NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR EXTRACTION OF METALS FROM SOIL, DUST, AIR FILTER, AND SURFACE AND DERMAL SAMPLES FOR AA (GRAPHITE FURNACE OR FLAME) OR ICP-AES ANALYSIS (BCO-L-3.1)

EPA Science Inventory

The purpose of this SOP is to describe the acid digestion of soil, house dust, air filter, and surface or dermal wipe samples for analysis using inductively coupled plasma atomic emissions spectrometry (ICP-AES) and/or graphite furnace atomic absorption spectrometry (GFAAS) or fl...

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

PubMed

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.

Surface tuning laser desorption/ionization mass spectrometry (STLDI-MS) for the analysis of small molecules using quantum dots.

PubMed

Abdelhamid, Hani Nasser; Chen, Zhen-Yu; Wu, Hui-Fen

2017-08-01

In most applications of quantum dots (QDs) for surface-assisted laser desorption/ionization mass spectrometry (SALDI-MS), one side of QDs is supported by a solid substrate (stainless - steel plate), whereas the other side is in contact with the target analytes. Therefore, the surface capping agent of QDs is a key parameter for laser desorption/ionization mass spectrometry (LDI-MS). Cadmium telluride quantum dots (CdTe QDs) modified with different capping agents are synthesized, characterized, and applied for surface tuning laser desorption/ionization mass spectrometry (STLDI-MS). Data shows that CdTe quantum dot modified cysteine (cys@CdTe QDs) has an absorption that matches with the wavelength of the N 2 laser (337 nm). The synergistic effect of large surface area and absorption of the laser irradiation of cys@CdTe QDs enhances the LDI-MS process for small - molecule analysis, including α-, β-, and γ-cyclodextrin, gramicidin D, perylene, pyrene, and triphenylphosphine. Cys@CdTe QDs are also applied using Al foils as substrates. Aluminum foil combined with cys@CdTe QDs enhances the ionization efficiency and is cheap compared to traditional matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) with a stainless - steel plate.

Overcoming Matrix Effects in a Complex Sample: Analysis of Multiple Elements in Multivitamins by Atomic Absorption Spectroscopy

ERIC Educational Resources Information Center

Arnold, Randy J.; Arndt, Brett; Blaser, Emilia; Blosser, Chris; Caulton, Dana; Chung, Won Sog; Fiorenza, Garrett; Heath, Wyatt; Jacobs, Alex; Kahng, Eunice; Koh, Eun; Le, Thao; Mandla, Kyle; McCory, Chelsey; Newman, Laura; Pithadia, Amit; Reckelhoff, Anna; Rheinhardt, Joseph; Skljarevski, Sonja; Stuart, Jordyn; Taylor, Cassie; Thomas, Scott; Tse, Kyle; Wall, Rachel; Warkentien, Chad

2011-01-01

A multivitamin tablet and liquid are analyzed for the elements calcium, magnesium, iron, zinc, copper, and manganese using atomic absorption spectrometry. Linear calibration and standard addition are used for all elements except calcium, allowing for an estimate of the matrix effects encountered for this complex sample. Sample preparation using…

U.S.-MEXICO BORDER PROGRAM ARIZONA BORDER STUDY--STANDARD OPERATING PROCEDURE FOR EXTRACTION OF METALS FROM SOIL, DUST, AIR FILTER, AND SURFACE AND DERMAL WIPE SAMPLES FOR AA (GRAPHITE FURNACE OR FLAME) OR ICP-AES ANALYSIS (BCO-L-3.1)

EPA Science Inventory

The purpose of this SOP is to describe the acid digestion of soil, house dust, air filter, and surface or dermal wipe samples for analysis using inductively coupled plasma atomic emissions spectrometry (ICP-AES) and/or graphite furnace atomic absorption spectrometry (GFAAS) or fl...

Atomic Absorption, Atomic Fluorescence, and Flame Emission Spectrometry.

ERIC Educational Resources Information Center

Horlick, Gary

1984-01-01

This review is presented in six sections. Sections focus on literature related to: (1) developments in instrumentation, measurement techniques, and procedures; (2) performance studies of flames and electrothermal atomizers; (3) applications of atomic absorption spectrometry; (4) analytical comparisons; (5) atomic fluorescence spectrometry; and (6)…

A vastly improved method for in situ stable isotope analysis of very small water samples.

NASA Astrophysics Data System (ADS)

Coleman, M. L.; Christensen, L. E.; Kriesel, J.; Kelly, J.; Moran, J.; Vance, S.

2016-12-01

The stable isotope compositions of hydrogen and oxygen in water, ice and hydrated minerals are key characteristics to determine the origin and history of the material. Originally, analyses were performed by separating hydrogen and preparing CO2 from the oxygen in water for stable isotope ratio mass spectrometry. Subsequently, infrared absorption spectrometry in either a Herriot cell or by cavity ring down allowed direct analysis of water vapor. We are developing an instrument, intended for spaceflight and in situ deployment, which will exploit Capillary Absorption Spectrometry (CAS) for the H and O isotope analysis and a laser to sample planetary ices and hydrated minerals. The Tunable Laser Spectrometer (TLS) instrument (part of SAM on the MSL rover Curiosity) works by infrared absorption and we use its performance as a benchmark for comparison. TLS has a relatively large sample chamber to contain mirrors which give a long absorption pathlength. CAS works on the same principle but utilizes a hollow optic fiber, greatly reducing the sample volume. The fiber is a waveguide, enhancing the laser - water-vapor interaction and giving more than four orders of magnitude increase in sensitivity, despite a shorter optical path length. We have calculated that a fiber only 2 m long will be able to analyze 5 nanomoles of water with a precision of less than 1 per mil for D?H. The fiber is coiled to minimize instrument volume. Our instrument will couple this analytical capability with laser sampling to free water from hydrated minerals and ice and ideally we would use the same laser via a beam-splitter both for sampling and analysis. The ability to analyze very small samples is of benefit in two ways. In this concept it will allow much faster analysis of small sub-samples, while the high spatial sampling resolution offered by the laser will allow analysis of the heterogeneity of isotopic composition within grains or crystals, revealing the history of their growth.

Separation, identification and quantification of carotenoids and chlorophylls in dietary supplements containing Chlorella vulgaris and Spirulina platensis using High Performance Thin Layer Chromatography.

PubMed

Hynstova, Veronika; Sterbova, Dagmar; Klejdus, Borivoj; Hedbavny, Josef; Huska, Dalibor; Adam, Vojtech

2018-01-30

In this study, 14 commercial products (dietary supplements) containing alga Chlorella vulgaris and cyanobacteria Spirulina platensis, originated from China and Japan, were analysed. UV-vis spectrophotometric method was applied for rapid determination of chlorophylls, carotenoids and pheophytins; as degradation products of chlorophylls. High Performance Thin-Layer Chromatography (HPTLC) was used for effective separation of these compounds, and also Atomic Absorption Spectrometry for determination of heavy metals as indicator of environmental pollution. Based on the results obtained from UV-vis spectrophotometric determination of photosynthetic pigments (chlorophylls and carotenoids), it was confirmed that Chlorella vulgaris contains more of all these pigments compared to the cyanobacteria Spirulina platensis. The fastest mobility compound identified in Chlorella vulgaris and Spirulina platensis using HPTLC method was β-carotene. Spectral analysis and standard calibration curve method were used for identification and quantification of separated substances on Thin-Layer Chromatographic plate. Quantification of copper (Cu 2+ , at 324.7 nm) and zinc (Zn 2+ , at 213.9nm) was performed using Flame Atomic Absorption Spectrometry with air-acetylene flame atomization. Quantification of cadmium (Cd 2+ , at 228.8 nm), nickel (Ni 2+ , at 232.0nm) and lead (Pb 2+ , at 283.3nm) by Electrothermal Graphite Furnace Atomic Absorption Spectrometry; and quantification of mercury (Hg 2+ , at 254nm) by Cold Vapour Atomic Absorption Spectrometry. Copyright © 2017 Elsevier B.V. All rights reserved.

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

USGS Publications Warehouse

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

1981-01-01

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

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

NASA Astrophysics Data System (ADS)

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, < 0.4-6 ng g - 1 in gasoline, < 0.5-2 ng g - 1 in atmospheric oil, < 6-100 ng g - 1 in heavy vacuum oil and 140-300 ng g - 1 in distillation residue.

A comparison of geochemical exploration techniques and sample media within accretionary continental margins: an example from the Pacific Border Ranges, Southern Alaska, U.S.A.

USGS Publications Warehouse

Sutley, S.J.; Goldfarb, R.J.; O'Leary, R. M.; Tripp, R.B.

1990-01-01

The Pacific Border Ranges of the southern Alaskan Cordillera are composed of a number of allochthonous tectonostratigraphic terranes. Within these terranes are widespread volcanogenic, massive sulfide deposits in and adjacent to portions of accreted ophiolite complexes, bands and disseminations of chromite in accreted island-arc ultramafic rocks, and epigenetic, gold-bearing quartz veins in metamorphosed turbidite sequences. A geochemical pilot study was undertaken to determine the most efficient exploration strategy for locating these types of mineral deposits within the Pacific Border Ranges and other typical convergent continental margin environments. High-density sediment sampling was carried out in first- and second-order stream channels surrounding typical gold, chromite and massive sulfide occurrences. At each site, a stream-sediment and a panned-concentrate sample were collected. In the laboratory, the stream sediments were sieved into coarse-sand, fine- to medium-sand, and silt- to clay-size fractions prior to analysis. One split of the panned concentrates was retained for analysis; a second split was further concentrated by gravity separation in heavy liquids and then divided into magnetic, weakly magnetic and nonmagnetic fractions for analysis. A number of different techniques including atomic absorption spectrometry, inductively coupled plasma atomic emission spectrometry and semi-quantitative emission spectrography were used to analyze the various sample media. Comparison of the various types of sample media shows that in this tectonic environment it is most efficient to include a silt- to clay-size sediment fraction and a panned-concentrate sample. Even with the relatively low detection limits for many elements by plasma spectrometry and atomic absorption spectrometry, anomalies reflecting the presence of gold veins could not be identified in any of the stream-sediment fractions. Unseparated panned-concentrate samples should be analyzed by emission spectroscopy and atomic absorption spectrometry for Ag and Au. If, however, magnetic and nonmagnetic concentrate fractions are used in a reconnaissance program, semiquantitative emission spectrography is adequate for all analytical work. ?? 1990.

Accuracy of trace element determinations in alternate fuels

NASA Technical Reports Server (NTRS)

Greenbauer-Seng, L. A.

1980-01-01

A review of the techniques used at Lewis Research Center (LeRC) in trace metals analysis is presented, including the results of Atomic Absorption Spectrometry and DC Arc Emission Spectrometry of blank levels and recovery experiments for several metals. The design of an Interlaboratory Study conducted by LeRC is presented. Several factors were investigated, including: laboratory, analytical technique, fuel type, concentration, and ashing additive. Conclusions drawn from the statistical analysis will help direct research efforts toward those areas most responsible for the poor interlaboratory analytical results.

Application of Plackett-Burman and Doehlert designs for optimization of selenium analysis in plasma with electrothermal atomic absorption spectrometry.

PubMed

El Ati-Hellal, Myriam; Hellal, Fayçal; Hedhili, Abderrazek

2014-10-01

The aim of this study was the optimization of selenium determination in plasma samples with electrothermal atomic absorption spectrometry using experimental design methodology. 11 variables being able to influence selenium analysis in human blood plasma by electrothermal atomic absorption spectrometry (ETAAS) were evaluated with Plackett-Burman experimental design. These factors were selected from sample preparation, furnace program and chemical modification steps. Both absorbance and background signals were chosen as responses in the screening approach. Doehlert design was used for method optimization. Results showed that only ashing temperature has a statistically significant effect on the selected responses. Optimization with Doehlert design allowed the development of a reliable method for selenium analysis with ETAAS. Samples were diluted 1/10 with 0.05% (v/v) TritonX-100+2.5% (v/v) HNO3 solution. Optimized ashing and atomization temperatures for nickel modifier were 1070°C and 2270°C, respectively. A detection limit of 2.1μgL(-1) Se was obtained. Accuracy of the method was checked by the analysis of selenium in Seronorm™ Trace element quality control serum level 1. The developed procedure was applied for the analysis of total selenium in fifteen plasma samples with standard addition method. Concentrations ranged between 24.4 and 64.6μgL(-1), with a mean of 42.6±4.9μgL(-1). The use of experimental designs allowed the development of a cheap and accurate method for selenium analysis in plasma that could be applied routinely in clinical laboratories. Copyright © 2014 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

Considerations in As analysis and speciation

USGS Publications Warehouse

Edwards, M.; Patel, S.; McNeil, L.; Chen, H.W.; Frey, M.; Eaton, A.D.; Antweiler, Ronald C.; Taylor, Howard E.

1998-01-01

This article summarizes recent experiences in arsenic (As) quantification, preservation, and speciation developed during AWWA Research Foundation (AWWARF) and Water Industry Technical Action Fund (WITAF) projects. The goal of this article is to alert analysts and decision-makers to potential problems in As analysis and speciation, because there appear to be several unresolved problems with routine analytical approaches. In true split drinking water samples As was quantified by three accepted analytical methods in three laboratories. The techniques used were graphite furnace atomic absorption spectrometry (GFAAS), inductively coupled plasma mass spectrometry (ICP-MS), and hydride generation inductively coupled plasma-emission spectrometry (HG-ICP-AES). Experimental findings are organized into sections on As analysis, particulate As in water supplies, and examination of As speciation methods.

Measurements of sulfur compounds in CO 2 by diode laser atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Franzke, J.; Stancu, D. G.; Niemax, K.

2003-07-01

Two simple methods for the analysis of the total concentration of sulfur in CO 2 by diode laser atomic absorption spectrometry of excited, metastable sulfur atoms in a direct current discharge are presented. In the first method, the CO 2 sample gas is mixed with the plasma gas (Ar or He) while the second is based on reproducible measurements of the sulfur released from the walls in a helium discharge after being deposited as a result of operating the discharge in pure CO 2 sample gas. The detection limits obtained satisfy the requirements for the control of sulfur compounds in CO 2 used in the food and beverage industry.

Statistical evaluation of an inductively coupled plasma atomic emission spectrometric method for routine water quality testing

USGS Publications Warehouse

Garbarino, J.R.; Jones, B.E.; Stein, G.P.

1985-01-01

In an interlaboratory test, inductively coupled plasma atomic emission spectrometry (ICP-AES) was compared with flame atomic absorption spectrometry and molecular absorption spectrophotometry for the determination of 17 major and trace elements in 100 filtered natural water samples. No unacceptable biases were detected. The analysis precision of ICP-AES was found to be equal to or better than alternative methods. Known-addition recovery experiments demonstrated that the ICP-AES determinations are accurate to between plus or minus 2 and plus or minus 10 percent; four-fifths of the tests yielded average recoveries of 95-105 percent, with an average relative standard deviation of about 5 percent.

Two new advanced forms of spectrometry for space and commercial applications

NASA Technical Reports Server (NTRS)

Schlager, Kenneth J.

1991-01-01

Reagentless ultraviolet absorption spectrometry (UVAS) and Liquid Atomic Emission Spectrometry (LAES) represent new forms of spectrometry with extensive potential in both space and commercial applications. Originally developed under KSC sponsorship for monitoring nutrient solutions for the Controlled Ecological Life Support System (CELSS), both UVAS and LAES have extensive analytical capabilities for both organic and inorganic chemical compounds. Both forms of instrumentation involve the use of remote fiber optic probes and real-time measurements for on-line process monitoring. Commercial applications exist primarily in environmental analysis and for process control in the chemical, pulp and paper, food processing, metal plating, and water/wastewater treatment industries.

Chemometric evaluation of Cd, Co, Cr, Cu, Ni (inductively coupled plasma optical emission spectrometry) and Pb (graphite furnace atomic absorption spectrometry) concentrations in lipstick samples intended to be used by adults and children.

PubMed

Batista, Érica Ferreira; Augusto, Amanda dos Santos; Pereira-Filho, Edenir Rodrigues

2016-04-01

A method was developed for determining the concentrations of Cd, Co, Cr, Cu, Ni and Pb in lipstick samples intended to be used by adults and children using inductively coupled plasma optical emission spectrometry (ICP OES) and graphite furnace atomic absorption spectrometry (GF AAS) after treatment with dilute HNO3 and hot block. The combination of fractional factorial design and Desirability function was used to evaluate the ICP OES operational parameters and the regression models using Central Composite and Doehlert designs were calculated to stablish the best working condition for all analytes. Seventeen lipstick samples manufactured in different countries with different colors and brands were analyzed. Some samples contained high concentrations of toxic elements, such as Cr and Pb, which are carcinogenic and cause allergic and eczematous dermatitis. The maximum concentration detected was higher than the permissible safe limits for human use, and the samples containing these high metal concentrations were intended for use by children. Principal component analysis (PCA) was used as a chemometrics tool for exploratory analysis to observe the similarities between samples relative to the metal concentrations (a correlation between Cd and Pb was observed). Copyright © 2015 Elsevier B.V. All rights reserved.

Determination of mercury in hair: Comparison between gold amalgamation-atomic absorption spectrometry and mass spectrometry.

PubMed

Domanico, Francesco; Forte, Giovanni; Majorani, Costanza; Senofonte, Oreste; Petrucci, Francesco; Pezzi, Vincenzo; Alimonti, Alessandro

2017-09-01

Mercury is a heavy metal that causes serious health problems in exposed subjects. The most toxic form, i.e., methylmercury (MeHg), is mostly excreted through human hair. Numerous analytical methods are available for total Hg analysis in human hair, including cold vapour atomic fluorescence spectrometry (CV-AFS), inductively coupled plasma mass spectrometry (ICP-MS) and thermal decomposition amalgamation atomic absorption spectrometry (TDA-AAS). The aim of the study was to compare the TDA-AAS with the ICP-MS in the Hg quantification in human hair. After the washing procedure to minimize the external contamination, from each hair sample two aliquots were taken; the first was used for direct analysis of Hg by TDA-AAS and the second was digested for Hg determination by the ICP-MS. Results indicated that the two data sets were fully comparable (median; TDA-AAS, 475ngg -1 ; ICP-MS, 437ngg -1 ) and were not statistically different (Mann-Whitney test; p=0.44). The two techniques presented results with a good coefficient of correlation (r=0.94) despite different operative ranges and method limits. Both techniques satisfied internal performance requirements and the parameters for method validation resulting sensitive, precise and reliable. Finally, the use of the TDA-AAS can be considered instead of the ICP-MS in hair analysis in order to reduce sample manipulation with minor risk of contamination, less time consuming due to the absence of the digestion step and cheaper analyses. Copyright © 2016 Elsevier GmbH. All rights reserved.

Tungsten devices in analytical atomic spectrometry

NASA Astrophysics Data System (ADS)

Hou, Xiandeng; Jones, Bradley T.

2002-04-01

Tungsten devices have been employed in analytical atomic spectrometry for approximately 30 years. Most of these atomizers can be electrically heated up to 3000 °C at very high heating rates, with a simple power supply. Usually, a tungsten device is employed in one of two modes: as an electrothermal atomizer with which the sample vapor is probed directly, or as an electrothermal vaporizer, which produces a sample aerosol that is then carried to a separate atomizer for analysis. Tungsten devices may take various physical shapes: tubes, cups, boats, ribbons, wires, filaments, coils and loops. Most of these orientations have been applied to many analytical techniques, such as atomic absorption spectrometry, atomic emission spectrometry, atomic fluorescence spectrometry, laser excited atomic fluorescence spectrometry, metastable transfer emission spectroscopy, inductively coupled plasma optical emission spectrometry, inductively coupled plasma mass spectrometry and microwave plasma atomic spectrometry. The analytical figures of merit and the practical applications reported for these techniques are reviewed. Atomization mechanisms reported for tungsten atomizers are also briefly summarized. In addition, less common applications of tungsten devices are discussed, including analyte preconcentration by adsorption or electrodeposition and electrothermal separation of analytes prior to analysis. Tungsten atomization devices continue to provide simple, versatile alternatives for analytical atomic spectrometry.

A Very Much Faster and More Sensitive In Situ Stable Isotope Analysis Instrument

NASA Astrophysics Data System (ADS)

Coleman, M.; Christensen, L. E.; Kriesel, J. M.; Kelly, J. F.; Moran, J. J.; Vance, S.

2016-10-01

We are developing, Capillary Absorption Spectrometry (CAS) for H and O stable isotope analyses, giving > 4 orders of magnitude improved sensitivity, allowing analysis of 5 nano-moles of water and coupled to laser sampling to free water from hydrated minerals and ice.

Determination of Sodium, Potassium, Magnesium, and Calcium Minerals Level in Fresh and Boiled Broccoli and Cauliflower by Atomic Absorption Spectrometry

NASA Astrophysics Data System (ADS)

Nerdy

2018-01-01

Vegetables from the cabbage family vegetables consumed by many people, which is known healthful, by eaten raw, boiled, or cooked (stir fry or soup). Vegetables like broccoli and cauliflower contain vitamins, minerals, and fiber. This study aims to determine the decrease percentage of sodium, potassium, magnesium, and calcium minerals level caused by boiled broccoli and cauliflower by atomic absorption spectrometry. Boiled broccoli and cauliflower prepared by given boiled treatment in boiling water for 3 minutes. Fresh and boiled broccoli and cauliflower carried out dry destruction, followed by quantitative analysis of sodium, potassium, magnesium, and calcium minerals respectively at a wavelength of 589.0 nm; 766.5 nm; 285.2 nm; and 422.7 nm, using atomic absorption spectrometry methods. After the determination of the sodium, potassium, magnesium, and calcium minerals level followed by validation of analytical methods with accuracy, precision, linearity, range, limit of detection (LOD), and limit of quantitation (LOQ) parameters. Research results show a decrease in the sodium, potassium, magnesium, and calcium minerals level in boiled broccoli and cauliflower compared with fresh broccoli and cauliflower. Validation of analytical methods gives results that spectrometry methods used for determining sodium, potassium, magnesium, and calcium minerals level are valid. It concluded that the boiled gives the effect of decreasing the minerals level significantly in broccoli and cauliflower.

Mercury in Environmental and Biological Samples Using Online Combustion with Sequential Atomic Absorption and Fluorescence Measurements: A Direct Comparison of Two Fundamental Techniques in Spectrometry

ERIC Educational Resources Information Center

Cizdziel, James V.

2011-01-01

In this laboratory experiment, students quantitatively determine the concentration of an element (mercury) in an environmental or biological sample while comparing and contrasting the fundamental techniques of atomic absorption spectrometry (AAS) and atomic fluorescence spectrometry (AFS). A mercury analyzer based on sample combustion,…

EPA Method 3031 (SW-846): Acid Digestion of Oils for Metals Analysis by Atomic Absorption or ICP Spectrometry

EPA Pesticide Factsheets

Procedures are described for analysis of water samples and may be adapted for assessment of solid, particulate and liquid samples. The method uses real-time PCR assay for detecting Toxoplasma gondii DNA using gene-specific primers and probe.

40 CFR Appendix A to Subpart C of... - Alternative Testing Methods Approved for Analyses Under the Safe Drinking Water Act

Code of Federal Regulations, 2012 CFR

2012-07-01

... coupled plasma-atomic emission spectrometry (AVICP-AES) 200.5, Revision 4.2. 2 Arsenic Atomic Absorption... inductively coupled plasma-atomic emission spectrometry (AVICP-AES) 200.5, Revision 4.2. 2 Barium Inductively Coupled Plasma 3120 B Atomic Absorption; Direct 3111 D Atomic Absorption; Furnace 3113 B 3113 B-04 Axially...

40 CFR Appendix A to Subpart C of... - Alternative Testing Methods Approved for Analyses Under the Safe Drinking Water Act

Code of Federal Regulations, 2011 CFR

2011-07-01

... coupled plasma-atomic emission spectrometry (AVICP-AES) 200.5, Revision 4.2. 2 Arsenic Atomic Absorption... inductively coupled plasma-atomic emission spectrometry (AVICP-AES) 200.5, Revision 4.2. 2 Barium Inductively Coupled Plasma 3120 B Atomic Absorption; Direct 3111 D Atomic Absorption; Furnace 3113 B 3113 B-04 Axially...

Ultrasensitive determination of cadmium in seawater by hollow fiber supported liquid membrane extraction coupled with graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Peng, Jin-feng; Liu, Rui; Liu, Jing-fu; He, Bin; Hu, Xia-lin; Jiang, Gui-bin

2007-05-01

A new procedure, based on hollow fiber supported liquid membrane preconcentration coupled with graphite furnace atomic absorption spectrometry (GFAAS) detection, was developed for the determination of trace Cd in seawater samples. With 1-octanol that contained a mixture of dithizone (carrier) and oleic acid immobilized in the pores of the polypropylene hollow fiber as a liquid membrane, Cd was selectively extracted from water samples into 0.05 M HNO 3 that filled the lumen of the hollow fiber as a stripping solution. The main extraction related parameters were optimized, and the effects of salinity and some coexisting interferants were also evaluated. Under the optimum extraction conditions, an enrichment factor of 387 was obtained for a 100-mL sample solution. In combination with graphite furnace atomic absorption spectrometry, a very low detection limit (0.8 ng L - 1 ) and a relative standard deviation (2.5% at 50 ng L - 1 level) were achieved. Five seawater samples were analyzed by the proposed method without dilution, with detected Cd concentration in the range of 56.4-264.8 ng L - 1 and the relative spiked recoveries over 89%. For comparison, these samples were also analyzed by the Inductively Coupled Plasma Mass Spectrometry (ICP-MS) method after a 10-fold dilution for matrix effect elimination. Statistical analysis with a one-way ANOVA shows no significant differences (at 0.05 level) between the results obtained by the proposed and ICP-MS methods. Additionally, analysis of certified reference materials (GBW (E) 080040) shows good agreement with the certified value. These results indicate that this present method is very sensitive and reliable, and can effectively eliminate complex matrix interferences in seawater samples.

Concentration of Elements in Food: How Can It Reflect Impact of Environmental and Other Influencing Factors?

NASA Astrophysics Data System (ADS)

Vincevica-Gaile, Zane; Klavins, Maris

2013-12-01

Element content of food is variable and can be influenced by different factors. The aim of the present study was to discover the linkage between macro- and microelement concentrations in food produced in Latvia, and possible impacts of environmental factors. More than 300 fresh food samples such as eggs, cottage cheese, honey, root vegetables, apple juice, apple wine were collected in the time period from 2009 to 2011. Samples were mineralised or analysed directly by appropriate method of quantitative analysis: atomic absorption spectrometry, inductively coupled plasma mass spectrometry or total reflection X-ray fluorescence spectrometry. Statistical analysis of data revealed that food elemental content can be influenced by sitespecific factors such as geographical origin, seasonality, environmental pollution.

Evaluation of the memory effect on gold-coated silica adsorption tubes used for the analysis of gaseous mercury by cold vapor atomic absorption spectrometry.

PubMed

Rahman, Mohammad Mahmudur; Brown, Richard J C; Kim, Ki-Hyun; Yoon, Hye-On; Phan, Nhu-Thuc

2013-01-01

In an effort to reduce the experimental bias involved in the analysis of gaseous elemental mercury (Hg(o)), the blank response from gold-coated adsorption tubes has been investigated using cold vapor atomic absorption spectrometry (CVAAS). Our study has been compared with our recent investigation on memory effect in a cold vapour atomic fluorescence spectrometry (CVAFS). The pattern of blank responses was quantified after loading different amounts of mercury and after different time intervals of 1, 14, and 45 days. In case of the one day interval, the result of five to six instant blank heating cycles confirmed successful liberation of mercury following the second and third blank heating cycles. The results of 14 or 45 days generally suggest that liberation of excess mercury is affected by both the initial loading amount and the length of storage time prior to analysis. We have demonstrated a possibly effective way to reduce memory effects. Some similarities of these results with those from CVAFS experiment suggests that the blank response is caused by a combination of mercury absorbed within the bulk gold and micro- and nanoparticles liberated during heating and not from coabsorbing interfering gaseous species.

Evaluation of the Memory Effect on Gold-Coated Silica Adsorption Tubes Used for the Analysis of Gaseous Mercury by Cold Vapor Atomic Absorption Spectrometry

PubMed Central

Rahman, Mohammad Mahmudur; Brown, Richard J. C.; Yoon, Hye-On; Phan, Nhu-Thuc

2013-01-01

In an effort to reduce the experimental bias involved in the analysis of gaseous elemental mercury (Hgo), the blank response from gold-coated adsorption tubes has been investigated using cold vapor atomic absorption spectrometry (CVAAS). Our study has been compared with our recent investigation on memory effect in a cold vapour atomic fluorescence spectrometry (CVAFS). The pattern of blank responses was quantified after loading different amounts of mercury and after different time intervals of 1, 14, and 45 days. In case of the one day interval, the result of five to six instant blank heating cycles confirmed successful liberation of mercury following the second and third blank heating cycles. The results of 14 or 45 days generally suggest that liberation of excess mercury is affected by both the initial loading amount and the length of storage time prior to analysis. We have demonstrated a possibly effective way to reduce memory effects. Some similarities of these results with those from CVAFS experiment suggests that the blank response is caused by a combination of mercury absorbed within the bulk gold and micro- and nanoparticles liberated during heating and not from coabsorbing interfering gaseous species. PMID:23589708

Au36(SePh)24 nanomolecules: synthesis, optical spectroscopy and theoretical analysis.

PubMed

Rambukwella, Milan; Chang, Le; Ravishanker, Anish; Fortunelli, Alessandro; Stener, Mauro; Dass, Amala

2018-05-16

Here, we report the synthesis of selenophenol (HSePh) protected Au36(SePh)24 nanomolecules via a ligand-exchange reaction of 4-tert-butylbenzenethiol (HSPh-tBu) protected Au36(SPh-tBu)24 with selenophenol, and its spectroscopic and theoretical analysis. Matrix assisted laser desorption ionization (MALDI) mass spectrometry, electrospray ionization (ESI) mass spectrometry and optical characterization confirm that the composition of the as synthesized product is predominantly Au36(SePh)24 nanomolecules. Size exclusion chromatography (SEC) was employed to isolate the Au36(SePh)24 and temperature dependent optical absorption studies and theoretical analysis were performed. Theoretically, an Independent Component Maps of Oscillator Strength (ICM-OS) analysis of simulated spectra shows that the enhancement in absorption intensity in Au36(SePh)24 with respect to Au36(SPh)24 can be ascribed to the absence of interference and/or increased long-range coupling between interband metal core and ligand excitations. This work demonstrates and helps to understand the effect of Au-Se bridging on the properties of gold nanomolecules.

DETERMINATION OF TOTAL MERCURY IN FISH TISSUES USING PYROLYSIS ATOMIC ABSORPTION SPECTROMETRY WITH GOLD AMALGAMATION

EPA Science Inventory

A simple and rapid procedure for measuring total mercury in fish tissues is evaluated and
compared with conventional techniques. Using an automated instrument incorporating combustion, preconcentration by amalgamation with gold, and atomic absorption spectrometry (AAS), mill...

Use of High-Resolution Continuum Source Flame Atomic Absorption Spectrometry (HR-CS FAAS) for Sequential Multi-Element Determination of Metals in Seawater and Wastewater Samples

NASA Astrophysics Data System (ADS)

Peña-Vázquez, E.; Barciela-Alonso, M. C.; Pita-Calvo, C.; Domínguez-González, R.; Bermejo-Barrera, P.

2015-09-01

The objective of this work is to develop a method for the determination of metals in saline matrices using high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). Module SFS 6 for sample injection was used in the manual mode, and flame operating conditions were selected. The main absorption lines were used for all the elements, and the number of selected analytical pixels were 5 (CP±2) for Cd, Cu, Fe, Ni, Pb and Zn, and 3 pixels for Mn (CP±1). Samples were acidified (0.5% (v/v) nitric acid), and the standard addition method was used for the sequential determination of the analytes in diluted samples (1:2). The method showed good precision (RSD(%) < 4%, except for Pb (6.5%)) and good recoveries. Accuracy was checked after the analysis of an SPS-WW2 wastewater reference material diluted with synthetic seawater (dilution 1:2), showing a good agreement between certified and experimental results.

Determination of total mercury in environmental and biological samples by flow injection cold vapour atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Murphy, James; Jones, Phil; Hill, Steve J.

1996-12-01

A simple and accurate method has been developed for the determination of total mercury in environmental and biological samples. The method utilises an off-line microwave digestion stage followed by analysis using a flow injection system with detection by cold vapour atomic absorption spectrometry. The method has been validated using two certified reference materials (DORM-1 dogfish and MESS-2 estuarine sediment) and the results agreed well with the certified values. A detection limit of 0.2 ng g -1 Hg was obtained and no significant interference was observed. The method was finally applied to the determination of mercury in river sediments and canned tuna fish, and gave results in the range 0.1-3.0 mg kg -1.

Practical Problems in the Cement Industry Solved by Modern Research Techniques

ERIC Educational Resources Information Center

Daugherty, Kenneth E.; Robertson, Les D.

1972-01-01

Practical chemical problems in the cement industry are being solved by such techniques as infrared spectroscopy, gas chromatography-mass spectrometry, X-ray diffraction, atomic absorption and arc spectroscopy, thermally evolved gas analysis, Mossbauer spectroscopy, transmission and scanning electron microscopy. (CP)

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

NASA Astrophysics Data System (ADS)

Katskov, Dmitri A.; Sadagov, Yuri M.

2011-06-01

The methodology of simultaneous multi-element electrothermal atomic absorption spectrometry (ETAAS-Electrothermal Atomic Absorption Spectrometry) stipulates rigid requirements to the design and operation of the atomizer. It must provide high degree of atomization for the group of analytes, invariant respective to the vaporization kinetics and heating ramp residence time of atoms in the absorption volume and absence of memory effects from major sample components. For the low resolution spectrometer with a continuum radiation source the reduced compared to traditional ETAAS (Electrothermal Atomic Absorption Spectrometry) sensitivity should be, at least partially, compensated by creating high density of atomic vapor in the absorption pulse. The sought-for characteristics were obtained for the 18 mm in length and 2.5 mm in internal diameter longitudinally heated graphite tube atomizer furnished with 2-4.5 mg of ring shaped carbon fiber yarn collector. The collector located next to the sampling port provides large substrate area that helps to keep the sample and its residue in the central part of the tube after drying. The collector also provides a "platform" effect that delays the vaporization and stipulates vapor release into absorption volume having already stabilized gas temperature. Due to the shape of external surface of the tube, presence of collector and rapid (about 10 °C/ms) heating, an inverse temperature distribution along the tube is attained at the beginnings of the atomization and cleaning steps. The effect is employed for cleaning of the atomizer using the set of short maximum power heating pulses. Preparation, optimal maintenance of the atomizer and its compliance to the multi-element determination requirements are evaluated and discussed. The experimental setup provides direct simultaneous determination of large group of element within 3-4 order concentration range. Limits of detection are close to those for sequential single element 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.

Diamond nanowires for highly sensitive matrix-free mass spectrometry analysis of small molecules.

PubMed

Coffinier, Yannick; Szunerits, Sabine; Drobecq, Hervé; Melnyk, Oleg; Boukherroub, Rabah

2012-01-07

This paper reports on the use of boron-doped diamond nanowires (BDD NWs) as an inorganic substrate for matrix-free laser desorption/ionization mass spectrometry (LDI-MS) analysis of small molecules. The diamond nanowires are prepared by reactive ion etching (RIE) with oxygen plasma of highly boron-doped (the boron level is 10(19) B cm(-3)) or undoped nanocrystalline diamond substrates. The resulting diamond nanowires are coated with a thin silicon oxide layer that confers a superhydrophilic character to the surface. To minimize droplet spreading, the nanowires were chemically functionalized with octadecyltrichlorosilane (OTS) and then UV/ozone treated to reach a final water contact angle of 120°. The sub-bandgap absorption under UV laser irradiation and the heat confinement inside the nanowires allowed desorption/ionization, most likely via a thermal mechanism, and mass spectrometry analysis of small molecules. A detection limit of 200 zeptomole for verapamil was demonstrated.

Micro-sampling method based on high-resolution continuum source graphite furnace atomic absorption spectrometry for calcium determination in blood and mitochondrial suspensions.

PubMed

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

2017-08-01

A micro-sampling and straightforward method based on high resolution continuum source atomic absorption spectrometry (HR-CS AAS) was developed to determine extracellular and intracellular Ca in samples of interest in clinical and biomedical analysis. Solid sampling platforms were used to introduce the micro-samples into the graphite furnace atomizer. The secondary absorption line for Ca, located at 239.856nm, was selected to carry out the measurements. Experimental parameters such as pyrolysis and atomization temperatures and the amount of sample introduced for the measurements were optimized. Calibration was performed using aqueous standards and the approach to measure at the wings of the absorption lines was employed for the expansion of the linear response range. The limit of detection was of 0.02mgL -1 Ca (0.39ng Ca) and the upper limit of linear range was increased up to 8.0mgL -1 Ca (160ng Ca). The proposed method was used to determine Ca in mitochondrial suspensions and whole blood samples with successful results. Adequate recoveries (within 91-107%) were obtained in the tests performed for validation purposes. Copyright © 2017 Elsevier B.V. All rights reserved.

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

USGS Publications Warehouse

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 the remaining elements, Ba, Be, Ca, Cr, Mg, Mn, Sr, and Zn have roughly equivalent accuracy, precision, and detection limit by ICP and DCP. Cobalt and Ni were determined to be better analyzed by ICP, because of lower detection limits; B, Cu, Mo, and Si were determined to be better analyzed by DCP, because of relative freedom from interferences. The determination oral by DCP was far more sensitive, owing to the use of a more sensitive wavelength, compared with the ICP. However, there is a very serious potential interference from a strong Ca emission line near the 396.15 nanometer DCP wavelength. Thus, there is no clear choice between the plasma techniques tested, for the determination oral. The ICP and DCP detection limits are typically between 0.001 and 0.5 milligrams per liter in acid mine waters. For those metals best analyzed by ICP and/or DCP, but below these limits, GFAAS is the method of choice because of its relatively greater sensitivity and specificity. Six of the elements were not determined by DCP, ICP or Zeeman-corrected GFAAS, and are not discussed in this report. These elements are: Bi, Fe(11), Li, Sb, Se, and TI.

Emerging surface characterization techniques for carbon steel corrosion: a critical brief review.

PubMed

Dwivedi, D; Lepkova, K; Becker, T

2017-03-01

Carbon steel is a preferred construction material in many industrial and domestic applications, including oil and gas pipelines, where corrosion mitigation using film-forming corrosion inhibitor formulations is a widely accepted method. This review identifies surface analytical techniques that are considered suitable for analysis of thin films at metallic substrates, but are yet to be applied to analysis of carbon steel surfaces in corrosive media or treated with corrosion inhibitors. The reviewed methods include time of flight-secondary ion mass spectrometry, X-ray absorption spectroscopy methods, particle-induced X-ray emission, Rutherford backscatter spectroscopy, Auger electron spectroscopy, electron probe microanalysis, near-edge X-ray absorption fine structure spectroscopy, X-ray photoemission electron microscopy, low-energy electron diffraction, small-angle neutron scattering and neutron reflectometry, and conversion electron Moessbauer spectrometry. Advantages and limitations of the analytical methods in thin-film surface investigations are discussed. Technical parameters of nominated analytical methods are provided to assist in the selection of suitable methods for analysis of metallic substrates deposited with surface films. The challenges associated with the applications of the emerging analytical methods in corrosion science are also addressed.

Emerging surface characterization techniques for carbon steel corrosion: a critical brief review

NASA Astrophysics Data System (ADS)

Dwivedi, D.; Lepkova, K.; Becker, T.

2017-03-01

Carbon steel is a preferred construction material in many industrial and domestic applications, including oil and gas pipelines, where corrosion mitigation using film-forming corrosion inhibitor formulations is a widely accepted method. This review identifies surface analytical techniques that are considered suitable for analysis of thin films at metallic substrates, but are yet to be applied to analysis of carbon steel surfaces in corrosive media or treated with corrosion inhibitors. The reviewed methods include time of flight-secondary ion mass spectrometry, X-ray absorption spectroscopy methods, particle-induced X-ray emission, Rutherford backscatter spectroscopy, Auger electron spectroscopy, electron probe microanalysis, near-edge X-ray absorption fine structure spectroscopy, X-ray photoemission electron microscopy, low-energy electron diffraction, small-angle neutron scattering and neutron reflectometry, and conversion electron Moessbauer spectrometry. Advantages and limitations of the analytical methods in thin-film surface investigations are discussed. Technical parameters of nominated analytical methods are provided to assist in the selection of suitable methods for analysis of metallic substrates deposited with surface films. The challenges associated with the applications of the emerging analytical methods in corrosion science are also addressed.

Emerging surface characterization techniques for carbon steel corrosion: a critical brief review

PubMed Central

Dwivedi, D.; Becker, T.

2017-01-01

Carbon steel is a preferred construction material in many industrial and domestic applications, including oil and gas pipelines, where corrosion mitigation using film-forming corrosion inhibitor formulations is a widely accepted method. This review identifies surface analytical techniques that are considered suitable for analysis of thin films at metallic substrates, but are yet to be applied to analysis of carbon steel surfaces in corrosive media or treated with corrosion inhibitors. The reviewed methods include time of flight-secondary ion mass spectrometry, X-ray absorption spectroscopy methods, particle-induced X-ray emission, Rutherford backscatter spectroscopy, Auger electron spectroscopy, electron probe microanalysis, near-edge X-ray absorption fine structure spectroscopy, X-ray photoemission electron microscopy, low-energy electron diffraction, small-angle neutron scattering and neutron reflectometry, and conversion electron Moessbauer spectrometry. Advantages and limitations of the analytical methods in thin-film surface investigations are discussed. Technical parameters of nominated analytical methods are provided to assist in the selection of suitable methods for analysis of metallic substrates deposited with surface films. The challenges associated with the applications of the emerging analytical methods in corrosion science are also addressed. PMID:28413351

Absorption Mode FT-ICR Mass Spectrometry Imaging

DOE Office of Scientific and Technical Information (OSTI.GOV)

Smith, Donald F.; Kilgour, David P.; Konijnenburg, Marco

2013-12-03

Fourier transform ion cyclotron resonance mass spectrometry offers the highest mass resolving power for molecular imaging experiments. This high mass resolving power ensures that closely spaced peaks at the same nominal mass are resolved for proper image generation. Typically higher magnetic fields are used to increase mass resolving power. However, a gain in mass resolving power can also be realized by phase correction of the data for absorption mode display. In addition to mass resolving power, absorption mode offers higher mass accuracy and signal-to-noise ratio over the conventional magnitude mode. Here we present the first use of absorption mode formore » Fourier transform ion cyclotron resonance mass spectrometry imaging. The Autophaser algorithm is used to phase correct each spectrum (pixel) in the image and then these parameters are used by the Chameleon work-flow based data processing software to generate absorption mode ?Datacubes? for image and spectral viewing. Absorption mode reveals new mass and spatial features that are not resolved in magnitude mode and results in improved selected ion image contrast.« less

Determination of silver in irons and steels by atomic-absorption spectrometry with an induction furnace: Direct analysis of solid samples.

PubMed

Aziz-Alrahman, A M; Headridge, J B

1978-07-01

The silver contents of 17 irons and steels have been determined by dropping 0.5-20mg of millings or turnings of the metals into an induction furnace situated within an atomic-absorption spectrophotometer. The limit of detection was 0.005 mug/g and the relative standard deviations were 12% or better for silver contents of not less than 0.05 mug/g. Samples are added to the furnace at 4-5 min intervals.

Sample preparation for arsenic speciation analysis in baby food by generation of substituted arsines with atomic absorption spectrometry detection.

PubMed

Huber, Charles S; Vale, Maria Goreti R; Dessuy, Morgana B; Svoboda, Milan; Musil, Stanislav; Dědina, Jiři

2017-12-01

A slurry sampling procedure for arsenic speciation analysis in baby food by arsane generation, cryogenic trapping and detection with atomic absorption spectrometry is presented. Several procedures were tested for slurry preparation, including different reagents (HNO 3 , HCl and tetramethylammonium hydroxide - TMAH) and their concentrations, water bath heating and ultrasound-assisted agitation. The best results for inorganic arsenic (iAs) and dimethylarsinate (DMA) were reached when using 3molL -1 HCl under heating and ultrasound-assisted agitation. The developed method was applied for the analysis of five porridge powder and six baby meal samples. The trueness of the method was checked with a certified reference material (CRM) of total arsenic (tAs), iAs and DMA in rice (ERM-BC211). Arsenic recoveries (mass balance) for all samples and CRM were performed by the determination of the tAs by inductively coupled plasma mass spectrometry (ICP-MS) after microwave-assisted digestion and its comparison against the sum of the results from the speciation analysis. The relative limits of detection were 0.44, 0.24 and 0.16µgkg -1 for iAs, methylarsonate and DMA, respectively. The concentrations of the most toxic arsenic species (iAs) in the analyzed baby food samples ranged between 4.2 and 99µgkg -1 which were below the limits of 300, 200 and 100µgkg -1 set by the Brazilian, Chinese and European legislation, respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

Liquid-phase microextraction combined with graphite furnace atomic absorption spectrometry: A review.

PubMed

de la Calle, Inmaculada; Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos

2016-09-14

An overview of the combination of liquid-phase microextraction (LPME) techniques with graphite furnace atomic absorption spectrometry (GFAAS) is reported herein. The high sensitivity of GFAAS is significantly enhanced by its association with a variety of miniaturized solvent extraction approaches. LPME-GFAAS thus represents a powerful combination for determination of metals, metalloids and organometallic compounds at (ultra)trace level. Different LPME modes used with GFAAS are briefly described, and the experimental parameters that show an impact in those microextraction processes are discussed. Special attention is paid to those parameters affecting GFAAS analysis. Main issues found when coupling LPME and GFAAS, as well as those strategies reported in the literature to solve them, are summarized. Relevant applications published on the topic so far are included. Copyright © 2016 Elsevier B.V. All rights reserved.

In-situ pre-concentration through repeated sampling and pyrolysis for ultrasensitive determination of thallium in drinking water by electrothermal atomic absorption spectrometry.

PubMed

Liu, Liwei; Zheng, Huaili; Xu, Bincheng; Xiao, Lang; Chigan, Yong; Zhangluo, Yilan

2018-03-01

In this paper, a procedure for in-situ pre-concentration in graphite furnace by repeated sampling and pyrolysis is proposed for the determination of ultra-trace thallium in drinking water by graphite furnace atomic absorption spectrometry (GF-AAS). Without any other laborious enrichment processes that routinely result in analyte loss and contamination, thallium was directly concentrated in the graphite furnace automatically and subsequently subject to analysis. The effects of several key factors, such as the temperature for pyrolysis and atomization, the chemical modifier, and the repeated sampling times were investigated. Under the optimized conditions, a limit of detection of 0.01µgL -1 was obtained, which fulfilled thallium determination in drinking water by GB 5749-2006 regulated by China. Successful analysis of thallium in certified water samples and drinking water samples was demonstrated, with analytical results in good agreement with the certified values and those by inductively coupled plasma mass spectrometry (ICP-MS), respectively. Routine spike-recovery tests with randomly selected drinking water samples showed satisfactory results of 80-96%. The proposed method is simple and sensitive for screening of ultra-trace thallium in drinking water samples. Copyright © 2017. Published by Elsevier B.V.

Laser spectrometer for CO2 clumped isotope analysis

NASA Astrophysics Data System (ADS)

Prokhorov, Ivan; Kluge, Tobias; Janssen, Christof

2017-04-01

Carbon dioxide clumped isotope thermometry has proven to be a reliable method for biogeochemical and atmospheric research. We present a new laser spectroscopic instrument for doubly-substituted isotopologues analysis. In contrast to a conventional isotope ratio mass spectrometry (IRMS), tunable laser direct absorption spectroscopy (TLDAS) has the advantage of isotopologue-specific determination free of isobaric interferences. Tunable infrared laser based spectrometer for clumped isotope analysis is being developed in collaboration between Heidelberg University, Germany, and LERMA-IPSL, CNRS, France. The instrument employs two continuous intraband cascade lasers (ICL) tuned at 4439 and 4329 nm. The spectral windows covered by the lasers contain absorption lines of the six most abundant CO2 isotopologues, including the two doubly substituted species 16O13C18O and 16O13C17O, and all singly substituted isotopologues with 13C, 18O and 17O. A Herriott-type multi-pass cell provides two different absorption pathlengths to compensate the abundance difference between singly- and doubly-substituted isotopologues. We have reached the sub-permill precision required for clumped isotope measurements within the integration time of several seconds. The test version of the instrument demonstrates a performance comparable to state of the art IRMS. We highlight the following features of the instrument that are strong advantages compared to conventional mass spectrometry: measurement cycle in the minute range, simplified sample preparation routine, table-top layout with a potential for in-situ applications.

Determination of mercury in an assortment of dietary supplements using an inexpensive combustion atomic absorption spectrometry technique.

PubMed

Levine, Keith E; Levine, Michael A; Weber, Frank X; Hu, Ye; Perlmutter, Jason; Grohse, Peter M

2005-01-01

The concentrations of mercury in forty, commercially available dietary supplements, were determined using a new, inexpensive analysis technique. The method involves thermal decomposition, amalgamation, and detection of mercury by atomic absorption spectrometry with an analysis time of approximately six minutes per sample. The primary cost savings from this approach is that labor-intensive sample digestion is not required prior to analysis, further automating the analytical procedure. As a result, manufacturers and regulatory agencies concerned with monitoring lot-to-lot product quality may find this approach an attractive alternative to the more classical acid-decomposition, cold vapor atomic absorption methodology. Dietary supplement samples analyzed included astragalus, calcium, chromium picolinate, echinacea, ephedra, fish oil, ginger, ginkgo biloba, ginseng, goldenseal, guggul, senna, St John's wort, and yohimbe products. Quality control samples analyzed with the dietary supplements indicated a high level of method accuracy and precision. Ten replicate preparations of a standard reference material (NIST 1573a, tomato leaves) were analyzed, and the average mercury recovery was 109% (2.0% RSD). The method quantitation limit was 0.3 ng, which corresponded to 1.5 ng/g sample. The highest found mercury concentration (123 ng/g) was measured in a concentrated salmon oil sample. When taken as directed by an adult, this product would result in an approximate mercury ingestion of 7 mug per week.

Differential optical absorption spectrometer for measurement of tropospheric pollutants

NASA Astrophysics Data System (ADS)

Evangelisti, F.; Baroncelli, A.; Bonasoni, P.; Giovanelli, G.; Ravegnani, F.

1995-05-01

Our institute has recently developed a differential optical absorption spectrometry system called the gas analyzer spectrometer correlating optical absorption differences (GASCOAD), which features as a detector a linear image sensor that uses an artificial light source for long-path tropospheric-pollution monitoring. The GASCOAD, its method of eliminating interference from background sky light, and subsequent spectral analysis are reported and discussed. The spectrometer was used from 7 to 22 February 1993 in Milan, a heavily polluted metropolitan area, to measure the concentrations of SO2, NO2, O3, and HNO2 averaged over a 1.7-km horizontal light path. The findings are reported and briefly discussed.

Identification of carbohydrates by matrix-free material-enhanced laser desorption/ionisation mass spectrometry.

PubMed

Hashir, Muhammad Ahsan; Stecher, Guenther; Bakry, Rania; Kasemsook, Saowapak; Blassnig, Bernhard; Feuerstein, Isabel; Abel, Gudrun; Popp, Michael; Bobleter, Ortwin; Bonn, Guenther K

2007-01-01

Matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry (MALDI-TOF-MS) is a sensitive mass spectrometric technique which utilises acidic materials as matrices for laser energy absorption, desorption and ionisation of analytes. These matrix materials produce background signals particularly in the low-mass range and make the detection and identification of small molecules difficult and nearly impossible. To overcome this problem this paper introduces matrix-free material-enhanced laser desorption/ionisation mass spectrometry (mf-MELDI-MS) for the screening and analysis of small molecules such as carbohydrates. For this purpose, 4,4'-azo-dianiline was immobilised on silica gel enabling the absorption of laser energy sufficient for successful desorption and ionisation of low molecular weight compounds. The particle and pore sizes, the solvent system for suspension and the sample preparation procedures have been optimised. The newly synthesised MELDI material delivered excellent spectra with regard to signal-to-noise ratio and detection sensitivity. Finally, wheat straw degradation products and Salix alba L. plant extracts were analysed proving the high performance and excellent behaviour of the introduced material. Copyright (c) 2007 John Wiley & Sons, Ltd.

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

PubMed Central

2013-01-01

Background 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. Results 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 methods for 95% confidence interval. Conclusions High-resolution continuum source flame atomic absorption spectrometry can be successfully used for the rapid, multielemental determination of hazardous/priority hazardous metals in soil with similar analytical performances to those in inductively coupled plasma optical emission spectrometry. PMID:23452327

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.

PubMed

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 methods for 95% confidence interval. High-resolution continuum source flame atomic absorption spectrometry can be successfully used for the rapid, multielemental determination of hazardous/priority hazardous metals in soil with similar analytical performances to those in inductively coupled plasma optical emission spectrometry.

Determination of selenium in the environment and in biological material.

PubMed Central

Bem, E M

1981-01-01

This paper reviews the following problems, sampling, decomposition procedures and most important analytical methods used for selenium determination, e.g., neutron activation analysis, atomic absorption spectrometry, gas-liquid chromatography, spectrophotometry, fluorimetry, and x-ray fluorescence. This review covers the literature mainly from 1975 to 1977. PMID:7007035

The Moss Techniques for Air Pollution Study in Bulgaria

DOE Office of Scientific and Technical Information (OSTI.GOV)

Marinova, S.; Marinov, A.; Frontasyeva, M.

2010-01-21

The paper presents new results on atmospheric deposition of 41 elements in four areas of Bulgaria during the European moss survey in 2005. The results have been obtained by the moss biomonitoring technique. Ninety seven moss samples were analyzed by instrumental neutron activation analysis (ENAA) and atomic absorption spectrometry (AAS).

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

NASA Astrophysics Data System (ADS)

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.

Simultaneous determination of Cd and Fe in beans and soil of different regions of Brazil using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sampling.

PubMed

dos Santos, Lisia M G; Welz, Bernhard; Araujo, Rennan G O; Jacob, Silvana do C; Vale, Maria Goreti R; Martens, Andreas; Gonzaga Martens, Irland B; Becker-Ross, Helmut

2009-11-11

A fast routine screening method for the simultaneous determination of cadmium and iron in bean and soil samples is proposed, using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sampling. The primary absorption line at 228.802 nm has been used for the determination of cadmium, and an adjacent secondary line, at 228.726 nm, for iron. Fourteen bean samples and 10 soil samples from nine states all over Brazil have been analyzed. The limits of detection (3 sigma, n = 10) were 2.0 microg kg(-1) for Cd and 4.5 mg kg(-1) for Fe. The relative standard deviation ranged from 4 to 7% for Cd and from 5 to 28% for Fe, which is usually acceptable for a screening method. The accuracy of the method has been confirmed by the analysis of two certified reference materials; the results were in agreement with the certified values at a 95% confidence interval.

Determination of phospholipids in soybean lecithin samples via the phosphorus monoxide molecule by high-resolution continuum source graphite furnace molecular absorption spectrometry.

PubMed

Pires, Laís N; Brandão, Geovani C; Teixeira, Leonardo S G

2017-06-15

This paper presents a method for determining phospholipids in soybean lecithin samples by phosphorus determination using high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS) via molecular absorption of phosphorus monoxide. Samples were diluted in methyl isobutyl ketone. The best conditions were found to be 213.561nm with a pyrolysis temperature of 1300°C, a volatilization temperature of 2300°C and Mg as a chemical modifier. To increase the analytical sensitivity, measurement of the absorbance signal was obtained by summing molecular transition lines for PO surrounding 213nm: 213.561, 213.526, 213.617 and 213.637nm. The limit of detection was 2.35mgg -1 and the precision, evaluated as relative standard deviation (RSD), was 2.47% (n=10) for a sample containing 2.2% (w/v) phosphorus. The developed method was applied for the analysis of commercial samples of soybean lecithin. The determined concentrations of phospholipids in the samples varied between 38.1 and 45% (w/v). Copyright © 2017 Elsevier Ltd. All rights reserved.

Solid sampling determination of total fluorine in baby food samples by high-resolution continuum source graphite furnace molecular absorption spectrometry.

PubMed

Ozbek, Nil; Akman, Suleyman

2016-11-15

This study describes the applicability of solid sampling technique for the determination of fluorine in various baby foods via molecular absorption of calcium monofluoride generated in a graphite furnace of high-resolution continuum source atomic absorption spectrometry. Fluorine was determined at CaF wavelength, 606.440nm in a graphite tube applying a pyrolysis temperature of 1000°C and a molecule forming temperature of 2200°C. The limit of detection and characteristic mass of the method were 0.20ng and 0.17ng of fluorine, respectively. The fluorine concentrations determined in standard reference sample (bush branches and leaves) were in good agreement with the certified values. By applying the optimized parameters, the concentration of fluorine in various baby foods were determined. The fluorine concentrations were ranged from

Transmission ultrasonography. [time delay spectrometry for soft tissue transmission imaging

NASA Technical Reports Server (NTRS)

Heyser, R. C.; Le Croissette, D. H.

1973-01-01

Review of the results of the application of an advanced signal-processing technique, called time delay spectrometry, in obtaining soft tissue transmission images by transmission ultrasonography, both in vivo and in vitro. The presented results include amplitude ultrasound pictures and phase ultrasound pictures obtained by this technique. While amplitude ultrasonographs of tissue are closely analogous to X-ray pictures in that differential absorption is imaged, phase ultrasonographs represent an entirely new source of information based on differential time of propagation. Thus, a new source of information is made available for detailed analysis.

Multicomutation flow system for manganese speciation by solid phase extraction and flame atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Tobiasz, Anna; Sołtys, Monika; Kurys, Ewa; Domagała, Karolina; Dudek-Adamska, Danuta; Walas, Stanisław

2017-08-01

In the paper an application of solid phase extraction technique for speciation analysis of manganese in water samples with the use of flame atomic absorption spectrometry is presented. Two types of sorbents, activated silica gel and Dowex 1 × 4, were used respectively for simultaneously Mn2 + and MnO42 - retention and preconcentration. The whole procedure was realized in multicomutation flow system. Different conditions like: type and concentration of eluent, sample pH and loading time were tested during the study. Under appropriate conditions, it was possible to obtained enrichment factors of 20 and 16 for Mn(II) and Mn(VII), respectively. Precision of the procedure was close to 4% (measured as relative standard deviation), whereas the detection limit (3σ) was 1.4 μg·L- 1 for Mn(II) and 4.8 μg·L- 1 for Mn(VII).

Validation of a hydride generation atomic absorption spectrometry methodology for determination of mercury in fish designed for application in the Brazilian national residue control plan.

PubMed

Damin, Isabel C F; Santo, Maria A E; Hennigen, Rosmari; Vargas, Denise M

2013-01-01

In the present study, a method for the determination of mercury (Hg) in fish was validated according to ISO/IEC 17025, INMETRO (Brazil), and more recent European recommendations (Commission Decision 2007/333/EC and 2002/657/EC) for implementation in the Brazilian Residue Control Plan (NRCP) in routine applications. The parameters evaluated in the validation were investigated in detail. The results obtained for limit of detection and quantification were respectively, 2.36 and 7.88 μg kg(-1) of Hg. While the recovery varies between 90-96%. The coefficient of variation was of 4.06-8.94% for the repeatability. Furthermore, a comparison using an external proficiency testing scheme was realized. The results of method validated for the determination of the mercury in fish by Hydride generation atomic absorption spectrometry were considered suitable for implementation in routine analysis.

Increasing the throughput and productivity of Caco-2 cell permeability assays using liquid chromatography-mass spectrometry: application to resveratrol absorption and metabolism.

PubMed

Li, Yongmei; Shin, Young Geun; Yu, Chongwoo; Kosmeder, Jerome W; Hirschelman, Wendy H; Pezzuto, John M; van Breemen, Richard B

2003-12-01

The Caco-2 cell monolayer permeability assay has become a standard model of human intestinal absorption and transport. This paper reviews recent progress in increasing the throughput of Caco-2 cell monolayer assays and in expanding the scope of this assay to include modeling intestinal drug metabolism. The state-of-the-art in Caco-2 cell monolayer permeability assays combines multi-well plates fitted with semi-permeable inserts on which Caco-2 cells have been cultured with liquid chromatography-mass spectrometry (LC-MS) or LC-tandem mass spectrometry (LC-MS-MS) for the quantitative analysis of test compounds and the identification of their intestinal metabolites. After reviewing the progress in increasing the throughput of Caco-2 cell monolayer assays for both modeling human intestinal permeability or transport and the metabolism of xenobiotic compounds, we demonstrate the application of LC-MS and LC-MS-MS to the measurement of resveratrol permeability and metabolism in the Caco-2 model. trans-Resveratrol (trans-3,5,4'-trihydroxystilbene) is a polyphenolic compound occurring in grapes, peanuts and other food sources, that is under investigation as a cancer chemoprevention agent. The apparent permeability coefficient for apical (AP) to basolateral (BL) movement of resveratrol was 2.0 x 10(-5)cm/sec. Resveratrol was not a substrate for P-glycoprotein or the multi-drug resistance associated proteins (MRP). No phase I metabolites were observed, but the phase II conjugates resveratrol-3-glucuronide and resveratrol-3-sulfate was identified based on LC-MS and LC-MS-MS analysis and comparison with synthetic standards. Although these data indicate that resveratrol diffuses rapidly across the intestinal epithelium, extensive phase II metabolism during absorption might reduce resveratrol bioavailability.

Translational value of liquid chromatography coupled with tandem mass spectrometry-based quantitative proteomics for in vitro-in vivo extrapolation of drug metabolism and transport and considerations in selecting appropriate techniques.

PubMed

Al Feteisi, Hajar; Achour, Brahim; Rostami-Hodjegan, Amin; Barber, Jill

2015-01-01

Drug-metabolizing enzymes and transporters play an important role in drug absorption, distribution, metabolism and excretion and, consequently, they influence drug efficacy and toxicity. Quantification of drug-metabolizing enzymes and transporters in various tissues is therefore essential for comprehensive elucidation of drug absorption, distribution, metabolism and excretion. Recent advances in liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) have improved the quantification of pharmacologically relevant proteins. This report presents an overview of mass spectrometry-based methods currently used for the quantification of drug-metabolizing enzymes and drug transporters, mainly focusing on applications and cost associated with various quantitative strategies based on stable isotope-labeled standards (absolute quantification peptide standards, quantification concatemers, protein standards for absolute quantification) and label-free analysis. In mass spectrometry, there is no simple relationship between signal intensity and analyte concentration. Proteomic strategies are therefore complex and several factors need to be considered when selecting the most appropriate method for an intended application, including the number of proteins and samples. Quantitative strategies require appropriate mass spectrometry platforms, yet choice is often limited by the availability of appropriate instrumentation. Quantitative proteomics research requires specialist practical skills and there is a pressing need to dedicate more effort and investment to training personnel in this area. Large-scale multicenter collaborations are also needed to standardize quantitative strategies in order to improve physiologically based pharmacokinetic models.

Determination of mineral, trace element, and pesticide levels in honey samples originating from different regions of Malaysia compared to manuka honey.

PubMed

Moniruzzaman, Mohammed; Chowdhury, Muhammed Alamgir Zaman; Rahman, Mohammad Abdur; Sulaiman, Siti Amrah; Gan, Siew Hua

2014-01-01

The present study was undertaken to determine the content of six minerals, five trace elements, and ten pesticide residues in honeys originating from different regions of Malaysia. Calcium (Ca), magnesium (Mg), iron (Fe), and zinc (Zn) were analyzed by flame atomic absorption spectrometry (FAAS), while sodium (Na) and potassium (K) were analyzed by flame emission spectrometry (FAES). Trace elements such as arsenic (As), lead (Pb), cadmium (Cd), copper (Cu), and cobalt (Co) were analyzed by graphite furnace atomic absorption spectrometry (GFAAS) following the microwave digestion of honey. High mineral contents were observed in the investigated honeys with K, Na, Ca, and Fe being the most abundant elements (mean concentrations of 1349.34, 236.80, 183.67, and 162.31 mg/kg, resp.). The concentrations of the trace elements were within the recommended limits, indicating that the honeys were of good quality. Principal component analysis reveals good discrimination between the different honey samples. The pesticide analysis for the presence of organophosphorus and carbamates was performed by high performance liquid chromatography (HPLC). No pesticide residues were detected in any of the investigated honey samples, indicating that the honeys were pure. Our study reveals that Malaysian honeys are rich sources of minerals with trace elements present within permissible limits and that they are free from pesticide contamination.

Determination of Mineral, Trace Element, and Pesticide Levels in Honey Samples Originating from Different Regions of Malaysia Compared to Manuka Honey

PubMed Central

Moniruzzaman, Mohammed; Chowdhury, Muhammed Alamgir Zaman; Rahman, Mohammad Abdur; Sulaiman, Siti Amrah; Gan, Siew Hua

2014-01-01

The present study was undertaken to determine the content of six minerals, five trace elements, and ten pesticide residues in honeys originating from different regions of Malaysia. Calcium (Ca), magnesium (Mg), iron (Fe), and zinc (Zn) were analyzed by flame atomic absorption spectrometry (FAAS), while sodium (Na) and potassium (K) were analyzed by flame emission spectrometry (FAES). Trace elements such as arsenic (As), lead (Pb), cadmium (Cd), copper (Cu), and cobalt (Co) were analyzed by graphite furnace atomic absorption spectrometry (GFAAS) following the microwave digestion of honey. High mineral contents were observed in the investigated honeys with K, Na, Ca, and Fe being the most abundant elements (mean concentrations of 1349.34, 236.80, 183.67, and 162.31 mg/kg, resp.). The concentrations of the trace elements were within the recommended limits, indicating that the honeys were of good quality. Principal component analysis reveals good discrimination between the different honey samples. The pesticide analysis for the presence of organophosphorus and carbamates was performed by high performance liquid chromatography (HPLC). No pesticide residues were detected in any of the investigated honey samples, indicating that the honeys were pure. Our study reveals that Malaysian honeys are rich sources of minerals with trace elements present within permissible limits and that they are free from pesticide contamination. PMID:24982869

Spectral Quantitation Of Hydroponic Nutrients

NASA Technical Reports Server (NTRS)

Schlager, Kenneth J.; Kahle, Scott J.; Wilson, Monica A.; Boehlen, Michelle

1996-01-01

Instrument continuously monitors hydroponic solution by use of absorption and emission spectrometry to determine concentrations of principal nutrients, including nitrate, iron, potassium, calcium, magnesium, phosphorus, sodium, and others. Does not depend on extraction and processing of samples, use of such surrograte parameters as pH or electrical conductivity for control, or addition of analytical reagents to solution. Solution not chemically altered by analysis and can be returned to hydroponic process stream after analysis.

An improved methodology of asymmetric flow field flow fractionation hyphenated with inductively coupled mass spectrometry for the determination of size distribution of gold nanoparticles in dietary supplements.

PubMed

Mudalige, Thilak K; Qu, Haiou; Linder, Sean W

2015-11-13

Engineered nanoparticles are available in large numbers of commercial products claiming various health benefits. Nanoparticle absorption, distribution, metabolism, excretion, and toxicity in a biological system are dependent on particle size, thus the determination of size and size distribution is essential for full characterization. Number based average size and size distribution is a major parameter for full characterization of the nanoparticle. In the case of polydispersed samples, large numbers of particles are needed to obtain accurate size distribution data. Herein, we report a rapid methodology, demonstrating improved nanoparticle recovery and excellent size resolution, for the characterization of gold nanoparticles in dietary supplements using asymmetric flow field flow fractionation coupled with visible absorption spectrometry and inductively coupled plasma mass spectrometry. A linear relationship between gold nanoparticle size and retention times was observed, and used for characterization of unknown samples. The particle size results from unknown samples were compared to results from traditional size analysis by transmission electron microscopy, and found to have less than a 5% deviation in size for unknown product over the size range from 7 to 30 nm. Published by Elsevier B.V.

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.

PubMed

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.

On-line ionic liquid-based preconcentration system coupled to flame atomic absorption spectrometry for trace cadmium determination in plastic food packaging materials.

PubMed

Martinis, Estefanía M; Olsina, Roberto A; Altamirano, Jorgelina C; Wuilloud, Rodolfo G

2009-05-15

A novel on-line preconcentration method based on liquid-liquid (L-L) extraction with room temperature ionic liquids (RTILs) coupled to flame atomic absorption spectrometry (FAAS) was developed for cadmium determination in plastic food packaging materials. The methodology is based on the complexation of Cd with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) reagent after sample digestion followed by extraction of the complex with the RTIL 1-butyl-3-methylimidazolium hexafluorophosphate ([C(4)mim][PF(6)]). The mixture was loaded into a flow injection analysis (FIA) manifold and the RTIL rich-phase was retained in a microcolumn filled with silica gel. The RTIL rich-phase was then eluted directly into FAAS. A enhancement factor of 35 was achieved with 20 mL of sample. The limit of detection (LOD), obtained as IUPAC recommendation, was 6 ng g(-1) and the relative standard deviation (R.S.D.) for 10 replicates at 10 microg L(-1) Cd concentration level was 3.9%, calculated at the peak heights. The calibration graph was linear and a correlation coefficient of 0.9998 was achieved. The accuracy of the method was evaluated by both a recovery study and comparison of results with direct determination by electrothermal atomic absorption spectrometry (ETAAS). The method was successfully applied for Cd determination in plastic food packaging materials and Cd concentrations found were in the range of 0.04-10.4 microg g(-1).

Diode laser differential absorption spectrometry for measurements of some parameters of condensed media.

PubMed

Liger, V V; Bolshov, M A; Kuritsyn, Yu A; Krivtsun, V M; Zybin, A V; Niemax, K

2007-04-01

A method of diode laser differential absorption spectrometry (DLDAS) is proposed. The method is based on the detection of absorption spectra variations caused by the changes of a parameter of a condensed media (temperature, composition of the components of a mixture, pH, etc.). Some simple theoretical background of the proposed technique is presented. The potentialities of the method are demonstrated in the experiments on remote contactless measurement of the temperature of aqueous solutions and measurement of the deviations of the composition of a mixture of dyes from the equilibrium state.

SPECIATION ANALYSIS OF ARSENIC IN BIOLOGICAL MATRICES BY AUTOMATED HYDRIDE GENERATION-CRYOTRAPPING-ATOMIC ABSORPTION SPECTROMETRY WITH MULTIPLE MICROFLAME QUARTZ TUBE ATOMIZER (MULTIATOMIZER)

EPA Science Inventory

Abstract Analyses of arsenic (As) species in tissues and body fluids of individuals chronically exposed to inorganic arsenic (iAs) provide essential information about the exposure level and pattern of iAs metabolism. We have previously described an oxidation state-specifi...

Experimental analysis of energy absorption behaviour of Al-tube filled with pumice lightweight concrete under axial loading condition

NASA Astrophysics Data System (ADS)

Rajak, D. K.; Deshpande, P. G.; Kumaraswamidhas, L. A.

2017-08-01

This Paper aimed at experimental investigation of compressive behaviour of square tube filled with pumice lightweight concrete (PLC). Square section of 20×20×30 mm is investigated, which is the backbone structure. The compression deformation result shows the better folding mechanism, displacement value, and energy absorption. PLC concrete filled with aluminium thin-wall tubes has been revealed superior energy absorption capacity (EAC) under low strain rate at room temperature. Superior EAC resulted as a result of mutual deformation benefit between aluminium section and PLC is also analysed. PLC was characterised by Fourier Transform Infrared (FTIR) and Field Emission Scanning Electron Microscopy (FESEM), and Energy Dispersive X-ray Spectrometry (EDX) analysis for better understanding of material behaviour. Individual and comparative load bearing graphs is logged for better prospective of analysing. Novel approach aimed at validation of porous lightweight concrete for better lightweight EA filler material.

Tunable lasers and their application in analytical chemistry

NASA Technical Reports Server (NTRS)

Steinfeld, J. I.

1975-01-01

The impact that laser techniques might have in chemical analysis is examined. Absorption, scattering, and heterodyne detection is considered. Particular emphasis is placed on the advantages of using frequency-tunable sources, and dye solution lasers are regarded as the outstanding example of this type of laser. Types of spectroscopy that can be carried out with lasers are discussed along with the ultimate sensitivity or minimum detectable concentration of molecules that can be achieved with each method. Analytical applications include laser microprobe analysis, remote sensing and instrumental methods such as laser-Raman spectroscopy, atomic absorption/fluorescence spectrometry, fluorescence assay techniques, optoacoustic spectroscopy, and polarization measurements. The application of lasers to spectroscopic methods of analysis would seem to be a rewarding field both for research in analytical chemistry and for investments in instrument manufacturing.

[Application of atomic absorption spectrometry in the engine knock detection].

PubMed

Chen, Li-Dan

2013-02-01

Because existing human experience diagnosis method and apparatus for auxiliary diagnosis method are difficult to diagnose quickly engine knock. Atomic absorption spectrometry was used to detect the automobile engine knock in in innovative way. After having determined Fe, Al, Cu, Cr and Pb content in the 35 groups of Audi A6 engine oil whose travel course is 2 000 -70 000 kilometers and whose sampling interval is 2 000 kilometers by atomic absorption spectrometry, the database of primary metal content in the same automobile engine at different mileage was established. The research shows that the main metal content fluctuates within a certain range. In practical engineering applications, after the determination of engine oil main metal content and comparison with its database value, it can not only help to diagnose the type and location of engine knock without the disintegration and reduce vehicle maintenance costs and improve the accuracy of engine knock fault diagnosis.

Quality-assurance data for routine water analysis in the National Water-Quality Laboratory of the US Geological Survey for water year 1988

USGS Publications Warehouse

Lucey, K.J.

1989-01-01

The US Geological Survey maintains a quality assurance program based on the analysis of reference samples for its National Water Quality Laboratory located in Denver, Colorado. Reference samples containing selected inorganic, nutrient, and precipitation (low-level concentration) constituents are prepared at the Survey 's Water Quality Services Unit in Ocala, Florida, disguised as routine samples, and sent daily or weekly, as appropriate, to the laboratory through other Survey offices. The results are stored permanently in the National Water Data Storage and Retrieval System (WATSTORE), the Survey 's database for all water data. These data are analyzed statistically for precision and bias. An overall evaluation of the inorganic major ion and trace metal constituent data for water year 1988 indicated a lack of precision in the National Water Quality Laboratory for the determination of 8 out of 58 constituents: calcium (inductively coupled plasma emission spectrometry), fluoride, iron (atomic absorption spectrometry), iron (total recoverable), magnesium (atomic absorption spectrometry), manganese (total recoverable), potassium, and sodium (inductively coupled plasma emission spectrometry). The results for 31 constituents had positive or negative bias during water year 1988. A lack of precision was indicated in the determination of three of the six nutrient constituents: nitrate plus nitrite nitrogen as nitrogen, nitrite nitrogen as nitrogen, and orthophosphate as phosphorus. A biased condition was indicated in the determination of ammonia nitrogen as nitrogen, ammonia plus organic nitrogen as nitrogen, and nitrate plus nitrite nitrogen as nitrogen. There was acceptable precision in the determination of all 10 constituents contained in precipitation samples. Results for ammonia nitrogen as nitrogen, sodium, and fluoride indicated a biased condition. (Author 's abstract)

High purity polyimide analysis by solid sampling graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Santos, Rafael F.; Carvalho, Gabriel S.; Duarte, Fabio A.; Bolzan, Rodrigo C.; Flores, Erico M. M.

2017-03-01

In this work, Cr, Cu, Mn, Na and Ni were determined in high purity polyimides (99.5%) by solid sampling graphite furnace atomic absorption spectrometry (SS-GFAAS) using Zeeman effect background correction system with variable magnetic field, making possible the simultaneous measurement at high or low sensitivity. The following analytical parameters were evaluated: pyrolysis and atomization temperatures, feasibility of calibration with aqueous solution, linear calibration range, sample mass range and the use of chemical modifier. Calibration with aqueous standard solutions was feasible for all analytes. No under or overestimated results were observed and up to 10 mg sample could be introduced on the platform for the determination of Cr, Cu, Mn, Na and Ni. The relative standard deviation ranged from 3 to 20%. The limits of detection (LODs) achieved using the high sensitivity mode were as low as 7.0, 2.5, 1.7, 17 and 0.12 ng g- 1 for Cr, Cu, Mn, Na and Ni, respectively. No addition of chemical modifier was necessary, except for Mn determination where Pd was required. The accuracy was evaluated by analyte spike and by comparison of the results with those obtained by inductively coupled plasma optical emission spectrometry and inductively coupled plasma mass spectrometry after microwave-assisted digestion in a single reaction chamber system and also by neutron activation analysis. No difference among the results obtained by SS-GFAAS and those obtained by alternative analytical methods using independent techniques. SS-GFAAS method showed some advantages, such as the determination of metallic contaminants in high purity polyimides with practically no sample preparation, very low LODs, calibration with aqueous standards and determination in a wide range of concentration.

Lithogeochemistry of mineralized and altered rock samples from the northern Talkeetna Mountains, south-central Alaska

USGS Publications Warehouse

Light, Thomas D.; Schmidt, Jeanine M.

2011-01-01

Mineralized and altered rock samples collected from the northern Talkeetna Mountains, Alaska, were analyzed by two different inductively coupled plasma atomic-emission spectrometry (ICP-AES) methods for as many as 44 elements; by fire assay and either direct-coupled plasma (DCP) or atomic absorption spectrophotometry (AAS) for gold (Au); by cold vapor atomic absorption (CVAA) for mercury (Hg); and by irradiated neutron activation analysis (INAA) for tungsten (W). The analytical results showed that some samples contain high values of multiple elements and may be potential indicators of hydrothermal mineralization in the area.

Electrolytic preconcentration in instrumental analysis.

PubMed

Sioda, R E; Batley, G E; Lund, W; Wang, J; Leach, S C

1986-05-01

The use of electrolytic deposition as a separation and preconcentration step in trace metal analysis is reviewed. Both the principles and applications of the technique are dealt with in some detail. Electrolytic preconcentration can be combined with a variety of instrumental techniques. Special attention is given to stripping voltammetry, potentiometric stripping analysis, different combinations with atomic-absorption spectrometry, and the use of flow-through porous electrodes. It is pointed out that the electrolytic preconcentration technique deserves more extensive use as well as fundamental investigation.

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

PubMed

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.

Direct determination of Pb in raw milk by graphite furnace atomic absorption spectrometry (GF AAS) with electrothermal atomization sampling from slurries.

PubMed

de Oliveira, Tatiane Milão; Augusto Peres, Jayme; Lurdes Felsner, Maria; Cristiane Justi, Karin

2017-08-15

Milk is an important food in the human diet due to its physico-chemical composition; therefore, it is necessary to monitor contamination by toxic metals such as Pb. Milk sample slurries were prepared using Triton X-100 and nitric acid for direct analysis of Pb using graphite furnace atomic absorption spectrometry - GF AAS. After dilution of the slurries, 10.00µl were directly introduced into the pyrolytic graphite tube without use of a chemical modifier, which acts as an advantage considering this type of matrix. The limits of detection and quantification were 0.64 and 2.14µgl -1 , respectively. The figures of merit studied showed that the proposed methodology without pretreatment of the raw milk sample and using external standard calibration is suitable. The methodology was applied in milk samples from the Guarapuava region, in Paraná State (Brazil) and Pb concentrations ranged from 2.12 to 37.36µgl -1 . Copyright © 2017 Elsevier Ltd. All rights reserved.

Monitoring spacecraft atmosphere contaminants by laser absorption spectroscopy

NASA Technical Reports Server (NTRS)

Steinfeld, J. I.

1976-01-01

Laser-based spectrophotometric methods which have been proposed for the detection of trace concentrations of gaseous contaminants include Raman backscattering (LIDAR) and passive radiometry (LOPAIR). Remote sensing techniques using laser spectrometry are presented and in particular a simple long-path laser absorption method (LOLA), which is capable of resolving complex mixtures of closely related trace contaminants at ppm levels is discussed. A number of species were selected for study which are representative of those most likely to accumulate in closed environments, such as submarines or long-duration manned space flights. Computer programs were developed which will permit a real-time analysis of the monitored atmosphere. Estimates of the dynamic range of this monitoring technique for various system configurations, and comparison with other methods of analysis, are given.

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

PubMed

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.

[Determination of metal elements in Achyranthis bidentatae radix from various habitats].

PubMed

Tu, Wan-Qian; Zhang, Liu-Ji

2011-12-01

To establish an atomic absorption spectrometry method for determination of the contents of metal elements in Achyranthis Bidentatae Radix and analyze 21 batches of samples from different areas. Fe, Mn, Ca, Mg, K, Zn and Cu were detected by atomic absorption spectrometry with hydrogen flame detector, Pb, As and Cd were detected by graphite furnace atomic absorption, Hg was detected by cold atomic absorption. The heavy metal contents met the requirement of Chinese Pharmacopoeia. The contents of K, Mg, Cu and Mn in the samples of geo-authentic areas were higher,while the contents of Fe, Zn, Hg and Pb in the samples of non-authentic areas were higher. This method is sample, accurate, repeatable and could be used to evaluate the quality of Achyranthis Bidentatae Radix.

A comparison of laser ablation-inductively coupled plasma-mass spectrometry and high-resolution continuum source graphite furnace molecular absorption spectrometry for the direct determination of bromine in polymers

NASA Astrophysics Data System (ADS)

de Gois, Jefferson S.; Van Malderen, Stijn J. M.; Cadorim, Heloisa R.; Welz, Bernhard; Vanhaecke, Frank

2017-06-01

This work describes the development and comparison of two methods for the direct determination of Br in polymer samples via solid sampling, one using laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) and the other using high-resolution continuum source graphite furnace molecular absorption spectrometry with direct solid sample analysis (HR-CS SS-GF MAS). The methods were optimized and their accuracy was evaluated by comparing the results obtained for 6 polymeric certified reference materials (CRMs) with the corresponding certified values. For Br determination with LA-ICP-MS, the 79Br+ signal could be monitored interference-free. For Br determination via HR-CS SS-GF MAS, the CaBr molecule was monitored at 625.315 nm with integration of the central pixel ± 1. Bromine quantification by LA-ICP-MS was performed via external calibration against a single CRM while using the 12C+ signal as an internal standard. With HR-CS SS-GF MAS, Br quantification could be accomplished using external calibration against aqueous standard solutions. Except for one LA-ICP-MS result, the concentrations obtained with both techniques were in agreement with the certified values within the experimental uncertainty as evidenced using a t-test (95% confidence level). The limit of quantification was determined to be 100 μg g- 1 Br for LA-ICP-MS and 10 μg g- 1 Br for HR-CS SS-GF MAS.

Cobalt internal standard for Ni to assist the simultaneous determination of Mo and Ni in plant materials by high-resolution continuum source graphite furnace atomic absorption spectrometry employing direct solid sample analysis.

PubMed

de Babos, Diego Victor; Bechlin, Marcos André; Barros, Ariane Isis; Ferreira, Edilene Cristina; Gomes Neto, José Anchieta; de Oliveira, Silvana Ruella

2016-05-15

A new method is proposed for the simultaneous determination of Mo and Ni in plant materials by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GFAAS), employing direct solid sample analysis (DSS) and internal standardization (IS). Cobalt was used as internal standard to minimize matrix effects during Ni determinations, enabling the use of aqueous standards for calibration. Correlation coefficients for the calibration curves were typically better than 0.9937. The performance of the method was checked by analysis of six plant certified reference materials, and the results for Mo and Ni were in agreement with the certified values (95% confidence level, t-test). Analysis was made of different types of plant materials used as renewable sources of energy, including sugarcane leaves, banana tree fiber, soybean straw, coffee pods, orange bagasse, peanut hulls, and sugarcane bagasse. The concentrations found for Mo and Ni ranged from 0.08 to 0.63 ng mg(-1) and from 0.41 to 6.92 ng mg(-1), respectively. Precision (RSD) varied from 2.1% to 11% for Mo and from 3.7% to 10% for Ni. Limits of quantification of 0.055 and 0.074 ng were obtained for Mo and Ni, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

Bile acids: analysis in biological fluids and tissues

PubMed Central

Griffiths, William J.; Sjövall, Jan

2010-01-01

The formation of bile acids/bile alcohols is of major importance for the maintenance of cholesterol homeostasis. Besides their functions in lipid absorption, bile acids/bile alcohols are regulatory molecules for a number of metabolic processes. Their effects are structure-dependent, and numerous metabolic conversions result in a complex mixture of biologically active and inactive forms. Advanced methods are required to characterize and quantify individual bile acids in these mixtures. A combination of such analyses with analyses of the proteome will be required for a better understanding of mechanisms of action and nature of endogenous ligands. Mass spectrometry is the basic detection technique for effluents from chromatographic columns. Capillary liquid chromatography-mass spectrometry with electrospray ionization provides the highest sensitivity in metabolome analysis. Classical gas chromatography-mass spectrometry is less sensitive but offers extensive structure-dependent fragmentation increasing the specificity in analyses of isobaric isomers of unconjugated bile acids. Depending on the nature of the bile acid/bile alcohol mixture and the range of concentration of individuals, different sample preparation sequences, from simple extractions to group separations and derivatizations, are applicable. We review the methods currently available for the analysis of bile acids in biological fluids and tissues, with emphasis on the combination of liquid and gas phase chromatography with mass spectrometry. PMID:20008121

Direct sampling graphite furnace atomic absorption spectrometry - feasibility of Na and K determination in desalted crude oil

NASA Astrophysics Data System (ADS)

Seeger, Tassia S.; Machado, Eduarda Q.; Flores, Erico M. M.; Mello, Paola A.; Duarte, Fabio A.

2018-03-01

In this study, Na and K were determined in desalted crude oil by direct sampling graphite furnace atomic absorption spectrometry (DS-GF AAS), with the use of a Zeeman-effect background correction system with variable magnetic field. The analysis was performed in low and high sensitivity conditions. Sodium determination was performed in two low-sensitivity conditions: 1) main absorption line (589.0 nm), gas stop flow during the atomization step and 3-field dynamic mode (0.6-0.8 T); and 2) secondary absorption line (330.3 nm), gas stop flow during the atomization and 2-field mode (0.8 T). In K determination, some parameters, such as high-sensitivity mode, main absorption line (766.5 nm), gas stop flow during the atomization and 2-field mode (0.8 T), were used. Suitability of chemical modifiers, such as Pd and W-Ir was also evaluated. The heating program for Na and K was based on the pyrolysis and atomization curves. Calibration was performed by aqueous standards. Accuracy was evaluated by the analysis of Green Petroleum Coke (SRM NIST 2718) and Trace Elements in Fuel Oil (SRM NIST 1634c). Recovery tests were also performed and results were compared with those obtained by GF AAS after crude oil digestion by microwave-assisted digestion. The characteristic mass of Na was 17.1 pg and 0.46 ng in conditions 1 and 2, respectively, while the one of K was 1.4 pg. Limits of detection and quantification by DS-GF AAS were 30 and 40 ng g-1 for Na and 3.2 and 4.2 ng g-1 for K, respectively. Sodium and K were determined in three crude oil samples with API density ranging from 20.9 to 28.0. Sodium and K concentration ranged from 1.5 to 73 μg g-1 and from 23 to 522 ng g-1, respectively.

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

PubMed

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.

Optimisation of flame parameters for simultaneous multi-element atomic absorption spectrometric determination of trace elements in rocks

USGS Publications Warehouse

Kane, J.S.

1988-01-01

A study is described that identifies the optimum operating conditions for the accurate determination of Co, Cu, Mn, Ni, Pb, Zn, Ag, Bi and Cd using simultaneous multi-element atomic absorption spectrometry. Accuracy was measured in terms of the percentage recoveries of the analytes based on certified values in nine standard reference materials. In addition to identifying optimum operating conditions for accurate analysis, conditions resulting in serious matrix interferences and the magnitude of the interferences were determined. The listed elements can be measured with acceptable accuracy in a lean to stoicheiometric flame at measurement heights ???5-10 mm above the burner.

Macro elemental analysis of food samples by nuclear analytical technique

NASA Astrophysics Data System (ADS)

Syahfitri, W. Y. N.; Kurniawati, S.; Adventini, N.; Damastuti, E.; Lestiani, D. D.

2017-06-01

Energy-dispersive X-ray fluorescence (EDXRF) spectrometry is a non-destructive, rapid, multi elemental, accurate, and environment friendly analysis compared with other detection methods. Thus, EDXRF spectrometry is applicable for food inspection. The macro elements calcium and potassium constitute important nutrients required by the human body for optimal physiological functions. Therefore, the determination of Ca and K content in various foods needs to be done. The aim of this work is to demonstrate the applicability of EDXRF for food analysis. The analytical performance of non-destructive EDXRF was compared with other analytical techniques; neutron activation analysis and atomic absorption spectrometry. Comparison of methods performed as cross checking results of the analysis and to overcome the limitations of the three methods. Analysis results showed that Ca found in food using EDXRF and AAS were not significantly different with p-value 0.9687, whereas p-value of K between EDXRF and NAA is 0.6575. The correlation between those results was also examined. The Pearson correlations for Ca and K were 0.9871 and 0.9558, respectively. Method validation using SRM NIST 1548a Typical Diet was also applied. The results showed good agreement between methods; therefore EDXRF method can be used as an alternative method for the determination of Ca and K in food samples.

Multi-element fingerprinting as a tool in origin authentication of four east China marine species.

PubMed

Guo, Lipan; Gong, Like; Yu, Yanlei; Zhang, Hong

2013-12-01

The contents of 25 elements in 4 types of commercial marine species from the East China Sea were determined by inductively coupled plasma mass spectrometry and atomic absorption spectrometry. The elemental composition was used to differentiate marine species according to geographical origin by multivariate statistical analysis. The results showed that principal component analysis could distinguish samples from different areas and reveal the elements which played the most important role in origin diversity. The established models by partial least squares discriminant analysis (PLS-DA) and by probabilistic neural network (PNN) can both precisely predict the origin of the marine species. Further study indicated that PLS-DA and PNN were efficacious in regional discrimination. The models from these 2 statistical methods, with an accuracy of 97.92% and 100%, respectively, could both distinguish samples from different areas without the need for species differentiation. © 2013 Institute of Food Technologists®

Application of several physical techniques in the total analysis of a canine urinary calculus.

PubMed

Rodgers, A L; Mezzabotta, M; Mulder, K J; Nassimbeni, L R

1981-06-01

A single calculus from the bladder of a Beagle bitch has been analyzed by a multiple technique approach employing x-ray diffraction, infrared spectroscopy, scanning electron microscopy, x-ray fluorescence spectrometry, atomic absorption spectrophotometry and density gradient fractionation. The qualitative and quantitative data obtained showed excellent agreement, lending confidence to such an approach for the evaluation and understanding of stone disease.

Mass Spectrometry Imaging proves differential absorption profiles of well-characterised permeability markers along the crypt-villus axis.

PubMed

Nilsson, Anna; Peric, Alexandra; Strimfors, Marie; Goodwin, Richard J A; Hayes, Martin A; Andrén, Per E; Hilgendorf, Constanze

2017-07-25

Knowledge about the region-specific absorption profiles from the gastrointestinal tract of orally administered drugs is a critical factor guiding dosage form selection in drug development. We have used a novel approach to study three well-characterized permeability and absorption marker drugs in the intestine. Propranolol and metoprolol (highly permeable compounds) and atenolol (low-moderate permeability compound) were orally co-administered to rats. The site of drug absorption was revealed by high spatial resolution matrix-assisted laser desorption ionization mass spectrometry imaging (MALDI-MSI) and complemented by quantitative measurement of drug concentration in tissue homogenates. MALDI-MSI identified endogenous molecular markers that illustrated the villi structures and confirmed the different absorption sites assigned to histological landmarks for the three drugs. Propranolol and metoprolol showed a rapid absorption and shorter transit distance in contrast to atenolol, which was absorbed more slowly from more distal sites. This study provides novel insights into site specific absorption for each of the compounds along the crypt-villus axis, as well as confirming a proximal-distal absorption gradient along the intestine. The combined analytical approach allowed the quantification and spatial resolution of drug distribution in the intestine and provided experimental evidence for the suggested absorption behaviour of low and highly permeable compounds.

QA/QC Guidance for Sampling and Analysis of Sediments, Water, and Tissues for Dredged Material Evaluations: Chemical Evaluations

DTIC Science & Technology

1995-04-01

J. Biochem. Physiol. 37:911-917. Bloom, N.S., E.A. Crecelius, and S . Berman . 1983. Determination of mercury in seawater at sub-nanogram per liter...procedure for determination of trace metal in seawater by atomic absorption spectrometry with electrothermal atomization. Anal. Chern. Acta 98:47-55...Nakashima, S ., R.E. Sturgeon, S.N. Willie, and S.S. Berman . 1988. Acid digestion of marine sample for trace element analysis using microwave heating

Determination of trace amounts of cobalt in blood

DOE Office of Scientific and Technical Information (OSTI.GOV)

Godlewska, B.; Hulanicki, A.; Abou-Shakra, F.R.

1994-11-01

The analysis of cobalt in whole blood and blood fractions has been carried out using three different analytical techniques namely, electrothermal atomic absorption spectrometry, inductively coupled plasma mass spectrometry and cathodic stripping voltammetry. This study showed that inductively coupled plasma mass spectrometry was the better equipped technique for conducting such analyses due to its low detection limits and wide linear dynamic range. The results ranged between 0.7 - 2.62 {mu}g/l for plasma, 1.02 - 2.31 {mu}g/l for serum, and 0.66 - 1.28 {mu}g/l for whole blood. The introduction of different forms of cobalt to Wistar rats resulted in a differingmore » distribution of the element between serum and whole blood. This observation suggests that there are at least two modes of Co uptake and transport depending on the administered or taken chemical form.« less

Imaging-based molecular barcoding with pixelated dielectric metasurfaces

NASA Astrophysics Data System (ADS)

Tittl, Andreas; Leitis, Aleksandrs; Liu, Mingkai; Yesilkoy, Filiz; Choi, Duk-Yong; Neshev, Dragomir N.; Kivshar, Yuri S.; Altug, Hatice

2018-06-01

Metasurfaces provide opportunities for wavefront control, flat optics, and subwavelength light focusing. We developed an imaging-based nanophotonic method for detecting mid-infrared molecular fingerprints and implemented it for the chemical identification and compositional analysis of surface-bound analytes. Our technique features a two-dimensional pixelated dielectric metasurface with a range of ultrasharp resonances, each tuned to a discrete frequency; this enables molecular absorption signatures to be read out at multiple spectral points, and the resulting information is then translated into a barcode-like spatial absorption map for imaging. The signatures of biological, polymer, and pesticide molecules can be detected with high sensitivity, covering applications such as biosensing and environmental monitoring. Our chemically specific technique can resolve absorption fingerprints without the need for spectrometry, frequency scanning, or moving mechanical parts, thereby paving the way toward sensitive and versatile miniaturized mid-infrared spectroscopy devices.

Oral heroin in opioid-dependent patients: pharmacokinetic comparison of immediate and extended release tablets

PubMed Central

Perger, Ludwig; Rentsch, Katharina M.; Kullak-Ublick, Gerd A.; Verotta, Davide; Fattinger, Karin

2009-01-01

In diacetylmorphine prescription programs for heavily dependent addicts, diacetylmorphine is usually administered intravenously, but this may not be possible due to venosclerosis or when heroin abuse had occurred via non-intravenous routes. Since up to 25% of patients administer diacetylmorphine orally, we characterised morphine absorption after single oral doses of immediate and extended release diacetylmorphine in 8 opioid addicts. Plasma concentrations were determined by liquid chromatography-mass spectrometry. Non-compartmental methods and deconvolution were applied for data analysis. Mean (±SD) immediate and extended release doses were 719 ± 297 mg and 956 ± 404 mg, with high absolute morphine bioavailabilities of 56% to 61%, respectively. Immediate release diacetylmorphine caused rapid morphine absorption, peaking at 10 to 15 min. Morphine absorption was considerably slower and more sustained for extended release diacetylmorphine, with only ~30% of maximal immediate release absorption being reached after 10 min and maintained for 3 to 4 h, with no relevant food interaction. The relative extended to immediate release bioavailability was calculated to be 86% by non-compartmental analysis and 93% by deconvolution analysis. Thus, immediate and extended release diacetylmorphine produce the intended morphine exposures. Both are suitable for substitution treatments. Similar doses can be applied if used in combination or sequentially. PMID:19084595

Speciation of Mn(II), Mn(VII) and total manganese in water and food samples by coprecipitation-atomic absorption spectrometry combination.

PubMed

Citak, Demirhan; Tuzen, Mustafa; Soylak, Mustafa

2010-01-15

A speciation procedure based on the coprecipitation of manganese(II) with zirconium(IV) hydroxide has been developed for the investigation of levels of manganese species. The determination of manganese levels was performed by flame atomic absorption spectrometry (FAAS). Total manganese was determined after the reduction of Mn(VII) to Mn(II) by ascorbic acid. The analytical parameters including pH, amount of zirconium(IV), sample volume, etc., were investigated for the quantitative recoveries of manganese(II). The effects of matrix ions were also examined. The recoveries for manganese(II) were in the range of 95-98%. Preconcentration factor was calculated as 50. The detection limit for the analyte ions based on 3 sigma (n=21) was 0.75 microg L(-1) for Mn(II). The relative standard deviation was found to be lower than 7%. The validation of the presented procedure was performed by analysis of certified reference material having different matrices, NIST SRM 1515 (Apple Leaves) and NIST SRM 1568a (Rice Flour). The procedure was successfully applied to natural waters and food samples.

Quantification of 2D elemental distribution maps of intermediate-thick biological sections by low energy synchrotron μ-X-ray fluorescence spectrometry

NASA Astrophysics Data System (ADS)

Kump, P.; Vogel-Mikuš, K.

2018-05-01

Two fundamental-parameter (FP) based models for quantification of 2D elemental distribution maps of intermediate-thick biological samples by synchrotron low energy μ-X-ray fluorescence spectrometry (SR-μ-XRF) are presented and applied to the elemental analysis in experiments with monochromatic focused photon beam excitation at two low energy X-ray fluorescence beamlines—TwinMic, Elettra Sincrotrone Trieste, Italy, and ID21, ESRF, Grenoble, France. The models assume intermediate-thick biological samples composed of measured elements, the sources of the measurable spectral lines, and by the residual matrix, which affects the measured intensities through absorption. In the first model a fixed residual matrix of the sample is assumed, while in the second model the residual matrix is obtained by the iteration refinement of elemental concentrations and an adjusted residual matrix. The absorption of the incident focused beam in the biological sample at each scanned pixel position, determined from the output of a photodiode or a CCD camera, is applied as a control in the iteration procedure of quantification.

[Determination of iodine and its species in plant samples using ion chromatography-inductively coupled plasma mass spectrometry].

PubMed

Lin, Li; Chen, Guang; Chen, Yuhong

2011-07-01

A method was established for the determination of iodine and its species in plant samples using ion chromatography-inductively coupled plasma mass spectrometry (IC-ICP/ MS). Alkaline extraction and IC-ICP/MS were applied as the sample pre-treatment method and the detection technique respectively, for iodate and iodide determination. Moreover, high-temperature pyrolysis absorption was adopted as the pre-treatment method for total iodine analysis, which finally converted all the iodine species into iodide and measured the iodide by IC-ICP/MS. The recoveries of iodine for alkaline extraction and high-temperature pyrolysis absorption were 89.6%-97.5% and 95.2%-111.2%, respectively. The results were satisfactory. The detection limit of iodine was 0.010 mg/kg. The iodine and its speciation contents in several kinds of plant samples such as seaweeds, kelp, cabbage, tea leaf and spinach were investigated. It was shown that the iodine in seaweeds mainly existed as organic iodine; while the ones in kelp, cabbage, tea leaf and spinach mainly existed as inorganic iodine.

Mercury(II) and methyl mercury determinations in water and fish samples by using solid phase extraction and cold vapour atomic absorption spectrometry combination.

PubMed

Tuzen, Mustafa; Karaman, Isa; Citak, Demirhan; Soylak, Mustafa

2009-07-01

A method has been developed for mercury(II) and methyl mercury speciation on Staphylococcus aureus loaded Dowex Optipore V-493 micro-column in the presented work, by using cold vapour atomic absorption spectrometry. Selective and sequential elution with 0.1 molL(-1) HCl for methyl mercury and 2 molL(-1) HCl for mercury(II) were performed at the pH range of 2-6. Optimal analytical conditions including pH, amounts of biosorbent, sample volumes were investigated. The detection limits of the analytes were 2.5 ngL(-1) for Hg(II) and 1.7 ngL(-1) for methyl mercury. The capacity of biosorbent for mercury(II) and methyl mercury was 6.5 and 5.4 mgg(-1), respectively. The validation of the presented procedure is performed by the analysis of standard reference material. The speciation procedure established was successfully applied to the speciation of mercury(II) and methyl mercury in natural water and microwave digested fish samples.

Vapor-Phase Infrared Absorptivity Coefficient of HN1

DTIC Science & Technology

2013-08-01

the boil-off of a bulk liquid nitrogen tank, across an alumina Soxhlet thimble in a glass holder filled with the analyte. A vapor–liquid...with mass spectrometry (MS) yielded the results shown in Table 3. Table 3. Results from Analysis of HN1 Sample Used for Determination of...2 yields (3) Equation 3 can then be solved at each frequency using a least-squares approach. This was

LabVIEW interface with Tango control system for a multi-technique X-ray spectrometry IAEA beamline end-station at Elettra Sincrotrone Trieste

NASA Astrophysics Data System (ADS)

Wrobel, P. M.; Bogovac, M.; Sghaier, H.; Leani, J. J.; Migliori, A.; Padilla-Alvarez, R.; Czyzycki, M.; Osan, J.; Kaiser, R. B.; Karydas, A. G.

2016-10-01

A new synchrotron beamline end-station for multipurpose X-ray spectrometry applications has been recently commissioned and it is currently accessible by end-users at the XRF beamline of Elettra Sincrotrone Trieste. The end-station consists of an ultra-high vacuum chamber that includes as main instrument a seven-axis motorized manipulator for sample and detectors positioning, different kinds of X-ray detectors and optical cameras. The beamline end-station allows performing measurements in different X-ray spectrometry techniques such as Microscopic X-Ray Fluorescence analysis (μXRF), Total Reflection X-Ray Fluorescence analysis (TXRF), Grazing Incidence/Exit X-Ray Fluorescence analysis (GI-XRF/GE-XRF), X-Ray Reflectometry (XRR), and X-Ray Absorption Spectroscopy (XAS). A LabVIEW Graphical User Interface (GUI) bound with Tango control system consisted of many custom made software modules is utilized as a user-friendly tool for control of the entire end-station hardware components. The present work describes this advanced Tango and LabVIEW software platform that utilizes in an optimal synergistic manner the merits and functionality of these well-established programming and equipment control tools.

40 CFR Appendix A to Subpart C of... - Alternative Testing Methods Approved for Analyses Under the Safe Drinking Water Act

Code of Federal Regulations, 2010 CFR

2010-07-01

... Absorption D 3697-07 Atomic Absorption; Furnace 3113 B Axially viewed inductively coupled plasma-atomic... C Hydride Atomic Absorption 3114 B D 2972-08 B Axially viewed inductively coupled plasma-atomic emission spectrometry (AVICP-AES) 200.5, Revision 4.2. Barium Inductively Coupled Plasma 3120 B Atomic...

Analysis of beryllium and depleted uranium: An overview of detection methods in aerosols and soils

DOE Office of Scientific and Technical Information (OSTI.GOV)

Camins, I.; Shinn, J.H.

We conducted a survey of commercially available methods for analysis of beryllium and depleted uranium in aerosols and soils to find a reliable, cost-effective, and sufficiently precise method for researchers involved in environmental testing at the Yuma Proving Ground, Yuma, Arizona. Criteria used for evaluation include cost, method of analysis, specificity, sensitivity, reproducibility, applicability, and commercial availability. We found that atomic absorption spectrometry with graphite furnace meets these criteria for testing samples for beryllium. We found that this method can also be used to test samples for depleted uranium. However, atomic absorption with graphite furnace is not as sensitive amore » measurement method for depleted uranium as it is for beryllium, so we recommend that quality control of depleted uranium analysis be maintained by testing 10 of every 1000 samples by neutron activation analysis. We also evaluated 45 companies and institutions that provide analyses of beryllium and depleted uranium. 5 refs., 1 tab.« less

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

PubMed

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.

Naphtyl- and pyrenyl-flavylium dyads: Synthesis, DFT and optical properties

NASA Astrophysics Data System (ADS)

Aguilar-Castillo, Bethsy Adriana; Sánchez-Bojorge, Nora Aydee; Chávez-Flores, David; Camacho-Dávila, Alejandro A.; Pasillas-Ornelas, Eddie; Rodríguez-Valdez, Luz-María; Zaragoza-Galán, Gerardo

2018-03-01

A one-step preparation of flavylium salts containing naphtyl and pyrenyl moieties is described hereafter. Flavylium salts were successfully characterized by 1H NMR spectroscopy and ESI-MS spectrometry. Theoretical calculations were carried out by means of Density Functional Theory in order to simulate flavylium cation electronic transitions. Molecular simulation of -naphtyl derivatives displayed a coplanar conformation between naphthalene and benzopyrylium moieties. In contrast, DFT analysis exhibited a non-coplanar arrangement of pyrene and benzopyrylium units. These former statements in coherence with the absorption experiments where the naphtyl-flavylium dyads shows a red-shifted maximum absorption band with respect to pyrene dyads, led us to conclude that these bathochromic effects are associated with a more planar conformation.

Method of trivalent chromium concentration determination by atomic spectrometry

DOEpatents

Reheulishvili, Aleksandre N [Tbilisi, 0183, GE; Tsibakhashvili, Neli Ya [Tbilisi, 0101, GE

2006-12-12

A method is disclosed for determining the concentration of trivalent chromium Cr(III) in a sample. The addition of perchloric acid has been found to increase the atomic chromium spectrometric signal due to Cr(III), while leaving the signal due to hexavalent chromium Cr(VI) unchanged. This enables determination of the Cr(III) concentration without pre-concentration or pre-separation from chromium of other valences. The Cr(III) concentration may be measured using atomic absorption spectrometry, atomic emission spectrometry or atomic fluorescence spectrometry.

40 CFR 1065.1010 - Reference materials.

Code of Federal Regulations, 2010 CFR

2010-07-01

... § 1065.1010—Institute of Petroleum Materials Document No. and name Part 1065 reference IP-470... atomic absorption spectrometry 1065.705 IP-500, Determination of the phosphorus content of residual fuels by ultra-violet spectrometry 1065.705 IP-501, Determination of aluminum, silicon, vanadium, nickel...

Paleodiet characterisation of an Etrurian population of Pontecagnano (Italy) by Isotope Ratio Mass Spectrometry (IRMS) and Atomic Absorption Spectrometry (AAS)(#).

PubMed

Scarabino, Carla; Lubritto, Carmine; Proto, Antonio; Rubino, Mauro; Fiengo, Gilda; Marzaioli, Fabio; Passariello, Isabella; Busiello, Gaetano; Fortunato, Antonietta; Alfano, Davide; Sabbarese, Carlo; Rogalla, Detlef; De Cesare, Nicola; d'Onofrio, Antonio; Terrasi, Filippo

2006-06-01

Human bones recovered from the archaeological site of Pontecagnano (Salerno, Italy) have been studied to reconstruct the diet of an Etrurian population. Two different areas were investigated, named Library and Sant' Antonio, with a total of 44 tombs containing human skeletal remains, ranging in age from the 8th to the 3rd century B.C. This time span was confirmed by 14C dating obtained using Accelerator Mass Spectrometry (AMS) on one bone sample from each site. Atomic Absorption Spectrometry (AAS) was used to extract information about the concentration of Sr, Zn, Ca elements in the bone inorganic fraction, whilst stable isotope ratio measurements (IRMS) were carried out on bone collagen to obtain the delta13C and delta15N. A reliable technique has been used to extract and separate the inorganic and organic fractions of the bone remains. Both IRMS and AAS results suggest a mixed diet including C3 plant food and herbivore animals, consistent with archaeological indications.

Phytosterol glycosides reduce cholesterol absorption in humans

PubMed Central

Lin, Xiaobo; Ma, Lina; Racette, Susan B.; Anderson Spearie, Catherine L.; Ostlund, Richard E.

2009-01-01

Dietary phytosterols inhibit intestinal cholesterol absorption and regulate whole body cholesterol excretion and balance. However, they are biochemically heterogeneous and a portion is glycosylated in some foods with unknown effects on biological activity. We tested the hypothesis that phytosterol glycosides reduce cholesterol absorption in humans. Phytosterol glycosides were extracted and purified from soy lecithin in a novel two-step process. Cholesterol absorption was measured in a series of three single-meal tests given at intervals of 2 wk to each of 11 healthy subjects. In a randomized crossover design, participants received ∼300 mg of added phytosterols in the form of phytosterol glycosides or phytosterol esters, or placebo in a test breakfast also containing 30 mg cholesterol-d7. Cholesterol absorption was estimated by mass spectrometry of plasma cholesterol-d7 enrichment 4–5 days after each test. Compared with the placebo test, phytosterol glycosides reduced cholesterol absorption by 37.6 ± 4.8% (P < 0.0001) and phytosterol esters 30.6 ± 3.9% (P = 0.0001). These results suggest that natural phytosterol glycosides purified from lecithin are bioactive in humans and should be included in methods of phytosterol analysis and tables of food phytosterol content. PMID:19246636

Application of thermospray flame furnace atomic absorption spectrometry for investigation of silver nanoparticles.

PubMed

Sirirat, Natnicha; Tetbuntad, Kornrawee; Siripinyanond, Atitaya

2017-03-01

Thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) was applied to investigate the time-dependent absorption peak profile of various forms of silver. The thermospray flame furnace was set up with a 10-cm-long nickel tube with six holes, each 2.0 mm in diameter, to allow the flame to enter, and this nickel tube acted as a furnace. A sample of 300 μL was introduced into this furnace by use of water as a carrier at a flow rate of 0.5 mL min -1 through the ceramic capillary (0.5-mm inner diameter and 2.0-mm outer diameter), which was inserted into the front hole of the nickel tube. The system was applied to examine atomization behaviors of silver nanoparticles (AgNPs) with particle sizes ranging from 10 to 100 nm. The atomization rate of AgNPs was faster than that of the dissolved silver ion. With increased amount of silver, the decay time observed from the time-dependent absorption peak profile was shortened in the case of dissolved silver ion, but it was increased in the case of AgNPs. With the particle size ranging from 10 to 100 nm, the detection sensitivity was indirectly proportional to the particle size, suggesting that TS-FF-AAS may offer insights into the particle size of AgNPs provided that the concentration of the silver is known. To obtain quantitative information on AgNPs, acid dissolution of the particles was performed before TS-FF-AAS analysis, and recoveries of 80-110% were obtained.

Determination and Uncertainty Analysis of Inorganic Arsenic in Husked Rice by Solid Phase Extraction and Atomic Absorption Spectrometry with Hydride Generation.

PubMed

Saxena, Sushil Kumar; Karipalli, Agnes Raju; Krishnan, Anoop A; Rangasamy, Rajesh; Malekadi, Praveen; Singh, Dhirendra P; Vasu, Vimesh; Singh, Vijay K

2017-05-01

This study enables the selective determination of inorganic arsenic (iAs) with a low detection limit using an economical instrument [atomic absorption spectrometer with hydride generation (HG)] to meet the regulatory requirements as per European Commission (EC) and Codex guidelines. Dry rice samples (0.5 g) were diluted using 0.1 M HNO3-3% H2O2 and heated in a water bath (90 ± 2°C) for 60 min. Through this process, all the iAs is solubilized and oxidized to arsenate [As(V)]. The centrifuged extract was loaded onto a preconditioned and equilibrated strong anion-exchange SPE column (silica-based Strata SAX 500 mg/6 mL), followed by selective and sequential elution of As(V), enabling the selective quantification of iAs using atomic absorption spectrometry with HG. In-house validation showed a mean recovery of 94% and an LOQ of 0.025 mg/kg. The repeatability (HorRatr) and reproducibility (HorRatR) values were <2, meeting the performance criteria mandated by the EC. The combined standard measurement uncertainty by this method was less than the maximum standard measurement uncertainty; thus, the method can be considered for official control purposes. The method was applied for the determination of iAs in husked rice samples and has potential applications in other food commodities.

[Recent Development of Atomic Spectrometry in China].

PubMed

Xiao, Yuan-fang; Wang, Xiao-hua; Hang, Wei

2015-09-01

As an important part of modern analytical techniques, atomic spectrometry occupies a decisive status in the whole analytical field. The development of atomic spectrometry also reflects the continuous reform and innovation of analytical techniques. In the past fifteen years, atomic spectrometry has experienced rapid development and been applied widely in many fields in China. This review has witnessed its development and remarkable achievements. It contains several directions of atomic spectrometry, including atomic emission spectrometry (AES), atomic absorption spectrometry (AAS), atomic fluorescence spectrometry (AFS), X-ray fluorescence spectrometry (XRF), and atomic mass spectrometry (AMS). Emphasis is put on the innovation of the detection methods and their applications in related fields, including environmental samples, biological samples, food and beverage, and geological materials, etc. There is also a brief introduction to the hyphenated techniques utilized in atomic spectrometry. Finally, the prospects of atomic spectrometry in China have been forecasted.

Environmental assessment of a watertube boiler firing a coal-water slurry. Volume 2. Data supplement. Final report, January 1984-March 1985

DOE Office of Scientific and Technical Information (OSTI.GOV)

DeRosier, R.; Waterland, L.R.

1986-02-01

This report is a compendium of detailed test sampling and analysis data obtained in field tests of a watertube industrial boiler burning a coal/water slurry (CWS). Test data reported include preliminary stack test data, boiler operating data, and complete flue-gas emission results. Flue-gas emission measurements included continuous monitoring for criteria pollutants; onsite gas chromatography (GC) for volatile hydrocarbons (Cl-C6); Methods 5/8 sampling for particulate, SO/sub 2/, and SO/sub 3/ emissions; source assessment sampling system (SASS) for total organics in two boiling point ranges (100 to 300 C and > 300 C), organic compound category information using infrared spectrometry (IR), liquidmore » column (LC) chromatography separation, and low-resolution mass spectrometry (LRMS), specific quantitation of the semivolatile organic priority pollutants using gas chromatography/mass spectrometry (GC/MS), and trace-element emissions using spark-source mass spectrometry (SSMS) and atomic absorption spectroscopy (AAS); N/sub 2/O emissions by gas chromatography/electron-capture detector (GC/ECD); and biological assay testing of SASS and ash-stream samples.« less

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

PubMed

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.

Nuclear Fuel Assay through analysis of Uranium L-shell by Hybrid L-edge/XRF Densitometer using a Surrogate Material

NASA Astrophysics Data System (ADS)

Park, Seunghoon; Joung, Sungyeop; Park, Jerry AB(; ), AC(; )

2018-01-01

Assay of L-series of nuclear material solution is useful for determination of amount of nuclear materials and ratio of minor actinide in the materials. The hybrid system of energy dispersive X-ray absorption edge spectrometry, i.e. L-edge densitometry, and X-ray fluorescence spectrometry is one of the analysis methods. The hybrid L-edge/XRF densitometer can be a promising candidate for a portable and compact equipment due to advantage of using low energy X-ray beams without heavy shielding systems and liquid nitrogen cooling compared to hybrid K-edge/XRF densitometer. A prototype of the equipment was evaluated for feasibility of the nuclear material assay using a surrogate material (lead) to avoid radiation effects from nuclear materials. The uncertainty of L-edge and XRF characteristics of the sample material and volume effects was discussed in the article.

MALDI (matrix assisted laser desorption ionization) Imaging Mass Spectrometry (IMS) of skin: Aspects of sample preparation.

PubMed

de Macedo, Cristiana Santos; Anderson, David M; Schey, Kevin L

2017-11-01

MALDI (matrix assisted laser desorption ionization) Imaging Mass Spectrometry (IMS) allows molecular analysis of biological materials making possible the identification and localization of molecules in tissues, and has been applied to address many questions on skin pathophysiology, as well as on studies about drug absorption and metabolism. Sample preparation for MALDI IMS is the most important part of the workflow, comprising specimen collection and preservation, tissue embedding, cryosectioning, washing, and matrix application. These steps must be carefully optimized for specific analytes of interest (lipids, proteins, drugs, etc.), representing a challenge for skin analysis. In this review, critical parameters for MALDI IMS sample preparation of skin samples will be described. In addition, specific applications of MALDI IMS of skin samples will be presented including wound healing, neoplasia, and infection. Copyright © 2017 Elsevier B.V. All rights reserved.

A Comparison of Analytical and Data Preprocessing Methods for Spectral Fingerprinting

PubMed Central

LUTHRIA, DEVANAND L.; MUKHOPADHYAY, SUDARSAN; LIN, LONG-ZE; HARNLY, JAMES M.

2013-01-01

Spectral fingerprinting, as a method of discriminating between plant cultivars and growing treatments for a common set of broccoli samples, was compared for six analytical instruments. Spectra were acquired for finely powdered solid samples using Fourier transform infrared (FT-IR) and Fourier transform near-infrared (NIR) spectrometry. Spectra were also acquired for unfractionated aqueous methanol extracts of the powders using molecular absorption in the ultraviolet (UV) and visible (VIS) regions and mass spectrometry with negative (MS−) and positive (MS+) ionization. The spectra were analyzed using nested one-way analysis of variance (ANOVA) and principal component analysis (PCA) to statistically evaluate the quality of discrimination. All six methods showed statistically significant differences between the cultivars and treatments. The significance of the statistical tests was improved by the judicious selection of spectral regions (IR and NIR), masses (MS+ and MS−), and derivatives (IR, NIR, UV, and VIS). PMID:21352644

Oligopeptidase B from Serratia proteamaculans. III. Inhibition analysis. Specific interactions with metalloproteinase inhibitors.

PubMed

Mikhailova, A G; Khairullin, R F; Kolomijtseva, G Ya; Rumsh, L D

2012-03-01

Inhibition of the novel oligopeptidase B from Serratia proteamaculans (PSP) by basic pancreatic trypsin inhibitor, Zn2+ ions, and o- and m-phenanthroline was investigated. A pronounced effect of calcium ions on the interaction of PSP with inhibitors was demonstrated. Inversion voltamperometry and atomic absorption spectrometry revealed no zinc ions in the PSP molecule. Hydrophobic nature of the enzyme inhibition by o- and m-phenanthroline was established.

Changes in UV absorption of sunscreens after UV irradiation

NASA Astrophysics Data System (ADS)

Tarras-Wahlberg, N.; Stenhagen, G.; Larkö, O.; Rosén, A.; Wennberg, A.-M.; Wennerström, O.

2000-03-01

In the present investigation we have studied the change in the absorption spectrum of some photoactive organic species in sunscreens after UVA and UVB irradiation in a dose normally encountered during a full day in the sun. The absorbance of 2-ethylhexyl 4-methoxycinnamate was reduced significantly, while 3-(4-methylbenzyliden)camphor seemed to be rather stable. The benzophenones studied seemed to be relatively stable. In the case of 4-tert.butyl-4´-methoxy-dibenzoylmethane there was a rapid decrease in the UVA absorption leading to unsatisfactory protection in the UVA region. 4-Isopropyl-dibenzoylmethane also lost most of its UV protective capacity after irradiation with UVA. UVB seemed to have a minor effect on all the samples. The present study including gas chromatography and mass spectrometry analysis indicates that some of the photoactive organic species commonly used today in sunscreens are unstable following UV irradiation.

Distribution of potentially hazardous trace elements in coals from Shanxi province, China

USGS Publications Warehouse

Zhang, J.Y.; Zheng, C.G.; Ren, D.Y.; Chou, C.-L.; Liu, J.; Zeng, R.-S.; Wang, Z.P.; Zhao, F.H.; Ge, Y.T.

2004-01-01

Shanxi province, located in the center of China, is the biggest coal base of China. There are five coal-forming periods in Shanxi province: Late Carboniferous (Taiyuan Formation), Early Permian (Shanxi Formation), Middle Jurassic (Datong Formation), Tertiary (Taxigou Formation), and Quaternary. Hundred and ten coal samples and a peat sample from Shanxi province were collected and the contents of 20 potentially hazardous trace elements (PHTEs) (As, B, Ba, Cd, Cl, Co, Cr, Cu, F, Hg, Mn, Mo, Ni, Pb, Sb, Se, Th, U, V and Zn) in these samples were determined by instrumental neutron activation analysis, atomic absorption spectrometry, cold-vapor atomic absorption spectrometry, ion chromatography spectrometry, and wet chemical analysis. The result shows that the brown coals are enriched in As, Ba, Cd, Cr, Cu, F and Zn compared with the bituminous coals and anthracite, whereas the bituminous coals are enriched in B, Cl, Hg, and the anthracite is enriched in Cl, Hg, U and V. A comparison with world averages and crustal abundances (Clarke values) shows that the Quaternary peat is highly enriched in As and Mo, Tertiary brown coals are highly enriched in Cd, Middle Jurassic coals, Early Permian coals and Late Carboniferous coals are enriched in Hg. According to the coal ranks, the bituminous coals are highly enriched in Hg, whereas Cd, F and Th show low enrichments, and the anthracite is also highly enriched in Hg and low enrichment in Th. The concentrations of Cd, F, Hg and Th in Shanxi coals are more than world arithmetic means of concentrations for the corresponding elements. Comparing with the United States coals, Shanxi coals show higher concentrations of Cd, Hg, Pb, Se and Th. Most of Shanxi coals contain lower concentrations of PHTEs. ?? 2004 Elsevier Ltd. All rights reserved.

Simplified multi-element analysis of ground and instant coffees by ICP-OES and FAAS.

PubMed

Szymczycha-Madeja, Anna; Welna, Maja; Pohl, Pawel

2015-01-01

A simplified alternative to the wet digestion sample preparation procedure for roasted ground and instant coffees has been developed and validated for the determination of different elements by inductively coupled plasma optical emission spectrometry (ICP-OES) (Al, Ba, Cd, Co, Cr, Cu, Mn, Ni, Pb, Sr, Zn) and flame atomic absorption spectrometry (FAAS) (Ca, Fe, K, Mg, Na). The proposed procedure, i.e. the ultrasound-assisted solubilisation in aqua regia, is quite fast and simple, requires minimal use of reagents, and demonstrated good analytical performance, i.e. accuracy from -4.7% to 1.9%, precision within 0.5-8.6% and recovery in the range 93.5-103%. Detection limits of elements were from 0.086 ng ml(-1) (Sr) to 40 ng ml(-1) (Fe). A preliminary classification of 18 samples of ground and instant coffees was successfully made based on concentrations of selected elements and using principal component analysis and hierarchic cluster analysis.

Partitioning the relative contributions of inorganic plant composition and soil characteristics to the quality of Helichrysum italicum subsp. italicum (Roth) G. Don fil. essential oil.

PubMed

Bianchini, Ange; Santoni, François; Paolini, Julien; Bernardini, Antoine-François; Mouillot, David; Costa, Jean

2009-07-01

Composition of Helichrysum italicum subsp. italicum essential oil showed chemical variability according to vegetation cycle, environment, and geographic origins. In the present work, 48 individuals of this plant at different development stages and the corresponding root soils were sampled: i) 28 volatile components were identified and measured in essential oil by using GC and GC/MS; ii) ten elements from plants and soils have been estimated using colorimetry in continuous flux, flame atomic absorption spectrometry, or emission spectrometry (FAAS/FAES); iii) texture and acidity (real and potential) of soil samples were also reported. Relationships between the essential-oil composition, the inorganic plant composition, and the soil characteristics (inorganic composition, texture, and acidity) have been established using multivariate analysis such as Principal Component Analysis (PCA) and partial Redundancy Analysis (RDA). This study demonstrates a high level of intraspecific differences in oil composition due to environmental factors and, more particularly, soil characteristics.

[Analysis of biological material originating from the body of general Władysław Sikorski for inorganic poisons and diatoms presence].

PubMed

Sadlik, Józefa Krystyna; Brozek-Mucha, Zuzanna

2009-01-01

Results of the analysis of biological materials originating from the body of general Sikorski are presented in the paper. Samples of the liver, kidney, intestine and lung were analysed for metals and As content, and samples of the lung, liver, kidney, stomach, intestine and bone marrow--for diatoms presence. The analysis for metals and As was performed by atomic absorption spectrometry (AAS) and inductively coupled plasma optical emission spectrometry (ICP-OES). Before the analysis, the samples were wet digested by the classic and microwave assisted method. The analysis did not result in detecting the presence of As, Co, Ni, and Tl in any of the studied materials, while Hg was not revealed in the liver, intestines and lung and Pb in the intestines and lung. The content of Ba, Cd, Cr, Cu, Fe, Mn, Sr and Zn in all the studied materials, Hg in the kidney, and Pb in the liver and kidney did not indicate poisoning by the above-mentioned metals or arsenic. No diatoms were found in the studied materials.

Determination of uranium isotopes in food and environmental samples by different techniques: a comparison.

PubMed

Forte, M; Rusconi, R; Margini, C; Abbate, G; Maltese, S; Badalamenti, P; Bellinzona, S

2001-01-01

The uranium concentration in 59 samples of bottled and tap water, mainly from northern Italy, was measured by different techniques. Results obtained by inductively coupled plasma mass spectrometry (ICP-MS), semiconductor alpha spectrometry and low level liquid scintillation counting with alpha/beta discrimination (LSC) have been compared. High resolution gamma spectrometry and semiconductor alpha spectrometry have been used to analyse uranium in a variety of organic and inorganic samples. Isotopic secular equilibrium in the 238U series may be lacking or hidden by auto-absorption phenomena, so caution should be used in evaluating gamma spectrometry data. Alpha spectrometry has also been used to ascertain the possible pollution from depleted uranium in the environment.

Determination of cadmium and lead at low levels by using preconcentration at fullerene coupled to thermospray flame furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Pereira, M. G.; Pereira-Filho, E. R.; Berndt, H.; Arruda, M. A. Z.

2004-04-01

A new and sensitive method for Cd and Pb determinations, based on the coupling of thermospray flame furnace atomic absorption spectrometry and a preconcentrator system, was developed. The procedure comprised the chelating of Cd and Pb with ammonium pyrrolidinedithiocarbamate with posterior adsorption of the chelates on a mixture (40 mg) of C 60 and C 70 at a flow rate of 2.0 ml min -1. These chelates were eluted from the adsorbent by passing a continuous flow of ethanol (80% v/v) at 0.9 ml min -1 to a nickel tube placed in an air/acetylene flame. After sample introduction into the tube by using a ceramic capillary (0.5 mm i.d.), the analytical signals were registered as peak height. Under these conditions, improvement factors in detectability of 675 and 200 were obtained for Cd and Pb, respectively, when compared to conventional flame atomic absorption spectrometry. Spiked samples (mineral and tap waters) and drinking water containing natural concentrations of Cd were employed for evaluating accuracy by comparing the results obtained from the proposed methodology with those using electrothermal atomic absorption spectrometry. In addition, certified reference materials (rye grass, CRM 281 and pig kidney, CRM 186) were also adopted for the accuracy tests. Due to the good linearity ranges for Cd (0.5-5.0 μg l -1) and Pb (10-250 μg l -1), samples with different concentrations could be analyzed. Detection limits of 0.1 and 2.4 μg l -1 were obtained for Cd and Pb, respectively, and RSD values <4.5% were observed ( n=10). Finally, a sample throughput of 24 determinations per hour was possible.

Determination of metals in lubricating oils by flame atomic absorption spectrometry using a single-bore high-pressure pneumatic nebulizer.

PubMed

Mora, J; Todolí, J L; Sempere, F J; Canals, A; Hernandis, V

2000-12-01

The behaviour of a single-bore high-pressure pneumatic nebulizer (SBHPPN) as a tool for the analysis of lubricating oils by flame atomic absorption spectrometry (FAAS) was investigated. The effects of the sample oil content [from 10% to 100% (w/w) oil in 4-methylpentan-2-one, IBMK] and the carrier nature (IBMK and methanol) on the characteristics of the aerosols generated, on the analyte transport efficiency and on the analytical figures of merit in FAAS were studied. A pneumatic concentric nebulizer (PCN) was used for comparison. Increasing the oil content increases the viscosity of the sample. With the PCN this gives rise to coarser aerosols, making it impossible to nebulize samples with an oil content higher than 70% (w/w). Using the SBHPPN, the viscosity of the sample scarcely affects the characteristics of the primary aerosols. Hence, the SBHPPN is able, by using the appropriate carrier, to nebulize pure lubricating oils. Among the carriers tested, IBMK is the most advisable because it is fully miscible with all the oil samples. The SBHPPN provides higher sensitivities and lower limits of detection than the PCN. Compared with a method based on organic dilution, the use of the SBHPPN for the direct analysis of lubricating oils by FAAS makes it possible, in addition to increasing the analysis throughput, to detect elements at lower concentrations. Moreover, the SBHPPN provides similar results to those obtained using a previous acid digestion step.

Selenium analysis by an integrated microwave digestion-needle trap device with hydride sorption on carbon nanotubes and electrothermal atomic absorption spectrometry determination

NASA Astrophysics Data System (ADS)

Maratta Martínez, Ariel; Vázquez, Sandra; Lara, Rodolfo; Martínez, Luis Dante; Pacheco, Pablo

2018-02-01

An integrated microwave assisted digestion (MW-AD) - needle trap device (NTD) for selenium determination in grape pomace samples is presented. The NTD was filled with oxidized multiwall carbon nanotubes (oxMWCNTS) where Se hydrides were preconcentrated. Determination was carried out by flow injection-electrothermal atomic absorption spectrometry (FI-ETAAS). The variables affecting the system were established by a multivariate design (Plackett Burman), indicating that the following variables significantly affect the system: sample amount, HNO3 digestion solution concentration, NaBH4 volume and elution volume. A Box-Behnken design was implemented to determine the optimized values of these variables. The system improved Se atomization in the graphite furnace, since only trapped hydrides reached the graphite furnace, and the pyrolysis stage was eliminated according to the aqueous matrix of the eluate. Under optimized conditions the system reached a limit of quantification of 0.11 μg kg- 1, a detection limit of 0.032 μg kg- 1, a relative standard deviation of 4% and a preconcentration factor (PF) of 100, reaching a throughput sample of 5 samples per hour. Sample analysis show Se concentrations between 0.34 ± 0.03 μg kg- 1 to 0.48 ± 0.03 μg kg- 1 in grape pomace. This system provides minimal reagents and sample consumption, eliminates discontinuous stages between samples processing reaching a simpler and faster Se analysis.

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

USGS Publications Warehouse

Meier, A.L.

1982-01-01

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

Speciation of chromium (VI) and total chromium determination in welding dust samples by flow-injection analysis coupled to atomic absorption spectrometry.

PubMed

Girard, L; Hubert, J

1996-11-01

We have studied the speciation of chromium (VI) in stainless-steel welding dusts. The approach used for the analysis of Cr(VI) and total Cr relies on a flow-injection analyzer (FIA) equipped with two different sequential detectors. The system measures Cr(VI). by colorimetry (with 1,5-diphenyl carbohydrazide) and total chromium content by flame atomic absorption spectroscopy (AAS). The extraction of the samples of welding-fume dusts is achieved in a buffer solution (acetic acid and sodium acetate at pH 4). This extraction procedure gives a 96% recovery of chromium (VI). The FIA-AAS system that has been described is also more sensitive, has a lower detection limit (0.005 mug ml(-1)) and gives a better precision (< 1%) than other equivalent systems that have been previously described.

Bile acid profiling and quantification in biofluids using ultra-performance liquid chromatography tandem mass spectrometry.

PubMed

Sarafian, Magali H; Lewis, Matthew R; Pechlivanis, Alexandros; Ralphs, Simon; McPhail, Mark J W; Patel, Vishal C; Dumas, Marc-Emmanuel; Holmes, Elaine; Nicholson, Jeremy K

2015-10-06

Bile acids are important end products of cholesterol metabolism. While they have been identified as key factors in lipid emulsification and absorption due to their detergent properties, bile acids have also been shown to act as signaling molecules and intermediates between the host and the gut microbiota. To further the investigation of bile acid functions in humans, an advanced platform for high throughput analysis is essential. Herein, we describe the development and application of a 15 min UPLC procedure for the separation of bile acid species from human biofluid samples requiring minimal sample preparation. High resolution time-of-flight mass spectrometry was applied for profiling applications, elucidating rich bile acid profiles in both normal and disease state plasma. In parallel, a second mode of detection was developed utilizing tandem mass spectrometry for sensitive and quantitative targeted analysis of 145 bile acid (BA) species including primary, secondary, and tertiary bile acids. The latter system was validated by testing the linearity (lower limit of quantification, LLOQ, 0.25-10 nM and upper limit of quantification, ULOQ, 2.5-5 μM), precision (≈6.5%), and accuracy (81.2-118.9%) on inter- and intraday analysis achieving good recovery of bile acids (serum/plasma 88% and urine 93%). The ultra performance liquid chromatography-mass spectrometry (UPLC-MS)/MS targeted method was successfully applied to plasma, serum, and urine samples in order to compare the bile acid pool compositional difference between preprandial and postprandial states, demonstrating the utility of such analysis on human biofluids.

GFAAS determination of selenium in infant formulas using a microwave digestion method.

PubMed

Alegria, A; Barbera, R; Farré, R; Moreno, A

1994-01-01

A method for determining the selenium content of infant formulas is proposed. It includes wet digestion with nitric acid and hydrogen peroxide in medium pressure teflon bombs in a microwave oven and determination by graphite furnace atomic absorption spectrometry (GFAAS). The absence of interferences is checked. Values obtained for the limit of detection (19.4 ng/g), precision (RSD = 2.2%) and accuracy by analysis of a reference material show that the method is reliable.

Lead and cadmium in human placentas and maternal and neonatal blood (in a heavily polluted area) measured by graphite furnace atomic absorption spectrometry.

PubMed Central

Baranowska, I

1995-01-01

OBJECTIVE--To measure the concentrations of the trace elements lead and cadmium in human placenta and in maternal and neonatal (cord) blood. To assess the influence of the strongly polluted environment on the content of metals in tissues and on the permeability of placenta to cadmium and lead. Various methods of mineralisation were tested before analysis. METHODS--Graphite furnace atomic absorption spectrometry was used for the determination of lead and cadmium. The samples for analysis were prepared by mineralisation under pressure in a Teflon bomb (HNO3, 110 degrees C), by wet ashing under normal pressure (HNO3 + H2O2 for 12 hours), and by microwave digestion in concentrated nitric acid. RESULTS--In analysed samples the following mean concentrations of cadmium and lead were found: in venous blood Pb = 72.50 ng/ml, Cd = 4.90 ng/ml; in placenta Pb = 0.50 microgram/g, Cd = 0.11 microgram/g; in cord blood Pb = 38.31 ng/ml, Cd = 1.13 ng/ml. CONCLUSION--High concentrations of lead and cadmium were found in placentas and in maternal blood whereas in neonatal blood there was an increased concentration of lead and only traces of cadmium. It is concluded that the placenta is a better barrier for cadmium than for lead. Among the examined methods of mineralisation, microwave digestion was the best. PMID:7795737

Determining the arsenic, cadmium, lead, copper and chromium contents by atomic absorption spectrometry in Pangasius fillets from Vietnam.

PubMed

Molognoni, Luciano; Vitali, Luciano; Ploêncio, Leandro As; Santos, Jacson N; Daguer, Heitor

2016-07-01

Pangasius is a fish produced on a large scale in Vietnam and exported to many countries. Since river contamination from human activities can affect the safety of this food, fish consumption can cause exposure to potentially toxic elements for humans. The aim of this study, therefore, was to assess arsenic, cadmium, lead, copper and chromium contents by atomic absorption spectrometry in Pangasius fillet produced in the provinces of Dong Thap and Can Tho (Vietnam) and exported to Brazil. The limits of detection were: arsenic 0.5443 µg kg(-1) , cadmium 0.0040 mg kg(-1) , chromium 0.0004 mg kg(-1) , copper 0.0037 mg kg(-1) and lead 0.0284 mg kg(-1) . Analysis of 20 samples showed results below the limit of detection for arsenic, chromium and lead, while copper average concentration was 0.0234 mg kg(-1) . Cadmium average concentration was 0.0547 mg kg(-1) , with no significant difference between the two regions studied. The samples of Pangasius had no detectable concentrations of arsenic, chromium, copper and lead, and do not represent a hazard to public health. However, cadmium analysis revealed non-compliant samples, demonstrating the importance of monitoring the quality of imported Pangasius fish. © 2015 Society of Chemical Industry. © 2015 Society of Chemical Industry.

Reduction of interferences in graphite furnace atomic absorption spectrometry by multiple linear regression modelling

NASA Astrophysics Data System (ADS)

Grotti, Marco; Abelmoschi, Maria Luisa; Soggia, Francesco; Tiberiade, Christian; Frache, Roberto

2000-12-01

The multivariate effects of Na, K, Mg and Ca as nitrates on the electrothermal atomisation of manganese, cadmium and iron were studied by multiple linear regression modelling. Since the models proved to efficiently predict the effects of the considered matrix elements in a wide range of concentrations, they were applied to correct the interferences occurring in the determination of trace elements in seawater after pre-concentration of the analytes. In order to obtain a statistically significant number of samples, a large volume of the certified seawater reference materials CASS-3 and NASS-3 was treated with Chelex-100 resin; then, the chelating resin was separated from the solution, divided into several sub-samples, each of them was eluted with nitric acid and analysed by electrothermal atomic absorption spectrometry (for trace element determinations) and inductively coupled plasma optical emission spectrometry (for matrix element determinations). To minimise any other systematic error besides that due to matrix effects, accuracy of the pre-concentration step and contamination levels of the procedure were checked by inductively coupled plasma mass spectrometric measurements. Analytical results obtained by applying the multiple linear regression models were compared with those obtained with other calibration methods, such as external calibration using acid-based standards, external calibration using matrix-matched standards and the analyte addition technique. Empirical models proved to efficiently reduce interferences occurring in the analysis of real samples, allowing an improvement of accuracy better than for other calibration methods.

Multiwalled carbon nanotubes as a sorbent material for the solid phase extraction of lead from urine and subsequent determination by electrothermal atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Peña Crecente, Rosa M.; Lovera, Carlha Gutiérrez; García, Julia Barciela; Méndez, Jennifer Álvarez; Martín, Sagrario García; Latorre, Carlos Herrero

2014-11-01

The determination of lead in urine is a way of monitoring the chemical exposure to this metal. In the present paper, a new method for the Pb determination by electrothermal atomic absorption spectrometry (ETAAS) in urine at low levels has been developed. Lead was separated from the undesirable urine matrix by means of a solid phase extraction (SPE) procedure. Oxidized multiwalled carbon nanotubes have been used as a sorbent material. Lead from urine was retained at pH 4.0 and was quantitatively eluted using a 0.7 M nitric acid solution and was subsequently measured by ETAAS. The effects of parameters that influence the adsorption-elution process (such as pH, eluent volume and concentration, sampling and elution flow rates) and the atomic spectrometry conditions have been studied by means of different factorial design strategies. Under the optimized conditions, the detection and quantification limits obtained were 0.08 and 0.26 μg Pb L- 1, respectively. The results demonstrate the absence of a urine matrix effect and this is the consequence of the SPE process carried out. Therefore, the developed method is useful for the analysis of Pb at low levels in real samples without the influence of other urine components. The proposed method was applied to the determination of lead in urine samples of unexposed healthy people and satisfactory results were obtained (in the range 3.64-22.9 μg Pb L- 1).

Simple method for determination of selenium in biological materials by flameless atomic-absorption spectrometry using a carbon-tube atomizer.

PubMed

Ishizaki, M

1978-03-01

A method for determination of selenium in biological materials by flameless atomic-absorption spectrometry using a carbon-tube atomizer is described. The sample is burned by an oxygen-flask combustion procedure, the resulting solution is treated with a cation-exchange resin to eliminate interfering cations, the selenium is extracted with dithizone in carbon tetrachloride and the resulting selenium dithizonate is combined with nickel nitrate in the carbon tube to enhance the sensitivity for selenium and avoid volatilization losses. The method measures selenium concentrations as low as 0.01 mug/g with a relative standard deviation of 8%.

Determination of sulfur in bovine serum albumin and L-cysteine using high-resolution continuum source molecular absorption spectrometry of the CS molecule

NASA Astrophysics Data System (ADS)

Andrade-Carpente, Eva; Peña-Vázquez, Elena; Bermejo-Barrera, Pilar

2016-08-01

In this study, the content of sulfur in bovine serum albumin and L-cysteine was determined using high-resolution continuum source molecular absorption spectrometry of the CS molecule, generated in a reducing air-acetylene flame. Flame conditions (height above the burner, measurement time) were optimized using a 3.0% (v/v) sulfuric acid solution. A microwave lab station (Ethos Plus MW) was used for the digestion of both compounds. During the digestion step, sulfur was converted to sulfate previous to the determination. Good repeatability (4-10%) and analytical recovery (91-106%) was obtained.

[Determination of eight trace elements in the Swertia davidii Franch by flame atomic absorption spectrometry].

PubMed

Li, Tao; Wang, Yuan-zhong; Yu, Hon; Cao, Yu-juan; Zhang, Jing-jing; Liu, Qin

2007-12-01

The effects of different sample digestives on the determination of Swertia davidii Franch are compared. Eight trace elements in the Swertia davidii Franch were determined by flame atomic absorption spectrometry. The result shows that the RSD and recovery are better if the Swertia davidii Franch was digested with HNO3-HClO4 (5 : 1) mixed acid. The experimental results show that the detection limits were all smaller than 0.097 microg x mL(-1), the RSDs (n=8) all smaller than 2.34%, and the addition standard recovery (ASR) (n=8) was 89.32%-106.65% for all the elements.

Mesoporous Silica Nanoparticles as an Adsorbent for Preconcentration and Determination of Trace Amount of Nickel in Environmental Samples by Atom Trap Flame Atomic Absorption Spectrometry

NASA Astrophysics Data System (ADS)

Shirkhanloo, H.; Falahnejad, M.; Zavvar Mousavi, H.

2016-01-01

A rapid enrichment method based on solid-phase extraction (SPE) has been established for preconcentration and separation of trace Ni(II) ions in water samples prior to their determination by atom trap flame atomic absorption spectrometry. A column filled with bulky NH2-UVM7 was used as the novel adsorbent. Under optimal conditions, the linear range, limit of detection (LOD), and preconcentration factor (PF) were 3-92 μg/L, 0.8 μg/L, and 100, respectively. The validity of the method was checked by the standard reference material.

Working towards accreditation by the International Standards Organization 15189 Standard: how to validate an in-house developed method an example of lead determination in whole blood by electrothermal atomic absorption spectrometry.

PubMed

Garcia Hejl, Carine; Ramirez, Jose Manuel; Vest, Philippe; Chianea, Denis; Renard, Christophe

2014-09-01

Laboratories working towards accreditation by the International Standards Organization (ISO) 15189 standard are required to demonstrate the validity of their analytical methods. The different guidelines set by various accreditation organizations make it difficult to provide objective evidence that an in-house method is fit for the intended purpose. Besides, the required performance characteristics tests and acceptance criteria are not always detailed. The laboratory must choose the most suitable validation protocol and set the acceptance criteria. Therefore, we propose a validation protocol to evaluate the performance of an in-house method. As an example, we validated the process for the detection and quantification of lead in whole blood by electrothermal absorption spectrometry. The fundamental parameters tested were, selectivity, calibration model, precision, accuracy (and uncertainty of measurement), contamination, stability of the sample, reference interval, and analytical interference. We have developed a protocol that has been applied successfully to quantify lead in whole blood by electrothermal atomic absorption spectrometry (ETAAS). In particular, our method is selective, linear, accurate, and precise, making it suitable for use in routine diagnostics.

Liquid chromatography-hydride generation-atomic absorption spectrometry for the speciation of tin in seafoods.

PubMed

Viñas, Pilar; López-García, Ignacio; Merino-Meroño, Beatriz; Campillo, Natalia; Hernández-Cordóba, Manuel

2004-04-01

Liquid chromatography with hydride generation atomic absorption spectrometry as the detection system was applied to the separation and determination of inorganic tin, tributyltin, dibutyltin, monobutyltin, diphenyltin and monophenyltin. A reversed phase C18 column and a methanol/water/acetic acid (70:27:3, v/v/v) mixture containing 0.05%(v/v) triethylamine and 0.1%(w/v) tropolone as the mobile phase (isocratic elution) were used. Extraction of organotins from the samples was carried out using methanol containing 0.05%(w/v) tropolone, a process that was repeated twice. The supernatants were shaken with water and dichloromethane in a separating funnel and the organic phase was collected and evaporated to dryness. When the method was applied to the speciation of tin in fresh and canned mussels, no organotins above the detection limits were identified in any of the samples, inorganic tin being the only species detected. The reliability of the procedure was checked by analyzing the total tin content of the samples by electrothermal atomic absorption spectrometry and by speciation of tin in a certified reference material, mussel tissue (CRM 477). The method can be used for environmental monitoring of organotins contaminated samples.

Determination of gold and cobalt dopants in advanced materials based on tin oxide by slurry sampling high-resolution continuum source graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Filatova, Daria G.; Eskina, Vasilina V.; Baranovskaya, Vasilisa B.; Vladimirova, Svetlana A.; Gaskov, Alexander M.; Rumyantseva, Marina N.; Karpov, Yuri A.

2018-02-01

A novel approach is developed for the determination of Co and Au dopants in advanced materials based on tin oxide using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS GFAAS) with direct slurry sampling. Sodium carboxylmethylcellulose (Na-CMC) is an effective stabilizer for diluted suspensions. Use Na-CMC allows to transfer the analytes into graphite furnace completely and reproducibly. The relative standard deviation obtained by HR CS GFAAS was not higher than 4%. Accuracy was proven by means inductively coupled plasma mass spectrometry (ICP-MS) in solutions after decomposition as a comparative technique. To determine Au and Co in the volume of SnO2, the acid decomposition conditions (HCl, HF) of the samples were suggested by means of an autoclave in a microwave oven.

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

PubMed

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

2016-05-01

This work describes a new method for the extraction and determination of gold nanoparticles in environmental samples by means of in-situ suspended aggregate microextraction and electrothermal atomic absorption spectrometry. The method relies on the in-situ formation of a supramolecular aggregate phase through ion-association between a cationic surfactant and a benzene sulfonic acid derivative. Gold nanoparticles are physically entrapped into the aggregate phase which is separated from the bulk aqueous solution by vacuum filtration on the surface of a cellulose filter in the form of a thin film. The film is removed from the filter surface and is dissociated into an acidified methanolic solution which is used for analysis. Under the optimized experimental conditions, gold nanoparticles can be efficiently extracted from water samples with recovery rates between 81.0-93.3%, precision 5.4-12.0% and detection limits as low as 75femtomolL(-1) using only 20mL of sample volume. The satisfactory analytical features of the method along with the simplicity indicate the efficiency of this new approach to adequately collect and extract gold nanoparticle species from water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

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

PubMed

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.

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.

PubMed

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.

Trace mercury determination in drinking and natural water samples by room temperature ionic liquid based-preconcentration and flow injection-cold vapor atomic absorption spectrometry.

PubMed

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).

Ionic liquid-based extraction followed by graphite-furnace atomic absorption spectrometry for the determination of trace heavy metals in high-purity iron metal.

PubMed

Matsumiya, Hiroaki; Kato, Tatsuya; Hiraide, Masataka

2014-02-01

The analysis of high-purity materials for trace impurities is an important and challenging task. The present paper describes a facile and sensitive method for the determination of trace heavy metals in high-purity iron metal. Trace heavy metals in an iron sample solution were rapidly and selectively preconcentrated by the extraction into a tiny volume of an ionic liquid [1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide] for the determination by graphite-furnace atomic absorption spectrometry (GFAAS). A nitrogen-donating neutral ligand, 2,4,6-tris(2-pyridyl)-1,3,5-triazine (TPTZ), was found to be effective in the ionic liquid-based selective extraction, allowing the nearly complete (~99.8%) elimination of the iron matrix. The combination with the optimized GFAAS was successful. The detectability reached sub-μg g(-1) levels in iron metal. The novel use of TPTZ in ionic liquid-based extraction followed by GFAAS was successfully applied to the determination of traces of Co, Ni, Cu, Cd, and Pb in certified reference materials for high-purity iron metal. © 2013 Published by Elsevier B.V.

Preconcentration of lead using solidification of floating organic drop and its determination by electrothermal atomic absorption spectrometry

PubMed Central

Chamsaz, Mahmoud; Akhoundzadeh, Jeiran; Arbab-zavar, Mohammad Hossein

2012-01-01

A simple microextraction method based on solidification of a floating organic drop (SFOD) was developed for preconcentration of lead prior to its determination by electrothermal atomic absorption spectrometry (ETAAS). Ammonium pyrolidinedithiocarbamate (APDC) was used as complexing agent, and the formed complex was extracted into a 20 μL of 1-undecanol. The extracted complex was diluted with ethanol and injected into a graphite furnace. An orthogonal array design (OAD) with OA16 (45) matrix was employed to study the effects of different parameters such as pH, APDC concentration, stirring rate, sample solution temperature and the exposure time on the extraction efficiency. Under the optimized experimental conditions the limit of detection (based on 3 s) and the enhancement factor were 0.058 μg L−1 and 113, respectively. The relative standard deviation (RSD) for 8 replicate determinations of 1 μg L−1 of Pb was 8.8%. The developed method was validated by the analysis of certified reference materials and was successfully applied to the determination of lead in water and infant formula base powder samples. PMID:25685441

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

PubMed

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

2014-02-01

The present paper reported the differential scanning calorimetry-thermogravimetry curves and the infrared (IR) absorption spectrometry under the temperature program analyzed by the combined simultaneous thermal analysis-IR spectrometer. The gas products of coal were identified by the IR spectrometry. This paper emphasized on the combustion at high temperature-IR absorption method, a convenient and accurate method, which measures the content of sulfur in coal indirectly through the determination of the content of sulfur dioxide in the mixed gas products by IR absorption. It was demonstrated, when the instrument was calibrated by varied pure compounds containing sulfur and certified reference materials (CRMs) for coal, that there was a large deviation in the measured sulfur contents. It indicates that the difference in chemical speciations of sulfur between CRMs and the analyte results in a systematic error. The time-IR absorption curve was utilized to analyze the composition of sulfur at low temperatures and high temperatures and then the sulfur content of coal sample was determined by using a CRM for coal with a close composition of sulfur. Therefore, the systematic error due to the difference in chemical speciations of sulfur between the CRM and analyte was eliminated. On the other hand, in this combustion at high temperature-IR absorption method, the mass of CRM and analyte were adjusted to assure the sulfur mass equal and then the CRM and the analyte were measured alternately. This single-point calibration method reduced the effect of the drift of the IR detector and improved the repeatability of results, compared with the conventional multi-point calibration method using the calibration curves of signal intensity vs sulfur mass. The sulfur content results and their standard deviations of an anthracite coal and a bituminous coal with a low sulfur content determined by this modified method were 0.345% (0.004%) and 0.372% (0.008%), respectively. The uncertainty (U, k =2) of sulfur contents of two coal samples was evaluated to be 0.019% and 0.021%, respectively. Two main modifications, namely the calibration using the coal CRM with a similar composition of low-temperature sulfur and high temperature sulfur, and the single-point calibration alternating CRM and analyte, endow the combustion at high temperature-IR absorption method with an accuracy obviously better than that of the ASTM method. Therefore, this modified method has a well potential in the analysis of sulfur content.

Environmental assessment of a firetube boiler firing coal/oil/water mixtures. Volume 2. Data supplement. Final report, February 1981-November 1983

DOE Office of Scientific and Technical Information (OSTI.GOV)

DeRosier, R.

1984-09-01

This volume is a compendium of detailed emission and test data from field tests of a firetube industrial boiler burning a coal/oil/water (COW) mixture. The boiler was tested while burning COW fuel, and COW with soda ash added (COW+SA) to serve as an SO/sub 2/ sorbent. The test data include: preliminary equipment calibration data, boiler operating data for both tests, fuel analysis results, and complete flue gas emission measurement and laboratory analysis results. Flue gas emission measurements included: continuous monitoring for criteria gas pollutants; gas chromatography (GC) of gas grab samples for volatile organics (C1-C6); EPA Method 5 for particulate;more » controlled condensation system for SO2 emissions; and source assessment sampling system (SASS) for total organics in two boiling point ranges (100 to 300 C and > 300 C), organic compound category information using infrared spectrometry (IR) and low resolution mass spectrometry (LRMS), specific quantitation of the semivolatile organic priority pollutants using gas chromatography/mass spectrometry (GC/MS), liquid chromatography (LC) separation of organic extracts into seven polarity fractions with total organic and IR analyses of eluted fractions, flue gas concentrations of trace elements by spark source mass spectrometry (SSMS) and atomic absorption spectroscopy (AAS), and biological assays of organic extracts.« less

Investigation of heavy-metal accumulation in selected plant samples using laser induced breakdown spectroscopy and laser ablation inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Galiová, M.; Kaiser, J.; Novotný, K.; Novotný, J.; Vaculovič, T.; Liška, M.; Malina, R.; Stejskal, K.; Adam, V.; Kizek, R.

2008-12-01

Single-pulse Laser-Induced Breakdown Spectroscopy (LIBS) and Laser-Ablation Inductively Coupled Plasma Mass-Spectrometry (LA-ICP-MS) were applied for mapping the silver and copper distribution in Helianthus Annuus L. samples treated with contaminant in controlled conditions. For Ag and Cu detection the 328.07 nm Ag(I) and 324.75 nm Cu(I) lines were used, respectively. The LIBS experimental conditions (mainly the laser energy and the observation window) were optimized in order to avoid self-absorption effect in the measured spectra. In the LA-ICP-MS analysis the Ag 107 and Cu 63 isotopes were detected. The capability of these two analytical techniques for high-resolution mapping of selected trace chemical elements was demonstrated.

The Association Between Serum Selenium Levels with Rheumatoid Arthritis.

PubMed

Yu, Na; Han, Fang; Lin, Xiaojun; Tang, Chun; Ye, Jinghua; Cai, Xiaoyan

2016-07-01

There are conflicting reports on the correlation between serum selenium (Se) levels with rheumatoid arthritis (RA). Through a meta-analysis approach, the aim of the present study is to clarify the relationship between serum Se levels with RA. We searched literatures that met our predefined criteria in PubMed, ScienceDirect, and OVID published as of September 2015. Ten eligible articles with 14 case-control studies involving 716 subjects were identified. Overall, pooled analysis indicated that subjects with RA had lower serum levels of Se than the healthy controls (standardized mean difference (SMD) = -1.347, 95 % confidence interval (CI) = [-1.872, -0.823], p < 0.001). Further subgroup analysis indicated that subjects with RA had lower serum Se levels than healthy controls in Europe (SMD = -1.063, 95 % CI = [-1.571, -0.556], p < 0.001) and Asia (SMD = -3.254, 95 % CI = [-4.687, -1.821], p < 0.001) but not in USA (SMD = -0.322, 95 % CI = [-0.657, 0.012], p = 0.059). The serum Se levels were lower in RA than healthy controls measured by graphite furnace atom absorption spectrometry (GFAAS) (SMD = -1.026, 95 % CI = [-1.522, -0.530], p < 0.001), electrothermal absorption spectrometry (EAS) (SMD = -1.197, 95 % CI = [-2.373, -0.020], p < 0.05), flame atomic absorption spectrophotometry (FAAS) (SMD = -0.681, 95 % CI = [-1.049, -0.313], p < 0.001), and inductively coupled plasma-mass spectrophotometer (ICP-MS) (SMD = -11.707, 95 % CI = [-15.189, -8.224], p < 0.001) but not by neutron activation analysis (NAA) (SMD = -0.674, 95 % CI = [-1.350, 0.003], p = 0.051). In conclusion, this meta-analysis supports a significant association between low serum Se concentration with RA. However, this finding needs further confirmation by a trans-regional multicenter study to obtain better understanding of causal relationship between serum Se with RA of different human races or regions.

Major and trace element chemistry of Luna 24 samples from Mare Crisium

NASA Technical Reports Server (NTRS)

Blanchard, D. P.; Brannon, J. C.; Aaboe, E.; Budahn, J. R.

1978-01-01

Atomic absorption spectrometry and instrumental neutron activation analysis were employed to analyze six Luna 24 soils for major and trace elements. The analysis revealed well-mixed soils, though size fractions of each of the soils showed quite dissimilar compositions. Thus the regolith apparently has not been extensively reworked. Noritic breccia admixed preferentially to the finest size fractions and differential comminution of one or more other soil components accounted for the observed elemental distributions as a function of grain size. The ferrobasalt composition and one or more components with higher MgO contents have been identified in the samples.

Monosodium glutamate for simple photometric iron analysis

NASA Astrophysics Data System (ADS)

Prasetyo, E.

2018-01-01

Simple photometric method for iron analysis using monosodium glutamate (MSG) was proposed. The method could be used as an alternative method, which was technically simple, economic, quantitative, readily available, scientifically sound and environmental friendly. Rapid reaction of iron (III) with glutamate in sodium chloride-hydrochloric acid buffer (pH 2) to form red-brown complex was served as a basis in the photometric determination, which obeyed the range of iron (III) concentration 1.6 - 80 µg/ml. This method could be applied to determine iron concentration in soil with satisfactory results (accuracy and precision) compared to other photometric and atomic absorption spectrometry results.

Development of a High-Resolution Laser Absorption Spectroscopy Method with Application to the Determination of Absolute Concentration of Gaseous Elemental Mercury in Air.

PubMed

Srivastava, Abneesh; Hodges, Joseph T

2018-06-05

Isotope dilution-cold-vapor-inductively coupled plasma mass spectrometry (ID-CV-ICPMS) has become the primary standard for measurement of gaseous elemental mercury (GEM) mass concentration. However, quantitative mass spectrometry is challenging for several reasons including (1) the need for isotopic spiking with a standard reference material, (2) the requirement for bias-free passive sampling protocols, (3) the need for stable mass spectrometry interface design, and (4) the time and cost involved for gas sampling, sample processing, and instrument calibration. Here, we introduce a high-resolution laser absorption spectroscopy method that eliminates the need for sample-specific calibration standards or detailed analysis of sample treatment losses. This technique involves a tunable, single-frequency laser absorption spectrometer that measures isotopically resolved spectra of elemental mercury (Hg) spectra of 6 1 S 0 ← 6 3 P 1 intercombination transition near λ = 253.7 nm. Measured spectra are accurately modeled from first-principles using the Beer-Lambert law and Voigt line profiles combined with literature values for line positions, line shape parameters, and the spontaneous emission Einstein coefficient to obtain GEM mass concentration values. We present application of this method for the measurement of the equilibrium concentration of mercury vapor near room temperature. Three closed systems are considered: two-phase mixtures of liquid Hg and its vapor and binary two-phase mixtures of Hg-air and Hg-N 2 near atmospheric pressure. Within the experimental relative standard uncertainty, 0.9-1.5% congruent values of the equilibrium Hg vapor concentration are obtained for the Hg-only, Hg-air, Hg-N 2 systems, in confirmation with thermodynamic predictions. We also discuss detection limits and the potential of the present technique to serve as an absolute primary standard for measurements of gas-phase mercury concentration and isotopic composition.

Determination of Chlorine in Milk via Molecular Absorption of SrCl Using High-Resolution Continuum Source Graphite Furnace Atomic Absorption Spectrometry.

PubMed

Ozbek, Nil; Akman, Suleyman

2016-07-20

Total chlorine in milk was determined via the molecular absorption of diatomic strontium monochloride at 635.862 nm using high-resolution continuum source graphite furnace atomic absorption spectrometry. The effects of coating the graphite furnace, using different modifiers, amount of molecule-forming element, and different calibrants were investigated and optimized. Chlorine concentrations in milk samples were determined in a Zr-coated graphite furnace using 25 μg of Sr as the molecule-forming reagent and applying a pyrolysis temperature of 600 °C and a molecule-forming temperature of 2300 °C. Linearity was maintained up to 500 μg mL(-1) of Cl. The method was tested by analyzing a certified reference wastewater. The results were in the uncertainty limits of the certified value. The limit of detection of the method was 1.76 μg mL(-1). The chlorine concentrations in various cow milk samples taken from the market were found in the range of 588-1472 mg L(-1).

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

PubMed

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.

Oxidation State Specific Generation of Arsines from Methylated Arsenicals Based on L- Cysteine Treatment in Buffered Media for Speciation Analysis by Hydride Generation - Automated Cryotrapping - Gas Chromatography-Atomic Absorption Spectrometry with the Multiatomizer

PubMed Central

Matoušek, Tomáš; Hernández-Zavala, Araceli; Svoboda, Milan; Langrová, Lenka; Adair, Blakely M.; Drobná, Zuzana; Thomas, David J.; Stýblo, Miroslav; Dědina, Jiří

2008-01-01

An automated system for hydride generation - cryotrapping- gas chromatography - atomic absorption spectrometry with the multiatomizer is described. Arsines are preconcentrated and separated in a Chromosorb filled U-tube. An automated cryotrapping unit, employing nitrogen gas formed upon heating in the detection phase for the displacement of the cooling liquid nitrogen, has been developed. The conditions for separation of arsines in a Chromosorb filled U-tube have been optimized. A complete separation of signals from arsine, methylarsine, dimethylarsine, and trimethylarsine has been achieved within a 60 s reading window. The limits of detection for methylated arsenicals tested were 4 ng l−1. Selective hydride generation is applied for the oxidation state specific speciation analysis of inorganic and methylated arsenicals. The arsines are generated either exclusively from trivalent or from both tri- and pentavalent inorganic and methylated arsenicals depending on the presence of L-cysteine as a prereductant and/or reaction modifier. A TRIS buffer reaction medium is proposed to overcome narrow optimum concentration range observed for the L-cysteine modified reaction in HCl medium. The system provides uniform peak area sensitivity for all As species. Consequently, the calibration with a single form of As is possible. This method permits a high-throughput speciation analysis of metabolites of inorganic arsenic in relatively complex biological matrices such as cell culture systems without sample pretreatment, thus preserving the distribution of tri- and pentavalent species. PMID:18521190

Imaging-based molecular barcoding with pixelated dielectric metasurfaces.

PubMed

Tittl, Andreas; Leitis, Aleksandrs; Liu, Mingkai; Yesilkoy, Filiz; Choi, Duk-Yong; Neshev, Dragomir N; Kivshar, Yuri S; Altug, Hatice

2018-06-08

Metasurfaces provide opportunities for wavefront control, flat optics, and subwavelength light focusing. We developed an imaging-based nanophotonic method for detecting mid-infrared molecular fingerprints and implemented it for the chemical identification and compositional analysis of surface-bound analytes. Our technique features a two-dimensional pixelated dielectric metasurface with a range of ultrasharp resonances, each tuned to a discrete frequency; this enables molecular absorption signatures to be read out at multiple spectral points, and the resulting information is then translated into a barcode-like spatial absorption map for imaging. The signatures of biological, polymer, and pesticide molecules can be detected with high sensitivity, covering applications such as biosensing and environmental monitoring. Our chemically specific technique can resolve absorption fingerprints without the need for spectrometry, frequency scanning, or moving mechanical parts, thereby paving the way toward sensitive and versatile miniaturized mid-infrared spectroscopy devices. Copyright © 2018 The Authors, some rights reserved; exclusive licensee American Association for the Advancement of Science. No claim to original U.S. Government Works.

Statistical modelling coupled with LC-MS analysis to predict human upper intestinal absorption of phytochemical mixtures.

PubMed

Selby-Pham, Sophie N B; Howell, Kate S; Dunshea, Frank R; Ludbey, Joel; Lutz, Adrian; Bennett, Louise

2018-04-15

A diet rich in phytochemicals confers benefits for health by reducing the risk of chronic diseases via regulation of oxidative stress and inflammation (OSI). For optimal protective bio-efficacy, the time required for phytochemicals and their metabolites to reach maximal plasma concentrations (T max ) should be synchronised with the time of increased OSI. A statistical model has been reported to predict T max of individual phytochemicals based on molecular mass and lipophilicity. We report the application of the model for predicting the absorption profile of an uncharacterised phytochemical mixture, herein referred to as the 'functional fingerprint'. First, chemical profiles of phytochemical extracts were acquired using liquid chromatography mass spectrometry (LC-MS), then the molecular features for respective components were used to predict their plasma absorption maximum, based on molecular mass and lipophilicity. This method of 'functional fingerprinting' of plant extracts represents a novel tool for understanding and optimising the health efficacy of plant extracts. Copyright © 2017 Elsevier Ltd. All rights reserved.

Optical Measurement of Radiocarbon below Unity Fraction Modern by Linear Absorption Spectroscopy.

PubMed

Fleisher, Adam J; Long, David A; Liu, Qingnan; Gameson, Lyn; Hodges, Joseph T

2017-09-21

High-precision measurements of radiocarbon ( 14 C) near or below a fraction modern 14 C of 1 (F 14 C ≤ 1) are challenging and costly. An accurate, ultrasensitive linear absorption approach to detecting 14 C would provide a simple and robust benchtop alternative to off-site accelerator mass spectrometry facilities. Here we report the quantitative measurement of 14 C in gas-phase samples of CO 2 with F 14 C < 1 using cavity ring-down spectroscopy in the linear absorption regime. Repeated analysis of CO 2 derived from the combustion of either biogenic or petrogenic sources revealed a robust ability to differentiate samples with F 14 C < 1. With a combined uncertainty of 14 C/ 12 C = 130 fmol/mol (F 14 C = 0.11), initial performance of the calibration-free instrument is sufficient to investigate a variety of applications in radiocarbon measurement science including the study of biofuels and bioplastics, illicitly traded specimens, bomb dating, and atmospheric transport.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of chromium in water by graphite furnace atomic absorption spectrophotometry

USGS Publications Warehouse

McLain, B.J.

1993-01-01

Graphite furnace atomic absorption spectrophotometry is a sensitive, precise, and accurate method for the determination of chromium in natural water samples. The detection limit for this analytical method is 0.4 microg/L with a working linear limit of 25.0 microg/L. The precision at the detection limit ranges from 20 to 57 percent relative standard deviation (RSD) with an improvement to 4.6 percent RSD for concentrations more than 3 microg/L. Accuracy of this method was determined for a variety of reference standards that was representative of the analytical range. The results were within the established standard deviations. Samples were spiked with known concentrations of chromium with recoveries ranging from 84 to 122 percent. In addition, a comparison of data between graphite furnace atomic absorption spectrophotometry and direct-current plasma atomic emission spectrometry resulted in suitable agreement between the two methods, with an average deviation of +/- 2.0 microg/L throughout the analytical range.

The use of mosses as environmental metal pollution indicators.

PubMed

Aceto, Maurizio; Abollino, Ornella; Conca, Raffaele; Malandrino, Mery; Mentasti, Edoardo; Sarzanini, Corrado

2003-01-01

The possibility of using mosses as environmental indicators of metal pollution has been investigated. Mosses of the species Bryum argenteum were collected from different parts of Piedmont (Italy), ranging from highly polluted areas to nearly uncontaminated mountain areas. Periodical samplings were planned in every site on a monthly base, in order to check variations of metal uptake throughout one year; correlations with pluviometric and thermal patterns were investigated for all sampling stations. On every moss sample 20 elements, ranging from major (K, P, Al, Ca, Fe and Mg) to minor (Mn, Na, Ti and Zn) and trace (As, Ba, Cd, Co, Cr, Cu, Li, Ni, Pb and Sr), were quantitatively determined by inductively coupled plasma-atomic emission spectrometry or graphite furnace-atomic absorption spectrometry, depending on the needed sensitivity. Statistical analyses, carried out with principal component analysis and cluster analysis methods, revealed that a good correlation exists between metal content in mosses and pollution degree in the areas sampled.

The measurement of acetanilide in plasma by spectrophotometric and selected ion monitoring methods.

PubMed

Baty, J D; Playfer, J; Evans, D A; Lamb, J

1977-08-01

Plasma samples from volunteers who had received an oral dose of acetanilide have been analysed by gas chromatography mass spectrometry and ultraviolet absorption techniques. The gas chromatography mass spectrometry method involved extraction of the plasma and analysis of the acetanilide using selected ion monitoring with a deuterated internal standard. In the ultraviolet method the plasma was hydrolysed with acid to convert the acetanilide to aniline, and this compound was diazotized and coupled with N-1-naphthylethylene-diamine. The absorbance of the resulting complex was read at 550 nm. Acetanilide levels in plasma determined by the selected ion monitoring method were significantly lower than those measured by spectrophotometry. Pharmacokinetic data calculated from the results obtained using these two assays are very different and illustrate the need for an accurate and specific method of analysis. The major metabolites of acetanilide are shown not to interfere with these assays and the results suggest the possible presence of a new metabolite of acetanilide.

Sulfur determination in coal using molecular absorption in graphite filter vaporizer.

PubMed

Jim, Gibson; Katskov, Dmitri; Tittarelli, Paolo

2011-02-15

The vaporization of sulfur containing samples in graphite vaporizers for atomic absorption spectrometry is accompanied by modification of sulfur by carbon and, respectively, appearance at high temperature of structured molecular absorption in 200-210 nm wavelength range. It has been proposed to employ the spectrum for direct determination of sulfur in coal; soundness of the suggestion is evaluated by analysis of coal slurry using low resolution CCD spectrometer with continuum light source coupled to platform or filter furnace vaporizers. For coal in platform furnace losses of the analyte at low temperature and strong spectral background from the coal matrix hinder the determination. Both negative effects are significantly reduced in filter furnace, in which sample vapor efficiently interacts with carbon when transferred through the heated graphite filter. The method is verified by analysis of coals with sulfur content within 0.13-1.5% (m/m) range. The use of coal certified reference material for sulfur analyte addition to coal slurry permitted determination with random error 5-12%. Absolute and relative detection limits for sulfur in coal are 0.16 μg and 0.02 mass%, respectively. Copyright © 2010 Elsevier B.V. All rights reserved.

Simultaneous determination of iron, cadmium, zinc, copper, nickel, lead, and uranium in seawater by stable isotope dilution spark source mass spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mykytiuk, A.P.; Russell, D.S.; Sturgeon, R.E.

Trace concentrations (ng/mL) of Fe, Cd, Zn, Cu, Ni, Pb, U, and Co have been determined in seawater by stable isotope dilution spark source mass spectrometry. The seawater samples were preconcentrated on the ion exchanger Chelex-100 and the concentrate was evaporated on a graphite or silver electrode. The results are compared with those obtained by graphite furnace atomic absorption spectrometry and inductively coupled plasma emission spectrometry. The technique avoids the use of calibration standards and is capable of producing results in cases where the analyte is only partially recovered. 2 tables.

Quantification of the fluorine containing drug 5-fluorouracil in cancer cells by GaF molecular absorption via high-resolution continuum source molecular absorption spectrometry

NASA Astrophysics Data System (ADS)

Krüger, Magnus; Huang, Mao-Dong; Becker-Roß, Helmut; Florek, Stefan; Ott, Ingo; Gust, Ronald

The development of high-resolution continuum source molecular absorption spectrometry made the quantification of fluorine feasible by measuring the molecular absorption as gallium monofluoride (GaF). Using this new technique, we developed on the example of 5-fluorouracil (5-FU) a graphite furnace method to quantify fluorine in organic molecules. The effect of 5-FU on the generation of the diatomic GaF molecule was investigated. The experimental conditions such as gallium nitrate amount, temperature program, interfering anions (represented as corresponding acids) and calibration for the determination of 5-FU in standard solution and in cellular matrix samples were investigated and optimized. The sample matrix showed no effect on the sensitivity of GaF molecular absorption. A simple calibration curve using an inorganic sodium fluoride solution can conveniently be used for the calibration. The described method is sensitive and the achievable limit of detection is 0.23 ng of 5-FU. In order to establish the concept of "fluorine as a probe in medicinal chemistry" an exemplary application was selected, in which the developed method was successfully demonstrated by performing cellular uptake studies of the 5-FU in human colon carcinoma cells.

Investigation of an alternating current plasma as an element selective atomic emission detector for high-resolution capillary gas chromatography and as a source for atomic absorption and atomic emission spectrometry

NASA Astrophysics Data System (ADS)

Ombaba, Jackson M.

This thesis deals with the construction and evaluation of an alternating current plasma (ACP) as an element-selective detector for high resolution capillary gas chromatography (GC) and as an excitation source for atomic absorption spectrometry (AAS) and atomic emission spectrometry (AES). The plasma, constrained in a quartz discharge tube at atmospheric pressure, is generated between two copper electrodes and utilizes helium as the plasma supporting gas. The alternating current plasma power source consists of a step-up transformer with a secondary output voltage of 14,000 V at a current of 23 mA. The device exhibits a stable signal because the plasma is self-seeding and reignites itself every half cycle. A tesla coil is not required to commence generation of the plasma if the ac voltage applied is greater than the breakdown voltage of the plasma-supporting gas. The chromatographic applications studied included the following: (1) the separation and selective detection of the organotin species, tributyltin chloride (TBT) and tetrabutyltin (TEBT), in environmental matrices including mussels (Mvutilus edullus) and sediment from Boston Harbor, industrial waste water and industrial sludge, and (2) the detection of methylcyclopentadienyl manganesetricarbonyl (MMT) and similar compounds used as gasoline additives. An ultrasonic nebulizer (common room humidifier) was utilized as a sample introduction device for aqueous solutions when the ACP was employed as an atomization source for atomic absorption spectrometry and as an excitation source for atomic emission spectrometry. Plasma diagnostic parameters studied include spatial electron number density across the discharge tube, electronic, excitation and ionization temperatures. Interference studies both in absorption and emission modes were also considered. Figures of merits of selected elements both in absorption and emission modes are reported. The evaluation of a computer-aided optimization program, Drylab GC, using spearmint oil and Environmental Protection Agency (EPA) standard mixture as probes is also discussed. The program supplied by LC Resources (Lafayette, CA) is used for separation optimization and prediction of gas chromatographic parameters. Column dead-time and average plate number were used as input data in conjunction with the retention times and peak areas of solutes at two different temperature programming rates. Once input data are entered into an IBM or IBM compatible personal computer, the program produces a 'relative resolution map' (RRM) which guides the analyst in selecting the most favorable temperature programming rate for the separation.

[Determination of Al, Be, Cd, Co, Cr, Mn, Ni, Pb, Se and Tl in whole blood by atomic absorption spectrometry without preliminary sample digestion].

PubMed

Ivanenko, N B; Ivanenko, A A; Solov'ev, N D; Navolotskiĭ, D V; Pavlova, O V; Ganeev, A A

2014-01-01

Methods of whole blood trace element determination by Graphite furnace atomic absorption spectrometry (in the variant of Zeeman's modulation polarization spectrometry) have been proposed. They do not require preliminary sample digestion. Furnace programs, modifiers and blood dilution factors were optimized. Seronorm™ human whole blood reference materials were used for validation. Dynamic ranges (for undiluted blood samples) were: Al 8 ¸ 210 мg/L; Be 0.3 ¸ 50 мg/L; Cd 0.2 ¸ 75 мg/L; Сo 5 ¸ 350 мg/L; Cr 10 ¸ 100 мg/L; Mn 6 ¸ 250 мg/L; Ni 10 ¸ 350 мg/L; Pb 3 ¸ 240 мg/L; Se 10 ¸ 500 мg/L; Tl 2 ¸ 600 мg/L. Precision (RSD) for the middle of dynamic range ranged from 5% for Mn to 11 for Se.

Tandem Mass Spectrometry for Structural Identification of Sesquiterpene Alkaloids from the Stems of Dendrobium nobile Using LC-QToF.

PubMed

Wang, Yan-Hong; Avula, Bharathi; Abe, Naohito; Wei, Feng; Wang, Mei; Ma, Shuang-Cheng; Ali, Zulfiqar; Elsohly, Mahmoud A; Khan, Ikhlas A

2016-05-01

Dendrobium nobile is one of the fundamental herbs in traditional Chinese medicine. Sesquiterpene alkaloids are the main active components in this plant. Due to weak ultraviolet absorption and low content in D. nobile, these sesquiterpene alkaloids have not been extensively studied using chromatographic methods. Herein, tandem mass spectrometry combined with liquid chromatography separation provides a tool for the identification and characterization of the alkaloids from D. nobile. A total of nine sesquiterpene alkaloids were characterized by ultrahigh-performance liquid chromatography tandem mass spectrometry. These alkaloids can be classified into two subgroups that are represented by dendrobine and nobilonine. Tandem mass spectrometric studies revealed the fragmentation pathways of these two subgroup alkaloids that were used for the identification and characterization of other alkaloids in D. nobile. Characterization of these alkaloids using accurate mass and diagnostic fragments provided a reliable methodology for the analysis of D. nobile by ultrahigh-performance liquid chromatography tandem mass spectrometry. The limit of detection was defined as the signal-to-noise ratio equal to 3 : 1. Limits of detection of dendrobine and nobilonine were less than 30 ng/mL. The developed method was applied for the analysis of various Dendrobium species and related dietary supplements. Alkaloids were identified from D. nobile, but not detected from commercial samples including 13 other Dendrobium species and the 7 dietary supplements. Georg Thieme Verlag KG Stuttgart · New York.

Piezoelectric-tuned microwave cavity for absorption spectrometry

DOEpatents

Leskovar, Branko; Buscher, Harold T.; Kolbe, William F.

1978-01-01

Gas samples are analyzed for pollutants in a microwave cavity that is provided with two highly polished walls. One wall of the cavity is mechanically driven with a piezoelectric transducer at a low frequency to tune the cavity over a band of microwave frequencies in synchronism with frequency modulated microwave energy applied to the cavity. Absorption of microwave energy over the tuned frequencies is detected, and energy absorption at a particular microwave frequency is an indication of a particular pollutant in the gas sample.

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

USGS Publications Warehouse

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

1967-01-01

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

Synchrotron Photoionization Mass Spectrometry Measurements of Kinetics and Product Formation in the Allyl Radical (H2CCHCH2)Self Reaction

NASA Technical Reports Server (NTRS)

Selby, Talitha M.; Melini, giovanni; Goulay, Fabien; Leone, Stephen R.; Fahr, Askar; Taatjes, Craig A.; Osborn, David L.

2008-01-01

Product channels for the self-reaction of the resonance-stabilized allyl radical, C3H5 + C3H5, have been studied with isomeric specificity at temperatures from 300-600 K and pressures from 1-6 Torr using time-resolved multiplexed photoionization mass spectrometry. Under these conditions 1,5-hexadiene was the only C6H10 product isomer detected. The lack of isomerization of the C6H10 product is in marked contrast to the C6H6 product in the related C3H3 + C3H3 reaction, and is due to the more saturated electronic structure of the C6H10 system. The disproportionation product channel, yielding allene + propene, was also detected, with an upper limit on the branching fraction relative to recombination of 0.03. Analysis of the allyl radical decay at 298 K yielded a total rate coefficient of (2.7 +/- 0.8) x 10(exp -11) cu cm/molecule/s, in good agreement with pre.vious experimental measurements using ultraviolet kinetic absorption spectroscopy and a recent theoretical determination using variable reaction coordinate transition state theory. This result provides independent indirect support for the literature value of the allyl radical ultraviolet absorption cross-section near 223 nm.

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

PubMed

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.

Magnetic stirrer induced dispersive ionic-liquid microextraction for the determination of vanadium in water and food samples prior to graphite furnace atomic absorption spectrometry.

PubMed

Naeemullah; Kazi, Tasneem Gul; Tuzen, Mustafa

2015-04-01

A new dispersive liquid-liquid microextraction, magnetic stirrer induced dispersive ionic-liquid microextraction (MS-IL-DLLME) was developed to quantify the trace level of vanadium in real water and food samples by graphite furnace atomic absorption spectrometry (GFAAS). In this extraction method magnetic stirrer was applied to obtained a dispersive medium of 1-butyl-3-methylimidazolium hexafluorophosphate [C4MIM][PF6] in aqueous solution of (real water samples and digested food samples) to increase phase transfer ratio, which significantly enhance the recovery of vanadium - 4-(2-pyridylazo) resorcinol (PAR) chelate. Variables having vital role on desired microextraction methods were optimised to obtain the maximum recovery of study analyte. Under the optimised experimental variables, enhancement factor (EF) and limit of detection (LOD) were achieved to be 125 and 18 ng L(-1), respectively. Validity and accuracy of the desired method was checked by analysis of certified reference materials (SLRS-4 Riverine water and NIST SRM 1515 Apple leaves). The relative standard deviation (RSD) for 10 replicate determinations at 0.5 μg L(-1) of vanadium level was found to be <5.0%. This method was successfully applied to real water and acid digested food samples. Copyright © 2014 Elsevier Ltd. All rights reserved.

Investigation of chemical modifiers for the direct determination of arsenic in fish oil using high-resolution continuum source graphite furnace atomic absorption spectrometry.

PubMed

Pereira, Éderson R; de Almeida, Tarcísio S; Borges, Daniel L G; Carasek, Eduardo; Welz, Bernhard; Feldmann, Jörg; Campo Menoyo, Javier Del

2016-04-01

High-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS) has been applied for the development of a method for the determination of total As in fish oil samples using direct analysis. The method does not use any sample pretreatment, besides dilution with 1-propanole, in order to decrease the oil viscosity. The stability and sensitivity of As were evaluated using ruthenium and iridium as permanent chemical modifiers and palladium added in solution over the sample. The best results were obtained with ruthenium as the permanent modifier and palladium in solution added to samples and standard solutions. Under these conditions, aqueous standard solutions could be used for calibration for the fish oil samples diluted with 1-propanole. The pyrolysis and atomization temperatures were 1400 °C and 2300 °C, respectively, and the limit of detection and characteristic mass were 30 pg and 43 pg, respectively. Accuracy and precision of the method have been evaluated using microwave-assisted acid digestion of the samples with subsequent determination by HR-CS GF AAS and ICP-MS; the results were in agreement (95% confidence level) with those of the proposed method. Copyright © 2015 Elsevier B.V. All rights reserved.

Determination of trace nickel in hydrogenated cottonseed oil by electrothermal atomic absorption spectrometry after microwave-assisted digestion.

PubMed

Zhang, Gai

2012-01-01

Microwave digestion of hydrogenated cottonseed oil prior to trace nickel determination by electrothermal atomic absorption spectrometry (ETAAS) is proposed here for the first time. Currently, the methods outlined in U.S. Pharmacopeia 28 (USP28) or British Pharmacopeia (BP2003) are recommended as the official methods for analyzing nickel in hydrogenated cottonseed oil. With these methods the samples may be pre-treated by a silica or a platinum crucible. However, the samples were easily tarnished during sample pretreatment when using a silica crucible. In contrast, when using a platinum crucible, hydrogenated cottonseed oil acting as a reducing material may react with the platinum and destroy the crucible. The proposed microwave-assisted digestion avoided tarnishing of sample in the process of sample pretreatment and also reduced the cycle of analysis. The programs of microwave digestion and the parameters of ETAAS were optimized. The accuracy of the proposed method was investigated by analyzing real samples. The results were compared with the ones by pressurized-PTFE-bomb acid digestion and ones obtained by the U.S. Pharmacopeia 28 (USP28) method. The new method involves a relatively rapid matrix destruction technique compared with other present methods for the quantification of metals in oil. © 2011 Institute of Food Technologists®

Optimization of electrothermal atomization parameters for simultaneous multielement atomic absorption spectrometry

USGS Publications Warehouse

Harnly, J.M.; Kane, J.S.

1984-01-01

The effect of the acid matrix, the measurement mode (height or area), the atomizer surface (unpyrolyzed and pyrolyzed graphite), the atomization mode (from the wall or from a platform), and the atomization temperature on the simultaneous electrothermal atomization of Co, Cr, Cu, Fe, Mn, Mo, Ni, V, and Zn was examined. The 5% HNO3 matrix gave rise to severe irreproducibility using a pyrolyzed tube unless the tube was properly "prepared". The 5% HCl matrix did not exhibit this problem, and no problems were observed with either matrix using an unpyrolized tube or a pyrolyzed platform. The 5% HCl matrix gave better sensitivities with a pyrolyzed tube but the two matrices were comparable for atomization from a platform. If Mo and V are to be analyzed with the other seven elements, a high atomization temperature (2700??C or greater) is necessary regardless of the matrix, the measurement mode, the atomization mode, or the atomizer surface. Simultaneous detection limits (peak height with pyrolyzed tube atomization) were comparable to those of conventional atomic absorption spectrometry using electrothermal atomization above 280 nm. Accuracies and precisions of ??10-15% were found in the 10 to 120 ng mL-1 range for the analysis of NBS acidified water standards.

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

PubMed

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.

Blood-collection device for trace and ultra-trace metal specimens evaluated.

PubMed

Moyer, T P; Mussmann, G V; Nixon, D E

1991-05-01

We evaluated the evacuated phlebotomy tube designed specifically for trace metal analysis by Sherwood Medical Co. Pools of human serum containing known concentrations of aluminum, arsenic, calcium, cadmium, copper, chromium, iron, lead, magnesium, manganese, mercury, selenium, and zinc were exposed to the tube and rubber stopper for defined periods ranging from 5 min to 24 h. Analysis for each element was performed in a randomized fashion under rigidly controlled conditions by use of standard electrothermal atomization atomic absorption spectroscopy, inductively coupled plasma atomic emission spectroscopy, and cold vapor atomic absorption spectrometry. In addition, for comparative purposes, we collected blood samples from normal volunteers by use of ultra-clean polystyrene phlebotomy syringes as well as standard evacuated phlebotomy tubes. We conclude that, except for lead, there was no significant contribution of any trace element studied from the evaluated tube and stopper to the serum. Because whole blood is the usual specimen for lead testing, the observation of a trace amount of lead in this tube designed for serum collection is trivial.

Simulation of UV atomic radiation for application in exhaust plume spectrometry

NASA Astrophysics Data System (ADS)

Wallace, T. L.; Powers, W. T.; Cooper, A. E.

1993-06-01

Quantitative analysis of exhaust plume spectral data has long been a goal of developers of advanced engine health monitoring systems which incorporate optical measurements of rocket exhaust constituents. Discussed herein is the status of present efforts to model and predict atomic radiation spectra and infer free-atom densities from emission/absorption measurements as part of the Optical Plume Anomaly Detection (OPAD) program at Marshall Space Flight Center (MSFC). A brief examination of the mathematical formalism is provided in the context of predicting radiation from the Mach disk region of the SSME exhaust flow at nominal conditions during ground level testing at MSFC. Computational results are provided for Chromium and Copper at selected transitions which indicate a strong dependence upon broadening parameter values determining the absorption-emission line shape. Representative plots of recent spectral data from the Stennis Space Center (SSC) Diagnostic Test Facility (DTF) rocket engine are presented and compared to numerical results from the present self-absorbing model; a comprehensive quantitative analysis will be reported at a later date.

Synthesis, crystal structure, photophysical properties and theoretical studies of a novel bis(phenylisoxazolyl) benzene derivative

NASA Astrophysics Data System (ADS)

de Brito, A. C. F.; Correa, R. S.; Pinto, A. A.; Matos, M. J. S.; Tenorio, J. C.; Taylor, J. G.; Cazati, T.

2018-07-01

Isoxazoles have well established biological activities but, have been underexplored as synthetic intermediates for applications in materials science. The aims of this work are to synthesis a novel isoxazole and analyze its structural and photophysical properties for application in electronic organic materials. The novel bis (phenylisoxazolyl) benzene compound was synthesized in four steps and characterized by NMR, high resolution mass spectrometry, differential thermal analysis, infrared spectroscopy, cyclic voltammetry, ultraviolet-visible spectroscopy, fluorescence spectroscopy, DFT and TDDFT calculations. The molecule presented optical absorption in the ultraviolet region (from 290 nm to 330 nm), with maximum absorption length centered at 306 nm. The molar extinction coefficients (ε), fluorescence emission spectra and quantum efficiencies in chloroform and dimethylformamide solution were determined. Cyclic voltammetry analysis was carried out for estimating the HOMO energy level and these properties make it desirable material for photovoltaic device applications. Finally, the excited-state properties of present compound were calculated by time-dependent density functional theory (TDDFT).

Lead screening in DBS by solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry: application to newborns and pregnant women.

PubMed

Rello, Luis; Aramendía, Maite; Belarra, Miguel A; Resano, Martín

2015-01-01

DBS have become a clinical specimen especially adequate for establishing home-based collection protocols. In this work, high-resolution continuum source graphite furnace atomic absorption spectrometry is evaluated for the direct monitoring of Pb in DBS, both as a quantitative tool and a screening method. The development of the screening model is based on the establishment of the unreliability region around the threshold limits, 100 or 50 μg l(-1). More than 500 samples were analyzed to validate the model. The screening method demonstrated high sensitivity (the rate of true positives detected was always higher than 95%), an excellent LOD (1 µg l(-1)) and high throughput (10 min per sample).

Water dynamics of Ser-His-Glu-Cys-Asn powder and effects of moisture absorption on its chemical properties.

PubMed

Lin, Songyi; Xue, Peiyu; Yang, Shuailing; Li, Xingfang; Dong, Xiuping; Chen, Feng

2017-08-01

This study has elucidated moisture dynamics in the soybean peptide, Ser-His-Glu-Cys-Asn (SHECN) powder by using dynamic vapor sorption (DVS) and nuclear magnetic resonance (NMR). We also tried to investigate the effects of moisture absorption on the biological activity and chemical properties of SHECN with some effective methods such as mid-infrared (MIR) spectroscopy and gas chromatography-mass spectrometry (GC-MS). DVS results showed that the moisture absorption of SHECN could reach a maximum of 33%, and the SHECN powder after synthesis actually existed in a trihydrate state of SHECN.3H 2 O. Low-field NMR revealed that three water proportions including strong combined water, binding water and bulk water were involved in SHECN moisture absorption and absored water dominantly existed in the form of combined water. Magnetic resonance imaging (MRI) and MIR spectroscopy results indicated that moisture absorption could change the morphology and structure of SHECN. After moisture absorption at 50% and 75% relative humidity, 19 volatiles were identified by GC-MS analysis. Additionally, this study showed that a part of reductive groups in SHECN was oxidized and its antioxidant ability declined significantly (P < 0.05) after moisture absorption. Water absorbed into SHECN powder can significantly change its microstructure and cause its activity to decrease. We must prevent SHECN from absorbing moisture during storage because the water can accelerate the oxidation of samples and promote microbial reactions. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

A standards-based method for compositional analysis by energy dispersive X-ray spectrometry using multivariate statistical analysis: application to multicomponent alloys.

PubMed

Rathi, Monika; Ahrenkiel, S P; Carapella, J J; Wanlass, M W

2013-02-01

Given an unknown multicomponent alloy, and a set of standard compounds or alloys of known composition, can one improve upon popular standards-based methods for energy dispersive X-ray (EDX) spectrometry to quantify the elemental composition of the unknown specimen? A method is presented here for determining elemental composition of alloys using transmission electron microscopy-based EDX with appropriate standards. The method begins with a discrete set of related reference standards of known composition, applies multivariate statistical analysis to those spectra, and evaluates the compositions with a linear matrix algebra method to relate the spectra to elemental composition. By using associated standards, only limited assumptions about the physical origins of the EDX spectra are needed. Spectral absorption corrections can be performed by providing an estimate of the foil thickness of one or more reference standards. The technique was applied to III-V multicomponent alloy thin films: composition and foil thickness were determined for various III-V alloys. The results were then validated by comparing with X-ray diffraction and photoluminescence analysis, demonstrating accuracy of approximately 1% in atomic fraction.

Continuous Flow Atmospheric Pressure Laser Desorption/Ionization Using a 6–7-µm-Band Mid-Infrared Tunable Laser for Biomolecular Mass Spectrometry

PubMed Central

Hiraguchi, Ryuji; Hazama, Hisanao; Senoo, Kenichirou; Yahata, Yukinori; Masuda, Katsuyoshi; Awazu, Kunio

2014-01-01

A continuous flow atmospheric pressure laser desorption/ionization technique using a porous stainless steel probe and a 6–7-µm-band mid-infrared tunable laser was developed. This ion source is capable of direct ionization from a continuous flow with a high temporal stability. The 6–7-µm wavelength region corresponds to the characteristic absorption bands of various molecular vibration modes, including O–H, C=O, CH3 and C–N bonds. Consequently, many organic compounds and solvents, including water, have characteristic absorption peaks in this region. This ion source requires no additional matrix, and utilizes water or acetonitrile as the solvent matrix at several absorption peak wavelengths (6.05 and 7.27 µm, respectively). The distribution of multiply-charged peptide ions is extremely sensitive to the temperature of the heated capillary, which is the inlet of the mass spectrometer. This ionization technique has potential for the interface of liquid chromatography/mass spectrometry (LC/MS). PMID:24937686

Determination of mercury in fish tissue using a minianalyzer based on cold vapor atomic absorption spectrometry at the 184.9 nm line.

PubMed

Rizea, Maria-Cristina; Bratu, Maria-Cristina; Danet, Andrei Florin; Bratu, Adrian

2007-09-01

A sensitive method was proposed and optimized for the determination of total mercury in fish tissue by using wet digestion, followed by cold vapor atomic absorption spectrometry (CVAAS) at the main resonance line of mercury (184.9 nm). The measurements were made using a new type of a non-dispersive mercury minianalyzer. This instrument was initially designed and built for atmospheric mercury-vapor detection. For determining mercury in aqueous samples, the minianalyzer was linked with a mercury/hydride system, Perkin Elmer Model MHS-10. To check the method, the analyzed samples were spiked with a standard solution of mercury. The recoveries of mercury spiked to wet fish tissue were >90% for 0.5 - 0.8 g samples. The results showed a better sensitivity (about 2.5 times higher) when using the mercury absorption line at 184.9 nm compared with the sensitivity obtained by conventional CVAAS at 253.7 nm.

Secondary organic aerosol from atmospheric photooxidation of indole

NASA Astrophysics Data System (ADS)

Montoya-Aguilera, Julia; Horne, Jeremy R.; Hinks, Mallory L.; Fleming, Lauren T.; Perraud, Véronique; Lin, Peng; Laskin, Alexander; Laskin, Julia; Dabdub, Donald; Nizkorodov, Sergey A.

2017-09-01

Indole is a heterocyclic compound emitted by various plant species under stressed conditions or during flowering events. The formation, optical properties, and chemical composition of secondary organic aerosol (SOA) formed by low-NOx photooxidation of indole were investigated. The SOA yield (1. 3 ± 0. 3) was estimated from measuring the particle mass concentration with a scanning mobility particle sizer (SMPS) and correcting it for wall loss effects. The high value of the SOA mass yield suggests that most oxidized indole products eventually end up in the particle phase. The SOA particles were collected on filters and analysed offline with UV-vis spectrophotometry to measure the mass absorption coefficient (MAC) of the bulk sample. The samples were visibly brown and had MAC values of ˜ 2 m2 g-1 at λ = 300 nm and ˜ 0. 5 m2 g-1 at λ = 400 nm, comparable to strongly absorbing brown carbon emitted from biomass burning. The chemical composition of SOA was examined with several mass spectrometry methods. Direct analysis in real-time mass spectrometry (DART-MS) and nanospray desorption electrospray high-resolution mass spectrometry (nano-DESI-HRMS) were both used to provide information about the overall distribution of SOA compounds. High-performance liquid chromatography, coupled to photodiode array spectrophotometry and high-resolution mass spectrometry (HPLC-PDA-HRMS), was used to identify chromophoric compounds that are responsible for the brown colour of SOA. Indole derivatives, such as tryptanthrin, indirubin, indigo dye, and indoxyl red, were found to contribute significantly to the visible absorption spectrum of indole SOA. The potential effect of indole SOA on air quality was explored with an airshed model, which found elevated concentrations of indole SOA during the afternoon hours contributing considerably to the total organic aerosol under selected scenarios. Because of its high MAC values, indole SOA can contribute to decreased visibility and poor air quality.

Final report on CCQM-K125: elements in infant formula

NASA Astrophysics Data System (ADS)

Merrick, J.; Saxby, D.; Dutra, E. S.; Sena, R. C.; Araújo, T. O.; Almeida, M. D.; Yang, L.; Pihillagawa, I. G.; Mester, Z.; Sandoval, S.; Wei, C.; Castillo, M. E. D.; Oster, C.; Fisicaro, P.; Rienitz, O.; Pape, C.; Schulz, U.; Jährling, R.; Görlitz, V.; Lampi, E.; Kakoulides, E.; Sin, D. W. M.; Yip, Y. C.; Tsoi, Y. T.; Zhu, Y.; Okumu, T. O.; Yim, Y. H.; Heo, S. W.; Han, M.; Lim, Y.; Osuna, M. A.; Regalado, L.; Uribe, C.; Buzoianu, M. M.; Duta, S.; Konopelko, L.; Krylov, A.; Shin, R.; Linsky, M.; Botha, A.; Magnusson, B.; Haraldsson, C.; Thiengmanee, U.; Klich, H.; Can, S. Z.; Coskun, F. G.; Tunc, M.; Entwisle, J.; O'Reilly, J.; Hill, S.; Goenaga-Infante, H.; Winchester, M.; Rabb, S. A.; Pérez, R.

2017-01-01

CCQM-K125 was organized by the Inorganic Analysis Working Group (IAWG) of CCQM to assess and document the capabilities of the national metrology institutes (NMIs) or the designated institutes (DIs) to measure the mass fractions of trace elements (K, Cu and I) in infant formula. Government Laboratory, Hong Kong SAR (GLHK) acted as the coordinating laboratory. In CCQM-K125, 25 institutes submitted the results for potassium, 24 institutes submitted the results for copper and 8 institutes submitted the results for iodine. For examination of potassium and copper, most of the participants used microwave-assisted acid digestion methods for sample dissolution. A variety of instrumental techniques including inductively coupled plasma mass spectrometry (ICP-MS), isotope dilution inductively coupled plasma mass spectrometry (ID-ICP-MS), inductively coupled plasma optical emission spectrometry (ICP-OES), atomic absorption spectrometry (AAS), flame atomic emission spectrometry (FAES) and microwave plasma atomic emission spectroscopy (MP-AES) were employed by the participants for determination. For analysis of iodine, most of the participants used alkaline extraction methods for sample preparation. ICP-MS and ID-ICP-MS were used by the participants for the determination. Generally, the participants' results of CCQM-K125 were found consistent for all measurands according to their equivalence statements. Except with some extreme values, most of the participants obtained the values of di/U(di) within +/- 1 for the measurands. Main text To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).

Major- and Trace-Element Concentrations in Rock Samples Collected in 2005 from the Taylor Mountains 1:250,000-scale Quadrangle, Alaska

USGS Publications Warehouse

Klimasauskas, Edward P.; Miller, Marti L.; Bradley, Dwight C.; Bundtzen, Tom K.; Hudson, Travis L.

2006-01-01

The data consist of major- and minor-element concentrations for rock samples collected during 2005 by the U.S. Geological Survey. Samples were analyzed by fire assay (Au, Pd, Pt), cold vapor atomic absorption spectroscopy (Hg), and the inductively coupled plasma mass spectrometry (ICPMS) 10 and 42 element methods. For details of sample preparation and analytical techniques see USGS Open File Report 02-0223 (Analytical methods for chemical analysis of geologic and other materials, U.S. Geological Survey), available at .

Determination of copper and mercury in phosphate fertilizers employing direct solid sampling analysis and high resolution continuum source graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

de Oliveira Souza, Sidnei; François, Luciane Luiza; Borges, Aline Rocha; Vale, Maria Goreti Rodrigues; Araujo, Rennan Geovanny Oliveira

2015-12-01

The present study proposes the determination of copper and mercury in phosphate fertilizers by direct solid sampling analysis (SS) employing high resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS). For Cu determination, two analytical lines were used: 327.3960 nm and 249.2146 nm. Hg determination was carried out on the line 253.6521 nm and 100 μg KMnO4 was used as chemical modifier. The optimal pyrolysis temperature for Cu determination was 1300 °C. Atomization temperatures for Cu and Hg were 2400 and 1100 °C, respectively. External calibration with aqueous standard solutions was adopted for both elements. The limits of quantification (LoQs) and characteristic mass (m0) obtained for Cu determination were 0.4 μg g- 1 and 1.12 ng, respectively, on line 249.2146 nm, and 64 μg g- 1 and 25 pg on 327.3960 nm. For mercury, LoQ and m0 were 4.8 ng g- 1 and 39 pg, respectively. The accuracy of the proposed methods was confirmed by the analysis of standard reference material (SRM) of Trace Elements in Multi-Nutrient Fertilizer (SRM NIST 695). The precision expressed as relative standard deviation (RSD), was better than 8.2% for Hg and 7.7% for the Cu (n = 5), considered satisfactory for microanalysis in solid sample. Four fertilizer samples acquired in commercial establishments in the city of Salvador, Bahia, Brazil, were analyzed. The optimized analytical methods were simple, fast, accurate, precise and free of spectral interferences for the determination of Cu and Hg in phosphate fertilizer samples by SS-HR-CS GF AAS, avoiding the dissolution of the sample, the use of harmful reagents and the generation of residues.

Determination of palladium, platinum and rhodium in used automobile catalysts and active pharmaceutical ingredients using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sample analysis

NASA Astrophysics Data System (ADS)

Resano, Martín; Flórez, María del Rosario; Queralt, Ignasi; Marguí, Eva

2015-03-01

This work investigates the potential of high-resolution continuum source graphite furnace atomic absorption spectrometry for the direct determination of Pd, Pt and Rh in two samples of very different nature. While analysis of active pharmaceutical ingredients is straightforward and it is feasible to minimize matrix effects, to the point that calibration can be carried out against aqueous standard solutions, the analysis of used automobile catalysts is more challenging requiring the addition of a chemical modifier (NH4F·HF) to help in releasing the analytes, a more vigorous temperature program and the use of a solid standard (CRM ERM®-EB504) for calibration. However, in both cases it was possible to obtain accurate results and precision values typically better than 10% RSD in a fast and simple way, while only two determinations are needed for the three analytes, since Pt and Rh can be simultaneously monitored in both types of samples. Overall, the methods proposed seem suited for the determination of these analytes in such types of samples, offering a greener and faster alternative that circumvents the traditional problems associated with sample digestion, requiring a small amount of sample only (0.05 mg per replicate for catalysts, and a few milligrams for the pharmaceuticals) and providing sufficient sensitivity to easily comply with regulations. The LODs achieved were 6.5 μg g- 1 (Pd), 8.3 μg g- 1 (Pt) and 9.3 μg g- 1 (Rh) for catalysts, which decreased to 0.08 μg g- 1 (Pd), 0.15 μg g- 1 (Pt) and 0.10 μg g- 1 (Rh) for pharmaceuticals.

Investigating effects of sample pretreatment on protein stability using size-exclusion chromatography and high-resolution continuum source atomic absorption spectrometry.

PubMed

Rakow, Tobias; El Deeb, Sami; Hahne, Thomas; El-Hady, Deia Abd; AlBishri, Hassan M; Wätzig, Hermann

2014-09-01

In this study, size-exclusion chromatography and high-resolution atomic absorption spectrometry methods have been developed and evaluated to test the stability of proteins during sample pretreatment. This especially includes different storage conditions but also adsorption before or even during the chromatographic process. For the development of the size exclusion method, a Biosep S3000 5 μm column was used for investigating a series of representative model proteins, namely bovine serum albumin, ovalbumin, monoclonal immunoglobulin G antibody, and myoglobin. Ambient temperature storage was found to be harmful to all model proteins, whereas short-term storage up to 14 days could be done in an ordinary refrigerator. Freezing the protein solutions was always complicated and had to be evaluated for each protein in the corresponding solvent. To keep the proteins in their native state a gentle freezing temperature should be chosen, hence liquid nitrogen should be avoided. Furthermore, a high-resolution continuum source atomic absorption spectrometry method was developed to observe the adsorption of proteins on container material and chromatographic columns. Adsorption to any container led to a sample loss and lowered the recovery rates. During the pretreatment and high-performance size-exclusion chromatography, adsorption caused sample losses of up to 33%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Solid sampling determination of magnesium in lithium niobate crystals by graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Dravecz, Gabriella; Laczai, Nikoletta; Hajdara, Ivett; Bencs, László

2016-12-01

The vaporization/atomization processes of Mg in high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS-GFAAS) were investigated by evaporating solid (powder) samples of lithium niobate (LiNbO3) optical single crystals doped with various amounts of Mg in a transversally heated graphite atomizer (THGA). Optimal analytical conditions were attained by using the Mg I 215.4353 nm secondary spectral line. An optimal pyrolysis temperature of 1500 °C was found for Mg, while the compromise atomization temperature in THGAs (2400 °C) was applied for analyte vaporization. The calibration was performed against solid (powered) lithium niobate crystal standards. The standards were prepared with exactly known Mg content via solid state fusion of the oxide components of the matrix and analyte. The correlation coefficient (R value) of the linear calibration was not worse than 0.9992. The calibration curves were linear in the dopant concentration range of interest (0.74-7.25 mg/g Mg), when dosing 3-10 mg of the powder samples into the graphite sample insertion boats. The Mg content of the studied 19 samples was in the range of 1.69-4.13 mg/g. The precision of the method was better than 6.3%. The accuracy of the results was verified by means of flame atomic absorption spectrometry with solution sample introduction after digestion of several crystal samples.

Les fards rouges cosmétiques et rituels a base de cinabre et d'ocre de l'époque punique en Tunisie: analyse, identification et caractérisation.

PubMed

Alatrache, A; Mahjoub, H; Ayed, N; Ben Younes, H

2001-10-01

Natural antique colorants include mainly red pigments such as cinnabar and ochre. These archeological pigments were used especially as funeral and cosmetic makeup and are a material proof of handicraft activities and exchanges. The identification and characterization of a group of punic colorants, corresponding to samples discovered during excavations at several Tunisian archeological sites (Cartage, Ksour Essef, Kerkouane, Bekalta, Makthar, Bou Arada), were conducted using the least destructive analysis techniques such us scanning electron microscopy coupled to X-ray fluorescence microprobe, direct current plasma emission spectroscopy, atomic absorption spectrometry, Fourier transform infrared spectrometry and X-ray diffraction. Eleven natural red colorants from punic period were subject to this investigation and were compared to contemporary substances. Five colorants were cinnabar and the other six were ochre.

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

NASA Astrophysics Data System (ADS)

Zambrzycka, Elżbieta; Godlewska-Żyłkiewicz, Beata

2014-11-01

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

A simple heat-pipe cell for X-ray absorption spectrometry of potassium vapor

NASA Astrophysics Data System (ADS)

Pres̆eren, R.; Kodre, A.; Arc̆on, I.; Padez̆nik Gomils̆ek, J.; Hribar, M.

1999-01-01

The construction and operation of a simple high-temperature X-ray absorption cell for potassium vapor is described. The principle of "spectroscopic heat pipe" is exploited to separate kapton windows, indispensable for good transmission in the low-energy region, from the hot and aggressive vapor. High-resolution spectrum of the K-edge region of atomic potassium reveals fingerprints of multielectron photoexcitations.

A method for the routine determination of aluminium in serum and water by flameless atomic absorption spectrometry.

PubMed

Parkinson, I S; Ward, M K; Kerr, D N

1982-10-27

A simple but reliable method for the routine determination of aluminium in serum and water by flameless atomic absorption spectrometry is described. No preparatory procedures are required for water samples, although serum is mixed with a wetting agent (Triton X-100) to allow complete combustion of the samples and to improve analytical precision. Precautions to prevent contamination during sample handling are discussed and instrumental parameters are defined. The method has a sensitivity of 35.5 pg and detection limits of 2.3 micrograms Al/l for serum and 1.3 micrograms Al/l for water. The method was used to determine the aluminium concentration in serum of 46 normal subjects. The mean aluminium content was 7.3 micrograms/l (range 2--15 micrograms/l.

The microwave induced plasma with optical emission spectrometry (MIP-OES) in 23 elements determination in geological samples.

PubMed

Niedzielski, P; Kozak, L; Wachelka, M; Jakubowski, K; Wybieralska, J

2015-01-01

The article presents the optimisation, validation and application of the microwave induced plasma optical emission spectrometry (MIP-OES) dedicated for a routine determination of Ag, Al, B, Ba, Bi, Ca, Cd, Cr, Cu, Fe, Ga, In, K, Li, Mg, Mn, Mo, Na, Ni, Pb, Sr, Tl, Zn, in the geological samples. The three procedures of sample preparation has been proposed: sample digestion with the use of hydrofluoric acid for determination of total concentration of elements, extraction by aqua regia for determination of the quasi-total element concentration and extraction by hydrochloric acid solution to determine contents of the elements in acid leachable fraction. The detection limits were on the level 0.001-0.121 mg L(-1) (from 0.010-0.10 to 1.2-12 mg kg(-1) depend on the samples preparation procedure); the precision: 0.20-1.37%; accuracy 85-115% (for recovery for certified standards materials analysis and parallel analysis by independent analytical techniques: X-ray fluorescence (XRF) and flame absorption spectrometry (FAAS)). The conformity of the results obtained by MIP-OES analytical procedures with the results obtained by XRF and FAAS analysis allows to propose the procedures for studies of elemental composition of the fraction of the geological samples. Additionally, the MIP-OES technique is much less expensive than ICP techniques and much less time-consuming than AAS techniques. Copyright © 2014 Elsevier B.V. All rights reserved.

Determination of ultratrace elements in natural waters by solid-phase extraction and atomic spectrometry methods.

PubMed

Grotti, Marco; Abelmoschi, Maria Luisa; Soggia, Francesco; Frache, Roberto

2003-01-01

A study was carried out on the preconcentration of ultratrace amounts of cadmium, lead, manganese, copper and iron from high-salinity aqueous samples and determination by atomic spectrometry methods. Sample volume, amount of resin, loading flow rate, and elution volume were optimized in order to obtain the simultaneous preconcentration of all the analytes. Quantitative recoveries were obtained by using 200 mg of iminodiacetic resin with a loading flow rate of 2 mL min(-1), elution volume of 3 mL and sample volume of 50-450 mL. Only copper in seawater samples was not completely retained by the resin (60-70% recovery), due to unfavorable competition of iminodiacetic-active groups with organically bound metal.To quantify the metals in the eluates, two atomic spectrometry techniques were compared: electrothermal atomization atomic absorption spectrometry (ETAAS) and inductively coupled plasma-optical emission spectrometry (ICP-OES) with simultaneous CCD detection system. Both techniques are suitable for sample analysis with detection limits of 1.0, 4.7, 3.3, 6.8, and 53 ng L(-1) using ETAAS and 12, 122, 3.4, 17, and 21 ng L(-1) using ICP-OES for Cd, Pb, Mn, Cu, and Fe, respectively. Relative standard deviations of the procedures ranged from 1.7 to 14% at the sub-microg L(-1) concentration level. The accuracy of both methods was verified by analyzing various certified reference materials (river water, estuarine water, coastal and off-shore seawater).

Interference-free determination of trace copper in freshly ripened honeys by flame atomic absorption spectrometry following a preconcentration by solid-phase extraction and a two-step elution process.

PubMed

Pohl, Pawel; Stecka, Helena; Jamroz, Piotr

2014-02-01

A fast and straightforward procedure aimed at separating copper (Cu) ions from monosacharides and preconcentrating their traces before flame atomic absorption spectrometry (FAAS) measurements was developed, and its suitability was evaluated by the analysis of freshly ripened honeys on the content of this environmentally and physiologically relevant element. This procedure included the passage (at 20 mL/min) of 10 % (m/v) solutions of honeys (100 mL) through resin beds of Dowex 50 W × 8-400 to retain Cu by solid-phase extraction (SPE) and separate it from the glucose and fructose matrix. In turn, SPE columns were rinsed at 20 mL/min with 20 mL of water and subsequently washed with 20 mL of a 0.5 mol/L HNO3 solution (at 2.0 mL/min) to elute potassium and sodium. Preconcentrated Cu was stripped (at 2.0 mL/min) with 5.0 mL of a 2.0 mol/L HCl solution and determined by FAAS. The proposed procedure was used for the analysis of six ripened monoflower and multiflower honeys, enabling the measurement of Cu within the range of 0.17-0.42 μg/g and with a precision of 3-10%. Recoveries of Cu added to respective honey solutions were within 94-102%, proving the good accuracy of this procedure. The detection limit of Cu achieved with this SPE preconcentration/separation procedure and FAAS detection was 3.6 ng/g.

High-performance liquid chromatographic analysis of as-synthesised N,N'-dimethylformamide-stabilised gold nanoclusters product

NASA Astrophysics Data System (ADS)

Xie, Shunping; Paau, Man Chin; Zhang, Yan; Shuang, Shaomin; Chan, Wan; Choi, Martin M. F.

2012-08-01

Reverse-phase high-performance liquid chromatographic (RP-HPLC) separation and analysis of polydisperse water-soluble gold nanoclusters (AuNCs) stabilised with N,N'-dimethylformamide (DMF) were investigated. Under optimal elution gradient conditions, the separation of DMF-AuNCs was monitored by absorption and fluorescence spectroscopy. The UV-vis spectral characteristics of the separated DMF-AuNCs have been captured and they do not possess distinct surface plasmon resonance bands, indicating that all DMF-AuNCs are small AuNCs. The photoluminescence emission spectra of the separated DMF-AuNCs are in the blue-light region. Moreover, cationic DMF-AuNCs are for the first time identified by ion chromatography. Our proposed RP-HPLC methodology has been successfully applied to separate AuNCs of various Au atoms as well as DMF-stabilised ligands. Finally, the composition of the separated DMF-AuNCs was confirmed by matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry and electrospray ionisation mass spectrometry, proving that the as-synthesised DMF-AuNCs product consists of Au10+, Au10, Au11, Au12, Au13, and Au14 NCs stabilised with various numbers of DMF ligands.Reverse-phase high-performance liquid chromatographic (RP-HPLC) separation and analysis of polydisperse water-soluble gold nanoclusters (AuNCs) stabilised with N,N'-dimethylformamide (DMF) were investigated. Under optimal elution gradient conditions, the separation of DMF-AuNCs was monitored by absorption and fluorescence spectroscopy. The UV-vis spectral characteristics of the separated DMF-AuNCs have been captured and they do not possess distinct surface plasmon resonance bands, indicating that all DMF-AuNCs are small AuNCs. The photoluminescence emission spectra of the separated DMF-AuNCs are in the blue-light region. Moreover, cationic DMF-AuNCs are for the first time identified by ion chromatography. Our proposed RP-HPLC methodology has been successfully applied to separate AuNCs of various Au atoms as well as DMF-stabilised ligands. Finally, the composition of the separated DMF-AuNCs was confirmed by matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry and electrospray ionisation mass spectrometry, proving that the as-synthesised DMF-AuNCs product consists of Au10+, Au10, Au11, Au12, Au13, and Au14 NCs stabilised with various numbers of DMF ligands. This article was submitted as part of a Themed Issue on metallic clusters. Other papers on this topic can be found in issue 14 of vol. 4 (2012). This issue can be found from the Nanoscale homepage [http://www.rsc.org/nanoscale].

Rapid Determination of Clenbuterol in Pork by Direct Immersion Solid-Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry.

PubMed

Ye, Diru; Wu, Susu; Xu, Jianqiao; Jiang, Ruifen; Zhu, Fang; Ouyang, Gangfeng

2016-02-01

Direct immersion solid-phase microextraction (DI-SPME) coupled with gas chromatography-mass spectrometry (GC-MS) was developed for rapid analysis of clenbuterol in pork for the first time. In this work, a low-cost homemade 44 µm polydimethylsiloxane (PDMS) SPME fiber was employed to extract clenbuterol in pork. After extraction, derivatization was performed by suspending the fiber in the headspace of the 2 mL sample vial saturated with a vapor of 100 µL hexamethyldisilazane. Lastly, the fiber was directly introduced to GC-MS for analysis. All parameters that influenced absorption (extraction time), derivatization (derivatization reagent, time and temperature) and desorption (desorption time) were optimized. Under optimized conditions, the method offered a wide linear range (10-1000 ng g(-1)) and a low detection limit (3.6 ng g(-1)). Finally, the method was successfully applied in the analysis of pork from the market, and recoveries of the method for spiked pork were 97.4-105.7%. Compared with the traditional solvent extraction method, the proposed method was much cheaper and fast. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Evaluation of Macro- and Microelement Levels in Black Tea in View of Its Geographical Origin.

PubMed

Brzezicha-Cirocka, Justyna; Grembecka, Małgorzata; Ciesielski, Tomasz; Flaten, Trond Peder; Szefer, Piotr

2017-04-01

The aim of this study was to evaluate the elemental composition of black tea samples and their infusions in view of their geographical origin. In total, 14 elements were analyzed, 13 (Ca, K, Mg, Na, Mn, Fe, Zn, Cu, Cr, Ni, Co, Cd, and Pb) by flame atomic absorption spectrometry, and P by UV-Vis spectrometry, after mineralization of samples. It was found that K was the most abundant macroelement in the analyzed samples, whereas among microelements, the highest concentration was found for Mn. Based on the obtained data, the percentage of elements leached into the infusions as well as the daily elemental intake from tea were calculated. The daily intake from tea was compared to the recommended daily allowances (RDAs), and the highest percentages of the RDAs were found for Mn (15 %) and Co (10 %). To study the relations between elemental composition and country of origin of samples, factor analysis and cluster analysis were applied. These multivariate techniques proved to be efficient tools able to differentiate samples according to their provenance as well as plantation within the common regions.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ferrante, Marco, E-mail: marco.ferrante@lngs.infn.it; De Angelis, Francesco, E-mail: francesco.deangelis@univaq.it; Nisi, Stefano, E-mail: stefano.nisi@lngs.infn.it

2015-08-17

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

Methods of chemical and phase composition analysis of gallstones

NASA Astrophysics Data System (ADS)

Suvorova, E. I.; Pantushev, V. V.; Voloshin, A. E.

2017-11-01

This review presents the instrumental methods used for chemical and phase composition investigation of gallstones. A great body of data has been collected in the literature on the presence of elements and their concentrations, obtained by fluorescence microscopy, X-ray fluorescence spectroscopy, neutron activation analysis, proton (particle) induced X-ray emission, atomic absorption spectroscopy, high-resolution gamma-ray spectrometry, electron paramagnetic resonance. Structural methods—powder X-ray diffraction, infrared spectroscopy, Raman spectroscopy—provide information about organic and inorganic phases in gallstones. Stone morphology was studied at the macrolevel with optical microscopy. Results obtained by analytical scanning and transmission electron microscopy with X-ray energy dispersive spectrometry are discussed. The chemical composition and structure of gallstones determine the strategy of removing stone from the body and treatment of patients: surgery or dissolution in the body. Therefore one chapter of the review describes the potential of dissolution methods. Early diagnosis and appropriate treatment of the disease depend on the development of clinical methods for in vivo investigation, which gave grounds to present the main characteristics and potential of ultrasonography (ultrasound scanning), magnetic resonance imaging, and X-ray computed tomography.

Glutathione binding to dirhodium tetraacetate: a spectroscopic, mass spectral and computational study of an anti-tumour compound.

PubMed

Wong, Daisy L; Zhang, Angel; Faponle, Abayomi S; de Visser, Sam P; Stillman, Martin J

2017-05-24

Glutathione (γ-l-glutamyl-l-cysteinyl-glycine) is a ubiquitous tripeptide found in all plants and animals. Glutathione has key roles as a metallochaperone and as a cellular thiol involved in metabolism. Little is known about how glutathione interacts with organometallic compounds in vivo. Here, we report the reactions of glutathione in vitro with dirhodium(ii) tetraacetate (tetrakis(μ-acetato)dirhodium(ii), Rh 2 (OAc) 4 ), a compound with anti-tumour properties. Electrospray ionization mass spectrometry, UV-Visible absorption and circular dichroism spectroscopic methods were used to determine the stoichiometries and optical properties of the final conjugate. Computational analyses were used to predict the binding modes of glutathione to the Rh 2 (OAc) 4 , and report on the orbital assignments for the resulting products. We explored the competition by GSH for methionine-bound axial sites on Rh 2 (OAc) 4 to investigate the use of weak thioether to protect its cellular-based anti-cancer activity. Our study highlights the important role that axial ligation would play in deactivating or significantly decreasing the efficacy of this bimetallic anti-tumor drug. The computational data explain the stability of the mono-adduct and the appearance of new absorption bands in the UV region including retention of the Rh-Rh single bond. Additionally, these data show that glutathione can effectively disable the potency of these metallo-drugs through orbital overlap of the entire Rh-Rh core as a result of the strong binding. Electronic absorption spectroscopy, mass spectrometry and computational analysis are a powerful combination in understanding possible chemical reactions in vivo and this information can be used to synthetically tune dirhodium complexes for use in the fight against cancer.

Biodegradation of lignin by Agaricus Bisporus

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vane, C.H.; Abbott, G.D.; Head, I.M.

The lignolytic activity of Agaricus bisporus will be addressed in this paper. Sound and fungally degraded lignins were characterized by Pyrolysis-Gas Chromatography-Mass Spectrometry (Py-GC-MS), Fourier Transform Infrared Spectroscopy (FnR) and elemental analysis. Fungally degraded lignins displayed increased wt%N, wt%H and wt%O content and decreased wt%C content The FTIR spectrum of decayed lignin showed an increase in the relative intensity of absorption bands assigned to carbonyl and carboxyl functional groups located on the aliphatic side chain and a decrease in absorption bands assigned to aromatic skeletal vibration modes. Semiquantitative Py-GC-MS revealed an 82% decrease in lignin derived pyrolysis products upon biodegradation.more » No significant increase in pyrolysis products with an oxygenated aliphatic side chain were detected in the fungally degraded lignin however shortening of the aliphatic side chain via cleavage at the {alpha}, {beta} and {gamma} positions was observed.« less

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

NASA Astrophysics Data System (ADS)

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.

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

PubMed

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.

Can sample treatments based on advanced oxidation processes assisted by high-intensity focused ultrasound be used for toxic arsenic determination in human urine by flow-injection hydride-generation atomic absorption spectrometry?

PubMed

Correia, A; Galesio, M; Santos, H; Rial-Otero, R; Lodeiro, C; Oehmen, A; Conceição, Antonio C L; Capelo, J L

2007-05-15

Two advanced oxidation processes (AOPs), based on high-intensity focused ultrasound (HIFU), namely, KMnO(4)/HCl/HIFU and H(2)O(2)/HCl/HIFU are studied and compared for the determination of toxic arsenic in human urine [As(III)+As(V)+MMA+DMA] by flow-injection hydride-generation atomic absorption spectrometry (FI-HG-AAS). The KMnO(4)/HCl/HIFU procedure was found to be adequate for organic matter degradation in human urine. l-cysteine (letra minuscula) was used for As reduction to the trivalent state. The new procedure was assessed with seven urines certified in different As species. Results revealed that with KMnO(4)/HCl/HIFU plus l-cysteine the toxic arsenic can be accurately measured in human urine whilst the H(2)O(2)/HCl/HIFU procedure underestimates toxic As. DMA and MMA degradation in urine were observed, due to the effects of the ultrasonic field. Recoveries for As(III), As(V), MMA and DMA were within the certified ranges. Arsenobetaine was not degraded by the AOPs. The new procedure adheres well to the principles of analytical minimalism: (i) low reagent consumption, (ii) low reagent concentration, (iii) low waste production and (iv) low amount of time required for sample preparation and analysis.

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

PubMed

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.

Development of a flow system for the determination of cadmium in fuel alcohol using vermicompost as biosorbent and flame atomic absorption spectrometry.

PubMed

Bianchin, Joyce Nunes; Martendal, Edmar; Mior, Renata; Alves, Vanessa Nunes; Araújo, Cleide Sandra Tavares; Coelho, Nívia Maria Melo; Carasek, Eduardo

2009-04-30

In this study a method for the determination of cadmium in fuel alcohol using solid-phase extraction with a flow injection analysis system and detection by flame atomic absorption spectrometry was developed. The sorbent material used was a vermicompost commonly used as a garden fertilizer. The chemical and flow variables of the on-line preconcentration system were optimized by means of a full factorial design. The selected factors were: sorbent mass, sample pH, buffer concentration and sample flow rate. The optimum extraction conditions were obtained using sample pH in the range of 7.3-8.3 buffered with tris(hydroxymethyl)aminomethane at 50 mmol L(-1), a sample flow rate of 4.5 mL min(-1) and 160 mg of sorbent mass. With the optimized conditions, the preconcentration factor, limit of detection and sample throughput were estimated as 32 (for preconcentration of 10 mL sample), 1.7 microg L(-1) and 20 samples per hour, respectively. The analytical curve was linear from 5 up to at least 50 microg L(-1), with a correlation coefficient of 0.998 and a relative standard deviation of 2.4% (35 microg L(-1), n=7). The developed method was successfully applied to spiked fuel alcohol, and accuracy was assessed through recovery tests, with recovery ranging from 94% to 100%.

Intercalation of IR absorber into layered double hydroxides: Preparation, thermal stability and selective IR absorption

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhu, Haifeng; Tang, Pinggui; Feng, Yongjun, E-mail: yjfeng@mail.buct.edu.cn

2012-03-15

Highlights: Black-Right-Pointing-Pointer PMIDA anions were intercalated into Mg{sub 2}Al-NO{sub 3} LDH by anion-exchange method. Black-Right-Pointing-Pointer The prepared material has highly selective IR absorption property in 9-11 {mu}m. Black-Right-Pointing-Pointer The obtained material has practical applications as heat-retaining additive. -- Abstract: N-phosphonomethyl aminodiacetic acid (PMIDA) was intercalated into the interlayer spacing of layered double hydroxides (LDH) by an anion-exchange method. The intercalated LDHs were characterized by various techniques such as powder X-ray diffraction (XRD), FT-IR spectroscopy, elemental analysis and simultaneous thermogravimetric and mass spectrometry (TG-MS) in details. The results show the formation of Mg{sub 2}Al-PMIDA LDH based on the expansion of d-spacingmore » from 0.89 nm to 1.22 nm and the disappearance of the characteristic IR absorption band at 1384 cm{sup -1} for NO{sub 3}{sup -} anions. The incorporation of Mg{sub 2}Al-PMIDA LDH into the low density polyethylene (LDPE) as an additive enhances the selectivity of IR absorption in the main wavelength region 9-11 {mu}m for radiant heat loss at night. Mg{sub 2}Al-PMIDA LDH as a heat-retaining additive has practical application in agricultural plastic films.« less

Determination of trace heavy metals in soil and sediments by atomic spectrometry following preconcentration with Schiff bases on Amberlite XAD-4.

PubMed

Kara, Derya; Fisher, Andrew; Hill, Steve J

2009-06-15

A matrix separation and analyte preconcentration system using Amberlite XAD copolymer resins functionalized by Schiff base reactions coupled with atomic spectrometry has been developed. Three different functionalized Amberlite XAD resins were synthesized using 4-phenylthiosemicarbazide, 2,3-dihydroxybenzaldehyde and 2-thiophenecarboxaldehyde as reagents. These resins could be used to preconcentrate transition and other trace heavy metal analytes from nitric acid digests of soil and sediment samples. Analyte retention was shown to work well at pH 6.0. After treatment of the digests with sodium fluoride and buffering to pH 6, samples that contain extremely large concentrations of iron were analysed for trace analytes without the excess iron overloading the capacity of the resin. The analytes Cd, Co, Cu, Ni and Pb were preconcentrated from acid extracts of certified soil/sediment samples and then eluted with 0.1M HNO(3) directly to the detection system. Flame atomic absorption spectrometry was used as a means of detection during the studies. The efficiency of the chelating resin and the accuracy of the proposed method were evaluated by the analysis of soil (SO-2) and sediment (LGC 6157 and MESS-3) certified reference materials.

Conversion electron spectrometry of Pu isotopes with a silicon drift detector.

PubMed

Pommé, S; Paepen, J; Peräjärvi, K; Turunen, J; Pöllänen, R

2016-03-01

An electron spectrometry set-up was built at IRMM consisting of a vacuum chamber with a moveable source holder and windowless Peltier-cooled silicon drift detector (SDD). The SDD is well suited for measuring low-energy x rays and electrons emitted from thin radioactive sources with low self-absorption. The attainable energy resolution is better than 0.5keV for electrons of 30keV. It has been used to measure the conversion electron spectra of three plutonium isotopes, i.e. (238)Pu, (239)Pu, (240)Pu, as well as (241)Am (being a decay product of (241)Pu). The obtained mixed x-ray and electron spectra are compared with spectra obtained with a close-geometry set-up using another SDD in STUK and spectra measured with a Si(Li) detector at IRMM. The potential of conversion electron spectrometry for isotopic analysis of mixed plutonium samples is investigated. With respect to the (240)Pu/(239)Pu isotopic ratio, the conversion electron peaks of both isotopes are more clearly separated than their largely overlapping peaks in alpha spectra. Copyright © 2015 The Authors. Published by Elsevier Ltd.. All rights reserved.

Determination of Aluminum in Dialysis Concentrates by Atomic Absorption Spectrometry after Coprecipitation with Lanthanum Phosphate.

PubMed

Selvi, Emine Kılıçkaya; Şahin, Uğur; Şahan, Serkan

2017-01-01

This method was developed for the determination of trace amounts of aluminum(III) in dialysis concentrates using atomic absorption spectrometry after coprecipitation with lanthanum phosphate. The analytical parameters that influenced the quantitative coprecipitation of analyte including amount of lanthanum, amount of phosfate, pH and duration time were optimized. The % recoveries of the analyte ion were in the range of 95-105 % with limit of detection (3s) of 0.5 µg l -1 . Preconcentration factor was found as 1000 and Relative Standard Deviation (RSD) % value obtained from model solutions was 2.5% for 0.02 mg L -1 . The accuracy of the method was evaluated with standard reference material (CWW-TMD Waste Water). The method was also applied to most concentrated acidic and basic dialysis concentrates with satisfactory results.

On-line preconcentration system for lead(II) determination in waste water by atomic absorption spectrometry using active carbon loaded with Pyrogallol Red.

PubMed

Ensafi, Ali A; Khayamian, Taghi; Karbasi, Mohammad H

2003-06-01

An on-line system for enrichment and determination of lead(II) is presented. It is based on the adsorption of lead(II) ions on a minicolumn packed with active carbon loaded with Pyrogallol Red. After preconcentration step, the metal ions are eluted automatically by 5.0 ml of 0.50 M nitric acid solution and the lead ion contents were determined by atomic absorption spectrometry. The influence of chemicals, pH and flow variables were studied as well as effect of potential interfering ions. Under the optimum conditions, the lead ions in aqueous samples were concentrated about 100 fold by the column. The detection limit was 0.001 microg ml(-1). The recovery percent of spliced lead(II) was in the range of 98%-103%.

Determination of trace amount of cadmium using dispersive liquid-liquid microextraction-slotted quartz tube-flame atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Fırat, Merve; Bakırdere, Sezgin; Fındıkoğlu, Maral Selin; Kafa, Emine Betül; Yazıcı, Elif; Yolcu, Melda; Büyükpınar, Çağdaş; Chormey, Dotse Selali; Sel, Sabriye; Turak, Fatma

2017-03-01

This study was performed to develop a sensitive analytical method for the determination of cadmium by slotted quartz tube-flame atomic absorption spectrometry (SQT-FAAS) after dispersive liquid-liquid microextraction (DLLME). The parameters affecting the cadmium complex formation and its extraction output were optimized to obtain high extraction efficiency. These included the pH and amount of the buffer solution, and the concentration of the ligand. The DLLME method was comprehensively optimized based on the type and amount of extraction solvent, dispersive solvent and salt. The type and period of mixing needed for a more effective extraction was also investigated. In order to further improve the sensitivity for the determination of cadmium, the flame atomic absorption spectrometry was fitted with a slotted quartz tube to increase the residence time of cadmium atoms in the pathway of incident light from a hollow cathode lamp. The limits of detection and quantitation (LOD and LOQ) for the FAAS were found to be 42 and 140 μg L- 1, respectively. Under the optimum conditions, LOD and LOQ of the FAAS after DLLME were calculated as 1.3 and 4.4 μg L- 1, respectively. Combining both optimized parameters of the DLLME and SQT-FAAS gave 0.5 and 1.5 μg L- 1 as LOD and LOQ, respectively. Accuracy of the method was also checked using a wastewater certified reference material (EU-L-2), and the result was in good agreement with the certified value.

[Analysis and separation of organic and inorganic speciations of soluble zinc in edible flowers].

PubMed

Peng, Shan-shan; Huang, Guo-qing

2005-02-01

Considering the medicinal effects of the edible flowers, the authors studied the separation of trace element zinc's soluble organic and inorganic speciations in water decoction of three edible flowers: Chrysanthemum, Cottonrose hibiscus and Honeysucker by using the 0.45 microm membrane filter and amberlite XAD-2 macroreticular resins. And trace element zinc contents were determined by atomic absorption spectrometry. The optimal conditions for separation had been established. This study verifies the economic value of developing edible flowers, and provides theoretical basis for developing edible flowers as the third functional food materials.

Spices as a source of lead exposure: a market-basket survey in Sri Lanka.

PubMed

Senanayake, M P; Perera, R; Liyanaarachchi, L A; Dassanayake, M P

2013-12-01

We performed a laboratory analysis of spices sold in Sri Lanka for lead content. Samples of curry powder, chili powder and turmeric powder from seven provinces, collected using the market basket survey method, underwent atomic absorption spectrometry. Blanks and standards were utilised for instrument calibration and measurement accuracy. The results were validated in two different laboratories. All samples were found to have lead levels below the US Food and Drug Administration's action level of 0.5 μg/g. Spices sold in Sri Lanka contain lead concentrations that are low and within the stipulated safety standards.

Lithographically fabricated silicon microreactor for operando QEXAFS studies in exhaust gas catalysis during simulation of a standard driving cycle

NASA Astrophysics Data System (ADS)

Doronkin, D. E.; Baier, S.; Sheppard, T.; Benzi, F.; Grunwaldt, J.-D.

2016-05-01

Selective catalytic reduction of NOx by ammonia over Cu-ZSM-5 was monitored by operando QEXAFS during simulation of the New European Driving Cycle. The required fast temperature transients were realized using a novel silicon microreactor, enabling simultaneous spectroscopic and kinetic analysis by X-ray absorption spectroscopy (XAS) and mass spectrometry (MS). Periods of high temperature were correlated to an increase in both N2 production and change of coordination of Cu sites. This operando approach using Si microreactors can be applied to other heterogeneous catalytic systems involving fast temperature transients.

Spectral Interferences Manganese (Mn) - Europium (Eu) Lines in X-Ray Fluorescence Spectrometry Spectrum

NASA Astrophysics Data System (ADS)

Tanc, Beril; Kaya, Mustafa; Gumus, Lokman; Kumral, Mustafa

2016-04-01

X-ray fluorescence (XRF) spectrometry is widely used for quantitative and semi quantitative analysis of many major, minor and trace elements in geological samples. Some advantages of the XRF method are; non-destructive sample preparation, applicability for powder, solid, paste and liquid samples and simple spectrum that are independent from chemical state. On the other hand, there are some disadvantages of the XRF methods such as poor sensitivity for low atomic number elements, matrix effect (physical matrix effects, such as fine versus course grain materials, may impact XRF performance) and interference effect (the spectral lines of elements may overlap distorting results for one or more elements). Especially, spectral interferences are very significant factors for accurate results. In this study, semi-quantitative analyzed manganese (II) oxide (MnO, 99.99%) was examined. Samples were pelleted and analyzed with XRF spectrometry (Bruker S8 Tiger). Unexpected peaks were obtained at the side of the major Mn peaks. Although sample does not contain Eu element, in results 0,3% Eu2O3 was observed. These result can occur high concentration of MnO and proximity of Mn and Eu lines. It can be eliminated by using correction equation or Mn concentration can confirm with other methods (such as Atomic absorption spectroscopy). Keywords: Spectral Interferences; Manganese (Mn); Europium (Eu); X-Ray Fluorescence Spectrometry Spectrum.

Accuracy of trace element determinations in alternate fuels

NASA Technical Reports Server (NTRS)

Greenbauer-Seng, L. A.

1980-01-01

NASA-Lewis Research Center's work on accurate measurement of trace level of metals in various fuels is presented. The differences between laboratories and between analytical techniques especially for concentrations below 10 ppm, are discussed, detailing the Atomic Absorption Spectrometry (AAS) and DC Arc Emission Spectrometry (dc arc) techniques used by NASA-Lewis. Also presented is the design of an Interlaboratory Study which is considering the following factors: laboratory, analytical technique, fuel type, concentration and ashing additive.

Atomic and Molecular Gas Phase Spectrometry.

DTIC Science & Technology

1983-09-30

between the thermometric levels, k is the Boltzmann constant (k = 0.695 cm-I K-1 ), Aik (s- 1) is the transition probability for spontaneous emission from...monitoring of the atomic absorption of M; information about the reaction processes were deduced from the shapes of the titration curves; (5) measure- ment of...Changes During Titration Based Upon The Releasing Effect Atomic Absorption Spectroscopy," D. Stojanovic and J.D. Winefordner, Anal Chim. Acta, 114, 295

Study of the effects of MeV Ag, Cu, Au, and Sn implantation on the optical properties of LiNbO3

NASA Technical Reports Server (NTRS)

Williams, E. K.; Ila, D.; Sarkisov, S.; Curley, M.; Poker, D. B.; Hensley, D. K.; Borel, C.

1998-01-01

The authors present the results of characterization of linear absorption and nonlinear refractive index of Au, Ag, Cu and Sn ion implantation into LiNbO3. Ag was implanted at 1.5 MeV to fluences of 2 to 17 x 17(exp 16)/sq cm at room temperature. Au and Cu were implanted to fluences of 5 to 20 x 10(exp 16)/sq cm at an energy of 2.0 MeV. Sn was implanted to a fluence of 1.6 x 10(exp 17)/sq cm at 160 kV. Optical absorption spectrometry indicated an absorption peak for the Au implanted samples after heat treatment at 1,000 C at approx. 620 nm. The Ag implanted samples absorption peaks shifted from approx. 450 nm before heat treatment to 550 nm after 500 C for 1h. Heat treatment at 800 C returned the Ag implanted crystals to a clear state. Cu nanocluster absorption peaks disappears at 500 C. No Sn clusters were observed by optical absorption or XRD. The size of the Ag and Au clusters as a function of heat treatment were determined from the absorption peaks. The Ag clusters did not change appreciably in size with heat treatment. The Au clusters increased from 3 to 9 nm diameter upon heat treatment at 1000 C. TEM analysis performed on a Au implanted crystal indicated the formation of Au nanocrystals with facets normal to the c-axis. Measurements of the nonlinear refractive indices were carried out using the Z-scan method with a tunable dye laser pumped by a frequency doubled mode-locked Nd:YAG laser. The dye laser had a 4.5 ps pulse duration time and 76 MHz pulse repetition rate (575 nm).

[Determination of trace cobalt in human urine by graphite furnace atomic absorption spectrometr].

PubMed

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.

Synthesis and investigation of various properties of a novel series of nonlinear optical (NLO) chromophores bearing dicyanovinyl (DCV) moiety

NASA Astrophysics Data System (ADS)

Seferoğlu, Nurgul; Bayrak, Yasmina; Yalçın, Ergin; Seferoğlu, Zeynel

2017-12-01

A series of new nonlinear optic (NLO) chromophores containing a dimethine (vinyl) as π-bridge and electron acceptor dicyanomethine and different electron-donating groups and heterocyclic rings were synthesized. The structures of synthesized dyes were characterized by Fourier Transform Infrared (FTIR), proton and carbon nuclear magnetic resonance (1H/13C NMR) and mass spectrometry. Their electronic absorption spectra were evaluated in MeOH, THF and DCM. The absorption maxima exhibited little bathochromic shifts for each dye with the increasing dielectric constants of the solvents. The synthesized dyes can absorb in the range of 354-506 nm. The analysis of the electronic spectra showed that the dyes having electron-donating groups or heterocyclic rings showed significant changes relative to the model dye which has no substituent on the phenyl ring. In addition, the absorption maxima moved to the longest wavelength for dye containing N,N-dibutylamino substituent. Experimental absorption wavelengths for the compounds were found to be in good agreement with those predicted using the Time-Dependent Density Functional Theory (TD-DFT) [B3LYP/6-311 + g(d,p)]. Furthermore, the second order NLO responses of the dyes were calculated using density functional theory (DFT) calculations. The study reveals that the synthesized chromophores have large first hyperpolarizability (β) values, hence they may have potential applications in the development of NLO materials. For determination of the thermal behaviors of the compounds, thermogravimetric analysis (TGA) were done. The result showed that all the chromophores exhibited good thermal stabilities with the decomposition temperatures (Td) greater than 260 °C.

Blood lead levels and risk factors in pregnant women from Durango, Mexico.

PubMed

La-Llave-León, Osmel; Estrada-Martínez, Sergio; Manuel Salas-Pacheco, José; Peña-Elósegui, Rocío; Duarte-Sustaita, Jaime; Candelas Rangel, Jorge-Luís; García Vargas, Gonzalo

2011-01-01

In this cross-sectional study the authors determined blood lead levels (BLLs) and some risk factors for lead exposure in pregnant women. Two hundred ninety-nine pregnant women receiving medical attention by the Secretary of Health, State of Durango, Mexico, participated in this study between 2007 and 2008. BLLs were evaluated with graphite furnace atomic absorption spectrometry. The authors used Student t test, 1-way analysis of variance (ANOVA), and linear regression as statistical treatments. BLLs ranged from 0.36 to 23.6 μg/dL (mean = 2.79 μg/dL, standard deviation = 2.14). Multivariate analysis showed that the main predictors of BLLs were working in a place where lead is used, using lead glazed pottery, and eating soil.

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

PubMed

Siriangkhawut, Watsaka; Sittichan, Patcharee; Ponhong, Kraingkrai; Chantiratikul, Piyanete

2017-10-01

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. Copyright © 2017. Published by Elsevier B.V.

Determination of arsenic and cadmium in crude oil by direct sampling graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

de Jesus, Alexandre; Zmozinski, Ariane Vanessa; Damin, Isabel Cristina Ferreira; Silva, Márcia Messias; Vale, Maria Goreti Rodrigues

2012-05-01

In this work, a direct sampling graphite furnace atomic absorption spectrometry method has been developed for the determination of arsenic and cadmium in crude oil samples. The samples were weighed directly on the solid sampling platforms and introduced into the graphite tube for analysis. The chemical modifier used for both analytes was a mixture of 0.1% Pd + 0.06% Mg + 0.06% Triton X-100. Pyrolysis and atomization curves were obtained for both analytes using standards and samples. Calibration curves with aqueous standards could be used for both analytes. The limits of detection obtained were 5.1 μg kg- 1 for arsenic and 0.2 μg kg- 1 for cadmium, calculated for the maximum amount of sample that can be analyzed (8 mg and 10 mg) for arsenic and cadmium, respectively. Relative standard deviations lower than 20% were obtained. For validation purposes, a calibration curve was constructed with the SRM 1634c and aqueous standards for arsenic and the results obtained for several crude oil samples were in agreement according to paired t-test. The result obtained for the determination of arsenic in the SRM against aqueous standards was also in agreement with the certificate value. As there is no crude oil or similar reference material available with a certified value for cadmium, a digestion in an open vessel under reflux using a "cold finger" was adopted for validation purposes. The use of paired t-test showed that the results obtained by direct sampling and digestion were in agreement at a 95% confidence level. Recovery tests were carried out with inorganic and organic standards and the results were between 88% and 109%. The proposed method is simple, fast and reliable, being appropriated for routine analysis.

A potential model for drug screening by simulating the effect of shear stress in vivo on endothelium.

PubMed

Xu, Yingqian; Wang, Bochu; Deng, Jia; Liu, Zerong; Zhu, Liancai

2013-01-01

The purpose of this paper was to research the potential of a dynamic cell model in drug screening by studying the influence of microvascular wall shear stress on the drug absorption of endothelial cells compared to that in the static state. The cells were grown and seeded on gelatin-coated glass slides and were pretreated with extracts of Salviae miltiorrhizae (200 μg/ml) for 1 h. Then oxidative stress damage was produced by H2O2 (300 μmol/l) for 0.5 h under the 1.5 dyn/cm2 shear stress incorporated in a parallel plate flow chamber. Morphological analysis was conducted with an inverted microscope and image analysis software, and high performance liquid chromatography-mass spectrometry was used for the detection of active compounds. We compared the drug absorption in the dynamic group with that in the static group. In the dynamic model, five compounds and two new metabolite peaks were detected. However, in the static model, four compounds were absorbed by cells, and one metabolite peak was found. This study indicated that there were some effects on the absorption and metabolism of drugs under the microvascular shear stress compared to that under stasis. We infer that shear stress in the microcirculation situation in vivo played a role in causing the differences between drug screening in vitro and in vivo.

Water-soluble phosphine-protected Au9 clusters: Electronic structures and nuclearity conversion via phase transfer

NASA Astrophysics Data System (ADS)

Yao, Hiroshi; Tsubota, Shuhei

2017-08-01

In this article, isolation, exploration of electronic structures, and nuclearity conversion of water-soluble triphenylphosphine monosulfonate (TPPS)-protected nonagold (Au9) clusters are outlined. The Au9 clusters are obtained by the reduction of solutions containing TPPS and HAuCl4 and subsequent electrophoretic fractionation. Mass spectrometry and elemental analysis reveal the formation of [Au9(TPPS)8]5- nonagold cluster. UV-vis absorption and magnetic circular dichroism (MCD) spectra of aqueous [Au9(TPPS)8]5- are quite similar to those of [Au9(PPh3)8]3+ in organic solvent, so the solution-phase structures are likely similar for both systems. Simultaneous deconvolution analysis of absorption and MCD spectra demonstrates the presence of some weak electronic transitions that are essentially unresolved in the UV-vis absorption. Quantum chemical calculations for a model compound [Au9(pH3)8]3+ show that the possible (solution-phase) skeletal structure of the nonagold cluster has D2h core symmetry rather than C4-symmetrical centered crown conformation, which is known as the crystal form of the Au9 compound. Moreover, we find a new nuclearity conversion route from Au9 to Au8; that is, phase transfer of aqueous [Au9(TPPS)8]5- into chloroform using tetraoctylammonium bromide yields [Au8(TPPS)8]6- clusters in the absence of excess phosphine.

The Chemistry of Seashells.

ERIC Educational Resources Information Center

Kinard, W. Frank

1980-01-01

Describes the use of infrared and atomic absorption spectrometry in an introductory chemical oceanography course to introduce students to carbonate mineralogy by having them determine both the crystal structure and the magnesium content of seashells that they have collected. (Author/JN)

Determination of arsenic, antimony, bismuth, cadmium, copper, lead, molybdenum, silver and zinc in geological materials by atomic-absorption spectrometry

USGS Publications Warehouse

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.

Measurement of free radical kinetics in pulsed plasmas by UV and VUV absorption spectroscopy and by modulated beam mass spectrometry

NASA Astrophysics Data System (ADS)

Cunge, G.; Bodart, P.; Brihoum, M.; Boulard, F.; Chevolleau, T.; Sadeghi, N.

2012-04-01

This paper reviews recent progress in the development of time-resolved diagnostics to probe high-density pulsed plasma sources. We focus on time-resolved measurements of radicals' densities in the afterglow of pulsed discharges to provide useful information on production and loss mechanisms of free radicals. We show that broad-band absorption spectroscopy in the ultraviolet and vacuum ultraviolet spectral domain and threshold ionization modulated beam mass spectrometry are powerful techniques for the determination of the time variation of the radicals' densities in pulsed plasmas. The combination of these complementary techniques allows detection of most of the reactive species present in industrial etching plasmas, giving insights into the physico-chemistry reactions involving these species. As an example, we discuss briefly the radicals' kinetics in the afterglow of a SiCl4/Cl2/Ar discharge.

The determination of lead in sugar and sweets without digestion by electrothermal atomic absorption spectrometry (ETAAS) with a rhodium chemical modifier.

PubMed

Dias, V M C; Cardoso, A S B

2006-05-01

Reference methods for determining lead in food are usually time-consuming. This paper reports a straightforward procedure using electrothermal atomic absorption spectrometry (ETAAS), to determine lead (Pb) in fat-free sweets. Several chemical modifiers were examined and results showed that it is not necessary to digest the samples, when a rhodium (Rh) modifier was used. The samples were dissolved in nitric acid and the determination of Pb was performed by ETAAS, using Rh chemical modifier at a pyrolysis temperature of 900 degrees C and an atomization temperature of 1,500 degrees C. No ashing step was employed and aqueous standards were used, in the range 2-10 microg l(-1). The limit of quantification was 0.095 mg kg(-1), and the accuracy of the method was verified by analysing certified reference materials.

Study on the inclusion interaction of p-sulfonated calix[ n]arenes with Vitamin K 3 using methylene blue as a spectral probe

NASA Astrophysics Data System (ADS)

Lu, Qin; Gu, Jiashan; Yu, Huapeng; Liu, Chun; Wang, Lun; Zhou, Yunyou

2007-09-01

The characteristics of host-guest complexation between p-sulfonated calix[ n]arene ( SCnA, n = 4, 6) and Vitamin K 3 ( VK3) were investigated by fluorescence spectrometry and absorption spectrometry using methylene blue ( MB) as a probe. Interaction with MB and SCnA led to an obvious decrease in fluorescence intensity of MB, accompanying with shifts of emission peaks. Absorption peaks also showed interesting changes; however, when VK3 was added, fluorescence intensity and absorbance recovered and a slight and slow red shift was observed. The obtained results showed that the inclusion ability of p-sulphonated calix[ n]arenes towards VK3 was the order: p-sulphonated calix[6]arene ( SC6A) > p-sulphonated calix[4]arene ( SC4A). Relative mechanism was proposed to explain the inclusion process.

Study on the inclusion interaction of p-sulfonated calix[n]arenes with Vitamin K3 using methylene blue as a spectral probe.

PubMed

Lu, Qin; Gu, Jiashan; Yu, Huapeng; Liu, Chun; Wang, Lun; Zhou, Yunyou

2007-09-01

The characteristics of host-guest complexation between p-sulfonated calix[n]arene (SCnA, n = 4, 6) and Vitamin K(3) (VK(3)) were investigated by fluorescence spectrometry and absorption spectrometry using methylene blue (MB) as a probe. Interaction with MB and SCnA led to an obvious decrease in fluorescence intensity of MB, accompanying with shifts of emission peaks. Absorption peaks also showed interesting changes; however, when VK(3) was added, fluorescence intensity and absorbance recovered and a slight and slow red shift was observed. The obtained results showed that the inclusion ability of p-sulphonated calix[n]arenes towards VK(3) was the order: p-sulphonated calix[6]arene (SC6A) >p-sulphonated calix[4]arene (SC4A). Relative mechanism was proposed to explain the inclusion process.

Investigation of Pb species in soils, celery and duckweed by synchrotron radiation X-ray absorption near-edge structure spectrometry

NASA Astrophysics Data System (ADS)

Luo, Liqiang; Shen, Yating; Liu, Jian; Zeng, Yuan

2016-08-01

The Pb species play a key role in its translocation in biogeochemical cycles. Soils, sediments and plants were collected from farmlands around Pb mines, and the Pb species in them was identified by X-ray absorption near-edge structure spectrometry. In soils, Pb5(PO4)3Cl and Pb3(PO4)2 were detected, and in sediments, Pb-fulvic acids (FAs) complex was identified. A Pb complex with FA fragments was also detected in celery samples. We found that (1) different Pb species were present in soils and sediments; (2) the Pb species in celery, which was grown in sediments, was different from the species present in duckweed, which grew in water; and (3) a Pb-FA-like compound was present in celery roots. The newly identified Pb species, the Pb-FA-like compound, may play a key role in Pb tolerance and translocation within plants.

Cloud point extraction thermospray flame quartz furnace atomic absorption spectrometry for determination of ultratrace cadmium in water and urine

NASA Astrophysics Data System (ADS)

Wu, Peng; Zhang, Yunchang; Lv, Yi; Hou, Xiandeng

2006-12-01

A simple, low cost and highly sensitive method based on cloud point extraction (CPE) for separation/preconcentration and thermospray flame quartz furnace atomic absorption spectrometry was proposed for the determination of ultratrace cadmium in water and urine samples. The analytical procedure involved the formation of analyte-entrapped surfactant micelles by mixing the analyte solution with an ammonium pyrrolidinedithiocarbamate (APDC) solution and a Triton X-114 solution. When the temperature of the system was higher than the cloud point of Triton X-114, the complex of cadmium-PDC entered the surfactant-rich phase and thus separation of the analyte from the matrix was achieved. Under optimal chemical and instrumental conditions, the limit of detection was 0.04 μg/L for cadmium with a sample volume of 10 mL. The analytical results of cadmium in water and urine samples agreed well with those by ICP-MS.

Determination of silver, bismuth, cadmium, copper, lead, and zinc in geologic materials by atomic absorption spectrometry with tricaprylylmethylammonium chloride

USGS Publications Warehouse

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.

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

PubMed

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.

Speciation of organic and inorganic selenium in selenium-enriched rice by graphite furnace atomic absorption spectrometry after cloud point extraction.

PubMed

Sun, Mei; Liu, Guijian; Wu, Qianghua

2013-11-01

A new method was developed for the determination of organic and inorganic selenium in selenium-enriched rice by graphite furnace atomic absorption spectrometry detection after cloud point extraction. Effective separation of organic and inorganic selenium in selenium-enriched rice was achieved by sequentially extracting with water and cyclohexane. Under the optimised conditions, the limit of detection (LOD) was 0.08 μg L(-1), the relative standard deviation (RSD) was 2.1% (c=10.0 μg L(-1), n=11), and the enrichment factor for selenium was 82. Recoveries of inorganic selenium in the selenium-enriched rice samples were between 90.3% and 106.0%. The proposed method was successfully applied for the determination of organic and inorganic selenium as well as total selenium in selenium-enriched rice. Copyright © 2013 Elsevier Ltd. All rights reserved.

The Cu2ZnSnSe4 thin films solar cells synthesized by electrodeposition route

NASA Astrophysics Data System (ADS)

Li, Ji; Ma, Tuteng; Wei, Ming; Liu, Weifeng; Jiang, Guoshun; Zhu, Changfei

2012-06-01

An electrodeposition route for preparing Cu2ZnSnSe4 thin films for thin film solar cell absorber layers is demonstrated. The Cu2ZnSnSe4 thin films are prepared by co-electrodeposition Cu-Zn-Sn metallic precursor and subsequently annealing in element selenium atmosphere. The structure, composition and optical properties of the films were investigated by X-ray diffraction (XRD), Raman spectrometry, energy dispersive spectrometry (EDS) and UV-VIS absorption spectroscopy. The Cu2ZnSnSe4 thin film with high crystalline quality was obtained, the band gap and absorption coefficient were 1.0 eV and 10-4 cm-1, which is quite suitable for solar cells fabrication. A solar cell with the structure of ZnO:Al/i-ZnO/CdS/Cu2ZnSnSe4/Mo/glass was fabricated and achieved an conversion efficiency of 1.7%.

INFRARED SPECTRUM OF POTASSIUM-CATIONIZED TRIETHYLPHOSPHATE GENERATED USING TANDEM MASS SPECTROMETRY AND INFRARED MULTIPLE PHOTON DISSOCIATION

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gary S. Groenewold; Christopher M. Leavitt; Ryan P. Dain

2009-09-01

Tandem mass spectrometry and wavelength selective infrared photodissociation was used to generate an infrared spectrum of gas-phase triethylphosphate cationized by attachment of K+. Prominent absorptions were observed in the region of 900 to 1300 cm-1 that are characteristic of phosphate P=O and P-O-R stretches. The relative positions and intensities of the IR absorptions were reproduced well by density functional theory (DFT) calculations performed using the B3LYP functional and the 6-31+g(d), 6-311+g(d,p) and 6-311++G(3df,2pd) basis sets. Because of good correspondence between experiment and theory for the cation, DFT was then used to generate a theoretical spectrum for neutral triethylphosphate, which inmore » turn accurately reproduces the IR spectrum of the neat liquid when solvent effects are included in the calculations.« less

Remote laser evaporative molecular absorption spectroscopy

NASA Astrophysics Data System (ADS)

Hughes, Gary B.; Lubin, Philip; Cohen, Alexander; Madajian, Jonathan; Kulkarni, Neeraj; Zhang, Qicheng; Griswold, Janelle; Brashears, Travis

2016-09-01

We describe a novel method for probing bulk molecular and atomic composition of solid targets from a distant vantage. A laser is used to melt and vaporize a spot on the target. With sufficient flux, the spot temperature rises rapidly, and evaporation of surface materials occurs. The melted spot creates a high-temperature blackbody source, and ejected material creates a plume of surface materials in front of the spot. Molecular and atomic absorption occurs as the blackbody radiation passes through the ejected plume. Bulk molecular and atomic composition of the surface material is investigated by using a spectrometer to view the heated spot through the ejected plume. The proposed method is distinct from current stand-off approaches to composition analysis, such as Laser-Induced Breakdown Spectroscopy (LIBS), which atomizes and ionizes target material and observes emission spectra to determine bulk atomic composition. Initial simulations of absorption profiles with laser heating show great promise for Remote Laser-Evaporative Molecular Absorption (R-LEMA) spectroscopy. The method is well-suited for exploration of cold solar system targets—asteroids, comets, planets, moons—such as from a spacecraft orbiting the target. Spatial composition maps could be created by scanning the surface. Applying the beam to a single spot continuously produces a borehole or trench, and shallow subsurface composition profiling is possible. This paper describes system concepts for implementing the proposed method to probe the bulk molecular composition of an asteroid from an orbiting spacecraft, including laser array, photovoltaic power, heating and ablation, plume characteristics, absorption, spectrometry and data management.

Gold and gold-iron oxide magnetic glyconanoparticles: synthesis, characterization and magnetic properties.

PubMed

de la Fuente, Jesús M; Alcántara, David; Eaton, Peter; Crespo, Patricia; Rojas, Teresa C; Fernandez, Asunción; Hernando, Antonio; Penadés, Soledad

2006-07-06

The preparation, characterization and the magnetic properties of gold and gold-iron oxide glyconanoparticles (GNPs) are described. Glyconanoparticles were prepared in a single step procedure in the presence of aqueous solution of thiol functionalized neoglycoconjugates and either gold salts or both gold and iron salts. Neoglycoconjugates of lactose and maltose disaccharides with different linkers were used. Iron-free gold or gold-iron oxide GNPs with controlled gold-iron ratios were obtained. The average core-size diameters are in the range of 1.5-2.5 nm. The GNPs are fully characterized by (1)H NMR spectrometry, transmission electron microscopy (TEM), and UV-vis and X-ray absorption (XAS) spectroscopies. Inductive plasma-atomic emission spectrometry (ICP) and elemental analysis gave the average number of neoglycoconjugates per cluster. The magnetic properties were measured in a SQUID magnetometer. The most remarkable results was the observation of a permanent magnetism up to room temperature in the iron-free gold GNPs, that was not present in the corresponding gold-iron oxide GNPs.

Metabolic studies of an orally active platinum anticancer drug by liquid chromatography-electrospray ionization mass spectrometry.

PubMed

Poon, G K; Raynaud, F I; Mistry, P; Odell, D E; Kelland, L R; Harrap, K R; Barnard, C F; Murrer, B A

1995-09-29

Bis(acetato)amminedichloro(cyclohexylamine) platinum(IV) (JM216) is a new orally administered platinum complex with antitumor properties, and is currently undergoing phase II clinical trials. When JM216 was incubated with human plasma ultrafiltrate, 93% of the platinum species were protein-bound and 7% were unbound. The unbound platinum complexes in the ultrafiltrates of human plasma were analysed using a liquid chromatography-electrospray ionization-mass spectrometry (LC-ESI-MS) method. Apart from the parent drug, four metabolites were identified and characterised. These include JM118 [amminedichloro(cyclohexylamine) platinum(II)], JM383 [bis(acetato)ammine(cyclohexylamine)dihydroxo platinum(IV)] and the two isomers JM559 and JM518 [bis(acetato)amminechloro(cyclohexylamine) hydroxo platinum(IV)]. Their elemental compositions were determined by accurate mass measurement during the LC analysis, to confirm their identities. Quantitation of these metabolites by off-line LC atomic absorption spectroscopy demonstrated that JM118 is the major metabolite in plasma from patients receiving JM216 treatment.

Phytoremediation of heavy metal copper (Cu2+) by sunflower (Helianthus annuus l.)

NASA Astrophysics Data System (ADS)

Mahardika, G.; Rinanti, A.; Fachrul, M. F.

2018-01-01

A study in microcosmic condition has been carried out to determine the effectiveness of Helianthus annuus as a hyperaccumulator plant for heavy metal, Copper (Cu2+), that exposed in the soil. Artificial pollutants containing Copper (Cu2+) 0, 60, 120, 180 ppm are exposed to uncontaminated soil. The 12-weeks old H. annuus seedling were grown in Cu2+ contaminated soil, with variations of absorption time 3, 6, and 9 weeks. Analysis of Cu2+ concentration on soil and H. annuus (root, stem, leaf) was analised by Atomic Absorbtion Spectrometry (AAS). H. annuus are capable for Cu2+ removal, and the highest removal of Cu2+ is 85.56%, the highest metal accumulation/bioconcentration factor (BCF) is 0.99 occurred at roots with 9 weeks of exposure time and the highest translocation factor (TF) is 0.71. This highest removal is five times better than absorption by stems and leaves. The results concluded, the use of H. annuus for phytoextraction of heavy metals Cu2+ in contaminated soil can be an alternative to the absorption of heavy metal Cu2+ with low concentration metals which is generally very difficult to do in physical-chemical removal.

Determination of essential elements in beverages, herbal infusions and dietary supplements using a new straightforward sequential approach based on flame atomic absorption spectrometry.

PubMed

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

2017-03-15

A simple method based on FAAS was developed for the sequential multi-element determination of Cu, Zn, Mn, Mg and Si in beverages and food supplements with successful results. The main absorption lines for Cu, Zn and Si and secondary lines for Mn and Mg were selected to carry out the measurements. The sample introduction was performed using a flow injection system. Using the choice of the absorption line wings, the upper limit of the linear range increased up to 110mgL -1 for Mg, 200mgL -1 for Si and 13mgL -1 for Zn. The determination of the five elements was carried out, in triplicate, without the need of additional sample dilutions and/or re-measurements, using less than 3.5mL of sample to perform the complete analysis. The LODs were 0.008mgL -1 for Cu, 0.017mgL -1 for Zn, 0.011mgL -1 for Mn, 0.16mgL -1 for Si and 0.11mgL -1 for Mg. Copyright © 2016 Elsevier Ltd. All rights reserved.

Group 6 metal pentacarbonyl complexes of air-stable primary, secondary, and tertiary ferrocenylethylphosphines.

PubMed

Rabiee Kenaree, Amir; Sauvé, Ethan R; Ragogna, Paul J; Gilroy, Joe B

2016-02-21

The synthesis and characterization of a series of Group 6 metal pentacarbonyl complexes of air stable primary, secondary, and tertiary phosphines containing ferrocenylethyl substituents are reported [M(CO)5L: M = Cr, Mo, W; L = PH2(CH2CH2Fc), PH(CH2CH2Fc)2, P(CH2CH2Fc)3]. The structure and composition of the complexes were confirmed by multinuclear NMR spectroscopy, IR and UV-Vis absorption spectroscopy, mass spectrometry, X-ray crystallography, and elemental analysis. The solid-state structural data reported revealed trends in M-C and M-P bond lengths that mirrored those of the atomic radii of the Group 6 metals involved. UV-Vis absorption spectroscopy and cyclic voltammetry highlighted characteristics consistent with electronically isolated ferrocene units including wavelengths of maximum absorption between 435 and 441 nm and reversible one-electron (per ferrocene unit) oxidation waves between 10 and -5 mV relative to the ferrocene/ferrocenium redox couple. IR spectroscopy confirmed that the σ donating ability of the phosphines increased as ferrocenylethyl substituents were introduced and that the tertiary phosphine ligand described is a stronger σ donor than PPh3 and a weaker σ donor than PEt3, respectively.

Application of high-resolution continuum source flame atomic absorption spectrometry to reveal, evaluate and overcome certain spectral effects in Pb determination of unleaded gasoline

NASA Astrophysics Data System (ADS)

Kowalewska, Zofia; Laskowska, Hanna; Gzylewski, Michał

2017-06-01

High-resolution continuum source and line source flame atomic absorption spectrometry (HR-CS FAAS and LS FAAS, respectively) were applied for Pb determination in unleaded aviation or automotive gasoline that was dissolved in methyl-isobutyl ketone. When using HR-CS FAAS, a structured background (BG) was registered in the vicinity of both the 217.001 nm and 283.306 nm Pb lines. In the first case, the BG, which could be attributed to absorption by the OH molecule, directly overlaps with the 217 nm line, but it is of relatively low intensity. For the 283 nm line, the structured BG occurs due to uncompensated absorption by OH molecules present in the flame. BG lines of relatively high intensity are situated at a large distance from the 283 nm line, which enables accurate analysis, not only when using simple variants of HR-CS FAAS but also for LS FAAS with a bandpass of 0.1 nm. The lines of the structured spectrum at 283 nm can have ;absorption; (maxima) or ;emission; (minima) character. The intensity of the OH spectra can significantly depend on the flame character and composition of the investigated organic solution. The best detection limit for the analytical procedure, which was 0.01 mg L- 1 for Pb in the investigated solution, could be achieved using HR-CS FAAS with the 283 nm Pb line, 5 pixels for the analyte line measurement and iterative background correction (IBC). In this case, least squares background correction (LSBC) is not recommended. However, LSBC (available as the ;permanent structures; option) would be recommended when using the 217 nm Pb line. In LS FAAS, an additional phenomenon related to the nature of the organic matrix (for example, isooctane or toluene) can play an important role. The effect is of continuous character and probably due to the simultaneous efficient correction of the continuous background (IBC) it is not observed in HR-CS FAAS. The fact that the effect does not depend on the flame character indicates that it is not radiation scattering. For LS FAAS, the determination of Pb using the 283 nm line, a 0.1 nm bandpass and a fuel lean flame is strongly recommended. The analysis of certified reference materials, recovery studies and the analysis of real samples with low Pb content supported the satisfactory accuracy of Pb determination in automotive or aviation gasoline when the recommended analytical variants are applied. The studies in this work shed new light on spectral phenomena in air-acetylene flames. The structured background due to absorption by the OH molecules must be taken into account during Pb determination in other materials as well as in some other elemental determinations, especially at low absorbance levels. The usefulness of HR-CS FAAS for revealing and investigating a structured background was demonstrated. HR-CS FAAS does not reveal fully corrected spectral effects with a continuous character, which can be found in LS FAAS.

Interference of nitrite and nitrogen dioxide on mercury and selenium determination by chemical vapor generation atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Nunes, Dayana Lopes; dos Santos, Eliane Pereira; Barin, Juliano Smanioto; Mortari, Sergio Roberto; Dressler, Valderi Luiz; de Moraes Flores, Érico Marlon

2005-06-01

In this study, a systematic investigation was performed concerning the interference of nitrogen oxides on the determination of selenium and mercury by hydride generation atomic absorption spectrometry (HG AAS) and cold vapor atomic absorption spectrometry (CV AAS). The effect of nitrate, nitrite and NO 2 dissolved in the condensed phase was evaluated. No effect of NO 3- on Se and Hg determination was observed up to 100 mg of sodium nitrate added to the reaction vessel. The Se signal was reduced by about 80% upon the addition of 6.8 mg NO 2-. For Hg, no interference of nitrite was observed up to 20 mg of NO 2-. A complete suppression of the Se signal was observed when gaseous NO 2 was introduced into analytical solutions. For Hg, a signal decrease between 8 and 13% occurred. For Se, bubbling argon or heating the solution was not able to recover the original absorbance values, whereas Hg signals were recovered with these procedures. When gaseous NO 2 was passed directly into the atomizer, Se signals decreased similarly to when NO 2 was bubbled in analytical solutions. The addition of urea, hydroxylamine hydrochloride and sulfamic acid (SA) was investigated to reduce the NO 2 effect in sample digests containing residual NO 2, but only SA was effective in reducing the interference. Based on the results, it is possible to propose the use of SA to prevent interferences in Se and Hg determinations by HG AAS and CV AAS, respectively.

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

PubMed

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.

Noise-Immune Cavity-Enhanced Optical Heterodyne Molecular Spectrometry Modelling Under Saturated Absorption

NASA Astrophysics Data System (ADS)

Dupré, Patrick

2015-06-01

The Noise-Immune Cavity-Enhanced Optical Heterodyne Molecular Spectrometry (NICE-OHMS) is a modern technique renowned for its ultimate sensitivity, because it combines long equivalent absorption length provided by a high finesse cavity, and a detection theoretically limited by the sole photon-shot-noise. One fallout of the high finesse is the possibility to accumulating strong intracavity electromagnetic fields (EMF). Under this condition, molecular transitions can be easy saturated giving rise to the usual Lamb dips (or hole burning). However, the unusual shape of the basically trichromatic EMF (due to the RF lateral sidebands) induces nonlinear couplings, i.e., new crossover transitions. An analytical methodology will be presented to calculate spectra provided by NICE-OHMS experiments. It is based on the solutions of the equations of motion of an open two-blocked-level system performed in the frequency-domain (optically thin medium). Knowing the transition dipole moment, the NICE-OHMS signals (``absorption-like'' and ``dispersion-like'') can be simulated by integration over the Doppler shifts and by paying attention to the molecular Zeeman sublevels and to the EMF polarization The approach has been validated by discussion experimental data obtained on two transitions of {C2H2} in the near-infrared under moderated saturation. One of the applications of the saturated absorption is to be able to simultaneously determine the transition intensity and the density number while only one these 2 quantities can only be assessed in nonlinear absorption. J. Opt. Soc. Am. B 32, 838 (2015) Optics Express 16, 14689 (2008)

Poly(1-vinylimidazole) functionalized magnetic ion imprinted polymer for fast and selective extraction of trace gold in geological, environmental and biological samples followed by graphite furnace atomic absorption spectrometry detection

NASA Astrophysics Data System (ADS)

Zhao, Bingshan; He, Man; Chen, Beibei; Xu, Hongrun; Hu, Bin

2018-05-01

In this study, poly(1-vinylimidazole) functionalized gold ion imprinted polymer coated magnetic nanoparticles (MNPs@PVIM-Au-IIP) were prepared and characterized. The adsorption behaviors of the prepared MNPs@PVIM-Au-IIP toward gold ions (Au(III)) were studied, it was found that MNPs@PVIM-Au-IIP has good selectivity, high adsorption capacity (185.4 mg g-1) and fast adsorption kinetic for Au(III). Based on it, a new method of ion imprinted magnetic solid phase extraction (II-MSPE) coupled with graphite furnace atomic absorption spectrometry (GFAAS) detection was proposed for the analysis of trace Au(III) in real samples with complicated matrix. Factors affecting MSPE including sample pH, desorption reagent, elution concentration and volume, elution time, sample volume and adsorption time were optimized. With high enrichment factor of 100-fold, the detection limit of the proposed method is 7.9 ng L-1 for Au(III) with the relative standard deviation of 7.4% (c = 50 ng L-1, n = 7). In order to validate the accuracy of the proposed method, the Certified Reference Material of GBW07293 geological sample (platinpalladium ore) was analyzed, and the determined value was in good agreement with the certified value. The proposed II-MSPE-GFAAS method is simple, fast, selective, sensitive and has been successfully applied in the determination of trace Au in ore, sediment, environmental water and human urine samples with satisfactory results.

A comparative evaluation of APF gel, CPP/ACP paste alone and in combination with carbon dioxide laser on human enamel resistance to acid solubility using atomic absorption spectrometry: an in-vitro study.

PubMed

Nozari, Ali; Rafiee, Azade; Dehghan Khalili, Sara; Fekrazad, Reza

2018-04-01

The aim of this study was to compare the effects of acidulated phosphate fluoride (APF) gel, calcium phosphopeptide-amorphous calcium phosphate (CPP/ACP) paste alone and in combination with CO2 laser on the resistance of enamel to acid solubility. Ninety enamel sections were obtained from 15 extracted teeth and were randomly assigned to six groups: 1) control group; 2) APF group; 3) CPP-ACP group; 4) CO2 laser group; 5) APF + CO2 group; and 6) CPP-ACP + CO2 group. The specimens were individually demineralized in 0.1 M lactic acid solution with adjusted pH of 4.8 for 24h at 37 ºC. The acid solubility was determined using atomic absorption spectrometry. Statistical analysis was done using one-way ANOVA and Tukey-Kramer post hoc test (P<0.05). The average extent of calcium ion released (ppm) was estimated as follow: group 1: 6.974±1.757, group 2: 5.363±1.383, group 3: 6.962±1.489, group 4: 6.890±1.560, group 5: 4.803±1.080 and group 6: 6.789±1.218. Based on the between-group comparison results, group 2 and group 5 showed significant differences with the other groups. Under the studied conditions, only, the APF group alone and in combination with CO2 laser could decrease enamel acid solubility.

Ultratrace determination of arsenic in water samples by electrothermal atomic absorption spectrometry after pre-concentration with Mg-Al-Fe ternary layered double hydroxide nano-sorbent.

PubMed

Abdolmohammad-Zadeh, Hossein; Jouyban, Abolghasem; Amini, Roghayeh

2013-11-15

A selective solid phase extraction method, based on nano-structured Mg-Al-Fe(NO3(-)) ternary layered double hydroxide as a sorbent, is developed for the pre-concentration of ultra-trace levels of arsenic (As) prior to determination by electrothermal atomic absorption spectrometry. It is found that both As(III) and As(V) could be quantitatively retained on the sorbent within a wide pH range of 4-12. Accordingly, the presented method is applied to determination of total inorganic As in aqueous solutions. Maximum analytical signal of As is achieved when the pyrolysis and atomization temperatures are close to 900 °C and 2300 °C, respectively. Several variables affecting the extraction efficiency including pH, sample flow rate, amount of nano-sorbent, elution conditions and sample volume are optimized. Under the optimized conditions, the limit of detection (3Sb/m) and the relative standard deviation are 4.6 pg mL(-1) and 3.9%, respectively. The calibration graph is linear in the range of 15.0-650 pg mL(-1) with a correlation coefficient of 0.9979, sorption capacity and pre-concentration factor are 8.68 mg g(-1) and 300, respectively. The developed method is validated by the analysis of a standard reference material (SRM 1643e) and is successfully applied to the determination of ultra-trace amounts of As in different water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Tellurium speciation analysis using hydride generation in situ trapping electrothermal atomic absorption spectrometry and ruthenium or palladium modified graphite tubes.

PubMed

Yildirim, Emrah; Akay, Pınar; Arslan, Yasin; Bakirdere, Sezgin; Ataman, O Yavuz

2012-12-15

Speciation of tellurium can be achieved by making use of different kinetic behaviors of Te(IV) and Te(VI) upon their reaction with sodium borohydride using hydride generation. While Te(IV) can form H(2)Te, Te(VI) will not form any volatile species during the course of hydride formation and measurement by atomic absorption spectrometry. Quantitative reduction of Te(VI) was achieved through application of a microwave assisted prereduction of Te(VI) in 6.0 mol/L HCl solution. Enhanced sensitivity was achieved by in situ trapping of the generated H(2)Te species in a previously heated graphite furnace whose surface was modified using Pd or Ru. Overall efficiency for in situ trapping in pyrolytically coated graphite tube surface was found to be 15% when volatile analyte species are trapped for 60s at 300°C. LOD and LOQ values were calculated as 0.086 ng/mL and 0.29 ng/mL, respectively. Efficiency was increased to 46% and 36% when Pd and Ru surface modifiers were used, respectively. With Ru modified graphite tube 173-fold enhancement was obtained over 180 s trapping period with respect to ETAAS; the tubes could be used for 250 cycles. LOD values were 0.0064 and 0.0022 ng/mL for Pd and Ru treated ETAAS systems, respectively, for 180 s collection of 9.6 mL sample solution. Copyright © 2012 Elsevier B.V. All rights reserved.

Pigment identification in artwork using graphite furnace atomic absorption spectrometry.

PubMed

Goltz, D M; Coombs, J; Marion, C; Cloutis, E; Gibson, J; Attas, M; Choo-Smith, L-P; Collins, C

2004-06-17

The use of a sampling technique is described for the identification of metals from inorganic pigments in paint. The sampling technique involves gently contacting a cotton swab with the painted surface to physically remove a minute quantity ( approximately 1-2mug) of pigment. The amount of material removed from the painted surface is invisible to the unaided eye and does not cause any visible effect to the painted surface. The cotton swab was then placed in a 1.5ml polystyrene beaker containing HNO(3) to extract pigment metals prior to analysis using graphite furnace atomic absorption spectrometry (GFAAS). GFAAS is well suited for identifying pigment metals since it requires small samples and many pigments consist of main group elements (e.g. Al) as well as transition metals (e.g. Zn, Fe and Cd). Using Cd (cadmium red) as the test element, the reproducibility of sampling a paint surface with the cotton swab was approximately 13% in either a water or oil medium. To test the feasibility of cotton sampling for pigment identification, samples were obtained from paintings (watercolour and oil) of a local collection. Raman spectra provided complementary information to the GFAAS, which together are essential for positive identification of some pigments. For example, GFAAS indicated the presence of Cu, but the Raman spectra positively identified the modern copper pigment phthalocyanine green (Cu(C(32)Cl(16)N(8)). Both Raman spectroscopy and GFAAS were useful for identifying ZnO as a white pigment.

Lead concentrations and isotope ratios in street dust determined by electrothermal atomic absorption spectrometry and inductively coupled plasma mass spectrometry.

PubMed

Nageotte, S M; Day, J P

1998-01-01

A major source of environmental lead, particularly in urban areas, has been from the combustion of leaded petrol. Street dust has previously been used to assess urban lead contamination, and the dust itself can also be a potential source of lead ingestion, particularly to children. The progressive reduction of lead in petrol, in recent years, would be expected to have been reflected in a reduction of lead in urban dust. We have tested this hypothesis by repeating an earlier survey of Manchester street dust and carrying out a comparable survey in Paris. Samples were collected from streets and parks, lead was extracted by digestion with concentrated nitric acid and determined by electrothermal atomic absorption spectrometry. Lead isotope ratios were measured by inductively coupled plasma mass spectrometry. Results for Manchester show that lead concentrations have fallen by about 40% (street dust averages, 941 micrograms g-1 (ppm) in 1975 down to 569 ppm in 1997). In Paris, the lead levels in street dust are much higher and significant differences were observed between types of street (not seen in Manchester). Additionally, lead levels in parks were much lower than in Manchester. Samples collected under the Eiffel Tower had very high concentrations and lead isotope ratios showed that this was unlikely to be fallout from motor vehicles but could be due to the paint used on the tower. Isotope ratios measurements also revealed that lead additives used in France and the UK come from different sources.

Vaporization and atomization of uranium in a graphite tube electrothermal vaporizer: a mechanistic study using electrothermal vaporization inductively coupled plasma mass spectrometry and graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Goltz, D. M.; Grégoire, D. C.; Byrne, J. P.; Chakrabarti, C. L.

1995-07-01

The mechanism of vaporization and atomization of U in a graphite tube electrothermal vaporizer was studied using graphite furnace atomic absorption spectrometry (GFAAS) and electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS). Graphite furnace AAS studies indicate U atoms are formed at temperatures above 2400°C. Using ETV-ICP-MS, an appearance temperature of 1100°C was obtained indicating that some U vaporizes as U oxide. Although U carbides form at temperatures above 2000°C, ETV-ICP-MS studies show that they do not vaporize until 2600°C. In the temperature range between 2200°C and 2600°C, U atoms in GFAAS are likely formed by thermal dissociation of U oxide, whereas at higher temperatures, U atoms are formed via thermal dissociation of U carbide. The origin of U signal suppression in ETV-ICP-MS by NaCl was also investigated. At temperatures above 2000°C, signal suppression may be caused by the accelerated rate of formation of carbide species while at temperatures below 2000°C, the presence of NaCl may cause intercalation of the U in the graphite layers resulting in partial retention of U during the vaporization step. The use of 0.3% freon-23 (CHF 3) mixed with the argon carrier gas was effective in preventing the intercalation of U in graphite and U carbide formation at 2700°C.

Speciation analysis of arsenic in biological matrices by automated hydride generation-cryotrapping-atomic absorption spectrometry with multiple microflame quartz tube atomizer (multiatomizer)

PubMed Central

Hernández-Zavala, Araceli; Matoušek, Tomáš; Drobná, Zuzana; Paul, David S.; Walton, Felecia; Adair, Blakely M.; Jiří, Dědina; Thomas, David J.

2008-01-01

Analyses of arsenic (As) species in tissues and body fluids of individuals chronically exposed to inorganic arsenic (iAs) provide essential information about the exposure level and pattern of iAs metabolism. We have previously described an oxidation state-specific analysis of As species in biological matrices by hydride-generation atomic absorption spectrometry (HG-AAS), using cryotrapping (CT) for preconcentration and separation of arsines. To improve performance and detection limits of the method, HG and CT steps are automated and a conventional flame-in-tube atomizer replaced with a recently developed multiple microflame quartz tube atomizer (multiatomizer). In this system, arsines from AsIII-species are generated in a mixture of Tris-HCl (pH 6) and sodium borohydride. For generation of arsines from both AsIII- and AsV-species, samples are pretreated with L-cysteine. Under these conditions, dimethylthioarsinic acid, a newly described metabolite of iAs, does not interfere significantly with detection and quantification of methylated trivalent arsenicals. Analytical performance of the automated HG-CT-AAS was characterized by analyses of cultured cells and mouse tissues that contained mono- and dimethylated metabolites of iAs. The capacity to detect methylated AsIII- and AsV-species was verified, using an in vitro methylation system containing recombinant rat arsenic (+3 oxidation state) methyltransferase and cultured rat hepatocytes treated with iAs. Compared with the previous HG-CT-AAS design, detection limits for iAs and its metabolites have improved significantly with the current system, ranging from 8 to 20 pg. Recoveries of As were between 78 and 117%. The precision of the method was better than 5% for all biological matrices examined. Thus, the automated HG-CT-AAS system provides an effective and sensitive tool for analysis of all major human metabolites of iAs in complex biological matrices. PMID:18677417

Direct determination of chromium in infant formulas employing high-resolution continuum source electrothermal atomic absorption spectrometry and solid sample analysis.

PubMed

Silva, Arlene S; Brandao, Geovani C; Matos, Geraldo D; Ferreira, Sergio L C

2015-11-01

The present work proposed an analytical method for the direct determination of chromium in infant formulas employing the high-resolution continuum source electrothermal atomic absorption spectrometry combined with the solid sample analysis (SS-HR-CS ET AAS). Sample masses up to 2.0mg were directly weighted on a solid sampling platform and introduced into the graphite tube. In order to minimize the formation of carbonaceous residues and to improve the contact of the modifier solution with the solid sample, a volume of 10 µL of a solution containing 6% (v/v) H2O2, 20% (v/v) ethanol and 1% (v/v) HNO3 was added. The pyrolysis and atomization temperatures established were 1600 and 2400 °C, respectively, using magnesium as chemical modifier. The calibration technique was evaluated by comparing the slopes of calibration curves established using aqueous and solid standards. This test revealed that chromium can be determined employing the external calibration technique using aqueous standards. Under these conditions, the method developed allows the direct determination of chromium with limit of quantification of 11.5 ng g(-1), precision expressed as relative standard deviation (RSD) in the range of 4.0-17.9% (n=3) and a characteristic mass of 1.2 pg of chromium. The accuracy was confirmed by analysis of a certified reference material of tomato leaves furnished by National Institute of Standards and Technology. The method proposed was applied for the determination of chromium in five different infant formula samples. The chromium content found varied in the range of 33.9-58.1 ng g(-1) (n=3). These samples were also analyzed employing ICP-MS. A statistical test demonstrated that there is no significant difference between the results found by two methods. The chromium concentrations achieved are lower than the maximum limit permissible for chromium in foods by Brazilian Legislation. Copyright © 2015. Published by Elsevier B.V.

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

PubMed

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.

Room-temperature synthesis and photoluminescence of hexagonal CePO4 nanorods

NASA Astrophysics Data System (ADS)

Zhu, J.; Zhang, K.; Zhao, H. Y.

2018-01-01

Hexagonal CePO4 nanorods were synthesized via a simple chemical precipitation route at room-temperature without the presence of surfactants and then characterized by powder X-ray diffraction (XRD), energy-dispersive X-ray (EDX) spectrometry, scanning electron microscopy (SEM), transmission electron microscopy (TEM), ultraviolet-visible (UV-vis) absorption and photoluminescence (PL) spectroscopy. Hexagonal CePO4 nanorods exhibit strong ultraviolet absorption and ultraviolet luminescence, which correspond to the electronic transitions between 4f and 5d state of Ce3+ ions.

Identification of Microalgae by Laser Desorption/Ionization Mass Spectrometry Coupled with Multiple Nanomatrices.

PubMed

Peng, Lung-Hsiang; Unnikrishnan, Binesh; Shih, Chi-Yu; Hsiung, Tung-Ming; Chang, Jeng; Hsu, Pang-Hung; Chiu, Tai-Chia; Huang, Chih-Ching

2016-04-01

In this study, we demonstrate a simple method to identify microalgae by surface-assisted laser desorption/ionization mass spectrometry (SALDI-MS) using three different substrates: HgSe, HgTe, and HgTeSe nanostructures. The fragmentation/ionization processes of complex molecules in algae varied according to the heat absorption and transfer efficiency of the nanostructured matrices (NMs). Therefore, the mass spectra obtained for microalgae showed different patterns of m/z values for different NMs. The spectra contained both significant and nonsignificant peaks. Constructing a Venn diagram with the significant peaks obtained for algae when using HgSe, HgTe, and HgTeSe NMs in m/z ratio range 100-1000, a unique relationship among the three sets of values was obtained. This unique relationship of sets is different for each species of microalgae. Therefore, by observing the particular relationship of sets, we successfully identified different algae such as Isochrysis galbana, Emiliania huxleyi, Thalassiosira weissflogii, Nannochloris sp., Skeletonema cf. costatum, and Tetraselmis chui. This simple and cost-effective SALDI-MS analysis method coupled with multi-nanomaterials as substrates may be extended to identify other microalgae and microorganisms in real samples. Graphical Abstract Identification of microalgae by surface-assisted laser desorption/ionization mass spectrometry coupled with three different mercury-based nanosubstrates.

Determination of Mercury in Aqueous and Geologic Materials by Continuous Flow-Cold Vapor-Atomic Fluorescence Spectrometry (CVAFS)

USGS Publications Warehouse

Hageman, Philip L.

2007-01-01

New methods for the determination of total mercury in geologic materials and dissolved mercury in aqueous samples have been developed that will replace the methods currently (2006) in use. The new methods eliminate the use of sodium dichromate (Na2Cr2O7 ?2H2O) as an oxidizer and preservative and significantly lower the detection limit for geologic and aqueous samples. The new methods also update instrumentation from the traditional use of cold vapor-atomic absorption spectrometry to cold vapor-atomic fluorescence spectrometry. At the same time, the new digestion procedures for geologic materials use the same size test tubes, and the same aluminum heating block and hot plate as required by the current methods. New procedures for collecting and processing of aqueous samples use the same procedures that are currently (2006) in use except that the samples are now preserved with concentrated hydrochloric acid/bromine monochloride instead of sodium dichromate/nitric acid. Both the 'old' and new methods have the same analyst productivity rates. These similarities should permit easy migration to the new methods. Analysis of geologic and aqueous reference standards using the new methods show that these procedures provide mercury recoveries that are as good as or better than the previously used methods.

Apparatus and method for transient thermal infrared spectrometry

DOEpatents

McClelland, John F.; Jones, Roger W.

1991-12-03

A method and apparatus for enabling analysis of a material (16, 42) by applying a cooling medium (20, 54) to cool a thin surface layer portion of the material and to transiently generate a temperature differential between the thin surface layer portion and the lower portion of the material sufficient to alter the thermal infrared emission spectrum of the material from the black-body thermal infrared emission spectrum of the material. The altered thermal infrared emission spectrum of the material is detected by a spectrometer/detector (28, 50) while the altered thermal infrared emission spectrum is sufficiently free of self-absorption by the material of the emitted infrared radiation. The detection is effected prior to the temperature differential propagating into the lower portion of the material to an extent such that the altered thermal infrared emission spectrum is no longer sufficiently free of self-absorption by the material of emitted infrared radiation, so that the detected altered thermal infrared emission spectrum is indicative of the characteristics relating to the molecular composition of the material.

Slurry sampling high-resolution continuum source electrothermal atomic absorption spectrometry for direct beryllium determination in soil and sediment samples after elimination of SiO interference by least-squares background correction.

PubMed

Husáková, Lenka; Urbanová, Iva; Šafránková, Michaela; Šídová, Tereza

2017-12-01

In this work a simple, efficient, and environmentally-friendly method is proposed for determination of Be in soil and sediment samples employing slurry sampling and high-resolution continuum source electrothermal atomic absorption spectrometry (HR-CS-ETAAS). The spectral effects originating from SiO species were identified and successfully corrected by means of a mathematical correction algorithm. Fractional factorial design has been employed to assess the parameters affecting the analytical results and especially to help in the development of the slurry preparation and optimization of measuring conditions. The effects of seven analytical variables including particle size, concentration of glycerol and HNO 3 for stabilization and analyte extraction, respectively, the effect of ultrasonic agitation for slurry homogenization, concentration of chemical modifier, pyrolysis and atomization temperature were investigated by a 2 7-3 replicate (n = 3) design. Using the optimized experimental conditions, the proposed method allowed the determination of Be with a detection limit being 0.016mgkg -1 and characteristic mass 1.3pg. Optimum results were obtained after preparing the slurries by weighing 100mg of a sample with particle size < 54µm and adding 25mL of 20% w/w glycerol. The use of 1μg Rh and 50μg citric acid was found satisfactory for the analyte stabilization. Accurate data were obtained with the use of matrix-free calibration. The accuracy of the method was confirmed by analysis of two certified reference materials (NIST SRM 2702 Inorganics in Marine Sediment and IGI BIL-1 Baikal Bottom Silt) and by comparison of the results obtained for ten real samples by slurry sampling with those determined after microwave-assisted extraction by inductively coupled plasma time of flight mass spectrometry (TOF-ICP-MS). The reported method has a precision better than 7%. Copyright © 2017 Elsevier B.V. All rights reserved.

Geochemical background of zinc, cadmium and mercury in anthropically influenced soils in a semi-arid zone (SE, Spain)

NASA Astrophysics Data System (ADS)

García-Lorenzo, M. L.; Pérez-Sirvent, C.; Martínez-Sánchez, M. J.; Molina, J.; Tudela, M. L.; Hernández-Córdoba, M.

2009-04-01

This work seeks to establish the geochemical background for three potentially toxic trace elements (Zn, Cd and Hg) in a pilot zone included in the DesertNet project in the province of Murcia. The studied area, known as Campo de Cartagena, Murcia (SE Spain) is an area of intensive agriculture and has been much affected over the years by anthropic activity. The zone can be considered an experimental pilot zone for establishing background levels in agricultural soils. Sixty four samples were collected and corresponded to areas subjected to high and similar agricultural activity or soils with natural vegetation, which correspond to abandoned agricultural areas. The Zn content was determined by flame atomic absorption spectrometry. The Cd content was determined by electrothermal atomization atomic absorption spectrometry and mercury content was determined by atomic fluorescence spectrometry. Geostatistical analysis consisting of kriging and mapping was performed using the geostatistical analyst extension of ArcGIS 8.3. Zinc values ranged from 10 mg kg-1 to 151 mg kg-1, with an average value of 45 mg kg-1. Cadmium values ranged between 0.1 mg kg-1 and 0.9mg kg-1, with a mean value of 0.3 mg kg-1 and mercury values ranged from 0.1 mg kg-1 to 2.3 mg kg-1, with a mean value of 0.5 mg kg-1. At a national level, the Spanish Royal Decree 9/2005 proposes toxicological and statistical approaches to establish background values. According to the statistical approach, background values consist of the median value for the selected element. The background values for Zn, Cd and Hg in the studied area were 40 mg kg-1 for Zn, 0.3 mg kg-1 for Cd and 0.4 mg kg-1 for Hg.

Non linear optical investigations of silver nanoparticles synthesised by curcumin reduction

NASA Astrophysics Data System (ADS)

Dhanya, N. P.

2017-11-01

Metal nanoparticles have considerable applications in assorted fields like medicine, biology, photonics, metallurgy etc. Optical applications of Silver nanoparticles are of significant interest among researchers nowadays. In this paper, we report a single step chemical reduction of silver nanoparticles with Curcumin both as a reducing and stabilising agent at room temperature. Structural, plasmonic and non linear optical properties of the prepared nanoparticles are explored using Scanning Electron Microscope, Transmission Electron Microscope, UV absorption spectrometry, Spectroflurometry and Z scan. UV-Vis absorption studies affirm the Surface Plasmon Resonance (SPR) absorption and spectroflurometric studies announce the emission spectrum of the prepared silvernanoparticles at 520 nm. SEM and TEM images uphold the existence of uniform sized, spherical silvernanoparticles. Nonlinear optical studies are accomplished with the open aperture z scan technique in the nanosecond regime. The nonlinearity is in virtue of saturable absorption, two-photon absorption and excited state absorption. The marked nonlinearity and optical limiting of the Curcumin reduced silvernanoparticles enhances its photonic applications.

Water-chemistry data for selected springs, geysers, and streams in Yellowstone National Park, Wyoming, 1999-2000

USGS Publications Warehouse

Ball, James W.; McCleskey, R. Blaine; Nordstrom, D. Kirk; Holloway, JoAnn M.; Verplanck, Philip L.; Sturtevant, Sabin A.

2002-01-01

Sixty-seven water analyses are reported for samples collected from 44 hot springs and their overflow drainages and two ambient-temperature acid streams in Yellowstone National Park (YNP) during 1990-2000. Thirty-seven analyses are reported for 1999, 18 for June of 2000, and 12 for September of 2000. These water samples were collected and analyzed as part of research investigations in YNP on microbially mediated sulfur oxidation in stream water, arsenic and sulfur redox speciation in hot springs, and chemical changes in overflow drainages that affect major ions, redox species, and trace elements. Most samples were collected from sources in the Norris Geyser Basin. Two ambient-temperature acidic stream systems, Alluvium and Columbine Creeks and their tributaries in Brimstone Basin, were studied in detail. Analyses were performed at or near the sampling site, in an on-site mobile laboratory truck, or later in a USGS laboratory, depending on stability of the constituent and whether or not it could be preserved effectively. Water temperature, specific conductance, pH, Eh, dissolved oxygen (D.O.), and dissolved H2S were determined on-site at the time of sampling. Alkalinity, acidity, and F were determined within a few days of sample collection by titration with acid, titration with base, and ion-selective electrode or ion chromatography (IC), respectively. Concentrations of S2O3 and SxO6 were determined as soon as possible (minutes to hours later) by IC. Concentrations of Br, Cl, NH4, NO2, NO3, SO4, Fe(II), and Fe(total) were determined within a few days of sample collection. Densities were determined later in the USGS laboratory. Concentrations of Li and K were determined by flame atomic absorption spectrometry. Concentrations of Al, As(total), B, Ba, Be, Ca, Cd, Co, Cr, Cu, Fe(total), K, Li, Mg, Mn, Na, Ni, Pb, Se, Si, Sr, V, and Zn were determined by inductively-coupled plasma-optical emission spectrometry. Trace concentrations of Cd, Cr, Cu, Pb, and Sb were determined by Zeeman-corrected graphitefurnace atomic-absorption spectrometry. Trace concentrations of As(total) and As(III) were determined by hydride generation atomic-absorption spectrometry using a flow-injection analysis system. Concentrations of Cl, NO3, Br, and SO4 were determined by IC. Concentrations of Fe(II) and Fe(total) were determined by the ferrozine colorimetric method. Concentrations of NO2 were determined by colorimetry using matrix-matched standards. Concentrations of NH4 were determined by IC, with reanalysis by colorimetry where separation of Na and NH4 peaks was poor. Dissolved organic carbon (DOC) concentrations were determined by the wet persulfate oxidation method.

Effects of gamma-ray irradiation on the optical properties of amorphous Se100-xHgx thin films

NASA Astrophysics Data System (ADS)

Ahmad, Shabir; Islam, Shama; Nasir, Mohd.; Asokan, K.; Zulfequar, M.

2018-06-01

In this study, the thermal quenching technique was employed to prepare bulk samples of Se100-xHgx (x = 0, 5, 10, 15). Thin films with a thickness of ∼250 nm were deposited on glass substrates using the thermal evaporation technique. These films were irradiated with gamma rays at doses of 25-100 kGy. The elemental compositions of the as-deposited thin films were confirmed by energy dispersive X-ray analysis and Rutherford backscattering spectrometry. X-ray diffraction analysis confirmed the crystalline nature of these thin films upto the dose of 75 kGy. Fourier transform-infrared spectroscopy showed that the concentration of defects decreased after gamma irradiation. Microstructural analysis by field emission scanning electron microscopy indicated that the grain size increases after irradiation. Optical study based on spectrophotometry showed that the optical band gap values of these films increase after the addition of Hg whereas they decrease after gamma irradiation. We found that the absorption coefficient increases with doses up to 75 kGy but decreases at higher doses. These remarkable shifts in the optical band gap and absorption coefficient values are interpreted in terms of the creation and annihilation of defects, which are the main effects produced by gamma irradiation.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of arsenic and selenium in water and sediment by graphite furnace atomic absorption spectrometry

USGS Publications Warehouse

Jones, Sandra R.; Garbarino, John R.

1999-01-01

Graphite furnace-atomic absorption spectrometry (GF-AAS) is a sensitive, precise, and accurate technique that can be used to determine arsenic and selenium in samples of water and sediment. The GF-AAS method has been developed to replace the hydride generation-atomic absorption spectrometry (HG-AAS) methods because the method detection limits are similar, bias and variability are comparable, and interferences are minimal. Advantages of the GF-AAS method include shorter sample preparation time, increased sample throughput from simultaneous multielement analysis, reduced amount of chemical waste, reduced sample volume requirements, increased linear concentration range, and the use of a more accurate digestion procedure. The linear concentration range for arsenic and selenium is 1 to 50 micrograms per liter in solution; the current method detection limit for arsenic in solution is 0.9 microgram per liter; the method detection limit for selenium in solution is 1 microgram per liter. This report describes results that were obtained using stop-flow and low-flow conditions during atomization. The bias and variability of the simultaneous determination of arsenic and selenium by GF-AAS under both conditions are supported with results from standard reference materials--water and sediment, real water samples, and spike recovery measurements. Arsenic and selenium results for all Standard Reference Water Samples analyzed were within one standard deviation of the most probable values. Long-term spike recoveries at 6.25, 25.0, 37.5 micrograms per liter in reagent-, ground-, and surface-water samples for arsenic averaged 103 plus or minus 2 percent using low-flow conditions and 104 plus or minus 4 percent using stop-flow conditions. Corresponding recoveries for selenium were 98 plus or minus 13 percent using low-flow conditions and 87 plus or minus 24 percent using stop-flow conditions. Spike recoveries at 25 micrograms per liter in 120 water samples ranged from 97 to 99 percent for arsenic and from 82 to 93 percent for selenium, depending on the flow conditions used. Statistical analysis of dissolved and whole-water recoverable analytical results for the same set of water samples indicated that there is no significant difference between the GF-AAS and HG-AAS methods. Interferences related to various chemical constituents were also identified. Although sulfate and chloride in association with various cations might interfere with the determination of arsenic and selenium by GF-AAS, the use of a magnesium nitrate/palladium matrix modifier and low-flow argon during atomization helped to minimize such interferences. When using stabilized temperature platform furnace conditions where stop flow is used during atomization, the addition of hydrogen (5 percent volume/volume) to the argon minimized chemical interferences. Nevertheless, stop flow during atomization was found to be less effective than low flow in reducing interference effects.

Determination of Total Selenium in Infant Formulas: Comparison of the Performance of FIA and MCFA Flow Systems

PubMed Central

Pistón, Mariela; Knochen, Moisés

2012-01-01

Two flow methods, based, respectively, on flow-injection analysis (FIA) and on multicommutated flow analysis (MCFA), were compared with regard to their use for the determination of total selenium in infant formulas by hydride-generation atomic absorption spectrometry. The method based on multicommutation provided lower detection and quantification limits (0.08 and 0.27 μg L−1 compared to 0.59 and 1.95 μ L−1, resp.), higher sampling frequency (160 versus. 70 samples per hour), and reduced reagent consumption. Linearity, precision, and accuracy were similar for the two methods compared. It was concluded that, while both methods proved to be appropriate for the purpose, the MCFA-based method exhibited a better performance. PMID:22505923

Mapping of lead, magnesium and copper accumulation in plant tissues by laser-induced breakdown spectroscopy and laser-ablation inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Kaiser, J.; Galiová, M.; Novotný, K.; Červenka, R.; Reale, L.; Novotný, J.; Liška, M.; Samek, O.; Kanický, V.; Hrdlička, A.; Stejskal, K.; Adam, V.; Kizek, R.

2009-01-01

Laser-Induced Breakdown Spectroscopy (LIBS) and Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) were utilized for mapping the accumulation of Pb, Mg and Cu with a resolution up to 200 μm in a up to cm × cm area of sunflower ( Helianthus annuus L.) leaves. The results obtained by LIBS and LA-ICP-MS are compared with the outcomes from Atomic Absorption Spectrometry (AAS) and Thin-Layer Chromatography (TLC). It is shown that laser-ablation based analytical methods can substitute or supplement these techniques mainly in the cases when a fast multi-elemental mapping of a large sample area is needed.

Application of chitosan and its N-heterocyclic derivatives for preconcentration of noble metal ions and their determination using atomic absorption spectrometry.

PubMed

Azarova, Yu A; Pestov, A V; Ustinov, A Yu; Bratskaya, S Yu

2015-12-10

Chitosan and its N-heterocyclic derivatives N-2-(2-pyridyl)ethylchitosan (2-PEC), N-2-(4-pyridyl) ethylchitosan (4-PEC), and N-(5-methyl-4-imidazolyl) methylchitosan (IMC) have been applied in group preconcentration of gold, platinum, and palladium for subsequent determination by atomic absorption spectroscopy (AAS) in solutions with high background concentrations of iron and sodium ions. It has been shown that the sorption mechanism, which was elucidated by XPS, significantly influences the sorption capacity of materials, the efficiency of metal ions elution after preconcentration, and, as a result, the accuracy of metal determination by AAS. We have shown that native chitosan was not suitable for preconcentration of Au(III), if the elution step was used as a part of the analysis scheme. The group preconcentration of Au(III), Pd(II), and Pt(IV) with subsequent quantitative elution using 0.1M HCl/1M thiourea solution was possible only on IMC and 4-PEC. Application of IMC for analysis of the national standard quartz ore sample proved that gold could be accurately determined after preconcentration/elution with the recovery above 80%. Copyright © 2015 Elsevier Ltd. All rights reserved.

Quantitative analysis of a brass alloy using CF-LIBS and a laser ablation time-of-flight mass spectrometer

NASA Astrophysics Data System (ADS)

Ahmed, Nasar; Abdullah, M.; Ahmed, Rizwan; Piracha, N. K.; Aslam Baig, M.

2018-01-01

We present a quantitative analysis of a brass alloy using laser induced breakdown spectroscopy, energy dispersive x-ray spectroscopy (EDX) and laser ablation time-of-flight mass spectrometry (LA-TOF-MS). The emission lines of copper (Cu I) and zinc (Zn I), and the constituent elements of the brass alloy were used to calculate the plasma parameters. The plasma temperature was calculated from the Boltzmann plot as (10 000  ±  1000) K and the electron number density was determined as (2.0  ±  0.5)  ×  1017 cm-3 from the Stark-broadened Cu I line as well as using the Saha-Boltzmann equation. The elemental composition was deduced using these techniques: the Boltzmann plot method (70% Cu and 30% Zn), internal reference self-absorption correction (63.36% Cu and 36.64% Zn), EDX (61.75% Cu and 38.25% Zn), and LA-TOF (62% Cu and 38% Zn), whereas, the certified composition is (62% Cu and 38% Zn). It was observed that the internal reference self-absorption correction method yields analytical results comparable to that of EDX and LA-TOF-MS.

A DNA-Encapsulated and Fluorescent Ag 10 6+ Cluster with a Distinct Metal-Like Core

DOE Office of Scientific and Technical Information (OSTI.GOV)

Petty, Jeffrey T.; Ganguly, Mainak; Rankine, Ian J.

Silver cluster–DNA complexes are optical chromophores, and pairs of these conjugates can be toggled from fluorescently dim to bright states using DNA hybridization. This paper highlights spectral and structural differences for a specific cluster pair. We have previously characterized a cluster with low emission and violet absorption that forms a compact structure with single-stranded oligonucleotides. We now consider its counterpart with blue absorption and strong green emission. This cluster develops with a single-stranded/duplex DNA construct and is favored by low silver concentrations with ≲8 Ag+:DNA, an oxygen atmosphere, and neutral pH. The resulting cluster displays key signatures of a molecularmore » metal with well-defined absorption/emission bands at 490/550 nm, and with a fluorescence quantum yield of 15% and lifetime of 2.4 ns. The molecular cluster conjugates with the larger DNA host because it chromatographically elutes with the DNA and it exhibits circular dichroism. The silver cluster is identified as Ag106+ using two modes of mass spectrometry and elemental analysis. Our key finding is that it adopts a low-dimensional shape, as determined from a Ag K-edge extended X-ray absorption fine structure analysis. The Ag0 in this oxidized cluster segregates from the Ag+ via a sparse number of metal-like bonds and a denser network of silver–DNA bonds. This structure contrasts with the compact, octahedral-like shape of the violet counterpart to the blue cluster, which is also a Ag106+ species. We consider that the blue- and violet-absorbing clusters may be isomers with shapes that are controlled by the secondary structures of their DNA templates.« less

Improved high-intensity microwave discharge lamp for atomic resonance absorption and fluorescence spectrometry.

PubMed

Lifshitz, A; Skinner, G B; Wood, D R

1978-09-01

An unusually good combination of high intensity and narrow line has been achieved in a microwave discharge lamp by placing the optical window in the center of the microwave cavity. Construction details and performance characteristics are described.

CaI and SrI molecules for iodine determination by high-resolution continuum source graphite furnace molecular absorption spectrometry: Greener molecules for practical application.

PubMed

Zanatta, Melina Borges Teixeira; Nakadi, Flávio Venâncio; da Veiga, Márcia Andreia Mesquita Silva

2018-03-01

A new method to determine iodine in drug samples by high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS) has been developed. The method measures the molecular absorption of a diatomic molecule, CaI or SrI (less toxic molecule-forming reagents), at 638.904 or 677.692nm, respectively, and uses a mixture containing 5μg of Pd and 0.5μg of Mg as chemical modifier. The method employs pyrolysis temperatures of 1000 and 800°C and vaporization temperatures of 2300 and 2400°C for CaI and SrI, respectively. The optimized amounts of Ca and Sr as molecule-forming reagents are 100 and 150µg, respectively. On the basis of interference studies, even small chlorine concentrations reduce CaI and SrI absorbance significantly. The developed method was used to analyze different commercial drug samples, namely thyroid hormone pills with three different iodine amounts (15.88, 31.77, and 47.66µg) and one liquid drug with 1% m v -1 active iodine in their compositions. The results agreed with the values informed by the manufacturers (95% confidence level) regardless of whether CaI or SrI was determined. Therefore, the developed method is useful for iodine determination on the basis of CaI or SrI molecular absorption. Copyright © 2017 Elsevier B.V. All rights reserved.

Comparison between design and installed acoustic characteristics of NASA Lewis 9- by 15-foot low-speed wind tunnel acoustic treatment

NASA Technical Reports Server (NTRS)

Dahl, Milo D.; Woodward, Richard P.

1990-01-01

The test section of the NASA Lewis 9- by 15-Foot Low-Speed Wind Tunnel was acoustically treated to allow the measurement of sound under simulated free-field conditions. The treatment was designed for high sound absorption at frequencies above 250 Hz and for withstanding the environmental conditions in the test section. In order to achieve the design requirements, a fibrous, bulk-absorber material was packed into removable panel sections. Each section was divided into two equal-depth layers packed with material to different bulk densities. The lower density was next to the facing of the treatment. The facing consisted of a perforated plate and screening material layered together. Sample tests for normal-incidence acoustic absorption were also conducted in an impedance tube to provide data to aid in the treatment design. Tests with no airflow, involving the measurement of the absorptive properties of the treatment installed in the 9- by 15-foot wind tunnel test section, combined the use of time-delay spectrometry with a previously established free-field measurement method. This new application of time-delay spectrometry enabled these free-field measurements to be made in nonanechoic conditions. The results showed that the installed acoustic treatment had absorption coefficients greater than 0.95 over the frequency range 250 Hz to 4 kHz. The measurements in the wind tunnel were in good agreement with both the analytical prediction and the impedance tube test data.

On-line ion-exchange preconcentration and determination of traces of platinum by electrothermal atomic absorption spectrometry.

PubMed

González García, M M; Sánchez Rojas, F; Bosch Ojeda, C; García de Torres, A; Cano Pavón, J M

2003-04-01

A method to determine trace amounts of platinum in different samples based on electrothermal atomic absorption spectrometry is described. The preconcentration step is performed on a chelating resin microcolumn [1,5-bis(2-pyridyl)-3-sulfophenyl methylene thiocarbonohydrazide (PSTH) immobilized on an anion-exchange resin (Dowex 1x8-200)] placed in the autosampler arm. The combination of a peristaltic pump for sample loading and the atomic absorption spectrometer pumps for elution through a selection valve simplifies the hardware. The peristaltic pump and the selection valve are easily controlled electronically with two switches placed in the autosampler, which are activated when the autosampler arm is down. Thus, the process is fully automated without any modification of the software of the atomic absorption spectrometer. Under the optimum conditions with a 60-s preconcentration time, a sample flow rate of 2.4 mL min(-1), and an injection volume of eluent of 40 microL, a linear calibration graph was obtained in the range 0-100 ng mL(-1). The enrichment factor was 14. The detection limit under these conditions is 1 ng mL(-1), and the relative standard deviation (RSD) is 1.6% for 10 ng mL(-1) of Pt. The method has been applied to the determination of platinum in catalyst, vegetation, soil, and natural water samples. The results showed good agreement with the certified value and the recoveries of Pt added to samples were 98-105%.

Analysis of coke beverages by total-reflection X-ray fluorescence

NASA Astrophysics Data System (ADS)

Fernández-Ruiz, Ramón; von Bohlen, Alex; Friedrich K, E. Josue; Redrejo, M. J.

2018-07-01

The influence of the organic content, sample preparation process and the morphology of the depositions of two types of Coke beverage, traditional and light Coke, have been investigated by mean of Total-reflection X-ray Fluorescence (TXRF) spectrometry. Strong distortions of the nominal concentration values, up to 128% for P, have been detected in the analysis of traditional Coke by different preparation methods. These differences have been correlated with the edge X-ray energies of the elements analyzed being more pronounced for the lighter elements. The influence of the organic content (mainly sugar) was evaluated comparing traditional and light Coke analytical TXRF results. Three sample preparation methods have been evaluated as follows: direct TXRF analysis of the sample only adding internal standard, TXRF analysis after open vessel acid digestion and TXRF analysis after high pressure and temperature microwave-assisted acid digestion. Strong correlations were detected between quantitative results, methods of preparation and energies of the X-ray absorption edges of quantified elements. In this way, a decay behavior for the concentration differences between preparation methods and the energies of the X-ray absorption edges of each element were observed. The observed behaviors were modeled with exponential decay functions obtaining R2 correlation coefficients from 0.989 to 0.992. The strong absorption effect observed, and even possible matrix effect, can be explained by the inherent high organic content of the evaluated samples and also by the morphology and average thickness of the TXRF depositions observed. As main conclusion of this work, the analysis of light elements in samples with high organic content by TXRF, i.e. medical, biological, food or any other organic matrixes should be taken carefully. In any case, the direct analysis is not recommended and a previous microwave-assisted acid digestion, or similar, is mandatory, for the correct elemental quantification by TXRF.

Flow injection for the determination of Se(IV) and Se(VI) by hydride generation atomic absorption spectrometry with microwave oven on-line prereduction of Se(VI) to Se(IV)

NASA Astrophysics Data System (ADS)

Burguera, J. L.; Carrero, P.; Burguera, M.; Rondon, C.; Brunetto, M. R.; Gallignani, M.

1996-12-01

An on-line flow injection system has been developed for the selective determination of Se(IV) and Se(VI) in citric fruit juices and geothermal waters by hydride generation atomic absorption spectrometry with microwave-aided heating prereduction of Se(VI) to Se(IV). The samples and the prereductant solutions (4 mol l -1 HCl for Se(IV) and 12 mol l -1 HCl for Se(VI)) which circulated in a closed-flow circuit were injected by means of a time-based injector. This mixture was displaced by a carrier solution of 1% v/v of hydrochloric acid through a PTFE coil located inside the focused microwave oven and mixed downstream with a borohydride solution to generate the hydride. The linear ranges were 0-120 and 0-100 μg l -1 of Se(IV) and Se(VI), respectively. The detection limits were 1.0 μg l -1 for Se(IV) and 1.5 μg l -1 for Se(VI). The precision (about 2.0-2.5% RSD) and recoveries (96-98% for Se(IV) and 94-98% for Se(VI)) were good. Total selenium values were also obtained by electrothermal atomic absorption spectrometry which agreed with the content of both selenium species. The sample throughput was about 50 measurements per hour. The main advantage of the method is that the selective determination of Se(IV) and Se(VI) in citric fruit juices and geothermal waters is performed in a closed system with a minimum sample manipulation, exposure to the environment, minimum sample waste and operator attention.

Fabrication of a Dipole-assisted Solid Phase Extraction Microchip for Trace Metal Analysis in Water Samples

PubMed Central

Chen, Ping-Hung; Chen, Shun-Niang; Tseng, Sheng-Hao; Deng, Ming-Jay; Lin, Yang-Wei; Sun, Yuh-Chang

2016-01-01

This paper describes a fabrication protocol for a dipole-assisted solid phase extraction (SPE) microchip available for trace metal analysis in water samples. A brief overview of the evolution of chip-based SPE techniques is provided. This is followed by an introduction to specific polymeric materials and their role in SPE. To develop an innovative dipole-assisted SPE technique, a chlorine (Cl)-containing SPE functionality was implanted into a poly(methyl methacrylate) (PMMA) microchip. Herein, diverse analytical techniques including contact angle analysis, Raman spectroscopic analysis, and laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) analysis were employed to validate the utility of the implantation protocol of the C-Cl moieties on the PMMA. The analytical results of the X-ray absorption near-edge structure (XANES) analysis also demonstrated the feasibility of the Cl-containing PMMA used as an extraction medium by virtue of the dipole-ion interactions between the highly electronegative C-Cl moieties and the positively charged metal ions. PMID:27584954

Nonlinear absorption of short intense laser pulse in multispecies plasma

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kargarian, A.; Hajisharifi, K.; Mehdian, H.

In the present paper, the detailed investigation concerning the effect of inclusion of heavy negative ions into the finite background plasma on the laser absorption has been carried out by employing particle-in-cell simulation method. For this purpose, in this configuration, the laser energy absorption relying on the nonlinear phenomena such as phase-mixing, wave-breaking, and scattering has been studied in the Raman-Brillouin regime. It is shown that the inclusion of heavy negative ions suppresses the scattering while increases the phase-mixing time. Moreover, it is illustrated that this inclusion can increase the laser absorption in finite plasma environment, after saturation. The obtainedmore » results are expected to be relevant to the experiments on the mass spectrometry with laser desorption techniques as well as on the laser-plasma interaction with application to particles acceleration.« less

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

PubMed

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.

Antibiotic toxicity and absorption in zebrafish using liquid chromatography-tandem mass spectrometry.

PubMed

Zhang, Fan; Qin, Wei; Zhang, Jing-Pu; Hu, Chang-Qin

2015-01-01

Evaluation of drug toxicity is necessary for drug safety, but in vivo drug absorption is varied; therefore, a rapid, sensitive and reliable method for measuring drugs is needed. Zebrafish are acceptable drug toxicity screening models; we used these animals with a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method in a multiple reaction monitoring mode to quantify drug uptake in zebrafish to better estimate drug toxicity. Analytes were recovered from zebrafish homogenate by collecting supernatant. Measurements were confirmed for drugs in the range of 10-1,000 ng/mL. Four antibiotics with different polarities were tested to explore any correlation of drug polarity, absorption, and toxicity. Zebrafish at 3 days post-fertilization (dpf) absorbed more drug than those at 6 h post-fertilization (hpf), and different developmental periods appeared to be differentially sensitive to the same compound. By observing abnormal embryos and LD50 values, zebrafish embryos at 6 hpf were considered to be suitable for evaluating embryotoxicity. Also, larvae at 3 dpf were adapted to measure acute drug toxicity in adult mammals. Thus, we can exploit zebrafish to study drug toxicity and can reliably quantify drug uptake with LC-MS/MS. This approach will be helpful for future studies of toxicology in zebrafish.

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).

PubMed

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.

Determination of trace concentrations of chlorine in aqueous solutions by high-resolution continuum source graphite furnace molecular absorption spectrometry

NASA Astrophysics Data System (ADS)

Machyňák, Ľubomír; Čacho, František; Němeček, Martin; Beinrohr, Ernest

2016-11-01

Trace concentrations of total chlorine were determined by means of molecular absorption of indium mono-chloride (InCl) at 267.217 nm using high-resolution continuum source graphite furnace molecular absorption spectrometry. The effects of chemical modifiers and the amount of In on the sensitivity and accuracy were investigated. The optimum pyrolysis and vaporization temperatures were 600 °C and 1400 °C, respectively. The limit of detection and characteristic mass were found to be 0.10 ng and 0.21 ng, respectively. Potential non-spectral and spectral interferences were tested for various metals and non-metals at concentrations up to 50 mg L- 1 and for phosphoric, sulphuric and nitric acids. No spectral interferences were observed. Significant non-spectral interferences were observed with F, Br, and I at concentrations higher than 1 mg L- 1, 5 mg L- 1 and 25 mg L- 1, respectively, which is probably caused by formation of competitive indium halogen molecules. Higher concentrations of mineral acids depressed the signal owing to the formation of volatile HCl. The calibration curve was linear in the range between 0.3 and 10 ng with a correlation coefficient of R = 0.993. The elaborated method was used for the chlorine determination in various waters and a drug sample.

Volatile Organic Silicon Compounds in Biogases: Development of Sampling and Analytical Methods for Total Silicon Quantification by ICP-OES

PubMed Central

Julien, Jennifer; Dumont, Nathalie; Lebouil, David; Germain, Patrick

2014-01-01

Current waste management policies favor biogases (digester gases (DGs) and landfill gases (LFGs)) valorization as it becomes a way for energy politics. However, volatile organic silicon compounds (VOSiCs) contained into DGs/LFGs severely damage combustion engines and endanger the conversion into electricity by power plants, resulting in a high purification level requirement. Assessing treatment efficiency is still difficult. No consensus has been reached to provide a standardized sampling and quantification of VOSiCs into gases because of their diversity, their physicochemical properties, and the omnipresence of silicon in analytical chains. Usually, samplings are done by adsorption or absorption and quantification made by gas chromatography-mass spectrometry (GC-MS) or inductively coupled plasma-optical emission spectrometry (ICP-OES). In this objective, this paper presents and discusses the optimization of a patented method consisting in VOSiCs sampling by absorption of 100% ethanol and quantification of total Si by ICP-OES. PMID:25379538

Impurity profiling of liothyronine sodium by means of reversed phase HPLC, high resolution mass spectrometry, on-line H/D exchange and UV/Vis absorption.

PubMed

Ruggenthaler, M; Grass, J; Schuh, W; Huber, C G; Reischl, R J

2017-09-05

For the first time, a comprehensive investigation of the impurity profile of the synthetic thyroid API (active pharmaceutical ingredient) liothyronine sodium (LT 3 Na) was performed by using reversed phase HPLC and advanced structural elucidation techniques including high resolution tandem mass spectrometry (HRMS/MS) and on-line hydrogen-deuterium (H/D) exchange. Overall, 39 compounds were characterized and 25 of these related substances were previously unknown to literature. The impurity classification system recently developed for the closely related API levothyroxine sodium (LT 4 Na) could be applied to the newly characterized liothyronine sodium impurities resulting in a wholistic thyroid API impurity classification system. Furthermore, the mass-spectrometric CID-fragmentation of specific related substances was discussed and rationalized by detailed fragmentation pathways. Moreover, the UV/Vis absorption characteristics of the API and selected impurities were investigated to corroborate chemical structure assignments derived from MS data. Copyright © 2017 Elsevier B.V. All rights reserved.

Discussion of parameters associated with the determination of arsenic by electrothermal atomic absorption spectrometry in slurried environmental samples.

PubMed

Vassileva, E; Baeten, H; Hoenig, M

2001-01-02

A slurry sampling-fast program procedure has been developed for the determination of arsenic in plants, soils and sediments by electrothermal atomic absorption spectrometry. Efficiencies of various single and mixed modifiers for thermal stabilization of arsenic and for a better removal of the matrix during pyrolysis step were compared. The influence of the slurry concentration, amounts of modifier and parameters of the pyrolysis step on the As integrated absorbance signals have been studied and a comparison between fast and conventional furnace programs was also made. The ultrasonic agitation of the slurry followed by a fast electrothermal program using an Ir/Mg modifier provides the most consistent performance in terms of precision and accuracy. The reliability of the whole procedure has been compared with results obtained after application of a wet digestion method with an HF step and validated by analyzing eleven certified reference materials. Arsenic detection and quantitation limits expressed on dry sample matter were about 30 and 100 micrograms kg-1, respectively.

[Determination of trace gallium by graphite furnace atomic absorption spectrometry in urine].

PubMed

Zhou, L Z; Fu, S; Gao, S Q; He, G W

2016-06-20

To establish a method for determination trace gallium in urine by graphite furnace atomic absorption spectrometry (GFAAS). The ammonium dihydrogen phosphate was matrix modifier. The temperature effect about pyrolysis (Tpyr) and atomization temperature were optimized for determination of trace gallium. The method of technical standard about within-run, between-run and recoveries of standard were optimized. The method showed a linear relationship within the range of 0.20~80.00 μg/L (r=0.998). The within-run and between-run relative standard deviations (RSD) of repetitive measurement at 5.0, 10.0, 20.0 μg/L concentration levels were 2.1%~5.5% and 2.3%~3.0%. The detection limit was 0.06 μg/L. The recoveries of gallium were 98.2%~101.1%. This method is simple, low detection limit, accurate, reliable and reproducible. It has been applied for determination of trace gallium in urine samples those who need occupation health examination or poisoning diagnosis.

Volatile organic silicon compounds in biogases: development of sampling and analytical methods for total silicon quantification by ICP-OES.

PubMed

Chottier, Claire; Chatain, Vincent; Julien, Jennifer; Dumont, Nathalie; Lebouil, David; Germain, Patrick

2014-01-01

Current waste management policies favor biogases (digester gases (DGs) and landfill gases (LFGs)) valorization as it becomes a way for energy politics. However, volatile organic silicon compounds (VOSiCs) contained into DGs/LFGs severely damage combustion engines and endanger the conversion into electricity by power plants, resulting in a high purification level requirement. Assessing treatment efficiency is still difficult. No consensus has been reached to provide a standardized sampling and quantification of VOSiCs into gases because of their diversity, their physicochemical properties, and the omnipresence of silicon in analytical chains. Usually, samplings are done by adsorption or absorption and quantification made by gas chromatography-mass spectrometry (GC-MS) or inductively coupled plasma-optical emission spectrometry (ICP-OES). In this objective, this paper presents and discusses the optimization of a patented method consisting in VOSiCs sampling by absorption of 100% ethanol and quantification of total Si by ICP-OES.

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

PubMed

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.

Temperature-controlled electrothermal atomization-atomic absorption spectrometry using a pyrometric feedback system in conjunction with a background monitoring device

NASA Astrophysics Data System (ADS)

Van Deijck, W.; Roelofsen, A. M.; Pieters, H. J.; Herber, R. F. M.

The construction of a temperature-controlled feedback system for electrothermal atomization-atomic absorption spectrometry (ETA-AAS) using an optical pyrometer applied to the atomization stage is described. The system was used in conjunction with a fast-response background monitoring device. The heating rate of the furnace amounted to 1400° s -1 with a reproducibility better than 1%. The precision of the temperature control at a steady state temperature of 2000°C was 0.1%. The analytical improvements offered by the present system have been demonstrated by the determination of cadmium and lead in blood and finally by the determination of lead in serum. Both the sensitivity and the precision of the method have been improved. The accuracy of the method was checked by determining the lead content for a number of scrum samples both by ETA-AAS and differential pulse anodic stripping voltametry (DPASV) and proved to be satisfactory.

Development of a certified reference material (NMIJ CRM 7505-a) for the determination of trace elements in tea leaves.

PubMed

Zhu, Yanbei; Narukawa, Tomohiro; Inagaki, Kazumi; Kuroiwa, Takayoshi; Chiba, Koichi

2011-01-01

A certified reference material (CRM) for trace elements in tea leaves has been developed in National Metrology Institute of Japan (NMIJ). The CRM was provided as a dry powder (<90 µm) after frozen pulverization of washed and dried fresh tea leaves from a tea plant farm in Shizuoka Prefecture, Japan. Characterization of the property value for each element was carried out exclusively by NMIJ with at least two independent analytical methods, including inductively coupled plasma mass spectrometry (ICP-MS), high-resolution (HR-) ICP-MS, isotope-dilution (ID-) ICP-MS, inductively coupled plasma optical emission spectrometry (ICP-OES), graphite-furnace atomic-absorption spectrometry (GF-AAS) and flame atomic-absorption spectrometry (FAAS). Property values were provided for 19 elements (Ca, K, Mg, P, Al, B, Ba, Cd, Cu, Fe, Li, Mn, Na, Ni, Pb, Rb, Sr, Zn and Co) and informative values for 18 elements (Ti, V, Cr, Y, and all of the lanthanides, except for Pm whose isotopes are exclusively radioactive). The concentration ranges of property values and informative values were from 1.59% (mass) of K to 0.0139 mg kg(-1) of Cd and from 0.6 mg kg(-1) of Ti to 0.0014 mg kg(-1) of Lu, respectively. Combined relatively standard uncertainties of the property values were estimated by considering the uncertainties of the homogeneity, analytical methods, characterization, calibration standard, and dry-mass correction factor. The range of the relative combined standard uncertainties was from 1.5% of Mg and K to 4.1% of Cd.

[Research progress on identification and quality evaluation of glues medicines].

PubMed

Li, Hui-Hu; Ren, Gang; Chen, Li-Min; Zhong, Guo-Yue

2018-01-01

Glues medicines is a special kind of traditional Chinese medicine.As the market demand is large, the raw materials are in short supply and lacks proper quality evaluation technology, which causes inconsistent quality of products on the market. Its authentic identification and evaluation stay a problem to be solved. In this paper, the research progress of the methods and techniques of the evaluation of the identification and quality of glues medicines were reviewed. The researches of medicinal glue type identification and quality evaluation mainly concentrated in four aspects of medicinal materials of physical and chemical properties, trace elements, organic chemicals and biological genetic methods and techniques. The methods of physicochemical properties include thermal analysis, gel electrophoresis, isoelectric focusing electrophoresis, infrared spectroscopy, gel exclusion chromatography, and circular dichroism. The methods including atomic absorption spectrometry, X-ray fluorescence spectrometry, plasma emission spectrometry and visible spectrophotometry were used for the study of the trace elements of glues medicines. The organic chemical composition was studied by methods of composition of amino acids, content detection, odor detection, lipid soluble component, organic acid detection. Methods based on the characteristics of biogenetics include DNA, polypeptide and amino acid sequence difference analysis. Overall, because of relative components similarity of the glues medicines (such as amino acids, proteins and peptides), its authenticity and quality evaluation index is difficult to judge objectively, all sorts of identification evaluation methods have different characteristics, but also their limitations. It indicates that further study should focus on identification of evaluation index and various technology integrated application combining with the characteristics of the production process. Copyright© by the Chinese Pharmaceutical Association.

Implications for Metabolite Quantification by Mass Spectrometry in the Absence of Authentic Standards.

PubMed

Hatsis, Panos; Waters, Nigel J; Argikar, Upendra A

2017-05-01

Quantification of metabolites by mass spectrometry in the absence of authentic reference standards or without a radiolabel is often called "semiquantitative," which acknowledges that mass spectrometric responses are not truly quantitative. For many researchers, it is tempting to pursue this practice of semiquantification in early drug discovery and even preclinical development, when radiolabeled absorption, distribution, metabolism, and excretion studies are being deferred to later stages of drug development. The caveats of quantifying metabolites based on parent drug response are explored in this investigation. A set of 71 clinically relevant drugs/metabolites encompassing common biotransformation pathways was subjected to flow injection analysis coupled with electrospray ionization (ESI) mass spectrometry. The results revealed a large variation in ESI response even for structurally similar parent drug/metabolite pairs. The ESI response of each metabolite was normalized to that of the parent drug to generate an ESI relative response factor. Overall, relative response factors ranged from 0.014 (>70-fold lower response than parent) to 8.6 (8.6-fold higher response than parent). Various two-dimensional molecular descriptors were calculated that describe physicochemical, topological, and structural properties for each drug/metabolite. The molecular descriptors, along with the ESI response factors, were used in univariate analyses as well as a principal components analysis to ascertain which molecular descriptors best account for the observed discrepancies in drug/metabolite ESI response. This investigation has shown that the practice of using parent drug response to quantify metabolites should be used with caution. Copyright © 2017 by The American Society for Pharmacology and Experimental Therapeutics.

High-melting point sediment from refined coconut oil stored in a tank for a long term.

PubMed

Mochida, Yoshiyuki; Hasegawa, Fukiko

2008-01-01

A small amount of sediment occurs in refined coconut oil stored in a large-scale tank for a long term. This sediment is different from that generally called Cocos Wax, is insoluble in various organic solvents, and has an m.p. of about 100 degrees C. In this report, we have done a structural analysis of this sediment. The sediment was carried out by hydrolyzing with a KOH/ethyl alcohol solution including toluene. Samples were analyzed by elemental analysis, IR spectroscopy, EI-MS, CI-MS, field desorption mass spectrometry (FD-MS), and MALDI/TOF-MS. The hydrolyzates were a compound including an oxo group, and its relative molecular mass was 382 for the acid part and 412 for the unsaponified matter according to EI-MS (ionization energy was 70 eV and 15 eV) and CI-MS (reagent gases were i-butane, ammonia, and nitrogen monoxide). The relative molecular mass of the sediment was 1140 according to the mass spectrometry of FD, EI, and MALDI. It was elucidated based on the characteristic absorption analysis by IR and the fragmentation behavior of the EI-MS that the sediment was a wax ester, 3, 9-di-9-oxotetradocosanecarboxy-11-oxohexacosane, consisting of an acid part of 9-oxotetradocosanecarboxylic acid and an unsaponified matter of 3, 9-di-hydroxy-11-oxohexacosane.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Thomas, Sylvia -Monique; Wilson, Kathryn; Koch-Muller, Monika

Majoritic garnet, characterized by an excess of silicon (>3 Si per formula unit), is considered one of the major phases of the Earth’s transition zone from 410-660 km depth. Quantifying the H 2O content of nominally anhydrous mantle minerals is necessary to evaluate their water storage capacity from experiments and modeling the Earth’s deep water cycle. We present mineral-specific infrared absorption coefficients for the purpose of quantifying the amount of water incorporated into majorite as hydroxyl point defects. A suite of majoritic garnet samples with varying proportions of Si, Fe, Al, Cr and H 2O was synthesized at conditions ofmore » 18-19 GPa and 1500-1800°C. Single-crystals were characterized using X-ray diffraction, electron microprobe analysis, secondary Ion Mass spectrometry (SIMS), IR, Raman and Mössbauer spectroscopy. We utilize SIMS and Raman spectroscopy in combination with IR spectroscopy to provide IR absorption coefficients for water in majoritic garnets with the general mineral formula (Mg,Fe) 3(Si,Mg,Fe,Al,Cr) 2[SiO4] 3. Furthermore, the IR absorption coefficient for majoritic garnet in the OH stretching region is frequency-dependent and ranges from 10 470 ± 3100 Lmol-1cm-2 to 23 400 ± 2300 Lmol -1cm -2.« less

Determination of bioactive components in Chinese herbal formulae and pharmacokinetics of rhein in rats by UPLC-MS/MS.

PubMed

Hou, Mei-Ling; Chang, Li-Wen; Lin, Chi-Hung; Lin, Lie-Chwen; Tsai, Tung-Hu

2014-04-02

Rhein (4,5-dihydroxy-9,10-dioxoanthracene-2-carboxylic acid, cassic acid) is a pharmacological active component found in Rheum palmatum L. the major herb of San-Huang-Xie-Xin-Tang (SHXXT), a medicinal herbal product used as a remedy for constipation. Here we have determined multiple bioactive components in SHXXT and investigated the comparative pharmacokinetics of rhein in rats. A sensitive and specific method combining liquid chromatography with electrospray ionization tandem mass spectrometry has been developed and validated to simultaneously quantify six active compounds in the pharmaceutical herbal product SHXXT to further study their pharmacokinetics in rats. Multiple reaction monitoring (MRM) was employed for quantification with switching electrospray ion source polarity between positive and negative modes in a single run. There were no significant matrix effects in the quantitative analysis and the mean recovery for rhein in rat plasma was 91.6%±3.4%. The pharmacokinetic data of rhein demonstrate that the herbal formulae or the single herbal extract provide significantly higher absorption rate than the pure compound. This phenomenon suggests that the other herbal ingredients of SHXXT and rhubarb extract significantly enhance the absorption of rhein in rats. In conclusion, the herbal formulae (SHXXT) are more efficient than the single herb (rhubarb) or the pure compound (rhein) in rhein absorption.

Quantification of water in majoritic garnet

DOE PAGES

Thomas, Sylvia -Monique; Wilson, Kathryn; Koch-Muller, Monika; ...

2015-05-01

Majoritic garnet, characterized by an excess of silicon (>3 Si per formula unit), is considered one of the major phases of the Earth’s transition zone from 410-660 km depth. Quantifying the H 2O content of nominally anhydrous mantle minerals is necessary to evaluate their water storage capacity from experiments and modeling the Earth’s deep water cycle. We present mineral-specific infrared absorption coefficients for the purpose of quantifying the amount of water incorporated into majorite as hydroxyl point defects. A suite of majoritic garnet samples with varying proportions of Si, Fe, Al, Cr and H 2O was synthesized at conditions ofmore » 18-19 GPa and 1500-1800°C. Single-crystals were characterized using X-ray diffraction, electron microprobe analysis, secondary Ion Mass spectrometry (SIMS), IR, Raman and Mössbauer spectroscopy. We utilize SIMS and Raman spectroscopy in combination with IR spectroscopy to provide IR absorption coefficients for water in majoritic garnets with the general mineral formula (Mg,Fe) 3(Si,Mg,Fe,Al,Cr) 2[SiO4] 3. Furthermore, the IR absorption coefficient for majoritic garnet in the OH stretching region is frequency-dependent and ranges from 10 470 ± 3100 Lmol-1cm-2 to 23 400 ± 2300 Lmol -1cm -2.« less

Determination of the δ2H and δ18O of soil water and water in plant matter; RSIL lab code 1700

USGS Publications Warehouse

Revesz, Kinga M.; Buck, Bryan; Coplen, Tyler B.

2012-01-01

The purpose of the Reston Stable Isotope Laboratory lab code 1700 is to determine the δ2H/1H), abbreviated as δ2H, and the δ18O/16O), abbreviated as δ18O, of soil water and water in plant matter. This method is based on the observation that water and toluene form an azeotropic mixture at 84.1 °C. This temperature is substantially lower than the boiling points of water (100 °C) and toluene (110 °C), but water and toluene are immiscible at ambient temperature. The water content of a soil or plant is determined by weighing, drying, and reweighing a small amount of sample. Sufficient sample to collect 3 to 5 milliliters of water after distillation is loaded into a distillation flask. Sufficient toluene is added so that the sample is immersed throughout the entire distillation to minimize evaporation of water, which would affect the δ2H and δ18O values. The mixture of sample and toluene is heated in a flask to its boiling point (84.1 °C) so that water from the sample and toluene can distill together into a specially designed collection funnel. The temperature of 84.1 °C is maintained until the water has been quantitatively transferred to the collection funnel, at which time the temperature is raised to the boiling point of the remaining component (toluene, 110 °C). The collection funnel is maintained at ambient temperature so that the sample water and toluene can be separated physically. After separation, the sample water is purified by addition of paraffin wax to the container with the sample water, capping the container, and heating to approximately 60 °C to melt the wax. Trace amounts of toluene will dissolve in the wax, purifying the sample water for isotopic analysis. The isotopic composition of the purified water is then determined by equilibration with gaseous hydrogen or carbon dioxide, followed by dual-inlet isotope-ratio mass spectrometry. Because laser-absorption spectrometry is sensitive to organic compounds, such as trace toluene remaining in water samples, water samples should be analyzed for isotopic composition only by mass spectrometry and not by laser-absorption spectrometry.

Methylmercury determination in seafood by photochemical vapor generation capacitively coupled plasma microtorch optical emission spectrometry.

PubMed

Covaci, Eniko; Senila, Marin; Ponta, Michaela; Darvasi, Eugen; Petreus, Dorin; Frentiu, Maria; Frentiu, Tiberiu

2017-08-01

A non-chromatographic method based on double liquid-liquid extraction and measurements by UV photochemical vapor generation capacitively coupled plasma microtorch optical emission spectrometry was developed and characterized for methylmercury determination in seafood. Samples were prepared following the procedure recommended in JRC Technical Report of European Commission formerly proposed for the determination of methylmercury in seafood by thermal decomposition atomic absorption spectrometry, namely confinement of Hg species in 47% HBr solution, extraction of CH 3 Hg + in toluene and back-extraction in 1% l-cysteine aqueous solution. Mercury cold vapor was generated by flow injection UV photo-reduction from CH 3 Hg + in 0.6molL -1 HCOOH, while quantification was performed against external Hg 2+ aqueous standards and measuring Hg 253.652nm emission using a low power/Ar consumption plasma microtorch (15W, 100mLmin -1 ) and a low resolution microspectrometer (Ocean Optics). The figures of merit and analytical capability were assessed by analyzing certified reference materials and test samples of fish fillet and discussed in relation with requirements for Hg determination in seafood in European legislation (Decisions 2007/333/EC and 2002/657/EC) as well as compared to performances achieved in thermal decomposition atomic absorption spectrometry. The limit of detection and quantification of 2µgkg -1 and 6µgkg -1 respectively, precision of 2.7-9.4% and accuracy of 99±8% of the proposed method for the determination of CH 3 Hg + fulfill the demands of European legislation for Hg quantification. The limit of detection and quantification were better than those in the used reference method or other non-/chromatographic methods taken for comparison. The analysis of certified reference materials and the Bland and Altman test performed on 12 test samples confirmed trueness of the proposed method and its reliability for the determination of traces of CH 3 Hg + with 95% confidence level. The proposed method fulfills several demands of the eco-scale concept, is sensitive, simple and safe related to sample preparation through elimination of classical, harmful reductants and attractive by using economical miniaturized instrumentation incorporating a low power and low Ar consumption plasma. Copyright © 2017 Elsevier B.V. All rights reserved.

Lithographically fabricated silicon microreactor for in situ characterization of heterogeneous catalysts—Enabling correlative characterization techniques

NASA Astrophysics Data System (ADS)

Baier, S.; Rochet, A.; Hofmann, G.; Kraut, M.; Grunwaldt, J.-D.

2015-06-01

We report on a new modular setup on a silicon-based microreactor designed for correlative spectroscopic, scattering, and analytic on-line gas investigations for in situ studies of heterogeneous catalysts. The silicon microreactor allows a combination of synchrotron radiation based techniques (e.g., X-ray diffraction and X-ray absorption spectroscopy) as well as infrared thermography and Raman spectroscopy. Catalytic performance can be determined simultaneously by on-line product analysis using mass spectrometry. We present the design of the reactor, the experimental setup, and as a first example for an in situ study, the catalytic partial oxidation of methane showing the applicability of this reactor for in situ studies.

Lithographically fabricated silicon microreactor for in situ characterization of heterogeneous catalysts—Enabling correlative characterization techniques.

PubMed

Baier, S; Rochet, A; Hofmann, G; Kraut, M; Grunwaldt, J-D

2015-06-01

We report on a new modular setup on a silicon-based microreactor designed for correlative spectroscopic, scattering, and analytic on-line gas investigations for in situ studies of heterogeneous catalysts. The silicon microreactor allows a combination of synchrotron radiation based techniques (e.g., X-ray diffraction and X-ray absorption spectroscopy) as well as infrared thermography and Raman spectroscopy. Catalytic performance can be determined simultaneously by on-line product analysis using mass spectrometry. We present the design of the reactor, the experimental setup, and as a first example for an in situ study, the catalytic partial oxidation of methane showing the applicability of this reactor for in situ studies.

Metalloproteomics: Forward and Reverse Approaches in Metalloprotein Structural and Functional Characterization

PubMed Central

Shi, Wuxian; Chance, Mark R.

2010-01-01

About one-third of all proteins are associated with a metal. Metalloproteomics is defined as the structural and functional characterization of metalloproteins on a genome-wide scale. The methodologies utilized in metalloproteomics, including both forward (bottom-up) and reverse (top-down) technologies, to provide information on the identity, quantity and function of metalloproteins are discussed. Important techniques frequently employed in metalloproteomics include classical proteomics tools such as mass spectrometry and 2-D gels, immobilized-metal affinity chromatography, bioinformatics sequence analysis and homology modeling, X-ray absorption spectroscopy and other synchrotron radiation based tools. Combinative applications of these techniques provide a powerful approach to understand the function of metalloproteins. PMID:21130021

Proximate composition, nutritional attributes and mineral composition of Peperomia pellucida L. (Ketumpangan Air) grown in Malaysia.

PubMed

Ooi, Der-Jiun; Iqbal, Shahid; Ismail, Maznah

2012-09-17

This study presents the proximate and mineral composition of Peperomia pellucida L., an underexploited weed plant in Malaysia. Proximate analysis was performed using standard AOAC methods and mineral contents were determined using atomic absorption spectrometry. The results indicated Peperomia pellucida to be rich in crude protein, carbohydrate and total ash contents. The high amount of total ash (31.22%)suggests a high-value mineral composition comprising potassium, calcium and iron as the main elements. The present study inferred that Peperomia pellucida would serve as a good source of protein and energy as well as micronutrients in the form of a leafy vegetable for human consumption.

Fluorination of vertically aligned carbon nanotubes: from CF4 plasma chemistry to surface functionalization.

PubMed

Struzzi, Claudia; Scardamaglia, Mattia; Colomer, Jean-François; Verdini, Alberto; Floreano, Luca; Snyders, Rony; Bittencourt, Carla

2017-01-01

The surface chemistry of plasma fluorinated vertically aligned carbon nanotubes (vCNT) is correlated to the CF 4 plasma chemical composition. The results obtained via FTIR and mass spectrometry are combined with the XPS and Raman analysis of the sample surface showing the dependence on different plasma parameters (power, time and distance from the plasma region) on the resulting fluorination. Photoemission and absorption spectroscopies are used to investigate the evolution of the electronic properties as a function of the fluorine content at the vCNT surface. The samples suffer a limited ageing effect, with a small loss of fluorine functionalities after two weeks in ambient conditions.

Fluorination of vertically aligned carbon nanotubes: from CF4 plasma chemistry to surface functionalization

PubMed Central

Scardamaglia, Mattia; Colomer, Jean-François; Verdini, Alberto; Floreano, Luca; Snyders, Rony; Bittencourt, Carla

2017-01-01

The surface chemistry of plasma fluorinated vertically aligned carbon nanotubes (vCNT) is correlated to the CF4 plasma chemical composition. The results obtained via FTIR and mass spectrometry are combined with the XPS and Raman analysis of the sample surface showing the dependence on different plasma parameters (power, time and distance from the plasma region) on the resulting fluorination. Photoemission and absorption spectroscopies are used to investigate the evolution of the electronic properties as a function of the fluorine content at the vCNT surface. The samples suffer a limited ageing effect, with a small loss of fluorine functionalities after two weeks in ambient conditions. PMID:28904833

Environment friendly route of iron oxide nanoparticles from Zingiber officinale (ginger) root extract

NASA Astrophysics Data System (ADS)

Xin Hui, Yau; Yi Peng, Teoh; Wei Wen, Liu; Zhong Xian, Ooi; Peck Loo, Kiew

2016-11-01

Iron oxide nanoparticles were prepared from the reaction between the Zingiber officinale (ginger) root extracts and ferric chloride solution at 50°C for 2 h in mild stirring condition. The synthesized powder forms of nanoparticles were further characterized by using UV-Vis spectroscopy and X-ray Diffraction spectrometry. UV-Vis analysis shows the absorption peak of iron oxide nanoparticles is appeared at 370 nm. The calculation of crystallite size from the XRD showed that the average particle size of iron oxide nanoparticles was 68.43 nm. Therefore, this eco-friendly technique is low cost and large scale nanoparticles synthesis to fulfill the demand of various applications.

Development of new portable miniaturize solid phase microextraction of silver-APDC complex using micropipette tip in-syringe system couple with electrothermal atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Naeemullah; Kazi, Tasneem Gul; Afridi, Hassan Imran; Shah, Faheem; Arain, Sadaf Sadia; Arain, Salma Aslam; Panhwar, Abdul Haleem; Arain, Mariam Shahzadi; Samoon, Muhammad Kashif

2016-02-01

An innovative and simple miniaturized solid phase microextraction (M-SPME) method, was developed for preconcentration and determination of silver(I) in the fresh and waste water samples. For M-SPME, a micropipette tip packed with activated carbon cloth (ACC) as sorbent, in a syringe system. The size, morphology and elemental composition of ACC before and after adsorption of analyte have been characterized by scanning electron microscopy and energy dispersive spectroscopy. The sample solution treated with a complexing reagent, ammonium pyrrolidine dithiocarbamate (APDC), was drawn into the syringe filled with ACC and dispensed manually for 2 to 10 aspirating/dispensing cycle. Then the Ag- complex sorbed on the ACC in micropipette was quantitatively eluted by drawing and dispensing of different concentrations of acids for 2 to 5 aspirating/dispensing cycles. The extracted Ag ions with modifier were injected directly into the electrothermal atomic absorption spectrometry for analysis. The influence of different variables on the extraction efficiency, including the concentration of ligand, pH, sample volume, eluent type, concentration and volume was investigated. Validity and accuracy of the developed method was checked by the standard addition method. Reliability of the proposed methodology was checked by the relative standard deviation (%RSD), which was found to be < 5%. Under the optimized experimental variables, the limits of detection (LOD) and enhancement factors (EF), were obtained to be 0.86 ng L- 1 and 120, respectively. The proposed method was successfully applied for the determination of trace levels of silver ions in fresh and waste water samples.

Selective and sensitive speciation analysis of Cr(VI) and Cr(III), at sub-μgL-1 levels in water samples by electrothermal atomic absorption spectrometry after electromembrane extraction.

PubMed

Tahmasebi, Zeinab; Davarani, Saied Saeed Hosseiny

2016-12-01

In this work, electromembrane extraction in combination with electrothermal atomic absorption spectrometry (ET-AAS) was investigated for speciation, preconcentration and quantification of Cr(VI) and Cr(III) in water samples through the selective complexation of Cr(VI) with 1,5-diphenylcarbazide (DPC) as a complexing agent. DPC reduces Cr(VI) to Cr(III) ions and then Cr(III) species are extracted based on electrokinetic migration of their cationic complex (Cr(III)-DPC) toward the negative electrode placed in the hollow fiber. Also, once oxidized to Cr(VI), Cr(III) ions in initial sample were determined by this procedure. The influence of extraction parameters such as pH, type of organic solvent, chelating agent concentration, stirring rate, extraction time and applied voltage were evaluated following a one-at-a-time optimization approach. Under optimized conditions, the extracted analyte was quantified by ETAAS, with an acceptable linearity in the range of 0.05-5ngmL -1 (R 2 value=0.996), and a repeatability (%RSD) between 3.7% and 12.2% (n=4) for 5.0 and 1.0ngmL -1 of Cr(VI), respectively. Also, we obtained an enrichment factor of 110 that corresponded to the recovery of 66%. The detection limit (S/N ratio of 3:1) was 0.02ngmL -1 . Finally, this new method was successfully employed to determine Cr(III) and Cr(VI) species in real water samples. Copyright © 2016. Published by Elsevier B.V.

Heavy metals and its chemical speciation in sewage sludge at different stages of processing.

PubMed

Tytła, Malwina; Widziewicz, Kamila; Zielewicz, Ewa

2016-01-01

The analysis of heavy metal concentrations and forms in sewage sludge constitutes an important issue in terms of both health and environmental hazards the metals pose. The total heavy metals concentration enables only the assessment of its contamination. Hence the knowledge of chemical forms is required to determine their environmental mobility and sludge final disposal. Heavy metals speciation was studied by using four-stage sequential extraction BCR (Community Bureau of Reference). This study was aimed at determining the total concentration of selected heavy metals (Zn, Cu, Ni, Pb, Cd, Cr and Hg) and their chemical forms (except for Hg) in sludge collected at different stages of its processing at two municipal Wastewater Treatment Plants in southern Poland. Metals contents in sludge samples were determined by using flame atomic absorption spectrometry (FAAS) and electrothermal atomic absorption spectrometry (ETAAS). This study shows that Zn and Cu appeared to be the most abundant in sludge, while Cd and Hg were in the lowest concentrations. The sewage sludge revealed the domination of immobile fractions over the mobile ones. The oxidizable and residual forms were dominant for all the heavy metals. There was also a significant difference in metals speciation between sludges of different origin which was probably due to differences in wastewater composition and processes occurring in biological stage of wastewater treatment. The results indicate a negligible capability of metals to migrate from sludge into the environment. Our research revealed a significant impact of thickening, stabilization and hygienization on the distribution of heavy metals in sludge and their mobility.

Recent developments in cyanide detection: A review

PubMed Central

Ma, Jian; Dasgupta, Purnendu K.

2010-01-01

The extreme toxicity of cyanide and environmental concerns from its continued industrial use continue to generate interest in facile and sensitive methods for cyanide detection. In recent years there is also additional recognition of HCN toxicity from smoke inhalation and potential use of cyanide as a weapon of terrorism. This review summarizes the literature since 2005 on cyanide measurement in different matrices ranging from drinking water and wastewater, to cigarette smoke and exhaled breath to biological fluids like blood, urine and saliva. The dramatic increase in the number of publications on cyanide measurement is indicative of the great interest in this field not only from analytical chemists, but also researchers from diverse environmental, medical, forensic and clinical arena. The recent methods cover both established and emerging analytical disciplines and include naked eye visual detection, spectrophotometry/colorimetry, capillary electrophoresis with optical absorbance detection, fluorometry, chemiluminescence, near-infrared cavity ring down spectroscopy, atomic absorption spectrometry, electrochemical methods (potentiometry/amperometry/ion chromatography-pulsed amperometry), mass spectrometry (selected ion flow tube mass spectrometry, electrospray ionization mass spectrometry, gas chromatography-mass spectrometry), gas chromatography (nitrogen phosphorus detector, electron capture detector) and quartz crystal mass monitors. PMID:20599024

Speciation of chromium using reversed phase-high performance liquid chromatography coupled to different spectrometric detection methods

NASA Astrophysics Data System (ADS)

Andrle, C. M.; Jakubowski, N.; Broekaert, J. A. C.

1997-02-01

Speciation of Cr(III) and Cr(VI) based on the formation of different complexes with ammonium-pyrrolidinedithioate (APDC) in a continuous flow technique and their preconcentration using solid phase extraction (SPE) have been elaborated and applied to the analysis of waste waters from the galvanic industry. The Cr complexes were separated and determined using reversed phase-high performance liquid chromatography (RP-HPLC) coupled to different detection methods, namely UV-detection, graphite furnace-atomic absorption spectrometry (GF-AAS) and inductively coupled plasma mass spectrometry with hydraulic high pressure nebulization (HHPN/ICP-MS). After optimization the detection limits for Cr(III) and Cr(VI) of all methods are at the μg 1 -1 level and the precision in terms of RSD is 5% ( cCr = 100 μg 1 -1, N = 10). The procedure was applied to the determination of Cr(III) and Cr(VI) at the μg 1 -1 level in galvanic waste waters, and its accuracy was approved by comparing the results with those of independent methods.

Transformation of tributyltin in zebrafish eleutheroembryos (Danio rerio).

PubMed

Borges, Aline Rocha; López-Serrano Oliver, Ana; Gallego-Gallegos, Mercedes; Muñoz-Olivas, Riansares; Rodrigues Vale, Maria Goreti; Cámara, Carmen

2014-12-01

Organotin compounds are highly versatile group of organometallic chemicals used in industrial and agricultural applications. Their endocrine-disrupting effects are well known and their extensive uses as biocide materials, e.g., in antifouling paints, for many years have led to serious environmental problems. So far, attention has mainly been given to tributyltin pollution in water, sediments, and marine organisms because of its highly toxic effects and high accumulation levels at very low concentrations. In this study, we will focus on the conversion of tributyltin after it is absorbed by zebrafish eleutheroembryos, presented here as an alternative model to adult fish for describing bioconcentration. A simplified analytical extraction procedure based on the use of an assisted ultrasonic probe and derivatization by ethylation, followed by gas chromatography with a flame photometric detector (GC-FPD) is proposed. This classical methodology for organotin determination has been validated by inductively coupled plasma mass spectrometry (ICP-MS) and Zeeman graphite furnace atomic absorption spectrometry (ZGF-AAS) in terms of total tin content. The speciation analysis results show that zebrafish eleutheroembryos absorb high amounts of tributyltin and convert it into monobutyltin and likely in inorganic tin.

[Ultraviolet-visible spectrometry analysis of insoluble xanthate heavy metal complexes].

PubMed

Qiu, Bo; Liu, Jin-Feng; Liu, Yao-Chi; Yang, Zhao-Guang; Li, Hai-Pu

2014-11-01

A ultraviolet-visible spectrometry method of determining insoluble xanthate heavy metal complexes in flotation wastewater was the first time to be put forward. In this work, the changes of ultraviolet-visible spectra of xanthate solution after the addition of various heavy metal ions were investigated firstly. It was found that Pb2+ and Cu2+ can form insoluble complexes with xanthate, while Fe2+, Zn2+ and Mn2+ have little effect on the ultraviolet absorption of xanthate solution. Then the removal efficiencies of filter membrane with different pore sizes were compared, and the 0.22 μm membrane was found to be effective to separate copper xanthate or lead xanthate from the filtrate. Furthermore, the results of the study on the reaction of sodium sulfide and insoluble xanthate heavy metal complexes showed that S(2-) can release the xanthate ion quantitatively from insoluble complexes to solution. Based on the above research, it was concluded that the amount of insoluble xanthate heavy metal complexes in water samples can be obtained through the increase of free xanthate in the filtrate after the addition of sodium sulfide. Finally, the feasibility of this method was verified by the application to the analysis of flotation wastewater from three ore-dressing plants in the Thirty-six Coves in Chenzhou.

Novel ionic liquid matrices for qualitative and quantitative detection of carbohydrates by matrix assisted laser desorption/ionization mass spectrometry.

PubMed

Zhao, Xiaoyong; Shen, Shanshan; Wu, Datong; Cai, Pengfei; Pan, Yuanjiang

2017-09-08

Analysis of carbohydrates based on matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) is still challenging and researchers have been devoting themselves to efficient matrices discovery. In the present study, the design, synthesis, qualitative and quantitative performance of non-derivative ionic liquid matrices (ILMs) were reported. DHB/N-methylaniline (N-MA) and DHB/N-ethylaniline (N-EA), performing best for carbohydrate detection, have been screened out. The limit of detection for oligosaccharide provided by DHB/N-MA and DHB/N-EA were as low as 10 fmol. DHB/N-MA and DHB/N-EA showed significantly higher ion generation efficiency than DHB. The comparison of capacity to probe polysaccharide between these two ILMs and DHB also revealed their powerful potential. Their outstanding performance were probably due to lower proton affinities and stronger UV absorption at λ = 355 nm. What is more, taking DHB/N-MA as an example, quantitative analysis of fructo-oligosaccharide mixtures extracted and identified from rice noodles has been accomplished sensitively using an internal standard method. Overall, DHB/N-MA and DHB/N-EA exhibited excellent performance and might be significant sources as the carbohydrate matrices. Copyright © 2017 Elsevier B.V. All rights reserved.

Multi-element atmospheric deposition in Macedonia studied by the moss biomonitoring technique.

PubMed

Barandovski, Lambe; Frontasyeva, Marina V; Stafilov, Trajče; Šajn, Robert; Ostrovnaya, Tatyana M

2015-10-01

Moss biomonitoring technique using moss species Homolothecium lutescens (Hedw.) Robins and Hypnum cupressiforme (Hedw.) was applied to air pollution studies in the Republic of Macedonia. The study was performed in the framework of the International Cooperative Programme on Effects of Air Pollution on Natural Vegetation and Crops under the auspices of the United Nations Economic Commission for Europe (UNECE) Convention on Long-Range Transboundary Air Pollution (LRTAP). The presence of 47 elements was determined by instrumental epithermal neutron activation analysis, atomic absorption spectrometry and atomic emission spectrometry with inductively coupled plasma. Normality of the datasets of elements was investigated, and Box-Cox transformation was used in order to achieve normal distributions of the data. Different pollution sources were identified and characterized using principal component analysis (PCA). Distribution maps were prepared to point out the regions most affected by pollution and to relate this to the known sources of contamination. The cities of Veles, Skopje, Tetovo, Radoviš and Kavadarci were determined to experience particular environmental stress. Moreover, three reactivated lead-zinc mines were also shown to contribute to a high content of lead and zinc in the eastern part of the country. However, a comparison with the previous moss survey conducted in 2005 showed a decreasing trend of pollution elements that are usually associated with emission from industrial activities.

Several methods to determine heavy metals in the human brain

NASA Astrophysics Data System (ADS)

Andrási, Erzsébet; Igaz, Sarolta; Szoboszlai, Norbert; Farkas, Éva; Ajtony, Zsolt

1999-05-01

The determination of naturally occurring heavy metals in various parts of the human brain is discussed. The patients had no diseases in their central nervous systems (five individuals, mean age 70 years). Twenty brain parts were selected from both hemispheres. The analysis was carried out by graphite furnace atomic absorption spectrometry, inductively coupled plasma atomic emission spectrometry and instrumental neutron activation analysis methods. Accuracy and precision of the applied techniques were tested by using standard reference materials. Two digestion methods were used to dissolve the brain samples for ICP-AES and GF-AAS. One was performed in a Parr-bomb and the second in a microwave oven. The present results show a non-homogeneous distribution of the essential elements (Cu, Fe, Mn, Zn) in normal human brain. Corresponding regions in both hemispheres showed an almost identical concentration of these elements. In the case of toxic elements (Pb, Cd) an average value in different brain regions can not be established because of the high variability of individual data. This study indicates that beside differences in Pb and Cd intake with foods or cigarette smoke inhalation, the main factors of the high inter-individual variability of these element concentrations in human brain parts may be a marked difference in individual elimination or accumulation capabilities.

Solid phase extraction and trace monitoring of cadmium ions in environmental water and food samples based on modified magnetic nanoporous silica

NASA Astrophysics Data System (ADS)

Omidi, Fariborz; Behbahani, Mohammad; Kalate Bojdi, Majid; Shahtaheri, Seyed Jamaleddin

2015-12-01

A new method has been developed for trace separation/preconcentration of cadmium ions using pyridine-functionalized magnetic nanoporous silica material (called Py-Fe3O4@MCM-41) as a new magnetic sorbent and their determination by flame atomic absorption spectrometry (FAAS). The Py-Fe3O4@MCM-41 sorbent was characterized by thermogravimetric analysis, differential thermal analysis, transmission electron microscopy, Fourier transform infrared spectrometry and X-ray diffraction. The modified Fe3O4@MCM-41 can be easily separated from an aqueous solution by applying an external magnetic field. Effects of pH, amount of functionalized Fe3O4@MCM-41, extraction time, type and quantity of eluent, desorption time, and interfering ions on the extraction efficiency were evaluated and optimized. Under the optimized conditions, the detection limit and relative standard deviation was 0.04 μg L-1 and 2.9%, respectively and the maximum adsorption capacity of the synthesized sorbent for cadmium ions was 154 mg g-1. The proposed method has been applied to the determination of Cd ions at trace levels in real samples such as, rice, onion, carrot, lettuce, parsley, basil, tap water, river water and seawater with satisfactory results.

Quantification of absorption, retention and elimination of two different oral doses of vitamin A in Zambian boys using accelerator mass spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Aklamati, E K; Mulenga, M; Dueker, S R

A recent survey indicated that high-dose vitamin A supplements (HD-VAS) had no apparent effect on vitamin A (VA) status of Zambian children <5 y of age. To explore possible reasons for the lack of response to HD-VAS among Zambian children, we quantified the absorption, retention, and urinary elimination of either a single HDVAS (60 mg) or a smaller dose of stable isotope (SI)-labeled VA (5 mg), which was used to estimate VA pool size, in 3-4 y old Zambian boys (n = 4 for each VA dose). A 25 nCi tracer dose of [{sup 14}C{sub 2}]-labeled VA was co-administered withmore » the HD-VAS or SI-labeled VA, and 24-hr stool and urine samples were collected for 3 and 7 consecutive days, respectively, and 24-hr urine samples at 4 later time points. Accelerator Mass Spectrometry (AMS) was used to measure the cumulative excretion of {sup 14}C in stool and urine 3d after dosing to estimate, respectively, absorption and retention of the VAS and SI-labeled VA. The urinary elimination rate (UER) was estimated by plotting {sup 14}C in urine vs. time, and fitting an exponential equation to the data. Estimates of mean absorption, retention and the UER were 83.8 {+-} 7.1%, 76.3 {+-} 6.7%, and 1.9 {+-} 0.6%/d, respectively, for the HD-VAS and 76.5 {+-} 9.5%, 71.1 {+-} 9.4%, and 1.8 {+-} 1.2%/d, respectively for the smaller dose of SI-labeled VA. Estimates of absorption, retention and the UER did not differ by size of the VA dose administered (P=0.26, 0.40, 0.88, respectively). Estimated absorption and retention were negatively associated with reported fever (P=0.011) and malaria (P =0.010). HD-VAS and SI-labeled VA were adequately absorbed, retained and utilized in apparently healthy Zambian preschool-age boys, although absorption and retention may be affected by recent infections.« less

High-Resolution Fast-Neutron Spectrometry for Arms Control and Treaty Verification

DOE Office of Scientific and Technical Information (OSTI.GOV)

David L. Chichester; James T. Johnson; Edward H. Seabury

2012-07-01

Many nondestructive nuclear analysis techniques have been developed to support the measurement needs of arms control and treaty verification, including gross photon and neutron counting, low- and high-resolution gamma spectrometry, time-correlated neutron measurements, and photon and neutron imaging. One notable measurement technique that has not been extensively studied to date for these applications is high-resolution fast-neutron spectrometry (HRFNS). Applied for arms control and treaty verification, HRFNS has the potential to serve as a complimentary measurement approach to these other techniques by providing a means to either qualitatively or quantitatively determine the composition and thickness of non-nuclear materials surrounding neutron-emitting materials.more » The technique uses the normally-occurring neutrons present in arms control and treaty verification objects of interest as an internal source of neutrons for performing active-interrogation transmission measurements. Most low-Z nuclei of interest for arms control and treaty verification, including 9Be, 12C, 14N, and 16O, possess fast-neutron resonance features in their absorption cross sections in the 0.5- to 5-MeV energy range. Measuring the selective removal of source neutrons over this energy range, assuming for example a fission-spectrum starting distribution, may be used to estimate the stoichiometric composition of intervening materials between the neutron source and detector. At a simpler level, determination of the emitted fast-neutron spectrum may be used for fingerprinting 'known' assemblies for later use in template-matching tests. As with photon spectrometry, automated analysis of fast-neutron spectra may be performed to support decision making and reporting systems protected behind information barriers. This paper will report recent work at Idaho National Laboratory to explore the feasibility of using HRFNS for arms control and treaty verification applications, including simulations and experiments, using fission-spectrum neutron sources to assess neutron transmission through composite low-Z attenuators.« less

Determination of polycyclic aromatic hydrocarbons and their nitro-, amino-derivatives absorbed on particulate matter 2.5 by multiphoton ionization mass spectrometry using far-, deep-, and near-ultraviolet femtosecond lasers.

PubMed

Tang, Yuanyuan; Imasaka, Tomoko; Yamamoto, Shigekazu; Imasaka, Totaro

2016-06-01

Multiphoton ionization processes of parent-polycyclic aromatic hydrocarbons (PPAHs), nitro-PAHs (NPAHs), and amino-PAHs (APAHs) were examined by gas chromatography combined with time-of-flight mass spectrometry using a femtosecond Ti:sapphire laser as the ionization source. The efficiency of multiphoton ionization was examined using lasers emitting in the far-ultraviolet (200 nm), deep-ultraviolet (267 nm), and near-ultraviolet (345 nm) regions. The largest signal intensities were obtained when the far-ultraviolet laser was employed. This favorable result can be attributed to the fact that these compounds have the largest molar absorptivities in the far-ultraviolet region. On the other hand, APAHs were ionized more efficiently than NPAHs in the near-ultraviolet region because of their low ionization energies. A sample extracted from a real particulate matter 2.5 (PM2.5) sample was measured, and numerous signal peaks arising from PAH and its analogs were observed at 200 nm. On the other hand, only a limited number of signed peaks were observed at 345 nm, some of which were signed to PPAHs, NPAHs, and APAHs. Thus, multiphoton ionization mass spectrometry has potential for the use in comprehensive analysis of toxic environmental pollutants. Copyright © 2016 Elsevier Ltd. All rights reserved.

Comparison of several analytical methods for the determination of tin in geochemical samples as a function of tin speciation

USGS Publications Warehouse

Kane, J.S.; Evans, J.R.; Jackson, J.C.

1989-01-01

Accurate and precise determinations of tin in geological materials are needed for fundamental studies of tin geochemistry, and for tin prospecting purposes. Achieving the required accuracy is difficult because of the different matrices in which Sn can occur (i.e. sulfides, silicates and cassiterite), and because of the variability of literature values for Sn concentrations in geochemical reference materials. We have evaluated three methods for the analysis of samples for Sn concentration: graphite furnace atomic absorption spectrometry (HGA-AAS) following iodide extraction, inductively coupled plasma atomic emission spectrometry (ICP-OES), and energy-dispersive X-ray fluorescence (EDXRF) spectrometry. Two of these methods (HGA-AAS and ICP-OES) required sample decomposition either by acid digestion or fusion, while the third (EDXRF) was performed directly on the powdered sample. Analytical details of all three methods, their potential errors, and the steps necessary to correct these errors were investigated. Results showed that similar accuracy was achieved from all methods for unmineralized samples, which contain no known Sn-bearing phase. For mineralized samples, which contain Sn-bearing minerals, either cassiterite or stannous sulfides, only EDXRF and fusion ICP-OES methods provided acceptable accuracy. This summary of our study provides information which helps to assure correct interpretation of data bases for underlying geochemical processes, regardless of method of data collection and its inherent limitations. ?? 1989.

Matching the laser wavelength to the absorption properties of matrices increases the ion yield in UV-MALDI mass spectrometry.

PubMed

Wiegelmann, Marcel; Soltwisch, Jens; Jaskolla, Thorsten W; Dreisewerd, Klaus

2013-09-01

A high analytical sensitivity in ultraviolet matrix-assisted laser desorption ionization mass spectrometry (MALDI-MS) is only achieved if the laser wavelength corresponds to a high optical absorption of the matrix. Laser fluence and the physicochemical properties of the compounds, e.g., the proton affinity, also influence analytical sensitivity significantly. In combination, these parameters determine the amount of material ejected per laser pulse and the ion yield, i.e., the fraction of ionized biomolecules. Here, we recorded peptide ion signal intensities as a function of these parameters. Three cinnamic acid matrices were investigated: α-cyano-4-hydroxycinnamic acid, α-cyano-4-chlorocinnamic acid, and α-cyano-2,4-difluorocinnamic acid. In addition, 2,5-dihydroxybenzoic acid was used in comparison experiments. Ion signal intensities "per laser shot" and integrated ion signal intensities were acquired over 900 consecutive laser pulses applied on distinct positions on the dried-droplet sample preparations. With respect to laser wavelength, the two standard MALDI wavelengths of 337/355 nm were investigated. Also, 305 or 320 nm was selected to account for the blue-shifted absorption profiles of the halogenated derivatives. Maximal peptide ion intensities were obtained if the laser wavelength fell within the peak of the absorption profile of the compound and for fluences two to three times the corresponding ion detection threshold. The results indicate ways for improving the analytical sensitivity in MALDI-MS, and in particular for MALDI-MS imaging applications where a limited amount of material is available per irradiated pixel.

40 CFR 1065.1010 - Reference materials.

Code of Federal Regulations, 2011 CFR

2011-07-01

... Method for Phosphorus in Gasoline 1065.710 ASTM D3237-06e01, Standard Test Method for Lead in Gasoline By... atomic absorption spectrometry 1065.705 IP-500, Determination of the phosphorus content of residual fuels..., iron, sodium, calcium, zinc and phosphorus in residual fuel oil by ashing, fusion and inductively...

Formation of Oxidized Organic Aerosol (OOA) through Fog Processing in the Po Valley

NASA Astrophysics Data System (ADS)

Gilardoni, S.; Paglione, M.; Rinaldi, M.; Giulianelli, L.; Massoli, P.; Hillamo, R. E.; Carbone, S.; Lanconelli, C.; Laaksonen, A. J.; Russell, L. M.; Poluzzi, V.; Fuzzi, S.; Facchini, C.

2014-12-01

Aqueous phase chemistry might be responsible for the formation of a significant fraction of the organic aerosol (OA) observed in the atmosphere, and could explain some of the discrepancies between OA concentration and properties predicted by models and observed in the environment. Aerosol - fog interaction and its effect on submicron aerosol properties were investigated in the Po Valley (northern Italy) during fall 2011, in the framework of the Supersite project (ARPA Emilia Romagna). Composition and physical properties of submicron aerosol were measured online by a High Resolution- Time of Flight - Aerosol Mass Spectrometer (HR-TOF-AMS), a Soot Photometer - Aerosol Mass Spectrometer (SP-AMS), and a Tandem Differential Mobility Particle Sizer (TDMPS). Organic functional group analysis was performed off-line by Hydrogen - Nuclear Magnetic Resonance (H-NMR) spectrometry and by Fourier Transform Infrared (FTIR) spectrometry. Aerosol absorption, scattering, and total extinction were measured simultaneously with a Particle Soot Absorption Photometer (PSAP), a Nephelometer, and a Cavity Attenuated Phase Shift Spectrometer particle extinction monitor (CAPS PMex), respectively. Water-soluble organic carbon in fog-water was characterized off-line by HR-TOF-AMS. Fourteen distinct fog events were observed. Fog dissipation left behind an aerosol enriched in particles larger than 400 nm, typical of fog and cloud processing, and dominated by secondary species, including ammonium nitrate, ammonium sulfate and oxidized OA (OOA). Source apportionment of OA allowed us to identify OOA as the difference between total OA and primary OA (hydrocarbon like OA and biomass burning OA). The formation of OOA through fog processing is proved by the correlation of OOA concentration with hydroxyl methyl sulfonate signal and by the similarity of OOA spectra with organic mass spectra obtained by re-aerosolization of fog water samples. The oxygen to carbon ratio and the hydrogen to carbon ratio of this OOA fraction was about 0.6 and 1.3, respectively. Organic functional group analysis showed that OOA observed after fog dissipation was characterized by organic-sulfur and organic-nitrogen species.

An evaluation of a reagentless method for the determination of total mercury in aquatic life

USGS Publications Warehouse

Haynes, Sekeenia; Gragg, Richard D.; Johnson, Elijah; Robinson, Larry; Orazio, Carl E.

2006-01-01

Multiple treatment (i.e., drying, chemical digestion, and oxidation) steps are often required during preparation of biological matrices for quantitative analysis of mercury; these multiple steps could potentially lead to systematic errors and poor recovery of the analyte. In this study, the Direct Mercury Analyzer (Milestone Inc., Monroe, CT) was utilized to measure total mercury in fish tissue by integrating steps of drying, sample combustion and gold sequestration with successive identification using atomic absorption spectrometry. We also evaluated the differences between the mercury concentrations found in samples that were homogenized and samples with no preparation. These results were confirmed with cold vapor atomic absorbance and fluorescence spectrometric methods of analysis. Finally, total mercury in wild captured largemouth bass (n = 20) were assessed using the Direct Mercury Analyzer to examine internal variability between mercury concentrations in muscle, liver and brain organs. Direct analysis of total mercury measured in muscle tissue was strongly correlated with muscle tissue that was homogenized before analysis (r = 0.81, p < 0.0001). Additionally, results using this integrated method compared favorably (p < 0.05) with conventional cold vapor spectrometry with atomic absorbance and fluorescence detection methods. Mercury concentrations in brain were significantly lower than concentrations in muscle (p < 0.001) and liver (p < 0.05) tissues. This integrated method can measure a wide range of mercury concentrations (0-500 ??g) using small sample sizes. Total mercury measurements in this study are comparative to the methods (cold vapor) commonly used for total mercury analysis and are devoid of laborious sample preparation and expensive hazardous waste. ?? Springer 2006.

Electrothermal atomic absorption spectrometric determination of copper in nickel-base alloys with various chemical modifiers*1

NASA Astrophysics Data System (ADS)

Tsai, Suh-Jen Jane; Shiue, Chia-Chann; Chang, Shiow-Ing

1997-07-01

The analytical characteristics of copper in nickel-base alloys have been investigated with electrothermal atomic absorption spectrometry. Deuterium background correction was employed. The effects of various chemical modifiers on the analysis of copper were investigated. Organic modifiers which included 2-(5-bromo-2-pyridylazo)-5-(diethylamino-phenol) (Br-PADAP), ammonium citrate, 1-(2-pyridylazo)-naphthol, 4-(2-pyridylazo)resorcinol, ethylenediaminetetraacetic acid and Triton X-100 were studied. Inorganic modifiers palladium nitrate, magnesium nitrate, aluminum chloride, ammonium dihydrogen phosphate, hydrogen peroxide and potassium nitrate were also applied in this work. In addition, zirconium hydroxide and ammonium hydroxide precipitation methods have also been studied. Interference effects were effectively reduced with Br-PADAP modifier. Aqueous standards were used to construct the calibration curves. The detection limit was 1.9 pg. Standard reference materials of nickel-base alloys were used to evaluate the accuracy of the proposed method. The copper contents determined with the proposed method agreed closely with the certified values of the reference materials. The recoveries were within the range 90-100% with relative standard deviation of less than 10%. Good precision was obtained.

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

PubMed

Tuzen, Mustafa; Pekiner, Ozlem Zeynep

2015-12-01

A rapid and environmentally friendly ultrasound assisted ionic liquid dispersive liquid liquid microextraction (USA-IL-DLLME) was developed for the speciation of inorganic selenium in beverages and total selenium in food samples by using graphite furnace atomic absorption spectrometry. Some analytical parameters including pH, amount of complexing agent, extraction time, volume of ionic liquid, sample volume, etc. were optimized. Matrix effects were also investigated. Enhancement factor (EF) and limit of detection (LOD) for Se(IV) were found to be 150 and 12 ng L(-1), respectively. The relative standard deviation (RSD) was found 4.2%. The accuracy of the method was confirmed with analysis of LGC 6010 Hard drinking water and NIST SRM 1573a Tomato leaves standard reference materials. Optimized method was applied to ice tea, soda and mineral water for the speciation of Se(IV) and Se(VI) and some food samples including beer, cow's milk, red wine, mixed fruit juice, date, apple, orange, grapefruit, egg and honey for the determination of total selenium. Copyright © 2015 Elsevier Ltd. All rights reserved.

Study of the versatility of a graphite furnace atomic absorption spectrometric method for the determination of cadmium in the environmental field.

PubMed

Rucandio, M Isabel; Petit-Domínguez, M Dolores

2002-01-01

Cadmium is a representative example of trace elements that are insidious and widespread health hazards. In contemporary environmental analysis, there is a clear trend toward its determination over a wide range of concentrations in complex matrixes. This paper describes a versatile method for the determination of Cd at various levels (0.1-500 microg/g) in several sample types, such as soils, sediments, coals, ashes, sewage sludges, animal tissues, and plants, by graphite furnace atomic absorption spectrometry with Zeeman background correction. The effect of the individual presence of about 50 elements, with an interference/analyte concentration ratio of up to 10(5), was tested; recoveries of Cd ranged from 93 to 106%. The influence of different media, such as HNO3, HCI, HF, H2SO4, HClO4, acetic acid, hydroxylammonium chloride, and ammonium acetate, in several concentrations, was also tested. From these studies it can be concluded that the analytical procedure is scarcely matrix dependent, and the results obtained for a wide diversity of reference materials are in good agreement with the certified values.

Apparatus and method for transient thermal infrared spectrometry of flowable enclosed materials

DOEpatents

McClelland, John F.; Jones, Roger W.

1993-03-02

A method and apparatus for enabling analysis of a flowable material enclosed in a transport system having an infrared transparent wall portion. A temperature differential is transiently generated between a thin surface layer portion of the material and a lower or deeper portion of the material sufficient to alter the thermal infrared emission spectrum of the material from the black-body thermal infrared emission spectrum of the material, and the altered thermal infrared emission spectrum is detected through the infrared transparent portion of the transport system while the altered thermal infrared emission spectrum is sufficiently free of self-absorption by the material of emitted infrared radiation. The detection is effected prior to the temperature differential propagating into the lower or deeper portion of the material to an extent such that the altered thermal infrared emission spectrum is no longer sufficiently free of self-absorption by the material of emitted infrared radiation. By such detection, the detected altered thermal infrared emission spectrum is indicative of characteristics relating to molecular composition of the material.

Major- and trace-element concentrations in soils from two continental-scale transects of the United States and Canada

USGS Publications Warehouse

Smith, David B.; Cannon, William F.; Woodruff, Laurel G.; Garrett, Robert G.; Klassen, Rodney; Kilburn, James E.; Horton, John D.; King, Harley D.; Goldhaber, Martin B.; Morrison, Jean M.

2005-01-01

This report contains major- and trace-element concentration data for soil samples collected from 265 sites along two continental-scale transects in North America. One of the transects extends from northern Manitoba to the United States-Mexico border near El Paso, Tex. and consists of 105 sites. The other transect approximately follows the 38th parallel from the Pacific coast of the United States near San Francisco, Calif., to the Atlantic coast along the Maryland shore and consists of 160 sites. Sampling sites were defined by first dividing each transect into approximately 40-km segments. For each segment, a 1-km-wide latitudinal strip was randomly selected; within each strip, a potential sample site was selected from the most representative landscape within the most common soil type. At one in four sites, duplicate samples were collected 10 meters apart to estimate local spatial variability. At each site, up to four separate soil samples were collected as follows: (1) material from 0-5 cm depth; (2) O horizon, if present; (3) a composite of the A horizon; and (4) C horizon. Each sample collected was analyzed for total major- and trace-element composition by the following methods: (1) inductively coupled plasmamass spectrometry (ICP-MS) and inductively coupled plasma-atomic emission spectrometry (ICPAES) for aluminum, antimony, arsenic, barium, beryllium, bismuth, cadmium, calcium, cerium, cesium, chromium, cobalt, copper, gallium, indium, iron, lanthanum, lead, lithium, magnesium, manganese, molybdenum, nickel, niobium, phosphorus, potassium, rubidium, scandium, silver, sodium, strontium, sulfur, tellurium, thallium, thorium, tin, titanium, tungsten, uranium, vanadium, yttrium, and zinc; (2) cold vapor- atomic absorption spectrometry for mercury; (3) hydride generation-atomic absorption spectrometry for antimony and selenium; (4) coulometric titration for carbonate carbon; and (5) combustion for total carbon and total sulfur.

Rate constant for the reaction NH2 + NO from 216 to 480 K

NASA Technical Reports Server (NTRS)

Stief, L. J.; Brobst, W. D.; Nava, D. F.; Borkowski, R. P.; Michael, J. V.

1982-01-01

The absolute rate constant was measured by the technique of flash photolysis-laser induced fluorescence (FP-LIF). NH2 radicals were produced by the flash photolysis of ammonia and the fluorescent NH2 photons were measured by multiscaling techniques. At each temperature, the results were independent of variations in total pressure, and flash intensity. The results are compared with previous determinations using the techniques of mass spectrometry, absorption spectroscopy, laser absorption spectroscopy, and laser induced fluorescence. The implications of the results are discussed with regard to combustion, post combustion, and atmospheric chemistry. The results are also discussed theoretically.

Primary gas thermometry by means of laser-absorption spectroscopy: determination of the Boltzmann constant.

PubMed

Casa, G; Castrillo, A; Galzerano, G; Wehr, R; Merlone, A; Di Serafino, D; Laporta, P; Gianfrani, L

2008-05-23

We report on a new optical implementation of primary gas thermometry based on laser-absorption spectrometry in the near infrared. The method consists in retrieving the Doppler broadening from highly accurate observations of the line shape of the R(12) nu1+2nu2(0)+nu3 transition in CO2 gas at thermodynamic equilibrium. Doppler width measurements as a function of gas temperature, ranging between the triple point of water and the gallium melting point, allowed for a spectroscopic determination of the Boltzmann constant with a relative accuracy of approximately 1.6 x 10(-4).

Primary Gas Thermometry by Means of Laser-Absorption Spectroscopy: Determination of the Boltzmann Constant

NASA Astrophysics Data System (ADS)

Casa, G.; Castrillo, A.; Galzerano, G.; Wehr, R.; Merlone, A.; di Serafino, D.; Laporta, P.; Gianfrani, L.

2008-05-01

We report on a new optical implementation of primary gas thermometry based on laser-absorption spectrometry in the near infrared. The method consists in retrieving the Doppler broadening from highly accurate observations of the line shape of the R(12) ν1+2ν20+ν3 transition in CO2 gas at thermodynamic equilibrium. Doppler width measurements as a function of gas temperature, ranging between the triple point of water and the gallium melting point, allowed for a spectroscopic determination of the Boltzmann constant with a relative accuracy of ˜1.6×10-4.

A new concept of efficient therapeutic drug monitoring using the high-resolution continuum source absorption spectrometry and the surface enhanced Raman spectroscopy

NASA Astrophysics Data System (ADS)

Xing, Yanlong; Fuss, Harald; Lademann, Jürgen; Huang, Mao Dong; Becker-Ross, Helmut; Florek, Stefan; Patzelt, Alexa; Meinke, Martina C.; Jung, Sora; Esser, Norbert

2018-04-01

In this study, a new therapeutic drug monitoring approach has been tested based on the combination of CaF molecular absorption using high-resolution continuum source absorption spectrometry (HR-CSAS) and surface enhanced Raman spectroscopy (SERS). HR-CSAS with mini graphite tube was successfully tested for clinical therapeutic drug monitoring of the fluorine-containing drug capecitabine in sweat samples of cancer patients: It showed advantageous features of high selectivity (no interference from Cl), high sensitivity (characteristic mass of 0.1 ng at CaF 583.069 nm), low sample consumption (down to 30 nL) and fast measurement (no sample pretreatment and less than 1 min of responding time) in tracing the fluorine signal out of capecitabine. However, this technique has the disadvantage of the total loss of the drug's structure information after burning the sample at very high temperature. Therefore, a new concept of combining HR-CSAS with a non-destructive spectroscopic method (SERS) was proposed for the sensitive sensing and specific identification of capecitabine. We tested and succeed in obtaining the molecular characteristics of the metabolite of capecitabine (named 5-fluorouracil) by the non-destructive SERS technique. With the results shown in this work, it is demonstrated that the combined spectroscopic technique of HR-CSAS and SERS will be very useful in efficient therapeutic drug monitoring in the future.

Spectroscopic properties for identifying sapphire samples from Ban Bo Kaew, Phrae Province, Thailand

NASA Astrophysics Data System (ADS)

Mogmued, J.; Monarumit, N.; Won-in, K.; Satitkune, S.

2017-09-01

Gemstone commercial is a high revenue for Thailand especially ruby and sapphire. Moreover, Phrae is a potential gem field located in the northern part of Thailand. The studies of spectroscopic properties are mainly to identify gemstone using advanced techniques (e.g. UV-Vis-NIR spectrophotometry, FTIR spectrometry and Raman spectroscopy). Typically, UV-Vis-NIR spectrophotometry is a technique to study the cause of color in gemstones. FTIR spectrometry is a technique to study the functional groups in gem-materials. Raman pattern can be applied to identify the mineral inclusions in gemstones. In this study, the natural sapphires from Ban Bo Kaew were divided into two groups based on colors including blue and green. The samples were analyzed by UV-Vis-NIR spectrophotometer, FTIR spectrometer and Raman spectroscope for studying spectroscopic properties. According to UV-Vis-NIR spectra, the blue sapphires show higher Fe3+/Ti4+ and Fe2+/Fe3+ absorption peaks than those of green sapphires. Otherwise, green sapphires display higher Fe3+/Fe3+ absorption peaks than blue sapphires. The FTIR spectra of both blue and green sapphire samples show the absorption peaks of -OH,-CH and CO2. The mineral inclusions such as ferrocolumbite and rutile in sapphires from this area were observed by Raman spectroscope. The spectroscopic properties of sapphire samples from Ban Bo Kaew, Phrae Province, Thailand are applied to be the specific evidence for gemstone identification.

The influence of alkalinity of portland cement on the absorption characteristics of superabsorbent polymers (SAP) for use in internally cured concrete

NASA Astrophysics Data System (ADS)

Tabares Tamayo, Juan D.

The concrete industry increasingly emphasizes advances in novel materials that promote construction of more resilient infrastructure. Due to its potential to improve concrete durability, internal curing (IC) of concrete by means of superabsorbent polymers (SAP) has been identified as one of the most promising technologies of the 21st century. The addition of superabsorbent polymers into a cementitious system promotes further hydration of cement by providing internal moisture during the hardening and strength development periods, and thus limits self-desiccation, shrinkage, and cracking. This thesis presents the work performed on the series of cement pastes with varying alkalinity of their pore solutions to provide a better understanding of: (1) the influence of the chemistry of the pore solution (i.e. its level of alkalinity and the type of ionic species present) on the absorption capacity of SAP, and (2) the effectiveness of SAP with different absorption capacities as an internal curing agent. This research work was divided into three stages: (a) materials characterization, (b) measurement of absorption capacity of SAP in synthetic pore solutions, and (c) evaluation of the internal curing effectiveness of SAP. During the first stage (Materials Characterization), pore solutions were extracted from the fresh (5 minutes old) cement pastes prepared using cements with three different levels of alkalinity. The pH values of the extracted solutions were determined (using the pH meter) and their chemical analysis was performed by means of titration (concentration of hydroxyl), ion chromatography (sulfates and chlorides), atomic absorption (AA) and inductively coupled plasma optical emission spectrometry (ICP) (sodium, potassium and calcium). The commercial SAP adopted for this study was used with "as-supplied" gradation and with the finer gradation obtained by grinding the original polymer in the 6850 Cryomilling Freezer/Mill. The physical properties of these SAP's, such as the shape and size of the particles, were determined by optical microscopy combined with image analysis. The second stage, the absorption capacity of SAP's, involved determination of the swelling behavior and the absorption capacity of polymers exposed to artificial pore solutions with different levels of alkalinity. The swelling behavior was followed using the optical microscope while the absorption capacity was characterized using the tea bag method. It was found that changes in the chemical compositions of the pore solutions influence the adsorption kinetics and result in different absorption isotherms. In the third stage, the internal curing effects of inclusion of SAP in cement pastes were evaluated. Mixture proportions of pastes used in this stage of the study were selected based on the absorption capacity of the SAP determined in stage two. The testing of the pastes involved determination of their set times, heat of hydration, and autogenous shrinkage.

Rapid determination of six carcinogenic primary aromatic amines in mainstream cigarette smoke by two-dimensional online solid phase extraction combined with liquid chromatography tandem mass spectrometry.

PubMed

Bie, Zhenying; Lu, Wei; Zhu, You; Chen, Yusong; Ren, Hubo; Ji, Lishun

2017-01-27

A fully automated, rapid, and reliable method for simultaneous determination of six carcinogenic primary aromatic amines (AAs), including o-toluidine (o-TOL), 2, 6-dimethylaniline (2, 6-DMA), o-anisidine (o-ASD), 1-naphthylamine (1-ANP), 2-naphthylamine (2-ANP), and 4-aminobiphenyl (4-ABP), in mainstream cigarette smoke was established. The proposed method was based on two-dimensional online solid phase extraction combined with liquid chromatography tandem mass spectrometry (SPE/LC-MS/MS). The particulate phase of the mainstream cigarette smoke was collected on a Cambridge filter pad and pretreated via ultrasonic extraction with 2% formic acid (FA), while the gas phase was trapped by 2% FA without pretreatment for determination. The two-dimensional online SPE comprised of two cartridges with different absorption characteristics was applied for sample pretreatment. Analysis was performed by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) under multiple reaction monitoring mode. Each sample required about 0.5h for solid phase extraction and analysis. The limit of detections (LODs) for six AAs ranged from 0.04 to 0.58ng/cig and recoveries were within 84.5%-122.9%. The relative standard deviations of intra- and inter-day tests for 3R4F reference cigarette were less than 6% and 7%, respectively, while no more than 7% and 8% separately for a type of Virginia cigarette. The proposed method enabled minimum sample pretreatment, full automation, and high throughput with high selectivity, sensitivity, and accuracy. As a part of the validation procedure, fifteen brands of cigarettes were tested by the designed method. Copyright © 2016 Elsevier B.V. All rights reserved.

The Determination of Lead in Gasoline by Atomic Absorption Spectrometry.

ERIC Educational Resources Information Center

Coleman, M. F. M.

1985-01-01

Describes an experiment that involves the extraction of lead from gasoline into an aqueous solvent using iodine monochloride reagent. This method (which avoids the aspiration of organic solvents) also illustrates the use of wavelengths other than the most sensitive wavelength and effects of flame stoichiometry and burner height upon absorbance.…

Study on tannin–metal interaction in aqueous solution using spectrophotometric titration and micelle-mediated separation/atomic absorption spectrometry

USDA-ARS?s Scientific Manuscript database

Tannins, including hydrolysable and condensed tannins, are important secondary metabolites of vascular plants and are a major plant-derived carbon source in the environment. Due to the many phenolic hydroxyl groups characteristic of tannins, these compounds have been long been thought to play signi...

Quantitative Ultrasound-Assisted Extraction for Trace-Metal Determination: An Experiment for Analytical Chemistry

ERIC Educational Resources Information Center

Lavilla, Isela; Costas, Marta; Pena-Pereira, Francisco; Gil, Sandra; Bendicho, Carlos

2011-01-01

Ultrasound-assisted extraction (UAE) is introduced to upper-level analytical chemistry students as a simple strategy focused on sample preparation for trace-metal determination in biological tissues. Nickel extraction in seafood samples and quantification by electrothermal atomic absorption spectrometry (ETAAS) are carried out by a team of four…

Determination of lead in flour samples directly by solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Tinas, Hande; Ozbek, Nil; Akman, Suleyman

2018-02-01

In this study, lead concentrations in various flour samples were determined by high-resolution continuum source graphite furnace atomic absorption spectrometry with solid sampling. Since samples were analyzed directly, the risks and disadvantages of sample digestion were eliminated. Solid flour samples were dried, weighed on the platforms, Pd was added as a modifier and introduced directly into a graphite tube using a manual solid sampler. Platforms and tubes were coated with Zr. The optimized pyrolysis and atomization temperatures were 800 °C and 2200 °C, respectively. The sensitivities of lead in various flour certified reference materials (CRMs) and aqueous standards were not significantly different. Therefore, aqueous standards were safely used for calibration. The absolute limit of detection and characteristic mass were 7.2 pg and 9.0 pg of lead, respectively. The lead concentrations in different types of flour samples were found in the range of 25-52 μg kg- 1. Finally, homogeneity factors representing the heterogeneity of analyte distribution for lead in flour samples were determined.

Determination of Inorganic Arsenic in a Wide Range of Food Matrices using Hydride Generation - Atomic Absorption Spectrometry.

PubMed

de la Calle, Maria B; Devesa, Vicenta; Fiamegos, Yiannis; Vélez, Dinoraz

2017-09-01

The European Food Safety Authority (EFSA) underlined in its Scientific Opinion on Arsenic in Food that in order to support a sound exposure assessment to inorganic arsenic through diet, information about distribution of arsenic species in various food types must be generated. A method, previously validated in a collaborative trial, has been applied to determine inorganic arsenic in a wide variety of food matrices, covering grains, mushrooms and food of marine origin (31 samples in total). The method is based on detection by flow injection-hydride generation-atomic absorption spectrometry of the iAs selectively extracted into chloroform after digestion of the proteins with concentrated HCl. The method is characterized by a limit of quantification of 10 µg/kg dry weight, which allowed quantification of inorganic arsenic in a large amount of food matrices. Information is provided about performance scores given to results obtained with this method and which were reported by different laboratories in several proficiency tests. The percentage of satisfactory results obtained with the discussed method is higher than that of the results obtained with other analytical approaches.

Determination of total arsenic and arsenic(III) in phosphate fertilizers by hydride generation atomic absorption spectrometry after ultrasound-assisted extraction based on a control acid media.

PubMed

Rezende, Helen Cristine; Coelho, Nivia Maria Melo

2014-01-01

An ultrasound-assisted extraction procedure was developed for determination of inorganic arsenic (As) in phosphate fertilizer by hydride generation atomic absorption spectrometry. The variables that affect the hydride generation step were optimized, including the reducer, acid, sample flow rate, and concentrations of the acid and reducer. The determination of As(lll) was performed through the simple control of solution pH with a 0.5 M citric acid-sodium citrate buffer solution at pH 4.5, and total As was determined after a pre-reduction reaction with 1.0% (w/v) thiourea. Ultrasound-assisted acid extraction was performed, and the parameters sonication time and acid and Triton X-114 concentrations were optimized using a 23 factorial design and central composite design. LODs for As(lll) and total As were 0.029 and 0.022 microg/L, respectively. The accuracy of the method was confirmed with certified reference materials. The method was successfully applied in the determination of inorganic As in phosphate fertilizer samples.

A green and efficient procedure for the preconcentration and determination of cadmium, nickel and zinc from freshwater, hemodialysis solutions and tuna fish samples by cloud point extraction and flame atomic absorption spectrometry.

PubMed

Galbeiro, Rafaela; Garcia, Samara; Gaubeur, Ivanise

2014-04-01

Cloud point extraction (CPE) was used to simultaneously preconcentrate trace-level cadmium, nickel and zinc for determination by flame atomic absorption spectrometry (FAAS). 1-(2-Pyridilazo)-2-naphthol (PAN) was used as a complexing agent, and the metal complexes were extracted from the aqueous phase by the surfactant Triton X-114 ((1,1,3,3-tetramethylbutyl)phenyl-polyethylene glycol). Under optimized complexation and extraction conditions, the limits of detection were 0.37μgL(-1) (Cd), 2.6μgL(-1) (Ni) and 2.3μgL(-1) (Zn). This extraction was quantitative with a preconcentration factor of 30 and enrichment factor estimated to be 42, 40 and 43, respectively. The method was applied to different complex samples, and the accuracy was evaluated by analyzing a water standard reference material (NIST SRM 1643e), yielding results in agreement with the certified values. Copyright © 2013 Elsevier GmbH. All rights reserved.

Accuracy of a method based on atomic absorption spectrometry to determine inorganic arsenic in food: Outcome of the collaborative trial IMEP-41.

PubMed

Fiamegkos, I; Cordeiro, F; Robouch, P; Vélez, D; Devesa, V; Raber, G; Sloth, J J; Rasmussen, R R; Llorente-Mirandes, T; Lopez-Sanchez, J F; Rubio, R; Cubadda, F; D'Amato, M; Feldmann, J; Raab, A; Emteborg, H; de la Calle, M B

2016-12-15

A collaborative trial was conducted to determine the performance characteristics of an analytical method for the quantification of inorganic arsenic (iAs) in food. The method is based on (i) solubilisation of the protein matrix with concentrated hydrochloric acid to denature proteins and allow the release of all arsenic species into solution, and (ii) subsequent extraction of the inorganic arsenic present in the acid medium using chloroform followed by back-extraction to acidic medium. The final detection and quantification is done by flow injection hydride generation atomic absorption spectrometry (FI-HG-AAS). The seven test items used in this exercise were reference materials covering a broad range of matrices: mussels, cabbage, seaweed (hijiki), fish protein, rice, wheat, mushrooms, with concentrations ranging from 0.074 to 7.55mgkg(-1). The relative standard deviation for repeatability (RSDr) ranged from 4.1 to 10.3%, while the relative standard deviation for reproducibility (RSDR) ranged from 6.1 to 22.8%. Copyright © 2016 The Authors. Published by Elsevier Ltd.. All rights reserved.

Vortex-assisted switchable liquid-liquid microextraction for the preconcentration of cadmium in environmental samples prior to its determination with flame atomic absorption spectrometry.

PubMed

Fırat, Merve; Bodur, Süleyman; Tışlı, Büşra; Özlü, Cansu; Chormey, Dotse Selali; Turak, Fatma; Bakırdere, Sezgin

2018-06-12

In this study, a switchable solvent was used to preconcentrate trace amounts of Cd from aqueous solution for its determination by flame atomic absorption spectrometry (FAAS). Protonation of N,N-dimethylbenzylamine by dry ice (solid CO 2 ) made it water soluble, and addition of sodium hydroxide converted it back to its original nonionic state for phase separation and subsequent extraction of Cd. A slotted quartz tube (SQT) was attached to the flame burner head to increase the residence time of Cd atoms in the light path. Under the optimum conditions, limits of detection and quantification were determined as 0.7 and 2.6 μg L -1 , respectively. Low relative standard deviations calculated from seven replicate measurements of the lowest concentration indicated high precision. Accuracy of the developed method was checked by using a standard reference material (SRM 1633c). Spiked recovery tests were also performed on lake water and wastewater samples at different concentrations to check the applicability of the developed method, and the results obtained (90-103%) established high recovery.

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.

PubMed

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.

Coupled high performance liquid chromatography-microwave digestion-hydride generation-atomic absorption spectrometry for inorganic and organic arsenic speciation in fish tissue.

PubMed

Villa-Lojo, M C; Alonso-Rodríguez, E; López-Mahía, P; Muniategui-Lorenzo, S; Prada-Rodríguez, D

2002-06-10

A high performance liquid chromatography-microwave digestion-hydride generation-atomic absorption spectrometry (HPLC-MW-HG-AAS) coupled method is described for As(III), As(V), monomethylarsonic acid (MMA), dimethylarsinic acid (DMA), arsenobetaine (AsB) and arsenocholine (AsC) determination. A Hamilton PRP-X100 anion-exchange column is used for carrying out the arsenic species separation. As mobile phase 17 mM phosphate buffer (pH 6.0) is used for As(III), As(V), MMA and DMA separation, and ultrapure water (pH 6.0) for AsB and AsC separation. Prior to injection into the HPLC system AsB and AsC are isolated from the other arsenic species using a Waters Accell Plus QMA cartridge. A microwave digestion with K(2)S(2)O(8) as oxidizing agent is used for enhancing the efficiency of conversion of AsB and AsC into arsenate. Detection limits achieved were between 0.3 and 1.1 ng for all species. The method was applied to arsenic speciation in fish samples.

Determination of trace elements in automotive fuels by filter furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Anselmi, Anna; Tittarelli, Paolo; Katskov, Dmitri A.

2002-03-01

The determination of Cd, Cr, Cu, Pb and Ni was performed in gasoline and diesel fuel samples by electrothermal atomic absorption spectrometry using the Transverse Heated Filter Atomizer (THFA). Thermal conditions were experimentally defined for the investigated elements. The elements were analyzed without addition of chemical modifiers, using organometallic standards for the calibration. Forty-microliter samples were injected into the THFA. Gasoline samples were analyzed directly, while diesel fuel samples were diluted 1:4 with n-heptane. The following characteristic masses were obtained: 0.8 pg Cd, 6.4 pg Cr, 12 pg Cu, 17 pg Pb and 27 pg Ni. The limits of determination for gasoline samples were 0.13 μg/kg Cd, 0.4 μg/kg Cr, 0.9 μg/kg Cu, 1.5 μg/kg Pb and 2.5 μg/kg Ni. The corresponding limit of determination for diesel fuel samples was approximately four times higher for all elements. The element recovery was performed using the addition of organometallic compounds to gasoline and diesel fuel samples and was between 85 and 105% for all elements investigated.

Ligandless dispersive liquid--liquid microextraction of iron in biological and foodstuff samples and its determination by Electrothermal atomic absorption spectrometry.

PubMed

Madadizadeh, Mohadeseh; Taher, Mohammad Ali; Ashkenani, Hamid

2013-01-01

A new, simple, and efficient method comprising ligandless dispersive liquid-liquid microextraction combined with electrothermal atomic absorption spectrometry is reported for the preconcentration and determination of ultratrace amounts of Fe(III). Carbon tetrachloride and acetone were used as the extraction and disperser solvents, respectively. Some effective parameters of the microextraction such as choice of extraction and disperser solvents, their volume, extraction time and temperature, salt and surfactant effect, and pH were optimized. Under the optimum conditions, the calibration curve was linear in the range of 0.02 to 0.46 microg/L of Fe(III), with LOD and LOQ of 5.2 and 17.4 ng/L, respectively. The RSD for seven replicated determinations of Fe(IIl) ion at 0.1 microg/L concentration level was 5.2%. Operational simplicity, rapidity, low cost, good repeatability, and low consumption of extraction solvent are the main advantages of the proposed method. The method was successfully applied to the determination of iron in biological, food, and certified reference samples.

Tear copper and its association with liver copper concentrations in six adult ewes.

PubMed Central

Schoster, J V; Stuhr, C; Kiorpes, A

1995-01-01

Tear and liver copper concentrations from 6 clinically healthy adult mixed-breed ewes were measured by Atomic Absorption Electrothermal Atomization (graphite furnace) Spectrometry and Flame Absorption Spectrometry, respectively, 7 times over 227 d to determine if their tears contained copper and if so, whether tear copper concentrations could reliably predict liver copper concentrations. To produce changes in liver copper concentration, the diet was supplemented with copper at concentrations that increased from 23 mg to 45 mg Cu/kg feed/day/sheep during the study. This regimen raised liver copper for all sheep to potentially toxic hepatic tissue concentration of greater than 500 mg/kg dry (DM) matter (tissue). The results of the study showed that copper was present in the tears of all sheep. The mean tear copper concentration showed a positive correlation with liver copper concentration (P = 0.003), increasing from 0.07 mg/kg DM at the start to 0.44 mg/kg DM at the end of the study, but could not reliably predict liver copper concentration (R2 = 0.222). PMID:7648525

Proteomic analysis of the enterocyte brush border

PubMed Central

McConnell, Russell E.; Benesh, Andrew E.; Mao, Suli; Tabb, David L.

2011-01-01

The brush border domain at the apex of intestinal epithelial cells is the primary site of nutrient absorption in the intestinal tract and the primary surface of interaction with microbes that reside in the lumen. Because the brush border is positioned at such a critical physiological interface, we set out to create a comprehensive list of the proteins that reside in this domain using shotgun mass spectrometry. The resulting proteome contains 646 proteins with diverse functions. In addition to the expected collection of nutrient processing and transport components, we also identified molecules expected to function in the regulation of actin dynamics, membrane bending, and extracellular adhesion. These results provide a foundation for future studies aimed at defining the molecular mechanisms underpinning brush border assembly and function. PMID:21330445

Analysis of Fusarium mycotoxins by gas chromatography--Fourier transform infrared spectroscopy.

PubMed

Young, J C; Games, D E

1994-03-11

The Fourier transform infrared (FTIR) spectra of selected Fusarium mycotoxins of various structure types were determined. Absorptions were observed for the following functionalities: hydroxyl at 3625-65 cm-1 and 3482 cm-1, the latter being associated with a 7 alpha-hydroxyl adjacent to an 8-carbonyl in keto trichothecenes; carbonyl at 1760-6 cm-1 for 5-membered rings and at 1695-8 cm-1 for those conjugated to a single C = C in a six-membered ring; acetate carbonyl at 1765 cm-1 and acetate C-O at 1220-9 cm-1; and C = C at 1680 cm-1. Gas chromatography combined with FTIR and mass spectrometry was applied to the identification of some mycotoxins in a F. roseum liquid culture extract.

Lithographically fabricated silicon microreactor for in situ characterization of heterogeneous catalysts—Enabling correlative characterization techniques

DOE Office of Scientific and Technical Information (OSTI.GOV)

Baier, S.; Rochet, A.; Hofmann, G.

2015-06-15

We report on a new modular setup on a silicon-based microreactor designed for correlative spectroscopic, scattering, and analytic on-line gas investigations for in situ studies of heterogeneous catalysts. The silicon microreactor allows a combination of synchrotron radiation based techniques (e.g., X-ray diffraction and X-ray absorption spectroscopy) as well as infrared thermography and Raman spectroscopy. Catalytic performance can be determined simultaneously by on-line product analysis using mass spectrometry. We present the design of the reactor, the experimental setup, and as a first example for an in situ study, the catalytic partial oxidation of methane showing the applicability of this reactor formore » in situ studies.« less

A critical review of inductively coupled plasma-mass spectrometry for geoanalysis, geochemistry and hydrology, Part 1. Analytical performance

USGS Publications Warehouse

Brenner, I.B.; Taylor, Howard E.

1992-01-01

Present-day inductively coupled plasma-mass spectrometry (ICP-MS) instrumentation is described briefly. Emphasis is placed on performance characteristics for geoanalysis, geochemistry, and hydrology. Applications where ICP-MS would be indispensable are indicated. Determination of geochemically diagnostic trace elements (such as the rare earth elements [REE], U and Th), of isotope ratios for fingerprinting, tracer and other geo-isotope applications, and benchmark isotope dilution determinations are considered to be typical priority applications for ICP-MS. It is concluded that ICP-MS furnishes unique geoanalytical and environmental data that are not readily provided by conventional spectroscopic (emission and absorption) techniques.

Application of 1-(2-pyridylazo)-2-naphthol-modified nanoporous silica as a technique in simultaneous trace monitoring and removal of toxic heavy metals in food and water samples.

PubMed

Abolhasani, Jafar; Behbahani, Mohammad

2015-01-01

Solid-phase extraction is one the most useful and efficient techniques for sample preparation, purification, cleanup, preconcentration, and determination of heavy metals at trace levels. In this paper, functionalized MCM-48 nanoporous silica with 1-(2-pyridylazo)-2-naphthol was applied for trace determination of copper, lead, cadmium, and nickel in water and seafood samples. The experimental conditions such as pH, sample and eluent flow rate, type, concentration and volume of the eluent, breakthrough volume, and effect of coexisting ions were optimized for efficient solid-phase extraction of trace heavy metals in different water and seafood samples. The content of solutions containing the mentioned heavy metals was determined by flame atomic absorption spectrometry (FAAS), and the limits of detection were 0.3, 0.4, 0.6, and 0.9 ng mL(-1) for cadmium, copper, nickel, and lead, respectively. Recoveries and precisions were >98.0 and <4%, respectively. The adsorption capacity of the modified nanoporous silica was 178 mg g(-1) for cadmium, 110 mg g(-1) for copper, 98 mg g(-1) for nickel, and 210 mg g(-1) for lead, respectively. The functionalized MCM-48 nanoporous silica with 1-(2-pyridylazo)-2-naphthol was characterized by thermogravimetry analysis (TGA), differential thermal analysis (DTA), transmission electron microscopy (TEM), Fourier transform infrared spectrometry (FT-IR), X-ray diffraction (XRD), elemental analysis (CHN), and N2 adsorption surface area measurement.

Ethylene hydrogenation catalysis on Pt(111) single-crystal surfaces studied by using mass spectrometry and in situ infrared absorption spectroscopy

NASA Astrophysics Data System (ADS)

Tillekaratne, Aashani; Simonovis, Juan Pablo; Zaera, Francisco

2016-10-01

The catalytic hydrogenation of ethylene promoted by a Pt(111) single crystal was studied by using a ultrahigh-vacuum surface-science instrument equipped with a so-called high-pressure cell. Kinetic data were acquired continuously during the catalytic conversion of atmospheric-pressure mixtures of ethylene and hydrogen by using mass spectrometry while simultaneously characterizing the surface species in operando mode by reflection-absorption infrared spectroscopy (RAIRS). Many observations reported in previous studies of this system were corroborated, including the presence of adsorbed alkylidyne intermediates during the reaction and the zero-order dependence of the rate of hydrogenation on the pressure of ethylene. In addition, the high quality of the kinetic data, which could be recorded continuously versus time and processed to calculate time-dependent turnover frequencies (TOFs), afforded a more detailed analysis of the mechanism. Specifically, deuterium labeling could be used to estimate the extent of isotope scrambling reached with mixed-isotope-substituted reactants (C2H4 + D2 and C2D4 + H2). Perhaps the most important new observation from this work is that, although extensive H-D exchange takes place on ethylene before being fully converted to ethane, the average stoichiometry of the final product retains the expected stoichiometry of the gas mixture, that is, four regular hydrogen atoms and two deuteriums per ethane molecule in the case of the experiments with C2H4 + D2. This means that no hydrogen atoms are removed from the surface via their inter-recombination to produce X2 (X = H or D). It is concluded that, under catalytic conditions, hydrogen surface recombination is much slower than ethylene hydrogenation and H-D exchange.

Fast determination of trace elements in organic fertilizers using a cup-horn reactor for ultrasound-assisted extraction and fast sequential flame atomic absorption spectrometry.

PubMed

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.

Impact of breeding region and season on the content of some trace elements and heavy metals in the hair of cows.

PubMed

Cygan-Szczegielniak, Dorota; Stanek, Magdalena; Giernatowska, Emilia; Janicki, Bogdan

2014-01-01

The aim of the research was to determine the effect of the season and the breeding region on the content of selected minerals (Zn, Cu, Mn, Fe, Pb, Cd) in the hair of dairy cows. The research material covered 114 Holstein-Friesian breed cows from three breeding centres in Poland, hereafterreferred to as A, B and C. Breeding centre A is located in Opolskie province, breeding centre B in Podlaskie province and breeding centre C in Kujawsko-Pomorskie province. The cows were kept in freestanding cowsheds with den boxes. Animal nutrition involved the use of the TMR system, considering division into nutrition groups. Hair was sampled in summer and in the period of winter and spring from the side of the body, directly behind the coastal arch. The Zn, Cu, Mn, Fe analysis was performed with atomic absorption spectrometry. The Pb and Cd content was assayed with the use of the electrothermal atomic absorption spectrometry. The results demonstrated the effect of season and breeding region on the level of the minerals and heavy metals assayed in the hair of cows being in the period of drying-off. The hair sampled in winter from cows from C demonstrated a higher concentration of most elements except for Fe than in material derived in summer. Hair sampled in winter from cows from the B centre showed higher Zn, Cu and Pb concentrations as compared with summer. Higher Cu, Mn, Fe and Pb concentrations were determined in hair sampled during winter from cows from A than in the material obtained in summer. The Cd content in the cow hair did not exceed the admissible norm, however, normal levels were exceeded for Pb in hair sampled in winter from cows from breeding centre C.

Method validation for control determination of mercury in fresh fish and shrimp samples by solid sampling thermal decomposition/amalgamation atomic absorption spectrometry.

PubMed

Torres, Daiane Placido; Martins-Teixeira, Maristela Braga; Cadore, Solange; Queiroz, Helena Müller

2015-01-01

A method for the determination of total mercury in fresh fish and shrimp samples by solid sampling thermal decomposition/amalgamation atomic absorption spectrometry (TDA AAS) has been validated following international foodstuff protocols in order to fulfill the Brazilian National Residue Control Plan. The experimental parameters have been previously studied and optimized according to specific legislation on validation and inorganic contaminants in foodstuff. Linearity, sensitivity, specificity, detection and quantification limits, precision (repeatability and within-laboratory reproducibility), robustness as well as accuracy of the method have been evaluated. Linearity of response was satisfactory for the two range concentrations available on the TDA AAS equipment, between approximately 25.0 and 200.0 μg kg(-1) (square regression) and 250.0 and 2000.0 μg kg(-1) (linear regression) of mercury. The residues for both ranges were homoscedastic and independent, with normal distribution. Correlation coefficients obtained for these ranges were higher than 0.995. Limits of quantification (LOQ) and of detection of the method (LDM), based on signal standard deviation (SD) for a low-in-mercury sample, were 3.0 and 1.0 μg kg(-1), respectively. Repeatability of the method was better than 4%. Within-laboratory reproducibility achieved a relative SD better than 6%. Robustness of the current method was evaluated and pointed sample mass as a significant factor. Accuracy (assessed as the analyte recovery) was calculated on basis of the repeatability, and ranged from 89% to 99%. The obtained results showed the suitability of the present method for direct mercury measurement in fresh fish and shrimp samples and the importance of monitoring the analysis conditions for food control purposes. Additionally, the competence of this method was recognized by accreditation under the standard ISO/IEC 17025.

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.

PubMed

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

PubMed

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.

Development of new portable miniaturize solid phase microextraction of silver-APDC complex using micropipette tip in-syringe system couple with electrothermal atomic absorption spectrometry.

PubMed

Naeemullah; Kazi, Tasneem Gul; Afridi, Hassan Imran; Shah, Faheem; Arain, Sadaf Sadia; Arain, Salma Aslam; Panhwar, Abdul Haleem; Arain, Mariam Shahzadi; Samoon, Muhammad Kashif

2016-02-05

An innovative and simple miniaturized solid phase microextraction (M-SPME) method, was developed for preconcentration and determination of silver(I) in the fresh and waste water samples. For M-SPME, a micropipette tip packed with activated carbon cloth (ACC) as sorbent, in a syringe system. The size, morphology and elemental composition of ACC before and after adsorption of analyte have been characterized by scanning electron microscopy and energy dispersive spectroscopy. The sample solution treated with a complexing reagent, ammonium pyrrolidine dithiocarbamate (APDC), was drawn into the syringe filled with ACC and dispensed manually for 2 to 10 aspirating/dispensing cycle. Then the Ag- complex sorbed on the ACC in micropipette was quantitatively eluted by drawing and dispensing of different concentrations of acids for 2 to 5 aspirating/dispensing cycles. The extracted Ag ions with modifier were injected directly into the electrothermal atomic absorption spectrometry for analysis. The influence of different variables on the extraction efficiency, including the concentration of ligand, pH, sample volume, eluent type, concentration and volume was investigated. Validity and accuracy of the developed method was checked by the standard addition method. Reliability of the proposed methodology was checked by the relative standard deviation (%RSD), which was found to be <5%. Under the optimized experimental variables, the limits of detection (LOD) and enhancement factors (EF), were obtained to be 0.86 ng L(-1) and 120, respectively. The proposed method was successfully applied for the determination of trace levels of silver ions in fresh and waste water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Simultaneous determination of V, Ni and Fe in fuel fly ash using solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry.

PubMed

Cárdenas Valdivia, A; Vereda Alonso, E; López Guerrero, M M; Gonzalez-Rodriguez, J; Cano Pavón, J M; García de Torres, A

2018-03-01

A green and simple method has been proposed in this work for the simultaneous determination of V, Ni and Fe in fuel ash samples by solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry (SS HR CS GFAAS). The application of fast programs in combination with direct solid sampling allows eliminating pretreatment steps, involving minimal manipulation of sample. Iridium treated platforms were applied throughout the present study, enabling the use of aqueous standards for calibration. Correlation coefficients for the calibration curves were typically better than 0.9931. The concentrations found in the fuel ash samples analysed ranged from 0.66% to 4.2% for V, 0.23-0.7% for Ni and 0.10-0.60% for Fe. Precision (%RSD) were 5.2%, 10.0% and 9.8% for V, Ni and Fe, respectively, obtained as the average of the %RSD of six replicates of each fuel ash sample. The optimum conditions established were applied to the determination of the target analytes in fuel ash samples. In order to test the accuracy and applicability of the proposed method in the analysis of samples, five ash samples from the combustion of fuel in power stations, were analysed. The method accuracy was evaluated by comparing the results obtained using the proposed method with the results obtained by ICP OES previous acid digestion. The results showed good agreement between them. The goal of this work has been to develop a fast and simple methodology that permits the use of aqueous standards for straightforward calibration and the simultaneous determination of V, Ni and Fe in fuel ash samples by direct SS HR CS GFAAS. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of methylmercury and inorganic mercury in water samples by slurry sampling cold vapor atomic absorption spectrometry in a flow injection system after preconcentration on silica C(18) modified.

PubMed

Segade, Susana Río; Tyson, Julian F

2007-03-15

A novel method for preconcentration of methylmercury and inorganic mercury from water samples was developed involving the determination of ngl(-1) levels of analytes retained on the silica C(18) solid sorbent, previous complexation with ammonium pyrrolidine dithiocarbamate (APDC), by slurry sampling cold vapor atomic absorption spectrometry (SS-CVAAS) in a flow injection (FI) system. Several variables were optimized affecting either the retention of both mercury species, such as APDC concentration, silica C(18) amount, agitation times, or their determination, including hydrochloric acid concentration in the suspension medium, peristaltic pump speed and argon flow-rate. A Plackett-Burman saturated factorial design permitted to differentiate the influential parameters on the preconcentration efficiency, which were after optimized by the sequential simplex method. The contact time between mercury containing solution and APDC, required to reach an efficient sorption, was decreased from 26 to 3min by the use of sonication stirring instead of magnetic stirring. The use of 1moldm(-3) hydrochloric acid suspension medium and 0.75% (m/v) sodium borohydride reducing agent permitted the selective determination of methylmercury. The combination of 5moldm(-3) hydrochloric acid and 10(-4)% (m/v) sodium borohydride was used for the selective determination of inorganic mercury. The detection limits achieved for methylmercury and inorganic mercury determination under optimum conditions were 0.96 and 0.25ngl(-1), respectively. The reliability of the proposed method for the determination of both mercury species in waters was checked by the analysis of samples spiked with known concentrations of methylmercury and inorganic mercury; quantitative recoveries were obtained.

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

PubMed

Baytak, Sitki; Türker, A Rehber

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(-1), respectively. The capacity of the sorbent was found as 0.17 and 0.21 mmol g(-1) for Pb and Ni, respectively. The interferences of some cations, such as Mn2+, Co2+, Fe3+, Al3+, Zn2+, Cd2+, Ca2+, Mg2+, K+ and Na+ 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.

Air Pollution Study in the Republic of Moldova Using Moss Biomonitoring Technique.

PubMed

Zinicovscaia, Inga; Hramco, Constantin; Duliu, Octavian G; Vergel, Konstantin; Culicov, Otilia A; Frontasyeva, Marina V; Duca, Gheorghe

2017-02-01

Moss biomonitoring using the species Hypnum cupressiforme (Hedw.) and Pleurocarpous sp was applied to study air pollution in the Republic of Moldova. A total of 41 elements (Na, Mg, Al, Cl, K, Ca, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Br, Rb, Sr, Zr, Cd, Sb, Cs, Ba, La, Ce, Nd, Sm, Eu, Gd, Tb, Tm, Yb, Hf, Ta, W, Pb, Th, and U) were determined by instrumental epithermal neutron activation analysis and atomic absorption spectrometry. Principal component analysis was used to identify and characterize different pollution sources. Geographical distribution maps were prepared to point out the regions most affected by air pollution and relate this to potential sources of contamination. Median values of the elements studied were compared with data from the European moss biomonitoring program. The cities of Chisinau and Balti were determined to experience particular environmental stress.

Soft-landing ion mobility of silver clusters for small-molecule matrix-assisted laser desorption ionization mass spectrometry and imaging of latent fingerprints.

PubMed

Walton, Barbara L; Verbeck, Guido F

2014-08-19

Matrix-assisted laser desorption ionization (MALDI) imaging is gaining popularity, but matrix effects such as mass spectral interference and damage to the sample limit its applications. Replacing traditional matrices with silver particles capable of equivalent or increased photon energy absorption from the incoming laser has proven to be beneficial for low mass analysis. Not only can silver clusters be advantageous for low mass compound detection, but they can be used for imaging as well. Conventional matrix application methods can obstruct samples, such as fingerprints, rendering them useless after mass analysis. The ability to image latent fingerprints without causing damage to the ridge pattern is important as it allows for further characterization of the print. The application of silver clusters by soft-landing ion mobility allows for enhanced MALDI and preservation of fingerprint integrity.

Infiltration of trace metal ions in the oral mucosa of a rat analyzed using SRXRF, XAFS, and ICP-MS.

PubMed

Imamura, Toshihiro; Kanno, Zuisei; Imai, Haruki; Sugiyama, Tomoko; Wada, Takahiro; Yoshida, Midori; Sakama, Minoru; Ono, Takashi; Honda, Eiichi; Uo, Motohiro

2015-01-01

Although the accumulation and distribution of metals from metallic orthodontic appliances in the oral mucosa have been studied extensively, they remain unclear because their concentration is quite low. In this study, metal specimens (Ni, Ni-Ti, and Co-Cr) were sutured in the unilateral oral mucosa of rats, and the distribution of the eluted elements in the mucosal tissue was estimated using inductively coupled plasma mass spectrometry (ICP-MS) and synchrotron radiation X-ray fluorescence analysis (SR-XRF). While the infiltrations of Ni, Co, and Cr into the oral mucosal connective tissue were observed with SR-XRF, significant increases were only found in Ni from the pure Ni group and Cr from the Co-Cr group. Furthermore, Ni and Co were estimated as hydrated ions while Cr was estimated in oxide form through X-ray absorption fine structure (XAFS) analysis.

Vacuum ultraviolet detector for gas chromatography.

PubMed

Schug, Kevin A; Sawicki, Ian; Carlton, Doug D; Fan, Hui; McNair, Harold M; Nimmo, John P; Kroll, Peter; Smuts, Jonathan; Walsh, Phillip; Harrison, Dale

2014-08-19

Analytical performance characteristics of a new vacuum ultraviolet (VUV) detector for gas chromatography (GC) are reported. GC-VUV was applied to hydrocarbons, fixed gases, polyaromatic hydrocarbons, fatty acids, pesticides, drugs, and estrogens. Applications were chosen to feature the sensitivity and universal detection capabilities of the VUV detector, especially for cases where mass spectrometry performance has been limited. Virtually all chemical species absorb and have unique gas phase absorption cross sections in the approximately 120-240 nm wavelength range monitored. Spectra are presented, along with the ability to use software for deconvolution of overlapping signals. Some comparisons with experimental synchrotron data and computed theoretical spectra show good agreement, although more work is needed on appropriate computational methods to match the simultaneous broadband electronic and vibronic excitation initiated by the deuterium lamp. Quantitative analysis is governed by Beer-Lambert Law relationships. Mass on-column detection limits reported for representatives of different classes of analytes ranged from 15 (benzene) to 246 pg (water). Linear range measured at peak absorption for benzene was 3-4 orders of magnitude. Importantly, where absorption cross sections are known for analytes, the VUV detector is capable of absolute determination (without calibration) of the number of molecules present in the flow cell in the absence of chemical interferences. This study sets the stage for application of GC-VUV technology across a wide breadth of research areas.

Atmospheric pressure laser desorption/ionization using a 6-7 µm-band mid-infrared tunable laser and liquid water matrix.

PubMed

Hiraguchi, Ryuji; Hazama, Hisanao; Masuda, Katsuyoshi; Awazu, Kunio

2015-01-01

Due to the characteristic absorption peaks in the IR region, various molecules can be used as a matrix for infrared matrix-assisted laser desorption/ionization (IR-MALDI). Especially in the 6-7 µm-band IR region, solvents used as the mobile phase for liquid chromatography have absorption peaks that correspond to their functional groups, such as O-H, C=O, and CH3. Additionally, atmospheric pressure (AP) IR-MALDI, which is applicable to liquid-state samples, is a promising technique to directly analyze untreated samples. Herein we perform AP-IR-MALDI mass spectrometry of a peptide, angiotensin II, using a mid-IR tunable laser with a tunable wavelength range of 5.50-10.00 µm and several different matrices. The wavelength dependences of the ion signal intensity of [M + H](+) of the peptide are measured using a conventional solid matrix, α-cyano-4-hydroxycinnamic acid (CHCA) and a liquid matrix composed of CHCA and 3-aminoquinoline. Other than the O-H stretching and bending vibration modes, the characteristic absorption peaks are useful for AP-IR-MALDI. Peptide ions are also observed from an aqueous solution of the peptide without an additional matrix, and the highest peak intensity of [M + H](+) is at 6.00 µm, which is somewhat shorter than the absorption peak wavelength of liquid water corresponding to the O-H bending vibration mode. Moreover, long-lasting and stable ion signals are obtained from the aqueous solution. AP-IR-MALDI using a 6-7 µm-band IR tunable laser and solvents as the matrix may provide a novel on-line interface between liquid chromatography and mass spectrometry. Copyright © 2015 John Wiley & Sons, Ltd.

Speciation of Bio-Available Iodine in Abalone (Haliotis discus hannai) by High-Performance Liquid Chromatography Hyphenated with Inductively Coupled Plasma-Mass Spectrometry Using an In Vitro Method.

PubMed

Doh, Han Sol; Park, Hyun Jin

2018-06-01

Abalone is one of the most valuable marine products found in East Asia because it is rich in nutritious substances including iodine. In this study, the in vitro dialyzability approach was used to assess the bio-available iodine species in abalone. Iodide, iodate, 3-iodo-L-tyrosine (MIT), and 3,5-diiodo-L-tyrosine (DIT) were separated by high-performance liquid chromatography hyphenated with inductively coupled plasma-mass spectrometry (HPLC-ICP-MS). To assure the consistency, reliability, and accuracy of the data, the method was validated. Comparison of the total iodine in abalone muscle and viscera indicated that abalone muscle showed greater digestion/absorption efficiency than abalone viscera (digestion efficiency: 68.13 ± 2.59% and 47.88 ± 5.76% and absorption efficiency: 59.78 ± 2.93% and 35.12 ± 1.43% for abalone viscera and muscle, respectively). However, evaluation of the sum of the analyzed iodine species targeted in this study by HPLC-ICP-MS indicated that abalone muscle showed lower digestion efficiency and similar absorption efficiency compared to that of abalone viscera (digestion efficiency: 35.52 ± 5.41% and 28.84 ± 1.83%; absorption efficiency: 23.56 ± 4.38% and 27.56 ± 1.51% for abalone viscera and muscle, respectively). The main forms of iodine detected in abalone muscle were iodide and MIT, whereas iodide was the major form in abalone viscera. The bio-available iodine in abalone was quantified via an in vitro method employing HPLC-ICP-MS. The results of this study indicated that abalone is feasible as a new iodine source and may prospectively find application in iodine-fortified foods. © 2018 Institute of Food Technologists®.

Copper-65-absorption by men fed intrinsically and extrinsically labeled whole wheat bread

DOE Office of Scientific and Technical Information (OSTI.GOV)

Johnson, P.E.; Lykken, G.I.

Six men were fed a diet composed of conventional foods with all bread as whole wheat bread. Intrinsically labeled /sup 65/Cu bread (containing 6.5 ppm Cu and 48 atom % /sup 65/Cu) was substituted for unlabeled bread for 3 days, and stools were collected for 24 days. Extrinsically labeled bread was then substituted for 3 days and another 24-day stool collection made. /sup 65/Cu excretion was measured by mass spectrometry. Mean Cu intake was 1.10 mg of Cu/day. Average Cu balance was /minus/0.06 /+-/ 0.08 mg/day. Average absorption of the intrinsic copper was 72.2 /+-/ 9.3% and of extrinsic Cumore » 64.2 /+-/ 5.8%. The ratio of extrinsic to intrinsic absorption was 0.906 /+-/ 0.164. Absorption of intrinsic and extrinsic tracers did not differ significantly (p > 0.05) by a paired t-test, and the ratio (E/I) was not significantly different from 1. Use of extrinsic Cu tracers to assess Cu absorption is supported by these results.« less

Gas-Phase Dopant-Induced Conformational Changes Monitored with Transversal Modulation Ion Mobility Spectrometry.

PubMed

Meyer, Nicole Andrea; Root, Katharina; Zenobi, Renato; Vidal-de-Miguel, Guillermo

2016-02-16

The potential of a Transversal Modulation Ion Mobility Spectrometry (TMIMS) instrument for protein analysis applications has been evaluated. The Collision Cross Section (CCS) of cytochrome c measured with the TMIMS is in agreement with values reported in the literature. Additionally, it enables tandem IMS-IMS prefiltration in dry gas and in vapor doped gas. The chemical specificity of the different dopants enables interesting studies on the structure of proteins as CCS changed strongly depending on the specific dopant. Hexane produced an unexpectedly high CCS shift, which can be utilized to evaluate the exposure of hydrophobic parts of the protein. Alcohols produced higher shifts with a dual behavior: an increase in CCS due to vapor uptake at specific absorption sites, followed by a linear shift typical for unspecific and unstable vapor uptake. The molten globule +8 shows a very specific transition. Initially, its CCS follows the trend of the compact folded states, and then it rapidly increases to the levels of the unfolded states. This strong variation suggests that the +8 charge state undergoes a dopant-induced conformational change. Interestingly, more sterically demanding alcohols seem to unfold the protein more effectively also in the gas phase. This study shows the capabilities of the TMIMS device for protein analysis and how tandem IMS-IMS with dopants could provide better understanding of the conformational changes of proteins.

NBSGSC - a FORTRAN program for quantitative x-ray fluorescence analysis. Technical note (final)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tao, G.Y.; Pella, P.A.; Rousseau, R.M.

1985-04-01

A FORTRAN program (NBSGSC) was developed for performing quantitative analysis of bulk specimens by x-ray fluorescence spectrometry. This program corrects for x-ray absorption/enhancement phenomena using the comprehensive alpha coefficient algorithm proposed by Lachance (COLA). NBSGSC is a revision of the program ALPHA and CARECAL originally developed by R.M. Rousseau of the Geological Survey of Canada. Part one of the program (CALCO) performs the calculation of theoretical alpha coefficients, and part two (CALCOMP) computes the composition of the analyte specimens. The analysis of alloys, pressed minerals, and fused specimens can currently be treated by the program. In addition to using measuredmore » x-ray tube spectral distributions, spectra from seven commonly used x-ray tube targets could also be calculated with an NBS algorithm included in the program. NBSGSC is written in FORTRAN IV for a Digital Equipment Corporation (DEC PDP-11/23) minicomputer using RLO2 firm disks and an RSX 11M operating system.« less

Garlic (Allium sativum L.) as a potential antidote for cadmium and lead intoxication: cadmium and lead distribution and analysis in different mice organs.

PubMed

Massadeh, A M; Al-Safi, S A; Momani, I F; Alomary, A A; Jaradat, Q M; AlKofahi, A S

2007-01-01

Analysis and distribution of Pb and Cd in different mice organs including liver, kidney, spleen, heart and blood were evaluated after treatment with different aqueous concentrations of garlic (12.5-100 mg/l). Atomic absorption spectrometry (AAS) was used for analysis of Pb and Cd in these organs. Treatment of Cd-Pb exposed mice with garlic (12.5-100 mg/l) reduced Pb concentrations by 44.65, 42.61, 38.4, 47.56, and 66.62% in liver, kidney, heart, spleen and blood respectively. Moreover, garlic reduced Cd levels by 72.5, 87.7, 92.6, 95.6, and 71.7% in liver, kidney, heart, spleen and blood respectively. The suppressed immune responses in mice pretreated with Cd-Pb mixture were reversed by 48.85, 55.82, 81.4 and 90.7 in the presence of 100, 50, 25, and 12.5 mg/ml of garlic extract.

An x ray scatter approach for non-destructive chemical analysis of low atomic numbered elements

NASA Technical Reports Server (NTRS)

Ross, H. Richard

1993-01-01

A non-destructive x-ray scatter (XRS) approach has been developed, along with a rapid atomic scatter algorithm for the detection and analysis of low atomic-numbered elements in solids, powders, and liquids. The present method of energy dispersive x-ray fluorescence spectroscopy (EDXRF) makes the analysis of light elements (i.e., less than sodium; less than 11) extremely difficult. Detection and measurement become progressively worse as atomic numbers become smaller, due to a competing process called 'Auger Emission', which reduces fluorescent intensity, coupled with the high mass absorption coefficients exhibited by low energy x-rays, the detection and determination of low atomic-numbered elements by x-ray spectrometry is limited. However, an indirect approach based on the intensity ratio of Compton and Rayleigh scattered has been used to define light element components in alloys, plastics and other materials. This XRS technique provides qualitative and quantitative information about the overall constituents of a variety of samples.

IR and py/GC/MS examination of amber relics excavated from 6th century royal tomb in Korean Peninsula.

PubMed

Park, Jongseo; Yun, Eunyoung; Kang, Hyungtae; Ahn, Jooyoung; Kim, Gyuho

2016-08-05

Relics of amber were excavated from King Muryeong's tomb constructed in the 6th century on the Korean peninsula. To estimate the provenance, FTIR (Fourier transform infrared spectroscopy) and py/GC/MS (pyrolysis/gas chromatography/mass spectrometry) analysis were utilized. The reference Baltic amber sample was also analyzed with the same method for comparison. The relics were confirmed to be amber from the FTIR analysis where an absorption band near 1150cm(-1), characteristic one in Baltic amber, was also observed. In py/GC/MS analysis, pyrolyzed products like butanedioic acid and dehydroabietic acid, known constituents of amber, were observed. In addition, d-fenchyl alcohol, camphor, borneol and butanedioic acid, typical constituents of Baltic amber, were observed in some samples. From this, it appears that some of relics were made from Baltic amber and that Baltic amber was transported to the Korean peninsula in the time of tomb construction. Copyright © 2016 Elsevier B.V. All rights reserved.

Lipidomic analysis of glycerolipid and cholesteryl ester autooxidation products.

PubMed

Kuksis, Arnis; Suomela, Jukka-Pekka; Tarvainen, Marko; Kallio, Heikki

2009-06-01

Thin-layer chromatography (TLC), gas chromatography (GC), and liquid chromatography (LC) in combination with mass spectrometry (MS) have been adopted for the isolation and identification of oxolipids and for determining their functionality. TLC provides a rapid separation and access to most oxolipids as intact molecules and has recently been effectively interfaced with time-of-flight (TOF) MS (TOF-MS). GC with flame ionization (FI) (GC/FI) and electron impact (EI) MS (GC/EI-MS) has been extensively utilized in the analysis of isoprostanes and other low-molecular-weight oxolipids, although these methods require derivatization of the analytes. In contrast, LC with ultraviolet (UV) absorption (LC/UV) or evaporate light scattering detection (ELSD) (LC/ELSD) as well as electrospray ionization (ESI) or atmospheric pressure chemical ionization (APCI) MS (LC/ESI-MS) or LC/APCI-MS has proven to be well suited for the analysis of intact oxolipids and their conjugates without or with minimal derivatization. Nevertheless, kit-based colorimetric and fluorescent procedures continue to serve as sensitive indicators of the presence of hydroperoxides and aldehydes.

Dereplication-guided isolation of a new indole alkaloid triglycoside from the hooks of Uncaria rhynchophylla by LC with ion trap time-of-flight MS.

PubMed

Zhang, Jian-Gang; Huang, Xiao-Yan; Ma, Yun-Bao; Zhang, Xue-Mei; Chen, Ji-Jun; Geng, Chang-An

2018-04-01

Uncaria rhynchophylla (Gou-Teng) as the monarch herb of many formulae (Fufang), e.g. "Tian-Ma-Gou-Teng-Yin," "Ling-Jiao-Gou-Teng-Yin," and "Yi-Gan-San", is a famous traditional Chinese medicine documented in the Chinese pharmacopoeia for mental and cardiovascular diseases. In the traditional Chinese medicine system, only the hook-bearing stems are used as the crude materials for Gou-Teng, and the hooks are always considered more effective than the stems. Focusing on the mono-herb and its active constituents from combinatorial formulae is the core idea of reductionism of traditional Chinese medicine theory. Detailed liquid chromatography with mass spectrometry analysis on the hooks of U. rhynchophylla was performed to profile the chemical constituents based on tandem mass spectrometry fragmentation and UV absorption. Under the guidance of liquid chromatography with ion trap/time-of-flight mass spectrometry, one new indole alkaloid triglycoside (1), together with five known compounds 2-6 as the main constituents, were isolated from the hooks of U. rhynchophylla by various column chromatography methods. Compound 1 showed moderate activity on MT 1 and MT 2 melatonin receptors with agonistic rates of 79.6 and 46.3% at the concentration of 1 mM. This dereplication strategy can be equally applicable to rapidly disclose the active constituents of other Chinese herbs through targeted purification. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; preparation procedure for aquatic biological material determined for trace metals

USGS Publications Warehouse

Hoffman, Gerald L.

1996-01-01

A method for the chemical preparation of tissue samples that are subsequently analyzed for 22 trace metals is described. The tissue-preparation procedure was tested with three National Institute of Standards and Technology biological standard reference materials and two National Water Quality Laboratory homogenized biological materials. A low-temperature (85 degrees Celsius) nitric acid digestion followed by the careful addition of hydrogen peroxide (30-percent solution) is used to decompose the biological material. The solutions are evaporated to incipient dryness, reconstituted with 5 percent nitric acid, and filtered. After filtration the solutions were diluted to a known volume and analyzed by inductively coupled plasma-mass spectrometry (ICP-MS), inductively coupled plasma-atomic emission spectrometry (ICP-AES), and cold vapor-atomic absorption spectrophotometry (CV-AAS). Many of the metals were determined by both ICP-MS and ICP-AES. This report does not provide a detailed description of the instrumental procedures and conditions used with the three types of instrumentation for the quantitation of trace metals determined in this study. Statistical data regarding recovery, accuracy, and precision for individual trace metals determined in the biological material tested are summarized.

Italian Renaissance and Hispano-Moresque lustre-decorated majolicas: imitation cases of Hispano-Moresque style in central Italy

NASA Astrophysics Data System (ADS)

Padeletti, G.; Fermo, P.

An investigation was carried out on Renaissance lustre-decorated majolica shards, found during excavations made in Umbria (central Italy) and defined by experts, on the ground of the surface decoration, as imitations of the Hispano-Moresque style. A comparison between this particular kind of samples, produced in central Italy, and some Hispano-Moresque lustre shards has been performed. The ceramic bodies as well as the lustred surfaces have been analysed by means of several techniques: inductively coupled plasma optical emission spectrometry, X-ray diffraction (XRD), atomic absorption spectrometry with electrothermal atomisation and scanning electron microscopy. By means of XRD analysis the presence of cosalite (Pb2Bi2S5) has been disclosed in the Italian lustre decorations but was not observed in the Hispano-Moresque ones. A hypothesis has been made, considering bismuth as a discriminating element, between lustres produced in central Italy and the Hispano-Moresque ones. We thought that the Italian artisans were able to manage the use of bismuth. Therefore a recipe, quite similar to the one employed by the Spanish artisans, was used by the Italian ceramists if their aim was to imitate the Hispano-Moresque style.

Determination of As in tree-rings of poplar (Populus alba L.) by U-shaped DC arc.

PubMed

Marković, D M; Novović, I; Vilotić, D; Ignjatović, Lj

2009-04-01

An argon-stabilized U-shaped DC arc with a system for aerosol introduction was used for determination of As in poplar (Populus alba L.) tree-rings. After optimization of the operating parameters and selection of the most appropriate signal integration time (30 s), the limit of detection for As was reduced to 15.0 ng/mL. This detection limit obtained with the optimal integration time was compared with those for other methods: inductively coupled plasma-atomic emission spectrometry (ICP-AES), direct coupled plasma-atomic emission spectrometry (DCP-AES), microwave induced plasma-atomic emission spectrometry (MIP-AES) and improved thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS). Arsenic is toxic trace element which can adversely affect plant, animal and human health. As an indicator of environment pollution we collected poplar tree-rings from two locations. The first area was close to the "Nikola Tesla" (TENT-A) power plant, Obrenovac, while the other was in the urban area of Novi Sad. In all cases elevated average concentrations of As were registered in poplar tree-rings from the Obrenovac location.

Preparation and certification of arsenate [As(V)] reference material, NMIJ CRM 7912-a.

PubMed

Narukawa, Tomohiro; Kuroiwa, Takayoshi; Narushima, Izumi; Jimbo, Yasujiro; Suzuki, Toshihiro; Chiba, Koichi

2010-05-01

Arsenate [As(V)] solution reference material, National Metrology Institute of Japan (NMIJ) certified reference material (CRM) 7912-a, for speciation of arsenic species was developed and certified by NMIJ, the National Institute of Advanced Industrial Science and Technology. High-purity As(2)O(3) reagent powder was dissolved in 0.8 M HNO(3) solution and As(III) was oxidized to As(V) with HNO(3) to prepare 100 mg kg(-1) of As(V) candidate CRM solution. The solution was bottled in 400 bottles (50 mL each). The concentration of As(V) was determined by four independent analytical techniques-inductively coupled plasma mass spectrometry, inductively coupled plasma optical emission spectrometry, graphite furnace atomic absorption spectrometry, and liquid chromatography inductively coupled plasma mass spectrometry-according to As(V) calibration solutions, which were prepared from the arsenic standard of the Japan Calibration Service system and whose species was guaranteed to be As(V) by NMIJ. The uncertainties of all the measurements and preparation procedures were evaluated. The certified value of As(V) in the CRM is (99.53 +/- 1.67) mg kg(-1) (k = 2).

Stream-sediment samples reanalyzed for major, rare earth, and trace elements from seven 1:250,000-scale quadrangles, south-central Alaska, 2007-09

USGS Publications Warehouse

Gamble, Bruce M.; Bailey, Elizabeth A.; Shew, Nora B.; Labay, Keith A.; Schmidt, Jeanine M.; O'Leary, Richard M.; Detra, David E.

2010-01-01

During the 1960s through the 1980s, the U.S. Geological Survey conducted reconnaissance geochemical surveys of drainage basins throughout most of the Iliamna, Lake Clark, Lime Hills, and Talkeetna 1:250,000-scale quadrangles and parts of the McGrath, Seldovia, and Tyonek 1:250,000-scale quadrangles in Alaska. These geochemical surveys provide data necessary to assess the potential for undiscovered mineral resources and provide data that may be used to determine regional-scale element baselines. This report provides new data for 1,075 of the previously collected stream-sediment samples. The new analyses include a broader spectrum of elements and provide data that are more precise than the original analyses. All samples were analyzed for arsenic by hydride generation atomic absorption spectrometry, for gold, palladium, and platinum by inductively coupled plasma-mass spectrometry after lead button fire assay separation, and for a suite of 55 major, rare earth, and trace elements by inductively coupled plasma-atomic emission spectrometry and inductively coupled plasma-mass spectrometry after sodium peroxide sinter at 450 degrees Celsius.

Studies of the airglow, the aurora, the ion and neutral composition, and the chemistry of the terrestrial atmosphere

NASA Technical Reports Server (NTRS)

Zipf, E. C., Jr.

1974-01-01

Results obtained by rocket-borne optical spectrometry are presented. Composition measurements and auroral studies are reported. The production of N (D-2) atoms by photo-absorption processes, and by electron impact excitation of N2 are discussed along with vibrationally excited CO2(+) ions in planetary atmospheres.

Determination of vibration-rotation lines intensities from absorption Fourier spectra

NASA Technical Reports Server (NTRS)

Mandin, J. Y.

1979-01-01

The method presented allows the line intensities to be calculated from either their equivalent widths, heights, or quantities deduced from spectra obtained by Fourier spectrometry. This method has proven its effectiveness in measuring intensities of 60 lines of the molecule H2O with a precision of 10%. However, this method cannot be applied to isolated lines.

Tandem Mass Spectrometry for Structural Identification of Sesquiterpene alkaloids from the stems of dendrobium nobile using LC-QToF3

USDA-ARS?s Scientific Manuscript database

Dendrobium nobile is one of the fundamental herbs in traditional Chinese medicine (TCM). Sesquiterpene alkaloids are the main active components in this plant. Due to weak ultraviolet absorption and low content in D. nobile, these sesquiterpene alkaloids have not been extensively studied using chroma...

Characterization of reaction intermediate aggregates in aniline oxidative polymerization at low proton concentration.

PubMed

Ding, Zhongfen; Sanchez, Timothy; Labouriau, Andrea; Iyer, Srinivas; Larson, Toti; Currier, Robert; Zhao, Yusheng; Yang, Dali

2010-08-19

Aggregates of reaction intermediates form during the early stages of aniline oxidative polymerization whenever the initial mole ratio of proton concentration to aniline monomer concentration is low ([H(+)](0)/[An](0)

Rutherford Backscattering Spectrometry studies of 100 keV nitrogen ion implanted polypropylene polymer

NASA Astrophysics Data System (ADS)

Chawla, Mahak; Aggarwal, Sanjeev; Sharma, Annu

2017-09-01

The effect of nitrogen ion implantation on the structure and composition in polypropylene (PP) polymer has been studied. Implantation was carried out using 100 keV N+ ions at different fluences of 1 × 1015, 1 × 1016 and 1 × 1017 ions cm-2 with beam current density of ∼0.65 μA cm-2. Surface morphological changes in the pre- and post-implanted PP specimens have been studied using Rutherford Backscattering Spectrometry (RBS) and UV-Visible Spectroscopy. The spatial distribution of implantation induced modification in the form of carbonization and dehydrogenation in the near surface region of PP matrix, the projected range, retained dose of implanted nitrogen, the various elements present in the implanted layers and their differential cross-sections have been analyzed using RBS spectra. RUMP simulation yielded an increase in the concentration of carbon near the surface from 33 at.% (virgin) to 42 at.% at fluence of 1 × 1017 N+ cm-2. Further, optical absorption has been found to increase with a shift in the absorption edge from UV towards visible region with increasing fluence. UV-Vis absorption spectra also indicate a drastic decrease in optical energy gap from 4.12 eV (virgin) to 0.25 eV (1 × 1017 N+ cm-2) indicating towards the formation of carbonaceous network in the implanted region. All these changes observed using UV-Visible have been further correlated with the outcomes of the RBS characterization.

Use of electrothermal atomic absorption spectrometry for size profiling of gold and silver nanoparticles.

PubMed

Panyabut, Teerawat; Sirirat, Natnicha; Siripinyanond, Atitaya

2018-02-13

Electrothermal atomic absorption spectrometry (ETAAS) was applied to investigate the atomization behaviors of gold nanoparticles (AuNPs) and silver nanoparticles (AgNPs) in order to relate with particle size information. At various atomization temperatures from 1400 °C to 2200 °C, the time-dependent atomic absorption peak profiles of AuNPs and AgNPs with varying sizes from 5 nm to 100 nm were examined. With increasing particle size, the maximum absorbance was observed at the longer time. The time at maximum absorbance was found to linearly increase with increasing particle size, suggesting that ETAAS can be applied to provide the size information of nanoparticles. With the atomization temperature of 1600 °C, the mixtures of nanoparticles containing two particle sizes, i.e., 5 nm tannic stabilized AuNPs with 60, 80, 100 nm citrate stabilized AuNPs, were investigated and bimodal peaks were observed. The particle size dependent atomization behaviors of nanoparticles show potential application of ETAAS for providing size information of nanoparticles. The calibration plot between the time at maximum absorbance and the particle size was applied to estimate the particle size of in-house synthesized AuNPs and AgNPs and the results obtained were in good agreement with those from flow field-flow fractionation (FlFFF) and transmission electron microscopy (TEM) techniques. Furthermore, the linear relationship between the activation energy and the particle size was observed. Copyright © 2017 Elsevier B.V. All rights reserved.

Study on the Absorbed Fingerprint-Efficacy of Yuanhu Zhitong Tablet Based on Chemical Analysis, Vasorelaxation Evaluation and Data Mining

PubMed Central

Chen, Yanjun; Zhang, Yingchun; Tang, Shihuan; Wang, Shanshan; Shen, Dan; Wang, Xuguang; Lei, Yun; Li, Defeng; Zhang, Yi; Jin, Lan; Yang, Hongjun; Huang, Luqi

2013-01-01

Yuanhu Zhitong Tablet (YZT) is an example of a typical and relatively simple clinical herb formula that is widely used in clinics. It is generally believed that YZT play a therapeutical effect in vivo by the synergism of multiple constituents. Thus, it is necessary to build the relationship between the absorbed fingerprints and bioactivity so as to ensure the quality, safety and efficacy. In this study, a new combinative method, an intestinal absorption test coupled with a vasorelaxation bioactivity experiment in vitro, was a simple, sensitive, and feasible technique to study on the absorbed fingerprint-efficacy of YZT based on chemical analysis, vasorelaxation evaluation and data mining. As part of this method, an everted intestinal sac method was performed to determine the intestinal absorption of YZT solutions. YZT were dissolved in solution (n = 12), and the portion of the solution that was absorbed into intestinal sacs was analyzed using rapid-resolution liquid chromatography coupled with quadruple time-of-flight mass spectrometry (RRLC-Q-TOF/MS). Semi-quantitative analysis indicated the presence of 34 compounds. The effect of the intestinally absorbed solution on vasorelaxation of rat aortic rings with endothelium attached was then evaluated in vitro. The results showed that samples grouped by HCA from chemical profiles have similar bioactivity while samples in different groups displayed very different. Moreover, it established a relationship between the absorbed fingerprints and their bioactivity to identify important components by grey relational analysis, which could predict bioactive values based on chemical profiles and provide an evidence for the quantification of multi-constituents. PMID:24339904

Composition and Properties of Deposits Formed on the Internal Surface of Oil Pipelines

NASA Astrophysics Data System (ADS)

Gulieva, N. K.; Mustafaev, I. I.; Sabzaliev, A. A.; Garibov, R. G.

2018-03-01

The composition and physicochemical properties of oil deposits formed in pipelines during the transport of oil from Azerbaijani fields were studied by atomic absorption, chromatography-mass spectrometry, gamma spectrometry, and scanning electron microscopy methods. Up to 20% of the deposits were shown to be composed of paraffins, tars, and other heavy oil fractions, while asphaltenes and mechanical impurities (iron, sulfur, manganese, calcium, and silicon compounds) comprise about 80%. The contents of polycyclic aromatic hydrocarbons and radionuclides are within permissible levels, while the content of some heavy metals exceeds the permissible level by a factor of 1000. These data should be used in the management of waste products in petroleum pipelines.

Multivessel system for cold-vapor mercury generation. Determination of mercury in hair and fish.

PubMed

Boaventura, G R; Barbosa, A C; East, G A

1997-01-01

A multivessel system for the determination of mercury (Hg) by cold-vapor atomic absorption spectrometry (CV-AAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) was developed. The performance of the proposed device was tested by determining total Hg in quality-control samples of hair and fishes following acid digestion. Application of the apparatus to the determination of Hg by CV-AAS following alkaline digestion was studied as well. The detection limit obtained for CV-AAS was 0.11 ng/mL and for ICP-AES 1.39 ng/mL. The results show that the system is appropriate to be used in techniques involving cold-vapor generation of Hg.

The influence of organic-mineral complexes on micro-elements dynamic in ecological systems of vegetables cultivation

NASA Astrophysics Data System (ADS)

Bulgariu, D.; Buzgar, N.; Bulgariu, L.; Rusu, C.; Munteanu, N.

2009-04-01

In ecological systems of vegetable cultivation (hortic antrosols; soils from greenhouses), exists an ensemble of equilibriums between organic-mineral combinations, very sensitive even to relatively small variations of physical-chemical conditions in soils. As such, these can manifest a strong influence on organic matter, clay minerals and microelements from soil, which in turn impacts on the productivity of these soils and the quality of obtained products (vegetables, fruit). Although many studies consider these organic-mineral combinations are meta-stable combinations, our work has shown that the stability of organic-mineral combinations in hortic antrosols (especially for clay-humic, clay-ironhumic combinations and chelates) is higher. We believe that this is due to the higher flexibility of these combinations' structures with the variation of chemical-mineralogical composition and physical-chemical conditions in soil. This paper highlights the results of our research on the differentiation possibility of organic-mineral complexes, depending on their structure and composition (using Raman and FT-IR spectrometry) and the influences manifested by the organic-mineral complexes on the micro-elements dynamic from ecological systems of fresh vegetable cultivation. The non-destructive separation of organic-mineral compounds from soil samples was carried out through iso-dynamic magnetic separation and extraction in aqueous two-phase systems (PEG-based). The Raman and FT-IR spectrometry analyses on raw soil samples, extracts obtained from soil samples and separated mineral fractions have been supplemented by the results obtained through chemical, microscopic and thermal analyses and by UV-VIS absorption spectrometry. Ours experimental studies have been done on representative samples of hortic antrosol from Copou glasshouse (Iasi, Romania), and was studied five micro-elements: Zn, Ni, Cu, Mn, Cr and P. The total contents of the five microelements and their fractions differential bonded on mineral and organic components of hortic antrosols, have been determined by atomic absorption spectrometry after combined sequential extraction in solid phase extraction - aqueous biphasic (PEG based) systems. The specific mechanisms of the microelements interaction with organic components have been estimated on the basis of studies realized on fractions obtained after each extraction step by Raman and FTIR spectrometry. These data have been correlated with those obtained by chemical analysis and UV-VIS spectrometry. In conditions of hortic antrosol, from total contents of Zn, Ni, Cu, Mn and Cr, more than 65 % are binding on organic components. A specific phenomenon of hortic antrosols is the microelements complexation exclusively with the functional groups of organic macromolecules. This phenomenon has two important consequences: (i) the strong fixation of microelements (these can be extracted only in very extremely conditions, which implied the organic part destroying) and (ii) their presence determined major modifications in the structure, conformation and stability of organic macromolecules. Under these conditions, the type and structure of organic-mineral compounds represent determinant factors for the dynamic of micro-elements and organic compounds in ecological systems of vegetables cultivation. Acknowledgments The authors would like to acknowledge the financial support from Romanian Ministry of Education and Research (Project PNCDI 2-D5 no. 51045/07 an Project PNCDI 2-D5 no. 52141 / 08).

Identification and Quantification of Pesticides in Environmental Waters With Solid Phase Microextraction and Analysis Using Field-Portable Gas Chromatography-Mass Spectrometry

DTIC Science & Technology

2004-06-10

Microextraction and Analysis using Field-Portable Gas Chromatography-Mass Spectrometry Name of Candidate: CPT Michael J. Nack...and Analysis using Field-Portable Gas Chromatography-Mass Spectrometry Beyond brief excerpts is with the permission of the copyright owner, and...Pesticides in Environmental Waters with Solid Phase Microextraction and Analysis using Field-Portable Gas Chromatography-Mass Spectrometry

Diagnosis of gastroenterological diseases by metabolome analysis using gas chromatography-mass spectrometry.

PubMed

Yoshida, Masaru; Hatano, Naoya; Nishiumi, Shin; Irino, Yasuhiro; Izumi, Yoshihiro; Takenawa, Tadaomi; Azuma, Takeshi

2012-01-01

Recently, metabolome analysis has been increasingly applied to biomarker detection and disease diagnosis in medical studies. Metabolome analysis is a strategy for studying the characteristics and interactions of low molecular weight metabolites under a specific set of conditions and is performed using mass spectrometry and nuclear magnetic resonance spectroscopy. There is a strong possibility that changes in metabolite levels reflect the functional status of a cell because alterations in their levels occur downstream of DNA, RNA, and protein. Therefore, the metabolite profile of a cell is more likely to represent the current status of a cell than DNA, RNA, or protein. Thus, owing to the rapid development of mass spectrometry analytical techniques metabolome analysis is becoming an important experimental method in life sciences including the medical field. Here, we describe metabolome analysis using liquid chromatography-mass spectrometry, gas chromatography-mass spectrometry (GC-MS), capillary electrophoresis-mass spectrometry, and matrix assisted laser desorption ionization-mass spectrometry. Then, the findings of studies about GC-MS-based metabolome analysis of gastroenterological diseases are summarized, and our research results are also introduced. Finally, we discuss the realization of disease diagnosis by metabolome analysis. The development of metabolome analysis using mass spectrometry will aid the discovery of novel biomarkers, hopefully leading to the early detection of various diseases.

Apparatus and method for transient thermal infrared emission spectrometry

DOEpatents

McClelland, John F.; Jones, Roger W.

1991-12-24

A method and apparatus for enabling analysis of a solid material (16, 42) by applying energy from an energy source (20, 70) top a surface region of the solid material sufficient to cause transient heating in a thin surface layer portion of the solid material (16, 42) so as to enable transient thermal emission of infrared radiation from the thin surface layer portion, and by detecting with a spectrometer/detector (28, 58) substantially only the transient thermal emission of infrared radiation from the thin surface layer portion of the solid material. The detected transient thermal emission of infrared radiation is sufficiently free of self-absorption by the solid material of emitted infrared radiation, so as to be indicative of characteristics relating to molecular composition of the solid material.

CdZnTe substrate impurities and their effects on liquid phase epitaxy HgCdTe

NASA Astrophysics Data System (ADS)

Tower, J. P.; Tobin, S. P.; Kestigian, M.; Norton, P. W.; Bollong, A. B.; Schaake, H. F.; Ard, C. K.

1995-05-01

Impurity levels were tracked through the stages of substrate and liquid phase epitaxy (LPE) layer processing to identify sources of elements which degrade infrared photodetector performance. Chemical analysis by glow discharge mass spectrometry and Zeeman corrected graphite furnace atomic absorption effectively showed the levels of impurities introduced into CdZnTe substrate material from the raw materials and the crystal growth processes. A new purification process (in situ distillation zone refining) for raw materials was developed, resulting in improved CdZnTe substrate purity. Substrate copper contamination was found to degrade the LPE layer and device electrical properties, in the case of lightly doped HgCdTe. Anomalous HgCdTe carrier type conversion was correlated to certain CdZnTe and CdTe substrate ingots.

Micro-quantity tissue digestion for metal measurements by use of a microwave acid-digestion bomb.

PubMed

Nicholson, J R; Savory, M G; Savory, J; Wills, M R

1989-03-01

We describe a simple and convenient method for processing small amounts of tissue samples for trace-metal measurements by atomic absorption spectrometry, by use of a modified Parr microwave digestion bomb. Digestion proceeds rapidly (less than or equal to 90 s) in a sealed Teflon-lined vessel that eliminates contamination or loss from volatilization. Small quantities of tissue (5-100 mg dry weight) are digested in high-purity nitric acid, yielding concentrations of analyte that can be measured directly without further sample manipulation. We analyzed National Institute of Standards and Technology bovine liver Standard Reference Material to verify the accuracy of the technique. We assessed the applicability of the technique to analysis for aluminum in bone by comparison with a dry ashing procedure.

Analysis of Processed Foods Containing Oils and Fats by Time of Flight Mass Spectrometry with an APCI Direct Probe.

PubMed

Ito, Shihomi; Chikasou, Masato; Inohana, Shuichi; Fujita, Kazuhiro

2016-01-01

Discriminating vegetable oils and animal and milk fats by infrared absorption spectroscopy is difficult due to similarities in their spectral patterns. Therefore, a rapid and simple method for analyzing vegetable oils, animal fats, and milk fats using TOF/MS with an APCI direct probe ion source was developed. This method enabled discrimination of these oils and fats based on mass spectra and detailed analyses of the ions derived from sterols, even in samples consisting of only a few milligrams. Analyses of the mass spectra of processed foods containing oils and milk fats, such as butter, cheese, and chocolate, enabled confirmation of the raw material origin based on specific ions derived from the oils and fats used to produce the final product.

UV-Vis Action Spectroscopy Reveals a Conformational Collapse in Hydrogen-Rich Dinucleotide Cation Radicals.

PubMed

Korn, Joseph A; Urban, Jan; Dang, Andy; Nguyen, Huong T H; Tureček, František

2017-09-07

We report the generation of deoxyriboadenosine dinucleotide cation radicals by gas-phase electron transfer to dinucleotide dications and their noncovalent complexes with crown ether ligands. Stable dinucleotide cation radicals of a novel hydrogen-rich type were generated and characterized by tandem mass spectrometry and UV-vis photodissociation (UVPD) action spectroscopy. Electron structure theory analysis indicated that upon electron attachment the dinucleotide dications underwent a conformational collapse followed by intramolecular proton migrations between the nucleobases to give species whose calculated UV-vis absorption spectra matched the UVPD action spectra. Hydrogen-rich cation radicals generated from chimeric riboadenosine 5'-diesters gave UVPD action spectra that pointed to novel zwitterionic structures consisting of aromatic π-electron anion radicals intercalated between stacked positively charged adenine rings. Analogies with DNA ionization are discussed.

Analysis of UV-absorbing photoprotectant mycosporine-like amino acid (MAA) in the cyanobacterium Arthrospira sp. CU2556.

PubMed

Rastogi, Rajesh P; Incharoensakdi, Aran

2014-07-01

Mycosporine-like amino acids (MAAs) are ecologically important biomolecules with great photoprotective potential. The present study aimed to investigate the biosynthesis of MAAs in the cyanobacterium Arthrospira sp. CU2556. High-performance liquid chromatography (HPLC) with photodiode-array detection studies revealed the presence of a UV-absorbing compound with an absorption maximum at 310 nm. Based on its UV absorption spectrum and ion trap liquid chromatography/mass spectrometry (LC/MS) analysis, the compound was identified as a primary MAA mycosporine-glycine (m/z: 246). To the best of our knowledge this is the first report on the occurrence of MAA mycosporine-glycine (M-Gly) in Arthrospira strains studied so far. In contrast to photosynthetic activity under UV-A radiation, the induction of the biosynthesis of M-Gly was significantly more prominent under UV-B radiation. The content of M-Gly was found to increase with the increase in exposure time under UV-B radiation. The MAA M-Gly was highly stable under UV radiation, heat, strongly acidic and alkaline conditions. It also exhibited good antioxidant activity and photoprotective ability by detoxifying the in vivo reactive oxygen species (ROS) generated by UV radiation. Our results indicate that the studied cyanobacterium may protect itself by synthesizing the UV-absorbing/screening compounds as important defense mechanisms, in their natural brightly-lit habitat with high solar UV-B fluxes.

Chemical analysis of bioactive substances in seven siberian Saussurea species

NASA Astrophysics Data System (ADS)

Avdeeva, Elena; Reshetov, Yaroslav; Shurupova, Margarita; Zibareva, Larisa; Borisova, Evgeniia; Belousov, Mikhail

2017-11-01

Main groups of biologically active substances of seven siberian Saussurea species (S. controversa DC., S. latifolia Ledeb., S. parviflora (Poir.) DC., S. frolowii Ledeb, S. amara (L.) DC., S. salicifolia (L.) DC. and S. daurica Adams) have been studied using paper, thin-layer, performance liquid chromatography, IR spectroscopy, spectrophotometry and mass spectrometry with inductively coupled plasma. Siberian Saussurea species have a rich elemental composition and contain a variety of phenolic compounds, amino acids, polysaccharides. The majority of polysaccharides are accumulated by S. controversa, S. salicifolia and S. frolowii. These plants contain a significant amount of calcium that may be a species characteristic. All plants contain quercetin and its glycosides, in some species luteolin, kaempferol, glycosides of apigenin and myricetin were revealed. Phenolic acids with predominant content of caffeic, chlorogenic and cinnamic acids were found in all the species. The maximum amount of phenolic acids and flavonoids was determined in the grass of S. latifolia, S. controversa and S. daurica. Characteristic absorption bands of lactone carbonyl of sesquiterpenoids in IR spectrum found in S. latifolia, S. controversa, S. daurica, S. amara and S. salicifolia. HPLC / UV analysis showed that peaks with absorption maxima of 242-246 nm due to the presence of α,β-unsaturated ketone group in the structure of ecdysteroids were found in S. salicifolia, S. controversa, S. daurica and S. latifolia.

Rapid and on-site analysis of illegal drugs on the nano-microscale using a deep ultraviolet-visible reflected optical fiber sensor.

PubMed

Li, Qiang; Qiu, Tian; Hao, Hongxia; Zhou, Hong; Wang, Tongzhou; Zhang, Ye; Li, Xin; Huang, Guoliang; Cheng, Jing

2012-04-07

A deep ultraviolet-visible (DUV-Vis) reflected optical fiber sensor was developed for use in a simple spectrophotometric detection system to detect the absorption of various illegal drugs at wavelengths between 180 and 800 nm. Quantitative analyses performed using the sensor revealed a high specificity and sensitivity for drug detection at a wavelength of approximately 200 nm. Using a double-absorption optical path length, extremely small sample volumes were used (32 to 160 nL), which allowed the use of minimal amounts of samples. A portable spectrophotometric system was established based on our optical fiber sensor for the on-site determination and quantitative analysis of common illegal drugs, such as 3,4-methylenedioxymethamphetamine (MDMA), ketamine hydrochloride, cocaine hydrochloride, diazepam, phenobarbital, and barbital. By analyzing the absorbance spectra, six different drugs were quantified at concentrations that ranged from 0.1 to 1000 μg mL(-1) (16 pg-0.16 μg). A novel Matching Algorithm of Spectra Space (MASS) was used to accurately distinguish between each drug in a mixture. As an important supplement to traditional methods, such as mass spectrometry or chromatography, our optical fiber sensor offers rapid and low-cost on-site detection using trace amounts of sample. This rapid and accurate analytical method has wide-ranging applications in forensic science, law enforcement, and medicine.

Laser-Excited Atomic Fluorescence and Ionization in a Graphite Furnace for the Determination of Metals and Nonmetals

NASA Astrophysics Data System (ADS)

Butcher, David James

1990-01-01

Here is reported novel instrumentation for atomic spectrometry that combined the use of a pulsed laser system as the light source and an electrothermal atomizer as the atom cell. The main goal of the research was to develop instrumentation that was more sensitive for elemental analysis than commercially available instruments and could be used to determine elements in real sample matrices. Laser excited atomic fluorescence spectrometry (LEAFS) in an electrothermal atomizer (ETA) was compared to ETA atomic absorption spectrometry (AAS) for the determination of thallium, manganese, and lead in food and agricultural standard reference materials (SRMs). Compared to ETA AAS, ETA LEAFS has a longer linear dynamic range (LDR) (5-7 orders of magnitude compared to 2-3 orders of magnitude) and higher sensitivity (10 ^{-16} to 10^{ -14} g as compared to 10^{ -13} to 10^{-11} g). Consequently, ETA LEAFS allows elemental analysis to be done over a wider range of concentrations with less dilution steps. Thallium was accurately determined in biological samples by ETA LEAFS at amounts five to one hundred times below the ETA AAS detection limit. ETA AAS and ETA LEAFS were compared for the determination of lead and manganese, and in general, the accuracies and precisions of ETA AAS were the same, with typical precisions between 3% and 6%. Fluorine was determined using laser excited molecular fluorescence spectrometry (LEMOFS) in an ETA. Molecular fluorescence from magnesium fluoride was collected, and the detection limit of 0.3 pg fluorine was two to six orders of magnitude more sensitive than other methods commonly used for the determination of fluorine. Significant interferences from ions were observed, but the sensitivity was high enough that fluorine could be determined in freeze dried urine SRMs by diluting the samples by a factor of one hundred to remove the interferences. Laser enhanced ionization (LEI) in an ETA was used for the determination of metals. For thallium, indium, and lithium, detection limits between 0.7 and 2 pg were obtained, with an LDR of 3.5 orders of magnitude. Sodium was shown to severely depress the indium LEI signal in an ETA.

Structural evaluation of reduced graphene oxide in graphene oxide during ion irradiation: X-ray absorption spectroscopy and in-situ sheet resistance studies

NASA Astrophysics Data System (ADS)

Saravanan, K.; Jayalakshmi, G.; Suresh, K.; Sundaravel, B.; Panigrahi, B. K.; Phase, D. M.

2018-03-01

We report the structural evolution of reduced graphene oxide (rGO) in graphene oxide (GO) flakes during 1 MeV Si+ ion irradiation. In-situ electrical resistivity measurements facilitate monitoring the sheet resistance with the increase in the fluence. The electrical sheet resistance of the GO flake shows the exponential decay behaviour with the increasing ion fluence. Raman spectra of the GO flake reveal the increase in the ID/IG ratio, indicating restoration of the sp2 network upon irradiation. The C/O ratio estimated from resonant Rutherford backscattering spectrometry analysis directly evidenced the reduction of oxygen moieties upon irradiation. C K-edge X-ray absorption near edge structure spectra reveal the restoration of C=C sp2-hybridized carbon atoms and the removal of oxygen-containing functional groups in the GO flake. STM data reveal the higher conductance in the rGO regime in comparison with the regime, where the oxygen functional groups are present. The experimental investigation demonstrates that the ion irradiation can be employed for efficient reduction of GO with tunable electrical and structural properties.

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.

PubMed

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).

Design and reactivity of Ni-complexes using pentadentate neutral-polypyridyl ligands: Possible mimics of NiSOD.

PubMed

Snider, Victoria G; Farquhar, Erik R; Allen, Mark; Abu-Spetani, Ayah; Mukherjee, Anusree

2017-10-01

Superoxide plays a key role in cell signaling, but can be cytotoxic within cells unless well regulated by enzymes known as superoxide dismutases (SOD). Nickel superoxide dismutase (NiSOD) catalyzes the disproportion of the harmful superoxide radical into hydrogen peroxide and dioxygen. NiSOD has a unique active site structure that plays an important role in tuning the potential of the nickel center to function as an effective catalyst for superoxide dismutation with diffusion controlled rates. The synthesis of structural and functional analogues of NiSOD provides a route to better understand the role of the nickel active site in superoxide dismutation. In this work, the synthesis of a series of nickel complexes supported by nitrogen rich pentadentate ligands is reported. The complexes have been characterized through absorption spectroscopy, mass spectrometry, and elemental analysis. X-ray absorption spectroscopy was employed to establish the oxidation state and the coordination geometry around the metal center. The reactivity of these complexes toward KO 2 was evaluated to elucidate the role of the coordination sphere in controlling superoxide dismutation reactivity. Copyright © 2017 Elsevier Inc. All rights reserved.

Quantitative IR microscopy and spectromics open the way to 3D digital pathology.

PubMed

Bobroff, Vladimir; Chen, Hsiang-Hsin; Delugin, Maylis; Javerzat, Sophie; Petibois, Cyril

2017-04-01

Currently, only mass-spectrometry (MS) microscopy brings a quantitative analysis of chemical contents of tissue samples in 3D. Here, the reconstruction of a 3D quantitative chemical images of a biological tissue by FTIR spectro-microscopy is reported. An automated curve-fitting method is developed to extract all intense absorption bands constituting IR spectra. This innovation benefits from three critical features: (1) the correction of raw IR spectra to make them quantitatively comparable; (2) the automated and iterative data treatment allowing to transfer the IR-absorption spectrum into a IR-band spectrum; (3) the reconstruction of an 3D IR-band matrix (x, y, z for voxel position and a 4 th dimension with all IR-band parameters). Spectromics, which is a new method for exploiting spectral data for tissue metadata reconstruction, is proposed to further translate the related chemical information in 3D, as biochemical and anatomical tissue parameters. An example is given with oxidative stress distribution and the reconstruction of blood vessels in tissues. The requirements of IR microscopy instrumentation to propose 3D digital histology as a clinical routine technology is briefly discussed. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Hydrogen concentration analysis in clinopyroxene using proton-proton scattering analysis

NASA Astrophysics Data System (ADS)

Weis, Franz A.; Ros, Linus; Reichart, Patrick; Skogby, Henrik; Kristiansson, Per; Dollinger, Günther

2018-02-01

Traditional methods to measure water in nominally anhydrous minerals (NAMs) are, for example, Fourier transformed infrared (FTIR) spectroscopy or secondary ion mass spectrometry (SIMS). Both well-established methods provide a low detection limit as well as high spatial resolution yet may require elaborate sample orientation or destructive sample preparation. Here we analyze the water content in erupted volcanic clinopyroxene phenocrysts by proton-proton scattering and reproduce water contents measured by FTIR spectroscopy. We show that this technique provides significant advantages over other methods as it can provide a three-dimensional distribution of hydrogen within a crystal, making the identification of potential inclusions possible as well as elimination of surface contamination. The sample analysis is also independent of crystal structure and orientation and independent of matrix effects other than sample density. The results are used to validate the accuracy of wavenumber-dependent vs. mineral-specific molar absorption coefficients in FTIR spectroscopy. In addition, we present a new method for the sample preparation of very thin crystals suitable for proton-proton scattering analysis using relatively low accelerator potentials.

Recent Developments in the Speciation and Determination of Mercury Using Various Analytical Techniques

PubMed Central

Suvarapu, Lakshmi Narayana; Baek, Sung-Ok

2015-01-01

This paper reviews the speciation and determination of mercury by various analytical techniques such as atomic absorption spectrometry, voltammetry, inductively coupled plasma techniques, spectrophotometry, spectrofluorometry, high performance liquid chromatography, and gas chromatography. Approximately 126 research papers on the speciation and determination of mercury by various analytical techniques published in international journals since 2013 are reviewed. PMID:26236539

Determination of mercury distribution inside spent compact fluorescent lamps by atomic absorption spectrometry.

PubMed

Rey-Raap, Natalia; Gallardo, Antonio

2012-05-01

In this study, spent compact fluorescent lamps were characterized to determine the distribution of mercury. The procedure used in this research allowed mercury to be extracted in the vapor phase, from the phosphor powder, and the glass matrix. Mercury concentration in the three phases was determined by the method known as cold vapor atomic absorption spectrometry. Median values obtained in the study showed that a compact fluorescent lamp contained 24.52±0.4ppb of mercury in the vapor phase, 204.16±8.9ppb of mercury in the phosphor powder, and 18.74±0.5ppb of mercury in the glass matrix. There are differences in mercury concentration between the lamps since the year of manufacture or the hours of operation affect both mercury content and its distribution. The 85.76% of the mercury introduced into a compact fluorescent lamp becomes a component of the phosphor powder, while more than 13.66% is diffused through the glass matrix. By washing and eliminating all phosphor powder attached to the glass surface it is possible to classified the glass as a non-hazardous waste. Copyright © 2011 Elsevier Ltd. All rights reserved.

Determination of Hg(II) in waters by on-line preconcentration using Cyanex 923 as a sorbent — Cold vapor atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Duan, Taicheng; Song, Xuejie; Xu, Jingwei; Guo, Pengran; Chen, Hangting; Li, Hongfei

2006-09-01

Using a solid phase extraction mini-column home-made from a neutral extractant Cyanex 923, inorganic Hg could be on-line preconcentrated and simultaneously separated from methyl mercury. The preconcentrated Hg (II) was then eluted with 10% HNO 3 and subsequently reduced by NaBH 4 to form Hg vapor before determination by cold vapor atomic absorption spectrometry (CVAAS). Optimal conditions for and interferences on the Hg preconcentration and measurement were at 1% HCl, for a 25 mL sample uptake volume and a 10 mL min - 1 sample loading rate. The detection limit was 0.2 ng L - 1 and much lower than that of conventional method (around 15.8 ng L - 1 ). The relative standard deviation (RSD) is 1.8% for measurements of 40 ng L - 1 of Hg and the linear working curve is from 20 to 2000 ng L - 1 (with a correlation coefficient of 0.9996). The method was applied in determination of inorganic Hg in city lake and deep well water (from Changchun, Jilin, China), and recovery test results for both samples were satisfactory.

Dispersive liquid-liquid microextraction based on solidification of floating organic drop for preconcentration and determination of trace amounts of copper by flame atomic absorption spectrometry.

PubMed

Karadaş, Cennet; Kara, Derya

2017-04-01

A novel, simple, rapid, sensitive, inexpensive and environmentally friendly dispersive liquid-liquid microextraction method based on the solidification of a floating organic drop (DLLME-SFO) was developed for the determination of copper by flame atomic absorption spectrometry (FAAS). N-o-Vanillidine-2-amino-p-cresol was used as a chelating ligand and 1-undecanol was selected as an extraction solvent. The main parameters affecting the performance of DLLME-SFO, such as sample pH, volume of extraction solvent, extraction time, concentration of the chelating ligand, salt effect, centrifugation time and sample volume were investigated and optimized. The effect of interfering ions on the recovery of copper was also examined. Under the optimum conditions, the detection limit (3σ) was 0.93μgL -1 for Cu using a sample volume of 20mL, yielding a preconcentration factor of 20. The proposed method was successfully applied to the determination of Cu in tap, river and seawater, rice flour and black tea samples as well as certified reference materials. Copyright © 2016. Published by Elsevier Ltd.

Sequential injection ionic liquid dispersive liquid-liquid microextraction for thallium preconcentration and determination with flame atomic absorption spectrometry.

PubMed

Anthemidis, Aristidis N; Ioannou, Kallirroy-Ioanna G

2012-08-01

A novel, automatic on-line sequential injection dispersive liquid-liquid microextraction (SI-DLLME) method, based on 1-hexyl-3-methylimidazolium hexafluorophosphate ([Hmim][PF(6)]) ionic liquid as an extractant solvent was developed and demonstrated for trace thallium determination by flame atomic absorption spectrometry. The ionic liquid was on-line fully dispersed into the aqueous solution in a continuous flow format while the TlBr(4)(-) complex was easily migrated into the fine droplets of the extractant due to the huge contact area of them with the aqueous phase. Furthermore, the extractant was simply retained onto the surface of polyurethane foam packed into a microcolumn. No specific conditions like low temperature are required for extractant isolation. All analytical parameters of the proposed method were investigated and optimized. For 15 mL of sample solution, an enhancement factor of 290, a detection limit of 0.86 μg L(-1) and a precision (RSD) of 2.7% at 20.0 μg L(-1) Tl(I) concentration level, was obtained. The developed method was evaluated by analyzing certified reference materials while good recoveries from environmental and biological samples proved that present method was competitive in practical applications.

Acid effects on the measurement of mercury by cold vapor atomic absorption spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Adeloju, S.B.; Mann, T.F.

1987-07-01

The influence of nitric, hydrochloric and sulfuric acids on the measurement of mercury by cold vapor atomic absorption spectrometry has been investigated. Small pre-reduction peaks associated with the instability of mercury were observed in solutions containing less than or equal to 12.5, < 2 and less than or equal to 12.5% v/v of each acid, respectively. Mercury was found to be most stable in greater than or equal to 2% v/v hydrochloric acid and the measured absorbance was not greatly influenced by varying concentration of the acid. The mercury absorbance measurements were more sensitive in solutions containing less than ormore » equal to 6.3% v/v hydrochloric acid than in similar concentrations of nitric and sulfuric acids. The use of the three acids as a digestion mixture result in serious interference from nitrogen oxides. The interference was removed by use of expelling agents such as urea and sulfamic acid or overcome by use of excess stannous chloride, prior to the reduction of mercury(II) ions. The determination of mercury in NBS albacore tuna using both of these approaches to overcome the interference problem proved to be successful.« less

Determination of ultra-trace aluminum in human albumin by cloud point extraction and graphite furnace atomic absorption spectrometry.

PubMed

Sun, Mei; Wu, Qianghua

2010-04-15

A cloud point extraction (CPE) method for the preconcentration of ultra-trace aluminum in human albumin prior to its determination by graphite furnace atomic absorption spectrometry (GFAAS) had been developed in this paper. The CPE method was based on the complex of Al(III) with 1-(2-pyridylazo)-2-naphthol (PAN) and Triton X-114 was used as non-ionic surfactant. The main factors affecting cloud point extraction efficiency, such as pH of solution, concentration and kind of complexing agent, concentration of non-ionic surfactant, equilibration temperature and time, were investigated in detail. An enrichment factor of 34.8 was obtained for the preconcentration of Al(III) with 10 mL solution. Under the optimal conditions, the detection limit of Al(III) was 0.06 ng mL(-1). The relative standard deviation (n=7) of sample was 3.6%, values of recovery of aluminum were changed from 92.3% to 94.7% for three samples. This method is simple, accurate, sensitive and can be applied to the determination of ultra-trace aluminum in human albumin. 2009 Elsevier B.V. All rights reserved.

Blue emitting undecaplatinum clusters

NASA Astrophysics Data System (ADS)

Chakraborty, Indranath; Bhuin, Radha Gobinda; Bhat, Shridevi; Pradeep, T.

2014-07-01

A blue luminescent 11-atom platinum cluster showing step-like optical features and the absence of plasmon absorption was synthesized. The cluster was purified using high performance liquid chromatography (HPLC). Electrospray ionization (ESI) and matrix assisted laser desorption ionization (MALDI) mass spectrometry (MS) suggest a composition, Pt11(BBS)8, which was confirmed by a range of other experimental tools. The cluster is highly stable and compatible with many organic solvents.A blue luminescent 11-atom platinum cluster showing step-like optical features and the absence of plasmon absorption was synthesized. The cluster was purified using high performance liquid chromatography (HPLC). Electrospray ionization (ESI) and matrix assisted laser desorption ionization (MALDI) mass spectrometry (MS) suggest a composition, Pt11(BBS)8, which was confirmed by a range of other experimental tools. The cluster is highly stable and compatible with many organic solvents. Electronic supplementary information (ESI) available: Details of experimental procedures, instrumentation, chromatogram of the crude cluster; SEM/EDAX, DLS, PXRD, TEM, FT-IR, and XPS of the isolated Pt11 cluster; UV/Vis, MALDI MS and SEM/EDAX of isolated 2 and 3; and 195Pt NMR of the K2PtCl6 standard. See DOI: 10.1039/c4nr02778g

Direct extraction of lead (II) from untreated human blood serum using restricted access carbon nanotubes and its determination by atomic absorption spectrometry.

PubMed

Barbosa, Valéria Maria Pereira; Barbosa, Adriano Francisco; Bettini, Jefferson; Luccas, Pedro Orival; Figueiredo, Eduardo Costa

2016-01-15

Oxidized carbon nanotubes were covered with layers of bovine serum albumin to result in so-called restricted-access carbon nanotubes (RACNTs). This material can extract Pb(2+) ions directly from untreated human blood serum while excluding all the serum proteins. The RACNTs have a protein exclusion capacity of almost 100% and a maximum Pb(2+) adsorption capacity of 34.5mg g(-1). High resolution transmission electron microscopy, scanning transmission electron microscopy and energy dispersive spectroscopy were used to confirm the BSA layer and Pb(2+) adsorption sites. A mini-column filled with RACNTs was used in an on-line solid phase extraction system coupled to a thermospray flame furnace atomic absorption spectrometry. At optimized experimental conditions, the method has a detection limit as low as 2.1µg L(-1), an enrichment factor of 5.5, and inter- and intra-day precisions (expressed as relative standard deviation) of <8.1%. Recoveries of the Pb(2+) spiked samples ranged from 89.4% to 107.3% for the extraction from untreated human blood serum. Copyright © 2015 Elsevier B.V. All rights reserved.

Synthesis, characterization and application of a new chelating resin for solid phase extraction, preconcentration and determination of trace metals in some dairy samples by flame atomic absorption spectrometry.

PubMed

Daşbaşı, Teslima; Saçmacı, Şerife; Çankaya, Nevin; Soykan, Cengiz

2016-11-15

In this study, a simple and rapid solid phase extraction/preconcentration procedure was developed for determination of Cd(II), Co(II), Cr(III), Cu(II), Fe(III), Mn(II), Pb(II), and Zn(II) trace metals by flame atomic absorption spectrometry (FAAS). A new chelating resin, poly(N-cyclohexylacrylamide-co-divinylbenzene-co-2-acrylamido-2-methyl-1-propanesulfonic acid) (NCA-co-DVB-co-AMPS) (hereafter CDAP) was synthesized and characterized. The influences of the analytical parameters such as pH of the sample solution, type and concentration of eluent, flow rates of the sample and eluent, volume of the sample and eluent, amount of chelating resin, and interference of ions were examined. The limit of detection (LOD) of analytes were found (3s) to be in the range of 0.65-1.90μgL(-1). Preconcentration factor (PF) of 200 and the relative standard deviation (RSD) of ⩽2% were achieved (n=11). The developed method was applied for determination of analytes in some dairy samples and certified reference materials. Copyright © 2016 Elsevier Ltd. All rights reserved.

The role of atomic absorption spectrometry in geochemical exploration

USGS Publications Warehouse

Viets, J.G.; O'Leary, R. M.

1992-01-01

In this paper we briefly describe the principles of atomic absorption spectrometry (AAS) and the basic hardware components necessary to make measurements of analyte concentrations. Then we discuss a variety of methods that have been developed for the introduction of analyte atoms into the light path of the spectrophotometer. This section deals with sample digestion, elimination of interferences, and optimum production of ground-state atoms, all critical considerations when choosing an AAS method. Other critical considerations are cost, speed, simplicity, precision, and applicability of the method to the wide range of materials sampled in geochemical exploration. We cannot attempt to review all of the AAS methods developed for geological materials but instead will restrict our discussion to some of those appropriate for geochemical exploration. Our background and familiarity are reflected in the methods we discuss, and we have no doubt overlooked many good methods. Our discussion should therefore be considered a starting point in finding the right method for the problem, rather than the end of the search. Finally, we discuss the future of AAS relative to other instrumental techniques and the promising new directions for AAS in geochemical exploration. ?? 1992.

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

PubMed

Leal, L O; Elsholz, O; Forteza, R; Cerdà, V

2006-07-28

A new software-controlled time-based multisyringe flow injection system for mercury determination by cold-vapor atomic absorption spectrometry is proposed. Precise known volumes of sample, reducing agent (1.1% SnCl2 in 3% HCl) and carrier (3% HCl) are dispensed into a gas-liquid separation cell with a multisyringe burette coupled with one three-way solenoid valve. An argon flow delivers the reduced mercury to the spectrometer. The optimization of the system was carried out testing reaction coils and gas-liquid separators of different design as well as changing parameters, such as sample and reagents volumes, reagent concentrations and carrier gas flow rate, among others. The analytical curves were obtained within the range 50-5000 ng L(-1). The detection limit (3sigma(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.

Synthesis and application of a nanoporous ion-imprinted polymer for the separation and preconcentration of trace amounts of vanadium from food samples before determination by electrothermal atomic absorption spectrometry.

PubMed

Dadfarnia, Shayessteh; Haji Shabani, Ali Mohammad; Dehghanpoor Frashah, Shahab

2016-04-01

A vanadium ion-imprinted polymer was synthesized in the presence of V(V) and N-benzoyl-N-phenyl hydroxyl amine using 4-vinyl pyridine as the monomer, ethylene glycol dimethacrylate as the cross linker and 2,2'-azobis(isobutyronitrile) as the initiator. The imprinted V(V) ions were completely removed by leaching the polymer with 5 mol/L nitric acid, and the polymer structure was characterized by Fourier transform infrared spectroscopy and scanning electron microscopy. The ion-imprinted polymer was used as the sorbent in the development of the solid-phase extraction method for V(V) prior to its determination by electrothermal atomic absorption spectrometry. The maximum sorption capacity for V(V) ions was 26.7 mg/g at pH 4.0. Under the optimum conditions, for a sample volume of 150.0 mL, an enrichment factor of 289.0 and a detection limit of 6.4 ng/L were obtained. The developed method was successfully applied to the determination of vanadium in parsley, zucchini, black tea, rice, and water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of Ultra-trace Rhodium in Water Samples by Graphite Furnace Atomic Absorption Spectrometry after Cloud Point Extraction Using 2-(5-Iodo-2-Pyridylazo)-5-Dimethylaminoaniline as a Chelating Agent.

PubMed

Han, Quan; Huo, Yanyan; Wu, Jiangyan; He, Yaping; Yang, Xiaohui; Yang, Longhu

2017-03-24

A highly sensitive method based on cloud point extraction (CPE) separation/preconcentration and graphite furnace atomic absorption spectrometry (GFAAS) detection has been developed for the determination of ultra-trace amounts of rhodium in water samples. A new reagent, 2-(5-iodo-2-pyridylazo)-5-dimethylaminoaniline (5-I-PADMA), was used as the chelating agent and the nonionic surfactant TritonX-114 was chosen as extractant. In a HAc-NaAc buffer solution at pH 5.5, Rh(III) reacts with 5-I-PADMA to form a stable chelate by heating in a boiling water bath for 10 min. Subsequently, the chelate is extracted into the surfactant phase and separated from bulk water. The factors affecting CPE were investigated. Under the optimized conditions, the calibration graph was linear in the range of 0.1-6.0 ng/mL, the detection limit was 0.023 ng/mL for rhodium and relative standard deviation was 3.67% ( c = 1.0 ng/mL, n = 11)．The method has been applied to the determination of trace rhodium in water samples with satisfactory results.

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

PubMed

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.

Separation/preconcentration and determination of vanadium with dispersive liquid-liquid microextraction based on solidification of floating organic drop (DLLME-SFO) and electrothermal atomic absorption spectrometry.

PubMed

Asadollahi, Tahereh; Dadfarnia, Shayessteh; Shabani, Ali Mohammad Haji

2010-06-30

A novel dispersive liquid-liquid microextraction based on solidification of floating organic drop (DLLME-SFO) for separation/preconcentration of ultra trace amount of vanadium and its determination with the electrothermal atomic absorption spectrometry (ETAAS) was developed. The DLLME-SFO behavior of vanadium (V) using N-benzoyl-N-phenylhydroxylamine (BPHA) as complexing agent was systematically investigated. The factors influencing the complex formation and extraction by DLLME-SFO method were optimized. Under the optimized conditions: 100 microL, 200 microL and 25 mL of extraction solvent (1-undecanol), disperser solvent (acetone) and sample volume, respectively, an enrichment factor of 184, a detection limit (based on 3S(b)/m) of 7 ng L(-1) and a relative standard deviation of 4.6% (at 500 ng L(-1)) were obtained. The calibration graph using the preconcentration system for vanadium was linear from 20 to 1000 ng L(-1) with a correlation coefficient of 0.9996. The method was successfully applied for the determination of vanadium in water and parsley. Copyright 2010 Elsevier B.V. All rights reserved.

Transport of hop aroma compounds across Caco-2 monolayers.

PubMed

Heinlein, A; Metzger, M; Walles, H; Buettner, A

2014-11-01

Although being reported and used as a sedative remedy for several years, the bioactive principle of hop preparations is still not decisively clarified. Understanding absorption and transformation processes of potential physiologically active constituents is essential to evaluate the likeliness of biological effects on humans. Therefore, single hop aroma compounds as well as digestive transformation products thereof have been investigated in view of their human intestinal absorption, applying Caco-2 transport experiments as well as investigations on potential biotransformation processes. Selective and sensitive identification and quantification were thereby achieved by application of two-dimensional high resolution gas chromatography-mass spectrometry in conjunction with stable isotope dilution analysis, leading to the determination of apparent permeability values by different mathematical approaches considering sink and non-sink conditions. Overall, calculated permeability values ranged from 2.6 × 10(-6) to 1.8 × 10(-4) cm s(-1) with all mathematical approaches, indicating high absorption potential and almost complete bioavailability for all tested compounds with hydroxyl-functionalities. Considering this high permeability together with the high lipophilicity of these substances, a passive transcellular uptake route can be speculated. Investigated sesquiterpenes and β-myrcene showed flat absorption profiles while the investigated esters showed decreasing profiles. In view of the lipophilic and volatile nature of the investigated substances, special attention was paid to recovery and mass balance determination. Furthermore, in the course of the transport experiments of 1-octen-3-ol and 3-methyl-2-buten-1-ol, additional biotransformation products were observed, namely 3-octanone and 3-methyl-2-butenal, respectively. The absence of these additional substances in control experiments strongly indicates an intestinal first-pass metabolism of the α,β-unsaturated alcohols 1-octen-3-ol and 3-methyl-2-buten-1-ol in Caco-2 cells.

Direct detection of saponins in crude extracts of soapnuts by FTIR.

PubMed

Almutairi, Meshari Saad; Ali, Muhammad

2015-01-01

Direct detection of saponins in soapnuts (Sapindus mukorossi) using Fourier transform infrared (FTIR) spectroscopy is investigated in this project. Potassium bromide powder was mixed with extracted powder of soapnuts and compressed to a thin pellet for examination process. The outcome of the FTIR spectra of saponin demonstrated characteristic triterpenoid saponin absorptions of OH, C = O, C-H, and C = C, while the glycoside linkages to the sapogenins were indicated by the absorptions of C-O. The significance of this study is that saponin absorption peaks are directly detectable in crude aqueous and 95% ethanol extracts of soapnuts powder using FTIR spectroscopy, thereby eliminating the need of further expensive and exhaustive purification steps. The extracts of soapnuts were screened for saponins along with controls by phytochemical tests, and advanced spectroscopic techniques such as ultra fast liquid chromatography and ultra performance liquid chromatography quadrupole-time of flight-mass spectrometry were also implemented to validate the saponins.

Risk assessment of dissolved trace metals in drinking water of Karachi, Pakistan.

PubMed

Karim, Zahida

2011-06-01

Health risk caused by the exposure to trace metals in water through different exposure pathways was investigated. Graphite furnace atomic absorption spectrometry was used for the determination of trace metals (nickel, copper, chromium, lead, cobalt, manganese and iron) in drinking water samples. The concentration of metals was compared with the world health organization (WHO) drinking water quality guideline values. Risk of metals on human health was evaluated using Hazard Quotient (HQ). Hazard quotients of all metals through oral ingestion and dermal absorption are found in the range of 1.11 × 10⁻² to 1.35 × 10⁻¹ and 8.52 × 10⁻⁵ to 9.75 × 10⁻², respectively. The results of the present study reflect the unlikely potential for adverse health effects to the inhabitants of Karachi due to the oral ingestion and dermal absorption of water containing these metals.

The study of trace metal absoption using stable isotopes and mass spectrometry

NASA Astrophysics Data System (ADS)

Fennessey, P. V.; Lloyd-Kindstrand, L.; Hambidge, K. M.

1991-12-01

The absorption and excretion of zinc stable isotopes have been followed in more than 120 human subjects. The isotope enrichment determinations were made using a standard VG 7070E HF mass spectrometer. A fast atom gun (FAB) was used to form the ions from a dry residue on a pure silver probe tip. Isotope ratio measurements were found to have a precision of better than 2% (relative standard deviation) and required a sample size of 1-5 [mu]g. The average true absorption of zinc was found to be 73 ± 12% (2[sigma]) when the metal was taken in a fasting state. This absorption figure was corrected for tracer that had been absorbed and secreted into the gastrointestinal (GI) tract over the time course of the study. The average time for a majority of the stable isotope tracer to pass through the GI tract was 4.7 ± 1.9 (2[sigma]) days.

Optical absorption, electron spin resonance, and electron spin echo studies of the photoionization of tetramethylbenzidine in cationic and anionic synthetic vesicles: comparison with analogous micellar systems

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, A.S.W.; Kevan, L.

1983-09-07

The photoionization of N,N,N',N'-tetramethylbenzidine (TMB) in dihexadecylphosphate anionic vesicles and in dioctadecyldimethylammonium chloride cationic vesicles has been studied by optical absorption and electron spin resonance in liquid and frozen solutions. The TMB cation has been observed to be stabilized in both types of vesicles. The photoionization efficiency is about twofold greater in the cationic vesicles compared to the anionic vesicles. Shifts in the optical absorption maximum between micellar and vesicle solutions indicate that TMB is in a less polar environment in the vesicle systems. Electron spin echo modulation spectrometry has been used to detect TMB cation-water interactions that are foundmore » to be weaker than in previously studied micellar solutions. This is consistent with the optical absorption results and with an asymmetric solubilization site for TMB and TMB/sup +/ within the vesicular structure. A new absorption in the photoionized vesicles is assigned to a nonparamagnetic diamine-diimine charge-transfer complex between two TMB cations in the same vesicle. This complex is not formed in micellar systems. 5 figures.« less

The quantitative analysis of OH in vesuvianite: a polarized FTIR and SIMS study

NASA Astrophysics Data System (ADS)

Bellatreccia, Fabio; della Ventura, Giancarlo; Ottolini, Luisa; Libowitzky, Eugen; Beran, Anton

2005-05-01

A well-characterized suite of vesuvianite samples from the volcanic ejecta (skarn or syenites) from Latium (Italy) was studied by single-crystal, polarized radiation, Fourier-transform infrared (FTIR) spectroscopy and secondary-ion mass-spectrometry (SIMS). OH-stretching FTIR spectra consist of a rather well-defined triplet of broad bands at higher-frequency (3,700 3,300 cm-1) and a very broad composite absorption below 3,300 cm-1. Measurements with E//c or E⊥c show that all bands are strongly polarized with maximum absorption for E//c. They are in agreement with previous band assignments (Groat et al. Can Mineral 33:609, 1995) to the two O(11) H(1) and O(10) H(2) groups in the structure. Pleochroic measurements with changing direction of the E vector of the incident radiation show that the orientation of the O(11) H(1) dipole is OH∧c~35°, in excellent agreement with the neutron data of Lager et al. (Can Mineral 37:763, 1999). A SIMS-based calibration curve at ~10% rel. accuracy has been worked out and used as reference for the quantitative analysis of H2O in vesuvianite by FTIR. Based on previous SIMS results for silicate minerals (Ottolini and Hawthorne in J Anal At Spectrom 16:1266, 2001; Ottolini et al. in Am Mineral 87:1477, 2002) the SiO2 and FeO content of the matrix were assumed as the major factors to be considered at a first approximation in the selection of the standards for H. The lack of vesuvianite standards for quantitative SIMS analysis of H2O has been here overcome by selecting low-silica elbaite crystals (Ottolini et al. in Am Mineral 87:1477, 2002). The resulting integrated molar absorption FTIR coefficient for vesuvianite is ɛi=100.000±2.000 l mol-1 cm-2. SIMS data for Li, B, F, Sr, Y, Be, Ba REE, U and Th are also provided in the paper.

Soluble Corn Fiber Increases Calcium Absorption Associated with Shifts in the Gut Microbiome: A Randomized Dose-Response Trial in Free-Living Pubertal Females.

PubMed

Whisner, Corrie M; Martin, Berdine R; Nakatsu, Cindy H; Story, Jon A; MacDonald-Clarke, Claire J; McCabe, Linda D; McCabe, George P; Weaver, Connie M

2016-07-01

Soluble corn fiber (SCF; 12 g fiber/d) is shown to increase calcium absorption efficiency, associated with shifts in the gut microbiota in adolescent males and females who participated in a controlled feeding study. We evaluated the dose response of 0, 10, and 20 g fiber/d delivered by PROMITOR SCF 85 (85% fiber) on calcium absorption, biochemical bone properties, and the fecal microbiome in free-living adolescents. Healthy adolescent females (n = 28; aged 11-14 y) randomly assigned into a 3-phase, double-blind, crossover study consumed SCF for 4 wk at each dose (0, 10, and 20 g fiber/d from SCF) alongside their habitual diet and were followed by 3-d clinical visits and 3-wk washout periods. Stable isotope ((44)Ca and (43)Ca) enrichment in pooled urine was measured by inductively coupled plasma mass spectrometry. Fecal microbial community composition was assessed by high-throughput sequencing (Illumina) of polymerase chain reaction-amplified 16S rRNA genes. Mixed model ANOVA and Friedman analysis were used to determine effects of SCF on calcium absorption and to compare mean microbial proportions, respectively. Calcium absorption increased significantly with 10 (13.3% ± 5.3%; P = 0.042) and 20 g fiber/d (12.9% ± 3.6%; P = 0.026) from SCF relative to control. Significant differences in fecal microbial community diversity were found after consuming SCF (operational taxonomic unit measures of 601.4 ± 83.5, 634.5 ± 83.8, and 649.6 ± 75.5 for 0, 10, and 20 g fiber/d, respectively; P < 0.05). Proportions of the genus Parabacteroides significantly increased with SCF dose (1.1% ± 0.8%, 2.1% ± 1.6%, and 3.0% ± 2.0% for 0, 10, and 20 g fiber/d from SCF, respectively; P < 0.05). Increases in calcium absorption positively correlated with increases in Clostridium (r = 0.44, P = 0.023) and unclassified Clostridiaceae (r = 0.40, P = 0.040). SCF, a nondigestible carbohydrate, increased calcium absorption in free-living adolescent females. Two groups of bacteria may be involved, one directly fermenting SCF and the second fermenting SCF metabolites further, thereby promoting increased calcium absorption. This trial was registered at clinicaltrials.gov as NCT01660503. © 2016 American Society for Nutrition.

Questa baseline and pre-mining ground-water quality investigation. 2. Low-flow (2001) and snowmelt (2002) synoptic/tracer water chemistry for the Red River, New Mexico

USGS Publications Warehouse

McCleskey, R. Blaine; Nordstrom, D. Kirk; Steiger, Judy I.; Kimball, Briant A.; Verplanck, Philip L.

2003-01-01

Water analyses are reported for 259 samples collected from the Red River, New Mexico, and its tributaries during low-flow(2001) and spring snowmelt (2002) tracer studies. Water samples were collected along a 20-kilometer reach of the Red River beginning just east of the town of Red River and ending at the U.S. Geological Survey streamflow-gaging station located east of Questa, New Mexico. The study area was divided into three sections where separate injections and synoptic sampling events were performed during the low-flow tracer study. During the spring snowmelt tracer study, three tracer injections and synoptic sampling events were performed bracketing the areas with the greatest metal loading into the Red River as determined from the low-flow tracer study. The lowflow tracer synoptic sampling events were August 17, 20, and 24, 2001. The synoptic sampling events for the spring snowmelt tracer were March 30, 31, and April 1, 2002. Stream and large inflow water samples were sampled using equal-width and depth-integrated sampling methods and composited into half-gallon bottles. Grab water samples were collected from smaller inflows. Stream temperatures were measured at the time of sample collection. Samples were transported to a nearby central processing location where pH and specific conductance were measured and the samples processed for chemical analyses. Cations, trace metals, iron redox species, and fluoride were analyzed at the U.S. Geological Survey laboratory in Boulder, Colorado. Cations and trace metal concentrations were determined using inductively coupled plasma-optical emission spectrometry and graphite furnace atomic absorption spectrometry. Arsenic concentrations were determined using hydride generation atomic absorption spectrometry, iron redox species were measured using ultraviolet-visible spectrometry, and fluoride concentrations were determined using an ion-selective electrode. Alkalinity was measured by automated titration, and sulfate, chloride, and bromide were analyzed by ion chromatography at the U.S. Geological Survey laboratory in Salt Lake City, Utah.

Concentration and distribution of sixty-one elements in coals from DPR Korea

USGS Publications Warehouse

Hu, Jiawen; Zheng, B.; Finkelman, R.B.; Wang, B.; Wang, M.; Li, S.; Wu, D.

2006-01-01

Fifty coal samples (28 anthracite and 22 lignites) were collected from both main and small coal mines in DPR Korea prioritized by resource distribution and coal production. The concentrations of 61 elements in 50 coal samples were determined by several multielement and element-specific techniques, including inductively coupled plasma atomic emission spectrometry (ICP-AES), and inductively coupled plasma mass spectrometry (ICP-MS), ion chromatogram (IC), cold-vapor atomic absorption spectrometry (CV-AAS), and hydride generation atomic absorption spectrometry (HGAAS). The ranges, arithmetic means and geometric means of concentrations of these elements are presented. A comparison with crustal abundances (Clarke values) shows that some potentially hazardous elements in the coals of DPR Korea are highly enriched Li, B, S, Cl, Zn, As, Se, Cd, Sn, Sb, W, Te, Hg, Ag, Pb, and La, Ce, Dy, Tm, Ge, Mo, Cs, Tl, Bi, Th and U are moderately enriched. A comparison of ranges and means of elemental concentrations in DPR Korea, Chinese, and world coals shows the ranges of most elements in DPR Korea coals are very close to the ranges of world coals. Arithmetic means of most elements in DPR Korea coals are close to that of American coals. Most elements arithmetic means are higher in Jurassic and Paleogene coals than coals of other ages. In DPR Korea coals, only seven elements in early Permian coals are higher than other periods: Li, Zn, Se, Cd, Hg, Pb, and Bi. Only five elements B, As, Sr, Mo, W in Neogene coals have arithmetic means higher than others. SiO2 and Al2O 3 in ashes are more than 70% except six samples. The correlation between ash yields and major elements from high to low is in the order of Si>Al>Ti>K>Mg>Fe>Na>Ca>P>S. Most elements have high positive correlation with ash (r>0.5) and show high inorganic affinity. ?? 2005 Elsevier Ltd. All rights reserved.

Advancements in mass spectrometry for biological samples: Protein chemical cross-linking and metabolite analysis of plant tissues

DOE Office of Scientific and Technical Information (OSTI.GOV)

Klein, Adam

2015-01-01

This thesis presents work on advancements and applications of methodology for the analysis of biological samples using mass spectrometry. Included in this work are improvements to chemical cross-linking mass spectrometry (CXMS) for the study of protein structures and mass spectrometry imaging and quantitative analysis to study plant metabolites. Applications include using matrix-assisted laser desorption/ionization-mass spectrometry imaging (MALDI-MSI) to further explore metabolic heterogeneity in plant tissues and chemical interactions at the interface between plants and pests. Additional work was focused on developing liquid chromatography-mass spectrometry (LC-MS) methods to investigate metabolites associated with plant-pest interactions.

Crux: Rapid Open Source Protein Tandem Mass Spectrometry Analysis

PubMed Central

2015-01-01

Efficiently and accurately analyzing big protein tandem mass spectrometry data sets requires robust software that incorporates state-of-the-art computational, machine learning, and statistical methods. The Crux mass spectrometry analysis software toolkit (http://cruxtoolkit.sourceforge.net) is an open source project that aims to provide users with a cross-platform suite of analysis tools for interpreting protein mass spectrometry data. PMID:25182276

Major- and Trace-Element Concentrations in Soils from Two Geochemical Surveys (1972 and 2005) of the Denver, Colorado, Metropolitan Area

USGS Publications Warehouse

Kilburn, James E.; Smith, David B.; Closs, L. Graham; Smith, Steven M.

2007-01-01

Introduction This report contains major- and trace-element concentration data for soil samples collected in 1972 and 2005 from the Denver, Colorado, metropolitan area. A total of 405 sites were sampled in the 1972 study from an area approximately bounded by the suburbs of Golden, Thornton, Aurora, and Littleton to the west, north, east, and south, respectively. This data set included 34 duplicate samples collected in the immediate vicinity of the primary sample. In 2005, a total of 464 sites together with 34 duplicates were sampled from the same approximate localities sampled in 1972 as well as additional sites in east Aurora and the area surrounding the Rocky Mountain Arsenal. Sample density for both surveys was on the order of 1 site per square mile. At each site, sample material was collected from a depth of 0-5 inches. Each sample collected was analyzed for near-total major- and trace-element composition by the following methods: (1) inductively coupled plasma-mass spectrometry (ICP-MS) and inductively coupled plasma-atomic emission spectrometry (ICP-AES) for aluminum, antimony, arsenic, barium, beryllium, bismuth, cadmium, calcium, cerium, cesium, chromium, cobalt, copper, gallium, indium, iron, lanthanum, lead, lithium, magnesium, manganese, molybdenum, nickel, niobium, phosphorus, potassium, rubidium, scandium, silver, sodium, strontium, sulfur, tellurium, thallium, thorium, tin, titanium, tungsten, uranium, vanadium, yttrium, and zinc; and (2) hydride generation-atomic absorption spectrometry for selenium. The samples collected in 2005 were also analyzed by a cold vapor-atomic absorption method for mercury. This report makes available the analytical results of these studies.

Intratracheal instillation of pravastatin for the treatment of murine allergic asthma: a lung-targeted approach to deliver statins

PubMed Central

Zeki, Amir A; Bratt, Jennifer M; Chang, Kevin Y; Franzi, Lisa M; Ott, Sean; Silveria, Mark; Fiehn, Oliver; Last, Jerold A; Kenyon, Nicholas J

2015-01-01

Systemic treatment with statins mitigates allergic airway inflammation, TH2 cytokine production, epithelial mucus production, and airway hyperreactivity (AHR) in murine models of asthma. We hypothesized that pravastatin delivered intratracheally would be quantifiable in lung tissues using mass spectrometry, achieve high drug concentrations in the lung with minimal systemic absorption, and mitigate airway inflammation and structural changes induced by ovalbumin. Male BALB/c mice were sensitized to ovalbumin (OVA) over 4 weeks, then exposed to 1% OVA aerosol or filtered air (FA) over 2 weeks. Mice received intratracheal instillations of pravastatin before and after each OVA exposure (30 mg/kg). Ultra performance liquid chromatography – mass spectrometry was used to quantify plasma, lung, and bronchoalveolar lavage fluid (BALF) pravastatin concentration. Pravastatin was quantifiable in mouse plasma, lung tissue, and BALF (BALF > lung > plasma for OVA and FA groups). At these concentrations pravastatin inhibited airway goblet cell hyperplasia/metaplasia, and reduced BALF levels of cytokines TNFα and KC, but did not reduce BALF total leukocyte or eosinophil cell counts. While pravastatin did not mitigate AHR, it did inhibit airway hypersensitivity (AHS). In this proof-of-principle study, using novel mass spectrometry methods we show that pravastatin is quantifiable in tissues, achieves high levels in mouse lungs with minimal systemic absorption, and mitigates some pathological features of allergic asthma. Inhaled pravastatin may be beneficial for the treatment of asthma by having direct airway effects independent of a potent anti-inflammatory effect. Statins with greater lipophilicity may achieve better anti-inflammatory effects warranting further research. PMID:25969462

Use of filler limestone and construction and demolition residues for remediating soils contaminated with heavy metals: an assessment by means of plant uptake.

NASA Astrophysics Data System (ADS)

Banegas, Ascension; Martinez-Sanchez, Maria Jose; Agudo, Ines; Perez-Sirvent, Carmen

2010-05-01

A greenhouse trial was carried out to evaluate the assimilation of heavy metals by three types of horticultural plants (lettuce, broccoli and alfalfa), different parts of which are destined for human and animal consumption (leaves, roots, fruits). The plants were cultivated in four types of soil, one uncontaminated (T1), one soil collected in the surrounding area of Sierra Minera (T2), the third being remediated with residues coming from demolition and construction activities (T3) and the four remediated with filler limestone (T4). To determine the metal content, soil samples were first ground to a fine powder using an agate ball mill. Fresh vegetable samples were separated into root and aboveground biomass and then lyophilized. The DTPA-extractable content was also determined to calculate the bioavailable amount of metal. Finally, the translocation factor (TF) and bioconcentration factor (BCF) were calculated. Arsenic levels were obtained by using atomic fluorescence spectrometry with an automated continuous flow hydride generation (HG-AFS) spectrometer and Cd, Pb and Zn was determined by electrothermal atomization atomic absorption spectrometry (ETAAS) or flame atomic absorption spectrometry (FAAS). Samples of the leached water were also obtained and analyzed. According to our results, the retention of the studied elements varies with the type of plant and is strongly decreased by the incorporation of filler limestone and/or construction and demolition residues to the soils. This practice represents a suitable way to reduce the risk posed to the biota by the presence of high levels of heavy metal in soil.

Relationships between Molecular Composition and Optical Properties of Dissolved Organic Matter

NASA Astrophysics Data System (ADS)

Cooper, W. T.; Tfaily, M.; Osborne, D.; Paul, A.; Podgorski, D. C.; Corbett, J.; Chanton, J.

2009-12-01

Our focus is on the relationships between the optical properties of dissolved organic matter (DOM) and its molecular composition. For example, we demonstrated that changes in the absorption and fluorescence characteristics of DOM in outwelling from Brazilian mangrove forests correlated with decreases in highly unsaturated organic compounds as DOM was transported from mangrove porewaters to the continental shelf. In that work we combined ultrahigh resolution Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) that provided detailed compositional information with absorption and Excitation/Emission Matrix (EEM) spectroscopy This presentation will highlight new results utilizing the combination of optical spectroscopy and FT-ICR mass spectrometry to illuminate the processes which control DOM cycling. Our focus will be on the contributions of the heteroatom components of DOM (i.e. organic sulfur and organic nitrogen) to its optical properties and how changes in optical properties correlate with important environmental processes like humification and bioavailability. Figure 1 below includes a narrow 0.20 Dalton window from a mass spectrum which demonstrates the ability of ultrahigh resolution mass spectrometry to resolve and identify nitrogen heteroatom compounds in DOM. Our study sites include the Glacial Lake Agassiz Peatlands (GLAP) in northern Minnesota and wetlands in the Caloosahatchee River basin in South Florida. Figure 1. Isolated 0.20 Da window of an ESI-FT-ICR mass spectrum of DOM from a GLAP bog. Labels identify N1 (d,e,f) and N3 classes of nitrogen heteroatoms. The 0.0031 Da mass spacing is used to confirm the N3 class.

Skin contamination as pathway for nicotine intoxication in vapers.

PubMed

Maina, Giovanni; Castagnoli, Carlotta; Ghione, Giordana; Passini, Valter; Adami, Gianpiero; Larese Filon, Francesca; Crosera, Matteo

2017-06-01

Growing warnings on health effects related to electronic cigarettes have met inconclusive findings at present. This study analyzed the in vitro percutaneous absorption of nicotine resulting by skin contamination with two e-liquids (refill 1 and 2) containing nicotine at 1.8%. Donor chambers of 6 Franz cells for each refill liquid were filled with 1mL of nicotine e-liquid for 24h; at selected intervals, 1.5mL of the receptor solutions were collected for nicotine concentration analysis by mean gas chromatography-mass spectrometry (LOD: 0.01μg/mL). The experiment was repeated removing the nicotine donor solution after 10min from the application and rinsing the skin surface three times with 3.0mL of milliQ water. A total of 12 cells with 24h exposure and 12 cells washed were studied. The mean concentration of nicotine in the receiving phase at the end of the experiment was 54.9±29.5 and 30.2±18.4μg/cm 2 for refill 1 and 2 respectively and significantly lower in washed cells (4.7±2.4 and 3.5±1.3μg/cm 2 ). The skin absorption of nicotine can lead to minor health illness in vapers, while caution must be paid to dermal contamination by e liquids in children. The skin cleaning significantly reduced the transdermal absorption kinetic and intradermal deposition of nicotine. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of total arsenic in fish by hydride-generation atomic absorption spectrometry: method validation, traceability and uncertainty evaluation

NASA Astrophysics Data System (ADS)

Nugraha, W. C.; Elishian, C.; Ketrin, R.

2017-03-01

Fish containing arsenic compound is one of the important indicators of arsenic contamination in water monitoring. The high level of arsenic in fish is due to absorption through food chain and accumulated in their habitat. Hydride generation (HG) coupled with atomic absorption spectrometric (AAS) detection is one of the most popular techniques employed for arsenic determination in a variety of matrices including fish. This study aimed to develop a method for the determination of total arsenic in fish by HG-AAS. The method for sample preparation from American of Analytical Chemistry (AOAC) Method 999.10-2005 was adopted for acid digestion using microwave digestion system and AOAC Method 986.15 - 2005 for dry ashing. The method was developed and validated using Certified Reference Material DORM 3 Fish Protein for trace metals for ensuring the accuracy and the traceability of the results. The sources of uncertainty of the method were also evaluated. By using the method, it was found that the total arsenic concentration in the fish was 45.6 ± 1.22 mg.Kg-1 with a coverage factor of equal to 2 at 95% of confidence level. Evaluation of uncertainty was highly influenced by the calibration curve. This result was also traceable to International Standard System through analysis of Certified Reference Material DORM 3 with 97.5% of recovery. In summary, it showed that method of preparation and HG-AAS technique for total arsenic determination in fish were valid and reliable.

Mass spectrometry based on a coupled Cooper-pair box and nanomechanical resonator system

NASA Astrophysics Data System (ADS)

Jiang, Cheng; Chen, Bin; Li, Jin-Jin; Zhu, Ka-Di

2011-10-01

Nanomechanical resonators (NRs) with very high frequency have a great potential for mass sensing with unprecedented sensitivity. In this study, we propose a scheme for mass sensing based on the NR capacitively coupled to a Cooper-pair box (CPB) driven by two microwave currents. The accreted mass landing on the resonator can be measured conveniently by tracking the resonance frequency shifts because of mass changes in the signal absorption spectrum. We demonstrate that frequency shifts induced by adsorption of ten 1587 bp DNA molecules can be well resolved in the absorption spectrum. Integration with the CPB enables capacitive readout of the mechanical resonance directly on the chip.

The Synthesis and Characterization of a Group of Transition Metal Octabutoxynaphthalocyanines and the Absorption and Emission Properties of the Co, Rh, Ir, Ni, Pd and Pt Members of This Group

PubMed Central

Kim, Junhwan; Soldatova, Alexandra V.; Rodgers, Michael A. J.; Kenney, Malcolm E.

2013-01-01

The synthesis and photophysical properties of new metallo-octabutoxynaphthalocyanines with Rh(III), Ir(III), and Pt(II) are reported. Various metals were inserted into the metal-free octabutoxynaphthalocyanine and the resultant metal complexes were fully characterized by NMR, UV-vis spectroscopy, and mass spectrometry. The absorption and emission properties of these new complexes were also examined and compared to those of Co(II), Ni(II), and Pd(II) octabutoxynaphthalocyanines. The results provide useful information to understand the effect of these transition metals on the properties of this macrocyclic ring. PMID:23745014

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

USGS Publications Warehouse

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.

High Resolution Spectrometry of Leaf and Canopy Chemistry for Biochemical Cycling

NASA Technical Reports Server (NTRS)

Spanner, M. A.; Peterson, D. L.; Acevedo, W.; Matson, P.

1985-01-01

High-resolution laboratory spectrophotometer and Airborne Imaging Spectrometer (AIS) data were used to analyze forest leaf and canopy chemistry. Fundamental stretching frequencies of organic bonds in the visible, near infrared and short-wave infrared are indicative of concentrations and total content of nitrogen, phosphorous, starch and sugar. Laboratory spectrophotometer measurements showed very strong negative correlations with nitrogen (measured using wet chemistry) in the visible wavelengths. Strong correlations with green wet canopy weight in the atmospheric water absorption windows were observed in the AIS data. A fairly strong negative correlation between the AIS data at 1500 nm and total nitrogen and nitrogen concentration was evident. This relationship corresponds very closely to protein absorption features near 1500 nm.

Imaging mass spectrometry statistical analysis.

PubMed

Jones, Emrys A; Deininger, Sören-Oliver; Hogendoorn, Pancras C W; Deelder, André M; McDonnell, Liam A

2012-08-30

Imaging mass spectrometry is increasingly used to identify new candidate biomarkers. This clinical application of imaging mass spectrometry is highly multidisciplinary: expertise in mass spectrometry is necessary to acquire high quality data, histology is required to accurately label the origin of each pixel's mass spectrum, disease biology is necessary to understand the potential meaning of the imaging mass spectrometry results, and statistics to assess the confidence of any findings. Imaging mass spectrometry data analysis is further complicated because of the unique nature of the data (within the mass spectrometry field); several of the assumptions implicit in the analysis of LC-MS/profiling datasets are not applicable to imaging. The very large size of imaging datasets and the reporting of many data analysis routines, combined with inadequate training and accessible reviews, have exacerbated this problem. In this paper we provide an accessible review of the nature of imaging data and the different strategies by which the data may be analyzed. Particular attention is paid to the assumptions of the data analysis routines to ensure that the reader is apprised of their correct usage in imaging mass spectrometry research. Copyright © 2012 Elsevier B.V. All rights reserved.

The in vivo pharmacokinetics, tissue distribution and excretion investigation of mesaconine in rats and its in vitro intestinal absorption study using UPLC-MS/MS.

PubMed

Liu, Xiuxiu; Tang, Minghai; Liu, Taohong; Wang, Chunyan; Tang, Qiaoxin; Xiao, Yaxin; Yang, Ruixin; Chao, Ruobing

2017-12-27

1. Mesaconine, an ingredient from Aconitum carmichaelii Debx., has been proven to have cardiac effect. For further development and better pharmacological elucidation, the in vivo process and intestinal absorptive behavior of mesaconine should be investigated comprehensively. 2. An ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and validated for the quantitation of mesaconine in rat plasma, tissue homogenates, urine and feces to investigate the in vivo pharmacokinetic profiles, tissue distribution and excretion. The intestinal absorptive behavior of mesaconine was investigated using in vitro everted rat gut sac model. 3. Mesaconine was well distributed in tissues and a mass of unchanged form was detected in feces. It was difficultly absorbed into blood circulatory system after oral administration. The insufficient oral bioavailability of mesaconine may be mainly attributed to its low intestinal permeability due to a lack of lipophilicity. The absorption of mesaconine in rat's intestine is a first-order process with the passive diffusion mechanism.

Determination of sulfur in kerosene by combustion and molecular absorption spectrometry in the gas phase

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ruschak, M.L.; Syty, A.

1982-08-01

A technique of nonflame molecular adsorption in the gas phase developed for the determination of sulfite trapped in tetrachloromercurate, is described herein for application to the determination of total sulfur in kerosene. The burner head is removed from the atomic absorption spectrometer and replaced with a flow-through absorption cell. A special reaction vessel is used to evolve SO/sub 2/ from the sulfite in a precise and convenient manner. The transient absorbance caused by the SO/sub 2/, as it is carried through the absorption cell, is measured. Both spiked and unspiked samples of kerosene were analyzed, and the reproducibility of themore » repeated runs is evidenced by a relative standard deviation from the mean of 5% for the unspiked kerosene and 4% for the spiked kerosene. If the detection level is defined as that concentration of S which gives a % S twice the standard deviation from the mean yields, the detection limit for the present method is 0.002% S by weight in kerosene.« less

Time-resolved photoion imaging spectroscopy: Determining energy distribution in multiphoton absorption experiments

NASA Astrophysics Data System (ADS)

Qian, D. B.; Shi, F. D.; Chen, L.; Martin, S.; Bernard, J.; Yang, J.; Zhang, S. F.; Chen, Z. Q.; Zhu, X. L.; Ma, X.

2018-04-01

We propose an approach to determine the excitation energy distribution due to multiphoton absorption in the case of excited systems following decays to produce different ion species. This approach is based on the measurement of the time-resolved photoion position spectrum by using velocity map imaging spectrometry and an unfocused laser beam with a low fluence and homogeneous profile. Such a measurement allows us to identify the species and the origin of each ion detected and to depict the energy distribution using a pure Poisson's equation involving only one variable which is proportional to the absolute photon absorption cross section. A cascade decay model is used to build direct connections between the energy distribution and the probability to detect each ionic species. Comparison between experiments and simulations permits the energy distribution and accordingly the absolute photon absorption cross section to be determined. This approach is illustrated using C60 as an example. It may therefore be extended to a wide variety of molecules and clusters having decay mechanisms similar to those of fullerene molecules.

Scientific issues and potential remote-sensing requirements for plant biochemical content

NASA Technical Reports Server (NTRS)

Peterson, David L.; Hubbard, G. S.

1992-01-01

Application of developments in imaging spectrometry to the study of terrestrial ecosystems, which began in 1983, demonstrate the potential to estimate lignin and nitrogen concentrations of plant canopies by remote-sensing techniques. Estimation of these parameters from the first principles of radiative transfer and the interactions of light with plant materials is not presently possible, principally because of lack of knowledge about internal leaf scattering and specific absorption involving biochemical compounds. From the perspective of remote-sensing instrumentation, sensors are needed to support derivative imaging spectroscopy. Biochemical absorption features tend to occur in functional groupings throughout the 1100- to 2500-nm region. Derivative spectroscopy improves the information associated with the weaker, narrower absorption features of biochemical absorption that are superimposed on the strong absolute variations due to foliar biomass, pigments, and leaf water content of plant canopies. Preliminary sensor specifications call for 8-nm bandwidths at 2-nm centers in four spectral regions (about 400 bands total) and a signal-to-noise performance of at least 1000:1 for 20 percent albedo targets in the 2000-nm region.

Development of a certified reference material (NMIJ CRM 7531-a) for the determination of trace cadmium and other elements in brown rice flour.

PubMed

Miyashita, Shin-ichi; Inagaki, Kazumi; Narukawa, Tomohiro; Zhu, Yanbei; Kuroiwa, Takayoshi; Hioki, Akiharu; Chiba, Koichi

2012-01-01

A certified reference material (CRM) for trace cadmium and other elements in brown rice flour was developed at the National Metrology Institute of Japan (NMIJ). The CRM was provided as a dry powder after drying and frozen pulverization of fresh brown rice obtained from a Japanese domestic market. Characterization of the property value for each element was carried out exclusively by NMIJ with at least two independent analytical methods, including inductively coupled plasma mass spectrometry (ICP-MS), ICP high-resolution mass spectrometry, isotope-dilution ICP-MS, ICP optical emission spectrometry, and graphite-furnace atomic-absorption spectrometry. Property values were provided for six elements (Mn, Fe, Cu, Zn, As, and Cd). The concentration range of the property values was from 0.280 mg kg(-1) of As to 31.8 mg kg(-1) of Zn. The combined relative standard uncertainties of the property values were estimated by considering the uncertainties of the homogeneity, characterization, difference among analytical methods, dry-mass correction factor, and calibration standard. The range of the relative combined standard uncertainties was from 1.1% of Zn to 1.6% of As.

ICP OES and CV AAS in determination of mercury in an unusual fatal case of long-term exposure to elemental mercury in a teenager.

PubMed

Lech, Teresa

2014-04-01

In this work, a case of deliberate self-poisoning is presented. A 14-year-old girl suddenly died during one of the several hospitalizations. Abdominal computer tomography showed a large number of metallic particles in the large intestine. Analysis of blood and internal organs for mercury and other toxic metals carried out by inductively coupled plasma optical emission spectrometry (ICP OES) revealed high concentrations of mercury in kidneys and liver (64,200 and 2470ng/g, respectively), less in stomach (90ng/g), and none in blood. Using cold vapor-atomic absorption spectrometry (CV AAS), high levels of mercury were confirmed in all examined materials, including blood (87ng/g), and additionally in hair. The results of analysis obtained by two techniques revealed that the exposure to mercury was considerable (some time later, it was stated that the mercury originated from thermometers that had been broken over the course of about 1 year, because of Münchausen syndrome). CV AAS is a more sensitive technique, particularly for blood samples (negative results using ICP OES), and tissue samples - with LOQ: 0.63ng/g of Hg (CV AAS) vis-à-vis 70ng/g of Hg (ICP OES). However, ICP OES may be used as a screening technique for autopsy material in acute poisoning by a heavy metal, even one as volatile as mercury. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of whole-water recoverable arsenic, boron, and vanadium using inductively coupled plasma-mass spectrometry

USGS Publications Warehouse

Garbarino, John R.

2000-01-01

Analysis of in-bottle digestate by using the inductively coupled plasma?mass spectrometric (ICP?MS) method has been expanded to include arsenic, boron, and vanadium. Whole-water samples are digested by using either the hydrochloric acid in-bottle digestion procedure or the nitric acid in-bottle digestion procedure. When the hydrochloric acid in-bottle digestion procedure is used, chloride must be removed from the digestate by subboiling evaporation before arsenic and vanadium can be accurately determined. Method detection limits for these elements are now 10 to 100 times lower than U.S. Geological Survey (USGS) methods using hydride generation? atomic absorption spectrophotometry (HG? AAS) and inductively coupled plasma? atomic emission spectrometry (ICP?AES), thus providing lower variability at ambient concentrations. The bias and variability of the methods were determined by using results from spike recoveries, standard reference materials, and validation samples. Spike recoveries in reagent-water, surface-water, ground-water, and whole-water recoverable matrices averaged 90 percent for seven replicates; spike recoveries were biased from 25 to 35 percent low for the ground-water matrix because of the abnormally high iron concentration. Results for reference material were within one standard deviation of the most probable value. There was no significant difference between the results from ICP?MS and HG?AAS or ICP?AES methods for the natural whole-water samples that were analyzed.

Elemental imaging at the nanoscale: NanoSIMS and complementary techniques for element localisation in plants.

PubMed

Moore, Katie L; Lombi, Enzo; Zhao, Fang-Jie; Grovenor, Chris R M

2012-04-01

The ability to locate and quantify elemental distributions in plants is crucial to understanding plant metabolisms, the mechanisms of uptake and transport of minerals and how plants cope with toxic elements or elemental deficiencies. High-resolution secondary ion mass spectrometry (SIMS) is emerging as an important technique for the analysis of biological material at the subcellular scale. This article reviews recent work using the CAMECA NanoSIMS to determine elemental distributions in plants. The NanoSIMS is able to map elemental distributions at high resolution, down to 50 nm, and can detect very low concentrations (milligrams per kilogram) for some elements. It is also capable of mapping almost all elements in the periodic table (from hydrogen to uranium) and can distinguish between stable isotopes, which allows the design of tracer experiments. In this review, particular focus is placed upon studying the same or similar specimens with both the NanoSIMS and a wide range of complementary techniques, showing how the advantages of each technique can be combined to provide a fuller data set to address complex scientific questions. Techniques covered include optical microscopy, synchrotron techniques, including X-ray fluorescence and X-ray absorption spectroscopy, transmission electron microscopy, electron probe microanalysis, particle-induced X-ray emission and inductively coupled plasma mass spectrometry. Some of the challenges associated with sample preparation of plant material for SIMS analysis, the artefacts and limitations of the technique and future trends are also discussed.

An analytical method to screen for six thyreostatic drug residues in the thyroid gland and muscle tissues of food producing animals by liquid chromatography with ultraviolet absorption detection and liquid chromatography/mass spectrometry.

PubMed

Asea, Philip E; MacNeil, James D; Boison, Joe O

2006-01-01

A method was developed and validated to screen for residues of the thyreostatic drugs, tapazole (TAP), mercaptobenzimidazole (MBI), thiouracil (TU), methylthiouracil (MTU), propylthiouracil (PrTU), and phenylthiouracil (PhTU) in bovine, equine, ovine, and porcine thyroid and muscle tissues at concentrations > or = 5 ng/g using 2-methoxy-mercaptobenzimidazole (MeMBI) and dimethylthiouracil (DMTU) as internal standards. In this method, the drugs were solvent extracted from thyroid and muscle tissue and cleaned up on an amino-propyl solid-phase extraction (SPE) cartridge. The unretained fraction containing TAP and MBI and the internal standard, MeMBI, was collected as Fraction 1. The retained fraction containing TU, MTU, PrTU, PhTU, and the internal standard, DMTU, was eluted with 3% acetic acid-isopropanol as Fraction 2. Fraction 1 was further cleaned up on an alumina B SPE cartridge and analyzed by gradient elution on a C18 high-performance liquid chromatography (HPLC) column with ultraviolet detection at wavelengths of 255 and 300 nm. Fraction 2 was taken to dryness, derivatized with 4-chloro-7-nitrobenzo-2-furazan at pH 8, and analyzed by gradient elution on a C18 LC column with mass spectrometry (MS) detection. Any "presumptive positive" test results were submitted for further analysis by LC/MS/MS. The validated method was applied to the analysis of over 300 thyroid tissue samples.

Determination of Pesticides by Gas Chromatography Combined with Mass Spectrometry Using Femtosecond Lasers Emitting at 267, 400, and 800 nm as the Ionization Source.

PubMed

Yang, Xixiang; Imasaka, Tomoko; Imasaka, Totaro

2018-04-03

A standard sample mixture containing 51 pesticides was separated by gas chromatography (GC), and the constituents were identified by mass spectrometry (MS) using femtosecond lasers emitting at 267, 400, and 800 nm as the ionization source. A two-dimensional display of the GC/MS was successfully used for the determination of these compounds. A molecular ion was observed for 38 of the compounds at 267 nm and for 30 of the compounds at 800 nm, in contrast to 27 among 50 compounds when electron ionization was used. These results suggest that the ultraviolet laser is superior to the near-infrared laser for molecular weight determinations and for a more reliable analysis of these compounds. In order to study the conditions for optimal ionization, the experimental data were examined using the spectral properties (i.e., the excitation and ionization energies and absorption spectra for the neutral and ionized species) obtained by quantum chemical calculations. A few molecules remained unexplained by the currently reported rules, requiring additional rules for developing a full understanding of the femtosecond ionization process. The pesticides in the homogenized matrix obtained from kabosu ( citrus sphaerocarpa) were measured using lasers emitting at 267 and 800 nm. The pesticides were clearly separated and measured on the two-dimensional display, especially for the data measured at 267 nm, suggesting that this technique would have potential for use in the practical trace analysis of the pesticides in the environment.

Studies Concerning the Accumulation of Minerals and Heavy Metals in Fruiting Bodies of Wild Mushrooms

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stihi, Claudia; Radulescu, Cristiana; Gheboianu, Anca

2011-10-03

The minerals and heavy metals play an important role in the metabolic processes, during the growth and development of mushrooms, when they are available in appreciable concentration. In this work the concentrations of Cr, Mn, Fe, Ni, Cu, Zn, Se, Cd and Pb were analyzed using the Flame Atomic Absorption spectrometry (FAAS) together with Energy Dispersive X-ray Fluorescence spectrometry (EDXRF) in 3 wild mushrooms species and their growing substrate, collected from various forestry fields in Dambovita County, Romania. The analyzed mushrooms were: Amanita phalloides, Amanita rubescens and Armillariella mellea. The accumulation coefficients were calculated to assess the mobility of mineralsmore » and heavy metals from substrate to mushrooms [1].« less

The application of Westcott Formalism k0 NAA method to estimate short and medium lived elements in some Ghanaian herbal medicines complemented by AAS

NASA Astrophysics Data System (ADS)

Ayivor, J. E.; Okine, L. K. N.; Dampare, S. B.; Nyarko, B. J. B.; Debrah, S. K.

2012-04-01

The epithermal neutron shape factor, α of the inner and outer irradiation sites of the Ghana Research Reactor-1 (GHARR-1) was determined obtaining results of 0.105 for the inner (Channel 1) Irradiation site and 0.020 for the outer (channel 6) irradiation site. The neutron temperatures for the inner and outer irradiation sites were 27 °C and 20 °C, respectively. The α values used in Westcott Formalism k0 INAA was applied to determine multi elements in 13 Ghanaian herbal medicines used by the Centre for Scientific Research into Plant Medicine (CSRPM) for the management of various diseases complemented by Atomic Absorption Spectrometry. They are namely Mist. Antiaris, Mist. Enterica, Mist. Morazia, Mist. Nibima, Mist. Modium, Mist. Ninger, Mist Sodenia, Mist. Tonica, Chardicca Powder, Fefe Powder, Olax Powder, Sirrapac powder and Lippia Tea. Concentrations of Al, As, Br, K, Cl, Cu, Mg, Mn, Na and V were determined by short and medium irradiations at a thermal neutron flux of 5×1011 ncm-2 s-1. Fe, Cr, Pb, Co, Ni, Sn, Ca, Ba, Li and Sb were determined using Atomic Absorption Spectrometry (AAS). Ba, Cu, Li and V were present at trace levels whereas Al, Cl, Na, Ca were present at major levels. K, Br, Mg, Mn, Co, Ni, Fe and Sb were also present at minor levels. Arsenic was not detected in all samples. Standard Reference material, IAEA-V-10 Hay Powder was simultaneously analysed with samples. The precision and accuracy of the method using real samples and standard reference materials were evaluated and within ±10% of the reported value. Multivariate analytical techniques, such as cluster analysis (Q-mode and R-mode CA) and principal component analysis (PCA)/factor analysis (FA), have been applied to evaluate the chemical variations in the herbal medicine dataset. All the 13 samples may be grouped into 2 statistically significant clusters (liquid based and powdered herbal medicines), reflecting the different chemical compositions. R-mode CA and PCA suggest common sources for Co, Mg, Fe, Ca, Cr, Ni, Sn, Li and Sb and Na, V, Cl, Mn, Al, Br and K. The PCA/FA identified 3 dominant factors as responsible for the data structure, explaining 84.5% of the total variance in the dataset.

Human vitamin B12 absorption measurement by accelerator mass spectrometry using specifically labeled 14C-cobalamin

PubMed Central

Carkeet, Colleen; Dueker, Stephen R.; Lango, Jozsef; Buchholz, Bruce A.; Miller, Joshua W.; Green, Ralph; Hammock, Bruce D.; Roth, John R.; Anderson, Peter J.

2006-01-01

There is a need for an improved test of human ability to assimilate dietary vitamin B12. Assaying and understanding absorption and uptake of B12 is important because defects can lead to hematological and neurological complications. Accelerator mass spectrometry is uniquely suited for assessing absorption and kinetics of carbon-14 (14C)-labeled substances after oral ingestion because it is more sensitive than decay counting and can measure levels of 14C in microliter volumes of biological samples with negligible exposure of subjects to radioactivity. The test we describe employs amounts of B12 in the range of normal dietary intake. The B12 used was quantitatively labeled with 14C at one particular atom of the dimethylbenzimidazole (DMB) moiety by exploiting idiosyncrasies of Salmonella metabolism. To grow aerobically on ethanolamine, Salmonella enterica must be provided with either preformed B12 or two of its precursors, cobinamide and DMB. When provided with 14C-DMB specifically labeled in the C2 position, cells produced 14C-B12 of high specific activity (2.1 GBq/mmol, 58 mCi/mmol) (1 Ci = 37 GBq) and no detectable dilution of label from endogenous DMB synthesis. In a human kinetic study, a physiological dose (1.5 μg, 2.2 kBq/59 nCi) of purified 14C-B12 was administered and showed plasma appearance and clearance curves consistent with the predicted behavior of the pure vitamin. This method opens new avenues for study of B12 assimilation. PMID:16585531

Formation of nitrogen- and sulfur-containing light-absorbing compounds accelerated by evaporation of water from secondary organic aerosols

NASA Astrophysics Data System (ADS)

Nguyen, Tran B.; Lee, Paula B.; Updyke, Katelyn M.; Bones, David L.; Laskin, Julia; Laskin, Alexander; Nizkorodov, Sergey A.

2012-01-01

Aqueous extracts of secondary organic aerosols (SOA) generated from the ozonolysis of d-limonene were subjected to dissolution, evaporation, and re-dissolution in the presence and absence of ammonium sulfate (AS). Evaporation with AS at pH 4-9 produced chromophores that were stable with respect to hydrolysis and had a distinctive absorption band at 500 nm. Evaporation accelerated the rate of chromophore formation by at least three orders of magnitude compared to the reaction in aqueous solution, which produced similar compounds. Absorption spectroscopy and high-resolution nanospray desorption electrospray ionization (nano-DESI) mass spectrometry experiments suggested that the molar fraction of the chromophores was small (<2%), and that they contained nitrogen atoms. Although the colored products represented only a small fraction of SOA, their large extinction coefficients (>105 L mol-1 cm-1 at 500 nm) increased the effective mass absorption coefficient of the residual organics in excess of 103 cm2 g-1 - a dramatic effect on the optical properties from minor constituents. Evaporation of SOA extracts in the absence of AS resulted in the production of colored compounds only when the SOA extract was acidified to pH ˜ 2 with sulfuric acid. These chromophores were produced by acid-catalyzed aldol condensation, followed by a conversion into organosulfates. The presence of organosulfates was confirmed by high resolution mass spectrometry experiments. Results of this study suggest that evaporation of cloud or fog droplets containing dissolved organics leads to significant modification of the molecular composition and serves as a potentially important source of light-absorbing compounds.

Investigating the variability in brown carbon light-absorption properties

NASA Astrophysics Data System (ADS)

Saleh, R.; Cheng, Z.; Atwi, K.

2017-12-01

Combustion of biomass fuels contributes a significant portion of brown carbon (BrC), the light-absorbing fraction of organic aerosols. BrC exhibits highly variable light-absorption properties, with imaginary part of the refractive indices (k) reported in the literature varying over two orders of magnitude. This high variability in k is attributed to the chaotic nature of combustion; however, there is a major gap in the fundamental understanding of this variability. To address this gap, we hypothesize that BrC is comprised of black carbon (BC) precursors whose transformation to BC has not seen fruition. Depending on the combustion conditions, these BC precursors exhibit different maturity levels which dictate their light-absorption properties (k). The more mature are the precursors, the more absorptive (or BC-like) they are. Therefore, k of BrC obtained from a certain measurement depends on the specific combustion conditions associated with the measurement, leading to the aforementioned variability in the literature. To test this hypothesis, we performed controlled combustion experiments in which the combustion conditions (temperature and air/fuel ratio) were varied and k was retrieved from real-time multi-wavelength light-absorption measurements at each condition. We used benzene, the inception of which during combustion is the initial critical step leading to BC formation, as a model fuel. By varying the combustion conditions from relatively inefficient (low temperature and/or air/fuel ratio) to relatively efficient (high temperature and/or air/fuel ratio), we isolated BrC components with progressively increasing k, spanning the wide range reported in the literature. We also performed thermodenuder measurements to constrain the volatility of the BrC, as well as laser desorption ionization mass spectrometry analysis to constrain its molecular mass. We found that as the combustion conditions approached the BC-formation threshold, the increase in k was associated with an increase in molecular mass and decrease in volatility. This confirms our hypothesis, since the BC precursors are expected to grow in size and become less volatile as they mature. These results provide the first correlation between the BrC physical, chemical, and consequent light-absorption properties.

LC-MS of Metmyoglobin at pH = 2: Separation and Characterization of Apomyoglobin and Heme by ESI-MS and UV-Vis

ERIC Educational Resources Information Center

Stynes, Helen Cleary; Layo, Araceli; Smith, Richard W.

2004-01-01

The protein species of apomyoglobin (apoMb) and heme are freed and segregated from the aqueous protein solution of metmyoglobin by liquid chromatography, and are distinguished by UV-Vis absorption or electrospray ionization mass spectrometry (ESI-MS). This is an ingenious and effective approach to characterize apomyoglobin and heme, while students…

Matrix modification with silver for the electrothermal atomization of arsenic and selenium

USGS Publications Warehouse

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

1981-01-01

Silver as a matrix modifier is shown to improve the carbon-rod atomization of both arsenic and selenium for atomic absorption spectrometry. Compared to nickel, the efficiency of silver is greater for arsenic and about the same for selenium. Silver fulfils two functions in its reaction, namely stabilization during the ashing stage and enhancement of absorbance in the final atomization. ?? 1981.

NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR OPERATION, CALIBRATION AND MAINTENANCE OF THE JOBIN-YVON MODEL 70 INDUCTIVELY COUPLED PLASMA ATOMIC ABSORPTION SPECTROMETER (BCO-L-7.1)

EPA Science Inventory

The purpose of this SOP is to detail the operation and maintenance of an Instruments, SA Inc., Jobin-Yvon Model 70 (JY-70) inductively coupled plasma atomic emissions spectrometry (ICP-AES). This procedure was followed to ensure consistent data retrieval during the Arizona NHEXA...