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Sample records for absorption spectrometric determinations

  1. Spectrofluorimetric, Atomic Absorption Spectrometric and Spectrophotometric Determination of Some Fluoroquinolones

    Hesham Salem

    2005-01-01

    Simple, accurate, sensitive and selective spectrofluorimetric, atomic absorption spectrometric and spectrophotometric methods are described for the quantitative determination of ten fluoroquinolones (amifloxacin, ciprofloxacin hydrochloride, difloxacin hydrochloride, enoxacin, enrofloxacin, lomefloxacin hydrochloride, levofloxacin, norfloxacin, ofloxacin and pefloxacin mesylate). The first method was a spectrofluorimetric method in which samples of the studied drugs in 0.1 N H2SO4 showed nati...

  2. Spectrofluorimetric, Atomic Absorption Spectrometric and Spectrophotometric Determination of Some Fluoroquinolones

    Hesham Salem

    2005-01-01

    Full Text Available Simple, accurate, sensitive and selective spectrofluorimetric, atomic absorption spectrometric and spectrophotometric methods are described for the quantitative determination of ten fluoroquinolones (amifloxacin, ciprofloxacin hydrochloride, difloxacin hydrochloride, enoxacin, enrofloxacin, lomefloxacin hydrochloride, levofloxacin, norfloxacin, ofloxacin and pefloxacin mesylate. The first method was a spectrofluorimetric method in which samples of the studied drugs in 0.1 N H2SO4 showed native fluorescence at 450 nm when excitation was at 290 nm. The calibration graph was rectilinear from 0.3-1.4 μg mL-1 (method I. Cobalt sulphate was used for precipitation of the ion associates formed from the reaction with the cited drugs. The formation and solubility of the solid complexes at the optimum conditions of pH and ionic strength values have been studied. The method depends on direct determination of the ions in the precipitate or indirect determination of the ions in the filtrate by atomic absorption spectroscopy. The optimum conditions for precipitation were carefully studied. Rectilinear calibration graphs were obtained in the range of 3-30 μg mL-1 for each of the investigated drugs. The molar ratios of the formed chelats were determined by Job's method and their association constants were also calculated (method II. Ammonium vanadate was used for the spectrophotometric determination of the selected fluoroquinolones by oxidation in sulphuric acid medium resulting in the development of a greenish blue colour measured at 766 nm which was attributed to the vanadium (IV produced by reduction of vanadium (V by the selected drugs. The optimum conditions for heating time, reagent concentration and sulphuric acid concentration were carefully studied. The accuracy and precision of the proposed method was confirmed by estimating five or six replicates within Beer's law limits were obtained in the range 10-40 μg mL-1 for each of the investigated drugs

  3. Atomic absorption spectrometric determination of mineral elements in mammalian bones

    The phosphorus content of the major bones of male and female selected mammals was determined using the yellow vanadomolybdate colorimetric method. For each animal, the bone with the highest phosphorus content was used as pilot sample. Varying concentrations of strontium were added to solutions of the ashed pilot samples to minimize phosphorus interference in the determination of calcium and magnesium using flame atomic absorption spectrophotometry operated on the air-acetylene mode. At least 6,000 ppm (0.6%) of strontium was required to give optimum results for calcium. The amount of magnesium obtained from the analysis was not affected by the addition of strontium. With the incorporation of strontium in the sample solution, all elements of interest can be determined in the same sample solution. Based on this, a procedure is proposed for the determination of calcium and other elements in bones. Average recoveries of spiked calcium and magnesium were 97.85% and 98.16%, respectively at the 95% confidence level. The coefficients of variation obtained for replicate determinations using one of the samples were 0.00% for calcium, lead and sodium, 2.93% for magnesium, 3.27% for iron and 3.92% for zinc at the concentration levels found in that sample. Results from the proposed procedure compared well with those from classical chemical methods at the 95% confidence level. It is evident that calcium phosphorus, magnesium and sodium which are the most abundant elements in the bones are distributed in varying amounts both in the different types of bones and different animal species, although the general trend is Ca > P > Na > Mg for each bone considered. The calcium - phosphorus ratio is generally 3:1. The work set out to propose an atomic absorption spectrometric method for the multi-element analysis of mammalian bones with a single sample preparation and to study the distribution pattern of these elements in the bones. (Author)

  4. Electrothermal atomization atomic absorption spectrometric determination of trace metals in uranium-plutomium fuel materials

    Atomic absorption spectrometric methods using the electrothermal mode of atomization developed for the determination of Ag, Be, Ca, Cd, Cr, Co, Cu, Fe, Li, Mn, Na, Ni, Sn and Zn in (U, Pu) solution with 4% plutonium have been described. The carbon rod atomizer has been adapted for glove box operation to enable handling of plutonium containing solution samples. Multielement solution standards with graded concentrations of the analytes and fixed concentration of the matrix are used in the standardization process. Nanogram to sub-nanogram quantities of the analytes have been determined with a precision of better than 9% RSD using 5 μl of the sample aliquots. (orig.)

  5. Separation of trace antimony and arsenic prior to hydride generation atomic absorption spectrometric determination

    A separation method utilizing a synthetic zeolite (mordenite) was developed in order to eliminate the gas phase interference of Sb(III) on As(III) during quartz furnace hydride generation atomic absorption spectrometric (HGAAS) determination. The efficiency of the proposed separation method in the reduction of suppression effects of transition metal ions on As(III) signal was also investigated. Among the volatile hydride-forming elements and their different oxidation states tested (Sb(III), Sb(V), Se(IV), Se(VI), Te(IV), and Te(VI)), only Sb(III) was found to have a signal depression effect even at low (μg l-1) concentrations under the experimental conditions employed. It has been shown that mordenite adsorbs Sb(III) quantitatively, even at a concentration of 1000 μg l-1, at pHs greater than two, and also, it reduces the initial concentrations of the transition metal ions to lower levels which can be tolerated in many studies. The adsorption of Sb(III) on mordenite follows the Freundlich isotherm and is endothermic in nature

  6. Atomic-absorption spectrometric determination of trace metals in zirconium and zircaloy by discrete sample nebulization

    A discrete sample nebulization technique was employed to determine trace metals in nuclear grade zirconium and Zircaloy by flame atomic-absorption spectrometry. With 10% (w/v) sample solutions, detection limits for Cd, Cu, Mn, Ni and Pb were 0.6, 2, 1, 3, and 10 μg/g. Micro standard-addition procedures and background correction were employed to minimize matrix interferences produced by the high salt content of the aspirated solutions. (author)

  7. Colorimetric and atomic absorption spectrometric determination of mucolytic drug ambroxol through ion-pair formation with iron and thiocyanate.

    Levent, Abdulkadir; Sentürk, Zühre

    2010-09-01

    Colorimetric and atomic absorption spectrometric methods have been developed for the determination of mucolytic drug Ambroxol. These procedures depend upon the reaction of iron(III) metal ion with the drug in the presence of thiocyanate ion to form stable ion-pair complex which extractable chloroform. The red-coloured complex was determined either colorimetrically at 510 nm or by indirect atomic absorption spectrometry (AAS) via the determination of the iron content in the formed complex. The optimum experimental conditions for pH, concentrations of Fe(3+) and SCN(-), shaking time, phase ratio, and the number of extractions were determined. Under the proposed conditions, linearity was obeyed in the concentration ranges 4.1x10(-6) - 5.7x10(-5) M (1.7-23.6 µg mL(-1)) using both methods, with detection limits of 4.6x10(-7) M (0.19 µg mL(-1)) for colorimetry and 1.1x10(-6) M (0.46 µg mL(-1)) for AAS. The proposed methods were applied for the determination of Ambroxol in tablet dosage forms. The results obtained were statistically analyzed and compared with those obtained by applying the high-performance liquid chromatographic method with diode-array detection. PMID:20426742

  8. An indirect atomic absorption spectrometric determination of ciprofloxacin, amoxycillin and diclofenac sodium in pharmaceutical formulations

    MAHMOUD MOHAMED ISSA

    2008-05-01

    Full Text Available A highly sensitive indirect atomic absorption spectrophotometric (AAS method has been developed for the determination of very low concentrations of ciprofloxacin, amoxycillin and diclofenac sodium. The method is based on the oxidation of these drugs with iron(III. The excess of iron(III was extracted into diethyl ether and then the iron(II in the aqueous layer was aspirated into an air–acetylene flame and determined by AAS. The linear concentration ranges were 25–400, 50–500 and 60–600 ng ml-1 for ciprofloxacin, amoxycillin and diclofenac sodium, respectively. The results were statistically compared with the official method using t- and f-test at p < 0.05. There were insignificant interferences from most of the excipients present. The intra- and inter-day assay coefficients of variation were less than 6.1 % and the recoveries ranged from 95 to 103 %. The method was applied for the analysis of these drug substances in their commercial pharmaceutical formulations.

  9. Atomic-absorption spectrometric determination of cobalt, nickel, and copper in geological materials with matrix masking and chelation-extraction

    Sanzolone, R.F.; Chao, T.T.; Crenshaw, G.L.

    1979-01-01

    An atomic-absorption spectrometric method is reported for the determination of cobalt, nickel, and copper in a variety of geological materials including iron- and manganese-rich, and calcareous samples. The sample is decomposed with HP-HNO3 and the residue is dissolved in hydrochloric acid. Ammonium fluoride is added to mask iron and 'aluminum. After adjustment to pH 6, cobalt, nickel, and copper are chelated with sodium diethyl-dithiocarbamate and extracted into methyl isobutyl ketone. The sample is set aside for 24 h before analysis to remove interferences from manganese. For a 0.200-g sample, the limits of determination are 5-1000 ppm for Co, Ni, and Cu. As much as 50% Fe, 25% Mn or Ca, 20% Al and 10% Na, K, or Mg in the sample either individually or in various combinations do not interfere. Results obtained on five U.S. Geological Survey rock standards are in general agreement with values reported in the literature. ?? 1979.

  10. Electrothermal atomic absorption spectrometric determination of total and hexavalent chromium in atmospheric aerosols

    A method was developed which allow separate determination of Cr(VI) and total Cr from the same minute sample of atmospheric aerosols. Cr(VI) was leached was with 0.1 M Na2CO3 and the total Cr concentrations were determined after acid digestion. The method was validated by the analysis of certified reference materials, CRM 545, Mess-3 and Pacs-2 with good agreement between certified and found values. Cr concentrations in air samples taken around the chromium smelter show concentrations that exceed the maximum allowed levels in 8 h with higher values closer to the smelter. The limit of detection (LOD) of the method for Cr(VI) determination in air samples was found to be 0.2 ng m-3, i.e. lower than offered by the commonly preferred spectrophotometric and colorimetric techniques

  11. Flame atomic absorption spectrometric determinations of some trace metals after coprecipitation with gold-APDC

    Complete text of publication follows. For the determination of trace metals in various samples, preconcentration is an inevitable step to overcome interferences. Among various techniques for the separation of trace metals proposed until now, coprecipitation is one of the most useful ones. Many different coprecipitation procedures including use of organic and inorganic collectors have been developed. So far, in the literature, it is reported that APDC, NaDDTC, PAN, TAR, Oxine, etc. as chelating agent for metal-chelate collector have been extensively used for coprecipitation of trace metals. However, metal chelates, especially dithocarbamates, as collectors are ideal for their sensitivities, simplicities and tolerances to interferences.Therefore, in the present work, fundamental studies on the coprecipitation with gold/APDC chelate have been carried out for determination of trace metals in environmental samples by FAAS with microinjection. According to our literature survey, gold/APDC is not used for the coprecipitation of heavy metal ions, until now. In this work, the coprecipitation was carried out in a centrifuge tube. Firstly, the main factors, such as amount of coprecipitant reagent and carrier element, pH of the solution, standing time, sample volume and diverse ions, affecting the coprecipitation of some trace metals were evaluated. Under optimized conditions, the recoveries of Cu, Ni, Pb and Cd were ≥ 95 %. R.S.D. values for ten replicates were lower than 5.0 %. Preconcentration factors were found to be 20. The coprecipitation was applied to various water samples and non-alcoholic beverage.

  12. Determination of trace elements in Egyptian cane sugar (Deshna Factories) by neutron activation, atomic absorption spectrophotometric and inductively coupled plasma-atomic emission spectrometric analysis

    Multielement instrumental neutron activation (INAA), inductively coupled plasma-atomic emission spectrometric (ICP-AES) and atomic absorption spectrophotometric (AAS) analyses were utilized for the determination of Ag, Al, As, Au, Ba, Be, Br, Ca, Cd, Ce, Cl, Co, Cr, Cu, Eu, Fe, Ga, Hf, K, La, Li, Lu, Mg, Mn, Na, Nb, Ni, P, Pb, Sb, Sc, Se, Sm, Sn, Sr, Ta, Th, Ti, U, V, W and Zn in sugar cane plant, raw juice, juice in different stages, syrup, deposits, molasses, A, B and C sugar, refinery 1 and 2 sugar, and in soil samples picked up from the immediate vicinity of the cane plant roots at surface, 30 and 60 cm depth, respectively. (author)

  13. Flame atomic absorption spectrometric determination of trace cadmium in alloys and biological samples after solid-liquid extraction and preconcentration with use of nitroso-S

    Cadmium is quantitatively retained by 2-nitroso-1-naphthol-4-sulfonic acid (nitroso-S) and tetradecyldimethylbenzylammonium chloride (TDBA) on microcrystalline naphthalene in the pH range 5.7-10.5 from a large volumes of aqueous solutions of various samples. After filtration, the solid mass consisting of cadmium complex and naphthalene is dissolved with 5 mL of dimethylformamide and the metal was determined by flame atomic absorption spectrometric. Cadmium complex can alternatively be quantitatively adsorbed on tetradecyldimethylbenzylammonium-naphthalene adsorbent packed in a column and determined similarly. About 25 ng of cadmium can be concentrated in a column from 500 mL of aqueous sample, where its concentration is as low as 0.05 ng/mL. Eight replicate determinations of 0.1 μg/mL of cadmium in final DMF solution gave a mean absorbance of 0.060 with a relative standard deviation of 1.8 %. The sensitivity for 1 % absorption was 7.3 ng/mL. The interference of a large number of anions and cations has been studied and the optimized conditions developed were utilized for the trace determination of cadmium in various alloys and biological samples. (author)

  14. Development of a cloud point extraction and preconcentration method for Cd and Ni prior to flame atomic absorption spectrometric determination

    Manzoori, Jamshid L. [Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz (Iran, Islamic Republic of)]. E-mail: manzoori@tabrizu.ac.ir; Karim-Nezhad, Ghasem [Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz (Iran, Islamic Republic of)

    2004-09-13

    In this work a new cloud point extraction (CPE) methodology was developed for the separation and preconcentration of cadmium and nickel. The analyte in the initial aqueous solution was complexed with dithizone and Triton X-114 was added as surfactant. After phase separation, based on the cloud point of the mixture, and dilution of the surfactant-rich phase with tetrahydrofuran (THF), the enriched analytes were determined by flame atomic absorption spectrometry. After optimization of the complexation and extraction conditions and preconcentration of only 10 ml of sample in the presence of 0.05% Triton X-114, the enhancement factors of 52 and 39 and the detection limits of 0.31 {mu}g l{sup -1} and 1.2 {mu}g l{sup -1} were obtained for cadmium and nickel respectively. The proposed method was applied satisfactorily to the determination of cadmium and nickel in water samples.

  15. Multi-element coprecipitation for separation and enrichment of heavy metal ions for their flame atomic absorption spectrometric determinations

    A preconcentration-separation technique for lead(II), cadmium(II), chromium(III), nickel(II) and manganese(II) ions has been established. The procedure is based on coprecipitation of these ions by the aid of Cu(II)-dibenzyldithiocarbamate precipitate. The precipitate was dissolved in 0.5 mL of concentrated HNO3, and made up to 5 mL with distilled water. The heavy metals were determined by flame atomic absorption spectrometer. The effects of analytical parameters like pH, amounts of reagents, sample volume, etc. on the recoveries of heavy metals were investigated. The influences of matrix ions were also examined. The detection limits for the heavy metals based on 3 sigma (N = 21) were found in the range of 0.34-0.87 μg L-1. In order to validate the proposed method, two certified reference materials of NIST SRM 2711 Montana soil and NIST SRM 1515 Apple leaves were analyzed with satisfactory results. The proposed method was applied for the determination of lead, cadmium, chromium, nickel and manganese in environmental samples

  16. Standard test method for graphite furnace atomic absorption spectrometric determination of lead and cadmium extracted from ceramic foodware

    American Society for Testing and Materials. Philadelphia

    2000-01-01

    1.1 This test method covers procedures for using graphite furnace atomic absorption spectroscopy (GFAAS) to quantitatively determine lead and cadmium extracted by acetic acid at room temperature from the food-contact surface of foodware. The method is applicable to food-contact surfaces composed of silicate-based materials (earthenware, glazed ceramicware, decorated ceramicware, decorated glass, and lead crystal glass) and is capable of determining lead concentrations greater than 0.005 to 0.020 g/mL and cadmium concentrations greater than 0.0005 to 0.002 g/mL, depending on instrument design. 1.2 This test method also describes quality control procedures to check for contamination and matrix interference during GFAAS analyses and a specific sequence of analytical measurements that demonstrates proper instrument operation during the time period in which sample solutions are analyzed. 1.3 Cleaning and other contamination control procedures are described in this test method. Users may modify contamination cont...

  17. Graphite furnace atomic absorption spectrometric determination of Ni and Pb in diesel and gasoline samples stabilized as microemulsion using conventional and permanent modifiers

    A procedure for the graphite furnace atomic absorption spectrometric determination of Ni and Pb in diesel and gasoline samples was developed. Sample stabilization was necessary because of evident analyte losses that occurred immediately after sampling. Excellent long-term sample stabilization was observed by mixing different organic solvents with propan-1-ol and 50% vol/vol HNO3 at a 3.3:6.5:1 volume ratio. For Pb, efficient thermal stabilization was obtained using aqueous Pd-Mg modifier as well as for Ir as permanent modifier. The drying temperature and ramp rate influenced the sensitivity obtained for Ni, and had to be carefully optimized. Taking this into account, the same sensitivity was attained in all investigated organic media stabilized as microemulsion. Thus, calibration with microemulsions prepared with a single organic solvent was possible, using aqueous or organic stock solutions. Commercial gasoline and diesel samples were directly analyzed after stabilization as microemulsion and by comparative UOP procedures. n-Hexane microemulsions were used for calibration, and good agreement was obtained between the results using the proposed and comparative procedures. Typical coefficients of variation (n = 6) ranged from 1% to 4%, and from 1% to 3% for Ni and Pb, respectively. Detection limits (k = 3) in the original gasoline or diesel samples, derived from 10 blank measurements, were 4.5 and 3.6 μg l-1 for Ni and Pb, respectively, comfortably below the values found in the analyzed samples

  18. Flame atomic absorption spectrometric determination of cadmium(II) and lead(II) after their solid phase extraction as dibenzyldithiocarbamate chelates on Dowex Optipore V-493

    An enrichment procedure for cadmium and lead after their solid phase extraction as dibenzyldithiocarbamate chelates on Dowex Optipore V-493 has been established prior to their flame atomic absorption spectrometric determinations. The analytical parameters including pH, amounts of dibenzyldithiocarbamate, sample volume, etc., were investigated. The effects of alkaline and earth alkaline ions and some metal ions on the retentions of analytes on Dowex Optipore V-493 resin were examined. Under the optimized conditions, the detection limits (3s, n = 21) for cadmium and lead were 0.43 μg L-1 and 0.65 μg L-1, respectively. The relative standard deviation (R.S.D.), and the recoveries of standard addition for this method were lower than 5% (n = 11) and 95-102%, respectively. Three standard reference samples (LGC 6010 Hard drinking water, NIST SRM 2711 Montana soil and GBW 07605 Tea) were introduced for accuracy and precision of analytical data. The proposed solid phase extraction system was successfully applied to the analysis of environmental samples

  19. Graphite furnace atomic absorption spectrometric determination of Ni and Pb in diesel and gasoline samples stabilized as microemulsion using conventional and permanent modifiers

    Reyes, Mariela N. Matos; Campos, Reinaldo C.

    2005-06-01

    A procedure for the graphite furnace atomic absorption spectrometric determination of Ni and Pb in diesel and gasoline samples was developed. Sample stabilization was necessary because of evident analyte losses that occurred immediately after sampling. Excellent long-term sample stabilization was observed by mixing different organic solvents with propan-1-ol and 50% vol/vol HNO 3 at a 3.3:6.5:1 volume ratio. For Pb, efficient thermal stabilization was obtained using aqueous Pd-Mg modifier as well as for Ir as permanent modifier. The drying temperature and ramp rate influenced the sensitivity obtained for Ni, and had to be carefully optimized. Taking this into account, the same sensitivity was attained in all investigated organic media stabilized as microemulsion. Thus, calibration with microemulsions prepared with a single organic solvent was possible, using aqueous or organic stock solutions. Commercial gasoline and diesel samples were directly analyzed after stabilization as microemulsion and by comparative UOP procedures. n-Hexane microemulsions were used for calibration, and good agreement was obtained between the results using the proposed and comparative procedures. Typical coefficients of variation ( n = 6) ranged from 1% to 4%, and from 1% to 3% for Ni and Pb, respectively. Detection limits ( k = 3) in the original gasoline or diesel samples, derived from 10 blank measurements, were 4.5 and 3.6 μg l - 1 for Ni and Pb, respectively, comfortably below the values found in the analyzed samples.

  20. Determination of Cr(VI) in welding fumes by anion-exchange fast protein liquid chromatography with electrothermal atomic absorption spectrometric detection.

    Milacic, Radmila; Scancar, Janez; Tusek, Janez

    2002-02-01

    The applicability of an anion-exchange fast protein liquid chromatographic-electrothermal atomic absorption spectrometric procedure (FPLC-ETAAS) was investigated for the determination of Cr(VI) in welding fumes after alkaline extraction of aerosols loaded on filters. Gas tungsten arc welding (GTAW) of stainless steel was applied. Samples of welding fumes were collected during regular welding on polycarbonate membrane filters of 8 microm and 0.4 microm pore size (inhalable and respirable aerosols). Alkaline extraction (2% NaOH-3% Na2CO3) of filters in a heated ultrasonic bath was applied to leach Cr from the airborne particulate matter. 0.5 cm3 of sample extract was then injected onto an anion-exchange FPLC column. Tris-HCl buffer (0.005 mol dm(-3), pH 8.0) and the same buffer with NaCl (0.5 mol dm(-3)) were employed in gradient elution (15 min, flow rate 1 cm3 min(-1)). The separated Cr species were determined "off line" by ETAAS in 0.5 cm3 fractions. Cr(VI) was reproducibly and quantitatively eluted from 12.0 to 13.0 min with a maximum peak at 12.5 min. Good repeatability of measurement (+/-3.0%) of alkaline extracts was obtained for Cr(VI). The LOD (3s) was found to be 0.035 microg m(-3) Cr(VI), when 2 m3 of aerosols were collected on the filter. Validation of the procedure was performed by spiking alkaline extracts and by the analysis of standard reference material CRM 545, Cr(VI) in welding dust loaded on a filter. The technique was successfully applied for the determination of Cr(VI) in welding fumes. PMID:11939630

  1. Cloud Point Extraction and Flame Atomic Absorption Spectrometric Determination of Lead, Cadmium and Palladium in Some Food and Biological Samples

    M. Soylak

    2011-12-01

    Full Text Available The proposed method is based on the complexation of the Pb2+, Cd2+ and Pd2+ ions with 3-(1-(1-H-Indol-3-Yl-3-phenylallyl-1H-indole (IPAI at pH 8.0 in the presence of Triton X-114. The phase separation occured when micellar solution was heated at 55 ◦C. The surfactant-rich phase, diluted to 0.5 mL via 1.0 mol L−1 nitric acid in methanol was directly introduced into the nebulizer of the flame atomic absorption spectrometry (FAAS. Influence of variables such as pH, amount of ligand and Triton X-114, heating time and temperature were evaluated and optimized. The optimized enhancement factors for Pb2+, Cd2+ and Pd2+ ions were 22, 33 and 23, respectively and the detection limit (DLs was between of 1.6–2.6 µgL−1. The relative standard deviation (RSD of each ion was found to be less than 4.6% at 100 µgL−1. In addition, the calibration graphs were linear in the range of 0.01-0.22 μg mL−1 for Cd2+ ion, 0.018-0.26 μg mL−1 for Pb2+ ion and 0.02-0.27 μg mL−1 for Pd2+ ion with the correlation coefficients in the range of 0.995–0.999.

  2. Electrothermal atomic absorption spectrometric determination of lithium, sodium, potassium and copper in uranium without preliminary chemical separation

    Graphite furnace atomization is used for the direct determination of Li (0.25-4 ppm), Na (8-70 ppm), K (20-300 ppm) and Cu (0.5-25 ppm) in uranium dissolved in nitric acid, with relative standard deviations of 4-9%. Only iron seriously depresses the signals from the alkali metals. (Auth.)

  3. Biosorption of platinum and palladium for their separation/preconcentration prior to graphite furnace atomic absorption spectrometric determination

    Inexpensive baker's yeast Saccharomyces cerevisiae and green algae Chlorella vulgaris, either free or immobilized on silica gel have been shown to selectively accumulate platinum and palladium from water samples in acidic medium (pH 1.6-1.8). Optimization of conditions of metals biosorption (sample pH, algae and yeast masses, adsorption time, temperature) was performed in batch mode. The procedure of matrix separation based on biosorption of platinum and palladium on algae C. vulgaris covalently immobilized on silica gel in flow mode was developed. The use of algae in flow procedure offers several advantages compared with its use in the batch mode. The procedure shows better reproducibility (-1 thiourea in 1 mol l-1 hydrochloric acid. The influence of thiourea on analytical signals of examined metals during GFAAS determination is discussed. The procedure has been applied for separation of noble metals from tap and waste water samples spiked with platinum and palladium

  4. Novel atomic absorption spectrometric and rapid spectrophotometric methods for the quantitation of paracetamol in saliva: Application to pharmacokinetic studies

    Issa M

    2008-01-01

    Full Text Available A novel atomic absorption spectrometric method and two highly sensitive spectrophotometric methods were developed for the determination of paracetamol. These techniques based on the oxidation of paracetamol by iron (III (method I; oxidation of p-aminophenol after the hydrolysis of paracetamol (method II. Iron (II then reacts with potassium ferricyanide to form Prussian blue color with a maximum absorbance at 700 nm. The atomic absorption method was accomplished by extracting the excess iron (III in method II and aspirates the aqueous layer into air-acetylene flame to measure the absorbance of iron (II at 302.1 nm. The reactions have been spectrometrically evaluated to attain optimum experimental conditions. Linear responses were exhibited over the ranges 1.0-10, 0.2-2.0 and 0.1-1.0 µg/ml for method I, method II and atomic absorption spectrometric method, respectively. A high sensitivity is recorded for the proposed methods I and II and atomic absorption spectrometric method value indicate: 0.05, 0.022 and 0.012 µg/ml, respectively. The limit of quantitation of paracetamol by method II and atomic absorption spectrometric method were 0.20 and 0.10 µg/ml. Method II and the atomic absorption spectrometric method were applied to demonstrate a pharmacokinetic study by means of salivary samples in normal volunteers who received 1.0 g paracetamol. Intra and inter-day precision did not exceed 6.9%.

  5. Determination of Palladium in Resin by Lead Fire Assaying-Flame Atomic Absorption Spectrometric Method%铅试金富集-火焰原子吸收光谱法测定树脂中钯

    王芳; 陈小兰; 林海山; 李小玲; 肖红新

    2013-01-01

    通过铅试金富集树脂中的钯并用银作钯灰吹保护,得到的银钯合粒用王水溶解,在5%的盐酸介质中,采用原子吸收光谱法测定钯,该法测钯的相对标准偏差RSD为0.53%,加标回收率在99.04%~100.10%之间。%Palladium in resin was enriched by lead assaying, using silver as a protective agent to produce silver-palladium alloy, and then the alloy was dissolved in aqua regia. Air acetylene flame atomic absorption spectrometric method was used to determinate palladium in 5%hydrochloric acid solution. The relative standard deviation (RSD) in determination of palladium is 0.53%and the recovery rate is between 99.04%~100.10%.

  6. A solid liquid extraction and preconcentration method for the atomic absorption spectrometric determination of trace cobalt in various alloys and biological samples

    Cobalt is quantitatively retained as cobalt-2-nitroso-4-sulfonic acid (nitros-S)-tetradecyldimethylbenzylammonium (TDBA+) ion-pair complex on microcrystalline naphthalene in the pH range 6.2-9.0 from a large volume of its aqueous solution of various complex samples. After filtration, the solid mass consisting of cobalt complex and naphthalene is dissolved in 5 ml of dimethylformamide (DMF) and the metal is determined by flame atomic absorption spectrometry (FAAS). Cobalt complex can alternatively be quantitatively adsorbed on tetradecyldimethylbenzylammonium chloride-naphthalene adsorbent packed in a column and determined similarly. The calibration curve is linear over the concentration range 0.2-11.5 μg of cobalt in 5 ml of the final DMF solution. In this case, 0.2 μg of cobalt may be concentrated in a column from 250 ml of aqueous sample where its concentration is as low as 0.8 ng/ml. Eight replicate determinations of 3.0 μg of cobalt in the final DMF solution give a mean absorbance of 0.045 with a relative standard deviation of 1.8%. The sensitivity for 1% absorption is 59 ng/ml. The interference of a large number of anions and cations on the determination of cobalt has been studied and the optimum conditions developed utilized for its trace determination in various alloys and biological samples. The method may also be used for the determination of cobalt in some environmental samples

  7. Graphite furnace and hydride generation atomic absorption spectrometric determination of cadmium, lead, and tin traces in natural surface waters: Study of preconcentration technique performance

    In this study three major types of preconcentration methods based upon different principles (cation exchange, physical absorption and hydrophobic extraction) were evaluated and optimized for the extraction and determination of three highly toxic heavy metals namely Cd, Pb and Sn by graphite furnace and hybrid generation atomic absorption spectrometry in real samples. The optimum analytical conditions were examined and the analytical features of each method were revealed and compared. Detection limits as low as 0.003-0.025 μg L-1 for Cd2+, 0.05-0.10 μg L-1 for Pb2+ and 0.1-0.25 μg L-1 for Sn4+ depending on the extraction method were obtained with RSD values between 3.08% and 6.11%. A preliminary assessment of the pollution status of three important natural ecosystems in Epirus region (NW Greece) was performed and some early conclusions were drawn and discussed

  8. Preconcentration and atomic absorption spectrometric determination of cadmium, cobalt, copper, iron, lead, manganese, nickel and zinc in water samples using 6-methyl-2-pyridinecarboxaldehyde-4-phenyl-3-thiosemicarbazone

    The reagent 6-methyl-2-pyridinecarboxaldehyde-4-phenyl-3-thiosemicarbazone (MPAPT) has been examined for the pre-concentration of metal ions and determination using air acetylene flame atomic absorption spectrometer. The method is based on the complexation and extraction of cadmium (II), cobalt(III), copper(II), lead(II), nickel(II), iron(II), iron(II), manganese(II) and zinc(II) in chloroform. The metal iron are back extracted in nitric acid (1:1) or after evaporation of solvent the residue is digested in nitric acid. After necessary adjustment of volume the metal ions were determined in aqueous solution. Pre-concentration is obtained 10-25 times. Metal ions recovery was 95.4-100.8% with coefficient of variation 0.2-7.5%. The method used for the determination of metals in canal and sewerage waters, within 2-6433 mu g/L with C. V 0.-5.2%. (author)

  9. Inclusion of riboflavin in β-cyclodextrin: A fluorimetric and absorption spectrometric study

    Roy, Dalim Kumar; Deb, Nipamanjari; Ghosh, Bankim Chandra; Mukherjee, Asok K.

    2009-07-01

    Formation of inclusion complexes between riboflavin and β-cyclodextrin (β-CD) with both 1:1 and 1:2 stoichiometry has been established by fluorimetric titration. However, in absorption spectrometric experiment, spectral change of riboflavin in the visible range could be observed only by taking β-CD at a much higher concentration (about 100 times) than riboflavin and under such condition only 1:2 complexes could be detected. Its formation constant ( K) was determined by a multiple linear regression analysis of the absorption data. The reliability of the K value was confirmed by the consistency achieved on analyzing the data at two different wavelengths.

  10. Atomic absorption spectrometric determination of some metal ions after preconcentration by solid phase extraction using amberlite XAD 16 resin loaded with thenoyltrifluoroacetone

    Complete text of publication follows. The direct determination of extremely low concentrations of trace elements by modern atomic spectroscopic methods, such as atomic absorption spectrometry and inductively coupled plasma atomic emission spectrometry is often difficult because of insufficient sensitivity and selectivity of the methods used. For this reason, the preliminary separation and preconcentration of trace elements from the matrix are often required. Solid phase extraction shows several major advantages such as simplicity, rapidity and high enrichment factor, the ability of combination with different detection techniques in the form of on-line or off-line mode and finally cost saving (Tokalioglu et al., Microchim Acta 164 (2009) 471-477.). A new solid phase extraction method for the separation and preconcentration of Cu(II), Pb(II), Ni(II), Co(II), Mn(II) and Fe(III) ions was developed. As solid phase material, Amberlite XAD-16 resin loaded with thenoyltrifluoroacetone (TTA) was used. For this purpose, 0.5 g of the resin was saturated with 10 mL of 0.5% (w/v) TTA solution. After preconcentrating, the metals retained on the resin were eluted with 10 mL of 2 mol L-1 HCl and then determined by flame atomic absorption spectrometry. The effect of some parameters for the preconcentration of the metal ions was investigated. The optimum pH was found as 6. Eluent for quantitative elution was 10 mL of 2 mol L-1 HCl.

  11. Atomic-absorption spectrometric, neutron-activation and radioanalytical techniques for the determination of trace metals in environmental, biochemical and toxicological research

    Radioanalytical techniques and atomic-absorption spectrometry have been used for the micro-determination of vanadium in biological specimens such as human tissues and body fluids in environmental, biochemical and toxicological research. The use of 48V as a radiotracer permitted investigations on the vaporisation and retention mechanisms of vanadium. Higher vanadium oxides are probably converted into lower oxides, decomposing to VO in gaseous form, followed by the dissociation to 'free vanadium' and oxygen. It was found that about 20% of the 48V radioactivity was consistently retained in the graphite tube after 10 repeated introductions and firings of 50 μl of 50 ng ml-148V-labelled vanadium solution. However, the amount retained, probably in the form of carbide, does not vaporise under the conditions used for the analysis. Determinations of vanadium at the parts per billion level in 10 urine samples by neutron-activation analysis and by graphite furnace atomic-absorption spectrometry showed agreement that can be considered satisfactory for practical purposes. (author)

  12. Selective cloud point extraction and preconcentration of trace amounts of silver as a dithizone complex prior to flame atomic absorption spectrometric determination

    Manzoori, Jamshid L.; Karim-Nezhad, Ghasem

    2003-05-19

    Dithizone (diphenylthiocarbazone) was used as a complexing agent in cloud point extraction for the first time and applied for selective preconcentration of trace amounts of silver. The analyte in the initial aqueous solution was acidified with sulfuric acid (pH<1) and Triton X-114 was added as a surfactant. After phase separation, based on the cloud point separation of the mixture, the surfactant rich phase was diluted with tetrahydrofuran (THF) and the analyte determined in the enriched solution by flame atomic absorption spectrometry. After optimization of the complexation and extraction conditions, a preconcentration factor of 43 was obtained for only 10 ml of sample. The analytical curve was linear in the range of 3-200 ng ml{sup -1} and the limit of detection was 0.56 ng ml{sup -1}. The proposed method was applied to the determination of silver in water samples.

  13. The determination of trace amounts of heavy metals in waters by a flow-injection system including ion-exchange preconcentration and flame atomic absorption spectrometric detection

    The flow-injection system combines on-line ion-exchange preconcentration with atomic absorption spectrometry (a.a.s.) for the determination of traces (μg l-1) of heavy metals in water samples. A multifunctional rotary sampling valve which incorporated two parallel sampling columns allows sampling, exchange, elution and a.a.s. to be achieved sequentially. The increases in sensitivity for nickel, copper, lead and cadmium were 20-28-fold at a sampling rate of 40 h-1 with 5-ml samples. Relative standard deviations were 1.5-4.1%. The recoveries of these four metals added to tap, sea and polluted waters were generally satisfactory, except for cadmium in polluted water. The effects of column diameter and elution flow rates on sensitivity are discussed. Possible interferences are described. (Auth.)

  14. Flame atomic absorption spectrometric determination of trace amounts of heavy metal ions after solid phase extraction using modified sodium dodecyl sulfate coated on alumina

    A sensitive and selective solid phase extraction procedure for the determination of traces of Cu(II), Zn(II), Pb(II) and Fe(III) has been developed. An alumina-sodium dodecyl sulfate (SDS) coated on with meso-phenyl bis(indolyl) methane (MPBIM) was used for preconcentration and determination of Cu(II), Zn(II), Pb(II) and Fe(III) ions by flame atomic absorption spectrometry. The analyte ions were adsorbed quantitatively on adsorbent due to their complexation with MPBIM. Adsorbed metals were quantitatively eluted using 6 mL of 4 mol L-1 nitric acid. The effects of parameters such as pH, amount of alumina, amount of MBITP, flow rate, type and concentration of eluting agent were examined. The effects of interfering ions on the separation-preconcentration of analytes were also investigated. The relative standard deviation of the method was found to be less than 3.0%. The presented procedure was successfully applied for determination of analytes in real samples

  15. A biosorption system for metal ions on Penicillium italicum - loaded on Sepabeads SP 70 prior to flame atomic absorption spectrometric determinations

    A solid phase extraction (SPE) preconcentration system, coupled to a flame atomic absorption spectrometer (FAAS), was developed for the determination of copper(II), cadmium(II), lead(II), manganese(II), iron(III), nickel(II) and cobalt(II) ions at the μg L-1 levels on Penicillium italicum - loaded on Sepabeads SP 70. The analytes were adsorbed on biosorbent at the pH range of 8.5-9.5. The adsorbed metals were eluted with 1 mol L-1 HCl. The influences of the various analytical parameters including pH of the aqueous solutions, sample volume, flow rates were investigated for the retentions of the analyte ions. The recovery values are ranged from 95-102%. The influences of alkaline, earth alkaline and some transition metal ions were also discussed. Under the optimized conditions, the detection limits (3 s, n = 21) for analytes were in the range of 0.41 μg L-1 (cadmium) and 1.60 μg L-1 (iron). The standard reference materials (IAEA 336 Lichen, NIST SRM 1573a Tomato leaves) were analyzed to verify the proposed method. The method was successfully applied for the determinations of analytes in natural water, cultivated mushroom, lichen (Bryum capilare Hedw), moss (Homalothecium sericeum) and refined table salt samples

  16. Cloud point extraction and flame atomic absorption spectrometric determination of cadmium(II), lead(II), palladium(II) and silver(I) in environmental samples

    The phase-separation phenomenon of non-ionic surfactants occurring in aqueous solution was used for the extraction of cadmium(II), lead(II), palladium(II) and silver(I). The analytical procedure involved the formation of understudy metals complex with bis((1H-benzo [d] imidazol-2yl)ethyl) sulfane (BIES), and quantitatively extracted to the phase rich in octylphenoxypolyethoxyethanol (Triton X-114) after centrifugation. Methanol acidified with 1 mol L-1 HNO3 was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The concentration of BIES, pH and amount of surfactant (Triton X-114) was optimized. At optimum conditions, the detection limits of (3 sdb/m) of 1.4, 2.8, 1.6 and 1.4 ng mL-1 for Cd2+, Pb2+, Pd2+ and Ag+ along with preconcentration factors of 30 and enrichment factors of 48, 39, 32 and 42 for Cd2+, Pb2+, Pd2+ and Ag+, respectively, were obtained. The proposed cloud point extraction has been successfully applied for the determination of metal ions in real samples with complicated matrix such as radiology waste, vegetable, blood and urine samples.

  17. Cloud point extraction and flame atomic absorption spectrometric determination of cadmium(II), lead(II), palladium(II) and silver(I) in environmental samples

    Ghaedi, Mehrorang, E-mail: m_ghaedi@mail.yu.ac.ir [Chemistry Department, Yasouj University, Yasouj 75914-353 (Iran, Islamic Republic of); Shokrollahi, Ardeshir [Chemistry Department, Yasouj University, Yasouj 75914-353 (Iran, Islamic Republic of); Niknam, Khodabakhsh [Chemistry Department, Persian Gulf University, Bushehr (Iran, Islamic Republic of); Niknam, Ebrahim; Najibi, Asma [Chemistry Department, Yasouj University, Yasouj 75914-353 (Iran, Islamic Republic of); Soylak, Mustafa [Chemistry Department, University of Erciyes, 38039 Kayseri (Turkey)

    2009-09-15

    The phase-separation phenomenon of non-ionic surfactants occurring in aqueous solution was used for the extraction of cadmium(II), lead(II), palladium(II) and silver(I). The analytical procedure involved the formation of understudy metals complex with bis((1H-benzo [d] imidazol-2yl)ethyl) sulfane (BIES), and quantitatively extracted to the phase rich in octylphenoxypolyethoxyethanol (Triton X-114) after centrifugation. Methanol acidified with 1 mol L{sup -1} HNO{sub 3} was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The concentration of BIES, pH and amount of surfactant (Triton X-114) was optimized. At optimum conditions, the detection limits of (3 sdb/m) of 1.4, 2.8, 1.6 and 1.4 ng mL{sup -1} for Cd{sup 2+}, Pb{sup 2+}, Pd{sup 2+} and Ag{sup +} along with preconcentration factors of 30 and enrichment factors of 48, 39, 32 and 42 for Cd{sup 2+}, Pb{sup 2+}, Pd{sup 2+} and Ag{sup +}, respectively, were obtained. The proposed cloud point extraction has been successfully applied for the determination of metal ions in real samples with complicated matrix such as radiology waste, vegetable, blood and urine samples.

  18. Development of on-line single-drop micro-extraction sequential injection system for electrothermal atomic absorption spectrometric determination of trace metals

    A novel automatic sequential injection (SI) single-drop micro-extraction (SDME) system is proposed as versatile approach for on-line metal preconcentration and/or separation. Coupled to electrothermal atomic absorption spectrometry (ETAAS) the potentials of this SI scheme are demonstrated for trace cadmium determination in water samples. A non-charged complex of cadmium with ammonium diethyldithiophosphate (DDPA) was produced and extracted on-line into a 60 μL micro-drop of di-isobutyl ketone (DIBK). The extraction procedure was performed into a newly designed flow-through extraction cell coupled on a sequential injection manifold. As the complex Cd(II)-DDPA flowed continuously around the micro-droplet, the analyte was extracting into the solvent micro-drop. All the critical parameters were optimized and offered good performance characteristics and high preconcentration ratios. For 600 s micro-extraction time, the enhancement factor was 10 and the sampling frequency was 6 h-1. The detection limit was 0.01 μg L-1 and the precision (RSD at 0.1 μg L-1 of cadmium) was 3.9%. The proposed method was evaluated by analyzing certified reference material

  19. Selective solid phase extraction of platinum on an ion imprinted polymers for its electrothermal atomic absorption spectrometric determination in environmental samples

    An ion-imprinted polymer (IIP) was obtained by copolymerization of methacrylic acid (as a functional monomer) and ethylene glycol dimethacrylate (as a crosslinking agent) in the presence of various chelators for Pt(II) ion and using 2,2'-azo-bis-isobutyronitrile as the initiator. Specifically, acetaldehyde thiosemicarbazone (AcTSn) and benzaldehyde thiosemicarbazone (BnTSn) were used as chelators. The IIPs were applied as sorbents for solid-phase extraction of Pt(II) and Pt(IV) ions from aqueous solutions. The effects of acidity and flow rate of the sample, of elution conditions and of potentially interfering ions were investigated. The imprinting effect of analyte is clearly demonstrated by the fact that only the IIP is capable of quantitative retention of Pt(II) and Pt(IV) ions. The method works best in the pH range from 0.5 to 1 and from 3.5 to 9.5. The ions can be recovered with an acidic solution of thiourea. The Pt-AcTSn polymer displays better sorption properties for the separation of analytes. The selectivity coefficients of the Pt-AcTSn and control polymers for Pt(IV) in the presence Pd(II), Rh(III), Ru(III), Al(III) and Cu(II) were calculated, and the sorbent capacity for Pt(IV) was found to be 4.56 μg g-1. The method was successfully applied to the determination of Pt(IV) by electrothermal atomic absorption spectrometry in tap water, tunnel dust and anode slime samples. (author)

  20. On-line sequential injection dispersive liquid-liquid microextraction system for flame atomic absorption spectrometric determination of copper and lead in water samples.

    Anthemidis, Aristidis N; Ioannou, Kallirroy-Ioanna G

    2009-06-30

    A simple, sensitive and powerful on-line sequential injection (SI) dispersive liquid-liquid microextraction (DLLME) system was developed as an alternative approach for on-line metal preconcentration and separation, using extraction solvent at microlitre volume. The potentials of this novel schema, coupled to flame atomic absorption spectrometry (FAAS), were demonstrated for trace copper and lead determination in water samples. The stream of methanol (disperser solvent) containing 2.0% (v/v) xylene (extraction solvent) and 0.3% (m/v) ammonium diethyldithiophosphate (chelating agent) was merged on-line with the stream of sample (aqueous phase), resulting a cloudy mixture, which was consisted of fine droplets of the extraction solvent dispersed entirely into the aqueous phase. By this continuous process, metal chelating complexes were formed and extracted into the fine droplets of the extraction solvent. The hydrophobic droplets of organic phase were retained into a microcolumn packed with PTFE-turnings. A portion of 300 microL isobutylmethylketone was used for quantitative elution of the analytes, which transported directly to the nebulizer of FAAS. All the critical parameters of the system such as type of extraction solvent, flow-rate of disperser and sample, extraction time as well as the chemical parameters were studied. Under the optimum conditions the enhancement factor for copper and lead was 560 and 265, respectively. For copper, the detection limit and the precision (R.S.D.) were 0.04 microg L(-1) and 2.1% at 2.0 microg L(-1) Cu(II), respectively, while for lead were 0.54 microg L(-1) and 1.9% at 30.0 microg L(-1) Pb(II), respectively. The developed method was evaluated by analyzing certified reference material and applied successfully to the analysis of environmental water samples. PMID:19376348

  1. Electrothermal atomic absorption spectrometric determination of cadmium and lead in traces in aquatic systems following flotation by two chromium(III) collectors.

    Kormusoska, Natasa Bakreska; Cundeva, Katarina; Stafilov, Trajce

    2009-10-01

    A fast flotation method for determination of cadmium and lead in aquatic systems by two chromium(III) collectors is described. The first collector is a colloid precipitate of hydrated chromium(III) oxide, Cr2O3 x xH2O, while the second is a bulk chromium(III) pentamethylenedithiocarbamate, Cr(PMDTC)3. Cadmium and lead present in water are incorporated into the collector mass at pH 7.5 by addition of 20 mg of Cr(III) and 0.4 mmol of pentamethyleneammonium pentamethylenedithiocarbamate, PMA-PMDTC, to 0.5 L water sample. A solid precipitate was separated from the processed water system by air bubbles. After dissolving with strong acid, the solution is tested by electrothermal atomic absorption spectrometry (ETAAS). The limit of detection for Cd by flotation/ETAAS method is 0.002 microg L(-1), while for Pb is 0.04 microg L(-1). The precision of the method is expressed as relative standard deviations ranging of 5.0% for Cd (concentration range from 0.1 to 0.5 microg L(-1)) and 4.25% for Pb (concentration range from 0.5 to 5 microg L(-1)). The characteristic mass (mass that gives an integrated absorbance of 0.0044 s) of 1.06 pg for Cd and 16.7 pg for Pb were obtained. The method was validated by the standard additions and by its application to the reference materials (Surface water-SPS-SW-1, River Thames Water-LGC-6019). PMID:19847715

  2. Enrichment of trace amounts of copper(II) ions in water samples using octadecyl silica disks modified by a Schiff base ionophore prior to flame atomic absorption spectrometric determination

    Fathi, S.A.M. [Department of Chemistry, Faculty of Science, Zanjan University, PO Box 45195-313 Zanjan (Iran, Islamic Republic of); Yaftian, M.R. [Department of Chemistry, Faculty of Science, Zanjan University, PO Box 45195-313 Zanjan (Iran, Islamic Republic of)], E-mail: yaftian@znu.ac.ir

    2009-05-15

    Bis(5-bromo-2-hydroxybenzaldehyde)-1,2-propanediimine is synthesized by the reaction of 5-bromo-2-hydroxybenzaldehyde and 1,2-diaminopropane in ethanol. This ligand is used as a modifier of octadecyl silica disks for preconcentration of trace amounts of copper(II) ions, followed by nitric acid elution and flame atomic absorption spectrometric (FAAS) determination. The effect of parameters influencing the extraction efficiency, i.e. pH of the sample solutions, amount of the Schiff base, type and volume of stripping reagent, sample and eluent flow rates were evaluated. Under optimum experimental conditions, the capacity of the membrane disks modified by 4 mg of the ligand was found to be 247.7 ({+-}2.1) {mu}g of copper. The detection limit and the concentration factor of the presented method are 2.4 ng/l and greater than 400, respectively. The method was applied to the extraction, recovery and detection of copper in different synthetic and water samples.

  3. Separation and flame atomic absorption spectrometric determination of total chromium and chromium (III) in phosphate rock used for production of fertilizer.

    El-Sheikh, Amjad H; Al-Degs, Yahya S; Sweileh, Jamal A; Said, Adi J

    2013-11-15

    Due to the commercial value of phosphate rock (PR) as a fertilizer precursor, it is necessary to investigate its heavy metals content. Chromium (Cr) may present as Cr(III) or Cr(VI) in PR; but quantitative differentiation between them is not an easy task. This is due to possible interconversion of Cr species during the digestion/leaching process. In this work, ultrasound digestion (USD) of PR was optimized (300 mg PR, 4.0 mL of 4.0 mol L(-1) nitric acid, 15 min sonication) for the sake of leaching Cr species prior to their determination by flame atomic absorption spectroscopy. Using multi-walled carbon nanotube (MWCNT) as adsorbent, solid phase extraction (SPE) was used to separate Cr(III) from the digestate at pH 9, while total Cr was estimated after reducing Cr(VI) into Cr(III). The optimum USD/SPE method gave LOQ and LOD of Cr(III) of 0.96 mg kg(-1) and 0.288 mg kg(-1), respectively. The method sensitivity was 1.44×10(-3) AU kg mg(-1) within the studied Cr concentration range (5-400 mg kg(-1)). The USD/SPE method was validated by analyzing lake sediments LKSD-4 certified reference material, and by comparison with classical digestion method (CD). Application of USD/SPE on Jordanian PR samples gave total Cr rang 29.1-122.0 mg kg(-1) (±1.4-6.3), while Cr(III) ranged between 23.8 and 101.7 mg kg(-1) (±1.3-5.5). AFPC Rock Check Program samples gave total Cr range 238.9-394.7 mg kg(-1) (±11.5-24.1), while Cr(III) ranged between 202.4 and 335.8 mg kg(-1) (±11.4-18.3). These results were very close to the results obtained by the CD method. PMID:24148433

  4. Cloud point extraction and flame atomic absorption spectrometric determination of trace lead in freshwater fish%浊点萃取-火焰原子吸收光谱法测定淡水鱼中痕量铅

    王秀峰; 李龙; 张春丽; 林朋; 崔书亚

    2012-01-01

    采用以双硫腙为络合剂、Triton X- 100为表面活性剂的新型浊点萃取体系富集淡水鱼中的痕量铅,并用火焰原子吸收光谱法对其进行测定.探讨了溶液pH、表面活性剂浓度、络合剂用量、平衡温度、平衡时间等对浊点萃取及测定灵敏度的影响,优化了实验条件.在最佳条件下测得铅的检出限为0.090μg/L,校准曲线相关系数为0.9999.该方法已用于淡水鱼中痕量铅的测定.%A new cloud point extraction-flame atomic absorption spectrometric method has been developed to determine trace lead. Dithizone was selected as the complex reagent and Triton X - 100 as the surfactant. Effects of pH, concentrations of surfactant and complex reagent, equilibrium temperature and time on the efficiency and sensitivity of cloud point extraction were investigated. Under optimal conditions, the calibration curve was linear over the concentration range of 0. 1 - 60μg/L with correlation coefficient of 0. 9999 and detection limit of 0. 090 μg/L. The present method was applied to the determination of trace lead in freshwater fish samples with satisfactory results.

  5. Flame atomic absorption spectrometric determination of μg amounts of Fe (III) ions after solid phase extraction using modified octadecyl silica membrane disks

    A simple, rapid and reliable method has been developed to selectively separate and concentrate ultra trace amounts of Fe (III) ions from aqueous samples for the measurement by flame atomic absorption spectrometry (FAAS). By the passage of aqueous samples through an octadecyl silica membrane disk modified by a recently synthesized Schiff base (Bis-(4-nitro phenyl azo) salisilidine-1,3-diamino propane), Fe(III) ions adsorb quantitatively and most of matrix elements will pass through the disk to drain. The retained iron ions are then stripped from the disk by minimal amount of 0.1 mol l-1 sulfuric acid as eluent. Extraction efficiency and the influence of pH, flow rates, amount of ligand, type and least amount of stripping acid as eluent were evaluated. The recovery of the iron from aqueous solution on the membrane disk modified with 3 mg Schiff's base was quantitative over pH 2-4.5. The linear dynamic range of the proposed method for Fe (III) ions was found in a wide concentration range of 0.20 (± 0.05)-680 (± 2) μg l-1. The detection limit and preconcentration factor of this solid phase extraction method were found 20.0 (± 0.7) ng l-1 and 100 respectively. The reproducibility of the procedure is at the most 1.5%

  6. Bi(III)4-methylpiperidinedithiocarbamate coprecipitation procedure for separation-pre-concentration of trace metal ions in water samples by flame atomic absorption spectrometric determination

    A pre-concentration method was developed for determination of trace amounts of cadmium, copper and lead in water samples by FAAS after coprecipitation by using potassium 4-methylpiperidinedithiocarbamate (K4-MPDC) as a chelating agent and Bi(III) as a carrier element. This procedure is based on filtration of the solution containing precipitate on a cellulose nitrate membrane filter following Cd(II), Cu(II) and Pb(II) coprecipitation with Bi(III)4-MPDC and then the precipitates together with membrane filter were dissolved in concentrated nitric acid. The metal contents of the final solution were determined by FAAS. Several parameters including pH of sample solution, amount of carrier element and reagent, standing time, sample volume for precipitation and the effects of diverse ions were examined. The accuracy of the method was tested with standard reference material (MBH, C31XB20 and CRM BCR-32) and Cd, Cu and Pb added samples. Determination of Cd, Cu and Pb was carried out in sea water, river water and tap water samples. The recoveries were >95%. The relative standard deviations of determination were less than 10%

  7. Flame Atomic Absorption Spectrometric Determination of Gold After Solid-Phase Extraction of Its 2-Aminobenzothiazole Complex on Diaion SP-207.

    Unsal, Yunus Emre; Tuzen, Mustafa; Soylak, Mustafa

    2016-03-01

    An SPE of Au (III) on a 2-aminobenzothiazole-coated Diaion SP 207-column system has been developed. The parameters, including pH of solution, amount of 2-aminobenzothiazole, eluent type, sample volume, and flow rates, were examined. The effects of alkali, alkali earth, and some metals were also studied. The recovery values at optimal conditions and detection limits for Au (III) were found as >95% and 3.8 μg L(-1), respectively. The factor of preconcentration was 250. The RSD value was determination of gold was applied to water, mine, soil, and anodic slime samples. PMID:26964845

  8. A new preconcentration and separation method for flame atomic absorption spectrometric determinations of some trace metal ions on a diaion HP-20 column

    A preconcentration/separation method for determination of Cr(3), Cd(2), Bi(3) and Co(2) has been proposed. The analytes were adsorbed on a column filled Diaion HP-20 resin as metal-8-hydroxiquinoline complexes and desorbed from the column by using 10 ml of 1M HNO3 in acetone. The influences of some analytical parameters such as pH, amounts of oxine, type of eluent etc on the recoveries of chromium, cadmium, bismuth and cobalt were discussed. Effects of the various alkaline salts on the recoveries of the investigated ions were also examined. The method was applied for the determination of Cr(3), Cd(2), Bi(3), and Co(2) contents of table salt samples, some chemical grade alkaline salts produced in Turkey and a stream sediment standard reference material sample (GBW 07309) with satisfactory results (recoveries > 95%, relative standard deviations < 9%). The limit of detection for analyte ions (3s, N=20) was between 23-305 ng/g

  9. Determination of actinides by alpha spectrometric methods

    attributes of mass activities of radionuclides in oyster mushroom's sporocarps compared to their sub-base. We used two methods to separate the monitored radionuclides in a radiochemical analyse. The first of them was an extraction fluid - fluid with Aliquat-336 to separate Pu and TOPO to separate Am. The second method was a proceeding modified by us and utilizing principles of an extraction chromatography with TRU Resin and DGA Resin sorbents made by Eichrom Company. An effectivity and a suitability of both applied methods were monitored following the attributes of radiochemical extractions used in tracer's radionuclides 242Pu a 243Am in this particular type of environmental samples. The reliability of the modified methodology, in accordance to selected criteria for validation of analytical method, was proved by comparison of both above mentioned methods. material delivered from IAEA, which presented a soil sample with code identification Soil IAEA-375. The obtained values of mass activities of 239+240Pu, 239Pu and 241Am used in reference material, demonstrated a conformity with IAEA values, whereby we fulfilled one of the significant conditions of validate process. At the end of this thesis we applied the modified method of extraction chromatography with UTEVA Resin sorbent to define mass activities of uranium on soil and water samples where we monitored attributes of radiochemical extractions of 232U tracer's radionuclide as the criteria of utilizability. The reliability of our modified method was verified by participation in international interlaboratory comparative proficiency tests and our results were in accordance with results of the reference laboratory. It means also a fulfilment of notable standard of the validate process. The results of all realized experimentations of radionuclides separation whether by extraction fluid - fluid or by extraction chromatography were determined by alpha-spectrometric measurements. (author)

  10. Flame atomic absorption spectrometric (FAAS) determination of copper, iron and zinc in food samples after solid-phase extraction on Schiff base-modified duolite XAD 761

    The present study involves the development of solid-phase extraction (SPE) procedure for the preconcentration of trace amounts of copper (Cu2+), iron (Fe3+) and zinc (Zn2+) ions on duolite XAD 761 modified by bis(2-hydroxyacetophenone)-2,2-dimethyl-1,3-propanediimine(BHAPDMPDI). The complexation between the metal ions and the proposed ligand was investigated potentiometrically. The metal ions retained on the sorbent were quantitatively determined via complexation with BHAPDMPDI. The complexed metal ions were efficiently eluted using 6 mL of 4 mol L−1 nitric acid in acetone. The influences of the analytical parameters, including pH, amounts of the ligand and the solid phase, eluent conditions and sample volume, on the recoveries of the metal ions were optimized. Using the optimized parameters, the linear response of the SPE method for Cu2+, Zn2+ and Fe3+ ions were in the ranges of 0.01–0.34, 0.01–0.28 and 0.02–0.31 μg mL−1, respectively, and the detection limits for Cu2+, Zn2+ and Fe3+ ions were 1.8, 1.6 and 2.4 μg mL−1, respectively. The proposed method exhibits a preconcentration factor of 208 for all of the ions studied and an enhancement factor for Cu2+, Fe3+ and Zn2+ ions of 34, 28 and 38, respectively. The presented results demonstrate the successful application of the proposed method for the determination of these metal ions in some real samples with high recoveries (> 95%) and reasonable relative standard deviation (RDS < 5%). Highlights: ► Highly efficient adsorbent for dye removal was synthesized. ► The sorbent was fully characterized. ► The proposed method has a potential of a waste water treatment alternative. ► Excellent properties of the sorbent have been illustrated in detail

  11. Accuracy of X-ray fluorescence spectrometric determination of Rb and Sr concentrations in rock samples

    It is shown that application of the Compton scattering for matrix correction in the X-ray fluorescence spectrometric determination of the trace elements Rb and Sr in rock samples can provide concentrations at a relative accuracy level of 1%. The empirical method applies to rock samples showing differences in mass absorption up to a factor of two. The accuracy of the method has been tested by analysis of 57 samples analysed for Rb and Sr by mass spectrometric isotope dilution. In addition a few of the U.S. Geological Survey reference rock powders, showing significantly different mass absorption, were analysed for Rb and Sr. It is demonstrated that the mica effect, if significant, is smaller than 1% relative. There is no advantage in the use of the LiF(220) analysing crystal as a substitute for the LiF(200). The method appears to be insensitive to the pellet thickness. (author)

  12. Determination of trace metal ions via on-line separation and preconcentration by means of chelating Sepharose beads in a sequential injection lab-on-valve (SI-LOV) system coupled to electrothermal atomic absorption spectrometric detection

    Long, Xiangbao; Hansen, Elo Harald; Miró, Manuel

    2005-01-01

    The analytical performance of an on-line sequential injection lab-on-valve (SI-LOV) system using chelating Sepharose beads as sorbent material for the determination of ultra trace levels of Cd(II), Pb(II) and Ni(II) by electrothermal atomic absorption spectrometry (ETAAS) is described and discussed...

  13. Photometric and emission-spectrometric determination of boron in steels

    A method for the photometric determination of boron in unalloyed and alloyed steels is described, in which Curcumine is used as reagent. A separation of boron is not necessary. Limit of detection: 0.0003% B. The decomposition of boron nitride in the steel is achieved by heating the whole sample in fuming sulphuric acid/phosphoric acid. For the emission spectrometric investigation of solid steel samples and for the spectrochemical analysis of solutions with plasma excitation working parameters are given and possibilities of interferences are demonstrated. (orig.)

  14. Photometric and emission-spectrometric determination of boron in steels

    Thierig, D.

    1982-01-01

    A method for the photometric determination of boron in unalloyed and alloyed steels is described, in which Curcumine is used as reagent. A separation of boron is not necessary. Limit of detection: 0.0003% B. The decomposition of boron nitride in the steel is achieved by heating the whole sample in fuming sulphuric acid/phosphoric acid. For the emission spectrometric investigation of solid steel samples and for the spectrochemical analysis of solutions with plasma excitation working parameters are given and possibilities of interferences are demonstrated.

  15. Spectrometric analysis of process etching solutions of the photovoltaic industry--determination of HNO3, HF, and H2SiF6 using high-resolution continuum source absorption spectrometry of diatomic molecules and atoms.

    Bücker, Stefan; Acker, Jörg

    2012-05-30

    The surface of raw multicrystalline silicon wafers is treated with HF-HNO(3) mixtures in order to remove the saw damage and to obtain a well-like structured surface of low reflectivity, the so-called texture. The industrial production of solar cells requires a consistent level of texturization for tens of thousands of wafers. Therefore, knowing the actual composition of the etch bath is a key element in process control in order to maintain a certain etch rate through replenishment of the consumed acids. The present paper describes a novel approach to quantify nitric acid (HNO(3)), hydrofluoric acid (HF), and hexafluosilicic acid (H(2)SiF(6)) using a high-resolution continuum source graphite furnace absorption spectrometer. The concentrations of Si (via Si atom absorption at the wavelength 251.611 nm, m(0),(Si)=130 pg), of nitrate (via molecular absorption of NO at the wavelength 214.803 nm, [Formula: see text] ), and of total fluoride (via molecular absorption of AlF at the wavelength 227.46 nm, m(0,F)=13 pg) were measured against aqueous standard solutions. The concentrations of H(2)SiF(6) and HNO(3) are directly obtained from the measurements. The HF concentration is calculated from the difference between the total fluoride content, and the amount of fluoride bound as H(2)SiF(6). H(2)SiF(6) and HNO(3) can be determined with a relative uncertainty of less than 5% and recoveries of 97-103% and 96-105%, respectively. With regards to HF, acceptable results in terms of recovery and uncertainty are obtained for HF concentrations that are typical for the photovoltaic industry. The presented procedure has the unique advantage that the concentration of both, acids and metal impurities in etch solutions, can be routinely determined by a single analytical instrument. PMID:22608457

  16. Flame atomic absorption spectrometric determination of zinc, nickel, iron and lead in different matrixes after solid phase extraction on sodium dodecyl sulfate (SDS)-coated alumina as their bis (2-hydroxyacetophenone)-1, 3-propanediimine chelates

    A sensitive and simple solid phase extraction method for the simultaneous determination of trace and toxic metals in food samples has been reported. The method is based on the adsorption of zinc, nickel, iron and lead on sodium dodecyl sulfate (SDS)-coated alumina, which is also chelated with bis (2-hydroxyacetophenone)-1, 3-propanediimine (BHAPN). The retained analyte ions on modified solid phase were eluted using 8 mL of 4 mol L-1 HNO3. The analyte determinations were carried out by flame atomic absorption spectrometry. The influences of some metal ions and anions on the recoveries of understudy analyte ions were investigated. The proposed method has been successfully applied for the evaluation of these trace and toxic metals in some traditional food samples from Iran.

  17. Solid phase extraction of cadmium on 2-mercaptobenzothiazole loaded on sulfur powder in the medium of ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate and cold vapor generation-atomic absorption spectrometric determination

    A novel solid phase extractor for preconcentration of cadmium at ng L-1 levels has been developed. Cadmium ions were retained on a column packed with sulfur powder modified with 2-mercaptobenzothiazole (2-MBT) in the medium of 1-butyl-3-methylimidazolium hexafluorophosphate ([bmim]+PF6-) ionic liquid. The presence of ionic liquid during modification of sulfur enhanced the retention of cadmium ions on the column. The retained cadmium ions were eluted with 2 mol L-1 solution of HCl and measured by cold vapor generation-atomic absorption spectrometry (CVG-AAS). By using reaction cell-gas liquid separator (RC-GLS), gaseous cadmium vapors were produced and reached the atomic absorption spectrometer, instantaneously. The influence of different variables on both processes of solid phase extraction and CVG-AAS determination of cadmium ions was investigated. The calibration curve was linear in the range of 10-200 ng L-1of cadmium in the initial solution with r = 0.9992 (n = 8) under optimum conditions. The limit of detection based on three times the standard deviation of the blank (3Sb, n = 10) was 4.6 ng L-1. The relative standard deviation (R.S.D.) of 25 and 150 ng L-1 of cadmium was 4.1 and 2.2% (n = 8), respectively. The procedure was validated by the analysis of a certified reference material (DORM-3), water and fish samples.

  18. Determination of iodine to compliment mass spectrometric measurements

    The dose of iodine-129 to facility personnel and the general public as a result of past, present, and future activities at DOE sites is of continuing interest, WINCO received about 160 samples annually in a variety of natural matrices, including snow, milk, thyroid tissue, and sagebrush, in which iodine-129 is determined in order to evaluate this dose, Currently, total iodine and the isotopic ratio of iodine-127 to iodine-129 are determined by mass spectrometry. These two measurements determine the concentration of iodine-129 in each sample, These measurements require at least 16 h of mass spectrometer operator time for each sample. A variety of methods are available which concentrate and determine small quantities of iodine. Although useful, these approaches would increase both time and cost. The objective of this effort was to determine total iodine by an alternative method in order to decrease the load on mass spectrometry by 25 to 50%. The preparation of each sample for mass spectrometric analysis involves a common step--collection of iodide on an ion exchange bed. This was the focal point of the effort since the results would be applicable to all samples

  19. Flame atomic absorption spectrometric determination of trace amounts of Pb(II) and Cr(III) in biological, food and environmental samples after preconcentration by modified nano-alumina

    A new solid-phase extraction sorbent was used for the preconcentration of Pb(II) and Cr(III) ions prior to their determination by flame atomic absorption spectrometry. It was prepared by immobilization of 2,4-dinitrophenylhydrazine on nano-alumina coated with sodium dodecyl sulfate. The sorbent was characterized by scanning electron microscopy, N2 adsorption and Fourier transform infrared spectrometry, and used for preconcentration and separation of Pb(II) and Cr(III) from aqueous solutions. The ions on the sorbent were eluted with a mixture of nitric acid and methanol. The effects of sample pH, flow rates of samples and eluent, type of eluent, breakthrough volume and potentially interfering ions were studied. Linearity is maintained between 1.2 and 350 μg L-1 of Pb(II), and between 2.4 and 520 μg L-1 of Cr(III) for an 800-mL sample. The detection limit (3 s, N=10) for Pb(II) and Cr(III) ions is 0.43 and 0.55 μg L-1, respectively, and the maximum preconcentration factor is 267. The method was successfully applied to the evaluation of these trace and toxic metals in various water, food, industrial effluent and urine samples. (author)

  20. Electrothermal atomic absorption spectrometric determination of vanadium in extracts of soil and sewage sludge certified reference materials after fractionation by means of the Communities Bureau of Reference modified sequential extraction procedure

    A modified three-step sequential extraction procedure proposed by the Commission of European Communities Bureau of Reference (BCR) was applied to certified reference materials of three different soil groups (rendzina, luvisol, cambisol) and sewage sludge of different composition originating from a municipal water treatment plant in order to assess potential mobility and the distribution of vanadium in the resulting fractions. Analysis of the extracts was carried out by electrothermal atomic absorption spectrometry with Zeeman background correction using transversely heated graphite atomizers. Extracts showed significant matrix interferences which were overcome by the standard addition technique. The original soil and sludge certified reference materials (CRMs) and the extraction residue from the sequential extraction were decomposed by a mixture of HNO3-HClO4-HF in an open system. The content of V determined after decomposition of the samples was in very good agreement with the certified total values. The accuracy of the sequential extraction procedure was checked by comparing the sum of the vanadium contents in the three fractions and in the extraction residue with the certified total content of V. The amounts of vanadium leached were in good correlation with the certified total contents of V in the CRMs of soils and sewage sludge. In the soils examined, vanadium was present almost entirely in the mineral lattice, while in the sewage sludge samples 9-14% was found in the oxidizable and almost 25% in the reducible fractions. The recovery ranged from 93-106% and the precision (RSD) was below 10%

  1. Method of double tracer addition for determining uranium in geological samples by mass spectrometric isotope dilution

    The present work shows the experimental details on the uranium determination in materials by mass spectrometric isotope dilution technique with double tracer (233U + 235U). The mass discrimination phenomenon effect is studied. The uranium concentration values obtained by mass spectrometric isotope dilution technique with double tracer are compared with other techniques. The influence of the sampling in the accurate determination of uranium in the rock sample is discussed. (author)

  2. Uranium determination using atomic spectrometric techniques: An overview

    This review focuses on the determination of uranium using spectroanalytical techniques that are aimed at total determination such as flame atomic absorption spectrometry (FAAS), electrothermal atomic absorption spectrometry (ETAAS), inductively coupled plasma optical emission spectrometry (ICP-OES); and inductively coupled plasma mass spectrometry (ICP-MS) that also enables the determination of uranium isotopes. The advantages and shortcomings related to interferences, precision, accuracy, sample type and equipment employed in the analysis are taken into account, as well as the complexity and costs (i.e., acquisition, operation and maintenance) associated with each of the techniques. Strategies to improve their performance that employ separation and/or preconcentration steps are considered, with an emphasis given to solid-phase extraction because of its advantages compared to other preconcentration procedures.

  3. Highly selective micro-sequential injection lab-on-valve (μSI-LOV) method for determination of ultra trace concentrations of nickel in saline matrices using detection by electrothermal atomic absorption spectrometr

    Long, Xiangbao; Miró, Manuel; Jensen, Rikard;

    2006-01-01

    electrothermal atomic absorption spectrometry (ETAAS). Based on the dimethylglyoxime (DMG) gravimetric procedure used for nickel analysis, the sample, as contained in pH 9.0 buffer, is, after on-line merging with the chelating reagent, transported to a reaction coil attached to one of the external ports of the...

  4. Radioisotope spectrometric method to determine diffusion coefficients in metals and alloys

    A brief description of the spectrometric installation to study diffusion in metals using #betta#-decay radio-isotopes is presented. Diffusion coefficients of nickel in 70% Co-5% Fe-15% Si-10% B amorphous alloy are determined according to #betta#-radiation absorption in diffusion zone. Plate samples of 10x10 mm size and about 300 μm in thickness are used. Diffusion annealing is conducted during 100 hrs. The calculation of the diffusion coefficients has been carried out by the formula I/I0= esup(μsup(2)Dtau)erfc μ √ Dtau, where I0, I is an initial and a final radiation intensity; μ- an absorption coefficient of 63Ni #betta#-ray in the given material (at calculation μ=1.3x106 m-1 was taken); tau- duration of diffusion annealing; D- diffusion coefficient at the designed temperature. The value of the diffusion coefficient of nickel in 70% Co-5% Fe-15% S-10% B amorphous alloy at the temperature of 200 deg C is turned out to be equal to 4x10-21 m2/s. It should be noted that the self-diffusion coefficient of cobalt in Co-Fe alloy, found by extrapolation from high-temperature region, is equal to 10-35 m2/s, i.e. in 14 orders lower than that of the same basis in amorphous alloy

  5. Spectrometric methods for the determination of chlorine in crude oil and petroleum derivatives — A review

    Doyle, Adriana [Department of Chemistry, Pontifical Catholic University of Rio de Janeiro, Rua Marquês de São Vicente 225, Gávea, Rio de Janeiro, RJ 22451-900 (Brazil); Saavedra, Alvaro; Tristão, Maria Luiza B.; Mendes, Luiz A.N. [Leopoldo Américo Miguez de Mello Research Center — Petrobras (CENPES), Cidade Universitária, Quadra 7, Ilha do Fundão, Rio de Janeiro 21949-900 (Brazil); Aucélio, Ricardo Q., E-mail: aucelior@puc-rio.br [Department of Chemistry, Pontifical Catholic University of Rio de Janeiro, Rua Marquês de São Vicente 225, Gávea, Rio de Janeiro, RJ 22451-900 (Brazil)

    2013-08-01

    Chlorine determination in crude oil is made in order to guarantee that the oil does not contain levels of this element that might cause damages in the oil processing equipment. In petroleum products, the determination of chlorine is made, for instance, to evaluate if there are proper concentrations of organochloride compounds, which are used as additives. Such determinations are currently performed following official guidelines from the ASTM International and from the United States Environmental Protection Agency as well as protocols indicated by the Universal Oil Products. X-ray fluorescence spectroscopy plays an important role in many of these official methods. In contrast, other spectrometric methods based on optical and mass detection are plagued by limitations related to both the fundamental characteristics of non-metals and to the complex sample matrices, which reflects in the small number of articles devoted to these applications. In this review, the current status of the spectrometric methods, especially the role played by X-ray fluorescence spectrometry, is evaluated in terms of the determination of chlorine in crude oil and petroleum derivatives. Comparison of the performance of the methods, limitations and potential new approaches to ensure proper spectrometric determinations of chlorine is indicated. - Highlights: • Critical evaluation of spectrometric methods for chlorine in petroleum products. • Reviews on element determination in petroleum have not address the case of chlorine. • Peculiarities of the spectrometric determination of Cl in petroleum are discussed. • The spectrometric approaches are detailed and compared to the official methods. • New trends in chlorine determination in petroleum products are indicated.

  6. Spectrometric methods for the determination of chlorine in crude oil and petroleum derivatives — A review

    Chlorine determination in crude oil is made in order to guarantee that the oil does not contain levels of this element that might cause damages in the oil processing equipment. In petroleum products, the determination of chlorine is made, for instance, to evaluate if there are proper concentrations of organochloride compounds, which are used as additives. Such determinations are currently performed following official guidelines from the ASTM International and from the United States Environmental Protection Agency as well as protocols indicated by the Universal Oil Products. X-ray fluorescence spectroscopy plays an important role in many of these official methods. In contrast, other spectrometric methods based on optical and mass detection are plagued by limitations related to both the fundamental characteristics of non-metals and to the complex sample matrices, which reflects in the small number of articles devoted to these applications. In this review, the current status of the spectrometric methods, especially the role played by X-ray fluorescence spectrometry, is evaluated in terms of the determination of chlorine in crude oil and petroleum derivatives. Comparison of the performance of the methods, limitations and potential new approaches to ensure proper spectrometric determinations of chlorine is indicated. - Highlights: • Critical evaluation of spectrometric methods for chlorine in petroleum products. • Reviews on element determination in petroleum have not address the case of chlorine. • Peculiarities of the spectrometric determination of Cl in petroleum are discussed. • The spectrometric approaches are detailed and compared to the official methods. • New trends in chlorine determination in petroleum products are indicated

  7. Carbon nanotubes as solid-phase extraction sorbents prior to atomic spectrometric determination of metal species: A review

    Highlights: ► The use of CNTs as sorbent for metal species in solid phase extraction has been described. ► Physical and chemical strategies for functionalization of carbon nanotubes have been discussed. ► Published analytical methods concerning solid phase extraction and atomic spectrometric determination have been reviewed. - Abstract: New materials have significant impact on the development of new methods and instrumentation for chemical analysis. From the discovery of carbon nanotubes in 1991, single and multi-walled carbon nanotubes – due to their high adsorption and desorption capacities – have been employed as sorption substrates in solid-phase extraction for the preconcentration of metal species from diverse matrices. Looking for successive improvements in sensitivity and selectivity, in the past few years, carbon nanotubes have been utilized as sorbents for solid phase extraction in three different ways: like as-grown, oxidized and functionalized nanotubes. In the present paper, an overview of the recent trends in the use of carbon nanotubes for solid phase extraction of metal species in environmental, biological and food samples is presented. The determination procedures involved the adsorption of metals on the nanotube surface, their quantitative desorption and subsequent measurement by means of atomic spectrometric techniques such as flame atomic absorption spectrometry, electrothermal atomic absorption spectrometry or inductively coupled plasma atomic emission spectrometry/mass spectrometry, among others. Synthesis, purification and types of carbon nanotubes, as well as the diverse chemical and physical strategies for their functionalization are described. Based on 140 references, the performance and general properties of the applications of solid phase extraction based on carbon nanotubes for metal species atomic spectrometric determination are discussed.

  8. Carbon nanotubes as solid-phase extraction sorbents prior to atomic spectrometric determination of metal species: A review

    Herrero Latorre, C., E-mail: carlos.herrero@usc.es [Universidad de Santiago de Compostela, Dpto. Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Alfonso X el Sabio s/n, 27002 Lugo (Spain); Alvarez Mendez, J.; Barciela Garcia, J.; Garcia Martin, S.; Pena Crecente, R.M. [Universidad de Santiago de Compostela, Dpto. Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Alfonso X el Sabio s/n, 27002 Lugo (Spain)

    2012-10-24

    Highlights: Black-Right-Pointing-Pointer The use of CNTs as sorbent for metal species in solid phase extraction has been described. Black-Right-Pointing-Pointer Physical and chemical strategies for functionalization of carbon nanotubes have been discussed. Black-Right-Pointing-Pointer Published analytical methods concerning solid phase extraction and atomic spectrometric determination have been reviewed. - Abstract: New materials have significant impact on the development of new methods and instrumentation for chemical analysis. From the discovery of carbon nanotubes in 1991, single and multi-walled carbon nanotubes - due to their high adsorption and desorption capacities - have been employed as sorption substrates in solid-phase extraction for the preconcentration of metal species from diverse matrices. Looking for successive improvements in sensitivity and selectivity, in the past few years, carbon nanotubes have been utilized as sorbents for solid phase extraction in three different ways: like as-grown, oxidized and functionalized nanotubes. In the present paper, an overview of the recent trends in the use of carbon nanotubes for solid phase extraction of metal species in environmental, biological and food samples is presented. The determination procedures involved the adsorption of metals on the nanotube surface, their quantitative desorption and subsequent measurement by means of atomic spectrometric techniques such as flame atomic absorption spectrometry, electrothermal atomic absorption spectrometry or inductively coupled plasma atomic emission spectrometry/mass spectrometry, among others. Synthesis, purification and types of carbon nanotubes, as well as the diverse chemical and physical strategies for their functionalization are described. Based on 140 references, the performance and general properties of the applications of solid phase extraction based on carbon nanotubes for metal species atomic spectrometric determination are discussed.

  9. Mass spectrometric determination of early and advanced glycation in biology.

    Rabbani, Naila; Ashour, Amal; Thornalley, Paul J

    2016-08-01

    Protein glycation in biological systems occurs predominantly on lysine, arginine and N-terminal residues of proteins. Major quantitative glycation adducts are found at mean extents of modification of 1-5 mol percent of proteins. These are glucose-derived fructosamine on lysine and N-terminal residues of proteins, methylglyoxal-derived hydroimidazolone on arginine residues and N(ε)-carboxymethyl-lysine residues mainly formed by the oxidative degradation of fructosamine. Total glycation adducts of different types are quantified by stable isotopic dilution analysis liquid chromatography-tandem mass spectrometry (LC-MS/MS) in multiple reaction monitoring mode. Metabolism of glycated proteins is followed by LC-MS/MS of glycation free adducts as minor components of the amino acid metabolome. Glycated proteins and sites of modification within them - amino acid residues modified by the glycating agent moiety - are identified and quantified by label-free and stable isotope labelling with amino acids in cell culture (SILAC) high resolution mass spectrometry. Sites of glycation by glucose and methylglyoxal in selected proteins are listed. Key issues in applying proteomics techniques to analysis of glycated proteins are: (i) avoiding compromise of analysis by formation, loss and relocation of glycation adducts in pre-analytic processing; (ii) specificity of immunoaffinity enrichment procedures, (iii) maximizing protein sequence coverage in mass spectrometric analysis for detection of glycation sites, and (iv) development of bioinformatics tools for prediction of protein glycation sites. Protein glycation studies have important applications in biology, ageing and translational medicine - particularly on studies of obesity, diabetes, cardiovascular disease, renal failure, neurological disorders and cancer. Mass spectrometric analysis of glycated proteins has yet to find widespread use clinically. Future use in health screening, disease diagnosis and therapeutic monitoring, and

  10. Cinchocaine hydrochloride determination by atomic absorption spectrometry and spectrophotometry.

    Abdel-Ghani, Nour T; Youssef, Ahmed F A; Awady, Mohamed A

    2005-05-01

    Two sensitive spectrophotometric and atomic absorption spectrometric procedures have been developed for determination of cinchocaine hydrochloride (Cin.Cl) in pure form and in pharmaceutical formulation. The spectrophotometric method was based on formation of an insoluble colored ion-associate between the cited drug and tetrathiocyanatocobaltate (CoTC) or hexathiocyanatochromate (CrTC) which dissolved and extracted in an organic solvent. The optimal experimental conditions for quantitative extraction such as pH, concentration of the reagents and solvent were studied. Toluene and iso-butyl alcohol proved to be the most suitable solvents for quantitative extraction of Cin-CoTC and Cin-CrTC ion-associates with maximum absorbance at 620 and 555 nm, respectively. The optimum concentration ranges, molar absorptivities, Ringbom ranges and Sandell sensitivities were also evaluated. The atomic absorption spectrometric method is based on measuring of the excess cobalt or chromium in the aqueous solution, after precipitation of the drug, at 240.7 and 357.9 nm, respectively. Linear application ranges, characteristic masses and detection limits were 57.99-361.9, 50.40 and 4.22 microg ml(-1) of Cin.Cl, in case of CoTC, while 37.99-379.9, 18.94 and 0.81 microg ml(-1) in case of CrTC. PMID:15910814

  11. X-ray spectrometric determination of thorium in bone and other biological materials

    An x-ray spectrometric method has been developed for the determination of thorium in bone and other biological materials. The limit of detection at the 95% confidence level is 20 ng. This corresponds to a concentration of 2 ppb in a 10-g sample of bone ash

  12. Atomic Absorption Spectrometric Method for Estimation of Diclofenac sodium and Mefenamic acid in Pharmaceutical Formulations

    Sunil Jawla

    2010-01-01

    Full Text Available Diclofenac sodium and Mefenamic acid have been quantified in tablet dosage form by atomic absorption spectrometry (AAS. These methods are based on formation of the metal complexes of Diclofenac sodium and Mefenamic acid with cupric chloride and cobaltous chloride. The first method is based on reaction of both the drugs with cupric chloride to give light blue colored metal complexes, which are then extracted with dichloromethane and digested with 0.1 M nitric acid. Both the drugs are indirectly estimated via determination of copper content in the formed complexes by AAS. The second method is based on the formation of pink colored complexes of both the drugs with cobaltous chloride. These metal complexes are extracted with dichloromethane and estimated via determination of cobalt content in the formed complexes after digestion with 0.1 M nitric acid by AAS.

  13. The accuracy of X-ray fluorescence spectrometric determination of Rb and Sr contents in rock sample

    It is shown that application of the Compton scattering method in the X-ray fluorescence spectrometric determination of the trace elements Rb and Sr in rock samples can provide element contents at an accuracy level +- 1 %

  14. Continuous flow hydride generation-atomic fluorescence spectrometric determination and speciation of arsenic in wine

    Methods for the atomic fluorescence spectrometric (AFS) determination of total arsenic and arsenic species in wines based on continuous flow hydride generation (HG) with atomization in miniature diffusion flame (MDF) are described. For hydride-forming arsenic, L-cysteine is used as reagent for pre-reduction and complexation of arsenite, arsenate, monomethylarsonate and dimethylarsinate. Concentrations of hydrochloric acid and tetrahydroborate are optimized in order to minimize interference by ethanol. Procedure permits determination of the sum of these four species in 5-10-fold diluted samples with limit of detection (LOD) 0.3 and 0.6 μg l-1 As in white and red wines, respectively, with precision between 2% and 8% RSD at As levels within 0.5-10 μg l-1. Selective arsine generation from different reaction media is used for non-chromatographic determination of arsenic species in wines: citrate buffer at pH 5.1 for As(III); 0.2 mol l-1 acetic acid for arsenite + dimethylarsinate (DMA); 8 mol l-1 HCl for total inorganic arsenic [As(III) + As(V)]; and monomethylarsonate (MMA) calculated by difference. Calibration with aqueous and ethanol-matched standard solutions of As(III) is used for 10- and 5-fold diluted samples, respectively. The LODs are 0.4 μg l-1 for As(III) and 0.3 μg l-1 for the other three As species and precision is within 4-8% RSDs. Arsenic species in wine were also determined by coupling of ion chromatographic separation on an anion exchange column and HG-flame AFS detection. Methods were validated by means of recovery studies and comparative analyses by HG-AFS and electrothermal atomic absorption spectrometry after microwave digestion. The LODs were 0.12, 0.27, 0.15 and 0.13 μg l-1 (as As) and RSDs were 2-6%, 5-9%, 3-7% and 2-5% for As(III), As(V), MMA and DMA arsenic species, respectively. Bottled red and white wines from Bulgaria, Republic of Macedonia and Italy were analyzed by non-chromatographic and chromatographic procedures and the As

  15. Mass spectrometric methods for studying nutrient mineral and trace element absorption and metabolism in humans using stable isotopes: a review

    Mass spectrometric methods for determining stable isotopes of nutrient minerals and trace elements in human metabolic studies are described and discussed. The advantages and disadvantages of the techniques of electron ionization, fast atom bombardment, thermal ionization, and inductively coupled plasma and gas chromatography mass spectrometry are evaluated with reference to their accuracy, precision, sensitivity, and convenience, and the demands of human nutrition research. Examples of specific applications are described and the significance of current developments in mass spectrometry are discussed with reference to present and probable future research needs. (Author)

  16. Extraction-mass spectrometric determination of platinum metals in materials of complex composition

    A method is developed for the extraction mass-spectrometric determination of platinum metals, including ruthenium. The loWer limit of detectable contents is 1.6x10-6 mass.% (a coefficient of concentration is 50). The relative standard deviation is 0.19-0.38. Relative sensitivity coefficients determined experimentally with the aid of reference samples for platinum metals enable the systematic errors of analysis results to be taken into account. The method is most advisably used for the simultaneous determination of platinum metals in complex objects (minerals, rocks, etc.)

  17. Determination of Mass Spectrometric Sensitivity of Different Metalloporphyrin Esters Relative to Porphyrin Ester

    Larsen, Elfinn; Egsgaard, Helge; Møller, J.; With, T. K.

    1977-01-01

    Quantitative determination of metalloporphyrin contamination in preparations of biologically important porphyrins was achieved mass spectrometrically by application of the integrated ion current technique. For this purpose, the relative molecular ion sensitivities of the contaminating metal compl...... complexes were determined from the ratios of the integrated molecular ion currents of a series of calibration samples containing a porphyrin ester and one of its metal complexes in known molar ratio. Complexes formed with divalent ions of Cu, Zn, Fe, Co and Ni of copro- as well as uro...

  18. Determination of spectrophotometric absorptivity by analytical ultracentrifugation

    M Senthilraja

    2011-01-01

    Full Text Available Rapid determination of the absorptivity for a recombinant IgG monoclonal antibody using the Beckman equipped with both Raleigh interference and UV absorbance optical systems. The analytical ultracentrifuge data for determining spectrophotometric absorptivities is compared to experimental data from quantitative amino acid analysis and an enzymatic digestion method.

  19. Flame atomic absorption determination of ultra trace zinc after preconcentration

    Complete text of publication follows. The determination of toxic metal ions is becoming increasingly important because of the increased interest in environmental samples including water, soil, plant, etc. Although flame atomic absorption spectrometry is widely used because of its low cost, its sensitivity is usually insufficient for the low concentrations found in environmental samples. Matrix interferences are another problem in atomic absorption spectrometric determinations of trace elements. Solving these problems requires a preconcentration and a matrix elimination step (A. Uzun et al., Talanta, 54, (2001)197). Zinc is a biologically essential micronutrient, and coordinates with macromolecules as a cofactor to confer catalytic function of structural integrity. Such metalloproteins have been implicated in diverse functions ranging from protein, nucleic acid, carbohydrate, and lipid metabolism, to gene transcription (B.L. Vallee et al., Physio. Revs, 73:1 (1993) 99). Zinc is frequently present at trace level in cadmium and their compounds. Numerous methods have been published for such determination. However, they are not simple and usually require extensive and laborious steps for separation of zinc from cadmium (C.W. McDonald et al., Anal. Chem., 46 (1974) 300). In this work a simple, reliable and rapid method for determination of ultra trace zinc by flame atomic absorption spectrometry is presented. The limit of detection (LOD), of the proposed method for the determination of Zn2+ ion was studied under the optimal experimental conditions. The LOD obtained from CLOD=KbSbm-1 (J.D. Ingle et al., Spectrochemical Analysis, Prentice Hall, Englewood Cliffs, NJ, 1988) for a numerical factor Kb=3 is 120 ng.L-1.The method was successfully applied for the determination of zinc ion in different samples, especially determination of ultra trace amount of zinc in waters and plants.

  20. Determination of trace quantities of uranium in rocks mass spectrometric isotope dilution technique

    A detailed experimental investigation on the thermionic emission of uranium deposited on a single flat type rhenium filament has been carried out. The study was aimed at determining the influence of various forms of deposition on the emission sensitivity and thermal stability of U+ , UO+ and UO2+ ions. Based on these investigations, a technique, involving an addition of a small quantity of colloidal suspension of graphite on top of the uranyl nitrate sample deposited, was chosen because of its higher, emission sensitivity for uranium metal ions. The experimental parameters of the technique were optimised and the technique was employed in the determination of trace quantities of uranium in rock samples using mass spectrometric isotope dilution method. For the mass spectrometric isotope dilution analysis National Bureau of Standards uranium isotopic standard NBS-U 970 was employed as a tracer, where as the mass discrimination effect in the uranium isotope analysis was corrected using the uranium isotopic standard NBS-U500. Uranium was determined in each of the seven granite samples from Wyoming, USA and two USGS standard rocks. The precision of the analysis was found to be ±1% . The uranium values obtained on the rock samples were compared with the analyses of other investigators. Influence of the sample splitting on the uranium analysis was discussed in the light of the analytical results obtained.(author)

  1. A simple method for determination of formaldehyde in seafood sample using spectrometric detection

    Complete text of publication follows. A simple method for determination of formaldehyde using spectrometric detection was developed. The reaction was based on the oxidation of methylene blue with hydrogen peroxide in acidic media. The decreased in absorbance of the reaction mixture was measured at 664 nm. The optimum reaction conditions were 1 x 10-6 M methylene blue, 0.01 M sulfuric acid and 0.02 M hydrogen peroxide. The linearity was 0-20 mg/l with the limit of determination 1.60 μg/g of sample. Extraction of formaldehyde in seafood samples were investigated by ultrasonic method. The percentage recovery in spiking sample was 98% with 30 min ultrasonic extraction. This proposed method was applied to determination of formaldehyde in seafood samples. The researcher gratefully acknowledge the support from Center of Excellence for Innovation in Chemistry (PERCH-CIC), Commission on Higher Education, Ministry of Education.

  2. Mass-spectrometric determination of trace elements in aqueous media without preconcentration

    Foss, G. O.

    1981-10-01

    Feasibility of using a low pressure glow discharge as an ion source for the mass spectrometric determination of trace elements in aqueous media was investigated. A cryogenically cooled hollow cathode ion source was developed to analyze aqueous samples without external preconcentration. Aqueous solutions containing seventy elements were analyzed and the detection limits, sensitivity factors, and linear regression correlation coefficients were determined. A standard test solution of trace elements in water was analyzed and the concentrations of trace elements were calculated using the sensitivity factors determined previously. The results compared favorably within the error limits predicted by the semiquantitative survey methods used. Tap water and natural lake water samples were examined and minimal interference effects due to organic compounds and biological compounds were noted. A research ion optical system (RIOS) was developed as a flexible mass analyzer for the development of new ion sources. The RIOS is a double focussing mass analyzer designed utilizing the Mattauch-Herzog geometry with externally adjustable slit assemblies.

  3. Particle size independent spectrometric determination of wear metals in aircraft lubricating oils

    A method for the particle size independent determination of Ni, Fe, Mg, Cu, Al, Sn, Mo, and Ti in synthetic ester lubricating oils by spectrometric analysis is presented. Partial dissolution of Cr, Si, Pb, and Ag also occurs. Used ester lubricating oils as well as samples prepared with -325 mesh (44 μm) or -200 mesh (74 μm) metal powders were reacted with a small amount of hydrofluoric acid and aqua regia at 650C for 45 min with ultrasonic agitation. The reacted mixture was then diluted with a methyl isobutyl ketone and isopropyl alcohol mixture and analyzed spectrometrically. The recoveries for metal powder suspensions of Ni, Fe, Mg, Cu, Al, Sn, Mo, and Ti ranged from 97 to 103% and the relative standard deviation ranged from 4 to 10%. In addition to the metal powder suspensions, over 200 aircraft oil samples were analyzed. The method is much faster and more convenient than previously reported particle size independent methods using ashing techniques

  4. Critical comparison of radiometric and mass spectrometric methods for the determination of radionuclides in environmental, biological and nuclear waste samples

    Hou, Xiaolin; Roos, Per

    2008-01-01

    The radiometric methods, alpha (alpha)-, beta (beta)-, gamma (gamma)-spectrometry, and mass spectrometric methods, inductively coupled plasma mass spectrometry, accelerator mass spectrometry, thermal ionization mass spectrometry resonance ionization mass spectrometry, secondary ion mass spectrometry, and glow discharge mass spectrometry are reviewed for the determination of radionuclides. These methods are critically compared for the determination of long-lived radionuclides important for rad...

  5. Determination of Mass Spectrometric Sensitivity of Different Metalloporphyrin Esters Relative to Porphyrin Ester

    Larsen, Elfinn; Egsgaard, Helge; Møller, J.;

    1977-01-01

    Quantitative determination of metalloporphyrin contamination in preparations of biologically important porphyrins was achieved mass spectrometrically by application of the integrated ion current technique. For this purpose, the relative molecular ion sensitivities of the contaminating metal...... complexes were determined from the ratios of the integrated molecular ion currents of a series of calibration samples containing a porphyrin ester and one of its metal complexes in known molar ratio. Complexes formed with divalent ions of Cu, Zn, Fe, Co and Ni of copro- as well as uro......-prophyrin permethylester were all found to have the same molecular ion sensitivities as their metal-free porphyrin ester. The relative metalloporphyrin ester content in a sample of porphyrin ester was thus obtained directly as the integrated ion current ratios of the normalized molecular ions. The preparation of...

  6. Quantitative analysis of sodium di-uranate for Al, Ca, Fe, Mg, Mn, Na by flame-atomic absorption spectrometric method

    Nuclear Fuel Complex (NFC) receives Sodium Di-Uranate (SDU) from Uranium Corporation of India Limited (UCIL) for producing sinterable UO2 pellets for manufacturing fuel sub assemblies. Several impurities present in ore find their way into SDU during its conversion. Stringent specification have been laid down by the reactor designs for achieving the optimum performance of the fuel and several impurity element like Al, Ca, Fe, Mg, Mn, Na among others affects severely performance of UO2 fuel. Most of the impurity including the above mentioned elements are generally analysed by ICP-OES method. However, determination of Al, Ca, Fe, Mg, Mn and Na by ICP-OES requires lot of dilution as they are present at high levels in SDU. Apart from introducing dilution error, dilution process is very tedious and time consuming work and not a preferred choice in an industrial lab like control lab where large analytical load exists and time bound analysis is a requirement. To avoid these difficulties a simple and reliable Flame Atomic absorption spectrometric technique has been developed for regular analysis. Present method involves dissolution of SDU sample in Conc. HNO3 and after the complete dissolution the sample solution has been evaporated to near dryness on a hot plate. Subsequently sample solution has been brought into 4N HNO3 medium

  7. Atomic-spectrometric determination of lithium, sodium, potassium and strontium in high-pure scandium

    Determination of lithium, sodium and potassium in strontium by flame photometry with atomic-absorption spectrophotometer is described. Scandium effect on value of Li, K. Na analytical signal in flame is studied. It is shown, that the base understates analytical signals. Determination of strontium by flame photometry is impossible. Determination of strontium (1x10-13 kg/ml) by atomic-absorption method with electrothermal atomization is possible

  8. Optical Path Length Calibration: A Standard Approach for Use in Absorption Cell-Based IR-Spectrometric Gas Analysis

    Javis Anyangwe Nwaboh; Oliver Witzel; Andrea Pogány; Olav Werhahn; Volker Ebert

    2014-01-01

    We employed a comparison method to determine the optical path length of gas cells which can be used in spectroscopic setup based on laser absorption spectroscopy or FTIR. The method is based on absorption spectroscopy itself. A reference gas cell, whose length is a priori known and desirably traceable to the international system of units (SI), and a gas mixture are used to calibrate the path length of a cell under test. By comparing spectra derived from pressure-dependent measurements on the ...

  9. Separation Techniques for Uranium and Plutonium at Trace Levels for the Thermal Ionization Mass Spectrometric Determination

    This report describes the state of the art and the progress of the chemical separation and purification techniques required for the thermal ionization mass spectrometric determination of uranium and plutonium in environmental samples at trace or ultratrace levels. Various techniques, such as precipitation, solvent extraction, extraction chromatography, and ion exchange chromatography, for separation of uranium and plutonium were evaluated. Sample preparation methods and dissolution techniques for environmental samples were also discussed. Especially, both extraction chromatographic and anion exchange chromatographic procedures for uranium and plutonium in environmental samples, such as soil, sediment, plant, seawater, urine, and bone ash were reviewed in detail in order to propose some suitable methods for the separation and purification of uranium and plutonium from the safeguards environmental or swipe samples. A survey of the IAEA strengthened safeguards system, the clean room facility of IAEA's NWAL(Network of Analytical Laboratories), and the analytical techniques for safeguards environmental samples was also discussed here

  10. Separation Techniques for Uranium and Plutonium at Trace Levels for the Thermal Ionization Mass Spectrometric Determination

    Suh, M. Y.; Han, S. H.; Kim, J. G.; Park, Y. J.; Kim, W. H

    2005-12-15

    This report describes the state of the art and the progress of the chemical separation and purification techniques required for the thermal ionization mass spectrometric determination of uranium and plutonium in environmental samples at trace or ultratrace levels. Various techniques, such as precipitation, solvent extraction, extraction chromatography, and ion exchange chromatography, for separation of uranium and plutonium were evaluated. Sample preparation methods and dissolution techniques for environmental samples were also discussed. Especially, both extraction chromatographic and anion exchange chromatographic procedures for uranium and plutonium in environmental samples, such as soil, sediment, plant, seawater, urine, and bone ash were reviewed in detail in order to propose some suitable methods for the separation and purification of uranium and plutonium from the safeguards environmental or swipe samples. A survey of the IAEA strengthened safeguards system, the clean room facility of IAEA's NWAL(Network of Analytical Laboratories), and the analytical techniques for safeguards environmental samples was also discussed here.

  11. Liquid chromatography-mass spectrometric determination of rufinamide in low volume plasma samples.

    Gáll, Zsolt; Vancea, Szende; Dogaru, Maria T; Szilágyi, Tibor

    2013-12-01

    Quantification of rufinamide in plasma was achieved using a selective and sensitive liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) method. The chromatographic separation was achieved on a reversed phase column (Zorbax SB-C18 100mm×3mm, 3.5μm) under isocratic conditions. The mobile phase consisted of a mixture of water containing 0.1% formic acid and methanol (50:50, v/v). The mass spectrometric detection of the analyte was in multiple reaction monitoring mode (MRM) using an electrospray positive ionization (ESI positive). The monitored ions were 127m/z derived from 239m/z rufinamide and 108m/z derived from 251m/z the internal standard (lacosamide). Protein precipitation with methanol was applied for sample preparation using only 50μl aliquots. The concentration range was 40-2000ng/ml for rufinamide in plasma. The limit of detection was 1.25ng/ml and the lower limit of quantification was established at 5ng/ml rufinamide concentration. Selectivity and matrix effect was verified using individual human, rat and rabbit plasma samples. Short-term, post-preparative and freeze-thaw stability was also investigated. The proposed method provides accuracy, precision and high-throughput (short runtime 4.5min) for quantitative determination of rufinamide in plasma. This is the first reported liquid chromatography-tandem mass spectrometric (LC-MS/MS) method for analysis of rufinamide from low volume plasma samples. The LC-MS/MS method was validated according to the current official guidelines and can be applied to accurately measure rufinamide level of large number of plasma samples from clinical studies or therapeutic drug monitoring. PMID:24140655

  12. Determination of Lead Content in Phosphate Rock and Concentrate Rock——Flame Atomic Absorption Spectrometric Method%火焰原子吸收光谱法测定磷矿石和精磷矿中的铅含量

    沈治荣; 梁聪; 甘丽; 何红莲

    2011-01-01

    This article describes determination of trace harmful heavy metal-lead element in phosphate rock and concentrate rock with flame atomic absorption spectrometry method.The relative standard deviation of this method is 3.1~14.2%,recovery rate is 90%~104%,the sample detection limit is 0.0008%.The method is accurate,fast,easy,make up for method of determination lead in phosphate rock.It provides effective control method for production of feed additives and fertilizers and so on.%研究了用火焰原子吸收光谱法测定磷矿石或磷精矿中微量的铅的检测方法。此方法的相对标准偏差为3.1%-14.2%,回收率为90%-104%,样品检测下限为0.0008%。

  13. Method Validation for the Gamma-ray Spectrometric Determination of Natural Radioactive Nuclides in NORM Samples - Method Validation for the Gamma-ray Spectrometric Determination of Natural Radionuclides in raw materials and by-products

    It has established the 'Act on safety control of radioactive rays around living environment' in Korea, since 2011, to protect the public from natural occurring radioactive materials (NORM) and their by-products. The increasing concerns regarding the radioactivity of those materials therefore dictate many demands for the radioactive analysis for them. There are several methods to determine the concentration of natural radionuclides, such as 235U, 238U, 226Ra, 232Th, and so on, through a radiochemical analysis using an alpha spectrometer, mass spectrometer and liquid scintillation counter. However, gamma-ray spectroscopy still has an effect on the assessment of radioactive concentration for these nuclides and their progenies. To adapt a gamma spectrometer to the determination of natural radionuclides, the feasibility of their analysis methods should be first verified and validated with respect to accuracy and time and cost constraints. In general, one of the well-known processes in analyzing uranium with a gamma spectrometer is an indirect measurement using the secular equilibrium state with their progenies in a sample. This method, however, demands the time elapsed about 3 weeks to reach the equilibrium state between 226Ra and 222Rn and the sufficient integrity of a sample bottle to prevent the leakage of radon isotopes which is a form of noble gas. The simple and quick method is to directly measure a full energy absorption peak of 186.2 keV from 226Ra without the secular equilibrium state between 226Ra and 222Rn in the common sample bottle. However, this direct measurement also has difficulties about the interference with a full energy absorption peak of 185.7 keV from 235U. In this study, direct measurement with the interference correction technique, which uses several reference peaks for gamma-rays from 235U and 234Th, and indirect measurement, which means the identification of 226Ra indicators such as 214Pb and 214Bi after the secular equilibrium in the NORM

  14. Determination of U and Th content in the zirconium purification process using alpha spectrometric method

    It has been performed determination of U and Th and decay daughter in the zirconium purification process using alpha spectrometric method. U and Th analysis applications as well as decay daughter of zirconium purification process done, from Na2ZrO3 dissolved stage, Na2ZrO3 dissolved with 4 M HCl, dissolving Chloride Zircon Oxide (ZOC) with 6M H2SO4 at 105°C the heating. The purpose of this study is to determine the concentration of U and Th and decay daughter of Na2ZrO3 dissolved process, Na2ZrO3 dissolved with 4 M HCl, dissolving Chlorid Zircon oxide (ZOC) with 6M H2SO4 at 105° C the heating. From the experiments it can be concluded that the Na2ZrO3 solution and ZrOCI2, there is no U and Th nuclides, where as in solution Zr5O8(SO4)2 there are U and Th content. (author)

  15. Determination of ash content of coal using nuclear borehole logging spectrometric gamma-gamma technique

    During the past decade, increasing effort has been given to monitoring coal quality in the search, production and preparation sequence. Considerable research and development has been carried out on nuclear methods for determination of ash in coal. A number of nuclear techniques are now well established for coal analysis. In particular, the spectrometric gamma-gamma technique is based on the existence of a simple correlation between the ash content and the equivalent atomic number of coal. This technique records and uses the count rates of the backscatter spectrum. These count rates describe the changes in spectral shape which are due to ash content variations. This method is presented along with a short review of the physical background. The report includes the simulation of in situ borehole probe readings using a MONTE CARLO tracking program. Simulating the transport through matter of gamma-rays by MONTE CARLO techniques essentially attempts to reproduce the actual statistical nature of the interaction processes. Random numbers are used throughout, along with known nuclear data, to select the parameters which influence a particle's history. Such an approach can deal with complex geometries through which the particles move. Biaising or weightening techniques are applied for variance reduction, so as to minimise the statistical errors. The basic features of biaising as well as the description of the program are given. A semi-theoretical approach is discussed for the determination of ash content of coal seam using the simulated spectrum

  16. Determination of fission cross-section and absolute fission yields using track-cum gamma-ray spectrometric technique

    The fission cross-section of 233Pa(2nth, f) using fission track technique has been determined for the first time using thermal neutron flux of the reactor APSARA. This is important from the point of view of advance heavy water reactor (AHWR), which is to be described. On the other hand, the yields of fission products in the fast neutron induced fission of minor actinides are important from the point accelerator driven sub critical system (ADSS). In view of that, absolute yields of fission products in the fast neutron induced fission of 238U, 237Np, 238,240Pu, 243Am and 244Cm have been determined using the fission track-cum gamma-ray spectrometric technique. The total number of fission occurring in the target was estimated by track technique, whereas the activities of the fission products have been determined using gamma-ray spectrometric technique. Detailed procedure and its importance are to be discussed. (author)

  17. Nasal absorption studies of granisetron in rats using a validated high-performance liquid chromatographic method with mass spectrometric detection.

    Woo, Jong Soo

    2007-06-01

    Granisetron is a selective 5-HT3 receptor antagonist that is used therapeutically for the prevention of vomiting and nausea associated with emetogenic cancer chemotherapy. Although forms of the drug are commercially available for intravenous and oral dosage, there is a need for intranasal delivery formulations in specific patient populations in which the use of these dosage forms may be unfeasible and/or inconvenient. A rapid and specific high-performance liq uid chromatography method with mass spectrometric detection (LC-MS) was developed and validated for the analysis of granisetron in plasma after nasal administration in rats. Granisetron was separated in a reverse-phase C-18 column without interference from other components of plasma. This method involves a rapid assay for the determination of granisetron in a small volume of plasma with a run time of 12 min using ondansetron as an internal standard. Data were acquired in the electrospray ionization (ESI) mode with positive ion detection and application of single ion recording (SIR). Granisetron and ondansetron were detected at m/z values of 313.2 and 294.2, respectively. The method described was found to be suitable for the analysis of all samples collected during preclinical pharmacokinetic investigations of granisetron in rats after nasal administration. To date, the first pharmacokinetic study after intranasal administration of granisetron was performed and some pharmacokinetic parameters were presented in this paper. Granisetron was found to be well absorbed through nasal route and the bioavailability of this drug following nasal administration was comparable with that of intravenous administration. PMID:17679558

  18. Arsenic and antimony determination in refined and unrefined table salts by means of hydride generation atomic absorption spectrometry--comparison of sample decomposition and determination methods

    AKSUNER, Nur; TİRTOM, Vedia Nüket; HENDEN, Emür

    2011-01-01

    An evaluation was made of different digestion methods for the determination of arsenic and antimony in table salt samples prior to hydride generation atomic absorption spectrometric analysis. Microwave acid digestion, classical wet digestion, dry ashing, and fusion were applied to the decomposition of salt samples and optimum conditions were investigated. Samples were decomposed by changing heating time, digestion techniques, and the amount and composition of acid, and then the concen...

  19. Column solid phase extraction and flame atomic absorption spectrometric determination of manganese(II) and iron(III) ions in water, food and biological samples using 3-(1-methyl-1H-pyrrol-2-yl)-1H-pyrazole-5-carboxylic acid on synthesized graphene oxide.

    Pourjavid, Mohammad Reza; Sehat, Ali Akbari; Arabieh, Masoud; Yousefi, Seyed Reza; Hosseini, Majid Haji; Rezaee, Mohammad

    2014-02-01

    A modified, selective, highly sensitive and accurate procedure for the determination of trace amounts of manganese and iron ions is established in the presented work. 3-(1-Methyl-1H-pyrrol-2-yl)-1H-pyrazole-5-carboxylic acid (MPPC) and graphene oxide (GO) were used in a glass column as chelating reagent and as adsorbent respectively prior to their determination by flame atomic absorption spectrometry. The adsorption mechanism of titled metals complexes on GO was investigated by using computational chemistry approach based on PM6 semi-empirical potential energy surface (PES). The effect of some parameters including pH, flow rate and volume of sample and type, volume and concentration of eluent, as well as the adsorption capacity of matrix ions on the recovery of Mn(II) and Fe(III) was investigated. The limit of detection was 145 and 162 ng L(-1) for Mn(II) and Fe(III), respectively. Calibration was linear over the range of 0.31-355 μg L(-1) for Mn(II) and 0.34-380 μg L(-1) for Fe(III) ions. The method was successfully applied for the determination of understudied ions in water, food and biological samples. PMID:24411390

  20. Determination of phytoplankton composition using absorption spectra

    Martínez Guijarro, Mª Remedios; Romero Gil, Inmaculada; Paches Giner, Maria Aguas Vivas; González del Rio Rams, Julio; Martí Insa, Carmen Mª; GIL SEGUÍ, GERMA; Ferrer, Alberto; FERRER, J.

    2009-01-01

    Characterisation of phytoplankton communities in aquatic ecosystems is a costly task in terms of time, material and human resources. The general objective of this paper is not to replace microscopic counts but to complement them, by fine-tuning a technique using absorption spectra measurements that reduces the above-mentioned costs. Therefore, the objective proposed in this paper is to assess the possibility of achieving a qualitative determination of phytoplankton communities by ...

  1. Determination of ractopamine in pig hair using liquid chromatography with tandem mass spectrometric detection.

    Wu, Junlin; Liu, Xiaoyun; Peng, Yunping

    2014-01-01

    A quantitative analytical procedure for the determination of ractopamine in pig hair has been developed and validated. The hair samples were washed and incubated at 75°C with isoxuprine and hair extraction buffer. The drug present was quantified using mixed solid-phase extraction and liquid chromatography with tandem mass spectrometric detection. The limit of quantization (LOQ) was 10pg/mg and the intra-day precision at 25pg/mg and 750pg/mg was 0.49% and 2.8% respectively. Inter-day precision was 0.88% and 3.52% at the same concentrations. The hair extraction percentage recovery at 25pg/mg and 50ng/mL was 99.47% and 103.83% respectively. The extraction percentage recovery at 25pg/mg and 50ng/mg was 93.52% and 100.26% respectively. Our results showed that ractopamine residues persist in hair in 24days of withdrawal and also showed the possibility to test ractopamine from pig hair samples. PMID:24548851

  2. Column solid phase extraction and flame atomic absorption spectrometric determination of manganese(II) and iron(III) ions in water, food and biological samples using 3-(1-methyl-1H-pyrrol-2-yl)-1H-pyrazole-5-carboxylic acid on synthesized graphene oxide

    Pourjavid, Mohammad Reza, E-mail: pourjavid@gmail.com [NFCRS, Nuclear Science and Technology Research Institute, P.O. Box 11365-8486, Tehran (Iran, Islamic Republic of); Sehat, Ali Akbari [Department of Analytical Chemistry, Faculty of Chemistry, University College of Science, University of Tehran, P.O. Box 14155-6455, Tehran (Iran, Islamic Republic of); Arabieh, Masoud; Yousefi, Seyed Reza; Hosseini, Majid Haji; Rezaee, Mohammad [NFCRS, Nuclear Science and Technology Research Institute, P.O. Box 11365-8486, Tehran (Iran, Islamic Republic of)

    2014-02-01

    A modified, selective, highly sensitive and accurate procedure for the determination of trace amounts of manganese and iron ions is established in the presented work. 3-(1-Methyl-1H-pyrrol-2-yl)-1H-pyrazole-5-carboxylic acid (MPPC) and graphene oxide (GO) were used in a glass column as chelating reagent and as adsorbent respectively prior to their determination by flame atomic absorption spectrometry. The adsorption mechanism of titled metals complexes on GO was investigated by using computational chemistry approach based on PM6 semi-empirical potential energy surface (PES). The effect of some parameters including pH, flow rate and volume of sample and type, volume and concentration of eluent, as well as the adsorption capacity of matrix ions on the recovery of Mn(II) and Fe(III) was investigated. The limit of detection was 145 and 162 ng L{sup −1} for Mn(II) and Fe(III), respectively. Calibration was linear over the range of 0.31–355 μg L{sup −1} for Mn(II) and 0.34–380 μg L{sup −1} for Fe(III) ions. The method was successfully applied for the determination of understudied ions in water, food and biological samples. - Highlights: • We use synthesized graphene oxide as adsorbent for SPE of Mn(II) and Fe(III) ions. • Adsorption mechanism was investigated by PM6 semi-empirical potential energy surface. • Detection limits were 145 and 162 ng L{sup −1} for Mn and Fe, respectively. • The preconcentration factor was 325 and sample flow rate is 8 mL min{sup −1}. • It was successfully applied to the determination of Mn and Fe ions in real samples.

  3. Analytical Method Validation of Gamma Spectrometric Procedure for the Determination of γ-Emitters in Environmental Samples

    It is internationally recognized that validation is necessary in analytical laboratories. The use of validated methods is important for an analytical laboratory to show its qualification and competency. This work describes the methods for validation of gamma spectrometric analytical procedure in the determination of some gamma emitters in environmental samples. The method was tested and validated in terms of repeatability, trueness, reproducibility in accordance with ISO guidelines using IAEA reference materials with different matrixes and compositions

  4. Determination of phytoplankton composition using absorption spectra.

    Martínez-Guijarro, R; Romero, I; Pachés, M; Del Río, J G; Martí, C M; Gil, G; Ferrer-Riquelme, A; Ferrer, J

    2009-05-15

    Characterisation of phytoplankton communities in aquatic ecosystems is a costly task in terms of time, material and human resources. The general objective of this paper is not to replace microscopic counts but to complement them, by fine-tuning a technique using absorption spectra measurements that reduces the above-mentioned costs. Therefore, the objective proposed in this paper is to assess the possibility of achieving a qualitative determination of phytoplankton communities by classes, and also a quantitative estimation of the number of phytoplankton cells within each of these classes, using spectrophotometric determination. Samples were taken in three areas of the Spanish Mediterranean coast. These areas correspond to estuary systems that are influenced by both continental waters and Mediterranean Sea waters. 139 Samples were taken in 7-8 stations per area, at different depths in each station. In each sample, the absorption spectrum and the phytoplankton classes (Bacyllariophyceae (diatoms), Cryptophyceae, Clorophyceae, Chrysophyceae, Prasynophyceae, Prymnesophyceae, Euglenophyceae, Cyanophyceae, Dynophyceae and the Synechococcus sp.) were determined. Data were analysed by means of the Partial Least Squares (PLS) multivariate statistical technique. The absorbances obtained between 400 and 750 nm were used as the independent variable and the cell/l of each phytoplankton class was used as the dependent variable, thereby obtaining models which relate the absorbance of the sample extract to the phytoplankton present in it. Good results were obtained for diatoms (Bacillarophyceae), Chlorophyceae and Cryptophyceae. PMID:19269434

  5. Microwave Digestion and Continuum Source Atomic Absorption Spectrometric Determination of Six Metal Elements in Medlar(Mespilus germanica L.) Fruit%微波消解-连续光源原子吸收法快速顺序测定枸杞果中的6种金属元素

    高向阳; 王银娟; 卢彬

    2011-01-01

    A new rapid method was established to determine metal elements in medlar fruit by microwave digestion and continuum source atomic absorption spectrometry.Samples were subjected to microwave digestion before simultaneous determination of six metal elements,including iron,zinc,copper,manganese,cadmium and lead.The established method presented a limit of detection ranging from 0.006070 to 0.04975 μg/L.The precision RSDs were between 1.5% and 5.0%(n = 12).The mean spike recoveries for the six metal elements ranged from 86.68% to 111.7%(n = 6).This method has been used to simultaneously determine iron,zinc,copper,manganese,cadmium and lead in medlar fruit with the benefits of rapidity,simplicity and low cost and satisfying results.%建立一种微波消解-连续光源原子吸收法快速测定枸杞果中金属元素的新方法。通过微波消解快速处理样品,用连续光源原子吸收法同时顺序测定枸杞果中的铁、锌、铜、锰、镉、铅6种金属元素,并对仪器使用条件、金属元素含量、精密度、检出限、回收率等进行研究。结果表明:方法检出限为0.006 07 0~0.04975μg/L,RSD为1.5%~5.0%,回收率为86.68%~111.7%。该法用于枸杞中6种金属元素的同时顺序测定,具有快速、简便、成本低廉等特点,分析结果令人满意。

  6. Atomic absorbtion spectrometric determination of platinum, palladium and rhodium in catalysts for automotive exhaust

    Analytical parameters of the electrothermal atomic absorption spectrometry method have been optimized for determination of platinum, palladium and rhodium in ceramic-supported catalysts for automobile exhaust gas treatment. Two chemical sample preparation methods have been proposed. In order to simplify the sample preparation procedure and to prevent the possible losses of platinum group metals the treatment of the previously ground sample with a mixture of mineral acids is recommended. (authors)

  7. Solid Phase Extraction of Lead Using Eggshell Membrane in Water Samples Prior to Graphite Furnace Atomic Absorption Spectrometric Determination%鸡蛋膜固相萃取-石墨炉原子吸收光谱法测定水样中的微量铅

    刘金; 彭元; 陈红梅; 程先忠

    2012-01-01

    鸡蛋膜是由蛋白质组成的一种纤维状的生物膜.本研究利用扫描电镜和红外光谱对鸡蛋膜的结构进行分析表征,证实其具有网状结构,表面存在着—OH、—COOH、—NH2等官能团,能与一些金属离子产生吸附和交换作用.在pH =6的条件下,用蛋膜作吸附剂分离富集水样中的微量铅,5 mL 3%的硝酸进行洗脱,然后采用石墨炉原子吸收光谱法进行测定.实验中对吸附分离介质、溶液流速、蛋膜用量、洗脱剂浓度及共存离子的影响等条件进行了优化和讨论.在最佳的实验条件下,蛋膜对铅的富集倍数为30,方法检出限(3σ)为0.017 ng/mL,相对标准偏差(RSD,n=11)为3.45%,加标回收率为96.0% ~ 104.2%.与现行的分离富集方法相比,建立的方法具有简单、无毒、成本低的优点,用于实际水样中铅的分析能够获得满意的结果.%A chicken eggshell membrane (ESM) is composed of many protein fibers, and available in large quantities as a by-product of the food industry. According to a study by Scanning Electron Microscope ( SEM ) and Fourier Transform Infrared ( FTIR) Spectrometry, the ESM with an intricate lattice network of stable and water-insoluble fibers, and special functional groups such as hydroxyl ( —OH) , carboxyl ( —COOH) , aminol ( —NH2 ) , showed an excellent potential for adsorption and exchange of metal ions. In this paper, the ESM was applied to separate and enrich Pb (II) from a water sample under a pH of 6. The trace lead eluted by 5 mL 3% HN03 was determined by using Graphite Furnace Atomic Absorption Spectrometry ( GFAAS ) . Important parameters, such as the sample pH, sample flow rate, concentration and volume of eluent, and interference of coexisting ions were comprehensively studied and optimized. Under the optimized conditions, an enrichment factor of 30 was obtained. The method detection limit for lead was 0.017 ng/mL (3

  8. Atomic emission and atomic absorption spectrometric analysis of high-purity powders for the production of ceramics

    Direct analysis methods and multistage combined analytical procedures for the determination of impurities at the μg/g level and the upper ng/g level in high-purity powders of Al2O3, AlN, Si3N4 and SiC are described. Results obtained with a novel direct slurry-atomization technique using a Babington nebulizer and inductively coupled plasma optical emission spectrometry (ICP-OES) are presented. A comparison of analysis results of combined analytical procedures including wet chemical decomposition and determinations with graphite furnace atomic absorption spectrometry (ETAAS) or ICP-OES with those of slurry-atomization ICP-OES show the capabilities of this technique for routine analysis in production control. Detection limits for Al, B, Ca, Co, Cu, Fe, Mg, Mn, Si, Ti, W, V, and Zn in the matrices mentioned are between 0.03 and 2.5 μg/g. For elemental concentrations ≥10 μg/g relative standard deviations of the measurements are generally below 10%. The technique is shown to be a powerful tool for trace determinations in powder samples. This is shown by its use for analysis of a series of the ceramic powders mentioned and comparative results of other direct techniques such as total reflection X-ray fluorescence spectrometry and instrumental neutron activation analysis. (orig.)

  9. Chromatographic separation and inductively coupled plasma atomic emission spectrometric determination of the rare earth metals contained in terbium

    The chromatographic separation of rare earth elements (REEs), prior to inductively coupled plasma atomic emission spectrometric (ICP-AES) measurements, using a column packed with 2-ethylexyl hydrogen 2-ethyl-hexylphosphonate (PC-88A)-loaded polymer resin in order to exclude spectral interferences was examined. A favourable separation of trace amounts of metals (La, Nd and Sm) from a large amount of terbium was achieved simply by elution with dilute hydrochloric acid. Trace lanthanum and neodymium in metallic terbium were determined by separation of the analyte ions from the matrix element followed by ICP-AES analysis. (author). 16 refs.; 5 figs.; 2 tabs

  10. Determination of gold by chemical hydride generation atomic absorption spectrometry

    Complete text of publication follows. The chemical vapour generation (CVG) of transition and noble metals opens a novel route for introduction of these elements into atomic spectrometric sources. It can be accomplished by merging an acidic sample with tetrahydroborate reductant solution (Y. L. Feng et al., J. of Anal. At. Spectrom., 20 (2005) 255-265). There have been some studies for determination of Au; however, only mg L-1 levels of gold have been determined by CVG - Atomic Absorption Spectrometry (AAS) (G. Ertas et al., Applied Spectroscopy, 60 (2006) 423-429). Volatile Au species were generated in flow injection arrangement from acid environment in presence of surfactants. The core of the system is a mixing manifold based on 3 concentric capillaries (T. Matousek et al., J. of Anal. At. Spectrom., 18 (2003) 487-494) protruding into the glass gas-liquid separator (glass, volume 3 ml). Optimum flow rate of Ar as a carrier gas was found at 240 mL/min. The study of generation parameters as well as the use of reaction modifiers-surfactants and dithiocarbamate- will be presented. Quartz tube multiatomizer for AAS was employed for atomization. Atomization conditions including composition of carrier gases and their flow rates and atomization temperature were optimized. 900 deg C was found as the optimum atomization temperature; over 900 deg C, peak area of Au signal decreased; in addition, peak shape was altered. A sharp maximum of 6 mL/min oxygen as the outer gas was observed. Another important point was that hydrogen-rich atmosphere caused signal depression. Analytical performance of this approach to generation and atomization will be discussed and perspectives of its future will be outlined. This work was supported by the GA ASCR (grant No. A400310507 and IAA400310704) and Institute of Analytical Chemistry of the ASCR, v.v.i. (project no. AV0Z40310501). This work also was supported from OYP (Faculty Development Program) from the Middle East Technical University

  11. Critical comparison of radiometric and mass spectrometric methods for the determination of radionuclides in environmental, biological and nuclear waste samples.

    Hou, Xiaolin; Roos, Per

    2008-02-11

    The radiometric methods, alpha (alpha)-, beta (beta)-, gamma (gamma)-spectrometry, and mass spectrometric methods, inductively coupled plasma mass spectrometry, accelerator mass spectrometry, thermal ionization mass spectrometry, resonance ionization mass spectrometry, secondary ion mass spectrometry, and glow discharge mass spectrometry are reviewed for the determination of radionuclides. These methods are critically compared for the determination of long-lived radionuclides important for radiation protection, decommissioning of nuclear facilities, repository of nuclear waste, tracer application in the environmental and biological researches, these radionuclides include (3)H, (14)C, (36)Cl, (41)Ca, (59,63)Ni, (89,90)Sr, (99)Tc, (129)I, (135,137)Cs, (210)Pb, (226,228)Ra, (237)Np, (241)Am, and isotopes of thorium, uranium and plutonium. The application of on-line methods (flow injection/sequential injection) for separation of radionuclides and automated determination of radionuclides is also discussed. PMID:18215644

  12. Development of a mass spectrometrical isotope dilution analysis for determination of trace iodine levels and its application for food samples

    A mass spectrometrical isotope dilution procedure for the determination of trace amounts of iodine in various materials was developed using 129I as indicator isotope, based on the determination of the 129I/127I isotope relationship. Negative thermionization was used as ionization method. The analysis procedure, which worked with a standard deviation of between 0,1 and 10% (depending on material tested), was used to determine the iodine level of table salt - both iodized and normal salt (3-6 ppm and less than 0,006 ppm respectively), and food samples with an organic matrix. For comparison the iodine levels were also measured with an iodine-selective electrode. Special preparation and separation procedures were done to suit the sample material. A comparison of the levels of iodine concentration in various powdered milks which were measured by international collaborators using varying methods shows the superior reproducibility of the MS-IDA. (RB)

  13. Application of wall-stabilized plasma arc for the spectrometric determination of impurity elements in uranium yellow cake

    The application of a seeded wall-stabilized argon plasma arc as an excitation source for the emission spectrometric determination of some impurity elements in a sample of uranium yellow cake has been investigated. The sample was dissolved in nitric acid. Uranium was extracted from the sample solution using tributyl phosphate (TBP), and the aqueous solution was injected into the arc. The elements determined were Al, Ca, Fe, Mg, Mn, Mo, Sr and Zr. Limits of detection and precision of the technique are presented. The study of the influence of residual uranium in the nebulized solution on the intensity of spectral lines revealed that uranium concentrations up to 100 μg mL-1 have no significant interfering effect

  14. Determination of Cd(II, Zn(II and Ag(Iin different matrixes after solid phase extraction on sodium dodecyl sulfate(SDS-coated alumina as their 2,3 Di Hydro 2,3 paratolylQinazoline (1 H- 4 one (DPTQO by Flame atomic absorption spectrometric

    Farveh Raoufi

    2016-03-01

    Full Text Available A sensitive and selective solid phase extraction procedure for the determination of traces of Cd(II, Zn(II and Ag(I ions has been developed. An alumina-sodium dodecyl sulfate (SDS coated on with 2,3 Di Hydro 2,3 paratolylQinazoline (1 H- 4 one (DPTQO. The influences of the analytical parameters including pH and sample volume were investigated.Common coexisting ions did not interfere on the separation and determination of analytes under study. The adsorbed analytes were desorbed by using 6mL of 4 mol L−1 nitric acid. The responses are linear 0.02–0.85 µg mL-1 for Cd2+ ion0.01–0.90 µg mL-1 for Zn2+and0.02–0.92µg mL-1for Ag+ detection limit for Cd(II, Zn(II and Ag(I ions were found to be 1.4, 1.3 and1.12(ng mL-1, respectively.It was found that the recovery for Cd2+, Zn2+and Ag+ ions were 97.7, 98.2 and 98.0 with RSD of 1.9, 1.8 and 1.7. It was also observed that recovery for repeated recovery on the same solid phase not varies more than 3%. The presented procedurewas successfully applied for determination of analytes in radiology wastewater, amalgam, natural water and blood samples.

  15. Application and evaluation of the mass spectrometric isotope dilution technique in the determination of rare earths in geological materials

    Establishment of the experimental procedures employed in the rare earth element determination of geological samples by mass spectrometric isotope dilution analysis is discussed in the present work. The procedures involve preparation and calibration of the isotope tracers isotope dilution, dissolution in a teflon pressure vessel, chemical separation and isotope analysis using a fully automated Micromass VG ISOTOPES model 354 thermal ionization mass spectrometer. For the initial chemical separation of total rare earths the cationic resin was employed and HC1 and HNO3 acids as eluents. In the second step rare earths elements were separated into individual (La, Ce and Nd) and subgroups (Sm-Eu-Gd, Yb-Er-Dy) fractions using the same cationic resin and α-HIBA as eluent. Nine elements La, Ce, Nd, Sm, Eu, Gd, Dy, Er and Yb are determined by this method in the ''United States Geological Survey'' (USGS) standard samples GSP-1, AGV-1 and G-2, with an overall precision of +- 1 to 2% and an accuracy of 5%. The concentration of rare earth element determined in the standard sample PCC-1 showed that the total analytical blanks are in submicrogram levels. The concentration of rare earth elements in the same USGS standard samples were also determined by Instrumental neutron activation analysis, neutron activation analysis with chemical separation before irradiation and inductively coupled argon plasma spectroscopy. The chemical procedures employed for these methods are the same as that used for mass spectrometric isotope dilution. Based on the results obtained, each method was evaluated pointing out their merits and defects. The study clearly showed that the chemical procedure employed for all these techniques was satisfactory. (author)

  16. Determining Absorption, Emissivity Reduction, and Local Suppression Coefficients inside Sunspots

    Ilonidis, Stathis; Zhao, Junwei

    2010-01-01

    The power of solar acoustic waves is reduced inside sunspots mainly due to absorption, emissivity reduction, and local suppression. The coefficients of these power-reduction mechanisms can be determined by comparing time-distance cross-covariances obtained from sunspots and from the quiet Sun. By analyzing 47 active regions observed by SOHO/MDI without using signal filters, we have determined the coefficients of surface absorption, deep absorption, emissivity reduction, and local suppression....

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

    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 μg 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)

  18. Geração eletroquímica do hidreto de selênio em sistema de injeção em fluxo com detecção por espectrometria de absorção atômica com chama Ar-Glp Electrochemical hydride generation for selenium determination in a flow injection system with Air-GLP flame atomic absorption spectrometric detection

    Luís Fernando Rebel Machado; Antonio Octavio Jacintho; Maria Fernanda Giné

    2000-01-01

    This paper presents a system for electrochemical hydride generation using flow-injection and atomic absorption spectrometry to determine selenium in biological materials. The electrolytic cell was constructed by assembling two reservoirs, one for the sample and the other for the electrolytic solution separated by a Nafion membrane. Each compartment had a Pt electrode. The sample and electrolyte flow-rates, acidic media, and applied current were adjusted to attain the best analytical performan...

  19. Determination of lithium and potassium in uranium oxide powders and pellets by Flame Atomic Emission Spectrometric method

    The present paper describes a method developed at Control Laboratory, NFC which includes prior separation of lithium and potassium from uranium matrix before their measurements. Solvent extraction, using Tri-n-Butyl Phosphate (TBP) in CCI4 followed by Tri-n-Octyl Phosphine Oxide (TOPO) in CCI4, is employed for prior separation of Li and K. The resultant aqueous solution was analyzed by Flame-Atomic Emission Spectrometric (AES) method. Solvent extraction conditions are optimized for measurement of Li and K in the same aliquot. Experimental conditions such as instrument calibration, flame condition, fuel flow, sample flow rate through nebulizer, burner height etc. are also optimized. Under the optimal condition the detection limits achieved for lithium is 0.02 ppm and 0.2 ppm for potassium. A RSD of ± 3 % for Li at 0.05 ppm and ± 4% for K at 1 ppm level has been achieved in this method. The results of lithium in the sample are compared with the values obtained by Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES). Similarly, values of potassium are compared with Flame-Atomic Absorption Spectrometry (Flame-AAS) technique. The comparisons are in good agreement. The above method is simple, sensitive, reproducible and can be used for measurement of lithium and potassium in UO2 powder and pellets on regular basis

  20. Atomic absorption spectroscopic, conductometric and colorimetric methods for determination of some fluoroquinolone antibacterials using ammonium reineckate

    Al-Ghannam, Sheikha M.

    2008-04-01

    Three accurate, rapid and simple atomic absorption spectrometric (AAS), conductometric and colorimetric methods were developed for the determination of gatifloxacin (GTF), moxifloxacin (MXF) and sparfloxacin (SPF). The proposed methods depend upon the reaction of ammonium reineckate with the studied drugs to form stable precipitate of ion-pair complexes, which was dissolved in acetone. The pink coloured complexes were determined either by AAS or colorimetrically at λmax 525 nm directly using the dissolved complex. Using conductometric titration, the studied drugs could be evaluated in 50% (v/v) acetone. The optimizations of various experimental conditions were described. Optimum concentration ranges for the determination of GTF, MXF and SPF were 5.0-150, 40-440 μg mL -1 and 0.10-1.5 mg mL -1 using atomic absorption (AAS), conductometric and colorimetric methods, respectively. Detection and quantification limits are ranges from 1.5 to 2.3 μg mL -1 using AAS method or 30-45 μg mL -1 using colorimetric method. The proposed procedures have been applied successfully to the analysis of these drugs in pharmaceutical formulations and the results are favourably comparable to the reference methods.

  1. Automated sequential injection-microcolumn approach with on-line flame atomic absorption spectrometric detection for implementing metal fractionation schemes of homogeneous and non-homogeneous solid samples of environmental interest

    Chomchoei, Roongrat; Miró, Manuel; Hansen, Elo Harald;

    2005-01-01

    spectrometric detection and used for the determination of Cu as a model analyte, the potentials of this novel hyphenated approach are demonstrated by the ability of handling up to 300 mg sample of a nonhomogeneous sewage amended soil (viz., CRM 483). The three steps of the endorsed Standards, Measurements, and...

  2. The Flame Spectrometric Determination of Calcium in Fruit Juice by Standard Addition.

    Strohl, Arthur N.

    1985-01-01

    Provides procedures to measure the calcium concentration in fruit juice by atomic absorption. Fruit juice is used because: (1) it is an important consumer product; (2) large samples are available; and (3) calcium exists in fruit juice at concentrations that do not require excessive dilution or preconcentration prior to measurement. (JN)

  3. Internal standard method in α spectrometric determination of uranium and thorium radioisotopes using instrumental neutron activation analysis

    A new approach to α spectrometric determination of the radioisotopes of uranium and thorium was developed for environmental samples based on 238U and 232Th as internal standards. 238U and 232Th were accurately determined in the sample by simultaneous instrumental neutron activation analysis. Other aliquots of the sample were totally dissolved, uranium and thorium separated by anion exchange, and thin sources electroplated for α spectrometry. From the known mass concentrations of 238U and 232Th, their activity concentrations were obtained, and thus from the relative ratios of uranium (234U, 235U, 238U) and thorium (228Th, 230Th, 232Th) radioisotopes in the α spectra, the absolute isotopic activity concentrations were derived. The advantages of the procedure are that neither the chemical recovery of the radiochemical separation nor the counting efficiency of the α spectrometer is required; the use of internal standards eliminates the need for addition of expensive, calibrated, external radioisotopic tracers such as 232U and 229Th. The new approach was tested on some certified environmental reference materials and compared with the classical method using external radioisotopic tracers. It may advantageously be combined with the standard approach to obtain an independent set of data for quality control. 25 refs

  4. Determination of nickel in active pharmaceutical ingredients by electrothermal atomic absorption spectrometry.

    Bubnič, Zoran; Urleb, Uroš; Kreft, Katjuša; Veber, Marjan

    2010-03-01

    An electrothermal atomic absorption spectrometric procedure for the determination of nickel in active pharmaceutical ingredients was developed. Since the recoveries of nickel by the direct dissolution of samples in diluted nitric acid were low and caused errors in the determination of Ni in pharmaceutical samples, different approaches for sample pre-treatment were examined. It was found that the microwave digestion was the most suitable way for sample preparation. Various combinations of digestion agents and different microwave conditions were tested. The combination of nitric acid and hydrogen peroxide was found to be the most appropriate. The validity of the method was evaluated by recovery studies of spiked samples and by the comparison of the results obtained by inductively coupled plasma mass spectrometry (ICP-MS). The recovery ranged from 87.5 to 104.0% and a good agreement was achieved between both methods. The detection limit and the limit of quantification were 0.6 and 2.1 µg g-1 respectively. The precision of the method was confirmed by the determination of Ni in the spiked samples and was below 4%, expressed in terms of a relative standard deviation. The method was applied to the determination of nickel in production samples of active pharmaceutical ingredients and intermediates. PMID:24061653

  5. Partial vapor-phase hydrolysis of peptide bonds: A method for mass spectrometric determination of O-glycosylated sites in glycopeptides

    Mirgorodskaya, E; Hassan, H; Wandall, H H;

    1999-01-01

    resulting mass spectra allowed unambiguous determination of the glycosylation sites. Examples are shown with mannosyl- and mucin-type glycopeptides. Performing the hydrolysis in vapor eliminates the risk for contamination of the sample with impurities from the reagents, thus allowing analysis of the......In this study we present a method for determination of O-glycosylation sites in glycopeptides, based on partial vapor-phase acid hydrolysis in combination with mass spectrometric analysis. Pentafluoropropionic acid and hydrochloric acid were used for the hydrolysis of glycosylated peptides. The...... reaction conditions were optimized for efficient polypeptide backbone cleavages with minimal cleavage of glycosidic bonds. The glycosylated residues were identified by mass spectrometric analysis of the hydrolytic cleavage products. Although glycosidic bonds are partially cleaved under acid hydrolysis, the...

  6. Determination of the total absorption peak in an electromagnetic calorimeter

    Cheng, Jia-Hua; Wang, Zhe; Lebanowski, Logan; Lin, Guey-Lin; Chen, Shaomin

    2016-08-01

    A physically motivated function was developed to accurately determine the total absorption peak in an electromagnetic calorimeter and to overcome biases present in many commonly used methods. The function is the convolution of a detector resolution function with the sum of a delta function, which represents the complete absorption of energy, and a tail function, which describes the partial absorption of energy and depends on the detector materials and structures. Its performance was tested with the simulation of three typical cases. The accuracy of the extracted peak value, resolution, and peak area was improved by an order of magnitude on average, relative to the Crystal Ball function.

  7. Determination of the total absorption peak in an electromagnetic calorimeter

    Cheng, Jia-Hua; Lebanowski, Logan; Lin, Guey-Lin; Chen, Shaomin

    2016-01-01

    A physically-motivated function was developed to accurately determine the total absorption peak in an electromagnetic calorimeter and to overcome biases present in many commonly used methods. The function is the convolution of a detector resolution function with the sum of a delta function, which represents the complete absorption of energy, and a tail function, which describes the partial absorption of energy and depends on the detector materials and structures. Its performance was tested with the simulation of three typical cases. The accuracy of the extracted peak value, resolution, and peak area was improved by an order of magnitude on average, relative to the Crystal Ball function.

  8. Determination of trace amounts of scandium by atomic absorption spectroscopy.

    Chau, Y K

    1968-05-01

    Optimum instrumental conditions were investigated for the determination of trace quantities of scandium by atomic-absorption spectroscopy. Enhancement effects by organic solvents and by complex extractions were also studied. (46)Sc was used to establish the optimum extraction conditions. A sensitivity of 0.06 ppm of Sc was observed when using extraction into oxine-butanol and atomic absorption was measured with an acetylene-nitrous oxide flame. PMID:18960315

  9. Direct atomic absorption determination of cadmium in solid foodstuffs

    A procedure is proposed for the direct rapid determination of cadmium in solid foodstuff samples by atomic absorption analysis using a modified Lvov furnace equipped with a graphite partition filter. The use of this furnace eliminates the step of transferring a solid sample to solution, allows calibration solutions to be employed properly in the direct analysis of solid samples, suppresses unselective absorption, and substantially shortens the time of analysis. 12 refs., 3 figs., 2 tabs

  10. Spectrometric Methods Used to Determine Heavy Metals and Total Cyanides in Accidental Polluted Soils

    A. Mihaly-Cozmuta; L. M. Cozmuta; V. Viman; Gh. Vatca; Varga, C.

    2005-01-01

    The study presents the level of soil pollution in the area adjacent to three sedimentation ponds as a result of an environmental accident. Soil samples from various sites have been collected and analyzed to determine the concentration of heavy metals (Cu, Pb, Zn) and total cyanides. The analysis methods used were ICP-AES for heavy metals and the colorimetric for total cyanides. The accuracy of both methods is determined subject to the reproducibility of the results. The values of determined c...

  11. Determination of cadmium in aluminium by atomic absorption spectrometry

    A direct method for the determination of cadmium in elemental aluminium is described. Metal samples are dissolved in diluted hydrochloric acid and cadmium is determined by atomic absorption spectrometry in an air-acetylene flame. Interference by non-specific absorption observed at the analytical wavelength incorrected for by means of a non-absorbing line emitted by the hollow-cathode lamp. Relatively large amounts of arsenic do not interfere. The minimun determinable concentration of cadmium for this procedure is 2-3 ppm, expressed on aluminium basis. (author)

  12. Determination of trace elements in cosmetic by X-ray spectrometric techniques (1994-95)

    Trace elements in cosmetic such as talcum powder, baby powder, Myanma Thanakh were determined by EDXRF analysis. The measurement system consists of a Cd-109 annual excitation source, a Si(Li) detector, H.V. power supply, a spectroscopy amplifier, a multichannel analyser and a personnel computer. The samples were prepared as pressed pellets and measured by emission transmission technique. The accuracy was determined by analysing standard reference material, SOIL-7 from IAEA. (author)

  13. Comparison of accelerator mass spectrometric measurement with liquid scintillation counting measurement for the determination of {sup 14}C in environmental samples

    Yasuike, Kaeko, E-mail: k-yasuike@hokuriku-u.ac.j [Faculty of Pharmaceutical Sciences, Hokuriku University, Ho-3, Kanagawa-machi, Kanazawa, Ishikawa 920-1181 (Japan); Yamada, Yoshimune [Faculty of Pharmaceutical Sciences, Hokuriku University, Ho-3, Kanagawa-machi, Kanazawa, Ishikawa 920-1181 (Japan); Amano, Hikaru [AMS Management Section, Japan Atomic Energy Agency, 4-24, Minato-machi, Mutsu, Aomori 035-0064 (Japan)

    2010-04-15

    The concentrations of organically-bound {sup 14}C in tree-ring cellulose of a Japanese Black Pine grown in Shika-machi (37.0 deg. N, 136.8 deg. E) and those of a Japanese Cedar grown in Kanazawa (36.5 deg. N, 136.7 deg. E), Japan, were analyzed for the ring-years from 1989 to 1998 by the accelerator mass spectrometric measurement. The results were compared with those of the same samples analyzed by the liquid scintillation counting measurement to determine the reliability of liquid scintillation counting measurement. An important result of this study is that the sensitivity and reproducibility of accelerator mass spectrometric measurement was almost equal to that of liquid scintillation counting measurement.

  14. 'Age' determination of irradiated materials utilizing inductively coupled plasma mass spectrometric (ICP-MS) detection

    A gas pressurized extraction chromatography (GPEC) system has been developed to perform elemental separations on radioactive samples to determine total and isotopic compositions of Cs and Ba from an irradiated salt sample, fuel sample and two sealed radiation sources. The GPEC system employs compressed nitrogen to move liquid through the system, compared to gravity or pumped liquids that are typically used for separations. A commercially available Sr-ResinTM was used to perform the separation for the above mentioned analytes. A 1% acetic acid solution was determined to be the best extractant for Ba. A flow rate of 0.1 mL/min was determined to be optimal for the separation of Ba. Complete recovery of the Cs and Ba was achieved, within the systematic uncertainties of the experiments. (author)

  15. Advanced miniaturized plasmas as atomic spectrometric detectors for elemental determinations and speciation in environmental sciences

    Miniaturized plasmas can be well used for determinations of the elements in a wide variety of environmentally relevant samples. All analytes, which can be brought in the gaseous phase can be easily determined with a wide diversity of microplasmas, whereas in liquids glow discharges where the sample solution serves as one of the electrodes is useful. For monitoring metals in gases also possibilities are available. The range of applications of the devices certainly still can be widened considerably when using mass spectrometry detection. By on-line combinations with chromatography the devices certainly also are very useful for metal speciation work.

  16. Determination of rhenium in molybdenite by X-ray fluorescence. A combined chemical-spectrometric technique

    Solt, M.W.; Wahlberg, J.S.; Myers, A.T.

    1969-01-01

    Rhenium in molybdenite is separated from molybdenum by distillation of rhenium heptoxide from a perchloric-sulphuric acid mixture. It is concentrated by precipitation of the sulphide and then determined by X-ray fluorescence. From 3 to 1000 ??g of rhenium can be measured with a precision generally within 2%. The procedure tolerates larger amounts of molybdenum than the usual colorimetric methods. ?? 1969.

  17. Simultaneous Laser Thermal Lens Spectrometric Determination of Trace Platinum and Palladium in an Aqueous Solution

    ZHANG,Xiao-Ling(张小玲); YAN,Hong-Tao(阎宏涛)

    2002-01-01

    A selective and sensitive method for determination of platinum and palladium(Ⅱ) in an aqueous solntion simultaneously by laser thermal lens spectrometry, based on the complex reaction of 2- (3,5-dichloropyridylazo)-5- dimethylaminoamiline (3,5-diCl-PADMA) with platinum and palladium, has been developed. It is shown that the palladium complex can be formed at room temperature, while the platinum complex can be only formed after being heated in a boiling water bath. By using this difference of reaction temperature and the characteristic of the complexes mentioned above, the method for simultaneous determination of platinum and palladium was established in an aqueous solution without a pre-separation. The results show that the dynamic linear ranges of determination for platinum and pallladium are 0.005-0.04 μg/mL and 0.005-0.25 μg/mL respectively, and that the detection limits are both 0.002 μg/mL. The method has been applied to the determination of platinum and palladium simultaneously in alloy and catalyst samples with satisfactory results.

  18. Simultaneous Laser Thermal Lens Spectrometric Determination of Trace Platinum and Palladium in an Aquesous Solution

    张小玲; 阎宏涛

    2002-01-01

    A selective and sensitive method for determination of platinum and palladium(Ⅱ)in an aqueous solution simultaneously by laser thermal lens spectrometry,based on the complex reaction of 2-(3,5-dichloropyridylazo)-5-dimethylaminoamiline(3,5-diCl-PADMA) with platinum and palladium,has been developed.It is shown that the palladium complex can be fromed at room temperature, while the platinum complex can be only formed after being heated in a boiling water bath.By using this difference of reaction temperature and the characteristic of the complexes mentioned above,the method for simultaneous determination of platinum and palladium was established in an aqueous solution without a pre-separation.The results show that the dynamic linear ranges of determination for platinum and palladium are 0.005-0.04μg/mL and 0.005-0.25μg/mL respectively,and that the detection limits are both 0.002/μg/mL.The method has been applied to the determination of platinum and palladium simultaneously in alloy and catalyst samples with satisfactory results.

  19. A photon spectrometric dose-rate constant determination for the Advantage Pd-103 brachytherapy source

    Purpose: Although several dosimetric characterizations using Monte Carlo simulation and thermoluminescent dosimetry (TLD) have been reported for the new Advantage Pd-103 source (IsoAid, LLC, Port Richey, FL), no AAPM consensus value has been established for the dosimetric parameters of the source. The aim of this work was to perform an additional dose-rate constant (Λ) determination using a recently established photon spectrometry technique (PST) that is independent of the published TLD and Monte Carlo techniques. Methods: Three Model IAPD-103A Advantage Pd-103 sources were used in this study. The relative photon energy spectrum emitted by each source along the transverse axis was measured using a high-resolution germanium spectrometer designed for low-energy photons. For each source, the dose-rate constant was determined from its emitted energy spectrum. The PST-determined dose-rate constant (PSTΛ) was then compared to those determined by TLD (TLDΛ) and Monte Carlo (MCΛ) techniques. A likely consensus Λ value was estimated as the arithmetic mean of the average Λ values determined by each of three different techniques. Results: The average PSTΛ value for the three Advantage sources was found to be (0.676±0.026) cGyh-1 U-1. Intersource variation in PSTΛ was less than 0.01%. The PSTΛ was within 2% of the reported MCΛ values determined by PTRAN, EGSnrc, and MCNP5 codes. It was 3.4% lower than the reported TLDΛ. A likely consensus Λ value was estimated to be (0.688±0.026) cGyh-1 U-1, similar to the AAPM consensus values recommended currently for the Theragenics (Buford, GA) Model 200 (0.686±0.033) cGyh-1 U-1, the NASI (Chatsworth, CA) Model MED3633 (0.688±0.033) cGyh-1 U-1, and the Best Medical (Springfield, VA) Model 2335 (0.685±0.033) cGyh-1 U-1103Pd sources. Conclusions: An independent Λ determination has been performed for the Advantage Pd-103 source. The PSTΛ obtained in this work provides additional information needed for establishing a more

  20. Determination of fixed water in rocks by infrared absorption

    Breger, I.A.; Chandler, J.C.

    1969-01-01

    An infrared absorption technique has been developed for the quantitative determination of "fixed water" (H2O+) in rocks. Potassium bromide disks containing 2-mg samples are scanned in the 3-??m spectral region and absorption at 2.96 ??m is determined. Although the exact nature of this peak is not known, other than that it is caused by an interaction between the potassium bromide and hydroxyl groups and water, it can be used for quantitative analysis. Rock samples, other than those containing significant percentages of clay minerals, can be analyzed with a standard deviation of 0.26%.

  1. Determination of γ-spectrometric parameters for some chloride salt solutions

    The mass attenuation coefficients, atomic cross-sections and effective atomic numbers are determined for LiCl, NaCl and KCl solutions with contents up to 0.2 g cm-3.The energies used are 0.511, 0.662 and 1.274 keV. The combined results were employed to determine the mass attenuation coefficients and atomic cross-sections of the salts and water in the solutions. The results are compared with the calculated values from elemental data. It was found that the mass attenuation coefficients and corresponding total cross-sections are, in general, less from measurement than from tabulated data, either for water or for the chloride salts

  2. Mass-spectrometric determination of serum cortisol: comparison of data from two independent laboratories

    Isotope dilution and mass spectrometry were used in two independent laboratories to determine cortisol in 15 plasma and serum pools used in the British and German national schemes for the external quality assessment of routine assays. For the concentration range 240-700 nmol/L, differences between the data obtained by the two laboratories were generally less than 4% but were approximately 7% in two instances. The discrepancies are nevertheless small in comparison with the bias observed for many routine assays

  3. Determination of rhenium in molybdenite by X-ray fluorescence: A combined chemical-spectrometric technique.

    Solt, M W; Wahlberg, J S; Myers, A T

    1969-01-01

    Rhenium in molybdenite is separated from molybdenum by distillation of rhenium heptoxide from a perchloric-sulphuric acid mixture. It is concentrated by precipitation of the sulphide and then determined by X-ray fluorescence. From 3 to 1000 microg of rhenium can be measured with a precision generally within 2%. The procedure tolerates larger amounts of molybdenum than the usual colorimetric methods. PMID:18960464

  4. Microwave plasma atomic emission spectrometric determination of Ca, K and Mg in various cheese varieties.

    Ozbek, Nil; Akman, Suleyman

    2016-02-01

    Microwave plasma-atomic emission spectrometry (MP-AES) was used to determine calcium, magnesium and potassium in various Turkish cheese samples. Cheese samples were dried at 100 °C for 2 days and then digested in a mixture of nitric acid/hydrogen peroxide (3:1). Good linearities (R(2) > 0.999) were obtained up to 10 μg mL(-1) of Ca, Mg and K at 445.478 nm, 285.213 nm and 766.491 nm, respectively. The analytes in a certified reference milk powder sample were determined within the uncertainty limits. Moreover, the analytes added to the cheese samples were recovered quantitatively (>90%). All determinations were performed using aqueous standards for calibration. The LOD values for Ca, Mg and K were 0.036 μg mL(-1), 0.012 μg mL(-1) and 0.190 μg mL(-1), respectively. Concentrations of Ca, K and Mg in various types of cheese samples produced in different regions of Turkey were found between 1.03-3.70, 0.242-0.784 and 0.081-0.303 g kg(-1), respectively. PMID:26304350

  5. A mass spectrometric method to determine activities of enzymes involved in polyamine catabolism

    Moriya, Shunsuke; Iwasaki, Kaori [Department of Molecular Medicine, Tokyo Metropolitan Institute of Medical Science, 2-1-6 Kami-kitazawa, Setagaya-ku, Tokyo 156-8506 (Japan); Samejima, Keijiro, E-mail: samejima-kj@igakuken.or.jp [Department of Molecular Medicine, Tokyo Metropolitan Institute of Medical Science, 2-1-6 Kami-kitazawa, Setagaya-ku, Tokyo 156-8506 (Japan); Takao, Koichi [Faculty of Pharmaceutical Sciences, Josai University, 1-1 Keyakidai, Sakado, Saitama 350-0295 (Japan); Kohda, Kohfuku [Research Institute of Pharmaceutical Sciences, Musashino University, 1-1-20 Shinmachi, Nishitokyo, Tokyo 202-8585 (Japan); Hiramatsu, Kyoko; Kawakita, Masao [Department of Molecular Medicine, Tokyo Metropolitan Institute of Medical Science, 2-1-6 Kami-kitazawa, Setagaya-ku, Tokyo 156-8506 (Japan)

    2012-10-20

    Highlights: Black-Right-Pointing-Pointer Compounds in polyamine catabolic pathway were determined by a column-free ESI-TOF MS. Black-Right-Pointing-Pointer N{sup 1}- and N{sup 8}-acetylspermidine were determined by a column-free ESI-MS/MS. Black-Right-Pointing-Pointer The method was applied to determine activities of APAO, SMO, and SSAT in the pathway. Black-Right-Pointing-Pointer The assay method contained stable isotope-labeled natural substrates. Black-Right-Pointing-Pointer It is applicable to biological samples containing natural substrate and product. - Abstract: An analytical method for the determination of three polyamines (putrescine, spermidine, and spermine) and five acetylpolyamines [N{sup 1}-acetylspermidine (N{sup 1}AcSpd), N{sup 8}-acetylspermidine (N{sup 8}AcSpd), N{sup 1}-acetylspermine, N{sup 1},N{sup 8}-diacetylspermidine, and N{sup 1},N{sup 12}-diacetylspermine] involved in the polyamine catabolic pathway has been developed using a hybrid tandem mass spectrometer. Heptafluorobutyryl (HFB) derivatives of these compounds and respective internal standards labeled with stable isotopes were analyzed simultaneously by TOF MS, based on peak areas appearing at appropriate m/z values. The isomers, N{sup 1}AcSpd and N{sup 8}AcSpd were determined from their fragment ions, the acetylamidopropyl and acetylamidobutyl groups, respectively, using MS/MS with {sup 13}C{sub 2}-N{sup 1}AcSpd and {sup 13}C{sub 2}-N{sup 8}AcSpd which have the {sup 13}C{sub 2}-acetyl group as an internal standard. The TOF MS method was successfully applied to measure the activity of enzymes involved in polyamine catabolic pathways, namely N{sup 1}-acetylpolyamine oxidase (APAO), spermine oxidase (SMO), and spermidine/spermine N{sup 1}-acetyltransferase (SSAT). The following natural substrates and products labeled with stable isotopes considering the application to biological samples were identified; for APAO, [4,9,12-{sup 15}N{sub 3}]-N{sup 1}-acetylspermine and [1,4,8-{sup 15}N{sub 3

  6. Determination of suvorexant in human plasma using 96-well liquid-liquid extraction and HPLC with tandem mass spectrometric detection.

    Breidinger, S A; Simpson, R C; Mangin, E; Woolf, E J

    2015-10-01

    A method, using liquid chromatography with tandem mass spectrometric detection (LC-MS/MS), was developed for the determination of suvorexant (MK-4305, Belsomra(®)), a selective dual orexin receptor antagonist for the treatment insomnia, in human plasma over the concentration range of 1-1000ng/mL. Stable isotope labeled (13)C(2)H3-suvorexant was used as an internal standard. The sample preparation procedure utilized liquid-liquid extraction, in the 96-well format, of a 100μL plasma sample with methyl t-butyl ether. The compounds were chromatographed under isocratic conditions on a Waters dC18 (50×2.1mm, 3μm) column with a mobile phase consisting of 30/70 (v/v %) 10mM ammonium formate, pH3/acetonitrile at a flow rate of 0.3mL/min. Multiple reaction monitoring of the precursor-to-product ion pairs for suvorexant (m/z 451→186) and (13)C(2)H3-suvorexant (m/z 455→190) on an Applied Biosystems API 4000 tandem mass spectrometer was used for quantitation. Intraday assay precision, assessed in six different lots of control plasma, was within 10% CV at all concentrations, while assay accuracy ranged from 95.6 to 105.0% of nominal. Quality control (QC) samples in plasma were stored at -20°C. Initial within day analysis of QCs after one freeze-thaw cycle showed accuracy within 9.5% of nominal with precision (CV) of 6.7% or less. The plasma QC samples were demonstrated to be stable for up to 25 months at -20°C. The method described has been used to support clinical studies during Phase I through III of clinical development. PMID:26343269

  7. Gas chromatographic-mass spectrometric determination of ethyl carbamate in alcoholic beverages.

    Lau, B P; Weber, D; Page, B D

    1987-07-31

    A sensitive and specific method based on gas chromatography-mass spectrometry for the quantitative determination of ethyl carbamate in table wines, fortified wines (such as ports and sherries), distilled spirits, brandies and liqueurs has been developed. Three characteristic ions from ethyl carbamate [m/z 89 (molecular ion), 74 and 62] were monitored in the selected-ion monitoring (SIM) mode. The lowest detection limit (based on the response on the m/z 62 ion) was estimated to be 0.5 ng/g (ppb). Additional confirmation techniques, including high-resolution SIM, and methane or isobutane chemical ionization are described. PMID:3654867

  8. A computer program for nuclear fuel burnup determination using gamma spectrometric methods

    In the end of its service life in the reactor, the fuel needs to be characterized for reasons relating both to safety and economy. The main investigations carried out are oriented towards verifying the fuel cladding integrity and determining the fissile content and the fuel burnup. A computer program for fast burnup evaluation was developed at the Post-Irradiation Examination Laboratory (PIEL) from INR Pitesti, the only laboratory of this kind in Romania. The input data consists, on one hand, of axial and radial gamma-scanning profiles (for the experimental evaluation of the number of nuclei of a given fission product - selected as burnup monitor - in the end of irradiation) and, on the other hand, of the history of irradiation (the time length and relative value of the neutron flux for each step of irradiation). Using the equation for the build-up and decay of the burnup monitor during irradiation the flux value is iteratively adjusted until the calculated number of nucleus is equal to the experimental one. Then the flux value is used in the equations of evolution of the fissile and fertile nuclei to determine the number of fissions and consequently the fuel burnup. The program was successfully used in the analysis of more then one hundred of TRIGA and CANDU-type fuel rods. An experimental result is reported in some details. (authors)

  9. Segregation during crystal growth from melt and absorption cross section determination by optical absorption method

    ZHANG QingLi; YIN ShaoTang; SUN DunLu; WAN SongMing

    2008-01-01

    Segregation during crystal growth from melt under two conditions is studied by using crystal mass, which can be measured easily, as an independent variable, and a method to determine the effective segregation coefficient and absorption cross section of optical dopant is given. When the segregated solute disperses into the whole or just a part of melt homogenously, the concentration Cs in solid interface will change by different formulas. If the crystal growth interface is conical and segregated solute disperses into melt in total or part, the solute concentration at r=2/3R, where r is the distance from the growth cross section center and R the crystal radius, is independent on the shape of the crystal growth interface, and its variation at r=2/3R can be regarded as the result from crystal growth in flat interface. With Cs variation formula in solid and absorption cross section σ for optical dopant, the absorption coefficients along the crystal growth direction can be calculated, and the corresponding experimental value can be obtained through the crystal optical absorption spectra. By minimizing the half sum, whose independent variables are k, △W or σ, of the difference square between the calculated and experimental absorp-tion coefficients from one or more absorption peaks along the crystal growth di-rection, k and σ, or k and △W, can be determined at the same time through the Levenberg-Marquardt iteration method. Finally, the effective segregation coefficient k, △W and absorption cross sections of Nd:GGG were determined, the results fitted by two formula gave more closed effective segregation coefficient, and the value △W also indicates that the segregated dopant had nearly dispersed into the whole melt. Experimental results show that the method to determine effective segregation coefficient k, △W and absorption cross sections σ is convenient and reliable, and the two segregation formulas can describe the segregation during the crystal growth from

  10. Simultaneous kinetic spectrometric determination of three flavonoid antioxidants in fruit with the aid of chemometrics

    Sun, Ruiling; Wang, Yong; Ni, Yongnian; Kokot, Serge

    2014-03-01

    A simple, inexpensive and sensitive kinetic spectrophotometric method was developed for the simultaneous determination of three anti-carcinogenic flavonoids: catechin, quercetin and naringenin, in fruit samples. A yellow chelate product was produced in the presence neocuproine and Cu(I) - a reduction product of the reaction between the flavonoids with Cu(II), and this enabled the quantitative measurements with UV-vis spectrophotometry. The overlapping spectra obtained, were resolved with chemometrics calibration models, and the best performing method was the fast independent component analysis (fast-ICA/PCR (Principal component regression)); the limits of detection were 0.075, 0.057 and 0.063 mg L-1 for catechin, quercetin and naringenin, respectively. The novel method was found to outperform significantly the common HPLC procedure.

  11. Determination of rare earth elements by liquid chromatographic separation using inductively coupled plasma mass spectrometric detection

    High-performance liquid chromatography (HPLC) is used to separate the rare earth elements (REEs) prior to detection by inductively coupled plasma mass spectrometry (ICP-MS). The use of HPLC-ICP-MS in series combines the separation power and speed of HPLC with the sensitivity, isotopic selectivity and speed of ICP-MS. The detection limits for the REEs are in the sub-ng ml-1 range and the response is linear over four orders of magnitude. A preliminary comparison of isotope dilution and external standard results for the determination of REEs in National Institute of Standards and Technology (NIST) Standard Reference Material (SRM 1633a) Fly Ash is presented. (author)

  12. Gamma-ray spectrometric enrichment determination of a low enriched UF6 sample

    Non-destructive gamma-ray spectroscopic measurements have been done on a solid 80-gram UF6 sample in the framework of an interlaboratory measurement evaluation programme for isotopic abundance measurements on low enriched UF6. In the ECN measurements the photopeak areas of the 185.72 keV gamma-rays of 23'5U have been determined with different peak evaluation methods. In spite of the rather large spread in un-certainty values between the different methods, no statistically significant differences in the 235U atomic abundance values have been obtained. The average measured 235U atomic abundance in uranium is 3.480% with a relative uncertainty of 0.2% (2 σ confidence level). The certified value is 3.5001% with a relative uncertainty of 0.03% (2 σ). An explanation for this discrepancy has not been found. (author). 8 refs.; 7 figs.; 20 tabs

  13. The determination of zirconium by atomic absorption spectrophotometry

    The interference of iron in the determination of zirconium by atomic absorption spectrophotometry was studied. Attempts were made to emininate this interference by complexing the iron with EDTA, ascorbic acid and hydrazine; also by the addition of ammonium fluoride to the solution. Some experiments were carried out in order to explain the results obtained

  14. Determination of long-lived radionuclides at ultratrace level using advanced mass spectrometric techniques

    Determination of long-lived radionuclides at sub-fg concentration level is a challenging task in analytical chemistry. Inductively coupled plasma mass spectrometry (ICP-MS) with its ability to provide the sensitive and fast multielemental analysis is one of the most suitable method for the measurements of long lived radionuclides in the trace and ultra trace concentration range. In present the Ph.D. study a variety of procedures have been developed permitting the sub fg ml-1 determination of long-lived radionuclides (e.g. U, Th, Pu) as well as 226Ra (T1/2 = 1600 y) and 90Sr (T1/2= 28.1 y) in different samples. In order to avoid isobaric interferences, to increase the sensitivity, precision and accuracy of the methods the application of different techniques: pre-concentration of the sample, off-line separation on the crown resin, measurements under cold plasma conditions, using microconcentric nebulizers (e.g DIHEN, DS-5) or the application of LA-ICP-MS for sample introduction have been studied. The limits of detection for different radionuclides was significantly improved in comparison to the ones reported in the literature, and, depending on the method applied, was varied from 10-15 to 10-18 g ml-1 concentration range. In addition to the analysis of long lived radionuclides, some other elements, that can present potential interest to the analyzed sample, were measured within the framework of the present study. Laser ablation inductively coupled plasma mass spectrometry (LAICP- MS) was used to produce images of element distribution in 20μm m thin sections of human brain tissue. The sample surface was scanned (raster area ∝80 mm2) with a focused laser beam (wavelength 213 nm, diameter of laser crater 50μm, and laser power density 3x109 W cm-2) in a cooled laser ablation chamber developed for these measurements. Cross sections of human brain samples - hippocampus as well as brain tissues infected and non-infected with Glioblastoma Multiforme (tumor cells) were

  15. Honeybee Venom Proteome Profile of Queens and Winter Bees as Determined by a Mass Spectrometric Approach

    Ellen L. Danneels

    2015-10-01

    Full Text Available Venoms of invertebrates contain an enormous diversity of proteins, peptides, and other classes of substances. Insect venoms are characterized by a large interspecific variation resulting in extended lists of venom compounds. The venom composition of several hymenopterans also shows different intraspecific variation. For instance, venom from different honeybee castes, more specifically queens and workers, shows quantitative and qualitative variation, while the environment, like seasonal changes, also proves to be an important factor. The present study aimed at an in-depth analysis of the intraspecific variation in the honeybee venom proteome. In summer workers, the recent list of venom proteins resulted from merging combinatorial peptide ligand library sample pretreatment and targeted tandem mass spectrometry realized with a Fourier transform ion cyclotron resonance mass spectrometer (FT-ICR MS/MS. Now, the same technique was used to determine the venom proteome of queens and winter bees, enabling us to compare it with that of summer bees. In total, 34 putative venom toxins were found, of which two were never described in honeybee venoms before. Venom from winter workers did not contain toxins that were not present in queens or summer workers, while winter worker venom lacked the allergen Api m 12, also known as vitellogenin. Venom from queen bees, on the other hand, was lacking six of the 34 venom toxins compared to worker bees, while it contained two new venom toxins, in particularly serine proteinase stubble and antithrombin-III. Although people are hardly stung by honeybees during winter or by queen bees, these newly identified toxins should be taken into account in the characterization of a putative allergic response against Apis mellifera stings.

  16. Honeybee venom proteome profile of queens and winter bees as determined by a mass spectrometric approach.

    Danneels, Ellen L; Van Vaerenbergh, Matthias; Debyser, Griet; Devreese, Bart; de Graaf, Dirk C

    2015-11-01

    Venoms of invertebrates contain an enormous diversity of proteins, peptides, and other classes of substances. Insect venoms are characterized by a large interspecific variation resulting in extended lists of venom compounds. The venom composition of several hymenopterans also shows different intraspecific variation. For instance, venom from different honeybee castes, more specifically queens and workers, shows quantitative and qualitative variation, while the environment, like seasonal changes, also proves to be an important factor. The present study aimed at an in-depth analysis of the intraspecific variation in the honeybee venom proteome. In summer workers, the recent list of venom proteins resulted from merging combinatorial peptide ligand library sample pretreatment and targeted tandem mass spectrometry realized with a Fourier transform ion cyclotron resonance mass spectrometer (FT-ICR MS/MS). Now, the same technique was used to determine the venom proteome of queens and winter bees, enabling us to compare it with that of summer bees. In total, 34 putative venom toxins were found, of which two were never described in honeybee venoms before. Venom from winter workers did not contain toxins that were not present in queens or summer workers, while winter worker venom lacked the allergen Api m 12, also known as vitellogenin. Venom from queen bees, on the other hand, was lacking six of the 34 venom toxins compared to worker bees, while it contained two new venom toxins, in particularly serine proteinase stubble and antithrombin-III. Although people are hardly stung by honeybees during winter or by queen bees, these newly identified toxins should be taken into account in the characterization of a putative allergic response against Apis mellifera stings. PMID:26529016

  17. Liquid Chromatography-Tandem Mass Spectrometric Assay for Determination of Stavudine in Human Plasma

    Fengdan Jin

    2014-01-01

    Full Text Available A LC-MS/MS method for determination of stavudine in human plasma was established and validated, and it was applied to the pharmaceutical formulations bioequivalence study. 0.5 mL plasma sample was extracted by liquid-liquid extraction. Stavudine was detected by a LC-MS/MS system. The pharmacokinetic parameters of stavudine in different formulations were calculated by noncompartment model statistics. The method was linear over the concentration ranges 5.00–1000 ng/mL in plasma. The intra- and interassay relative standard deviation (RSD was <10%. The average accuracies for the assay at three concentrations (5.00, 80.0, and 900 ng/mL were from 100.2% to 102.5%. Pharmacokinetic parameters of stavudine reference formulation were obtained as follows: Tmax was 0.6±0.2 h, Cmax was 480.7±150.9 g/L, t1/2 was 1.7±0.4 h, and AUC0-t was 872.8±227.8 g·h/L, and pharmacokinetic parameters of stavudine test formulation were obtained as follows: Tmax was 0.5±0.2 h, Cmax was 537.5±178.5 g/L, t1/2 was 1.7±0.3 h, and AUC0-t was (914.1±284.5 g·h/L. Calculated with AUC0-t, the bioavailability of two formulations was 105.0%.

  18. A highly sensitive method for the determination of mercury using vapor generation gold wire microextraction and electrothermal atomic absorption spectrometry

    The study introduces a new simple and highly sensitive method for headspace solid phase microextraction (HS-SPME) coupled with electrothermal atomic absorption spectrometric determination of mercury. In the proposed method, a gold wire, mounted in the headspace of a sample solution in a sealed bottle, is used for collection of mercury vapor generated by addition of sodium tetrahydroborate. The gold wire is then simply inserted in the sample introduction hole of a graphite furnace of an electrothermal atomic absorption spectrometry instrument. By applying an atomization temperature of 600 deg. C, mercury is rapidly desorbed from the wire and determined with high sensitivity. Factorial design and response surface analysis methods were used for optimization of the effect of five different variables in order to maximize the mercury signal. By using a 0.75 mm diameter gold wire, a sample volume of about 8 ml and an extraction time of 11 min, the sensitivity of mercury determination was enhanced up to 104 times in comparison to its ordinary ETAAS determination with direct injection of 10 μl sample solutions. A detection limit of 0.006 ng ml-1 and a precision better than 4.6% (relative standard deviation) were obtained. The method was successfully applied to the determination of mercury in industrial wastewaters and tuna fish samples

  19. A highly sensitive method for the determination of mercury using vapor generation gold wire microextraction and electrothermal atomic absorption spectrometry

    Hashemi, Payman [Department of Chemistry, Lorestan University, Khorram Abad (Iran, Islamic Republic of)], E-mail: payman_hashemi@yahoo.com; Rahimi, Akram [Department of Chemistry, Lorestan University, Khorram Abad (Iran, Islamic Republic of)

    2007-04-15

    The study introduces a new simple and highly sensitive method for headspace solid phase microextraction (HS-SPME) coupled with electrothermal atomic absorption spectrometric determination of mercury. In the proposed method, a gold wire, mounted in the headspace of a sample solution in a sealed bottle, is used for collection of mercury vapor generated by addition of sodium tetrahydroborate. The gold wire is then simply inserted in the sample introduction hole of a graphite furnace of an electrothermal atomic absorption spectrometry instrument. By applying an atomization temperature of 600 deg. C, mercury is rapidly desorbed from the wire and determined with high sensitivity. Factorial design and response surface analysis methods were used for optimization of the effect of five different variables in order to maximize the mercury signal. By using a 0.75 mm diameter gold wire, a sample volume of about 8 ml and an extraction time of 11 min, the sensitivity of mercury determination was enhanced up to 10{sup 4} times in comparison to its ordinary ETAAS determination with direct injection of 10 {mu}l sample solutions. A detection limit of 0.006 ng ml{sup -1} and a precision better than 4.6% (relative standard deviation) were obtained. The method was successfully applied to the determination of mercury in industrial wastewaters and tuna fish samples.

  20. Extraction-atomic-absorption determination of vanadium in salt liquors

    An extraction-atomic-absorption method to determine 0.1-0.8 mg/l vanadium in salt liquors containing 300 g/l NaCl is developed. To separate the basis extraction concentrating with hydroxyquinoline solution in chloroform with subsequent reextraction of vanadium at pH 9.4 is used. Results of vanadium determination in the salt liquer are as follows: vanadium determined x=0.22 mg/l, n=10, ssub(x)=0.045 mg/l, confidence range (at α=0.95)-(0.22+-0.03) mg/l, relative standard deviation is 0.20

  1. Instrumental modification intended to save time, and volumes of sample and reagent solutions, in the atomic fluorescence spectrometric determination of mercury.

    Pérez-Sirvent, Carmen; Martínez-Sánchez, María J; García-Lorenzo, Mariluz; López-García, Ignacio; Hernández-Córdoba, Manuel

    2007-05-01

    Use of small membrane pumps, instead of peristaltic pumps, to introduce sample and reagent solutions into the spectrometer has several advantages in atomic fluorescence spectrometric determination of mercury. This simple modification results in a substantial saving in the time required for the measurements and so 90% of reagent solution volumes and 95% of sample solution volumes are saved, with a consequent decrease in the volume of waste generated. The sampling frequency is almost tripled, with no deterioration in sensitivity, which is similar to that obtained by use of peristaltic pumps. The relative standard deviation for ten consecutive measurements of a 1 microg L-1 mercury solution was approximately 2%. PMID:17351707

  2. Determination of burnup balance for nuclear reactor fuel on the basis of γ-spectrometric determination of fission products

    Results are given of experimental investigations in one of the versions of the method for determination of the balance of nuclear fuel burnup process by means of the γ-spectrometry of fission products. In the version being considered a balance of the burnup process was determined on the base of 106Ru, 134Cs.Activity was measured by means of a γ-spectrometer with Ge counter. Investigations were done on the natural uranium metal fuel from the heavy-water moderated reactor of the first Czechoslovakian nuclear power plant A1 in Yaslovske Bohunice. Possibility was checked of determination of the fuel burnup depth as well as of the isotope ratio and content of plutonium. Results were compared with the control data which had been obtained on the base of the mass-spectrometry of U, Pu and Nd. The reasors for deviations were estimated in the cases when they were greater tan error in the control data

  3. Column system using diaion HP-2MG for determination of some metal ions by flame atomic absorption spectrometry

    Tuzen, Mustafa; Soylak, Mustafa

    2004-02-23

    A column solid-phase extraction method for the preconcentration and determination of cadmium(II), copper(II), cobalt(II), iron(III), lead(II), nickel(II) and zinc(II) dithizone chelates by atomic absorption spectrometry has been described. Diaion HP-2MG was used as adsorbent for column studies. The influences of the various analytical parameters including pH of the aqueous solutions, amounts of ligand and resin were investigated for the retentions of the analyte ions. The recovery values are ranged from 95 to 102%. The influences of alkaline and earth alkaline ions were also discussed. The preconcentration factor was 375, when the sample volume and final volume are 750 and 2 ml, respectively. The detection limits of the analyte ions (k=3, N=21) were varying 0.08 {mu}g/l for cadmium to 0.25 {mu}g/l for lead. The relative standard deviations of the determinations at the concentration range of 1.8x10{sup -4} to 4.5x10{sup -5} mmol for the investigated elements were found to be lower than 9%. The proposed solid-phase extraction procedure were applied to the flame atomic absorption spectrometric determinations of analyte ions in natural waters (sea, tap, river), microwave digested samples (milk, red wine and rice) and two different reference standard materials (SRM1515 apple leaves and NRCC-SLRS-4 riverine water)

  4. Atomic absorption determination of yttrium in matallurgic materials

    Atomic absorption spectroscopy techniques have been developed for Y determination in Mg-, Cr-, Ni-, Ti base alloys. The lower limit of Y determination is 0.01%. The Sr amount equals 0.07 and 0.035 for the 0.01-0.1 and 0.1-1.0 mas.% ranges of Y concentration, respectively. The presence in solution of 0.5-5 M HCl, H2SO4 and HNO3 as well as of up to 1 mg/ml Fe, Co, Zr, Ce, Sn, Zn, Cu, Mo doesn't affect the analysis results

  5. High-Performance Liquid Chromatographic-Tandem Mass Spectrometric Determination of Itraconazole in Human Plasma for Bioavailability and Bioequivalence Studies

    Choi, Young Wook; Nam, Dae Young; Kang, Kyoung Hoon; Ha, Kyung Wook; Han, In Hee; Chang, Byung Kon; Yoon, Mi Kyeong; Lee, Jae Hwi [Chung-Ang University, Seoul (Korea, Republic of)

    2006-02-15

    A highly sensitive high-performance liquid chromatographic-tandem mass spectrometric method (HPLC-MSMS) has been developed to quantify itraconazole in human plasma for the purpose of pharmacokinetic studies. Sample preparation was carried out by liquid-liquid extraction using loratadine as an internal standard. Chromatographic separation used a YMC C{sub 18} column, giving an extremely fast total run time of 3 min. The method was validated and used for the bioequivalence study of itraconazole tablets in healthy male volunteers (n = 31). The lower limit of detection proved to be 0.2 ng /mL for itraconazole.

  6. High-Performance Liquid Chromatographic-Tandem Mass Spectrometric Determination of Itraconazole in Human Plasma for Bioavailability and Bioequivalence Studies

    A highly sensitive high-performance liquid chromatographic-tandem mass spectrometric method (HPLC-MSMS) has been developed to quantify itraconazole in human plasma for the purpose of pharmacokinetic studies. Sample preparation was carried out by liquid-liquid extraction using loratadine as an internal standard. Chromatographic separation used a YMC C18 column, giving an extremely fast total run time of 3 min. The method was validated and used for the bioequivalence study of itraconazole tablets in healthy male volunteers (n = 31). The lower limit of detection proved to be 0.2 ng /mL for itraconazole

  7. Determination of metals in atmospheric particulates using atomic absorption spectrometry

    Nineteen trace metals in atmospheric samples have been determined by atomic absorption spectrometry, using a graphite furnace for most elements. Paper filters have been used to collect air samples. The sample preparation procedure involves the removal of organic matter and the conversion of the metals to soluble salts by ashing the filters in an oxygen plasma at 125 deg C for 6 h. and by subsequent dissolution in HN03HCl solution. The sensitivities achieved are in the range of 2,5.10-5 and 6,3.10-3 μg/m3, for an air volume of 2000 m3. (author)

  8. Validation of a method to the addition the multiple standard in the analysis of Pb in reservoir waters for atomic absorption spectrometric

    The evaluation of a method is presented for the analysis of Pb in reservoir waters for atomic spectrometric with direct aspiration. For the validation of the analytic method a level of concentration of 0.05 mg/L was evaluated. The precision of the method was of 9.97% and the bias was 0.6% 8 samples of surface waters they were collected and of bottom of the tributaries of the reservoir Scorpions and the stocking of the concentrations in the tributaries was from 0,052 +- 0.026 inferior mg/L to the established one in the Cuban norm of evaluation of the hydirc objects of fishing use

  9. Determination of the Mean HI Absorption of the Intergalactic Medium

    A. Aghaee; P. Petitjean; R. Srianand; C. S. Stalin; R. Guimarães

    2010-06-01

    In recent years, the Lyman- forest in quasar spectra has been used, together with -body simulations, to determine the underlying matter distribution in the intergalactic medium (IGM). One of the key parameters to be known in order to compare observations and numerical simulations is the mean HI absorption in the IGM. To derive the latter, one has first to fit the quasar continuum.We have observed 20 high redshift and highly luminous QSOs (V ≤ 17.5 and 2.40 ≤ em ≤ 3.91) at intermediate spectral resolution, with either EMMI (ESO Multi-Mode Instrument) on the ESO-NTT telescope or CARELEC at the OHP (Observatoire de Haute-Provence), and applied different methods of determining the QSO continuum to this QSO sample. We have measured the amount of absorption, known as the flux decrement, , in the Lyman- forest for these different methods and compared the results. In addition, we have compared values measured along the same lines of sight observed at high and intermediate spectral resolutions.We discuss the systematics resulting from the use of automatic continuum fitting methods.

  10. Ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction combined with graphite furnace atomic absorption spectrometric for selenium speciation in foods and beverages.

    Tuzen, Mustafa; Pekiner, Ozlem Zeynep

    2015-12-01

    A rapid and environmentally friendly ultrasound assisted ionic liquid dispersive liquid liquid microextraction (USA-IL-DLLME) was developed for the speciation of inorganic selenium in beverages and total selenium in food samples by using graphite furnace atomic absorption spectrometry. Some analytical parameters including pH, amount of complexing agent, extraction time, volume of ionic liquid, sample volume, etc. were optimized. Matrix effects were also investigated. Enhancement factor (EF) and limit of detection (LOD) for Se(IV) were found to be 150 and 12 ng L(-1), respectively. The relative standard deviation (RSD) was found 4.2%. The accuracy of the method was confirmed with analysis of LGC 6010 Hard drinking water and NIST SRM 1573a Tomato leaves standard reference materials. Optimized method was applied to ice tea, soda and mineral water for the speciation of Se(IV) and Se(VI) and some food samples including beer, cow's milk, red wine, mixed fruit juice, date, apple, orange, grapefruit, egg and honey for the determination of total selenium. PMID:26041239

  11. Generation of volatile copper species after in situ ionic liquid formation dispersive liquid-liquid microextraction prior to atomic absorption spectrometric detection.

    Stanisz, Ewa; Zgoła-Grześkowiak, Agnieszka; Matusiewicz, Henryk

    2014-11-01

    The new procedure using in situ synthesis of ionic liquid extractant for dispersive liquid-liquid microextraction (in situ IL DLLME) combined with generation of volatile species prior to electrothermal atomic absorption spectrometry (ET AAS) for the determination of copper in soil samples was developed. Analytical signals were obtained without the back-extraction of copper from the IL phase prior to its determination. Under optimal conditions, the extraction in 10 mL of sample solution employing 8 μL of 1-hexyl-3-methylimidazolium bis[(trifluoromethyl)sulfonyl]imide (HmimNTf2) (as the extraction solvent) was conducted. The ionic liquid served as two-task reagent: the efficient extractant and enhancement substance for generation step. The chemical generation of volatile species was performed by reduction of acidified copper solution (HCl 0.8 mol L(-1)) with NaBH4 (1.5%). Some essential parameters of the chemical generation such as NaBH4 and HCl concentrations, the kind and concentration of ionic liquid, carrier gas (Ar) flow rate, reaction and trapping time as well as pyrolysis and atomization temperatures were studied. For photogeneration the effect of the parameters such as the kind and concentration of low molecular weight organic acids and ionic liquid, carrier gas (Ar) flow rate, UV irradiation and ultrasonication time on the analytical signals were studied. The detection limit was found as 1.8 ng mL(-1) and the relative standard deviation (RSD) for seven replicate measurements of 100 µg mL(-1) in sample solution was 7%. The accuracy of the proposed method was evaluated by analysis of the certified reference materials. The measured copper contents in the reference materials were in satisfactory agreement with the certified values. The method was successfully applied to analysis of the soil and sediment samples. PMID:25127592

  12. Determination of molybdenum in flotation concentrates by atomic absorption spectrophotometry

    Molybdenum was determined by atomic absorption spectrophotometry in 0.05 N ammoniacal solution after the decomposition of the concentrate with aqua regia. Negros ore from Philippines was used as a flotation feed, which contained chalcopyrites and calcium-magnesium minerals. Among the metals tested copper, iron and the alkaline earths interfered. Less than 50 ppm of copper yielded lower results for molybdenum. Higher results came out with more than 50 ppm of copper. In the presence of iron and citric acid (0.4 g/100 ml) which is a suppressor for hydroxide formation, a lower estimation resulted for molybdenum. Calcium interfered, lower results by 2 and >10% being obtained with respective 2.5 and 20 ppm of calcium. More than 20 ppm of magnesium behaved similarly. Sodium sulfate (0.5 g/100 ml) served as the suppressor for copper, iron and citric acid; 100 ppm each of copper and iron did not interfere in this way. Interferences due to calcium and magnesium (less than 60 ppm) was able to be masked by the addition of sodium silicate (200 ppm as silica). The analysis of flotation products and synthetic samples consisting of molybdenite, chalcopyrite, calcium chloride and magnesium sulfate revealed that the atomic absorption method can be applied to the analysis of the concentrates for molybdenum with an error of about 2%. (auth.)

  13. Determining photon energy absorption parameters for different soil samples.

    Kucuk, Nil; Tumsavas, Zeynal; Cakir, Merve

    2013-05-01

    The mass attenuation coefficients (μs) for five different soil samples were measured at 661.6, 1173.2 and 1332.5 keV photon energies. The soil samples were separately irradiated with (137)Cs and (60)Co (370 kBq) radioactive point gamma sources. The measurements were made by performing transmission experiments with a 2″ × 2″ NaI(Tl) scintillation detector, which had an energy resolution of 7% at 0.662 MeV for the gamma-rays from the decay of (137)Cs. The effective atomic numbers (Zeff) and the effective electron densities (Neff) were determined experimentally and theoretically using the obtained μs values for the soil samples. Furthermore, the Zeff and Neff values of the soil samples were computed for the total photon interaction cross-sections using theoretical data over a wide energy region ranging from 1 keV to 15 MeV. The experimental values of the soils were found to be in good agreement with the theoretical values. Sandy loam and sandy clay loam soils demonstrated poor photon energy absorption characteristics. However, clay loam and clay soils had good photon energy absorption characteristics. PMID:23179375

  14. The fuel burn-up determination by combined passive neutron and gamma - spectrometric ND - measurements. Final report for the period 1 July 1980 - 30 April 1988

    The non-destructive gamma-spectrometric method (HRGS) and the passive neutron technique (PNT) were applied to the determination of WWER 440 reactor spent fuel assemblies burn-up for safeguard purposes. Rapid codes FISPR-2 and BUNECO were compiled on HP-85 and OLIVETTI M24 computers for the IAEA inspectors. An improved equipment was constructed and tested for the fixation of the ''fork detector''. Measurements were carried-out at 1st unit of NPP Bohunice. The correlation between burn-up and fission product ratio 134Cs/137Cs or neutron count rate were analysed. Correlations between concentrations 235U, Pu and burn-up were analysed as well. A simplified procedure for assemblies burn-up check by PNT was proposed for the inspectors. Refs, figs and tabs

  15. Determination of plutonium isotopes (238Pu, 239Pu, 240Pu, 241Pu) in environmental samples using radiochemical separation combined with radiometric and mass spectrometric measurements

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

    2014-01-01

    This paper reports an analytical method for the determination of plutonium isotopes (238Pu, 239Pu, 240Pu, 241Pu) in environmental samples using anion exchange chromatography in combination with extraction chromatography for chemical separation of Pu. Both radiometric methods (liquid scintillation...... counting and alpha spectrometry) and inductively coupled plasma mass spectrometry (ICP-MS) were applied for the measurement of plutonium isotopes. The decontamination factors for uranium were significantly improved up to 7.5×105 for 20 g soil compared to the level reported in the literature......, this is critical for the measurement of plutonium isotopes using mass spectrometric technique. Although the chemical yield of Pu in the entire procedure is about 55%, the analytical results of IAEA soil 6 and IAEA-367 in this work are in a good agreement with the values reported in the literature or reference...

  16. Precise determination of magnesium and lutetium in input accountability tank solutions of nuclear reprocessing plants by the mass spectrometric stable isotope dilution technique

    This paper describes the procedures for the determination of Mg and Lu concentrations in input solutions of nuclear fuel dissolved in reprocessing plants. The main aim of this work is to supply an independent method for measuring the volume of input accountability tanks. The methods used include suitable radiochemical separations and isotope dilution mass spectrometric measurements. Chemical separations from highly radioactive solutions have been tested in order to obtain pure and ''cold'' samples of Mg and Lu to be measured by Mass Spectrometry. Different ionisation techniques have been used in obtaining precise isotopic ratios. Results are presented and compared with historical data. A critical evaluation of methods, results and apparatus is given. 17 refs

  17. Mass spectrometric immunoassay

    Nelson, Randall W; Williams, Peter; Krone, Jennifer Reeve

    2007-12-04

    Rapid mass spectrometric immunoassay methods for detecting and/or quantifying antibody and antigen analytes utilizing affinity capture to isolate the analytes and internal reference species (for quantification) followed by mass spectrometric analysis of the isolated analyte/internal reference species. Quantification is obtained by normalizing and calibrating obtained mass spectrum against the mass spectrum obtained for an antibody/antigen of known concentration.

  18. Micro-determination of ytterbium with electrothermal atomic absorption spectrometry

    This communication reports the use of a pyrolytic graphite coated tube, lined with tantalum-tungsten, and a local made atomic absorption spectrometer (Model WFD-Y3) for the determination of small amount Yb in pure Y2O3 and mixed rare earth oxides. It is found that the method proposed is sensitive, reproducible and simple in manipulation. Even as low as 0.2 μg Yb in one gram sample (n x 10-7) can be determined directly without pre-concentration. It is found experimentally that the optimum condition for drying is at 150 deg C. for 20 sec, ashing at 1000 deg C. for 20 sec and atomization at 2770 deg C. for 12 sec. Within the range 1.0-18ng Yb/ml the calibration curve of Yb is linear. Before injecting into the tube, the acidity of the sample solution should be ajusted to 0.1 to 2 M with nitric or hydrochloric acid. For 5ng Yb/ml, Al(III), Ca(II) and La(III) interference, when their amount present is 50 μg/ml or more. On the other hand, Cu(II), Fe(III), Mg(II), K(I) and Y(III) in amount up to 1 mg/ml do not interfere

  19. Evaluation of microwave digestion and solvent extraction for the determination of trace amounts of selenium in feeds and plant and animal tissues by electrothermal atomic absorption spectrometry.

    Hocquellet, P; Candillier, M P

    1991-05-01

    A sensitive method for the accurate determination of Se in agricultural products at sub-ppm levels is described. The proposed procedure involves the wet oxidation of samples by using a mixture of nitric, sulphuric and perchloric acids, co-extraction of Se and added Pd with diethylammonium N,N-diethyldithiocarbamate in chloroform, and electrothermal atomic absorption spectrometric determination of Se in the organic extract. Atomization and extraction conditions are discussed. Special attention is given to the wet oxidation step, and its advantages in speed and simplicity over conventional heating have been evaluated using an automated microwave digestion system. The results reported, obtained from several reference materials, confirm the accuracy of the method with which a detection limit of 0.002 micrograms g-1 of Se can be achieved. PMID:1877754

  20. Atomic absorption spectroscopic, conductometric and colorimetric methods for determination of fluoroquinolone antibiotics using ammonium reineckate ion-pair complex formation

    Ragab, Gamal H.; Amin, Alaa S.

    2004-03-01

    Three accurate, rapid and simple atomic absorption spectrometric, conductometric and colorimetric methods were developed for the determination of norfloxacin (NRF), ciprofloxacin (CIP), ofloxacin (OFL) and enrofloxacin (ENF). The proposed methods depend upon the reaction of ammonium reineckate with the studied drugs to form stable precipitate of ion-pair complexes, which was dissolved in acetone. The pink coloured complexes were determined either by AAS or colorimetrically at λmax 525 nm directly using the dissolved complex. Using conductometric titration, the studied drugs could be evaluated in 50% (v/v) acetone in the range 5.0-65, 4.0-48, 5.0-56 and 6.0-72 μg ml -1 of NRF, CPF, OFL and ENF, respectively. The optimizations of various experimental conditions were described. The results obtained showed good recoveries of 99.15±1.15, 99.30±1.40, 99.60±1.50, and 99.00±1.25% with relative standard deviations of 0.81, 1.06, 0.97, and 0.69% for NRF, CPF, OFL, and ENF, respectively. Applications of the proposed methods to representative pharmaceutical formulations are successfully presented.

  1. Simultaneous Preconcentration of Copper, Nickel, Cobalt and Lead Ions Prior to Their Flame Atomic Absorption Spectrometric Determination

    A sensitive and simple method for the simultaneous preconcentration of nutritionally important minerals in real samples has been reported. The method is based on the adsorption of Cu2+, Ni2+, Co2+ and Pb2+ on 4-propyl-2-thiouracil (PUT) loaded on activated carbon. The metals on the complexes are eluted using 5 mL 3 M HNO3 in acetone. The influences of the analytical parameters including pH and sample volume were investigated. The effects of matrix ions on the retentions of the analytes were also examined. The recoveries of analytes were generally higher than 95 %. The detection limits for Cu2+, Ni2+, Co2+ and Pb2+ were 1.6, 1.3, 1.2, 2.3 ng ml-1, respectively. The method has been successfully applied for these metals content evaluation in some real samples including natural water samples

  2. Uranium determination in zirconium

    The method used for the spectrometric uranium determination with 2-(2-thiolase)-5-diethylaminophenol was modified for its application in the zirconium samples analysis with an uranium content of the 0.1% order. The samples, previously dissolved in nitric acid, were submitted to a separative stage of liquid-liquid extraction, with a trioctylphosphine (TOPO) oxide diluted in cyclohexane. A sodium fluoride aqueous solution was necessary to be aggregated in the spectrometric determination so as to complex the zirconium vestiges, which could be present, originated by the Zr/U high relation of the initial sample. Under the established working conditions, different spectrometric assays, dyes absorption spectra and its uranium complex, complex stability, PH influence determination of the dyes-uranium relation, calculation of the complex's apparent formation constant and its molar absorption, were performed. (Author)

  3. Spectrometric techniques 4

    Vanasse, George A

    2013-01-01

    Spectrometric Techniques, Volume IV discusses three widely diversified areas of spectrometric techniques. The book focuses on three spectrometric methods. Chapter 1 discusses the phenomenology and applications of Coherent Anti-Stokes Raman Spectroscopy (CARS), the most commonly used optical technique that exploit the Raman effect. The second chapter is concerned with diffraction gratings and mountings for the Vacuum Ultraviolet Spectral Region. Chapter 3 accounts the uses of mass spectrometry, detectors, types of spectrometers, and ion sources. Physicists and chemists will find the book a go

  4. Luminescence and optical absorption determination in porous silicon

    Nogal, U.; Calderon, A.; Marin, E.; Rojas T, J. B.; Juarez, A. G., E-mail: u_nogal@hotmail.com [IPN, Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada, Calz. Legaria No. 694, Col. Irrigacion, 11500 Mexico D. F. (Mexico)

    2012-10-15

    We applied the photoacoustic spectroscopy technique in order to obtain the optical absorption spectrum in porous silicon samples prepared by electrochemical anodic etching on n-type, phosphorous doped, (100)-oriented crystal-line silicon wafer with thickness of 300 {mu}m and 1-5 {omega}cm resistivity. The porous layers were prepared with etching times of 13, 20, 30, 40 and 60 minutes. Also, we realized a comparison among the optical absorption spectrum with the photoluminescence and photo reflectance ones, both obtained at room temperature. Our results show that the absorption spectrum of the samples of porous silicon depends notably of the etching time an it consist of two distinguishable absorption bands, one in the Vis region and the other one in the UV region. (Author)

  5. Optimization of spectrometric gamma-gamma probe configuration using very low radioactivity sources for lead and zinc grade determination in borehole logging

    The suitability of spectrometric backscattered gamma - gamma well logging measurements to predict lead and zinc metal equivalent content is demonstrated. A centralised tool employing a gamma - ray source of very low radioactivity (1.8 MBq) is used. The logging tools is tested using 133 Ba and 137 Cs sources with a 37 mm (diameter) x 750 mm NaI (TI) scintillation detector. Five source - to - detector configurations were analysed for 18 geophysical models, 13 of which had a borehole diameter of 130 mm and the other 5 had a borehole diameter of 160 mm. Regression analysis on the laboratory logging data for each configuration in order to establish the calibration equation for a lead (Pb) and zinc metal equivalent (ZME) prediction is carried out. The optimum configuration for the logging probe using a 133 Ba source was determined to be 52 mm source - to - detector spacing. This configuration gives the best results for both Pb and ZME grade. The r.m.s deviations for Pb and ZME were 0.33 and 2.3%, respectively. The optimum configuration for the logging probe using a 137 Cs source was determined to be 64 mm source - to - detector spacing. This configuration gives the best results for both Pb and ZME grade. The r.m.s deviations for Pb and ZME were 0.36 and 2.2%, respectively. (author)

  6. Optimisation of spectrometric gamma-gamma probe configuration using very low radioactivity sources for lead and zinc grade determination in borehole logging

    The suitability of spectrometric backscattered gamma-gamma well logging measurements to predict lead and zinc metal equivalent content is demonstrated. A centralised tool employing a gamma-ray source of very low radioactivity (1.8 MBq) is used. The logging tool is tested using 133Ba and 137Cs sources with a 37 mm (diameter)x75 mm NaI (TI) scintillation detector. Five source-to-detector configurations were analysed for 18 geophysical models, 13 of which had a borehole diameter of 130 mm and the other 5 had a borehole diameter of 160 mm. Regression analysis on the laboratory logging data for each configuration in order to establish the calibration equation for a lead (Pb) and zinc metal equivalent (ZME) prediction is carried out. The optimum configuration for the logging probe using a 133Ba source was determined to be 52 mm source-to-detector spacing. This configuration gives the best results for both Pb and ZME grade. The rms deviations for Pb and ZME were 0.33 and 2.3%, respectively. The optimum configuration for the logging probe using a 137Cs source was determined to be 64 mm source-to-detector spacing. This configuration gives the best results for both Pb and ZME grade. The rms deviations for Pb and ZME were 0. 3 6 and 2.2 %, respectively

  7. Evaluation of mass spectrometric data using principal component analysis for determination of the effects of organic lakes on protein binder identification.

    Hrdlickova Kuckova, Stepanka; Rambouskova, Gabriela; Hynek, Radovan; Cejnar, Pavel; Oltrogge, Doris; Fuchs, Robert

    2015-11-01

    Matrix-assisted laser desorption/ionisation-time of flight (MALDI-TOF) mass spectrometry is commonly used for the identification of proteinaceous binders and their mixtures in artworks. The determination of protein binders is based on a comparison between the m/z values of tryptic peptides in the unknown sample and a reference one (egg, casein, animal glues etc.), but this method has greater potential to study changes due to ageing and the influence of organic/inorganic components on protein identification. However, it is necessary to then carry out statistical evaluation on the obtained data. Before now, it has been complicated to routinely convert the mass spectrometric data into a statistical programme, to extract and match the appropriate peaks. Only several 'homemade' computer programmes without user-friendly interfaces are available for these purposes. In this paper, we would like to present our completely new, publically available, non-commercial software, ms-alone and multiMS-toolbox, for principal component analyses of MALDI-TOF MS data for R software, and their application to the study of the influence of heterogeneous matrices (organic lakes) for protein identification. Using this new software, we determined the main factors that influence the protein analyses of artificially aged model mixtures of organic lakes and fish glue, prepared according to historical recipes that were used for book illumination, using MALDI-TOF peptide mass mapping. PMID:26505772

  8. Recent developments in automated determinations of trace level concentrations of elements and on-line fractionations schemes exploiting the micro-sequential injection - lab-on-valve approach

    Hansen, Elo Harald; Miró, Manuel; Long, Xiangbao;

    2006-01-01

    The determination of trace level concentrations of elements, such as metal species, in complex matrices by atomic absorption or emission spectrometric methods often require appropriate pretreatments comprising separation of the analyte from interfering constituents and analyte preconcentration...

  9. Liquid chromatography-tandem mass spectrometric methods for the determination of spinosad, thiacloprid and pyridalyl in spring onions and estimation of their pre-harvest interval values.

    Dasenaki, Marilena E; Bletsou, Anna A; Hanafi, Ahmad H; Thomaidis, Nikolaos S

    2016-12-15

    Two liquid chromatography-tandem mass spectrometric methods were developed and validated to determine spinosyn A and D, thiacloprid and pyridalyl in spring onions cultivated under Egyptian field conditions. The degradation rates, the pre-harvest interval (PHI) values and the half-life values of the three pesticides were estimated. QuEChERS was used for sample preparation and the separation was performed on an X-Bridge C18 column with ACN-formic acid 0.1% as the mobile phase. Linear range, method detection limits (MDLs), precision, recovery and matrix effects were estimated. The multi-residue MDLs ranged from 0.02μg/kg (spinosyn A & D) to 0.05μg/kg for pyridalyl. All the investigated pesticides showed high degradation rates. For spinosad the half-life value was 1.2days, for thiacloprid it reached 2.2days and for pyridalyl 4.4days. Furthermore, the calculated PHI values, according to the maximum residue levels set by the EU, were 0days for spinosad, 9.8days for thiacloprid and 39.4days for pyridalyl. PMID:27451196

  10. Optimisation of spectrometric gamma-gamma probe configuration using very low radioactivity sources for lead and zinc grade determination in borehole logging

    Asfahani, J

    1999-01-01

    The suitability of spectrometric backscattered gamma-gamma well logging measurements to predict lead and zinc metal equivalent content is demonstrated. A centralised tool employing a gamma-ray source of very low radioactivity (1.8 MBq) is used. The logging tool is tested using sup 1 sup 3 sup 3 Ba and sup 1 sup 3 sup 7 Cs sources with a 37 mm (diameter)x75 mm NaI (TI) scintillation detector. Five source-to-detector configurations were analysed for 18 geophysical models, 13 of which had a borehole diameter of 130 mm and the other 5 had a borehole diameter of 160 mm. Regression analysis on the laboratory logging data for each configuration in order to establish the calibration equation for a lead (Pb) and zinc metal equivalent (ZME) prediction is carried out. The optimum configuration for the logging probe using a sup 1 sup 3 sup 3 Ba source was determined to be 52 mm source-to-detector spacing. This configuration gives the best results for both Pb and ZME grade. The rms deviations for Pb and ZME were 0.33 and ...

  11. [Determination of nine estrogenic steroids in milk using matrix solid phase dispersion-ultra performance liquid chromatography with mass spectrometric detector].

    Liu, Hongcheng; Li, Ning; Lin, Tao; Shao, Jinliang; Li, Qiwan

    2015-11-01

    An analytical method for the multiresidue determination of nine estrogenic steroids in milk was developed by modified matrix solid phase dispersion (MSPD) purification and ultra performance liquid chromatography (UPLC) with mass spectrometric detector (MSD). The sensitivity and accuracy of MSD were better than that of ultraviolet detector. In comparison with traditional mass spectrometry, the merits of MSD were simpler in operation and shorter in starting time (5 min). The results showed that the limits of detection of the compounds with nucleophilic substitution were high in positive ion mode of MSD and were easily affected by environmental conditions. The matrix effects of milk samples reduced from 84%-160% to 80%-121% after MSPD purification. The intraday precision and interday precision of the nine estrogenic steroids were 0.87%-1.78% and 1.82%-3.79%, respectively. The average recoveries were 68.7%-94.7%, and the relative standard deviations (RSDs) were less than 10%. The limits of detection (LODs) were 0.5-10 μg/kg. The limits of quantification (LOQ) were 2-20 μg/kg. PMID:26939362

  12. A liquid chromatography-atmospheric pressure photoionization tandem mass spectrometric method for the determination of organosulfur compounds in petroleum asphalt cements.

    da Silveira, Géssica Domingos; Faccin, Henrique; Claussen, Luis; Goularte, Rayane Bueno; Do Nascimento, Paulo C; Bohrer, Denise; Cravo, Margareth; Leite, Leni F M; de Carvalho, Leandro Machado

    2016-07-29

    We present a sensitive liquid chromatography-atmospheric pressure photoionization tandem mass spectrometric (UHPLC-APPI-MS/MS) method for the determination of selected organosulfur compounds in Brazilian asphalt cements. It was possible to detect 14 organosulfur compounds of different classes where sulfoxides and sulfones presented higher sensibility in ionization than thiophenes and aromatic sulfides. A dopant-assisted APPI method was also tested, however, when chromatographic flow rate was optimized a decrease in signal was observed for all compounds. PAHs were tested and ruled out as possible interfering compounds and the matrix effect of asphalt cements was within an acceptable range for the quantification of organosulfur compounds. The proposed method was found to have satisfactory linearity and accuracy with recoveries between 83.85 and 110.28% for thianaphthene and 3-methylbenzothiophene, respectively. Therefore, the method allowed the characterization of organosulfur compounds in Brazilian asphalt cements and demonstrated changes in the amount quantified in asphaltenic and maltenic fractions after the RTFOT+SUNTEST aging process. PMID:27342135

  13. Qualification and application of a liquid chromatography-quadrupole time-of-flight mass spectrometric method for the determination of trastuzumab in rat plasma.

    Park, Min-Ho; Lee, Min-Woo; Shin, Young G

    2016-04-01

    An liquid chromatography-quadrupole time-of-flight (QqTOF) mass spectrometric method was developed for the determination of humanized or human monoclonal antibodies in rat plasma at the early drug discovery stage. Trastuzumab was used as a model monoclonal antibody. The method consisted of immunoprecipitation followed by tryptic digestion for sample preparation and LC-TOF-MS/MS analysis of specific signature peptides in the positive ion mode using electrospray ionization for analysis. A stable isotope-labeled signature peptide was also used as internal standard. A quadratic regression (weighted 1/concentration(2) ), with an equation y = ax(2)  + bx + c, was used to fit calibration curves over the concentration range of 0.500-100 µg/mL for trastuzumab. Samples from a pharmacokinetic study in rat were analyzed by this qualified LC-TOF-MS/MS method and concentrations were compared with those generated by enzyme linked immunosorbent assays method. The LC-TOF-MS/MS method was accurate and precise, with quantitative results comparable with those of ELISA. The qualification run met the acceptance criteria of ±25% accuracy and precision values for quality control samples. Within-run accuracy ranged from 1.53 to 9.20% with precision values ≤10.29%. This LC-TOF-MS/MS method approach could be used as a complementary method for humanized or human monoclonal antibodies at the early drug discovery stage. Copyright © 2015 John Wiley & Sons, Ltd. PMID:26317190

  14. Influence of particle size of wear metal on the spectrometric oil analysis programme (SOAP), demonstrated by the determination of iron by AAS

    The possibility that there might be a relation between particle size of wear metal and spectrometric determination, (e.g. of the iron content in used lubricating oils) has been examined. In this connection it had to be clarified from which particle size of the iron wear the Fe content determined by direct AAS (solution of the oil sample) is in agreement with the true value in the used oil. The determination of the absolute iron content was performed by a colorimetric method preceded by an incineration of the used oil. Contrary to other publications, in which work is based on spherical iron particles as a simulated wear, the test described here relates to true wear particles. To obtain the total iron wear from a gear oil it was filtered off from the used oil and afterwards separated into defined particle size ranges by a procedure specially developed for this purpose. The different groups of scaly particles, which were collected in this way, were then mixed homogeneously into fresh luboil samples according to their sizes. The determination of the iron content from these newly mixed luboil samples was carried out 1. by direct AAS, 2. by AAS after incineration of the oil samples and 3. by a colorimetric method (to obtain the absolute value of the iron content). The results showed a recovery of the iron of only 50% if the wear particles were bigger than about 2 μm. That means that the true value of the iron content in a used lubricating oil is found by direct AAS only if the particle size is <=1 μm. (orig.)

  15. Determining the Fraction of Intrinsic CIV Absorption in Quasi-Stellar Object Absorption Line Systems

    Richards, G T; Yanny, B; Kollgaard, R I; Laurent-Mühleisen, S A; Vanden Berk, Daniel E; Richards, Gordon T.; York, Donald G.; Yanny, Brian; Kollgaard, Ronald I.; Berk, Daniel E. Vanden

    1999-01-01

    We present the results of a study of QSO Absorption Line Systems (QSOALSs) with respect to intrinsic QSO properties using an updated catalog of data in the literature. We have searched the literature for 6 and 20 cm radio flux densities and have studied 20 cm maps from the FIRST VLA Survey in order to compare the absorption properties with radio luminosity, radio spectral index and radio morphology. This work focuses particularly on the nature of CIV QSOALSs and their distribution in velocity space in light of intrinsic QSO properties. We find that the distribution of narrow, CIV absorption systems with relative velocities exceeding 5000 km/s is dependent not only on the optical luminosity of the QSOs, but also on the radio luminosity, the radio spectral index and the radio morphology of the QSOs. These observations are apparently inconsistent with the hypothesis that these systems are entirely due to intervening galaxies and it would seem that the contamination of the intervening systems (from 5000 to 75000 ...

  16. Determination of trace elements in dolomite and gypsum by atomic absorption spectrometry: overcoming the matrix interference by flotation separation

    Stafilov, Trajče; Zendelovska, Dragica; Pavlovska, Gorica; Čundeva, Katarina

    2002-05-01

    The interferences of Ca and Mg as matrix elements in dolomite and gypsum on Ag, Cd, Cr, Mn, Tl and Zn absorbances during their electrothermal atomic absorption spectrometric (ETAAS) determination are investigated. The results reveal that Ca and Mg do not interfere on Zn and Mn, tend to decrease absorbances of Ag, Cd and Cr, while Tl suffers the most significant influence. A flotation separation method is proposed to eliminate matrix interferences. Hydrated iron(III) oxide, Fe 2O 3· xH 2O, and iron(III) hexamethylenedithiocarbamate, Fe(HMDTC) 3, are applied as flotation collectors. The influence of hydrophobic dithiocarbamate anion, HMDTC, on flotation recoveries of each analyte is studied. The most suitable concentrations of dolomite and gypsum solutions for flotation are determined. To avoid flotation suppression due to the reaction of Ca 2+ and Mg 2+ with surfactant ions, a fit foaming agent was selected. The elements present in dolomite and gypsum as traces have been analyzed by ETAAS. Their ETAAS limits of detection following flotation are found to be 0.021 μg·g -1 for Ag, 0.019 μg·g -1 for Cd, 0.014 μg·g -1 for Cr and 0.11 μg·g -1 for Tl. The determination of Mn and Zn can be performed by flame AAS (FAAS). The limit of detection for Mn is 1.5 μg·g -1, while for Zn 0.8 μg·g -1.

  17. A high-performance liquid chromatographic-atmospheric pressure chemical ionization-tandem mass spectrometric method for determination of risperidone and 9-hydroxyrisperidone in human plasma.

    Moody, David E; Laycock, John D; Huang, Wei; Foltz, Rodger L

    2004-09-01

    Risperidone, a benzisoxazole derivative, is an antipsychotic agent used for the treatment of schizophrenia. We developed a liquid chromatographic-atmospheric pressure chemical ionization-tandem mass spectrometric (LC-APCI-MS-MS) method with improved sensitivity, selectivity, and dynamic range for determination of risperidone and 9-hydroxyrisperidone in human plasma. A structural analogue of risperidone, RO68808 (5 ng/mL), is added as the internal standard to 1 mL of human plasma. Plasma is made basic, extracted with pentane/methylene chloride (3:1), the organic phase evaporated to dryness, and the residue is reconstituted in water with 0.1% formic acid/acetonitrile (20:1). For LC-MS-MS analysis, a Metachem Inertsel HPLC column (2.1 x 150 mm, 5-microm particle size) is connected to a Finnigan TSQ7000 tandem MS via the Finnigan API interface. Both electrospray (ESI) and APCI produced predominantly MH(+) ions for the two analytes and the internal standard. Ions detected by selected reaction monitoring correspond to the following transitions: m/z 411 to 191 for risperidone, m/z 427 to 207 for 9-hydroxyrisperidone, and m/z 421 to 201 for the internal standard. APCI provided a larger dynamic range (0.1 to 25 ng/mL) and better precision and accuracy than ESI. Intrarun accuracy and precision determined at 0.1, 0.25, 2.5, and 15 ng/mL were within 12% of target with %CVs not exceeding 10.9%. Interrun accuracy and precision determined at the same concentrations were within 9.6% of target with %CVs not exceeding 6.7%. Analytes were stable in plasma after 24 h at room temperature, 2 freeze-thaw cycles, and 490 days at -20 degrees C. PMID:15516302

  18. Mechanistic Determinants of Biotherapeutics Absorption Following SC Administration

    Richter, Wolfgang F; Bhansali, Suraj G.; Morris, Marilyn E.

    2012-01-01

    The subcutaneous (SC) route is of growing interest for the administration of biotherapeutics. Key products on the biotherapeutic market such as insulins, but also several immunoglobulins or Fc-fusion proteins, are administered SC. Despite the importance of the SC route, the available knowledge about the processes involved in the SC absorption of biotherapeutics is limited. This review summarizes available information on the physiology of the SC tissue and on the pharmacokinetic processes afte...

  19. Pathlength Determination for Gas in Scattering Media Absorption Spectroscopy

    Liang Mei

    2014-02-01

    Full Text Available Gas in scattering media absorption spectroscopy (GASMAS has been extensively studied and applied during recent years in, e.g., food packaging, human sinus monitoring, gas diffusion studies, and pharmaceutical tablet characterization. The focus has been on the evaluation of the gas absorption pathlength in porous media, which a priori is unknown due to heavy light scattering. In this paper, three different approaches are summarized. One possibility is to simultaneously monitor another gas with known concentration (e.g., water vapor, the pathlength of which can then be obtained and used for the target gas (e.g., oxygen to retrieve its concentration. The second approach is to measure the mean optical pathlength or physical pathlength with other methods, including time-of-flight spectroscopy, frequency-modulated light scattering interferometry and the frequency domain photon migration method. By utilizing these methods, an average concentration can be obtained and the porosities of the material are studied. The last method retrieves the gas concentration without knowing its pathlength by analyzing the gas absorption line shape, which depends upon the concentration of buffer gases due to intermolecular collisions. The pathlength enhancement effect due to multiple scattering enables also the use of porous media as multipass gas cells for trace gas monitoring. All these efforts open up a multitude of different applications for the GASMAS technique.

  20. New approaches for the mass spectrometric determination of trace concentrations and congener group patterns of chlorinated paraffins in biota

    Reth, Margot

    2006-01-01

    The determination of chlorinated paraffins (CPs) in the environment is important, since CPs are persistent, bioaccumulative and toxic. However, the analysis of these complex mixtures containing thousands of isomers is also a demanding task. CP analysis and especially the quantification of CPs are far from being well established. In this work, new methodologies were developed for the determination of CPs in biota by low-resolution mass spectrometry (LRMS). The use of expensiv...

  1. Determination of ultra trace amounts of bismuth in biological and water samples by electrothermal atomic absorption spectrometry (ET-AAS) after cloud point extraction

    Shemirani, Farzaneh; Baghdadi, Majid; Ramezani, Majid; Jamali, Mohammad Reza

    2005-04-04

    A new approach for a cloud point extraction electrothermal atomic absorption spectrometric method was used for determining bismuth. The aqueous analyte was acidified with sulfuric acid (pH 3.0-3.5). Triton X-114 was added as a surfactant and dithizone was used as a complexing agent. After phase separation at 50 deg. C based on the cloud point separation of the mixture, the surfactant-rich phase was diluted using tetrahydrofuran (THF). Twenty microliters of the enriched solution and 10 {mu}l of 0.1% (w/v) Pd(NO{sub 3}){sub 2} as chemical modifier were dispersed into the graphite tube and the analyte determined by electrothermal atomic absorption spectrometry. After optimizing extraction conditions and instrumental parameters, a preconcentration factor of 196 was obtained for a sample of only 10 ml. The detection limit was 0.02 ng ml{sup -1} and the analytical curve was linear for the concentration range of 0.04-0.60 ng ml{sup -1}. Relative standard deviations were <5%. The method was successfully applied for the extraction and determination of bismuth in tap water and biological samples (urine and hair)

  2. FTIR-spectrometer-determined absorption coefficients of seven hydrazine fuel gases - Implications for laser remote sensing

    Molina, L. T.; Grant, W. B.

    1984-01-01

    The absorption spectra of three hydrazines and four of their air-oxidation products were measured in the 9-12-micron spectral region with a Fourier transform infrared (FTIR) spectrometer with a 0.05-kayser resolution to determine absorption coefficients at CO2 and tunable diode laser wavelengths. The measurements agreed well with published CO2 laser determinations for many of the absorption coefficients, except where the published values are thought to be in error. The coefficients were then used to estimate the sensitivity for remote detection of these gases using CO2 and tunable diode lasers in long-path differential absorption measurements.

  3. Preconcentration of submicrogram amounts of metals from natural water for X-ray energy spectrometric determination using pyrrolidinecarbodithioic acid

    A method was developed for the routine determination of several trace metals in natural waters by X-ray energy spectrometry following precipitation with pyrrolidinecarbodithioate. Preoxidation with persulfate eliminates interferences by organic matter. By optimizing carrier ion selection and measurement conditions, one may determine dithioate-reactive elements with Z less than or equal to 50 by means of their K X-rays, and some with Z greater than or equal to 80 by means of their L X-rays. Determinations are feasible for several elements at concentrations down to 250 ng L-1, or below. Recoveries are generally greater than 90%, although some exceptions are noted. Reproducibility with real samples averaged about 25% relative standard deviation for five representative elements at concentrations above 250 ng L-1. 24 references, 5 figures, 4 tables

  4. Determining neutrino absorption spectra at Ultra-High Energies

    Scholten, Olaf; Van Vliet, Arjen

    2008-01-01

    A very efficient method to measure the flux of Ultra-high energy (UHE) neutrinos is through the detection of radio waves which are emitted by the particle shower in the lunar regolith. The highest acceptance is reached for radio waves in the frequency band of 100-200 MHz which can be measured with modern radio telescopes. In this work we investigate the sensitivity of this detection method to structures in the UHE neutrino spectrum caused by their absorption on the low-energy relic anti-neutr...

  5. Optimization of the preconcentration system of cadmium with 1(2-thiazolylazo)-p-cresol using a knotted reactor and flame atomic absorption spectrometric detection

    The present paper proposes an on-line preconcentration procedure for cadmium determination in drinking water samples. It is based on the precipitation of cadmium(II) ions on a knotted reactor (KR) using 1(2-thiazolylazo)-p-cresol (TAC) as complexing reagent. The optimization step was performed using a full factorial design involving the variables: pH, eluent concentration (nitric acid) and TAC concentration. The results of this experiment demonstrated that these variables at chosen levels are not statistically significant. Under optimized experimental established conditions, analytical parameters for the preconcentration method were: a detection limit of 40.0 ng/l, precision as relative standard deviation (RSD) of 1.2 and 1.0%, for cadmium concentration of 2.5 and 20.0 μg/l, respectively. The preconcentration factor considering the slopes of the analytical curves with and without preconcentration is 23 for a sample volume of 10 ml. This system shows a sampling frequency of 25 h-1. In order to check the accuracy, the standard reference material, NIST SRM 1643d trace elements in water was analyzed. A comparison, using t-test demonstrates that there is not significant difference among the achieved results with proposed method and the certified values. The addition/recovery experiments in the samples analyzed demonstrated the accuracy and applicability of the system developed for cadmium determination in water samples

  6. Spectrometric techniques 3

    Vanasse, George A

    2013-01-01

    Spectrometric Techniques, Volume III presents the applications of spectrometric techniques to atmospheric and space studies. This book reviews the spectral data processing and analysis techniques that are of broad applicability.Organized into five chapters, this volume begins with an overview of the instrumentation used for obtaining field data. This text then reviews the contribution that space-borne spectroscopy in the thermal IR has made to the understanding of the planets. Other chapters consider the instruments that have recorded the planetary emission spectra. This book discusses as well

  7. Determination of lithium isotopes at natural abundance levels by atomic absorption spectrometry

    Meier, A.L.

    1982-01-01

    The relationships of the absorption of 6Li and 7Li hollow cathode lamp emissions are used to determine lithium isotopic composition in the natural abundance range of geologic materials. Absorption was found to have a nonlinear dependence upon total lithium concentration and isotopic composition. A method using nonlinear equations to describe the relationship of the absorption of 6Li and 7Li lamp radiation is proposed as a means of calculating isotopic composition that is independent of total lithium concentration.

  8. A novel approach for speciation of airborne chromium by convective-interaction media fast-monolithic chromatography with electrothermal atomic-absorption spectrometric detection.

    Scancar, Janez; Milacic, Radmila

    2002-05-01

    A new analytical procedure using an anion-exchange separation support based on convective-interaction media (CIM) was developed for the speciation of chromium. The separation of Cr(VI) was performed on a weak anion-exchange CIM diethylamine (DEAE) fast-monolithic chromatographic disc. Buffer A (0.005 mol dm(-3) TRIS-HCl, pH 8.0) and buffer B (buffer A plus 3 mol dm(-3) NH4NO3) were employed in the separation procedure. The separated chromium species were determined 'off-line' by ETAAS in 0.5 cm3 fractions. The applicability of the CIM DEAE-ETAAS procedure was investigated for the determination of airborne Cr(VI) at a plasma cutting workplace. Aerosols were collected on polycarbonate membrane filters of 8 and 0.4 microm pore size (inhalable and respirable aerosols). Alkaline extraction of filters in a heated ultrasonic bath was applied to leach chromium. Good repeatability of measurement (+/-3.0%) of the alkaline extracts was obtained for Cr(VI). The LOD (3s) was found to be 0.30 microg m(-3) Cr(VI), when 0.25 m3 of air was collected on the filter. The validation of the procedure was performed by spiking filters with Cr(VI) and by the analysis of the standard reference material CRM 545, Cr(VI) in welding dust loaded on a filter. Good recoveries for spiked samples (101-102%) and good agreement between Cr(VI) found and the reported certified value for CRM 545 were obtained. The extracts were also analysed by the FPLC-ETAAS technique. Good agreement between two techniques (r2 = 0.9978) confirmed the reliability of the CIM DEAE-ETAAS procedure developed. The main advantage of the procedure lies in the speed of the chromatographic separation (chromatographic run completed in 15 min). PMID:12081040

  9. Determination of nine high-intensity sweeteners in various foods by high-performance liquid chromatography with mass spectrometric detection

    Zygler, Agata; Wasik, Andrzej; Kot-Wasik, Agata; Namieśnik, Jacek

    2011-01-01

    An analytical procedure involving solid-phase extraction (SPE) and high-performance liquid chromatography-mass spectrometry has been developed for the determination of nine high-intensity sweeteners authorised in the EU; acesulfame-K (ACS-K), aspartame (ASP), alitame (ALI), cyclamate (CYC), dulcin (DUL), neohesperidin dihydrochalcone (NHDC), neotame (NEO), saccharin (SAC) and sucralose (SCL) in a variety of food samples (i.e. beverages, dairy and fish products). After extraction with a buffer...

  10. Development of a high-speed MALDI-triple quadrupole mass spectrometric method for the determination of 3,4-methylenedioxymethamphetamine (MDMA) in oral fluid.

    Poetzsch, Michael; Steuer, Andrea E; Hysek, Cedric M; Liechti, Matthias E; Kraemer, Thomas

    2016-02-01

    3,4-Methylenedioxymethamphetamine (MDMA, ecstasy) is still a widely used illicit designer drug and its detection in different matrices is of major importance for forensic purposes (e.g. driving under the influence) as well as for workplace drug testing or abstinence control. Established analytical methods for the determination of MDMA are mainly employing high performance liquid chromatography (HPLC) or gas chromatography (GC) coupled to mass spectrometric detection. Matrix assisted laser desorption/ionization-triple quadrupole-tandem mass spectrometry (MALDI-QqQ-MS/MS) is so far rarely used in forensics and offers an ultrafast high-throughput platform. The Quantisal™ Oral Fluid Collection Device was used for sample collection. After addition of the deuterated internal standard and a carbonate buffer (0.75 M Na2 CO3 ), oral fluid samples were liquid-liquid extracted (ButOAc/EtOAc, 1:1). As little as 1 microlitre of a mixture of this extract and the MALDI matrix (alpha-cyano-4-hydroxycinnamic acid) was spotted onto the MALDI plate and could directly be analyzed. With MALDI omitting chromatographic separation, very short analysis times of about 10 s per sample were possible. The method was developed and validated according to international guidelines including specificity, recovery, matrix effects, accuracy and precision, stabilities and limit of quantification. All validation criteria were fulfilled except for ion suppression/enhancement. Comparison with a routine liquid chromatography-tandem mass spectrometry (LC-MS/MS) method showed good agreement of the results. Applicability of the method was shown by analyzing about 250 oral fluid samples collected after controlled administration of 125 mg MDMA in a pharmacokinetic study. The whole lot of samples could be analyzed in less than 1 h, proving the ultra-high-speed of the method. PMID:25990956

  11. Single-walled carbon nanotubes coated fibers for solid-phase microextraction and gas chromatography-mass spectrometric determination of pesticides in Tea samples.

    Wu, Fang; Lu, Wanping; Chen, Jinghua; Liu, Wei; Zhang, Lan

    2010-08-15

    Using a single-walled carbon nanotubes (SWCNTs) as stationary phase of solid-phase microextraction (SPME) fibers, a simple, low cost and environmentally friendly method for extraction of 13 pesticides in Tea samples has been developed following gas chromatography-mass spectrometric determination. Potential factors affecting the extraction efficiency were investigated and optimized, including extraction and desorption time, extraction temperature, stirring rate, solution pH and ionic strength. Under optimized conditions, the linearity of the developed method was in the range of 0.125-25 ng/mL with correlation coefficients greater than 0.9928 and the limits of detections (LODs) were 0.027-0.23 ng/mL (S/N=3). Meanwhile, the relative standard deviations (RSDs) for five successive measurements with single fiber, fiber-to-fiber, day-to-day were 2.3-13.0, 8.2-14.6 and 4.1-12.5%, respectively, indicating good reproducibility of the proposed method. The fiber had high extraction efficiency for studied pesticides in comparison with commercial poly(dimethylsiloxane) (PDMS) and polyacrylate (PA) fibers and could be used for more than 70 times without decrease of efficiency. The developed method was successfully applied for the analysis of real samples including green Tea, oolong Tea, white Tea, and flower Tea, and the recoveries of the pesticides spiked in these samples ranged from 75.1 to 118.4%. Chlorfenapyr and lambda-cyhalothrin were found in the Tea samples bought randomly from local market. The results demonstrated that the developed SWCNTs-SPME method was a simple, efficient pretreatment and enrichment procedure for pesticides in complex matrices. PMID:20678665

  12. A liquid chromatography-tandem mass spectrometric method for quantitative determination of native 5-methyltetrahydrofolate and its polyglutamyl derivatives in raw vegetables.

    Wang, Chao; Riedl, Ken M; Schwartz, Steven J

    2010-11-01

    Folate deficiency is a prevalent phenomenon worldwide especially in underprivileged countries. Polyglutamyl 5-methyltetrahydrofolate (5MTHF) species are the naturally occurring principle folate in store-bought vegetables. Here we report a simple and complete extraction method for the determination of native polyglutamyl 5-methyltetrahydrofolate in vegetables using high performance liquid chromatography with tandem mass spectrometric detection (HPLC-MS/MS). Coarsely chopped samples (18 different vegetables) were steamed to inactivate glutamylase enzymes and liberate folate from binding proteins and extracted in a reducing buffer with (13)C(5) 5MTHF stable isotope added as internal standard. The polyglutamyl 5-methyltetrahydrofolate species were separated in 9 min on a C(18) column using a reversed phase system. HPLC eluate was interfaced with a triple quadrupole mass spectrometer operated in electrospray positive mode. The respective pseudomolecular cation of each polyglutamyl 5-methyltetrahydrofolate species was selected for fragmentation to a common daughter ion for detection. We quantitated polyglutamyl 5-methyltetrahydrofolate in store-bought vegetables from families Brassicaceae, Asteraceae and Amaranthaceae (including mustard greens, romaine lettuce and Swiss chard) of which most have not been quantitated previously. Most vegetables from Asteraceae and those from Amaranthaceae contained similar amounts of monoglutamyl 5MTHF and polyglutamyl 5MTHF while Brassicaceae were dominated by polyglutamyls and endive species (Asteraceae) contained mainly monoglutamyl 5MTHF. The precision of the method for the various polyglutamyl 5-methyltetrahydrofolate forms was 1-9% RSD, recovery 84-91%, limit of detection 64-658 fmol and limit of quantitation 193-1994 fmol. Herein we describe a rapid, sensitive and selective HPLC-MS/MS technique to quantitate polyglutamyl 5-methyltetrahydrofolate species. This method may be suitable for analyzing the polyglutamyl 5

  13. Determination of trace elements in various kinds of bean by X-ray spectrometric techniques (1995-96)

    Various kinds of bean such as Peanut, Gram Whole, Black Eye Bean, Small Red Bean, Lab Lab Bean, Green Mung Bean, Filed Pea, Seasame Seed, Sultani, Maize, Butter Bean, Dolichos Lab Lab, Toor Whole, Small Yellow Bean, Cow Pea have been collected and analysed by EDXRF analysis for trace elements. The measurement system consists of a Cd-109 annual excitation source, a Si (Li) detector, H V power supply, a spectrometry amplifier, a multichannel analyser and a personal computer. The samples were prepared as pressed pellets and measured by Emission Transmission Technique. The accuracy was determined by analysing standard reference material, SOIL-7 form IAEA. (author)

  14. Energy dispersive x-ray fluorescence spectrometric determination of vanadium, nickel, and iron in petroleum and petroleum residua

    Trace metals such as vanadium, nickel, and iron in fluid catalytic cracking feedstocks deposit on the catalyst and adversely affect catalyst activity and product yields. Vanadium compounds can also cause damage to furnace linings and corrosion of boiler tubes or gas turbine blades. A rapid and sensitive analytical method is need to detect these metals in feedstocks, products, and residual. In this paper such a method using energy dispersive X-ray fluorescence (EDXRF) spectrometry for determination of vanadium, nickel, and iron in petroleum and petroleum residua is described. In order to eliminate matrix effects, samples containing an internal standard (cobalt) were decomposed by heating with concentrated sulfuric acid and the resulting carbonaceous residua were ashed. X-ray fluorescent spectral intensities of V, Ni, Fe, and Co were measured using established instrumental parameters. Since the Fe Kβ and Co Kα lines overlapped, the slope and the intercept of the ratio of Fe Kα to Fe Kβ intensities from the analysis of ash of several iron standards were used for correction of Co spectral intensities. Sample metal concentrations were determined by comparison of spectral ratios to those of ashed calibration standards

  15. A novel, donor-active solvent-assisted liquid-phase microextraction procedure for spectrometric determination of zinc

    Kocurova, Livia; Fatlova, Martina; Bazel, Yaroslav; Serbin, Rastislav; Andruch, Vasil, E-mail: liviamonika.kocurova@gmail.com [Department of Analytical Chemistry, University of P. J. Safarik, Kosice (Slovakia); Balogh, Ioseph S. [Department of Chemistry, College of Nyiregyhaza (Hungary); Simon, Andras [Department of General and Analytical Chemistry, Budapest University of Technology and Economics, Budapest (Hungary); Badida, Miroslav; Rusnak, Radoslav [Department of Environmentalistics, Faculty of Mechanical Engineering, Technical University of Kosice (Slovakia)

    2014-02-15

    Based on the reaction of Zn(II), thiocyanate and 2-[2-(5-dimethylamino-thiophen-2-yl)-vinyl]- 1,3,3-trimethyl-3H-indolium bromide (DTVTI), a donor-active solvent-assisted liquid-phase microextraction procedure followed by spectrophotometric determination of zinc at 570 nm was developed. The optimum experimental conditions were investigated and found to be as follows: concentration of NH{sub 4}SCN 0.02 mol L{sup -1} concentration of DTVTI 4 x 10{sup -5} mol L{sup -1}. Various extraction solvents were studied alone as well as in mixtures with different improvers, and a mixture of toluene as the extraction solvent and tributylphosphate as the donor-active solvent in a 4:1 v/v ratio was selected. The calibration plot was linear up to 2.62 mg L{sup 1} of zinc with limit of detection 0.09 mg L{sup -1}. The developed procedure was applied for zinc determination in dietary supplements. (author)

  16. A novel, donor-active solvent-assisted liquid-phase microextraction procedure for spectrometric determination of zinc

    Based on the reaction of Zn(II), thiocyanate and 2-[2-(5-dimethylamino-thiophen-2-yl)-vinyl]- 1,3,3-trimethyl-3H-indolium bromide (DTVTI), a donor-active solvent-assisted liquid-phase microextraction procedure followed by spectrophotometric determination of zinc at 570 nm was developed. The optimum experimental conditions were investigated and found to be as follows: concentration of NH4SCN 0.02 mol L-1 concentration of DTVTI 4 x 10-5 mol L-1. Various extraction solvents were studied alone as well as in mixtures with different improvers, and a mixture of toluene as the extraction solvent and tributylphosphate as the donor-active solvent in a 4:1 v/v ratio was selected. The calibration plot was linear up to 2.62 mg L1 of zinc with limit of detection 0.09 mg L-1. The developed procedure was applied for zinc determination in dietary supplements. (author)

  17. Spectrometric mixture analysis: An unexpected wrinkle

    Robert De Levie

    2009-09-01

    The spectrometric analysis of a mixture of two chemically and spectroscopically similar compounds is illustrated for the simultaneous spectrometric determination of caffeine and theobromine, the primary stimulants in coffee and tea, based on their ultraviolet absorbances. Their analysis indicates that such measurements may need an unexpectedly high precision to yield accurate answers, because of an artifact of inverse cancellation, in which a small noise or drift signal is misinterpreted in terms of a concentration difference. The computed sum of the concentrations is not affected.

  18. Determination of gold in geologic materials by solvent extraction and atomic-absorption spectrometry

    Huffman, Claude; Mensik, J.D.; Riley, L.B.

    1967-01-01

    The two methods presented for the determination of traces of gold in geologic materials are the cyanide atomic-absorption method and the fire-assay atomic-absorption method. In the cyanide method gold is leached with a sodium-cyanide solution. The monovalent gold is then oxidized to the trivalent state and concentrated by extracting into methyl isobutyl ketone prior to estimation by atomic absorption. In the fire-assay atomic-absorption method, the gold-silver bead obtained from fire assay is dissolved in nitric and hydrochloric acids. Gold is then concentrated by extracting into methyl isobutyl ketone prior to determination by atomic absorption. By either method concentrations as low as 50 parts per billion of gold can be determined in a 15-gram sample.

  19. A laboratory manual for the determination of metals in water and wastewater by atomic absorption spectrophotometry

    This guide presents, in addition to a brief discussion of the basic principles and practical aspects of atomic absorption spectrophotometry, a scheme of analysis for the determination of 19 metals in water and wastewater, 16 by flame atomic absorption and 3 by vapour generation techniques. Simplicity, speed and accuracy were the main criteria considered in the selection of the various methods

  20. Simultaneous Atomic Absorption Spectrometry for Cadmium and Lead Determination in Wastewater: A Laboratory Exercise

    Correia, Paulo R. M.; Oliveira, Pedro V.

    2004-01-01

    The simultaneous determination of cadmium and lead by multi-element atomic absorption spectrometry with electrochemical atomization is proposed by employing a problem-based approach. The reports indicate that the students assimilated the principles of the simultaneous atomic absorption spectrometry (SIMAAS), the role of the chemical modifier, the…

  1. Fractionation of trace elements in agricultural soils using ultrasound assisted sequential extraction prior to inductively coupled plasma mass spectrometric determination.

    Matong, Joseph M; Nyaba, Luthando; Nomngongo, Philiswa N

    2016-07-01

    The main objectives of this study were to determine the concentration of fourteen trace elements and to investigate their distribution as well as a contamination levels in selected agricultural soils. An ultrasonic assisted sequential extraction procedure derived from three-step BCR method was used for fractionation of trace elements. The total concentration of trace elements in soil samples was obtained by total digestion method in soil samples with aqua regia. The results of the extractable fractions revealed that most of the target trace elements can be transferred to the human being through the food chain, thus leading to serious human health. Enrichment factor (EF), geo-accumulation index (Igeo), contamination factor (CF), risk assessment code (RAC) and individual contamination factors (ICF) were used to assess the environmental impacts of trace metals in soil samples. The EF revealed that Cd was enriched by 3.1-7.2 (except in Soil 1). The Igeo results showed that the soils in the study area was moderately contaminated with Fe, and heavily to extremely polluted with Cd. The soil samples from the unplanted field was found to have highest contamination factor for Cd and lowest for Pb. Soil 3 showed a high risk for Tl and Cd with RAC values of greater than or equal to 50%. In addition, Fe, Ni, Cu, V, As, Mo (except Soil 2), Sb and Pb posed low environmental risk. The modified BCR sequential extraction method provided more information about mobility and environmental implication of studied trace elements in the study area. PMID:27058917

  2. Gamma spectrometric assessment of nuclear fuel

    Krištof, Edvard; Pregl, Gvido

    1990-12-01

    A description is given of a gamma spectrometric technique which has been developed with the aim of determining the amount of a certain radioactive fission product taking into consideration local variations of the linear attenuation coefficient of gamma rays. Also, an experiment using a fuel element of the TRIGA Mark II reactor in Ljubljana is presented.

  3. Determination of nine high-intensity sweeteners in various foods by high-performance liquid chromatography with mass spectrometric detection.

    Zygler, Agata; Wasik, Andrzej; Kot-Wasik, Agata; Namieśnik, Jacek

    2011-06-01

    An analytical procedure involving solid-phase extraction (SPE) and high-performance liquid chromatography-mass spectrometry has been developed for the determination of nine high-intensity sweeteners authorised in the EU; acesulfame-K (ACS-K), aspartame (ASP), alitame (ALI), cyclamate (CYC), dulcin (DUL), neohesperidin dihydrochalcone (NHDC), neotame (NEO), saccharin (SAC) and sucralose (SCL) in a variety of food samples (i.e. beverages, dairy and fish products). After extraction with a buffer composed of formic acid and N,N-diisopropylethylamine at pH 4.5 in ultrasonic bath, extracts were cleaned up using Strata-X 33 μm Polymeric SPE column. The analytes were separated in gradient elution mode on C(18) column and detected by mass spectrometer working with an electrospray source in negative ion mode. To confirm that analytical method is suitable for its intended use, several validation parameters, such as linearity, limits of detection and quantification, trueness and repeatibilty were evaluated. Calibration curves were linear within a studied range of concentrations (r(2) ≥ 0.999) for six investigated sweeteners (CYC, ASP, ALI, DUL, NHDC, NEO). Three compounds (ACS-K, SAC, SCL) gave non-linear response in the investigated concentration range. The method detection limits (corresponding to signal-to-noise (S/N) ratio of 3) were below 0.25 μg mL(-1) (μg g(-1)), whereas the method quantitation limits (corresponding to S/N ratio of 10) were below 2.5 μg mL(-1) (μg g(-1)). The recoveries at the tested concentrations (50%, 100% and 125% of maximum usable dose) for all sweeteners were in the range of 84.2 ÷ 106.7%, with relative standard deviations sweeteners in drinks, yoghurts and fish products. The procedure described here is simple, accurate and precise and is suitable for routine quality control analysis of foodstuffs. PMID:21465096

  4. Determination of optical absorption edge in amorphous thin films of selenium and selenium dopped with sulphur

    The transmittance and the reflectance of three thin films of S-Se alloys have been determined for different wavelengths in the range 5000-11000 A. Accurate methods had been used to calculate the optical constants n and k as well as the absorption coefficient K. The determined absorption edges for S-Se alloys shifts to higher photon energies by increasing the concentration of sulphur content. (author)

  5. Complete determination of the reflection coefficient in neutron specular reflection by absorptive nonmagnetic media

    An experimental method is proposed which allows a complete determination of the complex reflection coefficient for absorptive media for positive and negative values of the momenta. It makes use of magnetic reference layers, and is a modification of a recently proposed technique for phase determination based on polarization measurements. The complex reflection coefficient resulting from a simulated application of the method is used for a reconstruction of the scattering density profiles of absorptive nonmagnetic media by inversion

  6. Determinants of drug absorption in different ECMO circuits

    E.D. Wildschut (Enno); M.J. Ahsman (Maurice); K. Allegaert (Karel); R.A.A. Mathot (Ron); D. Tibboel (Dick)

    2010-01-01

    textabstractPurpose: The aim of this in vitro study was to evaluate potential determinants of drug loss in different ECMO circuits. Methods: Midazolam, morphine, fentanyl, paracetamol, cefazolin, meropenem and vancomycin were injected into three neonatal roller pump, two paediatric roller pump and t

  7. Characterization of the oral absorption of several aminopenicillins: determination of intrinsic membrane absorption parameters in the rat intestine in situ

    Sinko, P. J.; Amidon, G. L.

    1992-01-01

    The absorption mechanism of several penicillins was characterized using in situ single-pass intestinal perfusion in the rat. The intrinsic membrane parameters were determined using a modified boundary layer model (fitted value +/- S.E.): Jmax* = 11.78 +/- 1.88 mM, Km = 15.80 +/- 2.92 mM, Pm* = 0, Pc* = 0.75 +/- 0.04 for ampicillin; Jmax* = 0.044 +/- 0.018 mM, Km = 0.058 +/- 0.026 mM, Pm* = 0.558 +/- 0.051, Pc* = 0.757 +/- 0.088 for amoxicillin; and Jmax* = 16.30 +/- 3.40 mM, Km = 14.00 +/- 3.30 mM, Pm* = 0, Pc* = 1.14 +/- 0.05 for cyclacillin. All of the aminopenicillins studied demonstrated saturable absorption kinetics as indicated by their concentration-dependent wall permeabilities. Inhibition studies were performed to confirm the existence of a nonpassive absorption mechanism. The intrinsic wall permeability (Pw*) of 0.01 mM ampicillin was significantly lowered by 1 mM amoxicillin and the Pw* of 0.01 mM amoxicillin was reduced by 2 mM cephradine consistent with competitive inhibition.

  8. Determinants of drug absorption in different ECMO circuits

    Wildschut, Enno; Ahsman, Maurice; Allegaert, Karel; Mathot, Ron; Tibboel, Dick

    2010-01-01

    textabstractPurpose: The aim of this in vitro study was to evaluate potential determinants of drug loss in different ECMO circuits. Methods: Midazolam, morphine, fentanyl, paracetamol, cefazolin, meropenem and vancomycin were injected into three neonatal roller pump, two paediatric roller pump and two clinically used neonatal roller pump circuits, all with a silicone membrane, and two neonatal centrifugal pump circuits with polypropylene hollow-fibre membranes. Serial blood samples were taken...

  9. Determination of iron absorption and excretion by whole-body counting

    Using a whole-body counter, the authors have studied 59Fe absorption and loss in 8 normal subjects and in 30 iron deficient patients. Results showed that whole-body counting provided an excellent and simple method for iron retention measurements, obviating many inaccuracies of previous technic. Normal absorption of radio iron with this procedure has ranged from 9 per cent to 20 per cent of the administered tracer in normal subjects, with a mean of 15 per cent. A significant increase in 59Fe absorption was noted in 21 iron-deficient patients in whom the retention ranged from 40 to 100 per cent. However, 3 iron-deficient patients were found to have low absorption, and their severe iron deficiency could be correlated with this defect in absorption. This method permits also the determination of the rate of iron excretion during the following months and therefore the study of the mechanism of some pathological loss. (authors)

  10. Determination of antimony by using tungsten trap atomic absorption spectrometry

    An electrically heated tungsten coil was used as a trap in the determination of antimony. The technique consists of three steps. Initially, SbH3 is formed by hydride generation procedure; then the analyte species in vapor form are transported to W-coil trap heated at 370 deg. C. Following the preconcentration step, the trap is heated to 895 deg. C; analyte species are revolatilized and transported to the flame-heated quartz atom cell where atomization and the formation of signal take place. The experimental parameters were optimized both for trap and no-trap studies. The most important experimental parameters are concentrations of HCl and NaBH4 solutions, H2 and Ar gas flow rates, and collection and revolatilization temperatures of W-coil. Accuracy was tested using a certified reference material, waste water EU-L-1. Limit of detection for the system is 16 ng l-1 using a sample of 36 ml collected in 4.0 min. Enhancement factor in sensitivity was 17

  11. Application of Fiber Bragg Grating for Determining Positions of Gas Absorption Lines

    韩文念; 汪曣; 马凤; 刘琨; 贾大功; 刘铁根; 张红霞

    2010-01-01

    Fiber Bragg grating(FBG) is used as a wavelength reference device to calibrate the position of gas absorption peak in the intracavity absorption gas sensor(ICAGS) based on erbium-doped fiberring laser.This system can detect both the reflectance spectrum of FBGs and absorption spectrum of measured gas during a single wavelength sweeping process by linearly varying the driving voltage of optic filter.The voltages corresponding to center wavelength positions of four FBGs in the spectrum are determined through ...

  12. Calcium Absorption in Infants and Small Children: Methods of Determination and Recent Findings

    Steven A. Abrams

    2010-04-01

    Full Text Available Determining calcium bioavailability is important in establishing dietary calcium requirements. In infants and small children, previously conducted mass balance studies have largely been replaced by stable isotope-based studies. The ability to assess calcium absorption using a relatively short 24-hour urine collection without the need for multiple blood samples or fecal collections is a major advantage to this technique. The results of these studies have demonstrated relatively small differences in calcium absorption efficiency between human milk and currently available cow milk-based infant formulas. In older children with a calcium intake typical of Western diets, calcium absorption is adequate to meet bone mineral accretion requirements.

  13. Determination of absorption cross-section of Si nanocrystals by two independent methods based on either absorption or luminescence

    Absorption cross-section (ACS) of silicon nanocrystals (SiNCs) is determined via two completely independent approaches: (i) Excitation-intensity-dependent photoluminescence (PL) kinetics under modulated (long square pulses) pumping and (ii) absorbance measured by the photothermal deflection spectroscopy combined with morphology information obtained by the high-resolution transmission electron microscopy. This unique comparison reveals consistent ACS values around 10−15 cm2 for violet excitation of SiNCs of about 3–5 nm in diameter and this value is comparable to most of direct band-gap semiconductor nanocrystals; however, it decreases steeply towards longer wavelengths. Moreover, we analyze the PL-modulation technique in detail and propose an improved experimental procedure which enables simpler implementation of this method to determine ACS of various (nano)materials in both solid and liquid states

  14. Determination of absorption cross-section of Si nanocrystals by two independent methods based on either absorption or luminescence

    Valenta, J., E-mail: jan.valenta@mff.cuni.cz; Greben, M. [Department of Chemical Physics and Optics, Faculty of Mathematics and Physics, Charles University, Ke Karlovu 3, 121 16 Prague 2 (Czech Republic); Remeš, Z. [Institute of Physics, Academy of Sciences of the Czech Republic, Cukrovarnická 10, Prague 6 (Czech Republic); Gutsch, S.; Hiller, D.; Zacharias, M. [Faculty of Engineering, IMTEK, Albert-Ludwigs-University Freiburg, Georges-Köhler-Allee 103, 79110 Freiburg (Germany)

    2016-01-11

    Absorption cross-section (ACS) of silicon nanocrystals (SiNCs) is determined via two completely independent approaches: (i) Excitation-intensity-dependent photoluminescence (PL) kinetics under modulated (long square pulses) pumping and (ii) absorbance measured by the photothermal deflection spectroscopy combined with morphology information obtained by the high-resolution transmission electron microscopy. This unique comparison reveals consistent ACS values around 10{sup −15} cm{sup 2} for violet excitation of SiNCs of about 3–5 nm in diameter and this value is comparable to most of direct band-gap semiconductor nanocrystals; however, it decreases steeply towards longer wavelengths. Moreover, we analyze the PL-modulation technique in detail and propose an improved experimental procedure which enables simpler implementation of this method to determine ACS of various (nano)materials in both solid and liquid states.

  15. Experimental determination of resonance absorption cross sections for Zircaloy-2 and zirconium

    The integral absorption cross section for the neutron spectrum and the thermal absorption cross section for zircaloy-2 have been determined using the pile oscillator technique. Using both values and a measured ratio of the epithermal to the thermal flux, the effective resonance integrals were obtained. After subtraction of the contributions for alloy and impurity elements, the effective resonance integrals for zirconium were evaluated. An extrapolated value of 0.91±0.10 was obtained for the dilute integral. (author)

  16. Determination of traces of cadmium in zinc by flameless atomic absorption spectrophotometry after extraction

    Janssen, A.; Willmann, K.H.; Simon, F.J.

    1985-01-01

    The suitability of dithizone, diethyldithiocarbamate and tetramethylendithiocarbamate as chelating agents for the extraction-photometric cadmium determination by flameless atomic absorption spectrophotometry in the presence of zinc was investigated. It has been found that the extraction of the dithizone chelate by carbon tetrachloride permits an uninfluenced determination of cadmium in the presence of a zinc excess up to 10/sup 5/. Therefore the use of flameless atomic absorption spectrophotometry raises the selectivity as compared to photometry, because photometry only permits a 1000-fold excess of zinc. With this method 2x10/sup -4/% of cadmium in zinc can be determined without further corrections of matrix effects.

  17. Coprecipitation of trace elements with Ni2+/2-Nitroso-1-naphthol-4-sulfonic acid and their determination by flame atomic absorption spectrometry

    Ni2+/2-Nitroso-1-naphthol-4-sulfonic acid precipitate was used for the coprecipitation of Co, Pb, Cu, Fe and Zn prior to their flame atomic absorption spectrometric (FAAS) determinations in environmental samples. The precipitate could be easily dissolved with concentrated nitric acid. The recovery values for analyte ions were higher than 95%. The parameters including pH, sample volume, centrifuge time, amounts of nickel and matrix effects were optimized for the quantitative recoveries of the analytes. The relative standard deviations of cobalt, lead, copper, iron and zinc were found 4.5, 5.7, 3.8, 6.1 and 7.5%, respectively. The limit of detection was calculated as 1.05, 2.67, 1.30, 1.38, and 0.50 μg L-1 for cobalt, lead, copper, iron and zinc. The validation of the procedure was checked by the analysis of IAEA 336 lichen and SLRS 4 Riverine water standard reference materials were analyzed with satisfactory results. The presented coprecipitation procedure was successfully applied to some environmental samples for determination of analyte ions.

  18. Capturing Absorptive Capacity: Concepts, Determinants, Measurement Modes and Role in Open Innovation

    Lewandowska Małgorzata Stefania

    2015-03-01

    Full Text Available Absorptive capacity (ACAP enables firm to adjust to a rapidly changing environment and achieve sustained competitive advantage. This study contributes to the existing body of knowledge on ACAP by providing a comprehensive literature review of the various conceptual attributes of the construct, its determinants, outcomes, and positive and negative consequences of using its input-oriented, output-oriented, and perceptive measurement modes. Proposals for constructing ACAP based on the Community Innovation Survey (CIS empirically illustrate for the conceptual part of the paper. Additionally, combining concepts of absorptive capacity and open innovation (which is still rare in the literature provides a new perspective on the role of absorptive capacity in opening up the innovation process. This advances the understanding of both inter-related proposals. The article also identifies key problems and formulates future research directions to improve the multi-level characteristics of absorptive capacity.

  19. Spectrometric techniques 2

    Vanasse, George A

    2013-01-01

    Spectrometric Techniques, Volume II provides information pertinent to vacuum ultraviolet techniques to complete the demonstration of the diversity of methods available to the spectroscopist interested in the ultraviolet visible and infrared spectral regions. This book discusses the specific aspects of the technique of Fourier transform spectroscopy.Organized into five chapters, this volume begins with an overview of the large number of systematic effects in the recording of an interferogram. This text then examines the design approach for a Fourier transform spectrometer with focus on optics.

  20. Direct determination of selenoproteins in polyvinylidene difluoride membranes by electrothermal atomic absorption spectrometry

    Sidenius, U; Gammelgaard, Bente

    2000-01-01

    A method for the direct determination of selenoproteins in plastic membranes after protein separation by gel electrophoresis was developed. Quantification was based on the determination of the selenium content of the proteins by electrothermal atomic absorption spectrometry (ET-AAS) after manual...... were excised and chemical modifier was added on top of the excised membrane prior to atomic absorption measurement. Acceptable linearity was achieved in the range 2-10 ng Se, corresponding to selenium concentrations close to 1 mg/L, when aqueous solutions of selenomethionine standard as well as...

  1. Application of Fiber Bragg Grating for Determining Positions of Gas Absorption Lines

    HAN Wennian; WANG Yan; MA Feng; LIU Kun; JIA Dagong; LIU Tiegen; ZHANG Hongxia

    2010-01-01

    Fiber Bragg grating(FBG)is used as a wavelength reference device to calibrate the position of gas absorption peak in the intracavity absorption gas sensor(ICAGS)based on erbium-doped fiberring laser.This system can detect both the reflectance spectrum of FBGs and absorption spectrum of measured gas during a single wavelength sweeping process by linearly varying the driving voltage of optic filter.The voltages corresponding to center wavelength positions of four FBGs in the spectrum are determined through Gaussian peak fitting.Then,the wavelengths of gas absorption lines are deduced from the correspondence between driving voltage and wavelength obtained by quadratic curve fitting.The maximum error of wavelength of acetylene absorption lines between experimental results and those from HITRAN database is 0.106 nm and the resolving accuracy of two adjacent absorption lines is about93.593%.By using this method,ICAGS can theoretically recognize the measured gas type and monitor multi-gas components.

  2. Peat as a natural solid-phase for copper preconcentration and determination in a multicommuted flow system coupled to flame atomic absorption spectrometry

    Gonzales, A.P.S. [Centro de Ciencias Naturais e Humanas, Universidade Federal do ABC, Rua Santa Adelia, 166, 09210-170 Santo Andre (Brazil); Firmino, M.A. [Departamento de Engenharia de Materiais, Escola de Engenharia, Universidade Presbiteriana Mackenzie, Rua da Consolacao, 930, 01302-970 Sao Paulo (Brazil); Nomura, C.S. [Centro de Ciencias Naturais e Humanas, Universidade Federal do ABC, Rua Santa Adelia, 166, 09210-170 Santo Andre (Brazil); Rocha, F.R.P.; Oliveira, P.V. [Departamento de Quimica Fundamental, Instituto de Quimica, Universidade de Sao Paulo, Av. Prof. Lineu Prestes, 748, 05508-000 Sao Paulo (Brazil); Gaubeur, I. [Centro de Ciencias Naturais e Humanas, Universidade Federal do ABC, Rua Santa Adelia, 166, 09210-170 Santo Andre (Brazil)], E-mail: ivanise.gaubeur@ufabc.edu.br

    2009-03-23

    The physical and chemical characteristics of peat were assessed through measurement of pH, percentage of organic matter, cationic exchange capacity (CEC), elemental analysis, infrared spectroscopy and quantitative analysis of metals by ICP OES. Despite the material showed to be very acid in view of the percentage of organic matter, its CEC was significant, showing potential for retention of metal ions. This characteristic was exploited by coupling a peat mini-column to a flow system based on the multicommutation approach for the in-line copper concentration prior to flame atomic absorption spectrometric determination. Cu(II) ions were adsorbed at pH 4.5 and eluted with 0.50 mol L{sup -1} HNO{sub 3}. The influence of chemical and hydrodynamic parameters, such as sample pH, buffer concentration, eluent type and concentration, sample flow-rate and preconcentration time were investigated. Under the optimized conditions, a linear response was observed between 16 and 100 {mu}g L{sup -1}, with a detection limit estimated as 3 {mu}g L{sup -1} at the 99.7% confidence level and an enrichment factor of 16. The relative standard deviation was estimated as 3.3% (n = 20). The mini-column was used for at least 100 sampling cycles without significant variation in the analytical response. Recoveries from copper spiked to lake water or groundwater as well as concentrates used in hemodialysis were in the 97.3-111% range. The results obtained for copper determination in these samples agreed with those achieved by graphite furnace atomic absorption spectrometry (GFAAS) at the 95% confidence level.

  3. Determination of vitamin B12 (cobalamine) absorption by means of a simple double-isotope technique

    The background, practical instruction and clinical results of a simplified method of determining the absorption of cobalamine (vitamin B12) are presented. The simultaneous administration of 57CO-CN-cobalamine, a non-absorbable marker (51CrCl3), and red carmine tablets enable quantitative assessments of the cobalamine absorption by collection of a small red feaces sample. In contrast to the classical Schilling-test, this vitamin B12 absorption test (B12-ABS-test) or faeces-spot-test is, independent of fasting, flushing dose, renal function and diurnal urinary collection. This is documented in a series of clinical studies. The B12-ABS-test provides accurate and precise results compared to the reference method (whole-body-counting). The Schilling test, on the contrary, gives approximately 50% false low values in a reference group of elderly hospitalized patients. A modification of the B12-ABS-test, has been used to determine the cobalamine absorption in children, and a set of age-related reference intervals have been established, together with quantitative measurements of the cobalamine absorption in children with small bowel diseases. Based on several years of practical experience, we recommend replacement of the Schilling test by this simple double-isotope technique. (author)

  4. Flow injection determination of copper in mussels by flame atomic absorption spectrometry after on-line continuous ultrasound-assisted extraction

    Moreno-Cid, A.; Yebra, M. C.

    2002-05-01

    Copper was extracted on-line from solid mussel samples by a simple and rapid continuous ultrasound-assisted extraction system (CUES). The CUES is connected to a flow injection manifold, which permits the on-line flame atomic absorption spectrometric determination of copper. The manifold is simple and the copper signal was obtained for a volume of 250 μl of acid leachate injected into an ultrapure water carrier stream. An experimental design was used for the optimization of the continuous leaching procedure. Compared to off-line ultrasonic-assisted extraction methods, sonication time is reduced by factors of 6-12, the leaching takes place at room temperature (20 °C), and the analysis time is reduced because centrifugation was not necessary to separate the liquid phase. The method allowed a total sampling frequency of 11 samples h -1, with a relative standard deviation for the complete procedure of 2.7% (for a sample containing 2.0 μg g -1 copper (wet mass, n=11). The limit of detection was 0.06 μg g -1 (wet mass) for 30 mg of sample. The analytical procedure was verified for a reference standard material (TORT-1). The analytical procedure was applied to mussel samples from Galicia (Spain).

  5. Preconcentration and determination of boron in milk, infant formula, and honey samples by solid phase extraction-electrothermal atomic absorption spectrometry

    This work presents alternative procedures for the electrothermal atomic absorption spectrometric determination of boron in milk, infant formulas, and honey samples. Honey samples (10% m/v) were diluted in a medium containing 1% v/v HNO3 and 50% v/v H2O2 and introduced in the atomizer. A mixture of 20 μg Pd and 0.5 μg Mg was used for chemical modification. Calibration was carried out using aqueous solutions prepared in the same medium, in the presence of 10% m/v sucrose. The detection limit was 2 μg g-1, equivalent to three times the standard error of the estimate (sy/x) of the regression line. For both infant formulas and milk samples, due to their very low boron content, we used a procedure based on preconcentration by solid phase extraction (Amberlite IRA 743), followed by elution with 2 mol L-1 hydrochloric acid. Detection limits were 0.03 μg g-1 for 4% m/v honey, 0.04 μg g-1 for 5% m/v infant formula and 0.08 μg mL-1 for 15% v/v cow milk. We confirmed the accuracy of the procedure by comparing the obtained results with those found via a comparable independent procedure, as well by the analysis of four certified reference materials

  6. Selenium determination in biological material by atomic absorption spectrophotometry in graphite furnace and using vapor generation

    The applicability of the atomic absorption spectrophotometry to the determination of selenium in biological material using vapor generation and electrothermal atomization in the graphite furnace was investigated. Instrumental parameters and the analytical conditions of the methods were studied. Decomposition methods for the samples were tested, and the combustion in the Wickbold apparatus was chosen. (author)

  7. Determination of atmospheric corrosion of coated steel surfaces by in situ infrared reflection absorption spectroscopy (IRRAS)

    Full text: Infrared reflection absorption spectroscopy (IRRAS) is a sensitive technique for measuring thin layers on metallic surfaces. The principal goal of this IRRAS study was the development of a reproducible and reliable in situ measurement procedure for the determination of corrosion of coated steel surfaces. (author)

  8. Quantitative determination of impurities in nuclear grade aluminum by Flame-Atomic Absorption Spectrometry

    The paper deals with quantitative determination of impurity elements in nuclear grade aluminum, used as fin tubes in research reactors, by Flame-Atomic Absorption Spectrometry (F-AAS). The results have been compared with those obtained by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) method. Experimental conditions used in both the methods are given in the paper. (author)

  9. Direct microcomputer controlled determination of zinc in human serum by flow injection atomic absorption spectrometry

    Simonsen, Kirsten Wiese; Nielsen, Bent; Jensen, Arne;

    1986-01-01

    A procedure is described for the direct determination of zinc in human serum by fully automated, microcomputer controlled flow injection atomic absorption spectrometry (Fl-AAS). The Fl system is pumpless, using the negative pressure created by the nebuliser. It only consists of a three-way valve...

  10. Chemical modifiers in electrothermal atomic absorption determination of Platinum and Palladium containing preparations in blood serum

    Аntonina Alemasova

    2012-11-01

    Full Text Available The biological liquids matrixes influence on the characteristic masses and repeatability of Pt and Pd electrothermal atomic absorption spectroscopy (ETAAS determination was studied. The chemical modifiers dimethylglyoxime and ascorbic acid for matrix interferences elimination and ETAAS results repeatability improvement were proposed while bioliquids ETAAS analysis, and their action mechanism was discussed.

  11. 运用HPLC-MS对鸦胆子油自微乳给药系统肠吸收的研究%High-performance Liquid Chromatography Coupled with Mass Spectrometric Method for the Intestinal Absorption Study of Brucea Javanica Oil SMEDDS

    陈瑾瑾; 张懿; 王睿锐; 李盈; 沈琦; 马依然

    2012-01-01

    Objective: To develop a rapid, sensitive and selective high-performance liquid chromatography coupled with mass spectrometric method (HPLC-MS) for detection oleic acid and linoleic acid. Methods: The chromatographic separation was achieved on C18 column at 35℃, with a mobile phase consisting of methanol-distilled water (95:5, v/v) at a flow rate of 0.4 mL/min. An in-vitro diffusion chamber system across isolated rat intestinal membranes was chosen as a model. A self-microemulsifying drug delivery system was used to enhance the intestinal absorption of bruces javanica oil. Results: Oleic acid and linoleic acid were separated with retention times of 10.46 ± 0.02 and 8.55 ± 0.01 min, respectively. A good linear relationship for oleic acid and linoleic acid were in the range of 0.50~50.0 ng/mL(oleic acid) and 5.06~101.2 ng/mL(linoleic acid) , respectively. The mean absolute recoveries of oleic acid and linoleic acid determined in middle concentrations were 97.49± 3.11 % and 105.76± 3.13 % respectively. The coefficients of variation for inter-day and intra-day assay were less than 5 %. The absorption of oleic acid and linoleic acid in bruces javanica oil were 2.8-fold and 4.1-fold enhancement in the presence of the self-microemulsifying drug delivery system respectively, compared with brucea javanica oil alone. Conclusion: HPLC-MS method will be of great utility in routine quality control procedure for the determination of oleic acid and linoleic acid in absorption experiments.%目的:建立高效液相色谱-串联质谱法检测油酸和亚油酸含量的方法,从而对鸦胆子油自微乳给药系统中鸦胆子油的肠吸收进行研究.方法:以甲醇-水(95∶5 v/v)为流动相,流速为0.4 mL/min,柱温为35℃作为高效液相色谱的检测条件.利用大鼠小肠膜建立体外药物扩散体系研究鸦胆子油的肠吸收特性.结果:油酸和亚油酸的保留时间分别为10.46± 0.02和8.55±0.01 min,线性范围分别为0.50~50.0 ng

  12. Determination of the Neutron Flux in the Reactor Zones with the Strong Neutron Absorption and Leakage

    The procedures for the numerical and experimental determination of the neutron flux in the zones with the strong neutron absorption and leakage are described in this paper. Numerical procedure is based on the application of the SCALE-4.4a code system where the Dancoff factors are determined by the VEGA2DAN code. Two main parts of the experimental methodology are measurement of the activity of irradiated foils and determination of the averaged neutron absorption cross-section in the foils by the SCALE-4.4a calculation procedure. The proposed procedures have been applied for the determination of the neutron flux in the internal neutron converter used with the RB reactor core configuration number 114. (author)

  13. Determination of iodine in seaweed and table salt by an indirect atomic absorption method

    Decomposition methods based on fusion with alkali are discussed, with respect to the determination of iodine in biological material. It is shown that sodium hydroxide can be used for the decomposition of seaweed without loss of iodine. In spite of the oxidizing conditions, the iodine will be present as iodide in the final ash. The iodide can be determined by an indirect atomic-absorption method, based on the reaction between iodide and mercury(II), with determination of mercury by cold vapour atomic-absorption spectrometry. The basis of the method is discussed, and it is shown that the use of tin(II) as reductant is essential. The effect of the oxidation state of the iodine on the sensitivity of the method is pointed out. High concentrations of chloride interfere, but it is still possible to determine iodide in iodinated table salt. (author)

  14. Atomic absorption determination of platinum and rhenium in deactivated catalysts based on γ-alumina

    A flame atomic absorption method has been developed for the determination of Pt and Re in deactivated catalysts based on γ-Al2O3. Hydrofluoric acid is used for catalyst dissolution. The lower determination limits are 1 μg/ml for Pt and 5 μg/ml for Re, RSD are 0.01-0.15 and 0.03-0.25 respectively

  15. Atomic Absorption and Spectrophotometeric Determinations of Salicylhydroxamic Acid in Its Pure and Pharmaceutical Dosage Forms

    SALEM, Alaa-Eldin AbdelAziz

    2003-01-01

    A new method for the indirect determination of salicylhydroxamic acid (SHAM) using atomic absorption spectrometry (AAS) was proposed. The method is based on precipitating the ion associate complex of SHAM with [Cu (NH3)4]2+. The excess, unreacted, Cu2+ ions were determined using AAS. Another spectrophotometric method based on measuring the absorbance of the formed [Cu (NH3)4]-SHAM complex in dioxane was proposed. The green color of the complex formed was measured at 330 nm. The two...

  16. Evaluation of a method for the determination of chromium in urine by atomic absorption spectrometry

    A method for the determination of chromium in urine by atomic absorption spectrometry, using electrothermic atomization with pyrolytic graphite tubes, is proposed. The determinations are performed by standard addition. The method is applicable to biologic monitoring of populations with different degrees of exposition. It is also used in the analysis of chromium in sediments. Results of chromium in urine of a population group non-exposed to the metal are presented. 11 refs

  17. Determination of vanadium in food and traditional Chinese medicine by graphite furnace atomic absorption spectroscopy

    2003-01-01

    Various experimental conditions were described for the vanadium determination by graphite furnace atomic ab-sorption spectroscopy (GFAAS). The experiments showed that when atomization took place under the conditions where thecombination of a pyrolytic coating graphite tube and fast raising temperature were used and the temperature was stable, thesignal peak shapes could be improved, the sensitivity was enhanced, and the memory effect was removed. The vanadium infood and traditional Chinese medicinal herbs can be accurately determined using the standard curve method.

  18. The determination of major and some minor constituents in lead zirconate-titanate compositions by x-ray fluorescence and atomic absorption spectrometry

    Willigen, van J.H.H.G.; Kruidhof, H.; Dahmen, E.A.M.F.

    1972-01-01

    An accurate X-ray fluorescence spectrometric method is described for the determination of lead, zirconium and titanium in lead zirconate-titanate ceramics. Careful matching of samples and standards by a borax fusion method resulted in a relative standard deviation of about 0.2% for the major constit

  19. Development of a coupled-column liquid chromatographic-tandem mass spectrometric method for the direct determination of betamethasone in urine.

    Polettini, A; Marrubini Bouland, G; Montagna, M

    1998-08-25

    Different hyphenated liquid chromatographic (LC) and mass spectrometric (MS) techniques were investigated in order to set-up a method for the fast, direct analysis of betamethasone in hydrolysed and non-hydrolysed urine using large-volume sample injection. After the optimisation of the LC parameters using a traditional UV detector and of the thermospray and mass spectrometric parameters by flow injection, urine samples (0.5 ml) were submitted to analysis by either LC combined with tandem mass spectrometry (MS-MS), coupled-column LC (LC-LC) combined with single quadrupole MS, and LC-LC-MS-MS. Both the three-step configurations (LC-MS-MS and LC-LC-MS) did not provide satisfactory results: loss of sensitivity was noted in the case of LC-MS-MS (likely due to reduced efficiency in the ionisation of betamethasone in the thermospray owing to the presence of large amounts of matrix interference), while in the case of LC-LC-MS a high chemical noise resulting in insufficient selectivity of detection was observed. On the contrary, LC-LC-MS-MS analysis proved to meet the demand of high speed of analysis (sample throughput, 4.5 h(-1)), selectivity, and sensitivity (LOQ, 1 ng/ml; LOD, 0.2 ng/ml). Notwithstanding the complex analytical system adopted, the developed procedure was manageable and very robust, provided that at the beginning of each analytical session the performance of the system was controlled by checking the retention time of the analytes on the first analytical column with UV detection and by optimising vaporiser temperature of the thermospray by flow injection. PMID:9746249

  20. Determination of cadmium as pollutant in tobaccos using atomic absorption analysis

    Atomic absorption spectroscopy has been used for the determination of cadmium in non-aqueous media. It was found that the determination of cadmium in methanol is more accurate and more precise. In this case a concentration of 0.1 ppm was accurately determined with a relative deviation not exceeding 3.2%. Using this technique, the amount of cadmium in Syrian as well as in imported tobacco was determined and found to be in the range 0.64-1.11 ppm. It was also established that the cadmium concentration in imported tobacco is higher than that in Syrian tobacco. (author)

  1. Development and validation of a supercritical fluid chromatography method for the direct determination of enantiomeric purity of provitamin B5 in cosmetic formulations with mass spectrometric detection.

    Khater, Syame; West, Caroline

    2015-01-01

    A rapid and efficient chiral supercritical fluid chromatography (SFC) method has been developed for the quantitative determination of panthenol enantiomers in cosmetic formulations (cream, lotion, wipe, and exfoliant). Indeed, the pharmacological effect only depends on the D form (Dexpanthenol) thus accurate measurement of its enantiomeric purity in formulated cosmetic products is of interest. The samples were prepared with liquid-liquid extraction followed by solid-phase extraction on Adsorbex amino cartridges. After testing several enantioselective columns in an attempt at reversing the elution order to have the minor enantiomer eluted first, the best separation of enantiomers and internal standard (N-acetyl-L-alanine) was achieved on a 3 μm-amylose-type immobilized polysaccharide chiral stationary phase (Chiralpak IA) in less than 6 min with a simple mobile phase comprising carbon dioxide and 11% methanol pumped at 2.3 mL/min, 25°C and 150 bar backpressure. Supercritical fluid chromatography coupled to both an optical diode-array detector and a user-friendly single-quadrupole mass spectrometer (Waters QDa) equipped with electrospray ionization source has been used. The on-line coupling ensures the technique to be more informative and improves detection sensitivity, as underivatized panthenol has a poor UV absorption. The limit of quantification (LOQ) achieved with single-ion recording was 0.5 μg/mL. The method was validated in terms of linearity, precision and accuracy and satisfactory results were obtained. PMID:25459930

  2. Determination of attenuation properties of some petroleum products in Ghana by gamma ray absorption technique

    The mass attenuation coefficient (µ/ ρ) and the mass energy absorption coefficient (µen⁄ρ) are important parameters to characterise the penetration and the interaction of gamma rays in chemical materials such as hydrocarbons. Accurate determination of values of (µ/ ρ) and (µen⁄ρ) are relevant in estimating certain important physical properties of petroleum products. In this study, gamma – ray absorption technique has been used to determine mass attenuation coefficients and mass energy absorption coefficients of the following petroleum products; Kerosene, Aviation Turbine Kerosene, Gasoline (Petrol) and Gasoil (Diesel). Gamma photon energy of 662 keV from a 30 mCi (137Cs) source was utilised together with NaI (Tl) Scintillation detector and Ludlum ratemeter (Gamma Counter). The Theoretical values of mass attenuation coefficient and the mass energy absorption coefficient of each petroleum products was calculated. Experimental results were compared with theoretical ones showing a good correlation between methods. These attenuation properties can be used to determine some physical parameters of petroleum products such as density and hence check adulterations in petroleum products. The experimental values of (µ/ ρ) of the petroleum samples range from 0. 0855 to 0.0911 (cm2/g), the theoretical values of (µ/ ρ) were between 0.0916 and 0.0932(cm2/g) with error deviation from 3% to 7%. The experimental and theoretical mass energy absorption coefficients (µen⁄ρ) recorded were in the range of 0.0330 to 0.0352(cm2/g) and 0.0336 to 0.0342 (cm2/g) respectively, having an error deviation between 1% and 3%. (au)

  3. The determination, by atomic-absorption spectrophotometry, of trace elements in sulphide concentrates

    The separation, concentration, and determination of trace elements in base-metal and sulphide concentrates are described. After the sample has been dissolved, the trace elements that form insoluble hydroxides are precipitated with lanthanum as the coprecipitant and are separated from those elements that form soluble amines with ammonia. The precipitate is dissolved, and the trace elements selenium, tellurium, arsenic, antimony, bismuth, tin, vanadium, chromium, manganese, and aluminium are determined by atomic-absorption spectrophotometry. Coefficients of variation between 1 and 10 per cent, depending on the amount of the element, were obtained, with limits of determination ranging from 0,1 to 50 p.p.m

  4. Determination of heavy metals in solid emission and immission samples using atomic absorption spectroscopy

    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. Spectral Absorption By Particulate Impurities in Snow Determined By Photometric Analysis Of Filters

    Grenfell, T. C.; Doherty, S. J.; Clarke, A. D.

    2009-12-01

    Our work is motivated by the 1983-84 survey by Clarke and Noone (Atmos. Environ., 1985) of soot in Arctic snow. Our objective is to resurvey the original area they covered and to extend the observations around the entire Arctic Basin under the auspices of the IPY program. We use the filtering and integrating sandwich techniques developed by Clarke and Noone to process the snow samples. Among the advantages of this method are that (a) it provides a direct measure of light absorption and the result is closely related to the actual absorption of sunlight in the snow or ice, (b) processing and filtering of the snow samples can be carried out in remote locations and (c) it is not necessary to transport large quantities of snow back to our home laboratory. Here we describe the construction, calibration, and some applications of an integrating sphere spectrophotometer system designed to take advantage of recent advances in instrumentation to improve the accuracy of measurements of absorption by particulate impurities collected on nuclepore filters used in our survey. Filter loading in terms of effective black carbon (BC) amount is determined together with the ratio of non-BC to BC concentrations using a set of reference filters with known loadings of Monarch 71 BC prepared by A. D. Clarke. The new spectrophotometer system has (a) system stability of approximately 0.5%; (b) precision relative to ADC standards of 3-4% for filter loadings greater than about 0.5 microgm Carbon/cm2. (c) We can distinguish BC from non-BC from relative spectral shapes of the energy absorption curves with an accuracy that depends on our knowledge of the spectral absorption curves of the non-BC components; and (d) by-eye estimates are consistent with spectrophotometric results. The major outstanding uncertainty is the appropriate value to use for the mass absorption efficiency for BC.

  6. Optimization of trace molybdenum content determination in human nails by graphite furnace atomic absorption spectrometry

    The accurate determination of molybdenum (Mo) in biological materials is of considerable importance in medical science because of the essential role played by this element in human metabolism. Molybdenum is a component of enzymes responsible for the initial stages of nitrogen, carbon and sulfur metabolism of plants, animals and humans. This element is usually determined by neutron activation analysis (NAA) in variety of samples, but direct measurement of low levels of molybdenum in biological samples by NAA is difficult. Recently instrumental analysis procedures such as atomic absorption spectrometry (AAS) have been used in clinical measurements for determination of many trace elements in the biological samples. These techniques are much simpler and cheaper than NAA. In this paper we are reporting a method of sample preparation for determining molybdenum by using graphite furnace atomic absorption spectrometry (GF-AAS). This method is the most readily available technique for determination of molybdenum at the ng/g level in biological samples. It can be used for the routine hospital laboratory determination of molybdenum and has appropriate sensitivity and simplicity. The best and reliable results for molybdenum analysis was achieved by digestion of nails in HNO3 2 N and was determined in the range from 0.11 to 5.10 μg/g

  7. A novel solidified floating organic drop microextraction method for preconcentration and determination of copper ions by flow injection flame atomic absorption spectrometry.

    Sahin, Ciğdem Arpa; Tokgöz, Ilknur

    2010-05-14

    A rapid, simple and cost effective solidified floating organic drop microextraction (SFODME) and flow injection flame atomic absorption spectrometric determination (FI-FAAS) method for copper was developed. In this method, a free microdrop of 1-undecanol containing 1,5-diphenyl carbazide (DPC) as the complexing agent was transferred to the surface of an aqueous sample including Cu(II) ions, while being agitated by a stirring bar in the bulk of the solution. Under the proper stirring conditions, the suspended microdrop can remain at the top-center position of the aqueous sample. After the completion of the extraction, the sample vial was cooled by placing it in a refrigerator for 10min. The solidified microdrop was then transferred into a conical vial, where it melted immediately and diluted to 300microL with ethanol. Finally, copper ions in 200microL of diluted solution were determined by FI-FAAS. Several factors affecting the microextraction efficiency, such as type of extraction solvent, pH, complexing agent concentration, extraction time, stirring rate, sample volume and temperature were investigated and optimized. Under optimized conditions for 100mL of solution, the preconcentration factor was 333 and the enrichment factor was 324. The limit of detection (3s) was 0.4ngmL(-1), the limit of quantification (10s) was 1.1ngmL(-1) and the relative standard deviation (RSD) for 10 replicate measurements of 10ngmL(-1) copper was 0.9%. The proposed method was successfully applied to the determination of copper in different water samples. PMID:20441870

  8. A simplified technique to determine the self-absorption correction for sediment samples

    A self-absorption correction factor is required for the determination of the radioactive isotope concentration in sediment samples at the low-energy region. A simplified technique for this correction factor for a well-type HP germanium detector is described. This correction is especially important when the ratio between the sample density and reference sample density (ρsa./ρre) is greater than approximately 1.4

  9. Capturing Absorptive Capacity: Concepts, Determinants, Measurement Modes and Role in Open Innovation

    Lewandowska Małgorzata Stefania

    2015-01-01

    Absorptive capacity (ACAP) enables firm to adjust to a rapidly changing environment and achieve sustained competitive advantage. This study contributes to the existing body of knowledge on ACAP by providing a comprehensive literature review of the various conceptual attributes of the construct, its determinants, outcomes, and positive and negative consequences of using its input-oriented, output-oriented, and perceptive measurement modes. Proposals for constructing ACAP based on the Community...

  10. Atomic-absorption determination of tantalum and niobium in ore concentrates

    A flame atom-absorption method was developed for determining tantalum and niobium at their level greater than 5% in Ta-Nb ore concentrates. Flame was produced by a nitrous oxide-acetylene mixture. The optimal composition of a buffer (3 mg/ml) of iron was determined by the method of factorial planning of the experiment and steep ascention by gradient. The optimizing parameter in factorial planning was obtained from the difference of optical densities of Ta and Nb, by taking the average value for two solutions which had dissimilar total composition and which imitated the real composition of the ore concentrates, i.e., the value of (ΔD/Dsub(av))sub(Ta) or (ΔD/Dsub(av))sub(Nb). The optimization of analytical conditions corresponded to the condition (ΔD/Dsub(av))→ 0, which indicated that the chosen optimizing parameter also facilitated the attainment of maximum D values. The variation coefficient in the determination of Ta and Nb was respectively 0.8 and 1.4%. There was a good agreement between the results obtained in Ta analysis by the atom-absorption and the extraction-gravimetric methods, and in Nb analysis by the atom-absorption, differential spectrophotometric and x-ray fluorescence methods

  11. Determination of sulfur in food by high resolution continuum source flame molecular absorption spectrometry

    Zambrzycka, Elżbieta; Godlewska-Żyłkiewicz, Beata

    2014-11-01

    In the present work, a fast, simple and sensitive analytical method for determination of sulfur in food and beverages by high resolution continuum source flame molecular absorption spectrometry was developed. The determination was performed via molecular absorption of carbon monosulfide, CS. Different CS rotational lines (257.959 nm, 258.033 nm, 258.055 nm), number of pixels and types of standard solution of sulfur, namely: sulfuric acid, sodium sulfate, ammonium sulfate, sodium sulfite, sodium sulfide, DL-cysteine, and L-cystine, were studied in terms of sensitivity, repeatability of results as well as limit of detection and limit of quantification. The best results were obtained for measurements of absorption of the CS molecule at 258.055 nm at the wavelength range covering 3 pixels and DL-cysteine in 0.2 mol L- 1 HNO3 solution as a calibration standard. Under optimized conditions the limit of detection and the limit of quantification achieved for sulfur were 10.9 mg L- 1 and 36.4 mg L- 1, respectively. The repeatability of the results expressed as relative standard deviation was typically determination of sulfur in milk (194 ± 10 mg kg- 1), egg white (2188 ± 29 mg kg- 1), mineral water (31.0 ± 0.9 mg L- 1), white wine (260 ± 4 mg L- 1) and red wine (82 ± 2 mg L- 1), as well as in sample rich in ions, such as bitter mineral water (6900 ± 100 mg L- 1).

  12. Determination of serum lithium: comparison between atomic emission and absorption spectrometry methods

    Carlos Elielton do Espírito Santo

    2014-02-01

    Full Text Available Introduction: The therapeutic monitoring of lithium, through concentration measurements, is important for individual dose adjustment, as a marker of treatment adherence and to prevent poisoning and side effects. Objectives: Validate and compare two methods - atomic emission and atomic absorption - for the determination of lithium in serum samples. Methodology: Parameters such as specificity, precision, accuracy, limit of detection (LOD and linearity were considered. The atomic absorption spectrometer was used, operating in either emission or absorption mode. For the quantitative comparison of 30 serum samples from patients with mood disorder treated with lithium, the results were submitted to Student's t-test, F-test and Pearson's correlation. Results: The limit of quantification (LOQ was established as 0.05 mEq/l of lithium, and calibration curves were constructed in the range of 0.05-2 mEq/l of lithium, using aqueous standards. Sample preparation time was reduced, what is important in medical laboratory. Conclusion: Both methods were considered satisfactory, precise and accurate and can be adopted for lithium quantification. In the comparison of quantitative results in lithium-treated patients through statistical tests, no significant differences were observed. Therefore the methods for lithium quantification by flame atomic absorption spectrometry (FAAS and flame atomic emission spectrometry (FAES may be considered similar.

  13. [Determination of the content of sulfur of coal by the infrared absorption method with high acccuracy].

    Wang, Hai-Feng; Lu, Hai; Li, Jia; Sun, Guo-Hua; Wang, Jun; Dai, Xin-Hua

    2014-02-01

    The present paper reported the differential scanning calorimetry-thermogravimetry curves and the infrared (IR) absorption spectrometry under the temperature program analyzed by the combined simultaneous thermal analysis-IR spectrometer. The gas products of coal were identified by the IR spectrometry. This paper emphasized on the combustion at high temperature-IR absorption method, a convenient and accurate method, which measures the content of sulfur in coal indirectly through the determination of the content of sulfur dioxide in the mixed gas products by IR absorption. It was demonstrated, when the instrument was calibrated by varied pure compounds containing sulfur and certified reference materials (CRMs) for coal, that there was a large deviation in the measured sulfur contents. It indicates that the difference in chemical speciations of sulfur between CRMs and the analyte results in a systematic error. The time-IR absorption curve was utilized to analyze the composition of sulfur at low temperatures and high temperatures and then the sulfur content of coal sample was determined by using a CRM for coal with a close composition of sulfur. Therefore, the systematic error due to the difference in chemical speciations of sulfur between the CRM and analyte was eliminated. On the other hand, in this combustion at high temperature-IR absorption method, the mass of CRM and analyte were adjusted to assure the sulfur mass equal and then the CRM and the analyte were measured alternately. This single-point calibration method reduced the effect of the drift of the IR detector and improved the repeatability of results, compared with the conventional multi-point calibration method using the calibration curves of signal intensity vs sulfur mass. The sulfur content results and their standard deviations of an anthracite coal and a bituminous coal with a low sulfur content determined by this modified method were 0.345% (0.004%) and 0.372% (0.008%), respectively. The uncertainty (U

  14. Determination of trace amounts of praseodymium by third-derivative molecular absorption spectrophotometry

    A third-derivative molecular absorption spectrophotometric procedure is described for the determination of trace amounts of praseodymium (Pr). The procedure is based on the reaction of praseodymium with Bromopyrogallol Red (BPR) in acetate-buffered medium. The influence of various instrumental parameters and reaction conditions on the colour development of the BPR-Pr complex has been investigated. The proposed method is free of interference from up to 100-fold amounts of other rare earth elements (except yttrium, lanthanum and neodymium). In conjunction with ion-exchange separation, the proposed method has been applied to the determination of praseodymium in aluminium metal samples. (author)

  15. Determination of Ca, Cu, Fe and Pb in sugarcane raw spirits by atomic absorption spectrophotometry

    The determination of Ca, Cu, Fe and Pb in sugarcane raw spirits by atomic absorption spectrophotometry was carried out. For 20 μL injected sample, calibration within the 0,5-25,0 mg. L-1 Ca; 0,25-5,0 mg. L-1 Cu, Pb and Cu intervals were established using the ratios Cu, Ca, Fe and Pb absorbance versus analyte concentration, respectively. Typical linear correlations of r = 0,999 were obtained. The proposed method was applied for the direct determination of Ca, Cu, Fe and Pb in sugar cane spirits, and in samples. The results obtained were in accordance to those obtained at 95% confidence level

  16. Determination of the coefficient of iodine absorption carbon materials adsorber ventilation NPP using stable isotopes

    Submitted by nuclear-physical methods of determining the coefficient of absorption of iodine carbon materials using stable isotopes of iodine. Designed and created by pumping and measuring iodine content units. The processes of dynamic sorption of iodine on industrial carbon adsorbents studied the possibility of determining the iodine content of nuclear-physical methods and presents the metrological characteristics x-ray method. Application methods allow for the certification of carbon adsorbents gas cleaning systems and improve the safety of nuclear power plant operation

  17. A method for determination of the absorption and scattering properties interstitially in turbid media

    Dimofte, Andreea; Finlay, Jarod C.; Zhu, Timothy C.

    2005-01-01

    We have developed a method to quickly determine tissue optical properties (absorption coefficient μa and transport scattering coefficient μs′) by measuring the ratio of light fluence rate to source power along a linear channel at a fixed distance (5 mm) from an isotropic point source. Diffuse light is collected by an isotropic detector whose position is determined by a computer-controlled step motor, with a positioning accuracy of better than 0.1 mm. The system automatically records and plots...

  18. Determination of lead traces in water and liqueurs by derivative atom trapping flame atomic absorption spectrometry

    Sun, H. [Department of Chemistry, Hebei University, Baoding, 071002 (China); Yang Lili [Department of Chemistry, Hebei University, Baoding, 071002 (China); Zhang Deqiang [Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P.O. Box 2871, Beijing (China); Wang Weixiao [Department of Chemistry, Hebei University, Baoding, 071002 (China); Sun Jianmin [Department of Chemistry, Hebei University, Baoding, 071002 (China)

    1997-07-01

    A new method for the direct determination of lead traces using derivative atom trapping flame atomic absorption spectrometry (DAT-FAAS) with an improved water-cooled stainless steel trapping equipment in an air-acetylene flame was investigated. The optimum conditions concerning the sensitivity were studied. For a 1 min collection, the characteristic concentration (given as derivative absorbance of 0.0044) and the detection limit (3s) were 1.4 ng/mL and 0.27 ng/mL, respectively. This is 361 and 74-fold better than those of the conventional flame atomic absorption spectrometry (FAAS) and comparable to those of graphite furnace atomic absorption spectrometry (GFAAS). The detection limit and sensitivity of DAT-FAAS for a 3 min collection time were 2 and 3 orders of magnitude higher than those of conventional FAAS. The present method was applied to the determination of lead in water and liqueur samples with a recovery range of 94-108% and a relative standard deviation of 3.5-5.6%. (orig.). With 5 figs., 5 tabs.

  19. Standard addition/absorption detection microfluidic system for salt error-free nitrite determination.

    Ahn, Jae-Hoon; Jo, Kyoung Ho; Hahn, Jong Hoon

    2015-07-30

    A continuous-flow microfluidic chip-based standard addition/absorption detection system has been developed for accurate determination of nitrite in water of varying salinity. The absorption detection of nitrite is made via color development using the Griess reaction. We have found the yield of the reaction is significantly affected by salinity (e.g., -12% error for 30‰ NaCl, 50.0 μg L(-1)N-NO2(-) solution). The microchip has been designed to perform standard addition, color development, and absorbance detection in sequence. To effectively block stray light, the microchip made from black poly(dimethylsiloxane) is placed on the top of a compact housing that accommodates a light-emitting diode, a photomultiplier tube, and an interference filter, where the light source and the detector are optically isolated. An 80-mm liquid-core waveguide mounted on the chip externally has been employed as the absorption detection flow cell. These designs for optics secure a wide linear response range (up to 500 μg L(-1)N-NO2(-)) and a low detection limit (0.12 μg L(-1)N-NO2(-) = 8.6 nM N-NO2(-), S/N = 3). From determination of nitrite in standard samples and real samples collected from an estuary, it has been demonstrated that our microfluidic system is highly accurate (<1% RSD, n = 3) and precise (<1% RSD, n = 3). PMID:26320643

  20. Measurement of gamma attenuation coefficients in UO2 and zirconium for self-absorption corrections of burn-up determination

    UO2 pellets from ALUOX fuel elements were used in measuring the absorption coefficient of gamma radiation in UO2. The results of measurements of the energy dependence of the linear absorption coefficient (within 622 to 796 keV) and of the dependence on pellet density showed that in the given density interval the absorption coefficient was almost constant. The density interval was chosen to be typical for pellet fuel used in water cooled and water moderated power reactors. The results are also shown of the dependence of the mass absorption coefficient of gamma radiation in Zr on radiation energy and compared with the mass absorption coefficient of Mo; these also showed the independence of the absorption coefficient on density. The linear and mass absorption coefficients of UO2 are considerably high and correspond approximately to the absorption coefficient of lead. For the measured energy range the variation of absorption coefficient is about 40%, which causes errors in burnup determination. The efficiency was also determined of Ge(Li) detectors for the energy range 0.5 to 1.2 MeV. The determination of the above coefficients was used for improving the gamma fuel scanning technique in determining the activity and burnup of spent fuel elements. (J.P.)

  1. Determination of total lead in 400 lipsticks on the U.S. market using a validated microwave-assisted digestion, inductively coupled plasma-mass spectrometric method.

    Hepp, Nancy M

    2012-01-01

    In 2009, the U.S. Food and Drug Administration (FDA) published lead (Pb) content results from a small survey of 20 tube lipsticks with red shades using a validated inductively coupled plasma-mass spectrometric (ICP-MS) method developed by FDA chemists. The study was prompted by a media report suggesting that potential exposure to lead from lipsticks under conditions of ordinary use might be harmful. The FDA has since investigated the lead content of tube lipsticks by conducting an expanded survey that included a variety of shades and manufacturers, at varying prices. The purposes of the expanded survey were to ascertain the levels of lead in lipsticks sold on the U.S. market, to identify any categories of lipstick with elevated levels of lead, and to compare the results to those from the initial small survey. Four hundred lipsticks available on the U.S. market in the spring of 2010 were tested for total lead content using the FDA's validated method. The analyses were performed by a private laboratory contracted by the FDA. The maximum lead level found was 7.19 mg Pb/kg. Thirteen of the 400 lipsticks were found to contain levels greater than 3.06 mg Pb/kg, the highest amount found in the initial survey. The average lead concentration found in the expanded survey was 1.11 mg Pb/kg, which was very close to the average of 1.07 mg Pb/kg found in the initial survey. Some statistically significant associations between lead level and parent company were found. The contract requirements, testing procedures, and findings from the expanded survey are described here. PMID:23193690

  2. Photoelectron and UV absorption spectroscopy for determination of electronic configurations of negative molecular ions: Chlorophenols

    Tseplin, E.E. [Institute of Molecular and Crystal Physics, Ufa Research Centre, Russian Academy of Sciences, October Prospect 151, Ufa 450075 (Russian Federation)], E-mail: tzeplin@mail.ru; Tseplina, S.N.; Tuimedov, G.M.; Khvostenko, O.G. [Institute of Molecular and Crystal Physics, Ufa Research Centre, Russian Academy of Sciences, October Prospect 151, Ufa 450075 (Russian Federation)

    2009-04-15

    The photoelectron and UV absorption spectra of p-, m-, and o-chlorophenols in the gas phase have been obtained. On the basis of DFT B3LYP/6-311++G(d, p) calculations, the photoelectron bands have been assigned to occupied molecular orbitals. From the TDDFT B3LYP/6-311++G(d, p) calculation results, the UV absorption bands have been assigned to excited singlet states of the molecules under investigation. For each excited state a dominant transition was found. It has been shown that the energies of these singlet transitions correlate with the energy differences between the ground-state molecular orbitals participating in them. Using the UV spectra interpretation, the electronic states of molecular anions detected earlier for the same compounds by means of the resonant electron capture mass-spectrometry have been determined.

  3. A model for absorption determination of radioactive materials: application in the radio dosimetry and nutrition study

    A three-parameter model of the sigmoidal relationship is proposed to explain the food passage by intestinal tube. These parameters are: U = intestinal non-absorbed radioactivity; d parameter related to intestinal food dispersion; and t50 = time to maximal appearance of material from the intestinal lumen. In order to illustrate the applications of this model and its validity, the absorption of 65Zn from casein semi-purified diet was evaluated in rats. There was a good agreement between the predicted values and the experimental data when the sigmoidal component was added to the conventional multicompartimental equations. With this kind of model the time to maximal appearance (hours), the true absorption level, the fecal concentration and the intestinal dispersion of the ingested radioactivity material may be determined. (author)

  4. Determination of RW3-to-water mass-energy absorption coefficient ratio for absolute dosimetry

    Full text: The measurement of absorbed dose to water in a d-phantom may require a conversion factor because it may be radiologically equivalent to water. One phantom eloped for the use of dosimetry is a solid water, RW3 te-polystyrene material by lEA. This has a lower mass energy absorption coefficient than water due to high bremsstrahlung yield, which affects the accuracy of absolute dosimetry measurements. In this paper, we demonstrate the calculation of mass-energy absorption coefficient ratios, relative to water, from measurements in plastic water and RW3 1 an Elekta Synergy linear accelerator (6 and 10 MY ton beams) as well as Monte Carlo modeling in BEAMnrc DOSXYZnrc. From this, the solid-phantom-to-water correction factor was determined for plastic water and RW3.

  5. Determination of metallic impurities in raw materials for radioisotope production by atomic absorption spectroscopy

    Atomic absorption spectrometry has been used for the determination of traces of calcium in scandium oxide, copper in zinc, iron in cobalt oxide, manganese In ferric oxide, nickel in copper and zinc in gallium oxide. The influences on the sensitivities arising from the hollow cathode currents, the gas pressures and the acid concentrations have been considered. A study of the interferences from the metallic matrices has also been performed, the interference due to the absorption of the manganese radiation by the atoms of iron being the most outstanding . In order to remove the interfering elements and increase sensitivity, pre-concentration methods have been tested. The addition methods has also been used. (Author) 14 refs

  6. Determination of tetraalkyllead compounds in gasoline by liquid chromatography-atomic absorption spectrometry

    Messman, J.D.; Rains, T.C.

    1981-01-01

    A liquid chromatography-atomic absorption spectrometry (LC-AAS) hybrid analytical technique is presented for metal speciation measurements on complex liquid samples. The versatility and inherent metal selectivity of the technique are Illustrated by the rapid determination of five tetraalkyllead compounds in commercial gasoline. Separation of the individual tetraalkyllead species is achieved by reversed-phase liquid chromatography using an acetonitrile/water mobile phase. The effluent from the liquid Chromatograph Is introduced directly into the aspiration uptake capillary of the nebulizer of an air/acetylene flame atomic absorption spectrometer. Spectral interferences due to coeluting hydrocarbon matrix constituents were not observed at the 283.3-nm resonance line of lead used for analysis. Detection limits of this LC-AAS hydrid analytical technique, based on a 20-??L injection, are approximately 10 ng Pb for each tetraalkyllead compound.

  7. Determination of absorption cross-section of Si nanocrystals by two independent methods based on either absorption or luminescence

    Valenta, J.; Greben, M.; Remeš, Zdeněk; Gutsch, S.; Hiller, D.; Zacharias, M.

    2016-01-01

    Roč. 102, č. 2 (2016), "023102-1"-"023102-5". ISSN 0003-6951 R&D Projects: GA ČR(CZ) GA14-05053S; GA MŠk(CZ) LD14011 Institutional support: RVO:68378271 Keywords : photoluminescence * absorption spectroscopy * photothermal spectroscopy * semiconductors * nanocrystals Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 3.302, year: 2014

  8. Determination of Absorptive Ability to the Heavy Metals in Different Parts of Rhizoma Curcumae Longae%姜黄各药用部位对土壤中重金属的富集能力分析

    周亚文; 刘璐; 何越; 吕瑞

    2015-01-01

    目的:探究植株姜黄对土壤中重金属的吸收富集情况,为植株姜黄的规范化栽培提供依据。方法:采用火焰原子吸收光谱法测定姜黄、黄丝郁金及其栽培土壤中Cu,Pb,Cd三种重金属元素的含量,并评价各部位对重金属元素的富集能力。结果:姜黄各部位对重金属元素的富集能力有一定差异,其中根茎对重金属的富集能力依次是Pbabsorption of heavy metals in soil by plant Curcuma Longa, The aim of the research was to provide basis for non-pollution cultivation of plant Curcumae Longae. Method:The flame atomic absorption spectrometric was applied to determine the heavy metal including Cu, Pb and Cd and the absorptive ability of the heavy metals was evaluated. Results:The quantization result showed that the concentrated coefficient of Rhizoma Curcumae Longae to the Cu, Pb, Cd was varied, in which the order for absorptive ability of Curcumae Longae L. was Pbabsorptive ability to the heavy metals in different part of Rhizoma Curcumae Longae. The result can give some useful information for the GAP cultivation of Rhizoma Curcumae Longae.

  9. 姜黄各药用部位对土壤中重金属的富集能力分析%Determination of Absorptive Ability to the Heavy Metals in Different Parts of Rhizoma Curcumae Longae

    周亚文; 刘璐; 何越; 吕瑞

    2015-01-01

    Objective:Explore the absorption of heavy metals in soil by plant Curcuma Longa, The aim of the research was to provide basis for non-pollution cultivation of plant Curcumae Longae. Method:The flame atomic absorption spectrometric was applied to determine the heavy metal including Cu, Pb and Cd and the absorptive ability of the heavy metals was evaluated. Results:The quantization result showed that the concentrated coefficient of Rhizoma Curcumae Longae to the Cu, Pb, Cd was varied, in which the order for absorptive ability of Curcumae Longae L. was Pbabsorptive ability to the heavy metals in different part of Rhizoma Curcumae Longae. The result can give some useful information for the GAP cultivation of Rhizoma Curcumae Longae.%目的:探究植株姜黄对土壤中重金属的吸收富集情况,为植株姜黄的规范化栽培提供依据。方法:采用火焰原子吸收光谱法测定姜黄、黄丝郁金及其栽培土壤中Cu,Pb,Cd三种重金属元素的含量,并评价各部位对重金属元素的富集能力。结果:姜黄各部位对重金属元素的富集能力有一定差异,其中根茎对重金属的富集能力依次是Pb

  10. Determination of sulfur in food by high resolution continuum source flame molecular absorption spectrometry

    Zambrzycka, Elżbieta; Godlewska-Żyłkiewicz, Beata, E-mail: bgodlew@uwb.edu.pl

    2014-11-01

    In the present work, a fast, simple and sensitive analytical method for determination of sulfur in food and beverages by high resolution continuum source flame molecular absorption spectrometry was developed. The determination was performed via molecular absorption of carbon monosulfide, CS. Different CS rotational lines (257.959 nm, 258.033 nm, 258.055 nm), number of pixels and types of standard solution of sulfur, namely: sulfuric acid, sodium sulfate, ammonium sulfate, sodium sulfite, sodium sulfide, DL-cysteine, and L-cystine, were studied in terms of sensitivity, repeatability of results as well as limit of detection and limit of quantification. The best results were obtained for measurements of absorption of the CS molecule at 258.055 nm at the wavelength range covering 3 pixels and DL-cysteine in 0.2 mol L{sup −1} HNO{sub 3} solution as a calibration standard. Under optimized conditions the limit of detection and the limit of quantification achieved for sulfur were 10.9 mg L{sup −1} and 36.4 mg L{sup −1}, respectively. The repeatability of the results expressed as relative standard deviation was typically < 5%. The accuracy of the method was tested by analysis of digested biological certified reference materials (soya bean flour, corn flour and herbs) and recovery experiment for beverage samples with added known amount of sulfur standard. The recovery of analyte from such samples was in the range of 93–105% with the repeatability in the range of 4.1–5.0%. The developed method was applied for the determination of sulfur in milk (194 ± 10 mg kg{sup −1}), egg white (2188 ± 29 mg kg{sup −1}), mineral water (31.0 ± 0.9 mg L{sup −1}), white wine (260 ± 4 mg L{sup −1}) and red wine (82 ± 2 mg L{sup −1}), as well as in sample rich in ions, such as bitter mineral water (6900 ± 100 mg L{sup −1}). - Highlights: • HR-CS FMAS technique was used for sulfur measurement via molecular absorption of carbon monosulfide, CS. • Organic DL

  11. Determination of sulfur in food by high resolution continuum source flame molecular absorption spectrometry

    In the present work, a fast, simple and sensitive analytical method for determination of sulfur in food and beverages by high resolution continuum source flame molecular absorption spectrometry was developed. The determination was performed via molecular absorption of carbon monosulfide, CS. Different CS rotational lines (257.959 nm, 258.033 nm, 258.055 nm), number of pixels and types of standard solution of sulfur, namely: sulfuric acid, sodium sulfate, ammonium sulfate, sodium sulfite, sodium sulfide, DL-cysteine, and L-cystine, were studied in terms of sensitivity, repeatability of results as well as limit of detection and limit of quantification. The best results were obtained for measurements of absorption of the CS molecule at 258.055 nm at the wavelength range covering 3 pixels and DL-cysteine in 0.2 mol L−1 HNO3 solution as a calibration standard. Under optimized conditions the limit of detection and the limit of quantification achieved for sulfur were 10.9 mg L−1 and 36.4 mg L−1, respectively. The repeatability of the results expressed as relative standard deviation was typically < 5%. The accuracy of the method was tested by analysis of digested biological certified reference materials (soya bean flour, corn flour and herbs) and recovery experiment for beverage samples with added known amount of sulfur standard. The recovery of analyte from such samples was in the range of 93–105% with the repeatability in the range of 4.1–5.0%. The developed method was applied for the determination of sulfur in milk (194 ± 10 mg kg−1), egg white (2188 ± 29 mg kg−1), mineral water (31.0 ± 0.9 mg L−1), white wine (260 ± 4 mg L−1) and red wine (82 ± 2 mg L−1), as well as in sample rich in ions, such as bitter mineral water (6900 ± 100 mg L−1). - Highlights: • HR-CS FMAS technique was used for sulfur measurement via molecular absorption of carbon monosulfide, CS. • Organic DL-cysteine in 0.2 mol L−1 HNO3 solution is proposed as a calibration

  12. Copper(II)-rubeanic acid coprecipitation system for separation-preconcentration of trace metal ions in environmental samples for their flame atomic absorption spectrometric determinations

    A simple and facile preconcentration procedure based on the coprecipitation of trace heavy metal ions with copper(II)-rubeanic acid complex has been developed. The analytical parameters including pH, amounts of rubeanic acid, sample volume, etc. was investigated for the quantitative recoveries of Pb(II), Fe(III), Cd(II), Au(III), Pd(II) and Ni(II). No interferic effects were observed from the concomitant ions. The detection limits for analyte ions by 3 sigma were in the range of 0.14 μg/l for iron-3.4 μg/l for lead. The proposed coprecipitation method was successfully applied to water samples from Palas Lake-Kayseri, soil and sediment samples from Kayseri and Yozgat-Turkey

  13. Determination of the number densities of argon metastables in argon-hydrogen plasma by absorption and self-absorption methods

    Gavare, Z [Institute of Atomic Physics and Spectroscopy, University of Latvia, Skunu str. 4, Riga LV -1050 (Latvia); Goett, D [Institute for Low Temperature Plasma Physics, 17489 Greifswald (Germany); Pipa, A V [Institute for Low Temperature Plasma Physics, 17489 Greifswald (Germany); Roepcke, J [Institute for Low Temperature Plasma Physics, 17489 Greifswald (Germany); Skudra, A [Institute of Atomic Physics and Spectroscopy, University of Latvia, Skunu str. 4, Riga LV -1050 (Latvia)

    2006-08-15

    The number densities of Ar 3s{sup 2}3p{sup 5}4s levels have been measured by means of two methods: a self-absorption method with a mirror behind the discharge vessel and an absorption method with a high-frequency electrodeless discharge lamp. Concentrations ranging from 6 x 10{sup 7}-4 x 10{sup 9} cm{sup -3} were obtained for the Ar 3s{sup 2}3p{sup 5}4s levels, depending on the argon content (10-100% Ar) in Ar/H{sub 2} microwave plasma. The populations of various sublevels of measured resonant and metastable states coincide within the experimental errors. It was observed that values from measurements of both methods are in good agreement.

  14. Pretreatment of oily samples for analysis by flow injection-spectrometric methods.

    Burguera, José Luis; Burguera, Marcela

    2011-01-15

    This review presents a critical discussion of selected reports dealing with the pretreatment methods of oily samples and the determination of their organic and inorganic constituents using flow systems and spectrometric methods. Special emphasis is given to the on-line couplings with detection systems based on UV-visible spectrophotometry and spectrofluorimetry, atomic absorption spectrometry either with flame or electrothermal atomization as well as inductively coupled plasma optical emission spectrometry or inductively coupled plasma-mass spectrometry. Simple dilution with organic solvents, digestion with concentrated acids under thermal heating, microwave or ultrasound radiation and emulsification procedures are mostly used. The empirical preparation of certain organized assemblies like micelles, emulsions and specially microemulsions added to the confusion of some of the terms, demand a brief description of their characteristics, the correct formulation and some of their applications to the manipulation and treatment of oily samples. The analytical capabilities of combining flow manifolds with spectrometric methods for the determination of specific parameters in oily samples apparently have not been sufficiently exploited yet. PMID:21147308

  15. Determination of absorption length of CO2 and high power diode laser radiation for ordinary Portland cement

    Lawrence, Jonathan; Johnston, Emma P.; Li, Lin

    2000-01-01

    The laser beam absorption lengths of CO2 and a high power diode laser (HPDL) radiation for the ordinary Portland cement (OPC) surface of concrete have been determined. By employing Beer-Lambert’s law the absorption lengths for concrete of CO2 and a HPDL radiation were 470±22 μm and 177±15 μm respectively.

  16. Determination of Trace Selenium in Electrolytic Manganese by Graphite Furnace Atomic Absorption Spectrometry

    YAO Jun; ZHOU Fang-qin; MA Cheng-jin; TUO Yong; LIU Jian-ben; WU Zhu-qin; TAN Zhu-zhong

    2003-01-01

    The effects of four types of graphite tube and five matrix modifiers on the determination of selenium by graphite furnace atomic absorption spectrometry were compared.The results show that platform thermolysis coat graphite tube and magnesium nitrate and cobaltco as matrix modifer can get a high sensitivity and a good recovery.The optimized working conditions and interference in the determination were invesigated.This result is consistent with that of XRF.The recovery is from 100.8 % to102.2 %,the relative standard deviation is from 3.47% to 5.56 % (n=9),and the detection limit of selenium is 378 pg (C=44.5μg/g to 97.3μg/g.).The proposed method can be applied to the rapid determination of selenium in electrolytic manganese.

  17. An atomic-absorption method for the determination of gold in large samples of geologic materials

    VanSickle, Gordon H.; Lakin, Hubert William

    1968-01-01

    A laboratory method for the determination of gold in large (100-gram) samples has been developed for use in the study of the gold content of placer deposits and of trace amounts of gold in other geologic materials. In this method the sample is digested with bromine and ethyl ether, the gold is extracted into methyl isobutyl ketone, and the determination is made by atomicabsorption spectrophotometry. The lower limit of detection is 0.005 part per million in the sample. The few data obtained so far by this method agree favorably with those obtained by assay and by other atomic-absorption methods. About 25 determinations can be made per man-day.

  18. Preconcentration of Vanadium(Ⅴ) on Crosslinked Chitosan and Determination by Graphite Furnace Atomic Absorption Spectrometry

    2002-01-01

    A new method is proposed for the preconcentration of vanadium(Ⅴ) with crosslinked chitosan (CCTS) and determination by graphite furnace atomic absorption spectrometry (GFAAS). The adsorption rate of vanadium(Ⅴ) by CCTS was 97% at pH 4.0, and vanadium(Ⅴ) was eluted from crosslinked chitosan with 2 mL 2.0 mol*L-1 chlorhydric acid and determined by GFAAS. The detection limit (3σ,n=7) for vanadium(Ⅴ) was 4.8×1 0-12g and the relative standard deviation (R.S.D) at concentration level of 2.6 μg*L-1 is less than 3.6%. The method shows a good selectivity and high sensitivity, and it was applied to determination of vanadium(Ⅴ) in oyster and water samples. The analytic recoveries are (97±5)%.

  19. Impurities determination of uranium metal flame spectrophotometry and atomic absorption spectrophotometry

    The atomic absorption flame spectrophotometry has been applied to the determination of chromium, copper, iron, lead, manganese and nickel in the metal of uranium. The first step to be done is to dissolve the uranium sample in nitric acid and then the uranium is extracted by a tributylphosphate-carbon tetrachloride solution. The aqueous phase which contains the chromium, copper, iron, lead, manganese and nickel is aspirated into an airacetylene flame. The results of this method are compared with the results of emission spectrographic method. It is found that this technique is competative to other methods in the sense that it is quite fast and accurate. (author)

  20. Direct determination of sodium and potassium in blood serum by flow injection and atomic absorption spectrophotometry

    A simple and reliable method for the measurement of sodium and potassium in blood serum without any sample dilution by using flow injection and atomic absorption spectrophotometry is described. A sample throughout of 100 measurements per hour is possible. The coefficient of variation for within-run determination was about 1,14 and 2,36% for sodium and potassium, respectively, in serum samples (n=10). The method is easily adaptable to pediatric research, because of the low required sample volume of 5ul. (Author)

  1. Exploiting flow Injection and sequential injection schemes for trace metal determinations by electrothermal atomic absorption spectrometry

    Hansen, Elo Harald

    Determination of low or trace-level amounts of metals by electrothermal atomic absorption spectrometry (ETAAS) often requires the use of suitable preconcentration and/or separation procedures in order to attain the necessary sensitivity and selectivity. Such schemes are advantageously executed in...... compensated by superior performance and versatility. In fact, two approaches are conceivable: The analyte-loaded ion-exchange beads might either be transported directly into the graphite tube where they are pyrolized and the measurand is atomized and quantified; or the loaded beads can be eluted and the...

  2. Determination of Scattering and Absorption Coefficients for Plasma-Sprayed Yttria-Stabilized Zirconia Thermal Barrier Coatings at Elevated Temperatures

    Eldridge, Jeffrey I.; Spuckler, Charles M.; Markham, James R.

    2009-01-01

    The temperature dependence of the scattering and absorption coefficients for a set of freestanding plasma-sprayed 8 wt% yttria-stabilized zirconia (8YSZ) thermal barrier coatings (TBCs) was determined at temperatures up to 1360 C in a wavelength range from 1.2 micrometers up to the 8YSZ absorption edge. The scattering and absorption coefficients were determined by fitting the directional-hemispherical reflectance and transmittance values calculated by a four-flux Kubelka Munk method to the experimentally measured hemispherical-directional reflectance and transmittance values obtained for five 8YSZ thicknesses. The scattering coefficient exhibited a continuous decrease with increasing wavelength and showed no significant temperature dependence. The scattering is primarily attributed to the relatively temperature-insensitive refractive index mismatch between the 8YSZ and its internal voids. The absorption coefficient was very low (less than 1 per centimeter) at wavelengths between 2 micrometers and the absorption edge and showed a definite temperature dependence that consisted of a shift of the absorption edge to shorter wavelengths and an increase in the weak absorption below the absorption edge with increasing temperature. The shift in the absorption edge with temperature is attributed to strongly temperature-dependent multiphonon absorption. While TBC hemispherical transmittance beyond the absorption edge can be predicted by a simple exponential decrease with thickness, below the absorption edge, typical TBC thicknesses are well below the thickness range where a simple exponential decrease in hemispherical transmittance with TBC thickness is expected. [Correction added after online publication August 11, 2009: "edge to a shorter wavelengths" has been updated as edge to shorter wavelengths."

  3. Method 200.12 - Determination of Trace Elements in Marine Waters by StabilizedTemperature Graphite Furnace Atomic Absorption

    This method provides procedures for the determination of total recoverable elements by graphite furnace atomic absorption (GFAA) in marine waters, including estuarine, ocean and brines with salinities of up to 35 ppt.

  4. Determination of lithium in coloured alcoholic beverages by atomic absorption spectrometry

    Complete text of publication follows. Lithium was first found in ashes from wine in 1878, and its presence was later confirmed by spectroscopy, but its determination in wine and beverages is not well documented, unlike the extensive research reported on other metals. Several methods can be implemented for determination of lithium, involving the use of atomic spectroscopy techniques. This paper reports on an analytical optimization to determine lithium by atomic absorption spectrometry (AAS). Good results in reproducibility, accuracy and precision were obtained. No significant interference was found. The method was applied for determination of lithium in six rum samples, eight brandy samples, four vermouth samples, eight whisky samples and two bourbon samples. The value of lithium content in samples ranges from 0,33 to 1,48 μg/ml. Recovery experiments were carried out in order to evaluate the accuracy of the method in samples determination. The values obtained ranges from 95,71% to 98%. The precision of the method in that samples determination was evaluated through variation coefficients. The values obtained ranges from 7,2% to 2,5%. The results have been statistically compared with those obtained using the Inductively Coupled Plasma Atomic Emission Spectrometry (ICP/AES) and reaches a 95% level of significance.

  5. Bovine serum albumin-Cu(II) hybrid nanoflowers: An effective adsorbent for solid phase extraction and slurry sampling flame atomic absorption spectrometric analysis of cadmium and lead in water, hair, food and cigarette samples.

    Yilmaz, Erkan; Ocsoy, Ismail; Ozdemir, Nalan; Soylak, Mustafa

    2016-02-01

    Herein, the synthesis of bovine serum albumin-Cu(II) hybrid nanoflowers (BSA-NFs) through the building blocks of bovine serum albumin (BSA) and copper(II) ions in phosphate buffered saline (PBS) and their use as adsorbent for cadmium and lead ions are reported. The BSA-NFs, for the first time, were efficiently utilized as novel adsorbent for solid phase extraction (SPE) of cadmium and lead ions in water, food, cigarette and hair samples. The method is based on the separation and pre-concentration of Cd(II) and Pb(II) by BSA-NFs prior to determination by slurry analysis via flame atomic absorption spectrometry (FAAS). The analytes were adsorbed on BSA-NFs under the vortex mixing and then the ion-loaded slurry was separated and directly introduced into the flame AAS nebulizer by using a hand-made micro sample introduction system to eliminate a number of drawbacks. The effects of analytical key parameters, such as pH, amount of BSA-NFs, vortexing time, sample volume, and matrix effect of foreign ions on adsorbing of Cd(II) and Pb(II) were systematically investigated and optimized. The limits of detection (LODs) for Cd(II) and Pb(II) were calculated as 0.37 μg L(-)(1) and 8.8 μg L(-)(1), respectively. The relative standard deviation percentages (RSDs) (N = 5) for Cd(II) and Pb(II) were 7.2%, and 5.0%, respectively. The accuracy of the developed procedure was validated by the analysis of certified reference materials (TMDA-53.3 Fortified Water, TMDA-70 Fortified Water, SPS-WW2 Waste Water, NCSDC-73349 Bush Branches and Leaves) and by addition/recovery analysis. The quantitative recoveries were obtained for the analysis of certified reference materials and addition/recovery tests. The method was successfully applied to the analysis of cadmium and lead in water, food, cigarette and hair samples. PMID:26772130

  6. Determination of the neutron flux in the reactor zones with the strong neutron absorption and leakage

    The procedures for the numerical and experimental determination of the neutron flux in the zones with the strong neutron absorption and leakage are described in this paper. The proposed procedures have been applied for the determination of the neutron flux in the internal neutron converter used with the RB reactor core configuration number 114. This paper shows: a) that the full heterogeneous core of complicate geometry, as the RB reactor core configuration No. 114, can be reliably calculated using the equivalence approach implemented in the VEGA2DAN code as a complement to the KENO-V.a multigroup Monte Carlo code; and b) a possibility of the RB reactor core configuration No. 114 for the irradiation of large samples in the field of fast neutrons.

  7. Determination of vanadium in mussels by electrothermal atomic absorption spectrometry without chemical modifiers

    Saavedra, Y.; Fernandez, P. [Centro de Control do Medio Marino, Peirao de Vilaxoan s/n, Vilagarcia de Arousa, 36611 Pontevedra (Spain); Gonzalez, A. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Quimica, 15706, Santiago de Compostela (Spain)

    2004-05-01

    A method was developed for the quantitative determination of total vanadium concentration in mussels via electrothermal atomic absorption spectrometry (ETAAS). After the microwave digestion of the samples, a program using temperatures of 1600 C and 2600 C for ashing and atomization respectively, without any matrix modifiers, allowed us to obtain results that were satisfactory since they agreed closely with certified reference material values. The detection limit was 0.03 mg kg{sup -1} (dry weight), indicating that the method is suitable for the analysis of mussel samples. This determination was compared with matrix modifiers that have been reported previously. The method was applied to various cultivated and wild mussels from the Galician coast, yielding levels below 1 mg kg{sup -1} (wet weight). (orig.)

  8. Electrochemical preconcentration and hydride generation methods for trace determination of selenium by atomic absorption spectrometry

    The use of atomic absorption spectrometry in combination with two different preconcentration/separation techniques for the determination of trace concentrations of selenium is described. Electrochemical preconcentration onto a platinum electrode with a subsequent atomization of selenium is discussed briefly. Several parameters are considered such as the presence of depolarizers, and the temperature of the electrolyzed solutions. Special attention is payed to the efficiency of the atomization step, and a method to improve this is proposed. Applications of the technique to real samples are also reported. Secondly, the separation of the selenium as the volatile selenium hydride from the sample solution is considered. Several papers in this thesis deal with commonly occurring interferants as nickel and copper and with ways of minimizing or avoiding the interferring effects, whereas other papers relate to more theoretical aspects of the hydride generation process. New methods for the determination of selenium in technical samples with high contents of nickel and copper are also presented

  9. Indirect determination of trace phenol in water by atomic-absorption spectrophotometry.

    Bo-Xing, X; Tong-Ming, X; Ming-Neng, S; Yu-Zhi, F

    1985-03-01

    An indirect method for determination of trace phenol in water by atomic-absorption spectrophotometry (AAS) is described. The phenol is brominated in acidic solution with KBrO(3)-KBr solution at room temperature. The excess of bromine is reacted with KI and the I(2) produced is extracted into cyclohexane and then reduced back to I(-) with ascorbic acid. The I(-) is then complexed with Cd(2+) in sulphuric acid medium and the complex extracted into MIBK. The extract is analysed by flame AAS for Cd (and hence indirectly for phenol). The linear concentration range for determination of phenol is 6 x 10(-7)-0.9 x 10(-5)M in aqueous solution. Several foreign ions and organic substances do not interfere. PMID:18963829

  10. Levels of trace elements in different varieties of wheat determined by Atomic Absorption Spectroscopy

    Trace elements Ag, Au, Ca, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, Sr and Zn were determined in six wheat samples purchased from the open market in different localities (Egypt, Saudi Arabia, Yemen, Oman, Dubai and Australia). The dried powdered samples were decomposed in HNO3-HClO4 acids mixtures and elements were determined using recording atomic absorption spectrophotometer. The results were within the safety baseline of all the assayed elements. Certified biological standards, Brown's Kale (BK), Orchard Leaves (OL) and tomato leaves (TOML) were used to assure the accuracy of results. However, Co, Pb and Sr were absent from samples except the Egyptian samples. The obtained databases were statistically treated. Several significant and strong positive correlation coefficients (r=0.506-1.00) between the groups of elements were observed. On the other hand, strong negative correlations (r=0.492-0.873) between another group of elements were also shown. (author)

  11. Determination of molybdenum in silicates through atomic absorption spectrometry using pre-concentration by active carbon

    An analytical procedure for molybdenum determination in geological materials through Atomic Absorption Spectrometry, after pre-concentration of the Mo-APDC complex in activated carbon, has been developed, which is needed in order to reduce the dilution effect in the sample decomposition. During the development of this method the influence of pH, the amount of APDC for complexation of Mo and the interference of Fe, Ca, Mn, Al, K, Na, Mg and Ti were tested. It was shown that none of these causes any significant effect on the Mo determination proposed. The results of the analysis at the international geochemical reference samples JB-1 (basalt) and GH (granite) were very accurate and showed that the detection limit in rocks (1,00g) is 0,6 ppm, when using sample dilution of 1 ml and microinjection techniques. (author)

  12. The direct determination of HgS by thermal desorption coupled with atomic absorption spectrometry

    Coufalík, Pavel; Zvěřina, Ondřej; Komárek, Josef

    2016-04-01

    This research was aimed at the direct determination of HgS in environmental samples by means of thermal desorption coupled with atomic absorption spectrometry. Operating parameters of the apparatus used for thermal desorption (including a prototype desorption unit) are described in this work, as well as the procedure for measuring mercury release curves together with an evaluation of the analytical signal including two methods of peak integration. The results of thermal desorption were compared with HgS contents obtained by sequential extraction. The limits of quantification of the proposed method for the selective determination of the black and red forms of HgS were 4 μg kg- 1 and 5 μg kg- 1, respectively. The limit of quantification of red HgS in soils was 35 μg kg- 1. The developed analytical procedure was applied to soil and sediment samples from historical mining areas.

  13. Study on the application of cold vapor atomic absorption spectrometry and hydride generation atomic absorption spectrometry for the determination of Hg and As traces in sea water samples

    The trace amount of total mercury (Hg) and arsenic (As) in sea water samples were quantitatively determined by using the Atomic Absorption Spectrometry connected with the hydride generation technique (HG-AAS) for As, and with the cold vapour technique (CV-AAS) for Hg. The experiments were carried out at room temperature on a Hydride System Module (HS55) combined with an Atomic Absorption Spectrometer (VARIO 6, Analytik Jena AG). The effect of reductants concentration, and that of matrix on the absorption intensity of each analyzed element was studied in details. The sea water sample after fitrating through a membrane with 0.45(μm-hole size was pre-treated with an oxidant or an reductant to obtain the identical medium. The absorption intensity of each element was then measured on the VARIO-6 under the optimum parameters for spectrometer such as: maximum wavelength, current of hollow cathode lamp, and that for hydride system such as cell temperature, speed of peristaltic pump, pump time, reaction time and rewash time, ect. The analytical procedures were set-up and applied for the determination of these above mentioned elements in the synthesized sea water sample and in the real sea water samples with high precision and accuracy. (author)

  14. Dual-isotope method for determination of human zinc absorption: the use of a test meal of turkey meat

    The percentage of 65Zn taken up (absorbed) from extrinsically labeled turkey meat was calculated from the amounts of 65Zn and a nonabsorbed 51Cr marker present in the body or in a single stool specimen after 1-2 d. 51CrCl3 proved to be a suitable marker for unabsorbed 65Zn and so the early determination of 65Zn absorption was possible. With stool counting, 65Zn absorption data from first stool samples after 1-2 d were accurate as judged by correlation with the amount of 65Zn in the body 7-10 d later (retention); results from subsequent stools gave lower absorption values due to the early excretion of some absorbed 65Zn. The dual-isotope method gave reproducible results when four successive tests of zinc absorption were carried out in a group of six subjects. The average (mean +/- SD) 65Zn absorption from turkey meals containing 31 mumol (2 mg) and 46 mumol (3 mg) of zinc was 39 +/- 8% and 29 +/- 6%, respectively, measured by stool counting; 65Zn absorption and retention correlated well in both studies. A series of different beverages was given in place of water with the turkey meal. Orange juice significantly reduced 65Zn absorption and milk also showed this tendency, but tea, whiskey, wine or beer had no significant effect on the absorption of 65Zn from the turkey meal. In groups of subjects the mean ratio of 65Zn absorption from extrinsically labeled turkey meat on two occasions (1.06) was not significantly different from that of the absorption of extrinsic to intrinsic 65Zn labels (1.16). The dual-isotope technique with either stool or body counting is suitable for the rapid determination of 65Zn absorption from extrinsically labeled turkey within 2 d

  15. The determination, by atomic-absorption spectrophotometry, of impurities in manganese dioxide

    This report describes various methods for the determination of impurities in electrolytic manganese dioxide by atomic-absorption spectrophotometry (AAS). The sample is dissolved in a mixture of acids, any residue being ignited and retreated with acid. Several AAS methods were applied so that the analysis required to meet the specifications could be attained. These involved conventional flame AAS, AAS with electrothermal atomization (ETA), hydride generation coupled with AAS, and cold-vapour AAS. Of the elements examined, copper, iron, zinc, and lead can be determined direct with confidence with or without corrections based on recoveries obtained from spiked solutions. Nickel can be determined direct by use of the method of standard additions, and copper, nickel, and lead by ETA with the method of standard additions. Arsenic and antimony are determined by hydride generation coupled with AAS, and mercury by cold-vapour AAS. The precision of analysis (relative standard deviation) is generally less than 0,050. Values were obtained for aluminium, molybdenum, magnesium, sodium, copper, chromium, and cadmium, but the accuracy of these determinations has not been fully established

  16. Density, ultrasound velocity, acoustic impedance, reflection and absorption coefficient determination of liquids via multiple reflection method.

    Hoche, S; Hussein, M A; Becker, T

    2015-03-01

    The accuracy of density, reflection coefficient, and acoustic impedance determination via multiple reflection method was validated experimentally. The ternary system water-maltose-ethanol was used to execute a systematic, temperature dependent study over a wide range of densities and viscosities aiming an application as inline sensor in beverage industries. The validation results of the presented method and setup show root mean square errors of: 1.201E-3 g cm(-3) (±0.12%) density, 0.515E-3 (0.15%) reflection coefficient and 1.851E+3 kg s(-1) m(-2) (0.12%) specific acoustic impedance. The results of the diffraction corrected absorption showed an average standard deviation of only 0.12%. It was found that the absorption change shows a good correlation to concentration variations and may be useful for laboratory analysis of sufficiently pure liquids. The main part of the observed errors can be explained by the observed noise, temperature variation and the low signal resolution of 50 MHz. In particular, the poor signal-to-noise ratio of the second reflector echo was found to be a main accuracy limitation. Concerning the investigation of liquids the unstable properties of the reference material PMMA, due to hygroscopicity, were identified to be an additional, unpredictable source of uncertainty. While dimensional changes can be considered by adequate methodology, the impact of the time and temperature dependent water absorption on relevant reference properties like the buffer's sound velocity and density could not be considered and may explain part of the observed deviations. PMID:25465962

  17. Development of a hydrophilic interaction liquid chromatography-tandem mass spectrometric method for the determination of kinsenoside, an antihyperlipidemic candidate, in rat plasma and its application to pharmacokinetic studies.

    Rehman, Shaheed Ur; Kim, In Sook; Choi, Min Sun; Luo, Zengwei; Yao, Guangming; Xue, Yongbo; Zhang, Yonghui; Yoo, Hye Hyun

    2016-02-20

    Kinsenoside is a major bioactive constituent isolated from Anoectochilus formosanus and is investigated as an antihyperlipidemic candidate. In this study, a rapid, sensitive, and reliable bioanalytical method was developed for the determination of kinsenoside in rat plasma using hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS). The plasma sample was pretreated with 1% acetic acid, followed by protein precipitation with acetonitrile:methanol (70:30). Chromatographic separation was performed on a HILIC silica column (2.1mm×100mm, 3μm). The mobile phases consisted of 0.1% acetic acid in distilled water (solvent A) and 0.1% acetic acid in acetonitrile (solvent B). A gradient program was used at a flow rate of 0.2mL/min. For mass spectrometric detection, the multiple reaction monitoring mode was used; the MRM transitions were m/z 265.2→m/z 102.9 for kinsenoside and m/z 163.3→m/z 132.1 for the internal standard (IS) nicotine in the positive ionization mode. A calibration curve was constructed in the range of 2-500ng/mL. The intra- and interday precision and accuracy were within 5%. The HILIC-MS/MS method was specific, accurate, and reproducible and was successfully applied in a pharmacokinetic study of kinsenoside in rats. PMID:26686829

  18. Quantitative determination of α-ionone, β-ionone, and β-damascenone and enantiodifferentiation of α-ionone in wine for authenticity control using multidimensional gas chromatography with tandem mass spectrometric detection.

    Langen, Johannes; Wegmann-Herr, Pascal; Schmarr, Hans-Georg

    2016-09-01

    Native concentrations of α-ionone, β-ionone, and β-damascenone were studied in various authentic and commercial wines. In addition, the enantiomeric distribution of α-ionone was determined and its merits as a potential marker for aroma adulteration in wine were discussed. For extraction of volatiles, headspace solid-phase microextraction (HS-SPME) was applied, followed by heart-cut multidimensional gas chromatography coupled to tandem mass spectrometric detection for trace-level analysis. The enantioselective analysis of α-ionone was achieved with octakis(2,3-di-O-pentyl-6-O-methyl)-γ-cyclodextrin as the chiral selector in the separation column for gas chromatography (GC). In all the authentic wines studied, α-ionone showed a high enantiomeric ratio in favor of the (R)-enantiomer. Since an illegal addition of α-ionone in a racemic form changes the enantiomeric ratio, this ratio may serve as an adulteration marker. Concentrations varied between authenticity markers in wine. PMID:27417694

  19. Determination of iron absorption and excretion by whole-body counting; Determination de l'absorption et de l'excretion du fer par la methode de comptage global humain

    Hollard, D.; Benabid, Y.; Berard, M.; Bonnin, J.; Darnault, J.; Millet, M. [Commissariat a l' Energie Atomique, Grenoble (France). Centre d' Etudes Nucleaires

    1969-07-01

    Using a whole-body counter, the authors have studied {sup 59}Fe absorption and loss in 8 normal subjects and in 30 iron deficient patients. Results showed that whole-body counting provided an excellent and simple method for iron retention measurements, obviating many inaccuracies of previous technic. Normal absorption of radio iron with this procedure has ranged from 9 per cent to 20 per cent of the administered tracer in normal subjects, with a mean of 15 per cent. A significant increase in {sup 59}Fe absorption was noted in 21 iron-deficient patients in whom the retention ranged from 40 to 100 per cent. However, 3 iron-deficient patients were found to have low absorption, and their severe iron deficiency could be correlated with this defect in absorption. This method permits also the determination of the rate of iron excretion during the following months and therefore the study of the mechanism of some pathological loss. (authors) [French] L'utilisation de la methode de comptage humain global a permis aux auteurs d'etudier l'absorption et l'excretion du fer-59 chez 8 sujets temoins et 30 sujets hyposideremiques. Les resultats montrent que cette technique simple et directe offre de nombreux avantages sur les methodes employees jusqu'a maintenant pour cette determination. La valeur normale de l'absorption du fer chez les temoins est d'environ 15 pour cent de la dose ingeree. Ce chiffre est tres fortement augmente chez 21 sujets hyposideremiques, pouvant atteindre 100 pour cent de la dose ingeree. Par contre, pour 3 malades, cette absorption est si faible qu'elle suggere une carence par defaut d'absorption. Cette methode permet egalement de suivre l'excretion du fer au cours des mois qui suivent l'examen et de determiner le mecanisme de fuites anormales. (auteurs)

  20. Determination of several physical properties of light petroleum products using IR

    Rashid, H.A.; Dekran, S.B.; Fakhri, N.A.; Aziz, H.J.; Hamoudi, N.A.

    1989-04-01

    In the present study IR spectrometric analysis was used to determine clear research octane number, heat of formation, specific gravity and mole fraction of methyl group, simultaneously in hydrocarbon mixtures. IR absorption spectrum can be used to provide information, that can be obtained by several existing test methods.

  1. A new method to determine the density and water absorption of fine recycled aggregates

    Fernando Rodrigues

    2013-01-01

    Full Text Available The construction industry keeps on demanding huge quantities of natural resources, mainly minerals for mortars and concrete production. The depletion of many quarries and environmental concerns about reducing the dumping of construction and demolition waste in quarries have led to an increase in the procuring and use of recycled aggregates from this type of waste. If they are to be incorporated in concrete and mortars it is essential to know their properties to guarantee the adequate performance of the end products, in both mechanical and durability-related terms. Existing regulated tests were developed for natural aggregates, however, and several problems arise when they are applied to recycled aggregates, especially fine recycled aggregates (FRA. This paper describes the main problems encountered with these tests and proposes an alternative method to determine the density and water absorption of FRA that removes them. The use of sodium hexametaphosphate solutions in the water absorption test has proven to improve its efficiency, minimizing cohesion between particles and helping to release entrained air.

  2. Determination of trace elements in ground water by two preconcentration methods using atomic absorption spectrometry

    This is a comparative study between two different methods of preconcentration done to separate the trace elements cadmium, nickel. chromium, manganese, copper, zinc, and lead in drinking (ground) water samples taken from different locations in Gezira State, central Sudan (the map); these methods are (coprecipitation) with aluminium hydroxide and by Ammonium Pyrrolidine Dithiocarbamate (APDC) using Methyl Isobutyl Ketone (MIBK) as an organic solvent; and subsequent analysis by Atomic Absorption Spectrometry (AAS) for both methods. The result of comparison showed the superiority of the (APDC) coprecipitation method over the aluminium hydroxide coprecipitation method in the total percentage recoveries of the studied trace elements in drinking (ground) water samples, such results confirm previous studies. This study also involves direct analysis of these water samples by atomic absorption spectrometry to determine the concentrations of trace elements Cadmium, Nickel, Chromium, Manganese, Copper, Zinc and Lead and compare it to the corresponding guide line values described by the World Health Organization and the maximum concentrations of trace elements in drinking water permitted by the Sudanese Standards and Metrology Organizations (SSMO), where the concentrations of some elements in some samples were found to be different than the described values by both of the organizations. The study includes a trial to throw light on the effect of the proximity of the water samples sources to the Blue Nile river on its trace elements concentrations; no relation was proved to exist in that respect.(Author)

  3. Mass spectrometric isotope dilution analysis of small calcium concentrations in minerals

    A mass spectrometric isotope dilution analysis for the determination of small calcium contents is developed. The different steps (decomposition of the mineral including isotope dilution technique, calcium separation and mass spectrometric measurement) of the analytical procedure are described. For a 42Ca spike the optimum spike addition is calculated. The dependence of the analysis error on the mass spectrometric measurements is discussed. Using a chromatographic method with a strong acidic ion exchanger calcium can be completely separated from potassium. The calcium content in the range of 0.15-0.004% of two feldspars and of one lepidolite is determined with external relative standard deviations of 0.9-5.1%. (orig.)

  4. Determination of iron in natural and mineral waters by flame atomic absorption spectrometry

    ROLANDAS KAZLAUSKAS

    2004-05-01

    Full Text Available Simple methods for the determination of Fe in natural and mineral waters by flame atomic absorption spectrometry (AAS are suggested. The results of the investigation of selectivity of the proposed AAS method proved that this procedure is not affected by high concentrations of other metals. The calibration graph for iron was linear at levels near the detection limit up to at least 0.10 mg ml-1. For the determination of microamounts of iron in mineral waters, an extraction AAS technique was developed. Iron was retained as Fe-8-oxyquinoline complex and extracted into chloroform. The optimal conditions for the extraction of the iron complex were determined. The AAS method was applied to the determination of Fe in mineral waters and natural waters from different areas of Lithuania. The accuracy of the developed method was sufficient and evaluated in comparison with a photometric method. The obtained results demonstrated that the procedure could be successfully applied for the analysis of water samples with satisfactory accuracy.

  5. Atomic absorption determination, in metal sulphide concentrates, of the elements that form gaseous hydrides

    An account is given of the investigational work on the determination of trace amounts of arsenic, antimony, bismuth, germanium, selenium, and tellurium by the technique using hydride generation and atomic-absorption spectrophotometry. The gaseous hydride is generated by reduction with sodium borohydride, and is subsequently swept by a flow of nitrogen into an air-entrained hydrogen-nitrogen flame. The generation equipment used is simple and inexpensive, and can be readily assembled in most laboratories. The optimum parameters were determined for each element. The effects of 31 probable interfering elements were investigated, and it was found that, although the majority did not interfere, severe interference was encountered when copper, nickel, and the noble metals were present. Methods for the elimination of copper and nickel were developed to allow the determination of arsenic, antimony, bismuth, selenium, and tellurium at the lower parts-per-million level in metal sulphide concentrates with an acceptable accuracy and precision. The determination of microgram amounts of germanium was found to be unsatisfactory

  6. X-ray absorption to determine the metal oxidation state of transition metal compounds

    Jiménez-Mier, J.; Olalde-Velasco, P.; Carabalí-Sandoval, G.; Herrera-Pérez, G.; Chavira, E.; Yang, W.-L.; Denlinger, J.

    2013-07-01

    We present three examples where x-ray absorption at the transition metal L2,3 edges is used to investigate the valence states of various strongly correlated (SC) and technological relevant materials. Comparison with ligand field multiplet calculations is needed to determine the metal oxidation states. The examples are CrF2, the La1-xSrxCoO3 family and YVO3. For CrF2 the results indicate a disproportionation reaction that generates Cr+, Cr2+ and Cr3+ in different proportions that can be quantified directly from the x-ray spectra. Additionally, it is shown that Co2+ is present in the catalytic La1-xSrxCoO3 perovskite family. Finally, surface effects that change the vanadium valence are also found in YVO3 nanocrystals.

  7. Determination of lanthanides in yttrium and praseodymium oxides by atomic absorption spectrophotometry using a graphite furnace

    The operational conditions for the graphite furnace, the instrumental parameters and the sensitivity for the determination of Pr, Nd, Sm, Eu, Y, Gd, Dy, Er, Ho, Tm, and Yb in Y2O3 and Pr2O3 by atomic absorption spectrophotometry are presented. The analyses were carried out into a highly pure argon atmosphere and using pyrolytic graphite tube and graphite supporting electrodes. The accuracy and precision of the method were checked through analyses of synthetic lanthanides mixtures. The concentration range of the lanthanides varied from 0,003 to 3,5% in Y2O3 and from 0,001 to 3,5% in Pr2O3. (Author)

  8. Study of interplanetary hydrogen from Lyman alpha emission and absorption determination

    The purpose of the work submitted in this paper is to contribute to the study of interplanetary hydrogen from Lyman alpha emission and absorption measurements, carried out on board the D2A, OSO-8 and Copernicus satellites. This study, which was undertaken from the D2A satellite, moved us to study the interplanetary environment as from observations made from the following experiments placed on board the OSO-8 and Copernicus satellites. The experiment set up on board the OSO-8 satellite made it possible to obtain the profile of the solar alpha Lyman emission. An absorption profile was observed for the first time on these profiles and this made it possible to attribute them to interplanetary hydrogen and enabled us to make a direct and local determination of the solar ionization rate. - The spectrometer set up on board Copernicus made it possible to obtain the emission spectrum of the interplanetary environment at the same time as the geocorona. The overall velocity of the interplanetary environment was deduced from the Doppler shift between the two spectra. In the first part, the principle of the REA and POLAR experiments is recalled but only the REA experiment is described in detail, particularly the problems arising from the construction and calibration of the cell. In the second part, a study of the interplanetary environment made from the D2A determinations is presented in synthesized form. On the other hand, the study to which theses initial results led us is presented in detail. Finally, in the third part, the results obtained by means of the OSO-8 and Copernicus satellites are given

  9. Determination of lead in dolomite by Zeeman electrothermal atomic absorption spectrometry

    The mineral lorandite (TlAsS2), present in the Alshar deposit (Republic of Macedonia), is a possible solar neutrino detector (Freedman et al., 1976). As a result of nuclear reaction between the isotopes of thallium 205Tl and the solar neutrino, 205 Pb is produced. The aim of the idea is to determine the content of Pb in the lorandite, that could give information for the value of solar neutrino flux over extended time (Pavicevic, 1994). A method for the lead determination in dolomite by Zeeman electrothermal atomic absorption spectrometry, is presented. After the dissolution of samples, lead was extracted with sodium diethyldithio-carbamate. The lead-diethyldithiocarbamate complex was extracted into methylisobutyl ketone from a medium of pH 6.0-10.0. The procedure was verified by method of standard additions and by analyzing referent standard samples. A calibration curve (for organic solutions containing up to 1 ng Pb) was made using the proposed extraction procedure for standard solutions of lead. The standard deviation (SD) for 0.5 ng Pb is 0.01 ng and the relative standard deviation ranges from 2.5 to 3.5%. The detection limit of the method, calculated as 3 SD of the blank, was found to be 1.5 ng.g-1. The operation conditions in electrothermal atomic absorption measurements (temperature and time) were: drying - 90oC, 20 s; charring - 400oC, 20 s; atomizing - 1900oC, 3 s; cleaning - 2650oC, 3 s (Author)

  10. Determination of tin in biological reference materials by atomic absorption spectrophotometry and neutron activation analysis

    Because of a lack of reliable analytical techniques for the determination of tin in biological materials, there have been no reference materials certified for this element. However, the authors' experience has shown that it is feasible to use both atomic absorption and nuclear activation techniques at least for selected matrices. Therefore, an investigation was undertaken to determine tin in several biological materials such as non-fat milk powder (NBS-SRM-1549), citrus leaves (NBS-SRM-1572), total diet (NIST-SRM-1548), mixed diet (NBS-RM-8431), and USDIET-I by atomic absorption spectrophotometry (AAS) and neutron activation analysis (NAA). AAS-ashed samples were extracted with MIBK and assayed using a Perkin Elmer model 5000 apparatus. NAA was carried out by irradiating the samples at the NIST reactor in the RT-4 facility and counting with the help of a Ge(Li) detector connected to a multichannel analyzer. The concentration of tin measured by both AAS and NAA agree well for USDIET-I, total diet, citrus leaves and non-fat milk powder (the concentration ranges for tin in these matrices were from 0.0025 to 3.8 micro g/g). However, in the case of mixed diet (RM-8431), the mean values found were 47 ± 5.6 (n = 19) by AAS and 55.5 ± 2.5 (n = 6) by INAA. Since RM-8431 is not certified it is difficult to draw conclusions. For apple and peach leaves, a distillation step was required. The results were apple leaves 0.085 ± 0.015 (n = 10) by AAS and < 0.2 (n = 3) by RNAA; for peach leaves 0.077 ± 0.02 (n = 9) by AAS and < 0.1 (n = 3) by RNAA. All concentrations are expressed in micro g/g dry weight

  11. [Study on determination of plume velocity by passive differential optical absorption spectroscopy].

    Li, Ang; Xie, Pin-hua; Liu, Wen-qing; Liu, Jian-guo; Dou, Ke; Lin, Yi-hui

    2008-10-01

    Differential optical absorption spectroscopy (DOAS) technique has been used to measure various trace gases in the atmosphere by their strongly structured absorption of radiation in the UV and visible spectral range. Passive DOAS using the zenith scattered sunlight as the light source can obtain the continuous column density distribution of air pollutants (such as SO2 and NO2) by scanning the plume emitted from sources on a mobile platform, then with the plume velocity information the total emission value can be ultimately estimated. In practice it is hard to calculate the total emission because there is no efficient way to accurately get the plume velocity which is the most important parameter. Usually the wind speed near ground is used as the actual plume speed, which constitutes the greatest source of uncertainty in the passive DOAS measurements for the total emission calculation. A passive DOAS method for the determination of plume velocity of pollution source was studied in the present paper. Two passive DOAS systems were placed under the plume along the plume transmission direction to observed the scattered sunlight at one fixed sepasation angle, and then the plume velocity was derived from the time delay resulting from the plume moving a certain distance, and also the plume height needed in the plume velocity calculation was measured by the same two passive DOAS systems. Measurement of the plume emitted from a certain power plant was carried out by the two passive DOAS systems and the plume velocities of 3.6 and 5.4 m x s(-1) at two separate moments were derived. The comparison with the wind speed measured at the same time by the single theodolite wind observation method indicates that this optical remote sensing method based on passive DOAS can be used to determine the plume velocity by monitoring the total emission from sources. PMID:19123375

  12. Solid-phase extraction of copper(II) in water and food samples using silica gel modified with bis(3-aminopropyl)amine and determination by flame atomic absorption spectrometry.

    Cagirdi, Duygu; Altundag, Hüseyin; Imamoglu, Mustafa; Tuzen, Mustafa

    2014-01-01

    A simple and selective separation and preconcentration method was developed for the determination of Cu(ll) ions. This method is based on adsorption of Cu(ll) ions from aqueous solution on a bis(3-aminopropyl)amine modified silica gel column and flame atomic absorption spectrometric determination after desorption. Various analytical parameters such as pH, type of eluent solution and its volume, flow rate of sample and eluent, and sample volume were optimized. Effects of some cation, anion, and transition metal ions on the recoveries of Cu(ll) ions were also investigated. Cu(ll) ions were quantitatively recovered at pH 6; 5.0 mL of 2 M HCI was used as the eluent. The preconcentration factor was found to be 150. The LOD was 0.12 microg/L for Cu(ll). The accuracy of the method was confirmed by analysis of Tea Leaves (INCT-TL-1) and Fish Protein (DORM-3) certified reference materials. The optimized method was applied to various water and food samples for the determination of Cu(ll). PMID:25145149

  13. Flow analysis-hydride generation-gas phase derivative molecular absorption spectrophotometric determination of antimony in antileishmanial drugs

    Máximo Gallignani

    2009-01-01

    Full Text Available In the present work, the development of a method based on the coupling of flow analysis (FA, hydride generation (HG, and derivative molecular absorption spectrophotometry (D-EAM in gas phase (GP, is described in order to determine total antimony in antileishmanial products. Second derivative order (D²224nm of the absorption spectrum (190 - 300 nm is utilized as measurement criterion. Each one of the parameters involved in the development of the proposed method was examined and optimized. The utilization of the EAM in GP as detection system in a continuous mode instead of atomic absorption spectrometry represents the great potential of the analytic proposal.

  14. Determination of 2-ethylhexyl 4-(dimethylamino) benzoate using membrane-assisted liquid-liquid extraction and gas chromatography-mass spectrometric detection.

    March, J G; Genestar, C; Simonet, B M

    2009-06-01

    A flow-cell for micro-porous membrane liquid-liquid extraction with a sheet membrane was used to extract 2-ethylhexyl 4-(dimethylamino) benzoate (EDB) from urine of solar-cream users and spiked wine samples. The cell enabled the target analyte to be extracted from 7.9 mL of donor solution into 200 microL of acceptor solution (decane). After extraction, the acceptor solution was transferred to a micro-vial for GC-MS analysis without derivation. In this work, variables affecting the enrichment factor were also studied, such as organic solvent, extraction time, recirculation flow of the donor solution through the donor chamber, presence of potassium chloride and ethanol in the donor solution and pH. The method has been evaluated in terms of linearity, sensitivity, precision, limits of detection and quantification and extraction efficiency. Limits of quantification were 1 and 3 microg L(-1) EDB for urine and wine, respectively. Quantitative analysis has been carried out by applying the method of standard additions. Within- and between-day relative standard deviations were lower than 12% and 20%, respectively. EDB was found in the urine of users of cream containing EDB in the concentration interval 1.2-7.2 microg L(-1). Therefore, this provides evidence of EDB dermal absorption and subsequent excretion through the urinary tract. EDB was not found in the analysed wine samples. PMID:19347661

  15. Methylmercury determination in biological samples using electrothermal atomic absorption spectrometry after acid leaching extraction

    Saber-Tehrani, Mohammad; Hashemi-Moghaddam, Hamid; Givianrad, Mohammad Hadi; Abroomand-Azar, Parviz [Islamic Azad University, Department of Chemistry, Science and Research Branch, Tehran (Iran)

    2006-11-15

    An efficient and sensitive method for the determination of methylmercury in biological samples was developed based on acid leaching extraction of methylmercury into toluene. Methylmercury in the organic phase was determined by electrothermal atomic absorption spectrometry (ETAAS). The methylmercury signal was enhanced and the reproducibility increased by formation of certain complexes and addition of Pd-DDC modifier. The complex of methylmercury with DDC produced the optimum analytical signal in terms of sensitivity and reproducibility compared to complexes with dithizone, cysteine, 1,10-phenanthroline, and diethyldithiocarbamate. Method performance was optimized by modifying parameters such as temperature of mineralization, atomization, and gas flow rate. The limit of detection for methylmercury determination was 0.015 {mu}g g{sup -1} and the RSD of the whole procedure was 12% for human teeth samples (n=5) and 15.8% for hair samples (n=5). The method's accuracy was investigated by using NIES-13 and by spiking the samples with different amounts of methylmercury. The results were in good agreement with the certified values and the recoveries were 88-95%. (orig.)

  16. Determination of cadmium in real water samples by flame atomic absorption spectrometry after cloud point extraction

    Water pollution is a global threat and it is the leading world wide cause of death and diseases. The awareness of the potential danger posed by heavy metals to the ecosystems and in particular to human health has grown tremendously in the past decades. Separation and preconcentration procedures are considered of great importance in analytical and environmental chemistry. Cloud point is one of the most reliable and sophisticated separation methods for determination of traces quantities of heavy metals. Cloud point methodology was successfully employed for preconcentration of trace quantities of cadmium prior to their determination by flame atomic absorption spectrometry (FAAS). The metals react with 8-hydroxquinoline in a surfactant Triton X-114 medium. The following parameters such as pH, concentration of the reagent and Triton X-114, equilibrating temperature and centrifuging time were evaluated and optimized to enhance the sensitivity and extraction efficiency of the proposed method. Dilution of the surfactant-rich phase with acidified ethanol was performed after phase separation and the cadmium content was measured by FAAS. The validation of the procedure was carried out by spiking addition methods. The method was applied for determination of Cd in water samples of different ecosystems (lake and river). (author)

  17. Some problems connected with boron determination by atomic absorption spectroscopy and the sensitivity improvement

    JELENA J. SAVOVIC

    2001-08-01

    Full Text Available Two atomizers were compared: an N2O–C2H2 flame and a stabilized U-shaped DC arc with aerosol supply. Both the high plasma temperature and the reducing atmosphere obtained by acetylene addition to the argon stream substantially increase the sensitivity of boron determination by atomic absorption spectroscopy (AAS when the arc atomizer is used. The results were compared with those for silicon as a control element. The experimental characteristic concentrations for both elements were compared with the computed values. The experimentally obtained characteristic concentration for boron when using the arc atomizer was in better agreement with the calculated value. It was estimated that the influence of stable monoxide formation on the sensitivity for both elements was about the same, but reduction of analyte and formation of non-volatile carbide particles was more important for boron, which is the main reason for the low sensitivity of boron determination using a flame atomizer. The use of an arc atomizer suppresses this interference and significantly improves the sensitivity of the determination.

  18. Determination of total tin in silicate rocks by graphite furnace atomic absorption spectrometry

    Elsheimer, H.N.; Fries, T.L.

    1990-01-01

    A method is described for the determination of total tin in silicate rocks utilizing a graphite furnace atomic absorption spectrometer with a stabilized-temperature platform furnace and Zeeman-effect background correction. The sample is decomposed by lithium metaborate fusion (3 + 1) in graphite crucibles with the melt being dissolved in 7.5% hydrochloric acid. Tin extractions (4 + 1 or 8 + 1) are executed on portions of the acid solutions using a 4% solution of tricotylphosphine oxide in methyl isobutyl ketone (MIBK). Ascorbic acid is added as a reducing agent prior to extraction. A solution of diammonium hydrogenphosphate and magnesium nitrate is used as a matrix modifier in the graphite furnace determination. The limit of detection is > 10 pg, equivalent to > 1 ??g l-1 of tin in the MIBK solution or 0.2-0.3 ??g g-61 in the rock. The concentration range is linear between 2.5 and 500 ??g l-1 tin in solution. The precision, measured as relative standard deviation, is < 20% at the 2.5 ??g l-1 level and < 7% at the 10-30 ??g l-1 level of tin. Excellent agreement with recommended literature values was found when the method was applied to the international silicate rock standards BCR-1, PCC-1, GSP-1, AGV-1, STM-1, JGb-1 and Mica-Fe. Application was made to the determination of tin in geological core samples with total tin concentrations of the order of 1 ??g g-1 or less.

  19. Application of multiwall carbon nanotubes impregnated with 5-dodecylsalicylaldoxime for on-line copper preconcentration and determination in water samples by flame atomic absorption spectrometry.

    Tobiasz, Anna; Walas, Stanisław; Soto Hernández, Arlene; Mrowiec, Halina

    2012-07-15

    The paper presents application of multiwall carbon nanotubes (MWCNTs) modified with 5-dodecylsalicylaldoxime to copper(II) flow-injection on-line preconcentration and flame atomic absorption spectrometric (FAAS) determination. Two new sorbents were obtained by impregnation of MWCNTs with Cu(II)-LIX 622(®) complex, however in the first case modification was preceded by carbon wall activation via oxidization (Cu-LIX-CNT-A sorbent), and in the second one no surface activation was performed (Cu-LIX-CNT sorbent). It was found that effective leaching of initially introduced copper and Cu(II) retained in preconcentration process could be realized with the use 7% and 5% (v/v) nitric acid, for particular sorbents. Testing the influence of loading solution pH and rate of loading on sorption it was found out that optimal range of loading solution pH was about 4.5-6.3 for activated and 6.15-6.25 for non-activated CNT. Investigation of sorption kinetics showed that the process can be described by pseudo-second order reaction model. Sorption equilibrium conditions (90% sorption) for LIX-CNT-A and LIX-CNT were obtained after 8-15min, respectively and maximum sorption capacity for the new sorbents amounted to 18.1mgg(-1) and 31.6mgg(-1), respectively. For the examined sorbents enrichment factors increased with extension of loading time up to 180s: linearly for activated and non-linearly for non-activated MWCNTs. Influence of potential interferents such as Cd(II), Zn(II), Fe(III), Mg(II) and Ca(II) ions on copper(II) sorption on the new CNT materials was examined individually and with the use of 2(5-2) factorial design. The study revealed significant interference from iron, magnesium and calcium ions at relatively high concentrations. Applicability of the proposed sorbents was tested for Cu(II) determination in various kinds of water samples and the results were compared with those obtained with the use of ICP MS as a reference technique. Copper(II) determination in two certified

  20. Alternative approaches to correct interferences in the determination of boron in shrimps by electrothermal atomic absorption spectrometry

    The aim of this study is to propose alternative techniques and methods in combination with the classical chemical modification to correct the major matrix interferences in the determination of boron in shrimps. The performance of an internal standard (Ge) for the determination of boron by the simultaneous multi-element atomic absorption spectrometry was tested. The use of internal standardization increased the recovery from 85.9% to 101% and allowed a simple correction of errors during sampling preparation and heating process. Furthermore, a new preparation procedure based on the use of citric acid during digestion and dilution steps improved the sensitivity of the method and decreased the limit of detection. Finally, a comparative study between the simultaneous multi-element atomic absorption spectrometry with a longitudinal Zeeman-effect background correction system, equipped with a transversely-heated graphite atomizer and the single element atomic absorption spectrometry with a D2 background correction system, equipped with an end-heated graphite atomizer was undertaken to investigate the different behavior of boron in both techniques. Different chemical modifiers for the determination of boron were tested with both techniques. Ni-citric acid and Ca were the optimal chemical modifiers when simultaneous multi-element atomic absorption spectrometry and single-element atomic absorption spectrometry were used, respectively. By using the single-element atomic absorption spectrometry, the calculated characteristic mass was 220 pg and the calculated limit of detection was 370 μg/kg. On the contrary, with simultaneous multi-element atomic absorption spectrometry, the characteristic mass was 2200 pg and the limit of detection was 5.5 mg/kg. - Highlights: • New approaches were developed to cope with interferences of B determination by ETAAS • Ge was used as internal standard for the determination of B by simultaneous ETAAS • Citric acid was used during digestion

  1. A method for determination of the absorption and scattering properties interstitially in turbid media.

    Dimofte, Andreea; Finlay, Jarod C; Zhu, Timothy C

    2005-05-21

    We have developed a method to quickly determine tissue optical properties (absorption coefficient mu(a) and transport scattering coefficient mu'(s)) by measuring the ratio of light fluence rate to source power along a linear channel at a fixed distance (5 mm) from an isotropic point source. Diffuse light is collected by an isotropic detector whose position is determined by a computer-controlled step motor, with a positioning accuracy of better than 0.1 mm. The system automatically records and plots the light fluence rate per unit source power as a function of position. The result is fitted with a diffusion equation to determine mu(a) and mu'(s). We use an integrating sphere to calibrate each source-detector pair, thus reducing uncertainty of individual calibrations. To test the ability of this algorithm to accurately recover the optical properties of the tissue, we made measurements in tissue simulating phantoms consisting of Liposyn at concentrations of 0.23, 0.53 and 1.14% (mu'(s) = 1.7-9.1 cm(-1)) in the presence of Higgins black India ink at concentrations of 0.002, 0.012 and 0.023% (mu(a) = 0.1-1 cm(-1)). For comparison, the optical properties of each phantom are determined independently using broad-beam illumination. We find that mu(a) and mu'(s) can be determined by this method with a standard (maximum) deviation of 8% (15%) and 18% (32%) for mu(a) and mu'(s), respectively. The current method is effective for samples whose optical properties satisfy the requirement of the diffusion approximation. The error caused by the air cavity introduced by the catheter is small, except when mu(a) is large (mu(a) > 1 cm(-1)). We presented in vivo data measured in human prostate using this method. PMID:15876668

  2. A method for determination of the absorption and scattering properties interstitially in turbid media

    We have developed a method to quickly determine tissue optical properties (absorption coefficient μa and transport scattering coefficient μ's) by measuring the ratio of light fluence rate to source power along a linear channel at a fixed distance (5 mm) from an isotropic point source. Diffuse light is collected by an isotropic detector whose position is determined by a computer-controlled step motor, with a positioning accuracy of better than 0.1 mm. The system automatically records and plots the light fluence rate per unit source power as a function of position. The result is fitted with a diffusion equation to determine μa and μ's. We use an integrating sphere to calibrate each source-detector pair, thus reducing uncertainty of individual calibrations. To test the ability of this algorithm to accurately recover the optical properties of the tissue, we made measurements in tissue simulating phantoms consisting of Liposyn at concentrations of 0.23, 0.53 and 1.14% (μ's = 1.7-9.1 cm-1) in the presence of Higgins black India ink at concentrations of 0.002, 0.012 and 0.023% (μa = 0.1-1 cm-1). For comparison, the optical properties of each phantom are determined independently using broad-beam illumination. We find that μa and μ's can be determined by this method with a standard (maximum) deviation of 8% (15%) and 18% (32%) for μa and μ's, respectively. The current method is effective for samples whose optical properties satisfy the requirement of the diffusion approximation. The error caused by the air cavity introduced by the catheter is small, except when μa is large (μa > 1 cm-1). We presented in vivo data measured in human prostate using this method

  3. Determination of cadmium, cobalt, manganese, copper, nickel, and chromium in concentrated solutions of calcium chloride by electrothermal atomic absorption spectrometry

    A procedure is developed for the direct determination of Cd, Co, Cr, Cu, Mn, and Ni in concentrated solutions of calcium chloride by electrothermal atomic absorption spectrometry. Ascorbic and oxalic acids and magnesium nitrate were examined as chemical modifiers. Oxalic acid was found to be the best modifier. Although an atomic absorption spectrometer with a background correction system of relatively low efficiency (deuterium lamp) was used, elements under study can be reliably determined in the presence of oxalic acid at concentrations of calcium chloride in the solution up to 6%. Because cadmium is evaporated before the major part of the given matrix, it can be determined without modifier

  4. Validation of a liquid chromatography-triple quadrupole mass spectrometric method for the determination of 5-nitro-5'-hydroxy-indirubin-3'-oxime (AGM-130) in human plasma and its application to microdose clinical trial.

    Park, Min-Ho; Lee, Yun Young; Cho, Kyung Hee; La, Sookie; Lee, Hee Joo; Yim, Dong-Seok; Ban, Sooho; Park, Moon-Young; Kim, Yong-Chul; Kim, Yoon-Gyoon; Shin, Young G

    2016-03-01

    A liquid chromatography-triple quadrupole mass spectrometric (LC-MS/MS) method was developed and validated for the determination of 5-nitro-5'-hydroxy-indirubin-3'-oxime (AGM-130) in human plasma to support a microdose clinical trial. The method consisted of a liquid-liquid extraction for sample preparation and LC-MS/MS analysis in the positive ion mode using TurboIonSpray(TM) for analysis. d3 -AGM-130 was used as the internal standard. A linear regression (weighted 1/concentration) was used to fit calibration curves over the concentration range of 10-2000 pg/mL for AGM-130. There were no endogenous interference components in the blank human plasma tested. The accuracy at the lower limit of quantitation was 96.6% with a precision (coefficient of variation, CV) of 4.4%. For quality control samples at 30, 160 and 1600 pg/mL, the between run CV was ≤5.0 %. Between-run accuracy ranged from 98.1 to 101.0%. AGM-130 was stable in 50% acetonitrile for 168 h at 4°C and 6 h at room temperature. AGM-130 was also stable in human plasma at room temperature for 6 h and through three freeze-thaw cycles. The variability of selected samples for the incurred sample reanalysis was ≤12.7% when compared with the original sample concentrations. This validated LC-MS/MS method for determination of AGM-130 was used to support a phase 0 microdose clinical trial. PMID:26139072

  5. Determination of Plutonium Contribution to the Total Burnup of a Spent Nuclear Fuel by Mass Spectrometric Measurements of Uranium and Ruthenium

    The U and Ru isotope patterns provide information on the real irradiation characteristics which are necessary for evaluating a fuel's performance in a reactor. A comparison of the Pu contribution values determined independently provides a promising way to check on the validity of the results. In order to check the consistency of the post-irradiation analysis results, correlations between the parameters of the irradiated nuclear fuels such as the concentration of the heavy elements and fission products, ratios of their isotopes and burnup were established. These correlations can be used to identify the reactor fuels and to estimate the burnup and Pu production. A new approach was carried out with Ru isotopic ratio for the determination of Pu contribution to the total burnup of a spent nuclear fuel from a power reactor. The principle of this approach was based on the use of the difference in the fission yield ratios of the Ru fission products involved for the three main fissionable nuclides such as 235U, 239Pu, and 241Pu. In this work, to determine the contribution of Pu to the total burnup of the fuel, the following two independent methods have been applied: by measuring the isotope ratios of the stable Ru fission products 101Ru/104Ru, and by determining the total burnup by Nd-148 method and subtracting partial burnup, which is determined form the measured values of U isotope ratios

  6. Experimental determination of the chemical changes in the electron density on indium nuclei by the γ-spectrometric ΔIγ/Iγ method

    The γ-spectrometry method for determination of the relative change ΔλEC/λEC in the partial probability λEC for the 114mIn decay branch by the electron capture (EC), when the nucleus is in different chemical environments, was developed. The method is based on an experimental determination of the relative change ΔIγ/Iγ in the intensity of the γ-radiation which is emitted by the excited daughter 114Cd nuclei after EC. The 114mIn decay by EC in indium metal, In2O3 and InAs was compared. The largest ΔIγ/Iγ=(2.5±0.8).10-4 has been found for InAs relatively to In2O3. The chemical changes in the electron density on the indium nucleus corresponding to the measured ΔIγ/Iγ values have been determined

  7. Highly sensitive spectrometric determination of erbium(3) with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol in geological materials and glasses

    The reaction between erbium(3) and 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol was studied for selecting optimal conditions for complexation. This reagent can be used for the spectrophotometric determination of erbium(3) in concentrations ranging from 0.02 to 1.30 mg/h [ε = (1.36 ± 0.05) x 105 mol-1 cm-1]; λ = 581 nm. The reaction takes place at pH from 9.0 to 10.9. In the presence of Triton X-100 this complex is soluble in water. The procedure has been successfully applied to the determination of erbium(3) in geological materials and glass samples

  8. Simultaneous determination of selenium and tellurium in native sulfur by atomic absorption spectrophotometry

    A method for the determination of selenium and tellurium in native sulfur has been investigated by means of atomic absorption spectrophotometry. Native sulfur collected from around fumarole or volcanic crater is ground down into powder, a portion of which weighing 1 g is subjected to analysis. A 2.6% (w/v) sodium hydroxide solution is added by 10 ml to the sample in a teflon beaker, and the mixture is then heated on a hot plate. Sulfur is decomposed and dissolved in the form of disulfide and thiosulfate. A 30% hydrogenperoxide solution is added by 10 ml to oxidize them to sulfate. At the same time selenium and tellurium contained in the sulfur sample are also thought to be oxidized to Se(VI) and Te(VI) states. The solution is neutralized with hydrochloric acid and diluted with distilled water to 100 ml. The sample solution thus prepared is sprayed into the air-acetylene flame of the atomic absorption spectrophotometer. The absorbance is measured at 195.9 nm for selenium and 214.2 nm for tellurium. Calibration curve is prepared by measuring the absorbances of the solutions prepared as follows. One gram portions of pure sulfur (99.9999%) are decomposed as for the samples. After neutralization, standard solutions containing each same amount of selenium and tellurium (0 -- 1000 μg) are added to the sulfur solution and then diluted with water to 100 ml. The standard deviations were estimated to be 50.4 ppm for selenium at 756 ppm and 16.6 ppm for tellurium at 587 ppm. For the check of the reliability of the method, results were compared with those obtained by neutron activation analysis. Results obtained by both methods showed good agreement. (author)

  9. Solid phase extraction and preconcentration of uranium(VI) and thorium(IV) on Duolite XAD761 prior to their inductively coupled plasma mass spectrometric determination.

    Aydin, Funda Armagan; Soylak, Mustafa

    2007-04-15

    A simple and effective method is presented for the separation and preconcentration of thorium(IV) and uranium(VI) by solid phase extraction on Duolite XAD761 adsorption resin. Thorium(IV) and uranium(VI) 9-phenyl-3-fluorone chelates are formed and adsorbed onto the Duolite XAD761. Thorium(IV) and uranium(VI) are quantitatively eluted with 2molL(-1) HCl and determined by inductively coupled plasma-mass spectrometry (ICP-MS). The influences of analytical parameters including pH, amount of reagents, amount of Duolite XAD761 and sample volume, etc. were investigated on the recovery of analyte ions. The interference of a large number of anions and cations has been studied and the optimized conditions developed have been utilized for the trace determination of uranium and thorium. A preconcentration factor of 30 for uranium and thorium was achieved. The relative standard deviation (N=10) was 2.3% for uranium and 4.5% for thorium ions for 10 replicate determinations in the solution containing 0.5mug of uranium and thorium. The three sigma detection limits (N=15) for thorium(IV) and uranium(VI) ions were found to be 4.5 and 6.3ngL(-1), respectively. The developed solid phase extraction method was successively utilized for the determination of traces thorium(IV) and uranium(VI) in environmental samples by ICP-MS. PMID:19071600

  10. Atomic absorption spectrophotometry for the determination of metallic impurities in coal

    The Brazilian Energetic Alternative Program expects the reduction of our dependence on foreign energy sources, through replacing fuel oil by mineral coal. Its gasification by means of nuclear energy must be also considered. However, the intensive burning of coal leads to serious environmental problems. During its combustion the release, to atmosphere, of toxic elements such as As, Hg, Pb, Sb, Se, Cd, Zn and others is of great concern. Increase in atmospheric pollution will take place by burning increased amounts of coal. In addition, some of those elements are concentrated in fly ashes. The determination of impurities in coal is also important for the Figueiras Project in the Nuclebras Mineral Prospection Program. Hence, it is important to have reliable analytical methods which can monitor inorganic constituents at various stages of coal production and utilization. The atomic absorption spectrophotometry is a suitable analytical technique to determine pollutants in coal because it is sensitive, simple, economic and cover a large range of concentrations. The need of a previous treatment of the sample is overcome by using an acid attack (HNO3 + HClO4 + HF) which has proved to be rapid and efficient. (Author)

  11. An empirical determination of the dust mass absorption coefficient, κd, using the Herschel Reference Survey

    Clark, Christopher J. R.; Schofield, Simon P.; Gomez, Haley L.; Davies, Jonathan I.

    2016-06-01

    We use the published photometry and spectroscopy of 22 galaxies in the Herschel Reference Survey to determine that the value of the dust mass absorption coefficient κd at a wavelength of 500 μm is kappa _{500} = 0.051^{+0.070}_{-0.026} m^{2 kg^{-1}}. We do so by taking advantage of the fact that the dust-to-metals ratio in the interstellar medium of galaxies appears to be constant. We argue that our value for κd supersedes that of James et al. - who pioneered this approach for determining κd - because we take advantage of superior data, and account for a number of significant systematic effects that they did not consider. We comprehensively incorporate all methodological and observational contributions to establish the uncertainty on our value, which represents a marked improvement on the oft-quoted `order-of-magnitude' uncertainty on κd. We find no evidence that the value of κd differs significantly between galaxies, or that it correlates with any other measured or derived galaxy properties. We note, however, that the availability of data limits our sample to relatively massive (109.7 < M⋆ < 1011.0 M⊙), high metallicity (8.61 < [ 12 + log_{10} fracOH ] < 8.86) galaxies; future work will allow us to investigate a wider range of systems.

  12. Determination of tellurium in indium antimonide semiconductor material by electrothermal atomic absorption spectrometry.

    Shiue, M Y; Sun, Y C; Yang, M H

    2001-08-01

    A method for the determination of the dopant concentration of tellurium in dissolved indium antimonide semiconductor material by electrothermal atomic absorption spectrometry (ETAAS) was developed. Efforts were made to investigate the optimal conditions of the furnace heating program and the effect of palladium modifier on the variation of tellurium and the background absorbance. According to the results obtained, the presence of palladium chemical modifier in the analysis of indium antimonide allowed the successful retention of tellurium in the graphite tube, and the optimum mass of palladium modifier was found to be dependent on the sample matrix concentration. The absorbance profile of tellurium and the background level were significantly improved when a pyrolysis temperature of 1100 degrees C and an atomization temperature of 2200 degrees C were employed in the optimized heating program. With the use of this method, a detection limit of 0.8 microg g(-1) tellurium in indium antimonide could be achieved. The applicability of the proposed method was evaluated by comparison with two independent methods, i.e. slurry sampling-ETAAS and ICP-MS. From the good agreement between the results, it was demonstrated that the proposed method is suitable for the determination of typical dopant concentrations of tellurium in indium antimonide. PMID:11534624

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

    Matusiewicz, H.; Krawczyk, M. [Politechn Poznanska, Poznan (Poland)

    2007-03-15

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

  14. Stabilizing Agents for Calibration in the Determination of Mercury Using Solid Sampling Electrothermal Atomic Absorption Spectrometry

    Hana Zelinková

    2012-01-01

    Full Text Available Tetramethylene dithiocarbamate (TMDTC, diethyldithiocarbamate (DEDTC, and thiourea were investigated as stabilizing agents for calibration purposes in the determination of mercury using solid sampling electrothermal atomic absorption spectrometry (SS-ETAAS. These agents were used for complexation of mercury in calibration solutions and its thermal stabilization in a solid sampling platform. The calibration solutions had the form of methyl isobutyl ketone (MIBK extracts or MIBK-methanol solutions with the TMDTC and DEDTC chelates and aqueous solutions with thiourea complexes. The best results were obtained for MIBK-methanol solutions in the presence of 2.5 g L-1 TMDTC. The surface of graphite platforms for solid sampling was modified with palladium or rhenium by using electrodeposition from a drop of solutions. The Re modifier is preferable due to a higher lifetime of platform coating. A new SS-ETAAS procedure using the direct sampling of solid samples into a platform with an Re modified graphite surface and the calibration against MIBK-methanol solutions in the presence of TMDTC is proposed for the determination of mercury content in solid environmental samples, such as soil and plants.

  15. A novel method to determine Poisson's ratio by beta-ray absorption experiment

    Fathi, Jafar [Department of Atomic and Molecular Physics, Faculty of Physics, University of Tabriz, Tabriz 51666 (Iran, Islamic Republic of); Ashrafi, Saleh [Department of Nuclear Physics, Faculty of Physics, University of Tabriz, Tabriz 51666 (Iran, Islamic Republic of); Movla, Hossein [Department of Solid State Physics, Faculty of Physics, University of Tabriz, Tabriz 51666 (Iran, Islamic Republic of); Sobhaian, Samad, E-mail: sobhanian@tabrizu.ac.ir [Department of Atomic and Molecular Physics, Faculty of Physics, University of Tabriz, Tabriz 51666 (Iran, Islamic Republic of)

    2012-05-15

    In this paper a new experimental method is applied to determine Poisson's ratio of an industrial rubber tape based on the attenuation of beta particles. A simple theoretical model is presented and the experimental results are compared with the model's prediction. Poisson's ratio of the rubber is obtained by applying a steady state strain force. The relatively good agreement between the model's prediction and the experimental results could be a verification test for the presented method. - Highlights: Black-Right-Pointing-Pointer This paper indicates a novel method to determine Poisson's ratio by beta absorption. Black-Right-Pointing-Pointer A simple model is presented and the experimental results are compared with its prediction. Black-Right-Pointing-Pointer The method utilizes typical values in defining properties such as Young's modulus. Black-Right-Pointing-Pointer Good agreement is obtained between the model's prediction and the experimental results.

  16. Determination of lead in croatian wines by graphite furnace atomic absorption spectrometry

    A method has been developed for direct determination of lead in wine by graphite furnace atomic absorption spectrometry (GFAAS) with Zeeman-effect background correction. The thermal behaviour of Pb during pyrolysis and atomisation stages was investigated without matrix modifier and in the presence of Pd(NO3)2, Pd(NO3)2 + Mg(NO3)2 x 6H2O, and NH4H2PO4 + Mg(NO3)2 x 6H2O as matrix modifiers. A simple 1:1 dilution of wine samples with Pd(NO3)2 as a matrix modifier proved optimal for accurate determination of Pb in wine. Mean recoveries were 106 % for red and 114 % for white wine, and the detection limit was 3 μg L-1. Within-run precision of measurements for red and white wine was 2.1 % and 1.8 %, respectively. The proposed method was applied for analysis of 23 Croatian wines. Median Pb concentrations were 33 μg L-1, range (16 to 49) μg L-1 in commercially available wines and 46 μg L-1, range (14 to 559) μg L-1 in home-made wines. There were no statistically significant differences (P<0.05) in Pb concentration between commercial and home-made wines or between red and white wines. (authors)

  17. Speciation and detection of arsenic in aqueous samples: A review of recent progress in non-atomic spectrometric methods

    Highlights: • Compilation of principal official documents and major review articles, including the toxicology and chemistry of As. • Review of non-atomic spectrometric methods for speciation and detection of arsenic in aqueous samples (2005–2013) of the performance of field-usable methods. - Abstract: Inorganic arsenic (As) displays extreme toxicity and is a class A human carcinogen. It is of interest to both analytical chemists and environmental scientists. Facile and sensitive determination of As and knowledge of the speciation of forms of As in aqueous samples are vitally important. Nearly every nation has relevant official regulations on permissible limits of drinking water As content. The size of the literature on As is therefore formidable. The heart of this review consists of two tables: one is a compilation of principal official documents and major review articles, including the toxicology and chemistry of As. This includes comprehensive official compendia on As speciation, sample treatment, recommended procedures for the determination of As in specific sample matrices with specific analytical instrument(s), procedures for multi-element (including As) speciation and analysis, and prior comprehensive reviews on arsenic analysis. The second table focuses on the recent literature (2005–2013, the coverage for 2013 is incomplete) on As measurement in aqueous matrices. Recent As speciation and analysis methods based on spectrometric and electrochemical methods, inductively coupled plasma-mass spectrometry, neutron activation analysis and biosensors are summarized. We have deliberately excluded atomic optical spectrometric techniques (atomic absorption, atomic fluorescence, inductively coupled plasma-optical emission spectrometry) not because they are not important (in fact the majority of arsenic determinations are possibly carried out by one of these techniques) but because these methods are sufficiently mature and little meaningful innovation has been

  18. Automated sequential injection-microcolumn approach with on-line flame atomic absorption spectrometric detection for implementing metal fractionation schemes of homogeneous and non-homogeneous solid samples of environmental interest

    Chomchoei, Roongrat; Miró, Manuel; Hansen, Elo Harald; Shiowatana, Juwadee

    2005-01-01

    An automated sequential injection (SI) system incorporating a dual-conical microcolumn is proposed as a versatile approach for the accommodation of both single and sequential extraction schemes for metal fractionation of solid samples of environmental concern. Coupled to flame atomic absorption...... Testing sequential extraction method have been also performed in a dynamic fashion and critically compared with the conventional batch-wise protocols. The ecotoxicological relevance of the data provided by both methods with different operationally defined conditions is thoroughly discussed. As compared to...... traditional batch systems, the developed SI assembly offers minimum risks of sample contamination, absence of metal re-distribution/re-adsorption, and dramatic saving of operational times (from 16 h to 40-80 min per partitioning step). It readily facilitates the accurate manipulation of the extracting...

  19. Lead determination at ng/mL level by flame atomic absorption spectrometry using a tantalum coated slotted quartz tube atom trap.

    Demirtaş, İlknur; Bakırdere, Sezgin; Ataman, O Yavuz

    2015-06-01

    Flame atomic absorption spectrometry (FAAS) still keeps its importance despite the relatively low sensitivity; because it is a simple and economical technique for determination of metals. In recent years, atom traps have been developed to increase the sensitivity of FAAS. Although the detection limit of FAAS is only at the level of µg/mL, with the use of atom traps it can reach to ng/mL. Slotted quartz tube (SQT) is one of the atom traps used to improve sensitivity. In atom trapping mode of SQT, analyte is trapped on-line in SQT for few minutes using ordinary sample aspiration, followed by the introduction of a small volume of organic solvent to effect the revolatilization and atomization of analyte species resulting in a transient signal. This system is economical, commercially available and easy to use. In this study, a sensitive analytical method was developed for the determination of lead with the help of SQT atom trapping flame atomization (SQT-AT-FAAS). 574 Fold sensitivity enhancement was obtained at a sample suction rate of 3.9 mL/min for 5.0 min trapping period with respect to FAAS. Organic solvent was selected as 40 µL of methyl isobutyl ketone (MIBK). To obtain a further sensitivity enhancement inner surface of SQT was coated with several transition metals. The best sensitivity enhancement, 1650 fold enhancement, was obtained by the Ta-coated SQT-AT-FAAS. In addition, chemical nature of Pb species trapped on quartz and Ta surface, and the chemical nature of Ta on quartz surface were investigated by X-ray photoelectron spectroscopy (XPS) and Raman Spectroscopy. Raman spectrometric results indicate that tantalum is coated on SQT surface in the form of Ta2O5. XPS studies revealed that the oxidation state of Pb in species trapped on both bare and Ta coated SQT surfaces is +2. For the accuracy check, the analyses of standard reference material were performed by use of SCP SCIENCE EnviroMAT Low (EU-L-2) and results for Pb were to be in good agreement with

  20. Determination of hexavalent chromium in plastic certified reference materials by X-ray absorption fine structure analysis

    Ohata, Masaki; Matsubayashi, Nobuyuki

    X-ray absorption fine structure (XAFS) analysis with transmission mode was used to determine the percentages of hexavalent chromium {Cr(VI)} in total Cr in plastic certified reference materials (CRMs). Cr-K edge X-ray absorption near-edge structure (XANES) spectra were observed and the normalized pre-edge peaks of the spectrum where absorption data was summed was acquired for the determination of Cr(VI). Examination of different number of data point and range of photon energy for summed absorption of the pre-edge peak resulted in reproducible absorption data, though the measurements were carried out at different beam time and beam line. The concentrations of Cr(VI) in the plastic CRMs were also estimated from both the certified value of total Cr and the determined percentage of Cr(VI). The analytical procedure and the estimated concentrations can be useful for the determination of Cr(VI) in plastics with respect to RoHS (restriction of the use of hazardous substances in electrical and electronics equipment) directive.

  1. Determination of hexavalent chromium in plastic certified reference materials by X-ray absorption fine structure analysis

    Ohata, Masaki, E-mail: m-oohata@aist.go.jp [Inorganic Standard Section, Inorganic Analytical Chemistry Division, National Metrology Institute of Japan (NMIJ), National Institute of Advanced Industrial Science and Technology (AIST) (Japan); Matsubayashi, Nobuyuki [Super-Spectroscopy System Research Group, Research Institute of Instrumentation Frontier (RIIF), National Institute of Advanced Industrial Science and Technology (AIST) (Japan)

    2014-03-01

    X-ray absorption fine structure (XAFS) analysis with transmission mode was used to determine the percentages of hexavalent chromium {Cr(VI)} in total Cr in plastic certified reference materials (CRMs). Cr-K edge X-ray absorption near-edge structure (XANES) spectra were observed and the normalized pre-edge peaks of the spectrum where absorption data was summed was acquired for the determination of Cr(VI). Examination of different number of data point and range of photon energy for summed absorption of the pre-edge peak resulted in reproducible absorption data, though the measurements were carried out at different beam time and beam line. The concentrations of Cr(VI) in the plastic CRMs were also estimated from both the certified value of total Cr and the determined percentage of Cr(VI). The analytical procedure and the estimated concentrations can be useful for the determination of Cr(VI) in plastics with respect to RoHS (restriction of the use of hazardous substances in electrical and electronics equipment) directive.

  2. Use of an oxidative destruction and quadrupole mass spectrometric (QMS) detection for the determination of the organic elemental composition of suspended matter in surface water

    Reijnders, H.F.R.; Onderdelinden, D.; Visser, M.G.; Griepink, B.

    1980-01-01

    A study was made of the applicability of a system consisting of a combustion followed by QMS-detection for the determination of the elemental composition of organic matter suspended in surface water. The solid material obtained from several types of water was collected by centrifugation. The results show possible applications e.g. in the field of water characterization. A complete elemental analysis including pretreatment takes about 30 min.

  3. Displacement solid-phase extraction on mercapto-functionalized magnetite microspheres for inductively coupled plasma mass spectrometric determination of trace noble metals

    A flow injection online displacement solid-phase extraction (DSPE) via magnetic immobilization of mercapto-functionalized magnetite microspheres onto the inner walls of a knotted reactor (KR) coupled with inductively coupled plasma mass spectrometry was developed for selective preconcentration and determination of trace noble metals (Ru, Rh, Pd, Pt, Ir and Au) in complex matrices. Online DSPE of 2.7 mL aqueous solution gave the enhancement factors of 32-46 for the six noble metals in comparison with direct nebulization of aqueous sample solution, and the detection limits (3 s) of 2.1 ng L-1 for Ru, 1.9 ng L-1 for Rh, 2.5 ng L-1 for Pd, 1.8 ng L-1 for Ir, 1.9 ng L-1 for Pt and 1.7 ng L-1 for Au. The sample throughput of the developed method was about 20 samples h-1, and the relative standard deviation for eleven replicate determinations of the noble metals at the 30 ng L-1 level ranged from 1.2% to 2.1%. The recoveries of Ru, Rh, Pd, Pt, Ir and Au still maintained 90% even after successive 140 cycles of DSPE. The developed method was successfully applied to selective determination of trace Ru, Rh, Pd, Pt, Ir and Au in complex matrices.

  4. XANES determination of chromium oxidation states in glasses: comparison with optical absorption spectroscopy

    Villain, Olivier; Calas, Georges; Galoisy, Laurence; Cormier, Laurent; Hazemann, Jean-Louis

    2007-01-01

    The oxidation state of chromium in glasses melted in an air atmosphere with and without refining agents was investigated by Cr K-edge X-ray Absorption Near-Edge Structure (XANES) and optical absorption spectroscopy. A good agreement in the relative proportion of Cr(III) and Cr(VI) is obtained between both methods. We show that the chemical dependence of the absorption coefficient of Cr(III) is less important in XANES than in optical absorption spectroscopy. The comparison of glasses melted un...

  5. Qualification and application of a liquid chromatography-tandem mass spectrometric method for the determination of human Aβ1-40 and Aβ1-42 peptides in transgenic mouse plasma using micro-elution solid phase extraction.

    Shin, Young G; Hamm, Lee; Murakami, Stanley; Buirst, Kenji; Buonarati, Michael H; Cox, April; Regal, Kelly; Hunt, Kevin W; Scearce-Levie, Kimberly; Watts, Ryan J; Liu, Xingrong

    2014-05-01

    A liquid chromatographic-tandem mass spectrometric (LC-MS/MS) method was developed and applied for the determination of human Aβ1-40 and Aβ1-42 peptides in transgenic mouse plasma to support preclinical pharmacodynamics studies. The method consisted of micro-elution solid phase extraction for sample preparation and LC-MS/MS analysis in the negative ion mode using electrospray ionization for analysis. (15)N53-Aβ1-40 and (15)N55-Aβ1-42 peptides were used as internal standards. A quadratic regression (weighted 1/concentrations), with an equation y = ax(2) + bx + c, was used to fit calibration curves over the concentration range of 0.500-100 ng/mL for both Aβ1-40 and Aβ1-42 peptides. For quality control samples at 6.00, 40.0 and 80.0 ng/mL from the qualification experiment, the within-run accuracy ranged from -2.69 to 0.583 % with precision values ≤8.23 % for Aβ1-40. Within-run accuracy ranged from -4.83 to 10.1 % with precision values ≤8.87 % for Aβ1-42. Samples from a pharmacodynamics study using Tg2576 transgenic mice were analyzed by this qualified LC-MS/MS method and concentrations were compared to those generated by ELISA. The two methods were shown to be comparable for Aβ1-40 quantification of samples from the Tg2576 amyloid precursor protein transgenic mouse model, but varied slightly for Aβ1-42. PMID:23888333

  6. [Determination of Iodine and Iodate in Brine and Seafood Simultaneously by Ultraviolet Absorption Spectrometry].

    Tan, Jun; Zhu, Xia-ping; Liu, Miao-miao; Wei, Zhi-cheng; Sang, Shi-hua

    2015-06-01

    The iodide in samples was oxidized to iodate by bromine water, which could be removed by formic acid, and iodate could be transformed to I3- with excess of I- in phosphoric acid, the iodate in samples could be transformed directly to I3- with excess of I- in phosphoric acid. The I3- solution had strong absorption at 350 and 288 nm, and the absorbance had a linear relationship to the concentration of I3- in a certain range. Total content of iodide and iodate had been detected after samples were oxidized by bromine water and the content of iodate had been detected directly, and the content of iodide was obtained by difference of the two results. Based on this, the method had been established to detect iodide and iodate in brine and seafood simultaneously by ultraviolet absorption spectrometry. The volumes of bromine water, formic acid, phosphoric acid and potassium iodide had been optimized. The effect of illumination, temperature and time also had been discussed. The optional reagents condition for iodide was: 2 drops of 3% bromine water, 0.5 mL of 10% formic acid, 4 mL of 20% phosphoric acid and 1 mL of 100 g x L(-1 KI. The optional reagents condition for iodate was: 0. 2 mL of 20% phosphoric acid and 1 mL of 100 g x L(-1) KI. The absorbance were determined after reacting for 30 min at room temperature and natural light conditions. Under the optimized conditions, the concentration of iodide and iodate in the range of 0 - 1.2 and 0 -1.5 mg x L(-1) were well agreed with Lambert Beer law. The sample blank was detected for twelve times and the detection limit of iodide and iodate were 1.54 and 14.8 μg x L(-1) respectively. The RSD of twelve times determination of 0.8 mg x L(-1) of iodide and iodate were 0.097% and 0.067%, respectively. The iodide and iodate in Zhabuye brine, Hong Feng underground brine, kelp, seaweed and sea cabbage had been detected, the recovery experiments also had been conducted at the same time, the recovery of iodide and iodate were between 80

  7. Determination of divalent iron content in igneous rocks of ultrabasic, basic and intermediate compositions by a wavelength-dispersive X-ray fluorescence spectrometric method

    This paper proposes the quantitative wavelength-dispersive X-ray fluorescence (XRF) technique of divalent iron content determination in igneous rocks and reports specifics of this technique in terms of classifying rocks into ultrabasic, basic, intermediate and acid ones. Unlike the widely used technique of titration, the proposed XRF technique does not require a labor-consuming procedure for sample preparation. In the fields of FeKβ5 line, and FeKβ′ and FeKβ″ satellites relative intensities of XRF emission spectrum lines are dependent on the valence state of iron in minerals. The ratio FeKβ5/FeKβ1,3 is preferred as the analytical parameter. The XRF method allows divalent iron content (expressed as FeO oxide) over 1.5% to be measured in igneous rocks of ultrabasic and basic compositions by the common calibration equation with the error below 10 rel. %, that is comparable with the error of titrimetric analysis. The samples of igneous rocks of intermediate composition and granodiorites should be analyzed using calibration equations obtained with certified reference materials corresponding in composition to the study samples. For the samples of alkaline rocks the errors of FeO content determination might be in excess of 50 rel. %. - Highlights: • The wavelength-dispersive X-ray fluorescence method allows the determination of divalent iron contents. • Separate calibrations should be used for different types of igneous rocks. • Errors of X-ray fluorescence method and titrimetric analysis are comparable

  8. Ultraviolet vapor generation atomic fluorescence spectrometric determination of mercury in natural water with enrichment by on-line solid phase extraction

    A novel method, which coupled an on-line solid phase extraction (SPE) enrichment with ultraviolet vapor generation (UVG) atomic fluorescence spectrometry (AFS), was developed to improve the sensitivity of mercury determination and to remove the interference of some anion and organics to UVG of mercury. A high mercury retention efficiency and maximum exclusion of inorganic and organic matrix in water samples were achieved by using C18 SPE mini cartridge modified with sodium diethyldithiocarbamate (DDTC). Fast and efficient elution from the cartridge was found by using L-cysteine mixing solution. Furthermore, through the investigation of different UV reactor designs, the most important factor was the structure of the reactor (which corresponded roughly to the photon flux) wherein the tubing was sintered into the UV lamp to give the highest UV generation efficiency. The second factor was the materials of the tubing (which roughly corresponded to the working wavelength). Synthetic quartz, characterized by the highest transparency at 185 nm, attained the highest UVG efficiency, suggesting that the most favorable wavelength for UVG was 185 nm. Under optimum conditions, the achievable detection limit (3σ) with sample loadings of 10.0 mL was 0.03 ng L−1 and 0.08 ng L−1 with different manifolds, respectively. The method was successfully applied to the determination of Hg in tap water, river water and lake water samples. - Graphical abstract: An interference free ultraviolet vapor generation based method was applied to determine ultratrace mercury in water sample. - Highlights: • Hg was enriched by on-line solid phase extraction. • Hg was detected by ultraviolet vapor generation AFS. • The interference of some anion and some organics was removed. • The effects of details of UV set were systemically discussed

  9. Determination of polybrominated diphenyl ethers in house dust using standard addition method and gas chromatography with electron capture and mass spectrometric detection.

    Król, Sylwia; Zabiegała, Bożena; Namieśnik, Jacek

    2012-08-01

    Monitoring of the environmental fate of polybrominated diphenyl ethers (PBDEs) involves determination of their concentration in air, airborne particles and settled dust. This requires the implementation of appropriate analytical tools like measuring instruments, reference materials and analytical procedures. In this study an analytical procedure was developed for determining PBDEs in samples with a complex matrix composition. The efficiencies of three different extraction techniques - Soxhlet extraction (SE), Accelerated Solvent Extraction (ASE) and Ultrasound Assisted Extraction (UAE) - were compared. The study investigated the possibility of using the standard addition method for estimating PBDEs levels. The GC-μECD system was successfully applied as an alternative to low resolution mass spectrometry (LRMS) for determining BDE-209 in dust samples. The developed analytical procedure was then used to analyze dust samples, collected from houses and computer suites in the Tri-city area (Gdansk, Gdynia and Sopot), in order to detect and quantify the presence of polybrominated diphenyl ethers (PBDEs) in the indoor environment. Concentrations of studied congeners (from triBDE to heptaBDE), obtained by chromatographic analysis of dust samples extracts, performed applying two measurement systems (GC-EIMS and GC-μECD) ranged between 331 and 3102 ng g(-1) for house dust and between

  10. Gas chromatographic–mass spectrometric validated method for the determination of Bisphenol A in public-supply water: An investigation in Campo Grande, MS, Brazil

    Émerson Montagner

    2013-01-01

    Full Text Available A new validated method is described for determining bisphenol A (BPA in surface and public-supply water samples. Recovery rates of 91% to 113%, with coefficients of variation below 8.9%, were obtained within the limit of detection (2.4 ng L–1. Concentrations of 13 to 113 ng L–1 were found in tap water. An analysis of BPA stability in solid-phase extraction cartridges revealed that the analyte can be stored in such containers for at least 90 days. An evaluation of BPA leached from polyvinyl chloride (PVC piping showed that BPA can contaminate water distribution systems.

  11. Ultraviolet vapor generation atomic fluorescence spectrometric determination of mercury in natural water with enrichment by on-line solid phase extraction

    Qin, Deyuan; Gao, Feng; Zhang, Zhaohui; Zhao, Liqian; Liu, Jixin; Ye, Jianping; Li, Junwei; Zheng, Fengxi

    2013-10-01

    A novel method, which coupled an on-line solid phase extraction (SPE) enrichment with ultraviolet vapor generation (UVG) atomic fluorescence spectrometry (AFS), was developed to improve the sensitivity of mercury determination and to remove the interference of some anion and organics to UVG of mercury. A high mercury retention efficiency and maximum exclusion of inorganic and organic matrix in water samples were achieved by using C18 SPE mini cartridge modified with sodium diethyldithiocarbamate (DDTC). Fast and efficient elution from the cartridge was found by using L-cysteine mixing solution. Furthermore, through the investigation of different UV reactor designs, the most important factor was the structure of the reactor (which corresponded roughly to the photon flux) wherein the tubing was sintered into the UV lamp to give the highest UV generation efficiency. The second factor was the materials of the tubing (which roughly corresponded to the working wavelength). Synthetic quartz, characterized by the highest transparency at 185 nm, attained the highest UVG efficiency, suggesting that the most favorable wavelength for UVG was 185 nm. Under optimum conditions, the achievable detection limit (3σ) with sample loadings of 10.0 mL was 0.03 ng L- 1 and 0.08 ng L- 1 with different manifolds, respectively. The method was successfully applied to the determination of Hg in tap water, river water and lake water samples.

  12. Comprehensive analysis of the spectrometric determination of voltage applied to X-ray tubes in the radiography and mammography energy ranges using a silicon PIN photodiode.

    Terini, R A; Pereira, M A G; Künzel, R; Costa, P R; Herdade, S B

    2004-05-01

    This work describes the analysis of factors which affect the results of estimation of the electron accelerating potential (kVp) applied to an X-ray tube, through determination of the end point of the energy spectrum of the emitted radiation beam. Measurements have been performed utilizing two spectrometers each with a silicon PIN photodiode: one operating at room temperature, and the other, a high resolution spectrometer, with a Peltier cooler. Both were directly irradiated by different X-ray beams. Both systems work at low voltage and without liquid nitrogen cooling, thus avoiding the drawbacks presented by germanium detectors. Each kVp value was determined by linear regression of the end of the spectrum, so as to give, simultaneously, the best fit to the experimental data and low standard deviation for the kVp value. Detector energy resolution and calibration, counting statistics and high voltage waveform ripple have been investigated in order to establish better experimental conditions and to optimize measurement time. Results of measurements carried out with X-ray tubes connected to single-phase, three-phase or constant potential units, using additional filtration of Cu, Al or Mo (for mammographic beams), are presented. The variations resulted in kVp uncertainties up to 0.1 kV. PMID:15121703

  13. QuEChERS Method Followed by Solid Phase Extraction Method for Gas Chromatographic-Mass Spectrometric Determination of Polycyclic Aromatic Hydrocarbons in Fish

    Mona Khorshid

    2015-01-01

    Full Text Available A gas chromatography equipped with mass spectrometer (GCMS method was developed and validated for determination of 16 polycyclic aromatic hydrocarbons (PAHs in fish using modified quick, easy, cheap, effective, rugged, and safe (QuEChERS method for extraction and solid phase extraction for sample cleanup to remove most of the coextract combined with GCMS for determination of low concentration of selected group of PAHs in homogenized fish samples. PAHs were separated on a GCMS with HP-5ms Ultra Inert GC Column (30 m, 0.25 mm, and 0.25 µm. Mean recovery ranged from 56 to 115%. The extraction efficiency was consistent over the entire range where indeno(1,2,3-cdpyrene and benzo(g,h,iperylene showed recovery (65, 69%, respectively, at 2 µg/kg. No significant dispersion of results was observed for the other remaining PAHs and recovery did not differ substantially, and at the lowest and the highest concentrations mean recovery and RSD% showed that most of PAHs were between 70% and 120% with RSD less than 10%. The measurement uncertainty is expressed as expanded uncertainty and in terms of relative standard deviation (at 95% confidence level is ±12%. This method is suitable for laboratories engaged daily in routine analysis of a large number of samples.

  14. Determination of divalent iron content in igneous rocks of ultrabasic, basic and intermediate compositions by a wavelength-dispersive X-ray fluorescence spectrometric method

    Chubarov, Victor M.; Finkelshtein, Alexandr L.

    2015-05-01

    This paper proposes the quantitative wavelength-dispersive X-ray fluorescence (XRF) technique of divalent iron content determination in igneous rocks and reports specifics of this technique in terms of classifying rocks into ultrabasic, basic, intermediate and acid ones. Unlike the widely used technique of titration, the proposed XRF technique does not require a labor-consuming procedure for sample preparation. In the fields of FeKβ5 line, and FeKβ‧ and FeKβ″ satellites relative intensities of XRF emission spectrum lines are dependent on the valence state of iron in minerals. The ratio FeKβ5/FeKβ1,3 is preferred as the analytical parameter. The XRF method allows divalent iron content (expressed as FeO oxide) over 1.5% to be measured in igneous rocks of ultrabasic and basic compositions by the common calibration equation with the error below 10 rel. %, that is comparable with the error of titrimetric analysis. The samples of igneous rocks of intermediate composition and granodiorites should be analyzed using calibration equations obtained with certified reference materials corresponding in composition to the study samples. For the samples of alkaline rocks the errors of FeO content determination might be in excess of 50 rel. %.

  15. Ultrasound-assisted emulsification of cosmetic samples prior to elemental analysis by different atomic spectrometric techniques.

    Lavilla, I; Cabaleiro, N; Costas, M; de la Calle, I; Bendicho, C

    2009-11-15

    In this work, ultrasound-assisted emulsification with a probe system is proposed as a rapid and simple sample treatment for atomic spectrometric determinations (Electrothermal Atomic Absorption Spectrometry, Inductively Coupled Plasma Optical Emission Spectrometry, Flame Atomic Absorption Spectrometry and Cold Vapour Atomic Absorption Spectrometry) of trace elements (As, Cd, Cr, Cu, Hg, Mg, Mn, Ni, Sr and Zn) in cosmetic samples such as shampoos, gel (hair gel), crèmes (body milk, hair conditioner) and oil (body oil). The type of dispersion medium, the sample mass-to-dispersion medium volume ratio, as well as the parameters related to the ultrasound-assisted emulsification (sonication amplitude and treatment time) were exhaustively studied. Only 1 min of ultrasonic shaking and a dispersion medium containing 0.5% (w/v) of SDS+3% (v/v) of HNO(3) or HCl allows obtaining a stable emulsion at least for 3 months. Thermal programs, nebulization of emulsions, speed of pumps and concentration of reagents used in cold vapour generation were optimized. Calibration using aqueous standards was feasible in all cases. Calibration by the standard addition method and recovery studies was also applied for validation. Microwave-assisted digestion and Inductively Coupled Plasma Mass Spectrometry were used for comparison purposes. Relative standard deviations from analysis of five independent emulsions were less than 9% in all cases. PMID:19782199

  16. Development of a portable mass spectrometric system for determination of isotopic composition of solid uranium samples using fluorine volatilization. Final report

    Using hardware and materials supplied by LANL, a prototype quadrupole mass spectrometer system designed for portable field analysis of isotopic composition of solid uranium samples was assembled and tested. The system contained the capability for fluorine volatilization of solid uranium samples with gas introduction, which was successfully tested and demonstrated using 100 mg samples of U3O8. Determination of precision and accuracy for measuring isotopic composition was performed using isotopic standards. Use with soil samples containing uranium were also attempted. Silicates in the soil forming SiF4 were found to be a kinetic bottleneck to the formation of UF6. This could be avoided by performing some sort of chemical separation as a pre-treatment step, which was demonstrated using nitric acid

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

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

  18. Enantioseparation and determination of isofenphos-methyl enantiomers in wheat, corn, peanut and soil with Supercritical fluid chromatography/tandem mass spectrometric method.

    Chen, Xixi; Dong, Fengshou; Xu, Jun; Liu, Xingang; Chen, Zenglong; Liu, Na; Zheng, Yongquan

    2016-03-15

    Supercritical fluid chromatography/tandem mass spectrometry (SFC-MS/MS) is an effective tool in separation science which uses the nontoxic CO2 fluid for better control of analyte retention. Also the technology of a postcolumn additive to complement MS/MS ensure the high-selectivity determination. In this paper, a green and sensitive analytical method was developed for the enantioselective separation and determination of isofenphos-methyl enantiomers in foodstuff and soil by SFC-MS/MS. The enantioseparation was performed within 3.50min using Chiralpak IA-3 column with CO2/isopropanol (90:10, v/v) as the mobile phase at 2.2mL/min flow rate. The postcolumn compensation technology provided with 0.1% formic acid/methanol greatly improved the ionization efficiency of mass spectrometry. Column temperature, auto back pressure regulator pressure, and flow rate of compensation solvent were optimized to 30°C, 2200psi, and 0.1mL/min, respectively. The QuEChERs method was adopted in this study, which mean recoveries of isofenphos-methyl enantiomers ranged from 75.7% to 111.4%, with relative standard deviations less than 11.3% at three concentration levels in all matrices. The limits of detection for both enantiomers varied from 0.02μg/kg to 0.15μg/kg, while the limit of quantification did not exceed 0.50μg/kg. The proposed method was then successfully applied to analyze authentic samples, confirming that it was a versatile strategy for the analysis of isofenphos-methyl enantiomers in food and environmental matrices. PMID:26894851

  19. Determination of chromium and molybdenum in medical foods by graphite furnace atomic absorption spectrophotometry.

    Phifer, E C

    1995-01-01

    Graphite furnace atomic absorption spectrophotometry was used to determine chromium and molybdenum in 7 medical foods from 5 manufacturers. Linear standard curves were obtained for both elements for concentrations between 5 and 25 ng/mL. Detection limits were 0.24 ng/mL for Cr and 0.67 ng/mL for Mo. Characteristic masses were 3.1 and 14.7 pg for Cr and Mo, respectively. No difference was detected between wet and dry ashing methods, and dry ashing was used to complete the study. The method was validated by assaying various National Institute of Standards and Technology standard reference materials. Analysis of these products for Cr and Mo were within certified values. One product was evaluated by this method for reproducibility (n = 5). Relative standard deviations were 6.8 and 4.8% for Cr and Mo, respectively. This product contained 0.31 +/= 0.02 micrograms Cr/g and 0.63 +/- 0.03 micrograms Mo/g. The remaining products contained 0.09-1.28 micrograms Cr/g and 0.07-2.3 micrograms Mo/g. Mean recovery values were 98 +/- 14% (n = 14) for Cr at spike levels of 0.20-1.89 micrograms/g and 102 +/- 24% (n = 10) for Mo at spike levels of 0.30-1.89 micrograms/g. PMID:8664588

  20. Determination of mercury by multisyringe flow injection system with cold-vapor atomic absorption spectrometry

    A new software-controlled time-based multisyringe flow injection system for mercury determination by cold-vapor atomic absorption spectrometry is proposed. Precise known volumes of sample, reducing agent (1.1% SnCl2 in 3% HCl) and carrier (3% HCl) are dispensed into a gas-liquid separation cell with a multisyringe burette coupled with one three-way solenoid valve. An argon flow delivers the reduced mercury to the spectrometer. The optimization of the system was carried out testing reaction coils and gas-liquid separators of different design as well as changing parameters, such as sample and reagents volumes, reagent concentrations and carrier gas flow rate, among others. The analytical curves were obtained within the range 50-5000 ng L-1. The detection limit (3σ b/S) achieved is 5 ng L-1. The relative standard deviation (R.S.D.) was 1.4%, evaluated from 16 successive injections of 250 ng L-1 Hg standard solution. The injection and sample throughput per hour were 44 and 11, respectively. This technique was validated by means of solid and water reference materials with good agreement with the certified values and was successfully applied to fish samples

  1. Determination of uranyl incorporation into biogenic manganese oxides using X-ray absorption spectroscopy and scattering

    Webb, S.M.; Fuller, C.C.; Tebo, B.M.; Bargar, J.R.

    2006-01-01

    Biogenic manganese oxides are common and an important source of reactive mineral surfaces in the environment that may be potentially enhanced in bioremediation cases to improve natural attenuation. Experiments were performed in which the uranyl ion, UO22+ (U(VI)), at various concentrations was present during manganese oxide biogenesis. At all concentrations, there was strong uptake of U onto the oxides. Synchrotron-based extended X-ray absorption fine structure (EXAFS) spectroscopy and X-ray diffraction (XRD) studies were carried out to determine the molecular-scale mechanism by which uranyl is incorporated into the oxide and how this incorporation affects the resulting manganese oxide structure and mineralogy. The EXAFS experiments show that at low concentrations (2 mol % U, >4 ??M U(VI) in solution), the presence of U(VI) affects the stability and structure of the Mn oxide to form poorly ordered Mn oxide tunnel structures, similar to todorokite. EXAFS modeling shows that uranyl is present in these oxides predominantly in the tunnels of the Mn oxide structure in a tridentate complex. Observations by XRD corroborate these results. Structural incorporation may lead to more stable U(VI) sequestration that may be suitable for remediation uses. These observations, combined with the very high uptake capacity of the Mn oxides, imply that Mn-oxidizing bacteria may significantly influence dissolved U(VI) concentrations in impacted waters via sorption and incorporation into Mn oxide biominerals. ?? 2006 American Chemical Society.

  2. Determination of heavy metals in imported food for Libyan marketing by using Atomic Absorption Spectrometer (AAS)

    Nowadays, it becomes difficult to differentiate between essential and toxic elements, since all elements are toxic if their concentration is exceeded the permissible level recommended by the world health organization (WHO). In some instances the recommended and toxicity levels are close, therefore; it is necessary to differentiate between these essential and toxic levels even in very low concentrations. Several thousands of imported food samples (5877), including: canned soft drinks and juices, biscuits, baking powder, canned tomato past, canned hot spice, canned infant milk, canned concentrated milk, chocolates, canned tuna, and canned oil, were collected randomly from different markets around the country. The samples were analyzed for heavy metals: Cu, Zn, Fe, Sn, As, Pb, and Hg, by atomic absorption spectrometer (AAS), using flame atomization for Cu, Zn, and Fe, hydride generation (HG) for Sn and As, cold vapor for Hg and electrothermal atomization for Pb determination. The obtained AAS results were compared with the Libyan and international food specifications. Most of the samples analyzed were within the specification range and only a little have higher heavy metals level. (Authors)

  3. Evaluation for the method for the determination of impurities in uranium products by atomic absorption spectrophotometry

    Objective: To establish a reliable method for the determination of Al, Ca, Cd, Co, Cr, Cu, Fe, Mn, Mo, Mg, Ni, Pb, V and Zn as impurities in a uranium oxide (U3 O8). Methodology: The sample, generally a solid or a powder, is solubilized by acid digestion with concentrated nitric acid, carrying to dryness for the recover with 6 N Nitric Acid to extract the uranium matrix, try butyl phosphate to 30 % in carbon tetrachloride (C Cl4), the aqueous phase containing the impurities is heat up with perchloric acid (HClO4) in order to eliminate the remainder organic solvent. A Perking Elmer Atomic Absorption spectrophotometer is used for the analysis of the samples which were read for 5 times and the average is reported as final result. The method is considered as valid since it comply with linearity in the concentration for each one of the elements. The accuracy of the method is check with the repeatability of the results. For the evaluation of the accuracy, reference certified standards are used. (Author)

  4. Organic solvents as interferents in arsenic determination by hydride generation atomic absorption spectrometry with flame atomization

    Karadjova, Irina B.; Lampugnani, Leonardo; Dědina, Jiri; D'Ulivo, Alessandro; Onor, Massimo; Tsalev, Dimiter L.

    2006-05-01

    Interference effects of various organic solvents miscible with water on arsenic determination by hydride generation atomic absorption spectrometry have been studied. Arsine was chemically generated in continuous flow hydride generation system and atomized by using a flame atomizer able to operate in two modes: miniature diffusion flame and flame-in-flame. The effects of experimental variables and atomization mode were investigated: tetrahydroborate and hydrochloric acid concentrations, argon, hydrogen and oxygen supply rates for the microflame, and the distance from the atomization region to the observation zone. The nature of the species formed in the flame due to the pyrolysis of organic solvent vapors entering the flame volume together with arsine is discussed. The observed signal depression in the presence of organic solvents has been mainly attributed to the atomization interference due to heterogeneous gas-solid reaction between the free arsenic atoms and finely dispersed carbon particles formed by carbon radicals recombination. The best tolerance to interferences was obtained by using flame-in-flame atomization (5-10 ml min - 1 of oxygen flow rate), together with higher argon and hydrogen supply rates and elevated observation heights.

  5. Validation of a liquid chromatography-electrospray ionization tandem mass spectrometric method to determine six polyether ionophores in raw, UHT, pasteurized and powdered milk.

    Pereira, Mararlene Ulberg; Spisso, Bernardete Ferraz; Jacob, Silvana do Couto; Monteiro, Mychelle Alves; Ferreira, Rosana Gomes; Carlos, Betânia de Souza; da Nóbrega, Armi Wanderley

    2016-04-01

    This study aimed to validate a method developed for the determination of six antibiotics from the polyether ionophore class (lasalocid, maduramicin, monensin, narasin, salinomycin and semduramicin) at residue levels in raw, UHT, pasteurized and powdered milk using QuEChERS extraction and high performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS). The validation was conducted under an in-house laboratory protocol that is primarily based on 2002/657/EC Decision, but takes in account the variability of matrix sources. Overall recoveries between 93% and 113% with relative standard deviations up to 16% were obtained under intermediate precision conditions. CCα calculated values did not exceed 20% the Maximum Residue Limit for monensin and 25% the Maximum Levels for all other substances. The method showed to be simple, fast and suitable for verifying the compliance of raw and processed milk samples regarding the limits recommended by Codex Alimentarius and those adopted in European Community for polyether ionophores. PMID:26593474

  6. Use of Ni/NixB Nanoparticles as a Novel Adsorbent for the Preconcentration of Mercury Species prior to Cold Vapor-Atomic Fluorescence Spectrometric Determination.

    Yayayürük, Onur; Henden, Emür

    2016-01-01

    A selective matrix separation/enrichment method, utilizing a simple batch procedure with nickel/nickel boride (Ni/NixB) nanoparticles was proposed for the determination of inorganic mercury(II), Hg(2+) and methyl mercury(I), CH3Hg(+) in waters prior to cold vapor-atomic fluorescence spectrometry (CV-AFS). The Ni/NixB nanoparticles, were synthesized by the chemical reduction of Ni(II) to Ni/NixB. The novel adsorbent was selective to Hg(2+) and CH3Hg(+) species between pH values of 4 - 10. Both of the mercury species were recovered from the adsorbent using 1.0 mol L(-1) hot HNO3 with high efficiency. It was observed that the adsorbent selectively removed Hg(2+) and CH3Hg(+) from the bulk solution in the presence of several competitor ions (As(3+), Sb(3+), Pb(2+), Zn(2+), Cu(2+), Cd(2+) and Fe(3+)) with ≥96% adsorption. The limit of detection (3σ above blank) was found to be 1.8 ng L(-1) with a preconcentration factor of 20. The validation of the method was tested through spike recovery experiments with several water samples (tap and seawater) at μg L(-1) concentration levels, and all recovery values were found to vary between 95 and 105%. PMID:27506713

  7. Rapid determination of acid herbicides in soil by liquid chromatography with tandem mass spectrometric detection based on dispersive solid phase extraction.

    Kaczyński, Piotr; Łozowicka, Bożena; Jankowska, Magdalena; Hrynko, Izabela

    2016-05-15

    This study determined twenty six the highly sensitive phenoxy, pyridines, aliphatic and aromatic acid compounds in soil with a liquid chromatography tandem mass spectrometry. The samples were prepared by modified quick, easy, cheap, effective, rugged and safe (QuEChERS) analytical procedure in solid samples. Herbicides extraction effectiveness was evaluated at three different spiking levels (0.01, 0.1 and 1.0mgkg(-1)). Fourteen different dispersive solid-phase extraction (d-SPE) sorbents in clean-up step were tested. The QuEChERS protocol with acidic alumina provided the highest number of pesticides with recoveries in the 70-120% range. The soil matrix effect was evaluated and for the majority of compounds were not significant, showing suppression or enhancement (±81-123%). The precision calculated as relative standard deviation (RSD) was below 22%. The linear relation was observed in the range 0.01-2.0mgkg(-1) and the correlation coefficient R>0.999. The expanded measurement uncertainty was estimated as being on average, and was between 9% and 33%. The validated method was employed in the analysis of 309 real soil samples. PMID:26992503

  8. Determination of total sulfur concentrations in different types of vinegars using high resolution flame molecular absorption spectrometry.

    Ozbek, Nil; Akman, Suleyman

    2016-12-15

    Total sulfur concentrations in vinegars were determined using molecular absorption of carbon monosulfide (CS) determined with a high-resolution continuum source flame atomic absorption spectrometer. The molecular absorption of CS was measured at 258.056nm in an air-acetylene flame. Due to non-spectral interference, as well as the different sensitivities to some sulfur compounds, all sulfur species were oxidized to sulfate using a HNO3 and H2O2 mixture and the analyte addition technique was applied for quantification. The limit of detection (LOD) and limit of quantification (LOQ) were 11.6 and 38.6mgL(-1), respectively. The concentrations of sulfur in various vinegars ranged from ⩽LOD to 163.6mgL(-1). PMID:27451213

  9. Comparison of coal digestion methods for atomic absorption determination of cadmium in coal

    Nakashima, Ryozo; Kamata, Eijiro; Goto, Kazuo; Shibata, Shozo (Government Industrial Research Inst., Nagoya (Japan))

    1983-08-01

    To determine cadmium in coals, the decomposition method of coal matrix by using nitric-perchloric acid digestion in the sealed PTFE vessel modified in the authors laboratory was compared, in referring the recovery of cadmium, with nitric-hydrofluoric acid digestion followed by perchloric-periodic acid digestion, low temperature ashing method, and ASTM ashing method. The analytical values of NBS 1632a coal using these decomposition methods were all agreed with that of NBS certified. The cadmium quantity over than 1.0 ppm found to be determine by the calibration method with a representative synthesized coal solution containing the same quantities of acids as used in the procedure, without matching the major elements in coal digests. One half a gram of coal samples were treated in the sealed PTFE vessel with 7 ml of 1:1 perchloric-nitric acid mixture, heating at 150/sup 0/C for 7 h followed by hydrofluoric acid digestion, addition of boric acid, aquatic dilution and filtration. The solutions were then nebulized for the atomic absorption measurement. In the cadmium quantity less than 1.0 ppm, both the acid digests and the ashed samples were treated with hydrofluoric acid to expel silicic materials and then with dithizone-CCL/sub 4/ reagent to extract cadmium in the presence of ammonium citrate at pH 9.5--10. The organic layer was back-extracted with 2:100 hydrochloric acid. Eight coals mined in Australia, Canada, China, and Japan were analyzed. The correlation coefficient of concentrations of cadmium upon those of zinc was calculated to be 0.75, which showed cadmium occurred closely with zinc in coal.

  10. Determination of Lead in Human Teeth by Hydride Generation Atomic Absorption Spectrometry

    Hassan T. Abdulsahib

    2011-01-01

    Full Text Available Problem statement: The determination of lead in human teeth at concentration levels of ìg/ml is proposed using Hydride Generation Atomic Absorption Spectrometry (HG-AAS. To do this, 2% (wv lanthanum chloride solution is employed as matrix modifying reagent to increase sensitivity and remove matrix interferences. Approach: About 100 µL of sample and 100 µL of 3.0% (m/v NaBH4 are simultaneously injected into carrier streams. The detection of limit of 0.46 µg L-1 for Pb was achieved and the relative standard deviation of 3.0% for 10 µg L-1 lead was obtained. The recovery percentage of the method has been found to be (92.8-100.5% for known quantities of lead added to teeth sample which were completely recovered. A comparison of the proposed method with standard addition method showed nearly results in the same samples of teeth and the results compared with other studies in the world. Results: The method was shown to be satisfactory for determination of traces of lead in teeth samples with excellent accuracy. Teeth analysis reveals that intact teeth contained the highest amounts of lead which provide an evidence that lead may reduce the prevalence of dantal caries. Statistically significant differences (pConclusion: Statistically significant difference between age groups were seen in the mean value of lead concentrations in human teeth, the concentration of lead increased with age. The differences may be due to the exposure of lead and others factors such as differences in diet and drinking water.

  11. Mass-spectrometric determination of O2 and CO 2 gas exchange in illuminated higher-plant cells : Evidence for light-inhibition of substrate decarboxylations.

    Avelange, M H; Thiéry, J M; Sarrey, F; Gans, P; Rébeillé, F

    1991-01-01

    In order to estimate photosynthetic and respiratory rates in illuminated photoautotrophic cells of carnation (Dianthus caryophyllus L.), simultaneous measurements of CO2 and O2 gas exchange were performed using (18)O2, (13)CO2 and a mass-spectrometry technique. This method allowed the determination, and thus the comparison, of unidirectional fluxes of O2 and CO2. In optimum photosynthetic conditions (i.e. in the presence of high light and a saturating level of CO2), the rate of CO2 influx represented 75±5% of the rate of gross O2 evolution. After a dark-to-light transition, the rate of CO2 efflux was inhibited by 50% whereas the O2-uptake rate was little affected. The effect of a recycling of respiratory CO2 through photosynthesis on the exchange of CO2 gas was investigated using a mathematical model. The confliction of the experimental data with the simulated gas-exchange rates strongly supported the view that CO2 recycling was a minor event in these cells and could not be responsible for the observed inhibition of CO2 efflux. On the basis of this assumption it was concluded that illumination of carnation cells resulted in a decrease of substrate decarboxylations, and that CO2 efflux and O2 uptake were not as tightly coupled in the light as in the dark. Furthermore, it could be calculated from the rate of gross photosynthesis that the chloroplastic electron-transport chain produced enough ATP in the light to account for the measured CO2-uptake rate without involving cyclic transfer of electrons around PS I or mitochondrial supplementation. PMID:24193614

  12. Determination of total lead in lipstick: development and validation of a microwave-assisted digestion, inductively coupled plasma-mass spectrometric method.

    Hepp, Nancy M; Mindak, William R; Cheng, John

    2009-01-01

    Recent reports describing the presence of lead (Pb) in lipsticks have suggested that, under ordinary use, the potential amount of Pb exposure is harmful. To permit independent assessment of the Pb contamination, a method for determining total Pb in lipstick using microwave-assisted digestion and analysis employing inductively coupled plasma-mass spectrometry (ICP-MS) was developed and validated. Since lipsticks may contain fats, oils, pigments, dyes, and minerals, several reference materials (RM) were analyzed, including coal, wear metals in oil, organic Pb in oil, milk powder, and estuarine sediment. With the exception of the RM with mineral content (estuarine sediment), complete recovery of Pb from the RMs was obtained by simple nitric acid (HNO(3)) digestion. Complete recovery of Pb from estuarine sediment was achieved only when hydrofluoric acid (HF) was added to the digestion mix, followed by treatment with excess boric acid (H(3)BO(3)) to neutralize the HF and to dissolve insoluble fluorides. Commercial lipsticks were tested for total Pb by the validated method. The detection limit was estimated to be 0.04 microg Pb/g. The average value obtained for the lipsticks was 1.07 microg/g. Undigested material was present in some lipstick digests when only HNO(3) was used, and generally lower Pb values were obtained. All of the Pb levels found by the U.S. Food and Drug Administration (FDA) were within the range the agency would expect to find in lipsticks formulated with permitted color additives and other ingredients prepared under good manufacturing practice (GMP) conditions. This method will be useful for the FDA and industry in helping to ensure the safety of cosmetic products. PMID:19691936

  13. Determination of cadmium in bovine tissue by spectrophotometry of atomic absorption

    The present work utilized the suggested method by Food Safety and Inspection Service (FSIS) for the analysis of cadmium in animal tissue, it was adapted by the Toxicology's Laboratory of MAG, where the project was organized. This method consist of a burning of sample and the instrumental analysis by means of the atomic absorption's technique. In the study there were determined parameters of carrying out of the analytical methodology, it was getting the following values: linearity : 0,020 -1,0 mg/L; homogeneity of the model: homoscedastic; limit of detection (LD) : 0,0049 mg/kg (4,9 μg/Kg); limit of quantification (LC): 0,016 μg/L (16 mg/kg); sensibility of calibration: 0,243 A * L/gm; analytical sensibility: 105 L/mg; instrumental repetitively: < 4,3%; repetitively of gauges < 3,5%; reproducibility of methodology: 13,4% (expressed like variation's coefficient); truthfulness: 86,5%; selectivity and specificity: there isn't interferences of matrix, chemical or of ionization when the wavelength utilized is of 228,8 nm. It was made an study to determinate the present cadmium's quantities in three tissues of bovine origin; of an total of 20 animals there were gotten the following averages: muscles: 37,5 μg/kg, liver: 93,7 μg/kg and kidney: 253,4 μg/kg. Additionally, it was determined the correlation that exist among the contents of the metal and other variations, like sex, approximate age, as well as the stock sort: dairy or meat, where there were observed significant differences to a level of confidence of 95%, among the contents of Cadmium in muscle of meat stock and the dairy stock, being major the accumulation to the meat stock and the dairy stock, this like a difference of the other variations where didn't find a significant difference. Besides, it was determined, the metal's accumulation in two different kidney's zones: medullar and cortical, being significantly major in the last one, with a correlation of 99,5%. (Author)

  14. Determination of cadmium in biodiesel using microemulsion and electrothermal atomization atomic absorption spectrometry.

    Lima, Adriana S; Silva, Deise G; Teixeira, Leonardo S G

    2015-01-01

    This work aimed to prepare biodiesel microemulsions for the subsequent quantification of cadmium via graphite furnace atomic absorption spectrometry (GFAAS). The biodiesel samples were prepared using n-propanol as an emulsifier, 10% (v/v) nitric acid as the aqueous phase, and biodiesel. Pseudoternary phase diagrams were constructed to determine the microemulsion region with the specified components. The optimized conditions for microemulsion formation were 57.6% (v/v) n-propanol, 21.2% (v/v) biodiesel, and 21.2% (v/v) nitric acid solution. The stability of the microemulsified system was investigated using aqueous and organic standards, and the system was found to be stable for at least 240 min. The applied pyrolysis and atomization temperatures were 800 and 2000 °C, respectively, and 5 μg of aluminum was used as the chemical modifier. The obtained limits of detection and quantification were 0.2 and 0.5 μg kg(-1), respectively, and the characteristic mass was 1.6 pg. The precision, expressed as the relative standard deviation (% R.S.D., n = 10), was 2.5% for a sample with a cadmium concentration of 6.5 μg kg(-1). The accuracy was determined from addition and recovery experiments, with results varying from 93 to 108% recovery. This study demonstrates that the proposed method based on the use of a microemulsion formation in sample preparation can be applied as an efficient alternative for the determination of cadmium in biodiesel by GFAAS. Cadmium determination in biodiesel samples of different origins (soybean, corn, cotton, and sunflower) was evaluated after acid digestion using the inductively coupled plasma-mass spectrometry (ICP-MS) technique, and the obtained results were compared to the results obtained using the proposed method. The paired t test (95% confidence level) did not show significant differences. The concentrations of cadmium found ranged from 5.3 to 8.0 μg kg(-1). PMID:25381584

  15. 邻菲啰啉-Fe^3+分光光度法测定食品中的亚硫酸盐%A Spectrometric Method for Sulfite Determination Using the System of Complex of Phenanthroline and Fe~(3+)

    廖文生; 刘中勇; 赵群; 谢思瑶; 伍冠红

    2012-01-01

    Phenanthroline can interact with Fe3+ and Fe2+ to form metal complexes of different colors.Phenanthroline-Fe3+ was changed to phenanthroline-Fe2+ due to the redox reaction between sulfite and Fe3+ with dramatic spectrum changes.Based on this,a spectrometric method for the determination of sulfite was developed.In pH5.00 NaAc-HAc buffer,the addition of sulfite to the phenanthroline-Fe3+ system results in significant absorption increase at 510 nm which is proportional to the concentration of sulfite over the range of 1.08 ×10-6-1.60 ×10-5mol/L with a limit of detection of 1.08×10-7mol/L.The proposed method was applied to determine sulfite in biscuits,the recovery being 92.2%-101.8%.%邻菲啰啉可与Fe3+和Fe2+结合形成不同颜色的金属配合物。利用亚硫酸对Fe3+离子的还原作用,使邻菲啰啉-Fe3+配合物转化为邻菲啰啉-Fe2+,产生显著的光谱变化,据此建立测定亚硫酸盐的光谱分析法。研究结果显示,在pH5.00的乙酸钠-乙酸缓冲溶液中,亚硫酸盐的加入使体系在510 nm处的吸光度显著增强,在一定浓度范围内510nm处吸光度的增加值与亚硫酸盐浓度呈良好线性关系,其线性范围为1.08×10-6-1.60×10-5mol/L,检测限为1.08×10-7mol/L。本方法用于测定饼干中的亚硫酸盐,回收率为92.2%-101.8%。

  16. Determination of Chlorine in Milk via Molecular Absorption of SrCl Using High-Resolution Continuum Source Graphite Furnace Atomic Absorption Spectrometry.

    Ozbek, Nil; Akman, Suleyman

    2016-07-20

    Total chlorine in milk was determined via the molecular absorption of diatomic strontium monochloride at 635.862 nm using high-resolution continuum source graphite furnace atomic absorption spectrometry. The effects of coating the graphite furnace, using different modifiers, amount of molecule-forming element, and different calibrants were investigated and optimized. Chlorine concentrations in milk samples were determined in a Zr-coated graphite furnace using 25 μg of Sr as the molecule-forming reagent and applying a pyrolysis temperature of 600 °C and a molecule-forming temperature of 2300 °C. Linearity was maintained up to 500 μg mL(-1) of Cl. The method was tested by analyzing a certified reference wastewater. The results were in the uncertainty limits of the certified value. The limit of detection of the method was 1.76 μg mL(-1). The chlorine concentrations in various cow milk samples taken from the market were found in the range of 588-1472 mg L(-1). PMID:27345208

  17. 原子吸收光谱技术在重元素测定方面的应用%Applications of Atomic Absorption Spectrometry in Determination of Heavy Elements

    韦鑫

    2012-01-01

    Heavy metal elements such as copper, lead, cobalt, manganese, cadmium, and mercury were closely re- lated to the human body health. If more than a certain concentration, it can cause harm to the human body. Atomic ab- sorption spectrometric (AAS) method was generally used to the determination of heavy metal elements. The atomic ab-sorption technique used in heavy metal was introduced from the applications of AAS.%重金属元素如铜、铅、钴、锰、镉、汞等如果超过一定的浓度会对人体产生危害,与人的身体健康可谓是息息相关。原子吸收光谱法一般用来测定样品中的重金属元素,本文从原子吸收光谱的应用等方面简单介绍了原子吸收技术在重金属研究方面的应用。

  18. A COMPARISON OF A SPECTROPHOTOMETRIC (QUERCETIN) METHOD AND AN ATOMIC-ABSORPTION METHOD FOR DETERMINATION OF TIN IN FOOD

    Engberg, Å

    1973-01-01

    Procedures for the determination of tin in food, which involve a spectrophotometric method (with the quercetin-tin complex) and an atomic-absorption method, are described. The precision of the complete methods and of the individual analytical steps required is evaluated, and the parameters that...

  19. Determination of metallic impurities in uranium compounds of nuclear purity by atomic absorption spectrophotometry with electrothermal atomization

    Atomic absorption spectrometry, with electrothermal atomization, has been used for the determination of Al, Cd, Cr, Fe, Mn and Ni in uranium oxide standards. The analysis were performed without sample dissolution and without uranium chemical separation. This technique is adequate for the qualification of uranium of nuclear purity according to the standard specifications. (Author)

  20. Determination of total selenium in nutritional supplements and selenised yeast by Zeeman-effect graphite furnace atomic absorption spectrometry

    Larsen, Erik Huusfeldt; Ekelund, J.

    1989-01-01

    -effect background corrected graphite furnace atomic absorption spectrometry. A furnace ashing step at 1100 °C was necessary in order to obtain a total recovery of selenium when present in the organic form. Palladium nitrate-magnesium nitrate was used as a matrix modifier. Independent methods were used to determine...

  1. Determination of arsenic and cadmium in crude oil by direct sampling graphite furnace atomic absorption spectrometry

    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

  2. Matrix elimination method for the determination of precious metals in ores using electrothermal atomic absorption spectrometry.

    Salih, Bekir; Celikbiçak, Omür; Döker, Serhat; Doğan, Mehmet

    2007-03-28

    Poly(N-(hydroxymethyl)methacrylamide)-1-allyl-2-thiourea) hydrogels, poly(NHMMA-ATU), were synthesized by gamma radiation using (60)Co gamma source in the ternary mixture of NHMMA-ATU-H(2)O. These hydrogels were used for the specific gold, silver, platinum and palladium recovery, pre-concentration and matrix elimination from the solutions containing trace amounts of precious metal ions. Elimination of inorganic matrices such as different transition and heavy metal ions, and anions was performed by adjusting the solution pH to 0.5 that was the selective adsorption pH of the precious metal ions. Desorption of the precious metal ions was performed by using 0.8 M thiourea in 3M HCl as the most efficient desorbing agent with recovery values more than 95%. In the desorption medium, thiourea effect on the atomic signal was eliminated by selecting proper pyrolysis and atomization temperatures for all precious metal ions. Precision and the accuracy of the results were improved in the graphite furnace-atomic absorption spectrometer (GFAAS) measurements by applying the developed matrix elimination method performing the adsorption at pH 0.5. Pre-concentration factors of the studied precious metal ions were found to be at least 1000-fold. Detection limits of the precious metal ions were found to be less than 10 ng L(-1) of the all studied precious metal ions by using the proposed pre-concentration method. Determination of trace levels of the precious metals in the sea-water, anode slime, geological samples and photographic fixer solutions were performed using GFAAS clearly after applying the adsorption-desorption cycle onto the poly(NHMMA-UTU) hydrogels. PMID:17386783

  3. Lead and cadmium determinations by atomic absorption technique in biological samples: blood, placenta and umbilical cord

    In order to determine the possibility contamination of lead and cadmium in pregnant women living in the mining-smelting city of La Oroya in Peru, lead and cadmium concentrations were assessed in maternal blood (pre-birth), umbilical cord blood and placental tissue. Forty deliveries with normal evolution were evaluated between October 2002 and January 2003. Samples were analyzed by atomic absorption on a graphite furnace at the Peruvian Institute of Nuclear Energy (IPEN) laboratories. Results are summarized as follows: a) Mean lead concentrations in maternal blood (MB), umbilical cord blood (UCB) and placental tissue (PT) were 27.23 μg/dL, 18.48 μg/dL and 363.97 μg/100g, respectively; b) Mean cadmium concentrations in MB, UCB and PT were 8.82 μg/dL, 12,0 μg/dL and 104,44 μg/100g, respectively; c) The correlation coefficient between lead concentration in maternal blood and umbilical cord was 0.122; d). The correlation coefficient of cadmium concentration between MB and UCB was 0.223; e). The correlation coefficient of lead concentration between MB and PT was 0.189; f). The correlation coefficient of cadmium concentration between MB and PT was 0.633. Trans-placental transport of lead was 67.84% (27,23 μg/dL in MB vs. 18.48 μg/dL in UCB); whereas in the case of cadmium, the concentration in UC (12,00 μg/dL) was greater than in MB (8.82 μg/dL.). These results could indicate that the placenta acts as a barrier trapping lead and cadmium. This barrier is efficient for lead since the concentration in cord blood is inferior to maternal blood but it is less efficient for cadmium. (author)

  4. Direct determination of lead in sweet fruit-flavored powder drinks by electrothermal atomic absorption spectrometry

    Lima, Éder C.; Krug, Francisco José; Arruda, Marco A. Z.

    1998-04-01

    A simplified method for direct determination of lead in sweet fruit-flavored powder drinks, syrups and honeys by electrothermal atomic absorption spectrometry without sample digestion is proposed. Samples were dissolved in water, acidified to 0.2% (v/v) HNO 3, and directly injected into an end-capped transversely heated graphite atomizer (THGA). Building up of carbonaceous residue inside the atomizer was effectively precluded for sugar solutions not exceeding 8.0% (m/v) when a heating program with two pyrolysis steps (600 and 1000°C) was carried out without air-ashing. Under these conditions one atomizer supported about 250 firings. Among various chemical modifiers tested, better recovery and repeatability results were obtained with a 5 μg Pd + 3 μg Mg(NO 3) 2 mixture. Tests carried out with individual concomitants containing up to 1.0 μg Na, K, Ca or Cl, and up to 10.0 μg phosphate or sulphate, and several mixtures of these six concomitants, did not reveal significant interferences on lead atomization. Characteristic mass and detection limit based on integrated absorbance were 15 and 11 pg Pb, respectively. The relative standard deviation based on 10 measurements for typical samples (20-60 ng g -1 Pb) was always lower than 5.5%. The detection limit of 7.0 ng g -1 Pb attained the Codex recommendation for the maximum allowed lead contents in the sugar samples. Application of t-test to the results obtained by the proposed direct analysis, and the official method adopted by Food Chemical Codex, demonstrated that there were no significant differences at the 5% probability level.

  5. Matrix elimination method for the determination of precious metals in ores using electrothermal atomic absorption spectrometry

    Poly(N-(hydroxymethyl)methacrylamide)-1-allyl-2-thiourea) hydrogels, poly(NHMMA-ATU), were synthesized by gamma radiation using 60Co γ source in the ternary mixture of NHMMA-ATU-H2O. These hydrogels were used for the specific gold, silver, platinum and palladium recovery, pre-concentration and matrix elimination from the solutions containing trace amounts of precious metal ions. Elimination of inorganic matrices such as different transition and heavy metal ions, and anions was performed by adjusting the solution pH to 0.5 that was the selective adsorption pH of the precious metal ions. Desorption of the precious metal ions was performed by using 0.8 M thiourea in 3 M HCl as the most efficient desorbing agent with recovery values more than 95%. In the desorption medium, thiourea effect on the atomic signal was eliminated by selecting proper pyrolysis and atomization temperatures for all precious metal ions. Precision and the accuracy of the results were improved in the graphite furnace-atomic absorption spectrometer (GFAAS) measurements by applying the developed matrix elimination method performing the adsorption at pH 0.5. Pre-concentration factors of the studied precious metal ions were found to be at least 1000-fold. Detection limits of the precious metal ions were found to be less than 10 ng L-1 of the all studied precious metal ions by using the proposed pre-concentration method. Determination of trace levels of the precious metals in the sea-water, anode slime, geological samples and photographic fixer solutions were performed using GFAAS clearly after applying the adsorption-desorption cycle onto the poly(NHMMA-UTU) hydrogels

  6. Comparison between POES energetic electron precipitation observations and riometer absorptions: Implications for determining true precipitation fluxes

    Rodger, Craig J.; Kavanagh, Andrew J.; Clilverd, Mark A.; Marple, Steve R.

    2013-12-01

    electron precipitation (EEP) impacts the chemistry of the middle atmosphere with growing evidence of coupling to surface temperatures at high latitudes. To better understand this link, it is essential to have realistic observations to properly characterize precipitation and which can be incorporated into chemistry-climate models. The Polar-orbiting Operational Environmental Satellite (POES) detectors measure precipitating particles but only integral fluxes and only in a fraction of the bounce loss cone. Ground-based riometers respond to precipitation from the whole bounce loss cone; they measure the cosmic radio noise absorption (CNA), a qualitative proxy with scant direct information on the energy flux of EEP. POES observations should have a direct relationship with ΔCNA and comparing the two will clarify their utility in studies of atmospheric change. We determined ionospheric changes produced by the EEP measured by the POES spacecraft in ~250 overpasses of an imaging riometer in northern Finland. The ΔCNA modeled from the POES data is 10-15 times less than the observed ΔCNA when the >30 keV flux is reported as <106 cm-2 s-1 sr-1. Above this level, there is relatively good agreement between the space-based and ground-based measurements. The discrepancy occurs mostly during periods of low geomagnetic activity, and we contend that weak diffusion is dominating the pitch angle scattering into the bounce loss cone at these times. A correction to the calculation using measurements of the trapped flux considerably reduces the discrepancy and provides further support to our hypothesis that weak diffusion leads to underestimates of the EEP.

  7. Determination of Arsenic in Palm Kernel Expeller using Microwave Digestion and Graphite Furnace Atomic Absorption Spectrometry Method

    Abdul Niefaizal Abdul Hammid; Ainie Kuntom; RazaIi Ismail; Norazilah Pardi

    2013-01-01

    A study on the method to determine arsenic in palm kernel expeller wascarried out. Microwave digestion technique is widely applied in the analytical chemistry field. In comparison to conventional sample digestion method, the microwave technique is simple, reduced contamination, usage of safe reagent and matrix completely digested. A graphite furnace atomic absorption spectrometry method was used for the total determination of arsenic in palm kernel expeller. Arsenic was extracted from palm ke...

  8. Determination of attenuation coefficient for self-absorption correction in routine gamma ray spectrometry of environmental bulk sample

    A simple method to determine γ-ray attenuation coefficients using Ba-133 γ-rays was developed and applied to self-absorption correction in routine γ-ray spectrometry for environmental samples composed of unknown matrix elements. Experimental values of the mass attenuation coefficient obtained by the method agree well with calculated values for samples of known elemental composition which was determined by means of chemical analysis. (author)

  9. Mass Spectrometric Analysis of Water-soluble Gold Nanoclusters

    Batches of water-soluble gold nanoclusters of nominal 2.0 or 3.5-nm diameter were prepared to evaluate particle size determinations by a number of techniques such as transmission electron microscopy or atomic force microscopy and to validate estimates derived by mass spectrometric analysis using matrix-assisted laser desorption ionization (MALDI). Good agreement was found and MALDI lends itself to analyses even in the presence of aggregates

  10. Electrospray Ionization Mass Spectrometric Analysis of Highly Reactive Glycosyl Halides

    Lajos Kovács

    2012-07-01

    Full Text Available Highly reactive glycosyl chlorides and bromides have been analysed by a routine mass spectrometric method using electrospray ionization and lithium salt adduct-forming agents in anhydrous acetonitrile solution, providing salient lithiated molecular ions [M+Li]+, [2M+Li]+ etc. The role of other adduct-forming salts has also been evaluated. The lithium salt method is useful for accurate mass determination of these highly sensitive compounds.

  11. Determination of Pb in Biological Samples by Graphite Furnace Atomic Absorption Spectrophotometry: An Exercise in Common Interferences and Fundamental Practices in Trace Element Determination

    Spudich, Thomas M.; Herrmann, Jennifer K.; Fietkau, Ronald; Edwards, Grant A.

    2004-01-01

    An experiment is conducted to ascertain trace-level Pb in samples of bovine liver or muscle by applying graphite furnace atomic absorption spectrophotometry (GFAAS). The primary objective is to display the effects of physical and spectral intrusions in determining trace elements, and project the usual methods employed to minimize accuracy errors…

  12. Slurry sampling procedure for the determination of lead in human hair by electrothermal atomic absorption spectrometry

    Complete text of publication follows. Human hair is a stable matrix that presents numerous advantages for human biomonitoring, such as easy collection, low cost, easy transport and storage, information about short- and long-term exposure (Angerer J et al., Int. J. Hyg. Environ. Health, 2007, 201-228). The use of the slurry sampling procedure was applied for the determination of lead in human hair by electrothermal atomic absorption spectrometry (ETAAS). This technique presents high sensitivity, low cost and the possibility of direct determination. Hair samples were pulverized using a cryogenic mill. Ten milligrams of the hair powder were transferred into a polyethylene vial and 2 ml of 2.5% HNO3 and 1.5% H2O2 were added. The slurries were maintained homogeneous with air bubbling with an aquarium pump. Niobium and Rhodium were chosen from several potential permanent modifiers by evaluating the background and absorbance signals obtained under the conditions recommended by the manufacturer. A 23 factorial design and a central composite design (CCD) were realized to optimize permanent modifier and pyrolysis and atomization temperatures. The parameters of merit were obtained in the optimized conditions (Tp = 660 deg C, Ta = 1780 deg C and Rh), and they were as follows: linear working range up to 50 μg L-1; limit of detection (0.032 0.002) μg g-1; limit of quantification (0.106 0.005) μg g-1; matrix-matched calibration, with r2 > 0.99 and reproducibility ranged from 2.3 to 4.2 relative standard deviation (RSD). The accuracy was evaluated by recovery tests and comparing slurry sampling and microwave decomposition. The recovery values for different concentrations were in the range between 89 and 101% and non-significant differences were observed (t-test; p = 0.05) when comparing the average of lead values obtained from microwave decomposition method and proposed method. Lead concentrations in different samples ranged between 0.13 and 1.11 μg g-1. The authors kindly

  13. Simultaneous determination of cadmium and lead in wine by electrothermal atomic absorption spectrometry

    Freschi, Gian P. G.; Dakuzaku, Carolina S.; de Moraes, Mercedes; Nóbrega, Joaquim A.; Gomes Neto, José A.

    2001-10-01

    A method has been developed for the direct simultaneous determination of Cd and Pb in white and red wine by electrothermal atomic absorption spectrometry (ET-AAS) using a transversely heated graphite tube atomizer (THGA) with longitudinal Zeeman-effect background correction. The thermal behavior of both analytes during pyrolysis and atomization stages were investigated in 0.028 mol l -1 HNO 3 and in 1+1 v/v diluted wine using mixtures of Pd(NO 3) 2+Mg(NO 3) 2 and NH 4H 2PO 4+Mg(NO 3) 2 as chemical modifiers. With 5 μg Pd+3 μg Mg as the modifiers and a two-step pyrolysis (10 s at 400°C and 10 s at 600°C), the formation of carbonaceous residues inside the atomizer was avoided. For 20 μl of sample (wine+0.056 mol l -1 HNO 3, 1+1, v/v) dispensed into the graphite tube, analytical curves in the 0.10-1.0 μg l -1 Cd and 5.0-50 μg l -1 Pb ranges were established. The characteristic mass was approximately 0.6 pg for Cd and 33 pg for Pb, and the lifetime of the tube was approximately 400 firings. The limits of detection (LOD) based on integrated absorbance (0.03 μg l -1 for Cd, 0.8 μg l -1 for Pb) exceeded the requirements of Brazilian Food Regulations (decree #55871 from Health Department), which establish the maximum permissible level for Cd at 200 μg l -1 and for Pb at 500 μg l -1. The relative standard deviations ( n=12) were typically <8% for Cd and <6% for Pb. The recoveries of Cd and Pb added to wine samples varied from 88 to 107% and 93 to 103%, respectively. The accuracy of the direct determination of Cd and Pb was checked for 10 table wines by comparing the results with those obtained for digested wine using single-element ET-AAS, which were in agreement at the 95% confidence level.

  14. Determination of metallic elements in water by the combined preconcentration techniques of ion exchange and atomic absorption spectrophotometry

    Having as an aim the utilization of atomic absorption method with flame's excitement, the limits of detection in water of six metals (Ag, Co, Cr, Cu, Ni, Zn) were determined in synthetical samples through atomic absorption spectroscopy. Techniques to optimize the data have been pointed out and presented their statistical treatment. By means of the routine and the addition methods three 'real' samples have also been analysed in order to determine the contents of Cu and Zn. Aiming a pre-concentration and by utilizing the 60Co obtained activating a sample of cobalt in the CDTN/NUCLEBRAS TRIGA MARK-I reactor, the retainement of this cobalt in ion exchange resin and the variation of the factor of elution within different concentration of HCl in water have been determined. The limits of detection are presented and so are the quantitative ones, with and without pre-concentration in an ion exchanger resin and latter elution. (Author)

  15. Direct determination of selenium in rat blood plasma by Zeeman atomic absorption spectrometry.

    Kabirov, K K; Kapetanovic, I M; Lyubimov, A V

    2008-01-30

    The method was developed to be applied for direct determination of selenium in rat plasma by graphite-furnace atomic absorption spectrometry with Zeeman background correction. Blood was obtained from CD rats of both sexes 2h after dosing in weeks 7 and 13 in order to acquire data on the levels of selenium in these animals during 13-week gavage administration of l-seleno-methylselenocysteine (SeMC), a new candidate chemopreventive agent under development. Application of the commonly used method of standard addition was found to be unsuitable to calculate the selenium content in rat plasma (within-run and between-run accuracy and precision parameters were less than 85%). Therefore, a new analytical method was developed. In this method, samples of rat plasma (50 microL) were diluted 10-fold with a reducing agent containing l-ascorbic acid, a modifier solution containing palladium chloride and Triton X-100. Samples were atomized in pyrolytically coated graphite tubes and peak height signals were measured. Selenium concentrations were determined by linear least squares regression analysis based on the standard curve generated in pooled rat blank plasma. Since selenium is normally present in plasma, a three-step approach was used to calculate selenium plasma levels. Initially selenium levels were determined based on the standard curve with selenium-spiked pool plasma. In the second step, background selenium levels in the pooled plasma were determined based on the same standard curve. In the third step, background level was added to the previously derived number. The relative errors were in the range from -4.6 to 11.4% (intra-day assay) and from -0.4 to 8.8% (inter-day assay) which proved good accuracy. The relative standard deviations were in the range from 1.88 to 4.70% (intra-day precision) and from 3.28 to 5.38% (inter-day precision). In rat plasma, the following dose-dependent selenium levels (mean+/-S.D.) in males and females, respectively, were observed at 13 weeks

  16. Novel ratio difference at coabsorptive point spectrophotometric method for determination of components with wide variation in their absorptivities

    Saad, Ahmed S.; Abo-Talib, Nisreen F.; El-Ghobashy, Mohamed R.

    2016-01-01

    Different methods have been introduced to enhance selectivity of UV-spectrophotometry thus enabling accurate determination of co-formulated components, however mixtures whose components exhibit wide variation in absorptivities has been an obstacle against application of UV-spectrophotometry. The developed ratio difference at coabsorptive point method (RDC) represents a simple effective solution for the mentioned problem, where the additive property of light absorbance enabled the consideration of the two components as multiples of the lower absorptivity component at certain wavelength (coabsorptive point), at which their total concentration multiples could be determined, whereas the other component was selectively determined by applying the ratio difference method in a single step. Mixture of perindopril arginine (PA) and amlodipine besylate (AM) figures that problem, where the low absorptivity of PA relative to AM hinders selective spectrophotometric determination of PA. The developed method successfully determined both components in the overlapped region of their spectra with accuracy 99.39 ± 1.60 and 100.51 ± 1.21, for PA and AM, respectively. The method was validated as per the USP guidelines and showed no significant difference upon statistical comparison with reported chromatographic method.

  17. Gamow-Teller decay and nuclear deformation: implementing of a new total absorption spectrometer, study of isotopes N {approx_equal} Z krypton and strontium; Decroissance Gamow-Teller et deformation nucleaire: mise en oeuvre d'un nouveau spectrometre a absorption totale, etude d'isotopes N {approx_equal} Z de krypton et strontium

    Poirier, E

    2002-12-01

    Nuclei with A {approx} 70 along the N=Z line are known to be the scene of phenomena closely related to the nuclear deformation and are of particular interest since theoretical mean field calculations predict that a large part of the Gamow-Teller resonance might be located below the ground state of the mother nucleus and then be accessible through {beta}-decay studies. These results have shown the effect of the shape of the ground state on the intensity of the Gamow-Teller strength. Thus, the experimental determination, through {delta}-decay, of the Gamow-Teller strength distribution and the comparison to the theoretical predictions allow to pin down the quadrupolar deformation parameter of the ground state of the parent nucleus. In order to study the neutron deficient isotopes of krypton (A=72,73,74,75) and strontium (A=76,77,78) and to establish the {beta}-strength on the full energy range, a new total absorption spectrometer (TAgS) has been built in the frame of an international collaboration and installed at the (SOLDE/CERN mass separator. For the data analysis, the response function R of the spectrometer has been calculated by means of Monte-Carlo simulations, based on the GEANT4 code, and of a statistical description of the level scheme in the daughter nucleus. The {beta}-feeding distribution has been obtained from experimental spectra through a method based on Bayes theorem and then converted into Gamow-Teller strength. The results coming from the {sup 74}Kr decay analysis allow to describe the ground state of such a nucleus as the coexistence of an oblate shape and of a prolate shape. In the case of {sup 76}Sr, the experimental Gamow-Teller strength distribution strongly indicates a prolate deformation. (author)

  18. Analytical algorithm to determine the spherical particle size distribution from spectral absorption measurements

    Zhao, Jian-Qi; Li, Jiangnan

    2015-11-01

    A modified anomalous diffraction theory (MADT) by including the effects of reflection and refraction is proposed. With respect to MADT, an analytical technique for retrieval of spherical particle size distribution (PSD), based on absorption was developed. Also, an MADT transform pair between the size distribution and the absorption spectrum was constructed. This provides a new tool to study the related particle optical properties. By Gaver-Stehfest inversion method, the derived complex-inversion formula is finally converted into the new real-inversion formula so that the measured absorption data can be applied directly. The inversion experiments show that the use of extended precision instead of double precision arithmetic can produce more reliable results at the expense of CPU time. The effects of complex refractive index on retrieval of PSD were examined. Also it was found that an appropriate reduction of the truncation number with the smoothing technique improved the anti-noise ability for the algorithm.

  19. Solvent sublation and spectrometric determination of iron(II) and total iron using 3-(2-pyridyl)-5,6-bis(4-phenylsulfonic acid)-1,2,4-triazine and tetrabutylammonium bromide.

    Akl, Magda Ali; Mori, Yoshihito; Sawada, Kiyoshi

    2006-09-01

    Solvent sublation has been studied for the separation and determination of trace iron(II) in various kinds of water samples. A strongly magenta-colored anionic [Fe(FZ)3](4-) complex was formed at pH 5.0 upon adding 3-(2-pyridyl)-5,6-bis(4-phenylsulfonic acid)-1,2,4-triazine (ferrozine, FZ) to the sample solution. Tetrabutylammonium bromide (TBAB) was added in the solution to form the (TBA)4[Fe(FZ)3)] ion pair, and an oleic acid (HOL) surfactant was added. Then, the (TBA)4[Fe(FZ)3] ion pairs were floated by vigorous shaking in the flotation cell and extracted into methyl isobutyl ketone (MIBK) on the surface of the aqueous solution. The iron collected in the MIBK layer was measured directly by spectrophotometry and/or flame atomic-absorption spectrophotometry. Different experimental variables that may affect the sublation efficiency were thoroughly investigated. The molar absorptivity of the (TBA)4[Fe(FZ)3] ion pair was 2.8 x 10(4) l mol(-1) cm(-1) in the aqueous layer. Beer's law held up to 1.0 mg L(-1) Fe(II) in the aqueous as well as in the organic layers. The adopted solvent sublation method was successfully applied for the determination of Fe(II) in natural water samples with a preconcentration factor of 200. The application was extended to determine iron in pharmaceutical samples. PMID:16966804

  20. Fluorine determination in coal using high-resolution graphite furnace molecular absorption spectrometry and direct solid sample analysis

    The absorption of the calcium mono-fluoride (CaF) molecule has been employed in this study for the determination of fluorine in coal using direct solid sample analysis and high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS). The rotational line at 606.440 nm was used for measuring the molecular absorption in the gas phase. The pyrolysis and vaporization temperatures were 700 °C and 2100 °C, respectively. Different chemical modifiers have been studied, such as Pd and Ir as permanent modifiers, and Pd and the mixed Pd/Mg modifier in solution. The limit of detection and the characteristic mass were 0.3 and 0.1 ng F, respectively. One certified reference material (CRM) of coal (NIST 1635) and four CRMs with a non-certified value for F (SARM 18, SARM 20, BCR 40, BCR 180) were used to evaluate the accuracy and precision of the method, obtaining good agreement (104%) with the certified value and with the informed values (ranging from 90 to 103%). - Highlights: • High-resolution Graphite Furnace Molecular Absorption Spectrometry (HR-GF MAS) • Fluorine has been determined using HR-GF MAS of the CaF molecule. • The CaF molecule was generated in a graphite furnace at a temperature of 2100 °C • Coal samples have been analyzed using direct solid sample introduction. • Aqueous standard solutions have been used for calibration

  1. Fluorine determination in coal using high-resolution graphite furnace molecular absorption spectrometry and direct solid sample analysis

    Machado, Patrícia M.; Morés, Silvane; Pereira, Éderson R. [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Welz, Bernhard, E-mail: w.bernardo@terra.com.br [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil); Carasek, Eduardo [Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil); Andrade, Jailson B. de [Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, 40170-115 Salvador, BA (Brazil)

    2015-03-01

    The absorption of the calcium mono-fluoride (CaF) molecule has been employed in this study for the determination of fluorine in coal using direct solid sample analysis and high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS). The rotational line at 606.440 nm was used for measuring the molecular absorption in the gas phase. The pyrolysis and vaporization temperatures were 700 °C and 2100 °C, respectively. Different chemical modifiers have been studied, such as Pd and Ir as permanent modifiers, and Pd and the mixed Pd/Mg modifier in solution. The limit of detection and the characteristic mass were 0.3 and 0.1 ng F, respectively. One certified reference material (CRM) of coal (NIST 1635) and four CRMs with a non-certified value for F (SARM 18, SARM 20, BCR 40, BCR 180) were used to evaluate the accuracy and precision of the method, obtaining good agreement (104%) with the certified value and with the informed values (ranging from 90 to 103%). - Highlights: • High-resolution Graphite Furnace Molecular Absorption Spectrometry (HR-GF MAS) • Fluorine has been determined using HR-GF MAS of the CaF molecule. • The CaF molecule was generated in a graphite furnace at a temperature of 2100 °C • Coal samples have been analyzed using direct solid sample introduction. • Aqueous standard solutions have been used for calibration.

  2. Determination of Self - absorption Corrections Factor for Radioactivity Measurement of Seawater and Plankton Samples by Gross α/β Counter

    In environmental survey, gross alpha/beta activity is one of the parameters to be determined and used to decide whether further radiological analyses are necessary. To obtain correct results, samples shall be counted under the same conditions (geometric setup, chemical composition, density). If not possible, the self absorption corrections factor was necessary. In this study, sea water and plankton samples were prepared by coprecipitation and filtration, respectively. The standards used to determine the self-absorption corrections factor were prepared by adding 243Am and 90Sr, respectively for standard gross alpha and gross beta, to distilled water and varying the amount of carriers to increase the weight of final precipitates and filtrates. The range of weight obtained was 20 to 75 mg. The self-absorption corrections factor was calculated using the following equation. Fa = Ex/E0 where Fa is the absorption corrections factor, Ex is the mean efficiency of the different points of the curve and E0 is the mean efficiency of the first point of the curve. The mass thickness of studied range have effect on the counting of gross alpha/beta in plankton samples and gross alpha in seawater samples and caused no effect of gross beta counting in seawater samples.

  3. Determination of trace impurities in titanium dioxide by direct solid sampling electrothermal atomic absorption spectrometry

    Vojtková, Blanka; Dočekal, Bohumil

    2005-01-01

    Roč. 99, S (2005), s489-s491. ISSN 0009-2770. [Meeting on Chemistry and Life /3./. Brno, 20.09.2005-22.09.2005] Institutional research plan: CEZ:AV0Z40310501 Keywords : solid sampling * electrothermal atomic absorption spectrometry * trace analysis Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 0.445, year: 2005

  4. Determination of absorption efficiency of side pumped Nd:YAG laser and effect of pumped polarization

    Three and four array side pumped diode lasers are considered for Nd:YAG rod. The pumped beams are designed to illuminate the rod symmetrically. The effect of P and S polarization on the rod absorption efficiency as a function of light illumination (slit width) is also calculated.

  5. Determination of the dipole moment of OCS with a microwave absorption cavity

    Dijkerman, H.A.; Ruitenberg, G.

    1969-01-01

    The electric dipole moment of OCS has been measured with a resonance cavity as a Stark absorption cell. The result: μOCS = 0.7149 ± 0.0003. Debye agrees well with the dipole moment data obtained with an electric resonance beam experiment.

  6. Direct determination of fluorine in niobium oxide using slurry sampling electrothermal high-resolution continuum source molecular absorption spectrometry

    Aiming for a round-robin test, a new method for the direct determination of fluorine in niobium oxide has been developed. It is based on the use of high-resolution molecular absorption spectra of calcium mono-fluoride (CaF) generated in the graphite tube, combined with the slurry sampling technique. The absorption measurement was performed at the 606.44 nm CaF rotational line. By using graphite tubes with zirconium carbide (ZrC) modified platform, the molecular absorption sensitivity of CaF has been improved by a factor of 20, and no additional chemical modifier was necessary. Generally, non-spectral interferences were observed in the presence of HCl, H2SO4, and H3PO4. For HCl, additional spectral interference occurred due to an overlap of the absorption spectra of CaF and CaCl. However, due to the absence of these mentioned substances in the current material, such interferences do not exist for this application. The characteristic mass found for the CaF 606.44 nm line was 0.1 ng; the limit of detection was 5 mg fluorine per kg solid sample (3σ criterion). The results obtained by the method were within the range of certified values. Comparing to the classical method such as the pyrohydrolysis-photometric method, the developed new method showed clear advantages regarding sensitivity and specificity. The time requirement for one sample analysis was strongly shortened from several hours to only some minutes. - Highlights: • First time determination of fluorine in niobium oxide using the slurry sampling technique • Application of calcium fluoride molecular absorption in graphite tube with ZrC modification • Higher specificity, better sensitivity, and huge time saving compared with the classical method based on pyrohydrolysis • New method verified by successful participation in round robin test

  7. Direct determination of fluorine in niobium oxide using slurry sampling electrothermal high-resolution continuum source molecular absorption spectrometry

    Huang, Mao Dong; Becker-Ross, Helmut [Leibniz-Institut für Analytische Wissenschaften—ISAS—e.V., Department Berlin, Albert-Einstein-Str. 9, 12489 Berlin (Germany); Okruss, Michael, E-mail: michael.okruss@isas.de [Leibniz-Institut für Analytische Wissenschaften—ISAS—e.V., Department Berlin, Albert-Einstein-Str. 9, 12489 Berlin (Germany); Geisler, Sebastian; Florek, Stefan [Leibniz-Institut für Analytische Wissenschaften—ISAS—e.V., Department Berlin, Albert-Einstein-Str. 9, 12489 Berlin (Germany); Richter, Silke; Meckelburg, Angela [BAM Federal Institute for Materials Research and Testing, Department of Analytical Chemistry, Reference Materials, Richard-Willstätter-Str. 11, 12489 Berlin (Germany)

    2014-04-01

    Aiming for a round-robin test, a new method for the direct determination of fluorine in niobium oxide has been developed. It is based on the use of high-resolution molecular absorption spectra of calcium mono-fluoride (CaF) generated in the graphite tube, combined with the slurry sampling technique. The absorption measurement was performed at the 606.44 nm CaF rotational line. By using graphite tubes with zirconium carbide (ZrC) modified platform, the molecular absorption sensitivity of CaF has been improved by a factor of 20, and no additional chemical modifier was necessary. Generally, non-spectral interferences were observed in the presence of HCl, H{sub 2}SO{sub 4}, and H{sub 3}PO{sub 4}. For HCl, additional spectral interference occurred due to an overlap of the absorption spectra of CaF and CaCl. However, due to the absence of these mentioned substances in the current material, such interferences do not exist for this application. The characteristic mass found for the CaF 606.44 nm line was 0.1 ng; the limit of detection was 5 mg fluorine per kg solid sample (3σ criterion). The results obtained by the method were within the range of certified values. Comparing to the classical method such as the pyrohydrolysis-photometric method, the developed new method showed clear advantages regarding sensitivity and specificity. The time requirement for one sample analysis was strongly shortened from several hours to only some minutes. - Highlights: • First time determination of fluorine in niobium oxide using the slurry sampling technique • Application of calcium fluoride molecular absorption in graphite tube with ZrC modification • Higher specificity, better sensitivity, and huge time saving compared with the classical method based on pyrohydrolysis • New method verified by successful participation in round robin test.

  8. Determination of trace amounts of selenium in minerals and rocks by flame less atomic-absorption spectrometry

    The determination of trace amounts of selenium In silicate rocks and feldspar by solvent extraction and graphite furnace atomic-absorption spectrometry has been stu- died. Sodium diethyl-ditio carbamate and ammonium pyrrolidine dithiocarbamate have been tried as chelating agents. The best results are achieved when selenium is extracted Into carbon tetrachloride as the sodium diethyldithiocarbamate complex. The method allows to detect 0,75 ppm of selenium in the sample. Recoveries are about 100%. (Author) 7 refs

  9. Dispersive Liquid-Liquid Microextraction of Bismuth in Various Samples and Determination by Flame Atomic Absorption Spectrometry

    Teslima Daşbaşı; Şenol Kartal; Şerife Saçmacı; Ahmet Ülgen

    2016-01-01

    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 ...

  10. Determination of Copper-Based Fungicides by Flame Atomic Absorption Spectrometry Using Digestion Procedure with Sulfuric and Nitric Acid

    Jelena Milinović; Rada Đurović

    2007-01-01

    Copper-based fungicides can be effectively digested by treatment with a mixture of concentrated sulfuric and nitric acid in exactly 15 minutes for the rapid determination via copper using flame atomic absorption spectrometry (AAS). Under optimum conditions, the results of copper fungicide analysis were consistent to those obtained by the AOAC’s recommended method. Recovery values ranged from 98.63 to 103.40%. Relative standard deviation values are lower than 2%. The proposed digestion procedu...

  11. Determination of Trace Silver in Water Samples by Online Column Preconcentration Flame Atomic Absorption Spectrometry Using Termite Digestion Product

    Joyce Nunes Bianchin; Eduardo Carasek; Edmar Martendal

    2011-01-01

    A new method for Ag determination in water samples using solid phase extraction (SPE) coupled to a flow injection system and flame atomic absorption spectrometry was developed. The sorbent used for Ag preconcentration and extraction was the termite digestion product. Flow and chemical variables of the system were optimized through a multivariate procedure. The factors selected were adsorbent mass, buffer type and concentration, sample pH, and sample flow rate. The detection limit and precisio...

  12. Determination of the total photo-absorption cross section of 197Au from (γ,chin) reaction cross sections

    Cross sections for the reaction 197Au(γ, chin)(chi<=12) have been measured for bremsstrahlung end-point energies in the range 60-340 MeV. From these dominant cross sections, the total photon absorption cross section is determined using a cascade-evaporation calculation to account for the missing reaction channels. The enhancement factor for the classical E1 sum rule is found to be 0.93+-0.10. (orig.)

  13. Determination of the relative concentrations of rare earth ions by x-ray absorption spectroscopy: Application to terbium mixed oxides

    Laan, van der, Paul Maarten; Fuggle, J.C.; van Dijk; Burggraaf, A.J.; Esteva, J.-M.; Karnatak, R.

    1986-01-01

    A method, based on X-ray absorption spectroscopy (XAS) in the range 0.8–1.5 keV, to determine the relative amounts of rare earth ions in different valencies is explained and tested for the case of terbium mixed oxides. The results are in agreement with those obtained by existing analytical methods. The XAS method is advantageous in that it can be applied where other, conventional, methods break down.

  14. Comparative investigation of sample preparation techniques for atomic-absorption determination of copper, nickel, cadmium in wood flour

    Comparative study of two methods of sample preparation (acid decomposition and dry calculation) for atomic-absorption content of copper, nickel and cadmium in wood flour, has been conducted. It is shown that for a certain content of copper and nickel (from 6 to 40 μg/g) it is recommended that the method of dry calcination is used, for cadmium determination (its content being 1-2 μg/g) both methods are applicable

  15. Comparative studies of method for determining total mercury in fish. Dithizone and flameless atomic absorption spectrophotometry techniques

    Two methods for determining total mercury in fish were compared: the dithizone and flameless atomic absorption spectrophotometry techniques. The studies involved determination of recovery when 1μg of mercury as solutions of HgCl2 or CH3HgC were added to each sample of herring flesh. Mean recoveries in the dithizone method were found to be 91.4+-7.47% and 90.25+-4.73% for the two solutions respectively, while the recoveries obtained with the flameless atomic absorption spectrophotometry were 95.00+-9.13% and 98.70+-7.14%, respectively. Both techniques were used to determine the mercury content in the same herring flesh sample. The first technique showed the content of 0.050+-0.018μg Hg g-1 while the result obtained with the other one was 0.062+-0.013μg Hg g-1. The statistical treatment of the results obtained showed no difference between the two techniques, the significance level being α=0.05. Therefore, the results obtained with the dithizone method are comparable with those obtained with the flameless atomic absorption spectrophotometry for mercury contents of the magnitude order of 0.050 ug.g-1. (author)

  16. Determination of site of absorption of propranolol in rat gut using In situ single-pass intestinal perfusion

    Nagare N

    2010-01-01

    Full Text Available Previously, permeability and site of intestinal absorption of propranolol have been reported using the Ussing chamber. In the present study, the utility of Single-Pass Intestinal Perfusion to study permeability and site of intestinal absorption of propranolol was evaluated in rats. Drug permeability in different regions of rat intestine viz. duodenum, jejunum, ileum and colon was measured. Propranolol (30 μg/ml solution was perfused in situ in each intestinal segment of rats. Effective permeability (Peff of propranolol in each segment was calculated and site of absorption was determined. The Peff of propranolol in rat duodenum, jejunum, ileum and colon was calculated to be 0.3316Χ10 -4 cm/s, 0.4035Χ10 -4 cm/s, 0.5092Χ10 -4 cm/s and 0.7167Χ10 -4 cm/s, respectively. The above results suggest that permeability of propranolol was highest through colon compared to other intestinal sites, which is in close agreement to that reported previously. In conclusion, in situ single pass intestinal perfusion can be used effectively to study intestinal permeability as well as site of intestinal absorption of compounds in rats.

  17. Direct determination of fluorine in niobium oxide using slurry sampling electrothermal high-resolution continuum source molecular absorption spectrometry

    Huang, Mao Dong; Becker-Ross, Helmut; Okruss, Michael; Geisler, Sebastian; Florek, Stefan; Richter, Silke; Meckelburg, Angela

    Aiming for a round-robin test, a new method for the direct determination of fluorine in niobium oxide has been developed. It is based on the use of high-resolution molecular absorption spectra of calcium mono-fluoride (CaF) generated in the graphite tube, combined with the slurry sampling technique. The absorption measurement was performed at the 606.44 nm CaF rotational line. By using graphite tubes with zirconium carbide (ZrC) modified platform, the molecular absorption sensitivity of CaF has been improved by a factor of 20, and no additional chemical modifier was necessary. Generally, non-spectral interferences were observed in the presence of HCl, H2SO4, and H3PO4. For HCl, additional spectral interference occurred due to an overlap of the absorption spectra of CaF and CaCl. However, due to the absence of these mentioned substances in the current material, such interferences do not exist for this application. The characteristic mass found for the CaF 606.44 nm line was 0.1 ng; the limit of detection was 5 mg fluorine per kg solid sample (3σ criterion). The results obtained by the method were within the range of certified values. Comparing to the classical method such as the pyrohydrolysis-photometric method, the developed new method showed clear advantages regarding sensitivity and specificity. The time requirement for one sample analysis was strongly shortened from several hours to only some minutes.

  18. Effect of Sn on the optical band gap determined using absorption spectrum fitting method

    Heera, Pawan, E-mail: sramanb70@mailcity.com [Department of Physics, Himachal Pradesh University, Shimla, INDIA, 171005 (India); Govt. College Amb, Himachal Pradesh, INDIA,177203 (India); Kumar, Anup, E-mail: kumar.anup.sml@gmail.com [Department of Physics, Himachal Pradesh University, Shimla, INDIA, 171005 (India); Physics Department, Govt. College, Kullu, H. P., INDIA, 175101 (India); Sharma, Raman, E-mail: pawanheera@yahoo.com [Department of Physics, Himachal Pradesh University, Shimla, INDIA, 171005 (India)

    2015-05-15

    We report the preparation and the optical studies on tellurium rich glasses thin films. The thin films of Se{sub 30}Te{sub 70-x} Sn{sub x} system for x= 0, 1.5, 2.5 and 4.5 glassy alloys prepared by melt quenching technique are deposited on the glass substrate using vacuum thermal evaporation technique. The analysis of absorption spectra in the spectral range 400nm–4000 nm at room temperature obtained from UV-VIS-NIR spectrophotometer [Perkin Elmer Lamda-750] helps us in the optical characterization of the thin films under study. The absorption spectrum fitting method is applied by using the Tauc’s model for estimating the optical band gap and the width of the band tail of the thin films. The optical band gap is calculated and is found to decrease with the Sn content.

  19. Procedure for intercomparison study for trace elements determination in soil samples by absorption spectroscopy

    In the environmental sampling analysis there is very important to establish an adequate methodologies on the laboratories for improvement the quality of the results obtained, so the establishment of a qualified laboratories network for environmental analysis. The objective of this work is to show the working plan for the analysis of eight elements on a Russian soil sample for an interlaboratory comparison with IAEA, by the Absorption spectroscopy technique using flame. (Author)

  20. Third order nonlinear optical susceptibility of fluorescein-containing polymers determined by electro-absorption spectroscopy

    Gomez-Sosa, Gustavo; Beristain, Miriam F.; Ortega, Alejandra; Martínez-Viramontes, Jaquelin; Ogawa, Takeshi; Fernández-Hernández, Roberto C.; Tamayo-Rivera, Lis; Reyes-Esqueda, Jorge-Alejandro; Isoshima, Takashi; Hara, Masahiko

    2012-03-01

    Novel polymers containing xanthene groups with high dye concentrations were prepared, and their third order nonlinear optical properties were studied by electroabsorption spectroscopy technique. The polymers were amorphous with refractive indices above 1.6 in the non-resonant region. The UV-Visible absorption spectra indicate the fluoresceins molecules in the polymers are H-aggregated. They showed third order nonlinear susceptibility, χ(3) (-ω:ω, 0, 0), of 2.5-3.5 × 10-12 esu.

  1. Convenient determination of luminescence quantum yield using a combined electronic absorption and emission spectrometer

    Prakash, John; Mishra, Ashok Kumar [Department of Chemistry, Indian Institute of Technology Madras, Chennai 600036 (India)

    2016-01-15

    It is possible to measure luminescence quantum yield in a facile way, by designing an optical spectrometer capable of obtaining electronic absorption as well as luminescence spectra, with a setup that uses the same light source and detector for both the spectral measurements. Employment of a single light source and single detector enables use of the same correction factor profile for spectral corrections. A suitable instrumental scaling factor is used for adjusting spectral losses.

  2. Standard test methods for chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade plutonium metal

    American Society for Testing and Materials. Philadelphia

    2004-01-01

    1.1 These test methods cover procedures for the chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade plutonium metal to determine compliance with specifications.

  3. Determination of U and Impurities Elements in The Uranium Tetra Fluoride by Potentiometric and Atomic Absorption Spectrophotometric Methods

    The determination of u and impurities contents in the Uranium tetra fluoride (UF4)has been carried out by potentiometric titration using modified 'Davies-Gray' and atomic absorption spectrophotometric methods. Dissolution process of the powder sample using saturated Al2(SO4)3 solution introduced to determine UF4 compound content in the UF4 sample. The uranium Content in the obtained filtrate is analyzed by potentiometric. The impurities content is determined by ato-Mic absorption spectrophotometric using ammonium oxalate powder in introducing of the sample preparation. The experiment covered the observation on influence of stirring time of UF4 sample dissolution in respect to separate UF4 from its impurities in determination of uranium content. Also the effects of Ammonium Oxalate added and agitating time were observed deal with the sample preparation for the determination of Impurities content.The analysis result found that UF4 content was 96.15 ± 0.04% the relative station 0.7%. However the best impurities determination was achieved by addition of ammonium oxalate powder and 15 Minutes of agitation time at temperature of 8000C

  4. Mass spectrometric detection, identification, and fragmentation of arseno-phytochelatins.

    Schmied-Tobies, Maria I H; Arroyo-Abad, Uriel; Mattusch, Jürgen; Reemtsma, Thorsten

    2014-11-01

    Phytochelatins (PC) are cystein-rich oligopeptides in plants for coordination with toxic metals and metalloids via their thiol groups. The composition, structure, and mass spectrometric fragmentation of arseno-PC (As-PC) with PC of different degree of oligomerization (PC2-PC5) in solution were studied using liquid chromatography coupled in parallel to inductively coupled plasma mass spectrometry and electrospray ionization quadrupole time-of-flight mass spectrometry. As-PC were detected from As(PC2) to As(PC5) with an increasing number of isomers that differ in the position of thiol groups bound to As. Thermodynamic modeling supported the identification process in case of these isomers. Mass spectrometric fragmentation of the As-PC does not follow the established pattern of peptides but is governed by the formation of series of As-containing annular cations, which coordinate to As via S, N, or O. Structure proposals for 30 As-PC fragment ions in the range m/z 147.92 to m/z 1290.18 are elaborated. Many of these fragment ions are characteristic to several As-PC and may be suited for a screening for As-PC in plant extracts. The mass spectrometric data offer the perspective for a future more sensitive determination of As-PC by means of liquid chromatography tandem mass spectrometry with multiple reaction monitoring. PMID:25395130

  5. In-house validation of a method for determination of silver nanoparticles in chicken meat based on asymmetric flow field-flow fractionation and inductively coupled plasma mass spectrometric detection

    Löschner, Katrin; Navratilova, Jana; Grombe, Ringo;

    2015-01-01

    spectrometric detection (AF4-ICP-MS) was applied for quantitative analysis of silver nanoparticles (AgNPs) in a chicken meat matrix following enzymatic sample preparation. For the first time an analytical validation of nanoparticle detection in a food matrix by AF4-ICP-MS has been carried out and the results......Nanomaterials are increasingly used in food production and packaging, and validated methods for detection of nanoparticles (NPs) in foodstuffs need to be developed both for regulatory purposes and product development. Asymmetric flow field-flow fractionation with inductively coupled plasma mass...

  6. Determination of Heavy Metals in Meat, Intestine, Liver, Eggs, and Chicken Using Neutron Activation Analysis and Atomic Absorption Spectrometry

    The elements As, Cd, Co, Cr, Fe, Hg, Ni, Pb, Sb, se and Zn in meat, intestine, and liver of cow and goat, as well as in broiler, local breed chicken and eggs have been determined using Neutron Activation Analysis and Atomic Absorption Spectrometry. Mercury was determined after being separated radiochemically. The results showed that concentration of the essential elements studied i.e. Cr, Cu, Fe, Zn, Co, and Ni were higher in liver and intestine than in the meat, but still in the normal range, while toxic elements As, Cd, and Pb were undetectable in all samples. (author). 8 refs., 6 tabs

  7. Determination of Gd, Sm, Eu and Dy in uranium compounds by atomic absorption spectrophotometry using a graphite furnace

    The separation of Gd, Sm, Eu and Dy from uranium and its determination by graphite furnace atomic absorption spectrophotometry is outlined. The lanthanides were separated by means of the percolation of the uranyl nitrate solution 0,3 M in HF (50-250g of U3O8 perliter) through an Al2O3 column. The lanthanides retained in the column were eluted with 1M HCl. As thorium is also retained into the column under these conditions, its interference was studied. The determination limits of the method range from 0,01 to 0,1 μg of lanthanide per gram of uranium. (Author)

  8. Influence of soil composition in the determination of chromium by atomic absorption spectrometry with flame air / acetylene

    The Air-acetylene Flame Atomic Absorption determination of chromium is a complex task, being strongly influenced by sample composition and instrumental conditions. The objective of this work was to study the influence of Al, Ca, Fe, K, Mg, and Na on the absorption of chromium in the air-acetylene flame, both separately and combined in solution, when acetylene flow and burner height vary. Dissolutions of the mixtures simulated the composition of four soils from the Quibu River Basin in Havana, Cuba. Chromium absorption first increased and then decreased with increment of acetylene flow for shorter burner heights (∼ 2-4 mm); while a continuous increase was observed for larger heights (> 4 mm). This behavior was the same in the presence and absence of interfering chemical element, mentioned above. On the other hand, the dependence of the magnitude of the interference with acetylene flow and burner height was complex and dependent on the interfering element, particularly at larger heights where the behavior of Al was remarkably different. The interference of the four mixtures of Al, Ca, K, Fe, Mg and Na decreased in comparison to individual interfering effects and was less dependent on acetylene flow and burner height. Finally, a significant reduction of interference on chromium determination in soil samples was achieved by an adequate selection of acetylene flow and burner height

  9. Determination of Na and Fe in high level liquid waste by closure atom absorption spectrum

    A method of measuring Na and Fe in High Level Liquid Waste (HLLW) by gloved fire atom absorption spectrometry was established. High Level Liquid Waste (HLLW) could be directly measured. The stabilization of the method is good. The operation is convenience and fast. The precision (RSD) of Na and Fe is better than 2% and 4% respectively. The precision (RSD) of Na and Fe is better than 2% and 4% respectively. The standard added-recovery for Na and Fe is 98.7% and 96.8% respectively. The results are well agreed with that obtained by other method and passed through F test. (authors)

  10. Determination Of Activity Of Radionuclides In Moss-Soil Sample With Self-Absorption Correction

    Hyper Pure Germanium (HPGe) spectrometer system is a very powerful tool for radioactivity measurements. The systematic uncertainty in the full energy peak efficiency is due to the differences between the matrix (density and chemical composition) of the reference and the other bulk samples. For getting precision from the gamma spectrum analysis, the absorbed correction in the sample should be considered. For gamma spectral analysis, a correction for absorption effects in sample should be considered, especially for bulk samples. The results were presented and discussed in this paper. (author)

  11. 火焰原子吸收光谱法间接测定药剂中的核黄素%Indirect determination of riboflavin in pharmaceuticals by flame atomic absorption spectrometry

    苏颖颖; 李晓红

    2011-01-01

    本文利用高碘酸钠对相邻羟基氧化作用的专属性,在一定介质中,高碘酸钠与核黄素完全反应后,过量的高碘酸的钠与硝酸铅或者硝酸铜生成沉淀,通过测定Pb或者Cu,建立了间接测定核黄素含量的方法.铅体系和铜体系测定的相对标准偏差(RSD)分别为4.8%和5.2%,检出限分别为0.6μg.mL和0.5μg·mL.用铅体系间接原子吸收光谱法测定维生素B片剂和针剂中的核黄素,测定结果与药典方法基本一致.%In the present work, a flame atomic absorption spectrometric method was developed for indirect determination of riboflavin. An excessive sodium periodate was used to react with riboflavin, and the remaining periodate was precipitated with excessive lead nitrate or copper nitrate. The precipitation, lead periodate or copper periodate formed was separated from the reaction medium by membrane filtration, and then was dissolved in 0.2 mol L-1 nitric acid following the determination of lead or copper by flame atomic absorption spectrometry. The calibration curve was linear over the range of 0. 001 ~ 0. 020 mg mL-1 and 0. 0025 ~ 0. 0500 mg mL-1; the relative standard deviation (RSD) for determination of 0. 005 mg mL-1 riboflavin was 4. 8% and 5. 2%; and the detection limit was 0. 0006 and 0. 0005 mg mL-1 , respectively, with lead or copper AAS measurement. The method was used for determination of riboflavin in Vitamin B2 tablets and injections.

  12. Determination of Elements by Atomic Absorption Spectrometry in Medicinal Plants Employed to Alleviate Common Cold Symptoms

    F Zehra Küçükbay; Ebru Kuyumcu

    2014-01-01

    Eleven important medicinal plants generally used by the people of Turkey for the treatment of com-mon cold have been studied for their mineral contents .Eleven minor and major elements (essential ,non-essen-tial and toxic) were identified in the Asplenium adiantum-nigrum L .,Althaea of ficinalis L .,Verbascum phlomoides L .,Euphorbiachamaesyce L .,Zizyphus jujube Miller ,Peganum harmala L .,Arum dioscori-dis Sm .,Sambucus nigra L .,Piper longum L .,Tussilago farfara L .and Elettariacardamomum Maton by employing flame atomic absorption and emission spectrometry and electro-thermal atomic absorption spectrom-etry .Microwave digestion procedure for total concentration was applied under optimized conditions for dissolu-tion of medicinal plants .Plant based biological certified reference materials (CRMs) served as standards for quantification .These elements are found to be present in varying concentrations in the studied plants .The baseline data presented in this work can be used in understanding the role of essential ,non-essential and toxic elements in nutritive ,preventive and therapeutic properties of medicinal plants .

  13. Absorption studies

    Absorption studies were once quite popular but hardly anyone does them these days. It is easier to estimate the blood level of the nutrient directly by radioimmunoassay (RIA). However, the information obtained by estimating the blood levels of the nutrients is not the same that can be obtained from the absorption studies. Absorption studies are primarily done to find out whether some of the essential nutrients are absorbed from the gut or not and if they are absorbed, to determine how much is being absorbed. In the advanced countries, these tests were mostly done to detect pernicious anaemia where vitamin B12 is not absorbed because of the lack of the intrinsic factor in the stomach. In the tropical countries, ''malabsorption syndrome'' is quire common. In this condition, several nutrients like fat, folic acid and vitamin B12 are not absorbed. It is possible to study absorption of these nutrients by radioisotopic absorption studies

  14. A comparison of simultaneous plasma, atomic absorption, and iron colorimetric determinations of major and trace constituents in acid mine waters

    Ball, J.W.; Nordstrom, D.K.

    1994-01-01

    Sixty-three water samples collected during June to October 1982 from the Leviathan/Bryant Creek drainage basin were originally analyzed by simultaneous multielement direct-current plasma (DCP) atomic-emission spectrometry, flame atomic-absorption spectrometry, graphite-furnace atomic-absorption spectrometry (GFAAS) (thallium only), ultraviolet-visible spectrometry, and hydride-generation atomic-absorption spectrometry.Determinations were made for the following metallic and semi-metallic constituents: AI, As, B, Ba, Be, Bi, Cd, Ca, Cr, Co, Cu, Fe(11), Fe(total), Li, Pb, Mg, Mn, Mo, Ni, K, Sb, Se, Si, Na, Sr, TI, V, and Zn. These samples were re-analyzed later by simultaneous multielement inductively coupled plasma (ICP) atomic-emission spectrometry and Zeeman-corrected GFAAS to determine the concentrations of many of the same constituents with improved accuracy, precision, and sensitivity. The result of this analysis has been the generation of comparative concentration values for a significant subset of the solute constituents. Many of the more recently determined values replace less-than-detection values for the trace metals; others constitute duplicate analyses for the major constituents. The multiple determinations have yielded a more complete, accurate, and precise set of analytical data. They also have resulted in an opportunity to compare the performance of the plasma-emission instruments operated in their respective simultaneous multielement modes. Flame atomic-absorption spectrometry was judged best for Na and K and hydride-generation atomic-absorption spectrometry was judged best for As because of their lower detection limit and relative freedom from interelement spectral effects. Colorimetric determination using ferrozine as the color agent was judged most accurate, precise, and sensitive for Fe. Cadmium, lead, and vanadium concentrations were too low in this set of samples to enable a determination of whether ICP or DCP is a more suitable technique. Of

  15. Incorporating a Generic Model of Subcutaneous Insulin Absorption into the AIDA v4 Diabetes Simulator 3. Early Plasma Insulin Determinations

    Lehmann, Eldon D.; Tarín, Cristina; Bondia, Jorge; Teufel, Edgar; Deutsch, Tibor

    2009-01-01

    Introduction AIDA is an interactive educational diabetes simulator that has been available without charge via the Internet for over 12 years. Recent articles have described the incorporation of a novel generic model of insulin absorption into AIDA as a way of enhancing its capabilities. The basic model components to be integrated have been overviewed, with the aim being to provide simulations of regimens utilizing insulin analogues, as well as insulin doses greater than 40 IU (the current upper limit within the latest release of AIDA [v4.3a]). Some preliminary calculated insulin absorption results have also recently been described. Methods This article presents the first simulated plasma insulin profiles from the integration of the generic subcutaneous insulin absorption model, and the currently implemented model in AIDA for insulin disposition. Insulin absorption has been described by the physiologically based model of Tarín and colleagues. A single compartment modeling approach has been used to specify how absorbed insulin is distributed in, and eliminated from, the human body. To enable a numerical solution of the absorption model, a spherical subcutaneous depot for the injected insulin dose has been assumed and spatially discretized into shell compartments with homogeneous concentrations, having as its center the injection site. The number of these compartments will depend on the dose and type of insulin. Insulin inflow arises as the sum of contributions to the different shells. For this report the first bench testing of plasma insulin determinations has been done. Results Simulated plasma insulin profiles are provided for currently available insulin preparations, including a rapidly acting insulin analogue (e.g., lispro/Humalog or aspart/Novolog), a short-acting (regular) insulin preparation (e.g., Actrapid), intermediate-acting insulins (both Semilente and neutral protamine Hagedorn types), and a very long-acting insulin analogue (e.g., glargine/Lantus), as

  16. Aspects of optical fibers and spectrometric sensors in chemical process and industrial environments

    For on-line control, the two alternatives of automatic sample transfer and in situ remote analysis are discussed. New concepts are emerging from the possibilities offered by optical fibers. Absorption in the visible, UV and IR, fluorescence and Raman spectrometric techniques are examined. The state of the art of optodes and devices in chemical process control are given, with some examples of applications in nuclear plants

  17. Determination Of Refractive Index And Reflectivity Of Thin Layer With Optical Absorption Method

    . The refractive index and reflectivity of ASi:H and Si Ox thin layer have been observed by optical absorption methods. Measurement has been done after the preparation of optical system which consists of a halogen lamp light source, monochromator, sample and light detector. The Monochromator output showed that measured halogen lamp spectrum light is between 470 nm -750 nm. The maximum voltage of halogen lamp is 220 Volt, the output light increases in intensity while the wave length increases. The inclination of intensity decrease at the wave length of 725 nm. The result of the calculation of refractive index varies in accordance with the wave length. The average refractive index of ASi:H is nf a = 1.753. The total reflectivity of air-thin layer-substrate is Rt a = 0.315. The refractive index of Si Ox sample is nf b2.182 and the total reflectivity is Rt b=O,514

  18. Fluorine determination in coal using high-resolution graphite furnace molecular absorption spectrometry and direct solid sample analysis

    Machado, Patrícia M.; Morés, Silvane; Pereira, Éderson R.; Welz, Bernhard; Carasek, Eduardo; de Andrade, Jailson B.

    2015-03-01

    The absorption of the calcium mono-fluoride (CaF) molecule has been employed in this study for the determination of fluorine in coal using direct solid sample analysis and high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS). The rotational line at 606.440 nm was used for measuring the molecular absorption in the gas phase. The pyrolysis and vaporization temperatures were 700 °C and 2100 °C, respectively. Different chemical modifiers have been studied, such as Pd and Ir as permanent modifiers, and Pd and the mixed Pd/Mg modifier in solution. The limit of detection and the characteristic mass were 0.3 and 0.1 ng F, respectively. One certified reference material (CRM) of coal (NIST 1635) and four CRMs with a non-certified value for F (SARM 18, SARM 20, BCR 40, BCR 180) were used to evaluate the accuracy and precision of the method, obtaining good agreement (104%) with the certified value and with the informed values (ranging from 90 to 103%).

  19. Determination of As, Cd, Cu, Hg and Pb in biological samples by modern electrothermal atomic absorption spectrometry

    Sardans, Jordi, E-mail: j.sardans@creaf.uab.ca [Ecophysiological and Global Change Unit CSIC-CREAF, Edifici C, Universitat Autonoma de Barcelona, Bellaterra 08193, Barcelona (Spain); Montes, Fernando [Departamento de Ciencias Analiticas, Facultad de Ciencias, Universidad Nacional de Educacion a Distancia (UNED), C/ Senda del Rey 9. 28040 Madrid (Spain); Penuelas, Josep [Ecophysiological and Global Change Unit CSIC-CREAF, Edifici C, Universitat Autonoma de Barcelona, Bellaterra 08193, Barcelona (Spain)

    2010-02-15

    Pollution from heavy metals has increased in recent decades and has become an important concern for environmental agencies. Arsenic, cadmium, copper, mercury and lead are among the trace elements that have the greatest impact and carry the highest risk to human health. Electrothermal atomic absorption spectrometry (ETAAS) has long been used for trace element analyses and over the past few years, the main constraints of atomic absorption spectrometry (AAS) methods, namely matrix interferences that provoked high background absorption and interferences, have been reduced. The use of new, more efficient modifiers and in situ trapping methods for stabilization and pre-concentration of these analytes, progress in control of atomization temperatures, new designs of atomizers and advances in methods to correct background spectral interferences have permitted an improvement in sensitivity, an increase in detection power, reduction in sample manipulation, and increase in the reproducibility of the results. These advances have enhanced the utility of Electrothermal atomic absorption spectrometry (ETAAS) for trace element determination at mug L{sup -1} levels, especially in difficult matrices, giving rise to greater reproducibility, lower economic cost and ease of sample pre-treatment compared to other methods. Moreover, the recent introduction of high resolution continuum source Electrothermal atomic absorption spectrometry (HR-CS-ETAAS) has facilitated direct solid sampling, reducing background noise and opening the possibility of achieving even more rapid quantitation of some elements. The incorporation of flow injection analysis (FIA) systems for automation of sample pre-treatment, as well as chemical vapor generation renders (ETAAS) into a feasible option for detection of As and Hg in environmental and food control studies wherein large numbers of samples can be rapidly analyzed. A relatively inexpensive approach with low sample consumption provide additional advantages

  20. Application of multiwalled carbon nanotubes treated by potassium permanganate for determination of trace cadmium prior to flame atomic absorption spectrometry

    2007-01-01

    In this study we investigated the enrichment ability of oxidized multiwalled carbon nanotubes (MWCNTs) and established a new method for the determination of trace cadmium in environment with flame atomic absorption spectrometry. The MWCNTs were oxidized by potassium permanganate under appropriate conditions before use as preconcentration packing. Parameters influencing the recoveries of target analytes were optimized. Under optimal conditions, the target analyte exhibited a good linearity (R2=0.9992)over the concentration range 0.5-50 ng/ml. The detection limit and precision of the proposed method were 0.15 ng/ml and 2.06%,respectively. The proposed method was applied to the determination of cadmium in real-world environmental samples and the recoveries were in the range of 91.3%-108.0%. All these experimental results indicated that this new procedure could be applied to the determination of trace cadmium in environmental waters.

  1. The determination of caesium and silver in soil and fungal fruiting bodies by electrothermal atomic absorption spectrometry

    Methods have been developed for the determination of caesium and silver in soil and fungal samples by microwave-assisted aqua regia digestion, followed by electrothermal atomic absorption spectrometry. The procedure was found to be repeatable (for soil, RSD -1, respectively, and for fungi, RSD -1, respectively) and reasonably efficient. Silver was recovered quantitatively from reference soils, but only about 80-85% of the caesium present could be extracted. Poorer caesium recoveries (< 70%) were obtained if, as part of the sample preparation procedure, solutions were taken to dryness in glass beakers prior to analysis. The detection limits were 0.02 mg Ag and 0.09 mg Cs per gram of dry soil, which are adequate for the determination of the analytes at typical environmental levels. The methods were applied in the analysis of three types of soil, a peaty podzol, a clay loam and a sandy loam and no significant matrix interferences were observed except in the determination of caesium in the sandy loam. For caesium, non-linear response curves, thought to be due to ionisation interference, were encountered using one atomic absorption spectrometer, but were not observed with the other instrument

  2. Determination of self-absorption corrections by computation in routine gamma-ray spectrometry for typical environmental samples

    A simple and practical method has been developed to quickly calculate self-absorption corrections and mass attenuation coefficients, μ/p, in common environmental samples being analyzed by gamma-ray spectrometry. The method involves using a sample computer program and estimates of the elemental compositions of typical environmental samples. The use of this method eliminates the need for gamma-ray-transmission measurements of individual samples, as well as expensive and time consuming elemental analyses of routine samples. The calculated percent attenuation of the beam through various samples, as determined by this method, agrees very well with experimentally measured values of percent attenuation

  3. Air quality status in Kinshasa as determined by instrumental neutron activation analysis, atomic absorption spectrometry and ion-exchange chromatography

    Three independent analytical techniques - instrumental neutron activation analysis. Atomic absorption spectrometry and ion-exchange chromatography - were applied to airborne particulate collected on filters and to atmospheric acid gases collected in carbonate buffer solutions. 20 trace elements and 7 acid gases and acid aerosols were determined. Results were compared with those observed elsewhere and showed that air pollution is low in Kinshasa and does not give rise to anxieties. The main known sources of pollutants are: vehicle exhaust and aeolian process on stripped soils. (author). 13 refs, 2 figs, 6 tabs

  4. Determination of the thermal neutron absorption cross section for rock samples by a single measurement of the time decay constant

    A calibration method for the determination of the thermal neutron macroscopic mass absorption cross section for rock samples is presented. The standard deviation of the final results is discussed in detail. A big advantage of the presented method is that the calibration curves have been found using the results obtained for a variety of natural rock samples of different stratigraphies and lithologies measured by Czubek's methods. An important part of the paper is a through analysis of the standard deviation of the final result. (author). 13 refs, 11 figs, 5 tabs

  5. Chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade uranium dioxide powders and pellets

    1981-01-01

    Uranium dioxide is used as a nuclear-reactor fuel. In order to be suitable for this purpose, the material must meet certain criteria for uranium content, stoichiometry, isotopic composition, impurity content. The following analytical procedures, which are described in detail, are designed to show whether or not a given material meets specifications: uranium by ferrous sulfate reduction in phosphoric acid and dichromate titration method; uranium and oxygen uranium atomic ratio by the ignition (gravimetric) impurity correction method; oxygen to uranium atomic ratios by the polarographic method; carbon (total) by direct combustion-thermal conductivity method; total chlorine and fluorine by pyrohydrolysis ion-selective electrode method; moisture by the coulometric, electrolytic moisture analyzer method; nitrogen by the Kjeldahl method; total sulfur by distillation-spectrophotometric method; isotopic uranium composition by multiple-filament surface-ionization mass spectrometric method; spectrochemical determination of trace elements in high-purity uranium dioxide; volatile fluoride impurities by spectrochemical method using the rotating-disk spark technique; spectrochemical determination of silver by gallium oxide carrier D-C arc technique; rare earths by copper spark-spectrochemical method; impurity elements by a spark-source mass spectrographic method; surface area by nitrogen absorption method; total gas in reactor-grade uranium dioxide pellets; thorium and rare earth elements by spectroscopy; hydrogen by inert gas fusion; and uranium isotopic analysis by mass spectrometry. (JMT)

  6. Chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade uranium dioxide powders and pellets

    Uranium dioxide is used as a nuclear-reactor fuel. In order to be suitable for this purpose, the material must meet certain criteria for uranium content, stoichiometry, isotopic composition, impurity content. The following analytical procedures, which are described in detail, are designed to show whether or not a given material meets specifications: uranium by ferrous sulfate reduction in phosphoric acid and dichromate titration method; uranium and oxygen uranium atomic ratio by the ignition (gravimetric) impurity correction method; oxygen to uranium atomic ratios by the polarographic method; carbon (total) by direct combustion-thermal conductivity method; total chlorine and fluorine by pyrohydrolysis ion-selective electrode method; moisture by the coulometric, electrolytic moisture analyzer method; nitrogen by the Kjeldahl method; total sulfur by distillation-spectrophotometric method; isotopic uranium composition by multiple-filament surface-ionization mass spectrometric method; spectrochemical determination of trace elements in high-purity uranium dioxide; volatile fluoride impurities by spectrochemical method using the rotating-disk spark technique; spectrochemical determination of silver by gallium oxide carrier D-C arc technique; rare earths by copper spark-spectrochemical method; impurity elements by a spark-source mass spectrographic method; surface area by nitrogen absorption method; total gas in reactor-grade uranium dioxide pellets; thorium and rare earth elements by spectroscopy; hydrogen by inert gas fusion; and uranium isotopic analysis by mass spectrometry

  7. Interplay of metabolism and transport in determining oral drug absorption and gut wall metabolism: a simulation assessment using the "Advanced Dissolution, Absorption, Metabolism (ADAM)" model.

    Darwich, A S; Neuhoff, S; Jamei, M; Rostami-Hodjegan, A

    2010-11-01

    systematic variation of drug characteristics, in accordance with the Biopharmaceutics Classification System (BCS) within one of the most physiological models of oral drug absorption currently available, respectively ADAM. Variables studied included the intrinsic clearance (CLint) and the Michaelis-Menten Constant (Km) for CYP3A4 and P-gp (C(Lint-CYP3A4) and K(m-CYP3A4), CL(int-P-gp) and K(m-P-gp)). The impact of CYP3A4 and P-gp intracellular topography were not investigated since a well-stirred enterocyte is assumed within ADAM. An increased CLint-CYP3A4 resulted in a reduced F(G) whereas an increase in C(Lint-P-gp) resulted in a reduced F(a), but interestingly decreased F(G) too. The reduction in FG was limited to certain conditions and was modest. Non-linear relationships between various parameters determining the permeability (e.g. P(app), C(Lint-P-gp,) and K(m-P-gp)) and gut wall metabolism (e.g. C(Lint-CYP3A4,) K(m-CYP3A4)) resulted in disproportionate changes in F(G) compared to the magnitude of singular effects. The results suggest that P-gp efflux decreases enterocytic drug concentration for drugs given at reasonably high dose which possess adequate passive permeability (high P(app)), by de-saturating CYP3A4 in the gut resulting in a lower F(G). However, these findings were observed only in a very limited area of the parameters space matching very few therapeutic drugs (a group with very high metabolism, high turn-over by efflux transporters and low F(a)). The systematic approach in this study enabled us to recognise the combination of parameters values where the potential interplay between metabolising enzymes and efflux transporters is expected to be highest, using a realistic range of parameter values taken from an intensive literature search. PMID:21189140

  8. Uniform Catalytic Site in Sn-beta Zeolite Determined using X-ray Absorption Fine Structure

    Bare,S.; Kelly, S.; Sinkler, W.; Low, J.; Modica, F.; Valencia, S.; Corma, A.; Nemeth, L.

    2005-01-01

    The Sn silicate zeolite, Sn-{beta}, has been shown to be an efficient, selective heterogeneous catalyst for Baeyer-Villiger oxidations. Using primarily a multishell fit to extended X-ray absorption fine structure (EXAFS) data, we show that the Sn does not randomly insert into the {beta}-zeolite structure but rather occupies identical, specific, crystallographic sites. These sites are the T5/T6 sites in the six-membered rings. Moreover, the Sn is substituted in pairs on opposite sides of these six-membered rings. We believe that it is the specific, uniform crystallographic location of the Sn in the crystal structure that leads to sites with uniform catalytic activity, and consequently to the high chemical selectivity demonstrated for this catalyst. This manifests itself in the almost enzyme-like selectivity of this catalyst in Baeyer-Villiger oxidations. This uniform site distribution of the Sn suggests that there is likely a symbiotic relationship between the structure-directing agent in the zeolite synthesis and the Sn heteroatoms during the framework formation.

  9. Determination of ruthenium and iridium in anode coatings by atomic-absorption spectroscopy.

    Harrington, D E; Bramstedt, W R

    A method is described for the determination of ruthenium and iridium coated on an electrode surface. The coating is chemically removed from the electrode by fusion with alkali, and the resulting solution prepared for analysis. Interelement interferences are eliminated by using a titanium-potassium matrix solution as a releasing agent. Recovery and precision data are given for ruthenium and iridium. The AAS determination of ruthenium compares favourably with a standard colorimetric method. PMID:18961657

  10. Determination of total selenium in pharmaceutical and herbal supplements by hydride generation and graphite furnace atomic absorption spectrometry.

    Kazi, Tasneem G; Kolachi, Nida F; Afridi, Hassan I; Brahman, Kapil Dev; Shah, Faheem

    2014-01-01

    The total selenium (Se) was determined in herbal and pharmaceutical supplements used for liver diseases. The total Se contents were determined in different pharmaceutical and herbal supplements by hydride generation atomic absorption spectrometry (HGAAS) and graphite furnace atomic absorption spectrometry (GFAAS) after microwave-assisted acid digestion. The accuracy of the techniques was evaluated by using certified reference material and the standard addition method. The recoveries of total Se were 99.4 and 99.0% for HGAAS and GFAAS, respectively. The precision of the techniques expressed as RSD were 2.34 and 4.54% for HGAAS and GFAAS measurements, respectively. The LOD values for HGAAS and GFAAS were 0.025 and 0.052 pglg, respectively. The concentrations of Se in pharmaceutical and herbal supplements were found in the range of 19.2-53.8 and 25.0-42.5 pg/g, respectively, corresponding to 35-76% and 45-76% of the total recommended dose of Se for adults. PMID:25632445

  11. D-xylose absorption

    D-xylose absorption is a laboratory test to determine how well the intestines absorb a simple sugar (D-xylose). The test ... test is primarily used to determine if nutrient absorption problems are due to a disease of the ...

  12. Studies on absorption coefficients of dual-energy γ-rays and measuring error correction for multiphase fraction determination

    2006-01-01

    In this article, principle and mathematical method of determining the phase fractions of multiphase flows by using a dual-energy γ-ray system have been described. The dual-energy γ-ray device is composed of radioactive isotopes of 241Am and 137Cs with γ-ray energies of 59.5 and 662 keV, respectively. A rational method to calibrate the absorption coefficient was introduced in detail. The modified arithmetic is beneficial to removing the extra Compton scattering from the measured value. The result shows that the dual-energy γ-ray technique can be used in three-phase flow with average accuracy greater than 95%, which enables us to determine phase fractions almost independent of the flow regime. Improvement has been achieved on measurement accuracy of phase fractions.

  13. Commercial Applications of X Ray Spectrometric Techniques

    In the 21st century, the X-ray fluorescence (XRF) technique is widely used in process control, industrial applications and for routine elemental analysis. The technique has a multielement capability capable of detecting elements with Z ≥ 10, with a few instruments capable of detecting also elements with Z ≥ 5. It is characterized by a non-destructive analysis process and relatively good detection limits, typically one part per million, for a wide range of elements. The first commercial XRF instruments were introduced to the market about 50 years ago. They were the wavelength dispersive X ray fluorescence (WDXRF) spectrometers utilizing Bragg’s law and reflection on crystal lattices for sequential elemental analysis of sample composition. The advances made in radiation detector technology, especially the introduction of semiconductor detectors, improvements in signal processing electronics, availability and exponential growth of personal computer market led to invention of energy dispersive X ray fluorescence (EDXRF) technique. The EDXRF is more cost effective as compared to WDXRF. It also allows for designing compact instruments. Such instruments can be easily tailored to the needs of different customers, integrated with industrial installations, and also miniaturized for the purpose of in-situ applications. The versatility of the technique has been confirmed in a spectacular way by using the XRF and X-ray spectrometric techniques, among few others, during the NASA and ESA missions in search for the evidence of life and presence of water on the surface of Mars. The XRF technique has achieved its strong position within the atomic spectroscopy group of analytical techniques not only due to its versatility but also due to relatively low running costs, as compared to the commonly used methods, e.g., atomic absorption spectrometry (AAS) or inductively coupled plasma atomic emission/mass spectrometry (ICP-AES/MS). Presently, the XRF technique together with X ray

  14. Evaluation of quartz tubes as atomization cells for gold determination by thermospray flame furnace atomic absorption spectrometry

    This work describes the development of a new analytical procedure able to determine gold by thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) using nickel tubes (NiT) and quartz tubes (QT) as atomization cells. Experiments involving changes in the flow injection operational parameters, reagent concentrations and sizes of the QT were performed in order to optimize sensitivity. Under the same operational conditions, it was observed that the employment of QT increases the sensitivity of gold determination when compared to the nickel tube. Since solutions of highly concentrated hydrochloric acid showed the best performance as carriers, quartz tubes were also preferred due to its greater tolerance to corrosion by mineral acids in comparison to NiT. In addition, changes in the internal diameter of the QT revealed an important improvement in sensitivity for smaller tubes. Under optimized conditions the main figures of merit showed values close to that of graphite furnace atomic absorption spectrometry with the addition of an excellent improvement of the sample throughput. They are: LOD (3 s): 0.004 μg mL−1, sensitivity: 0.306 (μg mL−1)−1, RSD% (n = 10, 1 μg mL−1): 2.5, linear range: 0.01–4 μg mL−1 and sample throughput: 72 h−1. This new method was employed for the determination of gold in homeopathic medicines with no need of sample digestion. Validation of the analytical results will be shown. A full discussion of the most relevant findings regarding the role of the atomization cell as a strategic key for improving sensitivity will be also provided. - Highlights: ► Quartz tubes as furnaces in TS-FFAAS. ► Small tubes for controlling radial dispersion. ► Improved figures of merit for gold determination. ► Analysis of homeopathic medicines.

  15. Indium determination by spectral overlappings of lines in atomic absorption spectrometry

    A molybdenum hollow-cathode lamp filled with neon can be used to determine indium. Characteristic concentration for this element is 4.5 mg/L in the 325 nm spectral region for the Mo(I) 325.621 nm line. In addition, values of 0.4 mg/L and 0.3 mg/L are obtained with the Mo(I) 410.215 nm and Ne(I) 451.151 nm lines, respectively. These spectral overlappings allow the determination of indium in silver-cadmium-indium alloys. (Author)

  16. DETERMINATION OF COPPER AND ZINC IN MINERAL WATERS BY ATOMIC ABSORPTION SPECTROPHOTOMETRY

    Tatiana Mitina

    2011-12-01

    Full Text Available The content of copper and zinc in mineral waters were determined by atomic spectroscopy with preliminary extraction of metals. Validation of the technique was carried out by the method of standard additions and proved the reliability of analytical data.

  17. PLUTONIUM CONTAMINATION VALENCE STATE DETERMINATION USING X-RAY ABSORPTION FINE STRUCTURE PERMITS CONCRETE RECYCLE

    This paper describes the determination of the speciation of plutonium contamination present on concrete surfaces at the Rocky Flats Environmental Technology Site (RFETS). At RFETS, the plutonium processing facilities have been contaminated during multiple events over their 50 year operating history. Contamination has resulted from plutonium fire smoke, plutonium fire fighting water, milling and lathe operation aerosols, furnace operations vapors and plutonium ''dust'' diffusion

  18. Significance of Airborne Gamma-ray spectrometric data of Umm bisilla Area, central Eastern Desert, Egypt

    Umm bisilla area, located in the Central Eastern Desert of Egypt, consists mainly of basement rocks. The present investigation of the airborne spectrometric data is to define the meaningful anomalies from the raw data by applying the significance factor techniques, by calculating the significant radioactive provinces. Determination of the gross structural pattern and broad variations in composition of the crystalline basement, to define the relationships between the tectonic features of the area as interpreted from aeromagnetic data, with the significant anomalies revealed from spectrometric data was carried out through the application of different magnetic techniques. Five significant uraniferous zones were detected associated with Umm Bisilla granite, amphibolite, and grey granite. The intersection of the structural lineaments interpreted from aeromagnetic data illustrated good correlation with the significant uranium anomalous zones interpreted from spectrometric data, and indicated that the concentration is structurally. 15 figs

  19. Radiative efficiencies and global warming potentials using theoretically determined absorption cross-sections for several hydrofluoroethers (HFEs) and hydrofluoropolyethers (HFPEs)

    Integrated infrared cross-sections and wavenumber positions for the vibrational modes of a range of hydrofluoroethers (HFEs) and hydrofluoropolyethers (HFPEs) have been calculated. Spectra were determined using a density functional method with an empirically derived correction for the wavenumbers of band positions. Radiative efficiencies (REs) were determined using the Pinnock et al. method and were used with atmospheric lifetimes from the literature to determine global warming potentials (GWPs). For the HFEs and the majority of the molecules in the HG series HFPEs, theoretically determined absorption cross-sections and REs lie within ca. 10% of those determined using measured spectra. For the larger molecules in the HG series and the HG' series of HFPEs, agreement is less good, with theoretical values for the integrated cross-sections being up to 35% higher than the experimental values; REs are up to 45% higher. Our method gives better results than previous theoretical approaches, because of the level of theory chosen and, for REs, because an empirical wavenumber correction derived for perfluorocarbons is effective in predicting the positions of C-F stretching frequencies at around 1250 cm-1 for the molecules considered here.

  20. Determination of Nickel in Water and Wastewater at Ultratrace Level by Solid-Phase Extraction-Flame Atomic Absorption Spectrometry

    Solid-phase extraction using octadecyl silica membrane disk modified with 2[(2-mercaptophenylimino)methyl] phenol (MPMP) ligand was utilized in FAAS determination of ultratrace amount of nickel in water and wastewater samples. Ni2+ ions were adsorbed quantitatively during the passage of an aqueous sample through the modified octadecyl silica membrane disk. The retained Ni2+ ions were then eluted from the disk with 5 mL of 0.5 mol L-1 nitric acid as an eluent, and subsequently determined by FAAS. The break-through volume of the method was 2000 mL, which corresponded to the enrichment factor of 400. Maximum capacity of the membrane disk modified with 6 mg of the ligand was 210 μg of Ni2+, and the limit of determination was 0.17 μg L-1. The effect of various ionic interferences on preconcentration and determination of nickel in binary mixture was studied. The method was successfully applied to determination of nickel in water and wastewater samples; accuracy was examined in recovery experiment and by independent GFAAS analysis (graphite furnace atomic absorption spectrometry). The accuracy was further confirmed by applying the proposed method to the analysis of standard reference alloy (BCR No 112) and comparing the result with the declared value. (authors)

  1. Direct determination of cadmium in Orujo spirit samples by electrothermal atomic absorption spectrometry: Comparative study of different chemical modifiers

    Vilar Farinas, M. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Barciela Garcia, J. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Garcia Martin, S. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Pena Crecente, R. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Herrero Latorre, C. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain)]. E-mail: cherrero@lugo.usc.es

    2007-05-22

    In this work, several analytical methods are proposed for cadmium determination in Orujo spirit samples using electrothermal atomic absorption spectrometry (ETAAS). Permanent chemical modifiers thermally coated on the platforms inserted in pyrolytic graphite tubes (such as W, Ir, Ru, W-Ir and W-Ru) were comparatively studied in relation to common chemical modifier mixtures [Pd-Mg(NO{sub 3}){sub 2} and (NH{sub 4})H{sub 2}PO{sub 4}-Mg(NO{sub 3}){sub 2}] for cadmium stabilization. Different ETAAS Cd determination methods based on the indicated modifiers have been developed. In each case, pyrolysis and atomization temperatures, atomization shapes, characteristic masses and detection limits as well as other analytical characteristics have been determined. All the assayed modifiers (permanent and conventional) were capable of achieving the appropriate stabilization of the analyte, with the exception of Ru and W-Ru. Moreover, for all developed methods, recoveries (99-102%) and precision (R.S.D. lower than 10%) were acceptable. Taking into account the analytical performance (best detection limit LOD = 0.01 {mu}g L{sup -1}), the ETAAS method based on the use of W as a permanent modifier was selected for further direct Cd determinations in Orujo samples from Galicia (NW Spain). The chosen method was applied in the determination of the Cd content in 38 representative Galician samples. The cadmium concentrations ranged

  2. Direct determination of cadmium in Orujo spirit samples by electrothermal atomic absorption spectrometry: Comparative study of different chemical modifiers

    In this work, several analytical methods are proposed for cadmium determination in Orujo spirit samples using electrothermal atomic absorption spectrometry (ETAAS). Permanent chemical modifiers thermally coated on the platforms inserted in pyrolytic graphite tubes (such as W, Ir, Ru, W-Ir and W-Ru) were comparatively studied in relation to common chemical modifier mixtures [Pd-Mg(NO3)2 and (NH4)H2PO4-Mg(NO3)2] for cadmium stabilization. Different ETAAS Cd determination methods based on the indicated modifiers have been developed. In each case, pyrolysis and atomization temperatures, atomization shapes, characteristic masses and detection limits as well as other analytical characteristics have been determined. All the assayed modifiers (permanent and conventional) were capable of achieving the appropriate stabilization of the analyte, with the exception of Ru and W-Ru. Moreover, for all developed methods, recoveries (99-102%) and precision (R.S.D. lower than 10%) were acceptable. Taking into account the analytical performance (best detection limit LOD = 0.01 μg L-1), the ETAAS method based on the use of W as a permanent modifier was selected for further direct Cd determinations in Orujo samples from Galicia (NW Spain). The chosen method was applied in the determination of the Cd content in 38 representative Galician samples. The cadmium concentrations ranged -1

  3. Spectrometric Determination of Metal Elements in Typha latifolia L.from Jianshui of Yunnan%云南建水草牙中金属元素的光谱测定

    郭俊明; 戴建辉; 白红丽; 张虹; 王宝森

    2011-01-01

    [目的]测定云南建水草牙(Typha lotifolia L.)中8种金属元素的含量,以期为这一资源的开发利用提供科学依据.[方法]采用火焰原子吸收光谱法测定草芽中的Fe、Zn、Cu、Ni、Co、Cd、Pb和Cr元素的含量.[结果]建水草牙分有多种时人体有益的矿物元素,7种金属元素含量顺序为Fe>Zn >Cu>Ni>C0>Cd >Pb,Cr未检测出;Fe元素含量较高,而Cu含量相对较低.[结论]建水草牙含矿物元素较丰富.%[Objective ] To determine the content of 8 metal elements in Typha latifolia L. from Jianshui County of Yunnan Province, so at to provide a scientific basis for development and utilization of this resources. [Method] Contents of 8 metal elements including Fe, Zn, Cu, Ni, Co, Cd, Pb and Cr were determined by flame atomic absorption spectrometry. [Result] Typha latifolia L. was rich in various mineral elements to human health. The content ordet of 7 analyzed mineral elements was Fe>Zn>Cu>Ni >Co >Cd>Pb. Cr element could not be detected in tested sample. The content( Fe was higher in Typha latifolia L. , while Cu was relatively lower. [ Conclusion ] There were abundant mineral el-ements which were necessary fur people in the Typha latifolia L..

  4. Determination of Cd and Pb in canned pineapple by atomic absorption spectroscopy using a graphite oven

    Owing to the food susceptibility to be contaminated it is necessary to realize pursuit studies or frequent monitoring about the content of certain metals which represent health risks by its toxicological effects in the human being and another living organisms. In this work the cadmium and lead concentrations are determined in six national brands of canned pineapple analysing separately sugar sirup and the fruit. (Author)

  5. On the fast response of spectrometric circuits

    Information capacity of spectrometric circuits obtianed by means of Monte Carlo method modeling is analysed. It is shown that working at high input pulse counting rate is not advisable, dead time of analog-to-digital converter should be compared with the pulse rise time of the amplifier

  6. Evaluation of the use of five laboratory determined ozone absorption cross sections in brewer and dobson retrieval algorithms

    Redondas, A.; Evans, R.; Stuebi, R.; Köhler, U.; Weber, M.

    2013-09-01

    The primary ground-based instruments used to report total column ozone (TOC) are Brewer and Dobson Spectrophotometers, in separate networks. These instruments make measurements of the UV irradiances, and through a well-defined process a TOC value is produced. Inherent in the algorithm is the use of a laboratory determined cross-section data set. We used five ozone cross section data sets: three Bass and Paur, Daumont, Malicet and Brion (DMB) and a new Institute of Environmental Physics (IUP), University of Bremen, set. The three Bass and Paur (1985) sets are: quadratic temperature coefficients from IGACO web page (IGQ4), the Brewer network operational calibration set (BOp), and the set used by Bernhard et al. (2005), in the reanalysis of the Dobson absorption coefficient values (B05). The ozone absorption coefficients for Brewer and Dobson are then calculated using the normal Brewer operative method which is essentially the same as used on Dobson. Considering the standard TOC algorithm for the Brewer instruments and comparing to the Brewer standard operational calibration data set, using the slit functions for the individual instruments: we find the UIP data set changes the calculated TOC by -0.5%, the DBM data set changes the calculate TOC by -3.2%, and the IGQ4 data set at -45 °C changes the calculated TOC by +1.3%. Considering the standard algorithm for the Dobson instruments, and comparing to results using the official 1992 ozone absorption coefficients values and the single set of slit functions defined for all Dobson instruments, the calculated TOC changes by +1%, with little variation depending on which data set is used We applied the changes to the European Dobson and Brewer reference instruments during the Izaña 2012 Absolute Calibration Campaign. The application of a common Langley calibration and the IUP cross section the differences between Brewer and Dobson vanish whereas using Bass and Paur and DBM produce differences of 1.5% and 2% respectively. A

  7. Evaluation of the use of five laboratory determined ozone absorption cross sections in brewer and dobson retrieval algorithms

    A. Redondas

    2013-09-01

    Full Text Available The primary ground-based instruments used to report total column ozone (TOC are Brewer and Dobson Spectrophotometers, in separate networks. These instruments make measurements of the UV irradiances, and through a well-defined process a TOC value is produced. Inherent in the algorithm is the use of a laboratory determined cross-section data set. We used five ozone cross section data sets: three Bass and Paur, Daumont, Malicet and Brion (DMB and a new Institute of Environmental Physics (IUP, University of Bremen, set. The three Bass and Paur (1985 sets are: quadratic temperature coefficients from IGACO web page (IGQ4, the Brewer network operational calibration set (BOp, and the set used by Bernhard et al. (2005, in the reanalysis of the Dobson absorption coefficient values (B05. The ozone absorption coefficients for Brewer and Dobson are then calculated using the normal Brewer operative method which is essentially the same as used on Dobson. Considering the standard TOC algorithm for the Brewer instruments and comparing to the Brewer standard operational calibration data set, using the slit functions for the individual instruments: we find the UIP data set changes the calculated TOC by −0.5%, the DBM data set changes the calculate TOC by −3.2%, and the IGQ4 data set at −45 °C changes the calculated TOC by +1.3%. Considering the standard algorithm for the Dobson instruments, and comparing to results using the official 1992 ozone absorption coefficients values and the single set of slit functions defined for all Dobson instruments, the calculated TOC changes by +1%, with little variation depending on which data set is used We applied the changes to the European Dobson and Brewer reference instruments during the Izaña 2012 Absolute Calibration Campaign. The application of a common Langley calibration and the IUP cross section the differences between Brewer and Dobson vanish whereas using Bass and Paur and DBM produce differences of 1.5% and 2

  8. Determination of Cd, Pb and As in sediments of the Sava River by electrothermal atomic absorption spectrometry

    SIMONA MURKO

    2010-01-01

    Full Text Available The applicability of nitric acid, palladium nitrate and a mixture of palladium and magnesium nitrate as matrix modifiers were estimated for the accurate and reproducible determination of cadmium (Cd, lead (Pb and arsenic (As in sediments of the Sava River by electrothermal atomic absorption spectrometry, ETAAS. Decomposition of the samples was done in a closed vessel microwave-assisted digestion system using nitric, hydrochloric and hydrofluoric acids, followed by the addition of boric acid to convert the fluorides into soluble complexes. The parameters for the determination of Cd, Pb and As in sediments were optimised for each individual element and for each matrix modifier. In addition, two sediment reference materials were also analysed. In determination of Cd and Pb, nitric acid was found to be the most appropriate matrix modifier. The accurate and reliable determination of Cd and Pb in sediments was possible also in the presence of boric acid. The use of a mixture of palladium and magnesium nitrate efficiently compensated for matrix effects and enabled the accurate and reliable determination of As in the sediments. Quantification of Cd and As was performed by calibration using acid matched standard solutions, while the standard addition method was applied for the quantification of Pb. The repeatability of the analytical procedure for the determination of Cd, Pb and As in sediments was ±5 % for Cd, ±4 % for Pb and ±2 % for As. The LOD values of the analytical procedure were found to be 0.05 mg/kg for Cd and 0.25 mg/kg for Pb and As, while the LOQ values were 0.16 mg/kg for Cd and 0.83 mg/kg for Pb and As. Finally, Cd, Pb and As were successfully determined in sediments of the Sava River in Slovenia.

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

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

  10. Use of atomic absorption spectrometry to determine metallic impurities in coal

    The Brazilian Energetic Alternative Program expects the reduction of our dependence on foreign energy sources, by replacing fuel oil by mineral coal. Its gasification by means of nuclear energy must be also considered. However, the intensive burning of coal leads to serious environmental problems. During its combustion the release to atmosphere of toxic elements such as As, Hg, Pb, Zn and others is of great concern. Hence, it is important to have reliable analytical methods which can monitor inorganic constituents at various stages of coal production and utilization. The AAS is a suitable analytical technique to determine pollutants in coal because it is sensitive, simple, economic and cover a large range of concentration. The need of a previous treatment of sample is overcome by using an acid attack (HNO3 + HClO4 + HF) which has been proved to be rapid and efficient. (Author)

  11. Study of new technique of solid combustible materials to determination of volatile elements by flame atomic absorption spectrophotometry

    A new technique for direct trace element analysis of solid combustible materials is described. The samples (up to 10 mg) are weighed on a graphite platform wich is then placed in a quartz tube, at the focal point of three infrared lamps. When the lamps are turned on, the sample burns in a stream of air, and the resulting dry aerosol containing volatile elements such as Hg, Cd, Bi, Tl, Zn, Pb and Cu is carried into the mixing chamber and thence into the flame, where the atomic absorption measurement is carried out. This technique overcomes chemical sample preparation steps, avoiding contaminations of losses associated with these steps. A ''furnace in flame'' system where the aerosol is transported to a flame heated T-tube is also described. The influence of flame stoichiometry, observation height, platform material and air flux intensity was studied inorder to determine optimal analytical conditions. (author)

  12. Standard Test Method for Determining Solar or Photopic Reflectance, Transmittance, and Absorptance of Materials Using a Large Diameter Integrating Sphere

    American Society for Testing and Materials. Philadelphia

    1987-01-01

    1.1 This test method covers the measurement of the absolute total solar or photopic reflectance, transmittance, or absorptance of materials and surfaces. Although there are several applicable test methods employed for determining the optical properties of materials, they are generally useful only for flat, homogeneous, isotropic specimens. Materials that are patterned, textured, corrugated, or are of unusual size cannot be measured accurately using conventional spectrophotometric techniques, or require numerous measurements to obtain a relevant optical value. The purpose of this test method is to provide a means for making accurate optical property measurements of spatially nonuniform materials. 1.2 This test method is applicable to large specimens of materials having both specular and diffuse optical properties. It is particularly suited to the measurement of the reflectance of opaque materials and the reflectance and transmittance of semitransparent materials including corrugated fiber-reinforced plastic, ...

  13. Noninvasive determination of absorption coefficient and reduced scattering coefficient of human skin tissues in vivo with oblique-incidence reflectometry

    Ping Sun; Yu Wang; Xiaoli Mo; Jinghui Xie

    2008-01-01

    A spatial distribution of diffuse reflectance produced by obliquely incident light is not centered about the point of light entry. The value of shift in the center of diffuse reflectance is directly related to the absorption coefficient μa and the effective attenuation coefficient μeff. μa and the reduced scattering coefficient μ's of human skin tissues in vivo are measured by oblique-incidence reflectometry based on the two-source diffuse theory model. For ten Chinese volunteers aged 15-63 years, μa and μ's are noninvasively determined to be 0.029 - 0.075 and 0.52 - 0.97 mm-1, respectively.

  14. Exposure study by determination of blood lead levels using electro-thermal atomic absorption in correlation with basophilic stippling

    Blood lead levels were determined in fifty traffic police personnel exposed to open traffic deputed at various crossings in Rawalpindi/Islamabad by electro-thermal atomic absorption spectrophotometric technique to monitor the levels. Blood comparison of lead concentration in the blood samples of policemen working at high density area versus those working at low density area was made. The range of the blood lead levels of subjects working in the high density traffic is 7.2 - 19.6 up/dl whereas the blood lead levels of subjects at lean traffic is 0.4 - 6.9 Mu g /dL. The accuracy of the method was checked by analyzing SRM wheat flour, rice flour and bovine liver. The results obtained were compared with reported values of other countries as well as with the exposure limits of WHO. (author)

  15. Determination of yttrium and rare-earth elements in rocks by graphite-furnace atomic-absorption spectrometry.

    Gupta, J G

    1981-01-01

    With use of synthetic solutions and several international standard reference materials a method has been developed for determining traces of Y, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu in rocks by electrothermal atomization in a pyrolytically-coated graphite furnace. Depending on the element, the sensitivity is of the order of 10(-9)-10(-12) g at 2500 degrees . To avoid matrix interferences the lanthanides are separated from the common elements by co-precipitation with calcium and iron as carriers. The data for Canadian reference rock SY-2 (syenite), U.S.G.S. reference rocks W-2 (diabase), DNC-1 (diabase) and BIR-1 (basalt), and South African reference rock NIM-18/69 (carbonatite) obtained by graphite-furnace atomization are compared with the values obtained by flame atomic-absorption. The results are in good agreement with literature values. PMID:18962852

  16. DIRECT DETERMINATION OF GOLD IN SUSPENSIONS OF ROCK AND ORE REFERENCE MATERIALS USING ELECTROTHERMAL HIGH RESOLUTION ATOMIC ABSORPTION SPECTROMETRY

    Zakharov, Y. А.; Irisov, D. S.; Okunev, R. V.; Musin, R. Kh.; Haibullin, R. R.

    2014-01-01

    High resolution continuum source atomic absorption spectrometer ContrAA-700 with graphite furnace is used for direct gold determination in rocks and ores on the level 10-6-10-3 % mas. Russian standard reference materials of gold containing ore СЗР-4 (2.13 ± 0.05 g/ton), black slates of Sykhoy Log СЛг-1 (2.50 ± 0.03 g/ton) and СЧС-1 (0.10 ± 0.02 g/ton) in mass 1 mg was inserted into the furnace in the suspension form prepared on the mix of concentrated HNO3 and HCl (1:3) with following sevenfo...

  17. Determination of total inorganic arsenic in potable water through spectroscopy of atomic absorption with generation of hydride

    Arsenic is an element that has been studied in the analysis of environmental samples for its toxicity showed in very low concentrations. The objective of this work is the validation of a method for the determination of total inorganic arsenic in drinking water. Through the spectrophotometric technique of atomic absorption an automatic system of flow injection for the generation of hydrides is used. The prereduction of Arsenic was made with potasium iodide 1,5% m/v and ascorbic acid 0.25% m/v dissolved in hydrochloric acid 3,7% m/v. The recuperation percentage of the method was 97 ± 3% in a dynamic range to 30 μg/L. The detection limit was 0,7 μg/L established over 0,5 mL of sample. The samples analyzed were found under the set limits of normative in Costa Rica of 10 μg/L. (author)

  18. Targeted quantitative mass spectrometric immunoassay for human protein variants

    Nedelkov Dobrin

    2011-04-01

    Full Text Available Abstract Background Post-translational modifications and genetic variations give rise to protein variants that significantly increase the complexity of the human proteome. Modified proteins also play an important role in biological processes. While sandwich immunoassays are routinely used to determine protein concentrations, they are oblivious to protein variants that may serve as biomarkers with better sensitivity and specificity than their wild-type proteins. Mass spectrometry, coupled to immunoaffinity separations, can provide an efficient mean for simultaneous detection and quantification of protein variants. Results Presented here is a mass spectrometric immunoassay method for targeted quantitative proteomics analysis of protein modifications. Cystatin C, a cysteine proteinase inhibitor and a potential marker for several pathological processes, was used as a target analyte. An internal reference standard was incorporated into the assay, serving as a normalization point for cystatin C quantification. The precision, linearity, and recovery characteristics of the assay were established. The new assay was also benchmarked against existing cystatin C ELISA. In application, the assay was utilized to determine the individual concentration of several cystatin C variants across a cohort of samples, demonstrating the ability to fully quantify individual forms of post-translationally modified proteins. Conclusions The mass spectrometric immunoassays can find use in quantifying specific protein modifications, either as a part of a specific protein biomarker discovery/rediscovery effort to delineate the role of these variants in the onset of the disease, progression, and response to therapy, or in a more systematic study to delineate and understand human protein diversity.

  19. Determination of K-shell absorption jump factors and jump ratios for La2O3, Ce and Gd using two different methods

    The K shell absorption jump factors and jump ratios for La2O3, Ce and Gd samples have been determined using the gamma or X-ray attenuation and EDXRF methods. It is the first time that the K shell absorption jump factor and jump ratio have been discussed for present elements using two different methods. To detect K X-rays, a high resolution Si(Li) detector was used. The experimental results of K shell absorption jump factors and jump ratios were compared with the theoretically calculated ones. - Highlights: • The K shell absorption jump factors and jump ratios were measured for La2O3, Ce and Gd. • These parameters were determined using two different methods. • The measured values of the parameters were found in good agreement with the theoretical ones

  20. Determination of microamounts of potassium in sodium iodide by atomic absorption spectrometry

    Microdetermination of potassium in sodium iodide was developed by the standard addition method. Twenty grams of sample were dissolved in 50 ml of water in a quartz beaker. To the solution, 30 ml of concentrated hydrochloric acid and 30 ml of 30% hydrogen peroxide were added, and evaporated to dryness. By this process sodium iodide was converted into sodium chloride. The cake thus obtained was dissolved in water and diluted to exactly 200 ml. To 25 ml aliquots of the solution, the standard potassium and cesium chloride solutions were added and diluted to 50 ml with water; the concentration of potassium was 0 -- 1 mg/l and that of cesium 4 mM. These solutions were introduced into an air-propane flame and the absorbances were measured at 769.9 nm. During the conversion reaction, hydrochloric acid was completely decomposed, and remained hydrogen peroxide had no influence for absorbance, and other backgrounds were negligible. The linear calibration curve was obtained in the range 0 -- 2 mg of potassium per liter. Potassium in sodium iodide was determined by this method within the coefficient of variation of +-(20 -- 3)% in the range (1.7 -- 32.5) ppm. (author)