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Sample records for absorption spectrometry analysis

  1. Chlorine analysis by diode laser atomic absorption spectrometry.

    PubMed

    Koch, J; Zybin, A; Niemax, K

    2000-04-01

    The general characteristics of Diode Laser Absorption Spectrometry (DLAAS) in low pressure plasmas particularly with respect to the detection of non-metals are comprehensively recapitulated and discussed. Furthermore, a detector, which is based on DLAAS in a microwave-induced low pressure plasma as an alternative technique for halogene-specific analysis of volatile compounds and polymeric matrices is described. The analytical capability of the technique is demonstrated on the chlorine-specific analysis of ablated polymer fragments as well as gas chromatographically separated hydrocarbons. Since the measurements were carried out by means of a balanced-heterodyne detection scheme, different technical noise contributions, such as laser excess and RAM noise could efficiently be suppressed and the registered absorption was limited only by the principal shot noise. Thus, in the case of the polymer analysis a chlorine-specific absolute detection limit of 10 pg could be achieved. Furthermore, fundamental investigations concerning the influence of hydrocarbons on the dissociation capability of the microwave induced plasma were performed. For this purpose, the carbon-, chlorine- and hydrogen-specific stoichiometry of the compounds were empirically determined. Deviations from the expected proportions were found to be insignificant, implying the possibility of internal standardization relative to the response of a reference sample. PMID:12953476

  2. COMPREHENSIVE ANALYSIS OF BIOLOGICALLY RELEVANT ARSENICALS BY PH-SELECTIVE HYDRIDE GENERATION-ATOMIC ABSORPTION SPECTROMETRY

    EPA Science Inventory


    A method based on pH-selective generation and separation of arsines is commonly used for analysis of inorganic, methylated, and dimethylated trivalent and pentavalent arsenicals by hydride generation-atomic absorption spectrometry (HG-AAS). We have optimized this method to pe...

  3. Laboratory verification of on-line lithium analysis using ultraviolet absorption spectrometry

    SciTech Connect

    Beemster, B.J.; Schlager, K.J.; Schloegel, K.M.; Kahle, S.J.; Fredrichs, T.L.

    1992-12-31

    Several laboratory experiments were performed to evaluate the capability of absorption spectrometry in the ultraviolet-visible wavelength range with the objective of developing methods for on-line analysis of lithium directly in the primary coolant of Pressurized Water Reactors using optical probes. Although initial laboratory tests seemed to indicate that lithium could be detected using primary absorption (detection of natural spectra unassisted by reagents), subsequent field tests demonstrated that no primary absorption spectra existed for lithium in the ultraviolet-visible wavelength range. A second series of tests that were recently conducted did, however, confirm results reported in the literature to the effect that reagents were available that will react with lithium to form chelates that possess detectable absorption and fluorescent signatures. These results point to the possible use of secondary techniques for on-line analysis of lithium.

  4. Automation of preparation of nonmetallic samples for analysis by atomic absorption and inductively coupled plasma spectrometry

    NASA Technical Reports Server (NTRS)

    Wittmann, A.; Willay, G.

    1986-01-01

    For a rapid preparation of solutions intended for analysis by inductively coupled plasma emission spectrometry or atomic absorption spectrometry, an automatic device called Plasmasol was developed. This apparatus used the property of nonwettability of glassy C to fuse the sample in an appropriate flux. The sample-flux mixture is placed in a composite crucible, then heated at high temperature, swirled until full dissolution is achieved, and then poured into a water-filled beaker. After acid addition, dissolution of the melt, and filling to the mark, the solution is ready for analysis. The analytical results obtained, either for oxide samples or for prereduced iron ores show that the solutions prepared with this device are undistinguished from those obtained by manual dissolutions done by acid digestion or by high temperature fusion. Preparation reproducibility and analytical tests illustrate the performance of Plasmasol.

  5. Direct analysis of silica by means of solid sampling graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Resano, M.; Mozas, E.; Crespo, C.; Pérez, J.; García-Ruiz, E.; Belarra, M. A.

    2012-05-01

    This paper reports on the use of solid sampling-graphite furnace atomic absorption spectrometry for the direct analysis of synthetic amorphous silica. In particular, determination of hazardous elements such As, Cd, Cr, Cu, Pb and Sb is investigated, as required by regulations of the food industry. The conclusion of the work is that, after proper optimization of the working conditions, paying particular attention to the atomization temperature and the use of proper modifiers (graphite powder, HNO3 or Pd), it is possible to develop suitable procedures that rely on the use of aqueous standard solutions to construct the calibration curves for all the elements investigated. The proposed method shows important benefits for the cost-effective analysis of such difficult samples in routine labs, permitting fast screening of those elements that are very rarely present in this type of sample, but also accurate quantification of those often found, while offering low limits of detection (always below 0.1 mg g- 1) that comply well with legal requirements, and precision levels that are fit for the purpose (approx. 6-9% R.S.D.).

  6. Ultraviolet and Light Absorption Spectrometry.

    ERIC Educational Resources Information Center

    Hargis, L. G.; Howell, J. A.

    1984-01-01

    Reviews developments in ultraviolet and light absorption spectrometry from December 1981 through November 1983, focusing on the chemistry involved in developing suitable reagents, absorbing systems, and methods of determination, and on physical aspects of the procedures. Includes lists of spectrophotometric methods for metals, non-metals, and…

  7. Atomic Absorption Spectrometry Analysis of Trace Elements in Degenerated Intervertebral Disc Tissue

    PubMed Central

    Kubaszewski, Łukasz; Zioła-Frankowska, Anetta; Frankowski, Marcin; Nowakowski, Andrzej; Czabak-Garbacz, Róża; Kaczmarczyk, Jacek; Gasik, Robert

    2014-01-01

    Background Few studies have investigated trace elements (TE) in human intervertebral disc (IVD) tissue. Trace element presence can have diverse meanings: essential TE show the metabolic modalities of the tissue, while environmentally-related TE indicate pollution and tissue-specific absorption and accumulation. IVD is a highly specific compartment with impaired communication with adjacent bone. Analysis of TE in IVD provides new insights regarding tissue metabolism and IVD communication with other tissues. Material/Methods Thirty intervertebral discs were acquired from 22 patients during surgical treatment for degenerative disease. Atomic absorption spectrometry was used to evaluate the concentrations of Al, Cd, Pb, Cu, Ni, Mo, Mg, and Zn. Results Al, Pb, Cu, Mg, and Zn were detected in all samples. Pb was significantly positively correlated with age, and Ni concentration was weakly correlated with population count in the patient’s place of residence. Only Cu was observed in higher concentrations in IVD compared to in other tissues. Significant positive correlations were observed between the following pairs: Mg/Zn, Mg/Al, Mg/Pb, Zn/Al, Zn/Pb, and Al/Pb. Negative correlations were observed between Mg/Cd, Zn/Cd, Mg/Mo, and Mo/Pb. Conclusions This study is one of few to profile the elements in intervertebral discs in patients with degenerative changes. We report significant differences between trace element concentrations in intervertebral discs compared to in other tissues. Knowledge of the TE accumulation pattern is vital for better understanding intervertebral disc nutrition and metabolism. PMID:25366266

  8. Accelerator mass spectrometry analysis of aroma compound absorption in plastic packaging materials

    NASA Astrophysics Data System (ADS)

    Stenström, Kristina; Erlandsson, Bengt; Hellborg, Ragnar; Wiebert, Anders; Skog, Göran; Nielsen, Tim

    1994-05-01

    Absorption of aroma compounds in plastic packaging materials may affect the taste of the packaged food and it may also change the quality of the packaging material. A method to determine the aroma compound absorption in polymers by accelerator mass spectrometry (AMS) is being developed at the Lund Pelletron AMS facility. The high sensitivity of the AMS method makes it possible to study these phenomena under realistic conditions. As a first test low density polyethylene exposed to 14C-doped ethyl acetate is examined. After converting the polymer samples with the absorbed aroma compounds to graphite, the {14C }/{13C } ratio of the samples is measured by the AMS system and the degree of aroma compound absorption is established. The results are compared with those obtained by supercritical fluid extraction coupled to gas chromatography (SFE-GC).

  9. Methods of calibration in the direct analysis of solid samples by electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Berglund, M.; Baxter, D. C.

    1992-12-01

    One of the major problems involved in the direct analysis of solid samples by electrothermal atomic absorption spectrometry (ETAAS) lies in the calibration step because non-spectral interference effects are often pronounced. Three standardization techniques have been described and used in solid sampling-ETAAS: (i) standard additions method; (ii) calibration relative to a certified reference material; and (iii) calibration curve technique. However, an adequate statistical evaluation of the uncertainty in the analyte concentration in the solid sample is most frequently neglected, and reported errors may be seriously underestimated. This can be attributed directly to the complexity of the statistical expressions required to accurately account for errors in each of the calibration techniques mentioned above, and the general lack of relevant reference literature. The object of this work has been to develop a computer package which will perform the necessary statistical analyses of solid sampling-ETAAS data; the result is the program "SOLIDS" described here in the form of an electronic publication in Spectrochimica Acta Electronica, the electronic section of Spectrochimica Acta Part B. The program could also be useful in other analytical fields where similar calibration methods are used. The hard copy text, outlining the calibration models and their associated errors, is accompanied by a diskette containing the program, some data files, and a manual. Use of the program is exemplified in the text, with some of the data files discussed included on the diskette which, together with the manual, should enable the reader to become familiarized with the operation of the program, and the results generated.

  10. Analysis of the Release Characteristics of Cu-Treated Antimicrobial Implant Surfaces Using Atomic Absorption Spectrometry

    PubMed Central

    Zietz, Carmen; Fritsche, Andreas; Finke, Birgit; Stranak, Vitezslav; Haenle, Maximilian; Hippler, Rainer; Mittelmeier, Wolfram; Bader, Rainer

    2012-01-01

    New developments of antimicrobial implant surfaces doped with copper (Cu) ions may minimize the risk of implant-associated infections. However, experimental evaluation of the Cu release is influenced by various test parameters. The aim of our study was to evaluate the Cu release characteristics in vitro according to the storage fluid and surface roughness. Plasma immersion ion implantation of Cu (Cu-PIII) and pulsed magnetron sputtering process of a titanium copper film (Ti-Cu) were applied to titanium alloy (Ti6Al4V) samples with different surface finishing of the implant material (polished, hydroxyapatite and corundum blasted). The samples were submersed into either double-distilled water, human serum, or cell culture medium. Subsequently, the Cu concentration in the supernatant was measured using atomic absorption spectrometry. The test fluid as well as the surface roughness can alter the Cu release significantly, whereby the highest Cu release was determined for samples with corundum-blasted surfaces stored in cell medium. PMID:22162672

  11. Analysis of the release characteristics of cu-treated antimicrobial implant surfaces using atomic absorption spectrometry.

    PubMed

    Zietz, Carmen; Fritsche, Andreas; Finke, Birgit; Stranak, Vitezslav; Haenle, Maximilian; Hippler, Rainer; Mittelmeier, Wolfram; Bader, Rainer

    2012-01-01

    New developments of antimicrobial implant surfaces doped with copper (Cu) ions may minimize the risk of implant-associated infections. However, experimental evaluation of the Cu release is influenced by various test parameters. The aim of our study was to evaluate the Cu release characteristics in vitro according to the storage fluid and surface roughness. Plasma immersion ion implantation of Cu (Cu-PIII) and pulsed magnetron sputtering process of a titanium copper film (Ti-Cu) were applied to titanium alloy (Ti6Al4V) samples with different surface finishing of the implant material (polished, hydroxyapatite and corundum blasted). The samples were submersed into either double-distilled water, human serum, or cell culture medium. Subsequently, the Cu concentration in the supernatant was measured using atomic absorption spectrometry. The test fluid as well as the surface roughness can alter the Cu release significantly, whereby the highest Cu release was determined for samples with corundum-blasted surfaces stored in cell medium. PMID:22162672

  12. Simple analysis of total mercury and methylmercury in seafood using heating vaporization atomic absorption spectrometry.

    PubMed

    Yoshimoto, Keisuke; Anh, Hoang Thi Van; Yamamoto, Atsushi; Koriyama, Chihaya; Ishibashi, Yasuhiro; Tabata, Masaaki; Nakano, Atsuhiro; Yamamoto, Megumi

    2016-01-01

    This study aimed to develop a simpler method for determining total mercury (T-Hg) and methylmercury (MeHg) in biological samples by using methyl isobutyl ketone (MIBK) in the degreasing step. The fat in the samples was extracted by MIBK to the upper phase. T-Hg transferred into the water phase. This was followed by the extraction of MeHg from the water phase using HBr, CuCl2 and toluene. The MeHg fraction was reverse-extracted into L-cysteine-sodium acetate solution from toluene. The concentrations of T-Hg and MeHg were determined by heating vaporization atomic absorption spectrometry. Certified reference materials for T-Hg and MeHg in hair and fish were accurately measured using this method. This method was then applied to determine T-Hg and MeHg concentrations in the muscle, liver and gonads of seafood for the risk assessment of MeHg exposure. The mean T-Hg and MeHg concentrations in squid eggs were 0.023 and 0.022 µg/g, and in squid nidamental glands 0.052 and 0.049 µg/g, respectively. The MeHg/T-Hg ratios in the eggs and nidamental glands of squid were 94.4% and 96.5%, respectively. The mean T-Hg and MeHg concentrations in the gonads of sea urchins were 0.043 and 0.001 µg/g, respectively, with a MeHg/T-Hg ratio of 3.5%. We developed an efficient analytical method for T-Hg and MeHg using MIBK in the degreasing step. The new information on MeHg concentration and MeHg/T-Hg ratios in the egg or nidamental glands of squid and gonads of sea urchin will also be useful for risk assessment of mercury in seafood. PMID:27432235

  13. Direct analysis of solids by graphite furnace atomic absorption spectrometry using a second surface atomizer

    SciTech Connect

    Rettberg, T.M.; Holcombe, J.A.

    1986-06-01

    The direct graphite furnace atomic absorption spectrometric analysis of solids using the second surface atomizer has been investigated. The atomizer features a gas-cooled Ta insert within the graphite furnace onto which the analyte can be condensed, after which atomization is performed by raising the furnace to a higher temperature and shutting off the coolant gas. The analyses were conducted on standard reference material fly ash, river sediment, and citrus leaves, in addition to filter paper samples. All analyses were conducted without sample pretreatment or use of matrix modifiers. Quantitation was done by using simple aqueous standards. By use of peak heights, the recoveries varied from 81% to 127%, although several determinations were within the certified concentration range. The procedures typically gave low background absorbances and peak shapes that were relatively independent of the original sample matrix.

  14. Fluorine determination in coal using high-resolution graphite furnace molecular absorption spectrometry and direct solid sample analysis

    NASA Astrophysics Data System (ADS)

    Machado, Patrícia M.; Morés, Silvane; Pereira, Éderson R.; Welz, Bernhard; Carasek, Eduardo; de Andrade, Jailson B.

    2015-03-01

    The absorption of the calcium mono-fluoride (CaF) molecule has been employed in this study for the determination of fluorine in coal using direct solid sample analysis and high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS). The rotational line at 606.440 nm was used for measuring the molecular absorption in the gas phase. The pyrolysis and vaporization temperatures were 700 °C and 2100 °C, respectively. Different chemical modifiers have been studied, such as Pd and Ir as permanent modifiers, and Pd and the mixed Pd/Mg modifier in solution. The limit of detection and the characteristic mass were 0.3 and 0.1 ng F, respectively. One certified reference material (CRM) of coal (NIST 1635) and four CRMs with a non-certified value for F (SARM 18, SARM 20, BCR 40, BCR 180) were used to evaluate the accuracy and precision of the method, obtaining good agreement (104%) with the certified value and with the informed values (ranging from 90 to 103%).

  15. Graphite filter atomizer in atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Katskov, Dmitri A.

    2007-09-01

    Graphite filter atomizers (GFA) for electrothermal atomic absorption spectrometry (ETAAS) show substantial advantages over commonly employed electrothermal vaporizers and atomizers, tube and platform furnaces, for direct determination of high and medium volatility elements in matrices associated with strong spectral and chemical interferences. Two factors provide lower limits of detection and shorter determination cycles with the GFA: the vaporization area in the GFA is separated from the absorption volume by a porous graphite partition; the sample is distributed over a large surface of a collector in the vaporization area. These factors convert the GFA into an efficient chemical reactor. The research concerning the GFA concept, technique and analytical methodology, carried out mainly in the author's laboratory in Russia and South Africa, is reviewed. Examples of analytical applications of the GFA in AAS for analysis of organic liquids and slurries, bio-samples and food products are given. Future prospects for the GFA are discussed in connection with analyses by fast multi-element AAS.

  16. High-resolution continuum source electrothermal atomic absorption spectrometry — An analytical and diagnostic tool for trace analysis

    NASA Astrophysics Data System (ADS)

    Welz, Bernhard; Borges, Daniel L. G.; Lepri, Fábio G.; Vale, Maria Goreti R.; Heitmann, Uwe

    2007-09-01

    The literature about applications of high-resolution continuum source atomic absorption spectrometry (HR-CS AAS) with electrothermal atomization is reviewed. The historic development of HR-CS AAS is briefly summarized and the main advantages of this technique, mainly the 'visibility' of the spectral environment around the analytical line at high resolution and the unequaled simultaneous background correction are discussed. Simultaneous multielement CS AAS has been realized only in a very limited number of cases. The direct analysis of solid samples appears to have gained a lot from the special features of HR-CS AAS, and the examples from the literature suggest that calibration can be carried out against aqueous standards. Low-temperature losses of nickel and vanadyl porphyrins could be detected and avoided in the analysis of crude oil due to the superior background correction system. The visibility of the spectral environment around the analytical line revealed that the absorbance signal measured for phosphorus at the 213.6 nm non-resonance line without a modifier is mostly due to the PO molecule, and not to atomic phosphorus. The future possibility to apply high-resolution continuum source molecular absorption for the determination of non-metals is discussed.

  17. Analysis of monolayer formation of α-mycolic acid derived from Mycobacterium bovis BCG pasteur strain by infrared reflection-absorption spectrometry with two-dimensional correlation analysis

    NASA Astrophysics Data System (ADS)

    Hasegawa, T.; Nishijo, J.; Umemura, J.; Watanabe, M.

    2000-03-01

    Monolayer formation mechanism of α-mycolic acid (α-MA) isolated from Mycobacterium bovis BCG Pasteur strain was investigated by infrared reflection-absorption (IRRA) spectrometry with two-dimensional (2D) correlation analysis. The raw IRRA spectra did not characterize the precise feature of the MA monolayer. 2D correlation analysis, however, clearly revealed that the longer or the major chain of the MA stood up earlier than the shorter chain or the α-alkyl group when the monolayer was compressed, and that the upright chains were in the form of ordered conformation.

  18. Multi-element analysis of manganese nodules by atomic absorption spectrometry without chemical separation

    USGS Publications Warehouse

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

    1982-01-01

    Five manganese nodules, including the USGS reference nodules A-1 and P-1, were analyzed for Co, Cu, Fe, K, Mg, Mn, Na, Ni and Zn without prior chemical separation by using a simultaneous multi-element atomic absorption spectrometer with an air-cetylene flame. The nodules were prepared in three digestion matrices. One of these solutions was measured using sixteen different combinations of burner height and air/acetylene ratios. Results for A-1 and P-1 are compared to recommended values and results for all nodules are compared to those obtained with an inductively coupled plasma. The elements Co, Cu, Fe, K, Mg, Mn, Na, Ni, and Zn are simultaneously determined with a composite recovery for all elements of 100 ?? 7%, independent of the digestion matrices, heights in the flame, or flame stoichiometries examined. Individual recoveries for Co, K, and Ni are considerably poorer in two digests than this composite figure, however. The optimum individual recoveries of 100 ?? 5% and imprecisions of 1-4%, except for zinc, are obtained when Co, K, Mn, Na and Ni are determined simultaneously in a concentrated digest, and in another analytical sequence, when Cu, Fe, Mg, Mn and Zn are measured simultaneously after dilution. Determination of manganese is equally accurate in the two sequences; its measurement in both assures internal consistency between the two measurement sequences. This approach improves analytical efficiency over that for conventional atomic absorption methods, while minimizing loss of accuracy or precision for individual elements. ?? 1982.

  19. Particular problems encountered in trace metal analysis of plant material by atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Hoenig, M.; de Borger, R.

    Various mineralization methods for plant material analysis by AAS are presented and their advantages and limits are discussed. Wet digestion by H 2SO 4HNO 3H 2O 2 mixture appears as a very rapid method which gives good recovery of trace elements and is thus suitable for routine analysis. Determination of relatively high concentrations of Cu, Zn, Fe, Mn, Ni, Cr, Co, Cd, Pb, As, Sb and Tl is carried out by flame AAS with a good analytical speed and without noticeable interferences. Pb, Cd, As, Sb and Tl appear generally in very low concentrations in plants so that electrothermal atomization is necessary. Various interferences are observed in this case. They are discussed and methods are presented for their correction.

  20. Automated continuous monitoring of inorganic and total mercury in wastewater and other waters by flow-injection analysis and cold-vapour atomic absorption spectrometry

    PubMed Central

    Birnie, S. E.

    1988-01-01

    An automated continuous monitoring system for the determination of inorganic and total mercury by flow-injection analysis followed by cold-vapour atomic absorption spectrometry is described. The method uses a typical flow-injection manifold where digestion and reduction of the injected sample takes place. Mercury is removed by aeration from the flowing stream in a specially designed air-liquid separator and swept into a silica cell for absorption measurement at a wavelength of 253.7 nm. A calibration curve up to 10 μg Hg ml-1 using three different path length cells is obtained with a detection limit of 0.02 μg Hg ml-1. The sampling rate of an injection every 3 min produces 20 results per hour from a flowing stream. PMID:18925201

  1. 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

    This paper describes an automated system for the oxidation state specific speciation of inorganic and methylated arsenicals by selective hydride generation - cryotrapping- gas chromatography - atomic absorption spectrometry with the multiatomizer. The corresponding arsines are ge...

  2. Fractionation analysis of manganese and zinc in beers by means of two sorbent column system and flame atomic absorption spectrometry.

    PubMed

    Pohl, Pawel; Prusisz, Bartlomiej

    2007-03-15

    In the present article, a method of operational fractionation of Mn and Zn in beer using flame atomic absorption spectrometry was developed. The proposed fractionation scheme was based on use of a hydrophobic adsorbing resin Amberlite XAD7 (first column, 2g resin bed) connected in a series with a strong cation exchanger Dowex 50Wx4 (second column, 1g resin bed). After passing the samples of beers through the columns, distinct groupings of Mn and Zn species retained on the sorbents, i.e., hydrophobic fraction of polyphenols bound metal species and cationic metal species fraction, respectively, were determined in respective eluates obtained after complete recovery of Mn and Zn species with 10ml of 2.0moll(-1) HNO(3) (first column) and 10ml of 4.0moll(-1) HCl (second column). In addition, the effluents collected were analyzed prior to the evaluation of the third, residual fraction, presumably attributed to any hydrophilic anionic and inert metal species. The established fractionation patterns for Mn and Zn were discussed in reference to likely associations of metals with endogenous food bioligands and possible availability of the distinguished metal species classes. The quality of the results was proved by the recovery experiments. PMID:19071499

  3. Analysis of lead in 55 brands of dietary calcium supplements by graphite furnace atomic absorption spectrometry after microwave digestion.

    PubMed

    Kim, Meehye; Kim, Changmin; Song, Insang

    2003-02-01

    The lead (Pb) contents of calcium (Ca) supplements available in Korea were determined by graphite furnace atomic absorption spectrometry using Zeeman background correction and peak area mode. All samples were microwave-digested in concentrated HNO(3). Ammonium dihydrogen phosphate and magnesium nitrate were used as matrix modifiers. Fifty-five brands of Ca supplements were classified into seven categories based on the major composite: bone, milk, oyster/clam shell, egg shell, algae, shark cartilage and chelated. The mean Pb contents of Ca supplements were 1.1 microg g(-1) (coefficient of variation 5.7%), ranging from n.d. (not detected) to 6.7 microg g(-1). Ca supplements made of bone have the highest Pb contents (2.3 microg g(-1)) with a wide range (0.1-6.7 microg g(-1)). The results were similar to those reported in other countries. The mean daily intakes of Pb from the supplement could be about 5 microg (mean Pb concentration 1.1 microg g(-1) x mean daily intake 4.5 g) taking 2% of provisional tolerable daily intake that the FAO/WHO Joint Food Additive and Contaminants Committee has set to evaluate its safety. However, measures to prevent potentials of Pb toxicity from overtaking some Ca supplements should be considered. PMID:12623663

  4. Restricted access carbon nanotubes for direct extraction of cadmium from human serum samples followed by atomic absorption spectrometry analysis.

    PubMed

    Barbosa, Adriano F; Barbosa, Valéria M P; Bettini, Jefferson; Luccas, Pedro O; Figueiredo, Eduardo C

    2015-01-01

    In this paper, we propose a new sorbent that is able to extract metal ions directly from untreated biological fluids, simultaneously excluding all proteins from these samples. The sorbent was obtained through the modification of carbon nanotubes (CNTs) with an external bovine serum albumin (BSA) layer, resulting in restricted access carbon nanotubes (RACNTs). The BSA layer was fixed through the interconnection between the amine groups of the BSA using glutaraldehyde as cross-linker. When a protein sample is percolated through a cartridge containing RACNTs and the sample pH is higher than the isoelectric point of the proteins, both proteins from the sample and the BSA layer are negatively ionized. Thus, an electrostatic repulsion prevents the interaction between the proteins from the sample on the RACNTs surface. At the same time, metal ions are adsorbed in the CNTs (core) after their passage through the chains of proteins. The Cd(2+) ion was selected for a proof-of-principle case to test the suitability of the RACNTs due to its toxicological relevance. RACNTs were able to extract Cd(2+) and exclude almost 100% of the proteins from the human serum samples in an online solid-phase extraction system coupled with thermospray flame furnace atomic absorption spectrometry. The limits of detection and quantification were 0.24 and 0.80 μg L(-1), respectively. The sampling frequency was 8.6h(-1), and the intra- and inter-day precisions at the 0.80, 15.0, and 30.0 μg L(-1) Cd(2+) levels were all lower than 10.1% (RSD). The recoveries obtained for human blood serum samples fortified with Cd(2+) ranged from 85.0% to 112.0%. The method was successfully applied to analyze Cd(2+) directly from six human blood serum samples without any pretreatment, and the observed concentrations ranged from

  5. Method development for the determination of bromine in coal using high-resolution continuum source graphite furnace molecular absorption spectrometry and direct solid sample analysis

    NASA Astrophysics Data System (ADS)

    Pereira, Éderson R.; Castilho, Ivan N. B.; Welz, Bernhard; Gois, Jefferson S.; Borges, Daniel L. G.; Carasek, Eduardo; de Andrade, Jailson B.

    2014-06-01

    This work reports a simple approach for Br determination in coal using direct solid sample analysis in a graphite tube furnace and high-resolution continuum source molecular absorption spectrometry. The molecular absorbance of the calcium mono-bromide (CaBr) molecule has been measured using the rotational line at 625.315 nm. Different chemical modifiers (zirconium, ruthenium, palladium and a mixture of palladium and magnesium nitrates) have been evaluated in order to increase the sensitivity of the CaBr absorption, and Zr showed the best overall performance. The pyrolysis and vaporization temperatures were 800 °C and 2200 °C, respectively. Accuracy and precision of the method have been evaluated using certified coal reference materials (BCR 181, BCR 182, NIST 1630a, and NIST 1632b) with good agreement (between 98 and 103%) with the informed values for Br. The detection limit was around 4 ng Br, which corresponds to about 1.5 μg g- 1 Br in coal, based on a sample mass of 3 mg. In addition, the results were in agreement with those obtained using electrothermal vaporization inductively coupled plasma mass spectrometry, based on a Student t-test at a 95% confidence level. A mechanism for the formation of the CaBr molecule is proposed, which might be considered for other diatomic molecules as well.

  6. Mineral content of vertebral trabecular bone: accuracy of dual energy quantitative computed tomography evaluated against neutron activation analysis and flame atomic absorption spectrometry.

    PubMed

    Louis, O; Van den Winkel, P; Covens, P; Schoutens, A; Osteaux, M

    1994-01-01

    The goal of this study was to evaluate the accuracy of preprocessing dual energy quantitative computed tomography (QCT) for assessment of trabecular bone mineral content (BMC) in lumbar vertebrae. The BMC of 49 lumbar vertebrae taken from 16 cadavers was measured using dual energy QCT with advanced software and hardware capabilities, including an automated definition of the trabecular region of interest (ROI). The midvertebral part of each vertebral body was embedded in a polyester resin and, subsequently, an experimental ROI was cut out using a scanjet image transmission procedure and a computer-assisted milling machine in order to mimic the ROI defined on QCT. After low temperature ashing, the experimental ROIs reduced to a bone powder were submitted to either nondestructive neutron activation analysis (n = 49) or to flame atomic absorption spectrometry (n = 45). BMC obtained with neutron activation analysis was closely related (r = 0.896) to that derived from atomic absorption spectrometry, taken as the gold standard, with, however, a slight overestimation. BMC values measured by QCT were highly correlated with those assessed using the two reference methods, all correlation coefficients being > 0.841. The standard errors of the estimate ranged 47.4-58.9 mg calcium hydroxyapatite in the regressions of BMC obtained with reference methods against BMC assessed by single energy QCT, 47.1-51.9 in the regressions involving dual energy QCT. We conclude that the trabecular BMC of lumbar vertebrae can be accurately measured by QCT and that the superiority in accuracy of dual energy is moderate, which is possible a characteristic of the preprocessing method. PMID:8024849

  7. Assessment of the Halogen Content of Brazilian Inhalable Particulate Matter (PM10) Using High Resolution Molecular Absorption Spectrometry and Electrothermal Vaporization Inductively Coupled Plasma Mass Spectrometry, with Direct Solid Sample Analysis.

    PubMed

    de Gois, Jefferson S; Almeida, Tarcisio S; Alves, Jeferson C; Araujo, Rennan G O; Borges, Daniel L G

    2016-03-15

    Halogens in the atmosphere play an important role in climate change and also represent a potential health hazard. However, quantification of halogens is not a trivial task, and methods that require minimum sample preparation are interesting alternatives. Hence, the aim of this work was to evaluate the feasibility of direct solid sample analysis using high-resolution continuum source molecular absorption spectrometry (HR-CS MAS) for F determination and electrothermal vaporization-inductively coupled plasma mass spectrometry (ETV-ICP-MS) for simultaneous Cl, Br, and I determination in airborne inhalable particulate matter (PM10) collected in the metropolitan area of Aracaju, Sergipe, Brazil. Analysis using HR-CS MAS was accomplished by monitoring the CaF molecule, which was generated at high temperatures in the graphite furnace after the addition of Ca. Analysis using ETV-ICP-MS was carried out using Ca as chemical modifier/aerosol carrier in order to avoid losses of Cl, Br, and I during the pyrolysis step, with concomitant use of Pd as a permanent modifier. The direct analysis approach resulted in LODs that were proven adequate for halogen determination in PM10, using either standard addition calibration or calibration against a certified reference material. The method allowed the quantification of the halogens in 14 PM10 samples collected in a northeastern coastal city in Brazil. The results demonstrated variations of halogen content according to meteorological conditions, particularly related to rainfall, humidity, and sunlight irradiation. PMID:26192198

  8. Isotope Enrichment Detection by Laser Ablation - Laser Absorption Spectrometry: Automated Environmental Sampling and Laser-Based Analysis for HEU Detection

    SciTech Connect

    Anheier, Norman C.; Bushaw, Bruce A.

    2010-01-01

    The global expansion of nuclear power, and consequently the uranium enrichment industry, requires the development of new safeguards technology to mitigate proliferation risks. Current enrichment monitoring instruments exist that provide only yes/no detection of highly enriched uranium (HEU) production. More accurate accountancy measurements are typically restricted to gamma-ray and weight measurements taken in cylinder storage yards. Analysis of environmental and cylinder content samples have much higher effectiveness, but this approach requires onsite sampling, shipping, and time-consuming laboratory analysis and reporting. Given that large modern gaseous centrifuge enrichment plants (GCEPs) can quickly produce a significant quantity (SQ ) of HEU, these limitations in verification suggest the need for more timely detection of potential facility misuse. The Pacific Northwest National Laboratory (PNNL) is developing an unattended safeguards instrument concept, combining continuous aerosol particulate collection with uranium isotope assay, to provide timely analysis of enrichment levels within low enriched uranium facilities. This approach is based on laser vaporization of aerosol particulate samples, followed by wavelength tuned laser diode spectroscopy to characterize the uranium isotopic ratio through subtle differences in atomic absorption wavelengths. Environmental sampling (ES) media from an integrated aerosol collector is introduced into a small, reduced pressure chamber, where a focused pulsed laser vaporizes material from a 10 to 20-µm diameter spot of the surface of the sampling media. The plume of ejected material begins as high-temperature plasma that yields ions and atoms, as well as molecules and molecular ions. We concentrate on the plume of atomic vapor that remains after the plasma has expanded and then cooled by the surrounding cover gas. Tunable diode lasers are directed through this plume and each isotope is detected by monitoring absorbance

  9. Determination of chlorine in coal via the SrCl molecule using high-resolution graphite furnace molecular absorption spectrometry and direct solid sample analysis

    NASA Astrophysics Data System (ADS)

    Pereira, Éderson R.; Rocha, Lucas M.; Cadorim, Heloisa R.; Silva, Vanessa D.; Welz, Bernhard; Carasek, Eduardo; de Andrade, Jailson B.

    2015-12-01

    In this study, the determination of chlorine in coal is described via molecular absorption of the strontium mono-chloride (SrCl) molecule at 635.862 nm using high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS) and direct solid sample analysis. The pyrolysis and vaporization temperatures were optimized and the measurements are accomplished with a platform coated with zirconium as a permanent chemical modifier in order to increase the sensitivity of the gaseous SrCl molecule generated in the graphite furnace. The optimum pyrolysis and vaporization temperatures were 700 °C and 2100 °C, respectively. Under optimized conditions, the limit of detection and characteristic mass of the method were 0.85 and 0.24 ng, respectively. The accuracy of the method has been verified using four certified reference materials and one not certified reference material of coal, and the results were in good agreement with the certified or reference values.

  10. 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)…

  11. On-line pre-reduction of pentavalent arsenicals by thioglycolic acid for speciation analysis by selective hydride generation cryotrapping atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Musil, Stanislav; Matoušek, Tomáš

    2008-06-01

    An improvement of current method of selective hydride generation based on pre-reduction for differentiation of tri- and pentavalent arsenicals is described, applied for the oxidation state specific speciation analysis of inorganic, mono-, di- and trimethylated arsenicals with minimum sample pretreatment using atomic absorption spectrometry with the multiatomizer. The preconcentration and separation of arsine, methylarsine, dimethylarsine and trimethylarsine are then carried out by means of cryotrapping. The presented study shows that 2% (m/v) L-cysteine hydrochloride monohydrate ( L-cys) currently used for off-line pre-reduction of pentavalent arsenicals can be substituted with 1% (m/v) thioglycolic acid (TGA). Much faster pre-reduction of pentavalent arsenicals at 25 °C with equal sensitivities as in the case of L-cys has been achieved with TGA. A setup for on-line pre-reduction by TGA has been optimized, with the application of segmented flow analysis for suppression of axial dispersion in the pre-reduction coil. Standard calibrations measured with or without on-line pre-reduction indicate uniform and equal sensitivities for all As forms. The possibility of standardization by water standards of single species (e.g. iAs(III)) for quantification of all other As forms in urine is demonstrated in the recovery study. Limits of detection were 100 ng l - 1 for iAs(III), 135 ng l - 1 for iAs(V) and 30 to 50 ng l - 1 for methylated arsenicals.

  12. Non-chromatographic screening procedure for arsenic speciation analysis in fish-based baby foods by using electrothermal atomic absorption spectrometry.

    PubMed

    López-García, Ignacio; Briceño, Marisol; Hernández-Córdoba, Manuel

    2011-08-01

    A procedure for the speciation analysis of arsenic in fish-based baby foods is presented. Inorganic arsenic, methylarsonic acid (MA), dimethylarsinic acid (DMA) and arsenobetaine (AB) were determined by electrothermal atomic absorption spectrometry (ETAAS) using suspensions prepared in a 0.01 mol L(-1) tetramethylammonium hydroxide (TMAH) solution. Speciation is based on the use of three different chemically modified ETAAS atomizers to obtain the analytical signals. Using a palladium salt as the chemical modifier, the signal corresponding to the total arsenic concentration is obtained. When palladium is replaced by Ce(IV), the signal is solely due to inorganic arsenic (III and V)+MA. If no signal is obtained in this latter case, it is possible to distinguish between DMA and AB using a zirconium coated atomizer. The signal obtained in this way is due solely to DMA, and the concentration of AB can be obtained by the difference with the total arsenic content. Determinations by ETAAS require the use of the standard additions method. The limits of detection for the determination of AB, DMA and inorganic arsenic (+MA) are 15, 25 and 50 ng g(-1) expressed as arsenic, respectively. These detection limits are good enough for the procedure to be appropriate for the rapid determination of these compounds, avoiding extraction processes and/or chromatographic separations. Data for commercial samples, as well as for four standard reference materials, are given. PMID:21704752

  13. Calculations of an effective solid angle including self-absorption correction applied to gamma-ray spectrometry analysis of natural samples

    NASA Astrophysics Data System (ADS)

    Fraczkiewicz, R.; Walkowiak, W.

    1992-09-01

    A new method is presented for determination of uranium and thorium contents in solid samples by gamma-ray spectrometry. The analytical procedure involved determination of uranium via the 63.288 keV gamma emission of its daughter 234Th and thorium on the basis of 238.578 keV 212Pb peak. The radiochemical equilibrium was assumed. Geometry effects and exact self-absorption were taken into account by measurements of sample linear absorption coefficients and calculation of effective solid angle. IAEA standards were used for determination of detector efficiency. The method provides reliable analytical measurements even for samples much different from standard reference materials in density and gamma absorption.

  14. 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

  15. 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. PMID:26452789

  16. 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.

  17. AIR MONITORING BY DIFFERENTIAL OPTICAL ABSORPTION SPECTROMETRY IN BAYTOWN, TEXAS

    EPA Science Inventory

    This report documents the results of a field study carried out in Baytown, Texas in August 1993. ne goal of the field study was to evaluate calibration and audit procedures for a differential optical absorption spectrometry (DOAS) system. he other major goal of the study was to c...

  18. [Determination of lead in beard hair by atomic absorption spectrometry (author's transl)].

    PubMed

    Graef, V

    1976-04-01

    The lead content of hair from the electric razor can be determined by atomic absorption spectrometry, using the micro-sampling technique of Delves. 1--5 mg of the washed and dried hair are partially oxidized with hydrogen peroxide prior to analysis. The method is simple and quick and therefore suited for the serial investigation of persons exposed to lead. PMID:1271019

  19. Absorption Mode FT-ICR Mass Spectrometry Imaging

    SciTech Connect

    Smith, Donald F.; Kilgour, David P.; Konijnenburg, Marco; O'Connor, Peter B.; Heeren, Ronald M.

    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 for 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.

  20. [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. PMID:23697150

  1. A technique coupling the analyte electrodeposition followed by in-situ stripping with electrothermal atomic absorption spectrometry for analysis of samples with high NaCl contents

    NASA Astrophysics Data System (ADS)

    Čánský, Zdeněk; Rychlovský, Petr; Petrová, Zuzana; Matousek, J. P.

    2007-03-01

    A technique coupling the analyte electrodeposition followed by in-situ stripping with electrothermal atomic absorption spectrometry has been developed for determination of lead and cadmium in samples with high salt contents. To separate the analyte from the sample matrix, the analyte was in-situ quantitatively electrodeposited on a platinum sampling capillary serving as the cathode (sample volume, 20 μL). The spent electrolyte containing the sample matrix was then withdrawn, the capillary with the analyte deposited was washed with deionized water and the analyte was stripped into a chemically simple electrolyte (5 g/L NH 4H 2PO 4) by reversing the polarity of the electrodeposition circuit. Electrothermal atomization using a suitable optimized temperature program followed. A fully automated manifold was designed for this coupled technique and the appropriate control software was developed. The operating conditions for determination of Pb and Cd in samples with high contents of inorganic salts were optimized, the determination was characterized by principal analytical parameters and its applicability was verified on analyses of urine reference samples. The absolute limits of detection for lead and cadmium (3 σ criterion) in a sample containing 30 g/L NaCl were 8.5 pg and 2.3 pg, respectively (peak absorbance) and the RSD values amounted to 1.6% and 1.9% for lead (at the 40 ng mL - 1 level) and cadmium (at the 4.0 ng mL - 1 level), respectively. These values (and also the measuring sensitivity) are superior to the results attained in conventional electrothermal atomic absorption spectrometric determination of Pb and Cd in pure solutions (5 g/L NH 4H 2PO 4). The sensitivity of the Pb and Cd determination is not affected by the NaCl concentration up to a value of 100 g/L, demonstrating an efficient matrix removal during the electrodeposition step.

  2. Investigation of chemical modifiers for sulfur determination in diesel fuel samples by high-resolution continuum source graphite furnace molecular absorption spectrometry using direct analysis

    NASA Astrophysics Data System (ADS)

    Huber, Charles S.; Vale, Maria Goreti R.; Welz, Bernhard; Andrade, Jailson B.; Dessuy, Morgana B.

    2015-06-01

    High-resolution continuum source graphite furnace molecular absorption spectrometry has been applied for sulfur determination in diesel fuel. The sharp rotational lines of the carbon monosulfide molecule (formed during the vaporization step) were used to measure the absorbance. The analytical line at 258.056 nm was monitored using the sum of three pixels. Different chemical modifiers were investigated and the mixture of palladium and magnesium was used as chemical modifier in combination with iridium as permanent modifier. L-Cysteine was chosen as sulfur standard and the calibration was done against aqueous standard solutions. The proposed method was applied for the analyses of four diesel samples: two S10 samples and two S500 samples. The trueness of the method was checked with a certified reference material (CRM) of sulfur in diesel fuel (NIST 2724b). Accurate results, for samples and CRM, were achieved after a dilution with propan-1-ol. The following figures of merit were obtained: characteristic mass of 17 ± 3 ng, limit of detection and limit of quantification of 1.4 mg kg- 1 and 4.7 mg kg- 1, respectively.

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

    ERIC Educational Resources Information Center

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

    2004-01-01

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

  4. 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.

  5. 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. PMID:26992542

  6. 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

    NASA Astrophysics Data System (ADS)

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

    2008-03-01

    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.

  7. Electrothermal atomic absorption spectrometry determination of molybdenum in whole blood

    NASA Astrophysics Data System (ADS)

    Burguera, J. L.; Rondón, C.; Burguera, M.; Roa, M. E.; Petit de Peña, Y.

    2002-03-01

    A method for the determination of molybdenum in whole blood by atomic absorption spectrometry with electrothermal atomization was developed and evaluated. Erbium (25 μg) was chosen from several potential chemical modifiers (Sm, Lu, Ho, Eu and Pd+Mg) as the most appropriate for the sensitive and reliable determination of molybdenum in such sample. The process used was direct dilution of the sample in a ratio 1:2 with a 0.1% (v/v) Triton X-100 solution. The injection of 20 μl of a solution of 15% (w/v) hydrogen peroxide and running the temperature program after 5 firings greatly reduced the effect of build-up of carbonaceous residues within the atomizer. The limit of detection and working ranges, respectively, were 0.6 and 2.0-100.0 μg l -1, and the characteristic mass was 7.2 pg. The relative standard deviation varied from 0.8 to 1.5% for within and between batch determinations, respectively. The determination of molybdenum in Seronorm™ Trace Elements in Whole Blood with known added amounts of the analyte was performed to asses the accuracy. The optimized procedure has been applied to the determination of molybdenum in whole blood specimens of 20 subjects taken before and 10-12 h after receiving an over-supply of 1 mg of molybdenum. The molybdenum concentrations (±S.D.) were 10.9±0.4 μg Mo l -1 (range 9.9-11.6 μg Mo l -1) and 15.4±0.4 μg Mo l -1 (range 13.1-16.9 μg Mo l -1) for the individuals before and after the administration of molybdenum.

  8. A thin-walled metallic hollow cathode as an atomizer for Zeeman atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Ganeyev, A. A.; Sholupov, S. E.

    1998-03-01

    A new kind of glow discharge atomizer, a thin-walled metallic hollow cathode (TMHC) combined with Zeeman atomic absorption spectrometry using high frequency modulated light polarization (ZAAS-HFM), is studied. A theoretically suggested, and experimentally confirmed, model of the atom confinement in the TMHC yields the appearance of the diffusion traps for atoms at both ends of the cathode, which increases the residence time of the analyte atoms in the analysis volume. The high atomization efficiency in the glow discharge atomizer (caused by the ionic-thermal mechanism of sputtering) and the high selectivity of ZAAS-HFM are demonstrated in the analysis of complex matrix samples such as whole blood and urine. The analytical system TMHC + ZAAS-HFM is characterized by low detection limits, which are comparable to those of graphite furnace atomic absorption spectrometry (GFAAS). Owing to its rather low average power consumption (30-50 W) the TMHC can be used in a portable and mobile spectrometer, and is therefore suitable for the in situ analysis of various sample materials.

  9. 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.

  10. 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...

  11. Redox speciation analysis of dissolved iron in estuarine and coastal waters with on-line solid phase extraction and graphite furnace atomic absorption spectrometry detection.

    PubMed

    Chen, Yaojin; Feng, Sichao; Huang, Yongming; Yuan, Dongxing

    2015-05-01

    An automatic on-line solid phase extraction (SPE) system employing the flow injection (FI) technique directly coupled to a graphite furnace atomic absorption spectrometer (GFAAS) was established for speciation and determination of dissolved iron in estuarine and coastal waters. Fe(II) was mixed with ferrozine solution in a sample stream to form the Fe(II)-ferrozine complex which was extracted onto a C18 SPE cartridge, eluted with eluent and detected with GFAAS. In a parallel flow channel, Fe(III) was reduced to Fe(II) with ascorbic acid and then detected in the same way as Fe(II). The home-made interface between FI-SPE and GFAAS efficiently realized the sample introduction to the furnace in a semi-automated way. Parameters of the FI-SPE system and graphite furnace program were optimized based on a univariate experimental design and an orthogonal array design. The salinity effect on the method sensitivity was investigated. The proposed method provided a detection limit of 1.38 nmol L(-1) for Fe(II) and 1.87 nmol L(-1) for Fe(II+III). With variation of the sample loading volume, a broadened determination range of 2.5-200 nmol L(-1) iron could be obtained. The proposed method was successfully applied to analyze iron species in samples collected from the Jiulongjiang Estuary, Fujian, China. With the 2-cartridge FI-SPE system developed, on-line simultaneous determination of Fe species with GFAAS was achieved for the first time. PMID:25770602

  12. Some interferences in atomic-absorption spectrometry and extraction of iron and copper.

    PubMed

    Yanagisawa, M; Kihara, H; Suzuki, M; Takeuchi, T

    1970-09-01

    The effect of complexing agents on the atomic-absorption spectrometry of iron and copper extracts was investigated Thiocyanate complexes gave a marked depression of absorption by iron and copper, especially in fuel-rich flames. Chloride, diethyldithiocarbamate and hydroxyquinoline complexes of iron behaved alike, but differently from the thiocyanate complex. PMID:18960816

  13. 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.

  14. 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

  15. 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. PMID:27566338

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

    PubMed

    Saavedra, Y; Fernández, P; González, A

    2004-05-01

    A method was developed for the quantitative determination of total vanadium concentration in mussels via electrothermal atomic absorption spectrometry (ETAAS). After the microwave digestion of the samples, a program using temperatures of 1600 degrees C and 2600 degrees C for ashing and atomization respectively, without any matrix modifiers, allowed us to obtain results that were satisfactory since they agreed closely with certified reference material values. The detection limit was 0.03 mg kg(-1) (dry weight), indicating that the method is suitable for the analysis of mussel samples. This determination was compared with matrix modifiers that have been reported previously. The method was applied to various cultivated and wild mussels from the Galician coast, yielding levels below 1 mg kg(-1) (wet weight). PMID:14745471

  17. 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.

  18. Cadmium, copper, lead, and zinc determination in precipitation: A comparison of inductively coupled plasma atomic emission spectrometry and graphite furnace atomization atomic absorption spectrometry

    USGS Publications Warehouse

    Reddy, M.M.; Benefiel, M.A.; Claassen, H.C.

    1987-01-01

    Selected trace element analysis for cadmium, copper, lead, and zinc in precipitation samples by inductively coupled plasma atomic emission Spectrometry (ICP) and by atomic absorption spectrometry with graphite furnace atomization (AAGF) have been evaluated. This task was conducted in conjunction with a longterm study of precipitation chemistry at high altitude sites located in remote areas of the southwestern United States. Coefficients of variation and recovery values were determined for a standard reference water sample for all metals examined for both techniques. At concentration levels less than 10 micrograms per liter AAGF analyses exhibited better precision and accuracy than ICP. Both methods appear to offer the potential for cost-effective analysis of trace metal ions in precipitation. ?? 1987 Springer-Verlag.

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

    PubMed

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

    2005-05-01

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

  20. Determination of arsenic and selenium in environmental and agricultural samples by hydride generation atomic absorption spectrometry

    SciTech Connect

    Hershey, J.W.; Oostdyk, T.S.; Keliher, P.N.

    1988-11-01

    Agricultural and environmental samples are digested with acid, and arsenic and selenium are determined using hydride generation atomic absorption spectrometry. Interelement interferences are eliminated by high acid concentrations or cation-exchange resins. Agreement with standard reference material is excellent. The technique is also applied to actual samples.

  1. Analytical control of wollastonite for biomedical applications by use of atomic absorption spectrometry and inductively coupled plasma atomic emission spectrometry.

    PubMed

    De Aza, P N; Guitián, F; De Aza, S; Valle, F J

    1998-04-01

    Preliminary in vitro experiments revealed that wollastonite (CaSiO3) is a potentially highly bioactive material that forms a hyroxyapatite (HA) surface layer on exposure to simulated body fluid with an ion concentration, pH and temperature virtually identical with those of human blood plasma. The formation of the HA layer is an essential requirement for an artificial material to be used as bioactive bone substitute. This finding opens up a wide field for biomedical applications of wollastonite. Biomaterials used as implants in the human body require strict control of trace elements and of the toxic species specified in American Society for Testing and Materials F-1185-88 (As, Cd, Hg and Pb) in ceramic hydroxyapatite for surgical implantation. In this work, two types of pseudowollastonite, the high temperature form of wollastonite, were analysed by using cold vapour atomic absorption spectrometry and hydride generation atomic absorption spectrometry, in order to determine the elements stated in the above-mentioned norm, and inductively coupled plasma atomic emission spectrometry to establish the SiO2/CaO ratio of the two materials and analyse for all other impurities introduced by the raw materials and by the processes of synthesis, sintering and grinding. Barium and Mg were especially prominent in raw materials, and Zr, Y, Mg, W, Co and Ni come mainly from the processing. PMID:9684401

  2. 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).

  3. Near edge X-ray absorption mass spectrometry on coronene

    SciTech Connect

    Reitsma, G.; Deuzeman, M. J.; Hoekstra, R.; Schlathölter, T.; Boschman, L.; Hoekstra, S.

    2015-01-14

    We have investigated the photoionization and photodissociation of free coronene cations C{sub 24}H{sub 12}{sup +} upon soft X-ray photoabsorption in the carbon K-edge region by means of a time-of-flight mass spectrometry approach. Core excitation into an unoccupied molecular orbital (below threshold) and core ionization into the continuum both leave a C 1s vacancy, that is subsequently filled in an Auger-type process. The resulting coronene dications and trications are internally excited and cool down predominantly by means of hydrogen emission. Density functional theory was employed to determine the dissociation energies for subsequent neutral hydrogen loss. A statistical cascade model incorporating these dissociation energies agrees well with the experimentally observed dehydrogenation. For double ionization, i.e., formation of intermediate C{sub 24}H{sub 12}{sup 3+⋆}trications, the experimental data hint at loss of H{sup +} ions. This asymmetric fission channel is associated with hot intermediates, whereas colder intermediates predominantly decay via neutral H loss.

  4. Simultaneous multielement atomic absorption spectrometry with graphite furnace atomization

    NASA Astrophysics Data System (ADS)

    Harnly, James M.; Miller-Ihli, Nancy J.; O'Haver, Thomas C.

    The extended analytical range capability of a simultaneous multielement atomic absorption continuum source spectrometer (SIMAAC) was tested for furnace atomization with respect to the signal measurement mode (peak height and area), the atomization mode (from the wall or from a platform), and the temperature program mode (stepped or ramped atomization). These parameters were evaluated with respect to the shapes of the analytical curves, the detection limits, carry-over contamination and accuracy. Peak area measurements gave more linear calibration curves. Methods for slowing the atomization step heating rate, the use of a ramped temperature program or a platform, produced similar calibration curves and longer linear ranges than atomization with a stepped temperature program. Peak height detection limits were best using stepped atomization from the wall. Peak area detection limits for all atomization modes were similar. Carry-over contamination was worse for peak area than peak height, worse for ramped atomization than stepped atomization, and worse for atomization from a platform than from the wall. Accurate determinations (100 ± 12% for Ca, Cu, Fe, Mn, and Zn in National Bureau of Standards' Standard Reference Materials Bovine Liver 1577 and Rice Flour 1568 were obtained using peak area measurements with ramped atomization from the wall and stepped atomization from a platform. Only stepped atomization from a platform gave accurate recoveries for K. Accurate recoveries, 100 ± 10%, with precisions ranging from 1 to 36 % (standard deviation), were obtained for the determination of Al, Co, Cr, Fe, Mn, Mo, Ni. Pb, V and Zn in Acidified Waters (NBS SRM 1643 and 1643a) using stepped atomization from a platform.

  5. Determination of mercury in phosphate fertilizers by cold vapor atomic absorption spectrometry.

    PubMed

    de Jesus, Robson M; Silva, Laiana O B; Castro, Jacira T; de Azevedo Neto, Andre D; de Jesus, Raildo M; Ferreira, Sergio L C

    2013-03-15

    In this paper, a method for the determination of mercury in phosphate fertilizers using slurry sampling and cold vapor atomic absorption spectrometry (CV QT AAS) is proposed. Because mercury (II) ions form strong complexes with phosphor compounds, the formation of metallic mercury vapor requires the presence of lanthanum chloride as a release agent. Thiourea increases the amount of mercury that is extracted from the solid sample to the liquid phase of the slurry. The method is established using two steps. First, the slurry is prepared using the sample, lanthanum chloride, hydrochloric acid solution and thiourea solution and is sonicated for 20 min. Afterward, mercury vapor is generated using an aliquot of the slurry in the presence of the hydrochloric acid solution and isoamylic alcohol with sodium tetrahydroborate solution as the reducing agent. The experimental conditions for slurry preparation were optimized using two-level full factorial design involving the factors: thiourea and lanthanum chloride concentrations and the duration of sonication. The method allows the determination of mercury by external calibration using aqueous standards with limits of detection and quantification of 2.4 and 8.2 μg kg(-1), respectively, and precision, expressed as relative standard deviation, of 6.36 and 5.81% for two phosphate fertilizer samples with mercury concentrations of 0.24 and 0.57 mg kg(-1), respectively. The accuracy was confirmed by the analysis of a certified reference material of phosphate fertilizer that was provided by the National Institute of Standards & Technology (NIST). The method was applied to determine mercury in six commercial samples of phosphate fertilizers. The mercury content varied from 33.97 to 209.28 μg kg(-1). These samples were also analyzed employing inductively coupled plasma mass spectrometry (ICP-MS). The ICP-MS results were consistent with the results from our proposed method. PMID:23598130

  6. Broadband Analysis of Bioagents by Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Fenselau, Catherine; Wynne, Colin; Edwards, Nathan

    Mass spectrometry was first reported to provide analysis of intact metabolite biomarkers from whole cells in 1975.1 Since then advances in ionization techniques have extended our capabilities to polar lipids and, eventually, to proteins.2, 3 Mass spectrometry provides a broadband detection system, which, however, has great specificity. Bioinformatics plays an important role in providing flexible and rapid characterization of species, based on protein and peptide mass spectra collected in the field.

  7. Inorganic trace analysis by mass spectrometry

    NASA Astrophysics Data System (ADS)

    Becker, Johanna Sabine; Dietze, Hans-Joachim

    1998-10-01

    Mass spectrometric methods for the trace analysis of inorganic materials with their ability to provide a very sensitive multielemental analysis have been established for the determination of trace and ultratrace elements in high-purity materials (metals, semiconductors and insulators), in different technical samples (e.g. alloys, pure chemicals, ceramics, thin films, ion-implanted semiconductors), in environmental samples (waters, soils, biological and medical materials) and geological samples. Whereas such techniques as spark source mass spectrometry (SSMS), laser ionization mass spectrometry (LIMS), laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), glow discharge mass spectrometry (GDMS), secondary ion mass spectrometry (SIMS) and inductively coupled plasma mass spectrometry (ICP-MS) have multielemental capability, other methods such as thermal ionization mass spectrometry (TIMS), accelerator mass spectrometry (AMS) and resonance ionization mass spectrometry (RIMS) have been used for sensitive mono- or oligoelemental ultratrace analysis (and precise determination of isotopic ratios) in solid samples. The limits of detection for chemical elements using these mass spectrometric techniques are in the low ng g -1 concentration range. The quantification of the analytical results of mass spectrometric methods is sometimes difficult due to a lack of matrix-fitted multielement standard reference materials (SRMs) for many solid samples. Therefore, owing to the simple quantification procedure of the aqueous solution, inductively coupled plasma mass spectrometry (ICP-MS) is being increasingly used for the characterization of solid samples after sample dissolution. ICP-MS is often combined with special sample introduction equipment (e.g. flow injection, hydride generation, high performance liquid chromatography (HPLC) or electrothermal vaporization) or an off-line matrix separation and enrichment of trace impurities (especially for characterization of

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

    PubMed

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

    2001-08-01

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

  9. Preconcentration and determination of tellurium in garlic samples by hydride generation atomic absorption spectrometry.

    PubMed

    Kaplan, Marcos M; Cerutti, Soledad; Salonia, José A; Gásquez, José A; Martinez, Luis D

    2005-01-01

    A procedure for the determination of traces of total tellurium (Te) in garlic (Allium sativa) is described that combines hydride generation atomic absorption spectrometry with preconcentration of the analyte by coprecipitation. The samples, each spiked with lanthanum nitrate (20 mg/L), are introduced into an Amberlite XAD-4 resin and mixed with ammonium buffer (pH 9.1). Te is preconcentrated by coprecipitation with the generated lanthanum hydroxide precipitate. The precipitate is quantitatively collected in the resin, eluted with hydrochloric acid, and then transferred into the atomizer device. Considering a sample consumption of 25 mL, an enrichment factor of 10 was obtained. The detection limit (3sigma) was 0.03 microg/L, and the precision (relative standard deviation) was 3.5% (n = 10) at the 10 microg/L level. The calibration graph using the preconcentration system for Te was linear with a correlation coefficient of 0.9993. Satisfactory results were obtained for the analysis of Te in garlic samples. PMID:16152948

  10. 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.

  11. Economical Analysis about Ammonia Absorption Refrigeration Plants

    NASA Astrophysics Data System (ADS)

    Takei, Toshitaka

    NH3-H2O absorption refrigeration plant is attractive from each standpoint of electric power saving, non-fluorocarbon and energy saving. The plant can be the economic alternative of power compression refrigeration for evaporation temperature range from 0°C to -60°C, using suitable waste heat (co-generation system, waste incinerator), oil and natural gas. In the application of the plant, the equipment cost and the COP must be reasonable from economical standpoint. Therefore, the paper shows the following. 1) Necessary heating temparature analysis for absorption plant 2) Equipment cost analysis for heating temperature 3) Equipment cost analysis for COP 4) Number of trays in the rectifying column for COP 5) Equipment cost analysis and COP in two-stage absorption

  12. Total Absorption Gamma-ray Spectrometer (TAGS) Intensity Distributions from INL's Gamma-Ray Spectrometry Center

    DOE Data Explorer

    Greenwood, R. E.

    A 252Cf fission-product source and the INL on-line isotope separator were used to supply isotope-separated fission-product nuclides to a total absorption -ray spectrometer. This spectrometer consisted of a large (25.4-cm diameter x 30.5-cm long) NaI(Tl) detector with a 20.3-cm deep axial well in which is placed a 300-mm2 x 1.0-mm Si detector. The spectra from the NaI(Tl) detector are collected both in the singles mode and in coincidence with the B-events detected in the Si detector. Ideally, this detector would sum all the energy of the B- rays in each cascade following the population of daughter level by B- decay, so that the event could be directly associated with a particular daughter level. However, there are losses of energy from attenuation of the rays before they reach the detector, transmission of rays through the detector, escape of secondary photons from Compton scattering, escape of rays through the detector well, internal conversion, etc., and the measured spectra are thus more complicated than the ideal case and the analysis is more complex. Analysis methods have been developed to simulate all of these processes and thus provide a direct measure of the B- intensity distribution as a function of the excitation energy in the daughter nucleus. These data yield more accurate information on the B- distribution than conventional decay-scheme studies for complex decay schemes with large decay energies, because in the latter there are generally many unobserved and observed but unplaced rays. The TAGS data have been analyzed and published [R. E. Greenwood et al., Nucl Instr. and metho. A390(1997)] for 40 fission product-nuclides to determine the B- intensity distributions. [Copied from the TAGS page at http://www.inl.gov/gammaray/spectrometry/tags.shtml]. Those values are listed on this page for quick reference.

  13. 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.

  14. Analysis of Electroblotted Proteins by Mass Spectrometry

    PubMed Central

    Luque-Garcia, Jose L.; Neubert, Thomas A.

    2015-01-01

    Summary Identification of proteins by mass spectrometry is crucial for better understanding of many biological, biochemical, and biomedical processes. Here we describe two methods for the identification of electroblotted proteins by on-membrane digestion prior to analysis by mass spectrometry. These on-membrane methods take approximately half the time of in-gel digestion and provide better digestion efficiency, due to the better accessibility of the protease to the proteins adsorbed onto the nitrocellulose, and better protein sequence coverage, especially for membrane proteins where large and hydrophobic peptides are commonly present. PMID:26139272

  15. Mass spectrometry for pectin structure analysis.

    PubMed

    Ralet, Marie-Christine; Lerouge, Patrice; Quéméner, Bernard

    2009-09-28

    Pectin are extremely complex biopolymers made up of different structural domains. Enzymatic degradation followed by purification and structural analysis of the degradation products proved to be efficient tools for the understanding of pectin fine structure, including covalent interactions between pectic structural domains or with other cell wall polysaccharides. Due to its high sensitivity, high throughput and capacity to analyze mixtures, mass spectrometry has gained more and more importance as a tool for oligosaccharides structural characterization in the past 10 years. This review will focus on the combined use of mass spectrometry and enzymatic digestion for pectins structural characterization. PMID:19058795

  16. 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.

  17. Determination of some trace elements in food and soil samples by atomic absorption spectrometry after coprecipitation with holmium hydroxide.

    PubMed

    Saracoglu, Sibel; Soylak, Mustafa; Cabuk, Dilek; Topalak, Zeynep; Karagozlu, Yasemin

    2012-01-01

    The determination of trace elements in food and soil samples by atomic absorption spectrometry was investigated. A coprecipitation procedure with holmium hydroxide was used for separation-preconcentration of trace elements. Trace amounts of copper(II), manganese(II), cobalt(II), nickel(ll), chromium(lll), iron(Ill), cadmium(ll), and lead(ll) ions were coprecipitated with holmium hydroxide in 2.0 M NaOH medium. The optimum conditions for the coprecipitation process were investigated for several commonly tested experimental parameters, such as amount of coprecipitant, effect of standing time, centrifugation rate and time, and sample volume. The precision, based on replicate analysis, was lower than 10% for the analytes. In order to verify the accuracy of the method, the certified reference materials BCR 141 R calcareous loam soil and CRM 025-050 soil were analyzed. The procedure was successfully applied for separation and preconcentration of the investigated ions in various food and soil samples. An amount of the solid samples was decomposed with 15 mL concentrated hydrochloric acid-concentrated nitric acid (3 + 1). The preconcentration procedure was then applied to the final solutions. The concentration of trace elements in samples was determined by atomic absorption spectrometry. PMID:22816279

  18. Determination of calcium, magnesium and strontium in soils by flow injection flame atomic absorption spectrometry.

    PubMed

    Arslan, Z; Tyson, J F

    1999-12-01

    Several procedures for the determination of Ca, Mg and Sr in soils have been compared on the basis of the accuracy of analysis of two NIST reference materials (Montana Soils SRM 2710 and SRM 2711). Samples were dissolved in a mixture of hydrofluoric and nitric acids in sealed vessels in a microwave oven and in teflon beakers on a hot plate. The digests obtained from both dissolution methods were evaporated to dryness in an attempt to remove silicon. Boric acid was added to prevent the precipitation of the lanthanum releasing agent (as lanthanum fluoride) and potassium was added as an ionization buffer. Determinations were made by flame atomic absorption spectrometry with both the nitrous oxide-acetylene flame and the air-acetylene flame, with calibration either by standard additions or against external standards matrix matched with respect to nitric acid, boric acid, lanthanum and potassium. The silicon remaining in the solution was also determined by external calibration. A single-line flow injection manifold was used to overcome any problems due to the presence of high dissolved solids. A volume of 300 mul was injected into a water carrier stream flowing at 8 ml min(-1). To determine Ca in the air-acetylene flame, it was necessary to remove silicon. Magnesium was determined in either flame without complete removal of the silicon, however, for the determination of Sr, it was necessary to remove the silicon and use the nitrous oxide-acetylene flame. The indicative value for Sr in SRM 2710 was too low: the value determined was 360+/-30 mug g(-1). PMID:18967785

  19. Direct determination of lead in sweet fruit-flavored powder drinks by electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Lima, Éder C.; Krug, Francisco José; Arruda, Marco A. Z.

    1998-04-01

    A simplified method for direct determination of lead in sweet fruit-flavored powder drinks, syrups and honeys by electrothermal atomic absorption spectrometry without sample digestion is proposed. Samples were dissolved in water, acidified to 0.2% (v/v) HNO 3, and directly injected into an end-capped transversely heated graphite atomizer (THGA). Building up of carbonaceous residue inside the atomizer was effectively precluded for sugar solutions not exceeding 8.0% (m/v) when a heating program with two pyrolysis steps (600 and 1000°C) was carried out without air-ashing. Under these conditions one atomizer supported about 250 firings. Among various chemical modifiers tested, better recovery and repeatability results were obtained with a 5 μg Pd + 3 μg Mg(NO 3) 2 mixture. Tests carried out with individual concomitants containing up to 1.0 μg Na, K, Ca or Cl, and up to 10.0 μg phosphate or sulphate, and several mixtures of these six concomitants, did not reveal significant interferences on lead atomization. Characteristic mass and detection limit based on integrated absorbance were 15 and 11 pg Pb, respectively. The relative standard deviation based on 10 measurements for typical samples (20-60 ng g -1 Pb) was always lower than 5.5%. The detection limit of 7.0 ng g -1 Pb attained the Codex recommendation for the maximum allowed lead contents in the sugar samples. Application of t-test to the results obtained by the proposed direct analysis, and the official method adopted by Food Chemical Codex, demonstrated that there were no significant differences at the 5% probability level.

  20. Determination of nanogram amounts of bismuth in rocks by atomic absorption spectrometry with electrothermal atomization

    USGS Publications Warehouse

    Kane, J.S.

    1979-01-01

    Bismuth concentrations as low as 10 ng g-1 in 100-mg samples of geological materials can be determined by atomic absorption spectrometry with electrothermal atomization. After HF-HClO4 decomposition of the sample, bismuth is extracted as the iodide into methyl isobutyl ketone and is then stripped with ethylenediaminetetraacetic acid into the aqueous phase. Aliquots of this solution are pipetted into the graphite furnace and dried, charred, and atomized in an automated sequence. Atomic absorbance at the Bi 223.1-nm line provides a measure of the amount of bismuth present. Results are presented for 14 U.S. Geological Survey standard rocks. ?? 1979.

  1. Gold analysis by the gamma absorption technique.

    PubMed

    Kurtoglu, Arzu; Tugrul, A Beril

    2003-01-01

    Gold (Au) analyses are generally performed using destructive techniques. In this study, the Gamma Absorption Technique has been employed for gold analysis. A series of different gold alloys of known gold content were analysed and a calibration curve was obtained. This curve was then used for the analysis of unknown samples. Gold analyses can be made non-destructively, easily and quickly by the gamma absorption technique. The mass attenuation coefficients of the alloys were measured around the K-shell absorption edge of Au. Theoretical mass attenuation coefficient values were obtained using the WinXCom program and comparison of the experimental results with the theoretical values showed generally good and acceptable agreement. PMID:12485656

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

    NASA Astrophysics Data System (ADS)

    Pasias, I. N.; Pappa, Ch.; Katsarou, V.; Τhomaidis, N. S.; Piperaki, E. A.

    2014-02-01

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

  3. Multielement continuum-source atomic-absorption spectrometry with an echelle-spectrometer/image-dissector system.

    PubMed

    Masters, R; Hsiech, C; Pardue, H L

    1989-01-01

    The continued development of the echelle-spectrometer/image-dissector system for multielement determination by continuum-source atomic-absorption spectrometry is presented. Modifications of the instruments include the use of a 20-groove/mm echelle grating blazed at 76 degrees , and the removal of the magnetic shield from the image dissector. The spectral range is from 300 to 430 nm and the observed resolution is better than 0.005 nm at 400 nm. Calibration curves are linear up to an absorbance of 0.2, and absorption sensitivities are up to 4-fold better than with the previous design. Fundamental characteristics of the detector limit the application of the instrument to sequential single-element quantifications with the electrothermal atomizer, and to sequential multielement quantification with the flame atomizer. The further development of the instrument for simultaneous multielement qualification is discussed. PMID:18964682

  4. Determination of selected elements in whole coal and in coal ash from the eight argonne premium coal samples by atomic absorption spectrometry, atomic emission spectrometry, and ion-selective electrode

    USGS Publications Warehouse

    Doughten, M.W.; Gillison, J.R.

    1990-01-01

    Methods for the determination of 24 elements in whole coal and coal ash by inductively coupled argon plasma-atomic emission spectrometry, flame, graphite furnace, and cold vapor atomic absorption spectrometry, and by ion-selective electrode are described. Coal ashes were analyzed in triplicate to determine the precision of the methods. Results of the analyses of NBS Standard Reference Materials 1633, 1633a, 1632a, and 1635 are reported. Accuracy of the methods is determined by comparison of the analysis of standard reference materials to their certified values as well as other values in the literature.

  5. Electrothermal atomization atomic absorption spectrometry for the determination of lead in urine: results of an interlaboratory study

    NASA Astrophysics Data System (ADS)

    Parsons, Patrick J.; Slavin, Walter

    1999-05-01

    Results of an interlaboratory study are reported for the determination of lead in urine. Two levels of a lyophilized material containing biologically-bound lead were prepared using pooled urine obtained from lead-poisoned children undergoing the CaNa 2EDTA mobilization test. The materials were circulated to a group of reference laboratories that participate in the `New York State Proficiency Testing Program for Blood Lead'. Results of the initial round-robin gave all-method consensus target values of 145±22 μg/l (S.D.) for lot 17 and 449±43 μg/l (S.D.) for lot 20. The interlaboratory exercise was repeated some 5 years later and consensus target values were re-calculated using the grand mean (excluding outliers) of results reported by laboratories using electrothermal atomization atomic absorption spectrometry (ETAAS). The re-calculated target values were 139±10 μg/l (S.D.) and 433±12 μg/l (S.D.). The urine reference materials were also analyzed for lead by several laboratories using other instrumental techniques including isotope dilution (ID), inductively coupled plasma (ICP) mass spectrometry (MS), flame atomic absorption with extraction, ICP-atomic emission spectrometry, ID-gas chromatography MS and flow injection-hydride generation AAS, thus providing a rich source of analytical data with which to characterize them. The materials were also used in a long-term validation study of an ETAAS method developed originally for blood lead determinations that has since been used unmodified for the determination of lead in urine also. Recently, urine lead method performance has been tracked in a proficiency testing program specifically for this analysis. In addition, a number of commercial control materials have been analyzed and evaluated.

  6. Determination of elements by atomic absorption spectrometry in medicinal plants employed to alleviate common cold symptoms.

    PubMed

    Küçükbay, F Zehra; Kuyumcu, Ebru

    2014-09-01

    Eleven important medicinal plants generally used by the people of Turkey for the treatment of common cold have been studied for their mineral contents. Eleven minor and major elements (essential, non-essential and toxic) were identified in the Asplenium adiantum-nigrum L. , Althaea officinalis L. , Verbascum phlomoides L., Euphorbia chamaesyce L., Zizyphus jujube Miller, Peganum harmala L., Arum dioscoridis Sm., Sambucus nigra L., Piperlongum L., Tussilago farfara L. and Elettaria cardamomum Maton by employing flame atomic absorption and emission spectrometry and electro-thermal atomic absorption spectrometry. Microwave digestion procedure for total concentration was applied under optimized conditions for dissolution of medicinal plants. Plant based biological certified reference materials (CRMs) served as standards for quantification. These elements are found to be present in varying concentrations in the studied plants. The baseline data presented in this work can be used in understanding the role of essential, non-essential and toxic elements in nutritive, preventive and therapeutic properties of medicinal plants. PMID:25532362

  7. [The application of atomic absorption spectrometry in automatic transmission fault detection].

    PubMed

    Chen, Li-dan; Chen, Kai-kao

    2012-01-01

    The authors studied the innovative applications of atomic absorption spectrometry in the automatic transmission fault detection. After the authors have determined Fe, Cu and Cr contents in the five groups of Audi A6 main metal in automatic transmission fluid whose travel course is respectively 10-15 thousand kilometers, 20-26 thousand kilometers, 32-38 thousand kilometers, 43-49 thousand kilometers, and 52-58 thousand kilometers by atomic absorption spectrometry, the authors founded the database of primary metal content in the Audi A6 different mileage automatic transmission fluid (ATF). The research discovered that the main metal content in the automatic transmission fluid increased with the vehicles mileage and its normal metal content level in the automatic transmission fluid is between the two trend lines. The authors determined the main metal content of automatic transmission fluid which had faulty symptoms and compared it with its database value. Those can not only judge the wear condition of the automatic transmission which had faulty symptoms but also help the automobile detection and maintenance personnel to diagnose automatic transmission failure reasons without disintegration. This reduced automobile maintenance costs, and improved the quality of automobile maintenance. PMID:22497168

  8. Alpha particle analysis using PEARLS spectrometry

    SciTech Connect

    McKlveen, J.W.; Klingler, G.W.; McDowell, W.J.; Case, G.N.

    1984-01-01

    Alpha particle assay by conventional plate-counting methods is difficult because chemical separation, tracer techniques, and/or self-absorption losses in the final sample may cause either non-reproducible results or create unacceptable errors. PEARLS (Photon-Electron Rejecting Alpha Liquid Scintillation) Spectrometry is an attractive alternative since radionuclides may be extracted into a scintillator in which there would be no self-absorption or geometry problems and in which up to 100% chemical recovery and counting efficiency is possible. Sample preparation may include extraction of the alpha emitter of interest by a specific organic-phase-soluble compound directly into the liquid scintillator. Detection electronics use energy and pulse-shape discrimination to provide discrete alpha spectra and virtual absence of beta and gamma backgrounds. Backgrounds on the order of 0.01 cpm are readily achievable. Accuracy and reproducibility are typically in the 100 +-1% range. Specific procedures have been developed for gross alpha, uranium, plutonium, thorium, and polonium assay. This paper will review liquid scintillation alpha counting methods and reference some of the specific applications. 8 refs., 1 fig.

  9. Impact of the analytical blank in the uncertainty evaluation of the copper content in waters by flame atomic absorption spectrometry.

    PubMed

    de Oliveira, Elcio Cruz; Monteiro, Maria Inês Couto; Pontes, Fernanda Veronesi Marinho; de Almeida, Marcelo Dominguez; Carneiro, Manuel Castro; da Silva, Lílian Irene Dias; Alcover Neto, Arnaldo

    2012-01-01

    Chemical analysts use analytical blanks in their analyses, but seldom is this source of uncertainty evaluated. Generally, there is great confusion. Although the numerical value of the blank, in some situations, can be negligible, its source of uncertainty cannot be. This article discusses the uncertainty contribution of the analytical blank using a numerical example of the copper content in waters by flame atomic absorption spectrometry. The results indicate that the uncertainties of the analytical blank can contribute up to 50% when the blank sample is considered in this analysis, confirming its high impact. This effect can be primarily observed where the analyte concentration approaches the lower range of the analytical curve. Even so, the blank is not always computed. Therefore, the relevance of the analytical blank can be confirmed by uncertainty evaluation. PMID:22649945

  10. 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. PMID:25078838

  11. 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.

  12. Rotary absorption heat pump sensitivity analysis

    NASA Astrophysics Data System (ADS)

    Bamberger, J. A.; Zalondek, F. R.

    1990-03-01

    Conserve Resources, Incorporated is currently developing an innovative, patented absorption heat pump. The heat pump uses rotation and thin film technology to enhance the absorption process and to provide a more efficient, compact system. The results are presented of a sensitivity analysis of the rotary absorption heat pump (RAHP) performance conducted to further the development of a 1-ton RAHP. The objective of the uncertainty analysis was to determine the sensitivity of RAHP steady state performance to uncertainties in design parameters. Prior to conducting the uncertainty analysis, a computer model was developed to describe the performance of the RAHP thermodynamic cycle. The RAHP performance is based on many interrelating factors, not all of which could be investigated during the sensitivity analysis. Confirmatory measurements of LiBr/H2O properties during absorber/generator operation will provide experimental verification that the system is operating as it was designed to operate. Quantities to be measured include: flow rate in the absorber and generator, film thickness, recirculation rate, and the effects of rotational speed on these parameters.

  13. Mass Spectrometry Methodology in Lipid Analysis

    PubMed Central

    Li, Lin; Han, Juanjuan; Wang, Zhenpeng; Liu, Jian’an; Wei, Jinchao; Xiong, Shaoxiang; Zhao, Zhenwen

    2014-01-01

    Lipidomics is an emerging field, where the structures, functions and dynamic changes of lipids in cells, tissues or body fluids are investigated. Due to the vital roles of lipids in human physiological and pathological processes, lipidomics is attracting more and more attentions. However, because of the diversity and complexity of lipids, lipid analysis is still full of challenges. The recent development of methods for lipid extraction and analysis and the combination with bioinformatics technology greatly push forward the study of lipidomics. Among them, mass spectrometry (MS) is the most important technology for lipid analysis. In this review, the methodology based on MS for lipid analysis was introduced. It is believed that along with the rapid development of MS and its further applications to lipid analysis, more functional lipids will be identified as biomarkers and therapeutic targets and for the study of the mechanisms of disease. PMID:24921707

  14. Determination of total mercury in human hair and animal fur by combustion atomic absorption spectrometry.

    PubMed

    Cizdziel, J V; Gerstenberger, Shawn

    2004-11-15

    A commercially available mercury (Hg) analyzer based on sample combustion, gold amalgamation, and atomic absorption spectrometry (AAS) was evaluated for the direct determination of Hg in composites of human hair and individual samples of horse fur. Results for human hair reference material (NIES No. 13) were within the certified range. Analyses of "blind" samples from an international interlaboratory (n>16) comparison study produced results within 1S.D. of the consensus means. Precision (%R.S.D.) was found to be <5% and total analyses time per sample was <10min. This study demonstrated that analyzers based on combustion-AAS are suitable for wide-scale monitoring of Hg in human hair and animal fur. PMID:18969690

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

    NASA Astrophysics Data System (ADS)

    Coufalík, Pavel; Zvěřina, Ondřej; Komárek, Josef

    2016-04-01

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

  16. Expressing self-absorption in the analytical function of inductively coupled plasma atomic emission spectrometry

    NASA Astrophysics Data System (ADS)

    Kántor, Tibor; Bartha, András

    2015-11-01

    The self-absorption of spectral lines was studied with up to date multi-element inductively coupled plasma atomic emission spectrometry (ICP-AES) instrumentation using radial and axial viewing of the plasma, as well, performing line peak height and line peak area measurements. Two resonance atomic and ionic lines of Cd and Mg were studied, the concentration range was extended up to 2000 mg/L. At the varying analyte concentration, constant matrix concentration of 10,000 mg/L Ca was ensured in the pneumatically nebulized solutions. The physical and the phenomenological formulation of the emission analytical function is overviewed and as the continuity of the earlier results the following equation is offered:

  17. Membrane composition analysis by imaging mass spectrometry

    SciTech Connect

    Boxer, S G; Kraft, M L; Longo, M; Hutcheon, I D; Weber, P K

    2006-03-29

    Membranes on solid supports offer an ideal format for imaging. Secondary ion mass spectrometry (SIMS) can be used to obtain composition information on membrane-associated components. Using the NanoSIMS50, images of composition variations in membrane domains can be obtained with a lateral resolution better than 100 nm. By suitable calibration, these variations in composition can be translated into a quantitative analysis of the membrane composition. Progress towards imaging small phase-separated lipid domains, membrane-associated proteins and natural biological membranes will be described.

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

    PubMed

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

    2004-12-01

    Tunable diode laser atomic absorption spectroscopy (DLAAS) combined with separation techniques and atomization in plasmas and flames is presented as a powerful method for analysis of molecular species. The analytical figures of merit of the technique are demonstrated by the measurement of Cr(VI) and Mn compounds, as well as molecular species including halogen atoms, hydrogen, carbon and sulfur. PMID:15561625

  19. Analysis of Glycosaminoglycans Using Mass Spectrometry

    PubMed Central

    Staples, Gregory O.; Zaia, Joseph

    2015-01-01

    The glycosaminoglycans (GAGs) are linear polysaccharides expressed on animal cell surfaces and in extracellular matrices. Their biosynthesis is under complex control and confers a domain structure that is essential to their ability to bind to protein partners. Key to understanding the functions of GAGs are methods to determine accurately and rapidly patterns of sulfation, acetylation and uronic acid epimerization that correlate with protein binding or other biological activities. Mass spectrometry (MS) is particularly suitable for the analysis of GAGs for biomedical purposes. Using modern ionization techniques it is possible to accurately determine molecular weights of GAG oligosaccharides and their distributions within a mixture. Methods for direct interfacing with liquid chromatography have been developed to permit online mass spectrometric analysis of GAGs. New tandem mass spectrometric methods for fine structure determination of GAGs are emerging. This review summarizes MS-based approaches for analysis of GAGs, including tissue extraction and chromatographic methods compatible with LC/MS and tandem MS. PMID:25705143

  20. 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. PMID:25938774

  1. Determination of ytterbium in animal faeces by tungsten coil electrothermal atomic absorption spectrometry.

    PubMed

    Lima, E C; Krug, F J; Nóbrega, J A; Nogueira, A R

    1998-11-01

    A method for ytterbium determination in animal faeces by tungsten coil electrothermal atomic absorption spectrometry (TCAAS) was developed. Faeces were dry-ashed in a muffle furnace, the ashes were treated with hydrochloric acid, and 10 mul of sample solution were delivered into 150-W tungsten coil atomizer. A matrix-matching procedure employing a 66-s heating program proved to be efficient for obtaining accurate results. Characteristic mass and detection limit were 7.1 pg and 0.35 mug g(-1) Yb, respectively. The tungsten coil atomizer lifetime exceeded 300 firings with digested solutions and R.S.D. of measurements was 1.9% after ten consecutive injections of 10.0 mug l(-1) Yb. Accuracy of the proposed method was assessed by employing a graphite furnace atomic absorption spectrometric procedure. Application of the paired t-test did not reveal any significant difference for ytterbium contents determined by both methods at 95% confidence level. It was demonstrated that the proposed procedure can successfully be used for evaluation of kinetic passage rate of feed through digestive tract of animals. PMID:18967363

  2. Antibiotic Toxicity and Absorption in Zebrafish Using Liquid Chromatography-Tandem Mass Spectrometry

    PubMed Central

    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. PMID:25938774

  3. Determination of sulfur in coal and ash slurry by high-resolution continuum source electrothermal molecular absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Nakadi, Flávio V.; Rosa, Lilian R.; da Veiga, Márcia A. M. S.

    2013-10-01

    We propose a procedure for the determination of sulfur in coal slurries by high resolution continuum source electrothermal molecular absorption spectrometry. The slurry, whose concentration is 1 mg mL- 1, was prepared by mixing 50 mg of the sample with 5% v/v nitric acid and 0.04% m/v Triton X-100 and was homogenized manually. It sustained good stability. The determination was performed via CS molecular absorption at 257.592 nm, and the optimized vaporization temperature was 2500 °C. The accuracy of the method was ensured by analysis of certified reference materials SRM 1632b (trace elements in coal) and SRM 1633b (coal fly ash) from the National Institute of Standards and Technology, using external calibration with aqueous standards prepared in the same medium and used as slurry. We achieved good agreement with the certified reference materials within 95% confidence interval, LOD of 0.01% w/w, and RSD of 6%, which confirms the potential of the proposed method.

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

    NASA Astrophysics Data System (ADS)

    Hashemi, Payman; Rahimi, Akram

    2007-04-01

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

  5. SPECIATION OF SELENIUM(IV) AND SELENIUM(VI) USING COUPLED ION CHROMATOGRAPHY: HYDRIDE GENERATION ATOMIC ABSORPTION SPECTROMETRY

    Technology Transfer Automated Retrieval System (TEKTRAN)

    A simple method was developed to speciate inorganic selenium in the microgram per liter range using coupled ion chromatography-hydride generation atomic absorption spectrometry. Because of the differences in toxicity and adsorption behavior, determination of the redox states selenite, Se(IV), and s...

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

    PubMed

    Bücker, Stefan; Acker, Jörg

    2012-05-30

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

  7. Determination of Hg, Cd, Mn, Pb and Sn in seafood by solid sampling Zeeman atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Detcheva, A.; Grobecker, K. H.

    2006-04-01

    Direct solid sampling Zeeman atomic absorption spectrometric methods were developed and applied to the determination of mercury, cadmium, manganese, lead and tin in seafood. All elements but mercury were measured by a third generation Zeeman atomic absorption spectrometry combined with an automatic solid sampler. In 3-field- and dynamic mode the calibrations concentration range was substantially extended and high amounts of analyte were detectable without laborious dilution of solid samples. The measurements were based on calibrations using certified reference materials of organic matrices. In case solid certified reference materials were not available calibration by aqueous standard solutions was proved to be an alternative. No matrix effects were observed under the optimized conditions. Results obtained were in good agreement with the certified values. Solid sampling Zeeman atomic absorption spectrometry proved to be a reliable, rapid and low-cost method for the control of trace elements in seafood.

  8. Crux: rapid open source protein tandem mass spectrometry analysis.

    PubMed

    McIlwain, Sean; Tamura, Kaipo; Kertesz-Farkas, Attila; Grant, Charles E; Diament, Benjamin; Frewen, Barbara; Howbert, J Jeffry; Hoopmann, Michael R; Käll, Lukas; Eng, Jimmy K; MacCoss, Michael J; Noble, William Stafford

    2014-10-01

    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

  9. Direct determination of selenium in rat blood plasma by Zeeman atomic absorption spectrometry.

    PubMed

    Kabirov, K K; Kapetanovic, I M; Lyubimov, A V

    2008-01-30

    The method was developed to be applied for direct determination of selenium in rat plasma by graphite-furnace atomic absorption spectrometry with Zeeman background correction. Blood was obtained from CD rats of both sexes 2h after dosing in weeks 7 and 13 in order to acquire data on the levels of selenium in these animals during 13-week gavage administration of l-seleno-methylselenocysteine (SeMC), a new candidate chemopreventive agent under development. Application of the commonly used method of standard addition was found to be unsuitable to calculate the selenium content in rat plasma (within-run and between-run accuracy and precision parameters were less than 85%). Therefore, a new analytical method was developed. In this method, samples of rat plasma (50 microL) were diluted 10-fold with a reducing agent containing l-ascorbic acid, a modifier solution containing palladium chloride and Triton X-100. Samples were atomized in pyrolytically coated graphite tubes and peak height signals were measured. Selenium concentrations were determined by linear least squares regression analysis based on the standard curve generated in pooled rat blank plasma. Since selenium is normally present in plasma, a three-step approach was used to calculate selenium plasma levels. Initially selenium levels were determined based on the standard curve with selenium-spiked pool plasma. In the second step, background selenium levels in the pooled plasma were determined based on the same standard curve. In the third step, background level was added to the previously derived number. The relative errors were in the range from -4.6 to 11.4% (intra-day assay) and from -0.4 to 8.8% (inter-day assay) which proved good accuracy. The relative standard deviations were in the range from 1.88 to 4.70% (intra-day precision) and from 3.28 to 5.38% (inter-day precision). In rat plasma, the following dose-dependent selenium levels (mean+/-S.D.) in males and females, respectively, were observed at 13 weeks

  10. Arsenic in marine tissues — The challenging problems to electrothermal and hydride generation atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Karadjova, Irina B.; Petrov, Panayot K.; Serafimovski, Ivan; Stafilov, Trajče; Tsalev, Dimiter L.

    2007-03-01

    Analytical problems in determination of arsenic in marine tissues are addressed. Procedures for the determination of total As in solubilized or extracted tissues with tetramethylammonium hydroxide and methanol have been elaborated. Several typical lyophilized tissues were used: NIST SRM 1566a 'Oyster Tissue', BCR-60 CRM 'Trace Elements in an Aquatic Plant ( Lagarosiphon major)', BCR-627 'Forms of As in Tuna Fish Tissue', IAEA-140/TM 'Sea Plant Homogenate', NRCC DOLT-1 'Dogfish Liver' and two representatives of the Black Sea biota, Mediterranean mussel ( Mytilus galloprovincialis) and Brown algae ( Cystoseira barbata). Tissues (nominal 0.3 g) were extracted in tetramethylammonium hydroxide (TMAH) 1 ml of 25% m/v TMAH and 2 ml of water) or 5 ml of aqueous 80% v/v methanol (MeOH) in closed vessels in a microwave oven at 50 °C for 30 min. Arsenic in solubilized or extracted tissues was determined by electrothermal atomic absorption spectrometry (ETAAS) after appropriate dilution (nominally to 25 ml, with further dilution as required) under optimal instrumental parameters (pyrolysis temperature 900 °C and atomization temperature 2100 °C) with 1.5 μg Pd as modifier on Zr-Ir treated platform. Platforms have been pre-treated with 2.7 μmol of zirconium and then with 0.10 μmol of iridium which served as a permanent chemical modifier in direct ETAAS measurements and as an efficient hydride sequestration medium in flow injection hydride generation (FI-HG)-ETAAS. TMAH and methanol extract 96-108% and 51-100% of As from CRMs. Various calibration approaches have been considered and critically evaluated. The effect of species-dependent slope of calibration graph or standard additions plot for total As determination in a sample comprising of several individual As species with different ETAAS behavior has been considered as a kind of 'intrinsic element speciation interference' that cannot be completely overcome by standard additions technique. Calibration by means of CRMs has

  11. [Determination of nine mineral elements in hulless barley by ultraviolet spectrophotometry and flame atomic absorption spectrometry].

    PubMed

    Liu, Jin; Zhang, Huai-Gang

    2010-04-01

    The contents of nine mineral elements, including sulphur, zinc, calcium, magnesium, potassium, sodium, iron, copper and manganese in five hulless barley (Hordeum vulgare L. var. nudum Hook. f.) lines were determined by ultraviolet spectrophotometry and flames atomic absorption spectrometry (FAAS). For the determination of sulphur, the samples were dissolved by magnesia and anhydrous sodium carbonate at 250 degrees C for 0. 5 h and at 550 degrees C for 3 h in the muffle furnace, and then a certain amount of barium chloride was put into the sample solution for colorimetry of the UV-Vs spectrophotometer. For the determination of other eight mineral elements, all of the samples were dissolved by a kind of incinerating method: first, the sample was put into the muffle furnace at 250 degrees C for 0. 5 h and at 550 degrees C for 2.5 h, then two droplets of 50%HNO3 were distributed into each sample, and the last step was putting the sample into the muffle furnace at 550 degrees C for 0.5 h. And then all of the ash was dissolved by 50%HNO3 to 50 milliliter and determined by flames atomic absorption spectrometry. The precision, accuracy, repeatability and stability of the method were discussed too. The results showed that the relative standard deviations (RSD) were between 1.2% and 3.7%; The average recoveries were 97.44%-101.52% and the relative standard deviations (RSD) of sample determination were 1.3%-3.8%. The repeatability experiment showed that the relative standard deviations (RSD) were 2.6%-6.1%. And the content of each mineral element was the same after 24 hours; All these showed that the method has a good precision, accuracy, repeatability and stability. In all the hulless barley samples, the average contents were in the order of K > S > Mg > Ca > Fe > Na > Zn > Mn > Cu, and the contents of zinc, iron and manganese closely related to people's health were relatively higher than other crops. The data of the experiment could provide an accurate and credible evidence

  12. In situ secondary ion mass spectrometry analysis

    SciTech Connect

    Groenewold, G.S.; Applehans, A.D.; Ingram, J.C.; Delmore, J.E.; Dahl, D.A.

    1993-01-01

    The direct detection of tributyl phosphate (TBP) on rocks using molecular beam surface analysis [MBSA or in situ secondary ion mass spectrometry (SIMS)] is demonstrated. Quantities as low as 250 ng were detected on basalt and sandstone with little or no sample preparation. Detection of TBP on soil has proven to be more problematic and requires further study. Ethylenediaminetetraacetic acid (EDTA) is more difficult to detect because it is very reactive with surfaces of interest. Nevertheless, it is possible to detect EDTA if the acidity of the surface is controlled. The detection of EDTA-metal complexes is currently an open question, but evidence is presented for the detection of ions arising from a EDTA-lead complex. Carboxylic acids (i.e., citric, ascorbic, malic, succinic, malonic, and oxalic) give characteristic SIM spectra, but their detection on sample surfaces awaits evaluation.

  13. Biological particle analysis by mass spectrometry

    NASA Technical Reports Server (NTRS)

    Vilker, V. L.; Platz, R. M.

    1983-01-01

    An instrument that analyzes the chemical composition of biological particles in aerosol or hydrosol form was developed. Efforts were directed toward the acquisition of mass spectra from aerosols of biomolecules and bacteria. The filament ion source was installed on the particle analysis by mass spectrometry system. Modifications of the vacuum system improved the sensitivity of the mass spectrometer. After the modifications were incorporated, detailed mass spectra of simple compounds from the three major classes of biomolecules, proteins, nucleic acids, and carbohydrates were obtained. A method of generating bacterial aerosols was developed. The aerosols generated were collected and examined in the scanning electron microscope to insure that the bacteria delivered to the mass spectrometer were intact and free from debris.

  14. Process analysis using ion mobility spectrometry.

    PubMed

    Baumbach, J I

    2006-03-01

    Ion mobility spectrometry, originally used to detect chemical warfare agents, explosives and illegal drugs, is now frequently applied in the field of process analytics. The method combines both high sensitivity (detection limits down to the ng to pg per liter and ppb(v)/ppt(v) ranges) and relatively low technical expenditure with a high-speed data acquisition. In this paper, the working principles of IMS are summarized with respect to the advantages and disadvantages of the technique. Different ionization techniques, sample introduction methods and preseparation methods are considered. Proven applications of different types of ion mobility spectrometer (IMS) used at ISAS will be discussed in detail: monitoring of gas insulated substations, contamination in water, odoration of natural gas, human breath composition and metabolites of bacteria. The example applications discussed relate to purity (gas insulated substations), ecology (contamination of water resources), plants and person safety (odoration of natural gas), food quality control (molds and bacteria) and human health (breath analysis). PMID:16132133

  15. Determination of mercury in gasoline by cold vapor atomic absorption spectrometry with direct reduction in microemulsion media

    NASA Astrophysics Data System (ADS)

    Brandão, Geisamanda Pedrini; de Campos, Reinaldo Calixto; Luna, Aderval Severino

    2005-06-01

    The determination of Hg in gasoline by cold vapor atomic absorption spectrometry, after direct aqueous NaBH 4 reduction in a three-component (microemulsion) medium, was investigated. Microemulsions were prepared by mixing gasoline with propan-1-ol and 50% v / v HNO 3 at a 20 : 15 : 1 volume ratio. A long-term homogeneous system was immediately formed this way. After reduction, the Hg vapor generated in a reaction flask was transported to an intermediate K 2Cr 2O 7/H 2SO 4 trap solution in order to avoid poisoning of the Au-Pt trap by the gasoline vapors. A second reduction step was then conducted and the generated Hg vapor transported to the Au-Pt trap, followed by thermal release of Hg 0 and atomic absorption measurement. Purified N 2 was used as purge and transport gas. After multivariate optimization by central composite design calibration graphs showed coefficients of correlation of 0.9999 and a characteristic mass of 2 ng was obtained. Typical coefficients of variation of 5% and 6% were found for ten consecutive measurements at concentration levels of 1 and 8 μg L -1 of Hg 2+, respectively. The limit of detection was 0.10 μg L -1 (0.14 μg kg -1) in the original sample. A total measurement cycle took 11 min, permitting duplicate analysis of 3 samples per hour. The results obtained with the proposed procedure in the analysis of commercial gasoline samples were in agreement with those obtained by a comparative procedure. Gasoline samples of the Rio de Janeiro city have shown Hg concentrations below 0.27 μg L -1.

  16. Evaluation of electrochemical generation of volatile zinc hydride by heated quartz tube atomizer atomic absorption spectrometry.

    PubMed

    Arbab-Zavar, Mohammad-Hossein; Chamsaz, Mahmoud; Youssefi, Abbas; Aliakbari, Mostafa

    2012-01-01

    Electrochemical hydride generation (EcHG) as a sample introduction system for determination of zinc was developed. It was directly coupled to an electrically heated quartz tube atomizer (QTA) atomic absorption spectrometry (AAS) system. The hydride generator is a laboratory-made semi-batch electrolytic cell that consists of a lead-tin alloy cathode and a platinum anode. The effects of typical parameters on the generation efficiency of the technique, such as types of cathode material and catholyte and anolyte solutions, were studied. The influences of numerical experimental operating parameters on the analytical signal were evaluated in detail and optimum conditions were obtained. The analytical figures of merit for the developed method were determined. The calibration curve was linear up to 300 ng mL(-1) of Zn. A concentration detection limit (3σ, n = 9) of 11 ng mL(-1) Zn and a relative standard deviation of 5.0% (RSD, n = 9) for 200 ng mL(-1) Zn were accessed. In addition, the susceptibility of interference from various ions was evaluated. The accuracy of the method was verified by determination of Zn in a certified reference material and in tap water. The achieved concentrations were found to be in good agreement with both the certified value and the data obtained using flame AAS. PMID:22790376

  17. Determination of silicon in serum and urine by electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Huang, Zhuo-er

    1995-09-01

    A sensitive, simple and accurate method for the routine determination of trace silicon in serum and urine by Zeeman electrothermal atomic absorption spectrometry is described. The samples are directly determined after 20-fold dilution of serum and 100-fold dilution of urine. No L'vov platform is used. The signal enhancement of silicon atomization in pyrolytic graphite coated graphite tubes is achieved by using a mixture of calcium chloride and lanthanum nitrate as chemical modifier. The interferences arising from the biological matrices have been eliminated by the addition of ammonium dihydrogenphosphate in the sample solutions. The aqueous calibration curve is linear to at least 300 μg l -1, the characteristic mass is 37 pg (integrated absorbance signal), whereas the detection limit (3SD) is 1.5 μg l -1 for silicon in both diluted serum and urine samples. The recoveries of silicon added to the diluted samples are 101 ± 1.8% for sera and 98.2 ± 3.5% for the urine specimens, independent of the dilution ratio. The silicon measurement results for the serum and urine from healthy adults and for the serum from the patients with chronic renal failure on hemodialysis are presented.

  18. Investigation on binding of nitric oxide to horseradish peroxidase by absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Qiang, Li; Zhu, Shuhua; Ma, Hongmei; Zhou, Jie

    2010-01-01

    Binding of nitric oxide to horseradish peroxidase (HRP) has been investigated by absorption spectrometry in 0.2 M anaerobic phosphate buffer solution (pH 7.4). Based on this binding equilibrium, a model equation for evaluating the binding constant of nitric oxide to HRP is developed and the binding constant is calculated to be (1.55 ± 0.06) × 10 4 M -1, indicating that HRP can form a stable complex with nitric oxide. The type of inhibition by nitric oxide is validated on the basis of studying initial reaction rates of HRP-catalyzed oxidation of guaiacol in the presence of hydrogen peroxide and nitric oxide. The inhibition mechanism is found to follow an apparent non-competitive inhibition by Lineweaver-Burk method. Based on this kinetic mechanism, the binding constant is also calculated to be (5.22 ± 0.06) × 10 4 M -1. The values of the binding constant determined by the two methods are almost identical. The non-competitive inhibition model is also applicable to studying the effect of nitric oxide on other metalloenzymes, which catalyze the two-substrate reaction with the "ping-pong" mechanism.

  19. Determination of arsenic in a nickel alloy by flow injection hydride generation atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Hanna, C. P.; Tyson, J. F.; Offley, S. G.

    1992-08-01

    The development of a method for the direct determination of trace arsenic quantities in nickel alloy digests, by flow injection hydride generation atomic absorption spectrometry, is described. An optimization study of the manifold and chemical parameters produced system performance, in terms of tolerance of the nickel matrix and sensitivity, such that matrix removal and pre-reduction of As(V) to As (III) prior to arsine generation were eliminated. Full recovery of the As(V) signal from a solution containing 5 ng ml -1 in the presence of 60 μg ml -1 nickel was obtained. Validation of the method was achieved by analyzing a British Chemical Standard (BCS) Certified Reference Material (CRM) #346 IN nickel alloy containing arsenic at a concentration of 50 μg g -1. Following dissolution in nitric and hydrofluoric acids by a microwave assisted procedure, the only subsequent preparation required was dilution by the appropriate factor. Up to 60 injections h -1 may be made, with a detection limit of 0.5 ng ml -1 arsenic (250 pg absolute) as As(V) in a 500 μl sample. The peak height characteristic concentration is 0.46 ng ml -1, with a relative standard deviation of 3.5% for a 10 ng ml -1 As(V) standard ( n = 6).

  20. Modular L-design of hydride atomizers for atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Řezáčová, Olga; Dědina, Jiří

    2009-07-01

    A novel modular L-shaped design of hydride atomizer for atomic absorption spectrometry is described. It makes it possible to replace the optical tube of the atomizer and, mainly, to employ optical tubes made also from other materials than fused quartz. The design is useful mainly for further improvement of hydride atomizers based on the multiatomizer concept. Employing selenium hydride as the analyte and arsine as the interferent, a preliminary evaluation of performance of three types of L-shaped multiatomizers based on various optical tubes in terms of sensitivity, linearity of calibration graph and resistance to atomization interferences is made. The "classical" T-shaped multiatomizer was employed as a reference. The L-shaped multiatomizer with the optical tube analogous to that employed in the "classical" T-shaped multiatomizer offers virtually the same performance as the reference multiatomizer. Optical tube made of fused quartz with holes with smaller diameters does not offer significantly better performance compared to the reference T-shaped multiatomizer. However, the L-shaped multiatomizer with optical tube fabricated from porous quartz glass overpowers all the other multiatomizers substantially in terms of the resistance against interferences: even the maximum As interferent concentration of 5 µg ml - 1 does not significantly influence the observed signal. This should be compared with multiatomizers based on plain fused quartz tubes with holes: tolerance limit around 0.5 µg ml - 1 ; interferent concentration of 1 µg ml - 1 causing 20% signal depression.

  1. Acid effects on the measurement of mercury by cold vapor atomic absorption spectrometry

    SciTech Connect

    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 or 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.

  2. Determination of gold in geological materials by carbon slurry sampling graphite furnace atomic absorption spectrometry.

    PubMed

    Dobrowolski, Ryszard; Kuryło, Michał; Otto, Magdalena; Mróz, Agnieszka

    2012-09-15

    A simple and cost effective preconcentration method on modified activated carbons is described for the determination of traces of gold (Au) in geological samples by carbon slurry sampling graphite furnace atomic absorption spectrometry (GFAAS). The basic parameters affecting the adsorption capacity of Au(III) ions on modified activated carbons were studied in detail and the effect of activated carbons modification has been determined by studying the initial runs of adsorption isotherms. The influence of chlorides and nitrates on adsorption ability of Au(III) ions onto the modified activated carbons for diluted aqueous solution was also studied in detail in respect to the determination of gold in solid materials after digestion steps in the analytical procedure, which usually involves the application of aqua regia. SEM-EDX and XPS studies confirmed that the surface reduction of Au(III) ions to Au(0) is the main gold adsorption mechanism on the activated carbon. Determination of gold after its preconcentration on the modified activated carbon was validated by applying certified reference materials. The experimental results are in good agreement with the certified values. The proposed method has been successfully applied for the determination of Au in real samples using aqueous standards. PMID:22967620

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

    NASA Astrophysics Data System (ADS)

    Karadjova, Irina B.; Lampugnani, Leonardo; Dědina, Jiri; D'Ulivo, Alessandro; Onor, Massimo; Tsalev, Dimiter L.

    2006-05-01

    Interference effects of various organic solvents miscible with water on arsenic determination by hydride generation atomic absorption spectrometry have been studied. Arsine was chemically generated in continuous flow hydride generation system and atomized by using a flame atomizer able to operate in two modes: miniature diffusion flame and flame-in-flame. The effects of experimental variables and atomization mode were investigated: tetrahydroborate and hydrochloric acid concentrations, argon, hydrogen and oxygen supply rates for the microflame, and the distance from the atomization region to the observation zone. The nature of the species formed in the flame due to the pyrolysis of organic solvent vapors entering the flame volume together with arsine is discussed. The observed signal depression in the presence of organic solvents has been mainly attributed to the atomization interference due to heterogeneous gas-solid reaction between the free arsenic atoms and finely dispersed carbon particles formed by carbon radicals recombination. The best tolerance to interferences was obtained by using flame-in-flame atomization (5-10 ml min - 1 of oxygen flow rate), together with higher argon and hydrogen supply rates and elevated observation heights.

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

    PubMed

    Saber-Tehrani, Mohammad; Hashemi-Moghaddam, Hamid; Givianrad, Mohammad Hadi; Abroomand-Azar, Parviz

    2006-11-01

    An efficient and sensitive method for the determination of methylmercury in biological samples was developed based on acid leaching extraction of methylmercury into toluene. Methylmercury in the organic phase was determined by electrothermal atomic absorption spectrometry (ETAAS). The methylmercury signal was enhanced and the reproducibility increased by formation of certain complexes and addition of Pd-DDC modifier. The complex of methylmercury with DDC produced the optimum analytical signal in terms of sensitivity and reproducibility compared to complexes with dithizone, cysteine, 1,10-phenanthroline, and diethyldithiocarbamate. Method performance was optimized by modifying parameters such as temperature of mineralization, atomization, and gas flow rate. The limit of detection for methylmercury determination was 0.015 mug g(-1) and the RSD of the whole procedure was 12% for human teeth samples (n=5) and 15.8% for hair samples (n=5). The method's accuracy was investigated by using NIES-13 and by spiking the samples with different amounts of methylmercury. The results were in good agreement with the certified values and the recoveries were 88-95%. PMID:16896613

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

    PubMed Central

    Zelinková, Hana; Červenka, Rostislav; Komárek, Josef

    2012-01-01

    Tetramethylene dithiocarbamate (TMDTC), diethyldithiocarbamate (DEDTC), and thiourea were investigated as stabilizing agents for calibration purposes in the determination of mercury using solid sampling electrothermal atomic absorption spectrometry (SS-ETAAS). These agents were used for complexation of mercury in calibration solutions and its thermal stabilization in a solid sampling platform. The calibration solutions had the form of methyl isobutyl ketone (MIBK) extracts or MIBK-methanol solutions with the TMDTC and DEDTC chelates and aqueous solutions with thiourea complexes. The best results were obtained for MIBK-methanol solutions in the presence of 2.5 g L−1 TMDTC. The surface of graphite platforms for solid sampling was modified with palladium or rhenium by using electrodeposition from a drop of solutions. The Re modifier is preferable due to a higher lifetime of platform coating. A new SS-ETAAS procedure using the direct sampling of solid samples into a platform with an Re modified graphite surface and the calibration against MIBK-methanol solutions in the presence of TMDTC is proposed for the determination of mercury content in solid environmental samples, such as soil and plants. PMID:22654606

  6. Direct determination of Cd, Pb and Cr in honey by slurry sampling electrothermal atomic absorption spectrometry.

    PubMed

    de Andrade, Camila Kulek; dos Anjos, Vanessa Egéa; Felsner, Maria Lurdes; Torres, Yohandra Reyes; Quináia, Sueli Pércio

    2014-03-01

    Slurry sampling electrothermal atomic absorption spectrometry was used for direct determination of Cr, Pb and Cd in honey without sample pretreatment. The honey slurries were prepared in aqueous solution containing hydrogen peroxide and nitric acid. The slurries were directly introduced in the pyrolytic graphite tubes. Pd-Mg was used as a chemical modifier only for Cd determination. Analytical curves were performed with aqueous standards for Pb and Cr and with addition of fructose for Cd. The quantification limits for Cd, Pb and Cr were 2.0, 5.4 and 9.4ngg(-1), respectively. Acceptable precision of the methodology was obtained through repeatability and intermediate precision. In the accuracy study, recoveries were satisfactory (94-101%) for the three elements. The methodology was applied in honey from Paraná (Brazil). The concentrations of Pb, Cd and Cr ranged from 141 to 228ngg(-1), <2.0 to 8ngg(-1) and 83 to 94ngg(-1), respectively. PMID:24176328

  7. Stabilizing agents for calibration in the determination of mercury using solid sampling electrothermal atomic absorption spectrometry.

    PubMed

    Zelinková, Hana; Červenka, Rostislav; Komárek, Josef

    2012-01-01

    Tetramethylene dithiocarbamate (TMDTC), diethyldithiocarbamate (DEDTC), and thiourea were investigated as stabilizing agents for calibration purposes in the determination of mercury using solid sampling electrothermal atomic absorption spectrometry (SS-ETAAS). These agents were used for complexation of mercury in calibration solutions and its thermal stabilization in a solid sampling platform. The calibration solutions had the form of methyl isobutyl ketone (MIBK) extracts or MIBK-methanol solutions with the TMDTC and DEDTC chelates and aqueous solutions with thiourea complexes. The best results were obtained for MIBK-methanol solutions in the presence of 2.5 g L(-1) TMDTC. The surface of graphite platforms for solid sampling was modified with palladium or rhenium by using electrodeposition from a drop of solutions. The Re modifier is preferable due to a higher lifetime of platform coating. A new SS-ETAAS procedure using the direct sampling of solid samples into a platform with an Re modified graphite surface and the calibration against MIBK-methanol solutions in the presence of TMDTC is proposed for the determination of mercury content in solid environmental samples, such as soil and plants. PMID:22654606

  8. Determination of rhodium: Since the origins until today Atomic absorption spectrometry.

    PubMed

    Bosch Ojeda, C; Sánchez Rojas, F

    2006-02-28

    Rhodium is present at about 0.001ppm in the earths crust. Rhodium metal is known for its stability in corrosive environments, physical beauty and unique physical and chemical properties. Recent interest in the medical and industrial significance of platinum and to a lesser extent palladium and rhodium has been accompanied by an increasing interest in their determination at low levels. Platinum group elements (PGEs: Pt, Pd, Rh, Ru, Ir and Os) play a decisive role in the performance of catalytic converters, world-wide applied in vehicles and in some household utensils, to reduce the emission of gaseous pollutants, such as carbon monoxide, nitrogen oxides and hydrocarbons. Since then, approximately 73% of the world production of rhodium is consumed in the production of autocatalyst. However, the hot exhaust gases flowing through the converter cause abrasion of these units, leading to the emission of these elements to the environment. The concentration level of rhodium (also platinum and palladium) is still very low in the nature; accordingly, their determination in environmental samples specially appears to be a challenging task for analytical chemists. In recent years, the development of analytical methods for the determination of rhodium has increased. The aim of the present review is to evaluate the utility of atomic absorption spectrometry, applied for the quantification of rhodium in different materials, such as environmental, biological, metallurgical and geological samples. PMID:18970480

  9. Use of atomic absorption spectrometry in assessment of biomonitor plants for lead, cadmium and copper pollution.

    PubMed

    Gokce, Kaya; Mehmet, Yaman

    2012-01-01

    Eleven plant species were collected from the vicinity of lead-battery plant in the city of Gaziantep, Turkey. Lead, cadmium and copper concentrations in the soil and leaves of plants were determined by atomic absorption spectrometry. Lead, Cd and Cu concentrations in the soil samples taken from battery area were found to be in the ranges of 304-602, 0.4-0.44 and 31-37 mg x kg(-1), respectively. Significantly increased lead concentration up to 2 750 mg x kg(-1) was found in the leaves of Eleagnus angustifolia L. plant. The lead concentrations in the other plant leaves taken from 50 m around battery factory followed the order Ailanthus altissima > Morus sp. > Juglans regia L. > Ficus carica L. > Cydonia oblonga Miller > Prunus x domestica L. The plants, Populus nigra L. , Eleagnus angustifolia L. and Salix sp. were found useful for Cd, and the plant, Eleagnus angusti folia L. for Pb, to be considered as potential biomonitor. Especially, leaves of trees and plants taken from the distance of 50 m from battery plant have relatively higher Pb concentrations. Therefore, people who and animals which live in this area and benefit from these soil and plants have vital risks. PMID:22497165

  10. 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.

  11. Evaluation of metal contents of household detergent samples from Turkey by flame atomic absorption spectrometry.

    PubMed

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

    2013-11-01

    The concentrations of cadmium, copper, chromium, cobalt, iron, lead, manganese, nickel, and zinc in detergent samples from Kayseri, Turkey were determined by flame atomic absorption spectrometry. HClO₄ (10 mL)/HNO₃ (10 mL) mixture was used for the digestion of household detergent samples. The correctness of the analytical procedures was checked with standard addition-recovery tests in different detergent samples for the investigated metal ions. The concentration ranges of the elements in the detergent samples were found as 17.2-60.1, 11.1-40.1, 2.5-32.3, 8.1-10.5, 7.2-21.6, 9.8-17.9, 1.7-3.8, 12.5-22.5, and 2.0-5.8 μg/g for iron, manganese, zinc, copper, lead, cobalt, cadmium, nickel, and chromium, respectively. The values found in this work were compared with some other studies around the world conducted on detergent samples. PMID:23722641

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

    PubMed

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

    2010-03-01

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

  13. Evaluation of four sample treatments for determination of platinum in automotive catalytic converters by graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Puig, Ana I.; Alvarado, José I.

    2006-09-01

    Conventional and microwave assisted digestion, both using aqua regia, alkaline fusion with lithium metaborate and aqueous slurries were evaluated as sample treatments for determination of Pt in automotive catalytic converters by Graphite Furnace Atomic Absorption Spectrometry (GF-AAS). Determination of platinum by GF-AAS in samples of the catalytic converter's substrates, prepared by the four methods described, indicates that the highest platinum concentration i.e. maximum Pt extraction in the range of 748 ± 15-998 ± 10 μg mL - 1 , is obtained for samples dissolved by alkaline fusion, closely followed by analysis of aqueous plus Triton X-100 slurries 708 ± 14-958 ± 10 μg mL - 1 , while neither one of the acid digestion procedures achieved total dissolution of the samples. Slurry analysis is thus shown to be a viable alternative and is recommended, based on its speed and ease of implementation. Aqueous standards calibration curves and the standard addition methods were also compared. The results showed that no appreciable matrix effects are present, regardless of the sample preparation procedure used. Precision of the measurements, expressed as percentage relative standard deviation, ranged between 2.5 to 4.9%. Accuracy of the results was assessed by recovery tests which rendered values between 98.9 and 100.9%.

  14. Cloud point extraction and flame atomic absorption spectrometry determination of lead (II) in environmental and food samples.

    PubMed

    Soylak, Mustafa; Yilmaz, Erkan; Ghaedi, Mehrorang; Montazerozohori, Mortaza; Sheibani, Marjan

    2012-01-01

    A cloud point extraction procedure for the preconcentration of Pb2+ in various samples following complexation with 2,2'-(1E,1'E)-1,1'-(2,2'-azanediylbis(ethane-2,1-diyl)bis(azan-1-yl-1-ylidene)) bis(ethan-1-yl-1-ylidene)diphenol in Triton X-114 after centrifugation is reported. A 0.5 mL portion of methanol acidified with 1.0 M HNO3 was added to the surfactant-rich phase prior to analysis by flame atomic absorption spectrometry. The influence of analytical parameters--including pH, concentrations of ligand, Triton X-114, and HNO3, bath temperature, heating time, and centrifugation rate and time--were optimized, and the effect of the matrix ions on the recovery of Pb2+ was investigated. An LOD of 1.9 ng/mL along with a preconcentration factor of 50 with RSD of 1.0% for Pb2+ were achieved. The proposed procedure was applied to the analysis of various real samples. PMID:23451399

  15. Analysis of frequency dependent pump light absorption

    NASA Astrophysics Data System (ADS)

    Wohlmuth, Matthias; Pflaum, Christoph

    2011-03-01

    Simulations have to accurately model thermal lensing in order to help improving resonator design of diode pumped solid state lasers. To this end, a precise description of the pump light absorption is an important prerequisite. In this paper, we discuss the frequency dependency of the pump light absorption in the laser crystal and its influence on the simulated laser performance. The results show that the pump light absorption has to include the spectral overlap of the emitting pump source and the absorbing laser material. This information can either be used for a fully frequency dependent absorption model or, at least in the shown examples, to compute an effective value for an exponential Beer-Lambert law of absorption. This is particularly significant at pump wavelengths coinciding with a peak of absorption. Consequences for laser stability and performance are analyzed for different pump wavelengths in a Nd:YAG laser.

  16. Investigations on Freon-assisted atomization of refractory analytes (Cr, Mo, Ti, V) in multielement electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Heinrich, Hans-Joachim; Matschat, Ralf

    2007-08-01

    Premixed 1% Freon in argon inner gas of various composition (CCl 2F 2, CHClF 2, CHF 3) was applied to graphite furnace atomizer to minimize unfavorable effects of carbide formation, such as signal tailing and memory effects in the simultaneous determination of Cr, Mo, Ti and V refractory analytes by electrothermal atomic absorption spectrometry using a multielement atomic absorption spectrometer. The effect of these gaseous additives was investigated when applied separately in atomization, pyrolysis and clean-out steps. The halogenation effects were analytically useful only under the precondition of using Ar-H 2 outer gas to the furnace to all heating steps, and also using this gas in the pre-atomization (drying, pyrolysis) steps. Optimum analytical performance was obtained when mixtures of 1% Freon in argon were applied just before and during the atomization step at a flow rate of 50 mL min - 1 and 2% hydrogen was used as purge gas. Using optimum conditions, signal tailings and carry-over contamination were reduced effectively and good precision (relative standard deviation below 1%) could be attained. Applying 1% CHClF 2 and an atomization temperature of 2550 °C, the characteristic masses obtained for simple aqueous solutions were 8.8 pg for Cr, 17 pg for Mo, 160 pg for Ti, and 74 pg for V. The limits of detection were 0.05, 0.2, 2.3 and 0.5 μg L - 1 for Cr, Mo, Ti and V, respectively. The developed method was applied to the analysis of digests of advanced ceramics. The accuracy of the procedure was confirmed by analyzing the certified reference material ERM-ED 102 (Boron Carbide Powder) and a silicon nitride powder distributed in the inter-laboratory comparison CCQM-P74.

  17. Determination of cadmium in biodiesel using microemulsion and electrothermal atomization atomic absorption spectrometry.

    PubMed

    Lima, Adriana S; Silva, Deise G; Teixeira, Leonardo S G

    2015-01-01

    This work aimed to prepare biodiesel microemulsions for the subsequent quantification of cadmium via graphite furnace atomic absorption spectrometry (GFAAS). The biodiesel samples were prepared using n-propanol as an emulsifier, 10% (v/v) nitric acid as the aqueous phase, and biodiesel. Pseudoternary phase diagrams were constructed to determine the microemulsion region with the specified components. The optimized conditions for microemulsion formation were 57.6% (v/v) n-propanol, 21.2% (v/v) biodiesel, and 21.2% (v/v) nitric acid solution. The stability of the microemulsified system was investigated using aqueous and organic standards, and the system was found to be stable for at least 240 min. The applied pyrolysis and atomization temperatures were 800 and 2000 °C, respectively, and 5 μg of aluminum was used as the chemical modifier. The obtained limits of detection and quantification were 0.2 and 0.5 μg kg(-1), respectively, and the characteristic mass was 1.6 pg. The precision, expressed as the relative standard deviation (% R.S.D., n = 10), was 2.5% for a sample with a cadmium concentration of 6.5 μg kg(-1). The accuracy was determined from addition and recovery experiments, with results varying from 93 to 108% recovery. This study demonstrates that the proposed method based on the use of a microemulsion formation in sample preparation can be applied as an efficient alternative for the determination of cadmium in biodiesel by GFAAS. Cadmium determination in biodiesel samples of different origins (soybean, corn, cotton, and sunflower) was evaluated after acid digestion using the inductively coupled plasma-mass spectrometry (ICP-MS) technique, and the obtained results were compared to the results obtained using the proposed method. The paired t test (95% confidence level) did not show significant differences. The concentrations of cadmium found ranged from 5.3 to 8.0 μg kg(-1). PMID:25381584

  18. Determination of platinum and palladium in road dust after their separation on immobilized fungus by electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Woińska, Sylwia; Godlewska-Żyłkiewicz, Beata

    2011-07-01

    A flow solid phase extraction procedure based on biosorption of Pt(IV) and Pd(II) on Aspergillus sp. immobilized on cellulose resin Cellex-T was proposed for the separation and preconcentration of Pt and Pd before their determination by electrothermal atomic absorption spectrometry (ETAAS). The analytical conditions including sample pH, eluent type, flow rates of sample and eluent solutions were examined. The analytes were selectively retained on the biosorbent in acidic medium (pH 1) and subsequently eluted from the column with 1 mL of thiourea solution (0.25 mol L - 1 thiourea in 0.3 mol L - 1 HCl). The reproducibility of the procedure was below 5%. The limit of detection of the method was 0.020 ng mL - 1 for Pt and 0.012 ng mL - 1 for Pd. The method validation was performed by analysis of certified reference materials BCR-723 (tunnel dust) and SARM-76 (platinum ore). The developed separation procedure was applied to the determination of Pt and Pd in road dust samples by ETAAS. The applied biosorbent is characterized by high sorption capacity: 0.47 mg g - 1 for Pt and 1.24 mg g - 1 for Pd.

  19. Determination of cadmium and lead in beverages after leaching from pewter cups using graphite furnace atomic absorption spectrometry.

    PubMed

    Dessuy, Morgana B; Vale, Maria Goreti R; Welz, Bernhard; Borges, Aline R; Silva, Márcia M; Martelli, Patrícia B

    2011-07-15

    Two simple methods have been developed to determine cadmium and lead in different kinds of beverages and vinegar leached from pewter cups produced in Brazil. Leaching experiments have been carried out with different solutions: beer, sugar cane spirit, red and white wine, vinegar and a 3% acetic acid solution. The solutions were kept in cups with and without solder for 24h. Lead and cadmium have been determined using graphite furnace atomic absorption spectrometry with deuterium background correction. The limits of detection were 0.05 and 1.4 μg L(-1), and the characteristic mass was 1.0 pg and 19 pg for Cd and Pb, respectively. With the developed methods it was possible to determine accurately cadmium and lead by direct analysis in these liquids and to evaluate the leaching of these metals from pewter cups. The results presented in this work show that pewter cups are not cadmium- and lead-free; this point goes against the manufacturers' declaration that their products are lead-free. PMID:21645758

  20. 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. PMID:26946014

  1. 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

  2. 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. PMID:22133102

  3. Determination of bismuth in environmental samples by slurry sampling graphite furnace atomic absorption spectrometry using combined chemical modifiers.

    PubMed

    Dobrowolski, Ryszard; Dobrzyńska, Joanna; Gawrońska, Barbara

    2015-01-01

    Slurry sampling graphite furnace atomic absorption spectrometry technique was applied for the determination of Bi in environmental samples. The study focused on the effect of Zr, Ti, Nb and W carbides, as permanent modifiers, on the Bi signal. Because of its highest thermal and chemical stability and ability to substantially increase Bi signal, NbC was chosen as the most effective modifier. The temperature programme applied for Bi determination was optimized based on the pyrolysis and atomization curves obtained for slurries prepared from certified reference materials (CRMs) of the soil and sediments. To overcome interferences caused by sulfur compounds, Ba(NO₃)₂ was used as a chemical modifier. Calibration was performed using the aqueous standard solutions. The analysis of the CRMs confirmed the reliability of the proposed analytical method. The characteristic mass for Bi was determined to be 16 pg with the detection limit of 50 ng/g for the optimized procedure at the 5% (w/v) slurry concentration. PMID:25384374

  4. Determination of Low Levels of Lead in Beer Using Solid-Phase Extraction and Detection by Flame Atomic Absorption Spectrometry

    PubMed Central

    Alves, Vanessa N.; Borges, Simone S. O.; Neto, Waldomiro B.; Coelho, Nívia M. M.

    2011-01-01

    In this study, a method for the determination of low concentrations of lead in beer samples using solid-phase extraction with a flow injection analysis system and detection by flame atomic absorption spectrometry (FAAS) was developed. Moringa oleifera seeds were used as a biosorbent material. Chemical and flow variables of the online preconcentration system, such as sample pH, preconcentration flow rate, eluent flow rate, eluent concentration, particle size, and sorbent mass, were studied. The optimum extraction conditions were obtained using a sample pH of 6.0, sample flow rate of 6.0 mL min−1, 63.0 mg of sorbent mass, and 2.0 mol L−1 HNO3 at a flow rate of 2.0 mL min−1 as the eluent. With the optimized conditions, the preconcentration factor, precision, detection limit, consumption index, and sample throughput were estimated as 93, 0.3% (10.0 μg L−1, n = 7), 7.5 μg L−1, 0.11 mL, and 23 samples per hour, respectively. The method developed was successfully applied to beer samples and recovery tests, with recovery ranging from 80% to 100%. PMID:22013389

  5. [Determination of Iodine and Iodate in Brine and Seafood Simultaneously by Ultraviolet Absorption Spectrometry].

    PubMed

    Tan, Jun; Zhu, Xia-ping; Liu, Miao-miao; Wei, Zhi-cheng; Sang, Shi-hua

    2015-06-01

    The iodide in samples was oxidized to iodate by bromine water, which could be removed by formic acid, and iodate could be transformed to I3- with excess of I- in phosphoric acid, the iodate in samples could be transformed directly to I3- with excess of I- in phosphoric acid. The I3- solution had strong absorption at 350 and 288 nm, and the absorbance had a linear relationship to the concentration of I3- in a certain range. Total content of iodide and iodate had been detected after samples were oxidized by bromine water and the content of iodate had been detected directly, and the content of iodide was obtained by difference of the two results. Based on this, the method had been established to detect iodide and iodate in brine and seafood simultaneously by ultraviolet absorption spectrometry. The volumes of bromine water, formic acid, phosphoric acid and potassium iodide had been optimized. The effect of illumination, temperature and time also had been discussed. The optional reagents condition for iodide was: 2 drops of 3% bromine water, 0.5 mL of 10% formic acid, 4 mL of 20% phosphoric acid and 1 mL of 100 g x L(-1 KI. The optional reagents condition for iodate was: 0. 2 mL of 20% phosphoric acid and 1 mL of 100 g x L(-1) KI. The absorbance were determined after reacting for 30 min at room temperature and natural light conditions. Under the optimized conditions, the concentration of iodide and iodate in the range of 0 - 1.2 and 0 -1.5 mg x L(-1) were well agreed with Lambert Beer law. The sample blank was detected for twelve times and the detection limit of iodide and iodate were 1.54 and 14.8 μg x L(-1) respectively. The RSD of twelve times determination of 0.8 mg x L(-1) of iodide and iodate were 0.097% and 0.067%, respectively. The iodide and iodate in Zhabuye brine, Hong Feng underground brine, kelp, seaweed and sea cabbage had been detected, the recovery experiments also had been conducted at the same time, the recovery of iodide and iodate were between 80

  6. Determination of mercury distribution inside spent compact fluorescent lamps by atomic absorption spectrometry

    SciTech Connect

    Rey-Raap, Natalia

    2012-05-15

    Highlights: Black-Right-Pointing-Pointer New treatments for CFL are required considering the aim of Directive 202/96/CE. Black-Right-Pointing-Pointer It is shown that most of the mercury introduced into a CFL is in the phosphor powder. Black-Right-Pointing-Pointer Experimental conditions for microwave-assisted sample digestion followed by AAS measurements are described. Black-Right-Pointing-Pointer By washing the glass it is possible to reduce the concentration below legal limits. - Abstract: 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 {+-} 0.4 ppb of mercury in the vapor phase, 204.16 {+-} 8.9 ppb of mercury in the phosphor powder, and 18.74 {+-} 0.5 ppb 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.

  7. Tributyl phosphate as a sensitivity-enhancing solvent for organotin in carbon furnace atomic absorption spectrometry.

    PubMed

    Li, H; Gong, B; Matsumoto, K

    1996-07-01

    Tributyl phosphate (TBP) has been found to be a sensitivity-enhancing solvent for organotin compounds in graphite furnace atomic absorption spectrometry; (C(4)H(9))(2)Sn(O(2)CCH(3))(2), (C(4)H(9))(2)Sn(O(2)CC(11)H(23))(2), (C(4)H(9))(3)SnCl, and (C(4)H(9))(4)Sn all give 1 order of magnitude higher sensitivities in TBP than in toluene or ethyl acetate. The sensitivities are enhanced further 1-2 orders of magnitude in TBP, when PdCl(2)(CH(3)CN)(2) is added as a matrix modifier in the organic solvent. Among the four organotin compounds, (C(4)H(9))(2)Sn(O(2)CCH(3))(2) and (C(4)H(9))(2)Sn(O(2)CC(11)H(23))(2) give better sensitivities than (C(4)H(9))(3)SnCl and (C(4)H(9))(4)Sn in the absence of palladium in any organic solvent, which suggests that the oxygen atom in the tin compound might form tin oxides that are resistant to volatilization loss during ashing. Scanning electron microscopic, electrothermal vaporization ICPMS, and powder X-ray diffraction studies show that the final products before atomization include phosphorus-containing compounds Sn(2)P(2)O(7), SnP(2)O(7), and Pd(9)P(2), besides tin-palladium alloys, PdSn, Pd(3)Sn, Pd(2)Sn, Pd(3)Sn(2), and PdSn(3). These phosphorus-containing compounds would more efficiently stabilize tin and suppress tin vaporization loss during ashing, to give higher sensitivity. PMID:21619315

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

    NASA Astrophysics Data System (ADS)

    Matusiewicz, Henryk; Krawczyk, Magdalena

    2007-03-01

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

  9. Preconcentration and Atomization of Arsane in a Dielectric Barrier Discharge with Detection by Atomic Absorption Spectrometry.

    PubMed

    Novák, Petr; Dědina, Jiří; Kratzer, Jan

    2016-06-01

    Atomization of arsane in a 17 W planar quartz dielectric barrier discharge (DBD) atomizer was optimized, and its performance was compared to that of a multiple microflame quartz tube atomizer (MMQTA) for atomic absorption spectrometry (AAS). Argon, at a flow rate of 60 mL min(-1), was the best DBD discharge gas. Free As atoms were also observed in the DBD with nitrogen, hydrogen, and helium discharge gases but not in air. A dryer tube filled with NaOH beads placed downstream from the gas-liquid separator to prevent residual aerosol and moisture transport to the atomizer was found to improve the response by 25%. Analytical figures of merit were comparable, reaching an identical sensitivity of 0.48 s ng (-1) As in both atomizers and limits of detection (LOD) of 0.15 ng mL(-1) As in MMQTA and 0.16 ng mL(-1) As in DBD, respectively. Compared to MMQTA, DBD provided 1 order of magnitude better resistance to interference from other hydride-forming elements (Sb, Se, and Bi). Atomization efficiency in DBD was estimated to be 100% of that reached in the MMQTA. A simple procedure of lossless in situ preconcentration of arsane was developed. Addition of 7 mL min(-1) O2 to the Ar plasma discharge resulted in a quantitative retention of arsane in the optical arm of the DBD atomizer. Complete analyte release and atomization was reached as soon as oxygen was switched off. Preconcentration efficiency of 100% was observed, allowing a decrease of the LOD to 0.01 ng mL(-1) As employing a 300 s preconcentration period. PMID:27159266

  10. Tandem mass spectrometry: analysis of complex mixtures

    SciTech Connect

    Singleton, K.E.

    1985-01-01

    Applications of tandem mass spectrometry (MS/MS) for the analysis of complex mixtures results in increased specificity and selectivity by using a variety of reagent gases in both negative and positive ion modes. Natural isotopic abundance ratios were examined in both simple and complex mixtures using parent, daughter and neutral loss scans. MS/MS was also used to discover new compounds. Daughter scans were used to identify seven new alkaloids in a cactus species. Three of these alkaloids were novel compounds, and included the first simple, fully aromatic isoquinoline alkaloids reported in Cactaceae. MS/MS was used to characterize the chemical reaction products of coal in studies designed to probe its macromolecular structure. Negative ion chemical ionization was utilized to study reaction products resulting from the oxidation of coal. Possible structural units in the precursor coal were predicted based on the reaction products identified, aliphatic and aromatic acids and their anhydrides. The MS/MS method was also used to characterize reaction products resulting from coal liquefaction and/or extraction. These studies illustrate the types of problems for which MS/MS is useful. Emphasis has been placed on characterization of complex mixtures by selecting experimental parameters which enhance the information obtained. The value of using MS/MS in conjunction with other analytical techniques as well as the chemical pretreatment is demonstrated.

  11. Liquid extraction surface analysis field asymmetric waveform ion mobility spectrometry mass spectrometry for the analysis of dried blood spots.

    PubMed

    Griffiths, Rian L; Dexter, Alex; Creese, Andrew J; Cooper, Helen J

    2015-10-21

    Liquid extraction surface analysis (LESA) is a surface sampling technique that allows electrospray mass spectrometry analysis of a wide range of analytes directly from biological substrates. Here, we present LESA mass spectrometry coupled with high field asymmetric waveform ion mobility spectrometry (FAIMS) for the analysis of dried blood spots on filter paper. Incorporation of FAIMS in the workflow enables gas-phase separation of lipid and protein molecular classes, enabling analysis of both haemoglobin and a range of lipids (phosphatidylcholine or phosphatidylethanolamine, and sphingomyelin species) from a single extraction sample. The work has implications for multiplexed clinical assays of multiple analytes. PMID:26198596

  12. Amount-ratio determinations of water isotopologues by dual-laser absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Castrillo, Antonio; Dinesan, Hemanth; Casa, Giovanni; Galzerano, Gianluca; Laporta, Paolo; Gianfrani, Livio

    2012-11-01

    We propose a method for the measurements of the 17O/16O isotope amount ratio in water, based upon the use of a pair of offset-frequency locked extended-cavity diode lasers at 1.39 μm. This method enables one to acquire absorption spectra with an extremely high fidelity, exploiting the highly accurate, absolute, and repeatable frequency axis. One of the two lasers, namely the so-called slave laser, is continuously scanned across a pair of H216O and H217O lines at 7183.5 cm-1 and it interacts with a water vapor sample inside a multiple reflections cell, thus producing absorption spectra with a signal-to-noise ratio of the order of 4000 for a detection bandwidth of 1 kHz. The determination of the isotope amount ratio is performed through a careful analysis of the acquired spectra, by using semiclassical line profiles. In this respect, the influence of the choice of the line shape model is investigated. The experimental reproducibility of the spectrometer has been carefully assessed by means of an Allan variance analysis. Finally, the application of the Kalman filtering technique has shown that a precision of 0.6‰ can be achieved, from repeated spectral acquisitions over a time span of 6000 s.

  13. Determination of macro- and micronutrients in plant leaves by high-resolution continuum source flame atomic absorption spectrometry combining instrumental and sample preparation strategies

    NASA Astrophysics Data System (ADS)

    Oliveira, Silvana R.; Gomes Neto, José A.; Nóbrega, Joaquim A.; Jones, Bradley T.

    2010-04-01

    A method for determination of B, Ca, Cu, Fe, K, Mg, Mn, Mo, P, S and Zn in plant tissues by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS) is proposed. This method is based on special features of HR-CS-AAS, such as side pixel registration, wavelength integrated absorbance, and molecular absorption bands, for determining macro- and micronutrients in foliar analysis without requiring several different strategies for sample preparation and adjustment of the analytes concentration ranges. Plant samples were analyzed and results for certified materials were in agreement at a 95% confidence level (paired t-test) with reference values. Recoveries of analytes added to plant digests varied within the 82-112% interval. Relative standard deviations ( n = 12) were lower than or equal to 5.7% for all analytes in all concentration ranges.

  14. Performance Analysis of Solution Transportation Absorption Chiller

    NASA Astrophysics Data System (ADS)

    Kiani, Behdad; Hamamoto, Yoshinori; Akisawa, Atsushi; Kashiwagi, Takao

    Thermally activated advanced absorption cycles are considered promising candidates to replace CFCs, HCFCs and HFCs for residential and commercial applications. In such absorption systems, it is desirable to utilize the waste heat from industries for heating and cooling applications in commercial and residential sectors. For this purpose, it is necessary to transport energy over some distance because the waste heat source and demand are generally located apart from each other. Transportation of steam, hot water or chilled water requires high construction costs for insulation. There is an efficient method of energy transportation using absorption system called “ Solution Transportation Absorption System (STA)”. The solution is transported at an ambient temperature so that tube-insulations not required. This paper shows the simulation of the abovementioned system and the optimal result, using mathematical optimization. The optimum system with industry‧s waste heat utilization is obtained. At the end, the effect on the pollution emission and energy conservation is obtained.

  15. 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,…

  16. Speciation of methylcyclopentadienyl manganese tricarbonyl by high-performance liquid chromatography-diode laser atomic absorption spectrometry.

    PubMed

    Butcher, D J; Zybin, A; Bolshov, M A; Niemax, K

    1999-12-01

    Methylcyclopentadienyl manganese tricarbonyl (MMT) is a fuel additive that has been marketed for use in unleaded gasoline since December 1995. The widespread use of this additive has been suggested to cause health risks, but limitations in data regarding its degradation products and their toxicity prevent an accurate evaluation. To monitor the organomanganese compounds, it is clearly advantageous to employ low-cost, high-sensitivity, manganese-specific instrumentation to perform speciation. In this work, instrumentation fitting these criteria was obtained by the combination of high-performance liquid chromatography (HPLC) with diode laser atomic absorption spectrometry (DLAAS) and was used to determine MMT, its nonmethylated derivative, cyclopentadienyl manganese tricarbonyl (CMT), and inorganic manganese. DLAAS was shown to be a versatile analytical technique for total Mn determination, with a detection limit of 1 ng/mL and a linear dynamic range (LDR) of almost 5 orders of magnitude. Analytical figures of merit for HPLC-DLAAS included a detection limit of 2 ng(as Mn)/mL, a LDR of 3 orders of magnitude, and an analysis time of three minutes. The organometallic compounds are characterized by rapid photolysis in sunlight, and hence, experiments were performed to evaluate whether normal laboratory lighting is suitable for their determination. Our results showed that normal laboratory protocols may be employed except that the organomanganese compounds should be stored away from light except during sample introduction procedures. The ability of the instrumentation to selectively preconcentrate organomanganese compounds while removing inorganic manganese was demonstrated. Sufficient resolution was obtained to determine a 20-fold excess of CMT compared with MMT. The ability of the system to do practical analysis was demonstrated by the accurate determination of MMT in spiked samples of gasoline, human urine, and tap water. These results demonstrate the suitability of

  17. Determination of manganese in diesel, gasoline and naphtha by graphite furnace atomic absorption spectrometry using microemulsion medium for sample stabilization

    NASA Astrophysics Data System (ADS)

    Brandão, Geisamanda Pedrini; de Campos, Reinaldo Calixto; de Castro, Eustáquio Vinicius Ribeiro; de Jesus, Honério Coutinho

    2008-08-01

    The determination of Mn in diesel, gasoline and naphtha samples at µg L - 1 level by graphite furnace atomic absorption spectrometry, after sample stabilization in a three-component medium (microemulsion) was investigated. Microemulsions were prepared by mixing appropriate volumes of sample, propan-1-ol and nitric acid aqueous solution, and a stable system was immediately and spontaneously formed. After multivariate optimization by central composite design the optimum microemulsion composition as well as the temperature program was defined. In this way, calibration using aqueous analytical solution was possible, since the same sensitivity was observed in the optimized microemulsion media and 0.2% v/v HNO 3. The use of modifier was not necessary. Recoveries at the 3 µg L - 1 level using both inorganic and organic Mn standards spiked solutions ranged from 98 to 107% and the limits of detection were 0.6, 0.5 and 0.3 µg L - 1 in the original diesel, gasoline and naphtha samples, respectively. The Mn characteristic mass 3.4 pg. Typical relative standard deviation ( n = 5) of 8, 6 and 7% were found for the samples prepared as microemulsions at concentration levels of 1.3, 0.8, and 1.5 µg L - 1 , respectively. The total determination cycle lasted 4 min for diesel and 3 min for gasoline and naphtha, equivalent to a sample throughput of 7 h - 1 for duplicate determinations in diesel and 10 h - 1 for duplicate determinations in gasoline and naphtha. Accuracy was also assessed by using other method of analysis (ASTM D 3831-90). No statistically significant differences were found between the results obtained with the proposed method and the reference method in the analysis of real samples.

  18. Cloud point extraction for the determination of cadmium and lead in biological samples by graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Maranhão, Tatiane De A.; Borges, Daniel L. G.; da Veiga, Márcia A. M. S.; Curtius, Adilson J.

    2005-06-01

    The phase-separation phenomenon of non-ionic surfactants occurring in aqueous solution was used for the extraction of Cd and Pb from digested biological samples. After complexation with O,O-diethyldithiophosphate (DDTP) in hydrochloric acid medium, the analytes are quantitatively extracted to the phase rich in the non-ionic surfactant octylphenoxypolyethoxyethanol (Triton X-114) after centrifugation. Methanol acidified with 0.1 mol L-1 HNO3 was added to the surfactant-rich phase prior to its analysis by electrothermal atomic absorption spectrometry (ET AAS). The adopted concentrations for DDTP, Triton X-114 and hydrochloric acid were all optimized. Pyrolysis and atomization temperatures were optimized using the extracts and pyrolysis temperatures of 700 °C for both elements and atomization temperatures of 1400 and 1600 °C for cadmium and lead, respectively, were used without adding any modifier, which shows that considerable analyte stabilization is provided by the medium itself. A more detailed investigation was carried out to determine which components of the extract were responsible for the high thermal stability achieved and it revealed that the amount of DDTP added and the phosphorus content of the digested samples contributed significantly to this phenomenon. Detection limits (3σB) of 6 and 40 ng g-1, along with enrichment factors of 129 and 18 for Cd and Pb, respectively, were achieved. The proposed procedure was applied to the analysis of five certified biological reference materials after microwave-assisted acid digestion in a mixture of H2O2 and HNO3. Comparison with certified values was performed for accuracy evaluation, resulting in good agreement according to the t-test for a 95% confidence level. The high efficiency of cloud point extraction to carry out the determination of the studied analytes in complex matrices was, therefore, demonstrated.

  19. Simultaneous determination of cadmium and lead in wine by electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Freschi, Gian P. G.; Dakuzaku, Carolina S.; de Moraes, Mercedes; Nóbrega, Joaquim A.; Gomes Neto, José A.

    2001-10-01

    A method has been developed for the direct simultaneous determination of Cd and Pb in white and red wine by electrothermal atomic absorption spectrometry (ET-AAS) using a transversely heated graphite tube atomizer (THGA) with longitudinal Zeeman-effect background correction. The thermal behavior of both analytes during pyrolysis and atomization stages were investigated in 0.028 mol l -1 HNO 3 and in 1+1 v/v diluted wine using mixtures of Pd(NO 3) 2+Mg(NO 3) 2 and NH 4H 2PO 4+Mg(NO 3) 2 as chemical modifiers. With 5 μg Pd+3 μg Mg as the modifiers and a two-step pyrolysis (10 s at 400°C and 10 s at 600°C), the formation of carbonaceous residues inside the atomizer was avoided. For 20 μl of sample (wine+0.056 mol l -1 HNO 3, 1+1, v/v) dispensed into the graphite tube, analytical curves in the 0.10-1.0 μg l -1 Cd and 5.0-50 μg l -1 Pb ranges were established. The characteristic mass was approximately 0.6 pg for Cd and 33 pg for Pb, and the lifetime of the tube was approximately 400 firings. The limits of detection (LOD) based on integrated absorbance (0.03 μg l -1 for Cd, 0.8 μg l -1 for Pb) exceeded the requirements of Brazilian Food Regulations (decree #55871 from Health Department), which establish the maximum permissible level for Cd at 200 μg l -1 and for Pb at 500 μg l -1. The relative standard deviations ( n=12) were typically <8% for Cd and <6% for Pb. The recoveries of Cd and Pb added to wine samples varied from 88 to 107% and 93 to 103%, respectively. The accuracy of the direct determination of Cd and Pb was checked for 10 table wines by comparing the results with those obtained for digested wine using single-element ET-AAS, which were in agreement at the 95% confidence level.

  20. 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.

  1. Coacervative extraction of trace lead from natural waters prior to its determination by electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Hagarová, Ingrid; Bujdoš, Marek; Matúš, Peter; Kubová, Jana

    2013-10-01

    In this work, a relatively simple and sensitive method for separation/preconcentration of trace lead from natural waters prior to its determination by electrothermal atomic absorption spectrometry has been proposed. The method is based on the extraction of Pb-dithizone chelate with coacervates made up of lauric acid in the presence of potassium ions and methanol. Several important factors affecting extraction efficiency such as pH, concentration of lauric acid and dithizone, ionic strength, incubation and centrifugation time were investigated and optimized. After separation of aqueous bulk solution from surfactant-rich phase, the final extract was redissolved by using 500 μl of methanol acidified with 0.2 mol l- 1 HNO3. Under the optimized conditions (using initial sample volume of 10 ml), enrichment factor of 17.0, detection limit of 0.12 μg l- 1, quantification limit of 0.38 μg l- 1, relative standard deviation of 4.2% (for 2 μg l- 1 of Pb; n = 26), linearity of the calibration graph in the range of 0.5-4.0 μg l- 1 (with correlation coefficient better than 0.995) were achieved. The method was validated by the analysis of certified reference material (TMDA-61). Extraction recoveries for the CRM, spiked model solutions and spiked natural water samples were in the range of 91-96%. Finally, the method was applied to the separation/preconcentration and determination of trace lead in natural waters.

  2. 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.

  3. 2. VIEW IN ROOM 111, ATOMIC ABSORPTION BERYLLIUM ANALYSIS LABORATORY. ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    2. VIEW IN ROOM 111, ATOMIC ABSORPTION BERYLLIUM ANALYSIS LABORATORY. AIR FILTERS AND SWIPES ARE DISSOLVED WITH ACIDS AND THE REMAINING RESIDUES ARE SUSPENDED IN NITRIC ACID SOLUTION. THE SOLUTION IS PROCESSED THROUGH THE ATOMIC ABSORPTION SPECTROPHOTOMETER TO DETECT THE PRESENCE AND LEVELS OF BERYLLIUM. - Rocky Flats Plant, Health Physics Laboratory, On Central Avenue between Third & Fourth Streets, Golden, Jefferson County, CO

  4. Metal Speciation in the ppt Range by HPLC and Diode Laser Atomic Absorption Spectrometry in a Flame.

    PubMed

    Zybin, A; Schaldach, G; Berndt, H; Niemax, K

    1998-12-01

    A simple, compact, and powerful instrument for metal speciation in the ppt range is described. The instrument includes a HPLC module for separation and a diode laser for element-selective detection by wavelength modulation absorption spectrometry in an analytical flame. The high detection power for metal species is due to a two-beam arrangement with logarithmic amplification of the normalized signal, which compensates the laser residual amplitude modulation noise, the offset, and its fluctuation. The analytical figures of merit are demonstrated by measurements of very low concentrations of Cr(VI) in tap water. PMID:21644686

  5. [Determination of trace elements in Spirulina platensis (Notdst.) Geitl. by flame atomic absorption spectrometry combined with microsampling pulse nebulization technique].

    PubMed

    Cheng, Cun-Gui; Hong, Qing-Hong; Li, Dan-Ting; Fan, Meng-Hai; Cai, Xiao-Dan

    2006-09-01

    The contents of trace elements Ni, Zn, Mn, Cu, Mg, Fe, Ca and Pb in Spirulina platensis (Notdst.) Geitl. were determined by flame atomic absorption spectrometry combined with microsampling pulse nebulization technique. The results of the determination show that Spirulina platensis (Notdst.) Geitl. are rich in the inorganic elements such as Mg, Zn, Fe, Ca and Cu. Its recovery ratio obtained by standard addition method ranged between 96.58% and 106.12%, and its RSD was lower than 4.26%. The result will provide scientific data for the study on the trace elements in Spirulina platensis (Notdst.) Geitl. and on their relativity of efficacy of medicine. PMID:17112058

  6. Determination of cobalt in samples containing cobalt and tungsten carbide by electrothermal atomic absorption spectrometry

    SciTech Connect

    Firriolo, J.M.; Kutzman, R.S.

    1985-09-01

    A method has been developed to determine the amount of cobalt (Co) in atmospheric dust samples which include free and sintered Co. Cobalt and tungsten carbide (WC) mixtures ranging from 0-100% Co were prepared for atomic absorption analysis by dissolving the Co in aqua regia. Using this method, the amount of Co in the samples assayed ranged from 90.9-100.1% of that gravimetrically added to the mixtures. The results of this aqua regia dissolution procedure for Co were compared to a hydrofluoric acid method which solubilized both the Co and the WC. Application of the aqua regia dissolution method to samples of sintered WC and Co dust resulted in complete recovery of the Co from these materials. These results were supported by x-ray analysis of the samples before and after dissolution of the Co with aqua regia. The described procedure is advantageous because it avoids the use of highly-caustic hydrofluoric acid and the results are quickly available.

  7. Chromium speciation by solid phase extraction on Dowex M 4195 chelating resin and determination by atomic absorption spectrometry.

    PubMed

    Saygi, Kadriye Ozlem; Tuzen, Mustafa; Soylak, Mustafa; Elci, Latif

    2008-05-30

    A solid phase extraction procedure has been established for chromium speciation in natural water samples prior to determination by atomic absorption spectrometry. The procedure is based on the solid phase extraction of the Cr(VI)- Dowex M 4195 chelating resin. After oxidation of Cr(III) to Cr(VI) by using H2O2, the presented method was applied to the determination of the total chromium. The level of Cr(III) is calculated by difference of total chromium and Cr(VI) levels. The procedure was optimized for some analytical parameters including pH, eluent type, flow rates of sample and eluent, matrix effects, etc. The presented method was applied for the speciation of chromium in natural water samples with satisfactory results (recoveries >95%, RSDs <10%). In the determinations of chromium species, flame atomic absorption spectrometer was used. The results were checked by using NIST SRM 2711 Montana soil and GBW 07603 Bush branched and leaves. PMID:17951001

  8. Organic, inorganic and total mercury determination in fish by chemical vapor generation with collection on a gold gauze and electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Duarte, Fábio Andrei; Bizzi, Cezar Augusto; Antes, Fabiane Goldschmidt; Dressler, Valderi Luiz; Flores, Érico Marlon de Moraes

    2009-06-01

    A method for organic, inorganic and total mercury determination in fish tissue has been developed using chemical vapor generation and collection of mercury vapor on a gold gauze inside a graphite tube and further atomization by electrothermal atomic absorption spectrometry. After drying and cryogenic grinding, potassium bromide and hydrochloric acid solution (1 mol L - 1 KBr in 6 mol L - 1 HCl) was added to the samples. After centrifugation, total mercury was determined in the supernatant. Organomercury compounds were selectively extracted from KBr solution using chloroform and the resultant solution was back extracted with 1% m/v L-cysteine. This solution was used for organic Hg determination. Inorganic Hg remaining in KBr solution was directly determined by chemical vapor generation electrothermal atomic absorption spectrometry. Mercury vapor generation from extracts was performed using 1 mol L - 1 HCl and 2.5% m/v NaBH 4 solutions and a batch chemical vapor generation system. Mercury vapor was collected on the gold gauze heated resistively at 80 °C and the atomization temperature was set at 650 °C. The selectivity of extraction was evaluated using liquid chromatography coupled to chemical vapor generation and determination by inductively coupled plasma mass spectrometry. The proposed method was applied for mercury analysis in shark, croaker and tuna fish tissues. Certified reference materials were used to check accuracy and the agreement was better than 95%. The characteristic mass was 60 pg and method limits of detection were 5, 1 and 1 ng g - 1 for organic, inorganic and total mercury, respectively. With the proposed method it was possible to analyze up to 2, 2 and 6 samples per hour for organic, inorganic and total Hg determination, respectively.

  9. 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.

  10. Isotope Enrichment Detection by Laser Ablation - Dual Tunable Diode Laser Absorption Spectrometry

    SciTech Connect

    Anheier, Norman C.; Bushaw, Bruce A.

    2009-07-01

    The rapid global expansion of nuclear energy is motivating the expedited development of new safeguards technology to mitigate potential proliferation threats arising from monitoring gaps within the uranium enrichment process. Current onsite enrichment level monitoring methods are limited by poor sensitivity and accuracy performance. Offsite analysis has better performance, but this approach requires onsite hand sampling followed by time-consuming and costly post analysis. These limitations make it extremely difficult to implement comprehensive safeguards accounting measures that can effectively counter enrichment facility misuse. In addition, uranium enrichment by modern centrifugation leads to a significant proliferation threat, since the centrifuge cascades can quickly produce a significant quantity of highly enriched uranium (HEU). The Pacific Northwest National Laboratory is developing an engineered safeguards approach having continuous aerosol particulate collection and uranium isotope analysis to provide timely detection of HEU production in a low enriched uranium facility. This approach is based on laser vaporization of aerosol particulate samples, followed by wavelength tuned laser diode spectroscopy, to characterize the 235U/238U isotopic ratio by subtle differences in atomic absorption wavelengths arising from differences in each isotope’s nuclear mass, volume, and spin (hyperfine structure for 235U). Environmental sampling media is introduced into a small, reduced pressure chamber, where a focused pulsed laser vaporizes a 10 to 20-µm sample diameter. The ejected plasma forms a plume of atomic vapor. A plume for a sample containing uranium has atoms of the 235U and 238U isotopes present. Tunable diode lasers are directed through the plume to selectively excite each isotope and their presence is detected by monitoring absorbance signals on a shot-to-shot basis. Single-shot detection sensitivity approaching the femtogram range and abundance uncertainty

  11. Application of High Resolution-Continuum Source Flame Atomic Absorption Spectrometry (HR-CS FAAS): determination of trace elements in tea and tisanes.

    PubMed

    Paz-Rodríguez, Beatriz; Domínguez-González, María Raquel; Aboal-Somoza, Manuel; Bermejo-Barrera, Pilar

    2015-03-01

    A new application of HR-CS FAAS (High Resolution-Continuum Source Flame Atomic Absorption Spectrometry) has been developed for the determination of several trace elements (Ca, Co, Cu, Fe, Mn, Ni, Na and Zn) in infusions made from tea, rooibos and tea with seaweed samples. The proposed methods are fast, inexpensive and show good performances: the mean analytical recovery was approximately 100%. The mean limit of detection was 29.4 μg/l, and the mean limit of quantification was 98.0 μg/l (both limits refer to the brewed samples). Due to the matrix effect observed, the standard addition method had to be applied. Preliminary classification (based on metal contents) using chemometric techniques such as PCA (Principal Component Analysis) and CA (Cluster Analysis), was successful for infusions made from rooibos and tea with seaweed, but inconclusive for black and green teas. PMID:25306375

  12. Germanium determination by flame atomic absorption spectrometry: an increased vapor pressure-chloride generation system.

    PubMed

    Kaya, Murat; Volkan, Mürvet

    2011-03-15

    A new chloride generation system was designed for the direct, sensitive, rapid and accurate determination of the total germanium in complex matrices. It was aimed to improve the detection limit of chloride generation technique by increasing the vapor pressure of germanium tetrachloride (GeCl(4)). In order to do so, a novel joint vapor production and gas-liquid separation unit equipped with a home-made oven was incorporated to an ordinary nitrous oxide-acetylene flame atomic absorption spectrometer. Several variables such as reaction time, temperature and acid concentration have been investigated. The linear range for germanium determination was 0.1-10 ng mL(-1) for 1 mL sampling volume with a detection limit (3s) of 0.01 ng mL(-1). The relative standard deviation (RSD) was 2.4% for nine replicates of a 1 ng mL(-1) germanium solution. The method was validated by the analysis of one non-certified and two certified geochemical reference materials, respectively, CRM GSJ-JR-2 (Rhyolite), and GSJ-JR-1 (Rhyolite), and GBW 07107 (Chinese Rock). Selectivity of the method was investigated for Cd(2+), Co(2+), Cu(2+), Fe(3+), Ga(3+), Hg(2+), Ni(2+), Pb(2+), Sn(2+), and Zn(2+) ions and ionic species of As(III), Sb(III), Te(IV), and Se(IV). PMID:21315908

  13. Permanent modification in electrothermal atomic absorption spectrometry — advances, anticipations and reality

    NASA Astrophysics Data System (ADS)

    Tsalev, Dimiter L.; Slaveykova, Vera I.; Lampugnani, Leonardo; D'Ulivo, Alessandro; Georgieva, Rositsa

    2000-05-01

    Permanent modification is an important recent development in chemical modification techniques which is promising in view of increasing sample throughput with 'fast' programs, reducing reagent blanks, preliminary elimination of unwanted modifier components, compatibility with on-line and in situ enrichment, etc. An overview of this approach based on the authors' recent research and scarce literature data is given, revealing both success and failure in studies with permanently modified surfaces (carbides, non-volatile noble metals, noble metals on carbide coatings, etc.), as demonstrated in examples of direct electrothermal atomic absorption spectrometric (ETAAS) applications to biological and environmental matrices and vapor generation (VG)-ETAAS coupling with in-atomizer trapping of hydrides and other analyte vapors. Permanent modifiers exhibit certain drawbacks and limitations such as: poorly reproducible treatment technologies — eventually resulting in poor tube-to-tube repeatability and double or multiple peaks; impaired efficiency compared with modifier addition to each sample aliquot; relatively short lifetimes; limitations imposed on temperature programs, the pyrolysis, atomization and cleaning temperatures being set somewhat lower to avoid excessive loss of modifier; applicability to relatively simple sample solutions rather than to high-salt matrices and acidic digests; side effects of overstabilization, etc. The most important niches of application appear to be the utilization of permanently modified surfaces in coupled VG-ETAAS techniques, analysis of organic solvents and extracts, concentrates and fractions obtained after enrichment and/or speciation separations and direct ETAAS determinations of highly volatile analytes in relatively simple sample matrices.

  14. Atomic absorption spectrometry for the automatic indirect determination of ascorbic acid based on-the reduction of manganese dioxide.

    PubMed

    Noroozifar, Meissam; Khorasani-Motlagh, Mozhgan; Akhavan, Kambiz

    2005-06-01

    A new and simple flow injection method followed by atomic absorption spectrometry has been developed for the indirect determination of ascorbic acid. The proposed method is based on oxidation of ascorbic acid to dehydroascorbic acid using a solid-phase manganese dioxide (30% m/m suspended on silica gel beads) reactor. The flow of the sample through the column reduces the MnO2 to Mn(II) in an acidic carrier stream of 6.3 mM HNO3 (pH 2.2) with flow rate of 4.0 ml/min at room temperature; Mn(II) is measured by atomic absorption spectrometry. The absorbance of Mn(II) is proportional to the concentration of ascorbic acid in the sample. The calibration curve was linear up to 30 mg/L, with a detection limit of 0.2 mg/L for a 220 microL injected sample volume. The developed procedure was found to be suitable for the determination of AsA in pharmaceuticals and foods with a relative standard deviation better than 1.09% and a sampling rate of about 95 h(-1). The results exhibit no interference from the presence of large amounts of organic compounds. The reliability of the method was established by parallel determination against the 2,6-dichlorophenol-indophenol methods. PMID:15984201

  15. Determination of total selenium in pharmaceutical and herbal supplements by hydride generation and graphite furnace atomic absorption spectrometry.

    PubMed

    Kazi, Tasneem G; Kolachi, Nida F; Afridi, Hassan I; Brahman, Kapil Dev; Shah, Faheem

    2014-01-01

    The total selenium (Se) was determined in herbal and pharmaceutical supplements used for liver diseases. The total Se contents were determined in different pharmaceutical and herbal supplements by hydride generation atomic absorption spectrometry (HGAAS) and graphite furnace atomic absorption spectrometry (GFAAS) after microwave-assisted acid digestion. The accuracy of the techniques was evaluated by using certified reference material and the standard addition method. The recoveries of total Se were 99.4 and 99.0% for HGAAS and GFAAS, respectively. The precision of the techniques expressed as RSD were 2.34 and 4.54% for HGAAS and GFAAS measurements, respectively. The LOD values for HGAAS and GFAAS were 0.025 and 0.052 pglg, respectively. The concentrations of Se in pharmaceutical and herbal supplements were found in the range of 19.2-53.8 and 25.0-42.5 pg/g, respectively, corresponding to 35-76% and 45-76% of the total recommended dose of Se for adults. PMID:25632445

  16. 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). PMID:27345208

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

    NASA Astrophysics Data System (ADS)

    Mandjukov, Petko; Orani, Anna Maria; Han, Eunmi; Vassileva, Emilia

    2015-01-01

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

  18. 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). PMID:26838401

  19. High-resolution continuum source electrothermal atomic absorption spectrometry: Linearization of the calibration curves within a broad concentration range

    NASA Astrophysics Data System (ADS)

    Katskov, Dmitri; Hlongwane, Miranda; Heitmann, Uwe; Florek, Stefan

    2012-05-01

    The calculation algorithm suggested provides linearization of the calibration curves in high-resolution continuum source electrothermal atomic absorption spectrometry. The algorithm is based on the modification of the function wavelength-integrated absorbance vs. concentration of analyte vapor in the absorption volume. According to the suggested approach, the absorption line is represented by a triangle for low and trapezium for high analyte vapor concentration in the absorption volume. The respective semi-empirical formulas include two linearization parameters, which depend on properties of the absorption line and characteristics of the atomizer and spectrometer. The parameters can be approximately evaluated from the theory and determined in practice from the original broad-range calibration curve. The parameters were found and the proposed calculation algorithm verified in the experiments on direct determination of Ag, Cd, Cu, Fe, Mn and Pb in the solutions within a concentration ranges from 0.15 to 625 μg·L- 1 using tube, platform tube and filter furnace atomizers. The use of various atomizers, lines, elements and atomization temperatures made possible the simulation of various practical analytical conditions. It was found that the algorithm and optimal linearization parameters made it possible to obtain for each line and atomizer linear approximations of the calibration curves within 3-4 orders of magnitude with correlation coefficients close to 0.999. The algorithm makes possible to employ a single line for the direct element determination over a broad concentration range. The sources of errors and the possibility of a priori theoretical evaluation of the linearization parameters are discussed.

  20. An improved impaction-graphite furnace system for the direct and near real-time determination of cadmium, chromium, lead and manganese in aerosols and cigarette smoke by simultaneous multielement atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Lee, Yong-Ill; Smith, Mark V.; Indurthy, Suneetha; Deval, Anupama; Sneddon, Joseph

    1996-01-01

    The design, operating characteristics, and preliminary evaluation of an improved impaction-graphite furnace system, based on a theoretical study of particle size collected, are presented. After direct collection, the graphite furnace from the system is inserted in an atomic absorption spectrometer for analysis by simultaneous multielement atomic absorption spectrometry. This system has the potential for the direct and near real-time (few minutes) determination of metals in aerosols. The system has been preliminarily evaluated using aqueous solutions of chromium, and has then been applied to the determination of cadmium, chromium, lead, and manganese in cigarette smoke. Results show an increase ranging from almost five (lead) to sixteen (cadmium) over background levels.

  1. HIGH RESOLUTION INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY ALLOWS RAPID ASSESSMENT OF IRON ABSORPTION IN INFANTS AND CHILDREN

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Stable isotope absorption studies of iron have been limited by the high cost and limited availability of isotope ratio analysis using thermal ionization MS (TIMS). The development of high-resolution double focusing inductively coupled plasma MS (ICP-MS) may permit more cost-efficient sample analysis...

  2. 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%. PMID:12733043

  3. Investigation of artifacts caused by deuterium background correction in the determination of phosphorus by electrothermal atomization using high-resolution continuum source atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Dessuy, Morgana B.; Vale, Maria Goreti R.; Lepri, Fábio G.; Borges, Daniel L. G.; Welz, Bernhard; Silva, Márcia M.; Heitmann, Uwe

    2008-02-01

    The artifacts created in the measurement of phosphorus at the 213.6-nm non-resonance line by electrothermal atomic absorption spectrometry using line source atomic absorption spectrometry (LS AAS) and deuterium lamp background correction (D 2 BC) have been investigated using high-resolution continuum source atomic absorption spectrometry (HR-CS AAS). The absorbance signals and the analytical curves obtained by LS AAS without and with D 2 BC, and with HR-CS AAS without and with automatic correction for continuous background absorption, and also with least-squares background correction for molecular absorption with rotational fine structure were compared. The molecular absorption due to the suboxide PO that exhibits pronounced fine structure could not be corrected by the D 2 BC system, causing significant overcorrection. Among the investigated chemical modifiers, NaF, La, Pd and Pd + Ca, the Pd modifier resulted in the best agreement of the results obtained with LS AAS and HR-CS AAS. However, a 15% to 100% higher sensitivity, expressed as slope of the analytical curve, was obtained for LS AAS compared to HR-CS AAS, depending on the modifier. Although no final proof could be found, the most likely explanation is that this artifact is caused by a yet unidentified phosphorus species that causes a spectrally continuous absorption, which is corrected without problems by HR-CS AAS, but which is not recognized and corrected by the D 2 BC system of LS AAS.

  4. Element-selective trace detection of toxic species in environmental samples using chromatographic techniques and derivative diode laser absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Koch, J.; Zybin, A.; Niemax, K.

    1998-10-01

    Very sensitive laser absorption techniques based on a double-beam scheme with logarithmic processing of the detector signals and wavelength modulation of laser diodes are presented. Detection limits equivalent to 10-7 absorption per square root of detection bandwidth are obtained if sufficient laser power is available and if the absorption is also subject to additional modulation. The analytical versatility of these techniques is demonstrated by quantitative analysis of very low concentrations of (i) Cr(VI) species in tap water and (ii) chlorinated poly-aromatics (chlorophenols) in plant extracts, both after chromatographic separation. The atomic absorption measurements were performed in an air-acetylene flame (Cr) and in a low-pressure microwave-induced plasma (chlorophenols).

  5. Determination of cadmium in the livers and kidneys of puffins by carbon furnace atomic absorption spectrometry.

    PubMed

    Ottaway, J M; Campbell, W C

    1976-01-01

    A carbon furnace atomic absorption procedure is described for the determination of cadmium in the livers and kidneys of puffins, fratercula arctica. Samples are dried and weighed and 2 to 100 mg are dissolved in sulphuric and nitric acids. These solutions are analysed directly in the carbon furnace against aqueous standards and provide accurate results in the range 0-1 to 100 micrograms/g dry weight. The method is simple and rapid and requires much less of the small total sample than would be required for flame atomic absorption. PMID:1030692

  6. Determination of serum aluminum by electrothermal atomic absorption spectrometry: A comparison between Zeeman and continuum background correction systems

    NASA Astrophysics Data System (ADS)

    Kruger, Pamela C.; Parsons, Patrick J.

    2007-03-01

    Excessive exposure to aluminum (Al) can produce serious health consequences in people with impaired renal function, especially those undergoing hemodialysis. Al can accumulate in the brain and in bone, causing dialysis-related encephalopathy and renal osteodystrophy. Thus, dialysis patients are routinely monitored for Al overload, through measurement of their serum Al. Electrothermal atomic absorption spectrometry (ETAAS) is widely used for serum Al determination. Here, we assess the analytical performances of three ETAAS instruments, equipped with different background correction systems and heating arrangements, for the determination of serum Al. Specifically, we compare (1) a Perkin Elmer (PE) Model 3110 AAS, equipped with a longitudinally (end) heated graphite atomizer (HGA) and continuum-source (deuterium) background correction, with (2) a PE Model 4100ZL AAS equipped with a transversely heated graphite atomizer (THGA) and longitudinal Zeeman background correction, and (3) a PE Model Z5100 AAS equipped with a HGA and transverse Zeeman background correction. We were able to transfer the method for serum Al previously established for the Z5100 and 4100ZL instruments to the 3110, with only minor modifications. As with the Zeeman instruments, matrix-matched calibration was not required for the 3110 and, thus, aqueous calibration standards were used. However, the 309.3-nm line was chosen for analysis on the 3110 due to failure of the continuum background correction system at the 396.2-nm line. A small, seemingly insignificant overcorrection error was observed in the background channel on the 3110 instrument at the 309.3-nm line. On the 4100ZL, signal oscillation was observed in the atomization profile. The sensitivity, or characteristic mass ( m0), for Al at the 309.3-nm line on the 3110 AAS was found to be 12.1 ± 0.6 pg, compared to 16.1 ± 0.7 pg for the Z5100, and 23.3 ± 1.3 pg for the 4100ZL at the 396.2-nm line. However, the instrumental detection limits (3

  7. Semi-permanent lutetium modifier for the determination of beryllium in urine by electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Burguera, J. L.; Burguera, M.; Rondón, C.; Carrero, P.

    1999-11-01

    The determination of beryllium using electrothermal atomic absorption spectrometry with deuterium background correction in the presence of various isomorphous metals and Mg(NO 3) 2 was studied. While, Eu, Ir and Sm had no effect on the transient signals, the addition of Lu and Mg(NO 3) 2 improved the sensitivity of the beryllium signal with respect to that obtained in the absence of modifier. Although, Mg(NO 3) 2 has improved the signal with respect to its sensitivity, it also increased the tail and the background (BG) signals, specially when urine samples are under study. Whereas, when Lu was used the analytical signal is virtually free of BG interference indicating that the urine matrix interference was almost eliminated. Besides, the addition of 6 μg of Lu ensured that the signals were effectively constant for five firings following the furnace program, which included: three drying, and the pyrolysis, atomization, cleaning and cooling steps. The effect of some components, likely to interfere in the accurate determination of beryllium (such as: Al, Ca, Cl, Co, Cr, Fe, Mg and Mn) were investigated. At the physiological levels, most of these elements had no effect, except in the case of chloride when Mg(NO 3) 2 was used as modifier. In this case, the tolerance limit was of 3000 mg Cl - l -1. The characteristic masses were 1.19, 0.45 and 0.48 pg, when integrated absorbance was measured for beryllium without the addition of any modifier and in the presence of Lu and Mg(NO 3) 2, respectively. The limits of detection (3σ) were 85, 19 and 58 fg, respectively. The accuracy and precision with the use of Lu and Mg(NO 3) 2 was tested for the direct determination of beryllium in urine samples. Quantification was performed with aqueous standards. The results obtained for the determination of beryllium in reference materials (Trace Elements in Urine), together with good recovery of spiked analyte, using either Lu or Mg(NO 3) 2 modification demonstrate the applicability of

  8. Determination of copper in airborne particulate matter using slurry sampling and chemical vapor generation atomic absorption spectrometry.

    PubMed

    Silva, Laiana O B; Leao, Danilo J; dos Santos, Debora C; Matos, Geraldo D; de Andrade, Jailson B; Ferreira, Sergio L C

    2014-09-01

    The present paper describes the development of a method for the determination of copper in airborne particulate matter using slurry sampling and chemical vapor generation atomic absorption spectrometry (CVG AAS). Chemometric tools were employed to characterize the influence of several factors on the generation of volatile copper species. First, a two-level full factorial design was performed that included the following chemical variables: hydrochloric acid concentration, tetrahydroborate concentration, sulfanilamide concentration and tetrahydroborate volume, using absorbance as the response. Under the established experimental conditions, the hydrochloric acid concentration had the greatest influence on the generation of volatile copper species. Subsequently, a Box-Behnken design was performed to determine the optimum conditions for these parameters. A second chemometric study employing a two-level full factorial design was performed to evaluate the following physical factors: tetrahydroborate flow rate, flame composition, alcohol volume and sample volume. The results of this study demonstrated that the tetrahydroborate flow rate was critical for the process. The chemometric experiments determined the following experimental conditions for the method: hydrochloric acid concentration, 0.208 M; tetrahydroborate concentration, 4.59%; sulfanilamide concentration, 0.79%; tetrahydroborate volume, 2.50 mL; tetrahydroborate flow rate, 6.50 mL min(-1); alcohol volume, 200 µL; and sample volume, 7.0 mL. Thus, this method, using a slurry volume of 500 µL and a final dilution of 7 mL, allowed for the determination of copper with limits of detection and quantification of 0.30 and 0.99 µg L(-1), respectively. Precisions, expressed as RSD%, of 4.6 and 2.8% were obtained using copper solutions at concentrations of 5.0 and 50.0 µg L(-1), respectively. The accuracy was evaluated by the analysis of a certified reference material of urban particulate matter. The copper concentration

  9. DIRECT DETERMINATION OF PHOSPHORUS IN GASOLINE BY FLAMELESS ATOMIC ABSORPTION SPECTROMETRY

    EPA Science Inventory

    A new method is presented for the determination of phosphorus in gasoline using flameless atomic absorption. Lanthanum nitrate solution is inserted in a graphite furnace prior to direct addition of gasoline. The organic matrix is charred prior to atomization of the phosphorus. Th...

  10. On-Line Synthesis and Analysis by Mass Spectrometry

    ERIC Educational Resources Information Center

    Bain, Ryan M.; Pulliam, Christopher J.; Raab, Shannon A.; Cooks, R. Graham

    2015-01-01

    In this laboratory experiment, students learn how to use ESI to accelerate chemical synthesis and to couple it with on-line mass spectrometry for structural analysis. The Hantzsch synthesis of symmetric 1,4-dihydropyridines is a classic example of a one-pot reaction in which multiple intermediates can serve to indicate the progress of the reaction…

  11. Multiple parallel mass spectrometry for lipid and vitamin D analysis

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Liquid chromatography (LC) coupled to mass spectrometry (MS) has become the method of choice for analysis of complex lipid samples. Two types of ionization sources have emerged as the most commonly used to couple LC to MS: atmospheric pressure chemical ionization (APCI) and electrospray ionization ...

  12. Method development for the determination of manganese, cobalt and copper in green coffee comparing direct solid sampling electrothermal atomic absorption spectrometry and inductively coupled plasma optical emission spectrometry.

    PubMed

    Oleszczuk, Nédio; Castro, Jacira T; da Silva, Márcia M; Korn, Maria das Graças A; Welz, Bernhard; Vale, Maria Goreti R

    2007-10-31

    A method has been developed for the determination of cobalt, copper and manganese in green coffee using direct solid sampling electrothermal atomic absorption spectrometry (SS-ET AAS). The motivation for the study was that only a few elements might be suitable to determine the origin of green coffee so that the multi-element techniques usually applied for this purpose might not be necessary. The three elements have been chosen as test elements as they were found to be significant in previous investigations. A number of botanical certified reference materials (CRM) and pre-analyzed samples of green coffee have been used for method validation, and inductively coupled plasma optical emission spectrometry (ICP OES) after microwave-assisted acid digestion of the samples as reference method. Calibration against aqueous standards could be used for the determination of Mn and Co by SS-ET AAS, but calibration against solid CRM was necessary for the determination of Cu. No significant difference was found between the results obtained with the proposed method and certified or independently determined values. The limits of detection for Mn, Cu and Co were 0.012, 0.006 and 0.004mugg(-1) using SS-ET AAS and 0.015, 0.13 and 0.10mugg(-1) using ICP OES. Seven samples of Brazilian green coffee have been analyzed, and there was no significant difference between the values obtained with SS-ET AAS and ICP OES for Mn and Cu. ICP OES could not be used as a reference method for Co, as essentially all values were below the limit of quantification of this technique. PMID:19073113

  13. Rapid Analysis of Isobaric Exogenous Metabolites by Differential Mobility Spectrometry Mass Spectrometry

    SciTech Connect

    Parson, Whitney B; Schneider, Bradley B; Kertesz, Vilmos; Corr, Jay; Covey, Thomas R.; Van Berkel, Gary J

    2011-01-01

    The direct separation of isobaric glucuronide metabolites from propranolol dosed tissue extracts by differential mobility spectrometry mass spectrometry (DMS-MS) with the use of a polar gas-phase chemical modifier was demonstrated. The DMS gas-phase separation was able to resolve the isobaric metabolites with separation times on the order of ms instead of mins to hrs typically required when using pre-ionization chromatographic separation methods. Direct separation of isobaric metabolites from the complex tissue extract was validated using standards as well as implementing an HPLC separation prior to the DMS-MS analysis to pre-separate the species of interest. The ability to separate isobaric exogenous metabolites directly from a complex tissue extract is expected to facilitate the drug development process by increasing analytical throughput without the requirement for pre-ionization cleanup or separation strategies.

  14. Ultra-violet and resonant laser ablation coupled with microwave induced plasma atomic emission spectrometry and determination of tin in nickel based alloys by electrothermal atomizer atomic absorption and laser excited atomic fluorescence spectrometry

    NASA Astrophysics Data System (ADS)

    Yang, Xiaodong

    Chapter 1 reviews laser ablation in analytical atomic spectrometry. Laser ablation is categorized into two functions: one is used as a sample introduction method, the other function is used as a microprobe analysis method. Both fundamental and applicational aspects are reviewed with the citations of related papers. This chapter also serves as an introduction to the work which is described in chapter 2 and chapter 3 as laser ablation is a relatively new research area for the research group. In chapter 2, instrumentation for excimer (308nm) laser ablation of samples was coupled with a microwave induced plasma (MLP), and evaluated for its potential as an approach to solid sampling for atomic emission spectrometry. Operating parameters were optimized, and the effects of laser repetition rate and number of laser shots on the emission signal were investigated. The UV excimer laser removed more material than would be expected of an infrared laser of similar energy. The chromium detection limit in the solid steel sample was estimated to be about 500 mug/g. In chapter 3, a wavelength tunable optical parametric oscillator (OPO) laser was used to ablate a steel sample into the same apparatus described in chapter 2. The emission signal for the elements was selectively enhanced when the ablation wavelength was tuned to be in resonance with any atomic transition of that element. This was the first report of the observation of resonant ablation by use of optical detection, as prior reports of resonant ablation have used mass spectrometric detectors. Chapter 4 reviews the publications in laser excited atomic fluorescence spectrometry in recent eight years. The focus of the review is on recent development on new instruments and applications of this technique. Chapter 5 studies the determination of tin in nickel-based alloys with laser excited atomic fluorescence in a graphite furnace. Zeeman electrothermal atomizer atomic absorption spectrometry and inductively coupled plasma mass

  15. 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.

  16. Diagnostics of reactive pulsed plasmas by UV and VUV absorption spectroscopy and by modulated beam Mass spectrometry

    NASA Astrophysics Data System (ADS)

    Cunge, Gilles

    2011-10-01

    Pulsed plasmas are promising for etching applications in the microelectronic industry. However, many new phenomena are involved when a high density discharge is pulsed. To better understand these processes it is necessary to probe the radicals' kinetics with a microsecond resolution. We have developed several diagnostics to reach this goal including broad band absorption spectroscopy with UV LEDs to detect small polyatomic radicals and with a deuterium VUV source to detect larger closed shell molecules and the modulated mass spectrometry to monitor atomic species. We will discuss the impact of the plasma pulsing frequency and duty cycle on the radical densities in Cl2 based plasmas, and the consequences on plasma processes. Work done in collaboration with Paul Bodart, Melisa Brihoum, Maxime Darnon, Erwin Pargon, Olivier Joubert, and Nader Sadeghi, CNRS/LTM.

  17. 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.

  18. 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.

  19. Speciation determination of chromium(III) and (VI) using preconcentration cloud point extraction with flame atomic absorption spectrometry (FAAS).

    PubMed

    Kiran, K; Kumar, K Suresh; Prasad, B; Suvardhan, K; Lekkala, Ramesh Babu; Janardhanam, K

    2008-02-11

    bis-[2-Hydroxy-1-naphthaldehyde] thiourea was synthesized and preconcentration cloud point extraction (CPE) for speciation determination of chromium(III) and (VI) in various environmental samples with flame atomic absorption spectrometry (FAAS) has been developed. Chromium(III) complexes with bis-[2-hydroxynaphthaldehyde] thiourea is subsequently entrapped in the surfactant micelles. After complexation of chromium(III) with reagent, the analyte was quantitatively extracted to the surfactant-rich phase in the non-ionic surfactant Triton X-100 after centrifugation. The effect of pH, concentration of chelating agent, surfactant, equilibration temperature and time on CPE was studied. The relative standard deviation was 2.13% and the limits of detection were around 0.18 microg L(-1). PMID:17583423

  20. Determination of trace amount of cobalt in feed grains and forages by solvent extraction and graphite furnace atomic absorption spectrometry.

    PubMed

    Blanchflower, W J; Cannavan, A; Kennedy, D G

    1990-10-01

    A method is described for the determination of trace amounts of cobalt in feed grains and forages with a detection limit of 1 ng g-1. Samples are ashed in a muffle furnace and complexed with 2-nitroso-1-naphthol. Following solvent extraction, cobalt is determined using graphite furnace atomic absorption spectrometry. The assay can be carried out in a normal analytical laboratory without the need for special "clean" rooms. Reagents have been selected to keep reagent blank values at low levels, and heptan-2-one is used as extracting solvent to avoid problems with evaporation. The assay has been used for diagnostic purposes and to formulate special low cobalt diets for sheep for experimental purposes. PMID:2270874

  1. Determination of cobalt in biological samples by line-source and high-resolution continuum source graphite furnace atomic absorption spectrometry using solid sampling or alkaline treatment

    NASA Astrophysics Data System (ADS)

    Ribeiro, Anderson Schwingel; Vieira, Mariana Antunes; da Silva, Alessandra Furtado; Borges, Daniel L. Gallindo; Welz, Bernhard; Heitmann, Uwe; Curtius, Adilson José

    2005-06-01

    Two procedures for the determination of Co in biological samples by graphite furnace atomic absorption spectrometry (GF AAS) were compared: solid sampling (SS) and alkaline treatment with tetramethylammonium hydroxide (TMAH) using two different instruments for the investigation: a conventional line-source (LS) atomic absorption spectrometer and a prototype high-resolution continuum source atomic absorption spectrometer. For the direct introduction of the solid samples, certified reference materials (CRM) were ground to a particle size ≤50 μm. Alkaline treatment was carried out by placing about 250 mg of the sample in polypropylene flasks, adding 2 mL of 25% m/v tetramethylammonium hydroxide and de-ionized water. Due to its unique capacity of providing a 3-D spectral plot, a high-resolution continuum source (HR-CS) graphite furnace atomic absorption spectrometry was used as a tool to evaluate potential spectral interferences, including background absorption for both sample introduction procedures, revealing that a continuous background preceded the atomic signal for pyrolysis temperatures lower than 700 °C. Molecular absorption bands with pronounced rotational fine structure appeared for atomization temperatures >1800 °C probably as a consequence of the formation of PO. After optimization had been carried out using high resolution continuum source atomic absorption spectrometry, the optimized conditions were adopted also for line-source atomic absorption spectrometry. Six biological certified reference materials were analyzed, with calibration against aqueous standards, resulting in agreement with the certified values (according to the t-test for a 95% confidence level) and in detection limits as low as 5 ng g -1.

  2. 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).

  3. Evaluation of quartz tubes as atomization cells for gold determination by thermospray flame furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Morzan, Ezequiel; Piano, Ornela; Stripeikis, Jorge; Tudino, Mabel

    2012-11-01

    This work describes the development of a new analytical procedure able to determine gold by thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) using nickel tubes (NiT) and quartz tubes (QT) as atomization cells. Experiments involving changes in the flow injection operational parameters, reagent concentrations and sizes of the QT were performed in order to optimize sensitivity. Under the same operational conditions, it was observed that the employment of QT increases the sensitivity of gold determination when compared to the nickel tube. Since solutions of highly concentrated hydrochloric acid showed the best performance as carriers, quartz tubes were also preferred due to its greater tolerance to corrosion by mineral acids in comparison to NiT. In addition, changes in the internal diameter of the QT revealed an important improvement in sensitivity for smaller tubes. Under optimized conditions the main figures of merit showed values close to that of graphite furnace atomic absorption spectrometry with the addition of an excellent improvement of the sample throughput. They are: LOD (3 s): 0.004 μg mL- 1, sensitivity: 0.306 (μg mL- 1)- 1, RSD% (n = 10, 1 μg mL- 1): 2.5, linear range: 0.01-4 μg mL- 1 and sample throughput: 72 h- 1. This new method was employed for the determination of gold in homeopathic medicines with no need of sample digestion. Validation of the analytical results will be shown. A full discussion of the most relevant findings regarding the role of the atomization cell as a strategic key for improving sensitivity will be also provided.

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

    NASA Astrophysics Data System (ADS)

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

    2005-06-01

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

  5. Total hydrocarbon analysis by ion mobility spectrometry

    NASA Technical Reports Server (NTRS)

    Cross, John H.; Limero, Thomas F.; James, John T.

    1994-01-01

    Astronauts must be alerted quickly to chemical leaks that compromise their health and the success of their missions. An ideal leak detector would be equally sensitive to all compounds that might constitute a hazard and insensitive to nontoxic compounds. No ideal sensor exists; thus, selection of a methodology is a series of compromises. The commonly used methods are either insensitive at the low exposure levels set by OSHA, NASA, and other organizations or are selectively insensitive to important classes of chemicals such as Freons. After extensive study and experience, the Toxicology Group at JSC has selected ion mobility spectrometry (IMS) for development into a broad range, sensitive detector. In addition to the sensing method, signal processing is important leak detection because a background signal can be expected at all times. The leak-detecting instrument must be programmed to discriminate between authentic leaks and background fluctuations caused by routine operations. The results of an evaluation of the prototype THA is presented in terms related to spacecraft operations. The evaluation included determination of instrumental parameters such as stability and response times. We also included responses to some common components of spacecraft atmospheres in pure form and in binary and ternary mixtures. The output of the four algorithms to the mixtures was found to be noticeably different. These responses are compared on the basis of their utility for signaling a chemical leak. As a means of evaluating its resistance to a falsely positive response, the THA was challenged with carbon dioxide and methane, compounds whose concentrations normally increase in spacecraft air during human habitation. The instrument showed virtually no response to these interferences. Although the prototype THA is designed for space flight, this detector is expected to be useful for field screening at chemical waste dumps and other environmentally sensitive locations.

  6. Fast sequential determination of antimony and lead in pewter alloys using high-resolution continuum source flame atomic absorption spectrometry.

    PubMed

    Dessuy, Morgana B; de Jesus, Robson M; Brandao, Geovani C; Ferreira, Sergio L C; Vale, Maria Goreti R; Welz, Bernhard

    2013-01-01

    A simple method has been developed to determine antimony and lead in pewter alloy cups produced in Brazil, using fast sequential determination by high-resolution continuum source flame atomic absorption spectrometry. The samples were dissolved in HCl and H(2)O(2), employing a cold finger system in order to avoid analyte losses. The main resonance line of lead at 217.001 nm and a secondary line of antimony at 212.739 nm were used. The limits of detection for lead and antimony were 0.02 and 5.7 mg L(-1), respectively. The trueness of the method was established by recovery tests and comparing the results obtained by the proposed method with those obtained by inductively coupled plasma optical emission spectrometry. The results were compared using a student's t-test and there was no significant difference at a 95% confidence interval. With the developed methods, it was possible to determine accurately antimony and lead in pewter samples. The lead concentration found in the analysed samples was around 1 mg g(-1), which means that they are not lead free; however, the content was below the maximum allowed level of 5 mg g(-1). The antimony content, which was found to be between 40 and 46 mg g(-1), is actually of greater concern, as antimony is known to be potentially toxic already at very low concentrations, although there is no legislation yet for this element. PMID:23046152

  7. Determination of chlorine in food samples via the AlCl molecule using high-resolution continuum source molecular absorption spectrometry in a graphite furnace

    NASA Astrophysics Data System (ADS)

    Fechetia, Miriam; Tognon, André Luiz; da Veiga, Márcia A. M. S.

    2012-05-01

    Determination of chlorine using the molecular absorption of aluminum mono-chloride (AlCl) at the 261.418 nm wavelength was accomplished by high-resolution continuum source molecular absorption spectrometry using a transversely heated graphite tube furnace with an integrated platform. For the analysis, 10 μL of the sample followed by 10 μL of a solution containing Al-Ag-Sr modifier, (1 g L- 1 each), were directly injected onto the platform. A spectral interference due to the use of Al-Ag-Sr as mixed modifier was easily corrected by the least-squares algorithm present in the spectrometer software. The pyrolysis and vaporization temperatures were 500 °C and 2200 °C, respectively. To evaluate the feasibility of a simple procedure for the determination of chlorine in food samples present in our daily lives, two different digestion methods were applied, namely (A) an acid digestion method using HNO3 only at room temperature, and (B) a digestion method with Ag, HNO3 and H2O2, where chlorine is precipitated as a low-solubility salt (AgCl), which is then dissolved with ammonia solution. The experimental results obtained with method B were in good agreement with the certified values and demonstrated that the proposed method is more accurate than method A. This is because the formation of silver chloride prevented analyte losses by volatilization. The limit of detection (LOD, 3σ/s) for Cl in methods A and B was 18 μg g- 1 and 9 μg g- 1, respectively, 1.7 and 3.3 times lower compared to published work using inductively coupled plasma optical emission spectrometry, and absolute LODs were 2.4 and 1.2 ng, respectively.

  8. Estimation of boron isotope ratios using high resolution continuum source atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Wiltsche, Helmar; Prattes, Karl; Zischka, Michael; Knapp, Günter

    2009-04-01

    In the production of 10B enriched steels, the production-recycling process needs to be closely monitored for inadvertent mix-up of materials with different B isotope levels. A quick and simple method for the estimation of boron isotope ratios in high alloyed steels using high resolution continuum source flame AAS (HR-CS-FAAS) was developed. On the 208.9 nm B line the wavelength of the peak absorption of 10B and 11B differs by 2.5 pm. The wavelength of the peak absorption of boron was determined by fitting a Gauss function through spectra simultaneously recorded by HR-CS-FAAS. It was shown that a linear correlation between the wavelength of the peak absorption and the isotope ratio exists and that this correlation is independent of the total boron concentration. Internal spectroscopic standards were used to compensate for monochromator drift and monochromator resolution changes. Accuracy and precision of the analyzed samples were thereby increased by a factor of up to 1.3. Three steel reference materials and one boric acid CRM, each certified for the boron isotope ratio were used to validate the procedure.

  9. Surfactant/oil/water system for the determination of selenium in eggs by graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Ieggli, C. V. S.; Bohrer, D.; Noremberg, S.; do Nascimento, P. C.; de Carvalho, L. M.; Vieira, S. L.; Reis, R. N.

    2009-06-01

    An oil-in-water formulation has been optimized to determine trace levels of selenium in whole hen eggs by graphite furnace atomic absorption spectrometry. This method is simpler and requires fewer reagents when compared with other sample pre-treatment procedures. Graphite furnace atomic absorption spectrometric (GF AAS) measurement was carried out using standard addition calibration and Pd as a modifier. The precision, expressed as relative standard deviation, was better than 5% and the limit of detection was 1 µg L - 1 . The validation of the method was performed against a standard reference material Whole Egg Powder (RM 8415), and the measured Se corresponded to 95.2% of the certified value. The method was used for the determination of the Se level in eggs from hens treated with Se dietary supplements. Inorganic and organic Se sources were added to hen feed. The Se content of eggs was higher when hens were fed with organic Se compared to the other treatments. The proposed method, including sample emulsification for subsequent Se determination by GF AAS has proved to be sensitive, reproducible, simple and economical.

  10. 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 analysis, micro-scale distribution of fluorine in the samples was also determined. PMID:27283621

  11. Automatic microemulsion preparation for metals determination in fuel samples using a flow-batch analyzer and graphite furnace atomic absorption spectrometry.

    PubMed

    Cunha, Francisco Antônio S; Sousa, Rafael A; Harding, David P; Cadore, Solange; Almeida, Luciano F; Araújo, Mário César U

    2012-05-21

    The principal thermodynamic advantages of using microemulsions over standard emulsions for flow metal analysis are the greatly increased analyte stability and emulsive homogeneity that improve both the ease of sample preparation, and the analytical result. In this study a piston propelled flow-batch analyzer (PFBA) for the determination of Cu, Cr and Pb in gasoline and naphtha by graphite furnace atomic absorption spectrometry (GF AAS) was explored. Investigative phase modeling for low dilution was conducted both for gasoline and naphtha microemulsions. Rheological considerations were also explored including a mathematical flow derivation to fine tune the system's operational parameters, and the GF AAS coupling. Both manual and automated procedures for microemulsion preparation were compared. The results of the paired t test at a 95% confidence level showed no significant differences between them. Further recovery test results confirmed a negligible matrix effect of the sample on the analyte absorption signals and an efficient stabilization of the samples (with metals) submitted to microemulsion treatment. The accuracy of the developed procedure was attested by good recovery percentages in the ranges of 100.0±3.5% for Pb in the naphtha samples, and 100.2±3.4% and 100.7±4.6% for Cu and Cr, respectively in gasoline samples. PMID:22541820

  12. 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.

  13. Speciation of arsenic(III)/arsenic(V) and selenium(IV)/ selenium(VI) using coupled ion chromatography - hydride generation atomic absorption spectrometry

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Simple analytical methods have been developed to speciate inorganic arsenic and selenium in the ppb range using coupled ion chromatography-hydride generation atomic absorption spectrometry. Because of the differences in toxicity and adsorption behavior, determinations of the redox states arsenite A...

  14. Direct determination of particulate elements in edible oils and fats using an ultrasonic slurry sampler with graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    van Dalen, Gerard; de Galan, Leo

    1994-12-01

    Through the use of an ultrasonic slurry mixer, graphite furnace atomic absorption spectrometry (GFAAS) can be applied for the fully automated determination of particulate iron and nickel in edible oils and fats. The unsupervised ultrasonic slurry autosampler yields the same accuracy and somewhat better precision than the much more laborious manual GFAAS method.

  15. Determination of mercury in soils and sediments by graphite furnace atomic absorption spectrometry with slurry sampling

    NASA Astrophysics Data System (ADS)

    López-García, Ignacio; Sánchez-Merlos, Mateo; Hernández-Córdoba, Manuel

    1997-12-01

    A graphite furnace atomic absorption spectrometric procedure for the determination of mercury is presented, in which the samples are suspended in a solution containing hydrofluoric and nitric acids. Silver nitrate (4% m/v) and potassium permanganate (3%) are incorporated, in the order specified, and aliquots are directly introduced into the graphite furnace. A fast heating programme with no conventional pyrolysis step is used. The detection limit for mercury in a 125 mg ml -1 suspension is 0.1 μg g -1. Calibration is performed by using aqueous standards. The reliability of the procedure is proved by analysing certified reference materials.

  16. Determination of sulphur in various vegetables by solid sampling high-resolution electrothermal molecular absorption spectrometry.

    PubMed

    Gunduz, Sema; Akman, Suleyman

    2015-04-01

    Sulphur was determined in various vegetables via molecular absorption of carbon monosulphide (CS) at 258.056 nm using a solid sampling high resolution continuum source electrothermal atomic absorption spectrometer (SS HR-CS ETAAS). Samples were dried, ground and directly introduced into the ruthenium coated graphite furnace as 0.05 to 0.50mg. All determinations were performed using palladium+citric acid modifier and applying a pyrolysis temperature of 1000 °C and a volatilisation temperature of 2400 °C. The results were in good agreement with certified sulphur concentrations of various vegetal CRM samples applying linear calibration technique prepared from thioacetamide. The limit of detection and characteristic mass of the method were 7.5 and 8.7 ng of S, respectively. The concentrations of S in various spinach, leek, lettuce, radish, Brussels sprouts, zucchini and chard samples were determined. It was showed that distribution of sulphur in CRM and grinded food samples were homogeneous even in micro-scale. PMID:25442545

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

    PubMed

    Burguera-Pascu, Margarita; Rodríguez-Archilla, Alberto; Burguera, José Luis; Burguera, Marcela; Rondón, Carlos; Carrero, Pablo

    2007-09-26

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

  18. Linked Gas Chromatography/Fourier Transform Infrared Spectrometry/Fourier Transform Mass Spectrometry For Mixture Analysis

    NASA Astrophysics Data System (ADS)

    Laude, David A., Jr.; Johlman, Carolyn; Wilkins, Charles L.

    1985-12-01

    During the past few years it has been demonstrated that linkage of multiple spectrometry systems with gas chromatography (GC) offers significant advantages for structural analysis of mixture components as they are sepa-rated. In the work to be described, a Fourier transform mass spectrometer (FTMS) has been linked in parallel with a Fourier transform infrared (FTIR) spectrometer for concurrent analysis of GC eluants from a fused silica capillary column. This system provides FTIR, electron impact, and chemical ionization mass spectral analysis of each mixture component as it emerges from the GC. Furthermore, mass measurement accuracy in the low ppm range in the absence of calibrant is made possible by the FTMS. Effective use of the com-plementary information obtained is shown to produce more reliable analytical performance than for any individual measurement.

  19. [Preliminary study on using acousto-optic tunable filter as wavelength selector for atomic absorption spectrometry].

    PubMed

    Zhao, Li-wei; Zhang, Yi-hua; Wang, Mei-jia; Song, Da-qian; Zhang, Han-qi; Jin, Qin-han

    2002-06-01

    An acousto-optic tunable filter (AOTF) is an all-solid-state, electronic monochromator that is based on the diffraction of light by an acoustic wave in an anisotropic crystal. It is a new kind of tunable small filter with narrow band compared with traditional unicolor filter. The filter can diffract incident white light at a specific wavelength when a specific radio frequency is applied into it. An AAS experimental setup using a microwave plasma torch (MPT) as the atomizer, and a visible AOTF as the wavelength selector was developed and the analytical performance was evaluated by determination of Na. The effect on the absorption signal of some operating conditions, including the observation height, the microwave forward power and the carrier and support gas flow rates for MPT, were investigated. The detection limit for Na was shown to be 0.23 microgram.mL-1 and the relative standard deviation was 2.6% (n = 6). PMID:12938338

  20. Arsenic Speciation of Waters from the Aegean Region, Turkey by Hydride Generation: Atomic Absorption Spectrometry.

    PubMed

    Çiftçi, Tülin Deniz; Henden, Emur

    2016-08-01

    Arsenic in drinking water is a serious problem for human health. Since the toxicity of arsenic species As(III) and As(V) is different, it is important to determine the concentrations separately. Therefore, it is necessary to develop an accurate and sensitive method for the speciation of arsenic. It was intended with this work to determine the concentrations of arsenic species in water samples collected from Izmir, Manisa and nearby areas. A batch type hydride generation atomic absorption spectrometer was used. As(V) gave no signal under the optimal measurement conditions of As(III). A certified reference drinking water was analyzed by the method and the results showed excellent agreement with the reported values. The procedure was applied to 34 water samples. Eleven tap water, two spring water, 19 artesian well water and two thermal water samples were analyzed under the optimal conditions. PMID:27236436

  1. 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.

  2. Determination of methane emission rates on a biogas plant using data from laser absorption spectrometry.

    PubMed

    Groth, Angela; Maurer, Claudia; Reiser, Martin; Kranert, Martin

    2015-02-01

    The aim of the work was to establish a method for emission control of biogas plants especially the observation of fugitive methane emissions. The used method is in a developmental stage but the topic is crucial to environmental and economic issues. A remote sensing measurement method was adopted to determine methane emission rates of a biogas plant in Rhineland-Palatinate, Germany. An inverse dispersion model was used to deduce emission rates. This technique required one concentration measurement with an open path tunable diode laser absorption spectrometer (TDLAS) downwind and upwind the source and basic wind information, like wind speed and direction. Different operating conditions of the biogas plant occurring on the measuring day (December 2013) could be represented roughly in the results. During undisturbed operational modes the methane emission rate averaged 2.8 g/s, which corresponds to 4% of the methane gas production rate of the biogas plant. PMID:25446786

  3. Direct analysis of traditional Chinese medicines by mass spectrometry.

    PubMed

    Wong, Melody Yee-Man; So, Pui-Kin; Yao, Zhong-Ping

    2016-07-15

    Analysis of traditional Chinese medicines (TCMs) plays important roles in quality control of TCMs and understanding their pharmacological effects. Mass spectrometry (MS) is a technique of choice for analysis of TCMs due to its superiority in speed, sensitivity and specificity. However, conventional MS analysis of TCMs typically requires extensive sample pretreatment and chromatographic separation, which could be time-consuming and laborious, prior to the analysis. The expanding usage of TCMs worldwide demands development of rapid, cost-effective and reliable methods for analysis of TCMs. In recent years, new sample preparation and ionization techniques have been developed to enable direct analysis of TCMs by MS, significantly reducing the analysis time and cost. In this review, various MS-based techniques, mainly including ambient ionization-MS and MALDI-MS based techniques, applied for direct analysis of TCMs are summarized and their applicability and future prospects are discussed. PMID:26657800

  4. Spectral aspects of the determination of Si in organic and aqueous solutions using high-resolution continuum source or line source flame atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Kowalewska, Zofia; Pilarczyk, Janusz; Gościniak, Łukasz

    2016-06-01

    High-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS) was applied to reveal and investigate spectral interference in the determination of Si. An intensive structured background was observed in the analysis of both aqueous and xylene solutions containing S compounds. This background was attributed to absorption by the CS molecule formed in the N2O-C2H2 flame. The lines of the CS spectrum at least partially overlap all five of the most sensitive Si lines investigated. The 251.611 nm Si line was demonstrated to be the most advantageous. The intensity of the structured background caused by the CS molecule significantly depends on the chemical form of S in the solution and is the highest for the most-volatile CS2. The presence of O atoms in an initial S molecule can diminish the formation of CS. To overcome this S effect, various modes of baseline fitting and background correction were evaluated, including iterative background correction (IBC) and utilization of correction pixels (WRC). These modes were used either independently or in conjunction with least squares background correction (LSBC). The IBC + LSBC mode can correct the extremely strong interference caused by CS2 at an S concentration of 5% w:w in the investigated solution. However, the efficiency of this mode depends on the similarity of the processed spectra and the correction spectra in terms of intensity and in additional effects, such as a sloping baseline. In the vicinity of the Si line, three lines of V were recorded. These lines are well-separated in the HR-CS FAAS spectrum, but they could be a potential source of overcorrection when using line source flame atomic absorption spectrometry (LS FAAS). The expected signal for the 251.625 nm Fe line was not registered at 200 mg L- 1 Fe concentration in the solution, probably due to the diminished population of Fe atoms in the high-temperature flame used. The observations made using HR-CS FAAS helped to establish a "safe" level

  5. Determination of Cd, Cr, Cu, Pb and Zn in human semen by graphite furnace atomic absorption spectrometry after microwave sample dissolution.

    PubMed

    Alvarado, J; Moreno, R; Cristiano, A R

    1991-09-01

    Human semen samples were analyzed by graphite furnace atomic absorption spectrometry, using L'vov platforms and the method of standard additions, to determine their Cd, Cr, Cu, Pb and Zn content. The samples were analyzed directly and after conventional and microwave wet acid dissolution. Matrix modification, using magnesium and palladium nitrates and ammonium biphosphate solutions, was evaluated for the analysis of the microwave-digested samples. The best results were obtained for Cr, Cu and Zn using Pd(NO3)2, and a mixture of Mg(NO3)2 and Pd(NO3)2 solutions. The direct analysis of water-diluted semen produced inaccurate results with unacceptably high standard deviations. The results obtained for the microwave-dissolved samples showed relative standard deviation values within the range 0.63-8.4%. The analysis of spiked semen solutions showed recoveries of the added analytes ranging from 96 to 104%. The accuracy of the measurements was checked against the NIST 1,577a, bovine liver, standard reference material. Sample dissolution time was drastically reduced from 3-4 hours, using the conventional method, to approximately 8 minutes using the microwave-assisted wet acid digestion procedure. PMID:1821719

  6. Determination of total tin in environmental biological and water samples by atomic absorption spectrometry with graphite furnace.

    PubMed

    Dogan, S; Haerdi, W

    1980-01-01

    Analysis of traces of tin using several analytical techniques (X-ray fluorescence, neutron activation, polarographic techniques and atomic absorption) have been tested. Parameters such as simplicity, rapidity, sensitivity and interferences are compared in order to choose the most useful method for practical purpose. Finally, flameless atomic absorption was chosen for the determination of total tin concentration in different natural samples. Digestion of biological samples (plant, plankton, fish, etc.) was achieved by using Lumatom (a trade organic chemical). Thus, the digested sample is directly injected into the graphite furnace. This digestion technique is suitable and rapid with a minimum of error (contamination and losses). For tin analysis in water samples, a preconcentration of tin is carried out by coprecipitation with 1, 10-phenanthroline and tetraphenyl boron. The precipitate is separated and dissolved in alcohol or in Lumatom. The sensitivity of this method is 0.1 ng absolute tin. PMID:7451013

  7. Slurry sampling graphite furnace atomic absorption spectrometry: determination of trace metals in mineral coal.

    PubMed

    Silva, M M; Goreti, M; Vale, R; Caramão, E B

    1999-12-01

    A procedure for lead, cadmium and copper determination in coal samples based on slurry sampling using an atomic absorption spectrometer equipped with a transversely heated graphite tube atomizer is proposed. The slurries were prepared by weighing the samples directly into autosampler cups (5-30 mg) and adding a 1.5 ml aliquot of a diluent mixture of 5% v/v HNO(3), 0.05% Triton X-100 and 10% ethanol. The slurry was homogenized by manual stirring before measurement. Slurry homogenization using ultrasonic agitation was also investigated for comparison. The effect of particle size and the use of different diluent compositions on the slurry preparation were investigated. The temperature programmes were optimized on the basis of pyrolysis and atomization curves. Absorbance characteristics with and without the addition of a palladium-magnesium modifier were compared. The use of 0.05% m/v Pd and 0.03% m/v Mg was found satisfactory for stabilizing Cd and Pb. The calibration was performed with aqueous standards. In addition, a conventional acid digestion procedure was applied to verify the efficiency of the slurry sampling. Better recoveries of the analytes were obtained when the particle size was reduced to <37 mum. Several certified coal reference materials (BCR Nos. 40, 180, and 181) were analyzed, and good agreement was obtained between the results from the proposed slurry sampling method and the certificate values. PMID:18967798

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

    USGS Publications Warehouse

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

    1990-01-01

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

  9. Direct determination of fluorine in niobium oxide using slurry sampling electrothermal high-resolution continuum source molecular absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Huang, Mao Dong; Becker-Ross, Helmut; Okruss, Michael; Geisler, Sebastian; Florek, Stefan; Richter, Silke; Meckelburg, Angela

    Aiming for a round-robin test, a new method for the direct determination of fluorine in niobium oxide has been developed. It is based on the use of high-resolution molecular absorption spectra of calcium mono-fluoride (CaF) generated in the graphite tube, combined with the slurry sampling technique. The absorption measurement was performed at the 606.44 nm CaF rotational line. By using graphite tubes with zirconium carbide (ZrC) modified platform, the molecular absorption sensitivity of CaF has been improved by a factor of 20, and no additional chemical modifier was necessary. Generally, non-spectral interferences were observed in the presence of HCl, H2SO4, and H3PO4. For HCl, additional spectral interference occurred due to an overlap of the absorption spectra of CaF and CaCl. However, due to the absence of these mentioned substances in the current material, such interferences do not exist for this application. The characteristic mass found for the CaF 606.44 nm line was 0.1 ng; the limit of detection was 5 mg fluorine per kg solid sample (3σ criterion). The results obtained by the method were within the range of certified values. Comparing to the classical method such as the pyrohydrolysis-photometric method, the developed new method showed clear advantages regarding sensitivity and specificity. The time requirement for one sample analysis was strongly shortened from several hours to only some minutes.

  10. Human Vitamin B12 Absorption and Metabolism are Measured by Accelerator Mass Spectrometry Using Specifically Labeled 14C-Cobalamin

    SciTech Connect

    Carkeet, C; Dueker, S R; Lango, J; Buchholz, B A; Miller, J W; Green, R; Hammock, B D; Roth, J R; Anderson, P J

    2006-01-26

    There is need for an improved test of human ability to assimilate dietary vitamin B{sub 12}. Assaying and understanding absorption and uptake of B{sub 12} is important because defects can lead to hematological and neurological complications. Accelerator mass spectrometry (AMS) is uniquely suited for assessing absorption and kinetics of {sup 14}C-labeled substances after oral ingestion because it is more sensitive than decay counting and can measure levels of carbon-14 ({sup 14}C) in microliter volumes of biological samples, with negligible exposure of subjects to radioactivity. The test we describe employs amounts of B{sub 12} in the range of normal dietary intake. The B{sub 12} used was quantitatively labeled with {sup 14}C at one particular atom of the DMB moiety by exploiting idiosyncrasies of Salmonellametabolism. In order to grow aerobically on ethanolamine, S. entericamust be provided with either pre-formed B{sub 12} or two of its precursors: cobinamide and dimethylbenzimidazole (DMB). When provided with {sup 14}C-DMB specifically labeled in the C2 position, cells produced {sup 14}C-B{sub 12} of high specific activity (2.1 GBq/mmol, 58 mCi/mmol) and no detectable dilution of label from endogenous DMB synthesis. In a human kinetic study, a physiological dose (1.5 mg, 2.2 KBq/59 nCi) of purified {sup 14}C-B{sub 12} 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 B{sub 12} assimilation.

  11. Application of wavelet transforms to determine peak shape parameters for interference detection in graphite-furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Sadler, D. A.; Littlejohn, D.; Boulo, P. R.; Soraghan, J. S.

    1998-08-01

    A procedure to quantify the shape of the absorbance-time profile, obtained during graphite furnace atomic absorption spectrometry, has been used to detect interference effects caused by the presence of a concomitant salt. The quantification of the absorption profile is achieved through the use of the Lipschitz regularity, α0, obtained from the wavelet transform of the absorbance-time profile. The temporal position of certain features and their associated values of α0 provide a unique description of the shape of the absorbance-time profile. Changes to the position or values of α0 between standard and sample atomizations may be indicative of uncorrected interference effects. A weak, but linear, dependence was found of the value of α0 upon the analyte concentration for Cr and Cu. The ability of the Lipschitz regularity to detect interference effects was illustrated for Pb, Se and Cu. For Pb, the lowest concentration of NaCl added, 0.005% m/v, changed both the values of α0 and the peak height absorbance. For Se, no change in the peak height and peak area absorbance signals was detected up to a NaCl concentration of 0.25% m/v. The values of the associated Lipschitz regularities were found to be invariant to NaCl concentration up to this value. For Cu, a concentration of 0.05% m/v NaCl reduced the peak height and peak area absorbance signals by approximately 25% and significantly altered the values of α0.

  12. A new derivative for oxosteroid analysis by mass spectrometry

    PubMed Central

    Rigdova, K.; Wang, Y.; Ward, M.; Griffiths, W.J.

    2014-01-01

    Here we report a new method for oxosteroid identification utilizing “tandem mass tag hydrazine” (TMTH) carbonyl-reactive derivatisation reagent. TMTH is a reagent with a chargeable tertiary amino group attached through a linker to a carbonyl-reactive hydrazine group. Thirty oxosteroids were analysed after derivatisation with TMTH by electrospray ionization mass spectrometry (ESI-MS) and were found to give high ion-currents compared to underivatised molecules. ESI-tandem mass spectrometry (MS/MS) analysis of the derivatives yielded characteristic fragmentation patterns with specific mass reporter ions derived from the TMT group. A shotgun ESI-MS method incorporating TMTH derivatisation was applied to a urine sample. PMID:24525129

  13. Analysis of tear glucose concentration with electrospray ionization mass spectrometry.

    PubMed

    Taormina, Christopher R; Baca, Justin T; Asher, Sanford A; Grabowski, Joseph J; Finegold, David N

    2007-02-01

    We have developed a mass spectrometry-based method that allows one to accurately determine the glucose concentration of tear fluid. We used a 1 microL micro-capillary to collect tear fluid from the tear meniscus with minimal irritation of the eye. We analyzed the 1 muL volume of collected tear fluid with liquid-chromatography electrospray ionization mass spectrometry with the use of D-glucose-6,6-d2 as an internal standard. Repeated measurements and a recovery experiment on pooled, onion-induced tears showed that the analysis of the glucose in tears was precise (4% relative standard deviation) and provided 100% recovery. We found the tear glucose concentration of one fasting nondiabetic subject to be 13 to 51 microM while the onion-induced tear glucose concentration of a different nondiabetic subject to be 211 to 256 microM. PMID:17084090

  14. Analysis of Tear Glucose Concentration with Electrospray Ionization Mass Spectrometry

    PubMed Central

    Taormina, Christopher R.; Baca, Justin T.; Finegold, David N.; Asher, Sanford A.; Grabowski, Joseph J.

    2007-01-01

    We have developed a mass spectrometry-based method which allows one to accurately determine the glucose concentration of tear fluid. We used a 1 μL micro-capillary to collect tear fluid from the tear meniscus with minimal irritation of the eye. We analyzed the 1 μL volume of collected tear fluid with liquid-chromatography electrospray ionization mass spectrometry with the use of D-glucose-6,6-d2 as an internal standard. Repeated measurements and a recovery experiment on pooled, onion-induced tears showed that the analysis of the glucose in tears was precise (4% relative standard deviation) and provided 100% recovery. We found the tear glucose concentration of one fasting non-diabetic subject to be 13 to 51 μM while the onion-induced tear glucose concentration of a different non-diabetic subject to be 211 to 256 μM. PMID:17084090

  15. Matrix elimination method for the determination of precious metals in ores using electrothermal atomic absorption spectrometry.

    PubMed

    Salih, Bekir; Celikbiçak, Omür; Döker, Serhat; Doğan, Mehmet

    2007-03-28

    Poly(N-(hydroxymethyl)methacrylamide)-1-allyl-2-thiourea) hydrogels, poly(NHMMA-ATU), were synthesized by gamma radiation using (60)Co gamma source in the ternary mixture of NHMMA-ATU-H(2)O. These hydrogels were used for the specific gold, silver, platinum and palladium recovery, pre-concentration and matrix elimination from the solutions containing trace amounts of precious metal ions. Elimination of inorganic matrices such as different transition and heavy metal ions, and anions was performed by adjusting the solution pH to 0.5 that was the selective adsorption pH of the precious metal ions. Desorption of the precious metal ions was performed by using 0.8 M thiourea in 3M HCl as the most efficient desorbing agent with recovery values more than 95%. In the desorption medium, thiourea effect on the atomic signal was eliminated by selecting proper pyrolysis and atomization temperatures for all precious metal ions. Precision and the accuracy of the results were improved in the graphite furnace-atomic absorption spectrometer (GFAAS) measurements by applying the developed matrix elimination method performing the adsorption at pH 0.5. Pre-concentration factors of the studied precious metal ions were found to be at least 1000-fold. Detection limits of the precious metal ions were found to be less than 10 ng L(-1) of the all studied precious metal ions by using the proposed pre-concentration method. Determination of trace levels of the precious metals in the sea-water, anode slime, geological samples and photographic fixer solutions were performed using GFAAS clearly after applying the adsorption-desorption cycle onto the poly(NHMMA-UTU) hydrogels. PMID:17386783

  16. On-site analysis of old deposited chemical warfare agents by combined use of ion mobility spectrometry and mass spectrometry

    SciTech Connect

    Stach, J.; Adler, J.; Brodacki, M.; Doering, H.R.; Flachowsky, J.; Loudon, A.

    1995-12-31

    The factory site of an old mustard gas plant was investigated with on-site analysis methods. Using ion mobility spectrometry and mass spectrometry a lot of degradation products of mustard gas could be detected. Sulfur mustard was found in one soil sample and in ceramic material of a bunker used for storage of the produced warfare agents. Concentrations of the mustard gas are in the sub ppb level. The results of ion mobility and mass spectrometry agreed in 95 % of the investigated samples.

  17. ACORNS: Analysis of Correlations Used in Neutron Spectrometry

    1988-05-01

    The program ACORNS performs the complete analysis of the input covariance and/or relative covariance and/or correlation matrices, first of all used in the activation neutron spectrometry. These matrices have to be positive definite. To check the fulfillment of this requirement, the program calculates the eigenvalues and eigenvectors of those. If all the eigenvalues are positive, the program optionally performs the factor analysis. The user's input can be either made manually, or the cross section librariesmore » generated by the code X333.« less

  18. Determination of trace amounts of molybdenum in plant tissue by solvent extraction-atomic-absorption and direct-current plasma emission spectrometry.

    PubMed

    Lajunen, L H; Kubin, A

    1986-03-01

    Methods are presented for determination of molybdenum in plant tissue by flame and graphite-furnace atomic-absorption spectrometry and direct-current argon-plasma emission spectrometry. The samples are digested in HNO(3)-H(2)SO(4)-HC1O(4) mixture, and Mo is separated and concentrated by chelation and extraction. Three organic solvents (methyl isobutyl ketone, di-isobutyl ketone and isoamyl alcohol) and two ligands (8-hydroxyquinoline and toluene-3,4-dithiol) were studied. The procedure were tested on pine needle and birch leaf samples. PMID:18964076

  19. Determination of lead, cadmium and mercury in blood for assessment of environmental exposure: A comparison between inductively coupled plasma mass spectrometry and atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Palmer, Christopher D.; Lewis, Miles E.; Geraghty, Ciaran M.; Barbosa, Fernando; Parsons, Patrick J.

    2006-08-01

    A biomonitoring method for the determination of Pb, Cd, and Hg at background levels in whole blood by inductively coupled plasma-mass spectrometry is described. While this method was optimized for assessing Pb, Cd and Hg at environmental levels, it also proved suitable for assessing concentrations associated with occupational exposure. The method requires as little as 200 μl of blood that is diluted 1 + 49 for direct analysis in the inductively coupled plasma-mass spectrometer. Method performance is compared to well-established AAS methods. Initial method validation was accomplished using National Institute of Standards and Technology (NIST) Standard Reference Material 966, Toxic Metals in Bovine Blood. Method detection limits (3s) are 0.05 μg dl - 1 for Pb, 0.09 μg l - 1 for Cd; and 0.17 μg l - 1 for Hg. Repeatability ranged from 1.4% to 2.8% for Pb; 3% to 10% for Cd; and 2.6% to 8.8% for Hg. In contrast, AAS method detection limits were 1 μg dl - 1 , 0.54 μg l - 1 , and 0.6 μg l - 1 , for Pb, Cd, and Hg, respectively. Further performance assessments were conducted over a 2-year period via participation in four international External Quality Assessment Schemes (EQAS) operated specifically for toxic metals in blood. This includes schemes operated by (a) the New York State Department of Health's Wadsworth Center, Albany, NY, USA (b) L'Institut National de Santé Publique du Québec, Centre de Toxicologie du Québec, Canada, (c) Friedrich-Alexander University, Erlangen, Germany, and (d) the University of Surrey, Guildford, UK Trace Elements scheme. The EQAS data reflect analytical performance for blind samples analyzed independently by both inductively coupled plasma-mass spectrometry and AAS methods.

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

    PubMed

    Gonzáles, A P S; Firmino, M A; Nomura, C S; Rocha, F R P; Oliveira, P V; Gaubeur, I

    2009-03-23

    The physical and chemical characteristics of peat were assessed through measurement of pH, percentage of organic matter, cationic exchange capacity (CEC), elemental analysis, infrared spectroscopy and quantitative analysis of metals by ICP OES. Despite the material showed to be very acid in view of the percentage of organic matter, its CEC was significant, showing potential for retention of metal ions. This characteristic was exploited by coupling a peat mini-column to a flow system based on the multicommutation approach for the in-line copper concentration prior to flame atomic absorption spectrometric determination. Cu(II) ions were adsorbed at pH 4.5 and eluted with 0.50 molL(-1) HNO(3). The influence of chemical and hydrodynamic parameters, such as sample pH, buffer concentration, eluent type and concentration, sample flow-rate and preconcentration time were investigated. Under the optimized conditions, a linear response was observed between 16 and 100 microgL(-1), with a detection limit estimated as 3 microgL(-1) at the 99.7% confidence level and an enrichment factor of 16. The relative standard deviation was estimated as 3.3% (n=20). The mini-column was used for at least 100 sampling cycles without significant variation in the analytical response. Recoveries from copper spiked to lake water or groundwater as well as concentrates used in hemodialysis were in the 97.3-111% range. The results obtained for copper determination in these samples agreed with those achieved by graphite furnace atomic absorption spectrometry (GFAAS) at the 95% confidence level. PMID:19264168

  1. The determination of wear metals in used lubricating oils by flame atomic absorption spectrometry using sulphanilic acid as ashing agent.

    PubMed

    Ekanem, E J; Lori, J A; Thomas, S A

    1997-11-01

    A simple and reliable ashing procedure is proposed for the preparation of used lubricating oil samples for the determination of calcium, magnesium, zinc, iron, chromium and nickel by flame atomic absorption spectrometry. Sulphanilic acid was added to oil samples and the mixture coked and the coke ashed at 550 degrees C. The solutions of the ash were analysed by flame AAS for the metals. The release of calcium, zinc, iron and chromium was improved by the addition of sulphanilic acid to samples. The relative standard deviations of metal concentration results in the initial oil samples were 1.5% for Ca (1500 mg l(-1) level), 0.3% for Mg (100 mg l(-1) level), 3.1% for Zn (1500 mg l(-1) level), 0.7% for Fe (500 mg l(-1) level), 0.02% for Cr (50 mg l(-1) level) and 0.002% for Ni (10 mg l(-1) level). The optimum sample size for efficient metal release was 20 g while the optimum sulphanilic acid to oil ratio was 0.05 g per gram of oil for Zn and Cr and 0.10 g for Ca and Fe. Results obtained by this procedure were highly reproducible and comparable with those obtained for the same samples using standard procedures. PMID:18966959

  2. Direct determination of cadmium in Orujo spirit samples by electrothermal atomic absorption spectrometry: comparative study of different chemical modifiers.

    PubMed

    Vilar Fariñas, M; Barciela García, J; García Martín, S; Peña Crecente, R; Herrero Latorre, C

    2007-05-22

    In this work, several analytical methods are proposed for cadmium determination in Orujo spirit samples using electrothermal atomic absorption spectrometry (ETAAS). Permanent chemical modifiers thermally coated on the platforms inserted in pyrolytic graphite tubes (such as W, Ir, Ru, W-Ir and W-Ru) were comparatively studied in relation to common chemical modifier mixtures [Pd-Mg(NO3)2 and (NH4)H2PO4-Mg(NO3)2] for cadmium stabilization. Different ETAAS Cd determination methods based on the indicated modifiers have been developed. In each case, pyrolysis and atomization temperatures, atomization shapes, characteristic masses and detection limits as well as other analytical characteristics have been determined. All the assayed modifiers (permanent and conventional) were capable of achieving the appropriate stabilization of the analyte, with the exception of Ru and W-Ru. Moreover, for all developed methods, recoveries (99-102%) and precision (R.S.D. lower than 10%) were acceptable. Taking into account the analytical performance (best detection limit LOD = 0.01 microg L(-1)), the ETAAS method based on the use of W as a permanent modifier was selected for further direct Cd determinations in Orujo samples from Galicia (NW Spain). The chosen method was applied in the determination of the Cd content in 38 representative Galician samples. The cadmium concentrations ranged

  3. Determination of Trace Silver in Water Samples by Online Column Preconcentration Flame Atomic Absorption Spectrometry Using Termite Digestion Product

    PubMed Central

    Bianchin, Joyce Nunes; Martendal, Edmar; Carasek, Eduardo

    2011-01-01

    A new method for Ag determination in water samples using solid phase extraction (SPE) coupled to a flow injection system and flame atomic absorption spectrometry was developed. The sorbent used for Ag preconcentration and extraction was the termite digestion product. Flow and chemical variables of the system were optimized through a multivariate procedure. The factors selected were adsorbent mass, buffer type and concentration, sample pH, and sample flow rate. The detection limit and precision were 3.4 μg L−1 and 3.8% (n = 6, 15 μg L−1), respectively. The enrichment factor and the linear working range were, respectively, 21 and 10–50 μg L−1. Results for recovery tests using different water samples were between 96 and 107%. The proposed methodology was applied with success for the determination of Ag in water used to wash clothes impregnated with silver nanoparticles, supplied by a factory located in Santa Catarina, Brazil. PMID:21804766

  4. Monitoring of Pd in airborne particulates by solid sampling high-resolution continuum source electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Atilgan, Semin; Akman, Suleyman; Baysal, Asli; Bakircioglu, Yasemin; Szigeti, Tamás; Óvári, Mihály; Záray, Gyula

    2012-04-01

    An analytical method has been developed for determination of palladium in PM2.5 fractions of urban airborne particulate matter by solid sampling high-resolution continuum source electrothermal atomic absorption spectrometry. For the optimization of the experimental conditions, a road dust certified reference material (BCR-723) was used. The influence of pyrolysis and atomization temperatures, the amount of sample introduced into the graphite furnace and the addition of acids, surfactants and modifiers on the analytical signal of Pd were investigated. The limit of detection, calculated based on three times the standard deviations of analytical signals obtained during the atomization of 10 blank filter pieces, was 0.07 pg/m3. Since the amount of solid certified reference material introduced into the graphite furnace was about 50-2000 times lower than those required in order to obtain the certified value, the precision was relatively poor. This analytical method was applied for investigation of urban airborne particulate matter collected onto quartz fiber filters by high-volume aerosol samplers in the city center of Istanbul (Turkey) and Budapest (Hungary). The measured Pd concentrations changed in the range of 0.22-0.64 and 0.25-0.86 pg/m3 in Istanbul and Budapest, respectively.

  5. Evaluation of ammonia as diluent for serum sample preparation and determination of selenium by graphite furnace atomic absorption spectrometry*1

    NASA Astrophysics Data System (ADS)

    Hernández-Caraballo, Edwin A.; Burguera, Marcela; Burguera, José L.

    2002-12-01

    A method for the determination of total selenium in serum samples by graphite furnace atomic absorption spectrometry was evaluated. The method involved direct introduction of 1:5 diluted serum samples (1% v/v NH 4OH+0.05% w/v Triton X-100 ®) into transversely heated graphite tubes, and the use of 10 μg Pd+3 μg Mg(NO 3) 2 as chemical modifier. Optimization of the modifier mass and the atomization temperature was conducted by simultaneously varying such parameters and evaluating both the integrated absorbance and the peak height/peak area ratio. The latter allowed the selection of compromise conditions rendering good sensitivity and adequate analyte peak profiles. A characteristic mass of 49 pg and a detection limit (3s) of 6 μg 1 -1 Se, corresponding to 30 μg l -1 Se in the serum sample, were obtained. The analyte addition technique was used for calibration. The accuracy was assessed by the determination of total selenium in Seronorm™ Trace Elements Serum Batch 116 (Nycomed Pharma AS). The method was applied for the determination of total selenium in ten serum samples taken from individuals with no known physical affection. The selenium concentration ranged between 79 and 147 μg l -1, with a mean value of 114±22 μg l -1.

  6. [Determination of aluminum in wheat flour food by microwave digestion-high resolution continuum source graphite furnace atomic absorption spectrometry].

    PubMed

    Ren, Ting; Zhao, Li-jiao; Zhong, Ru-gang

    2011-12-01

    The contents of aluminum (Al) in four kinds of wheat flour food (noodle, dumpling wrapper, twisted cruller and soda biscuit) were determined by high resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GFAAS) combined with microwave digestion. The samples were completely digested by the mixture of HNO3 and H2O2 in closed polytetrafluoroethylene (PTFE) vessels. The conditions for microwave digestion, pyrolysis temperature and atomization temperature were optimized. The optimum experimental conditions were determined as follows. The microwave digestion was performed with HNO3/H2O2 7:1 (volume ratio), microwave power 1000 W and 190 degrees C for 40 minutes. The optimum pyrolysis temperature was 1350 degrees C and the optimum atomization temperature was 2400 degrees C. Magnesium nitrate solution with the concentration of 1 g x L(-1) was used as the matrix modifier. The correlation coefficient for the standard curve was 0.9999, the relative standard deviation (RSD) was from 1.7% to 2.4%, and the recovery for the samples was from 98.16% to 102.67%. The assay method for the determination of Al in wheat flour food established in this study has referential importance for the constituent of the correlated food standards. PMID:22295801

  7. Investigation of lead contents in lipsticks by solid sampling high resolution continuum source electrothermal atomic absorption spectrometry.

    PubMed

    Gunduz, Sema; Akman, Suleyman

    2013-02-01

    In this study, the lead contents of different kinds of lipsticks were determined by solid sampling high resolution continuum source electrothermal atomic absorption spectrometry (SS-HR-CS ET AAS) and the results were compared with those obtained after microwave-assisted acid digestion of the samples. The experimental parameters for solid sampling such as the maximum amount of sample on the platforms of solid autosampler, graphite furnace program were optimized. Samples were directly loaded on the platforms of solid autosampler between 0.25 and 2.0mg and lead was determined applying 800 °C for pyrolysis and 2100 °C for atomization. Under optimized conditions, interference-free determination could be performed using aqueous standards. The LOD and the characteristic mass were 21.3 and 12.6 pg, respectively. The lead in the same lipstick samples was determined after microwave-assisted acid digestion and compared with those found by solid sampling. Mostly, there was no significant difference between the lead concentrations found by the two techniques. The lead in 25 lipstick samples with different properties were 0.11-4.48 ng mg(-1) which were not significantly different from those (<0.026-7.19 ng mg(-1)) reported by FDA for around 400 samples. PMID:23099440

  8. Species selective preconcentration and quantification of gold nanoparticles using cloud point extraction and electrothermal atomic absorption spectrometry.

    PubMed

    Hartmann, Georg; Schuster, Michael

    2013-01-25

    The determination of metallic nanoparticles in environmental samples requires sample pretreatment that ideally combines pre-concentration and species selectivity. With cloud point extraction (CPE) using the surfactant Triton X-114 we present a simple and cost effective separation technique that meets both criteria. Effective separation of ionic gold species and Au nanoparticles (Au-NPs) is achieved by using sodium thiosulphate as a complexing agent. The extraction efficiency for Au-NP ranged from 1.01 ± 0.06 (particle size 2 nm) to 0.52 ± 0.16 (particle size 150 nm). An enrichment factor of 80 and a low limit of detection of 5 ng L(-1) is achieved using electrothermal atomic absorption spectrometry (ET-AAS) for quantification. TEM measurements showed that the particle size is not affected by the CPE process. Natural organic matter (NOM) is tolerated up to a concentration of 10 mg L(-1). The precision of the method expressed as the standard deviation of 12 replicates at an Au-NP concentration of 100 ng L(-1) is 9.5%. A relation between particle concentration and the extraction efficiency was not observed. Spiking experiments showed a recovery higher than 91% for environmental water samples. PMID:23312311

  9. An automatic countercurrent liquid-liquid micro-extraction system coupled with atomic absorption spectrometry for metal determination.

    PubMed

    Mitani, Constantina; Anthemidis, Aristidis N

    2015-02-01

    A novel and versatile automatic sequential injection countercurrent liquid-liquid microextraction (SI-CC-LLME) system coupled with atomic absorption spectrometry (FAAS) is presented for metal determination. The extraction procedure was based on the countercurrent flow of aqueous and organic phases which takes place into a newly designed lab made microextraction chamber. A noteworthy feature of the extraction chamber is that it can be utilized for organic solvents heavier or lighter than water. The proposed method was successfully demonstrated for on-line lead determination and applied in environmental water samples using an amount of 120 μL of chloroform as extractant and ammonium diethyldithiophosphate as chelating reagent. The effect of the major experimental parameters including the volume of extractant, as well as the flow rate of aqueous and organic phases were studied and optimized. Under the optimum conditions for 6 mL sample consumption an enhancement factor of 130 was obtained. The detection limit was 1.5 μg L(-1) and the precision of the method, expressed as relative standard deviation (RSD) was 2.7% at 40.0 μg L(-1) Pb(II) concentration level. The proposed method was evaluated by analyzing certified reference materials and spiked environmental water samples. PMID:25435230

  10. Detection of silver nanoparticles in parsley by solid sampling high-resolution-continuum source atomic absorption spectrometry.

    PubMed

    Feichtmeier, Nadine S; Leopold, Kerstin

    2014-06-01

    In this work, we present a fast and simple approach for detection of silver nanoparticles (AgNPs) in biological material (parsley) by solid sampling high-resolution-continuum source atomic absorption spectrometry (HR-CS AAS). A novel evaluation strategy was developed in order to distinguish AgNPs from ionic silver and for sizing of AgNPs. For this purpose, atomisation delay was introduced as significant indication of AgNPs, whereas atomisation rates allow distinction of 20-, 60-, and 80-nm AgNPs. Atomisation delays were found to be higher for samples containing silver ions than for samples containing silver nanoparticles. A maximum difference in atomisation delay normalised by the sample weight of 6.27 ± 0.96 s mg(-1) was obtained after optimisation of the furnace program of the AAS. For this purpose, a multivariate experimental design was used varying atomisation temperature, atomisation heating rate and pyrolysis temperature. Atomisation rates were calculated as the slope of the first inflection point of the absorbance signals and correlated with the size of the AgNPs in the biological sample. Hence, solid sampling HR-CS AAS was proved to be a promising tool for identifying and distinguishing silver nanoparticles from ionic silver directly in solid biological samples. PMID:24292434

  11. A new coupling of ionic liquid based-single drop microextraction with tungsten coil electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Wen, Xiaodong; Deng, Qingwen; Wang, Jiwei; Yang, Shengchun; Zhao, Xia

    2013-03-01

    In this work, an improved method of ionic liquid based-single drop microextraction (IL-SDME) preconcentration was firstly coupled with tungsten coil electrothermal atomic absorption spectrometry (W-coil ET-AAS) detection. The new coupling was developed and applied for the determination of ultra-trace cadmium. Experimental parameters influencing the performance of IL-SDME as well as instrumental conditions were studied systematically, including IL-drop volume, chelating agent concentration, pH, stirring rate and time, heating program of W-coil ET-AAS, flow rate of carrier gas. Under the optimal conditions, the limit of detection (LOD) for cadmium was 0.015 μg L-1 (sampling amount on W-coil was 10 μL). The sensitivity enhancement factor was 42, while the improvement factor of LOD was 33. The established method was applied to determine cadmium in standard reference materials of rice and real water samples successfully. The developed IL-SDME-W-coil ET-AAS coupling represents a simple, green and highly sensitive method for cadmium determination.

  12. Determination of molybdenum in plants by vortex-assisted emulsification solidified floating organic drop microextraction and flame atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Oviedo, Jenny A.; Fialho, Lucimar L.; Nóbrega, Joaquim A.

    2013-08-01

    A fast and sensitive procedure for extraction and preconcentration of molybdenum in plant samples based on solidified floating organic drop microextraction combined with flame atomic absorption spectrometry and discrete nebulization was developed. 8-Hydroxyquinoline (8-HQ) was used as complexing agent. The experimental conditions established were: 0.5% m v- 1 of 8-HQ, 60 μL of 1-undecanol as the extractant phase, 2 min vortex extraction time, centrifugation for 2 min at 2000 rpm, 10 min into an ice bath and discrete nebulization by introducing 200 μL of solution. The calibration curve was linear from 0.02 to 4.0 mg L- 1 with a limit of detection of 4.9 μg L- 1 and an enhancement factor of 67. The relative standard deviations for ten replicate measurements of 0.05 and 1.0 mg L- 1 Mo were 6.0 and 14.5%, respectively. The developed procedure was applied for determining molybdenum in corn samples and accuracy was proved using certified reference materials.

  13. Dispersive Liquid-Liquid Microextraction of Bismuth in Various Samples and Determination by Flame Atomic Absorption Spectrometry.

    PubMed

    Daşbaşı, Teslima; Kartal, Şenol; Saçmacı, Şerife; Ülgen, Ahmet

    2016-01-01

    A dispersive liquid-liquid microextraction method for the determination of bismuth in various samples by flame atomic absorption spectrometry is described. In this method, crystal violet was used as counter positive ion for BiCl4 (-) complex ion, chloroform as extraction solvent, and ethanol as disperser solvent. The analytical parameters that may affect the extraction efficiency like acidity of sample, type and amount of extraction and disperser solvents, amount of ligand, and extraction time were studied in detail. The effect of interfering ions on the analyte recovery was also investigated. The calibration graph was linear in the range of 0.040-1.00 mg L(-1) with detection limit of 4.0 μg L(-1) (n = 13). The precision as relative standard deviation was 3% (n = 11, 0.20 mg L(-1)) and the enrichment factor was 74. The developed method was applied successfully for the determination of bismuth in various water, pharmaceutical, and cosmetic samples and the certified reference material (TMDA-64 lake water). PMID:26881186

  14. Determination of vanadium in soils and sediments by the slurry sampling graphite furnace atomic absorption spectrometry using permanent modifiers.

    PubMed

    Dobrowolski, Ryszard; Adamczyk, Agnieszka; Otto, Magdalena

    2013-09-15

    A new analytical procedure for vanadium (V) determination in soils and sediments by the slurry sampling graphite furnace atomic absorption spectrometry (slurry sampling GFAAS) using the mixed permanent modifiers is described. Moreover, the comparison of action of the modifiers based on the iridium (Ir) and carbide-forming elements: tungsten (W) and niobium (Nb) deposited on the graphite tubes is studied, especially in terms of their analytical utility and determination sensitivity. The mechanism of their action was investigated using an X-ray diffraction technique (XRD) and scanning electron microscopy (SEM) equipped with an energy dispersive X-ray detector (EDX). Finally, the mixture of 0.3 μg of Ir and 0.04 μg of Nb was used for the graphite tube permanent modification. The analytical procedure was optimized on the basis of the data from pyrolysis and atomization temperature curves studies. The results obtained for the four certified reference materials (marine sediments: PACS-1 and MESS-1, lake sediment: SL-1, soil: San Joaquin Soil SRM 2709), using the slurry sampling GFAAS and the standard calibration method, were in good agreement with the certified values. The detection and quantification limits and characteristic mass calculated for the proposed procedure were 0.04 µg/g, 0.16 µg/g and 11.9 pg, respectively. The precision (RSD% less than 8%) and the accuracy of vanadium determination in the soil and sediment samples were acceptable. PMID:23708618

  15. Determination of cadmium, aluminium, and copper in beer and products used in its manufacture by electrothermal atomic absorption spectrometry.

    PubMed

    Viñas, Pilar; Aguinaga, Nerea; López-García, Ignacio; Hernandez-Córdoba, Manuel

    2002-01-01

    Procedures were developed for determining cadmium, aluminium, and copper in beer and the products used in its manufacture by electrothermal atomic absorption spectrometry. Beer samples were injected into the furnace and solid samples were introduced as suspensions after preparation in a medium containing hydrogen peroxide, nitric acid, and ammonium dihydrogen phosphate for cadmium atomization. Calibration was performed with aqueous standards, and characteristic masses and detection limits were, respectively, 1 and 0.3 pg for cadmium, 18 and 5.4 pg for aluminium, and 5.6 and 6.8 pg for copper. Different samples of beer, wort, brewer's yeast, malt, raw grain, and hops were analyzed by the proposed procedures. Cadmium was found in low concentrations (0.001-0.08 microg/g and 0-1.3 ng/mL); copper (3-13 microg/g and 25-137 ng/mL) and aluminium (0.6-9 microg/g and 0.1-2 microg/mL) were found at higher levels. The reliability of the procedure was confirmed by comparing the results obtained with others based on microwave oven sample digestion, and by analyzing several certified reference materials. PMID:12083268

  16. Slurry sampling hydride generation atomic absorption spectrometry for the determination of extractable/soluble As in sediment samples

    NASA Astrophysics Data System (ADS)

    Mierzwa, Jerzy; Dobrowolski, Ryszard

    1998-01-01

    A method combining the sampling of slurry pretreated by ultrasonic agitation and microwave assisted extraction with hydride generation atomic absorption spectrometry (HGAAS) for the determination of arsenic in sediment samples is proposed and evaluated. The pretreatment of slurried samples by ultrasonication enabled the extraction of (approximately) up to 85% of arsenic from the studied sediment samples. The further (slight) improvement of the efficiency of extraction was accomplished by the introduction of a short microwave-accelerated treatment. L-cysteine was used as an efficient pre-reduction reagent. The accuracy and precision of the slurry sampling HGAAS method were studied using the certified reference materials: Sediment GBW 30043 (NRCCRM, People's Republic of China), Sediment NIST 2704 (NIST, USA) and Marine Sediment BCSS-1 (NRCC, Canada). The relative standard deviation of the full (overall) analytical procedure was 8.5% and an absolute limit of detection of 2.75 ng was achieved. Factors which influence the reliability of this method are, for example, the choice of slurry liquid phase (extraction medium), sample homogeneity and, in particular, very effective mixing of slurries.

  17. Determination of methylmercury by electrothermal atomic absorption spectrometry using headspace single-drop microextraction with in situ hydride generation

    NASA Astrophysics Data System (ADS)

    Gil, Sandra; Fragueiro, Sandra; Lavilla, Isela; Bendicho, Carlos

    2005-01-01

    A new method is proposed for preconcentration and matrix separation of methylmercury prior to its determination by electrothermal atomic absorption spectrometry (ETAAS). Generation of methylmercury hydride (MeHgH) from a 5-ml solution is carried out in a closed vial and trapped onto an aqueous single drop (3-μl volume) containing Pd(II) or Pt(IV) (50 and 10 mg/l, respectively). The hydrogen evolved in the headspace (HS) after decomposition of sodium tetrahydroborate (III) injected for hydride generation caused the formation of finely dispersed Pd(0) or Pt(0) in the drop, which in turn, were responsible for the sequestration of MeHgH. A preconcentration factor of ca. 40 is achieved with both noble metals used as trapping agents. The limit of detection of methylmercury was 5 and 4 ng/ml (as Hg) with Pd(II) or Pt(IV) as trapping agents, and the precision expressed as relative standard deviation was about 7%. The preconcentration system was fully characterised through optimisation of the following variables: Pd(II) or Pt(IV) concentration in the drop, extraction time, pH of the medium, temperatures of both sample solution and drop, concentration of salt in the sample solution, sodium tetrahydroborate (III) concentration in the drop and stirring rate. The method has been successfully validated against two fish certified reference materials (CRM 464 tuna fish and CRM DORM-2 dogfish muscle) following selective extraction of methylmercury in 2 mol/l HCl medium.

  18. Dispersive Liquid-Liquid Microextraction of Bismuth in Various Samples and Determination by Flame Atomic Absorption Spectrometry

    PubMed Central

    Daşbaşı, Teslima; Kartal, Şenol; Saçmacı, Şerife; Ülgen, Ahmet

    2016-01-01

    A dispersive liquid-liquid microextraction method for the determination of bismuth in various samples by flame atomic absorption spectrometry is described. In this method, crystal violet was used as counter positive ion for BiCl4− complex ion, chloroform as extraction solvent, and ethanol as disperser solvent. The analytical parameters that may affect the extraction efficiency like acidity of sample, type and amount of extraction and disperser solvents, amount of ligand, and extraction time were studied in detail. The effect of interfering ions on the analyte recovery was also investigated. The calibration graph was linear in the range of 0.040–1.00 mg L−1 with detection limit of 4.0 μg L−1 (n = 13). The precision as relative standard deviation was 3% (n = 11, 0.20 mg L−1) and the enrichment factor was 74. The developed method was applied successfully for the determination of bismuth in various water, pharmaceutical, and cosmetic samples and the certified reference material (TMDA-64 lake water). PMID:26881186

  19. Behaviour of chemical modifiers in the determination of arsenic by electrothermal atomic absorption spectrometry in petroleum products.

    PubMed

    Reboucas, Marcio V; Ferreira, Sergio L C; de Barros Neto, Benicio

    2005-07-15

    Most comparative studies on the efficiency of chemical modifiers have been conducted in aqueous media. In the present work, we proposed a detailed study of the use of different chemical modifiers for direct determination of arsenic in complex organic matrices by electrothermal atomic absorption spectrometry (ETAAS). Palladium, rhodium, tungsten, silver, lanthanum and a mixture of palladium and magnesium were tested. The figures of merit used for evaluation and comparison were acquired in the optimal conditions for each modifier, established by multivariate optimization of the main variables based on Doehlert designs. Singular features were observed for the chemical behaviour of some modifiers in organic matrices compared to aqueous media, such as the worse performance of Pd+Mg modifier and no notice of severe tube corrosion from La application. Lanthanum was chosen as the best chemical modifier for the present application, according to predefined criteria. Lanthanum showed the minimum limit of detection, characteristic concentration and blank signal among all tested species and no effect of the concomitants usually present in petrochemical feedstocks. Using a 200mgL(-1) lanthanum solution as a chemical modifier, the average relative standard deviations of 7 and 16% (at 3-15mugL(-1) level) and characteristic concentrations of 0.47 and 0.77mugL(-1) for naphtha and petroleum condensates, respectively, were observed. PMID:18970155

  20. Improvements in cobalt determination by thermospray flame furnace atomic absorption spectrometry using an on-line derivatization strategy.

    PubMed

    Matos, Geraldo Domingues; Arruda, Marco Aurélio Zezzi

    2008-07-15

    An on-line derivatization strategy was developed for improving cobalt sensitivity using thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) as the analytical technique. This strategy involves the generation of a volatile cobalt compound, providing better sample vaporization efficiency. The effect of sodium diethyldithiocarbamate (DDTC) as complexing agent on the integrated absorbance signal was evaluated. Parameters including the pH of complex formation, complex concentration and volume, sample volume, flame gas composition and tube atomization configuration were optimized. A wide linear range (from 23 microg L(-1) to 3 mg L(-1); r(2)=0.9786) was obtained, with the best one (r(2)=0.9992) attained from 23 to 400 microg L(-1) with a sample throughput of 30 h(-1). The improvement in the detection power was 17-fold when compared to FAAS, which provides 7 microg L(-1) as the limit of detection when considered TS-FF-AAS technique. A relative standard deviation (n=10) of 4% for a cobalt solution containing 50 microg L(-1) was attained, and the accuracy of the procedure was evaluated through certified reference materials (IAEA-SL-1, lake sediment; and ISS-MURST-A1, Antarctic marine sediment). Good agreement between the results at the 95% confidence level was observed. PMID:18585309

  1. 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

  2. Determination of sulfur in coal using direct solid sampling and high-resolution continuum source molecular absorption spectrometry of the CS molecule in a graphite furnace.

    PubMed

    Mior, Renata; Morés, Silvane; Welz, Bernhard; Carasek, Eduardo; de Andrade, Jailson B

    2013-03-15

    An analytical method has been developed for the determination of sulfur in coal using direct solid sample analysis in a graphite tube furnace and high-resolution continuum source molecular absorption spectrometry (HR-CS GF MAS). The molecular absorbance of the carbon monosulfide molecule (CS), which is formed in the vaporization stage, has been measured using the rotational line at 258.033 nm. Several chemical modifiers were tested and Ru, applied as permanent modifier was chosen, because it exhibited the best performance. The optimum pyrolysis and vaporization temperatures were found to be 500 °C and 2200 °C, respectively. Aqueous standard solutions prepared from l-cysteine were used for calibration, as the linear regression obtained for this standard was not significantly different from that for a certified coal reference material (CRM) according to a Student t-test. The results obtained for sulfur in three coal CRM and six additional samples also showed no significant difference for the two calibration techniques according to the same statistical test. The sulfur concentration in the coal samples was found between 3.5 mg g(-1) and 33.7 mg g(-1) with a typical repeatability around 10%. The limit of detection for the direct analysis of solid coal samples was better than 0.1 μg S. PMID:23598139

  3. The determination of total Se in urine and serum by graphite furnace atomic absorption spectrometry using Ir as permanent modifier and in situ oxidation for complete trimethylselenonium recovery.

    PubMed

    Grinberg, Patricia; Gonçalves, Rodrigo Araújo; de Campos, Reinaldo Calixto

    2005-12-01

    The present work evaluated the use of iridium (Ir) as permanent modifier for the determination of total selenium in urine and serum by graphite furnace atomic absorption spectrometry. Concerning urine, the presence of trimethylselenonium (TMSe(+)) was especially considered. Pyrolysis and atomization temperatures of 1,000 and 2,100 degrees C, respectively, were used. For nondigested urine and serum samples, 0.2% v/v HNO(3) and Triton X-100 were used as diluents, respectively, and the same initial platform Ir treatment was effective for up to 1,100 atomization cycles. Good precision [less than 5% relative standard deviation (RSD)] can be achieved with the proposed method. Low TMSe(+) recovery was observed for nondigested urine samples. Thus, if this species is to be considered in urine analysis, a previous external mineralization step was found to be necessary. Alternatively, an in situ oxidation treatment was developed. Detection limits of 8, 10, and 7 mug l(-1) were obtained after dilution, microwave-assisted digestion, and in situ oxidation procedures, respectively. The accuracy of the method was validated by the analysis of certified reference or commercial quality control materials and spiked samples. PMID:16267645

  4. The determination of silver in silicate rocks by electrothermal atomic absorption spectrometry

    USGS Publications Warehouse

    Aruscavage, P. J.; Campbell, E.Y.

    1979-01-01

    Silver is extracted from a 20% tartaric acid solution by using butyl acetate and diphenylthiourea, and the organic layer is analyzed directly by the graphite-furnace technique. The precisions is ca. 8% as estimated from multiple analysis of 13 standard rocks; there are no systematic errors. The detection limit is 2.4 ppb for 250-mg samples. ?? 1979.

  5. Measurement of copper in biological samples by flame or electrothermal atomic absorption spectrometry.

    PubMed

    Evenson, M A

    1988-01-01

    Guidelines presented here allow for copper analysis of biological materials by methods that are very sensitive, that require little sample preparation, that have few chemical or spectral interferences, that are inexpensive, and that require only usual care in contamination control. The commercial instruments for FAAS and ETAAS from Perkin-Elmer, from Varian, and from Instrumentation Laboratories Inc. (Allied Analytical Systems) all work well in either the flame or the flameless mode. Background correction techniques are not essential for copper analysis if care is taken with the sample preparation to minimize the background signals. Different types of burners will work adequately if one makes certain that the viscosity of the sample and the control products are similar to the calibration standards. Further, dilution of samples is preferred over increasing the viscosity of the calibration standards by the addition of a protein containing solution or a substance such as glycerol. A 1:10 dilution of blood plasma or serum with dilute nitric acid or water is all that is necessary for copper analysis by the FFAS methods. Cation and anion effects should be tested by bracketing the concentrations of the ions found in the sample with known amounts of ions in the sample solutions. Increasing the concentrations of the ions thought to interfere while keeping the copper concentration constant is another way to test for ion interferences.(ABSTRACT TRUNCATED AT 250 WORDS) PMID:3374386

  6. Native Liquid Extraction Surface Analysis Mass Spectrometry: Analysis of Noncovalent Protein Complexes Directly from Dried Substrates

    NASA Astrophysics Data System (ADS)

    Martin, Nicholas J.; Griffiths, Rian L.; Edwards, Rebecca L.; Cooper, Helen J.

    2015-08-01

    Liquid extraction surface analysis (LESA) mass spectrometry is a promising tool for the analysis of intact proteins from biological substrates. Here, we demonstrate native LESA mass spectrometry of noncovalent protein complexes of myoglobin and hemoglobin from a range of surfaces. Holomyoglobin, in which apomyoglobin is noncovalently bound to the prosthetic heme group, was observed following LESA mass spectrometry of myoglobin dried onto glass and polyvinylidene fluoride surfaces. Tetrameric hemoglobin [(αβ)2 4H] was observed following LESA mass spectrometry of hemoglobin dried onto glass and polyvinylidene fluoride (PVDF) surfaces, and from dried blood spots (DBS) on filter paper. Heme-bound dimers and monomers were also observed. The `contact' LESA approach was particularly suitable for the analysis of hemoglobin tetramers from DBS.

  7. Ultratrace Analysis of Uranium and Plutonium By Mass Spectrometry

    SciTech Connect

    Wacker, John F.; Wogman, Ned A.; Olsen, Khris B.; Petersen, Steven L.; Farmer, O T.; Kelley, James M.; Eiden, Greg C.; Maiti, Tapas C.

    2003-01-01

    At the Pacific Northwest National Laboratory (PNNL), we have developed highly sensitive methods to analyze uranium and plutonium in environmental samples. The development of an ultratrace analysis capability for measuring uranium and plutonium has arisen from a need to detect and characterize environmental samples for signatures associated with nuclear industry processes. Our most sensitive well-developed methodologies employ thermal ionization mass spectrometry (TIMS), however, recent advances in inductively coupled plasma mass spectrometry (ICP-MS) have shown considerable promise for use in detecting uranium and plutonium at ultratrace levels. The work at PNNL has included the development of both chemical separation and purification techniques, as well as the development of mass spectrometric instrumentation and techniques. At the heart of our methodology for TIMS analysis is a procedure that utilizes 100-microliter-volumes of analyte for chemical processing to purify, separate, and load actinide elements into resin beads for subsequent mass spectrometric analysis. The resin bead technique has been combined with a thorough knowledge of the physicochemistry of thermal ion emission to achieve femtogram detection limits for the TIMS analysis of plutonium in environmental samples.

  8. Transition of Iodine Analysis to Accelerator Mass Spectrometry

    SciTech Connect

    Watrous, Matthew George; Adamic, Mary Louise; Olson, John Eric; Baeck, D. L.; Fox, R. V.; Hahn, P. A.; Jenson, D. D.; Lister, T. E.

    2015-09-01

    The goal of the project, New Paradigms for Isotope Ratio Mass Spectrometry: Raising the Scientific Profile and Improved Performance for Accelerator Mass Spectrometry (AMS) and Thermal Ionization Mass Spectrometry (TIMS), is to ensure that the ongoing isotope ratio determination capability within the U.S. Department of Energy complex is the world’s best for application to nonproliferation. This report spells out the progress of Task 4, Transition of TIMS to AMS for Iodine Analysis, of the larger project. The subtasks under Task 4 and the accomplishments throughout the three year project life cycle are presented in this report. Progress was made in optimization of chemical extraction, determination of a detection limit for 127Iodine, production of standard materials for AMS analysis quality assurance, facilitation of knowledge exchange with respect to analyzing iodine on an AMS, cross comparison with a world-leading AMS laboratory, supercritical fluid extraction of iodine for AMS analysis and electrodeposition of seawater as a direct method of preparation for iodine analysis by AMS--all with the goal of minimizing the time required to stand up an AMS capability for iodine analysis of exposed air filters at INL. An effective extraction method has been developed and demonstrated for iodine analysis of exposed air filters. Innovative techniques to accomplish the cathode preparation for AMS analysis were developed and demonstrated and published. The known gap of a lack of available materials for reference standards in the analysis of iodine by AMS was filled by the preparation of homogenous materials that were calibrated against NIST materials. A minimum limit on the amount of abundant isotope in a sample was determined for AMS analysis. The knowledge exchange occurred with fantastic success. Scientists engaged the international AMS community at conferences, as well as in their laboratories for collaborative work. The supercritical fluid extraction work has positive

  9. [Investigations on ashing of animal tissues for the determinations of trace metals by means of polarography or atomic-absorption spectrometry (author's transl)].

    PubMed

    Suzutani, T

    1980-01-01

    A comparison has been made of three ashing methods for animal tissues with subsequent determination of minute quantities of metals by polarography or atomic-absorption spectrometry. Wet oxidation method with many disadvantages and few advantages has been shown not to be useful for the purpose. Both dry ashing in a muffle-furnace at 530 degrees C and low-temperature ashing are equally applicable to atomic-absorption spectrometry, but dry ashing in a furnace is more excellent with polarography. For obtaining ashes with constant compositions it is far more difficult with low-temperature ashing than with dry ashing in a furnace. Hence, dry ashing in a furnace is most widely applicable. PMID:7409725

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

    PubMed

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

    2015-01-01

    The fast sequential multi-element determination of 11 elements present at different concentration levels in environmental samples and drinking waters has been investigated using high-resolution continuum source flame atomic absorption spectrometry. The main lines for Cu (324.754 nm), Zn (213.857 nm), Cd (228.802 nm), Ni (232.003 nm) and Pb (217.001 nm), main and secondary absorption lines for Mn (279.482 and 279.827 nm), Fe (248.327, 248.514 and 302.064 nm) and Ca (422.673 and 239.856 nm), secondary lines with different sensitivities for Na (589.592 and 330.237 nm) and K (769.897 and 404.414 nm) and a secondary line for Mg (202.582 nm) have been chosen to perform the analysis. A flow injection system has been used for sample introduction so sample consumption has been reduced up to less than 1 mL per element, measured in triplicate. Furthermore, the use of multiplets for Fe and the side pixel registration approach for Mg have been studied in order to reduce sensitivity and extend the linear working range. The figures of merit have been calculated and the proposed method was applied to determine these elements in a pine needles reference material (SRM 1575a), drinking and natural waters and soil extracts. Recoveries of analytes added at different concentration levels to water samples and extracts of soils were within 88-115% interval. In this way, the fast sequential multi-element determination of major and minor elements can be carried out, in triplicate, with successful results without requiring additional dilutions of samples or several different strategies for sample preparation using about 8-9 mL of sample. PMID:25479863

  11. APPLICATION OF ABSORPTION SPECTROSCOPY TO ACTINIDE PROCESS ANALYSIS AND MONITORING

    SciTech Connect

    Lascola, R.; Sharma, V.

    2010-06-03

    The characteristic strong colors of aqueous actinide solutions form the basis of analytical techniques for actinides based on absorption spectroscopy. Colorimetric measurements of samples from processing activities have been used for at least half a century. This seemingly mature technology has been recently revitalized by developments in chemometric data analysis. Where reliable measurements could formerly only be obtained under well-defined conditions, modern methods are robust with respect to variations in acidity, concentration of complexants and spectral interferents, and temperature. This paper describes two examples of the use of process absorption spectroscopy for Pu analysis at the Savannah River Site, in Aiken, SC. In one example, custom optical filters allow accurate colorimetric measurements of Pu in a stream with rapid nitric acid variation. The second example demonstrates simultaneous measurement of Pu and U by chemometric treatment of absorption spectra. The paper concludes with a description of the use of these analyzers to supplement existing technologies in nuclear materials monitoring in processing, reprocessing, and storage facilities.

  12. Behaviour of the thermospray nebulizer as a system for the introduction of organic solutions in flame atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Mora, Juan; Canals, Antonio; Hernandis, Vicente

    1996-10-01

    The results obtained in the evaluation of the thermospray nebulizer for the introduction of organic solutions in atomic spectrometry are described. To this end, the influence of the nebulization variables (i.e., liquid flow, control temperature and inner diameter of the capillary) and of the nature of the solvent on the fraction of solvent vaporized, on the drop size distribution of the primary aerosol, on the rates of analyte and solvent transport to the atomization cell and on the analytical signal has been studied. Experimental fraction of solvent vaporized values obtained under different nebulization conditions are reported for the first time. The results show that the characteristics of the aerosol generated strongly depend on the nebulization variables since they determine the amount of energy available for surface generation. The median of the volume drop size distribution of the primary aerosol decreases when the control temperature or the liquid flow is increased or when the inner diameter of the capillary is decreased. As regards the physical properties of the solvent, the so-called expansion factor (i.e., the volume of vapour produced per unit volume of liquid solvent) is the most influential. Surface tension and viscosity are much less significant here than in ordinary pneumatic nebulization. The volatility of the solvent and the characteristics of the primary aerosol determine the solvent transport efficiency which reaches values close to 100% in many cases. The analytical signal is mainly determined by the analyte transport rate, although a severe negative effect appears which is related to the high solvent load to the flame. Due to this fact, the use of organic solvents instead of water in thermospray nebulization for Flame Atomic Absorption Spectrometry does not provide clear advantages, at least without desolvation. A new modified Nukiyama-Tanasawa equation has been presented and evaluated in order to predict the Sauter mean diameter of the thermal

  13. Graphene-based solid-phase extraction combined with flame atomic absorption spectrometry for a sensitive determination of trace amounts of lead in environmental water and vegetable samples.

    PubMed

    Wang, Yukun; Gao, Shutao; Zang, Xiaohuan; Li, Jingci; Ma, Jingjun

    2012-02-24

    Graphene, a novel class of carbon nanostructures, has great promise for use as sorbent materials because of its ultrahigh specific surface area. A new method using a column packed with graphene as sorbent was developed for the preconcentration of trace amounts of lead (Pb) using dithizone as chelating reagent prior to its determination by flame atomic absorption spectrometry. Some effective parameters on the extraction and complex formation were selected and optimized. Under optimum conditions, the calibration graph was linear in the concentration range of 10.0-600.0 μg L(-1) with a detection limit of 0.61 μg L(-1). The relative standard deviation for ten replicate measurements of 20.0 and 400.0 μg L(-1) of Pb were 3.56 and 3.25%, respectively. Comparative studies showed that graphene is superior to other adsorbents including C18 silica, graphitic carbon, and single- and multi-walled carbon nanotubes for the extraction of Pb. The proposed method was successfully applied in the analysis of environmental water and vegetable samples. Good spiked recoveries over the range of 95.3-100.4% were obtained. This work not only proposes a useful method for sample preconcentration, but also reveals the great potential of graphene as an excellent sorbent material in analytical processes. PMID:22284885

  14. Determination of sulfur in crude oil using high-resolution continuum source molecular absorption spectrometry of the SnS molecule in a graphite furnace.

    PubMed

    Cadorim, Heloisa R; Pereira, Éderson R; Carasek, Eduardo; Welz, Bernhard; de Andrade, Jailson B

    2016-01-01

    An analytical method for the determination of sulfur, as the tin mono-sulfide (SnS) molecule, in crude oil using high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS) has been developed. The molecular absorbance of the SnS has been measured using the wavelength at 271.624 nm and the crude oil samples were prepared as micro-emulsions due to their high viscosity. Several chemical modifiers (Ir, Pd, Ru, Zr) were tested and palladium was chosen, because it exhibited the best performance. The heating program was optimized by comparing the pyrolysis and vaporization curves obtained for an aqueous sulfur standard and a micro-emulsion of a crude oil certified reference material (CRM). The optimum pyrolysis and vaporization temperatures were found to be 600 and 2000°C, respectively. The limit of detection and the characteristic mass using micro-emulsion analysis of crude oil samples were 5.8 and 13.3 ng S. Accuracy and precision of the method has been evaluated using two crude oil CRM (NIST 2721 and NIST 2722), showing good agreement with the informed or certified values. PMID:26695253

  15. 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. PMID:26838392

  16. Ultrasound-assisted extraction for the determination of Cu, Mn, Ca, and Mg in alternative oilseed crops using flame atomic absorption spectrometry.

    PubMed

    Peronico, Vanessa Cruz Dias; Raposo, Jorge Luiz

    2016-04-01

    An ultrasound-assisted extraction procedure was evaluated for the multi-element determination of Cu, Mn, Ca, and Mg in alternative oilseed crops using flame atomic absorption spectrometry. The best results were obtained when 0.3g of samples were used to extract the mineral content using 10 mL of a 1.40 mol L(-1) HNO3 solution for 10 min at 25 °C. The accuracy and precision of the analysis were evaluated using two oilseed reference materials, and the results were in agreement with reference values at 95% confidence level (paired t-test). The method was used to analyze five oilseed samples and the results were in agreement with those obtained using a closed-vessel microwave-assisted acid digestion system for sample preparation. The relative standard deviations were 0.52-6.13% for all of the standard and sample measurements, and the limits of detection were 666.7, 416.7, 333.4 μg g(-1), and 3.5 mg g(-1) for Cu, Mn, Ca, and Mg, respectively. PMID:26593618

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

    PubMed Central

    Naeemullah; Kazi, Tasneem Gul; Shah, Faheem; Afridi, Hassan Imran; Khan, Sumaira; Arian, Sadaf Sadia; Brahman, Kapil Dev

    2012-01-01

    Cloud point extraction (CPE) has been used for the preconcentration and simultaneous determination of cobalt (Co) and lead (Pb) in fresh and wastewater samples. The extraction of analytes from aqueous samples was performed in the presence of 8-hydroxyquinoline (oxine) as a chelating agent and Triton X-114 as a nonionic surfactant. Experiments were conducted to assess the effect of different chemical variables such as pH, amounts of reagents (oxine and Triton X-114), temperature, incubation time, and sample volume. After phase separation, based on the cloud point, the surfactant-rich phase was diluted with acidic ethanol prior to its analysis by the flame atomic absorption spectrometry (FAAS). The enhancement factors 70 and 50 with detection limits of 0.26 μg L−1 and 0.44 μg L−1 were obtained for Co and Pb, respectively. In order to validate the developed method, a certified reference material (SRM 1643e) was analyzed and the determined values obtained were in a good agreement with the certified values. The proposed method was applied successfully to the determination of Co and Pb in a fresh surface and waste water sample. PMID:23227429

  18. Dispersive liquid-liquid microextraction for the determination of copper in cereals and vegetable food samples using flame atomic absorption spectrometry.

    PubMed

    Shrivas, Kamlesh; Jaiswal, Nitin Kumar

    2013-12-01

    Dispersive liquid-liquid microextraction (DLLME) is applied for the determination of copper in cereals and vegetable food samples using flame atomic absorption spectrometry (FAAS). The maximum extraction efficiency of copper was obtained after the optimisation of parameters such as extraction and dispersing solvents, pH, concentration of 2,9-dimethyl-1,10-phenanothroline (DPT), N-phenylbenzimidoyl thiourea (PBITU) and salt. The optimised methodology exhibited a good linearity in the range of 0.2-20 ng/mL copper with relative standard deviations percentage (RSD,%) from ±1.5% to 3.5%. The method is found to be simple and rapid for the analysis of copper in food samples with the limit of detection (LOD) and quantitation (LOQ) were 0.05 and 0.16 ng/mL, respectively. Good recoveries of copper were obtained in the range of 93.5-98.0% in food samples as well as in Certified Reference Material (99.1%). The application of the proposed method has been successfully tested for the determination of copper in cereals (maize, millet, rice, wheat, gram, lentils, kidney beans and green beans) and vegetable (potato, cauliflower, tomato, spinach, green beans, lettuce, egg plants and bitter gourd) food samples. PMID:23870956

  19. Determination of Lead in Water Samples Using a New Vortex-Assisted, Surfactant-Enhanced Emulsification Liquid-Liquid Microextraction Combined with Graphite Furnace Atomic Absorption Spectrometry.

    PubMed

    Peng, Guilong; He, Qiang; Lu, Ying; Mmereki, Daniel; Pan, Weiliang; Tang, Xiaohui; Zhou, Guangming; Mao, Yufeng; Su, Xaioxuan

    2016-04-01

    A low toxic solvent-based vortex-assisted surfactant-enhanced emulsification liquid-liquid microextraction (LT-VSLLME) combined with graphite furnace atomic absorption spectrometry was developed for the extraction and determination of lead (Pb) in water samples. In the LT-VSLLME method, the extraction solvent was dispersed into the aqueous samples by the assistance of vortex agitator. Meanwhile, the addition of a surfactant, which acted as an emulsifier, could enhance the speed of the mass-transfer from aqueous samples to the extraction solvent. The influences of analytical parameters, including extraction solvent type and its volume, surfactant type and its volume, pH, concentration of chelating agent, salt effect and extraction time were investigated. Under the optimized conditions, a good relative standard deviation of 3.69% at 10 ng L(-1) was obtained. The calibration graph showed a linear pattern in the ranges of 5-30 ngL(-1), with a limit of detection of 0.76 ng L(-1). The linearity was obtained by five points in the concentration range of 5-30 ngL(-1). The enrichment factor was 320. The procedure was applied to wastewater and river water, and the accuracy was assessed through the analysis of the recovery experiments. PMID:26614355

  20. Evaluation of solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry for direct determination of chromium in medicinal plants

    NASA Astrophysics Data System (ADS)

    Virgilio, Alex; Nóbrega, Joaquim A.; Rêgo, Jardes F.; Neto, José A. Gomes

    2012-12-01

    A method for Cr determination in medicinal plants using direct solid sampling graphite furnace high-resolution continuum source atomic absorption spectrometry was developed. Modifiers were dispensable. Pyrolysis and atomization temperatures were 1500 °C and 2400 °C, respectively. Slopes of calibration curves (50-750 pg Cr, R2 > 0.999) using aqueous and solid standards coincides in 96%, indicated feasibility of aqueous calibration for solid sampling of medicinal plants. Accuracy was checked by analysis of four plant certified reference materials. Results were in agreement at 95% confidence level with certified and non-certified values. Ten samples of medicinal plants were analyzed and Cr contents were in the 1.3-17.7 μg g- 1 Cr range. The highest RSD (n = 5) was 15.4% for the sample Melissa officinalis containing 13.9 ± 2.1 μg g- 1 Cr. The limit of detection was 3.3 ng g- 1 Cr.

  1. Solidified floating organic drop microextraction (SFODME) for simultaneous separation/preconcentration and determination of cobalt and nickel by graphite furnace atomic absorption spectrometry (GFAAS).

    PubMed

    Bidabadi, Mahboubeh Shirani; Dadfarnia, Shayessteh; Shabani, Ali Mohammad Haji

    2009-07-15

    Solidified floating organic drop microextraction (SFODME), combined with graphite furnace atomic absorption spectrometry (GFAAS) was proposed for simultaneous separation/enrichment and determination of trace amounts of nickel and cobalt in surface waters and sea water. 1-(2-Pyridylazo)-2-naphthol (PAN) was used as chelating agent. The main parameters affecting the performance of SFODME, such as pH, concentration of PAN, extraction time, stirring rate, extraction temperature, sample volume and nature of the solvent were optimized. Under the optimum experimental conditions, a good relative standard deviation for six determination of 20 ng l(-1) of Co(II) and Ni(II) were 4.6 and 3.6%, respectively. An enrichment factor of 502 and 497 and detection limits of 0.4 and 0.3 ng l(-1) for cobalt and nickel were obtained, respectively. The procedure was applied to tap water, well water, river water and sea water, and accuracy was assessed through the analysis of certified reference water or recovery experiments. PMID:19117672

  2. Separation and preconcentration of trace level of lead in one drop of blood sample by using graphite furnace atomic absorption spectrometry.

    PubMed

    Shrivas, Kamlesh; Patel, Devesh Kumar

    2010-04-15

    Drop-to-drop solvent microextraction (DDSME) assisted with ultrasonication is applied for the determination of lead in one drop (30 microL) of blood sample by using graphite furnace atomic absorption spectrometry (GF-AAS). The optimum extraction efficiency of lead was observed for 10 min extraction time at pH 5.0 with 2 microL of organic solvent that containing 0.5 M of Cyanex-302. The optimized methodology exhibited good linearity in the range of 0.3-30.0 ng mL(-1) lead with relative standard deviations (RSD) from 2.5 to 4.4%. The method is found to be simple and rapid for the analysis of lead in micro amount of blood sample with the limit of detection (LOD) of 0.08 ng mL(-1). The application of the proposed method has been successfully tested for the determination of lead in blood samples. The results showed that under the optimized experimental conditions, the method showed good sensitivity and recovery %, as well as advantages such as linearity, simplicity, low cost and high feasibility. PMID:20004520

  3. Ultra-trace determination of lead in water and food samples by using ionic liquid-based single drop microextraction-electrothermal atomic absorption spectrometry.

    PubMed

    Manzoori, Jamshid L; Amjadi, Mohammad; Abulhassani, Jafar

    2009-06-30

    An improved single drop microextraction procedure was developed for the preconcentration of lead prior to its determination by electrothermal atomic absorption spectrometry. Ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate [C4MIM][PF6], was used as an alternative to volatile organic solvents for extraction. Lead was complexed with ammonium pyrroldinedithiocarbamate (APDC) and extracted into a 7-microL ionic liquid drop. The extracted complex was directly injected into the graphite furnace. Several variables affecting microextraction efficiency and ETAAS signal, such as pyrolysis and atomization temperature, pH, APDC concentration, extraction time, drop volume and stirring rate were investigated and optimized. In the optimum experimental conditions, the limit of detection (3s) and the enhancement factor were 0.015 microg L(-1) and 76, respectively. The relative standard deviation (RSD) for five replicate determinations of 0.2 microg L(-1) Pb was 5.2%. The developed method was validated by the analysis of certified reference materials and applied successfully to the determination of lead in several real samples. PMID:19463561

  4. Ionic liquid-based single drop microextraction combined with electrothermal atomic absorption spectrometry for the determination of manganese in water samples.

    PubMed

    Manzoori, Jamshid L; Amjadi, Mohammad; Abulhassani, Jafar

    2009-02-15

    Room temperature ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate [C(4)MIM][PF(6)], was used as an alternative to volatile organic solvents in single drop microextraction-electrothermal atomic absorption spectrometry (SDME-ETAAS). Manganese was extracted from aqueous solution into a drop of the ionic liquid after complextaion with 1-(2-thiazolylazo)-2-naphthol (TAN) and the drop was directly injected into the graphite furnace. Several variables affecting microextraction efficiency and ETAAS signal, such as pyrolysis and atomization temperature, pH, TAN concentration, extraction time, drop volume and stirring rate were investigated and optimized. In the optimum experimental conditions, the limit of detection (3s) and the enhancement factor were 0.024 microg L(-1) and 30.3, respectively. The relative standard deviation (RSD) for five replicate determinations of 0.5 microg L(-1) Mn(II) was 5.5%. The developed method was validated by the analysis of a certified reference material (NIST SRM 1643e) and applied successfully to the determination of manganese in several natural water samples. PMID:19084676

  5. 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. PMID:24645524

  6. Determination of lead and cadmium using an ionic liquid and dispersive liquid-liquid microextraction followed by electrothermal atomic absorption spectrometry.

    PubMed

    López-García, Ignacio; Vicente-Martínez, Yesica; Hernández-Córdoba, Manuel

    2013-06-15

    A procedure for the determination of ultratrace levels of lead and cadmium using dispersive liquid-liquid microextraction followed by electrothermal atomic absorption spectrometry (ETAAS) has been developed. The ionic liquid, 1-octyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide ([C8MIm][NTf2]), is formed in situ and used to extract the lead and cadmium complexes with ammonium pyrrolidinedithiocarbamate. The very fine droplets of ([C8MIm][NTf2]) allow effective dispersion without the need for organic solvents. After centrifugation, the concentrations of lead and cadmium in the sedimented phase can be determined by ETAAS. Using a 10 mL aqueous sample, the enrichment factor of the procedure was 280 and detection limits of 0.2 and 3 ng L(-1) were obtained for cadmium and lead, respectively. The relative standard deviations for 10 replicates at the 10 ng L(-1) cadmium and 0.2 μg L(-1) lead levels were 6.5 and 7.3%, respectively. The method was successfully applied to the analysis of waters as well as to lixiviates obtained from toys made of plastic materials. PMID:23618174

  7. Improved determination of manganese in hair by use of a mini-autoclave and flameless atomic absorption spectrometry with Zeeman background correction: an evaluation in unexposed subjects

    SciTech Connect

    Guillard, O.; Brugier, J.C.; Piriou, A.; Menard, M.; Gombert, J.; Reiss, D.

    1984-10-01

    Motivated by the relatively wide range of values published hitherto, we offer a new, reliable method for determination of manganese in hair from unexposed human subjects. By using a mini-autoclave, we have developed a method that obviates loss of manganese during digestion and, thanks to use of a Teflon receptacle and rigorous methodology, contamination has been minimized. We used Zeeman flameless atomic absorption spectrometry, with the method of standard additions, for quantification. Within-run CVs for concentrations of Mn of 0.26 and 0.28 microgram/g of dry hair were 3.63 and 3.93%; the day-to-day CV for a Mn concentration of 0.29 microgram/g of dry hair was 5.84%. Mean (+/- SD) analytical recovery of Mn added to samples of hair was 104% (+/- 9.2%). The mean concentration of Mn found in the hair of 15 healthy unexposed subjects was 0.26 (+/- 0.05) microgram/g dry weight. This sensitive, reproducible procedure is suitable for use in analysis for traces of Mn in hair.

  8. Arsenic speciation in environmental samples by hydride generation and electrothermal atomic absorption spectrometry.

    PubMed

    Anawar, Hossain Md

    2012-01-15

    For the past few years many studies have been performed to determine arsenic (As) speciation in drinking water, food chain and other environmental samples due to its well-recognized carcinogenic and toxic effects relating to its chemical forms and oxidation states. This review provides an overview of analytical methods, preconcentration and separation techniques, developed up to now, using HGAAS and ETAAS for the determination of inorganic As and organoarsenic species in environmental samples. Specific advantages, disadvantages, selectivity, sensitivity, efficiency, rapidity, detection limit (DL), and some aspects of recent improvements and modifications for different analytical and separation techniques, that can define their application for a particular sample analysis, are highlighted. HG-AAS has high sensitivity, selectivity and low DL using suitable separation techniques; and it is a more suitable, affordable and much less expensive technique than other detectors. The concentrations of HCl and NaBH(4) have a critical effect on the HG response of As species. Use of l-cysteine as pre-reductant is advantageous over KI to obtain the same signal response for different As species under the same, optimum and mild acid concentration, and to reduce the interference of transition metals on the arsine generation. Use of different pretreatment, digestion, separation techniques and surfactants can determine As species with DL from ngL(-1) to μgL(-1). Out of all the chromatographic techniques coupled with HGAAS/ETAAS, ion-pair reversed-phase chromatography (IP-RP) is the most popular due to its higher separation efficiency, resolution selectivity, simplicity, and ability to separate up to seven As species for both non-ionic and ionic compounds in a signal run using the same column and short time. However, a combination of anion- and cation-exchange chromatography seems the most promising for complete resolution up to eight As species. The ETAAS method using different

  9. Intact MicroRNA Analysis Using High Resolution Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Kullolli, Majlinda; Knouf, Emily; Arampatzidou, Maria; Tewari, Muneesh; Pitteri, Sharon J.

    2014-01-01

    MicroRNAs (miRNAs) are small single-stranded non-coding RNAs that post-transcriptionally regulate gene expression, and play key roles in the regulation of a variety of cellular processes and in disease. New tools to analyze miRNAs will add understanding of the physiological origins and biological functions of this class of molecules. In this study, we investigate the utility of high resolution mass spectrometry for the analysis of miRNAs through proof-of-concept experiments. We demonstrate the ability of mass spectrometry to resolve and separate miRNAs and corresponding 3' variants in mixtures. The mass accuracy of the monoisotopic deprotonated peaks from various miRNAs is in the low ppm range. We compare fragmentation of miRNA by collision-induced dissociation (CID) and by higher-energy collisional dissociation (HCD) which yields similar sequence coverage from both methods but additional fragmentation by HCD versus CID. We measure the linear dynamic range, limit of detection, and limit of quantitation of miRNA loaded onto a C18 column. Lastly, we explore the use of data-dependent acquisition of MS/MS spectra of miRNA during online LC-MS and demonstrate that multiple charge states can be fragmented, yielding nearly full sequence coverage of miRNA on a chromatographic time scale. We conclude that high resolution mass spectrometry allows the separation and measurement of miRNAs in mixtures and a standard LC-MS setup can be adapted for online analysis of these molecules.

  10. Determination of inorganic and total mercury by vapor generation atomic absorption spectrometry using different temperatures of the measurement cell

    NASA Astrophysics Data System (ADS)

    Kaercher, Luiz Eduardo; Goldschmidt, Fabiane; Paniz, José Neri Gottfried; de Moraes Flores, Érico Marlon; Dressler, Valderi Luiz

    2005-06-01

    A simple and inexpensive laboratory-built flow injection vapor generation system coupled to atomic absorption spectrometry (FI-VG AAS) for inorganic and total mercury determination has been developed. It is based on the vapor generation of total mercury and a selective detection of Hg 2 + or total mercury by varying the temperature of the measurement cell. Only the inorganic mercury is measured when the quartz cell is at room temperature, and when the cell is heated to 650 °C or higher the total Hg concentration is measured. The organic Hg concentration in the sample is calculated from the difference between the total Hg and Hg 2 + concentrations. Parameters such as the type of acid (HCl or HNO 3) and its concentration, reductant (NaBH 4) concentration, carrier solution (HCl) flow rate, carrier gas flow rate, sample volume and quartz cell temperature, which influence FI-VG AAS system performance, were systematically investigated. The optimized conditions for Hg 2 + and total Hg determinations were: 1.0 mol l - 1 HCl as carrier solution, carrier flow rate of 3.5 ml min - 1 , 0.1% (m/v) NaBH 4, reductant flow rate of 1.0 ml min - 1 and carrier gas flow rate of 200 ml min - 1 . The relative standard deviation (RSD) is lower than 5.0% for a 1.0 μg l - 1 Hg solution and the limit of quantification (LOQ, 10 s) is 55 ng g - 1 . Certified samples of dogfish muscle (DORM-1 and DORM-2) and non-certified fish samples were analyzed, using a 6.0 mol l - 1 HCl solution for analyte extraction. The Hg 2 + and CH 3Hg + concentrations found were in agreement with certified ones.

  11. Model calculation of the characteristic mass for convective and diffusive vapor transport in graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Bencs, László; Laczai, Nikoletta; Ajtony, Zsolt

    2015-07-01

    A combination of former convective-diffusive vapor-transport models is described to extend the calculation scheme for sensitivity (characteristic mass - m0) in graphite furnace atomic absorption spectrometry (GFAAS). This approach encompasses the influence of forced convection of the internal furnace gas (mini-flow) combined with concentration diffusion of the analyte atoms on the residence time in a spatially isothermal furnace, i.e., the standard design of the transversely heated graphite atomizer (THGA). A couple of relationships for the diffusional and convectional residence times were studied and compared, including in factors accounting for the effects of the sample/platform dimension and the dosing hole. These model approaches were subsequently applied for the particular cases of Ag, As, Cd, Co, Cr, Cu, Fe, Hg, Mg, Mn, Mo, Ni, Pb, Sb, Se, Sn, V and Zn analytes. For the verification of the accuracy of the calculations, the experimental m0 values were determined with the application of a standard THGA furnace, operating either under stopped, or mini-flow (50 cm3 min- 1) of the internal sheath gas during atomization. The theoretical and experimental ratios of m0(mini-flow)-to-m0(stop-flow) were closely similar for each study analyte. Likewise, the calculated m0 data gave a fairly good agreement with the corresponding experimental m0 values for stopped and mini-flow conditions, i.e., it ranged between 0.62 and 1.8 with an average of 1.05 ± 0.27. This indicates the usability of the current model calculations for checking the operation of a given GFAAS instrument and the applied methodology.

  12. Simultaneous flow injection preconcentration of lead and cadmium using cloud point extraction and determination by atomic absorption spectrometry.

    PubMed

    Silva, Edson Luiz; Roldan, Paulo Dos Santos

    2009-01-15

    A flow injection (FI) micelle-mediated separation/preconcentration procedure for the determination of lead and cadmium by flame atomic absorption spectrometry (FAAS) has been proposed. The analytes reacted with 1-(2-thiazolylazo)-2-naphthol (TAN) to form hydrophobic chelates, which were extracted into the micelles of 0.05% (w/v) Triton X-114 in a solution buffered at pH 8.4. In the preconcentration stage, the micellar solution was continuously injected into a flow system with four mini-columns packed with cotton, glass wool, or TNT compresses for phase separation. The analytes-containing micelles were eluted from the mini-columns by a stream of 3molL(-1) HCl solution and the analytes were determined by FAAS. Chemical and flow variables affecting the preconcentration of the analytes were studied. For 15mL of preconcentrated solution, the enhancement factors varied between 15.1 and 20.3, the limits of detection were approximately 4.5 and 0.75microgL(-1) for lead and cadmium, respectively. For a solution containing 100 and 10microgL(-1) of lead and cadmium, respectively, the R.S.D. values varied from 1.6 to 3.2% (n=7). The accuracy of the preconcentration system was evaluated by recovery measurements on spiked water samples. The method was susceptible to matrix effects, but these interferences were minimized by adding barium ions as masking agent in the sample solutions, and recoveries from spiked sample varied in the range of 95.1-107.3%. PMID:18456398

  13. Determination of silicon and aluminum in silicon carbide nanocrystals by high-resolution continuum source graphite furnace atomic absorption spectrometry.

    PubMed

    Dravecz, Gabriella; Bencs, László; Beke, Dávid; Gali, Adam

    2016-01-15

    The determination of Al contaminant and the main component Si in silicon carbide (SiC) nanocrystals with the size-distribution of 1-8nm dispersed in an aqueous solution was developed using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS-GFAAS). The vaporization/atomization processes were investigated in a transversally heated graphite atomizer by evaporating solution samples of Al and Si preserved in various media (HCl, HNO3). For Si, the best results were obtained by applying a mixture of 5µg Pd plus 5µg Mg, whereas for Al, 10µg Mg (each as nitrate solution) was dispensed with the samples, but the results obtained without modifier were found to be better. This way a maximum pyrolysis temperature of 1200°C for Si and 1300°C for Al could be used, and the optimum (compromise) atomization temperature was 2400°C for both analytes. The Si and Al contents of different sized SiC nanocrystals, dispersed in aqueous solutions, were determined against aqueous (external) calibration standards. The correlation coefficients (R values) of the calibrations were found to be 0.9963 for Si and 0.9991 for Al. The upper limit of the linear calibration range was 2mg/l Si and 0.25mg/l Al. The limit of detection was 3µg/l for Si and 0.5µg/l for Al. The characteristic mass (m0) was calculated to be 389pg Si and 6.4pg Al. The Si and Al content in the solution samples were found to be in the range of 1.0-1.7mg/l and 0.1-0.25mg/l, respectively. PMID:26592606

  14. Rhodium as permanent modifier for atomization of lead from biological fluids using tungsten filament electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Zhou, Ying; Parsons, Patrick J.; Aldous, Kenneth M.; Brockman, Paul; Slavin, Walter

    2002-04-01

    Rhodium (Rh) was investigated as a permanent modifier for the atomization of Pb from biological fluids in W-filament atomic absorption spectrometry (AAS). Heating the W-filament with a Rh solution provided a protective coating for subsequent determinations of Pb in blood and urine matrices. The W-filament AAS instrumentation used was based on a prototype design that utilized self-reversal background correction scheme and peak area measurements. We found that Rh not only stabilized Pb during the pyrolysis step, but also facilitated the removal of carbonaceous residues during the cleaning step, requiring much less power than with phosphate modifier. Thus, the filament lifetime was greatly extended to over 300 firings. Periodic reconditioning with Rh was necessary every 30 firings or so. Conditioning the filament with Rh also permitted direct calibration using simple aqueous Pb standards. The method detection limit for blood Pb was approximately 1.5 μg dl -1, similar to that reported previously. Potential interferences from concomitants such as Na, K, Ca and Mg were evaluated. Accuracy was verified using lead reference materials from the National Institute of Standards and Technology and the New York State Department of Health. Blood lead results below 40 μg dl -1 were within ±1 μg dl -1 of certified values, and within ±10% above 40 μg dl -1; within-run precision was ±10% or better. Additional validation was reported using proficiency test materials and human blood specimens. All blood lead results were within the acceptable limits established by regulatory authorities in the US. When measuring Pb in urine, sensitivity was reduced and matrix-matched calibration became necessary. The method of detection limit was 27 μg l -1 for urine Pb. Urine lead results were also validated using an acceptable range comparable to that established for blood lead by US regulatory agencies.

  15. [Study of adsorption and desorption of behaviors of Pb2+ on thiol-modified bentonite by flame atomic absorption spectrometry].

    PubMed

    Chen, Wen; Xiong, Qiong-Xian; Pang, Xiao-Feng; Zhu, Xia-Ping; Han, Mei; Zhao, Qiu-Xiang; Liu, Wen-Hua

    2013-03-01

    A comparative analysis of the functional groups and surface structure of the Ca-bentonite (RB) and thiol-modified bentonite (TMB) were characterized by means of FTIR and SEM. The absorptive property of Pb2+ on TMB and RB and its influential factors was studied and the conditions for the adsorption were optimized by using FAAS method. Then the conditions for desorption of Pb2+ from the TMB by using simulated acid rain were studied and the contrast analysis of absorptive stability of Pb2+ on TMB and RB was given. The results showed that the adsorption rate of Pb2+ by TMB could reach more than 98%, when the initial Pb2+ concentration was 100 mg.L-1, the liquid-solid ratio was 5 g.L-1, pH was 6. 0, KNO3 ionic strength was 0. 1 mol.L-1 and adsorption period was 60min at 25 C. The saturated adsorption capacity of TMB was 67.27 mg.g-1; it's much more than that of RB (9.667 mg.g-1). The adsorption of Pb2+ on TMB follows Langmuir and Freundlich isotherm models well. Desorption experiments of Pb2+ from TMB with simulated acid rain (pH 3. 50) were done, and the desorption rate was 0. The results showed that TMB has a strong adsorption and fixation capacity for PbZ+; it is adapted to lead contaminated soil for chemical remediation. PMID:23705461

  16. Energy analysis of an ammonia-water absorption refrigeration system

    SciTech Connect

    Dincer, I.; Dost, S.

    1996-09-01

    Absorption refrigeration systems (ARSs) are run on heat-operated cycles. In these systems a secondary fluid (i.e., absorbent) is used to absorb the primary fluid (i.e., refrigerant) vaporized in the evaporator. ARSs for industrial and domestic applications have been attracting increasing interest throughout the world. A simple energy analysis technique for ammonia-water refrigeration systems is presented and verified with actual experimental data taken from the literature. Comparison was made in terms of the coefficient of performance, and very good agreement was found.

  17. Laser Desorption Mass Spectrometry for DNA Sequencing and Analysis

    NASA Astrophysics Data System (ADS)

    Chen, C. H. Winston; Taranenko, N. I.; Golovlev, V. V.; Isola, N. R.; Allman, S. L.

    1998-03-01

    Rapid DNA sequencing and/or analysis is critically important for biomedical research. In the past, gel electrophoresis has been the primary tool to achieve DNA analysis and sequencing. However, gel electrophoresis is a time-consuming and labor-extensive process. Recently, we have developed and used laser desorption mass spectrometry (LDMS) to achieve sequencing of ss-DNA longer than 100 nucleotides. With LDMS, we succeeded in sequencing DNA in seconds instead of hours or days required by gel electrophoresis. In addition to sequencing, we also applied LDMS for the detection of DNA probes for hybridization LDMS was also used to detect short tandem repeats for forensic applications. Clinical applications for disease diagnosis such as cystic fibrosis caused by base deletion and point mutation have also been demonstrated. Experimental details will be presented in the meeting. abstract.

  18. Field gas chromatography-mass spectrometry for fast analysis.

    PubMed

    Makas, Alexei L; Troshkov, Mikhail L

    2004-02-01

    The objective of this presentation is to demonstrate the original device and procedure for fast gas chromatography-mass spectrometry (GC-MS) analysis of gaseous and liquid samples and to discuss its features and capabilities. The concept was developed in order to expand the range of compounds suitable for GC separation and to reduce the time of analysis. Field GC-MS, consisting of original "concentrator-thermodesorber" (CTD) unit, multiple module GC system and compact magnetic mass spectrometer with powerful two-stage vacuum system and multicollector ion detector, is represented. The whole weight of the device is 90 kg. Power consumption is 250 W. The device and analytical procedures allow high speed screening of toxic substances in air and extracts within 100 s per sample. The examples of applications are described, including fast screening of tributyl phosphate (TBP) in air at low ppt level at the rate 1 sample/min. PMID:14698236

  19. Sequence analysis of styrenic copolymers by tandem mass spectrometry.

    PubMed

    Yol, Aleer M; Janoski, Jonathan; Quirk, Roderic P; Wesdemiotis, Chrys

    2014-10-01

    Styrene and smaller molar amounts of either m-dimethylsilylstyrene (m-DMSS) or p-dimethylsilylstyrene (p-DMSS) were copolymerized under living anionic polymerization conditions, and the compositions, architectures, and sequences of the resulting copolymers were characterized by matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS) and tandem mass spectrometry (MS(2)). MS analysis revealed that linear copolymer chains containing phenyl-Si(CH3)2H pendants were the major product for both DMSS comonomers. In addition, two-armed architectures with phenyl-Si(CH3)2-benzyl branches were detected as minor products. The comonomer sequence in the linear chains was established by MS(2) experiments on lithiated oligomers, based on the DMSS content of fragments generated by backbone C-C bond scissions and with the help of reference MS(2) spectra obtained from a polystyrene homopolymer and polystyrene end-capped with a p-DMSS block. The MS(2) data provided conclusive evidence that copolymerization of styrene/DMSS mixtures leads to chains with a rather random distribution of the silylated comonomer when m-DMSS is used, but to chains with tapered block structures, with the silylated units near the initiator, when p-DMSS is used. Hence, MS(2) fragmentation patterns permit not only differentiation of the sequences generated in the synthesis, but also the determination of specific comonomer locations along the polymer chain. PMID:25181590

  20. Analysis of hazardous biological material by MALDI mass spectrometry

    SciTech Connect

    KL Wahl; KH Jarman; NB Valentine; MT Kingsley; CE Petersen; ST Cebula; AJ Saenz

    2000-03-21

    Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-MS) has become a valuable tool for analyzing microorganisms. The speed with which data can be obtained from MALDI-MS makes this a potentially important tool for biological health hazard monitoring and forensic applications. The excitement in the mass spectrometry community in this potential field of application is evident by the expanding list of research laboratories pursuing development of MALDI-MS for bacterial identification. Numerous research groups have demonstrated the ability to obtain unique MALDI-MS spectra from intact bacterial cells and bacterial cell extracts. The ability to differentiate strains of the same species has been investigated. Reproducibility of MALDI-MS spectra from bacterial species under carefully controlled experimental conditions has also been demonstrated. Wang et al. have reported on interlaboratory reproducibility of the MALDI-MS analysis of several bacterial species. However, there are still issues that need to be addressed, including the careful control of experimental parameters for reproducible spectra and selection of optimal experimental parameters such as solvent and matrix.

  1. Laser desorption mass spectrometry for fast DNA analysis

    SciTech Connect

    Chen, C.H.; Ch`ang, L.Y.; Taranenko, N.I.; Allman, S.L.; Tang, K.; Matteson, K.J.

    1995-09-01

    During the past few years, major effort has been directed toward developing mass spectrometry to measure biopolymers because of the great potential benefit to biomedical research. Hellenkamp and his co-workers were the first to report that large polypeptide molecules can be ionized and detected without significant fragmentation when a greater number of nicotinic acid molecules are used as a matrix. This method is now well known as matrix-assisted laser desorption/ionization (MALDI). Since then, various groups have reported measurements of very large proteins by MALDI. Reliable protein analysis by MALDI is more or less well established. However, the application of MALDI to nucleic acids analysis has been found to be much more difficult. Most research on the measurement of nucleic acid by MALDI were stimulated by the Human Genome Project. Up to now, the only method for reliable routine analysis of nucleic acid is gel electrophoresis. Different sizes of nucleic acids can be separated in gel medium when a high electric field is applied to the gel. However, the time needed to separate different sizes of DNA segments usually takes from several minutes to several hours. If MALDI can be successfully used for nucleic acids analysis, the analysis time can be reduced to less than I millisecond. In addition, no tagging with radioactive materials or chemical dyes is needed. In this work, we will review recent progress related to MALDI for DNA analysis.

  2. Transition of Iodine Analysis to Accelerator Mass Spectrometry

    SciTech Connect

    M. L. Adamic; J. E. Olson; D. D. Jenson; J. G. Eisenmenger; M. G. Watrous

    2012-09-01

    This NA 22 funded research project investigated the transition of iodine isotopic analyses from thermal ionization mass spectrometry (TIMS) to an accelerator mass spectrometry (AMS) system. Previous work (Fiscal Year 2010) had demonstrated comparable data from TIMS and AMS. With AMS providing comparable data with improved background levels and vastly superior sample throughput, improvement in the sample extraction from environmental sample matrices was needed to bring sample preparation throughput closer to the operation level of the instrument. Previous research used an extraction chemistry that was not optimized for yield or refined for reduced labor to prove the principle. This research was done to find an extraction with better yield using less labor per sample to produce a sample ready for the AMS instrument. An extraction method using tetramethyl ammonium hydroxide (TMAH) was developed for removal of iodine species from high volume air filters. The TMAH with gentle heating was superior to the following three extraction methods: ammonium hydroxide aided by sonication, acidic and basic extraction aided by microwave, and ethanol mixed with sodium hydroxide. Taking the iodine from the extraction solvent to being ready for AMS analysis was accomplished by a direct precipitation, as well as, using silver wool to harvest the iodine from the TMAH. Portions of the same filters processed in FY 2010 were processed again with the improved extraction scheme followed by successful analysis by AMS at the Swiss Federal Institute of Technology. The data favorably matched the data obtained in 2010. The time required for analysis has been reduced over the aqueous extraction/AMS approach developed in FY 2010. For a hypothetical batch of 30 samples, the AMS methodology is about 10 times faster than the traditional gas phase chemistry and TIMS analysis. As an additional benefit, background levels for the AMS method are about 1000 times lower than TIMS. This results from the

  3. Determination of nickel in blood and serum samples of oropharyngeal cancer patients consumed smokeless tobacco products by cloud point extraction coupled with flame atomic absorption spectrometry.

    PubMed

    Arain, Sadaf Sadia; Kazi, Tasneem Gul; Arain, Jamshed Bashir; Afridi, Hassan Imran; Kazi, Atif Gul; Nasreen, Syeda; Brahman, Kapil Dev

    2014-10-01

    Oropharyngeal cancer is a significant public health issue in the world. The incidence of oropharyngeal cancer has been increased among people who have habit of chewing smokeless tobacco (SLT) in Pakistan. The aim of present study was to evaluate the concentration of nickel (Ni) in biological samples (whole blood, serum) of oral (n = 95) and pharyngeal (n = 84) male cancer patients. For comparison purposes, the biological samples of healthy age-matched referents (n = 150), who consumed and did not consumed SLT products, were also analyzed for Ni levels. As the Ni level is very low in biological samples, a preconcentration procedure has been developed, prior to analysis of analyte by flame atomic absorption spectrometry (FAAS). The Ni in acid-digested biological samples was complexed with ammonium pyrrolidinedithio carbamate (APDC), and a resulted complex was extracted in a surfactant Triton X-114. Acidic ethanol was added to the surfactant-rich phase prior to its analysis by FAAS. The chemical variables, such as pH, amounts of reagents (APDC, Triton X-114), temperature, incubation time, and sample volume were optimized. The resulted data indicated that concentration of Ni was higher in blood and serum samples of cancer patients as compared to that of referents who have or have not consumed different SLT products (p = 0.012-0.001). It was also observed that healthy referents who consumed SLT products have two to threefold higher levels of Ni in both biological samples as compared to those who were not chewing SLT products (p < 0.01). PMID:24920259

  4. In situ metathesis ionic liquid formation dispersive liquid-liquid microextraction for copper determination in water samples by electrothermal atomic absorption spectrometry.

    PubMed

    Stanisz, Ewa; Zgoła-Grześkowiak, Agnieszka

    2013-10-15

    In situ synthesis of ionic liquid extractant for dispersive liquid-liquid microextraction (in situ IL DLLME) combined with electrothermal atomic absorption spectrometry (ET AAS) for determination of copper in water samples was developed. Analytical signals were obtained without the back-extraction of copper from the IL phase prior to its determination by AAS. Some essential parameters of the microextraction and detection techniques such as the pH of sample solution, volume of components for in situ synthesis, matrix interferences and main parameters of graphite furnace atomizer have been studied. Under optimal conditions, high extraction efficiency for copper was achieved for the extraction of 0.7 µg L(-1) in 10.0 mL of sample solution employing 8 μL of 1-hexyl-3-methylimidazolium bis[(trifluoromethyl)sulfonyl]imide (HmimNTf2) as the extraction solvent. The detection limit was found as 0.004 µg L(-1) with an enrichment factor of 200. The relative standard deviation (RSD) for seven replicate measurements of 0.7 µg L(-1) in sample solution was 4%. The accuracy of the proposed method was evaluated by analysis of the Certified Reference Materials: NIST SRM 2709 (San Joaquin Soil), NBS SRM 2704 (Buffalo River Sediment), NRCC DOLT-2 (Dogfish Liver) and NIST SRM 1643e (Trace Element in Water). The measured copper contents in the reference materials were in satisfactory agreement with the certified values. The method was successfully applied to analysis of the tap, lake and mineral water samples. PMID:24054576

  5. On-line electrochemically controlled in-tube solid phase microextraction of inorganic selenium followed by hydride generation atomic absorption spectrometry.

    PubMed

    Asiabi, Hamid; Yamini, Yadollah; Seidi, Shahram; Shamsayei, Maryam; Safari, Meysam; Rezaei, Fatemeh

    2016-05-30

    In this work, for the first time, a rapid, simple and sensitive microextraction procedure is demonstrated for the matrix separation, preconcentration and determination of inorganic selenium species in water samples using an electrochemically controlled in-tube solid phase microextraction (EC-in-tube SPME) followed by hydride generation atomic absorption spectrometry (HG-AAS). In this approach, in which EC-in-tube SPME and HG-AAS system were combined, the total analysis time, was decreased and the accuracy, repeatability and sensitivity were increased. In addition, to increases extraction efficiency, a novel nanostructured composite coating consisting of polypyrrole (PPy) doped with ethyleneglycol dimethacrylate (EGDMA) was prepared on the inner surface of a stainless-steel tube by a facile electrodeposition method. To evaluate the offered setup and the new PPy-EGDMA coating, it was used to extract inorganic selenium species in water samples. Extraction of inorganic selenium species was carried out by applying a positive potential through the inner surface of coated in-tube under flow conditions. Under the optimized conditions, selenium was detected in amounts as small as 4.0 parts per trillion. The method showed good linearity in the range of 0.012-200 ng mL(-1), with coefficients of determination better than 0.9996. The intra- and inter-assay precisions (RSD%, n = 5) were in the range of 2.0-2.5% and 2.7-3.2%, respectively. The validated method was successfully applied for the analysis of inorganic selenium species in some water samples and satisfactory results were obtained. PMID:27154830

  6. On the possibilities of high-resolution continuum source graphite furnace atomic absorption spectrometry for the simultaneous or sequential monitoring of multiple atomic lines

    NASA Astrophysics Data System (ADS)

    Resano, M.; Rello, L.; Flórez, M.; Belarra, M. A.

    2011-05-01

    This paper explores the potential of commercially available high-resolution continuum source graphite furnace atomic absorption spectrometry instrumentation for the simultaneous or sequential monitoring of various atomic lines, in an attempt to highlight the analytical advantages that can be derived from this strategy. In particular, it is demonstrated how i) the monitoring of multiplets may allow for the simple expansion of the linear range, as shown for the measurement of Ni using the triplet located in the vicinity of 234.6 nm; ii) the use of a suitable internal standard may permit improving the precision and help in correcting for matrix-effects, as proved for the monitoring of Ni in different biological samples; iii) direct and multi-element analysis of solid samples may be feasible on some occasions, either by monitoring various atomic lines that are sufficiently close (truly simultaneous monitoring, as demonstrated in the determination of Co, Fe and Ni in NIST 1566a Oyster tissue) or, alternatively, by opting for a selective and sequential atomization of the elements of interest during every single replicate. Determination of Cd and Ni in BCR 679 White cabbage is attempted using both approaches, which permits confirming that both methods can offer very similar and satisfactory results. However, it is important to stress that the second approach provides more flexibility, since analysis is no longer limited to those elements that show very close atomic lines (closer than 0.3 nm in the ultraviolet region) with a sensitivity ratio similar to the concentration ratio of the analytes in the samples investigated.

  7. Performance analysis of solar powered absorption refrigeration system

    NASA Astrophysics Data System (ADS)

    Abu-Ein, Suleiman Qaseem; Fayyad, Sayel M.; Momani, Waleed; Al-Bousoul, Mamdouh

    2009-12-01

    The present work provides a detailed thermodynamic analysis of a 10 kW solar absorption refrigeration system using ammonia-water mixtures as a working medium. This analysis includes both first law and second law of thermodynamics. The coefficient of performance (COP), exergetic coefficient of performance (ECOP) and the exergy losses (Δ E) through each component of the system at different operating conditions are obtained. The minimum and maximum values of COP and ECOP were found to be at 110 and 200°C generator temperatures respectively. About 40% of the system exergy losses were found to be in the generator. The maximum exergy losses in the absorber occur at generator temperature of 130°C for all evaporator temperatures. A computer simulation model is developed to carry out the calculations and to obtain the results of the present study.

  8. Slag analysis with laser-induced breakdown spectrometry.

    PubMed

    Kraushaar, M; Noll, R; Schmitz, H U

    2003-10-01

    Laser-induced breakdown spectrometry (LIBS) has been applied for multi-elemental analysis of slag samples from a steel plant. In order to avoid the time-consuming step of sample preparation, the liquid slag material can be filled in special probes. After cooling of the liquid slag and solidification, the samples can be analyzed with LIBS. Chemical analysis of slag is an essential input parameter used for numerical simulations to control liquid steel processing. The relative variation range of element concentrations in slag samples from steel production can amount to up to 30%. A multivariate calibration model is used to take into account matrix effects caused by these varying concentrations. By optimizing the measuring parameters as well as the calibration models, an agreement between the standard X-ray fluorescence (XRF) analysis and LIBS analysis in terms of the coefficient of determination r2 of 0.99 for the main analytes CaO, SiO2, and Fetot of converter slag samples was achieved. The average repeatability of the LIBS measurement for these elements in terms of the relative standard deviation of the determined concentration is improved to less than 1.0%. With these results, the basis is established for future on-line applications of LIBS in the steel-making industry for slag analysis. PMID:14639759

  9. Effect of magnesium acetylacetonate on the signal of organic forms of vanadium in graphite furnace atomic absorption spectrometry.

    PubMed

    Kowalewska, Zofia; Welz, Bernhard; Castilho, Ivan N B; Carasek, Eduardo

    2013-01-15

    The aim of this work was to investigate the influence of magnesium acetylacetonate (MgA) on the signal of organic forms of vanadium in xylene solution by graphite furnace atomic absorption spectrometry. MgA alone or mixed with palladium acetylacetonate (PdA) was considered as a chemical modifier. It has been found that MgA does not improve, but decreases significantly the integrated absorbance of V in the form of alkyl-aryl sulfonates, acetylacetonates, porphyrins and in lubricating oils, while its effect is negligible in the case of "dark products" from petroleum distillation, i.e., heavy oil fractions and residues. The decrease is also observed in the presence of Pd. The MgA (or MgA+PdA) effect on the integrated absorbance of V has been studied using the following variants: different ways of modifier application, various pyrolysis temperature, additional application of air ashing, preliminary pretreatment with iodine and methyltrioctylammonium chloride, application of various graphite furnace heating systems (longitudinal or transverse) and various optical and background correction systems (medium-resolution line source spectrometer with deuterium background correction or high-resolution continuum source spectrometer). The experiments indicate formation of more refractory compounds as a possible reason for the decrease of the integrated absorbance for some forms of V in the presence of MgA. The application of MgA as a chemical modifier in V determination is not recommended. Results of this work have general importance as, apart from the intentional use of MgA as a modifier, organic Mg compounds, present in petroleum products for other reason (e.g. as an additive), can influence the signal of V compounds and hence the accuracy in V determination. Generally, petroleum products with known amount of V are recommended as standards; however, lubricating oils can be inadequate for "dark products" from petroleum distillation. In the case of unknown samples it is

  10. Dispersive liquid-liquid microextraction combined with graphite furnace atomic absorption spectrometry: ultra trace determination of cadmium in water samples.

    PubMed

    Zeini Jahromi, Elham; Bidari, Araz; Assadi, Yaghoub; Milani Hosseini, Mohammad Reza; Jamali, Mohammad Reza

    2007-03-01

    Dispersive liquid-liquid microextraction (DLLME) technique was successfully used as a sample preparation method for graphite furnace atomic absorption spectrometry (GF AAS). In this extraction method, 500 microL methanol (disperser solvent) containing 34 microL carbon tetrachloride (extraction solvent) and 0.00010 g ammonium pyrrolidine dithiocarbamate (chelating agent) was rapidly injected by syringe into the water sample containing cadmium ions (interest analyte). Thereby, a cloudy solution formed. The cloudy state resulted from the formation of fine droplets of carbon tetrachloride, which have been dispersed, in bulk aqueous sample. At this stage, cadmium reacts with ammonium pyrrolidine dithiocarbamate, and therefore, hydrophobic complex forms which is extracted into the fine droplets of carbon tetrachloride. After centrifugation (2 min at 5000 rpm), these droplets were sedimented at the bottom of the conical test tube (25+/-1 microL). Then a 20 microL of sedimented phase containing enriched analyte was determined by GF AAS. Some effective parameters on extraction and complex formation, such as extraction and disperser solvent type and their volume, extraction time, salt effect, pH and concentration of the chelating agent have been optimized. Under the optimum conditions, the enrichment factor 125 was obtained from only 5.00 mL of water sample. The calibration graph was linear in the rage of 2-20 ng L(-1) with detection limit of 0.6 ng L(-1). The relative standard deviation (R.S.D.s) for ten replicate measurements of 20 ng L(-1) of cadmium was 3.5%. The relative recoveries of cadmium in tap, sea and rivers water samples at spiking level of 5 and 10 ng L(-1) are 108, 95, 87 and 98%, respectively. The characteristics of the proposed method have been compared with cloud point extraction (CPE), on-line liquid-liquid extraction, single drop microextraction (SDME), on-line solid phase extraction (SPE) and co-precipitation based on bibliographic data. Therefore, DLLME

  11. Rapid determination of lead in water samples by dispersive liquid-liquid microextraction coupled with electrothermal atomic absorption spectrometry.

    PubMed

    Naseri, Mohammad Taghi; Hosseini, Mohammad Reza Milani; Assadi, Yaghoub; Kiani, Armin

    2008-03-15

    The need for highly reliable methods for the determination of trace and ultratrace elements has been recognized in analytical chemistry and environmental science. A simple and powerful microextraction technique was used for the detection of the lead ultratrace amounts in water samples using the dispersive liquid-liquid microextraction (DLLME), followed by the electrothermal atomic absorption spectrometry (ET AAS). In this microextraction technique, a mixture of 0.50 mL acetone (disperser solvent), containing 35 microL carbon tetrachloride (extraction solvent) and 5 microL diethyldithiophosphoric acid (chelating agent), was rapidly injected by syringe into the 5.00 mL water sample, spiked with lead. In this process, the lead ions reacted with the chelating agent and were extracted into the fine droplets of CCl(4). After centrifugation (2 min at 5000 rpm), the fine CCl4 droplets were sedimented at the bottom of the conical test tube (25+/-1 microL). Then, 20 microL from the sedimented phase, containing the enriched analyte, was determined by ET AAS. The next step was the optimization of various experimental conditions, affecting DLLME, such as the type and the volume of the extraction solvent, the type and the volume of the disperser solvent, the extraction time, the salt effect, pH and the chelating agent amount. Moreover, the effect of the interfering ions on the analytes recovery was also investigated. Under the optimum conditions, the enrichment factor of 150 was obtained from only a 5.00 mL water sample. The calibration graph was linear in the range of 0.05-1 microg L(-1) with the detection limit of 0.02 microg L(-1). The relative standard deviation (R.S.D.) for seven replicate measurements of 0.50 microg L(-1) of lead was 2.5%. The relative lead recoveries in mineral, tap, well and sea water samples at the spiking level of 0.20 and 0.40 microg L(-1) varied from 93.5 to 105.0. The characteristics of the proposed method were compared with the cloud point

  12. In situ secondary ion mass spectrometry analysis. 1992 Summary report

    SciTech Connect

    Groenewold, G.S.; Applehans, A.D.; Ingram, J.C.; Delmore, J.E.; Dahl, D.A.

    1993-01-01

    The direct detection of tributyl phosphate (TBP) on rocks using molecular beam surface analysis [MBSA or in situ secondary ion mass spectrometry (SIMS)] is demonstrated. Quantities as low as 250 ng were detected on basalt and sandstone with little or no sample preparation. Detection of TBP on soil has proven to be more problematic and requires further study. Ethylenediaminetetraacetic acid (EDTA) is more difficult to detect because it is very reactive with surfaces of interest. Nevertheless, it is possible to detect EDTA if the acidity of the surface is controlled. The detection of EDTA-metal complexes is currently an open question, but evidence is presented for the detection of ions arising from a EDTA-lead complex. Carboxylic acids (i.e., citric, ascorbic, malic, succinic, malonic, and oxalic) give characteristic SIM spectra, but their detection on sample surfaces awaits evaluation.

  13. A highly sensitive method for in vitro testing of fluorinated drug candidates using high-resolution continuum source molecular absorption spectrometry (HR-CS MAS).

    PubMed

    Würtenberger, Irene; Gust, Ronald

    2014-05-01

    We report here the development, optimization, and evaluation of a highly sensitive method for the determination of fluorine in biological matrices employing highresolution continuum source molecular absorption spectrometry (HR-CS MAS), suitable for pharmacological testing of fluorine-containing drug candidates. For this purpose, the most important parameters were studied in detail and subsequently optimized using a multivariate approach based on experimental design methodology. We developed a new approach employing a graphite tube lined with tantalum foil, thereby significantly enhancing sensitivity, while interferences from phosphorus monoxide (PO) molecular absorption due to the complex phosphate-rich matrix were completely eliminated. The limit of detection and the characteristic mass were 5.79 and 6.08 pg F, respectively. In order to evaluate the accuracy of the procedure, a recovery test was performed using spiked samples from three bioassays (i.e., DNA binding, protein binding, and cellular uptake) and the recovery rates ranged from 97.4 to 106.4%. The proposed method is applicable for preclinical in vitro testing of fluorinated drug molecules and thereby establishes HR-CS atomic absorption spectrometry instrumentation as a universal tool in medicinal chemistry. PMID:24760395

  14. Hollow fiber liquid phase microextraction combined with graphite furnace atomic absorption spectrometry for the determination of methylmercury in human hair and sludge samples

    NASA Astrophysics Data System (ADS)

    Jiang, Hongmei; Hu, Bin; Chen, Beibei; Zu, Wanqing

    2008-07-01

    Two methods, based on hollow fiber liquid-liquid-liquid (three phase) microextraction (HF-LLLME) and hollow fiber liquid phase (two phase) microextraction (HF-LPME), have been developed and critically compared for the determination of methylmercury content in human hair and sludge by graphite furnace atomic absorption spectrometry (GFAAS). In HF-LPME, methylmercury was extracted into the organic phase (toluene) prior to its determination by GFAAS, while inorganic mercury remained as a free species in the sample solution. In HF-LLLME, methylmercury was first extracted into the organic phase (toluene) and then into the acceptor phase (4% thiourea in 1 mol L - 1 HCl) prior to its determination by GFAAS, while inorganic mercury remained in the sample solution. The total mercury was determined by inductively coupled plasma-mass spectrometry (ICP-MS), and the levels of inorganic mercury in both HF-LLLME and HF-LPME were obtained by subtracting methylmercury from total mercury. The factors affecting the microextraction of methylmercury, including organic solvent, extraction time, stirring rate and ionic strength, were investigated and the optimal extraction conditions were established for both HF-LLLPME and HF-LPME. With a consumption of 3.0 mL of the sample solution, the enrichment factors were 204 and 55 for HF-LLLPME and HF-LPME, respectively. The limits of detection (LODs) for methylmercury were 0.1 μg L - 1 and 0.4 μg L - 1 (as Hg) with precisions (RSDs (%), c = 5 μg L - 1 (as Hg), n = 5) of 13% and 11% for HF-LLLPME-GFAAS and HF-LPME-GFAAS, respectively. For ICP-MS determination of total mercury, a limit of detection of 39 ng L - 1 was obtained. Finally, HF-LLLME-GFAAS was applied to the determination of methylmercury content in human hair and sludge, and the recoveries for the spiked samples were in the range of 99-113%. In order to validate the method, HF-LLLME-GFAAS was also applied to the analysis of a certified reference material of NRCC DORM-2 dogfish

  15. Fast heating induced impulse halogenation of refractory sample components in electrothermal atomic absorption spectrometry by direct injection of a liquid halogenating agent.

    PubMed

    György, Krisztina; Ajtony, Zsolt; Van Meel, Katleen; Van Grieken, René; Czitrovszky, Aladár; Bencs, László

    2011-09-15

    A novel electrothermal atomic absorption spectrometry (ETAAS) method was developed for the halogenation of refractory sample components (Er, Nd and Nb) of lithium niobate (LiNbO(3)) and bismuth tellurite (Bi(2)TeO(5)) optical single crystals to overcome memory effects and carry-over. For this purpose, the cleaning step of a regular graphite furnace heating program was replaced with a halogenation cycle. In this cycle, after the graphite tube cooled to room temperature, a 20 μL aliquot of liquid carbon tetrachloride (CCl(4)) was dispensed with a conventional autosampler into the graphite tube. The CCl(4) was partially dried at 80°C under the mini-flow (40 cm(3) min(-1)) condition of the Ar internal furnace gas (IFG), then the residue was decomposed (pyrolyzed) by fast furnace heating at 1900-2100°C under interrupted flow of the IFG. This step was followed by a clean-out stage at 2100°C under the maximum flow of the IFG. The advantage of the present method is that it does not require any alteration to the graphite furnace gas supply system in contrast to most of the formerly introduced halogenation techniques. The effectiveness of the halogenation method was verified with the determination of Er and Nd dopants in the optical crystals. In these analyses, a sensitivity decrease was observed, which was likely due to the enhanced deterioration of the graphite tube surface. Therefore, the application of mathematical correction (resloping) of the calibration was also required. The calibration curves were linear up to 1.5 and 10 μmol L(-1) for Er and Nd, respectively. Characteristic masses of 18 and 241 pg and the limit of detection (LOD) values of 0.017 and 0.27 μmol L(-1) were found for Er and Nd, respectively. These LOD data correspond to 0.68 μmol mol(-1) Er and 11 μmol mol(-1) Nd in solid bismuth tellurite samples. The analytical results were compared with those obtained by a conventional ETAAS method and validated with X-ray fluorescence spectrometry analysis

  16. Petroleomics by Direct Analysis in Real Time-Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Romão, Wanderson; Tose, Lilian V.; Vaz, Boniek G.; Sama, Sara G.; Lobinski, Ryszard; Giusti, Pierre; Carrier, Hervé; Bouyssiere, Brice

    2016-01-01

    The analysis of crude oil and its fractions by applying ambient ionization techniques remains underexplored in mass spectrometry (MS). Direct analysis in real time (DART) in the positive-ion mode was coupled to a linear quadrupole ion trap Orbitrap mass spectrometer (LTQ Orbitrap) to analyze crude oil, paraffin samples, and porphyrin standard compounds. The ionization parameters of DART-MS were optimized for crude oil analysis. DART-MS rendered the optimum conditions of the operation using paper as the substrate, T = 400°C, helium as the carrier gas, and a sample concentration ≥6 mg mL-1. In the crude oils analysis, the DART(+)-Orbitrap mass spectra detected the typical N, NO, and O-containing compounds. In the paraffin samples, oxidized hydrocarbon species (Ox classes, where x = 1-4) with double-bond equivalent of 1-4 were detected, and their structures and connectivity were confirmed by collision-induced dissociation (CID) experiments. DART(+)-MS has identified the porphyrin standard compounds as [M + H]+ ions of m/ z 615.2502 and 680.1763, where M = C44H30N4 and C44H28N4OV, respectively, based on the formula assignment and by phenyl losses observed on CID experiments.

  17. Petroleomics by Direct Analysis in Real Time-Mass Spectrometry.

    PubMed

    Romão, Wanderson; Tose, Lilian V; Vaz, Boniek G; Sama, Sara G; Lobinski, Ryszard; Giusti, Pierre; Carrier, Hervé; Bouyssiere, Brice

    2016-01-01

    The analysis of crude oil and its fractions by applying ambient ionization techniques remains underexplored in mass spectrometry (MS). Direct analysis in real time (DART) in the positive-ion mode was coupled to a linear quadrupole ion trap Orbitrap mass spectrometer (LTQ Orbitrap) to analyze crude oil, paraffin samples, and porphyrin standard compounds. The ionization parameters of DART-MS were optimized for crude oil analysis. DART-MS rendered the optimum conditions of the operation using paper as the substrate, T = 400°C, helium as the carrier gas, and a sample concentration ≥6 mg mL(-1). In the crude oils analysis, the DART(+)-Orbitrap mass spectra detected the typical N, NO, and O-containing compounds. In the paraffin samples, oxidized hydrocarbon species (Ox classes, where x = 1-4) with double-bond equivalent of 1-4 were detected, and their structures and connectivity were confirmed by collision-induced dissociation (CID) experiments. DART(+)-MS has identified the porphyrin standard compounds as [M + H](+) ions of m/z 615.2502 and 680.1763, where M = C44H30N4 and C44H28N4OV, respectively, based on the formula assignment and by phenyl losses observed on CID experiments. PMID:26432579

  18. Transition of Iodine Analysis to Accelerator Mass Spectrometry

    SciTech Connect

    J. E. Delmore

    2010-09-01

    Funding was received from NA-22 to investigate transitioning iodine isotopic analyses to an accelerator mass spectrometry (AMS) system. The present method uses gas-phase chemistry followed by thermal ionization mass spectrometry (TIMS). It was anticipated that the AMS approach could provide comparable data, with improved background levels and superior sample throughput. An aqueous extraction method was developed for removal of iodine species from high-volume air filters. Ethanol and sodium hydroxide, plus heating and ultrasonic treatment, were used to successfully extract iodine from loaded high-volume air filters. Portions of the same filters were also processed in the traditional method and analyzed by TIMS for comparison. Aliquot parts of the aqueous extracts were analyzed by AMS at the Swiss Federal Institute of Technology. Idaho National Laboratory (INL) personnel visited several AMS laboratories in the US, Spain, and Switzerland. Experience with AMS systems from several manufacturers was gained, and relationships were developed with key personnel at the laboratories. Three batches of samples were analyzed in Switzerland, and one in Spain. Results show that the INL extraction method successfully extracted enough iodine from high-volume air filters to allow AMS analysis. Comparison of the AMS and TIMS data is very encouraging; while the TIMS showed about forty percent more atoms of 129I, the 129/127 ratios tracked each other very well between the two methods. The time required for analysis is greatly reduced for the aqueous extraction/AMS approach. For a hypothetical batch of thirty samples, the AMS methodology is about five times faster than the traditional gas-phase chemistry and TIMS analysis. As an additional benefit, background levels for the AMS method are about 1000 times lower than for TIMS. This results from the fundamental mechanisms of ionization in the AMS system and cleanup of molecular interferences. We showed that an aqueous extraction of high

  19. Analysis of tungsten carbides by X-ray fluorescence spectrometry.

    PubMed

    Kinson, K; Knott, A C; Belcher, C B

    Five sample presentation techniques were examined for the X-ray fluorescence spectrometric analysis of tungsten carbide alloys in powder and cemented forms. Powder samples may be oxidized by air at 600 degrees before fusion (I), or preferably by lithium nitrate during fusion (II); the fusion is effected with lithium-lanthanum tetraborate followed by briquetting with graphite. Powder samples may also be blended with wax and briquetted (III). Cemented carbides are surface-prepared with silicon carbide before analysis (V). Briquettes prepared by blending carbide powder, lithium-lanthanum tetraborate and graphite (IV), give poor reproducibility, however, owing to micro-absorption effects the technique is not recommended. The determination of eight common elements in tungsten carbide is discussed and the relative standard deviations are 0.002-0.004 for major and 0.008-0.01 for minor elements. PMID:18961988

  20. 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.

  1. Determination of trace amounts of gold in acid-attacked environmental samples by atomic absorption spectrometry with electrothermal atomization after preconcentration.

    PubMed

    Medved, Ján; Bujdos, Marek; Matús, Peter; Kubová, Jana

    2004-05-01

    A method for determination of trace amounts of gold in environmental samples (rocks, soils, sediments, and waters) by atomic absorption spectrometry with electrothermal atomization (ETAAS) after preconcentration using a chelating sorbent Spheron Thiol 1000 is described. The method accurately determines gold between 0.001 and several tens of grams per ton in samples having complex variations in mineralogy. Pulverized samples are roasted at 650 degrees C to oxidize any sulfide and/or carbonaceous material. Samples are then subjected to a series of acid treatments to eliminate any silica matrix and to dissolve the sample. The Spheron Thiol 1000 is added to the sample solution, and then with sorbed gold is filtered out, washed, and ignited at 550 degrees C. The residue is dissolved in aqua regia, evaporated, dissolved in distilled water, transferred to a volumetric flask, and analyzed by ETAAS. The limits of detection of gold, based on the 3 sigma definition, were 0.5 ng g(-1) for 10-g samples (rocks, sediments, soils) and 0.05 ng mL(-1) for 1-L water samples. Precision of determination expressed by the relative standard deviation varied from 2.9% to 16.4%. The accuracy of the method is verified by analysis of certified reference materials. The obtained analytical results are in good agreement with attested values. The developed method was applied for gold determination in environmental samples affected by the acidification (acid mine drainage which is mainly a product of pyrite oxidation) from an open quartzite mine in the Sobov region situated NE of the city of Banská Stiavnica (Slovakia). PMID:14997262

  2. Dithiocarbamate functionalized or surface sorbed Merrifield resin beads as column materials for on line flow injection-flame atomic absorption spectrometry determination of lead.

    PubMed

    Praveen, R S; Naidu, G R K; Prasada Rao, T

    2007-09-26

    This article describes the preparation of dithiocarbamate immobilized/functionalized and diethylammonium dithiocarbamate (DDTC) sorbed Merrifield Chloromethylated Resin (MCR) beads and comparison of these materials for on-line flow injection (FI)-flame atomic absorption spectrometry (FAAS) determination of lead. The above two materials enrich lead quantitatively over an identical optimal pH range (8.0-9.0), a preconcentration/loading time (up to 4 min) and elution with acidified methanol (a minimum of 0.01 molL(-1) HNO(3) in methanol). However, the detection limit for lead using dithiocarbamate functionalized MCR beads is 1.3 microgL(-1) compared to 3 microgL(-1) for DDTC sorbed MCR beads. Again, the sensitivity enhancement over direct FAAS signal is 48- and 27-fold, respectively. In addition, dithiocarbamate functionalized MCR beads offers better precision compared to DDTC sorbed MCR beads as the corresponding relative standard deviation (R.S.D.) values for five successive determinations of 0.20 microgmL(-1) are 1.44 and 4.36%, respectively. The accuracy of the developed on-line FI-FAAS procedure employing dithiocarbamate functionalized MCR beads as column material was tested by analyzing Certified Reference Material (CRM) of soil (IAEA soil-7) and marine sediment reference material (MESS-3) supplied by International Atomic Energy Agency (IAEA), Vienna and National Research Council (NRC), Canada, respectively. Furthermore, the developed procedure has been successfully tested for the analysis of surface, pond, ground and effluent water and soil samples collected from the vicinity of lead acid battery industry in India. PMID:17903486

  3. A study of the distribution of aluminium in human placental tissues based on alkaline solubilization with determination by electrothermal atomic absorption spectrometry.

    PubMed

    Kruger, Pamela C; Schell, Lawrence M; Stark, Alice D; Parsons, Patrick J

    2010-09-01

    Aluminium (Al) is a nonessential element known to induce neurotoxic effects, such as dialysis dementia, in patients on hemodialysis, with compromised kidney function. The role of Al in the progression of some neurodegenerative diseases, such as Alzheimer's disease (AD), is controversial, and remains unclear. The effects of Al on other vulnerable populations, such as fetuses and infants, have been infrequently studied. In the present study, Al has been measured in human placenta samples, comprising ∼160 each of placenta bodies, placenta membranes, and umbilical cords, using electrothermal atomic absorption spectrometry (ETAAS) after atmospheric pressure digestion with tetramethylammonium hydroxide (TMAH) and ethylenediaminetetraacidic acid (EDTA). The sensitivity, or characteristic mass (m(0)), for Al at the 309.3-nm line was found to be 30 ± 4 pg. The instrumental detection limit (IDL) (3s) for Al in solution was calculated as 0.72 μg L(-1) while the method detection limit (MDL) (3s) was 0.25 μg g(-1). Accuracy was assessed through analysis of quality control (QC) materials, including certified reference materials (CRMs), in-house reference materials (RMs), and spike recovery experiments, of varying matrices. Placental tissue analyses revealed geometric mean concentrations of approximately 0.5 μg g(-1) Al in placenta bodies (n = 165) and membranes (n = 155), while Al concentrations in umbilical cords (n = 154) were about 0.3 μg g(-1). Al was detected in 95% of placenta bodies, and 81% of placenta membranes, but only in 46% of umbilical cords. PMID:21072353

  4. A study of the distribution of aluminum in human placental tissues based on alkaline solubilization with determination by electrothermal atomic absorption spectrometry

    PubMed Central

    Kruger, Pamela C.; Schell, Lawrence M.; Stark, Alice D.; Parsons, Patrick J.

    2010-01-01

    Summary Aluminum (Al) is a nonessential element known to induce neurotoxic effects, such as dialysis dementia, in patients on hemodialysis, with compromised kidney function. The role of Al in the progression of some neurodegenerative diseases, such as Alzheimer’s disease (AD), is controversial, and remains unclear. The effects of Al on other vulnerable populations, such as fetuses and infants, have been infrequently studied. In the present study, Al has been measured in human placenta samples, comprising ~160 each of placenta bodies, placenta membranes, and umbilical cords, using electrothermal atomic absorption spectrometry (ETAAS) after atmospheric pressure digestion with tetramethylammonium hydroxide (TMAH) and ethylenediaminetetraacidic acid (EDTA). The sensitivity, or characteristic mass (m0), for Al at the 309.3-nm line was found to be 30 ± 4 pg. The instrumental detection limit (IDL) (3s) for Al in solution was calculated as 0.72 μg L-1, while the method detection limit (MDL) (3s) was 0.25 μg g-1. Accuracy was assessed through analysis of quality control (QC) materials, including certified reference materials (CRMs), in-house reference materials (RMs), and spike recovery experiments, of varying matrices. Placental tissue analyses revealed geometric mean concentrations of approximately 0.5 μg g-1 Al in placenta bodies (n=165) and membranes (n=155), while Al concentrations in the umbilical cord (n=154) were about 0.3 μg g-1. Al was detected in 95% of placenta bodies, and 81% of placenta membranes, but only in 46% of umbilical cords. PMID:21072353

  5. 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

    2016-02-01

    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. PMID:26520476

  6. 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.

  7. Ionic liquid-based ultrasound-assisted dispersive liquid-liquid microextraction combined with electrothermal atomic absorption spectrometry for a sensitive determination of cadmium in water samples

    NASA Astrophysics Data System (ADS)

    Li, Shengqing; Cai, Shun; Hu, Wei; Chen, Hao; Liu, Hanlan

    2009-07-01

    A new method was developed for the determination of cadmium in water samples using ionic liquid-based ultrasound-assisted dispersive liquid-liquid microextraction (IL-based USA-DLLME) followed by electrothermal atomic absorption spectrometry (ETAAS). The IL-based USA-DLLME procedure is free of volatile organic solvents, and there is no need for a dispersive solvent, in contrast to conventional DLLME. The ionic liquid, 1-hexyl-3-methylimidazolium hexafluorophosphate (HMIMPF 6), was quickly disrupted by an ultrasonic probe for 1 min and dispersed in water samples like a cloud. At this stage, a hydrophobic cadmium-DDTC complex was formed and extracted into the fine droplets of HMIMPF 6. After centrifugation, the concentration of the enriched cadmium in the sedimented phase was determined by ETAAS. Some effective parameters of the complex formation and microextraction, such as the concentration of the chelating agent, the pH, the volume of the extraction solvent, the extraction time, and the salt effect, have been optimized. Under optimal conditions, a high extraction efficiency and selectivity were reached for the extraction of 1.0 ng of cadmium in 10.0 mL of water solution employing 73 µL of HMIMPF 6 as the extraction solvent. The enrichment factor of the method is 67. The detection limit was 7.4 ng L - 1 , and the characteristic mass ( m0, 0.0044 absorbance) of the proposed method was 0.02 pg for cadmium (Cd). The relative standard deviation (RSD) for 11 replicates of 50 ng L - 1 Cd was 3.3%. The method was applied to the analysis of tap, well, river, and lake water samples and the Environmental Water Reference Material GSBZ 50009-88 (200921). The recoveries of spiked samples were in the range of 87.2-106%.

  8. Activated carbon-modified knotted reactor coupled to electrothermal atomic absorption spectrometry for sensitive determination of arsenic species in medicinal herbs and tea infusions

    NASA Astrophysics Data System (ADS)

    Grijalba, Alexander Castro; Martinis, Estefanía M.; Lascalea, Gustavo E.; Wuilloud, Rodolfo G.

    2015-01-01

    A flow injection system based on a modified polytetrafluoroethylene (PTFE) knotted reactor (KR) was developed for arsenite [As(III)] and arsenate [As(V)] species preconcentration and determination by electrothermal atomic absorption spectrometry (ETAAS). Activated carbon (AC) was immobilized on the inner walls of a PTFE KR by a thermal treatment. A significant increase in analyte retention was obtained with the AC-modified KR (100%) as compared to the regular PTFE KR (25%). The preconcentration method involved the on-line formation of As(III)-ammonium pyrrolidinedithiocarbamate (As-APDC) complex, followed by its adsorption onto the inner walls of the AC-modified KR. After analyte retention, the complex was eluted with acetone directly into the graphite furnace of ETAAS. The parameters affecting the flow injection system were evaluated with a full central composite face centered design with three center points. Under optimum conditions, a preconcentration factor of 200 was obtained with 10 ml of sample. The detection limit was 4 ng L- 1 and the relative standard deviation (RSD) for six replicate measurements at 0.2 μg L- 1 of As were 4.3% and 4.7% for As(III) and As(V), respectively. The developed methodology was highly selective towards As(III), while As(V), monomethylarsonic acid [MMA(V)] and dimethylarsinic [DMA(V)] were not retained in the AC-modified KR. The proposed method was successfully applied for As speciation analysis in infusions originated from medicinal herbs and tea.

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

    PubMed

    Shokri, Masood; Beiraghi, Asadollah; Seidi, Shahram

    2015-08-19

    For the first time, a simple and efficient in situ emulsification microextraction method using a dicationic ionic liquid followed by magnetic assisted physisorption was presented to determine trace amounts of lead. In this method, 400 μL of 1.0 mol L(-1) lithium bis (trifluoromethylsulfonyl) imide aqueous solution, Li[NTf2], was added into the sample solution containing 100 μL of 1.0 mol L(-1) 1,3-(propyl-1,3-diyl) bis (3-methylimidazolium) chloride, [pbmim]Cl2, to form a water immiscible ionic liquid, [pbmim][NTf2]2. This new in situ formed dicationic ionic liquid was applied as the acceptor phase to extract the lead-ammonium pyrrolidinedithiocarbamate (Pb-APDC) complexes from the sample solution. Subsequently, 30 mg of Fe3O4 magnetic nanoparticles (MNPs) were added into the sample solution to collect the fine droplets of [pbmim][NTf2]2, physisorptively. Finally, MNPs were eluted by acetonitrile, separated by an external magnetic field and the obtained eluent was subjected to micro-sampling flame atomic absorption spectrometry (FAAS) for further analysis. Comparing with other microextraction methods, no special devices and centrifugation step are required. Parameters influencing the extraction efficiency such as extraction time, pH, concentration of chelating agent, amount of MNPs and coexisting interferences were studied. Under the optimized conditions, this method showed high extraction recovery of 93% with low LOD of 0.7 μg L(-1). Good linearity was obtained in the range of 2.5-150 μg L(-1) with determination coefficient (r(2)) of 0.9921. Relative standard deviation (RSD%) for seven repeated measurements at the concentration of 10 μg L(-1) was 4.1%. Finally, this method was successfully applied for determination of lead in some water and plant samples. PMID:26343434

  10. 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. PMID:27216654

  11. 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.

  12. A dried urine spot test to simultaneously monitor Mo and Ti levels using solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Rello, L.; Lapeña, A. C.; Aramendía, M.; Belarra, M. A.; Resano, M.

    2013-03-01

    Home-based collection protocols for clinical specimens are actively pursued as a means of improving life quality of patients that require frequent controls, such as patients with metallic prosthesis, for whom monitoring the evolution of Mo and Ti in biological fluids may play a decisive role to detect prosthesis mal-functioning. The collection of biological fluids on clinical filter papers provides a simple way to implement these protocols. This work explores the potential of solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry for the simultaneous and direct determination of Mo and Ti in urine, after its deposition onto clinical filter paper, giving rise to a dried urine spot. The approach used for depositing the sample was found crucial to develop a quantitative method, since the filter paper acts as a chromatographic support and produces a differential distribution of the target analytes. Furthermore, the high spreading of urine onto a filter paper results in a small amount of urine per surface unit, and thus, ultimately, in lack of sensitivity. In order to circumvent these problems, the use of an alternative approach based on the use of pre-cut 17 × 19 mm filter paper pieces onto which larger amounts of sample (500 μL) can be retained by single deposition was proposed and evaluated. In this way, an approximately 12-fold increase in sensitivity and a more homogeneous distribution of the target analytes were obtained, permitting the development of a quantification strategy based on the use of matrix-matched urine samples of known analyte concentrations, which were subjected to the same procedure as the samples. Accuracy of this method, which provides LODs of 1.5 μg L- 1 for Mo and 6.5 μg L- 1 for Ti, was demonstrated after analysis of urine reference materials. Overall, the performance of the method developed is promising, being likely suitable for determination of other analytes in dried urine spots.

  13. 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. PMID:24401409

  14. Noble metals as permanent chemical modifiers for the determination of mercury in environmental reference materials using solid sampling graphite furnace atomic absorption spectrometry and calibration against aqueous standards

    NASA Astrophysics Data System (ADS)

    da Silva, Alessandra Furtado; Welz, Bernhard; Curtius, Adilson J.

    2002-12-01

    Iridium, palladium, rhodium and ruthenium, thermally deposited on the platform, were investigated as permanent modifiers for the determination of mercury in ash, sludge, marine and river sediment reference materials, ground to a particle size of 50 μm, using solid sampling graphite furnace atomic absorption spectrometry. A total mass of 250 μg of each modifier was applied using 25 injections of 20 μl of modifier solution (500 mg l -1), and executing a temperature program for modifier conditioning after each injection. The performance of palladium was found to be most consistent, taking the characteristic mass as the major criterion, resulting in an excellent correlation between the measured integrated absorbance values and the certified mercury contents. Mercury was found to be lost in part from aqueous solutions during the drying stage in the presence of all the investigated permanent modifiers, as well as in the presence of the palladium and magnesium nitrates modifier added in solution. A loss-free determination of mercury in aqueous solutions could be reached only after the addition of potassium permanganate, which finally made possible the use of aqueous standards for the direct analysis of solid samples. A characteristic mass of 55-60 pg Hg was obtained for the solid samples, using Pd as a permanent modifier, and also in aqueous solutions after the addition of permanganate. The results obtained for mercury in ash, sludge and sediment reference materials, using direct solid sapling and calibration against aqueous standards, as well as the detection limit of 0.2 mg kg -1 were satisfactory for a routine procedure.

  15. 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. PMID:25996815

  16. L-tyrosine immobilized on multiwalled carbon nanotubes: a new substrate for thallium separation and speciation using stabilized temperature platform furnace-electrothermal atomic absorption spectrometry.

    PubMed

    Pacheco, Pablo H; Gil, Raúl A; Smichowski, Patricia; Polla, Griselda; Martinez, Luis D

    2009-12-10

    An approach for the separation and determination of inorganic thallium species is described. A new sorbent, L-tyrosine-carbon nanotubes (L-tyr-CNTs), was used and applied to the analysis of tap water samples. At pH 5.0, L-tyr was selective only towards Tl(III), while total thallium was determined directly by stabilized temperature platform furnace-electrothermal atomic absorption spectrometry (STPF-ETAAS). The Tl(III) specie, which was retained by L-tyrosine, was quantitatively eluted from the column with 10% of nitric acid. An on-line breakthrough curve was used to determine the column capacity, which resulted to be 9.00 micromol of Tl(III) g(-1) of L-tyr-CNTs with a molar ratio of 0.14 (moles of Tl bound to moles of L-tyr at pH 5). Transient peak areas revealed that Tl stripping from the column occurred instantaneously. Effects of sample flow rate, concentration and flow rate of the eluent, and interfering ions on the recovery of the analyte were systematically investigated. The detection limit for the determination of total thallium (3sigma) by STPF-ETAAS was 150 ng L(-1). The detection limit (3sigma) for Tl(III) employing the separation system was 3 ng L(-1), with an enrichment factor of 40. The precision of the method expressed as the relative standard deviation (RSD) resulted to be 3.4%. The proposed method was applied to the speciation and determination of inorganic thallium in tap water samples. The found concentrations were in the range of 0.88-0.91 microg L(-1) of Tl(III), and 3.69-3.91 microg L(-1) of total thallium. PMID:19932812

  17. Proteogenomic analysis of Mycobacterium tuberculosis by high resolution mass spectrometry.

    PubMed

    Kelkar, Dhanashree S; Kumar, Dhirendra; Kumar, Praveen; Balakrishnan, Lavanya; Muthusamy, Babylakshmi; Yadav, Amit Kumar; Shrivastava, Priyanka; Marimuthu, Arivusudar; Anand, Sridhar; Sundaram, Hema; Kingsbury, Reena; Harsha, H C; Nair, Bipin; Prasad, T S Keshava; Chauhan, Devendra Singh; Katoch, Kiran; Katoch, Vishwa Mohan; Kumar, Prahlad; Chaerkady, Raghothama; Ramachandran, Srinivasan; Dash, Debasis; Pandey, Akhilesh

    2011-12-01

    The genome sequencing of H37Rv strain of Mycobacterium tuberculosis was completed in 1998 followed by the whole genome sequencing of a clinical isolate, CDC1551 in 2002. Since then, the genomic sequences of a number of other strains have become available making it one of the better studied pathogenic bacterial species at the genomic level. However, annotation of its genome remains challenging because of high GC content and dissimilarity to other model prokaryotes. To this end, we carried out an in-depth proteogenomic analysis of the M. tuberculosis H37Rv strain using Fourier transform mass spectrometry with high resolution at both MS and tandem MS levels. In all, we identified 3176 proteins from Mycobacterium tuberculosis representing ~80% of its total predicted gene count. In addition to protein database search, we carried out a genome database search, which led to identification of ~250 novel peptides. Based on these novel genome search-specific peptides, we discovered 41 novel protein coding genes in the H37Rv genome. Using peptide evidence and alternative gene prediction tools, we also corrected 79 gene models. Finally, mass spectrometric data from N terminus-derived peptides confirmed 727 existing annotations for translational start sites while correcting those for 33 proteins. We report creation of a high confidence set of protein coding regions in Mycobacterium tuberculosis genome obtained by high resolution tandem mass-spectrometry at both precursor and fragment detection steps for the first time. This proteogenomic approach should be generally applicable to other organisms whose genomes have already been sequenced for obtaining a more accurate catalogue of protein-coding genes. PMID:21969609

  18. DETERMINATION OF TRACE AMOUNTS OF SELENIUM IN CORN, LETTUCE, POTATOES, SOYBEANS, AND WHEAT BY HYDRIDE GENERATION/CONDENSATION AND FLAME ATOMIC ABSORPTION SPECTROMETRY

    EPA Science Inventory

    Because of the nutritional and toxicological significance of low selenium concentrations in agricultural crops, a procedure utilizing wet digestion followed by hydride generation/condensation-flame atomic absorption was developed for the routine analysis of selenium in different ...

  19. 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.

  20. 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.

  1. Application of PERALS™ alpha spectrometry and gamma spectrometry for analysis and investigation of environmental spills at ISL uranium mining projects.

    PubMed

    Borysenko, A; Ostrowski, A; Bellifemine, D; Palmer, G; Haigh, P; Johnston, A

    2014-03-01

    Radiation protection and environmental monitoring in mining requires effective and reliable radionuclide analysis at all stages of the mine project-prior to mining, during operation and through to remediation and decommissioning. The approach presented in this paper was specially developed for the monitoring of radioactive waste resulting from spills during mining and mineral processing operations and uses a combination of high resolution gamma spectrometry, and PERALS™ alpha spectrometry to identify and reliably quantify the activity of the major members of the U-238 decay chain at activities down to 10 mBq g(-1) by direct radionuclide counting and by assessment of the activity of their decay products. This approach has reduced sample preparation and analysis time while providing effective analysis and quantification of naturally occurring radionuclides in environmental samples. It has been successfully applied to several in situ leach (ISL) mining-related projects involving investigations of process material spill impacts and also to routine environmental monitoring. PMID:24270399

  2. Quantifying uncertainty in the measurement of arsenic in suspended particulate matter by Atomic Absorption Spectrometry with hydride generator

    PubMed Central

    2011-01-01

    Arsenic is the toxic element, which creates several problems in human being specially when inhaled through air. So the accurate and precise measurement of arsenic in suspended particulate matter (SPM) is of prime importance as it gives information about the level of toxicity in the environment, and preventive measures could be taken in the effective areas. Quality assurance is equally important in the measurement of arsenic in SPM samples before making any decision. The quality and reliability of the data of such volatile elements depends upon the measurement of uncertainty of each step involved from sampling to analysis. The analytical results quantifying uncertainty gives a measure of the confidence level of the concerned laboratory. So the main objective of this study was to determine arsenic content in SPM samples with uncertainty budget and to find out various potential sources of uncertainty, which affects the results. Keeping these facts, we have selected seven diverse sites of Delhi (National Capital of India) for quantification of arsenic content in SPM samples with uncertainty budget following sampling by HVS to analysis by Atomic Absorption Spectrometer-Hydride Generator (AAS-HG). In the measurement of arsenic in SPM samples so many steps are involved from sampling to final result and we have considered various potential sources of uncertainties. The calculation of uncertainty is based on ISO/IEC17025: 2005 document and EURACHEM guideline. It has been found that the final results mostly depend on the uncertainty in measurement mainly due to repeatability, final volume prepared for analysis, weighing balance and sampling by HVS. After the analysis of data of seven diverse sites of Delhi, it has been concluded that during the period from 31st Jan. 2008 to 7th Feb. 2008 the arsenic concentration varies from 1.44 ± 0.25 to 5.58 ± 0.55 ng/m3 with 95% confidence level (k = 2). PMID:21466671

  3. Analysis of biogenic amines using corona discharge ion mobility spectrometry.

    PubMed

    Hashemian, Z; Mardihallaj, A; Khayamian, T

    2010-05-15

    A new method based on corona discharge ion mobility spectrometry (CD-IMS) was developed for the analysis of biogenic amines including spermidine, spermine, putrescine, and cadaverine. The ion mobility spectra of the compounds were obtained with and without n-Nonylamine used as the reagent gas. The high proton affinity of n-Nonylamine prevented ion formation from compounds with a proton affinity lower than that of n-Nonylamine and, therefore, enhanced its selectivity. It was also realized that the ion mobility spectrum of n-Nonylamine varied with its concentration. A sample injection port of a gas chromatograph was modified and used as the sample introduction system into the CD-IMS. The detection limits, dynamic ranges, and analytical parameters of the compounds with and without using the reagent gas were obtained. The detection limits and dynamic ranges of the compounds were about 2ng and 2 orders of magnitude, respectively. The wide dynamic range of CD-IMS originates from the high current of the corona discharge. The results revealed the high capability of the CD-IMS for the analysis of biogenic amines. PMID:20298897

  4. Proteogenomic Analysis of Mycobacterium smegmatis Using High Resolution Mass Spectrometry

    PubMed Central

    Potgieter, Matthys G.; Nakedi, Kehilwe C.; Ambler, Jon M.; Nel, Andrew J. M.; Garnett, Shaun; Soares, Nelson C.; Mulder, Nicola; Blackburn, Jonathan M.

    2016-01-01

    Biochemical evidence is vital for accurate genome annotation. The integration of experimental data collected at the proteome level using high resolution mass spectrometry allows for improvements in genome annotation by providing evidence for novel gene models, while validating or modifying others. Here, we report the results of a proteogenomic analysis of a reference strain of Mycobacterium smegmatis (mc2155), a fast growing model organism for the pathogenic Mycobacterium tuberculosis—the causative agent for Tuberculosis. By integrating high throughput LC/MS/MS proteomic data with genomic six frame translation and ab initio gene prediction databases, a total of 2887 ORFs were identified, including 2810 ORFs annotated to a Reference protein, and 63 ORFs not previously annotated to a Reference protein. Further, the translational start site (TSS) was validated for 558 Reference proteome gene models, while upstream translational evidence was identified for 81. In addition, N-terminus derived peptide identifications allowed for downstream TSS modification of a further 24 gene models. We validated the existence of six previously described interrupted coding sequences at the peptide level, and provide evidence for four novel frameshift positions. Analysis of peptide posterior error probability (PEP) scores indicates high-confidence novel peptide identifications and shows that the genome of M. smegmatis mc2155 is not yet fully annotated. Data are available via ProteomeXchange with identifier PXD003500. PMID:27092112

  5. Aerogel dust collection for in situ mass spectrometry analysis

    NASA Astrophysics Data System (ADS)

    Jones, S. M.; Anderson, M. S.; Davies, A. G.; Kirby, J. P.; Burchell, M. J.; Cole, M. J.

    2015-02-01

    The current technique for conducting in situ mass spectroscopic analysis of dust around extraterrestrial bodies is to have the dust impact a solid plate and analyze the atoms and molecular fragments resulting from the high speed impact. Due to the fact that the kinetic energy from the impact is converted primarily to thermal energy, much of the organic compounds present in the dust may be significantly altered or destroyed. To avoid this problem, aerogel could be used to capture the dust grains, largely intact, maintaining the integrity of the organic compounds in the interior of the dust grains. To demonstrate that organic molecules, present as minor components of silica particles, would survive hypervelocity capture in aerogel and can then be analyzed with mass spectrometry, several light gas gun impact tests and analyses were conducted. Fine particles containing polycyclic aromatic hydrocarbons (PAHs) were captured in aerogel at 5.5 km s-1. The flow of metastable helium from a Direct Analysis Real Time (DART) source was used to desorb and ionize the organics, which were then analyzed with a mass spectrometer. The PAHs were detected and identified by the DART-MS, demonstrating that this method could be used on future flight instruments.

  6. Total residue analysis of swabs by ion mobility spectrometry.

    PubMed

    Strege, Mark A

    2009-06-01

    Ion mobility spectrometry (IMS) is a technique attractive for use within the pharmaceutical industry for at-line determination of residues on swabs taken from the surfaces of manufacturing equipment for the purposes of cleaning validation or verification. In this study, the development of a novel IMS method to provide a measurement of total residue present on a swab is described. The technique is based upon quantitation of charged atmospheric gas reactant ion consumption (RIC) within the instrument as a direct measure of the mass of total ionizable residue. Coupled with the conventional analysis of the active pharmaceutical ingredient within a single 2 min analysis, RIC determination provided the benefit of a single measure representative of the presence of multiple residue components or unknown components. To account for differences in response between components of a model drug product (Cymbalta) and its associated cleaning agents, a strategy was proposed to determine a "worst case" total residue test result based on RIC. A limitation of the IMS method was its incompatibility with cleaners containing a high concentration of inorganic components. The methodology provided a range from 5-50 microg per 25 cm(2) surface area and acceptable analyte recovery (50-100%). PMID:19476393

  7. A versatile microcomputer interface and peripheral devices: An application in deuterium lamp background correction graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Gökmen, A.; Yalcin, S.

    1992-01-01

    A versatile interface card for Apple IIe computer and various peripheral devices are designed to control instruments which generates transient signals like in graphite furnace atomic spectrometer. The interface card consists of a multiplexed analog-to-digital converter, a digital-to-analog converter, and a timer/counter chip. The timer/counter chip with 16 built-in registers can be programmed in many modes which provides a time base for real-time measurements. A stepper motor runs under the control of timer/counter chip independent of computer. A light chopper connected to the stepper motor is controlled easily by computer. A dual high-voltage switch can modulate dc light sources under computer control. This system is applied to D2-lamp background correction graphite furnace atomic absorption spectrometer. The D2 lamp is chopped by a mechanical chopper driven by a stepper motor and a hollow cathode lamp is modulated electronically. The data acquisition program is written in machine language and synchronization between light sources and computer is provided by chopper position signal through the interrupts. A sampling rate of 16 during a signal period at 50-Hz chopping frequency is found to be the optimum value. A large number of data collected during atomization period is compressed in machine code. This saved storage space and analysis time.

  8. Environmental applications for the analysis of chlorinated dibenzo-p-dioxins and dibenzofurans using mass spectrometry/mass spectrometry

    SciTech Connect

    Reiner, E.J.; Schellenberg, D.H.; Taguchi, V.Y. )

    1991-01-01

    A mass spectrometry/mass spectrometry-multiple reaction monitoring (MS/MS-MRM) technique for the analysis of all tetra- through octachlorinated dibenzo-p-dioxins (Cl{sub x}DD, x = 4-8) and dibenzofurans (Cl{sub x}DF, x = 4-8) has been developed at the Ministry of the Environment (MOE) utilizing a triple quadrupole mass spectrometer. Optimization of instrumental parameters using the analyte of interest in a direct insertion probe (DIP) resulted in sensitivities approaching those obtainable by high-resolution mass spectrometric (HRMS) methods. All congeners of dioxins and furans were detected in the femtogram range. Results on selected samples indicated that for some matrices, fewer chemical interferences were observed by MS/MS than by HRMS. The technique used to optimize the instrument for chlorinated dibenzo-p-dioxins (CDDs) and chlorinated dibenzofurans (CDFs) analysis is adaptable to other analytes.

  9. Marine sediments monitoring studies for trace elements with the application of fast temperature programs and solid sampling high resolution continuum source atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Orani, Anna Maria; Han, Eunmi; Mandjukov, Petko; Vassileva, Emilia

    2015-01-01

    Analytical procedure for the determination of As, Cd, Cu, Ni, Co and Cr in marine sediment samples using high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS AAS) and direct solid sample analysis has been developed. The application of fast programs in combination with direct solid sampling allows to eliminate the drying and pretreatment steps, however makes impossible the use of liquid standards for calibration. Iridium treated platforms were applied throughout the present study. Calibration technique based on the use of solid certified reference materials (marine sediments) similar to the nature of the analyzed sample and statistics of regression analysis were applied to the real sediment samples. The instrumental parameters were optimized in order to obtain reproducible and interference free analytical signals. The ISO-17025 requirements and Eurachem guidelines were followed in the validation of the proposed analytical procedure. Accordingly, blanks, selectivity, calibration, linearity, working range, trueness, repeatability reproducibility, limits of detection and quantification and expanded uncertainty (k = 2) for all investigated elements were assessed. Two different approaches for the estimation of measurement uncertainty were applied and obtained results compared. The major contributors to the combined uncertainty of the analyte mass fraction were found to be the homogeneity of the samples and the microbalance precision. The influence of sample particle sizes on the total combined uncertainty was also evaluated. Traceability to SI system of units of the obtained by the proposed analytical procedure results was demonstrated. Additionally, validation of the methodology developed was effectuated by the comparison of the obtained results with independent method e.g. ICP-MS with external calibration. The use of solid sampling HR CS AAS for the determination of trace elements in marine sediment matrix gives significant advantages

  10. 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%. PMID:24964383

  11. Determination of lead in blood by chelation with ammonium pyrrolidine dithio-carbamate followed by tungsten-coil atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Salido, Arthur; Sanford, Caryn L.; Jones, Bradley T.

    1999-08-01

    An inexpensive, bench-top blood Pb analyzer has been developed. The system is based on tungsten-coil atomic absorption spectrometry. Pb atomization occurs on W-coils extracted from commercially available slide projector bulbs. The system has minimal power requirements: 120 ACV and 15 A. A small, computer-controlled CCD spectrometer is used as the detector. A Pb hollow cathode lamp is used as the source. Blood Pb is chelated with ammonium pyrrolidine dithio-carbamate and extracted into methyl iso-butyl ketone (4-methyl 2-pentanone). Twenty-microliter volumes of the organic phase are deposited on the W-coil, dried at 1.4 A, charred at 2.3 A and atomized at 6.0 A. Graphite furnace atomic absorption spectrometry is used as a comparison for W-coil results. Levels 1-4 of a NIST standard reference material 955b ‘lead in bovine blood’ are used to test accuracy and precision. The analytical figures of merit for the system are: 12-pg instrument detection limit, 24-pg blood detection limit and a characteristic mass of 28 pg.

  12. Advances in protein complex analysis using mass spectrometry.

    PubMed

    Gingras, Anne-Claude; Aebersold, Ruedi; Raught, Brian

    2005-02-15

    Proteins often function as components of larger complexes to perform a specific function, and formation of these complexes may be regulated. For example, intracellular signalling events often require transient and/or regulated protein-protein interactions for propagation, and protein binding to a specific DNA sequence, RNA molecule or metabolite is often regulated to modulate a particular cellular function. Thus, characterizing protein complexes can offer important insights into protein function. This review describes recent important advances in mass spectrometry (MS)-based techniques for the analysis of protein complexes. Following brief descriptions of how proteins are identified using MS, and general protein complex purification approaches, we address two of the most important issues in these types of studies: specificity and background protein contaminants. Two basic strategies for increasing specificity and decreasing background are presented: whereas (1) tandem affinity purification (TAP) of tagged proteins of interest can dramatically improve the signal-to-noise ratio via the generation of cleaner samples, (2) stable isotopic labelling of proteins may be used to discriminate between contaminants and bona fide binding partners using quantitative MS techniques. Examples, as well as advantages and disadvantages of each approach, are presented. PMID:15611014

  13. Lipidomic Analysis of Glioblastoma Multiforme Using Mass Spectrometry

    PubMed Central

    Ha, Soo Jung; Showalter, Gordon; Cai, Shanbao; Wang, Haiyan; Liu, Wei Michael; Cohen-Gadol, Aaron A.; Sarkaria, Jann N.; Rickus, Jenna; Springer, John; Adamec, Jiri; Pollok, Karen E.; Clase, Kari L.

    2016-01-01

    Glioblastoma multiforme (GBM) is the most common and malignant form of primary brain tumors. It is highly invasive and current treatment options have not improved the survival rate over the past twenty years. Novel approaches and technologies from systems biology have the potential to identify biomarkers that could serve as new therapeutic targets for GBM. This study employed lipid profiling technology to investigate lipid biomarkers in ectopic and orthotopic human GBM xenograft models. Primary patient cell lines, GBM10 and GBM43, were injected into the flank and the right cerebral hemisphere of NOD/SCID mice. Tumors were harvested from the brain and flank and proteins, metabolites, and lipids extracted from each sample. Reverse phase based high performance liquid chromatography coupled with Fourier transform ion cyclotron resonance mass spectrometry (LC-FTMS) was used to analyze the lipid profiles of tumor samples. Statistical and clustering analyses were performed to detect differences. Over 500 lipids were identified in each tumor model and lipids with the greatest fold effect in the comparison of ectopic versus orthotopic tumor models fell predominantly into four main classes of lipids: glycosphingolipids, glycerophoshpoethanolamines, triradylglycerols, and glycerophosphoserines. Lipidomic analysis revealed differences in glycosphingolipid and triglyceride profiles when the same tumor was propagated in the flank versus the brain. These results underscore the importance of the surrounding physiological environment on tumor development and are consistent with the hypothesis that specific classes of lipids are critical for GBM tumor growth in different anatomical sites. PMID:17929901

  14. Towards metals analysis using corona discharge ionization ion mobility spectrometry.

    PubMed

    Jafari, Mohammad T; Saraji, Mohammad; Sherafatmand, Hossein

    2016-02-25

    For the first time, the capability of corona discharge ionization ion mobility spectrometry (CD-IMS) in the determination of metal complex was evaluated. The extreme simplicity of dispersive liquid-liquid microextraction (DLLME) coupled to the high sensitivity of CD-IMS measurement could make this combination really useful for simple, rapid, and sensitive determination of metals in different samples. In this regard, mercury, as a model metal, was complexed with diethyldithiocarbamate (DEDTC), and then extracted into the carbon tetrachloride using DLLME. Some parameters affecting the extraction efficiency, including the type and volume of the extraction solvent, the type and volume of the disperser solvent, the concentration of the chelating agent, salt addition and, pH were exhaustively investigated. Under the optimized condition, the enrichment factor was obtained to be 142. The linear range of 0.035-10.0 μg mL(-1) with r(2) = 0.997 and the detection limit of 0.010 μg mL(-1) were obtained. The relative standard deviation values were calculated to be lower than 4% and 8% for intra-day and inter-day, respectively. Finally, the developed method was successfully applied for the extraction and determination of mercury in various real samples. The satisfactory results revealed the capability of the proposed method in trace analysis without tedious derivatization or hydride generation. PMID:26851088

  15. Subcellular analysis by laser ablation electrospray ionization mass spectrometry

    DOEpatents

    Vertes, Akos; Stolee, Jessica A; Shrestha, Bindesh

    2014-12-02

    In various embodiments, a method of laser ablation electrospray ionization mass spectrometry (LAESI-MS) may generally comprise micro-dissecting a cell comprising at least one of a cell wall and a cell membrane to expose at least one subcellular component therein, ablating the at least one subcellular component by an infrared laser pulse to form an ablation plume, intercepting the ablation plume by an electrospray plume to form ions, and detecting the ions by mass spectrometry.

  16. Analysis of Mass Spectrometry Data for Nucleolar Proteomics Experiments.

    PubMed

    Nicolas, Armel; Bensaddek, Dalila; Lamond, Angus I

    2016-01-01

    With recent advances in experiment design, sample preparation, separation and instruments, mass spectrometry (MS)-based quantitative proteomics is becoming increasingly more popular. This has the potential to usher a new revolution in biology, in which the protein complement of cell populations can be described not only with increasing coverage, but also in all of its dimensions with unprecedented precision. Indeed, while earlier proteomics studies aimed solely at identifying as many as possible of the proteins present in the sample, newer, so-called Next Generation Proteomics studies add to this the aim of determining and quantifying the protein variants present in the sample, their mutual associations within complexes, their posttranslational modifications, their variation across the cell-cycle or in response to stimuli or perturbations, and their subcellular distribution. This has the potential to make MS proteomics much more useful for researchers, but will also mean that researchers with no background in MS will increasingly be confronted with the less-than trivial challenges of preparing samples for MS analysis, then processing and interpreting the results. In Chapter 20 , we described a workflow for isolating the protein contents of a specific SILAC-labeled organelle sample (the nucleolus) and processing it into peptides suitable for bottom-up MS analysis. Here, we complete this workflow by describing how to use the freely available MaxQuant software to convert the spectra stored in the Raw files into peptide- and protein-level information. We also briefly describe how to visualize the data using the free R scripting language. PMID:27576726

  17. System Analysis on Absorption Chiller Utilizing Intermediate Wasted Heat

    NASA Astrophysics Data System (ADS)

    Yamada, Miki; Suzuki, Hiroshi; Usui, Hiromoto

    A system analysis has been performed for the multi-effect absorption chiller (MEAC) applied as a bottoming system of 30kW class hybrid system including micro gas turbine (MGT) and solid oxide fuel cell (SOFC) hybrid system. In this paper, an intermediate wasted heat utilization (IWHU) system is suggested for lifting up the energy efficiency of the whole system and coefficient of performance (COP) of MEAC. From the results, the suggested IWHU system was found to show the very high energy efficiency compared with a terminal wasted heat utilization (TWHU) system that uses only the heat exhausted from the terminal of MGT/SOFC system. When TWHU system is applied for MEAC, the utilized heat from the MGT/SOFC system is found to remain low because the temperature difference between the high temperature generator and the wasted heat becomes small. Then, the energy efficiency does not become high in spite of high COP of MEAC. On the other hand, the IWHU system could increase the utilized heat for MEAC as performs effectively. The exergy efficiency of IWHU system is also revealed to be higher than that of a direct gas burning system of MEAC, because the wasted heat is effectively utilized in the IWHU system.

  18. Analysis of paralytic shellfish toxins using high-field asymmetric waveform ion mobility spectrometry with liquid chromatography-mass spectrometry.

    PubMed

    Beach, Daniel G; Melanson, Jeremy E; Purves, Randy W

    2015-03-01

    The analysis of paralytic shellfish toxins (PSTs) by liquid chromatography-mass spectrometry remains a challenge because of their high polarity, large number of analogues and the complex matrix in which they occur. Here we investigate the potential utility of high-field asymmetric waveform ion mobility spectrometry (FAIMS) as a gas-phase ion separation tool for analysis of PSTs by mass spectrometry. We investigate the separation of PSTs using FAIMS with two divergent goals: using FAIMS as a primary separation tool for rapid screening by electrospray ionization (ESI)-FAIMS-MS or combined with LC in a multidimensional LC-ESI-FAIMS-MS separation. First, a survey of the parameters that affect the sensitivity and selectivity of PST analysis by FAIMS was carried out using ESI-FAIMS-MS. In particular, the use of acetonitrile as a gas additive in the carrier gas flow offered good separation of all PST epimeric pairs. A second set of FAIMS conditions was also identified, which focussed PSTs to a relatively narrow CV range allowing development of an LC-ESI-FAIMS-MS method for analysis of PST toxins in complex mussel tissue extracts. The quantitative capabilities of this method were evaluated by analysing a PST containing mussel tissue matrix material. Results compared favourably with analysis by an established LC-post-column oxidation-fluorescence method with recoveries ranging from 70 to 106%, although sensitivity was somewhat reduced. The current work represents the first successful separation of PST isomers using ion mobility and shows the promise of FAIMS as a tool for analysis of algal biotoxins in complex samples and outlines some critical requirements for its future improvement. PMID:25619987

  19. VACUUM DISTILLATION COUPLED WITH GAS CHROMATOGRAPHY/MASS SPECTROMETRY FOR THE ANALYSIS OF ENVIRONMENTAL SAMPLES

    EPA Science Inventory

    A procedure is presented that uses a vacuum distillation/gas chromatography/mass spectrometry system for analysis of problematic matrices of volatile organic compounds. The procedure compensates for matrix effects and provides both analytical results and confidence intervals from...

  20. AN EPA MANUAL FOR ORGANICS ANALYSIS USING GAS CHROMATOGRAPHY-MASS SPECTROMETRY

    EPA Science Inventory

    This procedural manual defines the areas of applicability of gas chromatography-mass spectrometry in environmental analysis. The manual includes sample preparation methods specifically adapted to this measurement technique, data processing and interpretation methods, quality cont...

  1. Absorption-Mode Fourier Transform Mass Spectrometry: The Effects of Apodization and Phasing on Modified Protein Spectra

    NASA Astrophysics Data System (ADS)

    Qi, Yulin; Li, Huilin; Wills, Rebecca H.; Perez-Hurtado, Pilar; Yu, Xiang; Kilgour, David P. A.; Barrow, Mark P.; Lin, Cheng; O'Connor, Peter B.

    2013-06-01

    The method of phasing broadband Fourier transform ion cyclotron resonance (FT-ICR) spectra allows plotting the spectra in the absorption-mode; this new approach significantly improves the quality of the data at no extra cost. Herein, an internal calibration method for calculating the phase function has been developed and successfully applied to the top-down spectra of modified proteins, where the peak intensities vary by 100×. The result shows that the use of absorption-mode spectra allows more peaks to be discerned within the recorded data, and this can reveal much greater information about the protein and modifications under investigation. In addition, noise and harmonic peaks can be assigned immediately in the absorption-mode.

  2. Determination of total sulfur concentrations in different types of vinegars using high resolution flame molecular absorption spectrometry.

    PubMed

    Ozbek, Nil; Akman, Suleyman

    2016-12-15

    Total sulfur concentrations in vinegars were determined using molecular absorption of carbon monosulfide (CS) determined with a high-resolution continuum source flame atomic absorption spectrometer. The molecular absorption of CS was measured at 258.056nm in an air-acetylene flame. Due to non-spectral interference, as well as the different sensitivities to some sulfur compounds, all sulfur species were oxidized to sulfate using a HNO3 and H2O2 mixture and the analyte addition technique was applied for quantification. The limit of detection (LOD) and limit of quantification (LOQ) were 11.6 and 38.6mgL(-1), respectively. The concentrations of sulfur in various vinegars ranged from ⩽LOD to 163.6mgL(-1). PMID:27451213

  3. Absorption-Mode Fourier Transform Mass Spectrometry: the Effects of Apodization and Phasing on Modified Protein Spectra

    PubMed Central

    Qi, Yulin; Li, Huilin; Wills, Rebecca H.; Perez-Hurtado, Pilar; Yu, Xiang; Kilgour, David. P. A.; Barrow, Mark P.; Lin, Cheng; O’Connor, Peter B.

    2014-01-01

    The method of phasing broadband FT-ICR spectra allows plotting the spectra in the absorption-mode; this new approach significantly improves the quality of the data at no extra cost. Herein, an internal calibration method for calculating the phase function has been developed, and successfully applied to the top-down spectra of modified proteins, where the peak intensities vary by >100×. The result shows that the use of absorption-mode spectra allows more peaks to be discerned within the recorded data, and this can reveal much greater information about the protein and modifications under investigation. In addition, noise and harmonic peaks can be assigned immediately in the absorption-mode. PMID:23568027

  4. Analysis of explosives using corona discharge ionization combined with ion mobility spectrometry-mass spectrometry.

    PubMed

    Lee, Jihyeon; Park, Sehwan; Cho, Soo Gyeong; Goh, Eun Mee; Lee, Sungman; Koh, Sung-Suk; Kim, Jeongkwon

    2014-03-01

    Corona discharge ionization combined with ion mobility spectrometry-mass spectrometry (IMS-MS) was utilized to investigate five common explosives: cyclonite (RDX), trinitrotoluene (TNT), pentaerythritol tetranitrate (PETN), cyclotetramethylenetetranitramine (HMX), and 2,4-dinitrotoluene (DNT). The MS scan and the selected ion IMS analyses confirmed the identities of the existing ion species and their drift times. The ions observed were RDX·NO3(-), TNT(-), PETN·NO3(-), HMX·NO3(-), and DNT(-), with average drift times of 6.93 ms, 10.20 ms, 9.15 ms, 12.24 ms, 11.30 ms, and 8.89 ms, respectively. The reduced ion mobility values, determined from a standard curve calculated by linear regression of (normalized drift times)(-1) versus literature K0 values, were 2.09, 1.38, 1.55, 1.15, 1.25, and 1.60 cm(2) V(-1) s(-1), respectively. The detection limits were found to be 0.1 ng for RDX, 10 ng for TNT, 0.5 ng for PETN, 5.0 ng for HMX, and 10 ng for DNT. Simplified chromatograms were observed when nitrogen, as opposed to air, was used as the drift gas, but the detection limits were approximately 10 times worse (i.e., less sensitivity of detection). PMID:24468343

  5. Optical absorption analysis and optimization of gold nanoshells.

    PubMed

    Tuersun, Paerhatijiang; Han, Xiang'e

    2013-02-20

    Gold nanoshells, consisting of a nanoscale dielectric core coated with an ultrathin gold shell, have wide biomedical applications due to their strong optical absorption properties. Gold nanoshells with high absorption efficiencies can help to improve these applications. We investigate the effects of the core material, surrounding medium, core radius, and shell thickness on the absorption spectra of gold nanoshells by using the light-scattering theory of a coated sphere. Our results show that the position and intensity of the absorption peak can be tuned over a wide range by manipulating the above-mentioned parameters. We also obtain the optimal absorption efficiencies and structures of hollow gold nanoshells and gold-coated SiO(2) nanoshells embedded in water at wavelengths of 800, 820, and 1064 nm. The results show that hollow gold nanoshells possess the maximum absorption efficiency (5.42) at a wavelength of 800 nm; the corresponding shell thickness and core radius are 4.8 and 38.9 nm, respectively. They can be used as the ideal photothermal conversation particles for biomedical applications. PMID:23435006

  6. Ion Mobility Mass Spectrometry Direct Isotope Abundance Analysis

    SciTech Connect

    Manuel J. Manard, Stephan Weeks, Kevin Kyle

    2010-05-27

    The nuclear forensics community is currently engaged in the analysis of illicit nuclear or radioactive material for the purposes of non-proliferations and attribution. One technique commonly employed for gathering nuclear forensics information is isotope analysis. At present, the state-of-the-art methodology for obtaining isotopic distributions is thermal ionization mass spectrometry (TIMS). Although TIMS is highly accurate at determining isotope distributions, the technique requires an elementally pure sample to perform the measurement. The required radiochemical separations give rise to sample preparation times that can be in excess of one to two weeks. Clearly, the nuclear forensics community is in need of instrumentation and methods that can expedite their decision making process in the event of a radiological release or nuclear detonation. Accordingly, we are developing instrumentation that couples a high resolution IM drift cell to the front end of a MS. The IM cell provides a means of separating ions based upon their collision cross-section and mass-to-charge ratio (m/z). Two analytes with the same m/z, but with different collision cross-sections (shapes) would exit the cell at different times, essentially enabling the cell to function in a similar manner to a gas chromatography (GC) column. Thus, molecular and atomic isobaric interferences can be effectively removed from the ion beam. The mobility selected chemical species could then be introduced to a MS for high-resolution mass analysis to generate isotopic distributions of the target analytes. The outcome would be an IM/MS system capable of accurately measuring isotopic distributions while concurrently eliminating isobaric interferences and laboratory radiochemical sample preparation. The overall objective of this project is developing instrumentation and methods to produce near real-time isotope distributions with a modular mass spectrometric system that performs the required gas-phase chemistry and

  7. Peculiarities of data interpretation upon direct tissue analysis by Fourier transform ion cyclotron resonance mass spectrometry.

    PubMed

    Chagovets, Vtaliy; Kononikhin, Aleksey; Starodubtseva, Nataliia; Kostyukevich, Yury; Popov, Igor; Frankevich, Vladimir; Nikolaev, Eugene

    2016-01-01

    The importance of high-resolution mass spectrometry for the correct data interpretation of a direct tissue analysis is demonstrated with an example of its clinical application for an endometriosis study. Multivariate analysis of the data discovers lipid species differentially expressed in different tissues under investigation. High-resolution mass spectrometry allows unambiguous separation of peaks with close masses that correspond to proton and sodium adducts of phosphatidylcholines and to phosphatidylcholines differing in double bond number. PMID:27553733

  8. Development of a simple method for the determination of nitrite and nitrate in groundwater by high-resolution continuum source electrothermal molecular absorption spectrometry.

    PubMed

    Brandao, Geovani C; Matos, Geraldo D; Pereira, Raimundo N; Ferreira, Sergio L C

    2014-01-01

    In this work, it was developed a method for the determination of nitrite and nitrate in groundwater by high-resolution continuum source electrothermal molecular absorption spectrometry of NO produced by thermal decomposition of nitrate in a graphite furnace. The NO line at 215.360 nm was used for all analytical measurements and the signal obtained by integrated absorbance of three pixels. A volume of 20 μL of standard solution or groundwater sample was injected into graphite furnace and 5 μL of a 1% (m/v) Ca solution was co-injected as chemical modifier. The pyrolisis and vaporization temperatures established were of 150 and 1300°C, respectively. Under these conditions, it was observed a difference of thermal stability among the two nitrogen species in the presence of hydrochloric acid co-injected. While that the nitrite signal was totally suppressed, nitrate signal remained nearly stable. This way, nitrogen can be quantified only as nitrate. The addition of hydrogen peroxide provided the oxidation of nitrite to nitrate, which allowed the total quantification of the species and nitrite obtained by difference. A volume of 5 μL of 0.3% (v/v) hydrochloric acid was co-injected for the elimination of nitrite, whereas that hydrogen peroxide in the concentration of 0.75% (v/v) was added to samples or standards for the oxidation of nitrite to nitrate. Analytical curve was established using standard solution of nitrate. The method described has limits of detection and quantification of 0.10 and 0.33 μg mL(-1) of nitrogen, respectively. The precision, estimated as relative standard deviation (RSD), was of 7.5 and 3.8% (n=10) for groundwater samples containing nitrate-N concentrations of 1.9 and 15.2 μg mL(-1), respectively. The proposed method was applied to the analysis of 10 groundwater samples and the results were compared with those obtained by ion chromatography method. In all samples analyzed, the concentration of nitrite-N was always below of the limit of

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

    PubMed

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

    2005-08-01

    The use of the chemically modified silica gel N-(3-propyl)-O-phenylenediamine (SiG-NPPDA) adsorbent, for the preconcentration and separation of trace heavy metals, was described. SiG-NPPDA sorbs quantitatively (90-100% recovery) trace amounts of nine heavy metals, viz., Cd(II), Zn(II), Fe(III), Cu(II), Pb(II), Mn(II), Cr(III), Co(II) and Ni(II) at pH 7-8. The sorption capacity varies from 350 to 450 micromol g(-1). Desorption was found to be quantitative with 1-2 M HNO3 or 0.05 M Na2EDTA. The distribution coefficient, Kd and the percentage concentration of the investigated metal ions on the adsorbent at equilibrium, C(M,eqm)% (Recovery, R%), were studied as a function of experimental parameters. The logarithmic values of the distribution coefficient, log Kd, ranges between 4.0 and 6.4. Some foreign ions caused little interference in the preconcentration and determination of the investigated nine metals by flame atomic absorption spectrometry (AAS). The adsorbent and its formed metal chelates were characterized by IR (absorbance and/or reflectance), potentiometric titrations and thermogravimetric analysis (TGA and DTG). The mode of chelation between the SiG-NPPDA adsorbent and the investigated metal ions is proposed to be due to the reaction of the investigated metal ions with the two nitrogen atoms of the SiG-NPPDA adsorbent. The present adsorbent coupled with flame AAS has been used to enrich and determine the nine metal ions in natural aqueous systems and in certified reference materials (RSD < or = 5%). The copper, iron, manganese and zinc present in some pharmaceutical vitamin samples were also preconcentrated on SiG-NPPDA adsorbent and determined by flame AAS (RSD < or = 4.2%). Nanogram concentrations (0.07-0.14 ng ml(-1)) of Cd(II), Zn(II), Fe(III), Pb(II), Cr(III), Mn(II), Cu(II), Co(II) and Ni(II) can be determined reliably with a preconcentration factor of 100. PMID:16122162

  10. Direct analysis of samples by mass spectrometry: From elements to bio-molecules using laser ablation inductively couple plasma mass spectrometry and laser desorption/ionization mass spectrometry

    SciTech Connect

    Perdian, David C.

    2009-01-01

    Mass spectrometric methods that are able to analyze solid samples or biological materials with little or no sample preparation are invaluable to science as well as society. Fundamental research that has discovered experimental and instrumental parameters that inhibit fractionation effects that occur during the quantification of elemental species in solid samples by laser ablation inductively coupled plasma mass spectrometry is described. Research that determines the effectiveness of novel laser desorption/ionization mass spectrometric methods for the molecular analysis of biological tissues at atmospheric pressure and at high spatial resolution is also described. A spatial resolution is achieved that is able to analyze samples at the single cell level.

  11. Mass Spectrometry Analysis of Pseudomonas aeruginosa Treated with Azithromycin

    NASA Astrophysics Data System (ADS)

    Phelan, Vanessa V.; Fang, Jinshu; Dorrestein, Pieter C.

    2015-06-01

    In microbiology, changes in specialized metabolite production (cell-to-cell signaling metabolites, virulence factors, and natural products) are measured using phenotypic assays. However, advances in mass spectrometry-based techniques including imaging mass spectrometry (IMS) now allow researchers to directly visualize the production of specialized metabolites from microbial colony biofilms. In this study, a combination of IMS and liquid chromatography-tandem mass spectrometry (LC-MS/MS) was used to visualize the effect of the macrolide antibiotic azithromycin (AZM) on colony biofilms of Pseudomonas aeruginosa. Although previous research suggested that AZM may inhibit cell-to-cell signaling of P. aeruginosa and thereby reduce pathogenicity, we observed no clear decrease in specialized metabolite production.

  12. Mass Spectrometry Analysis of Pseudomonas aeruginosa Treated With Azithromycin

    PubMed Central

    Phelan, Vanessa V.; Fang, Jinshu; Dorrestein, Pieter C.

    2015-01-01

    In microbiology, changes in specialized metabolite production (cell-to-cell signaling metabolites, virulence factors and natural products) are measured using phenotypic assays. However, advances in mass spectrometry based techniques including imaging mass spectrometry (IMS) now allow researchers to directly visualize the production of specialized metabolites from microbial colony biofilms. In this study, a combination of IMS and liquid chromatography-tandem mass spectrometry (LC-MS/MS) was used to visualize the effect of the macrolide antibiotic azithromycin (AZM) on colony biofilms of Pseudomonas aeruginosa. While previous research suggested that AZM may inhibit cell-to-cell signaling of P. aeruginosa and thereby reducing pathogenicity, we observed no clear decrease in specialized metabolite production. PMID:25801585

  13. Inductively coupled plasma mass spectrometry applied to isotopic analysis of iron in human fecal matter

    SciTech Connect

    Ting, B.T.G.; Janghorbani, M.

    1986-06-01

    Inductively coupled plasma mass spectrometry combined with stable isotope dilution is applied to accurate isotopic analysis of human fecal matter for /sup 54/Fe and /sup 58/Fe. Argon plasma generated interferences are of minor concern. The interference from /sup 54/Cr can be corrected instrumentally, whereas /sup 58/Ni must be removed chemically. The ratio of the stable isotopes of interest can be measured routinely with a relative standard deviation of about 1%. The overall accuracy of the method for quantitative isotopic analyses is evaluated in Standard Reference Material (SRM) 1577a (Bovine Liver), fecal homogenate subsamples, and synthetic solutions of iron. For SRM 1577a, the respective comparisons are (..mu..g/g) 192.2 +/- 2.2 (present method) vs. 194 +/- 20 (certified value). For the fecal matrix, the present method yields (..mu..g/mL) 15.14 +/- 0.36 vs. 15.82 +/- 0.48 based on atomic absorption spectrophotometry. For an iron solution (250 ppm), replicate analyses yield the value of 245.4 +/- 1.5 ppm.

  14. Microbeam titanium isotopic analysis by resonance ionization mass spectrometry

    SciTech Connect

    Spiegel, D.R.; Davis, A.M.; Clayton, R.N. . Enrico Fermi Inst.); Pellin, M.J.; Calaway, W.F.; Burnett, J.W.; Coon, S.R.; Young, C.E.; Gruen, D.M. )

    1991-01-01

    The importance of isotopic anomalies in refractory inclusions in meteorites is well established. Measurements of the anomalies using conventional mass spectrometry are often rendered difficult, however, by isobarically interfering isotopes: for example, {sup 48}Ti and {sup 48}Ca. Resonance ionization mass spectrometry (RIMS) can substantially reduce isobaric interferences in a number of systems. We have employed RIMS for the in situ detection of Ti atoms sputtered from pure Ti metal and from several terrestrial oxides containing both Ti and Ca. Tunable lasers were employed to resonantly ionize neutral Ti atoms. We have chosen Ti specifically because of the importance of Ti isotopic anomalies in cosmochemistry.

  15. A fast and accurate microwave-assisted digestion method for arsenic determination in complex mining residues by flame atomic absorption spectrometry.

    PubMed

    Pantuzzo, Fernando L; Silva, Julio César J; Ciminelli, Virginia S T

    2009-09-15

    A fast and accurate microwave-assisted digestion method for arsenic determination by flame atomic absorption spectrometry (FAAS) in typical, complex residues from gold mining is presented. Three digestion methods were evaluated: an open vessel digestion using a mixture of HCl:HNO(3):HF acids (Method A) and two microwave digestion methods using a mixture of HCl:H(2)O(2):HNO(3) in high (Method B) and medium-pressure (Method C) vessels. The matrix effect was also investigated. Arsenic concentration from external and standard addition calibration curves (at a 95% confidence level) were statistically equal (p-value=0.122) using microwave digestion in high-pressure vessel. The results from the open vessel digestion were statistically different (p-value=0.007) whereas in the microwave digestion in medium-pressure vessel (Method C) the dissolution of the samples was incomplete. PMID:19345010

  16. Dithizone chloroform single drop microextraction system combined with electrothermal atomic absorption spectrometry using Ir as permanent modifier for the determination of Cd in water and biological samples

    NASA Astrophysics Data System (ADS)

    Fan, Zhefeng; Zhou, Wei

    2006-07-01

    A simple and sensitive method using dithizone-chloroform single drop microextraction has been developed for separation and preconcentration of trace Cd prior to its determination by electrothermal atomic absorption spectrometry with Ir as permanent modifier. Parameters, such as pyrolysis and atomization temperature, solvent type, pH, dithizone concentration, extraction time, organic drop volume, stirring rate and sample volume were investigated. Under the optimized conditions, a detection limit (3 σ) of 0.7 ng/l and enrichment factor of 65 were achieved. The relative standard deviation was 7.4% ( c = 0.2 μg/l, n = 5). The developed method has been applied to the determination of trace Cd in water samples and biological reference materials with satisfactory results.

  17. Evaluation of cadmium in greenhouse soils and agricultural products of Jiroft (Iran) using microwave digestion prior to atomic absorption spectrometry determination.

    PubMed

    Afzali, Daryoush; Fathirad, Fariba; Afzali, Zahra; Majdzadeh-Kermani, Seyed Mohammad Javad

    2015-03-01

    This study determines total levels of potentially toxic trace element, Cd (II) in Jiroft (Kerman, Iran) greenhouse soil and agricultural products that are grown in these greenhouses (tomatoes and cucumbers), and the comparison with soil outside of greenhouse using microwave digestion prior to flame atomic absorption spectrometry determination. The results show that the cadmium concentration in greenhouse soil is 0.9-1.9 mg kg(-1) and out of greenhouse is 0.4-1.0 mg kg(-1). Also, cadmium concentration range in tomatoes and cucumbers is about 0.07-0.40 mg kg(-1). The obtained results show that the concentration of this metal in greenhouse soil is higher than outside soil samples and is below the safe limit. PMID:25697307

  18. 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. PMID:19138082

  19. 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.

  20. 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.

  1. X-ray absorption fine structure combined with fluorescence spectrometry for monitoring trace amounts of lead adsorption in the environmental conditions.

    PubMed

    Izumi, Yasuo; Kiyotaki, Fumitaka; Minato, Taketoshi; Seida, Yoshimi

    2002-08-01

    The local structure of trace amounts of lead in an adsorbent matrix that contains a high concentration of iron and magnesium (Mg6Fe2(OH)16(CO3) x 3H2O) was successfully monitored by means of X-ray absorption fine structure spectroscopy combined with fluorescence spectrometry. A eutectic mixture of PbCO3 and Pb(OH)2 coagulated when Pb2+ was adsorbed from a 1.0 ppm aqueous solution, and in contrast, the major species was ion-exchanged Pb2+ in the case of adsorption from a 100 ppb aqueous solution. The difference was ascribed to the balance between the precipitation equilibrium for coagulation and the rate of the ion exchange reaction with surface hydroxyl groups. PMID:12175171

  2. Early prediction of wheat quality: analysis during grain development using mass spectrometry and multivariate data analysis.

    PubMed

    Ghirardo, Andrea; Sørensen, Helle Aagaard; Petersen, Marianne; Jacobsen, Susanne; Søndergaard, Ib

    2005-01-01

    Matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry and multivariate data analysis have been used for the determination of wheat quality at different stages of grain development. Wheat varieties with one of two different end-use qualities (i.e. suitable or not suitable for bread-making purposes) were investigated. The samples were collected from grains from 15 until 45 days post-anthesis (dpa). Gluten proteins from wheat grains were extracted and subsequently analysed by mass spectrometry. Discrimination partial least-squares regression and soft independent modelling of class analogy were used to determine the quality of new and unknown wheat samples. With these methods, we were able to predict correctly the end-use qualities at every stage investigated. This new fast technique, based on the rapidity of mass spectrometry combined with the objectivity of multivariate data analysis, offers a method that can replace the traditional rather time-consuming ones such as gel electrophoresis. This study focused on the determination of wheat quality at 15 dpa, when the grain is due for harvest 1 month later. PMID:15655793

  3. Analysis of proteins using DIGE and MALDI mass spectrometry

    EPA Science Inventory

    In this work the sensitivity of the quantitative proteomics approach 2D-DIGE/MS (twoDimensional Difference Gel Electrophoresis / Mass Spectrometry) was tested by detecting decreasing amounts of a specific protein at the low picomole and sub-picomole range. Sensitivity of the 2D-D...

  4. Mass spectrometry and hyphenated instruments in food analysis

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Mass spectrometry (MS) has come a long way since the record of the first mass spectra of a simple low molecular weight substance by J.J. Thomson in 1912. Especially over the past decades, MS has been the subject of many developments. Particularly, the hyphenation of MS to gas chromatography (GC) a...

  5. Analysis of intact bacteria using rapid evaporative ionisation mass spectrometry.

    PubMed

    Strittmatter, Nicole; Jones, Emrys A; Veselkov, Kirill A; Rebec, Monica; Bundy, Jacob G; Takats, Zoltan

    2013-07-14

    An identification system for microorganisms based on recently developed rapid evaporative ionisation mass spectrometry (REIMS) is presented. Nine bacterial species cultured on various growth media were correctly identified to family-, genus-, and species-level based on their different mass spectral fingerprints using a cross-validated maximum margin criterion model. PMID:23736664

  6. Investigation of spectral interferences in the determination of lead in fertilizers and limestone samples using high-resolution continuum source graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Borges, Aline R.; Becker, Emilene M.; François, Luciane L.; de Jesus, Alexandre; Vale, Maria Goreti R.; Welz, Bernhard; Dessuy, Morgana B.; de Andrade, Jailson B.

    2014-11-01

    In the present work, spectral interferences on the determination of lead in fertilizer and limestone samples were investigated using high-resolution continuum source graphite furnace atomic absorption spectrometry at the main analytical lines: 217.001 and 283.306 nm. For these investigations, samples were introduced into the furnace as slurry together with a mixture of Pd and Mg as chemical modifier. Spectral interferences were observed for some samples at both analytical lines. In order to verify whether a wet digestion procedure would avoid these interferences, a reference method for wet digestion of fertilizers was employed as an alternative sample preparation procedure. However, the same interferences were also observed in the digested samples. In order to identify and eliminate the fine-structured background using a least-squares background correction, reference spectra were generated using the combination of different species. The use of the latter technique allowed the elimination of spectral interferences for most of the investigated samples, making possible the determination of lead in fertilizer and limestone samples free of interferences. The best results were found using a reference spectrum of NH4H2PO4 at 217.001 nm, and a mixture of H2SO4 + Ca and HNO3 + Ca at the 283.306 nm line. The accuracy of the method was evaluated using a certified reference material “Trace Elements in Multi-Nutrient Fertilizer”. Similar results were obtained using line source graphite furnace atomic absorption spectrometry with Zeeman-effect background correction, indicating that the latter technique was also capable to correct the spectral interferences, at least in part.

  7. An electrochemical flow-cell for permanent modification of graphite tube with palladium for mercury determination by electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Moreno, Ruben G. M.; de Oliveira, Elisabeth; Pedrotti, Jairo J.; Oliveira, Pedro V.

    2002-04-01

    An electrochemical procedure for palladium deposition on the inner surface of pyrolytic graphite-coated tubes for permanent chemical modification and a cold vapor generation system for the pre-concentration and determination of mercury trace levels in rain, potable, and non-potable water and lake sediment by electrothermal atomic absorption spectrometry is proposed. A tubular electrochemical flow-cell was assembled on the original geometry of the graphite tube, which operated as the working electrode. A stainless steel tube, positioned downstream from the working electrode, was used as the auxiliary electrode. The applied potential was measured against a micro Ag/AgCl (sat) reference electrode inserted in the auxiliary electrode. Palladium solution in acetate buffer (100 mmol l -1, pH=4.8), flowing at 0.5 ml min -1 for 60 min was used to perform the electrodeposition. A homemade cold vapor generation system composed of a peristaltic pump, an injector-commutator, a flow meter and a disposable polyethylene gas-liquid separator flask (approx. 4.0 ml volume) were used. Volumes of 1.0 ml of reagent (2.0% w/v NaBH 4 in 0.10 mol l -1 of NaOH) and 1.0 ml of reference or sample solution in 0.25 mol l -1 of HNO 3 were carried to the gas-liquid separator using the peristaltic pump. The mercury vapor was carried out to the modified graphite tube by argon flow (200 ml min -1), and pre-concentrated for 120 s. The characteristic mass for 1.0 ml of reference solution was 26 pg (R.S.D.=0.12%, n=5). The detection limit obtained was 93 pg ( n=20, 3δ). The reliability of the entire procedure was confirmed by addition and recovery tests and cold vapor atomic absorption spectrometry.

  8. Quantification of absorption, retention and elimination of two different oral doses of vitamin A in Zambian boys using accelerator mass spectrometry

    SciTech Connect

    Aklamati, E K; Mulenga, M; Dueker, S R; Buchholz, B A; Peerson, J M; Kafwembe, E; Brown, K H; Haskell, M J

    2009-10-12

    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 with 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.

  9. Laser desorption mass spectrometry for DNA analysis and sequencing

    SciTech Connect

    Chen, C.H.; Taranenko, N.I.; Tang, K.; Allman, S.L.

    1995-03-01

    Laser desorption mass spectrometry has been considered as a potential new method for fast DNA sequencing. Our approach is to use matrix-assisted laser desorption to produce parent ions of DNA segments and a time-of-flight mass spectrometer to identify the sizes of DNA segments. Thus, the approach is similar to gel electrophoresis sequencing using Sanger`s enzymatic method. However, gel, radioactive tagging, and dye labeling are not required. In addition, the sequencing process can possibly be finished within a few hundred microseconds instead of hours and days. In order to use mass spectrometry for fast DNA sequencing, the following three criteria need to be satisfied. They are (1) detection of large DNA segments, (2) sensitivity reaching the femtomole region, and (3) mass resolution good enough to separate DNA segments of a single nucleotide difference. It has been very difficult to detect large DNA segments by mass spectrometry before due to the fragile chemical properties of DNA and low detection sensitivity of DNA ions. We discovered several new matrices to increase the production of DNA ions. By innovative design of a mass spectrometer, we can increase the ion energy up to 45 KeV to enhance the detection sensitivity. Recently, we succeeded in detecting a DNA segment with 500 nucleotides. The sensitivity was 100 femtomole. Thus, we have fulfilled two key criteria for using mass spectrometry for fast DNA sequencing. The major effort in the near future is to improve the resolution. Different approaches are being pursued. When high resolution of mass spectrometry can be achieved and automation of sample preparation is developed, the sequencing speed to reach 500 megabases per year can be feasible.

  10. A simple and fast method for assessment of the nitrogen-phosphorus-potassium rating of fertilizers using high-resolution continuum source atomic and molecular absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Bechlin, Marcos André; Fortunato, Felipe Manfroi; da Silva, Ricardo Moutinho; Ferreira, Edilene Cristina; Gomes Neto, José Anchieta

    2014-11-01

    The determination of N, P, and K in fertilizers by high-resolution continuum source flame atomic and molecular absorption spectrometry is proposed. Under optimized conditions, measurements of the diatomic molecules NO and PO at 215.360 and 247.620 nm, respectively, and K using the wing of the alternative line at 404.722 nm allowed calibration curves to be constructed in the ranges 500-5000 mg L- 1 N (r = 0.9994), 100-2000 mg L- 1 P (r = 0.9946), and 100-2500 mg L- 1 K (r = 0.9995). Commercial fertilizers were analyzed by the proposed method and the concentrations of N, P, and K were found to be in agreement with those obtained by Kjeldahl, spectrophotometric, and flame atomic emission spectrometry methods, respectively, at a 95% confidence level (paired t-test). A phosphate rock certified reference material (CRM) was analyzed and the results for P and K were in agreement with the reference values. Recoveries from spiked CRM were in the ranges 97-105% (NO3--N), 95-103% (NH4+-N), 93-103% (urea-N), 99-108% (P), and 99-102% (K). The relative standard deviations (n = 12) for N, P, and K were 6, 4, and 2%, respectively.

  11. Feasibility of dispersive liquid-liquid microextraction for extraction and preconcentration of Cu and Fe in red and white wine and determination by flame atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Seeger, Tassia S.; Rosa, Francisco C.; Bizzi, Cezar A.; Dressler, Valderi L.; Flores, Erico M. M.; Duarte, Fabio A.

    2015-03-01

    A method for extraction and preconcentration of Cu and Fe in red and white wines using dispersive liquid-liquid microextraction (DLLME) and determination by flame atomic absorption spectrometry (F AAS) was developed. Extraction was performed using sodium diethyldithiocarbamate as chelating agent and a mixture of 40 μL of 1,2-dichlorobenzene (extraction solvent) and 900 μL of methanol (dispersive solvent). Some parameters that influencing the extraction efficiency such as pH (2 to 5), concentration of chelating agent (0 to 2%), effect of salt addition (0 to 10%), number of washing steps (1 to 4) and centrifugation time (0 to 15 min) were studied. Accuracy was evaluated after microwave-assisted digestion in closed vessels and analytes were determined by inductively coupled plasma optical emission spectrometry. Agreement with the proposed method ranged from 91 to 110 and from 89 to 113% for Cu and Fe, respectively. Calibration of F AAS instrument was performed using analyte addition method and limits of detection were 6.3 and 2.4 μg L- 1 for Cu and Fe, respectively. The proposed method was applied for the determination of Cu and Fe in five samples of red wine and three samples of white wine, with concentration ranging from 21 to 178 μg L- 1 and from 1.38 to 3.74 mg L- 1, respectively.

  12. Study on solid phase extraction and graphite furnace atomic absorption spectrometry for the determination of nickel, silver, cobalt, copper, cadmium and lead with MCI GEL CHP 20Y as sorbent.

    PubMed

    Yang, Guangyu; Fen, Weibo; Lei, Chun; Xiao, Weilie; Sun, Handong

    2009-02-15

    A solid phase extraction and graphite furnace atomic absorption spectrometry (GFAAS) for the determination of nickel, silver, cobalt, copper, cadmium and lead with MCI GEL CHP 20Y as sorbent was studied. Trace amounts of chromium, nickel, silver, cobalt, copper, cadmium and lead were reacted with 2-(2-quinolinil-azo)-4-methyl-1,3-dihydroxidobenzene (QAMDHB) followed by adsorption onto MCI GEL CHP 20Y solid phase extraction column, and 1.0molL(-1) HNO(3) was used as eluent. The metal ions in 300mL solution can be concentrated to 1.0mL, representing an enrichment factor of 300 was achieved. The recoveries of analytes at pH 8.0 with 1.0g of resin were greater than 95% without interference from alkaline, earth alkaline and some metal ions. When detected with graphite furnace atomic absorption spectrometry, the detection limits in the original samples were 1.4ngL(-1) for Cr(III), 1.0ngL(-1) for Ni(II), 0.85ngL(-1) for Ag(I), 1.2ngL(-1) for Co(II), 1.0ngL(-1) for Cu(II), 1.2ngL(-1) for Cd(II) and 1.3ngL(-1) for Pb(II). The validation of the procedure was performed by the analysis of the certified standard reference materials, and the presented procedure was applied to the determination of analytes in biological, water and soil samples with good results (recoveries range from 89 to 104%, and R.S.D.% lower than 3.2%. The results agreed with the standard value or reference method). PMID:18562094

  13. Cold vapor-solid phase microextraction using amalgamation in different Pd-based substrates combined with direct thermal desorption in a modified absorption cell for the determination of Hg by atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Romero, Vanesa; Costas-Mora, Isabel; Lavilla, Isela; Bendicho, Carlos

    2011-02-01

    In this work, different Pd-based substrates (i.e. Pd wire, Pd-coated stainless steel wire and Pd-coated SiO 2) are tried for microextraction of Hg prior to its release into a modified quartz T-cell so as to develop a cost-effective, sensitive and easy-to-handle coupling between solid-phase microextraction (SPME) and atomic absorption spectrometry. The new design allows a direct sample injection from the SPME device into a quartz T-cell thus avoiding analyte dilution. Mercury amalgamation onto a Pd wire provided the best performance in respect to sensitivity and fiber lifetime, but Pd wires could not be implemented in the SPME device due to their poor mechanical characteristics. On the contrary, Pd-coated SiO 2 fibers could be easily adapted to the typical sampling device used for SPME. Narrow time-dependent absorption signal profiles that could be integrated within 25 s were obtained. The detection limit was 90 pg mL -1 of Hg, and the repeatability expressed as relative standard deviation was 4.3%.

  14. Parametric analysis of a double-effect steam absorption chiller

    NASA Astrophysics Data System (ADS)

    Mohammed Salih Ahmed, Mojahid Sid Ahmed; Gilani, Syed Ihtsham Ul-Haq

    2012-06-01

    The development in the field of refrigeration and cooling systems based on absorption cycles has attained its own internal dynamic in the last decade. A major obstacle for developing model is the lack of available component specifications. These specifications are commonly proprietary of the chiller's manufacturers and normally the available information is not sufficient. This work presented a double-effect parallel-flow-type steam absorption chiller model based on thermodynamic and energy equations. The chiller studied is 1250 RT (Refrigeration Tons) using lithium bromide -water as working pair. The mathematical equations that govern the operation of the steam absorption chiller are developed, and from the available design data the values of the overall heat transfer coefficient multiplied by the heat exchanger surface area and the characteristics of each component of the absorption chiller at the design point are calculated. For thermo physical and thermodynamic properties for lithium bromide-water solution, set of computationally efficient formulations are used. The model gives the required information about temperature, concentration, and flow rate at each state point of the system. The model calculates the heat load at each component as well as the performance of the system.

  15. Preformance Analysis of NH3-H2O Absorption Cycle

    NASA Astrophysics Data System (ADS)

    Tsujimori, Atsushi; Ozaki, Eiichi

    Different from H2O-LiBr absorption cycle, it is necessary to have rectifier between generator and condenser in NH3-H2O absorption cycle, because there mixes some steam in refrigerant vapor in the process of regenerating refrigerant from the ammonia strong aqueous solution. And in some case ex. partial load or heating, the efficiency of rectifier might decrease, if the flow rate of refrigerant vapor and ammonia aqueous solution decrease. As a result, steam flow into condenser with ammonia refrigerant vapor, which reduces cycle COPs of cooling and heating. Accordingly in order to evaluate the effect of ammonia concentration in refrigerant for the performance of NH3-H2O absorption heat pump, the simple design approach of modeling condenser and evaporator is introduced in this paper. In the model, the calculation of heat rate in condenser and evaporator was simplified considering the characteristic of NH3-H2O liquid-vapor equilibrium. Then the simulation for cycle perforance based on GAX absorption cycle was made using the efficiency of rectifier that established the ammonia concentration in refrigerant and it was derived that 3 [%] decrease of ammonia concentration in refrigerant induced 15 [%] decrcase of cooling COP and 7 [%] decrease of heating COP and that there existed the most suitable circulation ratio for each ammonia concentration in refrigerant.

  16. Water-lithium bromide double-effect absorption cooling analysis

    NASA Astrophysics Data System (ADS)

    Vliet, G. C.; Lawson, M. B.; Lithgow, R. A.

    1980-12-01

    A numerical model was developed for the transient simulation of the double-effect, water-lithium bromide absorption cooling machine and was used to determine the effect of the various design and input variables on the absorption unit performance. The performance parameters considered were coefficient of performance and cooling capacity. The variables considered include source hot water, cooling water, and chilled water temperatures; source hot water, cooling water, and chilled water flow rates; solution circulation rate; heat exchanger areas; pressure drop between evaporator and absorber; solution pump characteristics; and refrigerant flow control methods. The performance sensitivity study indicates that the distribution of heat exchanger area among the various (seven) heat exchange components is a very important design consideration. Moreover, it indicated that the method of flow control of the first effect refrigerant vapor through the second effect is a critical design feature when absorption units operate over a significant range of cooling capacity. The model was used to predict the performance of the Trane absorption unit with fairly good accuracy.

  17. COMPUTER-ASSISTED FURNACE ATOMIC ABSORPTION SPECTROMETRIC ANALYSIS

    EPA Science Inventory

    The use of furnace atomic absorption instrumentation with a turnkey chromatography data system is described. A simple addition of relays to the furnace power supply allows for automatic start-up of A/D conversion and spectrophotometer zeroing at the proper time. Manipulations inv...

  18. Direct analysis of large living organism by megavolt electrostatic ionization mass spectrometry.

    PubMed

    Ng, Kwan-Ming; Tang, Ho-Wai; Man, Sin-Heng; Mak, Pui-Yuk; Choi, Yi-Ching; Wong, Melody Yee-Man

    2014-09-01

    A new ambient ionization method allowing the direct chemical analysis of living human body by mass spectrometry (MS) was developed. This MS method, namely Megavolt Electrostatic Ionization Mass Spectrometry, is based on electrostatic charging of a living individual to megavolt (MV) potential, illicit drugs, and explosives on skin/glove, flammable solvent on cloth/tissue paper, and volatile food substances in breath were readily ionized and detected by a mass spectrometer. PMID:24924518

  19. Direct Analysis of Large Living Organism by Megavolt Electrostatic Ionization Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Ng, Kwan-Ming; Tang, Ho-Wai; Man, Sin-Heng; Mak, Pui-Yuk; Choi, Yi-Ching; Wong, Melody Yee-Man

    2014-09-01

    A new ambient ionization method allowing the direct chemical analysis of living human body by mass spectrometry (MS) was developed. This MS method, namely Megavolt Electrostatic Ionization Mass Spectrometry, is based on electrostatic charging of a living individual to megavolt (MV) potential, illicit drugs, and explosives on skin/glove, flammable solvent on cloth/tissue paper, and volatile food substances in breath were readily ionized and detected by a mass spectrometer.

  20. Differentiation of the Chemical Profile of Piper arboreum Tissues Using NIR Spectrometry and Principal Component Analysis

    NASA Astrophysics Data System (ADS)

    Duarte, M. S.; Pontes, M. J. C.; Ramos, C. S.

    2016-01-01

    The differentiation of chemical profiles from Piper arboreum tissues using near infrared (NIR) spectrometry and principal component analysis (PCA) was addressed. The NIR analyses were performed with a small quantity of dried and ground tissues. Differences in the chemical composition of leaf, stem, and root tissues were observed. The results obtained were compared to those produced by gas chromatography-mass spectrometry (GC-MS) as the reference method, confirming the NIR results.

  1. Silver and lanthanum as effective modifiers in trace determination of cadmium in nickel-base alloys by electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Tsai, Suh-Jen Jane; Chang, Li-Lin; Chang, Shiow-Ing

    1997-01-01

    Trace cadmium in nickel-base superalloys was determined by a stabilized temperature platform furnace using atomic absorption spectrometry with a deuterium arc background correction system. The volatility of cadmium limits the pyrolysis temperature. This prevents the removal of the interfering alloy matrix at the thermal pretreatment step. Hence, an enormously high background signal has been observed. Chemical modifiers including ammonium citrate, 1-(2-pyridylazo)-naphthol, 4-(2pyridylazo)resorcinol, 2-(5-bromo-2-pyridylazo)-5-(diethylamino)-phenol, Triton-X 100, EDTA, potassium nitrate, palladium nitrate, magnesium nitrate, aluminum chloride, ammonium dihydrogen phosphate, lanthanum oxide, lanthanum chloride and silver nitrate have been studied. Matrix interferences were effectively reduced by silver and lanthanum. The 100-300°C increase in the pyrolysis temperature effectively reduced the non-specific absorption from the alloy matrix. Interferences from foreign ions were also investigated. The merit of the proposed method was increased by the excellent agreement between the certified and the experimental values of Cd in the standard reference material, IN100, and the recovery obtained (100-104%). The precision of six successive replicate measurements was 4.9% with Ag modifier and 2.5% with La modifier, respectively. The results of analysing Tracealloy B were also satisfactory.

  2. Synthesis of a new molecularly imprinted polymer for sorption of the silver ions from geological and antiseptic samples for determination by flame atomic absorption spectrometry.

    PubMed

    Hashemi-Moghaddam, Hamid; Yahyazadeh, Faegheh; Vardini, Mohammad Taghi

    2014-01-01

    A new molecularly imprinted polymer (MIP) was synthesized using methacrylic acid (functional monomer), ethylene glycol dimethacrylate (crosslinker), 2,2'-azobisisobutironitril (initiator), silver (Ag) dithizone complex (template), and chloroform (porogenic solvent). This process was a noncovalent, bulk, thermal radical-polymerization. To compare the performance of this polymer, control polymer (nonimprinted polymer) was prepared under well-defined conditions without the use of a template. Extraction experiments were performed on the MIP and a nonimprinted polymer. Then, various parameters were optimized, such as pH, time, concentration of sample, and type of eluent for elution of Ag from polymer. In addition, interfering effects were investigated on the absorption of Ag by the MIP. This polymer was used for the rapid extraction and preconcentration of Ag from an antiseptic and geological sample. Finally, the amount of Ag was measured by flame atomic absorption spectrometry after preconcentration by the synthesized MIP, and results were compared with a direct inductively coupled plasma method. The results showed high performance of this method in preconcentration of Ag. PMID:25902996

  3. Prediction of the furnace heat absorption by utilizing thermomechanical analysis for various kinds of coal firing

    SciTech Connect

    Ishinomori, T.; Watanabe, S.; Kiga, T.; Wall, T.F.; Gupta, R.P.; Gupta, S.K.

    1999-07-01

    In order to predict the furnace heat absorption, which is sensitive to coal properties, an attempt to make a model universally applicable for any kind of pulverized coal fired boiler is in progress. First of all, the heat absorption rates on to furnace wall were surveyed for 600MWe pulverized coal fired boiler, and they were ranked into four levels by indicating a furnace heat absorption index (FHAI). Some ash composition is relatively well related to the FHAI, while a new index from thermomechanical analysis (TMA) offers a good prediction of the furnace heat absorption.

  4. Applications of liquid chromatography-mass spectrometry for food analysis.

    PubMed

    Di Stefano, Vita; Avellone, Giuseppe; Bongiorno, David; Cunsolo, Vincenzo; Muccilli, Vera; Sforza, Stefano; Dossena, Arnaldo; Drahos, László; Vékey, Károly

    2012-10-12

    HPLC-MS applications in the agrifood sector are among the fastest developing fields in science and industry. The present tutorial mini-review briefly describes this analytical methodology: HPLC, UHPLC, nano-HPLC on one hand, mass spectrometry (MS) and tandem mass spectrometry (MS/MS) on the other hand. Analytical results are grouped together based on the type of chemicals analyzed (lipids, carbohydrates, glycoproteins, vitamins, flavonoids, mycotoxins, pesticides, allergens and food additives). Results are also shown for various types of food (ham, cheese, milk, cereals, olive oil and wines). Although it is not an exhaustive list, it illustrates the main current directions of applications. Finally, one of the most important features, the characterization of food quality (including problems of authentication and adulteration) is discussed, together with a future outlook on future directions. PMID:22560344

  5. Gallium trace on-line preconcentration/separation and determination using a polyurethane foam mini-column and flame atomic absorption spectrometry. Application in aluminum alloys, natural waters and urine.

    PubMed

    Anthemidis, Aristidis N; Zachariadis, George A; Stratis, John A

    2003-07-27

    A sensitive and selective flow injection time-based method for on-line preconcentration/separation and determination of gallium by flame atomic absorption spectrometry at trace levels was developed. The on-line formed gallium chloride complex is sorbed onto a polyether-type polyurethane foam mini-column, followed by on-line quantitative elution with isobutyl methyl ketone and direct introduction into the flame pneumatic nebulizer of the atomic absorption spectrometer. All chemical and flow variables of the system as well as the possible interferences were studied. The manner of strong HCl solutions propulsion was investigated and established using a combination of two displacement bottles. For 90 s preconcentration time, a sample frequency of 28 h(-1), an enhancement factor of 40, a detection limit of 6 microg l(-1) and a precision expressed as relative standard deviation (s(r)) of 3.3% (at 1.00 mg l(-1)) were achieved. The calibration curve is linear over the concentration range 0.02-3.00 mg l(-1). The accuracy of the developed method was sufficient and evaluated by the analysis of a silicon-aluminum alloy standard reference material. Finally, it was successfully applied to gallium determination in commercial aluminum alloys, natural waters and urine. PMID:18969117

  6. Computational and Statistical Analysis of Protein Mass Spectrometry Data

    PubMed Central

    Noble, William Stafford; MacCoss, Michael J.

    2012-01-01

    High-throughput proteomics experiments involving tandem mass spectrometry produce large volumes of complex data that require sophisticated computational analyses. As such, the field offers many challenges for computational biologists. In this article, we briefly introduce some of the core computational and statistical problems in the field and then describe a variety of outstanding problems that readers of PLoS Computational Biology might be able to help solve. PMID:22291580

  7. Speciation of methyl- and butyltin compounds and inorganic tin in oysters by hydride generation atomic absorption spectrometry

    SciTech Connect

    Han, J.S.; Weber, J.H.

    1988-02-15

    Because of the toxicity of tributyltin originating from many antifouling marine paints, there is much concern about its effect on aquatic life and, particularly, on shellfish. This paper describes speciation of inorganic tin, methyltin compounds, and butyltin compounds from oyster samples. The authors validated the hydride generation atomic absorption spectrophotometric technique by demonstrating ca. 100% recovery from spiked samples and by the absence of any organotin decomposition products. Absolute detection limits (3sigma) are 1.1-2.5 ng for 0.1-g oyster samples (wet weight). This method is superior to published techniques because of careful validation, low limits of detection, and minimal sample manipulation.

  8. Peptide-Centric Proteome Analysis: An Alternative Strategy for the Analysis of Tandem Mass Spectrometry Data

    SciTech Connect

    Ting, Ying S.; Egertson, Jarrett D.; Payne, Samuel H.; Kim, Sangtae; MacLean, Brendan; Kall, Lukas; Aebersold, Ruedi; Smith, Richard D.; Noble, William; MacCoss, Michael

    2015-09-01

    In mass spectrometry-based bottom-up proteomics, data-independent acquisition (DIA) is an emerging technique due to its comprehensive and unbiased sampling of precursor ions. However, current DIA methods use wide precursor isolation windows, resulting in co- fragmentation and complex mixture spectra. Thus, conventional database searching tools that identify peptides by interpreting individual MS/MS spectra are inherently limited in analyzing DIA data. Here we discuss an alternative approach, peptide-centric analysis, which tests directly for the presence and absence of query peptides. We discuss how peptide-centric analysis resolves some limitations of traditional spectrum-centric analysis, and we outline the benefits of peptide-centric analysis in general.

  9. Analysis of finite dose dermal absorption data: Implications for dermal exposure assessment

    PubMed Central

    Frasch, H Frederick; Dotson, G Scott; Bunge, Annette L; Chen, Chen-Peng; Cherrie, John W; Kasting, Gerald B; Kissel, John C; Sahmel, Jennifer; Semple, Sean; Wilkinson, Simon

    2014-01-01

    A common dermal exposure assessment strategy estimates the systemic uptake of chemical in contact with skin using the fixed fractional absorption approach: the dermal absorbed dose is estimated as the product of exposure and the fraction of applied chemical that is absorbed, assumed constant for a given chemical. Despite the prominence of this approach there is little guidance regarding the evaluation of experiments from which fractional absorption data are measured. An analysis of these experiments is presented herein, and limitations to the fixed fractional absorption approach are discussed. The analysis provides a set of simple algebraic expressions that may be used in the evaluation of finite dose dermal absorption experiments, affording a more data-driven approach to dermal exposure assessment. Case studies are presented that demonstrate the application of these tools to the assessment of dermal absorption data. PMID:23715085

  10. Applications of principal component analysis to breath air absorption spectra profiles classification

    NASA Astrophysics Data System (ADS)

    Kistenev, Yu. V.; Shapovalov, A. V.; Borisov, A. V.; Vrazhnov, D. A.; Nikolaev, V. V.; Nikiforova, O. Y.

    2015-12-01

    The results of numerical simulation of application principal component analysis to absorption spectra of breath air of patients with pulmonary diseases are presented. Various methods of experimental data preprocessing are analyzed.

  11. Determination of yttrium and rare-earth elements in rocks by graphite-furnace atomic-absorption spectrometry.

    PubMed

    Gupta, J G

    1981-01-01

    With use of synthetic solutions and several international standard reference materials a method has been developed for determining traces of Y, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu in rocks by electrothermal atomization in a pyrolytically-coated graphite furnace. Depending on the element, the sensitivity is of the order of 10(-9)-10(-12) g at 2500 degrees . To avoid matrix interferences the lanthanides are separated from the common elements by co-precipitation with calcium and iron as carriers. The data for Canadian reference rock SY-2 (syenite), U.S.G.S. reference rocks W-2 (diabase), DNC-1 (diabase) and BIR-1 (basalt), and South African reference rock NIM-18/69 (carbonatite) obtained by graphite-furnace atomization are compared with the values obtained by flame atomic-absorption. The results are in good agreement with literature values. PMID:18962852

  12. Improved limit of detection and quantitation development and validation procedure for quantification of zinc in Insulin by atomic absorption spectrometry.

    PubMed

    Qadir, Muhammad Abdul; Ahmed, Mahmood; Haq, Iftikharul; Ahmed, Saghir

    2015-05-01

    A simple and expeditious analytical method for determination of zinc in human insulin isophane suspension by flame atomic absorption spectrophotometer (FAAS) was validated. The method was carried out on atomic absorption spectrometer with 0.4 nm bandwidth, 1.0 filter factor on deuterium (D2) background correction. The integration time was set at 3.0 second with 5.0 mA lamp current. The parameters of method validation showed adequate linearity, efficiency and relative standard deviation values were between 0.64%-1.69% (n=7), 1.31%-1.58% (n=10) for repeatability and intermediate precision respectively. The limit of detection 0.0032 μg/mL, 0.0173 μg/mL, 0.0231 μg/mL and limit of quantitation 0.0107μg/mL, 0.0578 μg/mL, 0.0694 μg/mL based on signal to noise (SN), calibration curve method (CCM) and fortification of blank (FB) were obtained respectively. The percentages of recovery for low, medium and high spiked concentration levels of zinc in human insulin were 99.38 ± 0.04 to 100.3 ± 0.03, 98.45 ± 0.38 to 100.3 ± 0.07 and 99.42 ± 0.03 to 99.42 ± 0.08 respectively. With the use of this method, five samples from each vial of human insulin isophane suspension were analyzed and the zinc content was determined. The zinc content were 22.1 ± 0.025 μg/mL and 24.3 ± 0.028 μg/mL which compliance the British Pharmacopoeia standard. PMID:26004720

  13. Determination of boron in blood, urine and bone by electrothermal atomic absorption spectrometry using zirconium and citric acid as modifiers

    NASA Astrophysics Data System (ADS)

    Burguera, Marcela; Burguera, José Luis; Rondón, Carlos; Carrero, Pablo

    2001-10-01

    A comparative study of various potential chemical modifiers (Au, Ba, Be, Ca, Cr, Ir, La, Lu, Mg, Ni, Pd, Pt, Rh, Ru, Sr, V, W, and Zr), and different 'coating' treatments (Zr, W, and W+Rh) of the pyrolytic graphite platform of a longitudinally heated graphite tube atomizer for thermal stabilization and determination of boron was undertaken. The use of Au, Ba, Be, Cr, Ir, Pt, Rh, Ru, Sr and V as modifiers, and of W+Rh coating produced erratic, and noisy signals, while the addition of La, Ni and Pd as modifiers, and the W coating had positive effects, but with too high background absorption signals, rendering their use unsuitable for boron determination even in aqueous solutions. The atomic absorption signal for boron was increased and stabilized when the platform was coated with Zr, and by the addition of Ca, Mg, Lu, W or Zr as modifiers. Only the addition of 10 μg of Zr as a modifier onto Zr-treated platforms allowed the use of a higher pyrolysis temperature without analyte losses. The memory effect was minimized by incorporating a cleaning step with 10 μl of 50 g l -1 NH 4F HF after every three boron measurements. The addition of 10 μl of 15 g l -1 citric acid together with Zr onto Zr-treated platforms significantly improved the characteristic mass to m0=282 pg, which is adequate for biological samples such as urine and bone, although the sensitivity was still inadequate for the determination of boron in blood of subjects without supplementary diet. Under optimized conditions, the detection limit (3σ) was 60 μg l -1. The amount of boron found in whole blood, urine and femur head samples from patients with osteoporosis was in agreement with values previously reported in the literature.

  14. Dithizone immobilized silica gel on-line preconcentration of trace copper with detection by flame atomic absorption spectrometry.

    PubMed

    Yu, Hong-Mei; Song, Hua; Chen, Ming-Li

    2011-07-15

    A novel adsorbent-silica gel bound dithizone (H(2)Dz-SG) was prepared and used as solid-phase extraction of copper from complex matrix. The H(2)Dz-SG is investigated by means of FT-IR spectra and the SEM images, demonstrating the bonding of dithizone. The H(2)Dz-SG quantitatively adsorb copper ions, and the retained copper is afterwards collected by elution of 10% (v/v) nitric acid. An on-line flow injection solid-phase extraction procedure was developed for trace copper separation and preconcentration with detection by flame atomic spectrometry. By loading 5.4 mL of sample solution, a liner range of 0.5-120 μg L(-1), an enrichment factor of 42.6, a detection limit of 0.2 μg L(-1) and a precision of 1.7% RSD at the 40 μg L(-1) level (n=11) were obtained, along with a sampling frequency of 47 h(-1). The dynamic sorption capacity of H(2)Dz-SG to Cu(2+) was 0.76 mg g(-1). The accuracy of the proposed procedure was evaluated by determination of copper in reference water sample. The potential applications of the procedure for extraction of trace copper were successfully accomplished in water samples (tap, rain, snow, sea and river). The spiking recoveries within 91-107% are achieved. PMID:21645750

  15. Energy and Exergy Analysis of Vapour Absorption Refrigeration Cycle—A Review

    NASA Astrophysics Data System (ADS)

    Kanabar, Bhaveshkumar Kantilal; Ramani, Bharatkumar Maganbhai

    2016-07-01

    In recent years, an energy crisis and the energy consumption have become global problems which restrict the sustainable growth. In these scenarios the scientific energy recovery and the utilization of various kinds of waste heat become very important. The waste heat can be utilized in many ways and one of the best practices is to use it for vapour absorption refrigeration system. To ensure efficient working of absorption cycle and utilization of optimum heat, exergy is the best tool for analysis. This paper provides the comprehensive picture of research and development of absorption refrigeration technology, practical and theoretical analysis with different arrangements of the cycle.

  16. Energy and Exergy Analysis of Vapour Absorption Refrigeration Cycle—A Review

    NASA Astrophysics Data System (ADS)

    Kanabar, Bhaveshkumar Kantilal; Ramani, Bharatkumar Maganbhai

    2016-02-01

    In recent years, an energy crisis and the energy consumption have become global problems which restrict the sustainable growth. In these scenarios the scientific energy recovery and the utilization of various kinds of waste heat become very important. The waste heat can be utilized in many ways and one of the best practices is to use it for vapour absorption refrigeration system. To ensure efficient working of absorption cycle and utilization of optimum heat, exergy is the best tool for analysis. This paper provides the comprehensive picture of research and development of absorption refrigeration technology, practical and theoretical analysis with different arrangements of the cycle.

  17. Feasibility analysis of a vortex generator for absorption heat pumps

    SciTech Connect

    Fineblum, S.S.

    1996-12-31

    Significant thermal resources in the form of low temperature industrial waste heat, between 211 to 528 trillion kJ (200 and 500 trillion BTU`s) per annum, have the potential to drive absorption heat pumps. The proposed vortex generator permits a practical heat pump to operate efficiently with as much as 20 to 30 C below the boiling temperature of water (70--80 C (158--176 F)). Energy flows and auxiliary power requirements are computed. The system is shown to operate with relatively low temperature waste heat with higher specific capacity than conventional systems.

  18. Laser desorption mass spectrometry for high-throughput DNA analysis and its applications

    NASA Astrophysics Data System (ADS)

    Chen, C. H. Winston; Golovlev, Valeri V.; Taranenko, N. I.; Allman, S. L.; Isola, Narayana R.; Potter, N. T.; Matteson, K. J.; Chang, Linus Y.

    1999-05-01

    Laser desorption mass spectrometry (LDMS) has been developed for DNA sequencing, disease diagnosis, and DNA fingerprinting for forensic applications. With LDMS, the speed of DNA analysis can be much faster than conventional gel electrophoresis. No dye or radioactive tagging to DNA segments for detection is needed. LDMS is emerging as a new alternative technology for DNA analysis.

  19. Detection and analysis of polymerase chain reaction products by mass spectrometry

    SciTech Connect

    Hurst, G.B., Doktycz, M.J., Britt, P.F., Vass, A.A., Buchanan, M.V.

    1997-02-01

    This paper describes recent and ongoing efforts to overcome some of the obstacles to more routine and robust application of MALDI-TOF to analysis of polymerase chain reaction products and other information- bearing nucleic acid molecules. Methods for purifying nucleic acid samples are described, as is the application of delayed extraction TOF mass spectrometry to analysis of short oligonucleotides.

  20. Laser Desorption Mass Spectrometry for High Throughput DNA Analysis and Its Applications

    SciTech Connect

    Allman, S.L.; Chen, C.H.; Golovlev, V.V.; Isola, N.R.; Matteson, K.J.; Potter, N.T.; Taranenko, N.I.

    1999-01-23

    Laser desorption mass spectrometry (LDMS) has been developed for DNA sequencing, disease diagnosis, and DNA Fingerprinting for forensic applications. With LDMS, the speed of DNA analysis can be much faster than conventional gel electrophoresis. No dye or radioactive tagging to DNA segments for detection is needed. LDMS is emerging as a new alternative technology for DNA analysis.

  1. Use of Tritium Accelerator Mass Spectrometry for Tree Ring Analysis

    PubMed Central

    LOVE, ADAM H.; HUNT, JAMES R.; ROBERTS, MARK L.; SOUTHON, JOHN R.; CHIARAPPA - ZUCCA, MARINA L.; DINGLEY, KAREN H.

    2010-01-01

    Public concerns over the health effects associated with low-level and long-term exposure to tritium released from industrial point sources have generated the demand for better methods to evaluate historical tritium exposure levels for these communities. The cellulose of trees accurately reflects the tritium concentration in the source water and may contain the only historical record of tritium exposure. The tritium activity in the annual rings of a tree was measured using accelerator mass spectrometry to reconstruct historical annual averages of tritium exposure. Milligram-sized samples of the annual tree rings from a Tamarix located at the Nevada Test Site are used for validation of this methodology. The salt cedar was chosen since it had a single source of tritiated water that was well-characterized as it varied over time. The decay-corrected tritium activity of the water in which the salt cedar grew closely agrees with the organically bound tritium activity in its annual rings. This demonstrates that the milligram-sized samples used in tritium accelerator mass spectrometry are suited for reconstructing anthropogenic tritium levels in the environment. PMID:12144257

  2. Use of tritium accelerator mass spectrometry for tree ring analysis.

    PubMed

    Love, Adam H; Hunt, James R; Roberts, Mark L; Southon, John R; Chiarapp-Zucca, Marina L; Dingley, Karen H

    2002-07-01

    Public concerns over the health effects associated with low-level and long-term exposure to tritium released from industrial point sources have generated the demand for better methods to evaluate historical tritium exposure levels for these communities. The cellulose of trees accurately reflects the tritium concentration in the source water and may contain the only historical record of tritium exposure. The tritium activity in the annual rings of a tree was measured using accelerator mass spectrometry to reconstruct historical annual averages of tritium exposure. Milligram-sized samples of the annual tree rings from a Tamarix located at the Nevada Test Site are used for validation of this methodology. The salt cedar was chosen since it had a single source of tritiated water that was well-characterized as it varied over time. The decay-corrected tritium activity of the water in which the salt cedar grew closely agrees with the organically bound tritium activity in its annual rings. This demonstrates that the milligram-sized samples used in tritium accelerator mass spectrometry are suited for reconstructing anthropogenic tritium levels in the environment. PMID:12144257

  3. Simultaneous determination of iron and nickel in fluoropolymers by solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry.

    PubMed

    Soares, Bruno M; Santos, Rafael F; Bolzan, Rodrigo C; Muller, Edson I; Primel, Ednei G; Duarte, Fabio A

    2016-11-01

    This paper reports the development of a method of simultaneous determination of iron and nickel in fluoropolymers by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS) with direct solid sampling. In order to carry out simultaneous measurements, both the main resonance line of nickel (232.003nm) and the adjacent secondary line of iron (232.036nm) were monitored in the same spectral window. The proposed method was optimized with a perfluoroalkoxy (PFA) sample and was applied to the determination of iron and nickel in fluorinated ethylene propylene (FEP) and modified polytetrafluoroethylene (PTFE-TFM) samples. Pyrolysis and atomization temperatures, as well as the use of Pd and H2 (during pyrolysis) as chemical modifiers, were carefully investigated. Compromise temperatures for pyrolysis and atomization of both analytes were achieved at 800 and 2300°C, respectively, using only 0.5Lmin(-1) H2 as chemical modifier during pyrolysis. Calibration curves were performed with aqueous standards by using a single solution which contained both analytes. Limits of detection were 221 and 9.6ngg(-1) for iron and nickel, respectively. Analyte concentrations in all samples ranged from 3.53 to 12.4µgg(-1) for iron and from 37 to 78ngg(-1) for nickel, with relative standard deviation less than 19%. Accuracy was evaluated by comparing these results with those obtained by inductively coupled plasma mass spectrometry after sample digestion by microwave-induced combustion and no significant statistical difference was observed. PMID:27591638

  4. Slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry for steelmaking flue dust analysis

    NASA Astrophysics Data System (ADS)

    Coedo, A. G.; Dorado, T.; Padilla, I.; Maibusch, R.; Kuss, H.-M.

    2000-02-01

    A commercial atomic absorption graphite furnace (AAGF), with a self-made adapter and valve system, was used as a slurry sampling cell for electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS). The system was applied to the determination of As, Sn, Sb, Se, Te, Bi, Cd, V, Ti and Mo in steelmaking flue dusts. Experimental conditions with respect to ETV and ICP-MS operating parameters were optimized. Compared to aqueous solutions, slurry samples were found to present better analyte transport. Microgram amounts of Rh were used to reduce the difference in analyte response in sensitivity for aqueous solutions of the tested analytes. No such increasing effect was observed for slurry samples and aqueous standards. An added quantity of Rh acting as modifier/carrier resulted in an increase for the same analytes in matrix-slurry solutions, even the addition of an extra Rh quantity has resulted in a decrease in the signals. The effect of Triton X-100 (used as a dispersant agent) on analyte intensity and precision was also studied. External calibration from aqueous standards spiked with 100 μg ml -1 Rh was performed to quantified 0.010 g/100 ml slurry samples. Results are presented for a certified reference electrical arc furnace flue dust (EAF): CRM-876-1 (Bureau of Analysis Samples Ltd., Cleveland, UK), a reference sample of coke ashes X-3705 (from AG der Dillinger Hüttenwerke, Germany), and a representative sample of EAF flue dust from a Spanish steelmaking company (CENIM-1). For the two reference materials an acceptable agreement with certificate values was achieved, and the results for the CENIM sample matched with those obtained from conventional nebulization solution.

  5. From Raw Data to Biological Discoveries: A Computational Analysis Pipeline for Mass Spectrometry-Based Proteomics

    NASA Astrophysics Data System (ADS)

    Lavallée-Adam, Mathieu; Park, Sung Kyu Robin; Martínez-Bartolomé, Salvador; He, Lin; Yates, John R.

    2015-11-01

    In the last two decades, computational tools for mass spectrometry-based proteomics data analysis have evolved from a few stand-alone software solutions serving specific goals, such as the identification of amino acid sequences based on mass spectrometry spectra, to large-scale complex pipelines integrating multiple computer programs to solve a collection of problems. This software evolution has been mostly driven by the appearance of novel technologies that allowed the community to tackle complex biological problems, such as the identification of proteins that are differentially expressed in two samples under different conditions. The achievement of such objectives requires a large suite of programs to analyze the intricate mass spectrometry data. Our laboratory addresses complex proteomics questions by producing and using algorithms and software packages. Our current computational pipeline includes, among other things, tools for mass spectrometry raw data processing, peptide and protein identification and quantification, post-translational modification analysis, and protein functional enrichment analysis. In this paper, we describe a suite of software packages we have developed to process mass spectrometry-based proteomics data and we highlight some of the new features of previously published programs as well as tools currently under development.

  6. From raw data to biological discoveries: a computational analysis pipeline for mass spectrometry-based proteomics.

    PubMed

    Lavallée-Adam, Mathieu; Park, Sung Kyu Robin; Martínez-Bartolomé, Salvador; He, Lin; Yates, John R

    2015-11-01

    In the last two decades, computational tools for mass spectrometry-based proteomics data analysis have evolved from a few stand-alone software solutions serving specific goals, such as the identification of amino acid sequences based on mass spectrometry spectra, to large-scale complex pipelines integrating multiple computer programs to solve a collection of problems. This software evolution has been mostly driven by the appearance of novel technologies that allowed the community to tackle complex biological problems, such as the identification of proteins that are differentially expressed in two samples under different conditions. The achievement of such objectives requires a large suite of programs to analyze the intricate mass spectrometry data. Our laboratory addresses complex proteomics questions by producing and using algorithms and software packages. Our current computational pipeline includes, among other things, tools for mass spectrometry raw data processing, peptide and protein identification and quantification, post-translational modification analysis, and protein functional enrichment analysis. In this paper, we describe a suite of software packages we have developed to process mass spectrometry-based proteomics data and we highlight some of the new features of previously published programs as well as tools currently under development. Graphical Abstract ᅟ. PMID:26002791

  7. Extension of working range in Zeeman graphite furnace atomic absorption spectrometry by nonlinear calibration with prior correction for stray light

    NASA Astrophysics Data System (ADS)

    Lonardo, Robert F.; Yuzefovsky, Alexander I.; Zhou, Jack X.; McCaffrey, John T.; Michel, Robert G.

    1996-09-01

    The nonlinear working range of a Perkin-Elmer 4100Zl atomic absorption spectrometer was improved in three steps. Firstly, each absorbance datum within the transient profile was corrected for the presence of stray light by an algorithm originally developed by L'vov and co-workers (Spectrochim. Acta Part B, 47 (1992) 889-895 and 1187-1202), but with the incorporation of the Newton method of successive approximations (Spectrochim. Acta Part B, 49 (1994) 1643-1656. Secondly, a dip correction procedure was performed on temporal signal profiles that exhibited a dip due to rollover. In the final step, an analytically useful working curve was generated by the nonlinear calibration routine of Barnett (Spectrochim. Acta Part B, 39 (1984) 829). Goodness of fit between the resultant calibration curve and the data was measured by the method suggested by Miller-Ihli et al. (Spectrochim. Acta Part B, 39 (1984) 1603) that is based on the sum of squares of the percentage deviation (SSPD) and the root mean square (RMS) percentage deviation. For lead, silver, copper, thallium, and cadmium, the analytical nonlinear working range was increased by as much as one and a half orders of magnitude, without any significant effect on the RMS. For chromium and manganese, no significant improvement in the nonlinear working range was observed, while the RMS improved by 50%. In the case of nickel, neither the working range nor the RMS was improved.

  8. Fast determination of phosphorus in honey, milk and infant formulas by electrothermal atomic absorption spectrometry using a slurry sampling procedure

    NASA Astrophysics Data System (ADS)

    López-García, I.; Viñas, P.; Romero-Romero, R.; Hernández-Córdoba, M.

    2007-01-01

    A procedure for the electrothermal atomic absorption spectrometric determination of phosphorus in honey, milk and infant formulas using slurried samples is described. Suspensions prepared in a medium containing 50% v/v concentrated hydrogen peroxide, 1% v/v concentrated nitric acid, 10% m/v glucose, 5% m/v sucrose and 100 mg l - 1 of potassium were introduced directly into the furnace. For the honey samples, multiple injection of the sample was necessary. The modifier selected was a mixture of 20 μg palladium and 5 μg magnesium nitrate, which was injected after the sample and before proceeding with the drying and calcination steps. Calibration was performed using aqueous standards prepared in the same suspension medium and the graph was linear between 5 and 80 mg l - 1 of phosphorus. The reliability of the procedure was checked by comparing the results obtained by the new developed method with those found when using a reference spectrophotometric method after a mineralization step, and by analyzing several certified reference materials.

  9. Determination of nickel in water, food, and biological samples by electrothermal atomic absorption spectrometry after preconcentration on modified carbon nanotubes.

    PubMed

    Taher, Mohammad Ali; Mazaheri, Lida; Ashkenani, Hamid; Mohadesi, Alireza; Afzali, Daryoush

    2014-01-01

    A new and sensitive SPE method using modified carbon nanotubes for extraction and preconcentration, and electrothermal atomic absorption spectrometric determination of nickel (Ni) in real samples at ng/L levels was investigated. First, multiwalled carbon nanotubes were oxidized with concentrated HNO3, then modified with 2-(5-bormo-2-pyridylazo)-5-diethylaminophenol reagent. The adsorption was achieved quantitatively on a modified carbon nanotubes column in a pH range of 6.5 to 8.5; the adsorbed Ni(II) ions were then desorbed by passing 5.0 mL of 1 M HNO3. The effects of analytical parameters, including pH of the solution, eluent type and volume, sample volume, flow rate of the eluent, and matrix ions, were investigated for optimization of the presented procedure. The enrichment factor was 180, and the LOD for Ni was 4.9 ng/L. The method was applied to the determination of Ni in water, food, and biological samples, and reproducible results were obtained. PMID:24672882

  10. Speciation of inorganic lead and trialkyllead compounds by flame atomic absorption spectrometry following continuous selective preconcentration from aqueous solutions

    NASA Astrophysics Data System (ADS)

    Baena, Josefa R.; Gallego, Mercedes; Valcárcel, Miguel

    1999-12-01

    A new method for the speciation of inorganic lead and trialkyllead compounds involving the selective separation of the analytes in a continuous system and their subsequent introduction into a flame atomic absorption spectrometer was developed. The proposed flow system consists of two units. In the first unit, total inorganic lead at concentrations from 8 to 200 ng ml -1 is continuously precipitated as lead chromate and the filtrate, containing trialkyllead cations, is collected in a vessel, the precipitate then being dissolved in diluted acid and driven to the instrument. In the second unit, trimethyllead (TML +) and triethyllead (TEL +) cations at ng ml -1 levels are complexed with sodium diethyldithiocarbamate and retained on a C 60 pre-conditioned fullerene column; the mixture of both species was resolved by conditioning the sorbent column with n-hexane or isobutyl methyl ketone solvents. Detection limits of 1-2 ng ml -1 can be achieved by using a sample volume of 50 ml. Special attention was given to the reliability and robustness of the global flow injection method in assessing its applicability to both types of organolead compounds and inorganic lead present in different proportions. Trimethyllead provides the poorest results as consequence of its low adsorption constant on C 60; however, the three different types of species (Pb 2+/TML +/TEL +) can be effectively determined in proportions from 1:1:1 to 30:12:1 with relative errors less than 10%.

  11. The application of atomic absorption spectrometry for the determination of residual active pharmaceutical ingredients in cleaning validation samples.

    PubMed

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

    2011-03-01

    The objective of this work was the development and validation of atomic absorption spectrometric (AAS) methods for the determination of residual active pharmaceutical ingredients (API) in rinse samples for cleaning validation. AAS as an indirect method for the determination of API in rinse samples can be applied when it is in the form of salt with metal ions or when the metal ion is a part of the API's structure. The electrothermal AAS methods (aqueous and ethanol medium) for the determination of magnesium in esomeprazole magnesium and the flame AAS method for the determination of lithium in lithium carbonate in rinse samples were developed. Various combinations of solvents were tested and a combination of 1% aqueous or ethanol solution of nitric acid for esomeprazole magnesium and 0.1% aqueous solution of nitric acid for lithium carbonate were found to be the most suitable. The atomization conditions in the graphite furnace and in the flame were carefully studied to avoid losses of analyte and to achieve suitable sensitivity. The cleaning verification methods were validated with respect to accuracy, precision, linearity, limit of detection, and quantification. In all the cases, the limits of detection were at the microgram level. The methods were successfully applied for the determination of esomeprazole magnesium and lithium carbonate in rinse samples from cleaning procedures. PMID:20923390

  12. Back-extraction of trace elements from organometallic-halide extracts for determination by flameless atomic absorption spectrometry

    USGS Publications Warehouse

    Clark, J.R.; Viets, J.G.

    1981-01-01

    The Methyl isobutyl ketone-Amine synerGistic Iodkte Complex (MAGIC) extraction system offers the advantage that a large number of trace elements can be rapidly determined with a single sample preparation procedure. However, many of the elements extracted by the MAGIC system form volatile organometallic halide salts when the organic extract is heated in the graphite furnace. High concentrations of some elements such as Cu and Zn extracted by the system from anomalous geological samples produce serious interferences when certain other elements are determined by flameless atomic absorption. Stripping systems have been developed using solutions of HNO3, H2SO4, and CH3COOH individually or combined with H2O2 in order to circumvent these problems. With these systems most of the elements in the organic extract can be sequentially stripped into an aqueous phase. Organometallic volatilization and the most serious interelement interferences, therefore, can be eliminated by stripping with various combinations of reagents in a series of steps.

  13. Black-extraction of trace elements from organometallic-halide extracts for determination by flameless atomic absorption spectrometry

    SciTech Connect

    Clark, J.R.; Viets, J.G.

    1981-01-01

    The Methyl isobutyl ketone-Amine synerGistic Iodide Complex (MAGIC) extraction system offers the advantage that a large number of trace elements can be rapidly determined with a single sample preparation procedure. However, many of the elements extracted by the MAGIC system form volatile organometallic halide salts when the organic extract is heated in the graphite furnace. High concentrations of some elements such as Cu and Zn extracted by the system from anomalous geological samples produce serious interferences when certain other elements are determined by flameless atomic absorption. Stripping systems have been developed using solutions of HNO/sub 3/, H/sub 2/SO/sub 4/, and CH/sub 3/COOH individually or combined with H/sub 2/O/sub 2/ in order to circumvent these problems. With these systems most of the elements in the organic extract can be sequentially stripped into an aqueous phase. Organometallic volatilization and the most serious interelement interferences, therefore, can be eliminated by stripping with various combinations of reagents in a series of steps.

  14. Ultrasound-promoted cold vapor generation in the presence of formic acid for determination of mercury by atomic absorption spectrometry.

    PubMed

    Gil, Sandra; Lavilla, Isela; Bendicho, Carlos

    2006-09-01

    A new cold vapor technique within the context of green chemistry is described for determination of mercury in liquid samples following high-intensity ultrasonication. Volatile Hg evolved in a sonoreactor without the use of a chemical reducing agent is carried to a quartz cell kept at room temperature for measurement of the atomic absorption. The mechanism involved lies in the reduction of Hg(II) to Hg(0) by reducing gases formed upon sonication and subsequent volatilization of Hg(0) due to the degassing effect caused by the cavitation phenomenon. Addition of a low molecular weight organic acid such as formic acid favors the process, but vapor generation also occurs from Hg solutions in ultrapure water. The detection limit of Hg was 0.1 microg/L, and the repeatability, expressed as relative standard deviation, was 4.4% (peak height). Addition of small amounts of oxidizing substances such as the permanganate or dichromate anions completely suppressed the formation of Hg(0), which confirms the above mechanism. Effect of other factors such as ultrasound irradiation time, ultrasound amplitude, and the presence of concomitants are also investigated. Some complexing anions such as chloride favored the stabilization of Hg(II) in solution, hence causing an interference effect on the ultrasound-assisted reduction/volatilization process. PMID:16944910

  15. Wavelength-modulated tunable diode-laser absorption spectrometry for real-time monitoring of microbial growth.

    PubMed

    Shao, Jie; Xiang, Jindong; Axner, Ove; Ying, Chaofu

    2016-03-20

    It is important to monitor and assess the growth of micro-organisms under various conditions. Yet, thus far there has been no technique to do this with the required speed and accuracy. This work demonstrates swift and accurate assessment of the concentration of carbon dioxide that is produced by use of a wavelength-modulated tunable diode-laser based absorption spectroscopy (WM-TDLAS). It is shown by experiments on two types of bacteria, Staphylococcus aureus and Candida albicans, that the technique can produce high signal-to-noise-ratio data from bacteria grown in confined spaces and exposed to limited amounts of nutrients that can be used for extraction of growth parameters by fitting of the Gompertz model. By applying the technique to S. aureus bacteria at various temperatures (in the 25°C to 42°C range), it is specifically shown that both the maximum growth rate and the so-called lag time have a strong temperature dependence (under the specific conditions with a maximum of the former at 37°C) that matches conventional models well for bacterial growth. Hence, it is demonstrated that WM-TDLAS monitoring CO2 is a user-friendly, non-intrusive, and label-free technique that swiftly, and with high signal-to-noise-ratio, can be used for rapid (on the Hz scale) and accurate assessment of bacterial growth. PMID:27140571

  16. [Using the mass spectrometry analysis for hepatitis C virus typing].

    PubMed

    Il'ina, E N; Malakhova, M V; Generozov, E V; Govorun, V M; Archakov, A I; Pokrovskiĭ, V I

    2005-01-01

    Determination of the hepatitis C virus (HCV) genotype has become the standard procedure in laboratory diagnostics of HCV infection. Genotype elucidation has prognostic value assignment helps in assessing disease prognosis and promotes establishing appropriate duration of treatment. Now 11 major genotypes and more than 70 subtypes of HCV have been identified using the sequence variability within 5' non-coding region (5' NCR). In Russia the most common subtypes are 1a, 1b, 2a, 3a and more rare - 4 and 5 types. While the "gold standard" for testing is nucleic acid sequencing, a variety of other assays, including the line probe assay or type-specific amplification, has been developed to provide more rapid and cheaper forms of testing. The aim of this study was to determine the type-specific single nucleotide polymorphism (SNP) in 5' NCR HCV by the classical three-step minisequencing method with followed MALDI-TOF mass spectrometry detection The fragments of 5'NCR of HCV genomes were amplified by the nested RT PCR. The removal of excess nucleotides and primers was performed. Three oligonucleotide primers were design to detect two sets of type-specific SNP in 5' NCR HCV. The primer extension reaction was performed using modified thermostable DNA polymerase and in the presence of ddNTP. The molecular weights of primers extension reaction products were analyzed using MALDI-TOF mass spectrometry. The HCV genotype was determined according the presence in analyses sample the molecules with expected molecular weights. The suggested method was used to type HCV from 69 HCV-positive sera. The 1a genotype was determine in 4.5% samples, 1b - 48%, 2a - 4.5% 3a - 29%, 4 - 1.5%. The mixes of two genotypes were found in 13% samples. All data confirmed by direct nucleic acid sequence. Thus, the new method for HCV typing has been developed using the minisequencing reaction and mass spectrometry for the determination of nucleic acid molecular weight. PMID:15850217

  17. 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…

  18. Surface analysis of lipids by mass spectrometry: more than just imaging.

    PubMed

    Ellis, Shane R; Brown, Simon H; In Het Panhuis, Marc; Blanksby, Stephen J; Mitchell, Todd W

    2013-10-01

    Mass spectrometry is now an indispensable tool for lipid analysis and is arguably the driving force in the renaissance of lipid research. In its various forms, mass spectrometry is uniquely capable of resolving the extensive compositional and structural diversity of lipids in biological systems. Furthermore, it provides the ability to accurately quantify molecular-level changes in lipid populations associated with changes in metabolism and environment; bringing lipid science to the "omics" age. The recent explosion of mass spectrometry-based surface analysis techniques is fuelling further expansion of the lipidomics field. This is evidenced by the numerous papers published on the subject of mass spectrometric imaging of lipids in recent years. While imaging mass spectrometry provides new and exciting possibilities, it is but one of the many opportunities direct surface analysis offers the lipid researcher. In this review we describe the current state-of-the-art in the direct surface analysis of lipids with a focus on tissue sections, intact cells and thin-layer chromatography substrates. The suitability of these different approaches towards analysis of the major lipid classes along with their current and potential applications in the field of lipid analysis are evaluated. PMID:23623802

  19. Influence of citric acid as chemical modifier for lead determination in dietary calcium supplement samples by graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Cezar Paz de Mattos, Julio; Medeiros Nunes, Adriane; Figueiredo Martins, Ayrton; Luiz Dressler, Valderi; Marlon de Moraes Flores, Érico

    2005-06-01

    Citric acid was used as a chemical modifier for Pb determination by graphite furnace atomic absorption spectrometry in dietary supplement samples (calcium carbonate, dolomite and oyster shell samples) and its efficiency was compared to the use of palladium. Pyrolysis and atomization curves were established without use of chemical modifier, with the addition of 20, 100 and 200 μg of citric acid, and with 3 μg of palladium. The citric acid modifier made possible the interference-free Pb determination in the presence of high concentrations of Ca and Mg nitrates. Acid sample digestion involving closed vessels (microwave-assisted and conventional heating) and acid attack using polypropylene vessels at room temperature were compared. All digestion procedures presented similar results for calcium carbonate and dolomite samples. However, for oyster shell samples accurate results were obtained only with the use of closed vessel systems. Analyte addition and matrix-matched standards were used for calibration. The characteristic mass for Pb using citric acid and palladium were 16 and 25 pg, respectively. The relative standard deviation (RSD) was always less than 5% when citric acid was used. The relative and absolute limits of detection were 0.02 μg g - 1 and 8 pg with citric acid and 0.1 μg g - 1 and 44 pg with the Pd modifier, respectively ( n = 10, 3σ). The recovery of Pb in spiked calcium supplement samples (10 μg l - 1 ) was between 98% and 105%. With the use of 100 μg of citric acid as chemical modifier, problems such as high background absorption and high RSD values were minimized in comparison to the addition of 3 μg of palladium.

  20. Determination of cadmium, chromium, copper and lead in sediments and soil samples by electrothermal atomic absorption spectrometry using zirconium containing chemical modifiers.

    PubMed

    Acar, Orhan

    2006-05-01

    A method for direct determination of cadmium, chromium, copper and lead in sediments and soil samples by electrothermal atomic absorption spectrometry using Zr, Ir, etylenediamine acetic acid (EDTA), Zr + EDTA, Ir + EDTA, Zr + Ir and Zr + Ir + EDTA as chemical modifiers in 0.5% (v/v) Triton X-100 plus 0.2% (v/v) nitric acid mixture used as diluent was developed. The effects of mass and mass ratio of modifiers on analytes in sample solutions were studied. The optimum masses and mass ratios of modifiers: 20 microg of Zr, 4 microg of Ir, 100 microg of EDTA and 20 microg of Zr + 4 microg of Ir + 100 microg of EDTA, were used to enhance the analyte signals. Pyrolysis and atomization temperatures, atomization and background absorption profiles, characteristic masses, and detection limits of analytes in samples were compared in the presence or absence of a modifier. The detection limits and characteristic masses of analytes in a 0.5% (m/v) dissolved sample (dilution factor of 200 ml g(-1)) obtained with Zr + Ir + EDTA are 8.0 ng g(-1) and 1.2 pg for Cd, 61 ng g(-1) and 4.3 pg for Cr, 32 ng g(-1) and 23 pg for Cu, and 3.4 ng g(-1) and 19 pg for Pb, respectively. The Zr + Ir + EDTA modifier mixture was found to be preferable for the determination of analytes in sediment and soil-certified and standard reference materials. Depending on the sample type, the percent recoveries of analytes were increased from 81 to 103% by using the proposed modifier mixture; the results obtained are in good agreement with the certified values. PMID:16770053

  1. Data Analysis Methods for Synthetic Polymer Mass Spectrometry: Autocorrelation

    PubMed Central

    Wallace, William E.; Guttman, Charles M.

    2002-01-01

    Autocorrelation is shown to be useful in describing the periodic patterns found in high- resolution mass spectra of synthetic polymers. Examples of this usefulness are described for a simple linear homopolymer to demonstrate the method fundamentals, a condensation polymer to demonstrate its utility in understanding complex spectra with multiple repeating patterns on different mass scales, and a condensation copolymer to demonstrate how it can elegantly and efficiently reveal unexpected phenomena. It is shown that using autocorrelation to determine where the signal devolves into noise can be useful in determining molecular mass distributions of synthetic polymers, a primary focus of the NIST synthetic polymer mass spectrometry effort. The appendices describe some of the effects of transformation from time to mass space when time-of-flight mass separation is used, as well as the effects of non-trivial baselines on the autocorrelation function.

  2. Trace level perchlorate analysis by ion chromatography-mass spectrometry.

    PubMed

    Mathew, Johnson; Gandhi, Jay; Hedrick, Joe

    2005-08-26

    Perchlorate is commonly used as an oxidant in solid fuel propellant for rockets and missiles. Recently perchlorate contamination was found in many aquifers associated with Colorado River and other sites. Perchlorate was also found at elevated level in crops that use contaminated water for irrigation. Ion chromatography with conductivity detection could be used to measure perchlorate levels in drinking and wastewaters as per United States Environmental Protection Agency method 314, but at lower levels and with complexity of the matrix there could be false positive and/or false negative. This study was done to demonstrate the detection of perchlorate with lower detection limit with high ionic matrix by ion chromatography-mass spectrometry. PMID:16106848

  3. Method validation for the determination of total mercury in fish muscle by cold vapour atomic absorption spectrometry.

    PubMed

    Nascimento Neto, A P; Costa, L C S Magalhães; Kikuchi, A N S; Furtado, D M S; Araujo, M Q; Melo, M C C

    2012-01-01

    A method was validated for the determination of total Hg in fish muscle using continuous flow cold vapour atomic absorption (CVAAS) after microwave digestion in closed vessels. The method was validated according to European Union Regulations 333/2007 and 657/2002, considering the maximum level for the metal in fish, established by European Union regulation 1881/2006. The procedure for determining linear range, selectivity, recovery, precision, trueness, decision limit (CCα), detection capability (CCβ), measurement uncertainty and robustness of the method is reported. The results of the validation process demonstrate the method fulfils the provisions of the Commission Regulation. The selectivity study indicated that there was no matrix effect on the calibration curve between the concentration range of 1.0 and 30.0 µg Hg l(-1). The mean recovery calculated at six levels of fortification was in the range of 94-104%. The limit of detection (LOD) and limit of quantification (LOQ) values were 4.90 and 15.7 µg kg(-1), while the CCα and CCβ values were 0.517 and 0.533 mg kg(-1), respectively, for the maximum contaminant level of 0.500 mg kg(-1). The relative expanded measurement uncertainty of the method was 0.055 mg kg(-1). The method was not affected by slight variations of some critical factors (ruggedness minor changes) as sample mass and volume of the HNO(3) and H(2)O(2) used in the digestion step. The method allowed accurate confirmation analyses of the CRM DORM 3. In fact, the Z-scores attained in a proficiency test round were well below the reference value of 2.0, proving the excellent performance of the laboratory. PMID:22250927

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

    NASA Astrophysics Data System (ADS)

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

    2002-05-01

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

  5. Determination of inorganic arsenic species by flow injection hydride generation atomic absorption spectrometry with variable sodium tetrahydroborate concentrations*1

    NASA Astrophysics Data System (ADS)

    Sigrist, Mirna E.; Beldoménico, Horacio R.

    2004-07-01

    This work describes a study on the determination of inorganic arsenic species in ground water and synthetic experimental matrices, using a flow injection system with on-line hydride generation device coupled to an atomic absorption spectrometer with flame-heated quartz atomizer (FI HG AAS). Specific trivalent arsenic determination is based on the slow kinetics of As(V) on the hydride generation reaction using sufficiently low concentrations of sodium tetrahydroborate (NaBH 4) as reductant in highly acidic conditions (pH<0). Under these conditions, the efficiency of hydride generation from As(V) is much lower than that from As(III). The pentavalent form is determined by the difference between total inorganic arsenic and As(III). As(V) interferences were studied using As(III) solutions ranging from 0% to 50% of total inorganic As. The optimized NaBH 4 concentration was 0.035% (w/v). The detection limit was 1.4 μg l -1 As(III). As(V) interferences were 6% in the case of water samples with 6 μg l -1 As(III) in the presence of 54 μg l -1 As(V) (i.e. 10% As(III)). Interferences of methylated arsenic species (MMA and DMA) were evaluated. Speciation method was satisfactorily applied to 20 field arsenical water samples from Santa Fe, Argentina, with values ranging from 30 to 308 μg l -1 total As. We found from 0% to 36% As(III) in the 20 field samples. The developed methodology constitutes an economic, simple and reliable way to evaluate inorganic arsenic distribution in underground waters or similar systems with negligible or no content of organoarsenicals.

  6. Mass spectrometry.

    NASA Technical Reports Server (NTRS)

    Burlingame, A. L.; Johanson, G. A.

    1972-01-01

    Review of the current state of mass spectrometry, indicating its unique importance for advanced scientific research. Mass spectrometry applications in computer techniques, gas chromatography, ion cyclotron resonance, molecular fragmentation and ionization, and isotope labeling are covered. Details are given on mass spectrometry applications in bio-organic chemistry and biomedical research. As the subjects of these applications are indicated alkaloids, carbohydrates, lipids, terpenes, quinones, nucleic acid components, peptides, antibiotics, and human and animal metabolisms. Particular attention is given to the mass spectra of organo-inorganic compounds, inorganic mass spectrometry, surface phenomena such as secondary ion and electron emission, and elemental and isotope analysis. Further topics include mass spectrometry in organic geochemistry, applications in geochronology and cosmochemistry, and organic mass spectrometry.

  7. 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

  8. Rapid fingerprinting of sterols and related compounds in vegetable and animal oils and phytosterol enriched- margarines by transmission mode direct analysis in real time mass spectrometry.

    PubMed

    Alberici, Rosana M; Fernandes, Gabriel D; Porcari, Andréia M; Eberlin, Marcos N; Barrera-Arellano, Daniel; Fernández, Facundo M

    2016-11-15

    Plant-derived sterols, often referred to as phytosterols, are important constituents of plant membranes where they assist in maintaining phospholipid bilayer stability. Consumption of phytosterols has been suggested to positively affect human health by reducing cholesterol levels in blood via inhibition of its absorption in the small intestine, thus protecting against heart attack and stroke. Sterols are challenging analytes for mass spectrometry, since their low polarity makes them difficult to ionize by both electrospray ionization (ESI) and matrix-assisted laser desorption ionization (MALDI), typically requiring derivatization steps to overcome their low ionization efficiencies. We present a fast and reliable method to characterize the composition of phytosterols in vegetable oils and enriched margarines. The method requires no derivatization steps or sample extraction procedures thanks to the use of transmission mode direct analysis in real time mass spectrometry (TM-DART-MS). PMID:27283681

  9. Continuous wavelet-transform analysis of photoacoustic signal waveform to determine optical absorption coefficient

    NASA Astrophysics Data System (ADS)

    Hirasawa, T.; Ishihara, M.; Tsujita, K.; Hirota, K.; Irisawa, K.; Kitagaki, M.; Fujita, M.; Kikuchi, M.

    2012-02-01

    In photo-acoustic (PA) imaging, valuable medical applications based on optical absorption spectrum such as contrast agent imaging and blood oxygen saturation measurement have been investigated. In these applications, there is an essential requirement to determine optical absorption coefficients accurately. In present, PA signal intensities have been commonly used to determine optical absorption coefficients. This method achieves practical accuracy by combining with radiative transfer analysis. However, time consumption of radiative transfer analysis and effects of signal generation efficiencies were problems of this method. In this research, we propose a new method to determine optical absorption coefficients using continuous wavelet transform (CWT). We used CWT to estimate instantaneous frequencies of PA signals which reflects optical absorption distribution. We validated the effectiveness of CWT in determination of optical absorption coefficients through an experiment. In the experiment, planar shaped samples were illuminated to generate PA signal. The PA signal was measured by our fabricated PA probe in which an optical fiber and a ring shaped P(VDFTrFE) ultrasound sensor were coaxially aligned. Optical properties of samples were adjusted by changing the concentration of dye solution. Tunable Ti:Sapphire laser (690 - 1000 nm) was used as illumination source. As a result, we confirmed strong correlation between optical absorption coefficients of samples and the instantaneous frequency of PA signal obtained by CWT. Advantages of this method were less interference of light transfer and signal generation efficiency.

  10. Evaluation of Ion Mobility-Mass Spectrometry for Comparative Analysis of Monoclonal Antibodies.

    PubMed

    Ferguson, Carly N; Gucinski-Ruth, Ashley C

    2016-05-01

    Analytical techniques capable of detecting changes in structure are necessary to monitor the quality of monoclonal antibody drug products. Ion mobility mass spectrometry offers an advanced mode of characterization of protein higher order structure. In this work, we evaluated the reproducibility of ion mobility mass spectrometry measurements and mobiligrams, as well as the suitability of this approach to differentiate between and/or characterize different monoclonal antibody drug products. Four mobiligram-derived metrics were identified to be reproducible across a multi-day window of analysis. These metrics were further applied to comparative studies of monoclonal antibody drug products representing different IgG subclasses, manufacturers, and lots. These comparisons resulted in some differences, based on the four metrics derived from ion mobility mass spectrometry mobiligrams. The use of collision-induced unfolding resulted in more observed differences. Use of summed charge state datasets and the analysis of metrics beyond drift time allowed for a more comprehensive comparative study between different monoclonal antibody drug products. Ion mobility mass spectrometry enabled detection of differences between monoclonal antibodies with the same target protein but different production techniques, as well as products with different targets. These differences were not always detectable by traditional collision cross section studies. Ion mobility mass spectrometry, and the added separation capability of collision-induced unfolding, was highly reproducible and remains a promising technique for advanced analytical characterization of protein therapeutics. Graphical Abstract ᅟ. PMID:26988372

  11. Evaluation of Ion Mobility-Mass Spectrometry for Comparative Analysis of Monoclonal Antibodies

    NASA Astrophysics Data System (ADS)

    Ferguson, Carly N.; Gucinski-Ruth, Ashley C.

    2016-05-01

    Analytical techniques capable of detecting changes in structure are necessary to monitor the quality of monoclonal antibody drug products. Ion mobility mass spectrometry offers an advanced mode of characterization of protein higher order structure. In this work, we evaluated the reproducibility of ion mobility mass spectrometry measurements and mobiligrams, as well as the suitability of this approach to differentiate between and/or characterize different monoclonal antibody drug products. Four mobiligram-derived metrics were identified to be reproducible across a multi-day window of analysis. These metrics were further applied to comparative studies of monoclonal antibody drug products representing different IgG subclasses, manufacturers, and lots. These comparisons resulted in some differences, based on the four metrics derived from ion mobility mass spectrometry mobiligrams. The use of collision-induced unfolding resulted in more observed differences. Use of summed charge state datasets and the analysis of metrics beyond drift time allowed for a more comprehensive comparative study between different monoclonal antibody drug products. Ion mobility mass spectrometry enabled detection of differences between monoclonal antibodies with the same target protein but different production techniques, as well as products with different targets. These differences were not always detectable by traditional collision cross section studies. Ion mobility mass spectrometry, and the added separation capability of collision-induced unfolding, was highly reproducible and remains a promising technique for advanced analytical characterization of protein therapeutics.

  12. Analysis of Mammalian Sphingolipids by Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS) and Tissue Imaging Mass Spectrometry (TIMS)

    PubMed Central

    Sullards, M. Cameron; Liu, Ying; Chen, Yanfeng; Merrill, Alfred H.

    2011-01-01

    Sphingolipids are a highly diverse category of molecules that serve not only as components of biological structures but also as regulators of numerous cell functions. Because so many of the structural features of sphingolipids give rise to their biological activity, there is a need for comprehensive or “sphingolipidomic” methods for identification and quantitation of as many individual subspecies as possible. This review defines sphingolipids as a class, briefly discusses classical methods for their analysis, and focuses primarily on liquid chromatography tandem mass spectrometry (LC-MS/MS) and tissue imaging mass spectrometry (TIMS). Recently, a set of evolving and expanding methods have been developed and rigorously validated for the extraction, identification, separation, and quantitation of sphingolipids by LC-MS/MS. Quantitation of these biomolecules is made possible via the use of an internal standard cocktail. The compounds that can be readily analyzed are free long-chain (sphingoid) bases, sphingoid base 1-phosphates, and more complex species such as ceramides, ceramide 1-phosphates, sphingomyelins, mono- and di-hexosylceramides sulfatides, and novel compounds such as the 1-deoxy- and 1-(deoxymethyl)-sphingoid bases and their N-acyl-derivatives. These methods can be altered slightly to separate and quantitate isomeric species such as glucosyl/galactosylceramide. Because these techniques require the extraction of sphingolipids from their native environment, any information regarding their localization in histological slices is lost. Therefore, this review also describes methods for TIMS. This technique has been shown to be a powerful tool to determine the localization of individual molecular species of sphingolipids directly from tissue slices. PMID:21749933

  13. Multivariate optimization of ultrasound-assisted extraction for determination of Cu, Fe, Ni and Zn in vegetable oils by high-resolution continuum source atomic absorption spectrometry.

    PubMed

    Trindade, Alex S N; Dantas, Alailson F; Lima, Daniel C; Ferreira, Sérgio L C; Teixeira, Leonardo S G

    2015-10-15

    An assisted liquid-liquid extraction of copper, iron, nickel and zinc from vegetable oil samples with subsequent determination by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS) was optimized by applying a full factorial design in two levels and the response surface methodology, Box-Behnken. The effects of the acid concentration and the amplitude, cycle and time of sonication on the extraction of the analytes, as well as their interactions, were assessed. In the selected condition (sonication amplitude = 66%, sonication time = 79 s, sonication cycle = 74%), using 0.5 mol L(-1) HCl as the extractant, the limits of quantification were 0.14, 0.20, 0.21 and 0.04 μg g(-1) for Cu, Fe, Ni and Zn, respectively, with R.S.D. ranging from 1.4% to 3.6%. The proposed method was applied for the determination of the analytes in soybean, canola and sunflower oils. PMID:25952852

  14. Cloud point extraction combined with electrothermal atomic absorption spectrometry for the speciation of antimony(III) and antimony(V) in food packaging materials.

    PubMed

    Jiang, Xiuming; Wen, Shengping; Xiang, Guoqiang

    2010-03-15

    A simple, sensitive method for the speciation of inorganic antimony by cloud point extraction combined with electrothermal atomic absorption spectrometry (ETAAS) is presented and evaluated. The method based on the fact that formation of a hydrophobic complex of antimony(III) with ammonium pyrrolidine dithiocarbamate (APDC) at pH 5.0 and subsequently the hydrophobic complex enter into surfactant-rich phase, whereas antimony(V) remained in aqueous solutions. Antimony(III) in surfactant-rich phase was analyzed by ETAAS after dilution by 0.2 mL nitric acid in methanol (0.1M), and antimony(V) was calculated by subtracting antimony(III) from the total antimony after reducing antimony(V) to antimony(III) by l-cysteine. The main factors affecting the cloud point extraction, such as pH, concentration of APDC and Triton X-114, equilibrium temperature and incubation time, sample volume were investigated in detail. Under the optimum conditions, the detection limit (3 sigma) of the proposed method was 0.02 ng mL(-1) for antimony(III), and the relative standard deviation was 7.8% (c=1.0 ng mL(-1), n=7). The proposed method was successfully applied to speciation of inorganic antimony in the leaching solutions of different food packaging materials with satisfactory results. PMID:19853991

  15. Permanent iridium modifier deposited on tungsten and zirconium-treated platforms in electrothermal atomic absorption spectrometry: vaporization of bismuth, silver and tellurium

    NASA Astrophysics Data System (ADS)

    Slaveykova, Vera I.; Lampugnani, Leonardo; Tsalev, Dimiter L.; Sabbatini, L.; De Giglio, Elvira

    1999-04-01

    The stabilizing role of permanent iridium modifier deposited on tungsten-treated (WTP) and zirconium-treated (ZrTP) platforms of transversely heated graphite atomizer (THGA) was studied in detail by electrothermal atomic absorption spectrometry (ETAAS) and different surface techniques in model experiments for Ag, Bi and Te. The comparison of the stabilizing efficiency of permanent Ir modifier on WTP and ZrTP and each of the single components, reveals the better effect of Ir on WTP and Ir itself. The extent of analyte losses during pre-atomization and the strength of analyte association with the modifier were estimated by the plotting of `differential vaporization curves'. The existence of double peaks of Ag, Bi and Te in WTP and Ir on WTP was confirmed and possible reasons for their formation were discussed. The absorbance profiles presented as differential curves reveal an existence of at least two different types of precursors determining processes of atom generation. The observed differences in the behavior of Ir permanent modifier on WTP and ZrTP, respectively, were explained by the different extent of iridium-tungsten and iridium-zirconium interaction and surface distribution. XRF, ESCA and SEM studies reveal non-uniform distribution of the modifier on the graphite substrate and the presence of oxide containing species on the surface.

  16. 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%. PMID:27451169

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

    PubMed

    Rezvani, Seyyed Ahmad; Soleymanpour, Ahmad

    2016-03-01

    A very convenient, sensitive and precise solid phase extraction (SPE) system was developed for enrichment and determination of ultra-trace of cadmium ion in water and plant samples. This method was based on the retention of cadmium(II) ions by l-cystine adsorbed in Y-zeolite and carry out in a packed mini-column. The retained cadmium ions then were eluted and determined by flame atomic absorption spectrometry. The scanning electron microscopy (SEM), powder X-ray diffraction (XRD) and Fourier Transform Infrared (FT-IR) spectroscopy techniques were applied for the characterization of cystine modified zeolite (CMZ). Some experimental conditions affecting the analytical performance such as pH, eluent type, concentration of sample, eluent flow rate and also the presence of interfering ions were investigated. The calibration graph was linear within the range of 0.1-7.5ngmL(-1) and limit of detection was obtained 0.04ngmL(-1) with the preconcentration factor of 400. The relative standard deviation (RSD) was obtained 1.4%, indicating the excellent reproducibility of this method. The proposed method was successfully applied for the extraction and determination of cadmium(II) ion in black tea, cigarette's tobacco and also various water samples. PMID:26852265

  18. Imidazole-Modified Nanoporous Silica for Lead Ion Solid Phase Extraction Prior to Determination from Industrial Wastewaters by Flame Atomic Absorption Spectrometry.

    PubMed

    Behbahani, Ali; Ardjmand, Mehdi

    2015-01-01

    A new method was applied to produce modified nanoporous silica as a novel sorbent for Pb(II) ion SPE from industrial wastewater samples. In this modified method, the produced nanoporous silica has a higher functional group loading, which leads to a higher preconcentration factor as well as a lower LOD. This modified nanoporous silica was used for preconcentration prior to subsequent determination of Pb(II) ions by flame atomic absorption spectrometry. Various parameters such as the eluent, pH of the sample solution, and flow rate were optimized during this work. Also, the effect of a variety of ions on preconcentration and recovery of Pb(II) ions was investigated. The LOD, defined as five times the SD of the blank, was determined to be lower than 0.1 mg/L with an RSD of <2%. The accuracy of the method was established by analyzing standard reference materials with certified Pb concentrations. Finally, the established method was successfully applied for determination of the Pb(II) ion concentration in industrial wastewater samples. PMID:26525261

  19. Direct determination of bromine in plastic materials by means of solid sampling high-resolution continuum source graphite furnace molecular absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Flórez, M. R.; Resano, M.

    2013-10-01

    This work investigates the potential of high-resolution continuum source graphite furnace molecular absorption spectrometry for the direct determination of bromine in polymers, which could be interesting in view of the current regulations restricting the use of organobrominated compounds. The method developed is based on the addition of Ca (300 μg) and Pd (30 μg) to favor the formation of CaBr, which is monitored at the main molecular “lines” (rotational spectra) found in the vicinity of 625.315 nm. It was found that accurate results could be obtained for all the samples investigated (polyethylene, polypropylene and acrylonitrile butadiene styrene certified reference materials) using any of the lines studied and constructing the calibration curve with aqueous standards. Furthermore, the combined use of the main four CaBr lines available in the spectral area simultaneously monitored permits to easily expand the linear range up to 2000 ng, provides a limit of detection of 1.8 ng (1.8 μg g- 1 for a mass of 1 mg) and further improves precision to values between 3-7% RSD. Overall, the method proposed seems suited for the fast and simple control of these types of samples (approximately 10 min for sample are required), circumventing the traditional problems associated with sample digestion (e.g., losses of volatile compounds), and providing sufficient sensitivity to easily comply with regulations.

  20. Novel ion imprinted magnetic mesoporous silica for selective magnetic solid phase extraction of trace Cd followed by graphite furnace atomic absorption spectrometry detection

    NASA Astrophysics Data System (ADS)

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

    2015-05-01

    Determination of trace Cd in environmental, biological and food samples is of great significance to toxicological research and environmental pollution monitoring. While the direct determination of Cd in real-world samples is difficult due to its low concentration and the complex matrix. Herein, a novel Cd(II)-ion imprinted magnetic mesoporous silica (Cd(II)-II-MMS) was prepared and was employed as a selective magnetic solid-phase extraction (MSPE) material for extraction of trace Cd in real-world samples followed by graphite furnace atomic absorption spectrometry (GFAAS) detection. Under the optimized conditions, the detection limit of the proposed method was 6.1 ng L- 1 for Cd with the relative standard deviation (RSD) of 4.0% (c = 50 ng L- 1, n = 7), and the enrichment factor was 50-fold. To validate the proposed method, Certified Reference Materials of GSBZ 50009-88 environmental water, ZK018-1 lyophilized human urine and NIES10-b rice flour were analyzed and the determined values were in a good agreement with the certified values. The proposed method exhibited a robust anti-interference ability due to the good selectivity of Cd(II)-II-MMS toward Cd(II). It was successfully employed for the determination of trace Cd(II) in environmental water, human urine and rice samples with recoveries of 89.3-116%, demonstrating that the proposed method has good application potential in real world samples with complex matrix.

  1. Flow injection method for the rapid determination of chemical oxygen demand based on microwave digestion and chromium speciation in flame atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Cuesta, A.; Todoli, J. L.; Canals, A.

    1996-12-01

    The present paper describes a new flow injection method for the determination of Chemical Oxygen Demand (COD). This method consists of a first digestion step, where the sample is heated by microwave radiation, a second one where an anionic exchange resin retains the Cr(VI) that has not been reduced by the organic matter of the sample and a third one where Cr(VI), after being eluted, is determined by flame atomic absorption spectrometry. The microwave power applied, the sulphuric acid concentration, the liquid flow in the digestion step and the sample volume were the variables studied. The recovery and precision obtained with this method are similar to those obtained using a standard semi-micro method, whereas the throughput is much higher (up to 50 determinations per hour). As regards sensitivity, by changing the sample loop volume and the concentration of dichromate, one can analyze samples with Chemical Oxygen Demand values between 25 and 5000 mg/l. The limit of detection is about 7 mg/l COD. An interesting feature of the new method, which is not shared by most other flow injection methods of Chemical Oxygen Demand determination, is that there is no matrix effect in the determination step.

  2. Multi-element determination of Cu, Fe, Ni and Zn content in vegetable oils samples by high-resolution continuum source atomic absorption spectrometry and microemulsion sample preparation.

    PubMed

    Nunes, Luana S; Barbosa, José T P; Fernandes, Andréa P; Lemos, Valfredo A; Santos, Walter N L Dos; Korn, Maria Graças A; Teixeira, Leonardo S G

    2011-07-15

    The aim of this work was to evaluate the microemulsification as sample preparation procedure for determination of Cu, Fe, Ni and Zn in vegetable oils samples by High-Resolution Continuum Source Flame Atomic Absorption Spectrometry (HR-CS FAAS). Microemulsions were prepared by mixing samples with propan-1-ol and aqueous acid solution, which allowed the use of inorganic aqueous standards for the calibration. To a sample mass of 0.5g, 100μL of hydrochloric acid and propan-1-ol were added and the resulting mixture diluted to a final volume of 10mL. The sample was manually shaken resulting in a visually homogeneous system. The main lines were selected for all studied metals and the detection limits (3σ, n=10) were 0.12, 0.62, 0.58 and 0.12mgkg(-1) for Cu, Fe, Ni and Zn, respectively. The relative standard deviation (RSD) ranged from 5% to 11 % in samples spiked with 0.25 and 1.5μgmL(-1) of each metal, respectively. Recoveries varied from 89% to 102%. The proposed method was applied to the determination of Cu, Fe, Ni and Zn in soybean, olive and sunflower oils. PMID:23140735

  3. 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. PMID:24645530

  4. Ultrasound-Assisted Emulsification Microextraction Based on Solidification Floating Organic Drop Trace Amounts of Manganese Prior to Graphite Furnace Atomic Absorption Spectrometry Determination

    PubMed Central

    Mohadesi, Alireza; Falahnejad, Masoumeh

    2012-01-01

    In the present study, an ultrasound-assisted emulsification microextraction based on solidification floating organic drop method is described for preconcentration of trace amounts of Mn (II). 2-(5-Bromo-2-pyridylazo)-5 diethylaminophenol was added to a solution of Mn+2 at ph = 10.0. After this, 1-undecanol was added to the solution as an extraction solvent, and solution was stirred. Several factors influencing the microextraction efficiency, such as pH, the amount of chelating agent, nature and volume of extraction solvent, the volume of sample solution, stirring rate, and extraction time were investigated and optimized. Then sample vial was cooled by inserting into an ice bath, and the solidified was transferred into a suitable vial for immediate melting. Finally the sample was injected into a graphite furnace atomic absorption spectrometry. Under the optimum condition the linear dynamic range was 0.50–10.0 ng mL−1 with a correlation coefficient of 0.9926, and the detection limit of 0.3 ng mL−1 was obtained. The enrichment factor was 160. The proposed method was successfully applied for separation and determination of manganese in sea, rain, tap, and river water samples. PMID:22645504

  5. One-step displacement dispersive liquid-liquid microextraction coupled with graphite furnace atomic absorption spectrometry for the selective determination of methylmercury in environmental samples.

    PubMed

    Liang, Pei; Kang, Caiyan; Mo, Yajun

    2016-03-01

    A novel method for the selective determination of methylmercury (MeHg) was developed by one-step displacement dispersive liquid-liquid microextraction (D-DLLME) coupled with graphite furnace atomic absorption spectrometry. In the proposed method, Cu(II) reacted with diethyldithiocarbamate (DDTC) to form Cu-DDTC complex, which was used as the chelating agent instead of DDTC for the dispersive liquid-liquid microextraction (DLLME) of MeHg. Because the stability of MeHg-DDTC is higher than that of Cu-DDTC, MeHg can displace Cu from the Cu-DDTC complex and be preconcentrated in a single DLLME procedure. MeHg could be extracted into the extraction solvent phase at pH 6 while Hg(II) remained in the sample solution. Potential interference from co-existing metal ions with lower DDTC complex stability was largely eliminated without the need of any masking reagent. Under the optimal conditions, the limit of detection of this method was 13.6ngL(-1) (as Hg), and an enhancement factor of 81 was achieved with a sample volume of 5.0mL. The proposed method was successfully applied for the determination of trace MeHg in some environmental samples with satisfactory results. PMID:26717807

  6. Speciation of very low amounts of arsenic and antimony in waters using dispersive liquid-liquid microextraction and electrothermal atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Rivas, Ricardo E.; López-García, Ignacio; Hernández-Córdoba, Manuel

    2009-04-01

    A new procedure for the determination of inorganic arsenic (III,V) and antimony (III,V) in water samples by dispersive liquid-liquid micro extraction separation and electrothermal atomic absorption spectrometry (ETAAS) is presented. At pH 1, As(III) and Sb(III) are complexed with ammonium pyrrolidine dithiocarbamate and extracted into the fine droplets formed when mixing carbon tetrachloride (extraction solvent), methanol (disperser solvent) and the sample solution. After extraction, the phases are separated by centrifugation, and As(III) and Sb(III) are determined in the organic phase. As(V) and Sb(V) remain in the aqueous layer. Total inorganic As and Sb are determined after the reduction of the pentavalent forms with sodium thiosulphate. As(V) and Sb(V) are calculated by difference. The detection limits are 0.01 and 0.05 µg L - 1 for As(III) and Sb(III), respectively, with an enrichment factor of 115. The relative standard deviation is in the 2.9-4.5% range. The procedure has been applied to the speciation of inorganic As and Sb in bottled, tap and sea water samples with satisfactory results.

  7. Determination of macro and trace elements in multivitamin dietary supplements by high-resolution continuum source graphite furnace atomic absorption spectrometry with slurry sampling.

    PubMed

    Krawczyk, Magdalena

    2014-01-01

    In this research, three different commercially available multivitamin dietary supplements were analyzed by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GFAAS) with slurry sampling. The concentrations of Cr, Cu, Fe, Mn, and Se were determined and compared to the amounts stated by producers. The safety of multivitamin dietary supplements depends on various factors including the manufacturing process and the purity and origins of the raw ingredients. For this reason, this research determined concentrations of several toxic elements (As, Cd, and Pb). Microwave-assisted high pressure Teflon bomb digestion was used to determine total amounts of elements in samples. Samples were prepared as slurries at a concentration of 0.1% (m/v) for macro elements (Cr, Cu, Fe, Mn, and Se) and at a concentration of % (m/v) for trace elements (As, Cd, and Pb) in acidic media (3M HNO3). The influence of acid concentration, Triton X-100 addition, sonication time, and sonication power on absorbance was investigated. The accuracy of this method was validated by analyses of NRCC LUTS-1 (Lobster hepatopancreas), NRCC DORM-1 (Dogfish Muscle), NRCC DOLT-2 (Dogfish Liver), NBS SRM 1570 (Spinach Leaves) and NBS SRM 1573 (Tomato Leaves) certified reference materials. The measured elements contents in these reference materials (except NRCC DOLT-2) were in satisfactory agreement with the certified values according to the t-test for a 95% confidence level. PMID:24176741

  8. Direct determination of phosphorus in different food samples by means of solid sampling electrothermal atomic absorption spectrometry using Pd+Ca chemical modifier

    NASA Astrophysics Data System (ADS)

    Coşkun, Nihat; Akman, Süleyman

    2005-03-01

    In this study, direct determination of phosphorus in different food samples (milk powder, banana, and dried banana) and in various standard reference materials (apple leaves, bovine liver, pine needles) using solid sampling electrothermal atomic absorption spectrometry was investigated. Aqueous standards were used for all determinations. 5 μg Pd+5 μg Ca modifier mixture was used in all experiments. Pyrolysis temperature and atomization temperature were 1100 °C and 2500 °C, respectively. High background was reduced by applying a cool-down step in the furnace program. The accuracy of solid sampling results was checked by determination of the phosphorus content after dissolving samples. There was no significant error between results found by solid sampling and solution techniques. In addition solid certified materials were investigated. There were no significant differences between the phosphorus content of CRM and results obtained. The limit of detection, based on three times the standard deviation was 0.018 μg P.

  9. Validation and application of cavity-enhanced, near-infrared tunable diode laser absorption spectrometry for measurements of methane carbon isotopes at ambient concentrations.

    PubMed

    Mortazavi, Behzad; Wilson, Benjamin J; Dong, Feng; Gupta, Manish; Baer, Doug

    2013-10-15

    Methane is an effective greenhouse gas but has a short residence time in the atmosphere, and therefore, reductions in emissions can alleviate its greenhouse gas warming effect within a decadal time frame. Continuous and high temporal resolution measurements of methane concentrations and carbon isotopic ratios (δ(13)CH4) can inform on mechanisms of formation, provide constraints on emissions sources, and guide future mitigation efforts. We describe the development, validation, and deployment of a cavity-enhanced, near-infrared tunable diode laser absorption spectrometry system capable of quantifying δ(13)CH4 at ambient methane concentrations. Laboratory validation and testing show that the instrument is capable of operating over a wide dynamic range of methane concentration and provides a measurement precision for δ(13)CH4 of better than ± 0.5 ‰ (1σ) over 1000 s of data averaging at ambient methane concentrations. The analyzer is accurate to better than ± 0.5 ‰, as demonstrated by measurements of characterized methane/air samples with minimal dependence (<1 ‰) of measured carbon isotope ratio on methane concentration. Deployment of the instrument at a marsh over multiple days demonstrated how methane fluxes varied by an order of magnitude over 2 day deployment periods, and showed a 17 ‰ variability in δ(13)CH4 of the emitted methane during the growing season. PMID:24025121

  10. Determination of arsenobetaine, arsenocholine, and tetramethylarsonium cations in seafoods and human urine by high-performance liquid chromatography - thermochemical hydride generation - atomic absorption spectrometry

    SciTech Connect

    Momplaisir, G.M.; Blais, J.S.; Quinteiro, M.; Marshall, W.D. )

    1991-08-01

    A simple method was developed for the determination of arsonium compounds in edible marine tissues (lobster tail muscle, peeled deveined shrimp, cod fillet, and cod liver oil) and human urine. The homogenized marine tissue (5-10 g (or an equivalent weight of freeze-dried powder)) was blended with methanol; the extracts were combined and flash evaporated. Alternatively, urine (5 mL) was diluted with 50 mL of ethanol and placed in a dry ice-acetone bath for 20 min. Supernatant was separated from the resulting precipitate by centrifugation and flash evaporated. Residues from either sample type were resuspended in water, filtered through an anion exchanger, and acidified. The arsonium analytes were partitioned into liquefied phenol, which was diluted with diethyl ether and back extracted with water. The combined water extracts were taken to dryness, redissolved in methanol, concentrated to 1 mL, and separated on a cyanopropyl bonded-phase column using a methanolic mobile phase containing 19% (v/v) diethyl ether, 1% (v/v) acetic acid, 0.12% (v/v) triethylamine, and pricrylsulfonic acid (0.200 g/L). Analytes were detected on-line by thermochemical hydride generation-atomic absorption spectrometry. Recoveries from tissues or from urine which had been spiked at 0.1-3.4 {mu}g of cation/g of fresh weight were 83% or greater from each of the five sample types.

  11. Development of a simple method for the determination of lead in lipstick using alkaline solubilization and graphite furnace atomic absorption spectrometry.

    PubMed

    Soares, Aline Rodrigues; Nascentes, Clésia Cristina

    2013-02-15

    A simple method was developed for determining the total lead content in lipstick samples by graphite furnace atomic absorption spectrometry (GFAAS) after treatment with tetramethylammonium hydroxide (TMAH). Multivariate optimization was used to establish the optimal conditions of sample preparation. The graphite furnace heating program was optimized through pyrolysis and atomization curves. An aliquot containing approximately 50mg of the sample was mixed with TMAH and heated in a water bath at 60°C for 60 min. Using Nb as the permanent modifier and Pd as the chemical modifier, the optimal temperatures were 900°C and 1800°C for pyrolysis and atomization, respectively. Under optimum conditions, the working range was from 1.73 to 50.0 μg L(-1), with detection and quantification limits of 0.20 and 0.34 μg g(-1), respectively. The precision was evaluated under conditions of repeatability and intermediate precision and showed standard deviations of 2.37%-4.61% and 4.93%-9.75%, respectively. The % recovery ranged from 96.2% to 109%, and no significant differences were found between the results obtained using the proposed method and the microwave decomposition method for real samples. Lead was detected in 21 tested lipstick samples; the lead content in these samples ranged from 0.27 to 4.54 μg g(-1). PMID:23598019

  12. Development of an ultrasonic slurry sampling method for the determination of Cu and Mn in antibiotic tablets by electrothermal atomic absorption spectrometry.

    PubMed

    de Paula, Carlos Eduardo R; Caldas, Luiz Fernando S; Brum, Daniel M; Cassella, Ricardo J

    2012-07-01

    A new method is described for simple, efficient and rapid determination of Cu and Mn in tablets of antibiotics (ciprofloxacin and cephalexin) by electrothermal atomic absorption spectrometry (ETAAS) using slurry sampling. In order to optimize the procedure, several variables that could affect the performance of the method were investigated. In the best conditions, the tablets could be analyzed by introducing into the graphite tube 20 μl of a slurry prepared with approximately 90-100mg of the sample and 2 ml of a solution containing 5% m/v of Triton X-114 and 2.8 M of HNO(3). Before the introduction, the slurries were sonicated for 15 min at 40% of amplitude (130 W maximum power) with an ultrasonic probe. The developed method was applied in the determination of Cu and Mn in four samples, and the results were compared with those obtained by focused microwave acid digestion with aqua regia (1:3 mixture of HNO(3):HCl). There was no statistical difference between the obtained values at 95% confidence level when a paired Student t-test was applied. PMID:22542826

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

    PubMed

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

    2012-10-30

    A new method for the speciation of Cr(VI) and Cr(III) based on enhancement effect of room temperature ionic liquids (RTILs) for hollow fiber liquid phase microextraction (HF-LPME) combined with flame atomic absorption spectrometry (FAAS) was developed. Room temperature ionic liquids (RTILs) and diethyldithiocarbamate (DDTC) were used enhancement reagents and chelating reagent, respectively. The addition of room temperature ionic liquids led to 3.5 times improvement in the determination of Cr(VI). In this method, Cr(VI) reacts with DDTC yielding a hydrophobic complex, which is subsequently extracted into the lumen of hollow fiber, whereas Cr(III) is remained in aqueous solutions. The extraction organic phase was injected into FAAS for the determination of Cr(VI). Total Cr concentration was determined after oxidizing Cr(III) to Cr(VI) in the presence of KMnO(4) and using the extraction procedure mentioned above. Cr(III) was calculated by subtracting of Cr(VI) from the total Cr. Under optimized conditions, a detection limit of 0.7 ng mL(-1) and an enrichment factor of 175 were achieved. The relative standard deviation (RSD) was 4.9% for Cr(VI) (40 ng mL(-1), n=5). The proposed method was successfully applied to the speciation of chromium in natural water samples with satisfactory results. PMID:22981284

  14. Ultrasound-assisted emulsification microextraction based on solidification floating organic drop trace amounts of manganese prior to graphite furnace atomic absorption spectrometry determination.

    PubMed

    Mohadesi, Alireza; Falahnejad, Masoumeh

    2012-01-01

    In the present study, an ultrasound-assisted emulsification microextraction based on solidification floating organic drop method is described for preconcentration of trace amounts of Mn (II). 2-(5-Bromo-2-pyridylazo)-5 diethylaminophenol was added to a solution of Mn(+2) at ph = 10.0. After this, 1-undecanol was added to the solution as an extraction solvent, and solution was stirred. Several factors influencing the microextraction efficiency, such as pH, the amount of chelating agent, nature and volume of extraction solvent, the volume of sample solution, stirring rate, and extraction time were investigated and optimized. Then sample vial was cooled by inserting into an ice bath, and the solidified was transferred into a suitable vial for immediate melting. Finally the sample was injected into a graphite furnace atomic absorption spectrometry. Under the optimum condition the linear dynamic range was 0.50-10.0 ng mL(-1) with a correlation coefficient of 0.9926, and the detection limit of 0.3 ng mL(-1) was obtained. The enrichment factor was 160. The proposed method was successfully applied for separation and determination of manganese in sea, rain, tap, and river water samples. PMID:22645504

  15. 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. PMID:20685458

  16. Ultrasound-assisted emulsification solidified floating organic drops microextraction of ultra trace amount of Te (IV) prior to graphite furnace atomic absorption spectrometry determination.

    PubMed

    Fathirad, Fariba; Afzali, Daryoush; Mostafavi, Ali; Ghanbarian, Maryam

    2012-01-15

    In the present study, a new, simple and efficient method for the preconcentration of ultra trace amounts of Te (IV) is developed using ultrasound-assisted emulsification solidified floating organic drops microextraction (USAE-SFODME) before graphite furnace atomic absorption spectrometry determination. In this method, tellurium is extracted into the fine droplets of 1-undecanol after chelate formation with the water soluble ligand, ammonium pyrrolidinedithiocarbamate (APDC). Several factors such as pH, chelating agent amount, type and volume of the extracting solvent, sonication and centrifuging time that influence the extraction and complex formation are optimized. Under the optimum conditions, the calibration graph is linear in the range of 0.01-0.24ngmL(-1) of tellurium in the original solution, with limit of detection of 0.003ngmL(-1). The relative standard deviation (RSD) for seven replicated determinations of tellurium ion at 0.08ngmL(-1) concentration level is calculated as 3.4%. The proposed method was successfully applied to the determination of Te (IV) in a standard soil and several water samples. PMID:22265571

  17. Green Preconcentration of Trace Amounts of Copper from Water and Food Samples onto Novel Organo-Nanoclay Prior to Flame Atomic Absorption Spectrometry.

    PubMed

    Beyki, Mostafa Hossein; Shemirani, Farzaneh; Khani, Rouhollah

    2014-01-01

    In this work, the nanoclay was intercalated with acyclovir (9-[(2-hydroxyethoxy) methyl] guanine), the toxicity of which to mammalian cells is very low. We used no organic solvents for preparation of modified clay and desorption of Cu ions from the sorbent. Batch and column methods were used, and sorption of Cu was quantitative (>98%) in the pH range of 7.5 to 10.0. Quantitative desorption occurred with 5.0 mL of 3.0 M HCl, and the amount of Cu(II) was measured by using flame atomic absorption spectrometry. In the initial solution the linear dynamic range and the LOD were 3.0-1000.0 and 0.58 μg/L, respectively. With 500.0 mL of sample, an enrichment factor of 100 was obtained. The RSD was 2.0% (n = 8, concentration = 0.5 mg/L), and the maximum capacity of the sorbent was 45.0 mg/g. The influence of experimental parameters including sample pH, ionic strength, type and volume of the eluent, and interference of some ions on the recoveries of Cu was investigated. The proposed method using a new and easier prepared solid sorbent was applied to the determination of Cu in different real samples with satisfactory results. PMID:25902995

  18. Solid sampling determination of lithium and sodium additives in microsamples of yttrium oxyorthosilicate by high-resolution continuum source graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Laczai, Nikoletta; Kovács, László; Péter, Ágnes; Bencs, László

    2016-03-01

    Solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry (SS-HR-CS-GFAAS) methods were developed and studied for the fast and sensitive quantitation of Li and Na additives in microsamples of cerium-doped yttrium oxyorthosilicate (Y2SiO5:Ce) scintillator materials. The methods were optimized for solid samples by studying a set of GFAAS conditions (i.e., the sample mass, sensitivity of the analytical lines, and graphite furnace heating programs). Powdered samples in the mass range of 0.099-0.422 mg were dispensed onto graphite sample insertion boats, weighed and analyzed. Pyrolysis and atomization temperatures were optimized by the use of single-element standard solutions of Li and Na (acidified with 0.144 mol/L HNO3) at the Li I 610.353 nm and Na I 285.3013 nm analytical lines. For calibration purposes, the method of standard addition with Li and Na solutions was applied. The correlation coefficients (R values) of the calibration graphs were not worse than 0.9678. The limit of detection for oxyorthosilicate samples was 20 μg/g and 80 μg/g for Li and Na, respectively. The alkaline content of the solid samples were found to be in the range of 0.89 and 8.4 mg/g, respectively. The accuracy of the results was verified by means of analyzing certified reference samples, using methods of standard (solution) addition calibration.

  19. Investigation of novel rapidly synergistic cloud point extraction pattern for bismuth in water and geological samples coupling with flame atomic absorption spectrometry determination

    NASA Astrophysics Data System (ADS)

    Wen, Xiaodong; Zhao, Yu; Deng, Qingwen; Ji, Shoulian; Zhao, Xia; Guo, Jie

    2012-04-01

    Rapidly synergistic cloud point extraction (RS-CPE) greatly simplified and accelerated the procedure of traditional cloud point extraction (CPE). In order to expand the application of RS-CPE, this work was carried out after the establishment of the improved extraction technique. The new established extraction method was firstly applied for bismuth extraction and determination coupled with flame atomic absorption spectrometry (FAAS) in this work. The improved RS-CPE was accomplished in the room temperature in 1 min. Non-ionic surfactant Triton X-100 (TX-100) was used as extractant. Octanol worked as cloud point revulsant and synergic reagent. TX-100 has a relatively high cloud point temperature (CPT), which limited its application in CPE. In this work, TX-100 accomplished the RS-CPE procedure in room temperature successfully. The factors influencing RS-CPE, such as concentrations of reagents, pH, conditions of phase separation, effect of environmental temperatures, salt effect and instrumental conditions, were studied systematically. Under the optimal conditions, the limit of detection (LOD) for bismuth was 4.0 μg L-1, with sensitivity enhancement factor (EF) of 43. The proposed method greatly improved the sensitivity of FAAS for the determination of bismuth and was applied to the determination of trace bismuth in real and certified samples with satisfactory analytical results. The proposed method was rapid, simple, and sensitive.

  20. Direct determination of arsenic and antimony in naphtha by electrothermal atomic absorption spectrometry with microemulsion sample introduction and iridium permanent modifier.

    PubMed

    Cassella, Ricardo J; Barbosa, Bruno Alberto R S; Santelli, Ricardo E; Rangel, Alessandra T

    2004-05-01

    This paper reports the determination of arsenic and antimony in naphtha by employing electrothermal atomic absorption spectrometry (ETAAS) as the analytical technique. In order to promote the direct determination of the analytes in the very volatile naphtha, the formation of a microemulsion with different surfactants (Triton X-100 and Brij-35) and different chemical modification strategies were tested. The results indicated that Triton X-100 is the best emulsification agent for naphtha in both As and Sb determination when it is employed at a concentration of 1% w/v in the microemulsion. Under these conditions, the microemulsion was stabile for at least 2 h. By using Brij-35 it was possible to achieve good stability only in the first 15 min. Among all chemical modification approaches investigated (Ir permanent modifier, W-Ir permanent modifier, and Pd modifier), the Ir permanent modifier provided better sensitivity for both analytes and allowed a higher pyrolysis temperature, which decreased the background signals at lower levels. Under the best conditions established in this work, an RSD of 4.6% (20 microg L(-1)) and a detection limit of 2.7 microg L(-1) were observed for arsenic. For antimony, an RSD of 4.0% (20 microg L(-1)) and a detection limit of 2.5 microg L(-1) were obtained. The accuracy of the procedure was assessed by analyzing spiked samples of naphtha from different origins. PMID:14985916

  1. Solid phase chelating extraction and separation of inorganic antimony species in pharmaceutical and water samples for graphite furnace atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Zih-Perényi, Katalin; Jankovics, Péter; Sugár, Éva; Lásztity, Alexandra

    2008-03-01

    A separation procedure for antimony(III) and antimony(V) was developed with the use of chelating celluloses. Sb(III) was separately pre-concentrated on imino diacetic acid-ethyl cellulose in the acidic pH range, in which the uptake of Sb(V) was negligible in the μg L - 1 concentration range. On the other hand, both Sb species Sb(V) and Sb(III) were pre-concentrated on a chloride form of 2,2'-diaminodiethylamine-cellulose. These solid phase extraction procedures were combined with graphite furnace atomic absorption spectrometry (SPE-GFAAS) for Sb detection. Pharmaceutical compounds of organic and inorganic types (ten compounds), as well as mineral water samples (twelve types) were analyzed. Detection limits of 0.18 µg L - 1 Sb(III) and 0.25 µg L - 1 Sb(V) were found in aqueous sample solutions and water samples, respectively, considering a 25-fold pre-concentration. The total Sb, mostly in the form of Sb(V), could be determined in phosphate-containing pharmaceuticals, while in phosphoric acid, Sb(III) was the dominant form. In all other types of samples the Sb content was below the detection threshold, and therefore, the potential suitability of the SPE-GFAAS method for the determination of Sb(III) species was proven by recovery tests of spiked samples. This method ensures the required detection power with regard to the allowable Sb limits established by international organizations.

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

    PubMed

    Wang, Zheng; Fang, Dong-Mei; Li, Qing; Zhang, Ling-Xia; Qian, Rong; Zhu, Yan; Qu, Hai-Yun; Du, Yi-Ping

    2012-05-01

    A modified SBA-15 mesoporous silica material NH(2)-SBA-15 was synthesized successfully by grafting γ-aminopropyl-triethoxysilane. The material was characterized using transmission electron microscopy (TEM) and Fourier transform infrared/Raman (FT-IR/Raman) spectroscopy, and used for the first time in a flow injection on-line solid phase extraction (SPE) coupled with flame atomic absorption spectrometry (FAAS) to detect trace Cr (VI). Effective sorption of Cr (VI) was achieved at pH 2.0 with no interference from Cr (III) and other ions and 0.5 mol L(-1) NH(3)·H(2)O solution was found optimal for the complete elution of Cr (VI). An enrichment factor of 44 and was achieved under optimized experimental conditions at a sample loading of 2.0 mL min(-1) sample loading (300 s) and an elution flow rate of 2.0 mL min(-1) (24s). The precision of the 11 replicate Cr (VI) measurements was 2.1% at the 100 μg L(-1) level with a detection limit of 0.2 μg L(-1) (3s, n=10) using the FAAS. The developed method was successfully applied to trace chromium determination in waste water. The accuracy was validated using a certified reference material of riverine water (GBW08607). PMID:22502615

  3. Preparation of modified magnetic nanoparticles as a sorbent for the preconcentration and determination of cadmium ions in food and environmental water samples prior to flame atomic absorption spectrometry

    NASA Astrophysics Data System (ADS)

    Mirabi, Ali; Dalirandeh, Zeinab; Rad, Ali Shokuhi

    2015-05-01

    A new method has been developed for the separation/preconcentration of trace level cadmium ions using diphenyl carbazone/sodium dodecyl sulfate immobilized on magnetic nanoparticle Fe3O4 as a new sorbent SPE and their determination by flame atomic absorption spectrometry (FAAS). Synthesized nanoparticle was characterized by scanning electron microscope (SEM) and transmission electron microscope (TEM). Various influencing parameters on the separation and preconcentration of trace level cadmium ions such as, pH value, amount of nanoparticles, amount of diphenyl carbazone, condition of eluting solution, the effects of matrix ions were examined. The cadmium ions can be eluted from the modified magnetic nanoparticle using 1 mol L-1 HCl as a desorption reagent. The detection limit of this method for cadmium was 3.71 ng ml-1 and the R.S.D. was 0.503% (n=6). The advantages of this new method include rapidity, easy preparation of sorbents and a high concentration factor. The proposed method has been applied to the determination of Cd ions at trace levels in real samples such as, green tea, rice, tobacco, carrot, lettuce, ginseng, spice, tap water, river water, sea water with satisfactory results.

  4. 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. PMID:27283608

  5. An automated flow injection system for metal determination by flame atomic absorption spectrometry involving on-line fabric disk sorptive extraction technique.

    PubMed

    Anthemidis, A; Kazantzi, V; Samanidou, V; Kabir, A; Furton, K G

    2016-08-15

    A novel flow injection-fabric disk sorptive extraction (FI-FDSE) system was developed for automated determination of trace metals. The platform was based on a minicolumn packed with sol-gel coated fabric media in the form of disks, incorporated into an on-line solid-phase extraction system, coupled with flame atomic absorption spectrometry (FAAS). This configuration provides minor backpressure, resulting in high loading flow rates and shorter analytical cycles. The potentials of this technique were demonstrated for trace lead and cadmium determination in environmental water samples. The applicability of different sol-gel coated FPSE media was investigated. The on-line formed complex of metal with ammonium pyrrolidine dithiocarbamate (APDC) was retained onto the fabric surface and methyl isobutyl ketone (MIBK) was used to elute the analytes prior to atomization. For 90s preconcentration time, enrichment factors of 140 and 38 and detection limits (3σ) of 1.8 and 0.4μgL(-1) were achieved for lead and cadmium determination, respectively, with a sampling frequency of 30h(-1). The accuracy of the proposed method was estimated by analyzing standard reference materials and spiked water samples. PMID:27260436

  6. A Novel Method Using Solid-Phase Extraction with Slotted Quartz Tube Atomic Absorption Spectrometry for the Determination of Manganese in Walnut Samples.

    PubMed

    Bitirmis, Bedrana; Trak, Digdem; Arslan, Yasin; Kendüzler, Erdal

    2016-01-01

    Mn(2+) was separated and preconcentrated using both solid-phase extraction (SPE) and a slotted quartz tube (SQT), and detected by a flame atomic absorption spectrometry (FAAS) system. Firstly, Mn(2+) was retained on a column filled with Amberlite CG-120 resin, and then retained Mn(2+) ions on the Amberlite CG-120 resin eluted with 5 mL of 4 mol/L HNO3. This part was called the "first preconcentration step". Furthermore, to determine the Mn(2+) in a walnut sample, the SQT device was also used after the separation and preconcentration of Mn(2+) from the Amberlite CG-120 resin so as to further improve the sensitivity of system. This part was called the "second preconcentration step" in this study. The enrichment factor and limit of detection values were found to be 360 fold and 0.22 μg/L, in turn, after a two-step preconcentration method. The good accuracy of method was confirmed with the use of standard reference material (spinach leaves, NIST-1570a). PMID:27302588

  7. Study of the roles of chemical modifiers in determining boron using graphite furnace atomic absorption spectrometry and optimization of the temperature profile during atomization.

    PubMed

    Yamamoto, Yuhei; Shirasaki, Toshihiro; Yonetani, Akira; Imai, Shoji

    2015-01-01

    The measurement conditions for determining boron using graphite furnace-atomic absorption spectrometry (GF-AAS) were investigated. Differences in the boron absorbance profiles were found using three different commercially available GF-AAS instruments when the graphite atomizers in them were not tuned. The boron absorbances found with and without adjusting the graphite atomizers suggested that achieving an adequate absorbance for the determination of boron requires a sharp temperature profile that overshoots the target temperature during the atomization process. Chemical modifiers that could improve the boron absorbance without the need for using coating agents were tested. Calcium carbonate improved the boron absorbance but did not suppress variability in the peak height. Improvement of boron absorbance was comparatively less using iron nitrate or copper nitrate than using calcium carbonate, but variability in the peak height was clearly suppressed using iron nitrate or copper nitrate. The limit of detection was 0.0026 mg L(-1) when iron nitrate was used. It appears that iron nitrate is a useful new chemical modifier for the quick and simple determination of boron using GF-AAS. PMID:25958863

  8. Ultrasound-assisted ion-pair dispersive liquid-liquid microextraction of trace amounts of lead in water samples prior to graphite furnace atomic absorption spectrometry determination.

    PubMed

    Afzali, Daryoush; Mohadesi, Ali Reza; Falahnejad, Masoumeh; Bahadori, Behnoosh

    2013-01-01

    A new ion-pair dispersive liquid-liquid microextraction method is described for separation and preconcentration of trace amounts of lead in different water samples. Graphite furnace atomic absorption spectrometry was used for determination of lead. The ion association complex between lead and iodide ions that forms is PbI4(-2)-tetradecyl-dimethylbenzylammonium, which is extracted into fine droplets of chlorobenzene. In order to reach the optimized experimental conditions, the influence of different parameters, such as concentration of KI, nature and volume of extraction solvents, pH effect, extraction time, and the period and speed of sonication and centrifugation, were optimized. The LOD was 0.08 ng/mL and the linear dynamic range was 0.20-8.0 ng/mL in initial solution with a correlation coefficient of 0.9985. Under the optimum conditions, the enrichment factor was 555.5. The proposed method was successfully applied for separation and determination of lead in sea, rain, river, and drinking water samples. PMID:23513972

  9. Determination of Cu, Fe, Mn and Zn by flame atomic absorption spectrometry in multivitamin/multimineral dosage forms or tablets after an acidic extraction.

    PubMed

    Soriano, Sílvio; Netto, Annibal D Pereira; Cassella, Ricardo J

    2007-01-01

    This work presents the development of a methodology for the determination of Cu, Fe, Mn and Zn in samples of multivitamin/multimineral tablets, by flame atomic absorption spectrometry (FAAS), after extraction of the analytes with diluted hydrochloric acid solution. Several parameters that could influence the extraction process such as acid extraction solution concentration and nature, mixing mode (ultrasonic or magnetic stirring), extraction time and sample composition were evaluated. The obtained results showed that Fe, Mn and Zn were easily extracted with 1 mol/L HCl solution after 5 min of mixing with either ultrasonic or magnetic stirring for all studied samples. On the other hand, Cu extraction appeared to be more complex since it could only be extracted at the same conditions for silicate-free samples. For samples containing silicates the time of contact between solid sample and extraction solution presented remarkable influence, being necessary up to 12 h to achieve quantitative recovery with 1 mol/L HCl solution. The developed methodology was applied in the determination of Cu, Fe, Mn and Zn in seven commercially available multivitamin/multimineral tablets. The results obtained with the developed method were compared with those obtained after total digestion of samples using a closed-vessel microwave oven device. PMID:16842959

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

    PubMed

    Duran, Ali; Tuzen, Mustafa; Soylak, Mustafa

    2015-01-01

    This study proposes the application of multi-walled carbon nanotubes as a solid sorbent for the preconcentration of gold prior to its flame atomic absorption spectrometry determination. Extraction was achieved by using a glass column (15.0 cm in length and 1.0 cm in diameter). Quantitative recoveries were obtained in the pH range of 2.5-4.0; the elution step was carried out with 5.0 ml of 1.0 mol/L HNO3 in acetone. In the ligand-free study, variables such as pH, eluent type, sample volume, flow rates, and matrix effect were examined for the optimum recovery of gold ions. The gold ions were able to be pre-concentrated by a factor of 150 and their LOD was determined to be 1.71 μg/L. In order to evaluate the accuracy of the developed method, addition-recovery tests were applied for the tap water, mineral water, and sea water samples. Gold recovery studies were implemented using a wet digestion technique for mine and soil samples taken from various media, and this method was also applied for anodic slime samples taken from the factories located in the Kayseri Industrial Zone of Turkey. PMID:26651587

  11. Modular calibrant sets for the structural analysis of nucleic acids by ion mobility spectrometry mass spectrometry.

    PubMed

    Lippens, Jennifer L; Ranganathan, Srivathsan V; D'Esposito, Rebecca J; Fabris, Daniele

    2016-06-20

    This study explored the use of modular nucleic acid (NA) standards to generate calibration curves capable of translating primary ion mobility readouts into corresponding collision cross section (CCS) data. Putative calibrants consisted of single- (ss) and double-stranded (ds) oligo-deoxynucleotides reaching up to ∼40 kDa in size (i.e., 64 bp) and ∼5700 Å(2) in CCS. To ensure self-consistency among reference CCS values, computational data obtained in house were preferred to any experimental or computational data from disparate sources. Such values were obtained by molecular dynamics (MD) simulations and either the exact hard sphere scattering (EHSS) or the projection superposition approximation (PSA) methods, and then plotted against the corresponding experimental values to generate separate calibration curves. Their performance was evaluated on the basis of their correlation coefficients and ability to provide values that matched the CCS of selected test samples mimicking typical unknowns. The results indicated that the predictive power benefited from the exclusion of higher charged species that were more susceptible to the destabilizing effects of Coulombic repulsion. The results revealed discrepancies between EHSS and PSA data that were ascribable to the different approximations used to describe the ion mobility process. Within the boundaries defined by these approximations and the challenges of modeling NA structure in a solvent-free environment, the calibrant sets enabled the experimental determination of CCS with excellent reproducibility (precision) and error (accuracy), which will support the analysis of progressively larger NA samples of biological significance. PMID:27152369

  12. Determination of trace metals in urine with an on-line ultrasound-assisted digestion system combined with a flow-injection preconcentration manifold coupled to flame atomic absorption spectrometry.

    PubMed

    Cespón-Romero, R M; Yebra-Biurrun, M C

    2008-02-25

    A flow analysis method with on-line sample digestion/minicolumn preconcentration/flame atomic absorption spectrometry is described for the determination of trace metals in urine. First, urine sample was on-line ultrasound-assisted digested exploiting the stopped-flow mode, and then the metals were preconcentrated passing the pre-treated sample through a minicolumn containing a chelating resin. A home-made minicolumn of commercially available imminodiacetic functional group resin, Chelite Che was used to preconcentrate trace metals (Cu, Fe, Mn and Ni) from urine. The proposed procedure allowed the determination of the metals with detection limits of 0.5, 1.1, 0.8 and 0.8microgL(-1), for Cu, Fe, Mn and Ni, respectively. The precision based on replicate analysis was less than +/-10.0%, and the enrichment factor obtained was between 21.3 (Mn) and 44.1 (Ni), for sample volumes between 2.5 and 5.0mL, and an eluent volume of 110microL. This procedure was applied for determination of metals in urine of workers exposed to welding fumes and urine of unexposed persons (urine control). PMID:18261513

  13. Analysis of absorption performances of anechoic layers with steel plate backing.

    PubMed

    Meng, Hao; Wen, Jihong; Zhao, Honggang; Lv, Linmei; Wen, Xisen

    2012-07-01

    Rubber layers with air-filled cavities or local resonance scatters can be used as anechoic coatings. A lot of researches have focused on the absorption mechanism of the anechoic coatings. As the anechoic coatings are bonded to the hull of submarine, the vibration of the hull should not be neglected when the analysis of the absorption characters is carried out. Therefore, it is more reasonable to treat the anechoic coating and the backing as a whole when the acoustic performance is analyzed. Considering the effects of the steel plate backing, the sound absorption performances on different models of anechoic coatings are investigated in this paper. The Finite Element Method is used to illustrate the vibrational behaviors of the anechoic coatings under the steel backings by which the displacement contours is obtained for analysis. The theoretical results show that an absorption peak is induced by the resonance of the steel slab and rubber layer. At the frequency of this absorption peak, the steel plate and the coating vibrates longitudinally like a mass-spring system in which the steel slab serves for mass and the coating layer is the spring. To illuminate the effects of the steel slab backing on the acoustic absorption, the thicknesses of the steel slab and the anechoic layer are discussed. Finally, an experiment is performed and the results show a good agreement with the theoretical analysis. PMID:22779456

  14. Application of Derivative Spectrometry to the Analysis of Trace Gases

    NASA Technical Reports Server (NTRS)

    Hager, Robert N.

    1971-01-01

    A derivative spectrometer is sensitive to changes in spectral intensity over narrow wavelength internal. Specifically, a second derivative spectrometer senses the curvature of the incident spectral intensity, providing an output voltage signal proportional to the second derivative of intensity with respect to wavelength. When such an instrument is combined with multi-pass White cell, a unique trace gas analyzer results. The analyzer, operating within the middle ultraviolet spectral region, provides a highly amplified derivative spectrum of any molecular narrow band absorption which is used for trace gas identification. The intensity of any peak within a spectrum is proportional to the trace gas concentration. Such an analyzer, utilizing a 20 meter pathlength White cell, is presently being used to automatically monitor ambient air for SO2, NO, NO2, and O3 with minimum detectable concentration limits in the part per billion range.

  15. Multiresidue analysis of pesticides in straw roughage by liquid chromatography - tandem mass spectrometry

    Technology Transfer Automated Retrieval System (TEKTRAN)

    A multiresidue analytical method using a modification of the “quick, easy, cheap, effective, rugged, and safe” (QuEChERS) sample preparation approach combined with liquid chromatography–tandem mass spectrometry (LC-MS/MS) analysis was established and validated for the rapid determination of 69 pesti...

  16. Sugars, Stable Isotopes, and Spectrometry: New Methods for the Analysis of Carbohydrate Metabolism

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Structural analysis of carbohydrates involves three parameters: composition, linkage, and conformation, and tends to rely on the various forms of two techniques; mass spectrometry (MS) and nuclear magnetic resonance (NMR) spectroscopy. These techniques are enhanced and extended by the use of stable...

  17. ANALYSIS OF CHLORINATED HERBICIDES BY HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY/MASS SPECTROMETRY

    EPA Science Inventory

    A method that uses high performance liquid chromatography/mass spectrometry (HPLC/MS) for the analysis of chlorinated phenoxyacid herbicides is described. uring method development different techniques were used to increase both the sensitivity and the specificity of thermospray H...

  18. GAS CHROMATOGRAPHY/MATRIX ISOLATION - INFRARED SPECTROMETRY FOR AIR SAMPLE ANALYSIS

    EPA Science Inventory

    This report describes the application of gas chromatography/matrix- solation infrared (GC/MI-IR) spectrometry to the analysIs of environmental air sample extracts. Samples that were analyzed include extracts from woodsmoke-impacted air, XAD-2 blanks, indoor air, and carpet sample...

  19. MALDI imaging mass spectrometry and analysis of endogenous peptides.

    PubMed

    Chatterji, Bijon; Pich, Andreas

    2013-08-01

    In recent years, MALDI imaging mass spectrometry (MALDI-IMS) has developed as a promising tool to investigate the spatial distribution of biomolecules in intact tissue specimens. Ion densities of various molecules can be displayed as heat maps while preserving anatomical structures. In this short review, an overview of different biomolecules that can be analyzed by MALDI-IMS is given. Many reviews have covered imaging of lipids, small metabolites, whole proteins and enzymatically digested proteins in the past. However, little is known about imaging of endogenous peptides, for example, in the rat brain, and this will therefore be highlighted in this review. Furthermore, sample preparation of frozen or formalin-fixed, paraffin-embedded (FFPE) tissue is crucial for imaging experiments. Therefore, some aspects of sample preparation will be addressed, including washing and desalting, the choice of MALDI matrix and its deposition. Apart from mapping endogenous peptides, their reliable identification in situ still remains challenging and will be discussed as well. PMID:23992420

  20. Quantitative analysis of terbutaline by gas chromatography-mass spectrometry.

    PubMed

    Leferink, J G; Baillie, T A; Lindberg, C

    1984-01-01

    Over the past 6 years, several gas chromatography-mass spectrometry (GC-MS) methods for terbutaline have been developed, each with certain advantages and disadvantages. They all involve monitoring of an ion selected from the mass spectrum of a suitable terbutaline derivative. This technique, often referred to as mass fragmentography or selected ion monitoring, reduces the interference from other drugs and endogenous compounds. Different ionization techniques have been employed to obtain high sensitivity, viz. electron impact and chemical ionization. Typically, the methods can be used to measure terbutaline concentrations down to 0.1-0.3 ng/mL in plasma or serum. Isolation of terbutaline from biological materials is complicated by the low partition of the drug from water to organic solvents. Extraction with a large volume of ethyl acetate, ion pair extraction, or isolation on a cation exchange column have been used. These methods are time consuming, and attempts have therefore been made to modify them. Rapid extraction can be achieved on a disposable reversed-phase octadecylsilyl column with unimpaired sensitivity and selectivity. Preliminary results indicate that negative ion chemical ionization of a fluorine-containing derivative can further increase the sensitivity of the terbutaline assays. PMID:6586484