Indirect determination of uranium by atomic-absorption spectrophotometry using an air-acetylene flame

International Nuclear Information System (INIS)

Alder, J.F.; Das, B.C.

1977-01-01

An indirect method has been developed for the determination of uranium by atomic-absorption spectrophotometry using an air-acetylene flame. Use is made of the reduction of copper(II) by uranium(IV) followed by complex formation of the copper(I) ions so produced with neocuproine (2,9-dimethyl-1,10-phenanthroline) and finally the determination of copper in this complex by atomic-absorption spectrophotometry. The results show that the method can be recommended, provided that care is taken to ensure the complete reduction of uranium(VI) to uranium(IV). The sensitivity of the method is 4.9 μg of uranium and the upper limit 500 μg without dilution. (author)

Determination of Calcium in Cereal with Flame Atomic Absorption Spectroscopy: An Experiment for a Quantitative Methods of Analysis Course

Science.gov (United States)

Bazzi, Ali; Kreuz, Bette; Fischer, Jeffrey

2004-01-01

An experiment for determination of calcium in cereal using two-increment standard addition method in conjunction with flame atomic absorption spectroscopy (FAAS) is demonstrated. The experiment is intended to introduce students to the principles of atomic absorption spectroscopy giving them hands on experience using quantitative methods of…

Matrix effects on the determination of manganese in geological materials by atomic-absorption spectrophotometry under different flame conditions

Science.gov (United States)

Sanzolone, R.F.; Chao, T.T.

1978-01-01

Suppression caused by five of the seven matrix elements studied (Si, Al, Fe, Ca and Mg) was observed in the atomic-absorption determination of manganese in geological materials, when synthetic solutions and the recommended oxidizing air-acetylene flame were used. The magnitude of the suppression effects depends on (1) the kind and concentration of the interfering elements, (2) the type of acid medium, and (3) the concentration of manganese to be determined. All interferences noted are removed or alleviated by using a reducing nitrous oxide-acetylene flame. The atomic-absorption method using this flame can be applied to the determination of total and extractable manganese in a wide range of geological materials without interferences. Analyses of six U.S. Geological Survey rock standards for manganese gave results in agreement with the reported values. ?? 1978.

Sensitivity improvement for antimony determination by using in-situ atom trapping in a slotted quartz tube and flame atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Titretir, Serap, E-mail: serap.titretir@inonu.edu.tr [Department of Chemistry, Faculty of Arts and Sciences, Inoenue University, 44280 Malatya (Turkey); S Latin-Small-Letter-Dotless-I k, Ahmet Inanc [Department of Chemistry, Faculty of Arts and Sciences, Inoenue University, 44280 Malatya (Turkey); Arslan, Yasin [Department of Chemistry, Faculty of Arts and Sciences, Mehmet Akif Ersoy University, Istiklal Yerleskesi, 15030 Burdur (Turkey); Ataman, O. Yavuz [Department of Chemistry, Faculty of Arts and Sciences, Middle East Technical University, 06800 Ankara (Turkey)

2012-11-15

Significant improvement has been achieved for antimony determination using a slotted quartz tube (SQT) as an atom trap (AT) for in situ preconcentration and flame atomic absorption spectrometry (FAAS). The suggested technique consists of trapping analyte species during ordinary nebulization followed by releasing the collected analyte via introducing organic solvent. Procedures and analytical figures of merit have been presented for the techniques called FAAS, SQT-FAAS and finally SQT-AT-FAAS with the relevant comparisons. Analytical parameters, namely composition of the aqueous medium, sample flow rate, flame conditions, distance between burner head and SQT, sampling period and type of organic solvent and its volume have been optimized. Using SQT-AT-FAAS, a sensitivity enhancement of 369 fold has been obtained, 3 s limit of detection was 3.9 {mu}g L{sup -1} when 25.0 mL of sample was collected in 4.0 min. Interference effects of some elements on antimony signal were studied. - Highlights: Black-Right-Pointing-Pointer Atom trapping in a quartz tube was used for Sb with flame AAS. Black-Right-Pointing-Pointer An inexpensive, simple and sensitive analytical method was suggested for Sb. Black-Right-Pointing-Pointer Almost no background absorption was observed. Black-Right-Pointing-Pointer Range is in microgram per liter level.

Sensitivity improvement for antimony determination by using in-situ atom trapping in a slotted quartz tube and flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Titretir, Serap; Şık, Ahmet İnanç; Arslan, Yasin; Ataman, O. Yavuz

2012-01-01

Significant improvement has been achieved for antimony determination using a slotted quartz tube (SQT) as an atom trap (AT) for in situ preconcentration and flame atomic absorption spectrometry (FAAS). The suggested technique consists of trapping analyte species during ordinary nebulization followed by releasing the collected analyte via introducing organic solvent. Procedures and analytical figures of merit have been presented for the techniques called FAAS, SQT-FAAS and finally SQT-AT-FAAS with the relevant comparisons. Analytical parameters, namely composition of the aqueous medium, sample flow rate, flame conditions, distance between burner head and SQT, sampling period and type of organic solvent and its volume have been optimized. Using SQT-AT-FAAS, a sensitivity enhancement of 369 fold has been obtained, 3 s limit of detection was 3.9 μg L −1 when 25.0 mL of sample was collected in 4.0 min. Interference effects of some elements on antimony signal were studied. - Highlights: ► Atom trapping in a quartz tube was used for Sb with flame AAS. ► An inexpensive, simple and sensitive analytical method was suggested for Sb. ► Almost no background absorption was observed. ► Range is in microgram per liter level.

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

Energy Technology Data Exchange (ETDEWEB)

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.

A dispersive liquid--liquid microextraction methodology for copper (II) in environmental samples prior to determination using microsample injection flame atomic absorption spectrometry.

Science.gov (United States)

Alothman, Zeid A; Habila, Mohamed; Yilmaz, Erkan; Soylak, Mustafa

2013-01-01

A simple, environmentally friendly, and efficient dispersive liquid-liquid microextraction method combined with microsample injection flame atomic absorption spectrometry was developed for the separation and preconcentration of Cu(II). 2-(5-Bromo-2-pyridylazo)-5-(diethylamino)phenol (5-Br-PADAP) was used to form a hydrophobic complex of Cu(II) ions in the aqueous phase before extraction. To extract the Cu(II)-5-Br-PADAP complex from the aqueous phase to the organic phase, 2.0 mL of acetone as a disperser solvent and 200 microL of chloroform as an extraction solvent were used. The influences of important analytical parameters, such as the pH, types and volumes of the extraction and disperser solvents, amount of chelating agent, sample volume, and matrix effects, on the microextraction procedure were evaluated and optimized. Using the optimal conditions, the LOD, LOQ, preconcentration factor, and RSD were determined to be 1.4 microg/L, 4.7 microg/L, 120, and 6.5%, respectively. The accuracy of the proposed method was investigated using standard addition/recovery tests. The analysis of certified reference materials produced satisfactory analytical results. The developed method was applied for the determination of Cu in real samples.

In situ atom trapping of Bi on W-coated slotted quartz tube flame atomic absorption spectrometry and interference studies

Energy Technology Data Exchange (ETDEWEB)

Kılınç, Ersin, E-mail: kilincersin@gmail.com [Medical Laboratory Techniques, Vocational Higher School of Healthcare Studies, Mardin Artuklu University, 47200 Mardin (Turkey); Bakırdere, Sezgin [Yıldız Technical University, Art and Science Faculy, Department of Chemistry, Esenler, TR 34220 İstanbul (Turkey); Aydın, Fırat [Dicle University, Faculty of Science, Department of Chemistry, Laboratory of Chemical Analysis, TR 21280 Diyarbakır (Turkey); Ataman, O. Yavuz [Middle East Technical University, Faculty of Arts and Sciences, Department of Chemistry, 06800 Ankara (Turkey)

2013-11-01

Analytical performances of metal coated slotted quartz tube flame atomic absorption spectrometry (SQT-FAAS) and slotted quartz tube in situ atom trapping flame atomic absorption spectrometry (SQT-AT-FAAS) systems were evaluated for determination of Bi. Non-volatile elements such as Mo, Zr, W and Ta were tried as coating materials. It was observed that W-coated SQT gave the best sensitivity for the determination of Bi for SQT-FAAS and SQT-AT-FAAS. The parameters for W-coated SQT-FAAS and W-coated SQT-AT-FAAS were optimized. Sensitivity of FAAS for Bi was improved as 4.0 fold by W-coated SQT-FAAS while 613 fold enhancement in sensitivity was achieved by W-coated SQT-AT-FAAS using 5.0 min trapping with respect to conventional FAAS. MIBK was selected as organic solvent for the re-atomization of Bi from the trapping surface. Limit of detection values for W-coated SQT-FAAS and W-coated SQT-AT-FAAS was obtained as 0.14 μg mL{sup −1} and 0.51 ng mL{sup −1}, respectively. Linear calibration plot was obtained in the range of 2.5–25.0 ng mL{sup −1} for W-coated SQT-AT-FAAS. Accuracy of the W-coated SQT-AT-FAAS system was checked by analyzing a standard reference material, NIST 1643e. - Highlights: • Further increasing in sensitivity of SQT-AT-FAAS was obtained by using a W coated SQT. • 613 fold sensitivity enhancement was achieved by W coated SQT-AT-FAAS versus FAAS. • A sensitive, rapid and simple technique for Bi was developed with an LOD of 0.51 ng mL{sup −1}. • The technique is suggested for laboratories equipped with only a flame AA spectrometer.

In situ atom trapping of Bi on W-coated slotted quartz tube flame atomic absorption spectrometry and interference studies

International Nuclear Information System (INIS)

Kılınç, Ersin; Bakırdere, Sezgin; Aydın, Fırat; Ataman, O. Yavuz

2013-01-01

Analytical performances of metal coated slotted quartz tube flame atomic absorption spectrometry (SQT-FAAS) and slotted quartz tube in situ atom trapping flame atomic absorption spectrometry (SQT-AT-FAAS) systems were evaluated for determination of Bi. Non-volatile elements such as Mo, Zr, W and Ta were tried as coating materials. It was observed that W-coated SQT gave the best sensitivity for the determination of Bi for SQT-FAAS and SQT-AT-FAAS. The parameters for W-coated SQT-FAAS and W-coated SQT-AT-FAAS were optimized. Sensitivity of FAAS for Bi was improved as 4.0 fold by W-coated SQT-FAAS while 613 fold enhancement in sensitivity was achieved by W-coated SQT-AT-FAAS using 5.0 min trapping with respect to conventional FAAS. MIBK was selected as organic solvent for the re-atomization of Bi from the trapping surface. Limit of detection values for W-coated SQT-FAAS and W-coated SQT-AT-FAAS was obtained as 0.14 μg mL −1 and 0.51 ng mL −1 , respectively. Linear calibration plot was obtained in the range of 2.5–25.0 ng mL −1 for W-coated SQT-AT-FAAS. Accuracy of the W-coated SQT-AT-FAAS system was checked by analyzing a standard reference material, NIST 1643e. - Highlights: • Further increasing in sensitivity of SQT-AT-FAAS was obtained by using a W coated SQT. • 613 fold sensitivity enhancement was achieved by W coated SQT-AT-FAAS versus FAAS. • A sensitive, rapid and simple technique for Bi was developed with an LOD of 0.51 ng mL −1 . • The technique is suggested for laboratories equipped with only a flame AA spectrometer

Preconcentration and determination of iron and copper in spice samples by cloud point extraction and flow injection flame atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Sahin, Cigdem Arpa, E-mail: carpa@hacettepe.edu.tr [Hacettepe University, Chemistry Department, 06800 Beytepe, Ankara (Turkey); Tokgoez, Ilknur; Bektas, Sema [Hacettepe University, Chemistry Department, 06800 Beytepe, Ankara (Turkey)

2010-09-15

A flow injection (FI) cloud point extraction (CPE) method for the determination of iron and copper by flame atomic absorption spectrometer (FAAS) has been improved. The analytes were complexed with 3-amino-7-dimethylamino-2-methylphenazine (Neutral Red, NR) and octylphenoxypolyethoxyethanol (Triton X-114) was added as a surfactant. The micellar solution was heated above 50 {sup o}C and loaded through a column packed with cotton for phase separation. Then the surfactant-rich phase was eluted using 0.05 mol L{sup -1} H{sub 2}SO{sub 4} and the analytes were determined by FAAS. Chemical and flow variables influencing the instrumental and extraction conditions were optimized. Under optimized conditions for 25 mL of preconcentrated solution, the enrichment factors were 98 and 69, the limits of detection (3s) were 0.7 and 0.3 ng mL{sup -1}, the limits of quantification (10s) were 2.2 and 1.0 ng mL{sup -1} for iron and copper, respectively. The relative standard deviation (RSD) for ten replicate measurements of 10 ng mL{sup -1} iron and copper were 2.1% and 1.8%, respectively. The proposed method was successfully applied to determination of iron and copper in spice samples.

Computer programs in BASIC language for atomic absorption flame spectroscopy. Part 2. Documentation

International Nuclear Information System (INIS)

Boyle, W.G. Jr.

1977-01-01

There are three computer programs, written in the BASIC language, used for taking data from an atomic absorption spectrophotometer operating in the flame mode. The programs are divided into logical sections, and these have been flow-charted. The general features, the structure, the order of subroutines and functions, and the storage of data are discussed. In addition, variables are listed and defined, and a complete listing of each program with a symbol occurrence table is provided

Flow injection analysis-flame atomic absorption spectrometry system for indirect determination of sulfite after on-line reduction of solid-phase manganese (IV) dioxide reactor.

Science.gov (United States)

Zare-Dorabei, Rouholah; Boroun, Shokoufeh; Noroozifar, Meissam

2018-02-01

A new and simple flow injection method followed by atomic absorption spectrometry was developed for indirect determination of sulfite. The proposed method is based on the oxidation of sulfite to sulphate ion using solid-phase manganese dioxide (30% W/W suspended on silica gel beads) reactor. MnO 2 will be reduced to Mn(II) by sample injection in to the column under acidic carrier stream of HNO 3 (pH 2) with flow rate of 3.5mLmin -1 at room temperature. Absorption measurement of Mn(II) which is proportional to the concentration of sulfite in the sample was carried out by atomic absorption spectrometry. The calibration curve was linear up to 25mgL -1 with a detection limit (DL) of 0.08mgL -1 for 400µL injection sample volume. The presented method is efficient toward sulfite determination in sugar and water samples with a relative standard deviation (RSD) less than 1.2% and a sampling rate of about 60h -1 . Copyright © 2017 Elsevier B.V. All rights reserved.

Computer programs in BASIC language for atomic absorption flame spectroscopy. Part 1. Operating instructions

International Nuclear Information System (INIS)

Boyle, W.G. Jr.

1977-01-01

These instructions describe how to use three BASIC language programs to process data from atomic absorption spectrophotometers operated in the flame mode. These programs will also control an automatic sampler if desired. The instructions cover loading the programs, responding to computer prompts, choosing among various options for processing the data, operating the automatic sampler, and producing reports. How the programs differ is also explained. Examples of computer/operator dialogue are presented for typical cases

Development and Validation of a Sensitive Method for Trace Nickel Determination by Slotted Quartz Tube Flame Atomic Absorption Spectrometry After Dispersive Liquid-Liquid Microextraction.

Science.gov (United States)

Yolcu, Şükran Melda; Fırat, Merve; Chormey, Dotse Selali; Büyükpınar, Çağdaş; Turak, Fatma; Bakırdere, Sezgin

2018-05-01

In this study, dispersive liquid-liquid microextraction was systematically optimized for the preconcentration of nickel after forming a complex with diphenylcarbazone. The measurement output of the flame atomic absorption spectrometer was further enhanced by fitting a custom-cut slotted quartz tube to the flame burner head. The extraction method increased the amount of nickel reaching the flame and the slotted quartz tube increased the residence time of nickel atoms in the flame to record higher absorbance. Two methods combined to give about 90 fold enhancement in sensitivity over the conventional flame atomic absorption spectrometry. The optimized method was applicable over a wide linear concentration range, and it gave a detection limit of 2.1 µg L -1 . Low relative standard deviations at the lowest concentration in the linear calibration plot indicated high precision for both extraction process and instrumental measurements. A coal fly ash standard reference material (SRM 1633c) was used to determine the accuracy of the method, and experimented results were compatible with the certified value. Spiked recovery tests were also used to validate the applicability of the method.

[Evaluation of uncertainty for determination of tin and its compounds in air of workplace by flame atomic absorption spectrometry].

Science.gov (United States)

Wei, Qiuning; Wei, Yuan; Liu, Fangfang; Ding, Yalei

2015-10-01

To investigate the method for uncertainty evaluation of determination of tin and its compounds in the air of workplace by flame atomic absorption spectrometry. The national occupational health standards, GBZ/T160.28-2004 and JJF1059-1999, were used to build a mathematical model of determination of tin and its compounds in the air of workplace and to calculate the components of uncertainty. In determination of tin and its compounds in the air of workplace using flame atomic absorption spectrometry, the uncertainty for the concentration of the standard solution, atomic absorption spectrophotometer, sample digestion, parallel determination, least square fitting of the calibration curve, and sample collection was 0.436%, 0.13%, 1.07%, 1.65%, 3.05%, and 2.89%, respectively. The combined uncertainty was 9.3%.The concentration of tin in the test sample was 0.132 mg/m³, and the expanded uncertainty for the measurement was 0.012 mg/m³ (K=2). The dominant uncertainty for determination of tin and its compounds in the air of workplace comes from least squares fitting of the calibration curve and sample collection. Quality control should be improved in the process of calibration curve fitting and sample collection.

Manganese dioxide causes spurious gold values in flame atomic-absorption readings from HBr-Br2 digestions

Science.gov (United States)

Campbell, W.L.

1981-01-01

False readings, apparently caused by the presence of high concentrations of manganese dioxide, have been observed in our current flame atomic-absorption procedure for the determination of gold. After a hydrobromic acid (HBr)-bromine (Br2) leach, simply heating the sample to boiling to remove excess Br2 prior to extraction with methyl-isobutyl-ketone (MIBK) eliminates these false readings. ?? 1981.

Coupling continuous ultrasound-assisted extraction, preconcentration and flame atomic absorption spectrometric detection for the determination of cadmium and lead in mussel samples

International Nuclear Information System (INIS)

Yebra-Biurrun, M.C.; Cancela-Perez, S.; Moreno-Cid-Barinaga, A.

2005-01-01

Continuous ultrasound-assisted extraction has been coupled with preconcentration and flame atomic absorption spectrometry for the determination of cadmium and lead in mussel samples. Experimental designs were used for the optimisation of the leaching and preconcentration steps. The use of diluted nitric acid as extractant in the continuous mode at a flow rate of 3.5 ml min -1 and room temperature was sufficient for quantitative extraction of these trace metals. A minicolumn containing a chelating resin (Chelite P, with aminomethylphosphoric acid groups) was proved as an excellent material for the quantitative preconcentration of cadmium and lead prior to their flame atomic absorption detection. A flow injection manifold was used as interface for coupling the three analytical steps, which allowed the automation of the whole analytical process. A good precision of the whole procedure (2.0 and 2.3%), high enrichment factors (20.5 and 11.8) and a detection limit of 0.011 and 0.25 μg g -1 for cadmium and lead, respectively, were obtained for 80 mg of sample. The sample throughputs were ca. 16 and 14 samples h -1 for cadmium and lead, respectively. The accuracy of the analytical procedures was verified by using a standard reference material (BCR 278-R, mussel tissue) and the results were in good agreement with the certified values. The method was successfully applied to the determination of trace amounts of cadmium and lead in mussel samples from the coast of Galicia (NW, Spain)

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

Directory of Open Access Journals (Sweden)

Arpa Şahin Ç.

2013-04-01

Full Text Available A simple, rapid and inexpensive solidified floating organic drop microextraction (SFODME and flow injection flame atomic absorption spectrometric determination (FI-FAAS method for copper was developed. 3-amino-7-dimethylamino-2-methylphenazine (Neutral red, NR was used as the complexing agent. Several factors affecting the microextraction efficiency, such as, pH, NR and sodium dodecylbenzenesulfonate (SDBS concentration, extraction time, stirring rate, and temperature were investigated and optimized. Under optimized experimental conditions an enrichment factor of 541 was obtained for 100 mL of sample solution. The calibration graph was linear in the range of 0.5 – 20.0 ng mL–1 and the limit of detection (3s was 0.18 ng mL–1, the limit of quantification (10s was 0.58 ng mL–1. The relative standard deviation (RSD for 10 replicate measurements of 10 ng mL–1 copper was 2.7%. The developed method was successfully applied to the extraction and determination of copper in different certified reference materials (Estuarine water, Slew 3 and fortified water, TM 23.2 and real water samples and satisfactory results were obtained.

Spectral interferences in atomic absorption spectrometry, (5)

International Nuclear Information System (INIS)

Daidoji, Hidehiro

1979-01-01

Spectral interferences were observed in trace element analysis of concentrated solutions by atomic absorption spectrometry. Molecular absorption and emission spectra for strontium chloride and nitrate, barium chloride and nitrate containing 12 mg/ml of metal ion in airacetylene flame were measured in the wavelength range from 200 to 700 nm. The absorption and emission spectra of SrO were centered near 364.6 nm. The absorption spectra of SrOH around 606.0, 671.0 and 682.0 nm were very strong. And, emission spectrum of BaOH in the wavelength range from 480 to 550 nm was stronger. But, the absorption of this band spectrum was very weak. In the wavelength range from 200 to 400 nm, some unknown bands of absorption were observed for strontium and barium. Absorption spectra of SrCl and BaCl were observed in the argon-hydrogen flame. Also, in the carbon tube atomizer, the absorption spectra of SrCl and BaCl were detected clearly in the wavelength range from 185 to 400 nm. (author)

Elimination of the inter-element interferences of iron, gold, molybdenum, tin and antimony when determined in organic solvents by flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Aneva, Zara; Arpadjan, Sonja

1988-01-01

The mutual interferences in the flame atomic absorption spectrometric determination of iron, gold, molybdenum, tin and antimony after their extraction - pre-concentration as chloride complexes from platinum solutions into isobutyl methyl ketone are investigated. It is suggested that the interferences are caused by chemical reactions in the flame and are influenced by the flame characteristics. The possibility of eliminating the interferences by addition of long-chain quaternary ammonium salts is discussed. (author)

Molecular absorption spectrometry in flames and furnaces: A review

Energy Technology Data Exchange (ETDEWEB)

Butcher, David J., E-mail: butcher@email.wcu.edu

2013-12-04

Graphical abstract: -- Highlights: •Theory and analytical considerations for molecular absorption spectrometry (MAS). •Critical review of low resolution MAS. •Critical review of the analytical performance of high-resolution continuum source (HR-CS) flame MAS. •Critical review of the analytical performance of HR-CS graphite furnace MAS. •Current status of HR-CS MAS and its future prospects for elemental analysis. -- Abstract: Molecular absorption spectrometry (MAS), originally developed in the 1970s, is a technique to determine non-metals in flames and graphite furnaces by monitoring the absorbance of diatomic molecules. Early studies employed low resolution instruments designed for line source atomic absorption, which provided a limited choice of analytical wavelengths, insufficient spectral resolution, and spectral interferences. However, the development of high-resolution continuum source atomic absorption spectrometry (HR-CS AAS) instrumentation has allowed the analysis of challenging samples for non-metals as well as some difficult elements to determine by AAS, such as aluminum and phosphorus. In this review, theory and analytical considerations for MAS are discussed. The principles and limitations of low resolution MAS are described, along with its applications. HR-CS AAS instrumentation is reviewed, emphasizing performance characteristics most relevant for MAS. Applications of flame and HR-CS GFMAS are reviewed, highlighting the most significant work to date. The paper concludes with an evaluation of the enhanced analytical capabilities provided by HR-CS MAS.

Theory of analytical curves in atomic fluorescence flame spectrometry

NARCIS (Netherlands)

Hooymayers, H.P.

An explicit expression for the intensity of atomic resonance fluorescence as a function of atomic concentration in a flame is derived under certain idealized conditions. The expression is generally valid for a pure Doppler absorption line profile as well as for a combined Doppler and collisional

Atomic absorption spectrophotometer

International Nuclear Information System (INIS)

Stockdale, T. J.

1985-01-01

In atomic absorption spectrophotometer, a reference path may be provided for radiation which excludes the flame. This radiation provides a signal from a detector which varies only with the instrumental drift produced by variations in the radiation source brightness and by variations in detector gain. The signal can be used to compensate for drift in other signals received through a sample path including the flame. In the present invention, radiation passes through the sample path continuously during measurement, and only through the reference path between sample measurements. Movable mirrors shift the radiation between the paths upon externally applied commands. Conveniently, the reference path measurement is made while the flame is stabilized during the change between samples. The reference path measurements are stored and used to correct for drift

Combination of solid phase extraction and flame atomic absorption spectrometry for trace analysis of cadmium

OpenAIRE

Ensafi, Ali A.; Shiraz, Ameneh Zendegi

2008-01-01

A new selective method was developed for the separation and preconcentration of Cd(II) ions based on its complex formation with Xylenol orange loaded on activated carbon as a solid support in a mini-column. The preconcentrated ions were eluted by passing 5.0 mL 0.5 mol L-1 HNO3 solution through the solid support and then the Cd(II) contents was measured by flame atomic absorption spectrometry. Conditions for preparation of the modified activated carbon, pH and flow variables were studied, as ...

Determination of five trace elements in leaves in Nanfang sweet orange by flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Li Fangqing

2006-01-01

The five trace elements of copper, zinc, manganese, iron and cobalt in leaves of Nanfang sweet orange are determined by flame atomic absorption spectrometry. The technique is simple, precise and sensitive. The effect of the type of digesting solution (mixed acid), the ratio of mixed acid, the volume of digesting solution and the time of digesting are investigated in details. The results show that leaves of Nanfang sweet orange contain higher amount of iron and zinc. (authors)

Study of new technique of solid combustible materials to determination of volatile elements by flame atomic absorption spectrophotometry

International Nuclear Information System (INIS)

Campos, R.C. de.

1988-01-01

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) [pt

A new approach for the determination of sulphur in food samples by high-resolution continuum source flame atomic absorption spectrometer.

Science.gov (United States)

Ozbek, N; Baysal, A

2015-02-01

The new approach for the determination of sulphur in foods was developed, and the sulphur concentrations of various fresh and dried food samples determined using a high-resolution continuum source flame atomic absorption spectrometer with an air/acetylene flame. The proposed method was optimised and the validated using standard reference materials, and certified values were found to be within the 95% confidence interval. The sulphur content of foods ranged from less than the LOD to 1.5mgg(-1). The method is accurate, fast, simple and sensitive. Copyright © 2014 Elsevier Ltd. All rights reserved.

Modified mesoporous silica materials for on-line separation and preconcentration of hexavalent chromium using a microcolumn coupled with flame atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Wang Zheng, E-mail: wangzheng@mail.sic.ac.cn [Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050 (China); Fang Dongmei; Li Qing [Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050 (China); East China University of Science and Technology, Shanghai 200237 (China); Zhang Lingxia; Qian Rong; Zhu Yan; Qu Haiyun [Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050 (China); Du Yiping [East China University of Science and Technology, Shanghai 200237 (China)

2012-05-06

Highlights: Black-Right-Pointing-Pointer A modified SBA-15 mesoporous silica material (NH{sub 2}-SBA-15) was synthesized as sorbent. Black-Right-Pointing-Pointer The material was used for the first time in a flow injection on-line solid phase extraction (SPE) coupled with flame atomic absorption spectrometry (FAAS) to detect trace Cr (VI). Black-Right-Pointing-Pointer The NH{sub 2}-SBA-15 enables retain Cr (VI) with an enrichment factor of 44. Black-Right-Pointing-Pointer The micro-column of NH{sub 2}-SBA-15 underwent more than 100 adsorption/desorption cycles. - Abstract: A modified SBA-15 mesoporous silica material NH{sub 2}-SBA-15 was synthesized successfully by grafting {gamma}-aminopropyl-triethoxysilane. The material was characterized using transmission electron microscopy (TEM) and Fourier transform infrared/Raman (FT-IR/Raman) spectroscopy, and used for the first time in a flow injection on-line solid phase extraction (SPE) coupled with flame atomic absorption spectrometry (FAAS) to detect trace Cr (VI). Effective sorption of Cr (VI) was achieved at pH 2.0 with no interference from Cr (III) and other ions and 0.5 mol L{sup -1} NH{sub 3}{center_dot}H{sub 2}O solution was found optimal for the complete elution of Cr (VI). An enrichment factor of 44 and was achieved under optimized experimental conditions at a sample loading of 2.0 mL min{sup -1} sample loading (300 s) and an elution flow rate of 2.0 mL min{sup -1} (24 s). The precision of the 11 replicate Cr (VI) measurements was 2.1% at the 100 {mu}g L{sup -1} level with a detection limit of 0.2 {mu}g L{sup -1} (3 s, n = 10) using the FAAS. The developed method was successfully applied to trace chromium determination in waste water. The accuracy was validated using a certified reference material of riverine water (GBW08607).

Ionic liquid ultrasound assisted dispersive liquid-liquid microextraction method for preconcentration of trace amounts of rhodium prior to flame atomic absorption spectrometry determination

Energy Technology Data Exchange (ETDEWEB)

Molaakbari, Elaheh [Chemistry Department, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Young Research Society, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Mostafavi, Ali, E-mail: mostafavi.ali@gmail.com [Chemistry Department, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Afzali, Daryoush [Environment and Nanochemistry Department, Research Institute of Environmental Science, International Center for Science, High Technology and Environmental Science, Kerman (Iran, Islamic Republic of); Mineral Industries Research Center, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of)

2011-01-30

In this article, we consider ionic liquid based ultrasound-assisted dispersive liquid-liquid microextraction of trace amounts of rhodium from aqueous samples and show that this is a fast and reliable sample pre-treatment for the determination of rhodium ions by flame atomic absorption spectrometry. The Rh(III) was transferred into its complex with 2-(5-bromo-2-pyridylazo)-5-diethylamino phenol as a chelating agent, and an ultrasonic bath with the ionic liquid, 1-octyl-3-methylimidazolium bis (trifluoromethylsulfonyl) imide at room temperature was used to extract the analyte. The centrifuged rhodium complex was then enriched in the form of ionic liquid droplets and prior to its analysis by flame atomic absorption spectrometry, 300 {mu}L ethanol was added to the ionic liquid-rich phase. Finally, the influence of various parameters on the recovery of Rh(III) was optimized. Under optimum conditions, the calibration graph was linear in the range of 4.0-500.0 ng mL{sup -1}, the detection limit was 0.37 ng mL{sup -1} (3S{sub b}/m, n = 7) and the relative standard deviation was {+-}1.63% (n = 7, C = 200 ng mL{sup -1}). The results show that ionic liquid based ultrasound assisted dispersive liquid-liquid microextraction, combined with flame atomic absorption spectrometry, is a rapid, simple, sensitive and efficient analytical method for the separation and determination of trace amounts of Rh(III) ions with minimum organic solvent consumption.

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

International Nuclear Information System (INIS)

Sahin, Cigdem Arpa; Tokgoez, Ilknur

2010-01-01

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 10 min. The solidified microdrop was then transferred into a conical vial, where it melted immediately and diluted to 300 μL with ethanol. Finally, copper ions in 200 μL 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 100 mL of solution, the preconcentration factor was 333 and the enrichment factor was 324. The limit of detection (3 s) was 0.4 ng mL -1 , the limit of quantification (10 s) was 1.1 ng mL -1 and the relative standard deviation (RSD) for 10 replicate measurements of 10 ng mL -1 copper was 0.9%. The proposed method was successfully applied to the determination of copper in different water samples.

Atomic spectrometry based on metallic tube atomizers heated by flame: Innovative strategies from fundamentals to analysis

International Nuclear Information System (INIS)

Arruda, Marco Aurelio Zezzi; Figueiredo, Eduardo Costa

2009-01-01

This review describes recent developments in atomic absorption spectrometry using metallic tube atomizers heated by flames. Sample introduction in spray or gaseous form is emphasized, describing some proposed systems for this task and the fundamentals involved in each context. The latest challenges and future possibilities for use of metallic tubes in atomic/mass spectrometry are also considered.

Determination of hafnium by atomic absorption spectrometry

International Nuclear Information System (INIS)

Yoshida, Isao; Kobayashi, Hiroshi; Ueno, Keihei.

1977-01-01

Optimum conditions for atomic absorption spectrophotometric determination of hafnium were investigated by use of a Jarrel-Ash AA-1 instrument which was equipped with a premixed gas burner slotted 50 mm in length and 0.4 mm in width. Absorption of hafnium, which was atomized in an nitrous oxide-acetylene flame, was measured on a resonance line at 307.29 nm. The absorption due to hafnium was enhanced in the presence of ammonium fluoride and iron(III) ion, as shown in Figs. 2 and 3, depending on their concentration. The highest absorption was attained by the addition of (0.15 -- 0.3)M ammonium fluoride, 0.07 M of iron(III) ion and 0.05 M of hydrochloric acid. An excess of the additives decreased the absorption. The presence of zirconium, which caused a significant interference in the ordinary analytical methods, did not affect the absorption due to hafnium, if the zirconium concentration is less than 0.2 M. A standard procedure was proposed; A sample containing a few mg of hafnium was dissolved in a 25-ml volumetric flask, and ammonium fluoride, ferric nitrate and hydrochloric acid were added so that the final concentrations were 0.3, 0.07 and 0.05 M, respectively. Atomic absorption was measured on the aqueous solution in a nitrous oxide-acetylene flame and the hafnium content was calculated from the absorbance. Sensitivity was as high as 12.5 μg of Hf/ml/l% absorption. The present method is especially recommendable to the direct determination of hafnium in samples containing zirconium. (auth.)

[Determination of inorganic elements in different parts of Sonchus oleraceus L by flame atomic absorption spectrometry].

Science.gov (United States)

Wang, Nai-Xing; Cui, Xue-Gui; Du, Ai-Qin; Mao, Hong-Zhi

2007-06-01

Flame atomic absorption spectrometry with air-acetylene flame was used for the determination of inorganic metal elements in different parts ( flower, leaf, stem and root) of Sonchus oleraceus L. The contents of Ca, Mg, K, Na, Fe, Mn, Cu, Zn, Cr, Co, Ni, Pb and Cd in the flower, leaf, stem and root of Sonchus oleraceus L were compared. The order from high to low of the additive weight (microg x g(-1)) for the 13 kinds of metal elements is as follows: leaf (77 213.72) > flower (47 927.15) > stem(42 280.99) > root (28 131.18). From the experimental results it was found that there were considerable differences in the contents of the metal elements in different parts, and there were richer contents of Fe, Zn, Mn and Cu in root and flower, which are necessary to human health, than in other parts.

The coupling of rapidly synergistic cloud point extraction with thermospray flame furnace atomic absorption spectrometry

International Nuclear Information System (INIS)

Wen, X.; Deng, Q.; Guo, J.; Zhao, X.; Zhao, Y.; Ji, S.

2012-01-01

Rapidly synergistic cloud point extraction (RS-CPE) was coupled with thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) to result in new CPE patterns and accelerated (1 min) protocols. It is demonstrated, for the case of copper (II) ion, that TS-FF-AAS improves the sampling efficiency and the sensitivity of FAAS determinations. Problems of nebulization associated with previous methods based on the coupling of FAAS and RS-CPE are overcome. TS-FF-AAS also improves sensitivity and gives a limit of detection for copper of 0.20 μg L -1 , which is better by a factor of 32. Compared to direct FAAS, the factor is 114. (author)

A preconcentration system for determination of copper and nickel in water and food samples employing flame atomic absorption spectrometry.

Science.gov (United States)

Tuzen, Mustafa; Soylak, Mustafa; Citak, Demirhan; Ferreira, Hadla S; Korn, Maria G A; Bezerra, Marcos A

2009-03-15

A separation/preconcentration procedure using solid phase extraction has been proposed for the flame atomic absorption spectrometric determination of copper and nickel at trace level in food samples. The solid phase is Dowex Optipore SD-2 resin contained on a minicolumn, where analyte ions are sorbed as 5-methyl-4-(2-thiazolylazo) resorcinol chelates. After elution using 1 mol L(-1) nitric acid solution, the analytes are determinate employing flame atomic absorption spectrometry. The optimization step was performed using a full two-level factorial design and the variables studied were: pH, reagent concentration (RC) and amount of resin on the column (AR). Under the experimental conditions established in the optimization step, the procedure allows the determination of copper and nickel with limit of detection of 1.03 and 1.90 microg L(-1), respectively and precision of 7 and 8%, for concentrations of copper and nickel of 200 microg L(-1). The effect of matrix ions was also evaluated. The accuracy was confirmed by analyzing of the followings certified reference materials: NIST SRM 1515 Apple leaves and GBW 07603 Aquatic and Terrestrial Biological Products. The developed method was successfully applied for the determination of copper and nickel in real samples including human hair, chicken meat, black tea and canned fish.

A preconcentration system for determination of copper and nickel in water and food samples employing flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Tuzen, Mustafa; Soylak, Mustafa; Citak, Demirhan; Ferreira, Hadla S.; Korn, Maria G.A.; Bezerra, Marcos A.

2009-01-01

A separation/preconcentration procedure using solid phase extraction has been proposed for the flame atomic absorption spectrometric determination of copper and nickel at trace level in food samples. The solid phase is Dowex Optipore SD-2 resin contained on a minicolumn, where analyte ions are sorbed as 5-methyl-4-(2-thiazolylazo) resorcinol chelates. After elution using 1 mol L -1 nitric acid solution, the analytes are determinate employing flame atomic absorption spectrometry. The optimization step was performed using a full two-level factorial design and the variables studied were: pH, reagent concentration (RC) and amount of resin on the column (AR). Under the experimental conditions established in the optimization step, the procedure allows the determination of copper and nickel with limit of detection of 1.03 and 1.90 μg L -1 , respectively and precision of 7 and 8%, for concentrations of copper and nickel of 200 μg L -1 . The effect of matrix ions was also evaluated. The accuracy was confirmed by analyzing of the followings certified reference materials: NIST SRM 1515 Apple leaves and GBW 07603 Aquatic and Terrestrial Biological Products. The developed method was successfully applied for the determination of copper and nickel in real samples including human hair, chicken meat, black tea and canned fish

Monitoring content of cadmium, calcium, copper, iron, lead, magnesium and manganese in tea leaves by electrothermal and flame atomizer atomic absorption spectrometry

Directory of Open Access Journals (Sweden)

Prkić Ante

2017-08-01

Full Text Available Due to the simplicity of tea preparation (pouring hot water onto different dried herbs and its high popularity as a beverage, monitoring and developing a screening methodology for detecting the metal content is very important. The concentrations of Cd, Ca, Cu, Fe, Pb, Mg and Mn in 11 different samples of sage (Salvia officinalis L., linden (Tilia L. and chamomile (Matricaria chamomilla L. purchased at local herbal pharmacy were determined using electrothermal atomizer atomic absorption spectrometry (ETAAS and flame atomizer atomic absorption spectrometry (FAAS. The concentrations determined were: Cd (0.012 – 0.470 mg kg−1, Ca (5209 – 16340 mg kg−1, Cu (22.01 – 33.05 mg kg−1, Fe (114.2 – 440.3 mg kg−1, Pb (0.545 – 2.538 mg kg−1, Mg (2649 – 4325 mg kg−1 and Mn (34.00 – 189.6 mg kg−1. Principal Component Analysis (PCA was applied to identify factors (soil and climate influencing the content of the measured elements in herbal samples. The proposed methodology developed in this work was successfully applied to the detection of metals in herbal samples. The analysis showed that the content of toxic metals in herbal teas was below the maximum dose recommended by the World Health Organization (WHO.

Influence of soil composition in the determination of chromium by atomic absorption spectrometry with flame air / acetylene

International Nuclear Information System (INIS)

Duran Sosa, Ibis; Granda Valdes, Mayra; Pomares Alfonso, Mario Simeon

2014-01-01

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

Speciation of four selenium compounds using high performance liquid chromatography with on-line detection by inductively coupled plasma mass spectrometry or flame atomic absorption spectrometry

DEFF Research Database (Denmark)

Pedersen, Gitte Alsing; Larsen, Erik Huusfeldt

1997-01-01

An analytical method for the speciation of selenomethionine, selenocystine, selenite and selenate by high performance liquid chromatography (HPLC) with atomic spectrometric detection is presented. An organic polymeric strong anion exchange column was used as the stationary phase in combination...... spectrometry (ICP-MS). The signal-to-noise ratio of the FAAS detector was optimized using a hydrogen-argon entrained-air flame and a slotted-tube atom trap (STAT) in the flame. The limit of detection (3 sigma) achieved by the HPLC-FAAS system was 1 mg L-1 of selenium (100 mu L injections) for each of the four...

Determination of Fe Content of Some Food Items by Flame Atomic Absorption Spectroscopy (FAAS): A Guided-Inquiry Learning Experience in Instrumental Analysis Laboratory

Science.gov (United States)

Fakayode, Sayo O.; King, Angela G.; Yakubu, Mamudu; Mohammed, Abdul K.; Pollard, David A.

2012-01-01

This article presents a guided-inquiry (GI) hands-on determination of Fe in food samples including plantains, spinach, lima beans, oatmeal, Frosted Flakes cereal (generic), tilapia fish, and chicken using flame atomic absorption spectroscopy (FAAS). The utility of the GI experiment, which is part of an instrumental analysis laboratory course,…

A preconcentration system for determination of copper and nickel in water and food samples employing flame atomic absorption spectrometry

OpenAIRE

Tuzen, Mustafa; Soylak, Mustafa; Citak, Demirhan; Ferreira, Hadla S.; Korn, Maria das Graças Andrade; Bezerra, Marcos de Almeida

2009-01-01

Texto completo: acesso restrito. p. 1041-1045 A separation/preconcentration procedure using solid phase extraction has been proposed for the flame atomic absorption spectrometric determination of copper and nickel at trace level in food samples. The solid phase is Dowex Optipore SD-2 resin contained on a minicolumn, where analyte ions are sorbed as 5-methyl-4-(2-thiazolylazo) resorcinol chelates. After elution using 1 mol L−1 nitric acid solution, the analytes are determinate employing fla...

A method optimization study for atomic absorption ...

African Journals Online (AJOL)

Sadia Ata

2014-04-24

Apr 24, 2014 ... Manufacturer brand Win 2.1 software was used for data inte- gration and processing. ... reagents and analyst) is suitable for the intended application. The % relative standard deviation for absorbance ... flame atomic absorption spectrometry. Table 2 Linearity data for analysis of zinc in insulin using AAS.

A preconcentration system for determination of copper and nickel in water and food samples employing flame atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Tuzen, Mustafa [Department of Chemistry, Gaziosmanpasa University, 60250 Tokat (Turkey); Soylak, Mustafa [Department of Chemistry, Erciyes University, 38039 Kayseri (Turkey)], E-mail: soylak@erciyes.edu.tr; Citak, Demirhan [Department of Chemistry, Gaziosmanpasa University, 60250 Tokat (Turkey); Ferreira, Hadla S.; Korn, Maria G.A. [Universidade Federal da Bahia, Instituto de Quimica, 40170-290 Salvador (Brazil); Bezerra, Marcos A. [Universidade Estadual do Sudoeste da Bahia, 45200-190 Jequie (Brazil)

2009-03-15

A separation/preconcentration procedure using solid phase extraction has been proposed for the flame atomic absorption spectrometric determination of copper and nickel at trace level in food samples. The solid phase is Dowex Optipore SD-2 resin contained on a minicolumn, where analyte ions are sorbed as 5-methyl-4-(2-thiazolylazo) resorcinol chelates. After elution using 1 mol L{sup -1} nitric acid solution, the analytes are determinate employing flame atomic absorption spectrometry. The optimization step was performed using a full two-level factorial design and the variables studied were: pH, reagent concentration (RC) and amount of resin on the column (AR). Under the experimental conditions established in the optimization step, the procedure allows the determination of copper and nickel with limit of detection of 1.03 and 1.90 {mu}g L{sup -1}, respectively and precision of 7 and 8%, for concentrations of copper and nickel of 200 {mu}g L{sup -1}. The effect of matrix ions was also evaluated. The accuracy was confirmed by analyzing of the followings certified reference materials: NIST SRM 1515 Apple leaves and GBW 07603 Aquatic and Terrestrial Biological Products. The developed method was successfully applied for the determination of copper and nickel in real samples including human hair, chicken meat, black tea and canned fish.

Sensitive determination of bismuth by flame atomic absorption spectrometry using atom trapping in a slotted quartz tube and revolatilization with organic solvent pulse

International Nuclear Information System (INIS)

Kılınç, Ersin; Bakırdere, Sezgin; Aydın, Fırat; Ataman, O. Yavuz

2012-01-01

Sensitivity of flame atomic absorption spectrometry (FAAS) for Bi determination was improved by slotted quartz tube (SQT) that was used also for atom trapping (AT). The trapped analyte was released by aspirating a small volume of organic solvent after a reasonable analyte collection time. Sensitivity was improved by 2.9 times by SQT-FAAS and 256 times by SQT-AT-FAAS with respect to FAAS. Optimum trapping period was found to be 6.0 min (36.0 mL of solution). Limit of detection (LOD) for SQT-AT-FAAS was found to be 1.6 ng mL −1 . %RSD was calculated as 4.0% for five replicate measurements of 7.5 ng mL −1 Bi by SQT-AT-FAAS. Accuracy of the method developed was checked by analyzing a standard reference material of simulated fresh water (NIST 1643e) and result found was in good agreement with the certified one. The method can be applied in any laboratory equipped with a flame AA spectrometer. The consumption of time and sample volume is fairly low and application is simple and easy.

Sensitive determination of bismuth by flame atomic absorption spectrometry using atom trapping in a slotted quartz tube and revolatilization with organic solvent pulse

Energy Technology Data Exchange (ETDEWEB)

K Latin-Small-Letter-Dotless-I l Latin-Small-Letter-Dotless-I nc, Ersin, E-mail: ekilinc@dicle.edu.tr [Dicle University, Faculty of Science, Department of Chemistry, Laboratory of Chemical Analysis, TR 21280 Diyarbak Latin-Small-Letter-Dotless-I r (Turkey); Bak Latin-Small-Letter-Dotless-I rdere, Sezgin [Y Latin-Small-Letter-Dotless-I ld Latin-Small-Letter-Dotless-I z Technical University, Faculty of Education, Department of Science Education, TR 34210 Esenler-Istanbul (Turkey); Ayd Latin-Small-Letter-Dotless-I n, F Latin-Small-Letter-Dotless-I rat [Dicle University, Faculty of Science, Department of Chemistry, Laboratory of Chemical Analysis, TR 21280 Diyarbak Latin-Small-Letter-Dotless-I r (Turkey); Ataman, O. Yavuz [Middle East Technical University, Faculty of Arts and Sciences, Department of Chemistry, 06800 Ankara (Turkey)

2012-07-15

Sensitivity of flame atomic absorption spectrometry (FAAS) for Bi determination was improved by slotted quartz tube (SQT) that was used also for atom trapping (AT). The trapped analyte was released by aspirating a small volume of organic solvent after a reasonable analyte collection time. Sensitivity was improved by 2.9 times by SQT-FAAS and 256 times by SQT-AT-FAAS with respect to FAAS. Optimum trapping period was found to be 6.0 min (36.0 mL of solution). Limit of detection (LOD) for SQT-AT-FAAS was found to be 1.6 ng mL{sup -1}. %RSD was calculated as 4.0% for five replicate measurements of 7.5 ng mL{sup -1} Bi by SQT-AT-FAAS. Accuracy of the method developed was checked by analyzing a standard reference material of simulated fresh water (NIST 1643e) and result found was in good agreement with the certified one. The method can be applied in any laboratory equipped with a flame AA spectrometer. The consumption of time and sample volume is fairly low and application is simple and easy.

Atomic absorption analysis of serial titanium alloys

International Nuclear Information System (INIS)

Gorlova, M.N.; Feofanova, N.M.; Kornyushkova, Yu.D.

1977-01-01

Atom-absorption technique is described, which makes it possible to rapidly and precisely determine the following alloying elements and admixtures in titanium alloys: Al (2.0 - 8.5%); Mo (0.5 - 8%); Cr (0.5 - 12%); Si (0.2 - 0.5%); Mn(0.2 - 2.5%); V(0.5 - 6%); Sn(2.0 - 3.0%); Fe(0.1 - 1.0%); Zr(2.0 - 12.0%). The atom absorption method with flame atomization of the sample provides for best results if the alloy is dissolved in a mixture HCl + HBF 4 in the ratio 2:1. In order to obtain correct results the standard solutions must contain titanium in concentrations corresponding to the weight of the sample being analyzed. Sensitivity of zirconium determination may be increased approximately twofold by adding 10 mg/ml of FeCl 3 into the solution. Being as precise, as the classic analytical methods, the atom absorption technique is about 5 times more efficient

Validation of an analytical method based on the high-resolution continuum source flame atomic absorption spectrometry for the fast-sequential determination of several hazardous/priority hazardous metals in soil.

Science.gov (United States)

Frentiu, Tiberiu; Ponta, Michaela; Hategan, Raluca

2013-03-01

The aim of this paper was the validation of a new analytical method based on the high-resolution continuum source flame atomic absorption spectrometry for the fast-sequential determination of several hazardous/priority hazardous metals (Ag, Cd, Co, Cr, Cu, Ni, Pb and Zn) in soil after microwave assisted digestion in aqua regia. Determinations were performed on the ContrAA 300 (Analytik Jena) air-acetylene flame spectrometer equipped with xenon short-arc lamp as a continuum radiation source for all elements, double monochromator consisting of a prism pre-monocromator and an echelle grating monochromator, and charge coupled device as detector. For validation a method-performance study was conducted involving the establishment of the analytical performance of the new method (limits of detection and quantification, precision and accuracy). Moreover, the Bland and Altman statistical method was used in analyzing the agreement between the proposed assay and inductively coupled plasma optical emission spectrometry as standardized method for the multielemental determination in soil. The limits of detection in soil sample (3σ criterion) in the high-resolution continuum source flame atomic absorption spectrometry method were (mg/kg): 0.18 (Ag), 0.14 (Cd), 0.36 (Co), 0.25 (Cr), 0.09 (Cu), 1.0 (Ni), 1.4 (Pb) and 0.18 (Zn), close to those in inductively coupled plasma optical emission spectrometry: 0.12 (Ag), 0.05 (Cd), 0.15 (Co), 1.4 (Cr), 0.15 (Cu), 2.5 (Ni), 2.5 (Pb) and 0.04 (Zn). Accuracy was checked by analyzing 4 certified reference materials and a good agreement for 95% confidence interval was found in both methods, with recoveries in the range of 94-106% in atomic absorption and 97-103% in optical emission. Repeatability found by analyzing real soil samples was in the range 1.6-5.2% in atomic absorption, similar with that of 1.9-6.1% in optical emission spectrometry. The Bland and Altman method showed no statistical significant difference between the two spectrometric

Flame and flameless atomic-absorption determination of tellurium in geological materials

Science.gov (United States)

Chao, T.T.; Sanzolone, R.F.; Hubert, A.E.

1978-01-01

The sample is digested with a solution of hydrobromic acid and bromine and the excess of bromine is expelled. After dilution of the solution to approximately 3 M in hydrobromic acid, ascorbic acid is added to reduce iron(III) before extraction of tellurium into methyl isobutyl ketone (MIBK). An oxidizing air-acetylene flame is used to determine tellurium in the 0.1-20 ppm range. For samples containing 4-200 ppb of tellurium, a carbon-rod atomizer is used after the MIBK extract has been washed with 0.5 M hydrobromic acid to remove the residual iron. The flame procedure is useful for rapid preliminary monitoring, and the flameless procedure can determine tellurium at very low concentrations. ?? 1978.

Determination of calcium in Mashhad city tap water by flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Mashhadian, N.V.

2012-01-01

Summary: Calcium in drinking water is one of the sources of calcium that may contribute significantly to the daily calcium intake. In this study, the samples of tap water were randomly taken from five zones of Mashhad city. Calcium concentration was determined by flame atomic absorption spectrometry (FAAS) technique. The precision of the method was evaluated. The CV% of 6 replicate determinations at 5 macro g/ml Ca was 4.2 in one day and 4.5, among 6 consecutive days. The recovery of spiked samples (98.7%) also showed that the proposed method is reliable for the determination of amounts of calcium in water samples. The mean of calcium in tap water in the city of Mashhad was 52.61+-12.91 (SD) macro g/ml. At present, the amount of calcium in Mashhad tap waters is within the national standard. However, due to the climate and environmental changes, determination of calcium in tap water of Mashhad in different seasons is recommended. (author)

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

Directory of Open Access Journals (Sweden)

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.

Atomic-absorption determination of mercury in geological materials by flame and carbon-rod atomisation after solvent extraction and using co-extracted silver as a matrix modifier

Science.gov (United States)

Sanzolone, R.F.; Chao, T.T.

1983-01-01

Based on modifications and expansion of the original Tindall's solvent extraction flame atomic-absorption procedure, an atomic-absorption spectrophotometric method has been developed for the determination of mercury in geological materials. The sample is digested with nitric and hydrochloric acids in a boiling water-bath. The solution is made ammoniacal and potassium iodide and silver nitrate are added. The mercury is extracted into isobutyl methyl ketone as the tetraiodomercurate(ll). Added silver is co-extracted with mercury and serves as a matrix modifier in the carbon-rod atomiser. The mercury in the isobutyl methyl ketone extract may be determined by either the flame- or the carbon-rod atomisation method, depending on the concentration level. The limits of determination are 0.05-10 p.p.m. of mercury for the carbon-rod atomisation and 1 -200 p.p.m. of mercury for the flame atomisation. Mercury values for reference samples obtained by replicate analyses are in good agreement with those reported by other workers, with relative standard deviations ranging from 2.3 to 0.9%. Recoveries of mercury spiked at two levels were 93-106%. Major and trace elements commonly found in geological materials do not interfere.

Atomic Absorption Spectroscopy. The Present and the Future.

Science.gov (United States)

Slavin, Walter

1982-01-01

The status of current techniques and methods of atomic absorption (AA) spectroscopy (flame, hybrid, and furnace AA) is discussed, including limitations. Technological opportunities and how they may be used in AA are also discussed, focusing on automation, microprocessors, continuum AA, hybrid analyses, and others. (Author/JN)

Ion Imprinted Polymer for Preconcentration and Determination of Ultra-Trace Cadmium, Employing Flow Injection Analysis with Thermo Spray Flame Furnace Atomic Absorption Spectrometry.

Science.gov (United States)

do Lago, Ayla Campos; Marchioni, Camila; Mendes, Tássia Venga; Wisniewski, Célio; Fadini, Pedro Sergio; Luccas, Pedro Orival

2016-11-01

This work proposes a preconcentration method using an ion imprinted polymer (IIP) for determination of cadmium, in several samples, employing a mini-column filled with the polymer coupled into a flow injection analysis system with detection by thermospray flame furnace atomic absorption spectrometry (FIA-TS-FF-AAS). The polymer was synthesized via bulk using methacrylic acid and vinylimidazole as a functional monomer. For the FIA system initial assessment, the variables: pH, eluent concentration and buffer concentration were studied, employing a 23 full factorial design. To obtain the optimum values for each significant variable, a Doehlert matrix was employed. After the optimization conditions as: pH 5.8, eluent (HNO3) concentration of 0.48 mol L -1 and buffer concentration of 0.01 mol L -1 , were adopted. The proposed method showed a linear response in the range of 0.081-10.0 μg L -1 , limits detection and quantification of 0.024 and 0.081 μg L -1 , respectively; preconcentration factor of 165, consumptive index of 0.06 mL, concentration efficiency 132 min -1 , and frequency of readings equal to 26 readings h -1 The accuracy was checked by analysis of certified reference materials for trace metals and recovery tests. The obtained results were in agreement with 95% confidence level (t-test). The method was adequate to apply in samples of: jewelry (earrings) (2.38 ± 0.28 μg kg -1 ), black tea (1.09 ± 0.15 μg kg -1 ), green tea (3.85 ± 0.13 μg kg -1 ), cigarette tobacco (38.27 ± 0.22 μg kg -1 ), and hair (0.35 ± 0.02 μg kg -1 ). © The Author(s) 2016.

[Determination of mercury in Boletus impolitus by flow injection-atomic absorption spectrometry].

Science.gov (United States)

Li, Tao; Wang, Yuan-Zhong

2008-04-01

Various test conditions and effect factors for the determination of mercury by flow injection-atomic absorption spectrometry were discussed, and a method for the determination of mercury in Boletus impolitus has been developed. The linear range for mercury is 0-60 microg x L(-1). The relative standard deviation is less than 3.0%, and the recovery is 96%-107%. This method is simple, rapid and has been applied to the determination of mercury in Boletus impolitus samples with satisfactory results.

Lead determination at ng/mL level by flame atomic absorption spectrometry using a tantalum coated slotted quartz tube atom trap.

Science.gov (United States)

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

Simultaneous multi-element atomic absorption system using photodiode array detector

International Nuclear Information System (INIS)

Tong, S.L.; Chin, K.S.

1994-01-01

A photodiode array (PDA) detector-multichannel analyser (MCA) system has been coupled to a flame and a graphite furnace atomiser and tested for simultaneous multielement atomic absorption analysis. Multielement hollow cathode lamps (HCL) are used as light source. Spectral lines are dispersed through a spectrograph with triple gratings and detected by a 25.4 mm PDA detector consisting of 1024 elements. The optical MCA system is capable of recording multiple spectra spanned by the spectrograph/PDA. The transmitted intensity spectra obtained for the standard and analyte solutions during flame or graphite furnace atomisation are converted to absorbance spectra using the MCA software provided. Results from the comparison studies show that the linear range and sensitivities for Ni-Co-Fe and Cu-Cr obtained from the simultaneous measurements are within the same order of magnitudes as those from conventional single element determinations using photomultiplier tube detection. The study also shows that non-atomic absorption can be readily corrected by a two-line method where non-atomic absorption lines can be chosen from the spectra recorded simultaneously. The proposed system has been evaluated for the determination of trace elements using NBS standard reference water SRM 1643b

Visualizing the Solute Vaporization Interference in Flame Atomic Absorption Spectroscopy

Science.gov (United States)

Dockery, Christopher R.; Blew, Michael J.; Goode, Scott R.

2008-01-01

Every day, tens of thousands of chemists use analytical atomic spectroscopy in their work, often without knowledge of possible interferences. We present a unique approach to study these interferences by using modern response surface methods to visualize an interference in which aluminum depresses the calcium atomic absorption signal. Calcium…

On-line preconcentration system using a microcolumn packed with Alizarin Red S-modified alumina for zinc determination by flame atomic absorption spectrometry

Directory of Open Access Journals (Sweden)

A.M. Haji Shabani

2009-01-01

Full Text Available A simple and sensitive on-line flow injection system for determination of zinc with FAAS has been described. The method is based on the separation and preconcentration of zinc on a microcolumn of immobilized Alizarin Red S on alumina. The adsorbed analyte is then eluted with 250 µL of nitric acid (1 mol L-1 and is transported to flame atomic absorption spectrometer for quantification. The effect of pH, sample and eluent flow rates and presence of various cations and anions on the retention of zinc was investigated. The sorption of zinc was quantitative in the pH range of 5.5-8.5. For a sample volume of 25 mL an enrichment factor of 144 and a detection limit (3S of 0.2 µg L-1 was obtained. The precision (RSD, n=7 was 3.0% at the 20 µg L-1 level. The developed system was successfully applied to the determination of zinc in water samples, hair, urine and saliva.

Ultratrace Determination of Cr(VI and Pb(II by Microsample Injection System Flame Atomic Spectroscopy in Drinking Water and Treated and Untreated Industrial Effluents

Directory of Open Access Journals (Sweden)

Jameel Ahmed Baig

2013-01-01

Full Text Available Simple and robust analytical procedures were developed for hexavalent chromium (Cr(VI and lead (Pb(II by dispersive liquid-liquid microextraction (DLLME using microsample injection system coupled with flame atomic absorption spectrophotometry (MIS-FAAS. For the current study, ammonium pyrrolidine dithiocarbamate (APDC, carbon tetrachloride, and ethanol were used as chelating agent, extraction solvent, and disperser solvent, respectively. The effective variables of developed method have been optimized and studied in detail. The limit of detection of Cr(VI and Pb(II were 0.037 and 0.054 µg/L, respectively. The enrichment factors in both cases were 400 with 40 mL of initial volumes. The relative standard deviations (RSDs, were 96%. The proposed method was successfully applied to the determination of Cr(VI and Pb(II at ultratrace levels in natural drinking water and industrial effluents wastewater of Denizli. Moreover, the proposed method was compared with the literature reported method.

Application of Internal Standard Method for Several 3d-Transition Metallic Elements in Flame Atomic Absorption Spectrometry Using a Multi-wavelength High-resolution Spectrometer.

Science.gov (United States)

Toya, Yusuke; Itagaki, Toshiko; Wagatsuma, Kazuaki

2017-01-01

We investigated a simultaneous internal standard method in flame atomic absorption spectrometry (FAAS), in order to better the analytical precision of 3d-transition metals contained in steel materials. For this purpose, a new spectrometer system for FAAS, comprising a bright xenon lamp as the primary radiation source and a high-resolution Echelle monochromator, was employed to measure several absorption lines at a wavelength width of ca. 0.3 nm at the same time, which enables the absorbances of an analytical line and also an internal standard line to be estimated. In considering several criteria for selecting an internal standard element and the absorption line, it could be suggested that platinum-group elements: ruthenium, rhodium, or palladium, were suitable for an internal standard element to determine the 3d-transition metal elements, such as titanium, iron, and nickel, by measuring an appropriate pair of these absorption lines simultaneously. Several variances of the absorption signal, such as a variation in aspirated amounts of sample solution and a short-period drift of the primary light source, would be corrected and thus reduced, when the absorbance ratio of the analytical line to the internal standard line was measured. In Ti-Pd, Ni-Rh, and Fe-Ru systems chosen as typical test samples, the repeatability of the signal respnses was investigated with/without the internal standard method, resulting in better precision when the internal standard method was applied in the FAAS with a nitrous oxide-acetylene flame rather than an air-acetylene flame.

Design considerations regarding an atomizer for multi-element electrothermal atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Katskov, Dmitri A., E-mail: katskovda@tut.ac.za [Department of Chemistry, Tshwane University of Technology, Private Bag X680, Pretoria 0001 (South Africa); Sadagov, Yuri M. [All-Russian Scientific Research Institute of Optical and Physical Measurements (VNIIOFI), Ozernaya St. 46, Moscow 119361 (Russian Federation)

2011-06-15

determination in Flame AAS with primary line source that is 50-1000 times higher than the limits obtainable with common ETAAS (Electrothermal Atomic Absorption Spectrometry) instrumentation.

Bismuth as a general internal standard for lead in atomic absorption spectrometry.

Science.gov (United States)

Bechlin, Marcos A; Fortunato, Felipe M; Ferreira, Edilene C; Gomes Neto, José A; Nóbrega, Joaquim A; Donati, George L; Jones, Bradley T

2014-06-11

Bismuth was evaluated as internal standard for Pb determination by line source flame atomic absorption spectrometry (LS FAAS), high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS) and line source graphite furnace atomic absorption spectrometry (LS GFAAS). Analysis of samples containing different matrices indicated close relationship between Pb and Bi absorbances. Correlation coefficients of calibration curves built up by plotting A(Pb)/A(Bi)versus Pb concentration were higher than 0.9953 (FAAS) and higher than 0.9993 (GFAAS). Recoveries of Pb improved from 52-118% (without IS) to 97-109% (IS, LS FAAS); 74-231% (without IS) to 96-109% (IS, HR-CS FAAS); and 36-125% (without IS) to 96-110% (IS, LS GFAAS). The relative standard deviations (n=12) were reduced from 0.6-9.2% (without IS) to 0.3-4.3% (IS, LS FAAS); 0.7-7.7% (without IS) to 0.1-4.0% (IS, HR-CS FAAS); and 2.1-13% (without IS) to 0.4-5.9% (IS, LS GFAAS). Copyright © 2014 Elsevier B.V. All rights reserved.

Atomic-absorption determination of tantalum and niobium in ore concentrates

International Nuclear Information System (INIS)

Elinson, S.V.; Korovin, Yu.I.; Kuchumov, V.A.

1975-01-01

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

Rapid determination of main components by means of flame-atomic-absorption spectrometry for chromium, silicon and tungsten in CrSiW materials

International Nuclear Information System (INIS)

Mueller, E.; Stahlberg, R.

1985-01-01

The application of Flame-Atomic-Absorption Spectrometry (FAAS) for determining chromium, silicon and tungsten in CrSiW materials is described. The FAAS determinations of the main components are shown under optimum conditions. Sufficient precision and reliability have been achieved for routine analysis. The application of a mixture of acids for preparing CrSiW solutions is proposed. The preparation of samples is discussed in detail. Optimum conditions are recommended for determining chromium, silicon and tungsten using one solution only. (orig.) [de

Method development for the determination of fluorine in toothpaste via molecular absorption of aluminum mono fluoride using a high-resolution continuum source nitrous oxide/acetylene flame atomic absorption spectrophotometer.

Science.gov (United States)

Ozbek, Nil; Akman, Suleyman

2012-05-30

Fluorine was determined via the rotational molecular absorption line of aluminum mono fluoride (AlF) generated in C(2)H(2)/N(2)O flame at 227.4613 nm using a high-resolution continuum source flame atomic absorption spectrophotometer (HR-CS-FAAS). The effects of AlF wavelength, burner height, fuel rate (C(2)H(2)/N(2)O) and amount of Al on the accuracy, precision and sensitivity were investigated and optimized. The Al-F absorption band at 227.4613 nm was found to be the most suitable analytical line with respect to sensitivity and spectral interferences. Maximum sensitivity and a good linearity were obtained in acetylene-nitrous oxide flame at a flow rate of 210 L h(-1) and a burner height of 8mm using 3000 mg L(-1) of Al for 10-1000 mg L(-1)of F. The accuracy and precision of the method were tested by analyzing spiked samples and waste water certified reference material. The results were in good agreement with the certified and spiked amounts as well as the precision of several days during this study was satisfactory (RSD<10%). The limit of detection and characteristic concentration of the method were 5.5 mg L(-1) and 72.8 mg L(-1), respectively. Finally, the fluorine concentrations in several toothpaste samples were determined. The results found and given by the producers were not significantly different. The method was simple, fast, accurate and sensitive. Copyright © 2012 Elsevier B.V. All rights reserved.

Atomic absorption spectrophotometry of europium using an enhancing effect of ammonium perchlorate

International Nuclear Information System (INIS)

Oguro, Hiroshi

1976-01-01

In the atomic absorption spectrophotometry of europium in air-acetylene flame, ammonium perchlorate (NH 4 ClO 4 ) increases the absorption of europium. In the case of 0.5 M NH 4 ClO 4 , the increase is by about 1.5 times. In this paper, a method for eliminating the interferences of many coexisting compounds using an enhancing effect and a method for determining Eu 2 O 3 in La 2 O 3 were investigated. The working conditions using Nippon Jarrell-Ash model AA-1 atomic absorption/flame emission spectrophotometer were as follows; wavelength 4594 A, lamp current 15 mA, burner height 10 mm, air flow-rate 6.51/min, acetylene flow-rate 1.81/min. Though the enhancing or depressing effects of HCl, HNO 3 , HBr and HClO 4 in concentrations below 0.1 M were eliminated by 0.5 M NH 4 ClO 4 , the remarkable depressing effects of H 2 SO 4 and H 3 PO 4 on europium could not be eliminated. The interferences of Na + , K + , Cs + and Al 3+ in the concentration of 200 ppm were not eliminated, but those of other cations including rare earth elements were completely eliminated. Lanthanum in the range of (2000--10000) ppm increased the absorption of europium by about 1.4 times. But the effect of lanthanum in the range of (0--9000) ppm was also eliminated by NH 4 ClO 4 . The calibration curve for europium in the presence of NH 4 ClO 4 was linear in the range of (0--400) ppm with a sensitivity larger by about 1.5 times than that for europium alone. The analytical procedure is as follows. A sample is dissolved in HCl and NH 4 ClO 4 is added. Europium in the sample solution is determined by atomic absorption method using air-acetylene flame. For practical samples, the values obtained were in fair agreement with those by the flame emission method using a nitrous oxide-acetylene flame. The coefficients of variation by the present method were (3.7--2.4)% (Eu 2 O 3 content (1--3)%). (auth.)

Determination of microquantities of cesium in leaching tests by atomic absorption spectrometry with electrothermal atomization

International Nuclear Information System (INIS)

Crubellati, R.O.; Di Santo, N.R.

1988-01-01

An original method for cesium determinations by atomic absorption spectrometry with electrothermal atomization is described. The effect of foreign ions (alkali and earth alkaline metals) present in leaching test of glasses with incorporated radioactive wastes was studied. The effect of different mineral acids was also investigated. A comparison between the flame excitation method and the electrothermal atomization one was made. Under optimum conditions, cesium in quantities down to 700 ng in 1000 ml of sample could be determined. The calibration curve was linear in the range of 0.7 - 15 ng/mL. The fact that the proposed determinations can be performed in a short time and that a small sample volume is required are fundamental advantages of this method, compared with the flame excitation procedure. Besides, it is adaptable to be applied in hot cells and glove boxes. (Author) [es

Analysis of Fuel Injection and Atomization of a Hybrid Air-Blast Atomizer.

Science.gov (United States)

Ma, Peter; Esclape, Lucas; Buschhagen, Timo; Naik, Sameer; Gore, Jay; Lucht, Robert; Ihme, Matthias

2015-11-01

Fuel injection and atomization are of direct importance to the design of injector systems in aviation gas turbine engines. Primary and secondary breakup processes have significant influence on the drop-size distribution, fuel deposition, and flame stabilization, thereby directly affecting fuel conversion, combustion stability, and emission formation. The lack of predictive modeling capabilities for the reliable characterization of primary and secondary breakup mechanisms is still one of the main issues in improving injector systems. In this study, an unstructured Volume-of-Fluid method was used in conjunction with a Lagrangian-spray framework to conduct high-fidelity simulations of the breakup and atomization processes in a realistic gas turbine hybrid air blast atomizer. Results for injection with JP-8 aviation fuel are presented and compared to available experimental data. Financial support through the FAA National Jet Fuel Combustion Program is gratefully acknowledged.

Single-laboratory evaluation of SW-846 Methods 7090/7091 determination of beryllium by flame and furnace atomic absorption spectrophotometry. Summary report January-August 1987

International Nuclear Information System (INIS)

Hodge, V.F.; Darby, D.A.; Thompson, W.E.; Jones, C.L.

1988-02-01

The results of a single-laboratory study of the Determination of Beryllium by Flame and Furnace Atomic Absorption Spectrophotometry, are described. The study examined the application of these two powerful beryllium detection methods to the analysis of selected liquid and solid samples after digestion by appropriate SW-846 methods. Method performance data including detection limits, optimum concentration ranges (linearity), spike recoveries, interferences, precision, accuracy, and optimum operating parameters are presented and discussed

Direct atomic absorption determination of silicon in metallic niobium

International Nuclear Information System (INIS)

Blinova, Eh.S.; Guzeev, I.D.; Nedler, V.V.; Khokhrin, V.M.

1984-01-01

Consideration is being given to realization of the basic advantage of non-flame atomizer-analysis of directly solid samples-for silicon determination in niobium for the content of the first one of less than 1x10 -3 mass %. Analysis technique is described. Diagrams of the dependences of atomic silicon absorption in graphite cells of usual type as well as lined by tungsten carbide and atomic silicon absorption on the value of niobium weighed amount are presented. It is shown that Si determination in metallic niobium according to aqueous reference solutions results in understatement of results 2.4 times. The optimal conditions for Si determination in niobium are the following: 2400 deg C temperature, absence of carbon and oxygen. Different niobium specimens with the known silicon content were used as reference samples

Radiation trapping in atomic absorption spectroscopy at lead determination in different matricies

International Nuclear Information System (INIS)

El-Gohary, Z.

2005-01-01

The determination of lead by flame atomic absorption analysis in the presence of Sn and Fe atoms and different matrices such as OH and SO 3 was investigated with the objective of understanding the spectral interference processes at the analytical lines 283.31 nm for a wide range of concentration. The radiation trapping factor was interpreted and evaluated assuming Voigt distribution of the atomic and rotational lines in the flame. The radiation trapping factor was increased by increasing the number density (plasma of the absorbing medium is optically thick). In plasma, there is a certain point of equilibrium between the trapping and the escaping of radiation, which is relevant to 50% of absorption. The spectral background interference can cause a variation of the number density at equilibrium point as a result of the degree of overlap with the analytical line. The spectral background interference can be easily avoided by using another resonance absorption line for the analysis. The chemical modification of the matrix is applied to minimize the interference effect. Nitric acid, ammonium nitrate and magnesium nitrate are most commonly recommended as matrix modifiers

The determination of vanadium in brines by atomic absorption spectroscopy

Science.gov (United States)

Crump-Wiesner, Hans J.; Feltz, H.R.; Purdy, W.C.

1971-01-01

A standard addition method is described for the determination of vanadium in brines by atomic absorption spectroscopy with a nitrous oxide-acetylene flame. Sample pH is adjusted to 1.0 with concentrated hydrochloric acid and the vanadium is directly extracted with 5% cupferron in methyl isobutyl ketone (MIBK). The ketone layer is then aspirated into the flame and the recorded absorption values are plotted as a function of the concentration of the added metal. As little as 2.5 ??g l-1 of vanadium can be detected under the conditions of the procedure. Tungsten and tin interfere when present in excess of 5 and 10 ??g ml-1, respectively. The concentrations of the two interfering ions normally found in brines are well below interference levels. ?? 1971.

The relation of double peaks, observed in quartz hydride atomizers, to the fate of free analyte atoms in the determination of arsenic and selenium by atomic absorption spectrometry

International Nuclear Information System (INIS)

D'Ulivo, Alessandro; Dedina, Jiri

2002-01-01

The mechanism at the origin of double peaks formation in quartz hydride atomizers were investigated by continuous flow hydride generation atomic absorption spectrometry. Arsenic and selenium were used as model analytes. The effect of atomization mode (flame-in-gas-shield (FIGS), miniature diffusion flame and double flame (DF)) and some experimental parameters as oxygen supply rate for microflame and the distance from atomization to free atoms detection point, were investigated on the shape of both analytical signals and calibration graphs. Rollover of calibration graphs and double peak formation are strictly related each to the other and could be observed only in FIGS atomizer mode under some particular conditions. A mechanism based on incomplete atomization of hydrides cannot explain the collected experimental evidences because the microflame of FIGS is able to produce quantitative atomization of large amount of hydrides even at supply rate of oxygen close to extinction threshold of microflame. The heterogeneous gas-solid reactions between finely dispersed particles, formed by free atom recombination, and the free atoms in the gaseous phase are at the origin of double peak formation

Membrane filtration of nickel(II) on cellulose acetate filters for its preconcentration, separation, and flame atomic absorption spectrometric determination

Energy Technology Data Exchange (ETDEWEB)

Soylak, Mustafa [Chemistry Dept., Faculty of Science Arts, University of Erciyes, Kayseri (Turkey); Unsal, Yunus Emre; Aydin, Ayse [Fen Bilimleri Enstitusu, University of Erciyes, Kayseri (Turkey); Kizil, Nebiye [Saglik Bilimleri Enstitusu, University of Erciyes, Kayseri (Turkey)

2010-01-15

An enrichment method for trace amounts of Ni(II), as 8-hydroxyquinoline chelates, has been established on a cellulose acetate membrane filter. Ni(II)-8-hydroxyquinoline chelates adsorbed on a membrane filter were eluted using 5 mL of 1 M HNO{sub 3}. The eluent nickel concentration was determined by a flame atomic absorption spectrometer. The influence of some analytical parameters, including pH, amount of reagent, sample volume, etc., on recovery was investigated. The interference of co-existent ions was studied. The nickel detection limit was 4.87 {mu}g/L. The method was applied to real samples for the determination of nickel(II) ions. (Abstract Copyright [2010], Wiley Periodicals, Inc.)

Determination of cadmium in aluminium by atomic absorption spectrometry

International Nuclear Information System (INIS)

Batistoni, D.A.; Erlijman, L.H.

1978-12-01

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) [es

Determination of 17 impurity elements in nuclear quality uranium compounds by atomic absorption spectroscopy

International Nuclear Information System (INIS)

Andonie, O.; Smith, L.A.; Cornejo, S.

1985-01-01

A method is described for the determination of 17 elements (Al, Ca, Cd, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Mo, Na, Ni, Pb, V and Zn) in the ppm level, in nuclearly pure uranium compounds by flame atomic absorption spectroscopy. The analysis is performed by first dissolving the uranium sample in nitric acid and then extracting the uranium with tributyl phosphate solution. The aqueous phase, free of uranium, which contains the elements to analyze is inspirated into the flame of an atomic absorption spectrophotometer using air-acetylene or nitrous oxide-acetylene flame according to the element in study. This method allows to extract the uranium selectively in more than 99.0% and the recovery of the elements sudied was larger 90% (for K) to 100% (for Cr). The sensitivity of the method vary from 0.096 μg/g U (for Cd) to 5.5 μg/g U (for Na). (Author)

Enhancement of the atomic absorbance of Cr, Zn, Cd, and Pb in metal furnace atomic absorption spectrometry using absorption tubes

Directory of Open Access Journals (Sweden)

Yuya Koike

2017-03-01

Full Text Available Trace amounts of Cr, Zn, Cd, and Pb were determined by metal furnace atomic absorption spectrometry using absorption tubes. Various absorption tubes were designed as roof- and tube-types, and fixed above the metal furnace in order to extend the light path length. Aqueous standards and samples were injected in the metal furnace and atomized in a metal atomizer with an absorption tube (6 cm length, 15.5 mm diameter. The used of an absorption tube resulted in an enhancement of the atomic absorbance. The ratios of absorbance values with and without the roof- and tube-type absorption tubes were 1.33 and 1.11 for Cr; 1.42 and 1.99 for Zn; 1.66 and 1.98 for Cd; and 1.31 and 1.16 for Pb, respectively. The use of an absorption tube was effective for Zn and Cd analysis, as the absorbance values for these low boiling point metals doubled. The proposed method was successfully applied in the determination of Zn in tap water.

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

International Nuclear Information System (INIS)

Smith, R.

1983-01-01

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

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

DEFF Research Database (Denmark)

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......, programmable from the microcomputer, to control the sample volume. No pre-treatment of the samples is necessary. The limit of detection is 0.14 mg l–1, and only small amounts of serum (

Speciation of iron (II) and (III) by using solvent extraction and flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Yaman, Mehmet; Kaya, Gokce

2005-01-01

A method for speciation, preconcentration and separation of Fe 2+ and Fe 3+ in different matrices was developed using solvent extraction and flame atomic absorption spectrometry. PAN as complexing reagent for Fe 2+ and chloroform as organic solvent were used. The complex of Fe 2+ -PAN was extracted into chloroform phase in the pH range of 0.75-4.0 and Fe 3+ remains in water phase in the pH range 0.75-1.25. The optimum conditions for maximum recovery of Fe 2+ and minimum recovery of Fe 3+ were determined as pH = 1, the stirring time of 20 min, the PAN amount of 0.5 mg and chloroform volume of 8 mL. The developed method was applied to the determination of Fe 2+ and Fe 3+ in tea infusion, fruit juice, cola and pekmez. It is seen that there is high bioavailable iron (Fe 2+ ) in pekmez. The developed method is sensitive, simple and need the shorter time in comparison with other similar studies

Element selective detection of molecular species applying chromatographic techniques and diode laser atomic absorption spectrometry.

Science.gov (United States)

Kunze, K; Zybin, A; Koch, J; Franzke, J; Miclea, M; Niemax, K

2004-12-01

Tunable diode laser atomic absorption spectroscopy (DLAAS) combined with separation techniques and atomization in plasmas and flames is presented as a powerful method for analysis of molecular species. The analytical figures of merit of the technique are demonstrated by the measurement of Cr(VI) and Mn compounds, as well as molecular species including halogen atoms, hydrogen, carbon and sulfur.

Flow Injection and Atomic Absorption Spectrometry (FI-AAS) -

DEFF Research Database (Denmark)

Hansen, Elo Harald

1996-01-01

One of the advantages of the flow injection (FI) concept is that it is compatible with virtually all detection techniques. Being a versatile vehicle for enhancing the performance of the individual detection devices, the most spectacular results have possibly been obtained in conjunction with atomic...... the point of sample injection/introduction to the point of detection. Hence, in FI-fAAS this feature allows not only to obtain improved repeatability but also improved accuracy, and because the wash to sample ratio is high it permits the handling of samples with elevated salt contents - which...

Combination of dispersive liquid-liquid microextraction with flame atomic absorption spectrometry using microsample introduction for determination of lead in water samples.

Science.gov (United States)

Naseri, Mohammad Taghi; Hemmatkhah, Payam; Hosseini, Mohammad Reza Milani; Assadi, Yaghoub

2008-03-03

The dispersive liquid-liquid microextraction (DLLME) was combined with the flame atomic absorption spectrometry (FAAS) for determination of lead in the water samples. Diethyldithiophosphoric acid (DDTP), carbon tetrachloride and methanol were used as chelating agent, extraction solvent and disperser solvent, respectively. A new FAAS sample introduction system was employed for the microvolume nebulization of the non-flammable chlorinated organic extracts. Injection of 20 microL volumes of the organic extract into an air-acetylene flame provided very sensitive spike-like and reproducible signals. Some effective parameters on the microextraction and the complex formation were selected and optimized. These parameters include extraction and disperser solvent type as well as their volume, extraction time, salt effect, pH and amount of the chelating agent. Under the optimized conditions, the enrichment factor of 450 was obtained from a sample volume of 25.0 mL. The enhancement factor, calculated as the ratio of the slopes of the calibration graphs with and without preconcentration, which was about 1000. The calibration graph was linear in the range of 1-70 microgL(-1) with a detection limit of 0.5 microgL(-1). The relative standard deviation (R.S.D.) for seven replicate measurements of 5.0 and 50 microgL(-1) of lead were 3.8 and 2.0%, respectively. The relative recoveries of lead in tap, well, river and seawater samples at the spiking level of 20 microgL(-1) ranged from 93.8 to 106.2%. The characteristics of the proposed method were compared with those of the liquid-liquid extraction (LLE), cloud point extraction (CPE), on-line and off-line solid-phase extraction (SPE) as well as co-precipitation, based on bibliographic data. Operation simplicity, rapidity, low cost, high enrichment factor, good repeatability, and low consumption of the extraction solvent at a microliter level are the main advantages of the proposed method.

Direct determination of Cu, Mn, Pb, and Zn in beer by thermospray flame furnace atomic absorption spectrometry

International Nuclear Information System (INIS)

Nascentes, Clesia C.; Kamogawa, Marcos Y.; Fernandes, Kelly G.; Arruda, Marco A.Z.; Nogueira, Ana Rita A.; Nobrega, Joaquim A.

2005-01-01

In this work, thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) was employed for Cu, Mn, Pb, and Zn determination in beer without any sample digestion. The system was optimized and calibration was based on the analyte addition technique. A sample volume of 300 μl was introduced into the hot Ni tube at a flow-rate of 0.4 ml min -1 using 0.14 mol l -1 nitric acid solution or air as carrier. Different Brazilian beers were directly analyzed after ultrasonic degasification. Results were compared with those obtained by graphite furnace atomic absorption spectrometry (GFAAS). The detection limits obtained for Cu, Mn, Pb, and Zn in aqueous solution were 2.2, 18, 1.6, and 0.9 μg l -1 , respectively. The relative standard deviations varied from 2.7% to 7.3% (n=8) for solutions containing the analytes in the 25-50 μg l -1 range. The concentration ranges obtained for analytes in beer samples were: Cu: 38.0-155 μg l -1 ; Mn: 110-348 μg l -1 , Pb: 13.0-32.9 μg l -1 , and Zn: 52.7-226 μg l -1 . Results obtained by TS-FF-AAS and GFAAS were in agreement at a 95% confidence level. The proposed method is fast and simple, since sample digestion is not required and sensitivity can be improved without using expensive devices. The TS-FF-AAS presented suitable sensitivity for determination of Cu, Mn, Pb, and Zn in the quality control of a brewery

Combined discrete nebulization and microextraction process for molybdenum determination by flame atomic absorption spectrometry (FAAS); Avaliacao da combinacao da nebulizacao discreta e processos de microextracao aplicados a determinacao de molibdenio por espectrometria de absorcao atomica com chama (FAAS)

Energy Technology Data Exchange (ETDEWEB)

Oviedo, Jenny A.; Jesus, Amanda M.D. de; Fialho, Lucimar L.; Pereira-Filho, Edenir R., E-mail: erpf@ufscar.br [Universidade Federal de Sao Carlos (UFSCar), SP (Brazil). Departamento de Quimica

2014-04-15

Simple and sensitive procedures for the extraction/preconcentration of molybdenum based on vortex-assisted solidified floating organic drop microextraction (VA-SFODME) and cloud point combined with flame absorption atomic spectrometry (FAAS) and discrete nebulization were developed. The influence of the discrete nebulization on the sensitivity of the molybdenum preconcentration processes was studied. An injection volume of 200 μ resulted in a lower relative standard deviation with both preconcentration procedures. Enrichment factors of 31 and 67 and limits of detection of 25 and 5 μ L{sup -1} were obtained for cloud point and VA-SFODME, respectively. The developed procedures were applied to the determination of Mo in mineral water and multivitamin samples. (author)

Application of dual-cloud point extraction for the trace levels of copper in serum of different viral hepatitis patients by flame atomic absorption spectrometry: A multivariate study

Science.gov (United States)

Arain, Salma Aslam; Kazi, Tasneem G.; Afridi, Hassan Imran; Abbasi, Abdul Rasool; Panhwar, Abdul Haleem; Naeemullah; Shanker, Bhawani; Arain, Mohammad Balal

2014-12-01

An efficient, innovative preconcentration method, dual-cloud point extraction (d-CPE) has been developed for the extraction and preconcentration of copper (Cu2+) in serum samples of different viral hepatitis patients prior to couple with flame atomic absorption spectrometry (FAAS). The d-CPE procedure was based on forming complexes of elemental ions with complexing reagent 1-(2-pyridylazo)-2-naphthol (PAN), and subsequent entrapping the complexes in nonionic surfactant (Triton X-114). Then the surfactant rich phase containing the metal complexes was treated with aqueous nitric acid solution, and metal ions were back extracted into the aqueous phase, as second cloud point extraction stage, and finally determined by flame atomic absorption spectrometry using conventional nebulization. The multivariate strategy was applied to estimate the optimum values of experimental variables for the recovery of Cu2+ using d-CPE. In optimum experimental conditions, the limit of detection and the enrichment factor were 0.046 μg L-1 and 78, respectively. The validity and accuracy of proposed method were checked by analysis of Cu2+ in certified sample of serum (CRM) by d-CPE and conventional CPE procedure on same CRM. The proposed method was successfully applied to the determination of Cu2+ in serum samples of different viral hepatitis patients and healthy controls.

Application of a field flow preconcentration system with a minicolumn packed with amberlite XAD-4/1-(2-pyridylazo)-2-naphtol and a flow injection-flame atomic adsorption spectrometric system for lead determination in sea water

International Nuclear Information System (INIS)

Carmen Yebra, M. del; Rodriguez, L.; Puig, L.; Moreno-Cid, A.

2002-01-01

A field flow preconcentration technique involving a minicolumn containing Amberlite XAD-4 impregnated with the complexing agent 1-(2-pyridylazo)-2-naphthol was used to preconcentrate lead from seawater. Elution of retained lead on the minicolumns was performed by a flow-injection-flame atomic absorption spectrometric system. Factorial designs have been used to optimize the field flow preconcentration system and the flow injection elution process. Factors such as sample pH, sample flow-rate, eluent concentration and volume (hydrochloric acid), elution flow-rate and minicolumn diameter were considered. The results suggest that the sample flow-rate and the eluent volume are statistically significant factors. The detection limit (3σ) of the procedure was 5 ng/L for a sample volume of 1000 ml. The precision (expressed as relative standard deviation) for eleven independent determinations reached values of 4.0-3.1 % in lead solutions of 50-200 ng/L. This procedure has been successfully applied to the determination of lead in seawater from Galicia (Spain). (author)

Gold volatile species atomization and preconcentration in quartz devices for atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Arslan, Yasin [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic); Mehmet Akif Ersoy University, Faculty of Arts & Sciences, Chemistry Department, 15030 Burdur (Turkey); Musil, Stanislav; Matoušek, Tomáš; Kratzer, Jan [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic); Dědina, Jiří, E-mail: dedina@biomed.cas.cz [Institute of Analytical Chemistry of the ASCR, v. v. i., Veveří 97, 602 00 Brno (Czech Republic)

2015-01-01

The on-line atomization of gold volatile species was studied and the results were compared with thermodynamic calculations in several quartz atomizers, namely: diffusion flame, flame-in-gas-shield, flame-in-plain-tube, externally heated T-tube and externally heated flame-in-T-tube. Atomization mechanism in the explored devices is proposed, where volatile species are converted to thermodynamically stable AuH at elevated temperature over 500 °C and then atomized by an interaction with a cloud of hydrogen radicals. Because of its inherent simplicity and robustness, diffusion flame was employed as a reference atomizer. It yielded atomization efficiency of 70 to 100% and a very good long time reproducibility of peak area sensitivity: 1.6 to 1.8 s μg{sup −1}. Six and eleven times higher sensitivity, respectively, was provided by atomizers with longer light paths in the observation volume, i.e. externally heated T-tube and externally heated flame-in-T-tube. The latter one, offering limit of detection below 0.01 μg ml{sup −1}, appeared as the most prospective for on-line atomization. Insight into the mechanism of atomization of gold volatile species, into the fate of free atoms and into subsequent analyte transfer allowed to assess possibilities of in-atomizer preconcentration of gold volatile species: it is unfeasible with quartz atomizers but a sapphire tube atomizer could be useful in this respect. - Highlights: • On-line atomization of gold volatile species for AAS in quartz devices was studied. • Atomization mechanism was proposed and atomization efficiency was estimated. • Possibilities of in-atomizer preconcentration of gold volatile species were assessed.

Bismuth as a general internal standard for lead in atomic absorption spectrometry

International Nuclear Information System (INIS)

Bechlin, Marcos A.; Fortunato, Felipe M.; Ferreira, Edilene C.; Neto, José A. Gomes; Nóbrega, Joaquim A.; Donati, George L.; Jones, Bradley T.

2014-01-01

Highlights: • Single internal standard is commonly proposed for definite application in AAS. • Internal standard for general use in AAS techniques is original. • Bi showed efficiency as internal standard for Pb determinations by FAAS and GFAAS. • Assorted samples were analyzed and accurate results were found. - Abstract: Bismuth was evaluated as internal standard for Pb determination by line source flame atomic absorption spectrometry (LS FAAS), high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS) and line source graphite furnace atomic absorption spectrometry (LS GFAAS). Analysis of samples containing different matrices indicated close relationship between Pb and Bi absorbances. Correlation coefficients of calibration curves built up by plotting A Pb /A Bi versus Pb concentration were higher than 0.9953 (FAAS) and higher than 0.9993 (GFAAS). Recoveries of Pb improved from 52–118% (without IS) to 97–109% (IS, LS FAAS); 74–231% (without IS) to 96–109% (IS, HR-CS FAAS); and 36–125% (without IS) to 96–110% (IS, LS GFAAS). The relative standard deviations (n = 12) were reduced from 0.6–9.2% (without IS) to 0.3–4.3% (IS, LS FAAS); 0.7–7.7% (without IS) to 0.1–4.0% (IS, HR-CS FAAS); and 2.1–13% (without IS) to 0.4–5.9% (IS, LS GFAAS)

Separation and enrichment of gold(III) from environmental samples prior to its flame atomic absorption spectrometric determination

International Nuclear Information System (INIS)

Senturk, Hasan Basri; Gundogdu, Ali; Bulut, Volkan Numan; Duran, Celal; Soylak, Mustafa; Elci, Latif; Tufekci, Mehmet

2007-01-01

A simple and accurate method was developed for separation and enrichment of trace levels of gold in environmental samples. The method is based on the adsorption of Au(III)-diethyldithiocarbamate complex on Amberlite XAD-2000 resin prior to the analysis of gold by flame atomic absorption spectrometry after elution with 1 mol L -1 HNO 3 in acetone. Some parameters including nitric acid concentration, eluent type, matrix ions, sample volume, sample flow rate and adsorption capacity were investigated on the recovery of gold(III). The recovery values for gold(III) and detection limit of gold were greater than 95% and 16.6 μg L -1 , respectively. The preconcentration factor was 200. The relative standard deviation of the method was -1 . The validation of the presented procedure was checked by the analysis of CRM-SA-C Sandy Soil certified reference material. The presented procedure was applied to the determination of gold in some environmental samples

Determination of total antimony and inorganic antimony species by hydride generation in situ trapping flame atomic absorption spectrometry: a new way to (ultra)trace speciation analysis

Energy Technology Data Exchange (ETDEWEB)

Henryk Matusiewicz; Magdalena Krawczyk

2008-07-01

The analytical performance of non-chromatographic coupled hydride generation, integrated atom trap (HG-IAT) atomizer flame absorption spectrometry (FAAS) systems were evaluated for the speciation analysis of antimony in environmental samples. Antimony, using formation of stibine (SbH{sub 3}) vapors were atomized in an air-acetylene flame-heated IAT. A new design of HG-IAT-FAAS hyphenated technique that would exceed the operational capabilities of existing arrangements was investigated. For the estimation of Sb(III) and Sb(V) concentrations in samples, the difference between the analytical sensitivities of the absorbance signals obtained for antimony hydride without and with previous treatment of samples with L-cysteine can be used. The concentration of Sb(V) was calculated by the difference between total Sb and Sb(III). A dramatic improvement in detection limit was achieved compared with that obtained using either of the atom trapping techniques, presented above, separately. This novel approach decreases the detection limit down to low pg mL{sup -1} levels. The concentration detection limit, defined as 3 times the blank standard deviation was 0.2 ng mL{sup -1}. For a 120 s in situ pre-concentration time , sensitivity enhancement compared to flame AAS, was 550 fold for Sb, using hydride generation-atom trapping technique. The accuracy of the method was verified by the use of certified reference materials (NIST SRM 2704 Buffalo River Sediment, SRM 2710 Montana Soil, SRM 1633a Coal Fly Ash, SRM 1575 Pine Needles, SRM 1643e Trace Elements in Water) and by aqueous standard calibration technique. The measured Sb content, in reference materials, were in satisfactory agreement with the certified values. The hyphenated technique was applied for antimony determinations in soil, sediment, coal fly ash, sewage and river water.

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

Science.gov (United States)

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

2013-01-01

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

Application of atomic absorption in molecular analysis (spectrophotometry)

International Nuclear Information System (INIS)

Baliza, S.V.; Soledade, L.E.B.

1981-01-01

The apparatus of atomic absorption has been considered by all the experts in chemical analysis as one of the most important equipments in actual utilization in such field. Among its several applications one should emphasize direct and indirect metals analyses using flame, graphite furnace, cold vapor generator,... Besides such known applications, the authors have developed at the R and D Center of CSN a patent pendent method for the utilization of such equipment for molecular analysis, in substitution of a sophisticated and specific apparatus. (Author) [pt

Rapid Determination of Trace Palladium in Active Pharmaceutical Ingredients by Magnetic Solid-Phase Extraction and Flame Atomic Absorption Spectrometry

Science.gov (United States)

Yin, Q. H.; Zhu, D. M.; Yang, D. Z.; Hu, Q. F.; Yang, Y. L.

2018-01-01

Clutaraldehyde cross-linked magnetic chitosan nanoparticles were synthesized and used as an adsorbent for the dispersive solid-phase extraction of palladium in active pharmaceutical ingredients (APIs) prior to analysis by a flame atomic absorption spectrophotometer. FT-IR, X-ray diffraction, and TEM were used to characterize the adsorbent. Various parameters of experimental performance, such as adsorbent amount, pH, adsorption time, desorption solutions, coexisting ions, and adsorbent reusability, were investigated and optimized. Under the optimized conditions, good linearity was achieved in the 5.0-500 μg/L concentration range, with correlation coefficients of 0.9989. The limit of detection is 2.8 μg/L and the recoveries of spiked samples ranged from 91.7 to 97.6%. It was confirmed that the GMCNs nanocomposite was a promising adsorbing material for extraction and preconcentration of Pd in APIs.

Simultaneous preconcentration of Cu, Fe and Pb as methylthymol blue complexes on naphthalene adsorbent and flame atomic absorption determination

International Nuclear Information System (INIS)

Pourreza, Nahid; Hoveizavi, Reza

2005-01-01

A simultaneous preconcentration method was developed for determination of trace amounts of Cu, Fe and Pb by atomic absorption spectrometry. The method is based on the retention of their methylthymol blue complexes by naphthalene methyltrioctyl ammonium chloride adsorbent in a column. The adsorbed metal complexes were eluted from the column with nitric acid and Cu, Fe and Pb were determined by flame atomic absorption spectrometry. Several parameters such as pH of the sample solution, ligand concentration, volume of the sample and the amount of methyltrioctyl ammonium chloride loaded on naphthalene were evaluated. The effect of diverse ions on the preconcentration was also investigated. A preconcentration factor of up to 100 or more can easily be achieved depending on the volume of the sample taken. The calibration graphs were obtained in the range of 5-40, 10-100 and 10-200 ng ml -1 for Cu, Fe and Pb in the initial solution, respectively, when using 500 ml of the solution. The detection limit based on three standard deviations of the blank was 0.54, 3.1, and 4.5 ng ml -1 for Cu, Fe and Pb, respectively. The relative standard deviations (R.S.D.) of 0.62-1.4% for Cu, 1.9-3.4% for Fe and 1.0-2.2% for Pb were obtained. The method was applied to the determination of Cu, Fe and Pb in river and wastewater samples

Application of dual-cloud point extraction for the trace levels of copper in serum of different viral hepatitis patients by flame atomic absorption spectrometry: a multivariate study.

Science.gov (United States)

Arain, Salma Aslam; Kazi, Tasneem G; Afridi, Hassan Imran; Abbasi, Abdul Rasool; Panhwar, Abdul Haleem; Naeemullah; Shanker, Bhawani; Arain, Mohammad Balal

2014-12-10

An efficient, innovative preconcentration method, dual-cloud point extraction (d-CPE) has been developed for the extraction and preconcentration of copper (Cu(2+)) in serum samples of different viral hepatitis patients prior to couple with flame atomic absorption spectrometry (FAAS). The d-CPE procedure was based on forming complexes of elemental ions with complexing reagent 1-(2-pyridylazo)-2-naphthol (PAN), and subsequent entrapping the complexes in nonionic surfactant (Triton X-114). Then the surfactant rich phase containing the metal complexes was treated with aqueous nitric acid solution, and metal ions were back extracted into the aqueous phase, as second cloud point extraction stage, and finally determined by flame atomic absorption spectrometry using conventional nebulization. The multivariate strategy was applied to estimate the optimum values of experimental variables for the recovery of Cu(2+) using d-CPE. In optimum experimental conditions, the limit of detection and the enrichment factor were 0.046μgL(-1) and 78, respectively. The validity and accuracy of proposed method were checked by analysis of Cu(2+) in certified sample of serum (CRM) by d-CPE and conventional CPE procedure on same CRM. The proposed method was successfully applied to the determination of Cu(2+) in serum samples of different viral hepatitis patients and healthy controls. Copyright © 2014 Elsevier B.V. All rights reserved.

Separation of seven arsenic compounds by high performance liquid chromatography with on-line detection by hydrogen-argon flame atomic absorption spectrometry and inductively coupled plasma mass spectrometry

DEFF Research Database (Denmark)

Hansen, S. H.; Larsen, Erik Huusfeldt; Pritzl, G.

1992-01-01

-to-noise ratio of the on-line AAS detector was optimized. This involved the use of the hydrogen-argon-entrained air flame, a slotted tube atom trap in the flame for signal enhancement, electronic noise damping and a high-intensity light source. The detection limits in mu-g cm-3, using 100 mm3 injections...... of mixtures of arsenic standards into the HPLC system were: arsenite, As(III) 1.1; arsenate, As(V) 1.4; MMA 1.4; DMA 0.7; AsB 0.3; AsC 0.5; and the TMAs 0.4. The HPLC-AAS system was used for the analysis of arsenic species in aqueous extracts of soil samples from a polluted land site. Only arsenate was found...

Determination of mercury by multisyringe flow injection system with cold-vapor atomic absorption spectrometry

International Nuclear Information System (INIS)

Leal, L.O.; Elsholz, O.; Forteza, R.; Cerda, V.

2006-01-01

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% SnCl 2 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

Atomization of volatile compounds for atomic absorption and atomic fluorescence spectrometry: On the way towards the ideal atomizer

International Nuclear Information System (INIS)

Dedina, Jiri

2007-01-01

This review summarizes and discusses the individual atomizers of volatile compounds. A set of criteria important for analytical praxis is used to rank all the currently existing approaches to the atomization based on on-line atomization for atomic absorption (AAS) and atomic fluorescence spectrometry (AFS) as well as on in-atomizer trapping for AAS. Regarding on-line atomization for AAS, conventional quartz tubes are currently the most commonly used devices. They provide high sensitivity and low baseline noise. Running and investment costs are low. The most serious disadvantage is the poor resistance against atomization interferences and often unsatisfactory linearity of calibration graphs. Miniature diffusion flame (MDF) is extremely resistant to interferences, simple, cheap and user-friendly. Its essential disadvantage is low sensitivity. A novel device, known as a multiatomizer, was designed to overcome disadvantages of previous atomizers. It matches performance of conventional quartz tubes in terms of sensitivity and baseline noise as well as in running and investment costs. The multiatomizer, however, provides much better (i) resistance against atomization interferences and (ii) linearity of calibration graphs. In-atomizer trapping enhances the sensitivity of the determination and eliminates the effect of the generation kinetics and of surges in gas flow on the signal shape. This is beneficial for the accuracy of the determination. It could also be an effective tool for reducing some interferences in the liquid phase. In-situ trapping in graphite furnaces (GF) is presently by far the most popular approach to the in-atomizer trapping. Its resistance against interferences is reasonably good and it can be easily automated. In-situ trapping in GF is a mature method well established in various application fields. These are the reasons to rank in-situ trapping in GF as currently the most convenient approach to hydride atomization for AAS. The recently suggested

Separation and enrichment of gold(III) from environmental samples prior to its flame atomic absorption spectrometric determination

Energy Technology Data Exchange (ETDEWEB)

Senturk, Hasan Basri; Gundogdu, Ali [Department of Chemistry, Faculty of Arts and Sciences, Karadeniz Technical University, 61080 Trabzon (Turkey); Bulut, Volkan Numan [Department of Chemistry, Faculty of Arts and Sciences, Karadeniz Technical University, 28049 Giresun (Turkey); Duran, Celal [Department of Chemistry, Faculty of Arts and Sciences, Karadeniz Technical University, 61080 Trabzon (Turkey); Soylak, Mustafa [Department of Chemistry, Faculty of Arts and Sciences, Erciyes University, 38039 Kayseri (Turkey)], E-mail: soylak@erciyes.edu.tr; Elci, Latif [Department of Chemistry, Faculty of Arts and Sciences, Pamukkale University, 20020 Denizli (Turkey); Tufekci, Mehmet [Department of Chemistry, Faculty of Arts and Sciences, Karadeniz Technical University, 61080 Trabzon (Turkey)

2007-10-22

A simple and accurate method was developed for separation and enrichment of trace levels of gold in environmental samples. The method is based on the adsorption of Au(III)-diethyldithiocarbamate complex on Amberlite XAD-2000 resin prior to the analysis of gold by flame atomic absorption spectrometry after elution with 1 mol L{sup -1} HNO{sub 3} in acetone. Some parameters including nitric acid concentration, eluent type, matrix ions, sample volume, sample flow rate and adsorption capacity were investigated on the recovery of gold(III). The recovery values for gold(III) and detection limit of gold were greater than 95% and 16.6 {mu}g L{sup -1}, respectively. The preconcentration factor was 200. The relative standard deviation of the method was <6%. The adsorption capacity of the resin was 12.3 mg g{sup -1}. The validation of the presented procedure was checked by the analysis of CRM-SA-C Sandy Soil certified reference material. The presented procedure was applied to the determination of gold in some environmental samples.

Sensitive determination of cadmium using solidified floating organic drop microextraction-slotted quartz tube-flame atomic absorption spectroscopy.

Science.gov (United States)

Akkaya, Erhan; Chormey, Dotse Selali; Bakırdere, Sezgin

2017-09-20

In this study, solidified floating organic drop microextraction (SFODME) by 1-undecanol was combined with slotted quartz tube flame atomic absorption spectrometry (SQT-FAAS) for the determination of cadmium at trace levels. Formation of a complex with 4,4'-dimethyl-2,2'-bipyridine facilitated the extraction of cadmium from aqueous solutions. Several chemical variables were optimized in order to obtain high extraction outputs. Parameters such as concentration of the ligand, pH, and amount of buffer solution were optimized to enhance the formation of cadmium complex. The SFODME method was assisted by dispersion of extractor solvent into aqueous solutions using 2-propanol. Under the optimum extraction and instrumental conditions, the limit of detection and limit of quantitation values obtained for cadmium using the combined methods (SFODME-SQT-FAAS) were found to be 0.4 and 1.3 μg L -1 , respectively. Matrix effects on the method were also examined for tap water and wastewater, and spiked recovery results were found to be very satisfactory. Graphical Abstract SFODME-SQT-FAAS system for sensitive determination of cadmium.

Combination of dispersive liquid-liquid microextraction with flame atomic absorption spectrometry using microsample introduction for determination of lead in water samples

International Nuclear Information System (INIS)

Naseri, Mohammad Taghi; Hemmatkhah, Payam; Hosseini, Mohammad Reza Milani; Assadi, Yaghoub

2008-01-01

The dispersive liquid-liquid microextraction (DLLME) was combined with the flame atomic absorption spectrometry (FAAS) for determination of lead in the water samples. Diethyldithiophosphoric acid (DDTP), carbon tetrachloride and methanol were used as chelating agent, extraction solvent and disperser solvent, respectively. A new FAAS sample introduction system was employed for the microvolume nebulization of the non-flammable chlorinated organic extracts. Injection of 20 μL volumes of the organic extract into an air-acetylene flame provided very sensitive spike-like and reproducible signals. Some effective parameters on the microextraction and the complex formation were selected and optimized. These parameters include extraction and disperser solvent type as well as their volume, extraction time, salt effect, pH and amount of the chelating agent. Under the optimized conditions, the enrichment factor of 450 was obtained from a sample volume of 25.0 mL. The enhancement factor, calculated as the ratio of the slopes of the calibration graphs with and without preconcentration, which was about 1000. The calibration graph was linear in the range of 1-70 μg L -1 with a detection limit of 0.5 μg L -1 . The relative standard deviation (R.S.D.) for seven replicate measurements of 5.0 and 50 μg L -1 of lead were 3.8 and 2.0%, respectively. The relative recoveries of lead in tap, well, river and seawater samples at the spiking level of 20 μg L -1 ranged from 93.8 to 106.2%. The characteristics of the proposed method were compared with those of the liquid-liquid extraction (LLE), cloud point extraction (CPE), on-line and off-line solid-phase extraction (SPE) as well as co-precipitation, based on bibliographic data. Operation simplicity, rapidity, low cost, high enrichment factor, good repeatability, and low consumption of the extraction solvent at a microliter level are the main advantages of the proposed method

Determination of calcium and magnesium in hydroethanolic extracts of propolis by atomic absorption flame spectrophotometry

Directory of Open Access Journals (Sweden)

E. Q. SANTANA

2009-01-01

Full Text Available

Propolis is a natural product collected by honeybees and has a large range of pharmacological activity, including antimicrobial, antitumoral, antioxidant and anti-inflammatory. Its use as a popular medicine is increasing all over the world, creating a need for quality control of the commercial products. In this study the levels of calcium and magnesium in commercial hydroalcoholic propolis extracts from varios states of Brazil were determined by atomic absorption flame spectrophotometry and different values were obtained for northern and southern states. This study can be extended to the analysis of metals that are harmful to health. The results showed that the calibration curves were linear over a wide concentration range (0.5-4.0 µg.mL^-1 for calcium and 0.05-0.4 µg.mL^-1 for magnesium with good correlation coefficients (0.999 and 0.988, respectively. Good analytical recovery (94% was obtained. The proposed method showed adequate precision and relative standard deviation lower than 2 %. The method is accurate and precise as well as having advantages such as simplicity and speed. Keywords: hydroalcoholic propolis extract; mineralization; analysis; calcium; magnesium.

Evaluation of cadmium, lead, copper, iron and zinc in Turkish dietary vegetable oils and olives using electrothermal and flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Acar, O.

2012-01-01

The Cd, Pb, Cu, Fe and Zn contents of some edible vegetable oils (soybean, sunflower, flower, nut, corn and olive) and of olives (olive-1, black, green, black crushed with seeds and green crushed with seeds) were determined and evaluated by an electrothermal atomic absorption spectrometer (ETAAS) using an Sc + Ir + NH 4 H 2 PO 4 chemical modifier mixture and flame atomic absorption spectrometer (FAAS) after microwave digestion. The pyrolysis and atomization temperatures of Cd, Pb and Cu in sample solutions with and without the modifier mixture were investigated. The limits of detection (LOD) for analytes found are 0.1, 0.6, 0.9, 15.0 and 12.0 μg L - 1 for Cd, Cu, Pb, Fe and Zn, respectively. The accuracy of the procedure proposed was confirmed by analyzing bovine liver 1577b standard reference material (SRM) and a spiked sample solution. The results of the analytes found were compared with certified and added values. The relative standard deviations of the analytes found were lower than 7% and the percent of recoveries obtained ranges from 96 to 101%. The Sc + Ir + NH 4 H 2 PO 4 mixture proposed was applied for the determination of Cd, Pb and Cu in oils and olives. The results of analytes found in the samples were compared with international and national food quality guidelines as well as with literature values. (Author) 48 refs.

Evaluation of cadmium, lead, copper, iron and zinc in Turkish dietary vegetable oils and olives using electrothermal and flame atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Acar, O.

2012-07-01

The Cd, Pb, Cu, Fe and Zn contents of some edible vegetable oils (soybean, sunflower, flower, nut, corn and olive) and of olives (olive-1, black, green, black crushed with seeds and green crushed with seeds) were determined and evaluated by an electrothermal atomic absorption spectrometer (ETAAS) using an Sc + Ir + NH{sub 4}H{sub 2}PO{sub 4} chemical modifier mixture and flame atomic absorption spectrometer (FAAS) after microwave digestion. The pyrolysis and atomization temperatures of Cd, Pb and Cu in sample solutions with and without the modifier mixture were investigated. The limits of detection (LOD) for analytes found are 0.1, 0.6, 0.9, 15.0 and 12.0 {mu}g L{sup -}1 for Cd, Cu, Pb, Fe and Zn, respectively. The accuracy of the procedure proposed was confirmed by analyzing bovine liver 1577b standard reference material (SRM) and a spiked sample solution. The results of the analytes found were compared with certified and added values. The relative standard deviations of the analytes found were lower than 7% and the percent of recoveries obtained ranges from 96 to 101%. The Sc + Ir + NH{sub 4}H{sub 2}PO{sub 4} mixture proposed was applied for the determination of Cd, Pb and Cu in oils and olives. The results of analytes found in the samples were compared with international and national food quality guidelines as well as with literature values. (Author) 48 refs.

Determination of lead associated with airborne particulate matter by flame atomic absorption and wave-length dispersive x-ray fluorescence spectrometry

International Nuclear Information System (INIS)

Talebi, S.M.

1997-01-01

The lead content of airborne particulate matter was determined by flame atomic absorption spectrometry (FAAS) following digestion with a mixture of nitric acid and hydrogen peroxide and also by wave-length dispersive x-ray fluorescence (WDXRF). The extraction procedure was checked by analyzing a standard reference material of airborne particulate matter (NIST, SRM -1648). It was concluded that lead can quantitatively (98%) be extracted from airborne particulate matter by the leaching process. A five-stage sequential extraction was performed to assess the potential mobility of lead associated with airborne particulate matter. Comparison of the airborne particulate lead measured by WDXRF to that measured by FAAS showed good agreement. The WDXRF method requires no time-consuming sample preparation or use of environmentally unfriendly solvents. The technique is suggested for direct determination of lead in airborne particulate matter in air pollution studies. (author)

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

Directory of Open Access Journals (Sweden)

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.

On-line preconcentration using a resin functionalized with 3,4-dihydroxybenzoic acid for the determination of trace elements in biological samples by thermospray flame furnace atomic absorption spectrometry

International Nuclear Information System (INIS)

Lemos, Valfredo A.; Bezerra, Marcos A.; Amorim, Fabio A.C.

2008-01-01

In the present paper, an on-line preconcentration procedure for determination of cadmium, copper and zinc by thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) is proposed. Amberlite XAD-4 functionalized with 3,4-dihydroxybenzoic acid (XAD4-DHB) packed in a minicolumn was used as sorbent material. The metals were retained on the XAD-DHB resin, from which it could be eluted directly to the thermospray flame furnace system. The detection limits were 28 (Cd), 100 (Cu) and 77 ng L -1 (Zn) for 60 s preconcentration time, at a sample flow rate of 7.0 mL min -1 . Enrichment factors were 102, 91 and 62, for cadmium, copper and zinc, respectively. The procedure has been applied successfully to metal determination in biological standard reference materials

Estimation of perimortal percent carboxy-heme in nonstandard postmortem specimens using analysis of carbon monoxide by GC/MS and iron by flame atomic absorption spectrophotometry.

Science.gov (United States)

Middleberg, R A; Easterling, D E; Zelonis, S F; Rieders, F; Rieders, M F

1993-01-01

In decomposed, formalin-fixed, embalmed, exhumed, and some fire-dried cases in which normal blood is unavailable, the usual methods for determination of carboxyhemoglobin saturation frequently fail. To address these specimens, a method utilizing both gas chromatography/mass spectrometric (GC/MS) determination of carbon monoxide (CO) and flame atomic absorption spectrophotometry (FAAS) determination of iron (Fe), in the same specimen, was developed. The method is reported here, along with its application to seven pertinent forsensic death investigations. The CO analytical methodology involves acid liberation of the gas from the specimen aliquot in a headspace vial. After heating and equilibrating, a sample of the headspace vapor is injected into the GC/MS system with a gastight syringe. Quantitation is achieved by standard addition comparison utilizing the ideal gas law equation. Iron is quantified by FAAS analysis of the same aliquot used for the CO determination, following nitric acid digestion. The concentration is determined by comparison to a standard curve. A formula for determining the minimum percent carboxy-heme saturation was derived by using the ratio of the amount of CO to the amount of Fe in the aliquot analyzed. Tissue types analyzed include spleen, liver, muscle, dried blood, and unspecified decomposed tissue.

On-line micro-volume introduction system developed for lower density than water extraction solvent and dispersive liquid–liquid microextraction coupled with flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Anthemidis, Aristidis N.; Mitani, Constantina; Balkatzopoulou, Paschalia; Tzanavaras, Paraskevas D.

2012-01-01

Highlights: ► A dispersive liquid–liquid micro extraction method for lead and copper determination. ► A micro-volume transportation system for extractant solvent lighter than water. ► Analysis of natural water samples. - Abstract: A simple and fast preconcentration/separation dispersive liquid–liquid micro extraction (DLLME) method for metal determination based on the use of extraction solvent with lower density than water has been developed. For this purpose a novel micro-volume introduction system was developed enabling the on-line injection of the organic solvent into flame atomic absorption spectrometry (FAAS). The effectiveness and efficiency of the proposed system were demonstrated for lead and copper preconcentration in environmental water samples using di-isobutyl ketone (DBIK) as extraction solvent. Under the optimum conditions the enhancement factor for lead and copper was 187 and 310 respectively. For a sample volume of 10 mL, the detection limit (3 s) and the relative standard deviation were 1.2 μg L −1 and 3.3% for lead and 0.12 μg L −1 and 2.9% for copper respectively. The developed method was evaluated by analyzing certified reference material and it was applied successfully to the analysis of environmental water samples.

Simultaneous preconcentration of cadmium and lead in water samples with silica gel and determination by flame atomic absorption spectrometry.

Science.gov (United States)

Xu, Hongbo; Wu, Yun; Wang, Jian; Shang, Xuewei; Jiang, Xiaojun

2013-12-01

A new method that utilizes pretreated silica gel as an adsorbent has been developed for simultaneous preconcentration of trace Cd(II) and Pb(II) prior to the measurement by flame atomic absorption spectrometry. The effects of pH, the shaking time, the elution condition and the coexisting ions on the separation/preconcentration conditions of analytes were investigated. Under optimized conditions, the static adsorption capacity of Cd(II) and Pb(II) were 45.5 and 27.1mg/g, the relative standard deviations were 3.2% and 1.7% (for n = 11), and the limits of detection obtained were 4.25 and 0.60 ng/mL, respectively. The method was validated by analyzing the certified reference materials GBW 07304a (stream sediment) and successfully applied to the analysis of various treated wastewater samples with satisfactory results. Copyright © 2013 The Research Centre for Eco-Environmental Sciences, Chinese Academy of Sciences. Published by Elsevier B.V. All rights reserved.

Solid phase extraction method for the determination of lead, nickel, copper and manganese by flame atomic absorption spectrometry using sodium bispiperdine-1,1'-carbotetrathioate (Na-BPCTT) in water samples

International Nuclear Information System (INIS)

Rekha, D.; Suvardhan, K.; Kumar, J. Dilip; Subramanyam, P.; Prasad, P. Reddy; Lingappa, Y.; Chiranjeevi, P.

2007-01-01

A novel column solid phase extraction procedure was developed for the determination of lead, nickel, copper and manganese in various water samples by flame atomic absorption spectrometry (FAAS) after preconcentration on sodium bispiperdine-1,1'-carbotetrathioate (Na-BPCTT) supported by Amberlite XAD-7. The sorbed element was subsequently eluted with 1 M nitric acid and the acid eluates are analysed by Flame atomic absorption spectrometry (FAAS). Various parameters such as pH, amount of adsorbent, eluent type and volume, flow-rate of the sample solution, volume of the sample solution and matrix interference effect on the retention of the metal ions have been studied. The optimum pH for the sorption of above mentioned metal ions was about 6.0 ± 0.2. The loading capacity of adsorbent for Pb, Cu, Ni and Mn were found to 28, 26, 22 and 20 x 10 -6 g/mL, respectively. The recoveries of lead, copper, nickel and manganese under optimum conditions were found to be 96.7-99.2 at the 95% confident level. The limit of detection was 3.0, 3.2, 2.8 and 3.6 x 10 -6 g/mL for lead, copper, nickel and manganese, respectively by applying a preconcentration factor 50. The proposed enrichment method was applied for metal ions in various water samples. The results were obtained are good agreement with reported method

Absorption spectrum of a two-level atom in a bad cavity with injected squeezed vacuum

Science.gov (United States)

Zhou, Peng; Swain, S.

1996-02-01

We study the absorption spectrum of a coherently driven two-level atom interacting with a resonant cavity mode which is coupled to a broadband squeezed vacuum through its input-output mirror in the bad cavity limit. We study the modification of the two-photon correlation strength of the injected squeezed vacuum inside the cavity, and show that the equations describing probe absorption in the cavity environment are formally identical to these in free space, but with modified parameters describing the squeezed vacuum. The two photon correlations induced by the squeezed vacuum are always weaker than in free space. We pay particular attention to the spectral behaviour at line centre in the region of intermediate trength driving intensities, where anomalous spectral features such as hole-burning and dispersive profiles are displayed. These unusual spectral features are very sensitive to the squeezing phase and the Rabi frequency of the driving field. We also derive the threshold value of the Rabi frequency which gives rise to the transparency of the probe beam at the driving frequency. When the Rabi frequency is less than the threshold value, the probe beam is absorbed, whilst the probe beam is amplified (without population inversion under certain conditions) when the Rabi frequency is larger than this threshold. The anomalous spectral features all take place in the vicinity of the critical point dividing the different dynamical regimes, probe absorption and amplification, of the atomic radiation. The physical origin of the strong amplification without population inversion, and the feasibility of observing it, are discussed.

Organic solvents as interferents in arsenic determination by hydride generation atomic absorption spectrometry with flame atomization

Czech Academy of Sciences Publication Activity Database

Karadjova, I.B.; Lampugnani, L.; Dědina, Jiří; D'Ulivo, A.; Onor, M.; Tsalev, D.L.

2006-01-01

Roč. 61, č. 5 (2006), s. 525-531 ISSN 0584-8547 R&D Projects: GA AV ČR IAA400310507 Institutional research plan: CEZ:AV0Z40310501 Keywords : hydride generation * atomic absorption spectrometry * interferences Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.092, year: 2006

Absorption and scattering of laser radiation by the diffusion flame of aviation kerosene

Energy Technology Data Exchange (ETDEWEB)

Gvozdev, S V; Glova, A F; Dubrovskii, V Yu; Durmanov, S T; Krasyukov, A G; Lysikov, A Yu; Smirnov, G V; Solomakhin, V B

2012-04-30

The absorption coefficient of the radiation of a repetitively pulsed Nd : YAG laser with an average output power up to 6 W and of a cw ytterbium optical fibre laser with an output power up to 3 kW was measured in the diffusion flame of aviation kerosene burning on a free surface in the atmospheric air. The absorption coefficient as a function of flame length, radiation power, and radiation intensity, which was varied in the {approx}10{sup 3} - 5 Multiplication-Sign 10{sup 4} W cm{sup -2} range, was obtained for two distances (1 and 2 cm) between the laser beam axis and the surface. The coefficient of radiation absorption by kerosene flame was compared with that in ethanol and kerosene - ethanol mixture flames. The radiation power scattered by a small segment of the kerosene flame irradiated by Nd : YAG laser radiation was measured as a function of longitudinal and azimuthal coordinates. An estimate was made of the total scattered radiation power.

Absorption and scattering of laser radiation by the diffusion flame of aviation kerosene

International Nuclear Information System (INIS)

Gvozdev, S V; Glova, A F; Dubrovskii, V Yu; Durmanov, S T; Krasyukov, A G; Lysikov, A Yu; Smirnov, G V; Solomakhin, V B

2012-01-01

The absorption coefficient of the radiation of a repetitively pulsed Nd : YAG laser with an average output power up to 6 W and of a cw ytterbium optical fibre laser with an output power up to 3 kW was measured in the diffusion flame of aviation kerosene burning on a free surface in the atmospheric air. The absorption coefficient as a function of flame length, radiation power, and radiation intensity, which was varied in the ∼10 3 - 5×10 4 W cm -2 range, was obtained for two distances (1 and 2 cm) between the laser beam axis and the surface. The coefficient of radiation absorption by kerosene flame was compared with that in ethanol and kerosene - ethanol mixture flames. The radiation power scattered by a small segment of the kerosene flame irradiated by Nd : YAG laser radiation was measured as a function of longitudinal and azimuthal coordinates. An estimate was made of the total scattered radiation power.

Absorption and scattering of laser radiation by the diffusion flame of aviation kerosene

Science.gov (United States)

Gvozdev, S. V.; Glova, A. F.; Dubrovskii, V. Yu; Durmanov, S. T.; Krasyukov, A. G.; Lysikov, A. Yu; Smirnov, G. V.; Solomakhin, V. B.

2012-04-01

The absorption coefficient of the radiation of a repetitively pulsed Nd : YAG laser with an average output power up to 6 W and of a cw ytterbium optical fibre laser with an output power up to 3 kW was measured in the diffusion flame of aviation kerosene burning on a free surface in the atmospheric air. The absorption coefficient as a function of flame length, radiation power, and radiation intensity, which was varied in the ~103 — 5×104 W cm-2 range, was obtained for two distances (1 and 2 cm) between the laser beam axis and the surface. The coefficient of radiation absorption by kerosene flame was compared with that in ethanol and kerosene — ethanol mixture flames. The radiation power scattered by a small segment of the kerosene flame irradiated by Nd : YAG laser radiation was measured as a function of longitudinal and azimuthal coordinates. An estimate was made of the total scattered radiation power.

Solvent microextraction-flame atomic absorption spectrometry (SME-FAAS) for determination of ultratrace amounts of cadmium in meat and fish samples.

Science.gov (United States)

Goudarzi, Nasser

2009-02-11

A simple, low cost and highly sensitive method based on solvent microextraction (SME) for separation/preconcentration and flame atomic absorption spectrometry (FAAS) was proposed for the determination of ultratrace amounts of cadmium in meat and fish samples. The analytical procedure involved the formation of a hydrophobic complex by mixing the analyte solution with an ammonium pyrrolidinedithiocarbamate (APDC) solution. In suitable conditions, the complex of cadmium-APDC entered the micro organic phase, and thus, separation of the analyte from the matrix was achieved. Under optimal chemical and instrumental conditions, a detection limit (3 sigma) of 0.8 ng L(-1) and an enrichment factor of 93 were achieved. The relative standard deviation for the method was found to be 2.2% for Cd. The interference effects of some anions and cations were also investigated. The developed method has been applied to the determination of trace Cd in meat and fish samples.

An indirect method for determining phosphorus in aluminium alloys by atomic-absorption spectrometry.

Science.gov (United States)

Bernal, J L; Del Nozal, M A; Deban, L; Aller, A J

1981-07-01

An indirect method is described for the determination of phosphorus in aluminium alloys. Ammonium molybdate is added to a solution of the aluminium alloy and the molybdophosphoric acid formed is selectively extracted into n-butyl acetate. The twelve molybdenum atoms associated with each phosphate ion are determined by direct atomic-absorption spectrometry with the n-butyl acetate phase in a nitrous oxide-acetylene flame, with measurement at 313.2 nm. The most suitable conditions have been established and the effect of other ions has been studied.

[Determination of metals in waste bag filter of steel works by microwave digestion-flame atomic absorption spectrometry].

Science.gov (United States)

Ning, Xun-An; Zhou, Yun; Liu, Jing-Yong; Wang, Jiang-Hui; Li, Lei; Ma, Xiao-Guo

2011-09-01

A method of microwave digestion technique-flame atomic absorption spectrometry was proposed to determine the total contents of Cu, Zn, Pb, Cd, Cr and Ni in five different kinds of waste bag filters from a steel plant. The digestion effects of the six acid systems on the heavy metals digestion were studied for the first time. The relative standard deviation (RSD) of the method was between 1.02% and 9.35%, and the recovery rates obtained by standard addition method ranged from 87.7% to 105.6%. The results indicated that the proposed method exhibited the advantages of simplicity, speediness, accuracy and repeatability, and it was suitable for determining the metal elements of the waste bag filter. The results also showed that different digestion systems should be used according to different waste bag filters. The waste bag filter samples from different production processes had different metal elements content. The Pb and Zn were the highest in the waste bag filters, while the Cu, Ni, Cd and Cr were relatively lower. These determination results provided the scientific data for further treatment and disposal of the waste bag filter.

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

International Nuclear Information System (INIS)

Naeemullah, A.; Kazi, T.G.

2011-01-01

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)

Influences of the matrix effect in the sensibility of cobalt measurement by atomic absorption

International Nuclear Information System (INIS)

Avila, L.A. d'.

1977-06-01

The interferences caused by iron, aluminium, calcium, magnesium, manganese, copper, nickel, zinc, sodium and potassium in the determination of cobalt by atomic absorption, were studied. The concentrations of cobalt were varied in the range of 1 to 800 μg/ml and the concentrations of the interferents in the proportions occuring normally in soils, rocks, sediments, geological material in general, alloys, caustic liquors etc. To study the flame composition effect, the flame region effect and also the effect of different interferent concentrations on the cobalt for each selected spectral line, an air-acetilene flame was utilized. As an application of this study the effect was shown of 'simulated soil matrices' with respect to the interference of iron on cobalt [pt

Feasibility of high-resolution continuum source molecular absorption spectrometry in flame and furnace for sulphur determination in petroleum products

Science.gov (United States)

Kowalewska, Zofia

2011-07-01

For the first time, high-resolution molecular absorption spectrometry with a high-intensity xenon lamp as radiation source has been applied for the determination of sulphur in crude oil and petroleum products. The samples were analysed as xylene solutions using vaporisation in acetylene-air flame or in an electrothermally heated graphite furnace. The sensitive rotational lines of the CS molecule, belonging to the ∆ν = 0 vibrational sequence within the electronic transition X 1∑ + → A 1П, were applied. For graphite furnace molecular absorption spectrometry, the Pd + Mg organic modifier was selected. Strong interactions with Pd atoms enable easier decomposition of sulphur-containing compounds, likely through the temporal formation of Pd xS y molecules. At the 258.056 nm line, with the wavelength range covering central pixel ± 5 pixels and with application of interactive background correction, the detection limit was 14 ng in graphite furnace molecular absorption spectrometry and 18 mg kg -1 in flame molecular absorption spectrometry. Meanwhile, application of 2-points background correction found a characteristic mass of 12 ng in graphite furnace molecular absorption spectrometry and a characteristic concentration of 104 mg kg -1 in flame molecular absorption spectrometry. The range of application of the proposed methods turned out to be significantly limited by the properties of the sulphur compounds of interest. In the case of volatile sulphur compounds, which can be present in light petroleum products, severe difficulties were encountered. On the contrary, heavy oils and residues from distillation as well as crude oil could be analysed using both flame and graphite furnace vaporisation. The good accuracy of the proposed methods for these samples was confirmed by their mutual consistency and the results from analysis of reference samples (certified reference materials and home reference materials with sulphur content determined by X-ray fluorescence

Feasibility of high-resolution continuum source molecular absorption spectrometry in flame and furnace for sulphur determination in petroleum products

Energy Technology Data Exchange (ETDEWEB)

Kowalewska, Zofia, E-mail: zofia.kowalewska@obr.pl

2011-07-15

For the first time, high-resolution molecular absorption spectrometry with a high-intensity xenon lamp as radiation source has been applied for the determination of sulphur in crude oil and petroleum products. The samples were analysed as xylene solutions using vaporisation in acetylene-air flame or in an electrothermally heated graphite furnace. The sensitive rotational lines of the CS molecule, belonging to the {Delta}{nu} = 0 vibrational sequence within the electronic transition X{sup 1}{Sigma}{sup +} {yields} A{sup 1}{Pi}, were applied. For graphite furnace molecular absorption spectrometry, the Pd + Mg organic modifier was selected. Strong interactions with Pd atoms enable easier decomposition of sulphur-containing compounds, likely through the temporal formation of Pd{sub x}S{sub y} molecules. At the 258.056 nm line, with the wavelength range covering central pixel {+-} 5 pixels and with application of interactive background correction, the detection limit was 14 ng in graphite furnace molecular absorption spectrometry and 18 mg kg{sup -1} in flame molecular absorption spectrometry. Meanwhile, application of 2-points background correction found a characteristic mass of 12 ng in graphite furnace molecular absorption spectrometry and a characteristic concentration of 104 mg kg{sup -1} in flame molecular absorption spectrometry. The range of application of the proposed methods turned out to be significantly limited by the properties of the sulphur compounds of interest. In the case of volatile sulphur compounds, which can be present in light petroleum products, severe difficulties were encountered. On the contrary, heavy oils and residues from distillation as well as crude oil could be analysed using both flame and graphite furnace vaporisation. The good accuracy of the proposed methods for these samples was confirmed by their mutual consistency and the results from analysis of reference samples (certified reference materials and home reference materials with

Flow injection on-line dilution for zinc determination in human saliva with electrothermal atomic absorption spectrometry detection

Energy Technology Data Exchange (ETDEWEB)

Burguera-Pascu, Margarita [Department of Oral Medicine, School of Dentistry, University of Granada, Granada (Spain)], E-mail: margaburpas@hotmail.com; Rodriguez-Archilla, Alberto [Department of Oral Medicine, School of Dentistry, University of Granada, Granada (Spain); Burguera, Jose Luis; Burguera, Marcela; Rondon, Carlos; Carrero, Pablo [Department of Chemistry, Faculty of Sciences, University of Los Andes, Merida (Venezuela)

2007-09-26

An automated method is described for the determination of zinc in human saliva by electrothermal atomic absorption spectrometry (ET AAS) after on-line dilution of samples with a significant reduction of sample consumption per analysis (<0.4 mL including the dead volume of the system). In order to fulfill this aim without changing the sample transport conduits during the experiments, a flow injection (FI) dilution system was constructed. Its principal parts are: one propulsion device (peristaltic pump, PP) for either samples, standards or washing solution all located in an autosampler tray and for the surfactant solution (Triton X-100) used as diluent, and a two-position time based solenoid injector (TBSI{sub 1}) which allowed the introduction of 10 {mu}L of either solution in the diluent stream. To avoid unnecessary waste of samples, the TBSI{sub 1} also permitted the recirculation of the solutions to their respective autosampler cups. The downstream diluted solution fills a home made sampling arm assembly. The sequential deposition of 20 {mu}L aliquots of samples or standards on the graphite tube platform was carried out by air displacement with a similar time based solenoid injector (TBSI{sub 2}). The dilution procedure and the injection of solutions into the atomizer are computer controlled and synchronized with the operation of the temperature program. Samples or standards solutions were submitted to two drying steps (at 90 and 130 deg. C), followed by pyrolysis and atomization at 700 and 1700 deg. C, respectively. The aqueous calibration was linear up to 120.0 {mu}g L{sup -1} for diluted standard solutions/samples and its slope was similar (p > 0.05) to the standard addition curve, indicating lack of matrix effect. The precision tested by repeated analysis of real saliva samples was less than 3% and the detection limit (3{sigma}) was of 0.35 {mu}g L{sup -1}. To test the accuracy of the proposed procedure, recovery tests were performed, obtaining mean recovery

Preconcentration, Separation and Determination of lead(II) with Methyl Thymol Blue Adsorbed on Activated Carbon Using Flame Atomic Absorption Spectrometry

Energy Technology Data Exchange (ETDEWEB)

Ensafi, Ali A.; Ghaderi, Ali R. [Isfahan University of Technology, Isfahan (Iran, Islamic Republic of)

2008-02-15

An on-line system for preconcentration and separation of lead(II) is presented. The method is based on the complex formation of Pb(II) with adsorbed Methyl thymol blue on activated carbon. The conditions of preparing the solid phase reagent and of quantitative recovery of Pb(II) from diluted solutions, such as acidity of aqueous phase, solid phase capacity, and flow variables were studied as well as effect of potential interfering ions. After preconcentration step, the metal ions are eluted automatically by 5 ml of 0.5 M HNO{sub 3} solution and the lead ions content was determined by flame atomic absorption spectrometry. Under the optimum conditions, the lead ions in aqueous samples were separated and preconcentrated about 1000-fold by the column. The detection limit was 0.001 μg mL{sup -1}. Lead has been determined in river and tap water samples, with recovery of 98 to 102%.

Augmenting the Structures in a Swirling Flame via Diffusive Injection

Directory of Open Access Journals (Sweden)

Jonathan Lewis

2014-01-01

Full Text Available Small scale experimentation using particle image velocimetry investigated the effect of the diffusive injection of methane, air, and carbon dioxide on the coherent structures in a swirling flame. The interaction between the high momentum flow region (HMFR and central recirculation zone (CRZ of the flame is a potential cause of combustion induced vortex breakdown (CIVB and occurs when the HMFR squeezes the CRZ, resulting in upstream propagation. The diffusive introduction of methane or carbon dioxide through a central injector increased the size and velocity of the CRZ relative to the HMFR whilst maintaining flame stability, reducing the likelihood of CIVB occurring. The diffusive injection of air had an opposing effect, reducing the size and velocity of the CRZ prior to eradicating it completely. This would also prevent combustion induced vortex breakdown CIVB occurring as a CRZ is fundamental to the process; however, without recirculation it would create an inherently unstable flame.

Preconcentration of Co, Ni, Cd and Zn on naphthalene–2,4,6-trimorpholino-1,3,5-triazin adsorbent and flame atomic absorption determination

Directory of Open Access Journals (Sweden)

TAYYEBEH MADRAKIAN

2010-05-01

Full Text Available A preconcentration method was developed for the determination of trace amounts of Co, Ni, Cd and Zn by atomic absorption spectrometry. The method is based on the retention of the metal cations by naphthalene–2,4,6-trimorpholino-1,3,5-triazin adsorbent in a column. The adsorbed metals were then eluted from the column with hydrochloric acid and the Co, Ni, Cd and Zn were determined by flame atomic absorption spectrometry. The optimal extraction and elution conditions were studied. The effects of diverse ions on the preconcentration were also investigated. A preconcentration factor of 250 for Co(II, Ni(II and Zn(II, and 400 for Cd(II can easily be achieved. Calibration graphs were obtained and the detection limits of the method for Co(II, Ni(II, Cd(II and Zn(II were 0.51, 0.49, 0.17 and 0.10 ng mL-1, respectively. The relative standard deviations (RSD of 0.37–2.31 % for Co, 0.37–3.73 % for Ni, 2.20–2.40 % for Cd and 1.50–2.56 % for Zn were obtained. The method was also used for the simultaneous preconcentration of these elements and the method was successfully applied to their preconcentration and determination. The method was applied to the determination of Co, Ni, Cd and Zn in several real samples.

Separation/preconcentration of trace Pb(II and Cd(II with 2-mercaptobenzothiazole impregnated Amberlite XAD-1180 resin and their determination by flame atomic absorption spectrometry

Directory of Open Access Journals (Sweden)

Şerife Tokalıoğlu

2017-01-01

Full Text Available A new chelating resin, 2-mercaptobenzothiazole loaded Amberlite XAD-1180 was prepared and used for separation and preconcentration of Cd(II and Pb(II ions prior to their determinations by flame atomic absorption spectrometry. The optimum pH for simultaneous retention of the elements and the best elution means for their simultaneous elution were 9.5 and 2 mol L−1 HNO3, respectively. The detection limits for Cd(II and Pb(II were 0.35 and 5.0 μg L−1, respectively. The accuracy of the method was confırmed both by analyzing the certified reference material (RM 8704 Buffalo river sediment and performing recovery studies.

Determination of As(III) and As(V) by Flow Injection-Hydride Generation-Atomic Absorption Spectrometry via On-line Reduction of As(V) by KI

DEFF Research Database (Denmark)

Nielsen, Steffen; Hansen, Elo Harald

1997-01-01

A volume-based flow injection (FI) procedure is described for the determination and speciation of trace inorganic arsenic, As(III) and As(V), via hydride generation-atomic absorption spectrometry (HG-AAS) of As(III). The determination of total arsenic is obtained by on-line reduction of As(V) to As...

Tunable Diode Laser Atomic Absorption Spectroscopy for Detection of Potassium under Optically Thick Conditions.

Science.gov (United States)

Qu, Zhechao; Steinvall, Erik; Ghorbani, Ramin; Schmidt, Florian M

2016-04-05

Potassium (K) is an important element related to ash and fine-particle formation in biomass combustion processes. In situ measurements of gaseous atomic potassium, K(g), using robust optical absorption techniques can provide valuable insight into the K chemistry. However, for typical parts per billion K(g) concentrations in biomass flames and reactor gases, the product of atomic line strength and absorption path length can give rise to such high absorbance that the sample becomes opaque around the transition line center. We present a tunable diode laser atomic absorption spectroscopy (TDLAAS) methodology that enables accurate, calibration-free species quantification even under optically thick conditions, given that Beer-Lambert's law is valid. Analyte concentration and collisional line shape broadening are simultaneously determined by a least-squares fit of simulated to measured absorption profiles. Method validation measurements of K(g) concentrations in saturated potassium hydroxide vapor in the temperature range 950-1200 K showed excellent agreement with equilibrium calculations, and a dynamic range from 40 pptv cm to 40 ppmv cm. The applicability of the compact TDLAAS sensor is demonstrated by real-time detection of K(g) concentrations close to biomass pellets during atmospheric combustion in a laboratory reactor.

Solid-phase extraction and separation procedure for trace aluminum in water samples and its determination by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS).

Science.gov (United States)

Ciftci, Harun; Er, Cigdem

2013-03-01

In the present study, a separation/preconcentration procedure for determination of aluminum in water samples has been developed by using a new atomic absorption spectrometer concept with a high-intensity xenon short-arc lamp as continuum radiation source, a high-resolution double-echelle monochromator, and a charge-coupled device array detector. Sample solution pH, sample volume, flow rate of sample solution, volume, and concentration of eluent for solid-phase extraction of Al chelates with 4-[(dicyanomethyl)diazenyl] benzoic acid on polymeric resin (Duolite XAD-761) have been investigated. The adsorbed aluminum on resin was eluted with 5 mL of 2 mol L(-1) HNO(3) and its concentration was determined by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). Under the optimal conditions, limit of detection obtained with HR-CS FAAS and Line Source FAAS (LS-FAAS) were 0.49 μg L(-1) and 3.91 μg L(-1), respectively. The accuracy of the procedure was confirmed by analyzing certified materials (NIST SRM 1643e, Trace elements in water) and spiked real samples. The developed procedure was successfully applied to water samples.

Investigations into the Role of Modifiers for Entrapment of Hydrides in Flow Injection Hydride Generation Electrothermal Atomic Absorption Spectrometry as Exemplified for the Determination of Germanium

DEFF Research Database (Denmark)

Hilligsøe, Bo; Andersen, Jens Enevold Thaulov; Hansen, Elo Harald

1997-01-01

Pd-conditioned graphite tubes, placed in the furnace of an atomic absorption spectrometry instrument, are used for entrapment of germane as generated in an associated flow injection system. Two different approaches are tested with the ultimate aim to allow multiple determinations, that is...

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

Energy Technology Data Exchange (ETDEWEB)

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

2005-06-01

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

An expression for the atomic fluorescence and thermal-emission intensity under conditions of near saturation and arbitrary self-absorption

NARCIS (Netherlands)

Omenetto, N.; Winefordner, J.D.; Alkemade, C.T.J.

An expression for the effect of self-absorption on the fluorescence and thermal emission intensities is derived by taking into account stimulated emission. A simple, idealized case is considered, consisting of a two level atomic system, in a flame, homogeneous with respect to temperature and

Development of an automated sequential injection on-line solvent extraction-back extraction procedure as demonstrated for the determination of cadmium with detection by electrothermal atomic absorption spectrometry

DEFF Research Database (Denmark)

Wang, Jianhua; Hansen, Elo Harald

2002-01-01

An automated sequential injection (SI) on-line solvent extraction-back extraction separation/preconcentration procedure is described. Demonstrated for the assay of cadmium by electrothermal atomic absorption spectrometry (ETAAS), the analyte is initially complexed with ammonium pyrrolidinedithioc......An automated sequential injection (SI) on-line solvent extraction-back extraction separation/preconcentration procedure is described. Demonstrated for the assay of cadmium by electrothermal atomic absorption spectrometry (ETAAS), the analyte is initially complexed with ammonium....../preconcentration process of the ensuing sample. An enrichment factor of 21.4, a detection limit of 2.7 ng/l, along with a sampling frequency of 13s/h were obtained at a sample flow rate of 6.0mlmin/sup -1/. The precision (R.S.D.) at the 0.4 mug/l level was 1.8% as compared to 3.2% when quantifying the organic extractant...

Study of interferences in the atomic - absorption and emission of barium in nitrous oxide/acetylene flame

International Nuclear Information System (INIS)

Curtius, A.J.; Couto, M.I.

1979-01-01

The interferences of several ions that are present in oifield water and sea water in the atomic absorption and emission of barium were investigated. It was verified that the interferences of sodium, potassium, calcium, strontium and chloride are the most important. The indirect method for the determination of sulfate by measuring barium by atomic absorption after precipitating barium sulfate with an excess of barium chloride, should not be used for highly salted matrix. To avoid the interferences that are not compensated by an ionization supressor, the measurement of barium by the standard addition method or a previous sulfate separation is recommended. (Author) [pt

Introduction of Flame Atomic Absorption Spectrometry (FAAS) For River Water Samples Analysis

International Nuclear Information System (INIS)

Shakirah Abd Shukor; Mohd Suhaimi Hamzah; Shamsiah Abdul Rahman

2015-01-01

Metal contamination in water is a major component in the determination of water quality monitoring. In spite of the viability of several other metal ion analysis techniques for river water, atomic absorption spectroscopy (AAS) method is most commonly used due to the reproducibility results, short analysis time, cost effective, lower level detection and robust. Therefore, this article gives an overview on the principles, instrumentation techniques, sample preparations, instrument calibration and data analysis in a simple manner for beginner. (author)

Fast sequential multi-element determination of major and minor elements in environmental samples and drinking waters by high-resolution continuum source flame atomic absorption spectrometry.

Science.gov (United States)

Gómez-Nieto, Beatriz; Gismera, Ma Jesús; Sevilla, Ma Teresa; Procopio, Jesús R

2015-01-07

The fast sequential multi-element determination of 11 elements present at different concentration levels in environmental samples and drinking waters has been investigated using high-resolution continuum source flame atomic absorption spectrometry. The main lines for Cu (324.754 nm), Zn (213.857 nm), Cd (228.802 nm), Ni (232.003 nm) and Pb (217.001 nm), main and secondary absorption lines for Mn (279.482 and 279.827 nm), Fe (248.327, 248.514 and 302.064 nm) and Ca (422.673 and 239.856 nm), secondary lines with different sensitivities for Na (589.592 and 330.237 nm) and K (769.897 and 404.414 nm) and a secondary line for Mg (202.582 nm) have been chosen to perform the analysis. A flow injection system has been used for sample introduction so sample consumption has been reduced up to less than 1 mL per element, measured in triplicate. Furthermore, the use of multiplets for Fe and the side pixel registration approach for Mg have been studied in order to reduce sensitivity and extend the linear working range. The figures of merit have been calculated and the proposed method was applied to determine these elements in a pine needles reference material (SRM 1575a), drinking and natural waters and soil extracts. Recoveries of analytes added at different concentration levels to water samples and extracts of soils were within 88-115% interval. In this way, the fast sequential multi-element determination of major and minor elements can be carried out, in triplicate, with successful results without requiring additional dilutions of samples or several different strategies for sample preparation using about 8-9 mL of sample. Copyright © 2014 Elsevier B.V. All rights reserved.

Preconcentrative separation of chromium(III) species from chromium(VI) by cloud point extraction and determination by flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Yildiz, Z.; Arslan, G.; Tor, A.

2011-01-01

We describe a high-throughput technique for the determination of chromium species in water samples by flame atomic absorption spectrometry (FAAS) after preconcentrative separation of Cr(III) species from Cr(VI) by cloud point extraction (CPE) using diethyldithiocarbamate (DDTC) as the chelating agent and the nonionic surfactant Triton X-100 as the extractant. The Cr(III)-DDTC complex is extracted if the temperature is higher than the CPE temperature of Triton X-100, while Cr(VI) remains in the aqueous phase. The Cr(III) in the surfactant phase was analyzed by FAAS, and the concentration of Cr(VI) was calculated by subtraction of Cr(III) from total chromium which was directly determined by FAAS. The effect of pH, concentration of chelating agent, surfactant, and equilibration temperature were investigated. The detection limit for Cr(III) was 0. 08 μg L -1 with an enrichment factor of 98, and the relative standard deviation was 1. 2% (n = 3, c = 100 μg L -1 ). A certified reference material and several water samples were analyzed with satisfactory results. (author)

Direct analysis of Antarctic krill by slurry sampling: determination of copper, iron, manganese and zinc by flame atomic absorption spectrometry

Directory of Open Access Journals (Sweden)

Alves Flávia L.

2000-01-01

Full Text Available Slurry sampling in combination with flame atomic absorption spectrometry was employed for the direct determination of four essential trace elements, namely Cu, Fe, Mn and Zn in Antarctic krill. The effect of instrumental operating conditions and slurry sampling preparation on the analytical signal was investigated. For the determination of Cu, Fe and Zn, samples were suspended in a solution containing 2 mol L-1 HNO3. In the case of Mn, 4 mol L-1 HNO3 was necessary for the preparation of the slurry. The precision between sample replicates was better than 5%. The method was applied to the direct determination of Cu, Fe, Mn and Zn in Antarctic krill samples using aqueous reference solutions to prepare the calibration curves. The results obtained were in good agreement with those achieved by FAAS and ICP-AES after microwave-assisted wet digestion of the krill samples. The detection limits were 4.5, 1.0, 4.9 and 8.4 mug L-1 for Cu, Zn, Mn and Fe, respectively.

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

International Nuclear Information System (INIS)

Jat, J.R.; Balaji Rao, Y.; Prasada Rao, G.; Prahlad, B.

2012-01-01

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 CCI 4 followed by Tri-n-Octyl Phosphine Oxide (TOPO) in CCI 4 , 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 UO 2 powder and pellets on regular basis

Atomic-fluorescence spectrophotometry

International Nuclear Information System (INIS)

Bakhturova, N.F.; Yudelevich, I.G.

1975-01-01

Atomic-fluorescence spectrophotometry, a comparatively new method for the analysis of trace quantities, has developed rapidly in the past ten years. Theoretical and experimental studies by many workers have shown that atomic-fluorescence spectrophotometry (AFS) is capable of achieving a better limit than atomic absorption for a large number of elements. The present review examines briefly the principles of atomic-fluorescence spectrophotometry and the types of fluorescent transition. The excitation sources, flame and nonflame atomizers, used in AFS are described. The limits of detection achieved up to the present, using flame and nonflame methods of atomization are given

Determination numbers of ionized atoms from emission and absorption lines

International Nuclear Information System (INIS)

Alizadeh Azimi, A.; Shokouhi, N.

2002-01-01

Saha, M., (1920) estimated that salter chromosphere is not only due to radiation from neutral atoms, but from ionized atoms. The failure to observe these stellar lines in the laboratory was attributed to internal temperature and pressure about 10* E + 6 K 10* E-7 atm. In this research we found that emission lines of ionized atoms (like Cs) could be measured in laboratory condition, (about 10* E-3 atm and 2000 K) by using Graphite France Atomic Absorption with injection 124 u g C sel. We calculated the numbers of ionized atoms from Bottzman law. We also measured these numbers from area under the energy-time curve

Flame Atomic Absorption Determination of Gold Ion in Aqueous Samples after Preconcentration Using 9-Acridinylamine Functionalized γ-Alumina Nanoparticles

Directory of Open Access Journals (Sweden)

Mohammad Karimi

2013-01-01

Full Text Available A simple and sensitive solid phase extraction utilizing 9-acridinylamine functionalized alumina nanoparticles was developed, and their potential use for preconcentration and subsequent determination of gold by flame atomic absorption spectrometry (FAAS was investigated. A number of parameters, namely, type, concentration, and volume of eluent, pH of the sample solution, flow rate of extraction, and volume of the sample, were evaluated. The effect of a variety of ions on preconcentration and recovery was also investigated. Gold ions were found to be recovered quantitatively at pH 3.0, with 0.1 mol L−1 thiourea in 2 mol L−1 H2SO4 as eluent. The limit of detection (LOD, defined as five times the standard deviation of the blank, was determined to be lower than 13.0 ppb. Under optimum conditions, the accuracy and precision (RSD% of the method were >98.0 and <1.5%, respectively. To gauge its ability in terms of application to real samples, the proposed method was successfully applied for determination of gold concentration in waste water samples and one soil standard material, and satisfactory results were obtained.

Graphene for separation and preconcentration of trace amounts of cobalt in water samples prior to flame atomic absorption spectrometry

Directory of Open Access Journals (Sweden)

Yukun Wang

2016-09-01

Full Text Available A new sensitive and simple method was developed for the preconcentration of trace amounts of cobalt (Co using 1-(2-pyridylazo-2-naphthol (PAN as chelating reagent prior to its determination by flame atomic absorption spectrometry. The proposed method is based on the utilization of a column packed with graphene as sorbent. Several effective parameters on the extraction and complex formation were selected and optimized. Under optimum conditions, the calibration graph was linear in the concentration range of 5.0–240.0 μg L−1 with a detection limit of 0.36 μg L−1. The relative standard deviation for ten replicate measurements of 20.0 and 100.0 μg L−1 of Co were 3.45 and 3.18%, respectively. Comparative studies showed that graphene is superior to other adsorbents including C18 silica, graphitic carbon, and single- and multi-walled carbon nanotubes for the extraction of Co. The proposed method was successfully applied in the analysis of four real environmental water samples. Good spiked recoveries over the range of 95.8–102.6% were obtained.

Development of the Flame Test Concept Inventory: Measuring Student Thinking about Atomic Emission

Science.gov (United States)

Bretz, Stacey Lowery; Murata Mayo, Ana Vasquez

2018-01-01

This study reports the development of a 19-item Flame Test Concept Inventory, an assessment tool to measure students' understanding of atomic emission. Fifty-two students enrolled in secondary and postsecondary chemistry courses were interviewed about atomic emission and explicitly asked to explain flame test demonstrations and energy level…

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

DEFF Research Database (Denmark)

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...... 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 eluate forwarded...

Atomic absorption spectrophotometry in perspective

International Nuclear Information System (INIS)

Soffiantini, V.

1981-01-01

Atomic absorption spectrophotometry is essentially an analytical technique used for quantitative trace metal analysis in a variety of materials. The speed and specificity of the technique is its greatest advantage over other analytical techniques. What atomic absorption spectrophotometry can and cannot do and its advantages and disadvantages are discussed, a summary of operating instructions are given, as well as a summary of analytical interferences. The applications of atomic absorption spectrophotometry are also shortly discussed

Optimization of microwave assisted digestion procedure for the determination of zinc, copper and nickel in tea samples employing flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Soylak, Mustafa; Tuzen, Mustafa; Souza, Anderson Santos; Korn, Maria das Gracas Andrade; Ferreira, Sergio Luis Costa

2007-01-01

The present paper describes the development of a microwave assisted digestion procedure for the determination of zinc, copper and nickel in tea samples employing flame atomic absorption spectrometry (FAAS). The optimization step was performed using a full factorial design (2 3 ) involving the factors: composition of the acid mixture (CMA), microwave power (MP) and radiation time (RT). The experiments of this factorial were carried out using a certified reference material of tea GBW 07605 furnished by National Research Centre for Certified Reference Materials, China, being the metal recoveries considered as response. The relative standard deviations of the method were found below 8% for the three elements. The procedure proposed was used for the determination of copper, zinc and nickel in several samples of tea from Turkey. For 10 tea samples analyzed, the concentration achieved for copper, zinc and nickel varied at 6.4-13.1, 7.0-16.5 and 3.1-5.7 (μg g -1 ), respectively

Solid phase extraction of lead on octadecyl bonded silica membrane disk modified with Cyanex302 and determination by flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Karve, Manjusha; Rajgor, Reeta V.

2007-01-01

A simple, reliable and rapid method for preconcentration and determination of lead using octadecyl bonded silica membrane disk impregnated with Cyanex302 and flame atomic absorption spectrometry is presented. The influence of aqueous phase pH, type of eluent, flow rates of sample solution and eluent, volume of eluent and amount of extractant has been investigated. The break through volume is greater than 4.0 dm 3 with an enrichment factor of more than 400 and a detection limit of 1.0 μg dm -3 . The method developed for determination of lead is good as six replicate determinations using 100 cm 3 solution containing lead in the range 1-4900 μg provides a relative standard deviation (R.S.D.) of 0.4%. The selectivity of the proposed method was confirmed from the interference studies. The developed procedure was successfully applied for the determination of lead in spiked sea water, USGS standard soil sample, sludge and industrial effluents, medicinal formulation, plant, some food products and wine

Sequential injection on-line matrix removal and trace metal preconcentration using a PTFE beads packed column as demonstrated for the determination of cadmium by electrothermal atomic absorption spectrometry

DEFF Research Database (Denmark)

Wang, Jianhua; Hansen, Elo Harald

2002-01-01

A sequential injection (SI) on-line matrix removal and trace metal preconcentration procedure by using a novel microcolumn packed with PTFE beads is described, and demonstrated for trace cadmium analysis with detection by electrothermal atomic absorption spectrometry (ETAAS). The analyte...

Two-dimensional temperature and carbon dioxide concentration profiles in atmospheric laminar diffusion flames measured by mid-infrared direct absorption spectroscopy at 4.2 μm

Science.gov (United States)

Liu, Xunchen; Zhang, Guoyong; Huang, Yan; Wang, Yizun; Qi, Fei

2018-04-01

We present a multi-line flame thermometry technique based on mid-infrared direct absorption spectroscopy of carbon dioxide at its v_3 fundamental around 4.2 μm that is particularly suitable for sooting flames. Temperature and concentration profiles of gas phase molecules in a flame are important characteristics to understand its flame structure and combustion chemistry. One of the standard laboratory flames to analyze polycyclic aromatic hydrocarbons (PAH) and soot formation is laminar non-premixed co-flow flame, but PAH and soot introduce artifact to most non-contact optical measurements. Here we report an accurate diagnostic method of the temperature and concentration profiles of CO2 in ethylene diffusion flames by measuring its v_3 vibrational fundamental. An interband cascade laser was used to probe the R-branch bandhead at 4.2 μm, which is highly sensitive to temperature change, free from soot interference and ambient background. Calibration measurement was carried out both in a low-pressure Herriott cell and an atmospheric pressure tube furnace up to 1550 K to obtain spectroscopic parameters for high-temperature spectra. In our co-flow flame measurement, two-dimensional line-of-sight optical depth of an ethylene/N2 laminar sooting flame was recorded by dual-beam absorption scheme. The axially symmetrical attenuation coefficient profile of CO2 in the co-flow flame was reconstructed from the optical depth by Abel inversion. Spatially resolved flame temperature and in situ CO2 volume fraction profiles were derived from the calibrated CO2 spectroscopic parameters and compared with temperature profiles measured by two-line atomic fluorescence.

A low-cost vaporization-atomization system for atomic absorption spectrometry

International Nuclear Information System (INIS)

Bruhn F, C.G.; Ambiado V, F.; Woerner V, R.

1990-01-01

A low-cost vaporization-atomization system for atomic absorption spectrometry is developed as an alternative to the use of a graphite furnace in electrothermal atomic absorption spectrometry. (Author)

Analysis of impurities in silver matrix by atomic absorption spectrophotometry

International Nuclear Information System (INIS)

Hussain, R.; Ishaque, M.; Mohammad, D.

1999-01-01

A procedure for the analysis of aluminium, chromium, copper, lead, mercury, nickel and zinc mainly using flame lens atomic absorption spectrophotometry has been described. The results depict that the presence of silver does not introduce any significant interference, when standards are prepared in matching silver matrix solutions. The calibration curves obey the straight-line equations passing through the origin. Thus the separation of silver matrix from the analyte solutions is not necessary. The method has successfully been applied for the analysis of silver foils, wires, battery grade silver oxides and silver nitrate samples containing analyte elements in the concentration range 2 to 40 ppm. (author)

Zeeman atomic absorption spectroscopy

International Nuclear Information System (INIS)

Loos-Vollebregt, M.T.C. de.

1980-01-01

A new method of background correction in atomic absorption spectroscopy has recently been introduced, based on the Zeeman splitting of spectral lines in a magnetic field. A theoretical analysis of the background correction capability observed in such instruments is presented. A Zeeman atomic absorption spectrometer utilizing a 50 Hz sine wave modulated magnetic field is described. (Auth.)

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

Science.gov (United States)

Issa, M M; Nejem, R M; El-Abadla, N S; Al-Kholy, M; Saleh, Akila A

2008-01-01

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 mug/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 mug/ml, respectively. The limit of quantitation of paracetamol by method II and atomic absorption spectrometric method were 0.20 and 0.10 mug/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%.

[Determination of sulfur in plant using a high-resolution continuum source atomic absorption spectrometer].

Science.gov (United States)

Wang, Yu; Li, Jia-xi

2009-05-01

A method for the analysis of sulfur (S) in plant by molecular absorption of carbon monosulfide (CS) using a high-resolution continuum source atomic absorption spectrometer (CS AAS) with a fuel-rich air/acetylene flame has been devised. The strong CS absorption band was found around 258 nm. The half-widths of some absorption bands were of the order of picometers, the same as the common atomic absorption lines. The experimental procedure in this study provided optimized instrumental conditions (the ratio of acetylene to air, the burner height) and parameters, and researched the spectral interferences and chemical interferences. The influence of the organic solvents on the CS absorption signals and the different digestion procedures for the determination of sulfur were also investigated. The limit of detection achieved for sulfur was 14 mg x L(-1), using the CS wavelength of 257. 961 nm and a measurement time of 3 s. The accuracy and precision were verified by analysis of two plant standard reference materials. The major applications of this method have been used for the determination of sulfur in plant materials, such as leaves. Compared to the others, this method for the analysis of sulfur is rapid, easy and simple for sulfur determination in plant.

Cloud point extraction of palladium in water samples and alloy mixtures using new synthesized reagent with flame atomic absorption spectrometry (FAAS)

International Nuclear Information System (INIS)

Priya, B. Krishna; Subrahmanayam, P.; Suvardhan, K.; Kumar, K. Suresh; Rekha, D.; Rao, A. Venkata; Rao, G.C.; Chiranjeevi, P.

2007-01-01

The present paper outlines novel, simple and sensitive method for the determination of palladium by flame atomic absorption spectrometry (FAAS) after separation and preconcentration by cloud point extraction (CPE). The cloud point methodology was successfully applied for palladium determination by using new reagent 4-(2-naphthalenyl)thiozol-2yl azo chromotropic acid (NTACA) and hydrophobic ligand Triton X-114 as chelating agent and nonionic surfactant respectively in the water samples and alloys. 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. The preconcentration factor was found to be (50-fold) for 250 ml of water sample. Under optimum condition the detection limit was found as 0.067 ng ml -1 for palladium in various environmental matrices. The present method was applied for the determination of palladium in various water samples, alloys and the result shows good agreement with reported method and the recoveries are in the range of 96.7-99.4%

Determination of total inorganic arsenic in potable water through spectroscopy of atomic absorption with generation of hydride

International Nuclear Information System (INIS)

Rodriguez Roman, S.

1997-01-01

This study developed a method for the cuantitative analysis of arsenic in potable water , through the spectrophotometric technique of atomic absorption. It used an automatic system of injection of flux for the generation of hydrides. It studied the effect produced by reducer agents, in the prereduction of arsenic in water, obtaining the best result with the use of potasium iodide 1.5% and ascorbic acid 0.25% in hydrochloric acid 3.7%, for the direct determination of total inorganic arsenic. It observed the effect produced by cadmium and selenium to the half of the concentration of arsenic, chromium, lead and silver at the same concentration, and barium at a ten times higher concentration, in the recuperation of total inorganic arsenic. It also used sodium borohydride 0.3% in sodium hydroxide 0.05% (5mL/min), for the formation of the volatile hydrides. It used hydrochloric acid 3.7% (12 mL/min) as disolution of transport; argon as inert gas, and a flame air-acetylene, for the atomization of the hydrides. This method was applied to 19 samples of potable water, and the result was no detectable for all of them. (S. Grainger)

Preconcentration and determination of zinc and lead ions by a combination of cloud point extraction and flame atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Tavallali, H. [Chemistry Department, Payamenore University, Shiraz (Iran); Shokrollahi, A.; Zahedi, M. [Chemistry Department, Yasouj University, Yasouj (Iran); Niknam, K. [Chemistry Department, Persian Gulf University, Bushehr (Iran); Soylak, M. [Chemistry Department, University of Erciyes, Kayseri (Turkey); Ghaedi, M.

2009-04-15

The phase-separation phenomenon of non-ionic surfactants occurring in aqueous solution was used for the extraction of lead(II) and zinc(II). After complexation with 3-[(4-bromophenyl) (1-H-inden-3-yl)methyl]-1 H-indene (BPIMI), the analytes were quantitatively extracted to a phase rich in Triton X-114 after centrifugation. Methanol acidified with 1 mol/L HNO{sub 3} was added to the surfactant rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The concentration of bis((1H-benzo [d] imidazol-2yl)ethyl)sulfane, Triton X-114, pH and amount of surfactant were all optimized. Detection limits (3 SDb/m) of 2.5 and 1.6 ng/mL for Pb{sup 2+} and Zn{sup 2+} along with preconcentration factors of 30 and an enrichment factor of 32 and 48 for Pb{sup 2+}and Zn {sup 2+} ions were obtained, respectively. The proposed cloud point extraction was been successfully applied for the determination of these ions in real samples with complicated matrices such as food and soil samples, with high efficiency. (Abstract Copyright [2009], Wiley Periodicals, Inc.)

A pre-concentration procedure using coprecipitation for determination of lead and iron in several samples using flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Saracoglu, S.; Soylak, M.; Peker, D.S. Kacar; Elci, L.; Santos, W.N.L. dos; Lemos, V.A.; Ferreira, S.L.C.

2006-01-01

The present paper proposes a pre-concentration procedure for determination of lead and iron in several samples by flame atomic absorption spectrometry. In it, lead(II) and iron(III) ions are coprecipitated using the violuric acid-copper(II) system as collector. Afterwards, the precipitate is dissolved with 1 M HNO 3 solution and the metal ions are determined. The optimization step was performed using factorial design involving the variables: pH, violuric acid mass (VA) and copper concentration (Cu). Using the optimized experimental conditions, the proposed procedure allows the determination these metals with detection limits of 0.18 μg L -1 for iron and 0.16 μg L -1 for lead. The effects of foreign ions on the pre-concentration procedure were also evaluated and the results demonstrated that this method could be applied for determination of iron and lead in several real samples. The proposed method was successfully applied to the analysis of seawater, urine, mineral water, soil and physiological solution samples. The concentrations of lead and iron achieved in these samples agree well with others data reported in the literature

Absorption properties of identical atoms

International Nuclear Information System (INIS)

Sancho, Pedro

2013-01-01

Emission rates and other optical properties of multi-particle systems in collective and entangled states differ from those in product ones. We show the existence of similar effects in the absorption probabilities for (anti)symmetrized states of two identical atoms. The effects strongly depend on the overlapping between the atoms and differ for bosons and fermions. We propose a viable experimental verification of these ideas. -- Highlights: •The absorption rates of a pair of identical atoms in product and (anti)symmetrized states are different. •The modifications of the optical properties are essentially determined by the overlapping between the atoms. •The absorption properties differ, in some cases, for bosons and fermions

Separation and determination of copper in bottled water samples by combination of dispersive liquid--liquid microextraction and microsample introduction flame atomic absorption spectrometry.

Science.gov (United States)

Citak, Demirhan; Tuzen, Mustafa

2013-01-01

A new and simple method for the determination of trace amounts of Cu(II) was developed by combination of dispersive liquid-liquid microextraction (DLLME) preconcentration and microsample introduction flame atomic absorption spectrometry. In this method, ethanol and chloroform were chosen as disperser and extraction solvents, respectively, and 1-nitroso-2-naphthol was used as the complexing agent. The factors affecting the extraction efficiency and determination of Cu(II), including extraction and disperser solvent nature and volume, concentration of the complexing agent, pH of the solution, extraction time, and matrix ions, were investigated. Under optimal conditions, the LOD for Cu(II) was 0.95 microg/L with a preconcentration factor of 70. The RSD was 1.9%. The accuracy of the developed DLLME method was verified by determination of Cu(II) in a certified reference material (NRCC-SLRS-4 river water). The relative error was -3.31%. The developed preconcentration procedure was successfully applied to the analysis of bottled drinking water samples.

Determination of phosphorus, sulfur and the halogens using high-temperature molecular absorption spectrometry in flames and furnaces-A review

International Nuclear Information System (INIS)

Welz, Bernhard; Lepri, Fabio G.; Araujo, Rennan G.O.; Ferreira, Sergio L.C.; Huang Maodong; Okruss, Michael; Becker-Ross, Helmut

2009-01-01

The literature about the investigation of molecular spectra of phosphorus, sulfur and the halogens in flames and furnaces, and the use of these spectra for the determination of these non-metals has been reviewed. Most of the investigations were carried out using conventional atomic absorption spectrometers, and there were in essence two different approaches. In the first one, dual-channel spectrometers with a hydrogen or deuterium lamp were used, applying the two-line method for background correction; in the second one, a line source was used that emitted an atomic line, which overlapped with the molecular spectrum. The first approach had the advantage that any spectral interval could be accessed, but it was susceptible to spectral interference; the second one had the advantage that the conventional background correction systems could be used to minimize spectral interferences, but had the problem that an atomic line had to be found, which was overlapping sufficiently well with the maximum of the molecular absorption spectrum. More recently a variety of molecular absorption spectra were investigated using a low-resolution polychromator with a CCD array detector, but no attempt was made to use this approach for quantitative determination of non-metals. The recent introduction and commercial availability of high-resolution continuum source atomic absorption spectrometers is offering completely new possibilities for molecular absorption spectrometry and its use for the determination of non-metals. The use of a high-intensity continuum source together with a high-resolution spectrometer and a CCD array detector makes possible selecting the optimum wavelength for the determination and to exclude most spectral interferences.

Standardization of digestion procedure for the determination of heavy metals in biological materials by atomic absorption spectrometry

International Nuclear Information System (INIS)

Khalid, N.; Chaudhri, S.A.

1999-01-01

Proper decomposition of the sample is one of the basic requirements of the atomic absorption spectroscopic analysis. In the present studies, heavy metals (Cu, Fe, Mn and Zn) were determined in biological samples by designating them in a mixture of nitric acid and perchloric acid. The quantification was made with atomic absorption spectrometry using an air-acetylene flame. The reliability of the procedure used was checked by analysing standard reference materials from NBS and IAEA, such as Rice flour (NBS-SRM-1568), Horse Kidney (IAEA H-8), Mixed Human diet(IAEA H-9), Copepod (IAEA MA-A-1) and fish flesh (IAEA MA-A-2) under identical conditions. A good agreement was observed between determined and the certified values reported by NBS and IAEA. (author)

Separation/preconcentration of silver(I) and lead(II) in environmental samples on cellulose nitrate membrane filter prior to their flame atomic absorption spectrometric determinations

International Nuclear Information System (INIS)

Soylak, Mustafa; Cay, Rukiye Sungur

2007-01-01

An enrichment method for trace amounts of Ag(I) and Pb(II) has been established prior to their flame atomic absorption spectrometric determinations. The preconcentration/separation procedure is based on chelate formation of Ag(I) and Pb(II) with ammonium pyrrolidine dithiocarbamate (APDC) and on retention of the chelates on cellulose nitrate membrane filter. The influences of some analytical parameters including pH and amounts of reagent, etc. on the recoveries of analytes were investigated. The effects of interferic ions on the quantitative recoveries of analytes were also examined. The detection limits (k = 3, N = 11) were 4.6 μg L -1 for silver(I) and 15.3 μg L -1 for lead(II). The relative standard deviations (R.S.D.) of the determinations for analyte ions were below 3%. The method was applied to environmental samples for the determination of analyte ions with satisfactory results (recoveries >95%)

A new cloud point extraction procedure for determination of inorganic antimony species in beverages and biological samples by flame atomic absorption spectrometry.

Science.gov (United States)

Altunay, Nail; Gürkan, Ramazan

2015-05-15

A new cloud-point extraction (CPE) for the determination of antimony species in biological and beverages samples has been established with flame atomic absorption spectrometry (FAAS). The method is based on the fact that formation of the competitive ion-pairing complex of Sb(III) and Sb(V) with Victoria Pure Blue BO (VPB(+)) at pH 10. The antimony species were individually detected by FAAS. Under the optimized conditions, the calibration range for Sb(V) is 1-250 μg L(-1) with a detection limit of 0.25 μg L(-1) and sensitive enhancement factor of 76.3 while the calibration range for Sb(III) is 10-400 μg L(-1) with a detection limit of 5.15 μg L(-1) and sensitive enhancement factor of 48.3. The precision as a relative standard deviation is in range of 0.24-2.35%. The method was successfully applied to the speciative determination of antimony species in the samples. The validation was verified by analysis of certified reference materials (CRMs). Copyright © 2014 Elsevier Ltd. All rights reserved.

Atomic absorption instrument functional description

International Nuclear Information System (INIS)

Bystroff, R.I.; Boyle, W.G. Jr.; Barton, G.W. Jr.

1976-01-01

This report describes a proposed system for automating atomic absorption analysis. The system consists of two atomic absorption instruments and an automatic sampler that can be attached to either instrument. A computer program controls the sampling and gathers data. The program then uses the data to perform bookkeeping, data processing, and report writing

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

Energy Technology Data Exchange (ETDEWEB)

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

2008-06-30

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{sup -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.

The effect of CO{sub 2} dissolved in a diesel fuel on the jet flame characteristics

Energy Technology Data Exchange (ETDEWEB)

Xiao Jin; Huang Zhen; Qiao Xinqi; Hou Yuchun [Shanghai Jiao Tong University, Shanghai (China). Research Institute of Internal Combustion Engine

2008-03-15

This paper is concerned with an experimental study of the jet diffusion flame characteristics of fuel containing CO{sub 2}. Using diesel fuel containing dissolved CO{sub 2} gas, experiments were performed under atmospheric conditions with a diesel hole-type nozzle of 0.19 mm orifice diameter at constant injection pressure. In this study, four different CO{sub 2} mass fraction in diesel fuel such as 3.13%, 7.18%, 12.33% and 17.82% were used to study the effect of CO{sub 2} concentration on the jet flame characteristics. Jet flame characteristics were measured by direct photography, meanwhile the image colorimetry is used to assess the qualitative features of jet flame temperature. Experimental results show that the CO{sub 2} gas dilution effect and the atomization effect have a great influence on the flame structure and average temperature. When the injection pressure of diesel fuel increased from 4 MPa to 6 MPa, the low temperature flame length increased from 18.4 cm to 21.7 cm and the full temperature flame length decreased from 147.6 cm to 134.7 cm. With the increase of CO{sub 2} gas dissolved in the diesel fuel, the jet flame full length decreased for the jet atomization being improved greatly meanwhile the low temperature flame length increased for the CO{sub 2} gas dilution effect; with the increase of CO{sub 2} gas dissolved in the diesel fuel, the average temperature of flame increases firstly and then falls. Experimental results validate that higher injection pressure will improve jet atomization and then increased the flame average temperature. 27 refs., 13 figs.

Determination of calcium, copper, chromium, iron, magnesium, manganese, potassium, sodium and zinc in ethanol by atomic absorption spectrometry

International Nuclear Information System (INIS)

Fernandes, E.A.N.

1981-01-01

The direct determinacao of calcium, copper, chomium, iron, magnesium, manganese, potassium, sodium and zinc in ethanol by atomic absorption spectrometry with, air-acetylene flame is proposed. Effects of fuel/oxidant ratio, burner height and water content in the samples were investigated in detail. The method allows the determition of the elements with good precision (r.s.d. -1 for the elements tested. (author) [pt

Flow Injection and Atomic Absorption Spectrometry - An Effective and Attractive Analytical Chemical Combination

DEFF Research Database (Denmark)

Hansen, Elo Harald; Nielsen, Steffen

1998-01-01

One of the advantages of the flow injection (FI) concept is that it is compatible with virtually all detection techniques. Being a versatile vehicle for enhancing the performance of the individual detection devices, the most spectacular results have possibly been obtained in conjunction with atom...

Silica gel modified with N-(3-propyl)-O-phenylenediamine: functionalization, metal sorption equilibrium studies and application to metal enrichment prior to determination by flame atomic absorption spectrometry.

Science.gov (United States)

Akl, Magda Ali Abd-elAziz; Kenawy, Ibraheim Mohamed; Lasheen, Rabab Ramadan

2005-08-01

The use of the chemically modified silica gel N-(3-propyl)-O-phenylenediamine (SiG-NPPDA) adsorbent, for the preconcentration and separation of trace heavy metals, was described. SiG-NPPDA sorbs quantitatively (90-100% recovery) trace amounts of nine heavy metals, viz., Cd(II), Zn(II), Fe(III), Cu(II), Pb(II), Mn(II), Cr(III), Co(II) and Ni(II) at pH 7-8. The sorption capacity varies from 350 to 450 micromol g(-1). Desorption was found to be quantitative with 1-2 M HNO3 or 0.05 M Na2EDTA. The distribution coefficient, Kd and the percentage concentration of the investigated metal ions on the adsorbent at equilibrium, C(M,eqm)% (Recovery, R%), were studied as a function of experimental parameters. The logarithmic values of the distribution coefficient, log Kd, ranges between 4.0 and 6.4. Some foreign ions caused little interference in the preconcentration and determination of the investigated nine metals by flame atomic absorption spectrometry (AAS). The adsorbent and its formed metal chelates were characterized by IR (absorbance and/or reflectance), potentiometric titrations and thermogravimetric analysis (TGA and DTG). The mode of chelation between the SiG-NPPDA adsorbent and the investigated metal ions is proposed to be due to the reaction of the investigated metal ions with the two nitrogen atoms of the SiG-NPPDA adsorbent. The present adsorbent coupled with flame AAS has been used to enrich and determine the nine metal ions in natural aqueous systems and in certified reference materials (RSD < or = 5%). The copper, iron, manganese and zinc present in some pharmaceutical vitamin samples were also preconcentrated on SiG-NPPDA adsorbent and determined by flame AAS (RSD < or = 4.2%). Nanogram concentrations (0.07-0.14 ng ml(-1)) of Cd(II), Zn(II), Fe(III), Pb(II), Cr(III), Mn(II), Cu(II), Co(II) and Ni(II) can be determined reliably with a preconcentration factor of 100.

Survey of content of cadmium, calcium, chromium, copper, iron, lead, magnesium, manganese, mercury, sodium and zinc in chamomile and green tea leaves by electrothermal or flame atomizer atomic absorption spectrometry

Directory of Open Access Journals (Sweden)

Prkić Ante

2018-03-01

Full Text Available Due to the simplicity of tea preparation (pouring hot water onto different dried herbs and its high popularity as a beverage, monitoring and developing a screening methodology for detecting the metal content is very important. The concentrations of Cd, Ca, Cr, Cu, Fe, Pb, Mg, Mn, Hg, Na and Zn in 8 samples of green tea (Camellia sinesis and in 11 samples chamomile (Matricaria chamomilla L. purchased both at local herbal pharmacies and supermarkets were determined using electrothermal atomizer atomic absorption spectrometry (ETAAS and flame atomizer atomic absorption spectrometry (FAAS. The found concentrations in chamomile were: Cd (0.008 – 284 mg kg−1, Ca (2.42 – 6.29%, Cr (0.91 – 6.92 mg kg−1, Cu (6.27 – 11.39 mg kg−1, Fe (133.5 – 534 mg kg−1, Pb (0.561 – 1.277 mg kg−1, Mg (2.27 – 3.73%, Mn (62.2 – 165.6 mg kg−1, Hg (0.660 – 1.346 μg kg−1, Na (0.91 – 1.28% and Zn (63.37 – 108.5 mg kg−1, in green tea Cd (36.29 – 202.1 mg kg−1, Ca (2.77 – 6.40%, Cr (1.520 – 5.278 mg kg−1, Cu (9.354 – 22.56 mg kg−1, Fe (162.6 – 513.3 mg kg−1, Pb (1.808 – 4.770 mg kg−1, Mg (1.41 – 2.62 %, Mn (1.147 – 1.729 g kg−1, Hg (1.045 – 2.802 μg kg−1, Na (0.44 – 0.98% and Zn (30.65 – 115.6 mg kg−1, respectively. Principal Component Analysis (PCA was applied to identify factors (soil, climate and country of origin influencing the content of the measured elements in herbal samples. The proposed methodology developed in this work was successfully applied to the detection of metals in herbal samples. The analysis showed that the content of toxic metals in green tea samples was significantly higher and very close to the maximum dose recommended by the World Health Organization (WHO.

Zinc and palladium traces separation from uranium by tri-n-octylamine extraction. Direct determination in organic phase by atomic absorption

Energy Technology Data Exchange (ETDEWEB)

de Moraes, S; Cipriani, M; Abrao, A

1974-12-01

A procedure for the extraction and determination of Zn and Pd as traces from nuclear grade uranium ADU, UO/sub 2/, UO/sub 3/, U/sub 3/O/sub 8/ is introduced. The elements are extracted from UO/sub 2/Cl/sub 2/-HCl-KI solution with tri-n-octylamine in benzene and determined by atomic absorption spectrophotometry. The adition of potassium iodide to the UO/sub 2/Cl/sub 2/-HCl solutions improved the extraction of both elements. Direct burn of the organic phase in the atomic absorption spectrophotometer using hydrogen-air flame provided enhancement of the absorbance for both elements. The relative standard deviations were Zn, 3% and Pd, 2.9%.

Graphene oxide sheets immobilized polystyrene for column preconcentration and sensitive determination of lead by flame atomic absorption spectrometry.

Science.gov (United States)

Islam, Aminul; Ahmad, Hilal; Zaidi, Noushi; Kumar, Suneel

2014-08-13

A novel solid-phase extractant was synthesized by coupling graphene oxide (GO) on chloromethylated polystyrene through an ethylenediamine spacer unit to develop a column method for the preconcentration/separation of lead prior to its determination by flame atomic absorption spectrometry. It was characterized by Fourier transform infrared spectroscopy, far-infrared spectroscopy, thermogravimetric analysis/differential thermal analysis, scanning electron microscopy, energy-dispersive spectrometry, and transmission electron microscopy. The abundant oxygen-containing surface functional groups form a strong complex with lead, resulting in higher sorption capacity (227.92 mg g(-1)) than other nanosorbents used for sorption studies of the column method. Using the column procedure here is an alternative to the direct use of GO, which restricts irreversible aggregation of GO and its escape into the ecosystem, making it an environmentally sustainable method. The column method was optimized by varying experimental variables such as pH, flow rate for sorption/desorption, and elution condition and was observed to exhibit a high preconcentration factor (400) with a low preconcentration limit (2.5 ppb) and a high degree of tolerance for matrix ions. The accuracy of the proposed method was verified by determining the Pb content in the standard reference materials and by recovery experiments. The method showed good precision with a relative standard deviation <5%. The proposed method was successfully applied for the determination of lead in tap water, electroplating wastewater, river water, and food samples after preconcentration.

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

International Nuclear Information System (INIS)

Jat, J.R.; Balaji Rao, Y.; Subba Rao, Y.

2015-01-01

Nuclear Fuel Complex (NFC) receives Sodium Di-Uranate (SDU) from Uranium Corporation of India Limited (UCIL) for producing sinterable UO 2 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 UO 2 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. HNO 3 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 HNO 3 medium

Room temperature ionic liquids enhanced the speciation of Cr(VI) and Cr(III) by hollow fiber liquid phase microextraction combined with flame atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Zeng, Chujie, E-mail: cjzeng@126.com [Department of Chemistry and Material, Yulin Normal College, Yulin, Guangxi 537000 (China); Lin, Yao; Zhou, Neng; Zheng, Jiaoting; Zhang, Wei [Department of Chemistry and Material, Yulin Normal College, Yulin, Guangxi 537000 (China)

2012-10-30

Highlights: Black-Right-Pointing-Pointer First reported enhancement effect of RTILs in HF-LPME for the speciation of chromium. Black-Right-Pointing-Pointer The addition of RTILs led to 3.5 times improvement of the sensitivity of Cr(VI). Black-Right-Pointing-Pointer The proposed method is a simplicity, sensitivity, low cost, green method. - Abstract: A new method for the speciation of Cr(VI) and Cr(III) based on enhancement effect of room temperature ionic liquids (RTILs) for hollow fiber liquid phase microextraction (HF-LPME) combined with flame atomic absorption spectrometry (FAAS) was developed. Room temperature ionic liquids (RTILs) and diethyldithiocarbamate (DDTC) were used enhancement reagents and chelating reagent, respectively. The addition of room temperature ionic liquids led to 3.5 times improvement in the determination of Cr(VI). In this method, Cr(VI) reacts with DDTC yielding a hydrophobic complex, which is subsequently extracted into the lumen of hollow fiber, whereas Cr(III) is remained in aqueous solutions. The extraction organic phase was injected into FAAS for the determination of Cr(VI). Total Cr concentration was determined after oxidizing Cr(III) to Cr(VI) in the presence of KMnO{sub 4} and using the extraction procedure mentioned above. Cr(III) was calculated by subtracting of Cr(VI) from the total Cr. Under optimized conditions, a detection limit of 0.7 ng mL{sup -1} and an enrichment factor of 175 were achieved. The relative standard deviation (RSD) was 4.9% for Cr(VI) (40 ng mL{sup -1}, n = 5). The proposed method was successfully applied to the speciation of chromium in natural water samples with satisfactory results.

Room temperature ionic liquids enhanced the speciation of Cr(VI) and Cr(III) by hollow fiber liquid phase microextraction combined with flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Zeng, Chujie; Lin, Yao; Zhou, Neng; Zheng, Jiaoting; Zhang, Wei

2012-01-01

Highlights: ► First reported enhancement effect of RTILs in HF-LPME for the speciation of chromium. ► The addition of RTILs led to 3.5 times improvement of the sensitivity of Cr(VI). ► The proposed method is a simplicity, sensitivity, low cost, green method. - Abstract: A new method for the speciation of Cr(VI) and Cr(III) based on enhancement effect of room temperature ionic liquids (RTILs) for hollow fiber liquid phase microextraction (HF-LPME) combined with flame atomic absorption spectrometry (FAAS) was developed. Room temperature ionic liquids (RTILs) and diethyldithiocarbamate (DDTC) were used enhancement reagents and chelating reagent, respectively. The addition of room temperature ionic liquids led to 3.5 times improvement in the determination of Cr(VI). In this method, Cr(VI) reacts with DDTC yielding a hydrophobic complex, which is subsequently extracted into the lumen of hollow fiber, whereas Cr(III) is remained in aqueous solutions. The extraction organic phase was injected into FAAS for the determination of Cr(VI). Total Cr concentration was determined after oxidizing Cr(III) to Cr(VI) in the presence of KMnO 4 and using the extraction procedure mentioned above. Cr(III) was calculated by subtracting of Cr(VI) from the total Cr. Under optimized conditions, a detection limit of 0.7 ng mL −1 and an enrichment factor of 175 were achieved. The relative standard deviation (RSD) was 4.9% for Cr(VI) (40 ng mL −1 , n = 5). The proposed method was successfully applied to the speciation of chromium in natural water samples with satisfactory results.

International comparison of Cd content in a quality control material of Navajuelas (Tagelus dombeii) determined by anodic stripping voltammetry, atomic absorption spectrometry and neutron activation analysis

International Nuclear Information System (INIS)

Queirolo, F.; Forschungszentrum Juelich GmbH; Universidad de Extremadura, Badajoz; Ostapczuk, P.; Valenta, P.; Stegen, S.; Universidad de Extremadura, Badajoz; Marin, C.; Vinagre, F.; Sanchez, A.

1991-01-01

The determination of Cd was performed by neutron activation analysis (NAA), atomic absorption spectrometry (AAS) with flame or in the electrothermal mode and anodic stripping voltammetry in the differential pulse mode (DPASV) and the square wave mode (SWASV). (orig./EF)

Flame atomic absorption spectrometric determination of trace quantities of cadmium in water samples after cloud point extraction in Triton X-114 without added chelating agents

International Nuclear Information System (INIS)

Afkhami, Abbas; Madrakian, Tayyebeh; Siampour, Hajar

2006-01-01

A new micell-mediated phase separation method for preconcentration of ultra-trace quantities of cadmium as a prior step to its determination by flame atomic absorption spectrometry has been developed. The method is based on the cloud point extraction (CPE) of cadmium in iodide media with Triton X-114 in the absence of any chelating agent. The optimal extraction and reaction conditions (e.g., acid concentration, iodide concentration, effect of time) were studied, and the analytical characteristics of the method (e.g., limit of detection, linear range, preconcentration, and improvement factors) were obtained. Linearity was obeyed in the range of 3-300 ng mL -1 of cadmium. The detection limit of the method is 1.0 ng mL -1 of cadmium. The interference effect of some anions and cations was also tested. The method was applied to the determination of cadmium in tap water, waste water, and sea water samples

Speciation of mercury in fish samples by flow injection catalytic cold vapour atomic absorption spectrometry

International Nuclear Information System (INIS)

Zhang Yanlin; Adeloju, Samuel B.

2012-01-01

Highlights: ► Successful speciation of inorganic and organic Hg with Fe 3+ , Cu 2+ and thiourea as catalysts. ► Best sensitivity enhancement and similar sensitivity for MeHg and Hg 2+ with Fe 3+ . ► Successful use of Hg 2+ as the primary standard for quantification of inorganic and total-Hg. ► Quantitative extraction of Hg and MeHg with 2 M HCl which contained thiourea. ► Integration with FIA for rapid analysis with a sample throughput of 180 h −1 . - Abstract: A rapid flow injection catalytic cold vapour atomic absorption spectrometric (FI-CCV-AAS) method is described for speciation and determination of mercury in biological samples. Varying concentrations of NaBH 4 were employed for mercury vapour generation from inorganic and mixture of inorganic and organic (total) Hg. The presence of Fe 3+ , Cu 2+ and thiourea had catalytic effect on mercury vapour generation from methylmercury (MeHg) and, when together, Cu 2+ and thiourea had synergistic catalytic effect on the vapour generation. Of the two metal ions, Fe 3+ gave the best sensitivity enhancement, achieving the same sensitivity for MeHg and inorganic Hg 2+ . Due to similarity of resulting sensitivity, Hg 2+ was used successfully as a primary standard for quantification of inorganic and total Hg. The catalysis was homogeneous in nature, and it was assumed that the breaking of the C-Hg bond was facilitated by the delocalization of the 5d electron pairs in Hg atom. The extraction of MeHg and inorganic mercury (In-Hg) in fish samples were achieved quantitatively with hydrochloric acid in the presence of thiourea and determined by FI-CCV-AAS. The application of the method to the quantification of mercury species in a fish liver reference material DOLT-4 gave 91.5% and 102.3% recoveries for total and methyl mercury, respectively. The use of flow injection enabled rapid analysis with a sample throughput of 180 h −1 .

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

International Nuclear Information System (INIS)

Ghaedi, Mehrorang; Shokrollahi, Ardeshir; Niknam, Khodabakhsh; Niknam, Ebrahim; Najibi, Asma; Soylak, Mustafa

2009-01-01

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 HNO 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 -1 for Cd 2+ , Pb 2+ , Pd 2+ and Ag + along with preconcentration factors of 30 and enrichment factors of 48, 39, 32 and 42 for Cd 2+ , Pb 2+ , Pd 2+ 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.

X-ray absorption in atomic potassium

International Nuclear Information System (INIS)

Gomilsek, Jana Padeznik; Kodre, Alojz; Arcon, Iztok; Nemanic, Vincenc

2008-01-01

A new high-temperature absorption cell for potassium vapor is described. X-ray absorption coefficient of atomic potassium is determined in the energy interval of 600 eV above the K edge where thresholds for simultaneous excitations of 1s and outer electrons, down to [1s2p] excitation, appear. The result represents also the atomic absorption background for XAFS (X-ray absorption fine structure) structure analysis. The K ionization energy in the potassium vapor is determined and compared with theoretical data and with the value for the metal

[Study on lead absorption in pumpkin by atomic absorption spectrophotometry].

Science.gov (United States)

Li, Zhen-Xia; Sun, Yong-Dong; Chen, Bi-Hua; Li, Xin-Zheng

2008-07-01

A study was carried out on the characteristic of lead absorption in pumpkin via atomic absorption spectrophotometer. The results showed that lead absorption amount in pumpkin increased with time, but the absorption rate decreased with time; And the lead absorption amount reached the peak in pH 7. Lead and cadmium have similar characteristic of absorption in pumpkin.

Application of atomic absorption spectrophotometry to determine Cd, Cu, Pb, Zn,...in vegetable samples in Dalat

Energy Technology Data Exchange (ETDEWEB)

Giang, Nguyen; Tam, Nguyen Thanh; Ngoc Trinh, Le Thi; Mai, Truong Phuong; Minh, Nguyen Van [Nuclear Research Institute, Dalat (Viet Nam)

2004-08-01

Nowadays atomic absorption spectrometry has become valuable method for trace element analysis because high specificity; low detection litmus, easy to use; easy sample preparation, low investment and running costs... atomic absorption spectrometry is generally accepted as one the most suitable method for single - element analysis of trace elements in various kinds of materiel. In 2003, we applied flame - atomic absorption spectrometry for analyzing Ca, Cd, Cu, Pb, Zn...in vegetables and their extracted juices were collected form 11 locations of Dalat, including two kinds of vegetables (goods and safety) in both the summer and winter. Average concentration of Ca = 240 mg/kg wet, Cd = 0.035 mg/kg wet, Cu = 0.67 mg/kg wet, Mg = 131 mg/kg wet, Fe = 8.1/kg wet, Mn = 3.1/kg wet, Na = 3266 mg/kg wet, Pb = 0.345 mg/kg wet and Zn = 3.3 mg wet. In their extracted juices: Ca = 89 mg/kg wet, Cd = 0.008 mg/kg wet, Cu = 0.19 mg/kg wet, Mg = 43 mg/kg wet, Fe = 2.3 mg/kg wet, Mn = 0.61 mg/kg wet, Na = 971 mg/kg wet, Pb = 0.107 mg/kg wet and Zn = 0.65 mg/kg wet. (author)

Application of atomic absorption spectrophotometry to determine Cd, Cu, Pb, Zn,...in vegetable samples in Dalat

International Nuclear Information System (INIS)

Nguyen Giang; Nguyen Thanh Tam; Le Thi Ngoc Trinh; Truong Phuong Mai; Nguyen Van Minh

2004-01-01

Nowadays atomic absorption spectrometry has become valuable method for trace element analysis because high specificity; low detection litmus, easy to use; easy sample preparation, low investment and running costs... atomic absorption spectrometry is generally accepted as one the most suitable method for single - element analysis of trace elements in various kinds of materiel. In 2003, we applied flame - atomic absorption spectrometry for analyzing Ca, Cd, Cu, Pb, Zn...in vegetables and their extracted juices were collected form 11 locations of Dalat, including two kinds of vegetables (goods and safety) in both the summer and winter. Average concentration of Ca = 240 mg/kg wet, Cd = 0.035 mg/kg wet, Cu = 0.67 mg/kg wet, Mg = 131 mg/kg wet, Fe = 8.1/kg wet, Mn = 3.1/kg wet, Na = 3266 mg/kg wet, Pb = 0.345 mg/kg wet and Zn = 3.3 mg wet. In their extracted juices: Ca = 89 mg/kg wet, Cd = 0.008 mg/kg wet, Cu = 0.19 mg/kg wet, Mg = 43 mg/kg wet, Fe = 2.3 mg/kg wet, Mn = 0.61 mg/kg wet, Na = 971 mg/kg wet, Pb = 0.107 mg/kg wet and Zn = 0.65 mg/kg wet. (author)

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

International Nuclear Information System (INIS)

Mendil, Durali; Tuzen, Mustafa; Soylak, Mustafa

2008-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

Mendil, Durali; Tuzen, Mustafa [Gaziosmanpasa University, Faculty of Science and Arts, Chemistry Department, 60250 Tokat (Turkey); Soylak, Mustafa [Erciyes University, Faculty of Science and Arts, Chemistry Department, 38039 Kayseri (Turkey)], E-mail: msoylak@gmail.com

2008-04-15

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 {mu}g L{sup -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{sup -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 {mu}g L{sup -1} (cadmium) and 1.60 {mu}g L{sup -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.

Use of slurry sampling for the direct determination of zinc in yogurt by high resolution-continuum source flame atomic absorption spectrometry.

Science.gov (United States)

Brandao, Geovani C; de Jesus, Raildo M; da Silva, Erik G P; Ferreira, Sergio L C

2010-06-15

This paper presents an analytical procedure for the direct determination of zinc in yogurt employing sampling slurry and high resolution-continuum source flame atomic absorption spectrometry (HR-CS FAAS). The step optimization established the experimental conditions of: 2.0molL(-1) hydrochloric acid, a sonication time of 20min and a sample mass of 1.0g for a slurry volume of 25mL. This method allows the determination of zinc with a limit of quantification of 0.32microgg(-1). The precision expressed as relative standard deviation (RSD) were 0.82 and 2.08% for yogurt samples containing zinc concentrations of 4.85 and 2.49microgg(-1), respectively. The accuracy was confirmed by the analysis of a certified reference material of non-fat milk powder furnished by the National Institute of Standard and Technology. The proposed method was applied for the determination of zinc in seven yogurt samples. The zinc content was varied from 2.19 to 4.85microgg(-1). These results agreed with those reported in the literature. The samples were also analyzed after acid digestion and zinc determination by FAAS. No statistical difference was observed between the results obtained by both of the procedures performed.

Application of l-cystine modified zeolite for preconcentration and determination of ultra-trace levels of cadmium by flame atomic absorption spectrometry.

Science.gov (United States)

Rezvani, Seyyed Ahmad; Soleymanpour, Ahmad

2016-03-04

A very convenient, sensitive and precise solid phase extraction (SPE) system was developed for enrichment and determination of ultra-trace of cadmium ion in water and plant samples. This method was based on the retention of cadmium(II) ions by l-cystine adsorbed in Y-zeolite and carry out in a packed mini-column. The retained cadmium ions then were eluted and determined by flame atomic absorption spectrometry. The scanning electron microscopy (SEM), powder X-ray diffraction (XRD) and Fourier Transform Infrared (FT-IR) spectroscopy techniques were applied for the characterization of cystine modified zeolite (CMZ). Some experimental conditions affecting the analytical performance such as pH, eluent type, concentration of sample, eluent flow rate and also the presence of interfering ions were investigated. The calibration graph was linear within the range of 0.1-7.5ngmL(-1) and limit of detection was obtained 0.04ngmL(-1) with the preconcentration factor of 400. The relative standard deviation (RSD) was obtained 1.4%, indicating the excellent reproducibility of this method. The proposed method was successfully applied for the extraction and determination of cadmium(II) ion in black tea, cigarette's tobacco and also various water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

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

Energy Technology Data Exchange (ETDEWEB)

Fara, M.; Novak, F. [EGU Prague, PLC, Bichovice, Prague (Czechoslovakia)

1995-12-01

Both flame and electrothermal methods of atomic absorption spectroscopy (AAS) have been applied to the determination of Al, As, Be, Ca, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, TI, Se, V and Zn in emission and emission (deposition) samples decomposed in open PTFE test-tubes by individual fuming-off hydrofluoric, perchloroic and nitric acid. An alternative hydride technique was also used for As and Se determination and Hg was determined using a self-contained AAS analyzer. A graphite platform proved good to overcome non-spectral interferences in AAS-ETA. Methods developed were verified by reference materials (inc. NBS 1633a).

Synthesize of silver-nanoparticles by plant extract and its application for preconcentration of cadmium followed by flame atomic absorption spectrometry.

Science.gov (United States)

Almertaha, Abdul-Hossein; Eftekhari, Mohammad; Chamsaz, Mahmoud; Gheibi, Mohammad

2018-02-02

In this paper, Mentha pulegium leaves extract was used as a green reducing agent for the synthesis of silver-nanoparticles. The synthesized silver-nanoparticles were characterized by UV-VIS spectrophotometry, transmission electron microscopy, X-ray spectroscopy and used as an adsorbent for preconcentration of trace levels of cadmium (ІІ). After the desorption of cadmium (ІІ) in 5 mol L -1 formic acid, the desorbent solution was aspirated into the flame atomic absorption spectrometry for the determination of cadmium. In order to optimize the experimental condition, a response surface methodology based on central composite design was used. The optimum conditions are: pH: 8.6, amounts of adsorbent: 30 mg, 10 min extraction time and desorption time of 2 min. Under the optimum condition, the calibration curve was linear in the range of 5-200 μg L -1 cadmium (ІІ) ion with a correlation coefficient of 0.9995. The limit of detection was 1.1 μg L -1 and the relative standard deviation for 25 μg L -1 cadmium (ІІ) ion was 3.0% (n = 5). In order to check the applicability of the proposed method, different real samples were analyzed. Also, the accuracy of this method was successfully checked by the analysis of certified reference material and spike tests.

Determination of trace amounts of tin in geological materials by atomic absorption spectrometry

Science.gov (United States)

Welsch, E.P.; Chao, T.T.

1976-01-01

An atomic absorption method is described for the determination of traces of tin in rocks, soils, and stream sediments. A dried mixture of the sample and ammonium iodide is heated to volatilize tin tetraiodide -which is then dissolved in 5 % hydrochloric acid, extracted into TOPO-MIBK, and aspirated into a nitrous oxide-acetylene flame. The limit of determination is 2 p.p.m. tin and the relative standard deviation ranges from 2 to 14 %. Up to 20 % iron and 1000 p.p.m. Cu, Pb, Zn, Mn, Hg, Mo, V, or W in the sample do not interfere. As many as 50 samples can be easily analyzed per man-day. ?? 1976.

Application of the correction's system of bottom by deuterium's lamp of a spectrophotometer of atomic absorption to the obtaining of ultraviolet spectrums

International Nuclear Information System (INIS)

Villalobos Chaves, Alberto Enrique

2002-01-01

The correction system of bottom by lamp of deuterium's arch of a spectrophotometer of atomic absorption has been utilized with sweep's capacity of wavelength to get spectrums of ultraviolet absorption of samples in gaseous phase, whether in presence as in absence of flame, in the region between 200 nm and 365 nm. The spectral information was obtained after of a process of electronic subtraction of the source's signal, except for the source's signal plus the sample and its subsequent analysis by a programmed data's processor to give a report in terms of wavelength. The spectrums obtained in absence of flame were practiced in samples contained in a gas's sell for infrared spectroscopy with polyethylene's windows, it is located of the burner and directly in front to the radiation's beam, comparable spectrums with the reported in the literature were obtained and with a bigger resolution than the measure with an conventional ultraviolet absorption's spectrophotometer utilized like reference. The spectrums in presence of flame have been of flame have been obtained from dissolved samples and directly suctioned, it achieves to obtain spectral information that is normally not detected conveniently when it performs qualitative analysis by emission of flame in elements such like zinc, lead, cobalt, mercury and nickel among other. The information obtained on this way has been utilized like an alternative method to the elemental analysis by humid way with a view to increase the reliability of the results that have been utilized like basis in the determination of the tariff classification of imported or exported products. (Author) [es

Preconcentration of gold ions from water samples by modified organo-nanoclay sorbent prior to flame atomic absorption spectrometry determination

Energy Technology Data Exchange (ETDEWEB)

Afzali, Daryoush, E-mail: daryoush_afzali@yahoo.com [Nanochemistry Department, Research Institute of Environmental Sciences, International Center for Science, High Technology and Environmental Sciences, Kerman (Iran, Islamic Republic of); Mostafavi, Ali [Chemistry Department, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Mirzaei, Mohammad [Nanochemistry Department, Research Institute of Environmental Sciences, International Center for Science, High Technology and Environmental Sciences, Kerman (Iran, Islamic Republic of); Chemistry Department, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of)

2010-09-15

In this work, the applicability of modified organo nanoclay as a new and easy prepared solid sorbent for the preconcentration of trace amounts of Au(III) ion from water samples is studied. The organo nanoclay was modified with 5-(4'-dimethylamino benzyliden)-rhodanine and used as a sorbent for separation of Au(III) ions. The sorption of gold ions was quantitative in the pH range of 2.0-6.0. Quantitative desorption occurred with 6.0 mL of 1.0 mol L{sup -1} Na{sub 2}S{sub 2}O{sub 3}. The amount of eluted Au(III) was measured using flame atomic absorption spectrometry. In the initial solution the linear dynamic range was in the range of 0.45 ng mL{sup -1} to 10.0 {mu}g mL{sup -1}, the detection limit was 0.1 ng mL{sup -1} and the preconcentration factor was 105. Also, the relative standard deviation was {+-}2.3% (n = 8 and C = 2.0 {mu}g mL{sup -1}) and the maximum capacity of the sorbent was 3.9 mg of Au(III) per gram of modified organo nanoclay. The influences of the experimental parameters including sample pH, eluent volume and eluent type, sample volume, and interference of some ions on the recoveries of the gold ion were investigated. The proposed method was applied for preconcentration and determination of gold in different samples.

Influence of soil composition in the determination of chromium by atomic absorption spectrometry with flame air / acetylene; Influencia de la composicion del suelo en la determinacion de cromo por espectrometria de absorcion atomica con llama aire/acetileno

Energy Technology Data Exchange (ETDEWEB)

Duran Sosa, Ibis; Granda Valdes, Mayra [Departamento de Quimica Analitica, Facultad de Quimica, Universidad de La Habana, La Habana (Cuba); Pomares Alfonso, Mario Simeon, E-mail: mpomares@imre.oc.uh.cu [Instituto de Ciencias y Tecnologia de Materiales, Universidad de La Habana, La Habana (Cuba)

2014-07-01

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.

Determination of tellurium in lead and lead alloy using flow injection-hydride generation atomic absorption spectrometry

International Nuclear Information System (INIS)

Mesko, Marcia F.; Pozebon, Dirce; Flores, Erico M.M.; Dressler, Valderi L.

2004-01-01

A method based on flow injection-hydride generation atomic absorption spectrometry (FI-HG AAS) for the determination of trace amount of Te in lead and lead alloy is described. A flow injection system (FI) and related analytical parameters as well as Te determination and interference caused by Pb, Bi and Ag on Te were investigated. The Pb interference could be overcome by using a small sample volume, while the Bi interference could be overcome by thiourea. However, it was not possible to minimise the interference caused by Ag on Te. The optimised conditions for Te determination in the analysed samples were: 6 mol l -1 HCl as sample carrier solution, 0.75% (m/v) sodium tetrahydroborate as Te reductant, 40 μl of sample solution, and 200 ml min -1 Ar flow rate as carrier gas. The limit of quantification (LOQ) was 1.0 μg g -1 Te (using 250 mg of sample in 50 ml final solution), the limit of detection (LOD) was 2.5 μg l -1 and the relative standard deviation (RSD) was 6% for five consecutive measurements of sample solution. The standard addition calibration method was used. Relatively high sample throughput (ca. 45 sample runs can be performed in a working hour), reduced sample manipulation since matrix separation is not necessary, and minor waste generation are the main advantages of the proposed method for Te determination by FI-HG AAS

The use of atomic absorption spectroscopy to measure arsenic, selenium, molybdenum, and vanadium in water and soil samples from uranium mill tailings sites

International Nuclear Information System (INIS)

Hollenbach, M.H.

1988-01-01

The Technical Measurements Center (TMC) was established to support the environmental measurement needs of the various DOE remedial action programs. A laboratory intercomparison study conducted by the TMC, using soil and water samples from sites contaminated by uranium mill tailings, indicated large discrepancies in analytical results reported by participating laboratories for arsenic, selenium, molybdenum, and vanadium. The present study was undertaken to investigate the most commonly used analytical techniques for measuring these four elements, ascertain routine and reliable quantification, and assess problems and successes of analysts. Based on a survey of the technical literature, the analytical technique of atomic absorption spectroscopy was selected for detailed study. The application of flame atomic absorption, graphite furnace atomic absorption, and hydride generation atomic absorption to the analysis of tailings-contaminated samples is discussed. Additionally, laboratory sample preparation methods for atomic absorption spectroscopy are presented. The conclusion of this report is that atomic absorption can be used effectively for the determination of arsenic, selenium, molybdenum, and vanadium in water and soil samples if the analyst understands the measurement process and is aware of potential problems. The problem of accurate quantification of arsenic, selenium, molybdenum, and vanadium in water and soil contaminated by waste products from uranium milling operations affects all DOE remedial action programs [Surplus Facilities Management Program (SFMP), Formerly Utilized Site Remedial Action Program (FUSRAP), and Uranium Mill Tailings Remedial Action Program (UMTRAP)], since all include sites where uranium was processed. 96 refs., 9 figs

Atomic absorption spectrometry using tungsten and molybdenum tubes as metal atomizer

International Nuclear Information System (INIS)

Kaneco, Satoshi; Katsumata, Hideyuki; Ohta, Kiyohisa; Suzuki, Tohru

2007-01-01

We have developed a metal tube atomizer for the electrothermal atomization atomic absorption spectrometry (ETA-AAS). Tungsten, molybdenum, platinum tube atomizers were used as the metal atomizer for ETA-AAS. The atomization characteristics of various metals using these metal tube atomizers were investigated. The effects of heating rate of atomizer, atomization temperature, pyrolysis temperature, argon purge gas flow rate and hydrogen addition on the atomic absorption signal were investigated for the evaluation of atomization characteristics. Moreover, ETA-AAS with metal tube atomizer has been combined with the slurry-sampling techniques. Ultrasonic slurry-sampling ETA-AAS with metal tube atomizer were effective for the determination of trace metal elements in biological materials, calcium drug samples, herbal medicine samples, vegetable samples and fish samples. Furthermore, a preconcentration method of trace metals involving adsorption on a metal wire has been applied to ETA-AAS with metal tube atomizer. (author)

A Green Preconcentration Method for Determination of Cobalt and Lead in Fresh Surface and Waste Water Samples Prior to Flame Atomic Absorption Spectrometry

Directory of Open Access Journals (Sweden)

Naeemullah

2012-01-01

Full Text Available Cloud point extraction (CPE has been used for the preconcentration and simultaneous determination of cobalt (Co and lead (Pb in fresh and wastewater samples. The extraction of analytes from aqueous samples was performed in the presence of 8-hydroxyquinoline (oxine as a chelating agent and Triton X-114 as a nonionic surfactant. Experiments were conducted to assess the effect of different chemical variables such as pH, amounts of reagents (oxine and Triton X-114, temperature, incubation time, and sample volume. After phase separation, based on the cloud point, the surfactant-rich phase was diluted with acidic ethanol prior to its analysis by the flame atomic absorption spectrometry (FAAS. The enhancement factors 70 and 50 with detection limits of 0.26 μg L−1 and 0.44 μg L−1 were obtained for Co and Pb, respectively. In order to validate the developed method, a certified reference material (SRM 1643e was analyzed and the determined values obtained were in a good agreement with the certified values. The proposed method was applied successfully to the determination of Co and Pb in a fresh surface and waste water sample.

Determination of gold in copper-bearing sulphide ores and metallurgical flotation products by atomic-absorption spectrometry.

Science.gov (United States)

Strong, B; Murray-Smith, R

1974-12-01

A method is described which is specific for the determination of gold in sulphide copper ores and concentrates. Direct decomposition with aqua regia was found to be incomplete. A carefully controlled roasting stage followed by treatment with hydrochloric acid and then aqua regia was effective for dissolving all the gold. The gold is extracted into 4-methylpentan-2-one (methyli-sobutylketone) then aspirated into a very lean air-acetylene flame and the gold determined by atomic-absorption spectrometry. No interferences were observed from large concentrations of copper, iron or nickel.

Mechanism of selenium hydride atomization, fate of free atoms and temperature distribution in an argon shielded, highly fuel-rich, hydrogen-oxygen diffusion micro-flame studied by atomic absorption spectrometry

Czech Academy of Sciences Publication Activity Database

D'Ulivo, A.; Dědina, Jiří; Lampugnani, L.; Matoušek, Tomáš

2002-01-01

Roč. 17, č. 3 (2002), s. 253-257 ISSN 0267-9477 R&D Projects: GA ČR GA203/01/0453; GA ČR GA203/98/0754 Institutional research plan: CEZ:AV0Z4031919 Keywords : hydride atomization * hydride generation * atomic absorption spectrometry Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.250, year: 2002

The application of atomic absorption spectrometry to chemical analysis

International Nuclear Information System (INIS)

Walsh, A.

1980-01-01

YhThe history of the development of atomic absorption methods of elemental analysis is outlined. The theoretical basis of atomic absorption methods is discussed and the principle of modern methods of atomic absorption measurements is described. The advantages, scope and limations of these methods are discussed. Related methods based on the measurement of atomic fluorescence are also described

Evaluation of a novel PTFE material for use as a means for separation and preconcentration of trace levels of metal ions in sequential injection (SI) and sequential injection lab-on-valve (SI-LOV) systems. Determination of cadmium (II) with detection by electrothermal atomic absorption spectrometry

DEFF Research Database (Denmark)

Long, Xiangbao; Chomchoei, Roongrat; Hansen, Elo Harald

2004-01-01

with an external packed column and in a sequential injection lab-on-valve (SI-LOV) system. Employed for the determination of cadmium(II), complexed with diethyldithiophosphate (DDPA), and detection by electrothermal atomic absorption spectrometry (ETAAS), its performance was compared to that of a previously used...

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

International Nuclear Information System (INIS)

Shokri, Masood; Beiraghi, Asadollah; Seidi, Shahram

2015-01-01

For the first time, a simple and efficient in situ emulsification microextraction method using a dicationic ionic liquid followed by magnetic assisted physisorption was presented to determine trace amounts of lead. In this method, 400 μL of 1.0 mol L −1 lithium bis (trifluoromethylsulfonyl) imide aqueous solution, Li[NTf 2 ], was added into the sample solution containing 100 μL of 1.0 mol L −1 1,3-(propyl-1,3-diyl) bis (3-methylimidazolium) chloride, [pbmim]Cl 2 , to form a water immiscible ionic liquid, [pbmim][NTf 2 ] 2 . This new in situ formed dicationic ionic liquid was applied as the acceptor phase to extract the lead-ammonium pyrrolidinedithiocarbamate (Pb-APDC) complexes from the sample solution. Subsequently, 30 mg of Fe 3 O 4 magnetic nanoparticles (MNPs) were added into the sample solution to collect the fine droplets of [pbmim][NTf 2 ] 2 , physisorptively. Finally, MNPs were eluted by acetonitrile, separated by an external magnetic field and the obtained eluent was subjected to micro-sampling flame atomic absorption spectrometry (FAAS) for further analysis. Comparing with other microextraction methods, no special devices and centrifugation step are required. Parameters influencing the extraction efficiency such as extraction time, pH, concentration of chelating agent, amount of MNPs and coexisting interferences were studied. Under the optimized conditions, this method showed high extraction recovery of 93% with low LOD of 0.7 μg L −1 . Good linearity was obtained in the range of 2.5–150 μg L −1 with determination coefficient (r 2 ) of 0.9921. Relative standard deviation (RSD%) for seven repeated measurements at the concentration of 10 μg L −1 was 4.1%. Finally, this method was successfully applied for determination of lead in some water and plant samples. - Highlights: • A dicationic ionic liquid was used as the extraction solvent, for the first time. • A simple and efficient in situ emulsification microextraction

Flame Structure and Emissions of Strongly-Pulsed Turbulent Diffusion Flames with Swirl

Science.gov (United States)

Liao, Ying-Hao

This work studies the turbulent flame structure, the reaction-zone structure and the exhaust emissions of strongly-pulsed, non-premixed flames with co-flow swirl. The fuel injection is controlled by strongly-pulsing the fuel flow by a fast-response solenoid valve such that the fuel flow is completely shut off between pulses. This control strategy allows the fuel injection to be controlled over a wide range of operating conditions, allowing the flame structure to range from isolated fully-modulated puffs to interacting puffs to steady flames. The swirl level is controlled by varying the ratio of the volumetric flow rate of the tangential air to that of the axial air. For strongly-pulsed flames, both with and without swirl, the flame geometry is strongly impacted by the injection time. Flames appear to exhibit compact, puff-like structures for short injection times, while elongated flames, similar in behaviors to steady flames, occur for long injection times. The flames with swirl are found to be shorter for the same fuel injection conditions. The separation/interaction level between flame puffs in these flames is essentially governed by the jet-off time. The separation between flame puffs decreases as swirl is imposed, consistent with the decrease in flame puff celerity due to swirl. The decreased flame length and flame puff celerity are consistent with an increased rate of air entrainment due to swirl. The highest levels of CO emissions are generally found for compact, isolated flame puffs, consistent with the rapid quenching due to rapid dilution with excess air. The imposition of swirl generally results in a decrease in CO levels, suggesting more rapid and complete fuel/air mixing by imposing swirl in the co-flow stream. The levels of NO emissions for most cases are generally below the steady-flame value. The NO levels become comparable to the steady-flame value for sufficiently short jet-off time. The swirled co-flow air can, in some cases, increase the NO

Development of a Simple System for the Determination of Arsenic ...

African Journals Online (AJOL)

injected such that the excess molecular hydrogen evolved carries the generated arsine directly through the atomic absorption spectrophotometer nebuliser to a nitrogen-hydrogen entrained air flame for atomic absorption measurement is described. The average ... Gas flow rates affected sensitivity markedly, but the

Speciation of mercury in fish samples by flow injection catalytic cold vapour atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Zhang Yanlin [NanoScience and Sensor Technology Research Group, School of Applied Sciences and Engineering, Monash University, Churchill, Victoria 3842 (Australia); Adeloju, Samuel B., E-mail: Sam.Adeloju@monash.edu [NanoScience and Sensor Technology Research Group, School of Applied Sciences and Engineering, Monash University, Churchill, Victoria 3842 (Australia)

2012-04-06

Highlights: Black-Right-Pointing-Pointer Successful speciation of inorganic and organic Hg with Fe{sup 3+}, Cu{sup 2+} and thiourea as catalysts. Black-Right-Pointing-Pointer Best sensitivity enhancement and similar sensitivity for MeHg and Hg{sup 2+} with Fe{sup 3+}. Black-Right-Pointing-Pointer Successful use of Hg{sup 2+} as the primary standard for quantification of inorganic and total-Hg. Black-Right-Pointing-Pointer Quantitative extraction of Hg and MeHg with 2 M HCl which contained thiourea. Black-Right-Pointing-Pointer Integration with FIA for rapid analysis with a sample throughput of 180 h{sup -1}. - Abstract: A rapid flow injection catalytic cold vapour atomic absorption spectrometric (FI-CCV-AAS) method is described for speciation and determination of mercury in biological samples. Varying concentrations of NaBH{sub 4} were employed for mercury vapour generation from inorganic and mixture of inorganic and organic (total) Hg. The presence of Fe{sup 3+}, Cu{sup 2+} and thiourea had catalytic effect on mercury vapour generation from methylmercury (MeHg) and, when together, Cu{sup 2+} and thiourea had synergistic catalytic effect on the vapour generation. Of the two metal ions, Fe{sup 3+} gave the best sensitivity enhancement, achieving the same sensitivity for MeHg and inorganic Hg{sup 2+}. Due to similarity of resulting sensitivity, Hg{sup 2+} was used successfully as a primary standard for quantification of inorganic and total Hg. The catalysis was homogeneous in nature, and it was assumed that the breaking of the C-Hg bond was facilitated by the delocalization of the 5d electron pairs in Hg atom. The extraction of MeHg and inorganic mercury (In-Hg) in fish samples were achieved quantitatively with hydrochloric acid in the presence of thiourea and determined by FI-CCV-AAS. The application of the method to the quantification of mercury species in a fish liver reference material DOLT-4 gave 91.5% and 102.3% recoveries for total and methyl mercury

Sequential determination of arsenic, selenium, antimony, and tellurium in foods via rapid hydride evolution and atomic absorption spectrometry

International Nuclear Information System (INIS)

Fiorino, J.A.; Jones, J.W.; Capar, S.G.

1976-01-01

Analysis of acid digests of foods for As, Se, Sb, and Te was semiautomated. Hydrides generated by controlled addition of base stabilized NaBH 4 solution to acid digests are transported directly into a shielded, hydrogen (nitrogen diluted), entrained-air flame for atomic absorption spectrophotometric determination of the individual elements. The detection limits, based on 1 g of digested sample, are approximately 10 to 20 ng/g for all four elements. Measurement precision is 1 to 2 percent relative standard deviation for each element measured at 0.10 μg. A comparison is made of results of analysis of lyophilized fish tissues for As and Se by instrumental neutron activation (INAA), hydride generation with atomic absorption spectrometry, fluorometry, and spectrophotometry. NBS standard reference materials (orchard leaves and bovine liver) analyzed for As, Se, and Sb by this method show excellent agreement with certified values and with independent NAA values

A novel separation/preconcentration technique based on ultrasonic dispersion liquid-liquid microextraction for determination of trace cobalt by flame atomic absorption spectrometry

Directory of Open Access Journals (Sweden)

Jingci Li

2012-12-01

Full Text Available An improved method for the determination of trace cobalt in water samples has been developed using ultrasonic dispersion liquid-liquid microextraction (US-DLLME prior to flame atomic absorption spectrometry (FAAS analysis. In this method, cobalt was extracted into the fine droplets of carbon tetrachloride after chelate formation with the water soluble ligand, ammonium pyrrolidine dithiocarbamate (APDC. The fine droplets of carbon tetrachloride were formed and dispersed in the aqueous sample with the help of ultrasonic waves which accelerated the formation of the fine cloudy solution without using disperser solvents. Under optimum conditions, the calibration curve was linear in the range of 2.5-500 μg L-1, with a detection limit of 0.8 μg L-1. The relative standard deviation (RSD for ten replicate measurements of 20 and 500 μg L-1 of cobalt were 3.3 and 2.2%. This proposed method was successfully applied to tap water, river water, and sea water, and accuracy was assessed through the analysis of certified reference water or recovery experiments. Operation simplicity, low cost, high enrichment factor, and low consumption of the extraction solvent are the main advantages of the proposed method.DOI: http://dx.doi.org/10.4314/bcse.v26i1.2

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

Energy Technology Data Exchange (ETDEWEB)

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.

On-line preconcentration system using a minicolumn of polyurethane foam loaded with Me-BTABr for zinc determination by Flame Atomic Absorption Spectrometry

International Nuclear Information System (INIS)

Azevedo Lemos, Valfredo; Nei Lopes dos Santos, Walter; Silva Santos, Juracir; Bezerra de Carvalho, Marcilio

2003-01-01

In the present paper, an on-line system for preconcentration and determination of zinc by Flame Atomic Absorption Spectrometry (FAAS) is proposed. It is based in the sorption of zinc(II) ions on a minicolumn packed with polyurethane foam loaded with 2-[2'-(6-methyl-benzothiazolylazo)]-4-bromophenol (Me-BTABr) reagent. Chemical and flow variables as pH effect, sample flow rate and eluent concentration were optimized using univariate methodology. The results demonstrated that zinc can determinate using the sample pH in the range of 6.5-9.2, sample flow rate of 6.0 ml min -1 , and the elution step using 0.10 mol l -1 hydrochloric acid solution at flow rate of 5.5 ml min -1 . In these conditions, an enrichment factor of 23 and a sampling rate of 48 samples per hour were achieved. The detection limit (DL, 3σ) as IUPAC recommendation was 0.37 μg l -1 and the precision (assessed as the relative standard deviation, R.S.D.) reached values of 5.9-1.8% in zinc solutions of 1.0-10.0 μg l -1 concentration, respectively. The method was successfully applied to the determination of trace amounts of zinc in natural water samples from Salvador (Brazil)

Methane Formation by Flame-Generated Hydrogen Atoms in the Flame Ionization Detector

DEFF Research Database (Denmark)

Holm, Torkil; Madsen, Jørgen Øgaard

1996-01-01

, and conceivably all hydrocarbons are quantitatively converted into methane at temperatures below 600 C, that is, before the proper combustion has started. The splitting of the C-C bonds is preceded by hydrogenation of double and triple bonds and aromatic rings. The reactions, no doubt, are caused by hydrogen...... atoms, which are formed in the burning hydrogen and which diffuse into the inner core of the flame. The quantitative formation of methane appears to explain the "equal per carbon" rule for the detector response of hydrocarbons, since all carbons are "exchanged" for methane molecules....

Normal blood magnesium levels in volunteers of Rawalpindi by atomic absorption absorption technique

International Nuclear Information System (INIS)

Ahmed, I.; Rehman, S.; Yawar, W.; Rusheed, A.; Ahraf, M.; Syed, N.H.

1999-01-01

Magnesium levels in whole blood samples of 67 healthy volunteers (mean 6.46 -+ 0.221; range 1.345 - 13.163 mg/dL) of Rawalpindi district have been determined by flame atomic absorption spectrophotometric method. Magnesium levels of 41 male and 26 female subjects including doctors, nurses, patients attendees, medical students, sweepers and peons of Rawalpindi Medical College and Rawalpindi General Hospital revealed the normal mean blood levels of 6.088 - + 0.258 mg/dL (range 1.345 - 10.679 mg/dL)and 7.060 -+ 0.375 mg/dL (range 4.495 - 13.163 mg/dL),P<0.05 respectively. Only 10 male volunteers were smokers exhibiting 6.768 -+ 0.558 mg/dL (range 4.466 -10.679 mg/dL). Significant relationship was found in magnesium levels between males and females of poor socio-economic group (P<0.05). No relationship occurred between male smokers and non-smokers and magnesium levels in the age groups of males or females or both, when data was compared by 't' test. (author)

Contribution to diagnostics/prognostics of tuberculosis in children. I. New methods of assaying zinc and simultaneously copper and zinc in diluted sera by flame atomic-absorption spectrometry

Directory of Open Access Journals (Sweden)

Luterotti Svjetlana

2015-09-01

Full Text Available In an attempt to provide a reliable status of metal ions in children, new methods of analysis of children’s sera are proposed. New flame atomic-absorption spectrometric (FAAS methods are simple, cost- and time-effective and, above all, labor-, reagent- and sample-saving. Two methods were suggested: method A for simultaneous determination of Cu and Zn from 5-fold diluted sera, and method B, for assaying zinc alone in 10-fold diluted samples. Both methods are based on a single-step sample pretreatment (deproteinization with 3 mol dm–3 HCl. Method A uses a single-step calibration with a mixed standard. The main advantage of method B is an additional reduction in sample consumption. Both methods were fully validated against reference methods. Accuracy, sensitivity and precision have proven them to be comparable to the reference methods in terms of analytical performance, and applicable to analyses of children’s sera.

Solid-phase extraction of Mn(II), Co(II), Ni(II), Cu(II), Cd(II) and Pb(II) ions from environmental samples by flame atomic absorption spectrometry (FAAS)

Energy Technology Data Exchange (ETDEWEB)

Duran, Celal [Department of Chemistry, Faculty of Art and Science, Karadeniz Technical University, 61080 Trabzon (Turkey); Gundogdu, Ali [Department of Chemistry, Faculty of Art and Science, Karadeniz Technical University, 61080 Trabzon (Turkey); Bulut, Volkan Numan [Department of Chemistry, Giresun Faculty of Art and Science, Karadeniz Technical University, 28049 Giresun (Turkey); Soylak, Mustafa [Department of Chemistry, Faculty of Art and Science, Erciyes University, 38039 Kayseri (Turkey)]. E-mail: soylak@erciyes.edu.tr; Elci, Latif [Department of Chemistry, Faculty of Art and Science, Pamukkale University, 20020 Denizli (Turkey); Sentuerk, Hasan Basri [Department of Chemistry, Faculty of Art and Science, Karadeniz Technical University, 61080 Trabzon (Turkey); Tuefekci, Mehmet [Department of Chemistry, Faculty of Art and Science, Karadeniz Technical University, 61080 Trabzon (Turkey)

2007-07-19

A new method using a column packed with Amberlite XAD-2010 resin as a solid-phase extractant has been developed for the multi-element preconcentration of Mn(II), Co(II), Ni(II), Cu(II), Cd(II), and Pb(II) ions based on their complex formation with the sodium diethyldithiocarbamate (Na-DDTC) prior to flame atomic absorption spectrometric (FAAS) determinations. Metal complexes sorbed on the resin were eluted by 1 mol L{sup -1} HNO{sub 3} in acetone. Effects of the analytical conditions over the preconcentration yields of the metal ions, such as pH, quantity of Na-DDTC, eluent type, sample volume and flow rate, foreign ions etc. have been investigated. The limits of detection (LOD) of the analytes were found in the range 0.08-0.26 {mu}g L{sup -1}. The method was validated by analyzing three certified reference materials. The method has been applied for the determination of trace elements in some environmental samples.

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

International Nuclear Information System (INIS)

Balaes, G.E.E.; Robert, R.V.D.

1981-01-01

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

Behavioral Characteristics of the Non-Premixed Methane-Air Flame Oppositely Injected in a Narrow Channel

International Nuclear Information System (INIS)

Yun, Young Min; Lee, Min Jung; Cho, Sang Moon; Kim, Nam Il

2009-01-01

Characteristics of a counter flowing diffusion flame, which is formulated by an oppositely-injected methane-jet flow in a narrow channel of a uniform air flow. The location of the flame fronts and the flame lengths were compared by changing the flow rates of fuel. To distinguish the effects of the narrow channel on the diffusion flame, a numerical simulation for an ideal two-dimensional flame was conducted. Overall trends of the flame behavior were similar in both numerical and experimental results. With the increase of the ratio of jet velocity to air velocity flame front moved farther upstream. It is thought that the flow re-direction in the channel suppresses fuel momentum more significantly due to the higher temperature and increased viscosity of burned gas. Actual flames in a narrow channel suffer heat loss to the ambient and it has finite length of diffusion flame in contrast to the numerical results of infinite flame length. Thus a convective heat loss was additionally employed in numerical simulation and closer results were obtained. These results can be used as basic data in development of a small combustor of a nonpremixed flame

Behavioral Characteristics of the Non-Premixed Methane-Air Flame Oppositely Injected in a Narrow Channel

Energy Technology Data Exchange (ETDEWEB)

Yun, Young Min; Lee, Min Jung; Cho, Sang Moon; Kim, Nam Il [Chungang University, Seoul (Korea, Republic of)

2009-04-15

Characteristics of a counter flowing diffusion flame, which is formulated by an oppositely-injected methane-jet flow in a narrow channel of a uniform air flow. The location of the flame fronts and the flame lengths were compared by changing the flow rates of fuel. To distinguish the effects of the narrow channel on the diffusion flame, a numerical simulation for an ideal two-dimensional flame was conducted. Overall trends of the flame behavior were similar in both numerical and experimental results. With the increase of the ratio of jet velocity to air velocity flame front moved farther upstream. It is thought that the flow re-direction in the channel suppresses fuel momentum more significantly due to the higher temperature and increased viscosity of burned gas. Actual flames in a narrow channel suffer heat loss to the ambient and it has finite length of diffusion flame in contrast to the numerical results of infinite flame length. Thus a convective heat loss was additionally employed in numerical simulation and closer results were obtained. These results can be used as basic data in development of a small combustor of a nonpremixed flame.

Determination of gold, indium, tellurium and thallium in the same sample digest of geological materials by atomic-absorption spectroscopy and two-step solvent extraction

Science.gov (United States)

Hubert, A.E.; Chao, T.T.

1985-01-01

A rock, soil, or stream-sediment sample is decomposed with hydrofluoric acid, aqua regia, and hydrobromic acid-bromine solution. Gold, thallium, indium and tellurium are separated and concentrated from the sample digest by a two-step MIBK extraction at two concentrations of hydrobromic add. Gold and thallium are first extracted from 0.1M hydrobromic acid medium, then indium and tellurium are extracted from 3M hydrobromic acid in the presence of ascorbic acid to eliminate iron interference. The elements are then determined by flame atomic-absorption spectrophotometry. The two-step solvent extraction can also be used in conjunction with electrothermal atomic-absorption methods to lower the detection limits for all four metals in geological materials. ?? 1985.

Zeeman atomic absorption spectrometry

International Nuclear Information System (INIS)

Hadeishi, T.; McLaughlin, R.

1978-08-01

The design and development of a Zeeman atomic absorption spectrometer for trace element analysis are described. An instruction manual is included which details the operation, adjustment, and maintenance. Specifications and circuit diagrams are given

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

DEFF Research Database (Denmark)

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...

Determination of metallic elements in water by the combined preconcentration techniques of ion exchange and atomic absorption spectrophotometry

International Nuclear Information System (INIS)

Paula, M.H. de.

1981-01-01

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 60 Co 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) [pt

Determination of lead at trace levels in mussel and sea water samples using vortex assisted dispersive liquid-liquid microextraction-slotted quartz tube-flame atomic absorption spectrometry.

Science.gov (United States)

Erarpat, Sezin; Özzeybek, Gözde; Chormey, Dotse Selali; Bakırdere, Sezgin

2017-12-01

In this study, dispersive liquid-liquid microextraction (DLLME) and slotted quartz tube (SQT) were coupled to flame atomic absorption spectrometry (FAAS) to increase the sensitivity of lead. Conditions such as the formation of the lead-dithizone complex, efficiency of the DLLME method and the output of the SQT were systematically optimized to improve the detection limit for the analyte. The conventional FAAS system was improved upon by about 3.0 times with SQT-FAAS, 32 times with DLLME-FAAS and 142 times with DLLME-SQT-FAAS. The method was applicable over a wide linear range (10-500 μg L -1 ). The limit of detection (LOD) determined by DLLME-SQT-FAAS for seawater and mussel were 2.7 μg L -1 and 270 μg kg -1 , respectively. The percent recoveries obtained for mussel and seawater samples (spiked at 20 and 50 μg L -1 ) were 95-96% and 98-110%, respectively. Copyright © 2017 Elsevier Ltd. All rights reserved.

Determination of trace amounts of selenium in minerals and rocks by flame less atomic-absorption spectrometry

International Nuclear Information System (INIS)

Alduan, F. A.; Capdevilla, C.

1980-01-01

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

Influence of Steam Injection and Water-in-Oil Emulsions on Diesel Fuel Combustion Performance

Science.gov (United States)

Sung, Meagan

Water injection can be an effective strategy for reducing NOx because water's high specific heat allows it to absorb heat and lower system temperatures. Introducing water as an emulsion can potentially be more effective at reducing emissions than steam injection due to physical properties (such as microexplosions) that can improve atomization and increase mixing. Unfortunately, the immiscibility of emulsions makes them difficult to work with so they must be mixed properly. In this effort, a method for adequately mixing surfactant-free emulsions was established and verified using high speed cinematography. As the water to fuel mass ratio (W/F) increased, emulsion atomization tests showed little change in droplet size and spray angle, but a shorter overall breakup point. Dual-wavelength planar laser induced fluorescence (D-PLIF) patternation showed an increase in water near the center of the spray. Steam injection flames saw little change in reaction stability, but emulsion flames experienced significant losses in stability that limited reaction operability at higher W/F. Emulsions were more effective at reducing NOx than steam injection, likely because of liquid water's latent heat of vaporization and the strategic injection of water into the flame core. OH* chemiluminescence showed a decrease in heat release for both methods, though the decrease was greater for emulsions. Both methods saw decreases in flame length for W/F 0.15. Lastly, flame imaging showed a shift towards a redder appearance with the addition or more water, as well as a reduction in flame flares.

Atomic absorption determination of iron and copper impurities in rare earth compounds

International Nuclear Information System (INIS)

Zelyukova, Yu.V.; Kravchenko, J.B.; Kucher, A.A.

1978-01-01

An extraction atomic absorption method for the determination of copper and iron impurities in rare earth compounds has been developed. The extraction separation of determined elements as hydroxy quinolinates with isobuthyl alcohol was used. It increased the sensitivity of these element determination and excluded the effect of the analysed sample. Cu, Te, Zn, Bi, Sn, In, Ga, Tl and the some other elements can be determined at pH 2.0-3.0 but rare earths are remained in an aqueous phase. The condition of the flame combustion does not change during the introduction of isobutyl extract but the sensitivity of the determination of the elements increased 2-3 times. The limit of Fe determination is 0.01 mg/ml and the limit of Cu determination is 0.014 mg/ml

Investigation of phosphorus atomization using high-resolution continuum source electrothermal atomic absorption spectrometry

International Nuclear Information System (INIS)

Dessuy, Morgana B.; Vale, Maria Goreti R.; Lepri, Fabio G.; Welz, Bernhard; Heitmann, Uwe

2007-01-01

The atomization of phosphorus in electrothermal atomic absorption spectrometry has been investigated using a high-resolution continuum source atomic absorption spectrometer and atomization from a graphite platform as well as from a tantalum boat inserted in a graphite tube. A two-step atomization mechanism is proposed for phosphorus, where the first step is a thermal dissociation, resulting in a fast atomization signal early in the atomization stage, and the second step is a slow release of phosphorus atoms from the graphite tube surface following the adsorption of molecular phosphorus at active sites of the graphite surface. Depending on experimental conditions only one of the mechanisms or both might be active. In the absence of a modifier and with atomization from a graphite or tantalum platform the second mechanism appears to be dominant, whereas in the presence of sodium fluoride as a modifier both mechanisms are observed. Intercalation of phosphorus into the graphite platform in the condensed phase has also been observed; this phosphorus, however, appears to be permanently trapped in the structure of the graphite and does not contribute to the absorption signal

Underresolved absorption spectroscopy of OH radicals in flames using broadband UV LEDs

Science.gov (United States)

White, Logan; Gamba, Mirko

2018-04-01

A broadband absorption spectroscopy diagnostic based on underresolution of the spectral absorption lines is evaluated for the inference of species mole fraction and temperature in combustion systems from spectral fitting. The approach uses spectrally broadband UV light emitting diodes and leverages low resolution, small form factor spectrometers. Through this combination, the method can be used to develop high precision measurement sensors. The challenges of underresolved spectroscopy are explored and addressed using spectral derivative fitting, which is found to generate measurements with high precision and accuracy. The diagnostic is demonstrated with experimental measurements of gas temperature and OH mole fraction in atmospheric air/methane premixed laminar flat flames. Measurements exhibit high precision, good agreement with 1-D flame simulations, and high repeatability. A newly developed model of uncertainty in underresolved spectroscopy is applied to estimate two-dimensional confidence regions for the measurements. The results of the uncertainty analysis indicate that the errors in the outputs of the spectral fitting procedure are correlated. The implications of the correlation between uncertainties for measurement interpretation are discussed.

Absorption of femtosecond laser pulses by atomic clusters

International Nuclear Information System (INIS)

Lin Jingquan; Zhang Jie; Li Yingjun; Chen Liming; Lu Tiezheng; Teng Hao

2001-01-01

Energy absorption by Xe, Ar, He atomic clusters are investigated using laser pulses with 5 mJ energy in 150 fs duration. Experimental results show that the size of cluster and laser absorption efficiency are strongly dependent on several factors, such as the working pressure of pulse valve, atomic number Z of the gas. Absorption fraction of Xe clusters is as high as 45% at a laser intensity of 1 x 10 15 W/cm 2 with 20 x 10 5 Pa gas jet backing pressure. Absorption of the atomic clusters is greatly reduced by introducing pre-pulses. Ion energy measurements confirm that the efficient energy deposition results in a plasma with very high ion temperature

21 CFR 862.2850 - Atomic absorption spectrophotometer for clinical use.

Science.gov (United States)

2010-04-01

... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Atomic absorption spectrophotometer for clinical... Laboratory Instruments § 862.2850 Atomic absorption spectrophotometer for clinical use. (a) Identification. An atomic absorption spectrophotometer for clinical use is a device intended to identify and measure...

Characteristics of Early Flame Development in a Direct-Injection Spark-Ignition CNG Engine Fitted with a Variable Swirl Control Valve

Directory of Open Access Journals (Sweden)

Abd Rashid Abd Aziz

2017-07-01

Full Text Available An experimental study was conducted to investigate the effect of the structure of the induction flow on the characteristics of early flames in a lean-stratified and lean-homogeneous charge combustion of compressed natural gas (CNG fuel in a direct injection (DI engine at different engine speeds. The engine speed was varied at 1500 rpm, 1800 rpm and 2100 rpm, and the ignition timing was set at a 38.5° crank angle (CA after top dead center (TDC for all conditions. The engine was operated in a partial-load mode and a homogeneous air/fuel charge was achieved by injecting the fuel early (before the intake valve closure, while late injection during the compression stroke was used to produce a stratified charge. Different induction flow structures were obtained by adjusting the swirl control valves (SCV. Using an endoscopic intensified CCD (ICCD camera, flame images were captured and analyzed. Code was developed to analyze the level of distortion of the flame and its wrinkledness, displacement and position relative to the spark center, as well as the flame growth rate. The results showed a higher flame growth rate with the flame kernel in the homogeneous charge, compared to the stratified combustion case. In the stratified charge combustion scenario, the 10° SCV closure (medium-tumble resulted in a higher early flame growth rate, whereas a homogeneous charge combustion (characterized by strong swirl resulted in the highest rate of flame growth.

Coupling sequential injection on-line preconcentration by means of a renewable microcolumn with ion-exchange beads with detection by electrothermal atomic absorption spectrometry. Comparing the performance of eluting the loaded beads with transporting them directly into the graphite tube

DEFF Research Database (Denmark)

Wang, Jianhua; Hansen, Elo Harald

2001-01-01

The design of a flow injection/sequential injection (FIA/SIA) on-line preconcentration system incorporating a renewable microcolumn with ion-exchange beads and interfaced with an electrothermal atomic absorption spectrometry (ETAAS) detector is described, and its practical applicability.......4% for the procedure in which the loaded beads are transported directly to the graphite furnace for pyrolysis and atomization, and even improved in comparison to the traditional unidirectional and bidirectional repetitive elution procedures which under comparable conditions yield R.S.D.-values of 5.8 and 4...

A novel fiber-packed column for on-line preconcentration and speciation analysis of chromium in drinking water with flame atomic absorption spectrometry.

Science.gov (United States)

Monasterio, Romina P; Altamirano, Jorgelina C; Martínez, Luis D; Wuilloud, Rodolfo G

2009-02-15

A novel on-line preconcentration and determination system based on a fiber-packed column was developed for speciation analysis of Cr in drinking water samples prior to its determination by flame atomic absorption spectrometry (FAAS). All variables involved in the development of the preconcentration method including, pH, eluent type, sample and eluent flow rates, interfering effects, etc., were studied in order to achieve the best analytical performance. A preconcentration factor of 32 was obtained for Cr(VI) and Cr(III). The levels of Cr(III) species were calculated by difference of total Cr and Cr(VI) levels. Total Cr was determined after oxidation of Cr(III) to Cr(VI) with hydrogen peroxide. The calibration graph was linear with a correlation coefficient of 0.999 at levels near the detection limit and up to at least 50 microg L(-1). The relative standard deviation (R.S.D.) was 4.3% (C=5 microg L(-1) Cr(VI), n=10, sample volume=25 mL). The limit of detection (LOD) for both Cr(III) and Cr(VI) species was 0.3 microg L(-1). Verification of the accuracy was carried out by the analysis of a standard reference material (NIST SRM 1643e "Trace elements in natural water"). The method was successfully applied to the determination of Cr(III) and Cr(VI) species in drinking water samples.

Reliability of graphite furnace atomic absorption spectrometry as ...

African Journals Online (AJOL)

Purpose: To evaluate the comparative efficiency of graphite furnace atomic absorption spectrometry (GFAAS) and hydride generation atomic absorption spectrometry (HGAAS) for trace analysis of arsenic (As) in natural herbal products (NHPs). Method: Arsenic analysis in natural herbal products and standard reference ...

ESR studies of Bunsen-type methane-air flames. II. The effects of the addition of halogenated compounds to the secondary air on the hydrogen atoms in the flame

Energy Technology Data Exchange (ETDEWEB)

Noda, S; Fujimoto, S; Claesson, O; Yoshida, H

1983-09-01

Hydrogen atoms in a methane-air Bunsen-type flame were detected by the flame-in-cavity ESR method. The addition of a halogenated compound to the secondary air reduced the H-atom concentration linearly with an increase in additive concentration. These 8 halogenated compounds examined showed increased effectiveness in scavenging H atoms in this order: hydrochloric acid < dichlorodifluoromethane < chloroform < methyl chloride < methylene chloride < trichlorofluoromethane < carbon tetrachlorie < methyl bromide. The chemical effects of these additives on the combustion reactions agree well with the inhibitor indices for these compounds. 14 references, 3 figures.

Rapid food decomposition by H2O2-H2SO4 for determination of total mercury by flow injection cold vapor atomic absorption spectrometry.

Science.gov (United States)

Zenebon, Odair; Sakuma, Alice M; Dovidauskas, Sergio; Okada, Isaura A; de, MaioFrancaD; Lichtig, Jaim

2002-01-01

A mixture of 50% H2O2-H2SO4 (3 + 1, v/v) was used for decomposition of food in open vessels at 80 degrees C. The treatment allowed rapid total mercury determination by flow injection cold vapor atomic absorption spectrometry. Cabbage, potatoes, peanuts paste, hazelnuts paste, oats, tomatoes and their derivatives, oysters, shrimps, prawns, shellfish, marine algae, and many kinds of fish were analyzed by the proposed methodology with a limit of quantitation of 0.86 +/- 0.08 microg/L mercury in the final solution. Reference materials tested also gave excellent recovery.

Recent advances in on-line coupling of capillary electrophoresis to atomic absorption and fluorescence spectrometry for speciation analysis and studies of metal-biomolecule interactions

International Nuclear Information System (INIS)

Li Yan; Yin Xuebo; Yan Xiuping

2008-01-01

Speciation information is vital for the understanding of the toxicity, mobility and bioavailability of elements in environmental or biological samples. Hyphenating high resolving power of separation techniques and element-selective detectors provides powerful tools for studying speciation of trace elements in environmental and biological systems. During the last five years several novel hybrid techniques based on capillary electrophoresis (CE) and atomic spectrometry have been developed for speciation analysis and metal-biomolecule interaction study in our laboratory. These techniques include CE on-line coupled with atomic fluorescence spectrometry (AFS), chip-CE on-line coupled with AFS, CE on-line coupled with flame heated quartz furnace atomic absorption spectrometry (FHF-AAS), and CE on-line coupled with electrothermal atomic absorption spectrometry (ETAAS). The necessity for the development of these techniques, their interface design, and applications in speciation analysis and metal-biomolecule interaction study are reviewed. The advantages and limitations of the developed hybrid techniques are critically discussed, and further development is also prospected

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

International Nuclear Information System (INIS)

Ghaedi, M.; Tavallali, H.; Shokrollahi, A.; Zahedi, M.; Montazerozohori, M.; Soylak, M.

2009-01-01

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 HNO 3 . 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.

Qualitative and Quantitative Content Determination of Macro-Minor Elements in Bryonia Alba L. Roots using Flame Atomic Absorption Spectroscopy Technique.

Science.gov (United States)

Karpiuk, Uliana Vladimirovna; Al Azzam, Khaldun Mohammad; Abudayeh, Zead Helmi Mahmoud; Kislichenko, Viktoria; Naddaf, Ahmad; Cholak, Irina; Yemelianova, Oksana

2016-06-01

To determine the elements in Bryonia alba L. roots, collected from the Crimean Peninsula region in Ukraine. Dry ashing was used as a flexible method and all elements were determined using atomic absorption spectrometry (AAS) equipped with flame and graphite furnace. The average concentrations of the determined elements, expressed as mg/100 g dry weight of the sample, were as follow: 13.000 for Fe, 78.000 for Si, 88.000 for P, 7.800 for Al, 0.130 for Mn, 105.000 for Mg, 0.030 for Pb, 0.052 for Ni, 0.030 for Mo, 210.000 for Ca, 0.130 for Cu, 5.200 for Zn, 13.000 for Na, 1170.000 for K, 0.780 for Sr, 0.030 for Co, 0.010 for Cd, 0.010 for As, and 0.010 for Hg. Toxic elements such as Cd and Pb were also found but at very low concentration. Among the analyzed elements, K was the most abundant followed by Ca, Mg, P, Si, Fe, Na, and Zn, whereas Hg, As, Cd, Co, Mo, and Pb were found in low concentration. The results suggest that the roots of Bryonia alba L. plant has potential medicinal property through their high element contents present. Moreover, it showed that the AAS method is a simple, fast, and reliable for the determination of elements in plant materials. The obtained results of the current study provide justification for the usage of such fruit in daily diet for nutrition and for medicinal usage in the treatment of various diseases.

Analysis of Dithiocarbamate Fungicides in Vegetable Matrices Using HPLC-UV Followed by Atomic Absorption Spectrometry.

Science.gov (United States)

Al-Alam, Josephine; Bom, Laura; Chbani, Asma; Fajloun, Ziad; Millet, Maurice

2017-04-01

A simple method combining ion-pair methylation, high-performance liquid chromatography (HPLC) analysis with detection at 272 nm and atomic absorption spectrometry was developed in order to determine 10 dithiocarbamate fungicides (Dazomet, Metam-sodium, Ferbam, Ziram, Zineb, Maneb, Mancozeb, Metiram, Nabam and Propineb) and distinguish ethylenbisdithiocarbamates (EBDTCs) Zineb, Maneb and Mancozeb in diverse matrices. This method associates reverse phase analysis by HPLC analysis with detection at 272 nm, with atomic absorption spectrometry in order to distinguish, with the same extraction protocol, Maneb, Mancozeb and Zineb. The limits of detection (0.4, 0.8, 0.5, 1.25 and 1.97) and quantification (1.18, 2.5, 1.52, 4.2 and 6.52) calculated in injected nanogram, respectively, for Dazomet, Metam-Na, dimethyldithiocarbamates (DMDTCs), EBDTCs and propylenebisdithiocarbamates (PBDTCs) justify the sensitivity of the method used. The coefficients of determination R2 were 0.9985, 0.9978, 0.9949, 0.988 and 0.9794, respectively, for Dazomet, Metam-Na, DMDTCs, EBDTCs and PBDTCs, and the recovery from fortified apple and leek samples was above 90%. Results obtained with the atomic absorption method in comparison with spectrophotometric analysis focus on the importance of the atomic absorption as a complementary specific method for the distinction between different EBDTCs fungicides. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Determination of boron in natural waters using atomic-absorption spectrometry with electrothermal atomization

International Nuclear Information System (INIS)

Usenko, S.I.; Prorok, M.M.

1992-01-01

A method of direct determination of boron in natural waters using atomic-absorption spectrometry with electrothermal atomization was developed. Concomitant elements Si, K, Mg, Na, present in natural waters in the concentration of 0.05-100 mg/cv 3 , do not produce effect on the value of boron atomic absorption. Boron determination limit constituted 0.02 mg/cm 3 for 25 ml of solution introduced

Flame Atomic Absorption Spectrometric Determination of Ultra Traces of Thallium(I) ion after Solid Phase Extraction by Octadecyl Silica Membrane Disk Modified by a New Schiff Base

International Nuclear Information System (INIS)

Mashhadizadeh, Mohammad Hossein; Moatafavi, Ali; Allah-Abadi, Hossein; Zadmehr, Mohammad Reza

2004-01-01

A simple and reliable method has been developed to selectively separate and concentrate trace amounts of thallium ion from real samples for the subsequent measurement by flame atomic absorption spectrometry (FAAS). Thallium ions are absorbed quantitatively during passage of aqueous real samples through an octadecyl bonded silica membrane disk modified by 4-(4-Chloro-phenylazo)-2-[(4-hydroxy-phenylamino)- methyl]-phenol. The retained Tl + ions are then stripped from the disk quantitatively with a minimal amount of thiosulfate solution as eluent. The proposed method permitted large enrichment factors of about 130 and higher. The relative standard deviation for ten replicate extraction of thallium from 1 L samples containing 5 μg thallium is 1.2%. The break through volume for 5 μg thallium is 1000 mL. The limit of detection of the proposed method is 11.2 ng of Tl + per 1000 mL. The effects of various cationic interferences on the recovery of thallium in binary mixtures were studied. The method was applied to the recovery of Tl + ions from natural water and human hair samples

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.

Science.gov (United States)

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).

Efficient atom localization via probe absorption in an inverted-Y atomic system

Science.gov (United States)

Wu, Jianchun; Wu, Bo; Mao, Jiejian

2018-06-01

The behaviour of atom localization in an inverted-Y atomic system is theoretically investigated. For the atoms interacting with a weak probe field and several orthogonal standing-wave fields, their position information can be obtained by measuring the probe absorption. Compared with the traditional scheme, we couple the probe field to the transition between the middle and top levels. It is found that the probe absorption sensitively depends on the detuning and strength of the relevant light fields. Remarkably, the atom can be localized at a particular position in the standing-wave fields by coupling a microwave field to the transition between the two ground levels.

Salt-assisted liquid-liquid microextraction of Cr(VI) ion using an ionic liquid for preconcentration prior to its determination by flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Majidi, B.; Shemirani, F.

2012-01-01

We report on the salt-assisted liquid-liquid microextraction of cationic complexes of Cr(VI) ion using the hydrophilic ionic liquid (IL) 1-butyl-3-methylimidazolium tetrafluoraborate and potassium hydrogen phosphate. This is a novel, simple, non-toxic and effective technique for sample pretreatment technique that displays large extraction efficiency and represents a new platform where Cr(VI) is complexed with 1,5-diphenylcarbazide (DPC) in sulfuric acid medium. It was applied to the extraction of Cr(VI) in the form of the Cr(VI)-DPC complex prior to its determination by flame atomic absorption spectrometry. Cr(III) ion also can be determined by this procedure after oxidation to Cr(VI). Extraction is mainly affected by the amount of water-soluble IL, the kind and quantity of inorganic salts, by pH and the concentration of DPC. Calibration plots are linear in the range from 3 to 150 μg L -1 of Cr(VI), and the limit of detection is 1. 25 μg L -1 . The method was successfully applied to the speciation and determination of trace levels of Cr(III) and Cr(VI) in environmental water samples containing high levels of dissolved salts or food grade salts. (author)

H2O temperature sensor for low-pressure flames using tunable diode laser absorption near 2.9 νm

KAUST Repository

Li, Sijie

2011-10-19

Making use of a newly available rapid-tuning diode laser operating at wavelengths up to 2.9 νm, an absorption-based temperature sensor was developed for in situ measurements in low-pressure flames. Based on the systematic analysis of H2O vapor transitions in the fundamental vibrational bands (ν1 and ν3) of H2O in the range of 2.5-3.0 νm, an optimal closely-spaced spectral line pair near 2.9 νm was selected for its temperature sensitivity in the range of 1000-2500 K. The narrow-linewidth room-temperature laser was scanned repetitively across these spectral features at 5 kHz, enabling fast, accurate temperature sensing. Use of the temperature sensor was investigated in low-pressure flames supported on a McKenna burner at 15, 25 and 60 Torr. To avoid absorption by the cold gases in the flame edges and the recirculation region between the burner and the vacuum chamber wall, a variable-path in situ probe was designed and an optimal path length was determined to accurately measure the flame centerline temperature. Different flame conditions were investigated to illustrate the potential of this sensor system for sensitive measurements of combustion temperature in low-pressure flames. © 2011 IOP Publishing Ltd.

Atomic and molecular gas phase spectrometry

Science.gov (United States)

Winefordner, J. D.

1985-10-01

The major goals of this research have been to develop diagnostical spectroscopic methods for measuring spatial/temporal temperatures and species of combustion flames and plasmas and to develop sensitive, selective, precise, reliable, rapid spectrometric methods of trace analysis of elements present in jet engine lubricating oils, metallurgical samples, and engine exhausts. The diagnostical approaches have been based upon the measurement of metal probes introduced into the flame or plasmas and the measurement of OH in flames. The measurement approaches have involved the use of laser-excited fluorescence, saturated absorption, polarization, and linear absorption. The spatial resolution in most studies is less than 1 cu mm and the temporal resolution is less than 10 ns with the use of pulsed lasers. Single pulse temperature and species measurements have also been carried out. Other diagnostical studies have involved the measurement of collisional redistribution of radiatively excited levels of Na and Tl in acetylene/02/Ar flames and the measurement of lifetimes and quantum efficiencies of atoms and ions in the inductively coupled plasmas, ICP. The latter studies indicate that the high electron number densities in ICPs are not efficient quenchers of excited atoms/ions. Temperatures of microwave atmospheric plasmas produced capacitatively and cool metastable N2 discharge produced by a dielectric discharge have also been measured.

Direct determination of cadmium in unicellular green algae by flameless atomic absorption

International Nuclear Information System (INIS)

Meisch, H.U.; Reinle, W.

1977-01-01

Cadmium is detectable without any disturbance by direct injection of Cd-containing microorganisms (unicellular green algae) into the graphite furnace of an atomic absorption instrument, if the decomposition temperature is increased to 700 0 C. This has been done without loss of the trace method by charging the input suspension with a 10 7 fold molar excess of (NH 4 ) 2 SO 4 . The precision of the uncomplicated method is compared to the results of Cd-analysis after HNO 3 -decomposition. (author)

Emission flame spectrophotometry of chromium, cobalt, nickel trace amounts

International Nuclear Information System (INIS)

Prudnikov, Y.D.; Shapkina, Y.S.

1976-01-01

Chromium, cobalt, and nickel were determined in a flame spectrophotometer with a dual diffraction monochromator, DFS-12, in a high-temperature nitrogen-acetylene flame. The effect of ionization and the elements in the oxidizing flame was small. The lower limit of detection for the three elements is 1x10 -2 to 1 x10 -3 μg/ml, and the high selectivity of the analysis permits determining down to 10 -4 % Cr and Ni and to 10 -3 % Co. These elements may be determined in rocks and minerals from solutions prepared for analysis for alkali and alkali-earth elements. The possibilities of emission flame spectrophotometry are as great as those of atomic-absorption analysis, and it may be used for determining Cr, Co, and Ni in rocks and minerals, especially pure substances, metals, and other materials

Elemental investigation of momordica charantia linn. and syzigium jambolana linn. using atomic absorption spectrophotometer

International Nuclear Information System (INIS)

Kazi, T.G.

2002-01-01

Elemental investigation of very important medicinal plant i.e. momordica charantia linn and syzigium jambolana linn, and its decoction has been carried out using flame atomic absorption spectrophotometer. In present study fifteen essential, trace and toxic elements such as Zn, Cr, K, Mg, Ca, Na, Cu, Fe, Pb, Al, Ba, Mn, Co, Ni and Cd were determined in different parts of both plants and in its decoction. The level of essential elements was found high as compared to the level of toxic elements. Both plants are useful in the treatment of diabetes. The validation of the method was checked by employing NBS- 1570 (Spanish) as a standard reference material . The measured values of elements are in close agreement with certified values. (author)

Light absorption during alkali atom-noble gas atom interactions at thermal energies: a quantum dynamics treatment.

Science.gov (United States)

Pacheco, Alexander B; Reyes, Andrés; Micha, David A

2006-10-21

The absorption of light during atomic collisions is treated by coupling electronic excitations, treated quantum mechanically, to the motion of the nuclei described within a short de Broglie wavelength approximation, using a density matrix approach. The time-dependent electric dipole of the system provides the intensity of light absorption in a treatment valid for transient phenomena, and the Fourier transform of time-dependent intensities gives absorption spectra that are very sensitive to details of the interaction potentials of excited diatomic states. We consider several sets of atomic expansion functions and atomic pseudopotentials, and introduce new parametrizations to provide light absorption spectra in good agreement with experimentally measured and ab initio calculated spectra. To this end, we describe the electronic excitation of the valence electron of excited alkali atoms in collisions with noble gas atoms with a procedure that combines l-dependent atomic pseudopotentials, including two- and three-body polarization terms, and a treatment of the dynamics based on the eikonal approximation of atomic motions and time-dependent molecular orbitals. We present results for the collision induced absorption spectra in the Li-He system at 720 K, which display both atomic and molecular transition intensities.

Preconcentration of trace amounts of lead in water samples with cetyltrimethylammonium bromide coated magnetite nanoparticles and its determination by flame atomic absorption spectrometry

Directory of Open Access Journals (Sweden)

Mohammad Faraji

2016-11-01

Full Text Available A sensitive and simple magnetic solid phase extraction procedure was presented for the preconcentration of lead ions in environmental water samples. In the present study, lead ions form complexes with 1-(2-pyridilazo-2-naphthol reagent (PAN in basic medium, and then are quantitatively extracted to the surface of cetyltrimethylammonium bromide (CTAB-coated magnetite nanoparticles (Fe3O4 NPs. After magnetic separation of adsorbent, the adsorbent was eluted with 0.5% (v/v HCl in methanol prior to its analysis by flame atomic absorption spectrometry (FAAS. The pH of sample, concentrations of PAN, amounts of CTAB and Fe3O4 NPs, sample volume and desorption conditions were optimized. Under optimum conditions, the calibration curve was linear in the range of 0.05–100 ng mL−1 with R2 = 0.9996. Detection and quantification limits of the proposed method were 0.005 and 0.05 ng mL−1, respectively. Enhancement factor of 1050 was achieved using this method to extract 1000 mL of different environmental water samples. Compared with conventional solid phase extraction methods, the advantages of this method still include easy preparation of sorbents, short times of sample pre-treatment, high extraction yield, and high breakthrough volume. It shows great analytical potential in preconcentration of lead from large volume water samples.

Atomic absorption assessment of mineral iron quantity in ferritin

International Nuclear Information System (INIS)

Marinova, M.; Vladimirova, L.

2009-01-01

Possibilities for quantitative determination of the number of iron atoms in the mineral core of ferritin by atomic absorption spectroscopy (AAS) are investigated in the work. Different measurements with AAS show an iron content from 1000 up to 4500 atoms per molecule ferritin. This motivated us to investigate the amount of iron in the Horse Spleen Ferritin with atomic absorption spectroscopy under application of the Bulgarian standard BDS EN 14082/2003 Foodstuffs - Determination of trace elements - Determination of lead, cadmium, zinc, copper, iron and chromium by atomic absorption spectrometry (AAS) after dry ashing. The obtained results give approx. 1800 atoms per molecule Ferritin. It is in accordance with previous results, published by leading researchers. The investigation of the iron content with AAS under the use of the Bulgarian standard is a good opportunity to study many other objects of biological interest. (authors)

Development of an in situ solvent formation microextraction and preconcentration method based on ionic liquids for the determination of trace cobalt (II in water samples by flame atomic absorption spectrometry

Directory of Open Access Journals (Sweden)

Mohammad Reza Jamali

2017-02-01

Full Text Available A simple in situ solvent formation microextraction (ISFME methodology based on the application of ionic liquid (IL as an extractant solvent and sodium hexafluorophosphate (NaPF6 as an ion-pairing agent was proposed for the preconcentration of the trace levels of cobalt ions. In this method cobalt was complexed with 2-(5-bromo-2-pyridylazo-5-diethylaminophenol (5-Br-PADAP and extracted into an ionic liquid phase. After phase separation, the enriched analyte in the final solution is determined by flame atomic absorption spectrometry (FAAS. Some effective factors that influence the microextraction efficiency were investigated and optimized. Under the optimum experimental conditions, the limit of detection and the enrichment factor were 0.97 μg L−1 and 50, respectively. The relative standard deviation (R.S.D. was obtained as 2.4%. The proposed method was assessed through the analysis of certified reference water and recovery experiments.

Solid phase extraction of ultra traces silver(I) using octadecyl silica membrane disks modified by 1,3-bis(2-cyanobenzene) triazene (CBT) ligand prior to determination by flame atomic absorption

International Nuclear Information System (INIS)

Rofouei, Mohammad Kazem; Payehghadr, Mahmood; Shamsipur, Mojtaba; Ahmadalinezhad, Asieh

2009-01-01

A simple, reliable and rapid method for preconcentration and determination of the ultra trace amount of silver using octadecyl silica membrane disk modified by a recently synthesized triazene ligand, 1,3-bis(2-cyanobenzene)triazene (CBT), and flame atomic absorption spectrometry is presented. Various parameters including pH of aqueous solution, flow rates, the amount of ligand and the type of stripping solvents were optimized. The breakthrough volume was greater than 1800 ml with an enrichment factor of more than 360 and 6.0 ng l -1 detection limit. The capacity of the membrane disks modified by 5 mg of the ligand was found to be 1070 μg of silver. The effects of various cationic interferences on the percent recovery of silver ion were studied. The method was successfully applied to the determination of silver ion in different samples, especially determination of ultra trace amount of silver in the presence of large amount of lead.

Solid phase extraction of ultra traces silver(I) using octadecyl silica membrane disks modified by 1,3-bis(2-cyanobenzene) triazene (CBT) ligand prior to determination by flame atomic absorption

Energy Technology Data Exchange (ETDEWEB)

Rofouei, Mohammad Kazem, E-mail: rofouei@tmu.ac.ir [Faculty of Chemistry, Tarbiat Moalem University, Tehran (Iran, Islamic Republic of); Payehghadr, Mahmood [Department of Chemistry, Payame Noor University (PNU) (Iran, Islamic Republic of); Shamsipur, Mojtaba [Department of Chemistry, Razi University, Kermanshah (Iran, Islamic Republic of); Ahmadalinezhad, Asieh [Department of Chemistry, Lakehead University, Thunder Bay, Ontario P7B 5E1 (Canada)

2009-09-15

A simple, reliable and rapid method for preconcentration and determination of the ultra trace amount of silver using octadecyl silica membrane disk modified by a recently synthesized triazene ligand, 1,3-bis(2-cyanobenzene)triazene (CBT), and flame atomic absorption spectrometry is presented. Various parameters including pH of aqueous solution, flow rates, the amount of ligand and the type of stripping solvents were optimized. The breakthrough volume was greater than 1800 ml with an enrichment factor of more than 360 and 6.0 ng l{sup -1} detection limit. The capacity of the membrane disks modified by 5 mg of the ligand was found to be 1070 {mu}g of silver. The effects of various cationic interferences on the percent recovery of silver ion were studied. The method was successfully applied to the determination of silver ion in different samples, especially determination of ultra trace amount of silver in the presence of large amount of lead.

Study of absorption spectra for alkali and alkaline earth metal salts in flameless atomic absorption spectrometry using a carbon tube atomizer

International Nuclear Information System (INIS)

Yasuda, Seiji; Kakiyama, Hitoo

1975-01-01

Absorption spectra of various salts such as alkali metal salts, alkaline earth dichlorides, and ammonium halides were investigated and absorptions of some molecular species produced in the carbon tube were identified. The aqueous solution (20 μl) containing 1.0 mg/ml of each salt was placed in the carbon tube atomizer and heated in a similar manner to usual flameless atomic absorption method. D 2 -lamp was used as a continuous light source and argon gas was employed as an inert sheath gas. The spectra were obtained over the range of wavelength 200 to 350 nm. When alkali halides were feeded, the absorption spectra agreed with those of alkali halide vapors. Therefore, in such cases vapors of the alkali halides were probably produced by the sublimation or vaporization in the atomizer. The spectra of alkali perchlorates were considered to be those of alkali chlorides produced by the pyrolysis of the perchlorates in the atomizer. The absorptions of alkaline earth chlorides below 250 nm were probably due to their gaseous states. Sulfur dioxide was found to be produced by the pyrolysis of alkali sulfates, bisulfates and sulfites in the atomizer, Alkali phosphates and pyrophosphates gave almost identical spectra below 300 nm. Gamma band spectrum of nitrogen monoxide was observed from 200 to 240 nm during ashing at bout 330 0 C for alkali nitrates and nitrites. Ammonia vapor was produced from ammonium halides during drying at about 170 0 C. Although the absorptions of alkali carbonates and hydroxides were almost undetectable, the same spectra as those of alkali halides were observed by the addition of ammonium halides to the solutions of alkali compounds. This shows that alkali halides are produced in the atomizer by the addition of halide ions. (auth.)

Cloud point extraction-flame atomic absorption spectrometry for pre-concentration and determination of trace amounts of silver ions in water samples.

Science.gov (United States)

Yang, Xiupei; Jia, Zhihui; Yang, Xiaocui; Li, Gu; Liao, Xiangjun

2017-03-01

A cloud point extraction (CPE) method was used as a pre-concentration strategy prior to the determination of trace levels of silver in water by flame atomic absorption spectrometry (FAAS) The pre-concentration is based on the clouding phenomena of non-ionic surfactant, triton X-114, with Ag (I)/diethyldithiocarbamate (DDTC) complexes in which the latter is soluble in a micellar phase composed by the former. When the temperature increases above its cloud point, the Ag (I)/DDTC complexes are extracted into the surfactant-rich phase. The factors affecting the extraction efficiency including pH of the aqueous solution, concentration of the DDTC, amount of the surfactant, incubation temperature and time were investigated and optimized. Under the optimal experimental conditions, no interference was observed for the determination of 100 ng·mL -1 Ag + in the presence of various cations below their maximum concentrations allowed in this method, for instance, 50 μg·mL -1 for both Zn 2+ and Cu 2+ , 80 μg·mL -1 for Pb 2+ , 1000 μg·mL -1 for Mn 2+ , and 100 μg·mL -1 for both Cd 2+ and Ni 2+ . The calibration curve was linear in the range of 1-500 ng·mL -1 with a limit of detection (LOD) at 0.3 ng·mL -1 . The developed method was successfully applied for the determination of trace levels of silver in water samples such as river water and tap water.

Study on the application of electrothermal atomization atomic absorption spectrometry for the determination of metallic Cu, Pb, Zn, Cd traces in sea water samples

International Nuclear Information System (INIS)

Nguyen Thi Kim Dung; Doan Thanh Son; Tran Thi Ngoc Diep

2004-01-01

The trace amount of some heavy metallic elements (Cu, Zn, Pb, Cd) in sea water samples were determined directly (without separation) and quantitatively by using Electro-Thermal Atomization Atomic Absorption Spectrometry (ETA-AAS). The effect of mainly major constituents such as Na, Mg, Ca, K, and the mutual effect of the trace elements, which were present in the matrix on the absorption intensity of each analyzed element was studied. The adding of a certain chemical modification for each trace element was also investigated in order to eliminate the overall effect of the background during the pyrolysis and atomization. The sea water sample after fitrating through a membrane with 0.45 μm-hole size was injected in to the graphite tube via an autosampler (MPE50). 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 graphite furnace such as dry temperature, pyrolysis temperature, atomization temperature, 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)

A comparison of simultaneous plasma, atomic absorption, and iron colorimetric determinations of major and trace constituents in acid mine waters

Science.gov (United States)

Ball, J.W.; Nordstrom, D. Kirk

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

Determination of calcium, magnesium, sodium, and potassium in foodstuffs by using a microsampling flame atomic absorption spectrometric method after closed-vessel microwave digestion: method validation.

Science.gov (United States)

Chekri, Rachida; Noël, Laurent; Vastel, Christelle; Millour, Sandrine; Kadar, Ali; Guérin, Thierry

2010-01-01

This paper describes a validation process in compliance with the NFIEN ISO/IEC 17025 standard for the determination of the macrominerals calcium, magnesium, sodium, and potassium in foodstuffs by microsampling with flame atomic absorption spectrometry after closed-vessel microwave digestion. The French Standards Commission (Agence Francaise de Normalisation) standards NF V03-110, NF EN V03-115, and XP T-90-210 were used to evaluate this method. The method was validated in the context of an analysis of the 1322 food samples of the second French Total Diet Study (TDS). Several performance criteria (linearity, LOQ, specificity, trueness, precision under repeatability conditions, and intermediate precision reproducibility) were evaluated. Furthermore, the method was monitored by several internal quality controls. The LOQ values obtained (25, 5, 8.3, and 8.3 mg/kg for Ca, Mg, Na, and K, respectively) were in compliance with the needs of the TDS. The method provided accurate results as demonstrated by a repeatability CV (CVr) of < 7% and a reproducibility CV (CVR) of < 12% for all the elements. Therefore, the results indicated that this method could be used in the laboratory for the routine determination of these four elements in foodstuffs with acceptable analytical performance.

Molecular absorption spectra of beryllium, cerium, lanthanum, iron, and platinum salts

International Nuclear Information System (INIS)

Daidoji, Hidehiro

1980-01-01

The absorption spectra of some salts of beryllium, cerium, lanthanum, iron and platinum in air-acetylene flame were measured in the wavelength range from 200 to 400 nm. A Hitachi 207 type atomic absorption spectrophotometer was used. A deuterium lamp, a home-made continuous radiation lamp and some hollow cathode lamps were used as light sources. The new molecular absorption spectra of cerium, lanthanum and platinum and the absorption spectra due to Be(OH) 2 , LaO, PtH, FeO and FeCl in 200-400 nm region were obtained. Emission spectra of CeO, LaO and FeOH were also obtained. These molecular absorption bands were estimated as absorption errors of maximum 15 times to the sensitivity of each elements in atomic absorption spectrometry. In addition, spectral line interferences of iron were observed in atomic absorption spectrometry of Zn, Cd, Ni, Cu and Cr. (author)

Immersed single-drop microextraction interfaced with sequential injection analysis for determination of Cr(VI) in natural waters by electrothermal-atomic absorption spectrometry

International Nuclear Information System (INIS)

Pena, Francisco; Lavilla, Isela; Bendicho, Carlos

2008-01-01

Single-drop microextraction (SDME) and sequential injection analysis have been hyphenated for ultratrace metal determination by Electrothermal-Atomic Absorption Spectrometry (ETAAS). The novel method was targeted on extraction of the Cr(VI)-APDC chelate and encompasses the potential of SDME as a miniaturized and virtually solvent-free preconcentration technique, the ability of sequential injection analysis to handle samples and the versatility of furnace autosamplers for introducing microliter samples in ETAAS. The variables influencing the microextraction of Cr(VI) onto an organic solvent drop, i.e., type of organic solvent, microextraction time, stirring rate of the sample solution, drop volume, immersion depth of the drop, salting-out effect, temperature of the sample, concentration of the complexing agent and pH of the sample solution were fully investigated. For a 5 and 20 min microextraction time, the preconcentration factors were 20 and 70, respectively. The detection limit was 0.02 μg/L of Cr(VI) and the repeatability expressed as relative standard deviation was 7%. The SDME-SIA-ETAAS technique was validated against BCR CRM 544 (lyophilized solution) and applied to ultrasensitive determination of Cr(VI) in natural waters

Immersed single-drop microextraction interfaced with sequential injection analysis for determination of Cr(VI) in natural waters by electrothermal-atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Pena, Francisco; Lavilla, Isela [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Facultad de Quimica, Universidad de Vigo, Campus As Lagoas-Marcosende, s/n, 36310 Vigo (Spain); Bendicho, Carlos [Departamento de Quimica Analitica y Alimentaria, Area de Quimica Analitica, Facultad de Quimica, Universidad de Vigo, Campus As Lagoas-Marcosende, s/n, 36310 Vigo (Spain)], E-mail: bendicho@uvigo.es

2008-04-15

Single-drop microextraction (SDME) and sequential injection analysis have been hyphenated for ultratrace metal determination by Electrothermal-Atomic Absorption Spectrometry (ETAAS). The novel method was targeted on extraction of the Cr(VI)-APDC chelate and encompasses the potential of SDME as a miniaturized and virtually solvent-free preconcentration technique, the ability of sequential injection analysis to handle samples and the versatility of furnace autosamplers for introducing microliter samples in ETAAS. The variables influencing the microextraction of Cr(VI) onto an organic solvent drop, i.e., type of organic solvent, microextraction time, stirring rate of the sample solution, drop volume, immersion depth of the drop, salting-out effect, temperature of the sample, concentration of the complexing agent and pH of the sample solution were fully investigated. For a 5 and 20 min microextraction time, the preconcentration factors were 20 and 70, respectively. The detection limit was 0.02 {mu}g/L of Cr(VI) and the repeatability expressed as relative standard deviation was 7%. The SDME-SIA-ETAAS technique was validated against BCR CRM 544 (lyophilized solution) and applied to ultrasensitive determination of Cr(VI) in natural waters.

Trends in preconcentration procedures for metal determination using atomic spectrometry techniques

International Nuclear Information System (INIS)

Godoi Pereira, M. de; Arruda, M.A.Z.

2003-01-01

Methods for metal preconcentration are often described in the literature. However, purposes are often different, depending on whether the methods are applied in environmental, clinical or technological fields. The respective method needs to be efficient, give high sensitivity, and ideally also is selective which is useful when used in combination with atomic spectroscopy. This review presents the actual tendencies in metal preconcentration using techniques such as flame atomic absorption spectrometry (FAAS), electrothermal atomic absorption spectrometry (ETAAS), hydride generation atomic absorption spectrometry (HGAAS), inductively coupled plasma optical emission spectrometry (ICP OES) and inductively coupled plasma mass spectrometry (ICP-MS). Procedures based on related to electrochemical, coprecipitation/precipitation, liquid-liquid and solid-liquid extraction and atom trapping mechanisms are presented. (author)

On-line separation and preconcentration of lead(II) by solid-phase extraction using activated carbon loaded with xylenol orange and its determination by flame atomic absorption spectrometry.

Science.gov (United States)

Ensafi, Ali A; Shiraz, A Zendegi

2008-02-11

Activated carbon loaded with xylenol orange in a mini-column was used for the highly selective separation and preconcentration of Pb(II) ions. An on-line system for enrichment and the determination of Pb(II) was carried out on flame atomic absorption spectrometry. The conditions of preconcentration and quantitative recovery of Pb(II) from diluted solution, such as pH of aqueous phase, amount of the sorbent, volume of the solutions and flow variables were studied as well as effect of potential interfering ions. Under the optimum conditions, Pb(II) in an aqueous sample was concentrated about 200-fold and the detection limit was 0.4 ng mL(-1) Pb(II). The adsorption capacity of the solid phase was 0.20mg of lead per one gram of the modified activated carbon. The modified activated carbon is stable for several treatments of sample solutions without the need for using any chemical reagent. The recovery of lead(II) from river water, waste water, tap water, and in the following reference materials: SRM 2711 Montana soil and GBW-07605 tea were obtained in the range of 97-104% by the proposed method.

On-line separation and preconcentration of lead(II) by solid-phase extraction using activated carbon loaded with xylenol orange and its determination by flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Ensafi, Ali A.; Shiraz, A. Zendegi

2008-01-01

Activated carbon loaded with xylenol orange in a mini-column was used for the highly selective separation and preconcentration of Pb(II) ions. An on-line system for enrichment and the determination of Pb(II) was carried out on flame atomic absorption spectrometry. The conditions of preconcentration and quantitative recovery of Pb(II) from diluted solution, such as pH of aqueous phase, amount of the sorbent, volume of the solutions and flow variables were studied as well as effect of potential interfering ions. Under the optimum conditions, Pb(II) in an aqueous sample was concentrated about 200-fold and the detection limit was 0.4 ng mL -1 Pb(II). The adsorption capacity of the solid phase was 0.20 mg of lead per one gram of the modified activated carbon. The modified activated carbon is stable for several treatments of sample solutions without the need for using any chemical reagent. The recovery of lead(II) from river water, waste water, tap water, and in the following reference materials: SRM 2711 Montana soil and GBW-07605 tea were obtained in the range of 97-104% by the proposed method

On-line separation and preconcentration of lead(II) by solid-phase extraction using activated carbon loaded with xylenol orange and its determination by flame atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Ensafi, Ali A. [College of Chemistry, Isfahan University of Technology, Isfahan 84156-83111 (Iran, Islamic Republic of)], E-mail: Ensafi@cc.iut.ac.ir; Shiraz, A. Zendegi [College of Chemistry, Isfahan University of Technology, Isfahan 84156-83111 (Iran, Islamic Republic of)

2008-02-11

Activated carbon loaded with xylenol orange in a mini-column was used for the highly selective separation and preconcentration of Pb(II) ions. An on-line system for enrichment and the determination of Pb(II) was carried out on flame atomic absorption spectrometry. The conditions of preconcentration and quantitative recovery of Pb(II) from diluted solution, such as pH of aqueous phase, amount of the sorbent, volume of the solutions and flow variables were studied as well as effect of potential interfering ions. Under the optimum conditions, Pb(II) in an aqueous sample was concentrated about 200-fold and the detection limit was 0.4 ng mL{sup -1} Pb(II). The adsorption capacity of the solid phase was 0.20 mg of lead per one gram of the modified activated carbon. The modified activated carbon is stable for several treatments of sample solutions without the need for using any chemical reagent. The recovery of lead(II) from river water, waste water, tap water, and in the following reference materials: SRM 2711 Montana soil and GBW-07605 tea were obtained in the range of 97-104% by the proposed method.

Combination of flame atomic absorption spectrometry with ligandless-dispersive liquid- liquid microextraction for preconcentration and determination of trace amount of lead in water samples

Directory of Open Access Journals (Sweden)

Y.M. Baghelani

2013-05-01

Full Text Available A new ligandless-dispersive liquid–liquid microextraction method has been developed for the separation and flame atomic absorption spectrometry determination of trace amount of lead(II ion. In the proposed approach 1,2-dicholorobenzene and ethanol were used as extraction and dispersive solvents. Factors influencing the extraction efficiency of lead, including the extraction and dispersive solvent type and volume, pH of sample solution, concentration of chloride and extraction time were studied. Under the optimal conditions, the calibration curve was linear in the range of 7.0–6000 ng mL−1 of lead with R2 = 0.9992 (n = 10 and detection limit based on three times the standard deviation of the blank (3Sb was 0.5 ng mL−1 in original solution. The relative standard deviation for eight replicate determinations of 1.0 mg mL-1 lead was ±1.6%. The high efficiency of dispersive liquid-liquid microextraction to carry out the determination of trace amounts of lead in complex matrices was demonstrated. The proposed method has been applied for determination of trace amounts of lead in water samples and satisfactory results were obtained. The accuracy was checked by analyzing a certified reference material from the National Institute of Standard and Technology, Trace elements in water (NIST CRM 1643e.

Iron species determination by task-specific ionic liquid-based in situ solvent formation dispersive liquid-liquid microextraction combined with flame atomic absorption spectrometry.

Science.gov (United States)

Sadeghi, Susan; Ashoori, Vahid

2017-10-01

The task-specific ionic liquid (TSIL) of 1-ethyl-3-methylimidazolium bromide functionalized with 8-hydroxyquinoline was used as a chelating agent and extracting solvent for dispersive liquid-liquid microextraction and subsequent determination of Fe(III) by flame atomic absorption spectrometry. The in situ solvent formation of TSIL using KPF 6 provided the desired water-immiscible ionic liquid. The total Fe concentration could be determined after pre-oxidation of Fe(II) to Fe(III). Various factors affecting the proposed extraction procedure were optimized. The proposed analytical conditions were: sample pH 5, TSIL amount 0.3% (w/v), KPF 6 amount 0.15% (w/v), anti-sticking 0.1% (w/v) and salt concentration 5% (w/v). Under optimal conditions, the linear dynamic ranges for Fe(III) and total Fe were 20-80 and 20-110 ng mL -1 , respectively, with a detection limit of 6.9 ng mL -1 for Fe(III) and relative standard deviation of 2.2%. The proposed method was successfully applied to the determination of trace Fe(III) in water (underground, tap, refined water and artificial sea water) and beverage (apple, tomato, and tea) samples. The developed method offers advantages such as simplicity, ease of operation, and extraction of Fe(III) from aqueous solutions without the use of organic solvent. It was successfully applied for iron speciation in different real samples. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

Cloud point extraction-flame atomic absorption spectrometry for pre-concentration and determination of trace amounts of silver ions in water samples

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Xiupei Yang

2017-03-01

Full Text Available A cloud point extraction (CPE method was used as a pre-concentration strategy prior to the determination of trace levels of silver in water by flame atomic absorption spectrometry (FAAS The pre-concentration is based on the clouding phenomena of non-ionic surfactant, triton X-114, with Ag (I/diethyldithiocarbamate (DDTC complexes in which the latter is soluble in a micellar phase composed by the former. When the temperature increases above its cloud point, the Ag (I/DDTC complexes are extracted into the surfactant-rich phase. The factors affecting the extraction efficiency including pH of the aqueous solution, concentration of the DDTC, amount of the surfactant, incubation temperature and time were investigated and optimized. Under the optimal experimental conditions, no interference was observed for the determination of 100 ng·mL−1 Ag+ in the presence of various cations below their maximum concentrations allowed in this method, for instance, 50 μg·mL−1 for both Zn2+ and Cu2+, 80 μg·mL−1 for Pb2+, 1000 μg·mL−1 for Mn2+, and 100 μg·mL−1 for both Cd2+ and Ni2+. The calibration curve was linear in the range of 1–500 ng·mL−1 with a limit of detection (LOD at 0.3 ng·mL−1. The developed method was successfully applied for the determination of trace levels of silver in water samples such as river water and tap water.

Effects of self-absorption on simultaneous estimation of temperature distribution and concentration fields of soot and metal-oxide nanoparticles in nanofluid fuel flames using a spectrometer

Science.gov (United States)

Liu, Guannan; Liu, Dong

2018-06-01

An improved inverse reconstruction model with consideration of self-absorption effect for the temperature distribution and concentration fields of soot and metal-oxide nanoparticles in nanofluid fuel flames was proposed based on the flame emission spectrometry. The effects of self-absorption on the temperature profile and concentration fields were investigated for various measurement errors, flame optical thicknesses and detecting lines numbers. The model neglecting the self-absorption caused serious reconstruction errors especially in the nanofluid fuel flames with large optical thicknesses, while the improved model was used to successfully recover the temperature distribution and concentration fields of soot and metal-oxide nanoparticles for the flames regardless of the optical thickness. Through increasing detecting lines number, the reconstruction accuracy can be greatly improved due to more flame emission information received by the spectrometer. With the adequate detecting lines number, the estimations for the temperature distribution and concentration fields of soot and metal-oxide nanoparticles in flames with large optical thicknesses were still satisfying even from the noisy radiation intensities with signal to noise ratio (SNR) as low as 46 dB. The results showed that the improved reconstruction model was effective and robust to concurrently retrieve the temperature distribution and volume fraction fields of soot and metal-oxide nanoparticles for the exact and noisy data in nanofluid fuel sooting flames with different optical thicknesses.

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

International Nuclear Information System (INIS)

Afkhami, A.; Madrakian, T.; Saber-Tehrani, M.; Bagheri, H.

2011-01-01

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, N 2 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)

Effect of pointed and diffused air injection on premixed flame confined in a Rijke tube

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Nilaj N. Deshmukh

2016-12-01

Full Text Available The coupling between pressure fluctuations and unsteady heat release in a combustion systems results in acoustic oscillations inside the combustion system. These acoustic oscillations, when grow sufficiently, may cause serious structural damage thereby reducing the lifespan of jet engines, gas turbines, and industrial burners. The aim of the first part of study is to define acoustically stable and unstable regions. The second part is focused on studying the effect of change in pressure field near the flame on the amplitude and frequency of the oscillations of instability. This study is carried out for three-burner positions and equivalence ratio of 0.7 by varying heat supply and total flow rate. The results show two acoustically unstable regions for 0.1 and 0.2 burner positions and only one acoustically unstable region for 0.25 burner position. The effect of pointed injection and diffused injection over a premixed flame on the sound pressure level was studied. The results show for burner position of x/L = 0.2 there is 25 dB suppression is possible using pointed injection at higher total flow rate. The experiment of diffused injection shows sound amplification more than 12 dB was observed.

Extraction and preconcentration of trace levels of cobalt using functionalized magnetic nanoparticles in a sequential injection lab-on-valve system with detection by electrothermal atomic absorption spectrometry

International Nuclear Information System (INIS)

Wang Yang; Luo Xiaoyu; Tang Jie; Hu Xiaoya; Xu Qin; Yang Chun

2012-01-01

Graphical abstract: An approach to performing extraction and preconcentration employing functionalized magnetic particles for the determination of cobalt in the sequential injection lab-on-valve system using detection by electrothermal atomic absorption spectrometry. Highlights: ► New SPE method for cobalt separation/preconcentration was reported. ► Functionalized magnetic nanoparticles were used as adsorbent. ► Extraction, elution, and detection procedures were performed in the LOV system. ► This automatic extraction technique provided a good platform for metal analysis. - Abstract: A new approach to performing extraction and preconcentration employing functionalized magnetic nanoparticles for the determination of trace metals is presented. Alumina-coated iron oxide nanoparticles were synthesized and used as the solid support. The nanoparticles were functionalized with sodium dodecyl sulfate and used as adsorbents for solid phase extraction of the analyte. Extraction, elution, and detection procedures were performed sequentially in the sequential injection lab-on-valve (SI-LOV) system followed by electrothermal atomic absorption spectrometry (ETAAS). Mixtures of hydrophobic analytes were successfully extracted from solution using the synthesized magnetic adsorbents. The potential use of the established scheme was demonstrated by taking cobalt as a model analyte. Under the optimal conditions, the calibration curve showed an excellent linearity in the concentration range of 0.01–5 μg L −1 , and the relative standard deviation was 2.8% at the 0.5 μg L −1 level (n = 11). The limit of detection was 6 ng L −1 with a sampling frequency of 18 h −1 . The present method has been successfully applied to cobalt determination in water samples and two certified reference materials.

Atomic absorption spectrometric determination of copper, zinc, and lead in geological materials

Science.gov (United States)

Sanzolone, R.F.; Chao, T.T.

1976-01-01

An atomic absorption spectrometric method is described for the determination of copper, zinc, and lead in geological materials. The sample is digested with HF-HCl-H2O2; the final solution for analysis is in 10 % (v/v) HCl. Copper and zinc are determined directly by aspirating the solution into an air-acetylene flame. A separate aliquot of the solution is used for determination of lead; lead is extracted into TOPO-MIBK from the acidic solution in the presence of iodide and ascorbic acid. For a 0.50-g sample, the limits of determination are 10-2000 p.p.m. for Cu and Zn, and 5-5000 p.p.m. for Pb. As much as 40 % Fe or Ca. and 10 % Al, Mg, or Mn in the sample do not interfere. The proposed method can be applied to the determination of copper, zinc, and lead in a wide range of geological materials including iron- and manganese-rich, calcareous and carbonate samples. ?? 1976.

Robust parameterization of elastic and absorptive electron atomic scattering factors

International Nuclear Information System (INIS)

Peng, L.M.; Ren, G.; Dudarev, S.L.; Whelan, M.J.

1996-01-01

A robust algorithm and computer program have been developed for the parameterization of elastic and absorptive electron atomic scattering factors. The algorithm is based on a combined modified simulated-annealing and least-squares method, and the computer program works well for fitting both elastic and absorptive atomic scattering factors with five Gaussians. As an application of this program, the elastic electron atomic scattering factors have been parameterized for all neutral atoms and for s up to 6 A -1 . Error analysis shows that the present results are considerably more accurate than the previous analytical fits in terms of the mean square value of the deviation between the numerical and fitted scattering factors. Parameterization for absorptive atomic scattering factors has been made for 17 important materials with the zinc blende structure over the temperature range 1 to 1000 K, where appropriate, and for temperature ranges for which accurate Debye-Waller factors are available. For other materials, the parameterization of the absorptive electron atomic scattering factors can be made using the program by supplying the atomic number of the element, the Debye-Waller factor and the acceleration voltage. For ions or when more accurate numerical results for neutral atoms are available, the program can read in the numerical values of the elastic scattering factors and return the parameters for both the elastic and absorptive scattering factors. The computer routines developed have been tested both on computer workstations and desktop PC computers, and will be made freely available via electronic mail or on floppy disk upon request. (orig.)

Atomization mechanisms for barium in furnace atomic absorption spectrometry

International Nuclear Information System (INIS)

Styris, D.L.

1984-01-01

Atomic absorption spectrometry and mass spectrometry are used simultaneously in order to elucidate atomization mechanisms of barium dichloride in pyrolytic graphite, vitreous carbon, and tantalum furnaces. Gas-phase barium dicarbide is observed to appear concurrently with the free barium. Barium oxide and barium dihydroxide precursors appear with the chlorides. Surface reactions involving species that are absorbed on the various furnaces are postulated to explain the appearances of the species that are observed in the gas phase. 49 references, 4 figures, 1 table

Determination of cadmium in human urine by graphite furnace atomic absorption spectrometry

International Nuclear Information System (INIS)

Shimizu, Tokuo; Shijo, Yoshio; Sakai, Kaoru

1981-01-01

A trace amount of cadmium in human urine was determined by graphite furnace atomic absorption spectrometry. A urine sample (25 ml) was digested with 5 ml of HNO 3 and 30 ml of H 2 O 2 in a long-neck flask on a hot-plate (200 0 C), then diluted to 50 ml. The standard addition method was carried out before digesting. Ten μl of the resulted solution was injected into a tube treated with tungsten carbide, and the cadmium signal was measured with the ramp mode atomization. Interference induced by organic materials in urine was avoided by HNO 3 -H 2 O 2 digestion. Interference induced by inorganic salts could be reduced by 2-fold dilution and tungsten carbide treatment. The cadmium signal was separated sufficiently from the molecular absorption due to NaCl etc. by the ramp mode atomization. Since the blank level of H 2 O 2 was relatively high, the determination was limited to about 0.1 μg/l. The coefficient of variation was 1.76% at 0.36 μg/l in 24 h human urine (n = 4). The time required was (8 -- 10)h. The precision of this method was higher than those of direct methods, and the reasonable values of urine levels of cadmium were obtained. (author)

Water analysis. Determination of elements by atomic absorption

International Nuclear Information System (INIS)

Anon.

Analysis of homogeneous water solutions (plain water, polluted waters, effluents...) by atomic absorption spectrometry with correction for non specific absorption. The quantity ratio is determined by comparison with standard solutions, correction tables are given [fr

Lead preconcentration in synthetic samples with triton x-114 in the cloud point extraction and analysis by atomic absorption (EAAF)

International Nuclear Information System (INIS)

Zegarra Pisconti, Marixa; Cjuno Huanca, Jesus

2015-01-01

A methodology was developed about lead preconcentration in water samples that were added dithizone as complexing agent, previously dissolved in the nonionic surfactant Triton X-114, until the formation of the critical micelle concentration and the cloud point temperature. The centrifuged system gave a precipitate with high concentrations of Pb (II) that was measured by atomic absorption spectroscopy with flame (EAAF). The method has proved feasible to be implemented as a method of preconcentration and analysis of Pb in aqueous samples with concentrations less than 1 ppm. Several parameters were evaluated to obtain a percentage recovery of 89.8%. (author)

Separation and Enrichment of Gold in Water, Geological and Environmental Samples by Solid Phase Extraction on Multiwalled Carbon Nanotubes Prior to its Determination by Flame Atomic Absorption Spectrometry.

Science.gov (United States)

Duran, Ali; Tuzen, Mustafa; Soylak, Mustafa

2015-01-01

This study proposes the application of multi-walled carbon nanotubes as a solid sorbent for the preconcentration of gold prior to its flame atomic absorption spectrometry determination. Extraction was achieved by using a glass column (15.0 cm in length and 1.0 cm in diameter). Quantitative recoveries were obtained in the pH range of 2.5-4.0; the elution step was carried out with 5.0 ml of 1.0 mol/L HNO3 in acetone. In the ligand-free study, variables such as pH, eluent type, sample volume, flow rates, and matrix effect were examined for the optimum recovery of gold ions. The gold ions were able to be pre-concentrated by a factor of 150 and their LOD was determined to be 1.71 μg/L. In order to evaluate the accuracy of the developed method, addition-recovery tests were applied for the tap water, mineral water, and sea water samples. Gold recovery studies were implemented using a wet digestion technique for mine and soil samples taken from various media, and this method was also applied for anodic slime samples taken from the factories located in the Kayseri Industrial Zone of Turkey.

Atomic absorption spectrometry

International Nuclear Information System (INIS)

Haswell, S.J.

1991-01-01

Atomic absorption spectroscopy is now well established and widely used technique for the determination of trace and major elements in a wide range analyte types. There have been many advances in the atomic spectroscopy over the last decade and for this reason and to meet the demand, it was felt that there was a need for an updated book. Whilst interest in instrumental design has tended to dominate the minds of the spectrocopist, the analyst concerned with obtaining reliable and representative data, in diverse areas of application, has been diligently modifying and developing sample treatment and instrumental introduction techniques. Such methodology is de fundamental part of analysis and form the basis of the fourteen application chapters of this book. The text focuses in the main on AAS; however, the sample handling techniques described are in many cases equally applicable to ICP-OES and ICP-MS analysis. (author). refs.; figs.; tabs

Properties of plasma flames sustained by microwaves and burning hydrocarbon fuels

International Nuclear Information System (INIS)

Hong, Yong Cheol; Uhm, Han Sup

2006-01-01

Plasma flames made of atmospheric microwave plasma and a fuel-burning flame were presented and their properties were investigated experimentally. The plasma flame generator consists of a fuel injector and a plasma flame exit connected in series to a microwave plasma torch. The plasma flames are sustained by injecting hydrocarbon fuels into a microwave plasma torch in air discharge. The microwave plasma torch in the plasma flame system can burn a hydrocarbon fuel by high-temperature plasma and high atomic oxygen density, decomposing the hydrogen and carbon containing fuel. We present the visual observations of the sustained plasma flames and measure the gas temperature using a thermocouple device in terms of the gas-fuel mixture and flow rate. The plasma flame volume of the hydrocarbon fuel burners was more than approximately 30-50 times that of the torch plasma. While the temperature of the torch plasma flame was only 868 K at a measurement point, that of the diesel microwave plasma flame with the addition of 0.019 lpm diesel and 30 lpm oxygen increased drastically to about 2280 K. Preliminary experiments for methane plasma flame were also carried out, measuring the temperature profiles of flames along the radial and axial directions. Finally, we investigated the influence of the microwave plasma on combustion flame by observing and comparing OH molecular spectra for the methane plasma flame and methane flame only

Effect of oxygen atoms dissociated by non-equilibrium plasma on flame of methane oxygen and argon pre-mixture gas

Science.gov (United States)

Akashi, Haruaki; Yoshinaga, Tomokazu; Sasaki, Koichi

2014-10-01

For more efficient way of combustion, plasma-assisted combustion has been investigated by many researchers. But it is very difficult to clarify the effect of plasma even on the flame of methane. Because there are many complex chemical reactions in combustion system. Sasaki et al. has reported that the flame length of methane and air premixed burner shortened by irradiating microwave power. They also measured emission from Second Positive Band System of nitrogen during the irradiation. The emission indicates existence of high energy electrons which are accelerated by the microwave. The high energy electrons also dissociate oxygen molecules easily and oxygen atom would have some effects on the flame. But the dissociation ratio of oxygen molecules by the non-equilibrium plasma is significantly low, compared to that in the combustion reaction. To clarify the effect of dissociated oxygen atoms on the flame, dependence of dissociation ratio of oxygen on the flame has been examined using CHEMKIN. It is found that in the case of low dissociation ratio of 10-6, the ignition of the flame becomes slightly earlier. It is also found that in the case of high dissociation ratio of 10-3, the ignition time becomes significantly earlier by almost half. This work was supported by KAKENHI (22340170).

Laser-Induced Photofragmentation Fluorescence Imaging of Alkali Compounds in Flames.

Science.gov (United States)

Leffler, Tomas; Brackmann, Christian; Aldén, Marcus; Li, Zhongshan

2017-06-01

Laser-induced photofragmentation fluorescence has been investigated for the imaging of alkali compounds in premixed laminar methane-air flames. An ArF excimer laser, providing pulses of wavelength 193 nm, was used to photodissociate KCl, KOH, and NaCl molecules in the post-flame region and fluorescence from the excited atomic alkali fragment was detected. Fluorescence emission spectra showed distinct lines of the alkali atoms allowing for efficient background filtering. Temperature data from Rayleigh scattering measurements together with simulations of potassium chemistry presented in literature allowed for conclusions on the relative contributions of potassium species KOH and KCl to the detected signal. Experimental approaches for separate measurements of these components are discussed. Signal power dependence and calculated fractions of dissociated molecules indicate the saturation of the photolysis process, independent on absorption cross-section, under the experimental conditions. Quantitative KCl concentrations up to 30 parts per million (ppm) were evaluated from the fluorescence data and showed good agreement with results from ultraviolet absorption measurements. Detection limits for KCl photofragmentation fluorescence imaging of 0.5 and 1.0 ppm were determined for averaged and single-shot data, respectively. Moreover, simultaneous imaging of KCl and NaCl was demonstrated using a stereoscope with filters. The results indicate that the photofragmentation method can be employed for detailed studies of alkali chemistry in laboratory flames for validation of chemical kinetic mechanisms crucial for efficient biomass fuel utilization.

Two-dimensional atom localization via probe absorption in a four-level atomic system

International Nuclear Information System (INIS)

Wang Zhi-Ping; Ge Qiang; Ruan Yu-Hua; Yu Ben-Li

2013-01-01

We have investigated the two-dimensional (2D) atom localization via probe absorption in a coherently driven four-level atomic system by means of a radio-frequency field driving a hyperfine transition. It is found that the detecting probability and precision of 2D atom localization can be significantly improved via adjusting the system parameters. As a result, our scheme may be helpful in laser cooling or the atom nano-lithography via atom localization

Validation of the methodology for the quantitative determination of lead in cosmetics dyes available in the national market by atomic absorption spectroscopy with flame

International Nuclear Information System (INIS)

Silva Trejos, Paulina

2008-01-01

The analytical methodology was validated to quantify lead in cosmetics dyes available on the national market, by the method of atomic absorption spectroscopy with flame. The samples were digested by wet digestion with HNO 3 to 65% m/m in a microwave oven, the percentage of recovery for the digestion of samples of 0,25 g and 0,45 g in 5,00 mL was of 100,5±0,5. The field of optimal linearity detection limit was 5,0 mg/L with a correlation coefficient of 0,9998. The limits of detection and quantification limits determined graphically by the method of row errors for linear regression of 0,12±0,02 mg/L and 0,21±0,02 mg/L, respectively. Precision was evaluated determining the repeatability as standard deviation of five replicas of a positive dye for lead, according to the definition of the ISO, 2√2*, and obtained a value of 2,3. The veracity was determined through percentages of recovery assessed, adding aliquots of lead patterns to dye samples and compared with the same mass to which they are not make additions. The dye samples were obtained at point of sale, such as pharmacies, beauty suppliers, supermarkets, sales of natural products and the central market of San Jose. The dyes tested contain lead acetates active ingredient, these are: Doni, Mont D'Or, Matador y Siempre Joven; they are produced locally, Youthair brand and American manufacturing. (author) [es

Influence of atomization quality modulation on flame dynamics in a hypergolic rocket engine

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Moritz Schulze

2016-09-01

Full Text Available For the numerical evaluation of the thermoacoustic stability of rocket engines often hybrid methods are applied, which separate the computation of wave propagation in the combustor from the analysis of the flame response to acoustic perturbations. Closure requires a thermoacoustic feedback model which provides the heat release fluctuation in the source term of the employed wave transport equations. The influence of the acoustic fluctuations in the combustion chamber on the heat release fluctuations from the modulation of the atomization of the propellants in a hypergolic upper stage rocket engine is studied. Numerical modeling of a single injector provides the time mean reacting flow field. A network of transfer functions representing all aspects relevant for the feedback model is presented. Analytical models for the injector admittances and for the atomization transfer functions are provided. The dynamics of evaporation and combustion are studied numerically and the numerical results are analyzed. An analytical approximation of the computed flame transfer function is combined with the analytical models for the injector and the atomization quality to derive the feedback model for the wave propagation code. The evaluation of this model on the basis of the Rayleigh index reveals the thermoacoustic driving potential originating from the fluctuating spray quality.

Separation and Preconcentration of Ag(1) in Aqueous Samples by Flotation as an Ion-Associate Using Iodide and Ferroin Followed the Determination by Flame Atomic Absorption Spectrometry

International Nuclear Information System (INIS)

Hosseini, M.S.; Kardan-Moghaddam, G.; Hashemi-Moghaddam, M.

2007-01-01

A simple method for separation/preconcentration and determination of Ag (1) in aqueous samples is described. The method is based on formation of an ion-associate between Ag (1)-iodide complex and ferroin, which can be floated at the interface of the aqueous/n-heptane phases. The flotation process was carried out using 500-ml aliquot of the aqueous solution and the floated layer was dissolved in 5 ml of 1 M HNO 3 containing methanol (50% v/v) as the solvent. The Ag (1) content was then determined by flame atomic absorption spectrometry (FAAS). The method so could be considered as an enrichment process, was achieved to a quantitative feature, when the pH of the solution was adjusted to 4 and the concentrations of iodide and ferroin were about 3.2x10 -4 M and 6.25x10 -5 M, respectively. The LOD and RSD (n=7) were obtained 1.0x10 -8 M and 2.4%, respectively. It was found that a large number of cations and anions even at high considerably foreign ion/Ag(1) ratios were not interfered. The method was applied satisfactorily to recovery of Ag(I) from different aqueous samples

A preconcentration method for indirect determination of acrylamide from chips, crackers and cereal-based baby foods using flame atomic absorption spectrometry.

Science.gov (United States)

Altunay, Nail; Gürkan, Ramazan; Orhan, Ulaş

2016-12-01

Acrylamide is a toxic species for human health, and is a Maillard reaction product which forms spontaneously in heat treatment process of foods. Therefore, a simple, fast and cost-effective method was developed for the indirect determination of acrylamide in processed foods particularly consumed by children. The method is based on ion-pairing of acrylamide with fluorescein (F 2- ) in presence of Ni(II) ions at pH 9.0, and then extraction of the formed ternary complex into micellar phase of poly(ethyleneglycol-mono-p-nonylphenylether) (PONPE 7.5) before analysis by flame atomic absorption spectrometry (FAAS). The ultrasonic-assisted cloud point extraction (UA-CPE) has been used for the preconcentration of acrylamide in the samples prior to its FAAS detection. The matrix matched calibration curve is linear in range of 0.3-150µgkg -1 under optimal reagent conditions (1.75mL of 0.1molL -1 ammonia buffer at pH 9.0, 2.2mgL -1 Ni(II), 4.0×10 -4 molL -1 F 2- , 0.4% (w/v) NH 4 Cl and 0.7% (v/v) PONPE 7.5) with sensitivity enhancement of 160-fold. The proposed method has been validated by assessment of the following parameters; the limits of detection (LOD) and quantification (LOQ) (0.08µgkg -1 and 0.28µgkg -1 , respectively) with a relative standard deviation (RSD%) lower than 6.3%, and extractive recovery higher than 95% for acrylamide spiked at levels of 5 and 25µgkg -1 . The method was successfully applied to the indirect determination of acrylamide in the processed foods and two CRMs with satisfactory results. Copyright © 2016 Elsevier B.V. All rights reserved.

Novel analytical reagent for the application of cloud-point preconcentration and flame atomic absorption spectrometric determination of nickel in natural water samples

International Nuclear Information System (INIS)

Suvardhan, K.; Rekha, D.; Kumar, K. Suresh; Prasad, P. Reddy; Kumar, J. Dilip; Jayaraj, B.; Chiranjeevi, P.

2007-01-01

Cloud-point extraction was applied as a preconcentration of nickel after formation of complex with newly synthesized N-quino[8,7-b]azin-5-yl-2,3,5,6,8,9,11,12octahydrobenzo[b][1,4,7,10,13] pentaoxacyclopentadecin-15-yl-methanimine, and later determined by flame atomic absorption spectrometry (FAAS) using octyl phenoxy polyethoxy ethanol (Triton X-114) as surfactant. Nickel was complexed with N-quino[8,7-b]azin-5-yl-2,3,5,6,8,9,11,12 octahydrobenzo[b][1,4,7,10,13]pentaoxacyclopentadecin-15-yl-methanimine in an aqueous phase and was kept for 15 min in a thermo-stated bath at 40 deg. C. Separation of the two phases was accomplished by centrifugation for 15 min at 4000 rpm. The chemical variables affecting the cloud-point extraction were evaluated, optimized and successfully applied to the nickel determination in various water samples. Under the optimized conditions, the preconcentration system of 100 ml sample permitted an enhancement factor of 50-fold. The detailed study of various interferences made the method more selective. The detection limits obtained under optimal condition was 0.042 ng ml -1 . The extraction efficiency was investigated at different nickel concentrations (20-80 ng ml -1 ) and good recoveries (99.05-99.93%) were obtained using present method. The proposed method has been applied successfully for the determination of nickel in various water samples and compared with reported method in terms of Student's t-test and variance ratio f-test which indicate the significance of present method over reported and spectrophotometric methods at 95% confidence level

Quality assessment of trace Cd and Pb contaminants in Thai herbal medicines using ultrasound-assisted digestion prior to flame atomic absorption spectrometry

Directory of Open Access Journals (Sweden)

Watsaka Siriangkhawut

2017-10-01

Full Text Available A simple, efficient, and reliable ultrasound-assisted digestion (UAD procedure was used for sample preparation prior to quantitative determination of trace Cd and Pb contaminants in herbal medicines using flame atomic absorption spectrometry. The parameters influencing UAD such as the solvent system, sample mass, presonication time, sonication time, and digestion temperature were evaluated. The efficiency of the proposed UAD procedure was evaluated by comparing with conventional acid digestion (CAD procedure. Under the optimum conditions, linear calibration graphs in a range of 2–250 μg/L for Cd, and 50–1000 μg/L for Pb were obtained with detection limits of 0.56 μg/L and 10.7 μg/L for Cd and Pb, respectively. The limit of quantification for Cd and Pb were 1.87 μg/L and 40.3 μg/L, respectively. The repeatability for analysis of 10 μg/L for Cd and 100 μg/L for Pb was 2.3% and 2.6%, respectively. The accuracy of the proposed method was evaluated by rice flour certified reference materials. The proposed method was successfully applied for analysis of trace Cd and Pb in samples of various types of medicinal plant and traditional medicine consumed in Thailand. Most herbal medicine samples were not contaminated with Cd or Pb. The contaminant levels for both metals were still lower than the maximum permissible levels of elements in medicinal plant materials and finished herbal products sets by the Ministry of Public Health of Thailand. The exception was the high level of Cd contamination found in two samples of processed medicinal plants.

Theoretical calculation of saturated absorption for multilevel atoms

International Nuclear Information System (INIS)

O'Kane, T.J.; Scholten, R.E.; Farrell, P.M.

1998-01-01

We present the first theoretical saturated absorption spectra for general multi-level atoms, using a model based on extensions of the optical Bloch equations, and using Monte Carlo averaging of the absorption of individual atoms with random trajectories through a standing wave. We are for the first time able to accurately predict the merging of hyperfine and cross-over resonances due to intensity dependent phenomena such as power broadening. Results for 20-level sodium and 24-level rubidium models are presented and compared to experiment, demonstrating excellent agreement

Speciation of Tl(III and Tl(I in hair samples by dispersive liquid–liquid microextraction based on solidification of floating organic droplet prior to flame atomic absorption spectrometry determination

Directory of Open Access Journals (Sweden)

S.Z. Mohammadi

2016-11-01

Full Text Available Dispersive liquid–liquid microextraction based on solidification of floating organic droplet was successfully used as a sample preparation method prior to flame atomic absorption determination of trace amounts of Tl(III and Tl(I in hair samples. In the proposed method, 1-(2-pyridylazo-2-naphthol, 1-dodecanol and ethanol were used as chelating agent, extraction and dispersive solvent, respectively. Several factors that may be affected in the extraction process, such as type and volume of extraction and disperser solvents, pH, salting out effect, ionic strength and extraction time were studied. Under the optimal conditions, linearity was maintained between 6.0 and 900.0 ng mL−1 for Tl(III. The relative standard deviation for seven replicate determinations of 0.2 μg mL−1 Tl(III was 2.5%. The detection limit based on 3Sb for Tl(III in the original solution was 2.1 ng mL−1. The proposed method has been applied for the determination of trace amounts of thallium in hair samples and satisfactory results were obtained.

Influence of circulating epinephrine on absorption of subcutaneously injected insulin

International Nuclear Information System (INIS)

Fernqvist, E.; Gunnarsson, R.; Linde, B.

1988-01-01

Effects of epinephrine (Epi) infusion on the absorption of subcutaneously injected 125I-labeled soluble human insulin (10 U) from the thigh or the abdomen were studied in 16 healthy subjects and from the thigh in 10 insulin-dependent diabetic (IDDM) patients. Epi was infused at 0.3 (high dose) or 0.1 (low dose; healthy subjects) nmol.kg-1.min-1 i.v., resulting in arterial plasma Epi levels of approximately 6 and 2 nM, respectively. Saline was infused on a control day. Insulin absorption was measured as disappearance of radioactivity from the injection site and as appearance of plasma immunoreactive insulin (IRI). Adipose tissue blood flow was measured with the 133Xe clearance technique. First-order disappearance rate constants of 125I from the thigh depot decreased approximately 40-50% during the high dose of Epi compared with control (P less than .001). The corresponding decrease from the abdominal depot was approximately 40% (P less than .001), whereas no significant change was found during the low Epi dose. IRI fell compared with control in all groups at the high Epi dose. The Epi-induced depression of insulin absorption occurred despite unaltered or even slightly increased subcutaneous blood flow. The results indicate that circulating Epi at levels seen during moderate physical stress depresses the absorption of soluble insulin from subcutaneous injection sites to an extent that might be important for glycemic control in IDDM patients. Furthermore, dissociation is found between changes in insulin absorption and subcutaneous blood flow during Epi infusion, suggesting that factors other than blood flow may also influence the absorption of subcutaneously injected insulin

[The reconstruction of two-dimensional distributions of gas concentration in the flat flame based on tunable laser absorption spectroscopy].

Science.gov (United States)

Jiang, Zhi-Shen; Wang, Fei; Xing, Da-Wei; Xu, Ting; Yan, Jian-Hua; Cen, Ke-Fa

2012-11-01

The experimental method by using the tunable diode laser absorption spectroscopy combined with the model and algo- rithm was studied to reconstruct the two-dimensional distribution of gas concentration The feasibility of the reconstruction program was verified by numerical simulation A diagnostic system consisting of 24 lasers was built for the measurement of H2O in the methane/air premixed flame. The two-dimensional distribution of H2O concentration in the flame was reconstructed, showing that the reconstruction results reflect the real two-dimensional distribution of H2O concentration in the flame. This diagnostic scheme provides a promising solution for combustion control.

Analytical Absorption Cross-Section for Photon by a Hydrogen 2s Atom

International Nuclear Information System (INIS)

Ndinya, Boniface Otieno; Okeyo, Stephen Onyango

2011-01-01

We calculate the absorption cross-section for photon by a hydrogen 2s atom using the quantum-classical approximation for the total photo cross-section of many electron atoms. With the application of the first-order term of the Baker-Hausdorf expansion, the absorption cross-section for the hydrogen 2s atom decreases to a minimum, the Cooper pair minimum, at low photon energy. Such a minimum is absent in the exact absorption cross-section for photon by a hydrogen 2s atom. We have extended the calculation for the absorption cross-section of the hydrogen 2s atom using the quantum-classical approximation for the total photo cross-section of many electron to include the second-order term of the Baker-Hausdorf expansion and observed a great reduction in the dip associated with the Cooper pair minimum at the zero crossing. (atomic and molecular physics)

Determination of As, Cd, Cu, Hg and Pb in biological samples by modern electrothermal atomic absorption spectrometry

International Nuclear Information System (INIS)

Sardans, Jordi; Montes, Fernando; Penuelas, Josep

2010-01-01

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 μg L -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 of

Determination of As, Cd, Cu, Hg and Pb in biological samples by modern electrothermal atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

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

Atomic absorption spectrometric determination of mineral elements in mammalian bones

International Nuclear Information System (INIS)

Udoh, Anthony P.

2000-01-01

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)

Turbulent structure and emissions of strongly-pulsed jet diffusion flames

Science.gov (United States)

Fregeau, Mathieu

This current research project studied the turbulent flame structure, the fuel/air mixing, the combustion characteristics of a nonpremixed pulsed (unsteady) and unpulsed (steady) flame configuration for both normal- and microgravity conditions, as well as the flame emissions in normal gravity. The unsteady flames were fully-modulated, with the fuel flow completely shut off between injection pulses using an externally controlled valve, resulting in the generation of compact puff-like flame structures. Conducting experiments in normal and microgravity environments enabled separate control over the relevant Richardson and Reynolds numbers to clarify the influence of buoyancy on the flame behavior, mixing, and structure. Experiments were performed in normal gravity in the laboratory at the University of Washington and in microgravity using the NASA GRC 2.2-second Drop Tower facility. High-speed imaging, as well as temperature and emissions probes were used to determine the large-scale structure dynamics, the details of the flame structure and oxidizer entrainment, the combustion temperatures, and the exhaust emissions of the pulsed and steady flames. Of particular interest was the impact of changes in flame structure due to pulsing on the combustion characteristics of this system. The turbulent flame puff celerity (i.e., the bulk velocity of the puffs) was strongly impacted by the jet-off time, increasing markedly as the time between pulses was decreased, which caused the degree of puff interaction to increase and the strongly-pulsed flame to more closely resemble a steady flame. This increase occurred for all values of injection time as well as for constant fuelling rate and in both the presence and absence of buoyancy. The removal of positive buoyancy in microgravity resulted in a decrease in the flame puff celerity in all cases, amounting to as much as 40%, for both constant jet injection velocity and constant fuelling rate. The mean flame length of the strongly

Cu determination in crude oil distillation products by atomic absorption and inductively coupled plasma mass spectrometry after analyte transfer to aqueous solution

Science.gov (United States)

Kowalewska, Zofia; Ruszczyńska, Anna; Bulska, Ewa

2005-03-01

Cu was determined in a wide range of petroleum products from crude oil distillation using flame atomic absorption spectrometry (FAAS), electrothermal atomic absorption spectrometry (ETAAS) and inductively coupled plasma mass spectrometry (ICP-MS). Different procedures of sample preparation were evaluated: (i) mineralization with sulfuric acid in an open system, (ii) mineralization in a closed microwave system, (iii) combustion in hydrogen-oxygen flame in the Wickbold's apparatus, (iv) matrix evaporation followed by acid dissolution, and (v) acidic extraction. All the above procedures led to the transfer of the analyte into an aqueous solution for the analytical measurement step. It was found that application of FAAS was limited to the analysis of the heaviest petroleum products of high Cu content. In ICP-MS, the use of internal reference method (with Rh or In as internal reference element) was required to eliminate the matrix effects in the analysis of extracts and the concentrated solutions of mineralized heavy petroleum products. The detection limits (in original samples) were equal to, respectively, 10, 86, 3.3, 0.9 and 0.4 ng g - 1 in procedures i-v with ETAAS detection and 10, 78, 1.1 and 0.5 ng g - 1 in procedures i-iii and v with ICP-MS detection. The procedures recommended here were validated by recovery experiments, certified reference materials analysis and comparison of results, obtained for a given sample, in different ways. The Cu content in the analyzed samples was: 50-110 ng g - 1 in crude oil, oil, oil and 140-300 ng g - 1 in distillation residue.

Ligandless surfactant mediated solid phase extraction combined with Fe₃O₄ nano-particle for the preconcentration and determination of cadmium and lead in water and soil samples followed by flame atomic absorption spectrometry: multivariate strategy.

Science.gov (United States)

Jalbani, N; Soylak, M

2014-04-01

In the present study, a microextraction technique combining Fe3O4 nano-particle with surfactant mediated solid phase extraction ((SM-SPE)) was successfully developed for the preconcentration/separation of Cd(II) and Pb(II) in water and soil samples. The analytes were determined by flame atomic absorption spectrometry (FAAS). The effective variables such as the amount of adsorbent (NPs), the pH, concentration of non-ionic (TX-114) and centrifugation time (min) were investigated by Plackett-Burman (PBD) design. The important variables were further optimized by central composite design (CCD). Under the optimized conditions, the detection limits (LODs) of Cd(II) and Pb(II) were 0.15 and 0.74 µg/L, respectively. The validation of the proposed procedure was checked by the analysis of certified reference materials of TMDA 53.3 fortified water and GBW07425 soil. The method was successfully applied for the determination of Cd(II) and Pb(II) in water and soil samples. Copyright © 2014 Elsevier Inc. All rights reserved.

Separation and preconcentration of cadmium ions in natural water using a liquid membrane system with 2-acetylpyridine benzoylhydrazone as carrier by flame atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Granado-Castro, M.D.; Galindo-Riano, M.D. E-mail: dolores.galindo@uca.es; Garcia-Vargas, Manuel

2004-04-30

A method for the determination of Cd in natural water by flame atomic absorption spectrometry after separation and preconcentration with a bulk liquid membrane containing 2-acetylpyridine benzoylhydrazone as mobile carrier dissolved in toluene has been developed. Effects of carrier concentration, volume of organic phase and pH of feed and receiving solutions on the flux for Cd across the membrane have been studied, being optimized by the modified simplex method. Optimum values for these variables were: carrier concentration of 0.84 g l{sup -1}, 74 ml of toluene, pH 7.8 in the feed solution and 0.06 mol l{sup -1} of HNO{sub 3} in the receiving solution, allowing a preconcentration factor of 17.9. The preconcentration step required 7 h to be accomplished. The recovery of Cd at optimum conditions was 101.0{+-}2.7%, even with saline matrix, with good relative standard deviation (2.5%) at 95% confidence level. The detection limit of blank sample was 6 ng l{sup -1} of Cd. The method was validated using a certified reference material (TMDA-62) and also applied successfully to the analysis of Cd in four samples of seawater collected from the coast of Huelva (Spain). The relative errors of determinations were -7.6% for certified reference material and ranging between +2.4 and +7.1%, for samples of seawater (obtained between the results of the proposed and differential pulse anodic stripping voltammetry methods)

Buffer choice and effects of sample composition examined by experiment planning methods for determination of molybdenum by atomic absorption with a flame atomizer

International Nuclear Information System (INIS)

Zav'yalkov, P.I.; Danishehvskii, A.L.; Rakita, R.A.; Yakshinskii, A.I.

1986-01-01

The authors use orthogonal experiment planning to define the optimum form of buffer and to establish the effects of sample composition since there are high levels of cation and anion interference in the atomic-absorption determination of molybdenum. A spectroscopic buffer has been identified (HCLO 4 + NH 4 Cl mixture), which eliminates the interference from the elements tested and improves the analytical characteristics in determining molybdenum. A model has been formulated enabling one to estimate the buffer performance and the effects of the components on the determination of molybdenum. The model enables one to forecast the expected order of the effect without performing additional experiments

evaluation of atomic absorption spectrophotometry (ashing, non ...

African Journals Online (AJOL)

cistvr

1Department of Agricultural and Food Science and 2Department of ... used techniques, namely atomic absorption spectrophotometry (AAS-Ashing and ..... fact that more preparation steps were involved in the Ashing procedure and thus.

Atomic and ionic density measurement by laser absorption spectroscopy of magnetized or non-magnetized plasmas

International Nuclear Information System (INIS)

Le Gourrierec, P.

1989-11-01

Laser absorption spectroscopy is an appreciated diagnostic in plasma physics to measure atomic and ionic densities. We used it here more specifically on metallic plasmas. Firstly, a uranium plasma was created in a hollow cathode. 17 levels of U.I and U.II (12 for U.I and 5 for U.II) are measured by this method. The results are compared with the calculated levels of two models (collisional-radiative and LTE). Secondly, the theory of absorption in presence of a magnetic field is recalled and checked. Then, low-density magnetized plasma produced on our ERIC experiment (acronym for Experiment of Resonance Ionic Cyclotron), have been diagnosed successfully. The use of this technique on a low density plasma has not yet been published to our knowledge. The transverse temperature and the density of a metastable atomic level of a barium plasma has been derived. The evolution of a metastable ionic level of this element is studied in terms of two source parameters (furnace temperature and injected hyperfrequency power) [fr

Nonresonant absorption of one photon by one atom and resonant absorption of two photons by two atoms

International Nuclear Information System (INIS)

Mizushima, Masataka

1990-01-01

When a radiation field of frequency ω 1 interacts with atoms, etch of which has a transition frequency ω ba =(E b -E a )/h, with ω 1 -ω ba =Δ≠0, nonresonant absorption can take place with probability P 1 inversely proportional to Δ 2 (a pressure broadening). When another radiation field of frequency ω 2 , such that ω 1 +ω 2 =2ω ba, interacts simultaneously with the gas a resonant two-photon absorption can take place in addition to the nonresonant absorption. The probability of this two-photon absorption process, P 2 , is found to be inversely proportional to Δ 4 . If Ω=| | is the Rabi frequency of the transition, it is found that P 2 /(P 1 (Δ)+P 1 (-Δ)) is given by 12 {Ω(-Δ)Ω(-Δ)} 2 / {Δ 2 (Ω(-Δ) 2 + Ω(Δ) 2 )}. (author)

Automated atomic absorption spectrophotometer, utilizing a programmable desk calculator

International Nuclear Information System (INIS)

Futrell, T.L.; Morrow, R.W.

1977-01-01

A commercial, double-beam atomic absorption spectrophotometer has been interfaced with a sample changer and a Hewlett-Packard 9810A calculator to yield a completely automated analysis system. The interface electronics can be easily constructed and should be adaptable to any double-beam atomic absorption instrument. The calculator is easily programmed and can be used for general laboratory purposes when not operating the instrument. The automated system has been shown to perform very satisfactorily when operated unattended to analyze a large number of samples. Performance statistics agree well with a manually operated instrument

Evaluation of cadmium, lead, copper, iron and zinc in Turkish dietary vegetable oils and olives using electrothermal and flame atomic absorption spectrometry

Directory of Open Access Journals (Sweden)

Acar, Orhan

2012-10-01

Full Text Available The Cd, Pb, Cu, Fe and Zn contents of some edible vegetable oils (soybean, sunflower, flower, nut, corn and olive and of olives (olive-1, black, green, black crushed with seeds and green crushed with seeds were determined and evaluated by an electrothermal atomic absorption spectrometer (ETAAS using an Sc + Ir + NH₄H₂PO₄ chemical modifier mixture and flame atomic absorption spectrometer (FAAS after microwave digestion. The pyrolysis and atomization temperatures of Cd, Pb and Cu in sample solutions with and without the modifier mixture were investigated. The limits of detection (LOD for analytes found are 0.1, 0.6, 0.9, 15.0 and 12.0 μg L^–1 for Cd, Cu, Pb, Fe and Zn, respectively. The accuracy of the procedure proposed was confirmed by analyzing bovine liver 1577b standard reference material (SRM and a spiked sample solution. The results of the analytes found were compared with certified and added values. The relative standard deviations of the analytes found were lower than 7% and the percent of recoveries obtained ranges from 96 to 101%. The Sc + Ir + NH₄H₂PO₄ mixture proposed was applied for the determination of Cd, Pb and Cu in oils and olives. The results of analytes found in the samples were compared with international and national food quality guidelines as well as with literature values.

Se han determinado los metales Cd, Cu, Pb, Fe y Zn en aceites vegetales comestibles (soja, girasol, flores, nueces, maíz y aceite de oliva y aceitunas (aceitunas-1, negra, verde, negra machacadas con semillas y verde machacadas con semillas mediante espectrometría de absorción atómica electrotérmica (ETAAS utilizando como modificador químico la mezcla Sc + Ir + NH₄H₂PO₄ y mediante espectrometría de absorción atómica de llama (FAAS tras digestión con microondas. Se estudiaron las temperaturas de pirólisis y atomización para Cd

Cu determination in crude oil distillation products by atomic absorption and inductively coupled plasma mass spectrometry after analyte transfer to aqueous solution

International Nuclear Information System (INIS)

Kowalewska, Zofia; Ruszczynska, Anna; Bulska, Ewa

2005-01-01

Cu was determined in a wide range of petroleum products from crude oil distillation using flame atomic absorption spectrometry (FAAS), electrothermal atomic absorption spectrometry (ETAAS) and inductively coupled plasma mass spectrometry (ICP-MS). Different procedures of sample preparation were evaluated: (i) mineralization with sulfuric acid in an open system (ii) mineralization in a closed microwave system (iii) combustion in hydrogen-oxygen flame in the Wickbold's apparatus (iv) matrix evaporation followed by acid dissolution, and (v) acidic extraction. All the above procedures led to the transfer of the analyte into an aqueous solution for the analytical measurement step. It was found that application of FAAS was limited to the analysis of the heaviest petroleum products of high Cu content. In ICP-MS, the use of internal reference method (with Rh or In as internal reference element) was required to eliminate the matrix effects in the analysis of extracts and the concentrated solutions of mineralized heavy petroleum products. The detection limits (in original samples) were equal to, respectively, 10, 86, 3.3, 0.9 and 0.4 ng g -1 in procedures i-v with ETAAS detection and 10, 78, 1.1 and 0.5 ng g -1 in procedures i-iii and v with ICP-MS detection. The procedures recommended here were validated by recovery experiments, certified reference materials analysis and comparison of results, obtained for a given sample, in different ways. The Cu content in the analyzed samples was: 50-110 ng g -1 in crude oil, -1 in gasoline, -1 in atmospheric oil, -1 in heavy vacuum oil and 140-300 ng g -1 in distillation residue

On-line dynamic extraction and automated determination of readily bioavailable hexavalent chromium in solid substrates using micro-sequential injection bead-injection lab-on-valve hyphenated with electrothermal atomic absorption spectrometry

DEFF Research Database (Denmark)

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

2006-01-01

A novel and miniaturized micro-sequential injection bead injection lab-on-valve (μSI-BI-LOV) fractionation system was developed for in-line microcolumn soil extraction under simulated environmental scenarios and accurate monitoring of the content of easily mobilisable hexavalent chromium in soil...... environments at the sub-low parts-per-million level. The flow system integrates dynamic leaching of hexavalent chromium using deionized water as recommended by the German Standard DIN 38414-S4 method; on-line pH adjustment of the extract by a 0.01 mol L-1 Tris-HNO3 buffer solution; isolation of the chromate...... polluted agricultural soil material (San Joaquin Soil-Baseline Trace Element Concentrations) with water-soluble Cr(VI) salts at different concentration levels. The potential of the μSI-BI-LOV set-up with renewable surfaces for flame-AAS determination of high levels of readily bioavailable chromate...

Applicability of cloud point extraction for the separation trace amount of lead ion in environmental and biological samples prior to determination by flame atomic absorption spectrometry

Directory of Open Access Journals (Sweden)

Sayed Zia Mohammadi

2016-09-01

Full Text Available A sensitive cloud point extraction procedure(CPE for the preconcentration of trace lead prior to its determination by flame atomic absorption spectrometry (FAAS has been developed. The CPE method is based on the complex of Pb(II ion with 1-(2-pyridylazo-2-naphthol (PAN, and then entrapped in the non-ionic surfactant Triton X-114. The main factors affecting CPE efficiency, such as pH of sample solution, concentration of PAN and Triton X-114, equilibration temperature and time, were investigated in detail. A preconcentration factor of 30 was obtained for the preconcentration of Pb(II ion with 15.0 mL solution. Under the optimal conditions, the calibration curve was linear in the range of 7.5 ng mL−1–3.5 μg mL−1 of lead with R2 = 0.9998 (n = 10. Detection limit based on three times the standard deviation of the blank (3Sb was 5.27 ng mL−1. Eight replicate determinations of 1.0 μg mL−1 lead gave a mean absorbance of 0.275 with a relative standard deviation of 1.6%. The high efficiency of cloud point extraction to carry out the determination of analytes in complex matrices was demonstrated. The proposed method has been applied for determination of trace amounts of lead in biological and water samples with satisfactory results.

Gold volatile species atomization and preconcentration in quartz devices for atomic absorption spectrometry

Czech Academy of Sciences Publication Activity Database

Arslan, Y.; Musil, Stanislav; Matoušek, Tomáš; Kratzer, Jan; Dědina, Jiří

103-104, JAN-FEB (2015), s. 155-163 ISSN 0584-8547 R&D Projects: GA ČR GA14-23532S Grant - others:GA AV ČR(CZ) M200311202 Institutional support: RVO:68081715 Keywords : gold * volatile species generation * quartz atomizers * atomic absorption spectrometry Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.289, year: 2015

Anomalies in resonant absorption line profiles of atoms with large hyperfine splitting

International Nuclear Information System (INIS)

Parkhomenko, A.I.; Pod'yachev, S.P.; Privalov, T.I.; Shalagin, A.M.

1997-01-01

We examine a monochromatic absorption line in the velocity-nonselective excitation of atoms when the components of the hyperfine stricture of the electronic ground states are optically pumped. We show that the absorption lines possess unusual substructures for some values of the hyperfine splitting of the ground state (which exceed the Doppler absorption linewidth severalfold). These substructures in the absorption spectrum are most apparent if the hyperfine structure of the excited electronic state is taken into account. We calculate the absorption spectra of monochromatic light near the D 1 and D 2 lines of atomic rubidium 85,87 Rb. With real hyperfine splitting taken into account, the D 1 and D 2 lines are modeled by 4- and 6-level diagrams, respectively. Finally, we show that atomic rubidium vapor can be successfully used to observe the spectral features experimentally

Abdominal mesotherapy injection extended the absorption of follicle-stimulating hormone.

Science.gov (United States)

Hsu, Chao-Chin; Kuo, Hsin-Chih; Hsu, Chao-Tien; Gu, Qing

2011-05-01

Abdominal mesotherapy injection of recombinant human FSH (rhFSH) was well tolerated with increased net absorption (AUC0-∞ 4,655.3 IU·h/L and t1/2 247.6 h) up to 360 hours compared with those of 120 hours (AUC0-∞ 1,915.7 IU·h/L and t1/2 101.8 h). The extended absorption of rhFSH suggests that abdominal mesotherapy injection mode be considered for future administration of rhFSH in controlled ovarian hyperstimulation. Copyright © 2011 American Society for Reproductive Medicine. Published by Elsevier Inc. All rights reserved.

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

International Nuclear Information System (INIS)

Arikawa, Yoshiko; Hirai, Shoji; Ozawa, Takejiro.

1979-01-01

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)

Methylmercury determination using a hyphenated high performance liquid chromatography ultraviolet cold vapor multipath atomic absorption spectrometry system

Energy Technology Data Exchange (ETDEWEB)

Campos, Reinaldo C. [Department of Chemistry, Pontifical Catholic University of Rio de Janeiro, Rua Marques de S Vicente 225, 22453-900 Rio de Janeiro (Brazil)], E-mail: rccampos@puc-rio.br; Goncalves, Rodrigo A.; Brandao, Geisamanda P.; Azevedo, Marlo S. [Department of Chemistry, Pontifical Catholic University of Rio de Janeiro, Rua Marques de S Vicente 225, 22453-900 Rio de Janeiro (Brazil); Oliveira, Fabiana; Wasserman, Julio [Institut of Geosciences, Fluminense Federal University, Av. Gal. Milton Tavares de Souza, s/n, 24.210-340, Niteroi, Rio de Janeiro (Brazil)

2009-06-15

The present work investigates the use of a multipath cell atomic absorption mercury detector for mercury speciation analysis in a hyphenated high performance liquid chromatography assembly. The multipath absorption cell multiplies the optical path while energy losses are compensated by a very intense primary source. Zeeman-effect background correction compensates for non-specific absorption. For the separation step, the mobile phase consisted in a 0.010% m/v mercaptoethanol solution in 5% methanol (pH = 5), a C{sub 18} column was used as stationary phase, and post column treatment was performed by UV irradiation (60 deg. C, 13 W). The eluate was then merged with 3 mol L{sup -1} HCl, reduction was performed by a NaBH{sub 4} solution, and the Hg vapor formed was separated at the gas-liquid separator and carried through a desiccant membrane to the detector. The detector was easily attached to the system, since an external gas flow to the gas-liquid separator was provided. A multivariate approach was used to optimize the procedure and peak area was used for measurement. Instrumental limits of detection of 0.05 {mu}g L{sup -1} were obtained for ionic (Hg{sup 2+}) and HgCH{sub 3}{sup +}, for an injection volume of 200 {mu}L. The multipath atomic absorption spectrometer proved to be a competitive mercury detector in hyphenated systems in relation to the most commonly used atomic fluorescence and inductively coupled plasma mass spectrometric detectors. Preliminary application studies were performed for the determination of methyl mercury in sedi0011men.

Methylmercury determination using a hyphenated high performance liquid chromatography ultraviolet cold vapor multipath atomic absorption spectrometry system

International Nuclear Information System (INIS)

Campos, Reinaldo C.; Goncalves, Rodrigo A.; Brandao, Geisamanda P.; Azevedo, Marlo S.; Oliveira, Fabiana; Wasserman, Julio

2009-01-01

The present work investigates the use of a multipath cell atomic absorption mercury detector for mercury speciation analysis in a hyphenated high performance liquid chromatography assembly. The multipath absorption cell multiplies the optical path while energy losses are compensated by a very intense primary source. Zeeman-effect background correction compensates for non-specific absorption. For the separation step, the mobile phase consisted in a 0.010% m/v mercaptoethanol solution in 5% methanol (pH = 5), a C 18 column was used as stationary phase, and post column treatment was performed by UV irradiation (60 deg. C, 13 W). The eluate was then merged with 3 mol L -1 HCl, reduction was performed by a NaBH 4 solution, and the Hg vapor formed was separated at the gas-liquid separator and carried through a desiccant membrane to the detector. The detector was easily attached to the system, since an external gas flow to the gas-liquid separator was provided. A multivariate approach was used to optimize the procedure and peak area was used for measurement. Instrumental limits of detection of 0.05 μg L -1 were obtained for ionic (Hg 2+ ) and HgCH 3 + , for an injection volume of 200 μL. The multipath atomic absorption spectrometer proved to be a competitive mercury detector in hyphenated systems in relation to the most commonly used atomic fluorescence and inductively coupled plasma mass spectrometric detectors. Preliminary application studies were performed for the determination of methyl mercury in sediments.

Reliability of graphite furnace atomic absorption spectrometry as ...

African Journals Online (AJOL)

spectrometry as alternative method for trace analysis of ... Purpose: To evaluate the comparative efficiency of graphite furnace atomic absorption spectrometry .... Methods comparison and validation .... plasma-optical emission spectrometry.

Simultaneous determination of antimony and boron in beverage and dairy products by flame atomic absorption spectrometry after separation and pre-concentration by cloud-point extraction.

Science.gov (United States)

Altunay, Nail; Gürkan, Ramazan

2016-01-01

A new cloud-point extraction (CPE) method was developed for the pre-concentration and simultaneous determination of Sb(III) and B(III) by flame atomic absorption spectrometry (FAAS). The method was based on complexation of Sb(III) and B(III) with azomethine-H in the presence of cetylpyridinium chloride (CPC) as a signal-enhancing agent, and then extraction into the micellar phase of Triton X-114. Under optimised conditions, linear calibration was obtained for Sb(III) and B(III) in the concentration ranges of 0.5-180 and 2.5-600 μg l(-1) with LODs of 0.15 and 0.75 μg l(-1), respectively. Relative standard deviations (RSDs) (25 and 100 μg l(-1) of Sb(III) and B(III), n = 6) were in a range of 2.1-3.8% and 1.9-2.3%, respectively. Recoveries of spiked samples of Sb(III) and B(III) were in the range of 98-103% and 99-102%, respectively. Measured values for Sb and B in three standard reference materials were within the 95% confidence limit of the certified values. Also, the method was used for the speciation of inorganic antimony. Sb(III), Sb(V) and total Sb were measured in the presence of excess boron before and after pre-reduction with an acidic mixture of KI-ascorbic acid. The method was successfully applied to the simultaneous determination of total Sb and B in selected beverage and dairy products.

Control of electrolytic refinement of silver by atomic absorption method

International Nuclear Information System (INIS)

Kulish, N.G.; Burylev, B.P.

1983-01-01

Results of atomic absorption determination of 18 elements: Fe, Cu, Zn, Cd, Bi, Ga, In, Ca, Mg, K, Na, Sb, Te, Ni, Co, Cr, Mn, Pb in silver and electrolytes are presented. When determining impurities in silver the basis has been separated by the extraction of O-isopropyl-N-ethyl thiocarbamate in the 1M HN0 3 medium. Optimum measuring conditions and the range of linear dependence between concentration and atomic absorption value are given

Speciation analysis of arsenic by selective hydride generation- cryotrapping-atomic fluorescence spectrometry with flame-in-gas- shield atomizer: Achieving extremely low detection limits with inexpensive instrumentation

Czech Academy of Sciences Publication Activity Database

Musil, Stanislav; Matoušek, Tomáš; Currier, J. M.; Stýblo, M.; Dědina, Jiří

2014-01-01

Roč. 86, č. 20 (2014), s. 10422-10428 ISSN 0003-2700 R&D Projects: GA ČR GA14-23532S; GA MŠk LH12040 Institutional support: RVO:68081715 Keywords : speciation analysis of arsenic * selective hydride generation * flame-in-gas-shield atomizer * cryotrapping-atomic fluorescence spectrometry Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 5.636, year: 2014

Precision atomic beam density characterization by diode laser absorption spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Oxley, Paul; Wihbey, Joseph [Physics Department, The College of the Holy Cross, Worcester, Massachusetts 01610 (United States)

2016-09-15

We provide experimental and theoretical details of a simple technique to determine absolute line-of-sight integrated atomic beam densities based on resonant laser absorption. In our experiments, a thermal lithium beam is chopped on and off while the frequency of a laser crossing the beam at right angles is scanned slowly across the resonance transition. A lock-in amplifier detects the laser absorption signal at the chop frequency from which the atomic density is determined. The accuracy of our experimental method is confirmed using the related technique of wavelength modulation spectroscopy. For beams which absorb of order 1% of the incident laser light, our measurements allow the beam density to be determined to an accuracy better than 5% and with a precision of 3% on a time scale of order 1 s. Fractional absorptions of order 10{sup −5} are detectable on a one-minute time scale when we employ a double laser beam technique which limits laser intensity noise. For a lithium beam with a thickness of 9 mm, we have measured atomic densities as low as 5 × 10{sup 4} atoms cm{sup −3}. The simplicity of our technique and the details we provide should allow our method to be easily implemented in most atomic or molecular beam apparatuses.

Precision atomic beam density characterization by diode laser absorption spectroscopy

International Nuclear Information System (INIS)

Oxley, Paul; Wihbey, Joseph

2016-01-01

We provide experimental and theoretical details of a simple technique to determine absolute line-of-sight integrated atomic beam densities based on resonant laser absorption. In our experiments, a thermal lithium beam is chopped on and off while the frequency of a laser crossing the beam at right angles is scanned slowly across the resonance transition. A lock-in amplifier detects the laser absorption signal at the chop frequency from which the atomic density is determined. The accuracy of our experimental method is confirmed using the related technique of wavelength modulation spectroscopy. For beams which absorb of order 1% of the incident laser light, our measurements allow the beam density to be determined to an accuracy better than 5% and with a precision of 3% on a time scale of order 1 s. Fractional absorptions of order 10 −5 are detectable on a one-minute time scale when we employ a double laser beam technique which limits laser intensity noise. For a lithium beam with a thickness of 9 mm, we have measured atomic densities as low as 5 × 10 4 atoms cm −3 . The simplicity of our technique and the details we provide should allow our method to be easily implemented in most atomic or molecular beam apparatuses.

Precision atomic beam density characterization by diode laser absorption spectroscopy.

Science.gov (United States)

Oxley, Paul; Wihbey, Joseph

2016-09-01

We provide experimental and theoretical details of a simple technique to determine absolute line-of-sight integrated atomic beam densities based on resonant laser absorption. In our experiments, a thermal lithium beam is chopped on and off while the frequency of a laser crossing the beam at right angles is scanned slowly across the resonance transition. A lock-in amplifier detects the laser absorption signal at the chop frequency from which the atomic density is determined. The accuracy of our experimental method is confirmed using the related technique of wavelength modulation spectroscopy. For beams which absorb of order 1% of the incident laser light, our measurements allow the beam density to be determined to an accuracy better than 5% and with a precision of 3% on a time scale of order 1 s. Fractional absorptions of order 10 -5 are detectable on a one-minute time scale when we employ a double laser beam technique which limits laser intensity noise. For a lithium beam with a thickness of 9 mm, we have measured atomic densities as low as 5 × 10 4 atoms cm -3 . The simplicity of our technique and the details we provide should allow our method to be easily implemented in most atomic or molecular beam apparatuses.

Determination of lead and nickel in environmental samples by flame atomic absorption spectrometry after column solid-phase extraction on Ambersorb-572 with EDTA

Energy Technology Data Exchange (ETDEWEB)

Baytak, Sitki [Department of Chemistry, Faculty of Science and Arts, Harran University, 63100 Sanliurfa (Turkey); Tuerker, A. Rehber [Department of Chemistry, Faculty of Science and Arts, Gazi University, 06500 Ankara (Turkey)]. E-mail: aturker@gazi.edu.tr

2006-02-28

Lead and nickel were preconcentrated as their ethylenediaminetetraacedic acid (EDTA) complexes from aqueous sample solutions using a column containing Ambersorb-572 and determined by flame atomic absorption spectrometry (FAAS). pH values, amount of solid phase, elution solution and flow rate of sample solution have been optimized in order to obtain quantitative recovery of the analytes. The effect of interfering ions on the recovery of the analytes has also been investigated. The recoveries of Pb and Ni under the optimum conditions were 99 {+-} 2 and 97 {+-} 3%, respectively, at 95% confidence level. Seventy-five-fold (using 750 mL of sample solution and 10 mL of eluent) and 50-fold (using 500 mL of sample solution and 10 mL of eluent) preconcentration was obtained for Pb and Ni, respectively. Time of analysis is about 4.5 h (for obtaining enrichment factor of 75). By applying these enrichment factors, the analytical detection limits of Pb and Ni were found as 3.65 and 1.42 ng mL{sup -1}, respectively. The capacity of the sorbent was found as 0.17 and 0.21 mmol g{sup -1} for Pb and Ni, respectively. The interferences of some cations, such as Mn{sup 2+}, Co{sup 2+}, Fe{sup 3+}, Al{sup 3+}, Zn{sup 2+}, Cd{sup 2+}, Ca{sup 2+}, Mg{sup 2+}, K{sup +} and Na{sup +} usually present in water samples were also studied. This procedure was applied to the determination of lead and nickel in parsley, green onion, sea water and waste water samples. The accuracy of the procedure was checked by determining Pb and Ni in standard reference tea leaves sample (GBW-07605). The results demonstrated good agreement with the certified values.

Heavy metal adsorptivity of calcium-alginate-modified diethylenetriamine-silica gel and its application to a flow analytical system using flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Mori, Masanobu; Suzuki, Toshinobu; Sugita, Tsuyoshi; Nagai, Daisuke; Hirayama, Kazuo; Onozato, Makoto; Itabashi, Hideyuki

2014-01-01

Highlights: • Calcium-alginate-modified dien-silica gel adsorbed multivalent metal ions. • Metal ions adsorbed on CaAD were eluted using low acidic concentrations. • Flow system with CaAD-packed column enriched metal concentrations up to 50-fold. - Abstract: This study aimed to evaluate the heavy metal adsorptivity of calcium-alginate-modified diethylenetriamine-silica gel (CaAD) and incorporate this biosorbent into a flow analytical system for heavy metal ions using flame atomic absorption spectrometry (FAAS). The biosorbent was synthesized by electrostatically coating calcium alginate onto diethylenetriamine (dien)-silica gel. Copper ion adsorption tests by a batch method showed that CaAD exhibited a higher adsorption rate compared with other biosorbents despite its low maximum adsorption capacity. Next, CaAD was packed into a 1 mL microcolumn, which was connected to a flow analytical system equipped with an FAAS instrument. The flow system quantitatively adsorbed heavy metals and enriched their concentrations. This quantitative adsorption was achieved for pH 3–4 solutions containing 1.0 × 10 −6 M of heavy metal ions at a flow rate of 5.0 mL min −1 . Furthermore, the metal ions were successfully desorbed from CaAD at low nitric acid concentrations (0.05–0.15 M) than from the polyaminecarboxylic acid chelating resin (Chelex 100). Therefore, CaAD may be considered as a biosorbent that quickly adsorbs and easily desorbs analyte metal ions. In addition, the flow system enhanced the concentrations of heavy metals such as Cu 2+ , Zn 2+ , and Pb 2+ by 50-fold. This new enrichment system successfully performed the separation and determination of Cu 2+ (5.0 × 10 −8 M) and Zn 2+ (5.7 × 10 −8 M) in a river water sample and Pb 2+ (3.8 × 10 −9 M) in a ground water sample

Comparison of electrothermal atomization diode laser Zeeman- and wavelength-modulated atomic absorption and coherent forward scattering spectrometry

International Nuclear Information System (INIS)

Blecker, Carlo R.; Hermann, Gerd M.

2009-01-01

Atomic absorption and coherent forward scattering spectrometry by using a near-infrared diode laser with and without Zeeman and wavelength modulation were carried out with graphite furnace electrothermal atomization. Analytical curves and limits of detection were compared. The magnetic field was modulated with 50 Hz, and the wavelength of the diode laser with 10 kHz. Coherent forward scattering was measured with crossed and slightly uncrossed polarizers. The results show that the detection limits of atomic absorption spectrometry are roughly the same as those of coherent forward scattering spectrometry with crossed polarizers. According to the theory with bright flicker noise limited laser sources the detection limits and linear ranges obtained with coherent forward scattering spectrometry with slightly uncrossed polarizers are significantly better than those obtained with crossed polarizers and with atomic absorption spectrometry. This is due to the fact that employing approaches of polarization spectroscopy reduce laser intensity fluctuations to their signal carried fractions

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

Directory of Open Access Journals (Sweden)

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.

Liquid-Liquid Extraction and Determination of Trace Elements in Iron Minerals by Atomic Absorption Spectrometry

International Nuclear Information System (INIS)

Taseska, Milena; Stafilov, Trajche; Makreski, Petre; Jacimovic, Radojko; Jovanovski, Gligor

2006-01-01

Various trace elements (cadmium, chromium, cobalt, nickel, manganese) in some iron minerals were determined by flame (FAAS) and electrothermal atomic absorption spectrometry (ETAAS). The studied minerals were chalcopyrite (CuFeS 2 ), hematite (Fe 2 O 3 ) and pyrite (FeS 2 ). To avoid the interference of iron, a method for liquid-liquid extraction of iron and determination of investigated elements in the inorganic phase was proposed. Iron was extracted by diisopropyl ether in hydrochloride acid solution and the extraction method was optimized. Some parameters were obtained to be significantly important: Fe mass in the sample should not exceed 0.3 g, the optimal concentration of HCI should be 7.8 mol 1 -1 and ratio of the inorganic and organic phase should be 1: 1. The procedure was verified by the method of standard additions and by its applications to reference standard samples. The investigated minerals originate from various mines in the Republic of Macedonia. (Author)

Turbulent structure and dynamics of swirled, strongly pulsed jet diffusion flames

KAUST Repository

Liao, Ying-Hao

2013-11-02

The structure and dynamics of swirled, strongly pulsed, turbulent jet diffusion flames were examined experimentally in a co-flow swirl combustor. The dynamics of the large-scale flame structures, including variations in flame dimensions, the degree of turbulent flame puff interaction, and the turbulent flame puff celerity were determined from high-speed imaging of the luminous flame. All of the tests presented here were conducted with a fixed fuel injection velocity at a Reynolds number of 5000. The flame dimensions were generally found to be more impacted by swirl for the cases of longer injection time and faster co-flow flow rate. Flames with swirl exhibited a flame length up to 34% shorter compared to nonswirled flames. Both the turbulent flame puff separation and the flame puff celerity generally decreased when swirl was imposed. The decreased flame length, flame puff separation, and flame puff celerity are consistent with a greater momentum exchange between the flame and the surrounding co-flow, resulting from an increased rate of air entrainment due to swirl. Three scaling relations were developed to account for the impact of the injection time, the volumetric fuel-to-air flow rate ratio, and the jet-on fraction on the visible flame length. © 2013 Copyright Taylor and Francis Group, LLC.

H2O temperature sensor for low-pressure flames using tunable diode laser absorption near 2.9 νm

KAUST Repository

Li, Sijie; Farooq, Aamir; Hanson, Ronald Kenneth

2011-01-01

Making use of a newly available rapid-tuning diode laser operating at wavelengths up to 2.9 νm, an absorption-based temperature sensor was developed for in situ measurements in low-pressure flames. Based on the systematic analysis of H2O vapor

Midinfrared absorption measured at a lambda/400 resolution with an atomic force microscope.

Science.gov (United States)

Houel, Julien; Homeyer, Estelle; Sauvage, Sébastien; Boucaud, Philippe; Dazzi, Alexandre; Prazeres, Rui; Ortéga, Jean-Michel

2009-06-22

Midinfrared absorption can be locally measured using a detection combining an atomic force microscope and a pulsed excitation. This is illustrated for the midinfrared bulk GaAs phonon absorption and for the midinfrared absorption of thin SiO(2) microdisks. We show that the signal given by the cantilever oscillation amplitude of the atomic force microscope follows the spectral dependence of the bulk material absorption. The absorption spatial resolution achieved with microdisks is around 50 nanometer for an optical excitation around 22 micrometer wavelength.

Development of Dispersive Liquid-Liquid Microextraction Based on Solidification of Floating Organic Drop for the Sensitive Determination of Trace Copper in Water and Beverage Samples by Flame Atomic Absorption Spectrometry

International Nuclear Information System (INIS)

Wu, Chunxia; Zhao, Bin; Li, Yingli; Wu, Qiuhua; Wang, Chun; Wang, Zhi

2011-01-01

A dispersive liquid-liquid microextraction based on solidification of floating organic droplet (DLLME-SFO) has been developed as a new approach for the extraction of trace copper in water and beverage samples followed by the determination with flame atomic absorption spectrometry. In the DLLME-SFO, 8-hydroxy quinoline, 1-dodecanol, and methanol were used as chelating agent, extraction solvent and dispersive solvent, respectively. The experimental parameters related to the DLLME-SFO such as the type and volume of the extraction and dispersive solvent, extraction time, sample volume, the concentration of chelating agent and salt addition were investigated and optimized. Under the optimum conditions, the enrichment factor for copper was 122. The method was linear in the range from 0.5 to 300 ng mL -1 of copper in the samples with a correlation coefficient (r) of 0.9996 and a limit of detection of 0.1 ng mL -1 . The method was applied to the determination of copper in water and beverage samples. The recoveries for the spiked water and beverage samples at the copper concentration levels of 5.0 and 10.0 ng mL -1 were in the range between 92.0% and 108.0%. The relative standard deviations (RSD) varied from 3.0% to 5.6%

Solid Phase Extraction of Trace Al(III), Fe(II), Co(II), Cu(II), Cd(II) and Pb(II) Ions in Beverages on Functionalized Polymer Microspheres Prior to Flame Atomic Absorption Spectrometric Determinations.

Science.gov (United States)

Berber, Hale; Alpdogan, Güzin

2017-01-01

In this study, poly(glycidyl methacrylate-methyl methacrylate-divinylbenzene) was synthesized in the form of microspheres, and then functionalized by 2-aminobenzothiazole ligand. The sorption properties of these functionalized microspheres were investigated for separation, preconcentration and determination of Al(III), Fe(II), Co(II), Cu(II), Cd(II) and Pb(II) ions using flame atomic absorption spectrometry. The optimum pH values for quantitative sorption were 2 - 4, 5 - 8, 6 - 8, 4 - 6, 2 - 6 and 2 - 3 for Al(III), Fe(II), Co(II), Cu(II), Cd(II) and Pb(II), respectively, and also the highest sorption capacity of the functionalized microspheres was found to be for Cu(II) with the value of 1.87 mmol g -1 . The detection limits (3σ; N = 6) obtained for the studied metals in the optimal conditions were observed in the range of 0.26 - 2.20 μg L -1 . The proposed method was successfully applied to different beverage samples for the determination of Al(III), Fe(II), Co(II), Cu(II), Cd(II) and Pb(II) ions, with the relative standard deviation of <3.7%.

Subwavelength atom localization via amplitude and phase control of the absorption spectrum

International Nuclear Information System (INIS)

Sahrai, Mostafa; Tajalli, Habib; Kapale, Kishore T.; Zubairy, M. Suhail

2005-01-01

We propose a scheme for subwavelength localization of an atom conditioned upon the absorption of a weak probe field at a particular frequency. Manipulating atom-field interaction on a certain transition by applying drive fields on nearby coupled transitions leads to interesting effects in the absorption spectrum of the weak probe field. We exploit this fact and employ a four-level system with three driving fields and a weak probe field, where one of the drive fields is a standing-wave field of a cavity. We show that the position of an atom along this standing wave is determined when probe-field absorption is measured. We find that absorption of the weak probe field at a certain frequency leads to subwavelength localization of the atom in either of the two half-wavelength regions of the cavity field by appropriate choice of the system parameters. We term this result as sub-half-wavelength localization to contrast it with the usual atom localization result of four peaks spread over one wavelength of the standing wave. We observe two localization peaks in either of the two half-wavelength regions along the cavity axis

Flame visualization in power stations

Energy Technology Data Exchange (ETDEWEB)

Hulshof, H J.M.; Thus, A W; Verhage, A J.L. [KEMA - Fossil Power Plants, Arnhem (Netherlands)

1993-01-01

The shapes and temperature of flames in power stations, fired with powder coal and gas, have been measured optically. Spectral information in the visible and near infrared is used. Coal flames are visualized in the blue part of the spectrum, natural gas flames are viewed in the light of CH-emission. Temperatures of flames are derived from the best fit of the Planck-curve to the thermal radiation spectrum of coal and char, or to that of soot in the case of gas flames. A measuring method for the velocity distribution inside a gas flame is presented, employing pulsed alkali salt injection. It has been tested on a 100 kW natural gas flame. 3 refs., 9 figs.

Effects of injection angles on combustion processes using multiple injection strategies in an HSDI diesel engine

Energy Technology Data Exchange (ETDEWEB)

Tiegang Fang; Robert E. Coverdill; Chia-fon F. Lee; Robert A. White [North Carolina State University, Raleigh, NC (United States). Department of Mechanical and Aerospace Engineering

2008-11-15

Effects of injection angles and injection pressure on the combustion processes employing multiple injection strategies in a high-speed direct-injection (HSDI) diesel engine are presented in this work. Whole-cycle combustion and liquid spray evolution processes were visualized using a high-speed video camera. NOx emissions were measured in the exhaust pipe. Different heat release patterns are seen for two different injectors with a 70-degree tip and a 150-degree tip. No evidence of fuel-wall impingement is found for the first injection of the 150-degree tip, but for the 70-degree tip, some fuel impinges on the bowl wall and a fuel film is formed. For the second injection, a large amount of fuel deposition is observed for the 70-degree tip. Weak flame is seen for the first injection of the 150-degree tip while two sorts of flames are seen for the first injection of the 70-degree tip including an early weak flame and a late luminous film combustion flame. Ignition occurs near the spray tip in the vicinity of the bowl wall for the second injection events of the 150-degree tip, however, it is near the injector tip in the central region of the bowl for the 70-degree tip. The flame is more homogeneous for the 150-degree tip with higher injection pressure with little soot formation similar to a premixed-charge-compression-ignition (PCCI) combustion. For other cases, liquid fuel is injected into flames showing diffusion flame combustion. More soot luminosity is seen for the 70-degree tip due to significant fuel film deposition on the piston wall with fuel film combustion for both injection events. Lower NOx emissions were obtained for the narrow-angle injector due to the rich air-fuel mixture near the bowl wall during the combustion process. 30 refs., 11 figs., 3 tabs.

Proposal for efficient two-dimensional atom localization using probe absorption in a microwave-driven four-level atomic system

International Nuclear Information System (INIS)

Ding Chunling; Li Jiahua; Yang Xiaoxue; Xiong Hao; Zhang Duo

2011-01-01

The behavior of two-dimensional (2D) atom localization is explored by monitoring the probe absorption in a microwave-driven four-level atomic medium under the action of two orthogonal standing-wave fields. Because of the position-dependent atom-field interaction, the information about the position of the atom can be obtained via the absorption measurement of the weak probe field. It is found that the localization behavior is significantly improved due to the joint quantum interference induced by the standing-wave and microwave-driven fields. Most importantly, the atom can be localized at a particular position and the maximal probability of finding the atom in one period of the standing-wave fields reaches unity by properly adjusting the system parameters. The proposed scheme may provide a promising way to achieve high-precision and high-resolution 2D atom localization.

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

Science.gov (United States)

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…

Localization of a two-level atom via the absorption spectrum

International Nuclear Information System (INIS)

Xu, Jun; Hu, Xiang-Ming

2007-01-01

We show that it is possible to localize a two-level atom as it passes through a standing-wave field by measuring the probe-field absorption. There is 50% detecting probability of the atom at the nodes of the standing-wave field in the subwavelength domain when the probe field is tuned resonant with the atomic transition

Microcontroller-driven fluid-injection system for atomic force microscopy.

Science.gov (United States)

Kasas, S; Alonso, L; Jacquet, P; Adamcik, J; Haeberli, C; Dietler, G

2010-01-01

We present a programmable microcontroller-driven injection system for the exchange of imaging medium during atomic force microscopy. Using this low-noise system, high-resolution imaging can be performed during this process of injection without disturbance. This latter circumstance was exemplified by the online imaging of conformational changes in DNA molecules during the injection of anticancer drug into the fluid chamber.

Three-dimensional atom localization via probe absorption in a cascade four-level atomic system

Directory of Open Access Journals (Sweden)

Zeng Wei

2018-03-01

Full Text Available For an atomic system with cascade four-level type, a useful scheme about three-dimensional (3D atom localization is proposed. In our scheme the atomic system is coherently controlled by using a radio-frequency field to couple with two-folded levels under the condition of the existence of probe absorption. Our results show that detecting precision of 3D atom localization may be obviously improved by properly adjusting the frequency detuning and strength of the radio-frequency driving field. So our scheme could be helpful to realize 3D atom localization with high-efficiency and high-precision . In the field of laser cooling or the atom nano-lithography, our studies provide potential applications.

Three-dimensional atom localization via probe absorption in a cascade four-level atomic system

Science.gov (United States)

Zeng, Wei; Deng, Li; Chen, Aixi

2018-03-01

For an atomic system with cascade four-level type, a useful scheme about three-dimensional (3D) atom localization is proposed. In our scheme the atomic system is coherently controlled by using a radio-frequency field to couple with two-folded levels under the condition of the existence of probe absorption. Our results show that detecting precision of 3D atom localization may be obviously improved by properly adjusting the frequency detuning and strength of the radio-frequency driving field. So our scheme could be helpful to realize 3D atom localization with high-efficiency and high-precision . In the field of laser cooling or the atom nano-lithography, our studies provide potential applications.

A method optimization study for atomic absorption ...

African Journals Online (AJOL)

A sensitive, reliable and relative fast method has been developed for the determination of total zinc in insulin by atomic absorption spectrophotometer. This designed study was used to optimize the procedures for the existing methods. Spectrograms of both standard and sample solutions of zinc were recorded by measuring ...

Evaluation of atomic absorption Spectrophotometry (ashing, non ...

African Journals Online (AJOL)

Three commonly used techniques, namely atomic absorption spectrophotometry (AAS-Ashing and AAS-Non Ashing) and titrimetry (potassium permanganate titration) have been evaluated in this study to determine the calcium content in six food samples whose calcium levels ranged from 0 to more than 250mg/100g ...

Cloud point extraction for determination of lead in blood samples of children, using different ligands prior to analysis by flame atomic absorption spectrometry: A multivariate study

Energy Technology Data Exchange (ETDEWEB)

Shah, Faheem, E-mail: shah_ceac@yahoo.com [National Center of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080 (Pakistan); Kazi, Tasneem Gul, E-mail: tgkazi@yahoo.com [National Center of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080 (Pakistan); Afridi, Hassan Imran, E-mail: hassanimranafridi@yahoo.com [National Center of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080 (Pakistan); Naeemullah, E-mail: khannaeemullah@ymail.com [National Center of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080 (Pakistan); Arain, Muhammad Balal, E-mail: bilal_ku2004@yahoo.com [Department of Chemistry, University of Science and Technology, Bannu, KPK (Pakistan); Baig, Jameel Ahmed, E-mail: jab_mughal@yahoo.com [National Center of Excellence in Analytical Chemistry, University of Sindh, Jamshoro 76080 (Pakistan)

2011-09-15

Highlights: {yields} Trace levels of lead in blood samples of healthy children and with different kidney disorders {yields} Pre-concentration of Pb{sup +2} in acid digested blood samples after chelating with two complexing reagents. {yields} Multivariate technique was used for screening of significant factors that influence the CPE of Pb{sup +2} {yields} The level of Pb{sup +2} in diseased children was significantly higher than referents of same age group. - Abstract: The phase-separation phenomenon of non-ionic surfactants occurring in aqueous solution was used for the extraction of lead (Pb{sup 2+}) from digested blood samples after simultaneous complexation with ammonium pyrrolidinedithiocarbamate (APDC) and diethyldithiocarbamate (DDTC) separately. The complexed analyte was quantitatively extracted with octylphenoxypolyethoxyethanol (Triton X-114). The multivariate strategy was applied to estimate the optimum values of experimental factors. Acidic ethanol was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometer (FAAS). The detection limit value of Pb{sup 2+} for the preconcentration of 10 mL of acid digested blood sample was 1.14 {mu}g L{sup -1}. The accuracy of the proposed methods was assessed by analyzing certified reference material (whole blood). Under the optimized conditions of both CPE methods, 10 mL of Pb{sup 2+} standards (10 {mu}g L{sup -1}) complexed with APDC and DDTC, permitted the enhancement factors of 56 and 42, respectively. The proposed method was used for determination of Pb{sup 2+} in blood samples of children with kidney disorders and healthy controls.

A new ultrasonic-assisted cloud-point-extraction procedure for pre-concentration and determination of ultra-trace levels of copper in selected beverages and foods by flame atomic absorption spectrometry.

Science.gov (United States)

Altunay, Nail; Gürkan, Ramazan; Orhan, Ulaş

2015-01-01

A new ultrasonic-assisted cloud-point-extraction (UA-CPE) method was developed for the pre-concentration of Cu(II) in selected beverage and food samples prior to flame atomic absorption spectrometric (FAAS) analysis. For this purpose, Safranin T was used as an ion-pairing reagent based on charge transfer in the presence of oxalate as the primary chelating agent at pH 10. Non-ionic surfactant, poly(ethyleneglycol-mono-p-nonylphenylether) (PONPE 7.5) was used as an extracting agent in the presence of NH4Cl as the salting out agent. The variables affecting UA-CPE efficiency were optimised in detail. The linear range for Cu(II) at pH 10 was 0.02-70 µg l(-)(1) with a very low detection limit of 6.10 ng l(-)(1), while the linear range for Cu(I) at pH 8.5 was 0.08-125 µg l(-)(1) with a detection limit of 24.4 ng l(-)(1). The relative standard deviation (RSD %) was in the range of 2.15-4.80% (n = 5). The method was successfully applied to the quantification of Cu(II), Cu(I) and total Cu in selected beverage and food samples. The accuracy of the developed method was demonstrated by the analysis of two standard reference materials (SRMs) as well as recoveries of spiked samples.

Nitrogen dioxide and kerosene-flame soot calibration of photoacoustic instruments for measurement of light absorption by aerosols

International Nuclear Information System (INIS)

Arnott, W. Patrick; Moosmu''ller, Hans; Walker, John W.

2000-01-01

A nitrogen dioxide calibration method is developed to evaluate the theoretical calibration for a photoacoustic instrument used to measure light absorption by atmospheric aerosols at a laser wavelength of 532.0 nm. This method uses high concentrations of nitrogen dioxide so that both a simple extinction and the photoacoustically obtained absorption measurement may be performed simultaneously. Since Rayleigh scattering is much less than absorption for the gas, the agreement between the extinction and absorption coefficients can be used to evaluate the theoretical calibration, so that the laser gas spectra are not needed. Photoacoustic theory is developed to account for strong absorption of the laser beam power in passage through the resonator. Findings are that the photoacoustic absorption based on heat-balance theory for the instrument compares well with absorption inferred from the extinction measurement, and that both are well within values represented by published spectra of nitrogen dioxide. Photodissociation of nitrogen dioxide limits the calibration method to wavelengths longer than 398 nm. Extinction and absorption at 532 and 1047 nm were measured for kerosene-flame soot to evaluate the calibration method, and the single scattering albedo was found to be 0.31 and 0.20 at these wavelengths, respectively

Control of confined nonpremixed flames using a microjet

International Nuclear Information System (INIS)

Sinha, Ashok; Ganguly, Ranjan; Puri, Ishwar K.

2005-01-01

Industrial burners, such as those used in materials processing furnaces, require precise control over the flame length, width, overall shape and other physical flame attributes. The mechanism used to control the flame topology should be relatively simple, safe, and devoid of an emissions penalty. We have explored the feasibility of hydrodynamic control of confined nonpremixed flames by injecting air through a high-momentum microjet. An innovative strategy for the control of flame shape and luminosity is demonstrated based on a high-momentum coaxial microjet injected along the center of a confined nonpremixed flame burning in a coflowing oxidizer stream. The introduction of the microjet shortens a nonpremixed flame and reduces the amplitude of the buoyancy-induced flickering. For a microjet-assisted flame, the flame length is more sensitive to the fuel flowrate than for laminar or turbulent nonpremixed flames. This provides greater flexibility for the dynamic control of their flame lengths. Measurements of NO x and CO emissions show that the method is robust. Effective flame control without an emissions penalty is possible over a large range of microjet velocities that significantly alter the flame shape. Since the influence of the microjet is primarily of a hydrodynamic nature, inert microjet fluids like recirculated exhaust gas can also be used in practical devices

Control of confined nonpremixed flames using a microjet

Energy Technology Data Exchange (ETDEWEB)

Sinha, A.; Puri, I.K. [Virginia Polytechnic Inst. and State Univ., Blacksburg, VA (United States). Dept. of Engineering Science and Mechanics; Ganguly, R. [Virginia Polytechnic Inst. and State Univ., Blacksburg, VA (United States). Dept. of Engineering Science and Mechanics; Jadavpur Univ., Calcutta (India). Dept. of Power Engineering

2005-06-01

Industrial burners, such as those used in materials processing furnaces, require precise control over the flame length, width, overall shape and other physical flame attributes. The mechanism used to control the flame topology should be relatively simple, safe, and devoid of an emissions penalty. We have explored the feasibility of hydrodynamic control of confined nonpremixed flames by injecting air through a high-momentum microjet. An innovative strategy for the control of flame shape and luminosity is demonstrated based on a high-momentum coaxial microjet injected along the center of a confined nonpremixed flame burning in a coflowing oxidizer stream. The introduction of the microjet shortens a nonpremixed flame and reduces the amplitude of the buoyancy-induced flickering. For a microjet-assisted flame, the flame length is more sensitive to the fuel flowrate than for laminar or turbulent nonpremixed flames. This provides greater flexibility for the dynamic control of their flame lengths. Measurements of NO{sub x} and CO emissions show that the method is robust. Effective flame control without an emissions penalty is possible over a large range of microjet velocities that significantly alter the flame shape. Since the influence of the microjet is primarily of a hydrodynamic nature, inert microjet fluids like recirculated exhaust gas can also be used in practical devices. (Author)

Absorption of resonant electromagnetic radiation in electron-atom collisions

International Nuclear Information System (INIS)

Arslanbekov, T.U.; Pazdzerskii, V.A.; Usachenko, V.I.

1986-01-01

Nonrelativistic quantum theory is used to study the possibility of amplification of electromagnetic radiation in forced braking scattering of an electron beam on atoms. The interaction of the atom with the electromagnetic field is considered in the resonant approximation. Cases of large and small detuning from resonance are considered. It is shown that for any orientation of the electron beam relative to the field polarization vector, absorption of radiation occurs, with the major contribution being produced by atomic electrons

Measurement of the effective atomic numbers of compounds with cerium near to the absorption edge

International Nuclear Information System (INIS)

Polat, Recep; Icelli, Orhan

2010-01-01

In order to measure atomic, molecular and electronic cross-section; the effective atomic number, density of electron and absorption jump factor, we have first measured μ t values of compounds which are determined by mixture rule using transmission method. In order to measure experimentally the effective atomic number within absorption jump factors of compounds with Ce, the X-ray source used Am-241 whose gamma rays were stopped at secondary source (Sm), thus producing Kα and Kβ X-ray emission. The most crucial finding in this study is that measurement of the effective atomic number is not appropriate near to the absorption edge and the effective atomic number is affected by near to the absorption edge. The results obtained have been compared with theoretical values.

Modified Activated Carbon Prepared from Acorn Shells as a New Solid-Phase Extraction Sorbent for the Preconcentration and Determination of Trace Amounts of Nickel in Food Samples Prior to Flame Atomic Absorption Spectrometry.

Science.gov (United States)

Ebrahimi, Bahram

2017-03-01

A new solid-phase extraction (SPE) sorbent was introduced based on acidic-modified (AM) activated carbon (AC) prepared from acorn shells of native oak trees in Kurdistan. Hydrochloric acid (15%, w/w) and nitric acid (32.5%, w/w) were used to condition and modify AC. The IR spectra of AC and AM-AC showed that AM lead to the formation of increasing numbers of acidic functional groups on AM-AC. AM-AC was used in the SPE method for the extraction and preconcentration of Ni+2 prior to flame atomic absorption spectrometric determination at ng/mL levels in model and real food samples. Effective parameters of the SPE procedure, such as the pH of the solutions, sorbent dosage, extraction time, sample volume, type of eluent, and matrix ions, were considered and optimized. An enrichment factor of 140 was obtained. The calibration curve was linear with an R2 of 0.997 in the concentration range of 1-220 ng/mL. The RSD was 5.67% (for n = 7), the LOD was 0.352 ng/mL, and relative recoveries in vegetable samples ranged from 96.7 to 103.7%.

Fast determination of trace elements in organic fertilizers using a cup-horn reactor for ultrasound-assisted extraction and fast sequential flame atomic absorption spectrometry.

Science.gov (United States)

Teixeira, Leonel Silva; Vieira, Heulla Pereira; Windmöller, Cláudia Carvalhinho; Nascentes, Clésia Cristina

2014-02-01

A fast and accurate method based on ultrasound-assisted extraction in a cup-horn sonoreactor was developed to determine the total content of Cd, Co, Cr, Cu, Mn, Ni, Pb and Zn in organic fertilizers by fast sequential flame atomic absorption spectrometry (FS FAAS). Multivariate optimization was used to establish the optimal conditions for the extraction procedure. An aliquot containing approximately 120 mg of the sample was added to a 500 µL volume of an acid mixture (HNO3/HCl/HF, 5:3:3, v/v/v). After a few minutes, 500 µL of deionized water was added and eight samples were simultaneously sonicated for 10 min at 50% amplitude, allowing a sample throughput of 32 extractions per hour. The performance of the method was evaluated with a certified reference material of sewage sludge (CRM 029). The precision, expressed as the relative standard deviation, ranged from 0.58% to 5.6%. The recoveries of analytes were found to 100%, 109%, 96%, 92%, 101%, 104% and 102% for Cd, Cr, Cu, Mn, Ni, Pb and Zn, respectively. The linearity, limit of detection and limit of quantification were calculated and the values obtained were adequate for the quality control of organic fertilizers. The method was applied to the analysis of several commercial organic fertilizers and organic wastes used as fertilizers, and the results were compared with those obtained using the microwave digestion procedure. A good agreement was found between the results obtained by microwave and ultrasound procedures with recoveries ranging from 80.4% to 117%. Two organic waste samples were not in accordance with the Brazilian legislation regarding the acceptable levels of contaminants. © 2013 Published by Elsevier B.V.

Flame atomic absorption spectrometric determination of heavy metals in aqueous solution and surface water preceded by co-precipitation procedure with copper(II) 8-hydroxyquinoline

Science.gov (United States)

Ipeaiyeda, Ayodele Rotimi; Ayoade, Abisayo Ruth

2017-12-01

Co-precipitation procedure has widely been employed for preconcentration and separation of metal ions from the matrices of environmental samples. This is simply due to its simplicity, low consumption of separating solvent and short duration for analysis. Various organic ligands have been used for this purpose. However, there is dearth of information on the application of 8-hydroxyquinoline (8-HQ) as ligand and Cu(II) as carrier element. The use of Cu(II) is desirable because there is no contamination and background adsorption interference. Therefore, the objective of this study was to use 8-HQ in the presence of Cu(II) for coprecipitation of Cd(II), Co(II), Cr(III), Ni(II) and Pb(II) from standard solutions and surface water prior to their determinations by flame atomic absorption spectrometry (FAAS). The effects of pH, sample volume, amount of 8-HQ and Cu(II) and interfering ions on the recoveries of metal ions from standard solutions were monitored using FAAS. The water samples were treated with 8-HQ under the optimum experimental conditions and metal concentrations were determined by FAAS. The metal concentrations in water samples not treated with 8-HQ were also determined. The optimum recovery values for metal ions were higher than 85.0%. The concentrations (mg/L) of Co(II), Ni(II), Cr(III), and Pb(II) in water samples treated with 8-HQ were 0.014 ± 0.002, 0.03 ± 0.01, 0.04 ± 0.02 and 0.05 ± 0.02, respectively. These concentrations and those obtained without coprecipitation technique were significantly different. Coprecipitation procedure using 8-HQ as ligand and Cu(II) as carrier element enhanced the preconcentration and separation of metal ions from the matrix of water sample.

[Determination of soil exchangeable base cations by using atomic absorption spectrophotometer and extraction with ammonium acetate].

Science.gov (United States)

Zhang, Yu-ge; Xiao, Min; Dong, Yi-hua; Jiang, Yong

2012-08-01

A method to determine soil exchangeable calcium (Ca), magnesium (Mg), potassium (K), and sodium (Na) by using atomic absorption spectrophotometer (AAS) and extraction with ammonium acetate was developed. Results showed that the accuracy of exchangeable base cation data with AAS method fits well with the national standard referential soil data. The relative errors for parallel samples of exchangeable Ca and Mg with 66 pair samples ranged from 0.02%-3.14% and 0.06%-4.06%, and averaged to be 1.22% and 1.25%, respectively. The relative errors for exchangeable K and Na with AAS and flame photometer (FP) ranged from 0.06%-8.39% and 0.06-1.54, and averaged to be 3.72% and 0.56%, respectively. A case study showed that the determination method for exchangeable base cations by using AAS was proven to be reliable and trustable, which could reflect the real situation of soil cation exchange properties in farmlands.

A rapid method for determining tin and molybdenum in geological samples by flame atomic-absorption spectroscopy

Science.gov (United States)

Welsch, E.P.

1985-01-01

The proposed method uses a lithium metaborate fusion, dissolution of the fusion bead in 15% v v hydrochloric acid, extraction into a 4% solution of trioctylphosphine oxide in methyl isobutyl ketone, and aspiration into a nitrous oxide-acetylene flame. The limits of detection for tin and molybdenum are 1.0 and 0.5 ppm, respectively. Approximately 50 samples can be analysed per day. ?? 1985.

Trace mercury determination in drinking and natural water samples by room temperature ionic liquid based-preconcentration and flow injection-cold vapor atomic absorption spectrometry.

Science.gov (United States)

Martinis, Estefanía M; Bertón, Paula; Olsina, Roberto A; Altamirano, Jorgelina C; Wuilloud, Rodolfo G

2009-08-15

A liquid-liquid extraction procedure (L-L) based on room temperature ionic liquid (RTIL) was developed for the preconcentration and determination of mercury in different water samples. The analyte was quantitatively extracted with 1-butyl-3-methylimidazolium hexafluorophosphate ([C(4)mim][PF(6)]) under the form of Hg-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (Hg-5-Br-PADAP) complex. A volume of 500 microl of 9.0 mol L(-1) hydrochloric acid was used to back-extract the analyte from the RTIL phase into an aqueous media prior to its analysis by flow injection-cold vapor atomic absorption spectrometry (FI-CV-AAS). A preconcentration factor of 36 was achieved upon preconcentration of 20 mL of sample. The limit of detection (LOD) obtained under the optimal conditions was 2.3ngL(-1) and the relative standard deviation (RSD) for 10 replicates at 1 microg L(-1) Hg(2+) was 2.8%, calculated with peaks height. The method was successfully applied to the determination of mercury in river, sea, mineral and tap water samples and a certified reference material (CRM).

Trace mercury determination in drinking and natural water samples by room temperature ionic liquid based-preconcentration and flow injection-cold vapor atomic absorption spectrometry

International Nuclear Information System (INIS)

Martinis, Estefania M.; Berton, Paula; Olsina, Roberto A.; Altamirano, Jorgelina C.; Wuilloud, Rodolfo G.

2009-01-01

A liquid-liquid extraction procedure (L-L) based on room temperature ionic liquid (RTIL) was developed for the preconcentration and determination of mercury in different water samples. The analyte was quantitatively extracted with 1-butyl-3-methylimidazolium hexafluorophosphate ([C 4 mim][PF 6 ]) under the form of Hg-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (Hg-5-Br-PADAP) complex. A volume of 500 μl of 9.0 mol L -1 hydrochloric acid was used to back-extract the analyte from the RTIL phase into an aqueous media prior to its analysis by flow injection-cold vapor atomic absorption spectrometry (FI-CV-AAS). A preconcentration factor of 36 was achieved upon preconcentration of 20 mL of sample. The limit of detection (LOD) obtained under the optimal conditions was 2.3 ng L -1 and the relative standard deviation (RSD) for 10 replicates at 1 μg L -1 Hg 2+ was 2.8%, calculated with peaks height. The method was successfully applied to the determination of mercury in river, sea, mineral and tap water samples and a certified reference material (CRM).

Uranium determination using atomic spectrometric techniques: An overview

International Nuclear Information System (INIS)

Santos, Juracir S.; Teixeira, Leonardo S.G.; Santos, Walter N.L. dos; Lemos, Valfredo A.; Godoy, Jose M.; Ferreira, Sergio L.C.

2010-01-01

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.

Determination of lead and cadmium in urine by electrothermal atomization atomic absorption spectrometry

International Nuclear Information System (INIS)

Vasil'eva, L.A.; Grinshtejn, I.L.; Gucher, Sh.; Izgi, B.

2008-01-01

The applicability of a DETATA sorbent to the preconcentration of lead and cadmium followed by the determination of these elements in urine using atomic absorption spectrometry with electrothermal atomization was demonstrated. After preconcentration by a factor of 10, the limits of detection were 0.01 and 0.2 μg/l for cadmium and lead, respectively. The accuracy of the results was supported by the analysis of Seronorm TM Trace Elements Urine Batch no.101021 [ru

Method and apparatus for generating highly luminous flame

Energy Technology Data Exchange (ETDEWEB)

Gitman, G.M.

1992-05-12

A combustion process and apparatus are provided for generating a variable high temperature, highly luminous flame with low NOx emission by burning gaseous and liquid materials with oxygen and air. More particularly, the invention provides a process in which there is initial control of fuel, oxygen, and air flows and the delivery of the oxidizers to a burner as two oxidizing gases having different oxygen concentrations (for example, pure oxygen and air, or oxygen and oxygen-enriched air). A first oxidizing gas containing a high oxygen concentration is injected as a stream into the central zone of a combustion tunnel or chamber, and part of the fuel (preferably the major part) is injected into the central pyrolysis zone to mix with the first oxidizing gas to create a highly luminous high-temperature flame core containing microparticles of carbon of the proper size for maximum luminosity and high temperature, and a relatively small amount of hydrocarbon radicals. In addition, part of the fuel (preferably the minor part) is injected in a plurality of streams about the flame core to mix with a second oxidizing gas (containing a lower oxygen concentration than the first oxidizing gas) and injecting the second oxidizing mixture about the flame core and the minor fuel flow to mix with the minor fuel flow. This creates a plurality of fuel-lean (oxygen-rich) flames which are directed toward the luminous flame core to form a final flame pattern having high temperature, high luminosity, and low NOx content. 6 figs.

Human dermal absorption of chlorinated organophosphate flame retardants; implications for human exposure

Energy Technology Data Exchange (ETDEWEB)

Abou-Elwafa Abdallah, Mohamed, E-mail: mae_abdallah@yahoo.co.uk [Division of Environmental Health and Risk Management, School of Geography, Earth, and Environmental Sciences, University of Birmingham, Birmingham B15 2TT (United Kingdom); Department of Analytical Chemistry, Faculty of Pharmacy, Assiut University, 71526 Assiut (Egypt); Pawar, Gopal; Harrad, Stuart [Division of Environmental Health and Risk Management, School of Geography, Earth, and Environmental Sciences, University of Birmingham, Birmingham B15 2TT (United Kingdom)

2016-01-15

Tris-2-chloroethyl phosphate (TCEP), tris (1-chloro-2-propyl) phosphate (TCIPP) and tris-1,3-dichloropropyl phosphate (TDCIPP) are organophosphate flame retardants (PFRs) widely applied in a plethora of consumer products despite their carcinogenic potential. Human dermal absorption of these PFRs is investigated for the first time using human ex vivo skin and EPISKIN™ models. Results of human ex vivo skin experiments revealed 28%, 25% and 13% absorption of the applied dose (500 ng/cm{sup 2}, finite dose) of TCEP, TCIPP and TDCIPP, respectively after 24 h exposure. The EPISKIN™ model showed enhanced permeability values (i.e. weaker barrier), that were respectively 16%, 11% and 9% for TCEP, TCIPP and TDCIPP compared to human ex vivo skin. However, this difference was not significant (P > 0.05). Estimated permeability constants (K{sub p}, cm/h) showed a significant negative correlation with log K{sub ow} for the studied contaminants. The effect of hand-washing on dermal absorption of PFRs was investigated. Washing reduced overall dermal absorption, albeit to varying degrees depending on the physicochemical properties of the target PFRs. Moreover, slight variations of the absorbed dose were observed upon changing the dosing solution from acetone to 20% Tween 80 in water, indicating the potential influence of the dose vehicle on the dermal absorption of PFRs. Finally, estimated dermal uptake of the studied PFRs via contact with indoor dust was higher in UK toddlers (median ΣPFRs = 36 ng/kg bw day) than adults (median ΣPFRs = 4 ng/kg bw day). More research is required to fully elucidate the toxicological implications of such exposure. - Highlights: • Human dermal absorption of PFRs was studied using human ex vivo skin and EPISKIN™. • Absorbed fractions of TCEP, TCIPP and TDCIPP were 28%, 25% and 13% of applied dose. • Permeability constants showed significant negative correlation to log K{sub ow} of PFRs. • Skin washing reduced the overall dermal

Human dermal absorption of chlorinated organophosphate flame retardants; implications for human exposure

International Nuclear Information System (INIS)

Abou-Elwafa Abdallah, Mohamed; Pawar, Gopal; Harrad, Stuart

2016-01-01

Tris-2-chloroethyl phosphate (TCEP), tris (1-chloro-2-propyl) phosphate (TCIPP) and tris-1,3-dichloropropyl phosphate (TDCIPP) are organophosphate flame retardants (PFRs) widely applied in a plethora of consumer products despite their carcinogenic potential. Human dermal absorption of these PFRs is investigated for the first time using human ex vivo skin and EPISKIN™ models. Results of human ex vivo skin experiments revealed 28%, 25% and 13% absorption of the applied dose (500 ng/cm 2 , finite dose) of TCEP, TCIPP and TDCIPP, respectively after 24 h exposure. The EPISKIN™ model showed enhanced permeability values (i.e. weaker barrier), that were respectively 16%, 11% and 9% for TCEP, TCIPP and TDCIPP compared to human ex vivo skin. However, this difference was not significant (P > 0.05). Estimated permeability constants (K p , cm/h) showed a significant negative correlation with log K ow for the studied contaminants. The effect of hand-washing on dermal absorption of PFRs was investigated. Washing reduced overall dermal absorption, albeit to varying degrees depending on the physicochemical properties of the target PFRs. Moreover, slight variations of the absorbed dose were observed upon changing the dosing solution from acetone to 20% Tween 80 in water, indicating the potential influence of the dose vehicle on the dermal absorption of PFRs. Finally, estimated dermal uptake of the studied PFRs via contact with indoor dust was higher in UK toddlers (median ΣPFRs = 36 ng/kg bw day) than adults (median ΣPFRs = 4 ng/kg bw day). More research is required to fully elucidate the toxicological implications of such exposure. - Highlights: • Human dermal absorption of PFRs was studied using human ex vivo skin and EPISKIN™. • Absorbed fractions of TCEP, TCIPP and TDCIPP were 28%, 25% and 13% of applied dose. • Permeability constants showed significant negative correlation to log K ow of PFRs. • Skin washing reduced the overall dermal absorption of target PFRs

Flame emission spectroscopy measurement of a steam blast and air blast burner

Directory of Open Access Journals (Sweden)

Jozsa Viktor

2017-01-01

Full Text Available Control and online monitoring of combustion have become critical to meet the increasingly strict pollutant emission standards. For such a purpose, optical sensing methods, like flame emission spectrometry, seem to be the most feasible technique. Spectrometry is capable to provide information about the local equivalence ratio inside the flame through the chemiluminescence intensity ratio measurement of various radicals. In the present study, a 15 kW atmospheric burner was analyzed utilizing standard diesel fuel. Its plain jet type atomizer was operated with both air and steam atomizing mediums. Up to now, injection of steam into the reaction zone has attracted less scientific attention contrary to its practical importance. Spatial plots of OH*, CH*, and C2* excited radicals were analyzed at 0.35, 0.7, and 1 bar atomization gauge pressures, utilizing both atomizing mediums. The C2* was found to decrease strongly with increasing steam addition. The OH*/CH* and OH*/C2* chemiluminescence intensity ratios along the axis showed a divergent behavior in all the analyzed cases. Nevertheless, CH*/C2* chemiluminescence intensity ratio decreased only slightly, showing low sensitivity to the position of the spectrometer. The findings may be directly applied in steady operating combustion systems, i. e., gas turbines, boilers, and furnaces.

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

International Nuclear Information System (INIS)

Lorenzo, Magdalena; Reyes, Arlyn; Blanco, Idania; Vasallo, Maria C

2010-01-01

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

Radial plasma profile and neutron yield in an adiabatic trap with fast atom injection

International Nuclear Information System (INIS)

Panov, D.A.

1988-01-01

Radial profiles of ion densities depending on two dimensionless parameters, which values are determined by the trap, plasma and injected beam parameters are found in dimensionless units for a plasma generated by fast atom injection in an adiabatic trap. The calculated profiles are used for determining the neutron yield. Simple approximated dimensional relations permitting to estimate quickly neutron yield, required injection power, flux of charge exchange atoms on the wall around the plasma in a wide energy range of injected atoms, trap field modulud, injection angle, trap radius and length are determined. The energetic efficiency of neutron production is estimated and it is shown that it grows with the injection energy. 7 refs.; 7 figs

Visualization research on spray atomization, evaporation and combustion processes of ethanol–diesel blend under LTC conditions

International Nuclear Information System (INIS)

Huang, Sheng; Deng, Peng; Huang, Ronghua; Wang, Zhaowen; Ma, Yinjie; Dai, Hui

2015-01-01

Highlights: • Spray combustion of E20 diesel in LTC condition shows a U-shape flame structure. • The chasing behavior of fuel spray exists near the spray axis. • Fuel ignition doesn’t initiate at the spray tip but in peripheral regions behind it. • An improper chamber structure may lead to a long post-combustion duration. - Abstract: Utilization of ethanol in diesel engines has been widely studied by means of engine experiments and emission detection. However, pertinent studies on the spray combustion process of ethanol–diesel blends are scarce. In order to verify the effect of ethanol in modern diesel engines, an experiment is conducted to visualize the spray combustion process of ethanol–diesel blend under LTC conditions. Stages including atomization, evaporation and combustion, are investigated individually to realize synergistic analysis. Meanwhile, considering the long time scale of combustion after fuel injection finishes, characteristics during and after injection period are both targeted in this paper. Moreover, measurement of macroscopic characteristics, such as spray tip penetration, spray spreading cone angle and flame lift off length, provides a quantitative profile of the spray structure. Results show that, evaporation, different from atomization, has little influence on spray penetration, but promotes the spray spreading angle and spray projected area. So does combustion, which enlarges the spray projected area further. Ignition takes place on the periphery behind the spray tip, then quickly extends to the whole head of the spray and forms a U-shape diffusion structure. After the injection period, the residual spray tail develops into wavelike structures due to absence of subsequent entrainment force. Also, the penetration speed falls greatly to an extent much slower than flame propagation, which frees the flame from the lift-off effect. Subsequently, the flame propagates upstream towards the nozzle orifice. After consumed all fuel in

Induced absorption and stimulated emission in a driven two-level atom

International Nuclear Information System (INIS)

Mavroyannis, C.

1992-01-01

We have considered the induced processes that occur in a driven two-level atom, where a laser photon is absorbed and emitted by the ground and by the excited states of the atom, respectively. In the low-intensity limit of the laser field, the induced spectra arising when a laser photon is absorbed by the ground state of the atom consist of two peaks describing induced absorption and stimulated-emission processes, respectively, where the former prevails over the latter. Asymmetry of the spectral lines occurs at off-resonance and its extent depends on the detuning of the laser field. The physical. process where a laser photon is emitted by the excited state is the reverse of that arising from the absorption of a laser photon by the ground state of the atom. The former differs from the latter in that the emission of a laser photon by the excited state occurs in the low frequency regime and that the stimulated-emission process prevails over that of the induced absorption. In this case, amplification of ultrashort pulses is likely to occur without the need of population inversion between the optical transitions. The computed spectra are graphically presented and discussed. (author)

Determination of cobalt in human liver by atomic absorption spectrometry with electrothermal atomization

International Nuclear Information System (INIS)

Caldas, E.D.; Gine-Rosias, M.F.; Dorea, J.G.

1991-01-01

A detailed study of the use of electrothermal atomic absorption spectrometry for the determination of cobalt in human liver is described. Comparisons of sample digestion using nitric acid or nitric acid plus perchloric acid, atomization procedures and the application of palladium and magnesium nitrate chemical modifiers were studied using NBS SRM 1577a Bovine Liver. The best results were achieved with sample decomposition in nitric acid, atomization from the tube wall and no chemical modifier. Cobalt was determined in 90 samples of livers from foetuses and deceased newborns using the standard addition method with an average recovery of 99.8%. (author). 30 refs.; 4 figs.; 2 tabs

Atomic emission and atomic fluorescence spectroscopy in the direct current plasma

International Nuclear Information System (INIS)

Hendrick, M.S.

1985-01-01

The Direct Current Plasma (DCP) was investigated as a source for Atomic Emission (AE) and Atomic Fluorescence Spectrometry (AFS). The DCP was optimized for AE analyses using simplex optimization and Box-Behnken partial factorial experimental design, varying argon flows, and plasma position. Results were compared with a univariate search carried out in the region of the simplex optimum. Canonical analysis demonstrated that no true optimum exists for sensitivity, precision, or drift. A stationary ridge, where combinations of conditions gave comparable instrumental responses, was found. The DCP as an excitation source for AFS in a flame was used for diagnostic studies of the DCP. Moving the aerosol introduction tube behind the DCP with respect to the flame improved the characteristics of the DCP as a narrow line source, although self-absorption was observed at high concentrations of metal salt solutions in the DCP. Detection limits for Cd, Co, Cr, Cu, Fe, Mg, Mn, Zn, and Ni were in the low ng/mL region. Theoretical expressions for scatter correction with a two-line technique were derived, although no correction was necessary to achieve accurate results for standard reference materials

Determination of arsenic, antimony, bismuth, cadmium, copper, lead, molybdenum, silver and zinc in geological materials by atomic-absorption spectrometry

Science.gov (United States)

Viets, J.G.; O'Leary, R. M.; Clark, Robert J.

1984-01-01

Arsenic, antimony, bismuth, cadmium, copper, lead, molybdenum, silver and zinc are very useful elements in geochemical exploration. In the proposed method, geological samples are fused with potassium pyrosulphate and the fusate is dissolved in a solution of hydrochloric acid, ascorbic acid and potassium iodide. When this solution is shaken with a 10% V/V Aliquat 336 - isobutyl methyl ketone organic phase, the nine elements of interest are selectively partitioned in the organic phase. All nine elements can then be determined in the organic phase using flame atomic-absorption spectrometry. The method is rapid and allows the determination of Ag and Cd at levels down to 0.1 p.p.m., Cu, Mo, and Zn down to 0.5 p.p.m., Pb, Bi and Sb down to 1 p.p.m. and As down to 5 p.p.m. in geological materials.

Determination of silver, bismuth, cadmium, copper, lead, and zinc in geologic materials by atomic absorption spectrometry with tricaprylylmethylammonium chloride

Science.gov (United States)

Viets, J.G.

1978-01-01

Interferences commonly encountered in the determination of silver, bismuth, cadmium, copper, lead, and zinc at crustal abundance levels are effectively eliminated using a rapid, sensitive, organic extraction technique. A potassium chlorate-hydrochloric acid digestion solubilizes the metals not tightly bound in the silicate lattice of rocks, soils, and stream sediments. The six metals are selectively extracted into a 10% Aliquat 336-MIBK organic phase in the presence of ascorbic acid and potassium iodide. Metals in the organic extract are determined by flame atomic absorption spectrometry to the 0.02-ppm level for silver, cadmium, copper, and zinc and to the 0.2-ppm level for bismuth and lead with a maximum relative standard deviation of 18.8% for known reference samples. An additional hydrofluoric acid digestion may be used to determine metals substituted in the silicate lattice.

Effects of turbulence enhancement on combustion process using a double injection strategy in direct-injection spark-ignition (DISI) gasoline engines

International Nuclear Information System (INIS)

Kim, Taehoon; Song, Jingeun; Park, Sungwook

2015-01-01

Highlights: • Using double injection strategy, turbulent kinetic energy can be improved with slight decrease in mixture homogeneity. • Retarded first injection timing reduces vapor fuel loss to intake port. • Double injection increases tumble intensity. • High turbulent intensity caused by double injection increases flame propagation speed. - Abstract: Direct-injection spark-ignition (DISI) gasoline engines have been spotlighted due to their high thermal efficiency. Increase in the compression ratio that result from the heat absorption effect of fuel vaporization induces higher thermal efficiency than found in port fuel injection (PFI) engines. Since fuel is injected at the cylinder directly, various fuel injection strategies can be used. In this study, turbulent intensity was improved by a double injection strategy while maintaining mixture homogeneity. To analyze the turbulence enhancement effects using the double injection strategy, a side fuel injected, homogeneous-charge-type DISI gasoline engine with a multi-hole-type injector was utilized. The spray model was evaluated using experimental data for various injection pressures and the combustion model was evaluated for varied ignition timing. First and second injection timing was swept by 20 degree interval. The turbulent kinetic energy and mixture inhomogeneity index were mapped. First injection at the middle of the intake stroke and second injection early in the compression stroke showed improved turbulent characteristics that did not significantly decrease with mixture homogeneity. A double injection case that showed improved turbulent intensity while maintaining an adequate level of mixture homogeneity and another double injection case that showed significantly improved turbulent intensity with a remarkable decrease in mixture homogeneity were considered for combustion simulation. We found that the improved turbulent intensity increased the flame propagation speed. Also, the mixture homogeneity

[Determination of trace cobalt in human urine by graphite furnace atomic absorption spectrometr].

Science.gov (United States)

Zhong, L X; Ding, B M; Jiang, D; Liu, D Y; Yu, B; Zhu, B L; Ding, L

2016-05-20

To establish a method to determine cobalt in human urine by graphite furnace atomic absorption spectrometry. Urine with 2% nitric acid diluted two-fold, to quantify the curve, graphite furnace atomic absorption spectrometric detection. Co was linear within 2.5~40.0 ng/ml with r>0.999. Spike experiment showed that Co received good recovery rate, which was 90.8%~94.8%. Intra-assay precisions were 3.2%~5.1% for Co, inter-assay precisions were 4.4%~5.2% for Co. The method by using graphite furnace atomic absorption spectrometr to determine urine Co was fast, accurate and with low matrix effect. It could meet the requirement in GBZ/T 210.5-2008.

Theoretical experimental study of the factors that govern the molybdenum absorption signal by means of electro thermic atomic absorption spectroscopy

International Nuclear Information System (INIS)

Garaboto Farfan, M. A.

1996-01-01

The formation of molybdenum carbides in the atomizer, used in the electro thermic atomic absorption spectroscopy, is responsible for incomplete analyte removal in its analysis. This generates the apparition of the memory effect and little precision in the results. In this work, different variables that could affect the molybdenum absorption sign were investigated, as well as the influence of hydrochloric acid on the memory effect, by means of studies in the different stages: drying, calcination and atomization, and the samples deposition order in molybdenum solutions, either acidified or not acidified [es

Application of Box-Behnken design in the optimisation of an on-line pre-concentration system using knotted reactor for cadmium determination by flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Souza, Anderson S.; Santos, Walter N.L. dos; Ferreira, Sergio L.C.

2005-01-01

The present paper proposes an on-line pre-concentration system for cadmium determination in drinking water using flame atomic absorption spectrometry (FAAS). Cadmium(II) ions are retained as 1-(2-pyridylazo)-2-naphthol (PAN) complex at the walls of a knotted reactor, followed of elution using hydrochloric acid solution. The optimization was performed in two steps using factorial design for preliminary evaluation and a Box-Behnken design for determination of the critical experimental conditions. The variables involved were: sampling flow-rate, reagent concentration, pH and buffer concentration, and as response the analytical signal (absorbance). The validation process was performed considering the parameters: linearity and other characteristics of the calibration curve, analytical features of on-line pre-concentration system, precision, effect of other ions in the pre-concentration system and accuracy. Using the optimized experimental conditions, the procedure allows cadmium determination with a detection limit (3 σ / S) of 0.10 μg L -1 , a quantification limit (10 σ / S) of 0.33 μg L -1 , and a precision, calculated as relative standard deviation (RSD) of 2.7% (n = 7) and 2.4% (n = 7) for cadmium concentrations of 5 and 25 μg L -1 , respectively. A pre-concentration factor of 18 and a sampling frequency of 48 h -1 were obtained. The recovery for cadmium in the presence of several ions demonstrated that this procedure could be applied for the analysis of water samples. The method was applied for cadmium determination in drinking water samples collected in Salvador City, Brazil. The cadmium concentrations found in five samples were lower than the maximum permissible levels established by the World Health Organization

Feasibility of dispersive liquid–liquid microextraction for extraction and preconcentration of Cu and Fe in red and white wine and determination by flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Seeger, Tassia S.; Rosa, Francisco C.; Bizzi, Cezar A.; Dressler, Valderi L.; Flores, Erico M.M.; Duarte, Fabio A.

2015-01-01

A method for extraction and preconcentration of Cu and Fe in red and white wines using dispersive liquid–liquid microextraction (DLLME) and determination by flame atomic absorption spectrometry (F AAS) was developed. Extraction was performed using sodium diethyldithiocarbamate as chelating agent and a mixture of 40 μL of 1,2-dichlorobenzene (extraction solvent) and 900 μL of methanol (dispersive solvent). Some parameters that influencing the extraction efficiency such as pH (2 to 5), concentration of chelating agent (0 to 2%), effect of salt addition (0 to 10%), number of washing steps (1 to 4) and centrifugation time (0 to 15 min) were studied. Accuracy was evaluated after microwave-assisted digestion in closed vessels and analytes were determined by inductively coupled plasma optical emission spectrometry. Agreement with the proposed method ranged from 91 to 110 and from 89 to 113% for Cu and Fe, respectively. Calibration of F AAS instrument was performed using analyte addition method and limits of detection were 6.3 and 2.4 μg L −1 for Cu and Fe, respectively. The proposed method was applied for the determination of Cu and Fe in five samples of red wine and three samples of white wine, with concentration ranging from 21 to 178 μg L −1 and from 1.38 to 3.74 mg L −1 , respectively. - Highlights: • Determination of Cu and Fe in wine using DLLME and F AAS • High preconcentration factors and low LODs were achieved. • Alternative method for the determination of Cu and Fe in wine for routine analysis

Feasibility of dispersive liquid–liquid microextraction for extraction and preconcentration of Cu and Fe in red and white wine and determination by flame atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Seeger, Tassia S.; Rosa, Francisco C.; Bizzi, Cezar A.; Dressler, Valderi L.; Flores, Erico M.M.; Duarte, Fabio A., E-mail: fabioand@gmail.com

2015-03-01

A method for extraction and preconcentration of Cu and Fe in red and white wines using dispersive liquid–liquid microextraction (DLLME) and determination by flame atomic absorption spectrometry (F AAS) was developed. Extraction was performed using sodium diethyldithiocarbamate as chelating agent and a mixture of 40 μL of 1,2-dichlorobenzene (extraction solvent) and 900 μL of methanol (dispersive solvent). Some parameters that influencing the extraction efficiency such as pH (2 to 5), concentration of chelating agent (0 to 2%), effect of salt addition (0 to 10%), number of washing steps (1 to 4) and centrifugation time (0 to 15 min) were studied. Accuracy was evaluated after microwave-assisted digestion in closed vessels and analytes were determined by inductively coupled plasma optical emission spectrometry. Agreement with the proposed method ranged from 91 to 110 and from 89 to 113% for Cu and Fe, respectively. Calibration of F AAS instrument was performed using analyte addition method and limits of detection were 6.3 and 2.4 μg L{sup −1} for Cu and Fe, respectively. The proposed method was applied for the determination of Cu and Fe in five samples of red wine and three samples of white wine, with concentration ranging from 21 to 178 μg L{sup −1} and from 1.38 to 3.74 mg L{sup −1}, respectively. - Highlights: • Determination of Cu and Fe in wine using DLLME and F AAS • High preconcentration factors and low LODs were achieved. • Alternative method for the determination of Cu and Fe in wine for routine analysis.

Atomic absorption spectrophotometric determination of microamounts of beryllium in aluminum and copper using solvent extraction with acetylacetone

International Nuclear Information System (INIS)

Matsusaki, Koji

1975-01-01

A sensitive method for the determination of microamounts of beryllium in aluminum and copper by atomic absorption spectrophotometry using the methylisobutylketone (MIBK) extraction with acetylacetone (AA) was investigated. An aqueous sample solution containing (0.5--5)μg of beryllium and less than 100 mg of aluminum or less than 500 mg of copper was taken into a 100-ml separation funnel, and 2 ml of 5% AA, 20 mg of EDTA for 1 mg of aluminum or 8.8 mg of EDTA for 1 mg of copper, and 10 ml of saturated NaCl solution were added. The pH was adjusted to 5--7 with 10 ml of 2 M NaCH 3 COO-CH 3 COOH buffer, and the solution was diluted to 50 ml. After 10 minutes, the solution was shaken for 2 minutes with 10 ml of MIBK. The organic phase was introduced into a nitrous oxide-acetylene flame and the absorption measured at 234.9 nm against a reagent blank. None of metal elements interfered with the determination of beryllium, and beryllium above 0.001% in aluminum, and above 0.0002% in copper was determined. This method was successfully applied to the determination of beryllium in aluminum and copper alloys. (auth.)

Ultrasound-assisted extraction technique for establishing selenium contents in breast cancer biopsies by Zeeman-electrothermal atomic absorption spectrometry using multi-injection

International Nuclear Information System (INIS)

Lavilla, I.; Mosquera, A.; Millos, J.; Cameselle, J.; Bendicho, C.

2006-01-01

A solid-liquid extraction method is developed to establish the contents of selenium in breast cancer biopsies. The method is based on the ultrasound-assisted extraction of selenium from pretreated biopsies prior to Se determination by atomic absorption spectrometry with longitudinal-Zeeman background correction. Fifty-one breast biopsies were collected from the Cies Hospital (Vigo, Spain), 32 of which correspond to tumor tissue and 19 to normal tissue (parenchyma). Difficulties arising from the samples analyzed, i.e. small samples mass (50-100 mg), extremely low Se contents and sample texture modification including tissue hardening due to formaldehyde preservation are addressed and overcome. High intensity sonication using a probe together with addition of hydrogen peroxide succeeded in completely extracting Se from biopsies. The multiple injection technique was useful to tackle the low Se contents present in some biopsies. The detection limit was 25 ng g -1 of Se and the precision, expressed as relative standard deviation, was less than 10%. Se contents ranged from 0.08 to 0.4 μg g -1 for parenchyma samples and from 0.09 to 0.8 μg g -1 for tumor samples. In general, Se levels in tumor biopsies were higher as compared with the adjacent normal tissue in 19 patients by a factor of up to 6. Analytical data confirmed Se accumulation in the breast tumors

Preconcentration and determination of vanadium and molybdenum in milk, vegetables and foodstuffs by ultrasonic-thermostatic-assisted cloud point extraction coupled to flame atomic absorption spectrometry.

Science.gov (United States)

Gürkan, Ramazan; Korkmaz, Sema; Altunay, Nail

2016-08-01

A new ultrasonic-thermostatic-assisted cloud point extraction procedure (UTA-CPE) was developed for preconcentration at the trace levels of vanadium (V) and molybdenum (Mo) in milk, vegetables and foodstuffs prior to determination via flame atomic absorption spectrometry (FAAS). The method is based on the ion-association of stable anionic oxalate complexes of V(V) and Mo(VI) with [9-(diethylamino)benzo[a]phenoxazin-5-ylidene]azanium; sulfate (Nile blue A) at pH 4.5, and then extraction of the formed ion-association complexes into micellar phase of polyoxyethylene(7.5)nonylphenyl ether (PONPE 7.5). The UTA-CPE is greatly simplified and accelerated compared to traditional cloud point extraction (CPE). The analytical parameters optimized are solution pH, the concentrations of complexing reagents (oxalate and Nile blue A), the PONPE 7.5 concentration, electrolyte concentration, sample volume, temperature and ultrasonic power. Under the optimum conditions, the calibration curves for Mo(VI) and V(V) are obtained in the concentration range of 3-340µgL(-1) and 5-250µgL(-1) with high sensitivity enhancement factors (EFs) of 145 and 115, respectively. The limits of detection (LODs) for Mo(VI) and V(V) are 0.86 and 1.55µgL(-1), respectively. The proposed method demonstrated good performances such as relative standard deviations (as RSD %) (≤3.5%) and spiked recoveries (95.7-102.3%). The accuracy of the method was assessed by analysis of two standard reference materials (SRMs) and recoveries of spiked solutions. The method was successfully applied into the determination of trace amounts of Mo(VI) and V(V) in milk, vegetables and foodstuffs with satisfactory results. Copyright © 2016 Elsevier B.V. All rights reserved.

A Comprehensive X-Ray Absorption Model for Atomic Oxygen

Science.gov (United States)

Gorczyca, T. W.; Bautista, M. A.; Hasoglu, M. F.; Garcia, J.; Gatuzz, E.; Kaastra, J. S.; Kallman, T. R.; Manson, S. T.; Mendoza, C.; Raassen, A. J. J.;

Lithium determination in whole blood by flame atomic emission spectrometry

International Nuclear Information System (INIS)

Rahman, S.; Khalid, N.; Nasimullah; Iqbal, M.Z.

2003-01-01

A simple and rapid method for the determination of lithium in whole blood using Flame atomic emission spectrometry is described. No sample preparation was required apart from dilution with 0.02 N HNO/sub 3/. The reliability of the method was determined by analyzing Standard Reference Material (SRM) under identical experimental conditions and comparing the determined lithium concentration with the reported value. These were in good agreement with each other. The determined range of lithium in the whole blood of fifty-six healthy adult volunteers (28 males and 28 females) were 13.1 - 47.8 mg L-1. The determined average concentration of lithium in whole blood was compared with the reported values of other countries. The data was statistically analyzed with respect to sex and different age groups. (author)

Determination of silicon in biomass and products of pyrolysis process via high-resolution continuum source atomic absorption spectrometry.

Science.gov (United States)

Nakadi, Flávio V; Prodanov, Caroline; Boschetti, Wiliam; Vale, Maria Goreti R; Welz, Bernhard; de Andrade, Jailson B

2018-03-01

Thermochemical processes can convert the biomass into fuels, such as bio-oil. The biomass submitted to pyrolysis process, such as fibers, are generally rich in silicon, an element that can lead to damages in an engine when there is high concentration in a fuel. High-resolution continuum source atomic absorption spectrometry (HR-CS AAS) is an interesting alternative for Si determination in the products and byproducts of the pyrolysis process because, besides the flame (F) and graphite furnace (GF) atomizers, it has enhanced the application of direct analysis of solid samples (SS) within GF. This study aimed the development of methods to determine Si in biomass samples, their products and byproducts using HR-CS AAS. A high-resolution continuum source atomic absorption spectrometer contrAA 700 equipped with F and GF atomizers was used throughout the study. HR-CS F AAS (λ = 251.611nm, 1 detection pixel, N 2 O/C 2 H 2 flame) was used to evaluate Si content in biomass and ash, after a microwave-assisted acid digestion with HNO 3 and HF. HR-CS GF AAS (T pyr = 1400°C, T atom = 2650°C) has evaluated Si in pyrolysis water and bio-oil at 251.611nm, and in peach pit biomass and ash at 221.174nm using SS, both wavelengths with 1 detection pixel. Rhodium (300μg) was applied as permanent modifier and 10μgPd + 6μg Mg were pipetted onto the standards/samples at each analysis. Three different biomass samples were studied: palm tree fiber, coconut fiber and peach pit, and three certified reference materials (CRM) were used to verify the accuracy of the methods. The figures of merit were LOD 0.09-20mgkg -1 , and LOQ 0.3-20mgkg -1 , considering all the methods. There were no significant differences between the CRM certified values and the determined ones, using a Student t-test with a confidence interval of 95% (n = 5). Si concentration ranged from 0.11-0.92% mm -1 , 1.1-1.7mgkg -1 , 3.3-13mgkg -1 , and 0.41-1.4%mm -1 , in biomass, bio-oil, pyrolysis water and ash, respectively

Chemical analysis of carbonates and carbonate rocks by atomic absorption analysis

Energy Technology Data Exchange (ETDEWEB)

Tardon, S

1981-01-01

Evaluates methods of determining chemical composition of rocks surrounding black coal seams. Carbonate rock samples were collected in the Ostrava-Karvina coal mines. Sampling methods are described. Determination of the following elements and compounds in carbonate rocks is discussed: calcium, magnesium, iron, manganese, barium, silicon, aluminium, titanium, sodium, potassium, sulfur trioxide, phosphorus pentoxide, water and carbon dioxide. Proportion of compounds insoluble in water in the investigated rocks is also determined. Most of the elements are determined by means of atomic absorption analysis. Phosphorus is also determined by atomic absorption analysis. Other compounds are determined gravimetrically. The described procedure permits weight of a rock sample to be reduced to 0.5 g without reducing analysis accuracy. The results of determining carbonate rock components by X-ray analysis and by chemical analysis are compared. Equipment used for atomic absorption analysis is characterized (the 503 Perkin-Elmer and the CF-4 Optica-Milano spectrophotometers). The analyzed method for determining carbonate rock permits more accurate classification of rocks surrounding coal seams and rock impurities in run-of-mine coal. (22 refs.) (In Czech)

Two-dimensional atom localization via a coherence-controlled absorption spectrum in an N-tripod-type five-level atomic system

International Nuclear Information System (INIS)

Ding Chunling; Li Jiahua; Yang Xiaoxue; Zhan Zhiming; Liu Jibing

2011-01-01

A scheme of two-dimensional atom localization based on a coherence-controlled absorption spectrum in an N-tripod-type five-level system is proposed, in which the atom interacts with a weak probe field and three standing-wave fields. Position information of the atom can be achieved by measuring the probe absorption. It is found that the localization properties are significantly improved due to the interaction of dark resonances. It is also shown that the localization factors depend strongly on the system parameters that lead to such spatial structures of localization as chain-like, wave-like, '8'-like, spike-like, crater-like and heart-like patterns. By properly adjusting the system parameters, we can achieve a high-precision and high-resolution atom localization under certain conditions.

Ionisation of hydrogen-like atoms by a multiphoton absorption process; Ionisation des atomes hydrogenoides par un processus d'absorption multiphotonique

Energy Technology Data Exchange (ETDEWEB)

Gontier, Y; Trahin, M [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

1967-07-01

The general expression for the amplitude of the probability of ionisation by a multiphoton absorption process is derived. Its non-relativistic limit is taken and the bipolar approximation is used for calculating the ionisation cross-section of hydrogen-like atoms. This latter involves the summation over intermediate virtual states by means of: a) a recursion relationship concerning angular functions, b) a particular technique which when applied to radial functions makes it possible to solve a system of inhomogeneous first-order differential equations. (authors) [French] On etablit l'expression generale de l'amplitude de probabilite d'ionisation par un processus d'absorption multiphotonique. On en prend la limite non-relativiste et l'on utilise l'approximation dipolaire avant de calculer la section efficace d'ionisation d'atomes hydrogenoides. Cette derniere fait intervenir des sommations sur des etats virtuels intermediaires effectuees a l'aide: a) d'une relation de recurrence qui concerne les fonctions angulaires, b) d'une technique particuliere qui, appliquee aux fonctions radiales, conduit a resoudre un systeme d'equations differentielles inhomogenes du premier ordre. (auteur)

Optimization of trace elements determination (Arsenic and chromium) in blood and serum of human by electrothermal atomic absorption spectrometry

International Nuclear Information System (INIS)

Ahmadi Faghih, M. A.; Aflaki, F.

2003-01-01

Trace elements play an important role in the bio physiology of cells by affecting their growth and contributions to various biological processes such as wound healing. Determination of toxic trace elements in biological fluids is an important subject of interest for toxicological purposes. Increasing the concentration of these elements in the blood levels, cause serious diseases in patients. Recently instrumental analysis procedures such as atomic absorption spectrometry have been used in clinical measurements for determination of many toxic trace elements in the biological samples. In this paper we are reporting the study of various methods of blood and serum samples preparation for determining the toxic trace elements of Arsenic and Chromium. The measurement of this elements performed by using electrothermal atomic absorption spectrometry. The best and reliable results for Chromium analysis was achieved by injection of diluted serum samples, where the samples were diluted with H CI 0.1N. In Arsenic analysis, the best results obtained by extraction with aqueous solution of TCA. For determining all of these elements the RSD% was less than 5%

Optical measurements of atomic oxygen concentration, temperature and nitric oxide production rate in flames

Science.gov (United States)

Myhr, Franklin Henry

An optical method for measuring nitric oxide (NO) production rates in flames was developed and characterized in a series of steady, one-dimensional, atmospheric-pressure laminar flames of 0.700 Hsb2/0.199 Nsb2/0.101 COsb2 or 0.700 CHsb4/0.300 Nsb2 (by moles) with dry air, with equivalence ratios from 0.79 to 1.27. Oxygen atom concentration, (O), was measured by two-photon laser-induced fluorescence (LIF), temperature was measured by ultraviolet Rayleigh scattering, and nitrogen concentration was calculated from supplied reactant flows; together this information was used to calculate the NO production rate through the thermal (Zel'dovich) mechanism. Measurements by two other techniques were compared with results from the above method. In the first comparison, gas sampling was used to measure axial NO concentration profiles, the slopes of which were multiplied by velocity to obtain total NO production rates. In the second comparison, LIF measurements of hydroxyl radical (OH) were used with equilibrium water concentrations and a partial equilibrium assumption to find (O). Nitric oxide production rates from all three methods agreed reasonably well. Photolytic interference was observed during (O) LIF measurements in all of the flames; this is the major difficulty in applying the optical technique. Photolysis of molecular oxygen in lean flames has been well documented before, but the degree of interference observed in the rich flames suggests that some other molecule is also dissociating; the candidates are OH, CO, COsb2 and Hsb2O. An extrapolative technique for removing the effects of photolysis from (O) LIF measurements worked well in all flames where NO production was significant. Using the optical method to measure NO production rates in turbulent flames will involve a tradeoff among spatial resolution, systematic photolysis error, and random shot noise. With the conventional laser system used in this work, a single pulse with a resolution of 700 mum measured NO

Preparation of modified magnetic nanoparticles as a sorbent for the preconcentration and determination of cadmium ions in food and environmental water samples prior to flame atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Mirabi, Ali; Dalirandeh, Zeinab [Department of Chemistry, Qaemshahr Branch, Islamic Azad University, Qaemshahr (Iran, Islamic Republic of); Rad, Ali Shokuhi, E-mail: a.shokuhi@qaemshahriau.ac.ir [Department of Chemical Engineering, Qaemshahr Branch, Islamic Azad University, Qaemshahr (Iran, Islamic Republic of)

2015-05-01

A new method has been developed for the separation/preconcentration of trace level cadmium ions using diphenyl carbazone/sodium dodecyl sulfate immobilized on magnetic nanoparticle Fe{sub 3}O{sub 4} as a new sorbent SPE and their determination by flame atomic absorption spectrometry (FAAS). Synthesized nanoparticle was characterized by scanning electron microscope (SEM) and transmission electron microscope (TEM). Various influencing parameters on the separation and preconcentration of trace level cadmium ions such as, pH value, amount of nanoparticles, amount of diphenyl carbazone, condition of eluting solution, the effects of matrix ions were examined. The cadmium ions can be eluted from the modified magnetic nanoparticle using 1 mol L{sup −1} HCl as a desorption reagent. The detection limit of this method for cadmium was 3.71 ng ml{sup −1} and the R.S.D. was 0.503% (n=6). The advantages of this new method include rapidity, easy preparation of sorbents and a high concentration factor. The proposed method has been applied to the determination of Cd ions at trace levels in real samples such as, green tea, rice, tobacco, carrot, lettuce, ginseng, spice, tap water, river water, sea water with satisfactory results. - Highlights: • MNPs method is economical, simple, rapid and sensitive for trace analysis of Cd. • High preconcentration factor was obtained easily through this method. • A detection limit at ng mL{sup −1} level was achieved with 100.0 mL of sample. • This method provides good repeatability and extraction efficiency in a short time.