 mL) was removed to determine mercury species (methyl and inorganic Hg) by isotope dilution gas chromatography inductively coupled plasma mass spectrometry (ICP-MS). The leachate was then acidified to 9 M HNO(3) and digested in a microwave at 150 degrees C for 10 min, and total metal concentrations were determined by collision cell ICP-MS. The method was validated by analyzing five biological certified reference materials. Average percent recoveries for Zn, As, Se, Cd, MeHg, Hg(total) and Pb were 99.9%, 103.5%, 100.4%, 103.3%, 101%, 97.7%, and 97.1%, respectively. The correlation between the sum of MeHg and inorganic Hg from the speciation analysis and total Hg by conventional digestion of the sample was determined for a large sample set of aquatic invertebrates (n = 285). Excellent agreement between the two measured values was achieved. This method is advantageous in situations where sample size is limited, and where correlations between Hg species and other metals are required in the same sample. The method also provides further validation of speciation data, by

  19. Methods of liquid phase microextraction for the determination of cadmium in environmental samples.

    Science.gov (United States)

    Pires Santos, Analú; das Graças Andrade Korn, Maria; Azevedo Lemos, Valfredo

    2017-08-09

    Liquid phase microextraction (LPME) has been widely used in extraction and preconcentration systems as an excellent alternative to conventional liquid phase extraction. In this work, a critical review is presented on liquid phase microextraction techniques used in the determination of cadmium in environmental samples. LPME techniques are classified into three main groups: single-drop liquid phase microextraction (SDME), hollow fiber liquid phase microextraction (HF-LPME), and dispersive liquid-liquid microextraction (DLLME). Methods involving these liquid phase microextraction techniques are described, addressing advantages and disadvantages, samples, figures of merit, and trends.

  20. Short communication: appropriate and alternative methods to determine viable bacterial counts in cow milk samples.

    Science.gov (United States)

    Loss, G; Apprich, S; Kneifel, W; von Mutius, E; Genuneit, J; Braun-Fahrländer, C

    2012-06-01

    Farm milk consumption is reported to be inversely related to the development of asthma and atopy in children and it has been hypothesized that microorganisms in milk might contribute to this protective effect. The GABRIEL study was designed to investigate this hypothesis in a large population of European children, calling for a rapid alternative to classical culture techniques to determine bacteriological properties of milk samples. One objective was to evaluate 2 different rapid methods to determine bacteriological properties in a large number of cow milk samples collected under field conditions. BactoScan (Foss Analytical, Hillerød, Denmark), an automated standard flow cytometric method utilized for routine testing of milk quality, and TEMPO (bioMérieux, Marcy l'Etoile, France), an automated most-probable-number method, were used to assess the total viable bacterial count in farm and commercial milk samples. Both methods were compared with standard plate count method and each other. Measurements based on the TEMPO method were in good agreement with the standard plate count method and showed reliable results, whereas BactoScan results did not correlate with standard plate count measurements and yielded higher bacteria counts in heat-treated milk samples compared with raw milk samples. Most likely, these discrepant results were due to inferences with staining reactions and detection of bacteria in heat-treated milk samples. We conclude that, in contrast to the routinely used BactoScan method, the TEMPO method is an inexpensive and rapid alternative to standard culture methods suitable to assess total bacterial counts in processed and raw milk samples.

  1. Cloud point extraction for the preconcentration of silver and palladium in real samples and determination by atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Tavallali, Hossein; Yazdandoust, Saeed; Yazdandoust, Mozhdeh [Department of Chemistry, Payame Noor University (PNU), Shiraz (Iran)

    2010-03-15

    A cloud point extraction procedure is presented for the preconcentration and simultaneous determination of Ag{sup +} and Pd{sup 2+} in various samples. After complexation with 2-((2-((1H-benzo[d]imidazole-2-yl)methoxy)phenoxy)methyl)-1H-benzo[d]imidazol (BIMPI), which was used as a new chelating agent, analyte ions were quantitatively extracted to a phase rich in Triton X-114 following centrifugation, and determination was carried out by flame atomic absorption spectrometry (FAAS). Under the optimum experimental conditions (i. e., pH = 7.0, 15.0.10{sup -5} mol/L BIMPI and 0.036% (w/v) Triton X-114), calibration graphs were linear in the range of 28.0-430.0 {mu}g/L and 57.0-720.0 {mu}g/L with detection limits of 10.0 and 25.0 {mu}g/L for Ag{sup +} and Pd{sup 2+}, respectively. The enrichment factors were 35.0 and 28.0 for Ag{sup +} and Pd{sup 2+}, respectively. The method has been successfully applied to evaluate these metals in some real samples, including waste water, soil and hydrogenation catalyst samples. (Abstract Copyright [2010], Wiley Periodicals, Inc.)

  2. Dispersive Liquid-Liquid Microextraction of Bismuth in Various Samples and Determination by Flame Atomic Absorption Spectrometry

    Directory of Open Access Journals (Sweden)

    Teslima Daşbaşı

    2016-01-01

    Full Text Available A dispersive liquid-liquid microextraction method for the determination of bismuth in various samples by flame atomic absorption spectrometry is described. In this method, crystal violet was used as counter positive ion for BiCl4- complex ion, chloroform as extraction solvent, and ethanol as disperser solvent. The analytical parameters that may affect the extraction efficiency like acidity of sample, type and amount of extraction and disperser solvents, amount of ligand, and extraction time were studied in detail. The effect of interfering ions on the analyte recovery was also investigated. The calibration graph was linear in the range of 0.040–1.00 mg L−1 with detection limit of 4.0 μg L−1 (n=13. The precision as relative standard deviation was 3% (n=11, 0.20 mg L−1 and the enrichment factor was 74. The developed method was applied successfully for the determination of bismuth in various water, pharmaceutical, and cosmetic samples and the certified reference material (TMDA-64 lake water.

  3. Preconcentration and Determination of Trace Amounts of Heavy Metals in Water Samples Using Membrane Disk and Flame Atomic Absorption Spectrometry

    Institute of Scientific and Technical Information of China (English)

    ALI,Moghimi

    2007-01-01

    A fast and simple method for preconcentration of Ni2+, Cd2+, Pb2+, Zn2+, Cu2+ and Co2+ from natural water samples was developed. The metal ions were complexed with sodium diethyldithiocarbamate (Na-DDTC), then adsorbed onto octadecyl silica membrane disk, recovered and determined by FAAS. Extraction efficiency, influence of sample volume and eluent flow rates, effects of pH, amount of Na-DDTC, nature and amount of eluent for elution of metal ions from membrane disk, break through volume and limit of detection have been evaluated. The effect of foreign ions on the percent recovery of heavy metal ions has also been studied. The limit of detection of the proposed method for Ni2+, Cd2+, Pb2+, Zn2+, Cu2+ and Co2+was found to be 2.03, 0.47, 3.13, 0.44, 1.24 and 2.05ng·mL-1, respectively. The proposed (DDTC) method has been successfully applied to the recovery and determination of heavy metal ions in different water samples.

  4. Determination of arsenic and cadmium in crude oil by direct sampling graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Jesus, Alexandre de; Zmozinski, Ariane Vanessa [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970 Porto Alegre, RS (Brazil); Damin, Isabel Cristina Ferreira [Faculdade Dom Bosco de Porto Alegre, 90520-280, Porto Alegre, RS (Brazil); Silva, Marcia Messias, E-mail: mmsilva@iq.ufrgs.br [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciencia e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Vale, Maria Goreti Rodrigues [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciencia e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil)

    2012-05-15

    In this work, a direct sampling graphite furnace atomic absorption spectrometry method has been developed for the determination of arsenic and cadmium in crude oil samples. The samples were weighed directly on the solid sampling platforms and introduced into the graphite tube for analysis. The chemical modifier used for both analytes was a mixture of 0.1% Pd + 0.06% Mg + 0.06% Triton X-100. Pyrolysis and atomization curves were obtained for both analytes using standards and samples. Calibration curves with aqueous standards could be used for both analytes. The limits of detection obtained were 5.1 {mu}g kg{sup -1} for arsenic and 0.2 {mu}g kg{sup -1} for cadmium, calculated for the maximum amount of sample that can be analyzed (8 mg and 10 mg) for arsenic and cadmium, respectively. Relative standard deviations lower than 20% were obtained. For validation purposes, a calibration curve was constructed with the SRM 1634c and aqueous standards for arsenic and the results obtained for several crude oil samples were in agreement according to paired t-test. The result obtained for the determination of arsenic in the SRM against aqueous standards was also in agreement with the certificate value. As there is no crude oil or similar reference material available with a certified value for cadmium, a digestion in an open vessel under reflux using a 'cold finger' was adopted for validation purposes. The use of paired t-test showed that the results obtained by direct sampling and digestion were in agreement at a 95% confidence level. Recovery tests were carried out with inorganic and organic standards and the results were between 88% and 109%. The proposed method is simple, fast and reliable, being appropriated for routine analysis. - Highlights: Black-Right-Pointing-Pointer A direct sampling GF AAS method to determine As and Cd in crude oil was proposed. Black-Right-Pointing-Pointer The conventional chemical modifier Pd/Mg has been used to stabilize As and Cd. Black

  5. Determination of the complex linear electro-optic coefficient of GaAs and InP

    Energy Technology Data Exchange (ETDEWEB)

    Pristovsek, Markus [Technische Universitaet Berlin, Institut fuer Festkoerperphysik, Hardenbergstrasse 36, 10623 Berlin (Germany)

    2010-08-15

    The complex linear electro-optic coefficient d{sub 41} was determined for the first time above the fundamental band gap of GaAs and InP by measuring the doping induced band bending of several oxidized samples in reflectance anisotropy spectroscopy. From the real and imaginary part of the change of the spectra for different carrier concentrations the spectral change of d{sub 41} was calculated. This is the first determination of the imaginary part Im(d{sub 41}). (Abstract Copyright [2010], Wiley Periodicals, Inc.)

  6. Cloud point extraction for the determination of copper in environmental samples by flame atomic absorption spectrometry

    Directory of Open Access Journals (Sweden)

    Ardeshir Shokrollahi

    2008-01-01

    Full Text Available A simple cloud point extraction procedure is presented for the preconcentration of copper in various samples. After complexation by 4-hydroxy-2-mercapto-6-propylpyrimidine (PTU, copper ions are quantitatively extracted into the phase rich in Triton X-114 after centrifugation. Methanol acidified with 0.5 mol L-1 HNO3 was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS. Analytical parameters including concentrations for PTU, Triton X-114 and HNO3, bath temperature, centrifugation rate and time were optimized. The influences of the matrix ions on the recoveries of copper ions were investigated. The detection limits (3SDb/m, n=4 of 1.6 ng mL-1 along with enrichment factors of 30 for Cu were achieved. The proposed procedure was applied to the analysis of environmental samples.

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

    Science.gov (United States)

    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.

  8. A margin based approach to determining sample sizes via tolerance bounds.

    Energy Technology Data Exchange (ETDEWEB)

    Newcomer, Justin T.; Freeland, Katherine Elizabeth

    2013-09-01

    This paper proposes a tolerance bound approach for determining sample sizes. With this new methodology we begin to think of sample size in the context of uncertainty exceeding margin. As the sample size decreases the uncertainty in the estimate of margin increases. This can be problematic when the margin is small and only a few units are available for testing. In this case there may be a true underlying positive margin to requirements but the uncertainty may be too large to conclude we have sufficient margin to those requirements with a high level of statistical confidence. Therefore, we provide a methodology for choosing a sample size large enough such that an estimated QMU uncertainty based on the tolerance bound approach will be smaller than the estimated margin (assuming there is positive margin). This ensures that the estimated tolerance bound will be within performance requirements and the tolerance ratio will be greater than one, supporting a conclusion that we have sufficient margin to the performance requirements. In addition, this paper explores the relationship between margin, uncertainty, and sample size and provides an approach and recommendations for quantifying risk when sample sizes are limited.

  9. A new approach to determining cholinesterase activities in samples of whole blood.

    Science.gov (United States)

    Augustinsson, K B; Eriksson, H; Faijersson, Y

    1978-10-16

    A sensitive method, especially suitable for clinical laboratories, for the routine determination of cholinesterase activities in whole blood is presented. This method is based on the hydrolysis of propionylthiocholine and the spectrophotometric determination of the thiocholine produced by reaction with 4,4'-dithiodipyridine. The reaction product 4-thiopyridone has an absorption maximum at 324 nm, so that measurement in the presence of hemoglobin is possible. Propionylthiocholine is used at the substrate for both plasma butyrylcholinesterase and erythrocyte acetylcholinesterase. These two enzymes, in the relative amounts at which they are present in human blood, split this ester at about the same rate. Consequently, a first determination gives the total activity of which each individual activity is about 50%. A second determination in the presence of a selective inhibitor ("Astra 1397") for plasma butyrylcholinesterase gives the activity of the erythrocyte acetylcholinesterase. The difference between the two values represents the activity of the plasma enzyme. The validity of the method and the reliability of the results were checked with each blood sample in two ways: (1) by determining the activities of whole blood with an earlier gasometric technique which uses blood sample dried on filter paper; and (2) by measuring the activities in separated plasma and erythrocyte hemolysate eith propionylthiocholine as the substrate.

  10. A Kinetic Spectrophotometric Method for the Determination of Iron (Ⅲ) in Water Samples

    Institute of Scientific and Technical Information of China (English)

    JI Hongwei; XU Jian; XIN Huizhen; YANG Xiaoman

    2008-01-01

    A new kinetic spectrophotometric method has been developed for the determination of iron (Ⅲ). The method is based on the catalytic effect of iron (Ⅲ) on the oxidation of weak acid brilliant blue dye (RAWL) by KIO4 in acid medium. The advantages of the proposed method are that it is sensitive, accurate, rapid, inexpensive, can be operated under room temperature and has a large determination concentration range compared to other techniques. The obtained optimum conditions are: pH 3.15, RAWL (200 mgL-1) 5.00mL, Potassium periodate solution (0.01 molL-1) 0.30mL, phenanthroline (0.02molL-1) 1.00mL, reaction temperature 25℃ and reaction time 7 miu. With this method iron could quantitively be determined in the range 0.00-0.02 mgL-1, the detection limit being 4.10×10-10mL-1. The relative standard deviations (RSD) in five replicate determinations for 3 μgL-1 and 5μgL-1 iron (Ⅲ) are 3.1% and 1.9%, respectively. The method has been applied to the determination of iron (Ⅲ) in tap water samples and seawater samples (from the South China Sea), the recovery rates being 98.0% and 100.5%, respectively.

  11. Determination of Trace Copper (Ⅱ) in Water Samples by Kinetic-spectrophotometry

    Institute of Scientific and Technical Information of China (English)

    QI Yanxia; JI Hongwei; XIN Huizhen; LIU Li

    2007-01-01

    A new kinetic-spectrophotometric method is proposed for the determination of copper ( Ⅱ ). The method is based on the catalytic effect of copper ( Ⅱ ) on the oxidation of weak acid brilliant blue dye (RAWL) by hydrogen peroxide. The copper ( Ⅱ ) can be determined spectrophotometrically by measuring the decrease of absorbance of RAWL at λ = 626 nm using the fix-time method. The optimum reaction conditions are as follows: pH 7.20, buffer solution NaOH-KH2PO4, RAWL (200 mgL-1) 5.00 mL, H2O2 (30%) 0.50 mL, reaction temperature 80 ℃ and reaction time 20 min. The linear range of this method is between 0 μg L-1 and 12 μg L-1 and the limit of detection is 0.011 μg L-1, the relative standard deviation (RSD) in five replicate determinations for 2 and 8 μg L-1 copper ( Ⅱ ) are 3.2% and 2.3%, respectively. Twenty ions do not interfere in the determination of copper ( Ⅱ ). The method has been applied satisfactorily to the determination of copper ( Ⅱ ) in freshwater samples (tap water and Yellow River water from Lijin, Shandong, China) and seawater samples (from the South China Sea), the recovery rates are 98.0%, 102.5% and 96.0%, respectively.

  12. A review on determination of steroids in biological samples exploiting nanobio-electroanalytical methods.

    Science.gov (United States)

    Yadav, Saurabh K; Chandra, Pranjal; Goyal, Rajendra N; Shim, Yoon-Bo

    2013-01-31

    The applications of nanomaterial modified sensors, molecularly imprinting polymer based, aptamer based, and immunosensors have been described in the determination of steroids using electroanalytical techniques. After a brief description of the steroids and assays in biological fluids, the principles of electrochemical detection with the advantages and the limitations of the various sensors are presented. The nanomaterial modified sensors catalyze the oxidation/reduction of steroids and are suitable for sensing them in environmental samples and biological fluids. The determination of steroids based on their reduction has been found more useful in comparison to oxidation as the common metabolites present in the biological fluids do not undergo reduction in the usual potential window and hence, do not interfere in the determination. The sensors based on immunosensors and aptamers were found more sensitive and selective for steroid determination. Conducting polymer modified bio-sensors and microchip devices are suggested as possible future prospects for the ultra sensitive and simultaneous determination of steroids and their metabolites in various samples.

  13. Determination of uranium isotopes in environmental samples by anion exchange in sulfuric and hydrochloric acid media.

    Science.gov (United States)

    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.

  14. Anodic stripping voltammetric determination of Zn, Pb and Cu traces in whisky samples

    Energy Technology Data Exchange (ETDEWEB)

    Barbeira, P.J.S. [Departamento de Quimica - ICEx - UFMG, Belo Horizonte, MG (Brazil); Stradiotto, N.R. [Departamento de Quimica - FFCLRP - USP, Ribeirao Preto, SP (Brazil)

    1998-07-01

    The simultaneous ``in natura`` determination of trace Zn, Pb and Cu in whisky samples by anodic stripping voltammetry (ASV), using a hanging mercury drop electrode, without previous treatment or addition of supporting electrolyte is described. The choice of an appropriate stripping voltammetric method and deposition potential minimizes the influence of the organic content and ensures a good reproducibility of the measurements. The reliability of the method was tested comparing the results with those of atomic absorption spectroscopy (AAS), with differences of about 10%. The method allows the determination of heavy metal ions in the {mu}g L{sup -1} range. (orig.) With 3 figs., 1 tab., 18 refs.

  15. Simultaneous Voltammetric Determination of Three Herbicides in Food and Water Samples with the Aid of Chemometrics

    Institute of Scientific and Technical Information of China (English)

    NI Yong-nian; WANG Lin; KOKOT Serge

    2009-01-01

    Differential pulse stripping voltammetry method(DPSV) was applied to the determination of three herbicides,ametryn,cyanatryn,and dimethametryn.It was found that their voltammograms overlapped strongly,and it is difficult to determine these compounds individually from their mixtures.With the aid of chemometrics,classical least squares(CLS),principal component regression(PCR) and partial least squares(PLS),voltammogram resolution and quantitative analysis of the synthetic mixtures of the three compounds were successfully performed.The proposed method was also applied to the analysis of some real samples with satisfactory results.

  16. Accelerator Mass Spectrometric determination of radiocarbon in stratospheric CO2, retrieved from AirCore sampling.

    Science.gov (United States)

    Paul, Dipayan; Been, Henk A.; Chen, Huilin; Kivi, Rigel; Meijer, Harro A. J.

    2015-04-01

    In this decade, understanding the impact of human activities on climate is one of the key issues of discussion globally. The continuous rise in the concentration of greenhouse gases, e.g., CO2, CH4, etc. in the atmosphere, predominantly due to human activities, is alarming and requires continuous monitoring to understand the dynamics. Radiocarbon is an important atmospheric tracer and one of the many used in the understanding of the global carbon budget, which includes the greenhouse gases like CO2 and CH4. Measurement of 14C (or radiocarbon) in atmospheric CO2 generally requires collection of large air samples (few liters) from which CO2 is extracted and then the concentration of radiocarbon is determined. Currently, Accelerator Mass Spectrometry (AMS) is the most precise, reliable and widely used technique for atmospheric radiocarbon detection. However, the regular collection of air samples from troposphere and stratosphere, for example using aircraft, is prohibitively expensive. AirCore is an innovative atmospheric sampling system, developed by NOAA. It comprises of a long tube descending from a high altitude with one end open and the other closed, and has been demonstrated to be a reliable, cost-effective sampling system for high-altitude profile (up to ~ 30 km) measurements of CH4and CO2(Karion et al. 2010). In Europe, AirCore measurements are being performed on a regular basis near Sodankylä since September 2013. Here we describe the analysis of two such AirCore samples collected in July 2014, Finland, for determining the 14C concentration in stratospheric CO2. The two AirCore samples were collected on consecutive days. Each stratospheric AirCore sample was divided into six fractions, each containing ~ 35 μg CO2 (~9.5 μg C). Each fraction was separately trapped in 1 /4 inch coiled stainless steel tubing for radiocarbon measurements. The procedure for CO2 extraction from the stratospheric air samples; the sample preparation, with samples containing < 10

  17. Aluminium sensitized spectrofluorimetric determination of fluoroquinolones in milk samples coupled with salting-out assisted liquid-liquid ultrasonic extraction

    Science.gov (United States)

    Xia, Qinghai; Yang, Yaling; Liu, Mousheng

    2012-10-01

    An aluminium sensitized spectrofluorimetric method coupled with salting-out assisted liquid-liquid ultrasonic extraction for the determination of four widely used fluoroquinolones (FQs) namely norfloxacin (NOR), ofloxacin (OFL), ciprofloxacin (CIP) and gatifloxacin (GAT) in bovine raw milk was described. The analytical procedure involves the fluorescence sensitization of aluminium (Al3+) by complexation with FQs, salting-out assisted liquid-liquid ultrasonic extraction (SALLUE), followed by spectrofluorometry. The influence of several parameters on the extraction (the salt species, the amount of salt, pH, temperature and phase volume ratio) was investigated. Under optimized experimental conditions, the detection limits of the method in milk varied from 0.009 μg/mL for NOR to 0.016 μg/mL for GAT (signal-to-noise ratio (S/N) = 3). The relative standard deviations (RSD) values were found to be relatively low (0.54-2.48% for four compounds). The calibration graph was linear from 0.015 to 2.25 μg/mL with coefficient of determinations not less than 0.9974. The methodology developed was applied to the determination of FQs in bovine raw milk samples. The main advantage of this method is simple, accurate and green. The method showed promising applications for analyzing polar analytes especially polar drugs in various sample matrices.

  18. Determination of trace nickel in water samples by cloud point extraction preconcentration coupled with graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Sun Zhimei [Key Laboratory of Pesticide and Chemical Biology of Ministry of Education, College of Chemistry, Central China Normal University, Wuhan 430079 (China); Department of Chemistry and Biology, Huainan Normal University, Huainan 232001 (China); Liang Pei [Key Laboratory of Pesticide and Chemical Biology of Ministry of Education, College of Chemistry, Central China Normal University, Wuhan 430079 (China)]. E-mail: liangpei@mail.ccnu.edu.cn; Ding Qiong [Key Laboratory of Pesticide and Chemical Biology of Ministry of Education, College of Chemistry, Central China Normal University, Wuhan 430079 (China); Cao Jing [Key Laboratory of Pesticide and Chemical Biology of Ministry of Education, College of Chemistry, Central China Normal University, Wuhan 430079 (China)

    2006-09-21

    A new method based on the cloud point extraction (CPE) preconcentration and graphite furnace atomic absorption spectrometry (GFAAS) detection was proposed for the determination of trace nickel in water samples. When the micelle solution temperature is higher than the cloud point of surfactant p-octylpolyethyleneglycolphenyether (Triton X-100), the complex of Ni{sup 2+} with 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP) could enter surfactant-rich phase and be concentrated, then determined by GFAAS. The main factors affecting the cloud point extraction were investigated in detail. An enrichment factor of 27 was obtained for the preconcentration of Ni{sup 2+} with 10 mL solution. Under the optimal conditions, the detection limit of Ni{sup 2+} is 0.12 ng mL{sup -1} with R.S.D. of 4.3% (n = 10, c = 100 ng mL{sup -1}). The proposed method was applied to determination of trace nickel in water samples with satisfactory results.

  19. A screen-printed, amperometric biosensor for the determination of organophosphorus pesticides in water samples

    Institute of Scientific and Technical Information of China (English)

    Junfeng Dou; Fuqiang Fan; Aizhong Ding; Lirong Cheng; Raju Sekar; Hongting Wang; Shuairan Li

    2012-01-01

    An amperometric biosensor based on screen-printed electrodes (SPEs) was developed for the determination of organophosphorus pesticides in water samples.The extent of acetylcholinesterase (AChE) deactivation was determined and quantified for pesticideconcentrations in water samples.An enzyme immobilization adsorption procedure and polyacrylamide gel matrix polymerization were used for fabrication of the biosensor,with minimal losses in enzyme activity.The optimal conditions for enzyme catalytic reaction on the SPEs surfaces were acetylthiocholine chloride (ATChC(1)) concentration of 5 mmol/L,pH 7 and reaction time of 4 min.The detectionlimits for three organophosphorus pesticides (dichlorvos,monocrotophs and parathion) were in the range of 4 to 7 μg/L when an AChE amount of 0.1 U was used for immobilization.

  20. Determination of continuous system transfer functions from sampled pulse response data

    Science.gov (United States)

    Jordan, Jay B.; Watkins, Wendell R.; Palacios, Fernando R.; Billingsley, Daniel R.

    1994-12-01

    A method for determining the transfer function of a continuous system from sampled responses to single- and multiple-pulse excitation is presented. The method is an extension of the sampled-edge-response method pioneered by the theoretical work of A. Papoulis in 1962 and the application of the theory to optical systems by B. Tatian in 1965. Occasions arise when pulse rather than step-function stimuli are available for system excitations. In such cases, the method presented is useful for determining the system transfer function. The use of antialiasing filters and estimation of non-bandwidth-limited transfer functions are discussed. Practical application of the method to characterizing the system transfer function of a commercial 8- to 12-micrometers infrared imager is also presented.

  1. Examination of histological samples from submerged carrion to aid in the determination of postmortem submersion interval.

    Science.gov (United States)

    Humphreys, Michael Keith; Panacek, Edward; Green, William; Albers, Elizabeth

    2013-03-01

    The use of histology in the as a tool for estimating postmortem intervals has rarely been explored but it has the potential for offering medical examiners an additional means for estimating the postmortem submersion interval (PMSI) during a death investigation. This study used perinatal piglets as human analogs which were submerged in freshwater for various time intervals. Each piglet was extracted from the water and underwent a necropsy examination during which histological samples were collected. The samples revealed that the necrotic tissue decomposed relatively predictably over time and that this decompositional progression may have the potential to be used via a scoring system to determine or aid in determining the PMSI. This method for calculating PMSI allows for normalization between piglets of various mass and body types. It also prevents any contamination of the remains via algae growth and animal activity that may exacerbate and possibly exaggerate PMSI calculation.

  2. Differential Pulse Voltammetric Determination of Fulvestrant in Pharmaceutical Dosage Forms and Serum Samples

    Directory of Open Access Journals (Sweden)

    Dilek Kul

    2011-01-01

    Full Text Available The electrooxidation behavior and determination of fulvestrant at a glassy carbon electrode were investigated. The voltammetric study of the model compounds allowed elucidating the possible oxidation mechanism of fulvestrant. The dependence of the peak current and peak potentials on pH, concentration, nature of the buffer, and scan rate was determined. The oxidation of fulvestrant showed a single and irreversible peak at glassy carbon electrode, and the process was found diffusion controlled. Linear responses were obtained for the concentrations between 4×10−6 M and 6×10−5 M in standard samples and between 2×10−5 M and 1×10−4 M in serum samples. The repeatability of the method was found 0.93 RSD%. The repeatability, reproducibility, precision, and accuracy of proposed method were investigated.

  3. Cloud point extraction, preconcentration and spectrophotometric determination of nickel in water samples using dimethylglyoxime

    Directory of Open Access Journals (Sweden)

    Morteza Bahram

    2013-01-01

    Full Text Available A new and simple method for the preconcentration and spectrophotometric determination of trace amounts of nickel was developed by cloud point extraction (CPE. In the proposed work, dimethylglyoxime (DMG was used as the chelating agent and Triton X-114 was selected as a non-ionic surfactant for CPE. The parameters affecting the cloud point extraction including the pH of sample solution, concentration of the chelating agent and surfactant, equilibration temperature and time were optimized. Under the optimum conditions, the calibration graph was linear in the range of 10-150 ng mL-1 with a detection limit of 4 ng mL-1. The relative standard deviation for 9 replicates of 100 ng mL-1 Ni(II was 1.04%. The interference effect of some anions and cations was studied. The method was applied to the determination of Ni(II in water samples with satisfactory results.

  4. Osteryoung square wave voltammetric determination of lactose in food samples by a derivative procedure

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    A method for determination of lactose in food samples by Osteryoung square wave voltammetry (OSWV) was developed. It was based on the nucleophilic addition reaction between lactose and aqua ammonia. The carbonyl group of lactose can be changed into imido group, and this increases the electrochemical activity in reduction and the sensitivity. The optimal condition for the nucleophilic addition reaction was investigated and it was found that in NH4Cl-NH3 buffer of pH 10.1, the linear range between the peak current and the concentration of lactose was 0.6-8.4 mg L-1, and the detection limits was 0.44 mg L-1. The proposed method was applied to the "determination of lactose in food samples and satisfactory results were obtained.

  5. Analytical Methodologies for the Determination of Endocrine Disrupting Compounds in Biological and Environmental Samples

    Science.gov (United States)

    Sosa-Ferrera, Zoraida; Mahugo-Santana, Cristina; Santana-Rodríguez, José Juan

    2013-01-01

    Endocrine-disruptor compounds (EDCs) can mimic natural hormones and produce adverse effects in the endocrine functions by interacting with estrogen receptors. EDCs include both natural and synthetic chemicals, such as hormones, personal care products, surfactants, and flame retardants, among others. EDCs are characterised by their ubiquitous presence at trace-level concentrations and their wide diversity. Since the discovery of the adverse effects of these pollutants on wildlife and human health, analytical methods have been developed for their qualitative and quantitative determination. In particular, mass-based analytical methods show excellent sensitivity and precision for their quantification. This paper reviews recently published analytical methodologies for the sample preparation and for the determination of these compounds in different environmental and biological matrices by liquid chromatography coupled with mass spectrometry. The various sample preparation techniques are compared and discussed. In addition, recent developments and advances in this field are presented. PMID:23738329

  6. Analytical methodologies for the determination of endocrine disrupting compounds in biological and environmental samples.

    Science.gov (United States)

    Sosa-Ferrera, Zoraida; Mahugo-Santana, Cristina; Santana-Rodríguez, José Juan

    2013-01-01

    Endocrine-disruptor compounds (EDCs) can mimic natural hormones and produce adverse effects in the endocrine functions by interacting with estrogen receptors. EDCs include both natural and synthetic chemicals, such as hormones, personal care products, surfactants, and flame retardants, among others. EDCs are characterised by their ubiquitous presence at trace-level concentrations and their wide diversity. Since the discovery of the adverse effects of these pollutants on wildlife and human health, analytical methods have been developed for their qualitative and quantitative determination. In particular, mass-based analytical methods show excellent sensitivity and precision for their quantification. This paper reviews recently published analytical methodologies for the sample preparation and for the determination of these compounds in different environmental and biological matrices by liquid chromatography coupled with mass spectrometry. The various sample preparation techniques are compared and discussed. In addition, recent developments and advances in this field are presented.

  7. A Simple Spectrophotometric Determination of Phosphate in Sugarcane Juices, Water and Detergent Samples

    Directory of Open Access Journals (Sweden)

    Mahadevaiah

    2007-01-01

    Full Text Available A simple spectrophotometric method is developed for the determination of phosphate in sugar cane juice, water and detergent samples. The method is based on the formation of phosphomolybdate with added molybdate followed by its reduction with sodium sulphide in aqueous sulfuric acid medium. The system obeys Lambert-Beer’s law at 715 nm in the concentration range 0.3-12.24 ppm. Molar absorptivity, correlation coefficient and Sandell’s sensitivity values were found to be 6.1x103 mol-1 cm-1, 0.999 and 0.0156 µg cm-2 respectively. The results obtained were reproducible with acceptable standard deviation 3.7% and relative error 3.4%. For a comparison of the method phosphate present in various samples were also determined separately following an official method. The results of the developed method compare well with those of the official method.

  8. Determination of aniline in environmental water samples by alternating-current oscillopolarographic titration

    Institute of Scientific and Technical Information of China (English)

    Jun Ping Xiao; Qing Xiang Zhou; Xiao Ke Tian; Hua Hua Bai; Xian Fa Su

    2007-01-01

    A new method for the determination of aniline in environmental water based on oscillopolarographic titration was presented in this paper.Several factors including the kind, concentration, and volume of acid, the dosage of potassium bromide, the temperature and concentration of concomitant substances were investigated in detail.The experimental results indicated that this method was simple, rapid, and sensitive.The linear range was 8.367 x 10-4 to 2.789 x 10-2 mol L-1, the relative standard deviation (R.S.D.) was lower than 0.96%, and the spiked recoveries of aniline in environmental water samples were in the range of 99.4-106.9% under the optimal conditions.The results indicated that the present method could be used as an alternative method for aniline determination in realworld water samples.

  9. An analytical protocol for the determination of total mercury concentrations in solid peat samples

    DEFF Research Database (Denmark)

    Roos-Barraclough, F; Givelet, N; Martinez-Cortizas, A

    2002-01-01

    and Pseudevernia furfuracea) are particularly efficient Hg retainers. The disproportionally high Hg concentrations in these species can cause considerable variation in Hg concentrations within a peat slice. The variation of water content (1.6% throughout 17-cm core, 0.97% in a 10 x 10 cm slice), bulk density (40...... AMA 254, capable of determining mercury concentrations in solid samples. Finally, an analytical protocol for the determination of Hg concentrations in solid peat samples is proposed. This method allows correction for variation in factors such as vegetation type, bulk density, water content and Hg...... concentration in individual peat slices. Several subsamples from each peat slice are air dried, combined and measured for Hg using the AMA254, using a program of 30 s (drying), 125 s (decomposition) and 45 s (waiting). Bulk density and water content measurements are performed on every slice using separate...

  10. Sample treatment platform using nanoparticles to determine salinomycin in flesh and meat.

    Science.gov (United States)

    Park, Jihyun; Lim, H B

    2014-10-01

    In this work, we developed a sensitive and selective analytical method of determining salinomycin in flesh and meat using a lab-built laser induced fluorescence microscope (LIFM) with nanoparticles. Two types of nanoparticles, Cy5 doped core-shell silica nanoparticles as a probe and magnetic nanoparticles (MNPs) to extract the target antibiotic from the treated sample, were synthesized and modified for chemical and enzymatic binding. After optimization, the newly developed method was applied to ham, chicken, and meat samples for the quantitative determination of salinomycin. The limits of detection (LODs) obtained from the calibration curve were 48-590 pg/mL, which was about 100-fold lower than that of the ELISA method.

  11. Characterization of Complex Fractionated Atrial Electrograms by Sample Entropy: An International Multi-Center Study

    Directory of Open Access Journals (Sweden)

    Eva Cirugeda–Roldán

    2015-10-01

    Full Text Available Atrial fibrillation (AF is the most commonly clinically-encountered arrhythmia. Catheter ablation of AF is mainly based on trigger elimination and modification of the AF substrate. Substrate mapping ablation of complex fractionated atrial electrograms (CFAEs has emerged to be a promising technique. To improve substrate mapping based on CFAE analysis, automatic detection algorithms need to be developed in order to simplify and accelerate the ablation procedures. According to the latest studies, the level of fractionation has been shown to be promisingly well estimated from CFAE measured during radio frequency (RF ablation of AF. The nature of CFAE is generally nonlinear and nonstationary, so the use of complexity measures is considered to be the appropriate technique for the analysis of AF records. This work proposes the use of sample entropy (SampEn, not only as a way to discern between non-fractionated and fractionated atrial electrograms (A-EGM, Entropy 2015, 17 7494 but also as a tool for characterizing the degree of A-EGM regularity, which is linked to changes in the AF substrate and to heart tissue damage. The use of SampEn combined with a blind parameter estimation optimization process enables the classification between CFAE and non-CFAE with statistical significance (p < 0:001, 0.89 area under the ROC, 86% specificity and 77% sensitivity over a mixed database of A-EGM combined from two independent CFAE signal databases, recorded during RF ablation of AF in two EU countries (542 signals in total. On the basis of the results obtained in this study, it can be suggested that the use of SampEn is suitable for real-time support during navigation of RF ablation of AF, as only 1.5 seconds of signal segments need to be analyzed.

  12. Cloud point extraction, preconcentration and spectrophotometric determination of trace amount of manganese(II) in water and food samples

    Science.gov (United States)

    Gouda, Ayman A.

    2014-10-01

    A new cloud point extraction (CPE) process using the nonionic surfactant Triton X-114 to extract manganese(II) from aqueous solution was investigated. The method is based on the complexation reaction of manganese(II) with 1,2,5,8-tetrahydroxyanthracene-9,10-dione (quinalizarin) in the presence of borate buffer at pH 8.5 and micelle-mediated extraction of the complex. The enriched analyte in the surfactant-rich phase was determined by spectrophotometry at 528 nm. The optimal extraction and reaction conditions (e.g. pH, reagent and surfactant concentrations, temperature and centrifugation times) were evaluated and optimized. Under the optimized experimental conditions, the analytical characteristics of the method (e.g., limit of detection (LOD), linear range, preconcentration and improvement factors) were obtained. The proposed CPE method showed linear calibration within the range 5.0-200 ng mL-1 of manganese(II) and the limit of detection of the method was 0.8 ng mL-1 with an preconcentration factor of ∼50 when 25 mL of sample solution was preconcentrated to 0.5 mL. The relative standard deviation (RSD) and relative error were found to be 1.35% and 1.42%, respectively (CMn(II) = 150 ng mL-1, n = 6) for pure standard solutions. The interference effect of some cations and anions was also studied. In the presence of foreign ions, no significant interference was observed. The method was applied to the determination of manganese(II) in water and food samples with a recovery for the spiked samples in the range of 95.87-102.5%.

  13. Cloud point extraction, preconcentration and spectrophotometric determination of trace amount of manganese(II) in water and food samples.

    Science.gov (United States)

    Gouda, Ayman A

    2014-10-15

    A new cloud point extraction (CPE) process using the nonionic surfactant Triton X-114 to extract manganese(II) from aqueous solution was investigated. The method is based on the complexation reaction of manganese(II) with 1,2,5,8-tetrahydroxyanthracene-9,10-dione (quinalizarin) in the presence of borate buffer at pH 8.5 and micelle-mediated extraction of the complex. The enriched analyte in the surfactant-rich phase was determined by spectrophotometry at 528nm. The optimal extraction and reaction conditions (e.g. pH, reagent and surfactant concentrations, temperature and centrifugation times) were evaluated and optimized. Under the optimized experimental conditions, the analytical characteristics of the method (e.g., limit of detection (LOD), linear range, preconcentration and improvement factors) were obtained. The proposed CPE method showed linear calibration within the range 5.0-200ngmL(-1) of manganese(II) and the limit of detection of the method was 0.8ngmL(-1) with an preconcentration factor of ∼50 when 25mL of sample solution was preconcentrated to 0.5mL. The relative standard deviation (RSD) and relative error were found to be 1.35% and 1.42%, respectively (CMn(II)=150ngmL(-1), n=6) for pure standard solutions. The interference effect of some cations and anions was also studied. In the presence of foreign ions, no significant interference was observed. The method was applied to the determination of manganese(II) in water and food samples with a recovery for the spiked samples in the range of 95.87-102.5%.

  14. Rapid and sensitive hormonal profiling of complex plant samples by liquid chromatography coupled to electrospray ionization tandem mass spectrometry

    Directory of Open Access Journals (Sweden)

    Müller Maren

    2011-11-01

    Full Text Available Abstract Background Plant hormones play a pivotal role in several physiological processes during a plant's life cycle, from germination to senescence, and the determination of endogenous concentrations of hormones is essential to elucidate the role of a particular hormone in any physiological process. Availability of a sensitive and rapid method to quantify multiple classes of hormones simultaneously will greatly facilitate the investigation of signaling networks in controlling specific developmental pathways and physiological responses. Due to the presence of hormones at very low concentrations in plant tissues (10-9 M to 10-6 M and their different chemistries, the development of a high-throughput and comprehensive method for the determination of hormones is challenging. Results The present work reports a rapid, specific and sensitive method using ultrahigh-performance liquid chromatography coupled to electrospray ionization tandem spectrometry (UPLC/ESI-MS/MS to analyze quantitatively the major hormones found in plant tissues within six minutes, including auxins, cytokinins, gibberellins, abscisic acid, 1-amino-cyclopropane-1-carboxyic acid (the ethylene precursor, jasmonic acid and salicylic acid. Sample preparation, extraction procedures and UPLC-MS/MS conditions were optimized for the determination of all plant hormones and are summarized in a schematic extraction diagram for the analysis of small amounts of plant material without time-consuming additional steps such as purification, sample drying or re-suspension. Conclusions This new method is applicable to the analysis of dynamic changes in endogenous concentrations of hormones to study plant developmental processes or plant responses to biotic and abiotic stresses in complex tissues. An example is shown in which a hormone profiling is obtained from leaves of plants exposed to salt stress in the aromatic plant, Rosmarinus officinalis.

  15. Separation and enrichment of gold(III) from environmental samples prior to its flame atomic absorption spectrometric determination

    Energy Technology Data Exchange (ETDEWEB)

    Senturk, Hasan Basri; Gundogdu, Ali [Department of Chemistry, Faculty of Arts and Sciences, Karadeniz Technical University, 61080 Trabzon (Turkey); Bulut, Volkan Numan [Department of Chemistry, Faculty of Arts and Sciences, Karadeniz Technical University, 28049 Giresun (Turkey); Duran, Celal [Department of Chemistry, Faculty of Arts and Sciences, Karadeniz Technical University, 61080 Trabzon (Turkey); Soylak, Mustafa [Department of Chemistry, Faculty of Arts and Sciences, Erciyes University, 38039 Kayseri (Turkey)], E-mail: soylak@erciyes.edu.tr; Elci, Latif [Department of Chemistry, Faculty of Arts and Sciences, Pamukkale University, 20020 Denizli (Turkey); Tufekci, Mehmet [Department of Chemistry, Faculty of Arts and Sciences, Karadeniz Technical University, 61080 Trabzon (Turkey)

    2007-10-22

    A simple and accurate method was developed for separation and enrichment of trace levels of gold in environmental samples. The method is based on the adsorption of Au(III)-diethyldithiocarbamate complex on Amberlite XAD-2000 resin prior to the analysis of gold by flame atomic absorption spectrometry after elution with 1 mol L{sup -1} HNO{sub 3} in acetone. Some parameters including nitric acid concentration, eluent type, matrix ions, sample volume, sample flow rate and adsorption capacity were investigated on the recovery of gold(III). The recovery values for gold(III) and detection limit of gold were greater than 95% and 16.6 {mu}g L{sup -1}, respectively. The preconcentration factor was 200. The relative standard deviation of the method was <6%. The adsorption capacity of the resin was 12.3 mg g{sup -1}. The validation of the presented procedure was checked by the analysis of CRM-SA-C Sandy Soil certified reference material. The presented procedure was applied to the determination of gold in some environmental samples.

  16. Determination of Complex-Valued Parametric Model Coefficients Using Artificial Neural Network Technique

    Directory of Open Access Journals (Sweden)

    A. M. Aibinu

    2010-01-01

    Full Text Available A new approach for determining the coefficients of a complex-valued autoregressive (CAR and complex-valued autoregressive moving average (CARMA model coefficients using complex-valued neural network (CVNN technique is discussed in this paper. The CAR and complex-valued moving average (CMA coefficients which constitute a CARMA model are computed simultaneously from the adaptive weights and coefficients of the linear activation functions in a two-layered CVNN. The performance of the proposed technique has been evaluated using simulated complex-valued data (CVD with three different types of activation functions. The results show that the proposed method can accurately determine the model coefficients provided that the network is properly trained. Furthermore, application of the developed CVNN-based technique for MRI K-space reconstruction results in images with improve resolution.

  17. Determination of the self-attenuation correction factor for environmental samples analysis in gamma spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Talita O.; Rocha, Zildete; Knupp, Eliana A.N.; Kastner, Geraldo F.; Oliveira, Arno H. de, E-mail: talitaolsantos@yahoo.com.br, E-mail: rochaz@cdtn.br [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil); Oliveira, Arno H. de, E-mail: arnoheeren@gmail.com [Universidade Federal de Minas Gerais (PCTN/DEN/UFMG), Belo Horizonte, MG (Brazil). Departamento de Engenharia Nuclear

    2015-07-01

    Gamma spectrometry technique has been used in order to obtain the activity concentrations of natural and artificial radionuclides in environmental samples of different origins, compositions and densities. These samples characteristics may influence the calibration condition by the self-attenuation effect. The sample density has been considered the most important factor. For reliable results, it is necessary to determine self-attenuation correction factor which has been subject of great interest due to its effect on activity concentration. In this context, the aim of this work is to show the calibration process considering the correction by self-attenuation in the evaluation of the concentration of each radionuclide to a gamma HPGEe detector spectrometry system. (author)

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

    Science.gov (United States)

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

    2016-02-01

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

  19. Recent developments in fatty acids profile determination in biological samples - a review

    Directory of Open Access Journals (Sweden)

    Tiuca Ioana

    2015-12-01

    Full Text Available The present paper is a literature review of the recent years dealing with the most important separation techniques of fatty acids in biological samples. Our aim was to make a synthesis of the analytical methods used, to note the most used ones, but also to mention other methods that are less utilized, which can have important advantages (such as less time consuming, greener reagents, etc.. Gas-chromatographic separation methods were described and compared to liquid chromatographic separations of fatty acids in different types of biological samples. In the same time, the importance of determining fatty acids profiles in biological samples was revealed, pointing out the possible implications in diagnostics of different types of disorders or remarking different profiles compared to healthy states.

  20. RECOVERY OF A TRITIATED LANA SAMPLE FOR DOSE CONVERSION FACTOR DETERMINATION

    Energy Technology Data Exchange (ETDEWEB)

    Staack, G.

    2010-11-12

    The purpose of this work is to develop a technical basis for both estimating the dose of a worker exposed to respirable tritiated LaNi{sub 4.25}Al{sub 0.75} (LANA) and implementing hazard appropriate controls. Savannah River National Laboratory (SRNL) has agreed to provide Lovelace Respiratory Research Institute (LRRI) with a tritiated LANA sample. LRRI will determine the particle size distribution (PSD) as well as perform dissolution rate studies on the sample in serum ultrafiltrate (SUF), a simulated lung fluid. The rate of tritium release from the sample will be measured over a three month period. Tritium release rate information will be used to calculate a DCF for respirable tritiated LANA.

  1. Determination of the boron content in polyethylene samples using the reactor Orphée

    CERN Document Server

    Gunsing, F; Aberle, O

    2017-01-01

    The boron content of two unknown types of polyethylene has been determined relative to a known reference type. Samples of polyethylene, including a known boron-less one, were irradiated with thermal neutrons at the reactor Orphée at Saclay in France. Prompt gamma rays were measured with a CeBr$_3$ detector and the intensity of the 478~keV line from $^{10}${B}(n,$\\alpha_1\\gamma$)$^{7}{Li*} was extracted.

  2. Development of a sample preparation procedure of sewage sludge samples for the determination of polycyclic aromatic hydrocarbons based on selective pressurized liquid extraction.

    Science.gov (United States)

    Pena, Maria Teresa; Casais, Maria Carmen; Mejuto, Maria Carmen; Cela, Rafael

    2010-01-22

    An automated, simple and sensitive method based on selective pressurized liquid extraction (SPLE) was developed for the analysis of polycyclic aromatic hydrocarbons in sewage sludge samples. The new sample preparation procedure consists of on-line clean-up by inclusion of sorbents in the extraction cell, and combines elevated temperatures and pressures with liquid solvents to achieve fast and efficient removal of target analytes from complex sewage sludge matrices. The effects of various operational parameters (e.g. sample pretreatment, extraction solvent, temperature, pressure, static time, etc.) on the performance of SPLE procedure were carefully investigated, obtaining the best results when SPLE conditions were fixed at 140 degrees C, 1500 psi, static time of 5 min and n-hexane as extraction solvent. A new programmed temperature vaporization-gas chromatography-tandem mass spectrometry method based on large volume injection (PTV-LVI-GC-MS/MS) was also developed and analytical determinations were performed by high performance liquid chromatography coupled with fluorescence detection and GC-MS/MS. The extraction yields for the different compounds obtained by SPLE ranged from 84.8% to 106.6%. Quantification limits obtained for all of these studied compounds (between 0.0001 and 0.005 microg g(-1), dry mass) were well below the regulatory limits for all compounds considered. To test the accuracy of the SPLE technique, the optimized methodology was applied to the analysis of a certified reference material (sewage sludge (BCR088)) and a reference material (sewage sludge (RTC-CNS312-04)), with excellent results.

  3. Determination of the efficiency of a detector in gamma spectrometry of large-volume samples

    CERN Document Server

    Tertyshnik, E G

    2012-01-01

    The experimental - calculated method is proposed to determine the full energy peak efficiency (FEPE) of detectors {\\epsilon}(E) in case a measurement of the large-volume samples. Water is used as standard absorber in which the linear attenuation coefficients for photons {\\mu}0 (E) is well known. The value {\\mu} (E) in sample material (matrix of the sample) is determined experimentally by means of spectrometer. The formulas are given for calculation of the ratio {\\epsilon}(E)/ {\\epsilon}0(E), where {\\epsilon}0(E) is FEPE of the detector for photons those are arising in the container filled with water (it is found by adding in the container of the Reference radioactive solutions). To prove the validity of the method ethanol (density 0,8 g/cm3) and water solutions of salts (density 1,2 and 1,5 g/cm3) were used for simulation of the samples with different attenuation coefficients. Standard deviation between experimental and calculated efficiencies has been about 5 %.

  4. Determination of Pu in soil samples; Determinacion de Pu en muestras de suelo

    Energy Technology Data Exchange (ETDEWEB)

    Torres C, C. O.; Hernandez M, H.; Romero G, E. T. [ININ, Carretera Mexico-Toluca s/n, 52750 Ocoyoacac, Estado de Mexico (Mexico); Vega C, H. R., E-mail: carioli_32907@hotmail.com [Universidad Autonoma de Zacatecas, Unidad Academica de Estudios Nucleares, Cipres No. 10, Fracc. La Penuela, 98068 Zacatecas, Zac. (Mexico)

    2016-10-15

    The irreversible consequences of accidents occurring in nuclear plants and in nuclear fuel reprocessing sites are mainly the distribution of different radionuclides in different matrices such as the soil. The distribution in the superficial soil is related to the internal and external exposure to the radiation of the affected population. The internal contamination with radionuclides such as Pu is of great relevance to the nuclear forensic science, where is important to know the chemical and isotopic compositions of nuclear materials. The objective of this work is to optimize the radiochemical separation of plutonium (Pu) from soil samples and to determine their concentration. The soil samples were prepared using acid digestion assisted by microwave; purification of Pu was carried out with AG1X8 resin using ion exchange chromatography. Pu isotopes were measured using ICP-SFMS. In order to reduce the interference due to the presence of {sup 238}UH {sup +} in the samples, a solvent removal system (Apex) was used. In addition, the limit of detection and quantification of Pu was determined. It was found that the recovery efficiency of Pu in soil samples ranges from 70 to 93%. (Author)

  5. Rapid radiochemical method for determination of actinides in emergency concrete and brick samples.

    Science.gov (United States)

    Maxwell, Sherrod L; Culligan, Brian K; Kelsey-Wall, Angel; Shaw, Patrick J

    2011-09-02

    A new rapid method for the determination of actinides in emergency concrete and brick samples has been developed at the Savannah River Site Environmental Lab (Aiken, SC, USA) that can be used in emergency response situations or for routine analysis. If a radiological dispersive device (RDD), Improvised Nuclear Device (IND) or nuclear accident occurs, there will be a urgent need for rapid analyses of many different environmental matrices, including building materials such as concrete and brick, to support dose mitigation and environmental clean-up. The new method for actinides in concrete and brick method utilizes a rapid sodium hydroxide fusion method, a lanthanum fluoride matrix removal step, and a column separation process with stacked TEVA, TRU and DGA Resin cartridges. Alpha emitters are prepared using rare earth microprecipitation for counting by alpha spectrometry. The method showed high chemical recoveries and effective removal of interferences. The determination of actinides in concrete and brick sample analysis can be performed in less than 8h with excellent quality for emergency samples. The rapid fusion technique is a rugged sample digestion method that ensures that any refractory actinide particles are effectively digested.

  6. Comparison of two sample preparation procedures for HPLC determination of ochratoxin A

    Directory of Open Access Journals (Sweden)

    Vuković Gorica L.

    2009-01-01

    Full Text Available In preparation of samples for chromatographic determination of ochratoxin A, two types of columns were used for sample cleanup (SPE and immunoaffinity columns. The first method consisted of liquid-liquid extraction with a mixture of chloroform and phosphoric acid, followed by ion-exchange cleanup on Waters Oasis MAX columns. The sec­ond method consisted of extraction with a mixture of water and methanol, followed by LCTech OtaCLEAN immunoaf­finity column cleanup. Recoveries of the methods were determined at three levels in three repetitions for maize flour, and they were 84% (%RSD = 19.2 for the first method of sample preparation and 101% (%RSD = 2.2 for the second method. Values of LOQ for OTA were 0.25 and 1.00 μg/kg for the IAC and SPE clean-up procedures, respectively. Both methods comply with present regulations, but the MAX sample clean-up procedure should be used as an alternative, since the immunoaffinity column clean-up procedure is characterized by better reproducibility, accuracy, and efficiency.

  7. Preliminary study on element mass fraction determination on catfish samples from Paraguay

    Energy Technology Data Exchange (ETDEWEB)

    Moreira, Edson G.; Catharino, Marilia G.M.; Vasconcellos, Marina B.A., E-mail: emoreira@ipen.br, E-mail: mbvascon@ipen.br, E-mail: mariliasemmler@uol.com.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Frutos, Sixto A.; Insaurralde, Mario S., E-mail: tony8013@hotmail.com, E-mail: insaurraldemar9@hotmail.com [Universidad Nacional de Asuncion (FCV/UNA), San Lorenzo (Paraguay). Facultad de Ciencias Veterinarias. Departamento de Pesca y Acuicultura

    2013-07-01

    South American catfish (Pseudoplatystoma), commonly known in Spanish as atigrado or surubi and in Portuguese as surubim or pintado is a large fish that typically reaches 1 m long and weighs 60 kg to 80 kg and may be found at the basins of the Amazon, the Sao Francisco and de la Plata rivers, usually in riverbeds and deep wells. Being a much appreciated fish for human consumption, it is quite sought after by fishermen who have been contributing to the reduction of the stocks. This fact attracted the attention of the Paraguayan authorities to the point of imposing restrictions to free fishing and commercialization. This study aims to assist the conservation efforts towards this fish by investigating its exposure to possible pollutants. Preliminary results on element determination on six samples of catfish from Paraguayan rivers are presented. Cs, Co, Fe, Se and Zn were determined by applying an Instrumental Neutron Activation Analysis method. While these element levels were lower than the legislation for human consumption, the elements As, Cr e La were not detected in the samples as they are below the detection limit of the method employed. Atomic Absorption Spectrometry was used to investigate the presence of Cd, Hg and Pb in the samples. Hg was detected in the samples while Cd and Pb were below the detection limit of the method. (author)

  8. Determination of aflatoxins in rice samples by ultrasound-assisted matrix solid-phase dispersion.

    Science.gov (United States)

    Manoochehri, Mahboobeh; Asgharinezhad, Ali Akbar; Safaei, Mahdi

    2015-01-01

    This work describes the application of ultrasound-assisted matrix solid-phase dispersion as an extraction and sample preparation approach for aflatoxins (B1, B2, G1 and G2) and subsequent determination of them by high-performance liquid chromatography-fluorescence detection. A Box-Behnken design in combination with response surface methodology was used to determine the affecting parameters on the extraction procedure. The influence of different variables including type of dispersing phase, sample-to-dispersing phase ratio, type and quantity of clean-up phase, ultrasonication time, ultrasonication temperature, nature and volume of the elution solvent was investigated in the optimization study. C18, primary-secondary amine (PSA) and acetonitrile were selected as dispersing phase, clean-up phase and elution solvent, respectively. The obtained optimized values were sample-to-dispersing phase ratio of 1 : 1, 60 mg of PSA, 11 min ultrasonication time, 30°C ultrasonication temperature and 4 mL acetonitrile. Under the optimal conditions, the limits of detection were ranged from 0.09 to 0.14 ng g(-1) and the precisions [relative standard deviation (RSD%)] were <8.6%. The recoveries of the matrix solid-phase dispersion process ranged from 78 to 83% with RSD <10% in all cases. Finally, this method was successfully applied to the extraction of trace amounts of aflatoxins in rice samples. © The Author [2014]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  9. Electromembrane extraction and spectrophotometric determination of As(V) in water samples.

    Science.gov (United States)

    Kamyabi, Mohammad Ali; Aghaei, Ali

    2016-12-01

    In this study, for the first time electromembrane extraction (EME) was used as a highly efficient sample pre-treatment method for the UV-VIS spectrophotometric determination of As(V) in water samples. The influences of experimental parameters during EME were investigated and optimized using one-variable-at-a-time methodology as follows: organic solvent: 1-octanol+2.5% (V/V) di-(2-ethylhexyl) phosphate, applied voltage: 70V, extraction time: 15min, pH of acceptor: 13, stirring rate: 750rpm. The method allowed the determination of As(V) in the range of 5-300ngmL(-1). The relative standard deviation was found to be within the range of 3.4-7.6%. The limit of detection, corresponding to a signal to noise ratio of three, was 1.5ngmL(-1). The proposed method was finally applied to the determination of As(V) in water samples and relative recoveries ranging from 95 to 102% were obtained.

  10. Determination of primary explosive azides in environmental samples by sequential injection amperometry.

    Energy Technology Data Exchange (ETDEWEB)

    Echols, R. T.; James, R. R.; Aldstadt, J. H.; Environmental Research; Univ.of Minnesota; Univ of Minnesota

    1997-01-01

    The application of flow injection methodology to the determination of trace concentrations of primary explosives is presented. The approach is demonstrated with a sequential injection amperometric method for the determination of the azide ion (N{sub 3}{sup -}). The proposed method can be applied to the determination of sodium azide or lead azide, a primary explosive, without regard to other sources of lead in environmental samples. The sequential injection system used for the analysis forms the basis for a proposed field-portable instrument for the analysis of primary explosives. A microporous gas permeable membrane in a gas diffusion unit (GDU) is used to separate the analyte from other anions that can also be oxidized at the amperometric cell. The behavior of the GDU was optimized with respect to the pH of the donor stream and the timing of the preconcentration step. A study of anions that are commonly found in environmental samples showed that the species that will interfere with the analytical signal can be removed by the GDU. Results from three water samples that were spiked with 0.40 ppm of azide are presented. RSDs in the range 3-5% were typically obtained using the method. The useful working range of the method was linear up to 0.5 ppm and non-linear up to 20 ppm (second-order model). The limit of detection was 24.6 ppb.

  11. Determination of imidacloprid in water samples via photochemically induced fluorescence and second-order multivariate calibration.

    Science.gov (United States)

    Fuentes, Edwar; Cid, Camila; Báez, María E

    2015-03-01

    This paper presents a new method for the determination of imidacloprid in water samples; one of the most widely used neonicotinoid pesticides in the farming industry. The method is based on the measurement of excitation-emission spectra of photo-induced fluorescence (PIF-EEMs) associated with second-order multivariate calibration with a parallel factor analysis (PARAFAC) and unfolded partial least squares coupled to residual bilinearization (U-PLS/RBL). The second order advantage permitted the determination of imidacloprid in the presence of potential interferences, which also shows photo-induced fluorescence (other pesticides and/or unexpected compounds of the real samples). The photoreaction was performed in 100-μl disposable micropipettes. As a preliminary step, solid phase extraction on C18 (SPE-C18) was applied to concentrate the analyte and diminish the limit of detection. The LOD was approximately 1 ng mL(-1), which is suitable for detecting imidacloprid in water according to the guidelines established in North America and Europe. The PIF-EEMs coupled to PARAFAC or U-PLS/RBL was successfully applied for the determination of imidacloprid in different real water samples, with an average recovery of 101±10%.

  12. Platelet-neutrophil complex formation-a detailed in vitro analysis of murine and human blood samples.

    Science.gov (United States)

    Mauler, Maximilian; Seyfert, Julia; Haenel, David; Seeba, Hannah; Guenther, Janine; Stallmann, Daniela; Schoenichen, Claudia; Hilgendorf, Ingo; Bode, Christoph; Ahrens, Ingo; Duerschmied, Daniel

    2016-05-01

    Platelets form complexes with neutrophils during inflammatory processes. These aggregates migrate into affected tissues and also circulate within the organism. Several studies have evaluated platelet-neutrophil complexes as a marker of cardiovascular diseases in human and mouse. Although multiple publications have reported platelet-neutrophil complex counts, we noticed that different methods were used to analyze platelet-neutrophil complex formation, resulting in significant differences, even in baseline values. We established a protocol for platelet-neutrophil complex measurement with flow cytometry in murine and human whole blood samples. In vitro platelet-neutrophil complex formation was stimulated with ADP or PMA. We tested the effect of different sample preparation steps and cytometer settings on platelet-neutrophil complex detection and noticed false-positive counts with increasing acquisition speed. Platelet-neutrophil complex formation depends on platelet P-selectin expression, and antibody blocking of P-selectin consequently prevented ADP-induced platelet-neutrophil complex formation. These findings may help generating more comparable data among different research groups that examine platelet-neutrophil complexes as a marker for cardiovascular disease and novel therapeutic interventions.

  13. 40 CFR 761.283 - Determination of the number of samples to collect and sample collection locations.

    Science.gov (United States)

    2010-07-01

    ... sites at this example location: a loading dock, a transformer storage lot, and a disposal pit. The... (three samples). The non-liquid PCB remediation wastes present at the transformer storage lot are oily... north and one meter in the direction east of magnetic north. (2) Mark out a series of sampling points...

  14. Overcoming Matrix Effects in a Complex Sample: Analysis of Multiple Elements in Multivitamins by Atomic Absorption Spectroscopy

    Science.gov (United States)

    Arnold, Randy J.; Arndt, Brett; Blaser, Emilia; Blosser, Chris; Caulton, Dana; Chung, Won Sog; Fiorenza, Garrett; Heath, Wyatt; Jacobs, Alex; Kahng, Eunice; Koh, Eun; Le, Thao; Mandla, Kyle; McCory, Chelsey; Newman, Laura; Pithadia, Amit; Reckelhoff, Anna; Rheinhardt, Joseph; Skljarevski, Sonja; Stuart, Jordyn; Taylor, Cassie; Thomas, Scott; Tse, Kyle; Wall, Rachel; Warkentien, Chad

    2011-01-01

    A multivitamin tablet and liquid are analyzed for the elements calcium, magnesium, iron, zinc, copper, and manganese using atomic absorption spectrometry. Linear calibration and standard addition are used for all elements except calcium, allowing for an estimate of the matrix effects encountered for this complex sample. Sample preparation using…

  15. Determination of complexation capacity of trace metal-organic in natural water

    Institute of Scientific and Technical Information of China (English)

    1999-01-01

    The complexation capacity for heavy metals (Cu, Cd, Pb) were determined by anodic stripping voltammetry in South China Sea, Hulun Lake and Wuliang Suhai. The conditional stability constants and complexation capacity index were calculated. The data showed that the complexation capacity of the Hulun Lake was greater than that of seawater and Wuliang Suhai. The sequence of complexation capacity is C (CuL) > C (CdL) > C (PbL), the values are in concord with results of analysis on dissolved organic carbon. The conditional stability constants were in an opposite sequence: K (CuL) < K(CdL) < K (PbL). When logK are similar, the greater the complexation capacity, the greater the complexation capacity index.

  16. Cloud point extraction for the determination of copper, nickel and cobalt ions in environmental samples by flame atomic absorption spectrometry.

    Science.gov (United States)

    Ghaedi, M; Shokrollahi, A; Ahmadi, F; Rajabi, H R; Soylak, M

    2008-02-11

    A cloud point extraction procedure was presented for the preconcentration of copper, nickel and cobalt ions in various samples. After complexation with methyl-2-pyridylketone oxime (MPKO) in basic medium, analyte ions are quantitatively extracted to the phase rich in Triton X-114 following centrifugation. 1.0 mol L(-1) HNO(3) nitric acid in methanol was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The adopted concentrations for MPKO, Triton X-114 and HNO(3), bath temperature, centrifuge rate and time were optimized. Detection limits (3 SDb/m) of 1.6, 2.1 and 1.9 ng mL(-1) for Cu(2+), Co(2+) and Ni(2+) along with preconcentration factors of 30 and for these ions and enrichment factor of 65, 58 and 67 for Cu(2+), Ni(2+) and Co(2+), respectively. The high efficiency of cloud point extraction to carry out the determination of analytes in complex matrices was demonstrated. The proposed procedure was applied to the analysis of biological, natural and wastewater, soil and blood samples.

  17. Cloud point extraction for the determination of copper, nickel and cobalt ions in environmental samples by flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ghaedi, M. [Chemistry Department, University of Yasouj, Yasouj 75914-353 (Iran, Islamic Republic of)], E-mail: m_ghaedi@mail.yu.ac.ir; Shokrollahi, A.; Ahmadi, F.; Rajabi, H.R. [Chemistry Department, University of Yasouj, Yasouj 75914-353 (Iran, Islamic Republic of); Soylak, M. [Chemistry Department, University of Erciyes, 38039 Kayseri (Turkey)

    2008-02-11

    A cloud point extraction procedure was presented for the preconcentration of copper, nickel and cobalt ions in various samples. After complexation with methyl-2-pyridylketone oxime (MPKO) in basic medium, analyte ions are quantitatively extracted to the phase rich in Triton X-114 following centrifugation. 1.0 mol L{sup -1} HNO{sub 3} nitric acid in methanol was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The adopted concentrations for MPKO, Triton X-114 and HNO{sub 3}, bath temperature, centrifuge rate and time were optimized. Detection limits (3 SDb/m) of 1.6, 2.1 and 1.9 ng mL{sup -1} for Cu{sup 2+}, Co{sup 2+} and Ni{sup 2+} along with preconcentration factors of 30 and for these ions and enrichment factor of 65, 58 and 67 for Cu{sup 2+}, Ni{sup 2+} and Co{sup 2+}, respectively. The high efficiency of cloud point extraction to carry out the determination of analytes in complex matrices was demonstrated. The proposed procedure was applied to the analysis of biological, natural and wastewater, soil and blood samples.

  18. Determination of Antioxidant Flavonoids in Sudanese Honey Samples by Solid Phase Extraction and High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Suzan Zein Alabdeen Makawi

    2009-01-01

    Full Text Available Flavonoids were extracted by solid phase extraction (SPE from seven floral honey samples of different botanical origin from different regions of Sudan. The flavonoids were determined by high performance liquid chromatography (HPLC technique using photo diode array detector (PDA. An isocratic and gradient systems for the resolution, identification and quantification of five flavonoids, namely; quercetin, kaempferol, apigenin, hesperetin and isorhamnetin, were developed. Although the isocratic system resolved the five compounds, however it suffered from interference by the complex mixture of honey samples. The gradient system resolved three of five flavonoids, namely, quercetin, kaempferol, and isorhamnetin, without interference by the complex honey matrix. Two flavonoids, apigenin and hesperetin, were observed to elute at close retention times, which lead to their interference with each other when injected in a mixture; however, absorption wavelength selection was found indicative of the presence or absence of either compound. The quantification of these flavonoids was done through the calibration curves of their standards. The obtained results were compared with reported results.

  19. Determination of platinum in waste platinum-loaded carbon catalyst samples using microwave-assisted sample digestion and ICP-OES

    Science.gov (United States)

    Ma, Yinbiao; Wei, Xiaojuan

    2017-04-01

    A novel method for the determination of platinum in waste platinum-loaded carbon catalyst samples was established by inductively coupled plasma optical emission spectrometry after samples digested by microwave oven with aqua regia. Such experiment conditions were investigated as the influence of sample digestion methods, digestion time, digestion temperature and interfering ions on the determination. Under the optimized conditions, the linear range of calibration graph for Pt was 0 ˜ 200.00 mg L-1, and the recovery was 95.67% ˜ 104.29%. The relative standard deviation (RSDs) for Pt was 1.78 %. The proposed method was applied to determine the same samples with atomic absorption spectrometry with the results consistently, which is suitable for the determination of platinum in waste platinum-loaded carbon catalyst samples.

  20. Sensitive spectrophotometric methods for determination of some organophosphorus pesticides in vegetable samples

    Directory of Open Access Journals (Sweden)

    MAGDA A. AKL

    2010-03-01

    Full Text Available Three rapid, simple, reproducible and sensitive spectrophotometric methods (A, B and C are described for the determination of two organophosphorus pesticides, (malathion and dimethoate in formulations and vegetable samples. The methods A and B involve the addition of an excess of Ce4+ into sulphuric acid medium and the determination of the unreacted oxidant by decreasing the red color of chromotrope 2R (C2R at a suitable lmax = 528 nm for method A, or a decrease in the orange pink color of rhodamine 6G (Rh6G at a suitable lmax = = 525 nm. The method C is based on the oxidation of malathion or dimethoate with the slight excess of N-bromosuccinimide (NBS and the determination of unreacted oxidant by reacting it with amaranth dye (AM in hydrochloric acid medium at a suitable lmax = 520 nm. A regression analysis of Beer-Lambert plots showed a good correlation in the concentration range of 0.1-4.2 μg mL−1. The apparent molar absorptivity, Sandell sensitivity, the detection and quantification limits were calculated. For more accurate analysis, Ringbom optimum concentration ranges are 0.25-4.0 μg mL−1. The developed methods were successfully applied to the determination of malathion, and dimethoate in their formulations and environmental vegetable samples.

  1. Determination of air-loop volume and radon partition coefficient for measuring radon in water sample.

    Science.gov (United States)

    Lee, Kil Yong; Burnett, William C

    A simple method for the direct determination of the air-loop volume in a RAD7 system as well as the radon partition coefficient was developed allowing for an accurate measurement of the radon activity in any type of water. The air-loop volume may be measured directly using an external radon source and an empty bottle with a precisely measured volume. The partition coefficient and activity of radon in the water sample may then be determined via the RAD7 using the determined air-loop volume. Activity ratios instead of absolute activities were used to measure the air-loop volume and the radon partition coefficient. In order to verify this approach, we measured the radon partition coefficient in deionized water in the temperature range of 10-30 °C and compared the values to those calculated from the well-known Weigel equation. The results were within 5 % variance throughout the temperature range. We also applied the approach for measurement of the radon partition coefficient in synthetic saline water (0-75 ppt salinity) as well as tap water. The radon activity of the tap water sample was determined by this method as well as the standard RAD-H2O and BigBottle RAD-H2O. The results have shown good agreement between this method and the standard methods.

  2. Binary Contamination in the SEGUE sample: Effects on SSPP Determinations of Stellar Atmospheric Parameters

    CERN Document Server

    Schlesinger, Katharine J; Lee, Young Sun; Masseron, Thomas; Yanny, Brian; Rockosi, Constance M; Gaudi, B Scott; Beers, Timothy C

    2010-01-01

    Using numerical modeling and a grid of synthetic spectra, we examine the effects that unresolved binaries have on the determination of various stellar atmospheric parameters for SEGUE targets measured using the SEGUE Stellar Parameter Pipeline (SSPP). To model undetected binaries that may be in the SEGUE sample, we use a variety of mass distributions for the primary and secondary stars in conjunction with empirically determined relationships for orbital parameters to determine the fraction of G-K dwarf stars, as defined by SDSS color cuts, that will be blended with a secondary companion. We focus on the G-K dwarf sample in SEGUE as it records the history of chemical enrichment in our galaxy. To determine the effect of the secondary on the spectroscopic parameters, we synthesize a grid of model spectra from 3275 to 7850 K (~0.1 to 1.0 \\msun) and [Fe/H]=-0.5 to -2.5 from MARCS model atmospheres using TurboSpectrum. We analyze both "infinite" signal-to-noise ratio (S/N) models and degraded versions, at median S/...

  3. Detecting Determinism in Firing Activities of Retinal Ganglion Cells during Response to Complex Stimuli

    Institute of Scientific and Technical Information of China (English)

    CAI Chao-Feng; ZHANG Ying-Ying; LIU Xue; LIANG Pei-Ji; ZHANG Pu-Ming

    2008-01-01

    Complex stimuli are used to probe the response properties of the chicken's retinal ganglion cells (GCs). Thecorrelation dimension method and the nonlinear forecasting method are applied to detect the determinism in the firing activities of the retinal GCs during response to complex stimuli.The inter-spike interval (ISI) series and the first difference of the ISI (DISI) series are analysed.Two conclusions are drawn.Firstly,the first difference operation of the ISI series makes it comparatively easier for determinism detection in the firing activities of retinal GCs.Secondly,the nonlinear forecasting method is more efficient and reliable than the correlation dimension method for determinism detection.

  4. Selective virus detection in complex sample matrices with photonic crystal optical cavities.

    Science.gov (United States)

    Pal, Sudeshna; Yadav, Amrita R; Lifson, Mark A; Baker, James E; Fauchet, Philippe M; Miller, Benjamin L

    2013-06-15

    Rapid, sensitive, and selective detection of viruses is critical for applications in medical diagnostics, biosecurity, and environmental safety. In this article, we report the application of a point-defect-coupled W1 photonic crystal (PhC) waveguide biosensor to label-free optical detection of viruses. Fabricated on a silicon-on-insulator (SOI) substrate using electron-beam (e-beam) lithography and reactive-ion-etching, the PhC sensing platform allows optical detection based on resonant mode shifts in response to ambient refractive index changes produced by infiltration of target biomaterial within the holes of the PhC structure. Finite difference time domain (FDTD) calculations were performed to assist with design of the sensor, and to serve as a theoretical benchmark against which experimental results could be compared. Using Human Papillomavirus virus-like particles (VLPs) spiked in 10% fetal bovine serum as a model system, we observed a limit of detection of 1.5 nM in simple (buffer only) or complex (10% serum) sample matrices. The use of anti-VLP antibodies specific for intact VLPs with the PhC sensors provided highly selective VLP detection.

  5. A novel four-dimensional analytical approach for analysis of complex samples.

    Science.gov (United States)

    Stephan, Susanne; Jakob, Cornelia; Hippler, Jörg; Schmitz, Oliver J

    2016-05-01

    A two-dimensional LC (2D-LC) method, based on the work of Erni and Frei in 1978, was developed and coupled to an ion mobility-high-resolution mass spectrometer (IM-MS), which enabled the separation of complex samples in four dimensions (2D-LC, ion mobility spectrometry (IMS), and mass spectrometry (MS)). This approach works as a continuous multiheart-cutting LC system, using a long modulation time of 4 min, which allows the complete transfer of most of the first - dimension peaks to the second - dimension column without fractionation, in comparison to comprehensive two-dimensional liquid chromatography. Hence, each compound delivers only one peak in the second dimension, which simplifies the data handling even when ion mobility spectrometry as a third and mass spectrometry as a fourth dimension are introduced. The analysis of a plant extract from Ginkgo biloba shows the separation power of this four-dimensional separation method with a calculated total peak capacity of more than 8700. Furthermore, the advantage of ion mobility for characterizing unknown compounds by their collision cross section (CCS) and accurate mass in a non-target approach is shown for different matrices like plant extracts and coffee. Graphical abstract Principle of the four-dimensional separation.

  6. Monitoring prion protein expression in complex biological samples by SERS for diagnostic applications

    Energy Technology Data Exchange (ETDEWEB)

    Manno, D; Filippo, E; Fiore, R; Serra, A [Dipartimento di Scienza dei Materiali, Universita del Salento, Lecce (Italy); Urso, E; Rizzello, A; Maffia, M [Dipartimento di Scienze e Tecnologie Biologiche ed Ambientali, Universita del Salento, Lecce (Italy)

    2010-04-23

    Surface-enhanced Raman spectroscopy (SERS) allows a new insight into the analysis of cell physiology. In this work, the difficulty of producing suitable substrates that, besides permitting the amplification of the Raman signal, do not interact with the biological material causing alteration, has been overcome by a combined method of hydrothermal green synthesis and thermal annealing. The SERS analysis of the cell membrane has been performed with special attention to the cellular prion protein PrP{sup C}. In addition, SERS has also been used to reveal the prion protein-Cu(II) interaction in four different cell models (B104, SH-SY5Y, GN11, HeLa), expressing PrP{sup C} at different levels. A significant implication of the current work consists of the intriguing possibility of revealing and quantifying prion protein expression in complex biological samples by a cheap SERS-based method, replacing the expensive and time-consuming immuno-assay systems commonly employed.

  7. POP-ART: thermodynamically correct activated event sampling in complex materials

    Science.gov (United States)

    Chubynsky, M. V.; Vocks, Henk; Mousseau, Normand; Barkema, G. T.

    2006-03-01

    Dynamics of complex systems with a rugged energy landscape can be represented as a sequence of rare activated events during which the system jumps between different potential energy minima. The activation-relaxation technique (ART) [1] is an efficient method of sampling such events; however, because of an unknown bias in selecting these events it cannot easily provide thermodynamical information. We present a modification of ART, the properly obeying probability ART (POP-ART) [2]. POP-ART combines short molecular dynamics runs with ART-like activated moves, with an additional accept/reject step designed to satisfy detailed balance and thus reproduce correct thermodynamics. Both correctness and efficiency of the method have been tested using a variety of systems. We mention briefly some ways of extending the approach to obtain correct dynamics as well.[1] G.T. Barkema and N. Mousseau, Phys. Rev. Lett. 77, 4358 (1996)[2] H. Vocks, M.V. Chubynsky, G.T. Barkema and N. Mousseau, J. Chem. Phys., accepted

  8. Determination of atrazine in surface waters by combination of POCIS passive sampling and ELISA detection.

    Science.gov (United States)

    Cernoch, Ivo; Fránek, Milan; Diblíková, Iva; Hilscherová, Klára; Randák, Tomáš; Ocelka, Tomáš; Bláha, Luděk

    2011-09-01

    Polar organic compound integrative samplers (POCIS) in combination with instrumental techniques such as LC-MS-MS were previously used to monitor environmental pollutants but the performance of alternative immunochemical methods such as ELISA (enzyme-linked immunosorbent assay) has been explored less. In the present study, POCIS technology was applied to surface water sampling in the Czech Republic, and ELISA was used as a detection technique for the herbicide atrazine. In the first study, 28 samples from streams around small municipal waste water treatment plants (WWTPs) were collected using two different devices (POCISpest and POCISpharm) over the course of 21 days. Elevated atrazine concentrations (up to 25 ng per POCIS) were found in samples down-stream of WWTPs. This observation was also confirmed in another two year study (4 sampling periods) investigating 7 river sites around a major city of Brno as well as the inlet and outlet of the city's WWTP. High atrazine levels were systematically determined at the outlet from the WWTPs (120-605 ng per POCIS). A decreasing trend in the atrazine concentrations in rivers around the city of Brno has been observed, with the highest levels observed within the first sampling period in spring 2007 (100-600 ng per POCIS, with an extreme value of 2760 ng per POCIS). Results of the atrazine ELISA were closely correlated with LC-MS/MS, which confirmed good applicability of ELISA as a cost-effective screening tool.

  9. Determination of melamine in aquaculture feed samples based on molecularly imprinted solid-phase extraction.

    Science.gov (United States)

    Lian, Ziru; Liang, Zhenlin; Wang, Jiangtao

    2015-10-01

    This research highlights the application of highly efficient molecularly imprinted solid-phase extraction for the preconcentration and analysis of melamine in aquaculture feed samples. Melamine-imprinted polymers were synthesized employing methacrylic acid and ethylene glycol dimethacrylate as functional monomer and cross-linker, respectively. The characteristics of obtained polymers were evaluated by scanning electron microscopy, Fourier transform infrared spectroscopy and binding experiments. The imprinted polymers showed an excellent adsorption ability for melamine and were applied as special solid-phase extraction sorbents for the selective cleanup of melamine. An off-line molecularly imprinted solid-phase extraction procedure was developed for the separation and enrichment of melamine from aquaculture feed samples prior to high-performance liquid chromatography analysis. Optimum molecularly imprinted solid-phase extraction conditions led to recoveries of the target in spiked feed samples in the range 84.6-96.6% and the relative standard deviation less than 3.38% (n = 3). The aquaculture feed sample was determined, and there was no melamine found. The results showed that the molecularly imprinted solid-phase extraction protocols permitted the sensitive, uncomplicated and inexpensive separation and pre-treatment of melamine in aquaculture feed samples.

  10. Evaluation of sampling devices for the determination of polycyclic aromatic hydrocarbons in surface microlayer coastal waters.

    Science.gov (United States)

    Guitart, C; García-Flor, N; Dachs, J; Bayona, J M; Albaigés, J

    2004-05-01

    The sea surface microlayer (SML) may play an important role on the transport and fate of persistent organic pollutants in the marine environment. In order to evaluate the appropriateness of a number of sampling devices for the analysis of 14 parent polycyclic aromatic hydrocarbons (3-5 aromatic rings), marine SML waters were sampled using a glass plate, a rotating drum/roller, a metal screen and a surface slick sampler. The underlying waters were also sampled for the determination of the corresponding enrichment factors (EF = [C](microlayer)/[C](underlying water)). The EFs were phase dependent, ranging from 1 to 3 for the dissolved phase and between 4 and 7 for the particulate phase. In order to better assess the performance of the different sampling methods, in terms of phase partitioning, the truly dissolved and colloidal phases were also estimated. Generally, no significant differences were found for the enrichment factors provided by the different methods, due to the observed large variability in concentrations that can be attributed to small-scale coastal processes. However, the metal screen is recommended as the most efficient sampling method for the study of PAHs taking into account the amount of water collected versus time.

  11. Rapid and reliable determination of the halogenating peroxidase activity in blood samples.

    Science.gov (United States)

    Flemmig, Jörg; Schwarz, Pauline; Bäcker, Ingo; Leichsenring, Anna; Lange, Franziska; Arnhold, Jürgen

    2014-12-15

    By combining easy and fast leukocyte enrichment with aminophenyl-fluorescein (APF) staining we developed a method to quickly and specifically address the halogenating activity of the immunological relevant blood heme peroxidases myeloperoxidase and eosinophil peroxidase, respectively. For leukocyte enrichment a two-fold hypotonic lysis procedure of the blood with Millipore water was chosen which represents a cheap, fast and reliable method to diminish the amount of erythrocytes in the samples. This procedure is shown to be suitable both to human and murine blood micro-samples, making it also applicable to small animal experiments with recurring blood sampling. As all types of leukocytes are kept in the sample during the preparation, they can be analysed separately after discrimination during the flow cytometry analysis. This also holds for all heme peroxidase-containing cells, namely neutrophils, eosinophils and monocytes. Moreover additional parameters (e.g. antibody staining) can be combined with the heme peroxidase activity determination to gain additional information about the different immune cell types. Based on previous results we applied APF for specifically addressing the halogenating activity of leukocyte peroxidases in blood samples. This dye is selectively oxidized by the MPO and EPO halogenation products hypochlorous and hypobromous acid. This approach may provide a suitable tool to gain more insights into the immune-physiological role of the halogenating activity of heme peroxidases.

  12. Slurry sampling graphite furnace atomic absorption spectrometry: determination of trace metals in mineral coal.

    Science.gov (United States)

    Silva, M M; Goreti, M; Vale, R; Caramão, E B

    1999-12-06

    A procedure for lead, cadmium and copper determination in coal samples based on slurry sampling using an atomic absorption spectrometer equipped with a transversely heated graphite tube atomizer is proposed. The slurries were prepared by weighing the samples directly into autosampler cups (5-30 mg) and adding a 1.5 ml aliquot of a diluent mixture of 5% v/v HNO(3), 0.05% Triton X-100 and 10% ethanol. The slurry was homogenized by manual stirring before measurement. Slurry homogenization using ultrasonic agitation was also investigated for comparison. The effect of particle size and the use of different diluent compositions on the slurry preparation were investigated. The temperature programmes were optimized on the basis of pyrolysis and atomization curves. Absorbance characteristics with and without the addition of a palladium-magnesium modifier were compared. The use of 0.05% m/v Pd and 0.03% m/v Mg was found satisfactory for stabilizing Cd and Pb. The calibration was performed with aqueous standards. In addition, a conventional acid digestion procedure was applied to verify the efficiency of the slurry sampling. Better recoveries of the analytes were obtained when the particle size was reduced to <37 mum. Several certified coal reference materials (BCR Nos. 40, 180, and 181) were analyzed, and good agreement was obtained between the results from the proposed slurry sampling method and the certificate values.

  13. Determination of Metal Impurities in Carbon Nanotubes Sampled Using Surface Wipes

    Directory of Open Access Journals (Sweden)

    Mary-Luyza Avramescu

    2016-01-01

    Full Text Available Residual metal impurities in carbon nanotubes (CNTs provide a means to distinguish CNT from non-CNT sources of elemental carbon in environmental samples. A practical and cost-effective analytical approach is needed to support routine surface monitoring of CNT metal tracers using wipe sampling. Wipe sampling for CNT metal tracers is considered a qualitative indicator of the presence of CNTs, not a quantitative exposure metric. In this study, two digestion approaches (microwave-assisted nitric acid/H2O2 digestion and ultrasonic nitric/HF acid digestion in conjunction with Inductively Coupled Plasma Mass Spectrometry (ICP-MS determination were evaluated for their ability to extract metal impurities from CNT particles captured on wipe substrates. Aliquots of different carbon nanotubes (including NIST 2483 single-wall CNT with and without GhostWipes™ (ASTM E-1792 compliant were used to compare the performance of the digestion methods. The microwave digestion method accommodated the bulky wipe sample and also eliminated potential ICP-MS signal interferences related to incomplete digestion. Although quantitative recoveries requiring lengthy multistep digestion protocols may be necessary in other applications, the near-total recoveries achieved in the present study for CNT catalyst elements were adequate for identifying surface contamination of CNTs in the workplace using wipe sampling.

  14. Analysis of volatile organic compounds in compost samples: A potential tool to determine appropriate composting time.

    Science.gov (United States)

    Zhu, Fengxiang; Pan, Zaifa; Hong, Chunlai; Wang, Weiping; Chen, Xiaoyang; Xue, Zhiyong; Yao, Yanlai

    2016-12-01

    Changes in volatile organic compound contents in compost samples during pig manure composting were studied using a headspace, solid-phase micro-extraction method (HS-SPME) followed by gas chromatography with mass spectrometric detection (GC/MS). Parameters affecting the SPME procedure were optimized as follows: the coating was carbon molecular sieve/polydimethylsiloxane (CAR/PDMS) fiber, the temperature was 60°C and the time was 30min. Under these conditions, 87 compounds were identified from 17 composting samples. Most of the volatile components could only be detected before day 22. However, benzenes, alkanes and alkenes increased and eventually stabilized after day 22. Phenol and acid substances, which are important factors for compost quality, were almost undetectable on day 39 in natural compost (NC) samples and on day 13 in maggot-treated compost (MC) samples. Our results indicate that the approach can be effectively used to determine the composting times by analysis of volatile substances in compost samples. An appropriate composting time not only ensures the quality of compost and reduces the loss of composting material but also reduces the generation of hazardous substances. The appropriate composting times for MC and NC were approximately 22days and 40days, respectively, during the summer in Zhejiang.

  15. Kinetic spectrophotometric method for the determination of morphine in biological samples

    Science.gov (United States)

    Sheibani, A.; Shishehbore, M. Reza; Mirparizi, E.

    2010-10-01

    In this paper a simple, selective and inexpensive kinetic method was developed for the determination of morphine based on its inhibitory effect on the Janus green-bromate system in sulfuric acid media. The reaction was monitored spectrophotometrically at 618 nm by a fixed time method. The effect of different parameters such as concentration of reactants and temperature on the rate of reaction was investigated and optimum conditions were obtained. The calibration curve was linear in the concentration range 0.07-7.98 mg L -1 of morphine, and detection limit of the method was 3.0 × 10 -2 mg L -1. The relative standard deviation for five determinations of 3.74 mg L -1 of morphine was 0.57%. Finally, the proposed method was successfully applied to the determination of morphine in human urine and serum as real samples.

  16. Determination of trace impurities in titanium dioxide by direct solid sampling electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Docekal, Bohumil [Institute of Analytical Chemistry, Academy of Sciences of the Czech Republic, Veveri 97, CZ-61142, Brno (Czech Republic)], E-mail: docekal@iach.cz; Vojtkova, Blanka [Institute of Materials Science, Faculty of Chemistry, Brno University of Technology, Purkynova 118, CZ-61200 Brno (Czech Republic)

    2007-03-15

    A true direct solid sampling electrothermal atomic absorption spectrometry method with Zeeman-effect background correction (Analytik Jena ZEEnit 60 AAS) was developed for the determination of As, Cd, Hg, Pb, Sb and Zn in powdered titanium dioxide of pharmaceutical, food and cosmetics grade. The interaction of the titanium matrix and graphite surface of the sample carrier boat in a transversely heated graphite tube atomizer was investigated. Conversion of titanium dioxide to interfering TiO{sub 2}-TiC-liquid phase, running out the sampling boat, was observed at temperatures above 2000 deg. C. The temperature program was optimized accordingly for these volatile analytes in atomization and cleaning steps in order to prevent this interference and to prolong significantly the analytical lifetime of the boat to more than one thousand runs. For all elements, calibration by aqueous standard addition method, by wet-chemically analyzed samples with different content of analytes and/or by dosing one sample in different amounts, were proved as adequate quantification procedures. Linear dynamic calibration working ranges can be considerably expanded up to two orders of magnitude within one measurement run by applying three-field dynamic mode of the Zeeman background correction system. The results obtained by true direct solid sampling technique are compared with those of other independent, mostly wet-chemical methods. Very low limits of detection (3{sigma} criterion) of true solid sampling technique of 21, 0.27, 24, 3.9, 6.3 and 0.9 ng g{sup -1} were achieved for As, Cd, Hg, Pb, Sb and Zn, respectively.

  17. An asixymmetric diffusion experiment for the determination of diffusion and sorption coefficients of rock samples

    Energy Technology Data Exchange (ETDEWEB)

    Takeda, M.; Hiratsuka, T.; Ito, K.; Finsterle, S.

    2011-02-01

    Diffusion anisotropy is a critical property in predicting migration of substances in sedimentary formations with very low permeability. The diffusion anisotropy of sedimentary rocks has been evaluated mainly from laboratory diffusion experiments, in which the directional diffusivities are separately estimated by through-diffusion experiments using different rock samples, or concurrently by in-diffusion experiments in which only the tracer profile in a rock block is measured. To estimate the diffusion anisotropy from a single rock sample, this study proposes an axisymmetric diffusion test, in which tracer diffuses between a cylindrical rock sample and a surrounding solution reservoir. The tracer diffusion between the sample and reservoir can be monitored from the reservoir tracer concentrations, and the tracer profile could also be obtained after dismantling the sample. Semi-analytical solutions are derived for tracer concentrations in both the reservoir and sample, accounting for an anisotropic diffusion tensor of rank two as well as the dilution effects from sampling and replacement of reservoir solution. The transient and steady-state analyses were examined experimentally and numerically for different experimental configurations, but without the need for tracer profiling. These experimental configurations are tested for in- and out-diffusion experiments using Koetoi and Wakkanai mudstones and Shirahama sandstone, and are scrutinized by a numerical approach to identify favorable conditions for parameter estimation. The analysis reveals the difficulty in estimating diffusion anisotropy; test configurations are proposed for enhanced identifiability of diffusion anisotropy. Moreover, it is demonstrated that the axisymmetric diffusion test is efficient in obtaining the sorption parameter from both steady-state and transient data, and in determining the effective diffusion coefficient if isotropic diffusion is assumed. Moreover, measuring reservoir concentrations in an

  18. Determination of Kinetic Isotope Effects in Yeast Alcohol Dehydrogenase Using Transition Path Sampling

    Science.gov (United States)

    Varga, Matthew; Schwartz, Steven

    2015-03-01

    The experimental determination of kinetic isotope effects in enzymatic systems can be a difficult, time-consuming, and expensive process. In this study, we use the Chandler-Bolhius method for the determination of reaction rates within transition path sampling (rTPS) to determine the primary kinetic isotope effect in yeast alcohol dehydrogenase (YADH). In this study, normal mode centroid molecular dynamics (CMD) was applied to the transferring hydride/deuteride in order to correctly incorporate quantum effects into the molecular simulations. Though previous studies have used rTPS to calculate reaction rate constants in various model and real systems, it has not been applied to a system as large as YADH. Due to the fact that particle transfer is not wholly indicative of the chemical step, this method cannot be used to determine reaction rate constants in YADH. However, it is possible to determine the transition rate constant of the particle transfer, and the kinetic isotope effect of that step. This method provides a set of tools to determine kinetic isotope effects with the atomistic detail of molecular simulations.

  19. Uncertainty analysis of point-by-point sampling complex surfaces using touch probe CMMs DOE for complex surfaces verification with CMM

    DEFF Research Database (Denmark)

    Barini, Emanuele Modesto; Tosello, Guido; De Chiffre, Leonardo

    2010-01-01

    The paper describes a study concerning point-by-point sampling of complex surfaces using tactile CMMs. A four factor, two level completely randomized factorial experiment was carried out, involving measurements on a complex surface configuration item comprising a sphere, a cylinder and a cone......, combined in a single assembly. An investigation into the source and effects of different uncertainty contributors during this complex surface measurement was carried out. The factors involved were machine. probe, operator, and procedure dependent. The results obtained from the experiments were analysed...

  20. Spectrofluorometric determination of trace amounts of coenzyme II using norfioxacin-terbium complex as a fluorescent probe.

    Science.gov (United States)

    Wang, Yusheng; Liu, Jinkai; Jiang, Chongqiu

    2005-06-01

    When terbium ion (Tb3+)-norfloxacin (NFLX) complex is issued a fluorescent probe, in a buffer solution of pH = 7.6, NADP can remarkably enhance the fluorescence intensity of the Tb3+ -NFLX complex at lambda = 545 nm. The enhanced fluorescence intensity of Tb3+ is in proportion to the concentration of NADP. The dynamic range for the determination of NADP is 1.11 x 10(-7) - 6.16 x 10(-5) mol l(-1), with a detection limit of 4.31 x 10(-8) mol l(-1). This method is simple, practical and relatively free of interference from coexisting substances, so it can be successfully applied to determination of NADP in synthetic water samples.

  1. Determination of colloidal and dissolved silver in water samples using colorimetric solid-phase extraction.

    Science.gov (United States)

    Hill, April A; Lipert, Robert J; Porter, Marc D

    2010-03-15

    The increase in bacterial resistance to antibiotics has led to resurgence in the use of silver as a biocidal agent in applications ranging from washing machine additives to the drinking water treatment system on the International Space Station (ISS). However, growing concerns about the possible toxicity of colloidal silver to bacteria, aquatic organisms and humans have led to recently issued regulations by the US EPA and FDA regarding the usage of silver. As part of an ongoing project, we have developed a rapid, simple method for determining total silver, both ionic (silver(I)) and colloidal, in 0.1-1mg/L aqueous samples, which spans the ISS potable water target of 0.3-0.5mg/L (total silver) and meets the US EPA limit of 0.1mg/L in drinking water. The method is based on colorimetric solid-phase extraction (C-SPE) and involves the extraction of silver(I) from water samples by passage through a solid-phase membrane impregnated with the colorimetric reagent DMABR (5-[4-(dimethylamino)benzylidene]rhodanine). Silver(I) exhaustively reacts with impregnated DMABR to form a colored compound, which is quantified using a handheld diffuse reflectance spectrophotometer. Total silver is determined by first passing the sample through a cartridge containing Oxone, which exhaustively oxidizes colloidal silver to dissolved silver(I). The method, which takes less than 2 min to complete and requires only approximately 1 mL of sample, has been validated through a series of tests, including a comparison with the ICP-MS analysis of a water sample from ISS that contained both silver(I) and colloidal silver. Potential earth-bound applications are also briefly discussed.

  2. Embedded Measures of Performance Validity in the Rey Complex Figure Test in a Clinical Sample of Veterans.

    Science.gov (United States)

    Sugarman, Michael A; Holcomb, Erin M; Axelrod, Bradley N; Meyers, John E; Liethen, Philip C

    2016-01-01

    The purpose of this study was to determine how well scores from the Rey Complex Figure Test (RCFT) could serve as embedded measures of performance validity in a large, heterogeneous clinical sample at an urban-based Veterans' Affairs hospital. Participants were divided into credible performance (n = 244) and noncredible performance (n = 87) groups based on common performance validity tests during their respective clinical evaluations. We evaluated how well preselected RCFT scores could discriminate between the 2 groups using cut scores from single indexes as well as multivariate logistic regression prediction models. Additionally, we evaluated how well memory error patterns (MEPs) could discriminate between the 2 groups. Optimal discrimination occurred when indexes from the Copy and Recognition trials were simultaneous predictors in logistic regression models, with 91% specificity and at least 53% sensitivity. Logistic regression yielded superior discrimination compared with individual indexes and compared with the use of MEPs. Specific scores on the RCFT, including the Copy and Recognition trials, can serve as adequate indexes of performance validity, when using both cut scores and logistic regression prediction models. We provide logistic regression equations that can be applied in similar clinical settings to assist in determining performance validity.

  3. Presence and significant determinants of cognitive impairment in a large sample of patients with multiple sclerosis.

    Directory of Open Access Journals (Sweden)

    Martina Borghi

    Full Text Available OBJECTIVES: To investigate the presence and the nature of cognitive impairment in a large sample of patients with Multiple Sclerosis (MS, and to identify clinical and demographic determinants of cognitive impairment in MS. METHODS: 303 patients with MS and 279 healthy controls were administered the Brief Repeatable Battery of Neuropsychological tests (BRB-N; measures of pre-morbid verbal competence and neuropsychiatric measures were also administered. RESULTS: Patients and healthy controls were matched for age, gender, education and pre-morbid verbal Intelligence Quotient. Patients presenting with cognitive impairment were 108/303 (35.6%. In the overall group of participants, the significant predictors of the most sensitive BRB-N scores were: presence of MS, age, education, and Vocabulary. The significant predictors when considering MS patients only were: course of MS, age, education, vocabulary, and depression. Using logistic regression analyses, significant determinants of the presence of cognitive impairment in relapsing-remitting MS patients were: duration of illness (OR = 1.053, 95% CI = 1.010-1.097, p = 0.015, Expanded Disability Status Scale score (OR = 1.247, 95% CI = 1.024-1.517, p = 0.028, and vocabulary (OR = 0.960, 95% CI = 0.936-0.984, p = 0.001, while in the smaller group of progressive MS patients these predictors did not play a significant role in determining the cognitive outcome. CONCLUSIONS: Our results corroborate the evidence about the presence and the nature of cognitive impairment in a large sample of patients with MS. Furthermore, our findings identify significant clinical and demographic determinants of cognitive impairment in a large sample of MS patients for the first time. Implications for further research and clinical practice were discussed.

  4. Phosphite determination in fertilizers after online sequential sample preparation in a flow injection system.

    Science.gov (United States)

    Dametto, Patrícia Roberta; Franzini, Vanessa Pezza; Gomes Neto, José Anchieta

    2007-07-25

    A flow injection spectrophotometric system is proposed for phosphite determination in fertilizers by the molybdenum blue method after the processing of each sample two times on-line without and with an oxidizing step. The flow system was designed to add sulfuric acid or permanganate solutions alternately into the system by simply displacing the injector-commutator from one resting position to another, allowing the determination of phosphate and total phosphate, respectively. The concentration of phosphite is obtained then by difference between the two measurents. The influence of flow rates, sample volume, and dimension of flow line connecting the injector-commutator to the main analytical channel was evaluated. The proposed method was applied to phosphite determination in commercial liquid fertilizers. Results obtained with the proposed FIA system were not statistically different from those obtained by titrimetry at the 95% confidence level. In addition, recoveries within 94 and 100% of spiked fertilizers were found. The relative standard deviation (n = 12) related to the phosphite-converted-phosphate peak alone was sampling rate was calculated as 15 determinations per hour, and the reagent consumption was about 6.3 mg of KMnO4, 200 mg of (NH4)6Mo7O24.4H2O, and 40 mg of ascorbic acid per measurement.

  5. Evaluation of the hyplex® TBC PCR test for detection of Mycobacterium tuberculosis complex in clinical samples

    Directory of Open Access Journals (Sweden)

    Hoffmann Harald

    2010-03-01

    Full Text Available Abstract Background Tuberculosis (TB is one of the major public health concerns worldwide. The detection of the pathogen Mycobacterium tuberculosis complex (MTBC as early as possible has a great impact on the effective control of the spread of the disease. In our study, we evaluated the hyplex® TBC PCR test (BAG Health Care GmbH, a novel assay using a nucleic acid amplification technique (NAAT with reverse hybridisation and ELISA read out for the rapid detection of M. tuberculosis directly in clinical samples. Results A total of 581 respiratory and non-respiratory specimens from our pneumological hospital and the National TB Institute of Uzbekistan were used for the evaluation of the PCR assay. Of these, 292 were classified as TB samples and 289 as non-TB samples based on the results of the TB cultures as reference method. The PCR results were initially used to optimise the cut-off value of the hyplex® TBC test system by means of a ROC analysis. The overall sensitivity of the assay was determined to be 83.1%. In smear-positive TB samples, the sensitivity of the hyplex® TBC PCR test was estimated to 93.4% versus 45.1% in smear-negative samples. The specificity of the test was 99.25%. Of the two specimens (0.75% with false-positive PCR results, one yielded a culture positive for non-tuberculous mycobacteria. Based on the assumption of a prevalence of 8% TB positives among the samples in our diagnostic TB laboratory, the positive and negative predictive values were estimated to 90.4% and 98.5%, respectively. Conclusions The hyplex® TBC PCR test is an accurate NAAT assay for a rapid and reliable detection of M. tuberculosis in various respiratory and non-respiratory specimens. Compared to many other conventional NAAT assays, the hyplex® TBC PCR test is in a low price segment which makes it an attractive option for developing and emerging countries with high TB burdens.

  6. A Simple Spectrofluorimetric Method Based on Quenching of a Nickel(II)-Phthalocyanine Complex to Determine Iron (III).

    Science.gov (United States)

    Çağlar, Yasemin; Saka, Ece Tuğba; Alp, Hakan; Kantekin, Halit; Ocak, Ümmühan; Ocak, Miraç

    2016-07-01

    A new nickel(II)-phthalocyanine complex (NiPc) was synthesized and used as a fluorescent ligand in determination of iron in real samples. The NiPc compound, when excited at 350 nm, decreases of emission with increases of the iron(III) concentration at 425 nm were used analytical response in a modified standard addition method. The method was validated by analyzing two certified reference materials (CRM-SA-C Sandy Soil C and Mixed Polish Herbs (INCT-MPH-2). Food and drug samples were digested in a closed microwave system using nitric acid and hydrogen peroxide. Therefore, all iron in the samples converted to iron(III) ion. These solutions were used directly in determination of iron(III) ion. No cleanup or enrichment of the solutions was required. The calibration graph was linear until 14.00 μg mL(-1). Detection limit and quantification limit were 1.29 μg mL(-1) and 3.88 μg mL(-1), respectively. The method provided accurate results for the majority of the food samples tested, including spanich, dill, mint, purslane, rocket, red lentils, dry beans and two iron medicinal tablets. Also, the high recovery (95.6 %) was obtained for a fortified stream water sample. The simple and cost-effective method is suitable for monitoring total iron concentration in foods and drug samples.

  7. Preweighting method in Monte-Carlo sampling with complex action --- Strong-Coupling Lattice QCD with $1/g^2$ corrections, as an example ---

    CERN Document Server

    Ohnishi, Akira

    2015-01-01

    We investigate the QCD phase diagram in the strong-coupling lattice QCD with fluctuation and $1/g^2$ effects by using the auxiliary field Monte-Carlo simulations. The complex phase of the Fermion determinant at finite chemical potential is found to be suppressed by introducing a complex shift of integral path for one of the auxiliary fields, which corresponds to introducing a repulsive vector mean field for quarks. The obtained phase diagram in the chiral limit shows suppressed $T_c$ in the second order phase transition region compared with the strong-coupling limit results. We also argue that we can approximately guess the statistical weight cancellation from the complex phase in advance in the case where the complex phase distribution is Gaussian. We demonstrate that correct expectation values are obtained by using this guess in the importance sampling (preweighting).

  8. Williams Test Required Sample Size For Determining The Minimum Effective Dose

    Directory of Open Access Journals (Sweden)

    Mustafa Agah TEKINDAL

    2016-04-01

    Full Text Available Objective: The biological activity of a substance may be explored through a series of experiments on increased or decreased doses of such substance. One of the purposes in studies of this sort is the determination of minimum effective dose. Use of appropriate sample size has an indisputable effect on the reliability of the decisions made in studies made for this purpose. This study attempts to provide a summary of sample sizes, in different scenarios, needed by researchers during the use of Williams test by taking into consideration the number of groups in dose-response studies as well as minimal clinically significant difference, standard deviation, and the test’s power through asymptotic power analyses. Material and Methods: When Type I error was taken as 0.05, scenarios were determined in different sample sizes for each group (5 to 100 with an increase of 5 at a time and different numbers of groups (from 3 to 10, with an increase of 1 at a time. Minimal clinically significant difference refers to the difference between the control group and the experimental group. In this instance, when the control group is zero and takes a specific average value, it refers to the difference from the experimental group. In the resent study, such differences are defined from 1 to 10 with an increase of 1 at a time. For the test’s power would change when the standard deviation changed, the relevant value was changed in all scenarios from 1 to 10 with an increase of 1 at a time to explore the test’s power. Dose-response distributions are skew. In the present study, data were derived from the Poisson distribution with λ= 1 parameter that was determined in accordance with dose-response curves. Results: When changes occurring in the determined scenarios are considered, it can be said, in general, that the significant difference must be set between 1 and 3; and standard deviation must be set between 1 and 2. Conclusion: It is certain that change in the number

  9. Determination of radioactivity levels and hazards of soil and sediment samples in Firtina Valley (Rize, Turkey)

    Energy Technology Data Exchange (ETDEWEB)

    Kurnaz, A.; Kuecuekoemeroglu, B. [Department of Physics, Faculty of Arts and Sciences, Karadeniz Technical University, Trabzon, TR 61080 (Turkey); Keser, R.; Okumusoglu, N.T.; Korkmaz, F. [Department of Physics, University of Rize, Rize, TR 53100 (Turkey); Karahan, G. [Cekmece Nuclear Research and Training Center P.O. Box 1, Atatuerk Airport, Istanbul, TR 34381 (Turkey); Cevik, U. [Department of Physics, Faculty of Arts and Sciences, Karadeniz Technical University, Trabzon, TR 61080 (Turkey)], E-mail: ugurc@ktu.edu.tr

    2007-11-15

    The natural radioactivity levels in soil and sediment samples of Firtina Valley have been determined. To our knowledge, there seems to be no information about radioactivity level in the Firtina Valley soils and sediments so far. For this reason, soil and sediment samples were collected along the Firtina Valley and analysis on the collected samples were carried out to determine {sup 238}U, {sup 232}Th, {sup 40}K and {sup 137}Cs radioisotopes using high purity germanium detector. The activity concentrations obtained for {sup 226}Ra, {sup 214}Pb, {sup 214}Bi, {sup 228}Ac, {sup 208}Tl, {sup 40}K and {sup 137}Cs are given in the unit of Bq/kg. The results have been compared with other radioactivity measurements in different country's soils and sediments. The radium equivalent activity (Ra{sub eq}), the absorbed dose rate (D), the external hazard index (H{sub ex}), the annual gonadal dose equivalent (AGDE) and the annual effective dose equivalent (AEDE) were also calculated and compared with the international recommended values.

  10. Stripping Chronopotentiometry: An Alternative Method for the Determination of Gold in Geological Samples

    Directory of Open Access Journals (Sweden)

    Nipaporn MEEPUN

    2010-01-01

    Full Text Available A stripping chronopotentiometric method was developed for reliable determination of gold in geological samples. Gold in gold ore and steam sediment samples was determined by constant current film stripping chronopotentiometry at a bare glassy carbon working electrode. The following optimum conditions were obtained: 0.5 M hydrochloric acid as a supporting electrolyte, an electrolysis potential of –0.6 V vs. saturated calomel electrode (SCE, an electrolysis time of 2 min and a constant oxidative current of +4 μA. A linear concentration range was obtained from 1.0 to 20 mg/l. The detection limit was 0.27 mg/l (n = 10 and the relative a standard deviations of 1.0 mg/l Au(III was 2.8 % (n = 10. In order to check the analytical accuracy, standard solution was spiked in a sample and the recoveries were found at 100.1 to 105.8 %. The results revealed that the quantity of gold in gold ore and sediment were 0.6 to 3.3 % and 0.9 to 1.2 %, respectively.

  11. Screening and determination of sulphonamide residues in bovine milk samples using a flow injection system.

    Science.gov (United States)

    Fernandes, Flávio Cesar Bedatty; Silva, Aline Santana; Rufino, José Luiz; Pezza, Helena Redigolo; Pezza, Leonardo

    2015-01-01

    A new, simple, rapid and sensitive flow injection spectrophotometric method was developed for the screening and determination of sulphonamides in bovine milk samples. The method is based on the condensation of sulphathiazole, sulphamethazine, and sulphadimethoxine with p-dimethylaminobenzaldehyde (p-DAB) in acid medium, in the presence of sodium dodecyl sulphate (SDS), producing a yellow compound (λmax=465 nm). Optimisation of the experimental parameters was performed using a multivariate methodology. The linear range was 90-500 μg/L and the limits of detection and quantification were in the ranges 25-29 μg/L and 84-88 μg/L, respectively. The procedure was applied for the determination of sulphonamide antibiotics in bovine milk samples submitted to a prior extraction procedure based on QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) methodology. Recoveries of 60.5-70.5% were achieved for milk samples spiked with 0.09, 0.1, 0.2, and 0.3 μg/g of each sulphonamide.

  12. Determination of trace elements in refined gold samples by inductively coupled plasma atomic emission spectrometry

    Directory of Open Access Journals (Sweden)

    Steharnik Mirjana

    2013-01-01

    Full Text Available This paper presents a method for determination the trace contents of silver, copper, iron, palladium, zinc and platinum in refined gold samples. Simultaneous inductively coupled plasma atomic emission spectrometer with radial torch position and cross flow nebulizer was used for determination. In order to compare the different calibration strategies, two sets of calibration standards were prepared. The first set was based on matrix matched calibration standards and the second was prepared without the addition of matrix material. Detection limits for matrix matching calibrations were higher for some elements than those without matrix matching. In addition, the internal standardization method was applied and experiments indicated that indium was the best option as internal standard. The obtained results for gold sample by matrix matching and matrix free calibrations were compared with the obtained results by standard addition method. The accuracy of the methods was tested performing recovery test. Recoveries for spiked sample were in the range of 90-115 %. The accuracy of the methods was also tested by analysis of certified reference material of high pure goldAuGHP1. The best results were achieved by matrix free calibration and standard addition method using indium as internal standard at wavelength of 230 nm. [Projekat Ministarstva nauke Republike Srbije, br. 34024: Development of Technologies for Recycling of Precious, Rare and Associated Metals from Solid Waste in Serbia to High Purity Products

  13. Applications of a DAD-HPLC method for determination of loratadine on biological samples

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    Pavalache Georgeta

    2015-06-01

    Full Text Available The aim of research is to assess the active substance by a HPLC method for the separation and quantitative determination of loratadine. The method has been developed and validated on the standard solutions, in previous research. The current study was undertaken to present the results obtained from loratadine determination in biological samples (human serum, urine and breast milk. These results may be applicable on patients with different physiological conditions (aging, pregnancy or recently giving birth, etc. and pathological conditions which may interfere with the metabolism of loratadine. The used HPLC method detected loratadine concentrations in human serum samples, respectively urine samples, at 2 hours after drug administration. The method detected traces of loratadine which passed into breast milk, as well. Data were statistically interpreted using MED CALC 10.2 software. These results show that the applied method can be used for quantitative analysis of loratadine in biological fluids (all permissible limits of quality specifications being in the range 95- 105%.

  14. Resonance light scattering determination of metallothioneins using levofloxacin-palladium complex as a light scattering probe

    Science.gov (United States)

    Xue, Jin-Hua; Qian, Qiu-Mei; Wang, Yong-Sheng; Meng, Xia-Ling; Liu, Lu

    2013-02-01

    A novel method of resonance light scattering (RLS) was developed for the analysis of trace metallothioneins (MTs) in human urine. In a CH3COOH-CH3COONa buffer solution of pH 4.5, the formation of a complex between levofloxacin (LEV)-Pd and MTs led to enhance the RLS intensity of the system, and the enhanced RLS intensity at 468 nm was proportional to the concentration of MTs in the range of 0.059-22.4 μg mL-1. The linear regression equation was ΔI = 127.5 ρ (μg mL-1)-88.02 with a correlation coefficient of 0.9992, and the detection limit of 17.8 ng mL-1. The relative standard deviation and the average recovery were 3.8-5.4% (n = 11) and 92.15%, respectively. The proposed method is convenient, reliable and sensitive, and has been used successfully for the determination of trace MTs in human urine samples.

  15. Determination of tetracycline in milk by using nucleotide/lanthanide coordination polymer-based ternary complex.

    Science.gov (United States)

    Tan, Hongliang; Ma, Chanjiao; Song, Yonghai; Xu, Fugang; Chen, Shouhui; Wang, Li

    2013-12-15

    The meta-organic coordination polymers have been emerged as fascinating nanomaterials because of their tunable nature. In this work, we employed lanthanide coordination polymer self-assembled from adenosine monophosphate (AMP) and europium ion (Eu(3+)) as receptor reagent and citrate (Cit) as ancillary ligand to construct a fluorescent sensor for the detection of tetracycline (Tc) in milk. The co-coordination of Cit and Tc with Eu(3+) on the surface of the coordination polymer AMP/Eu leads to the formation of ternary complex which emitted strong fluorescence due to the removal of coordinated water molecules and an intramolecular energy transfer from Tc to Eu(3+). The fluorescent intensity of Eu(3+) displayed a good linear response to Tc concentrations in the range of 0.1-20 μM with a detection limit of 60 nM. This method was successfully applied to determine the levels of Tc in milk, which is the first application of coordination polymer as a fluorescent sensor in real sample. Compared with other Eu(3+)-based fluorescent methods for Tc detection, the presented method allows simple, direct analysis of Tc without requiring special reaction media or complicated prepreparation processes. This straightforward strategy could be extended to the preparation of other lanthanide coordination polymer-based fluorescent probes for applications in biosensing, imaging, drug delivery, and so on. Copyright © 2013 Elsevier B.V. All rights reserved.

  16. Speciation of potential anti-diabetic vanadium complexes in real serum samples.

    Science.gov (United States)

    Sanna, Daniele; Ugone, Valeria; Serra, Maria; Garribba, Eugenio

    2017-08-01

    In this work the speciation in real serum samples of five V(IV)O complexes with potential application in the therapy of diabetes was studied through EPR spectroscopy as a function of V concentration (45.4, 90.9 and 454.5μM) and time (0-180min). [VO(dhp)2], [VO(ma)2], [VO(acac)2], [VO(pic)2(H2O)], and [VO(mepic)2], where Hdhp indicates 1,2-dimethyl-3-hydroxy-4(1H)-pyridinone, Hma maltol, Hacac acetylacetone, Hpic picolinic acid, and Hmepic 6-methylpicolinic acid, were examined. The distribution of V(IV)O(2+) among the serum bioligands was calculated from the thermodynamic stability constants in the literature and compared with the experimental results. EPR results, which confirm the prediction, depend on the strength of the ligand L and geometry assumed by the bis-chelated species at physiological pH, cis-octahedral or square pyramidal. With dhp, the strongest chelator, the system is dominated by [VO(dhp)2] and/or cis-VO(dhp)2(Protein); with intermediate strength chelators, i.e. maltolate, acetylacetonate and picolinate, by cis-VO(ma)2(Protein), [VO(acac)2] or [VO(pic)(citrH-1)](3-)/[VO(pic)(lactH-1)](-) (citr=citrate and lact=lactate) when the V concentration overcomes 100-200μM and by (VO)(hTf)/(VO)2(hTf) when concentration is lower than 100μM; with the weakest chelator, 6-methylpicolinate, (VO)(hTf)/(VO)2(hTf), (VO)(HSA) (hTf = human serum transferrin and HSA = human serum albumin), and VO(mepic)(Protein)(OH) are the major species at concentration higher than 100-200μM, whereas hydrolytic processes are observed for lower concentrations. For [VO(dhp)2], [VO(ma)2], [VO(acac)2] and [VO(pic)2(H2O)], the EPR spectra remain unaltered with elapsing time, while for mepic they change significantly because the hydrolyzed V(IV)O species are complexed by the serum bioligands, in particular by lactate. The rate of oxidation in the serum is [VO(dhp)2]>[VO(ma)2]>[VO(acac)2] and reflects the order of E1/2 values. Copyright © 2017 Elsevier Inc. All rights reserved.

  17. Sensitive determination of trace mercury by UV-visible diffuse reflectance spectroscopy after complexation and membrane filtration-enrichment.

    Science.gov (United States)

    Yin, Changhai; Iqbal, Jibran; Hu, Huilian; Liu, Bingxiang; Zhang, Lei; Zhu, Bilin; Du, Yiping

    2012-09-30

    A simple, sensitive and selective solid phase reflectometry method is proposed for the determination of trace mercury in aqueous samples. The complexation reagent dithizone was firstly injected into the properly buffered solution with vigorous stirring, which started a simultaneous formation of nanoparticles suspension of dithizone and its complexation reaction with the mercury(II) ions to make Hg-dithizone nanoparticles. After a definite time, the mixture was filtered with membrane, and then quantified directly on the surface of the membrane by using integrating sphere accessory of the UV-visible spectrophotometer. The quantitative analysis was carried out at a wavelength of 485 nm since it yielded the largest difference in diffuse reflectance spectra before and after reaction with mercury(II).A good linear correlation in the range of 0.2-4.0 μg/L with a squared correlation coefficient (R(2)) of 0.9944 and a detection limit of 0.12 μg/L were obtained. The accuracy of the method was evaluated by the analysis of spiked mercury(II) concentrations determined using this method along with those determined by the atomic fluorescence mercury vapourmeter and the results obtained were in good agreement. The proposed method was applied to the determination of mercury in tap water and river water samples with the recovery in an acceptable range (95.7-105.3%). Copyright © 2012 Elsevier B.V. All rights reserved.

  18. Simple Sensitive Spectrophotometric Determination of Vanadium in Biological and Environmental Samples

    Directory of Open Access Journals (Sweden)

    B. Krishna Priya

    2006-01-01

    Full Text Available Novel, rapid, highly sensitive and selective spectrophotometric method for the determination of traces of vanadium (V in environmental and biological samples, pharmaceutical and steel samples was studied. The method is based on oxidation of 2,4- dinitro phenyl hydrazine(2,4-DNPH by vanadium (V followed by coupling reaction with N-(1-naphthalene-1-ylethane-1,2-diamine-dihydrochloride (NEDA in acidic medium to give red colored derivative or on oxidation of 4-Amino Pyridine by vanadium (V followed by coupling reaction with NEDA in basic medium to give pink colored derivative. The red colored derivative having an λmax 495 nm which is stable for 8 days and the pink colored derivative with 525 nm is stable for more than 7 days at 350C. Beer's law is obeyed for vanadium (V in the concentration range of 0.02 - 3.5 μg mL–1 (red derivative and 0.03 – 4.5 μg mL–1 (pink derivative at the wave length of maximum absorption. The optimum reaction conditions and other analytical parameters were investigated to enhance the sensitivity of the present method. The detailed study of various interferences made the method more selective. The proposed method was successfully applied to the analysis of vanadium in natural water samples, plant material, soil samples, synthetic mixtures, pharmaceutical samples and biological samples. The results obtained were agreed with the reported methods at the 95 % confidence level. The performance of proposed method was evaluated in terms of Student's t-test and Variance ratio f-test which indicates the significance of proposed method over reported method.

  19. METHODOLOGICAL ASPECTS OF MOLASSES SAMPLE PREPARATION IN SULFUR DIOXIDE CONTENT DETERMINING

    Directory of Open Access Journals (Sweden)

    M. I. Egorova

    2015-01-01

    Full Text Available Summary. Molasses is characterized as sugar production by-product from primary or secondary sacchariferous raw materials. The features of the appearance, the chemical composition, molasses and exit directions of its use, depending on the type of production, in which it is formed. The value of molasses is demonstrated according to its total composition as well as its use directions. Statistics on beet molasses amounts in Russia is presented. Described consumer market molasses in Russia and abroad with its exports. Shown regulations contain requirements for the quality and safety of molasses, including sulfur dioxide. The data on sulfur allergenic properties are presented. Showing source of the sulfur dioxide in the residual molasses number of processing aids and the impact of its level in the value of raw molasses for use in biotechnological processes and fodder production. The necessity to develop methodology for determining the sulfur dioxide content in the molasses to control its security. The iodometric method, which is used in practice for determination of sulphur dioxide in foods are characterized. Differences molasses and sugar as objects of iodometric determination of sulfur dioxide, which leads to the inability to ascertain the equivalence point. The variants eliminate interfering background of dark-colored foods common in analytical chemistry. Advantages and disadvantages of the background masking and stripping the determination of sulfur dioxide in the darkcolored products. It was characterized by clarifying sugar solutions in optical control methods. The hypothesis about preferability of its use in sample molasses preparation for equivalence point fixation in iodometric titration is suggested. The tasks of experimental research for the development of sample preparation algorithm molasses in determining the content of sulphurous acid.

  20. The alternative use of layered double hydroxides as extraction medium coupled with microcomplexation for determination of phosphate in water samples

    Science.gov (United States)

    Gissawong, Netsirin; Sansuk, Sira; Srijaranai, Supalax

    2017-02-01

    A simple, rapid, in situ, and green extraction combined with a microcomplexation has been developed for the spectrophotometric determination of phosphate in water samples. Through their formation, layered double hydroxides (LDHs) were employed as the extraction medium, instantly commenced by a rapid addition of a mixed solution of Mg2 + and Al3 + ions into alkaline phosphate solution. After the extraction, LDH precipitate containing phosphate was dissolved by sulfuric acid and the released phosphate was subsequently detected via its complexation with molybdate in the presence of antimonyl and ascorbic acid. Under optimum conditions, the linearity in the range of 5-200 μg L- 1, with the correlation coefficient (r2) of 0.9969, and the enrichment factor (EF) of 14 were obtained. The limit of detection (LOD) of 5 μg L- 1 and good precision, with the relative standard deviations (RSDs) less than 8.16%, were achieved. The proposed method was successfully applied to determine phosphate in water samples and the relative recoveries of 72.97-115.32% were obtained.