Science.gov

Sample records for antimony thiosemicarbazone precursors

  1. Antimony

    Integrated Risk Information System (IRIS)

    Antimony ; CASRN 7440 - 36 - 0 Human health assessment information on a chemical substance is included in the IRIS database only after a comprehensive review of toxicity data , as outlined in the IRIS assessment development process . Sections I ( Health Hazard Assessments for Noncarcinogenic Effects

  2. Antimony Toxicity

    PubMed Central

    Sundar, Shyam; Chakravarty, Jaya

    2010-01-01

    Antimony toxicity occurs either due to occupational exposure or during therapy. Occupational exposure may cause respiratory irritation, pneumoconiosis, antimony spots on the skin and gastrointestinal symptoms. In addition antimony trioxide is possibly carcinogenic to humans. Improvements in working conditions have remarkably decreased the incidence of antimony toxicity in the workplace. As a therapeutic, antimony has been mostly used for the treatment of leishmaniasis and schistosomiasis. The major toxic side-effects of antimonials as a result of therapy are cardiotoxicity (~9% of patients) and pancreatitis, which is seen commonly in HIV and visceral leishmaniasis co-infections. Quality control of each batch of drugs produced and regular monitoring for toxicity is required when antimonials are used therapeutically. PMID:21318007

  3. Alumina-supported bimetallics of palladium alloyed with germanium, tin, lead, or antimony from organometallic precursors I. Preparation and characterization

    SciTech Connect

    Aduriz, H.R.; Bodnariuk, P. , Bahia Blanca ); Coq, B.; Figueras, F. )

    1989-09-01

    Bimetallic PdSn, PdSb, PdPb, and PdGe on alumina catalysts with a low metal content have been prepared using either chloride or organometallic precursors. For the catalysts obtained from chloride precursors no interaction was observed between the two metals, and the catalysts behaved like pure Pd/Al{sub 2}O{sub 3}. In contrast, the reactions of (C{sub 4}H{sub 9}){sub 4}Sn, (C{sub 4}H{sub 9}){sub 4}Pb, (C{sub 4}H{sub 9}){sub 4}Ge, or (C{sub 4}H{sub 9}){sub 3}Sb in n-heptane solution with reduced Pd/Al{sub 2}O{sub 3} catalyst yielded a supported alloy. The interaction between metallic palladium and the organic modifier is highly selective and leads to the formation of a well-tailored bimetallic catalyst. When these final solids are reduced at 573 or 773 K, the second metal locates preferentially at the outer layer of the bimetallic aggregates. After reduction at 773 K large metallic aggregates are obtained (particle size 15 nm), and the formation of {beta}-palladium hydride, which can be formed with pure palladium catalysts, is suppressed by the addition of a small amount of the second metal. The specific activity of the palladium surface atoms for isoprene hydrogenation is then lowered, and the selectivity increased.

  4. Antimony trioxide

    Integrated Risk Information System (IRIS)

    Antimony trioxide ; CASRN 1309 - 64 - 4 Human health assessment information on a chemical substance is included in the IRIS database only after a comprehensive review of toxicity data , as outlined in the IRIS assessment development process . Sections I ( Health Hazard Assessments for Noncarcinogeni

  5. Recent advances on antimony(III/V) compounds with potential activity against tumor cells.

    PubMed

    Hadjikakou, S K; Ozturk, I I; Banti, C N; Kourkoumelis, N; Hadjiliadis, N

    2015-12-01

    Antimony one of the heavier pnictogens, has been in medical use against microbes and parasites as well. Antimony-based drugs have been prescribed against leishmaniasis since the parasitic transmission of the tropical disease was understood in the beginning of the 20th century. The activity of arsenic against visceral leishmaniasis led to the synthesis of an array of arsenic-containing parasitic agents, among them the less toxic pentavalent antimonials: Stibosan, Neostibosan, and Ureastibamine. Other antimony drugs followed: sodium stibogluconate (Pentostam) and melglumine antimoniate (Glucantim or Glucantime); both continue to be in use today despite their toxic side effects and increasing loss in potency due to the growing resistance of the parasite against antimony. Antimony compounds and their therapeutic potentials are under consideration from many research groups, while a number of early reviews recording advances of antimony biomedical applications are also available. However, there are only few reports on the screening for antitumor potential of antimony compounds. This review focuses upon results obtained on the anti-proliferative activity of antimony compounds in the past years. This survey shows that antimony(III/V) complexes containing various types of ligands such as thiones, thiosemicarbazones, dithiocarbamates, carboxylic acids, or ketones, nitrogen donor ligands, exhibit selectivity against a variety of cancer cells. The role of the ligand type of the complex is elucidated within this review. The complexes and their biological activity are already reported elsewhere. However quantitative structure-activity relationship (QSAR) modeling studies have been carried out and they are reported for the first time here. PMID:26092367

  6. Antimony: a flame fighter

    USGS Publications Warehouse

    Wintzer, Niki E.; Guberman, David E.

    2015-01-01

    In the 11th century, the word antimonium was used by medieval scholar Constantinus Africanus, but antimony metal was not isolated until the 16th century by Vannoccio Biringuccio, an Italian metallurgist. In the early 18th century, chemist Jons Jakob Berzelius chose the periodic symbol for antimony (Sb) based on stibium, which is the Latin name for stibnite.

  7. Oligosilanylated Antimony Compounds

    PubMed Central

    2015-01-01

    By reactions of magnesium oligosilanides with SbCl3, a number of oligosilanylated antimony compounds were obtained. When oligosilanyl dianions were used, either the expected cyclic disilylated halostibine was obtained or alternatively the formation of a distibine was observed. Deliberate formation of the distibine from the disilylated halostibine was achieved by reductive coupling with C8K. Computational studies of Sb–Sb bond energies, barriers of pyramidal inversion at Sb, and the conformational behavior of distibines provided insight for the understanding of the spectroscopic properties. PMID:25937691

  8. Extraction of antimony with tertiary amines.

    PubMed

    Alian, A; Sanad, W

    1967-06-01

    The extractability of antimony(III) and (V) with tridodecylamine from various aqueous solutions is reported. Extraction from nitric and hydrofluoric acid solutions is low, but extraction from sulphuric, hydrochloric and hydrobromic solutions is high. Antimony-(III) can be separated from antimony(V) in 7M nitric acid or 0.64M hydrobromic acid. The extraction of antimony from hydrochloric acid solutions in methanol, ethanol, and acetone-water mixtures is greater than from pure aqueous solutions of the same acidity. The elements from which antimony can be separated with tertiary amines are given. PMID:18960147

  9. Mineral Resource of the Month: Antimony

    USGS Publications Warehouse

    Guberman, David E.

    2015-01-01

    Antimony is a lustrous silvery-white semimetal or metalloid. Archaeological and historical studies indicate that antimony and its mineral sulfides have been used by humans for at least six millennia. The alchemist Basil Valentine is sometimes credited with “discovering” the element; he described the extraction of metallic antimony from stibnite in his treatise “The Triumphal Chariot of Antimony,” published sometime between 1350 and 1600. In the early 18th century, Jöns Jakob Berzelius chose the periodic symbol for antimony (Sb) based on stibium, which is the Latin name for stibnite.

  10. Alumina-supported bimetallics of palladium alloyed with germanium, tin, lead, or antimony from organometallic precursors. II. Gas-phase hydrogenation of 2-methyl-1-buten-3-yne (valylene) and 2-methyl-1,3-butadiene (isoprene)

    SciTech Connect

    Aduriz, H.R.; Bodnariuk, P. ); Coq, B.; Figueras, F. )

    1991-05-01

    A series of PdGe, PdSb, PdSn, and PdPb/{alpha}{minus}Al{sub 2}O{sub 3} catalysts, prepared by the controlled surface reaction (CSR) technique from organometallic precursors have been tested in the gas-phase hydrogenation of 2-methyl-1-buten-3-yne (valylene) and 2-methyl-1,3-butadiene (isoprene). On catalysts reduced at 573 K, the turnover frequencies for valylene (TON{sub v}) and isoprene (TON{sub 1}) hydrogenation were not modified by addition to the 0.09wt% Pd/{alpha}{minus}Al{sub 2}O{sub 3} base catalyst of Ge, Sb, Sn, or Pb, up to0.1 wt% (at 293 K: TON{sub v}= 20 s{sup {minus}1} and TON{sub 1} = 33 s{sup {minus}1}). Pd/{alpha}{minus}Al{sub 2}O{sub 3} reduced at 773 K was severely sintered (d{sub TEM} increased from 2.8nm to 12.4nm) and TON{sub v} and TON{sub 1} at 293 K increased to 190 and 283 s{sup {minus}1}, respectively, as a result of an apparent crystal size effect: the reactants adsorb more strongly on the smaller Pd particles. Upon alloying with Ge, Sb, Sn, or Pb and a subsequent reduction at 773 K, a modest decrease of both TON{sub v} (by a factor of 2) and TON{sub 1} (by a factor of 2{minus}5) was observed. At high conversion, both the selectivity to isoprene (S{sub I}) in valylene hydrogenation, and to olefins (S{sub 0}) in isoprene hydrogenation on Pd/{alpha}{minus}Al{sub 2}O{sub 3} were improved upon alloying with Sb, Sn, or Pb (Ge had no effect). In addition, the isomerization of 2-methyl-1-butene and 3-methyl-1-butene (double bond migration reaction) during isoprene hydrogenation was partially suppressed on PdSn and PdPb/{alpha}{minus}Al{sub 2}O{sub 3}. The improvement in selectivities was interpreted in terms of a change in the relative adsorption strength of the reactants and intermediate products over the new bimetallic sites.

  11. 40 CFR 421.140 - Applicability: Description of the primary antimony subcategory.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... primary antimony subcategory. 421.140 Section 421.140 Protection of Environment ENVIRONMENTAL PROTECTION... CATEGORY Primary Antimony Subcategory § 421.140 Applicability: Description of the primary antimony... antimony at primary antimony facilities....

  12. 40 CFR 421.140 - Applicability: Description of the primary antimony subcategory.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... primary antimony subcategory. 421.140 Section 421.140 Protection of Environment ENVIRONMENTAL PROTECTION... CATEGORY Primary Antimony Subcategory § 421.140 Applicability: Description of the primary antimony... antimony at primary antimony facilities....

  13. 40 CFR 421.140 - Applicability: Description of the primary antimony subcategory.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... primary antimony subcategory. 421.140 Section 421.140 Protection of Environment ENVIRONMENTAL PROTECTION... CATEGORY Primary Antimony Subcategory § 421.140 Applicability: Description of the primary antimony... antimony at primary antimony facilities....

  14. Observations on the measurement of total antimony and antimony species in algae, plant and animal tissues.

    PubMed

    Foster, S; Maher, W; Krikowa, F; Telford, K; Ellwood, M

    2005-12-01

    This paper describes our experiences with undertaking measurements of total antimony and antimony speciation in algae, plant and animal tissues. Digestion with nitric acid alone is suitable to release antimony from animal tissues. When organisms have high silica contents, e.g. some plants and algae, the addition of tetrafluorboric acid is required to dissolve silica as some antimony is retained by silica in extracts. Antimony in digested extracts is present as Sb5+ and hydride generation procedures can be used to determine total antimony concentrations, as total antimony in extracts will not be under estimated. Relatively non-aggressive solvents such as water, dilute nitric acid, sodium hydroxide and enzymes remove highly variable amounts of antimony (2-84%) from algae, plant and animal tissues. Addition of Sb3+ and Sb5+ to NIST CRM 1572 Citrus Leaves, pre- and post-extraction with water showed that Sb3+ is oxidised to Sb5+ while Sb5+ is redistributed amongst binding sites giving rise to artefacts. DOLT-2 and algae extracts indicated the presence of only inorganic antimony. A moss sample had inorganic antimony and a number of unknown antimony species in extracts. Future studies should explore the nature of the binding of antimony in tissues as solvents commonly used to extract metals and metalloids from algae, plant and animal tissues are not appropriate. PMID:16307074

  15. Antiretroviral activity of thiosemicarbazone metal complexes.

    PubMed

    Pelosi, Giorgio; Bisceglie, Franco; Bignami, Fabio; Ronzi, Paola; Schiavone, Pasqualina; Re, Maria Carla; Casoli, Claudio; Pilotti, Elisabetta

    2010-12-23

    Thiosemicarbazones display a wide antimicrobial activity by targeting bacteria, fungi, and viruses. Here, we report our studies on the antiviral activity of two thiosemicarbazone metal complexes, [bis(citronellalthiosemicarbazonato)nickel(II)] and [aqua(pyridoxalthiosemicarbazonato)copper(II)] chloride monohydrate, against the retroviruses HIV-1 and HTLV-1/-2. Both compounds exhibit antiviral properties against HIV but not against HTLVs . In particular, the copper complex shows the most potent anti-HIV activity by acting at the post-entry steps of the viral cycle. PMID:21121632

  16. Mineral resource of the month: antimony

    USGS Publications Warehouse

    U.S. Geological Survey

    2008-01-01

    The article describes the characteristics and industrial uses of antimony. Antimony, which is produced as a byproduct of mining other metals such as gold, lead or silver, is used in everything from flame retardants, batteries, ceramics and glass. It is also used in glass for television picture tubes, computer monitors, pigments and catalysts.

  17. ANTIMONY REMOVAL TECHNOLOGY FOR MINING INDUSTRY WASTEWATERS

    EPA Science Inventory

    This report assessed the current state-of-the-art of antimony removal technology for mining industry wastewaters. Through literature review and personal interviews, it was found that most mines and mills reporting significant quantities of antimony in their raw wastewater had app...

  18. 21 CFR 862.3110 - Antimony test system.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 21 Food and Drugs 8 2013-04-01 2013-04-01 false Antimony test system. 862.3110 Section 862.3110....3110 Antimony test system. (a) Identification. An antimony test system is a device intended to measure antimony, a heavy metal, in urine, blood, vomitus, and stomach contents. Measurements obtained by...

  19. 21 CFR 862.3110 - Antimony test system.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 21 Food and Drugs 8 2011-04-01 2011-04-01 false Antimony test system. 862.3110 Section 862.3110....3110 Antimony test system. (a) Identification. An antimony test system is a device intended to measure antimony, a heavy metal, in urine, blood, vomitus, and stomach contents. Measurements obtained by...

  20. 21 CFR 862.3110 - Antimony test system.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 21 Food and Drugs 8 2012-04-01 2012-04-01 false Antimony test system. 862.3110 Section 862.3110....3110 Antimony test system. (a) Identification. An antimony test system is a device intended to measure antimony, a heavy metal, in urine, blood, vomitus, and stomach contents. Measurements obtained by...

  1. 21 CFR 862.3110 - Antimony test system.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 21 Food and Drugs 8 2014-04-01 2014-04-01 false Antimony test system. 862.3110 Section 862.3110....3110 Antimony test system. (a) Identification. An antimony test system is a device intended to measure antimony, a heavy metal, in urine, blood, vomitus, and stomach contents. Measurements obtained by...

  2. 21 CFR 862.3110 - Antimony test system.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Antimony test system. 862.3110 Section 862.3110....3110 Antimony test system. (a) Identification. An antimony test system is a device intended to measure antimony, a heavy metal, in urine, blood, vomitus, and stomach contents. Measurements obtained by...

  3. Antimony and silicon environments in antimony silicate glasses

    SciTech Connect

    Mee, M.; Davies, B.C.; Orman, R.G.; Thomas, M.F.; Holland, D.

    2010-09-15

    Antimony silicate glasses, of general formula xSb{sub 2}O{sub 3}.(1-x)SiO{sub 2} (0.1{<=}x{<=}0.78), have been prepared by melt-quenching and their structures studied using {sup 29}Si MAS NMR spectroscopy, {sup 121}Sb Moessbauer spectroscopy and Raman spectroscopy. Oxidation during melting gives rise to Sb{sup 5+} in concentrations, which increase linearly with x to give a value of {approx}10% when x=0.78. {sup 121}Sb Moessbauer spectra show Moessbauer shifts and quadrupole splittings consistent with Sb{sup 3+} in a [:SbO{sub 3}] trigonal pyramid, similar to that in crystalline Sb{sub 2}O{sub 3}. A broad band in the Raman spectrum at {approx}410 cm{sup -1} is due to the vibrations of such a unit. The dependence of the silicon Q{sup n} speciation on x can be interpreted by the formation of Sb-O-Sb links possibly to form rings of 4 [:SbO{sub 3}] units such as are found in valentinite. - Graphical abstract: Antimony silicate glasses have been shown to contain Sb{sup 3+} in [:SbO{sub 3}] trigonal pyramid units using {sup 121}Sb Moessbauer spectroscopy and Raman spectroscopy. {sup 29}Si magic-angle-spinning NMR has shown silicon Q{sup n} speciation which can be interpreted as formation of rings of 4 [:SbO{sub 3}] units such as are found in valentinite.

  4. Antimony-doped graphene nanoplatelets

    PubMed Central

    Jeon, In-Yup; Choi, Min; Choi, Hyun-Jung; Jung, Sun-Min; Kim, Min-Jung; Seo, Jeong-Min; Bae, Seo-Yoon; Yoo, Seonyoung; Kim, Guntae; Jeong, Hu Young; Park, Noejung; Baek, Jong-Beom

    2015-01-01

    Heteroatom doping into the graphitic frameworks have been intensively studied for the development of metal-free electrocatalysts. However, the choice of heteroatoms is limited to non-metallic elements and heteroatom-doped graphitic materials do not satisfy commercial demands in terms of cost and stability. Here we realize doping semimetal antimony (Sb) at the edges of graphene nanoplatelets (GnPs) via a simple mechanochemical reaction between pristine graphite and solid Sb. The covalent bonding of the metalloid Sb with the graphitic carbon is visualized using atomic-resolution transmission electron microscopy. The Sb-doped GnPs display zero loss of electrocatalytic activity for oxygen reduction reaction even after 100,000 cycles. Density functional theory calculations indicate that the multiple oxidation states (Sb3+ and Sb5+) of Sb are responsible for the unusual electrochemical stability. Sb-doped GnPs may provide new insights and practical methods for designing stable carbon-based electrocatalysts. PMID:25997811

  5. Speciation of antimony in polyethylene terephthalate bottles

    SciTech Connect

    Martin, R.R.; Ablett, J.; Shotyk, W.S.; Naftel, S.; Northrup, P.

    2009-12-18

    Antimony contamination has been reported in drinking water from polyethylene terephthalate (PET) bottles. Micro-X-ray fluorescence (XRF) analysis has been used to identify the distribution and chemical form of residual antimony used as a catalyst in the manufacture of PET bottles. The results are consistent with clusters of Sb(III) having dimensions of the order of tens of micrometers, clearly showing the ability of synchrotron radiation analyses to both map elemental distribution and determine oxidation state.

  6. Tricarbonyl (99m)Tc(i) and Re(i)-thiosemicarbazone complexes: synthesis, characterization and biological evaluation for targeting bacterial infection.

    PubMed

    Nayak, Dipak Kumar; Baishya, Rinku; Natarajan, Ramalingam; Sen, Tuhinadri; Debnath, Mita Chatterjee

    2015-09-28

    Methyl, ethyl and phenyl nitrofuryl thiosemicarbazone ligands (, and respectively) were radiolabeled with freshly prepared aqueous solution of a fac[(99m)Tc(CO)3(H2O)3](+) precursor. The radiochemical yield was around 98% as determined by thin layer chromatography and HPLC. The complexes exhibited substantial stability. The corresponding Re(i) complexes were prepared from a Re(CO)5Br precursor to understand the coordination behavior of the ligands against a tricarbonyl rhenium(i) precursor. The rhenium(i) complexes were characterized by means of IR, NMR and mass spectroscopic studies as well as by X-ray crystallography, and correlated with the technetium complexes by means of HPLC studies. Electrochemical reduction of monomeric Re(CO)3-complexes of nitrofuryl ethyl thiosemicarbazone was also studied using cyclic voltammetry. Biodistribution studies of (99m)Tc(CO)3-labeled thiosemicarbazones in rats intramuscularly infected with S. aureus exhibited substantial in vivo stability of the complex and moderate accumulation at the site of focal infection. PMID:26289802

  7. 40 CFR 721.1930 - Butanoic acid, antimony (3=) salt.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Butanoic acid, antimony (3=) salt. 721... Substances § 721.1930 Butanoic acid, antimony (3=) salt. (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance identified as butanoic acid, antimony (3=) salt (PMN...

  8. 40 CFR 721.1930 - Butanoic acid, antimony (3=) salt.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 31 2014-07-01 2014-07-01 false Butanoic acid, antimony (3=) salt. 721... Substances § 721.1930 Butanoic acid, antimony (3=) salt. (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance identified as butanoic acid, antimony (3=) salt (PMN...

  9. 40 CFR 721.1930 - Butanoic acid, antimony (3=) salt.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 32 2012-07-01 2012-07-01 false Butanoic acid, antimony (3=) salt. 721... Substances § 721.1930 Butanoic acid, antimony (3=) salt. (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance identified as butanoic acid, antimony (3=) salt (PMN...

  10. 40 CFR 721.1930 - Butanoic acid, antimony (3=) salt.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 31 2011-07-01 2011-07-01 false Butanoic acid, antimony (3=) salt. 721... Substances § 721.1930 Butanoic acid, antimony (3=) salt. (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance identified as butanoic acid, antimony (3=) salt (PMN...

  11. 40 CFR 721.1930 - Butanoic acid, antimony (3=) salt.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 32 2013-07-01 2013-07-01 false Butanoic acid, antimony (3=) salt. 721... Substances § 721.1930 Butanoic acid, antimony (3=) salt. (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance identified as butanoic acid, antimony (3=) salt (PMN...

  12. 40 CFR 721.10713 - Antimony tris(dialkyldithiocarbamate) (generic).

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 31 2014-07-01 2014-07-01 false Antimony tris(dialkyldithiocarbamate... Specific Chemical Substances § 721.10713 Antimony tris(dialkyldithiocarbamate) (generic). (a) Chemical... as antimony tris(dialkyldithiocarbamate) (PMN P-13-259) is subject to reporting under this...

  13. 40 CFR 721.10712 - Antimony tris(dialkyldithiocarbamate) (generic).

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 31 2014-07-01 2014-07-01 false Antimony tris(dialkyldithiocarbamate... Specific Chemical Substances § 721.10712 Antimony tris(dialkyldithiocarbamate) (generic). (a) Chemical... as antimony tris(dialkyldithiocarbamate) (PMN P-13-217) is subject to reporting under this...

  14. 40 CFR 721.5547 - Antimony double oxide.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 32 2013-07-01 2013-07-01 false Antimony double oxide. 721.5547... Substances § 721.5547 Antimony double oxide. (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substances identified generically as antimony double oxide (PMNs P-95-677 and...

  15. 40 CFR 721.5547 - Antimony double oxide.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 31 2011-07-01 2011-07-01 false Antimony double oxide. 721.5547... Substances § 721.5547 Antimony double oxide. (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substances identified generically as antimony double oxide (PMNs P-95-677 and...

  16. 40 CFR 721.5547 - Antimony double oxide.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 32 2012-07-01 2012-07-01 false Antimony double oxide. 721.5547... Substances § 721.5547 Antimony double oxide. (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substances identified generically as antimony double oxide (PMNs P-95-677 and...

  17. 40 CFR 721.5547 - Antimony double oxide.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 31 2014-07-01 2014-07-01 false Antimony double oxide. 721.5547... Substances § 721.5547 Antimony double oxide. (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substances identified generically as antimony double oxide (PMNs P-95-677 and...

  18. 40 CFR 721.5547 - Antimony double oxide.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Antimony double oxide. 721.5547... Substances § 721.5547 Antimony double oxide. (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substances identified generically as antimony double oxide (PMNs P-95-677 and...

  19. Mononuclear ruthenium(III) complexes containing chelating thiosemicarbazones: Synthesis, characterization and catalytic property

    NASA Astrophysics Data System (ADS)

    Raja, N.; Ramesh, R.

    2010-02-01

    Mononuclear ruthenium(III) complexes of the type [RuX(EPh 3) 2(L)] (E = P or As; X = Cl or Br; L = dibasic terdentate dehydroacetic acid thiosemicarbazones) have been synthesized from the reaction of thiosemicarbazone ligands with ruthenium(III) precursors, [RuX 3(EPh 3) 3] (where E = P, X = Cl; E = As, X = Cl or Br) and [RuBr 3(PPh 3) 2(CH 3OH)] in benzene. The compositions of the complexes have been established by elemental analysis, magnetic susceptibility measurement, FT-IR, UV-vis and EPR spectral data. These complexes are paramagnetic and show intense d-d and charge transfer transitions in dichloromethane. The complexes show rhombic EPR spectra at LNT which are typical of low-spin distorted octahedral ruthenium(III) species. All the complexes are redox active and display an irreversible metal centered redox processes. Complex [RuCl(PPh 3) 2(DHA-PTSC)] ( 5) was used as catalyst for transfer hydrogenation of ketones in the presence of isopropanol/KOH and was found to be the active species.

  20. Ferromagnetism in Cu 3-thiosemicarbazone- 2,3-dioxoindole complexes

    NASA Astrophysics Data System (ADS)

    Zentková, M.; Kováč, J.; Zentko, A.; Košturiak, A.

    1991-12-01

    We report evidence for ferromagnetic ordering in Cu-chelates of 3-thiosemicarbazone-2,3-dioxoindole (isatine). It has been found that the Curie temperature is 16.8 K and is independent of the Cu content.

  1. Management of 3-aminopyridine-2-carboxaldehyde thiosemicarbazone-induced methemoglobinemia

    PubMed Central

    Kunos, Charles A; Radivoyevitch, Tomas; Ingalls, Stephen T; Hoppel, Charles L

    2012-01-01

    The anticancer agent 3-aminopyridine-2-carboxaldehyde thiosemicarbazone is a ribonucleotide reductase inhibitor. It inactivates ribonucleotide reductase by disrupting an iron-stabilized radical in ribonucleotide reductase's small subunits, M2 and M2b (p53R2). Unfortunately, 3-aminopyridine-2-carboxaldehyde thiosemicarbazone also alters iron II (Fe2+) in hemoglobin. This creates Fe3+ methemoglobin that does not deliver oxygen. Fe2+ in hemoglobin normally auto-oxidizes to inactive Fe3+ methemoglobin at a rate of nearly 3% per day and this is counterbalanced by a reductase system that normally limits methemoglobin concentrations to less than 1% of hemoglobin. This balance may be perturbed by symptomatic toxicity levels during 3-aminopyridine-2-carboxaldehyde thiosemicarbazone therapy. Indications of 3-aminopyridine-2-carboxaldehyde thiosemicarbazone sequelae attributable to methemoglobinemia include resting dyspnea, headaches and altered cognition. Management of methemoglobinemia includes supplemental oxygen, ascorbate and, most importantly, intravenously administered methylene blue as a therapeutic antidote. PMID:22335579

  2. The Membrane Electrowinning Separation of Antimony from a Stibnite Concentrate

    NASA Astrophysics Data System (ADS)

    Yang, Jian-Guang; Yang, Sheng-Hai; Tang, Chao-Bo

    2010-06-01

    The main purpose of this study was to characterize and to extract antimony from a stibnite concentrate through electrowinning. This article reports an account of a study conducted on the optimization of the process parameters for antimony pentachloride circular leaching, purification, and electrowinning of antimony from antimony trichloride solution. The effect of electrowinning parameters, such as antimony and sodium chloride concentration in the catholyte, temperature, current density, polar distance, etc., on the voltage requirement and the current efficiency (CE) of antimony electrodeposition was explored. A maximum CE of more than 97 pct was attained with a catholyte composition of 70-g/L antimony, 25-g/L NaCl, 4.5-mol/L hydrogen ion concentration, with an anolyte composition of 40-g/L antimony trichloride at a temperature of 328 K (55 °C), a 4-cm polar distance, and a cathode current density of 200 A/m2. Under the optimized conditions, the CE was more than 97 pct, and a 99.98 pct antimony plate was obtained on the cathode. The chemical content analysis of the resulting anolyte was indicated to be 97 pct antimony pentachloride and 3 pct antimony trichloride, which could be recycled to leaching tank as the leaching agent.

  3. Microbial antimony biogeochemistry: Enzymes, regulation, and related metabolic pathways

    USGS Publications Warehouse

    Li, Jingxin; Qian Wang; Oremland, Ronald S.; Kulp, Thomas R.; Rensing, Christopher; Wang, Gejiao

    2016-01-01

    Antimony (Sb) is a toxic metalloid that occurs widely at trace concentrations in soil, aquatic systems, and the atmosphere. Nowadays, with the development of its new industrial applications and the corresponding expansion of antimony mining activities, the phenomenon of antimony pollution has become an increasingly serious concern. In recent years, research interest in Sb has been growing and reflects a fundamental scientific concern regarding Sb in the environment. In this review, we summarize the recent research on bacterial antimony transformations, especially those regarding antimony uptake, efflux, antimonite oxidation, and antimonate reduction. We conclude that our current understanding of antimony biochemistry and biogeochemistry is roughly equivalent to where that of arsenic was some 20 years ago. This portends the possibility of future discoveries with regard to the ability of microorganisms to conserve energy for their growth from antimony redox reactions and the isolation of new species of “antimonotrophs.”

  4. Microbial Antimony Biogeochemistry: Enzymes, Regulation, and Related Metabolic Pathways.

    PubMed

    Li, Jingxin; Wang, Qian; Oremland, Ronald S; Kulp, Thomas R; Rensing, Christopher; Wang, Gejiao

    2016-09-15

    Antimony (Sb) is a toxic metalloid that occurs widely at trace concentrations in soil, aquatic systems, and the atmosphere. Nowadays, with the development of its new industrial applications and the corresponding expansion of antimony mining activities, the phenomenon of antimony pollution has become an increasingly serious concern. In recent years, research interest in Sb has been growing and reflects a fundamental scientific concern regarding Sb in the environment. In this review, we summarize the recent research on bacterial antimony transformations, especially those regarding antimony uptake, efflux, antimonite oxidation, and antimonate reduction. We conclude that our current understanding of antimony biochemistry and biogeochemistry is roughly equivalent to where that of arsenic was some 20 years ago. This portends the possibility of future discoveries with regard to the ability of microorganisms to conserve energy for their growth from antimony redox reactions and the isolation of new species of "antimonotrophs." PMID:27342551

  5. Vacuum Evaporation Technology for Treating Antimony-Rich Anode Slime

    NASA Astrophysics Data System (ADS)

    Qiu, Keqiang; Lin, Deqiang; Yang, Xuelin

    2012-11-01

    A vacuum evaporation technology for treating antimony-rich anode slime was developed in this work. Experiments were carried out at temperatures from 873 K to 1073 K and residual gas pressures from 50 Pa to 600 Pa. During vacuum evaporation, silver from the antimony-rich anode slime was left behind in the distilland in a silver alloy containing antimony and lead, and antimony trioxide was evaporated. The experimental results showed that 92% by weight of antimony can be removed, and the silver content in the alloy was up to 12.84%. The antimony trioxide content in the distillate was more than 99.7%, and the distillate can be used directly as zero-grade antimony trioxide (China standard).

  6. Thank God for Babel: Analysis, Articulation, Antimony.

    ERIC Educational Resources Information Center

    Nyberg, David

    1981-01-01

    Three approaches to philosophical inquiry (analysis, articulation, antimony) are explored in a commentary on "Philosophy and Education: Eightieth Yearbook of the National Society for the Study of Education." A discussion of the sometimes-contradictory school role in providing both educational excellence and socialization illustrates how these…

  7. Arsenic and Antimony Transporters in Eukaryotes

    PubMed Central

    Maciaszczyk-Dziubinska, Ewa; Wawrzycka, Donata; Wysocki, Robert

    2012-01-01

    Arsenic and antimony are toxic metalloids, naturally present in the environment and all organisms have developed pathways for their detoxification. The most effective metalloid tolerance systems in eukaryotes include downregulation of metalloid uptake, efflux out of the cell, and complexation with phytochelatin or glutathione followed by sequestration into the vacuole. Understanding of arsenic and antimony transport system is of high importance due to the increasing usage of arsenic-based drugs in the treatment of certain types of cancer and diseases caused by protozoan parasites as well as for the development of bio- and phytoremediation strategies for metalloid polluted areas. However, in contrast to prokaryotes, the knowledge about specific transporters of arsenic and antimony and the mechanisms of metalloid transport in eukaryotes has been very limited for a long time. Here, we review the recent advances in understanding of arsenic and antimony transport pathways in eukaryotes, including a dual role of aquaglyceroporins in uptake and efflux of metalloids, elucidation of arsenic transport mechanism by the yeast Acr3 transporter and its role in arsenic hyperaccumulation in ferns, identification of vacuolar transporters of arsenic-phytochelatin complexes in plants and forms of arsenic substrates recognized by mammalian ABC transporters. PMID:22489166

  8. Novel antimony doped tin oxide/carbon aerogel as efficient electrocatalytic filtration membrane

    NASA Astrophysics Data System (ADS)

    Liu, Zhimeng; Zhu, Mengfu; Wang, Zheng; Wang, Hong; Deng, Cheng; Li, Kui

    2016-05-01

    A facile method was developed to prepare antimony doped tin oxide (Sb-SnO2)/carbon aerogel (CA) for use as an electrocatalytic filtration membrane. The preparation process included synthesis of a precursor sol, impregnation, and thermal decomposition. The Sb-SnO2, which was tetragonal in phase with an average crystallite size of 10.8 nm, was uniformly distributed on the CA surface and firmly attached via carbon-oxygen-tin chemical bonds. Preliminary filtration tests indicated that the Sb-SnO2/CA membrane had a high rate of total organic carbon removal for aqueous tetracycline owing to its high current efficiency and electrode stability.

  9. Trypanotoxic activity of thiosemicarbazone iron chelators.

    PubMed

    Ellis, Samuel; Sexton, Darren W; Steverding, Dietmar

    2015-03-01

    Only a few drugs are available for treating sleeping sickness and nagana disease; parasitic infections caused by protozoans of the genus Trypanosoma in sub-Saharan Africa. There is an urgent need for the development of new medicines for chemotherapy of these devastating diseases. In this study, three newly designed thiosemicarbazone iron chelators, TSC24, Dp44mT and 3-AP, were tested for in vitro activity against bloodstream forms of Trypanosoma brucei and human leukaemia HL-60 cells. In addition to their iron chelating properties, TSC24 and Dp44mT inhibit topoisomerase IIα while 3-AP inactivates ribonucleotide reductase. All three compounds exhibited anti-trypanosomal activity, with minimum inhibitory concentration (MIC) values ranging between 1 and 100 µM and 50% growth inhibition (GI50) values of around 250 nM. Although the compounds did not kill HL-60 cells (MIC values >100 µM), TSC24 and Dp44mT displayed considerable cytotoxicity based on their GI50 values. Iron supplementation partly reversed the trypanotoxic and cytotoxic activity of TSC24 and Dp44mT but not of 3-AP. This finding suggests possible synergy between the iron chelating and topoisomerase IIα inhibiting activity of the compounds. However, further investigation using separate agents, the iron chelator deferoxamine and the topoisomerase II inhibitor epirubicin, did not support any synergy for the interaction of iron chelation and topoisomerase II inhibition. Furthermore, TSC24 was shown to induce DNA degradation in bloodstream forms of T. brucei indicating that the mechanism of trypanotoxic activity of the compound is topoisomerase II independent. In conclusion, the data support further investigation of thiosemicarbazone iron chelators with dual activity as lead compounds for anti-trypanosomal drug development. PMID:25595343

  10. High Temperature Interactions of Antimony with Nickel

    SciTech Connect

    Marina, Olga A.; Pederson, Larry R.

    2012-07-01

    In this chapter, the surface and bulk interactions of antimony with the Ni-based anodes in solid oxide fuel cells (SOFC) will be discussed. High fuel flexibility is a significant advantage of SOFCs, allowing the direct use of fossil and bio fuels without a hydrogen separation unit. Synthesis gas derived from coal and biomass consists of a mixture of hydrogen, carbon monoxide, carbon dioxide, and steam, but finite amounts of tars and trace impurities such as S, Se, P, As, Sb, Cd, Pb, Cl, etc, are also always present. While synthesis gas is commonly treated with a series of chemical processes and scrubbers to remove the impurities, complete purification is not economical. Antimony is widely distributed in coals. During coal gasification antimony is volatilized, such that contact with the SOFC anodes and other SOFC parts, e.g., interconnect, current collecting wires, fuel gas supplying tubing, is most likely. This chapter addresses the following topics: high temperature Ni - Sb interactions; alteration phase, Ni3Sb, Ni5Sb2, NiSb, formation; thermochemical modeling; impact of Sb on the electrocatalytic activity of Ni toward the fuel oxidation and the presence of other impurities (sulfur, in particular); converted anode structural instability during long-term SOFC operation; comparison with nickel heterogeneous catalysts.

  11. Methemoglobin formation by triapine, di-2-pyridylketone-4,4-dimethyl-3-thiosemicarbazone (Dp44mT), and other anticancer thiosemicarbazones: identification of novel thiosemicarbazones and therapeutics that prevent this effect.

    PubMed

    Quach, Patricia; Gutierrez, Elaine; Basha, Maram Talal; Kalinowski, Danuta S; Sharpe, Philip C; Lovejoy, David B; Bernhardt, Paul V; Jansson, Patric J; Richardson, Des R

    2012-07-01

    Thiosemicarbazones are a group of compounds that have received comprehensive investigation as anticancer agents. The antitumor activity of the thiosemicarbazone, 3-amino-2-pyridinecarboxaldehyde thiosemicarbazone (3-AP; triapine), has been extensively assessed in more than 20 phase I and II clinical trials. These studies have demonstrated that 3-AP induces methemoglobin (metHb) formation and hypoxia in patients, limiting its usefulness. Considering this problem, we assessed the mechanism of metHb formation by 3-AP compared with that of more recently developed thiosemicarbazones, including di-2-pyridylketone-4,4-dimethyl-3-thiosemicarbazone (Dp44mT). This was investigated using intact red blood cells (RBCs), RBC lysates, purified oxyhemoglobin, and a mouse model. The chelation of cellular labile iron with the formation of a redox-active thiosemicarbazone-iron complex was found to be crucial for oxyhemoglobin oxidation. This observation was substantiated using a thiosemicarbazone that cannot ligate iron and also by using the chelator, desferrioxamine, that forms a redox-inactive iron complex. Of significance, cellular copper chelation was not important for metHb generation in contrast to its role in preventing tumor cell proliferation. Administration of Dp44mT to mice catalyzed metHb and cardiac metmyoglobin formation. However, ascorbic acid administered together with the drug in vivo significantly decreased metHb levels, providing a potential therapeutic intervention. Moreover, we demonstrated that the structure of the thiosemicarbazone is of importance in terms of metHb generation, because the DpT analog, di-2-pyridylketone-4-cyclohexyl-4-methyl-3-thiosemicarbazone (DpC), does not induce metHb generation in vivo. Hence, DpC represents a next-generation thiosemicarbazone that possesses markedly superior properties. This investigation is important for developing more effective thiosemicarbazone treatment regimens. PMID:22508546

  12. [Study of the effect of thiosemicarbazones against Toxoplasma gondii].

    PubMed

    Gomes, Marco Antônio G B; Carreira, Gabriela M; Souza, Daniela P V; Nogueira, Paulo Marcos R; de Melo, Edésio J T; Maria, Edmilson J

    2013-04-01

    Toxoplasmosis is a neglected disease, with an estimated occurrence of one-third of the population worldwide. Research in medicinal chemistry has for some years been pursuing the development of new drugs against toxoplasmosis, because current treatments cause serious side effects in the patient. The use of thiosemicarbazones as an alternative option for the treatment of various diseases has been published in recent years, due to their, among others, anticancer, antimalarial, antitrypanosomal, antibacterial, and antitoxoplasmosis activities, the latter being the subject of this study, which is based upon biological analyses and tests of the response of Toxoplasma gondii in the presence of thiosemicarbazones. PMID:23849723

  13. The exposure to and health effects of antimony

    PubMed Central

    Cooper, Ross G.; Harrison, Adrian P.

    2009-01-01

    Context: This minireview describes the health effects of antimony exposure in the workplace and the environment. Aim: To collate information on the consequences of occupational and environmental exposure to antimony on physiological function and well-being. Methods: The criteria used in the current minireview for selecting articles were adopted from proposed criteria in The International Classification of Functioning, Disability and Health. Articles were classified from an acute and chronic exposure and toxicity thrust. Results: The proportion of utilised and non-utilised articles was tabulated. Antimony toxicity is dependent on the exposure dose, duration, route (breathing, eating, drinking, or skin contact), other chemical exposures, age, sex, nutritional status, family traits, life style, and state of health. Chronic exposure to antimony in the air at levels of 9 mg/m3 may exacerbate irritation of the eyes, skin, and lungs. Long-term inhalation of antimony can potentiate pneumoconiosis, altered electrocardiograms, stomach pain, diarrhea, vomiting, and stomach ulcers, results which were confirmed in laboratory animals. Although there were investigations of the effect of antimony in sudden infant death syndrome, current findings suggest no link. Antimony trioxide exposure is predominant in smelters. Mining and exposure via glass working, soldering, and brazing are also important. Conclusion: Antimony has some useful but undoubtedly harmful effects on health and well-being and measures need to be taken to prevent hazardous exposure of the like. Its biological monitoring in the workplace is essential. PMID:20165605

  14. Gold(III) complexes with ONS-Tridentate thiosemicarbazones: Toward selective trypanocidal drugs.

    PubMed

    Rettondin, Andressa R; Carneiro, Zumira A; Gonçalves, Ana C R; Ferreira, Vanessa F; Oliveira, Carolina G; Lima, Angélica N; Oliveira, Ronaldo J; de Albuquerque, Sérgio; Deflon, Victor M; Maia, Pedro I S

    2016-09-14

    Tridentate thiosemicarbazone ligands with an ONS donor set, H2L(R) (R = Me and Et) were prepared by reactions of 1-phenyl-1,3-butanedione with 4-R-3-thiosemicarbazides. H2L(R) reacts with Na[AuCl4]·2H2O in MeOH in a 1:1 M ratio under formation of green gold(III) complexes of composition [AuCl(L(R))]. These compounds represent the first examples of gold(III) complexes with ONS chelate-bonded thiosemicarbazones. The in vitro anti-Trypanosoma cruzi activity against both trypomastigote and amastigote forms (IC50try/ama) of CL Brener strains as well as the cytotoxicity against LLC-MK2 cells of the free ligands and complexes was evaluated. The complex [AuCl(L(Me))] was found to be more active and more selective than its precursor ligand and the standard drug benznidazole with a SItry/ama value higher than 200, being considered as a lead candidate for Chagas disease treatment. Moreover the in vitro activity against the replicative amastigote form (IC50ama) of T. cruzi was additionally investigated revealing that [AuCl(L(Me))] was also more potent than benznidazole still with a similar selectivity index. Finally, docking studies showed that free ligands and complexes interact with the same residues of the parasite protease cruzain but with different intensities, suggesting that this protease could be a possible target for the trypanocidal action of the obtained compounds. PMID:27191616

  15. Organometallic ruthenium complexes with thiosemicarbazone ligands: Synthesis, structure and cytotoxicity of [(η6-p-cymene)Ru(NS)Cl]+ (NS = 9-anthraldehyde thiosemicarbazones)

    PubMed Central

    Beckford, Floyd A.; Leblanc, Gabriel; Thessing, Jeffrey; Shaloski, Michael; Frost, Brian J.; Li, Liya; Seeram, Navindra P.

    2009-01-01

    A series of half-sandwich arene-ruthenium complexes of the type [(η6-p-cymene) Ru(thiosemicarbazone)Cl]+ have been synthesized and their biological activity investigated. The first structurally characterized arene-ruthenium half-sandwich complex with a thiosemicarbazone ligand is reported. PMID:20160909

  16. Undercooling and crystallization behaviour of antimony droplets

    NASA Technical Reports Server (NTRS)

    Graves, J. A.; Perepezko, J. H.

    1986-01-01

    The droplet emulsion technique is presently used to examine the undercooling and crystallization behavior of pure antimony. Control of droplet size and applied cooling rate allowed maximum undercooling to be extended from 0.08 to 0.23 T(m). A droplet coating was produced by means of emulsification which appears to furnish a favorable crystallographic matching for effective nucleation catalysis of a metastable simple cubic structure. Thermal analysis shows the melting temperature of the single cubic phase to be about 625 C.

  17. QSAR Studies of Copper Azamacrocycles and Thiosemicarbazones

    PubMed Central

    Wolohan, Peter; Yoo, Jeongsoo; Welch, Michael J.; Reichert, David E.

    2008-01-01

    Genetic algorithms (GA) were used to develop specific copper metal-ligand force field parameters for the MM3 force field, from a combination of crystallographic structures and ab initio calculations. These new parameters produced results in good agreement with experiment and previously reported copper metal-ligand parameters for the AMBER force field. The MM3 parameters were then used to develop several Quantitative Structure Activity Relationship (QSAR) models. A successful QSAR for predicting the lipophilicity (logPow) of several classes of Cu(II) chelating ligands, was built using a training set of thirty-two Cu(II) radiometal complexes and six simple molecular descriptors. The QSAR exhibited a correlation between the predicted and experimental logPow with a r2 = 0.95, q2 = 0.92. When applied to an external test set of eleven Cu(II) complexes the QSAR preformed with great accuracy; r2 = 0.93 and a q2 = 0.91 utilizing a leave-one-out cross-validation analysis. Additional QSAR models were developed to predict the biodistribution of a smaller set of Cu(II) bis(thiosemicarbazone) complexes. PMID:16107156

  18. Synthesis and biochemical evaluation of benzoylbenzophenone thiosemicarbazone analogues as potent and selective inhibitors of cathepsin L.

    PubMed

    Parker, Erica N; Song, Jiangli; Kishore Kumar, G D; Odutola, Samuel O; Chavarria, Gustavo E; Charlton-Sevcik, Amanda K; Strecker, Tracy E; Barnes, Ashleigh L; Sudhan, Dhivya R; Wittenborn, Thomas R; Siemann, Dietmar W; Horsman, Michael R; Chaplin, David J; Trawick, Mary Lynn; Pinney, Kevin G

    2015-11-01

    Upregulation of cathepsin L in a variety of tumors and its ability to promote cancer cell invasion and migration through degradation of the extracellular matrix suggest that cathepsin L is a promising biological target for the development of anti-metastatic agents. Based on encouraging results from studies on benzophenone thiosemicarbazone cathepsin inhibitors, a series of fourteen benzoylbenzophenone thiosemicarbazone analogues were designed, synthesized, and evaluated for their inhibitory activity against cathepsins L and B. Thiosemicarbazone inhibitors 3-benzoylbenzophenone thiosemicarbazone 1, 1,3-bis(4-fluorobenzoyl)benzene thiosemicarbazone 8, and 1,3-bis(2-fluorobenzoyl)-5-bromobenzene thiosemicarbazone 32 displayed the greatest potency against cathepsin L with low IC50 values of 9.9 nM, 14.4 nM, and 8.1 nM, respectively. The benzoylbenzophenone thiosemicarbazone analogues evaluated were selective in their inhibition of cathepsin L compared to cathepsin B. Thiosemicarbazone analogue 32 inhibited invasion through Matrigel of MDA-MB-231 breast cancer cells by 70% at 10 μM. Thiosemicarbazone analogue 8 significantly inhibited the invasive potential of PC-3ML prostate cancer cells by 92% at 5 μM. The most active cathepsin L inhibitors from this benzoylbenzophenone thiosemicarbazone series (1, 8, and 32) displayed low cytotoxicity toward normal primary cells [in this case human umbilical vein endothelial cells (HUVECs)]. In an initial in vivo study, 3-benzoylbenzophenone thiosemicarbazone (1) was well-tolerated in a CDF1 mouse model bearing an implanted C3H mammary carcinoma, and showed efficacy in tumor growth delay. Low cytotoxicity, inhibition of cell invasion, and in vivo tolerability are desirable characteristics for anti-metastatic agents functioning through an inhibition of cathepsin L. Active members of this structurally diverse group of benzoylbenzophenone thiosemicarbazone cathepsin L inhibitors show promise as potential anti-metastatic, pre

  19. Antimony ore in the Fairbanks district, Alaska

    USGS Publications Warehouse

    Killeen, Pemberton Lewis; Mertie, John B., Jr.

    1951-01-01

    Antimony-bearing ores in the Fairbanks district, Alaska, are found principally in two areas, the extremities of which are at points 10 miles west and 23 miles northeast of Fairbanks; and one of two minor areas lies along this same trend 30 miles farther to the northeast. These areas are probably only local manifestations of mineralization that affected a much broader area and formed antimony-bearing deposits in neighboring districts, the closest of which is 50 miles away. The ores were exposed largely as a result of lode gold mining, but at two periods in the past, high prices for antimony ore warranted an independent production and about 2500 tons of stibnite ore was shipped. The sulfide deposits occupy the same fractures along which a gold-quartz mineralization of greater economic importance occurred; and both are probably genetically related to igneous rocks which intrude the schistose country rock. The sulfide is in part contemporaneous with some late-stage quartz in which it occurs as disseminated crystals; and in part the latest filling in the mineralized zones where it forms kidney-shaped masses of essentially solid sulfide. One extremely long mass must have contained nearly 100 tons of ore, but the average of the larger kidneys is closer to several tons. Much of the ore is stibnite, with quartz as a minor impurity, and assays show the tenor to vary from 40 to 65 percent antimony. Sulphantimonites are less abundant but likewise occur as disseminated crystals and as kidney-shaped bodies. Antimony oxides appear on the weathered surface and along fractures within the sulfide ore. Deposits containing either stibnite or sulphantimonite are known at more than 50 localities, but only eighteen have produced ore and the bulk of this came from the mines. The geology of the deposit, and the nature, extent, and period of the workings are covered in the detailed descriptions of individual occurrences. Several geologic and economic factors, which greatly affect

  20. Selective determination of antimony(III) and antimony(V) with ammonium pyrrolidinedithiocarbamate, sodium diethyldithiocarbamate and dithizone by atomic-absorption spectrometry with a carbon-tube atomizer.

    PubMed

    Kamada, T; Yamamoto, Y

    1977-05-01

    The extraction behaviour of antimony(III) and antimony(V) with ammonium pyrrolidinedithiocarbamate, sodium diethyldithiocarbamate and dithizone in organic solvents has been investigated by means of frameless atomic-absorption spectrophotometry with a carbon-tube atomizer. The selective extraction of antimony(III) and differential determination of antimony(III) and antimony(V) have been developed. With ammonium pyrrolidinedithiocarbamate and methyl isobutyl ketone, when the aqueous phase/solvent volume ratio is 50 ml/10 ml and the injection volume in the carbon tube is 20 mul, the sensitivity for antimony is 0.2 ng/ml for 1% absorption. The relative standard deviations are ca. 2%. Interferences by many metal ions can be prevented by masking with EDTA. The proposed methods have been applied satisfactorily to determination of antimony(III) and antimony(V) in various types of water. PMID:18962096

  1. Disposition of antimony in rhesus monkeys infected with Leishmania braziliensis and treated with meglumine antimoniate.

    PubMed

    Friedrich, Karen; Vieira, Flávia A; Porrozzi, Renato; Marchevsky, Renato S; Miekeley, Norbert; Grimaldi, Gabriel; Paumgartten, Francisco J R

    2012-01-01

    Antimony (Sb) disposition and toxicity was evaluated in Leishmania braziliensis-infected monkeys (Macaca mulatta) treated with a 21-d course of low (LOW) or standard (STD) meglumine antimoniate (MA) dosage regimens (5 or 20 mg Sb(V)/kg body weight/d im). Antimony levels in biological matrices were determined by inductively coupled plasma mass spectrometry (ICPMS), while on-line ion chromatography coupled to ICPMS was used to separate and quantify Sb species in plasma. Nadir Sb levels rose steadily from 19.6 ± 4 and 65.1 ± 17.4 ng/g, 24 h after the first injection, up to 27.4 ± 5.8 and 95.7 ± 6.6 ng/g, 24 h after the 21st dose in LOW and SDT groups, respectively. Subsequently, Sb plasma levels gradually declined with a terminal elimination phase half-life of 35.8 d. Antimony speciation in plasma on posttreatment days 1-9 indicated that as total Sb levels declined, proportion of Sb(V) remained nearly constant (11-20%), while proportion of Sb(III) rose from 5% (d 1) to 50% (d 9). Plasma [Sb]/erythrocyte [Sb] ratio was >1 until 12 h after dosing and reversed thereafter. Tissue Sb concentrations (posttreatment days 55 and 95) were as follows: >1000 ng/g in thyroid, nails, liver, gall bladder and spleen; >200 and <1000 ng/g in lymph nodes, kidneys, adrenals, bones, skeletal muscles, heart and skin; and <200 ng/g in various brain structures, thymus, stomach, colon, pancreas. and teeth. Results from this study are therefore consistent with view that Sb(V) is reduced to Sb(III), the active form, within cells from where it is slowly eliminated. Localization of Sb active forms in the thyroid gland and liver and the pathophysiological consequences of marked Sb accumulation in these tissues warrant further studies. PMID:22129235

  2. Tissue distribution of residual antimony in rats treated with multiple doses of meglumine antimoniate

    PubMed Central

    Coelho, Deise Riba; Miranda, Elaine Silva; Saint’Pierre, Tatiana Dillenburg; Paumgartten, Francisco José Roma

    2014-01-01

    Meglumine antimoniate (MA) and sodium stibogluconate are pentavalent antimony (SbV) drugs used since the mid-1940s. Notwithstanding the fact that they are first-choice drugs for the treatment of leishmaniases, there are gaps in our knowledge of their toxicological profile, mode of action and kinetics. Little is known about the distribution of antimony in tissues after SbV administration. In this study, we evaluated the Sb content of tissues from male rats 24 h and three weeks after a 21-day course of treatment with MA (300 mg SbV/kg body wt/d, subcutaneous). Sb concentrations in the blood and organs were determined by inductively coupled plasma-mass spectrometry. In rats, as with in humans, the Sb blood levels after MA dosing can be described by a two-compartment model with a fast (t1/2 = 0.6 h) and a slow (t1/2 >> 24 h) elimination phase. The spleen was the organ that accumulated the highest amount of Sb, while bone and thyroid ranked second in descending order of tissues according to Sb levels (spleen >> bone, thyroid, kidneys > liver, epididymis, lungs, adrenals > prostate > thymus, pancreas, heart, small intestines > skeletal muscle, testes, stomach > brain). The pathophysiological consequences of Sb accumulation in the thyroid and Sb speciation in the liver, thyroid, spleen and bone warrant further studies. PMID:25075781

  3. Improved cytotoxicity of pyridyl-substituted thiosemicarbazones against MCF-7 when used as metal ionophores.

    PubMed

    Akladios, Fady N; Andrew, Scott D; Parkinson, Christopher J

    2016-02-01

    Zinc is the second most abundant transition metal in the human body, between 3 and 10% of human genes encoding for zinc binding proteins. We have investigated the interplay of reactive oxygen species and zinc homeostasis on the cytotoxicity of the thiosemicarbazone chelators against the MCF-7 cell line. The cytotoxicity of thiosemicarbazone chelators against MCF-7 can be improved through supplementation of ionic zinc provided the zinc ion is at a level exceeding the thiosemicarbazone concentration. Elimination of the entire cell population can be accomplished with this regime, unlike the plateau of cytotoxicity observed on thiosemicarbazone monotherapy. The cytotoxic effects of copper complexes of the thiosemicarbazone are not enhanced by zinc supplementation, displacement of copper from the complex being disfavoured. Treatment of MCF-7 with uncomplexed thiosemicarbazone initiates post G1 blockade alongside the induction of apoptosis, cell death being abrogated through subsequent supplementation with zinc ion after drug removal. This would implicate a metal depletion mechanism in the cytotoxic effect of the un-coordinated thiosemicarbazone. The metal complexes of the species, however, fail to initiate similar G1 blockade and apparently exert their cytotoxic effect through generation of reactive oxygen species, suggesting that multiple mechanisms of cytotoxicity can be associated with the thiosemicarbazones dependant on the level of metal ion association. PMID:26683314

  4. Reduced Antimony Accumulation in ARM58-Overexpressing Leishmania infantum

    PubMed Central

    Schäfer, Carola; Tejera Nevado, Paloma; Zander, Dorothea

    2014-01-01

    Antimony-based drugs are still the mainstay of chemotherapy against Leishmania infections in many countries where the parasites are endemic. The efficacy of antimonials has been compromised by increasing numbers of resistant infections, the basis of which is not fully understood and likely involves multiple factors. By using a functional cloning strategy, we recently identified a novel antimony resistance marker, ARM58, from the parasite Leishmania braziliensis that protects the parasites against antimony-based antileishmanial compounds. Here we show that the Leishmania infantum homologue also confers resistance against antimony but not against other antileishmanial drugs and that its function depends critically on one of four conserved domains of unknown function. This critical domain requires at least two hydrophobic amino acids and is predicted to form a transmembrane structure. Overexpression of ARM58 in antimony-exposed parasites reduces the intracellular Sb accumulation by over 70%, indicating a role for ARM58 in Sb extrusion pathways, but without involvement of energy-dependent transporter proteins. PMID:24366738

  5. Vibrational spectra of palladium 5-nitrofuryl thiosemicarbazone complexes: Experimental and theoretical study

    NASA Astrophysics Data System (ADS)

    Gambino, Dinorah; Otero, Lucía; Vieites, Marisol; Boiani, Mariana; González, Mercedes; Baran, Enrique J.; Cerecetto, Hugo

    2007-10-01

    The vibrational spectroscopic behavior of a series of 16 palladium(II) complexes with 8 bioactive nitrofuran containing thiosemicarbazones as ligands has been studied in the solid state. The IR and Raman spectra of these complexes and the free nitrofuran thiosemicarbazone ligands were recorded and analyzed. Experimental spectra were satisfactorily described by density functional theory (DFT) calculations. The combination of experimental and theoretical methods allowed us to perform the characterization of the main vibrations that show the mode of coordination of the thiosemicarbazone moiety to palladium even though these vibration bands are located in spectral regions showing a complicated pattern due to the presence of vibrations of the nitrofuran moiety and combination modes involving furan vibrations. A characteristic vibrational spectroscopic pattern has been defined for Pd(II) 5-nitrofuryl thiosemicarbazone complexes. This systematic knowledge may be useful for the analysis of the spectroscopic behavior of other coordination compounds holding the 5-nitrofuran thiosemicarbazone moiety.

  6. 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

  7. Crystal structures of copper(II) complexes of 2-formylpyridine substituted thiosemicarbazones; the first example of a coordinated thiosemicarbazone with a thiol function

    NASA Astrophysics Data System (ADS)

    West, D. X.; Swearingen, J. K.; Romack, T. J.; Billeh, I. S.; Jasinski, J. P.; Li, Y.; Staples, R. J.

    2001-08-01

    The crystal structures of two 5-coordinate copper(II) complexes containing neutral, tridentate 2-formylpyridine N(4)-substituted thiosemicarbazones have been determined. 2-Formylpyridine N(4)-cyclohexylthiosemicarbazone, HFo4CHex coordinates via the pyridine nitrogen, imine nitrogen and thione sulfur with two chloro ligands to produce [Cu(HFo4CHex)Cl 2]. Similarly, 2-formylpyridine 3-(4-methylpiperazine)thiosemicarbazone, HFoppz4M, produces [Cu(HFoppz4M)Cl 2] with one major difference; rather than the expected thione form of the thiosemicarbazone moiety, it coordinates as the thiol isomer. Both complexes are close to a square pyramid structure with axial and equatorial chloro ligands and the thiosemicarbazone moieties of both ligands nearly planar. Also included is the crystal structure of N-cyclohexylthiosemicarbazide, CHextsc.

  8. Antimony distribution and environmental mobility at an historic antimony smelter site, New Zealand.

    PubMed

    Wilson, N J; Craw, D; Hunter, K

    2004-05-01

    A historic antimony smelter site at Endeavour Inlet, New Zealand has smelter residues with up to 17 wt.% antimony. Residues include coarse tailings (cm scale particles, poorly sorted), sand tailings (well sorted) and smelter slag (blocks up to 30 cm across). All of this material has oxidised to some degree over the ca. 100 years since the site was abandoned. Oxidation has resulted in acidification of the residues down to pH 2-5. Smelter slag contains pyrrhotite (FeS) and metallic antimony, and oxidation is restricted to surfaces only. The coarse tailings are the most oxidised, and few sulfide grains persist. Unoxidised sand tailings contain 10-20 vol.% stibnite (Sb2S3) containing up to 5% As, with subordinate arsenopyrite (FeAsS), and minor pyrite (FeS2). The sand tailings are variably oxidised on a scale of 2-10 cm, but original depositional layering is preserved during oxidation and formation of senarmontite (Sb2O3). Oxidation of sand tailings has resulted in localised mobility of both Sb and As on the cm scale, resulting in redistribution of these metalloids with iron oxyhydroxide around sand grain boundaries. Experiments demonstrate that Sb mobility decreases with time on a scale of days. Attenuation of both As and Sb occurs due to adsorption on to iron oxyhydroxides which are formed during oxidation of the smelter residues. There is no detectable loss of Sb or As from the smelter site into the adjacent river, <50 m away, which has elevated Sb (ca. 20 microg/l) and As (ca. 7 microg/l) from mineralised rocks upstream. Despite the high concentrations of Sb and As in the smelter residues, these metalloids are not being released into the environment. PMID:14987811

  9. 40 CFR 421.140 - Applicability: Description of the primary antimony subcategory.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... primary antimony subcategory. 421.140 Section 421.140 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) EFFLUENT GUIDELINES AND STANDARDS NONFERROUS METALS MANUFACTURING POINT SOURCE CATEGORY Primary Antimony Subcategory § 421.140 Applicability: Description of the primary...

  10. 40 CFR 421.140 - Applicability: Description of the primary antimony subcategory.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... primary antimony subcategory. 421.140 Section 421.140 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) EFFLUENT GUIDELINES AND STANDARDS NONFERROUS METALS MANUFACTURING POINT SOURCE CATEGORY Primary Antimony Subcategory § 421.140 Applicability: Description of the primary...

  11. pH-dependent release characteristics of antimony and arsenic from typical antimony-bearing ores.

    PubMed

    Hu, Xingyun; Guo, Xuejun; He, Mengchang; Li, Sisi

    2016-06-01

    The pH-dependent leaching of antimony (Sb) and arsenic (As) from three typical Sb-bearing ores (Banxi, Muli and Tongkeng Antimony Mine) in China was assessed using a pH-static leaching experiment. The pH changes of the leached solutions and pH-dependent leaching of Sb and As occurred in different ways. For the Banxi and Muli Sb ores, alkaline conditions were more favorable for the release of Sb compared to neutral and acidic conditions, but the reverse was true for the pH-dependent release of As. For the Tongkeng Sb ore, unlike the previous two Sb-bearing ores, acidic conditions were more favorable for Sb release than neutral and alkaline conditions. The ores with lower Sb and As contents released higher percentages of their Sb and As after 16day leaching, suggesting that they are the largest potential sources of pollution. This work may provide key information on the geochemistry of Sb and As in the weathering zone. PMID:27266313

  12. Aryl- and heteroaryl-thiosemicarbazone derivatives and their metal complexes: a pharmacological template.

    PubMed

    Moorthy, Narayana S H N; Cerqueira, Nuno M F S A; Ramos, Maria J; Fernandes, Pedro A

    2013-05-01

    In this review, we discuss the current patents concerning aryl/heteroaryl thiosemicarbazone derivatives as regards to their activities and properties, including coordination (chelation) properties. The mode of action of the aryl/heteroaryl thiosemicarbazone derivatives involves metal coordination with proteins or biological fluids that have metal ions in their structure. Additionally, these molecules can also form multiple hydrogen bonds through their (thio) amide and N3 nitrogen that ensure a strong interaction with the receptor. In some cases, strong π-π interactions can be observed too. Special attention is given to pyridyl, bis-pyridyl, benzoylpyridyl and isatin thiosemicarbazone derivatives that exhibit significant anticancer, antiviral and other activities in free and in metal complexed forms. This key biological role is often related with their capability to inhibit the enzyme ribonucleotide reductase, similar to what is observed with potent anticancer drugs such as Triapine and methisazone. Recent studies have revealed that thiosemicarbazone can also inhibit topoisomerase II α enzyme. Thiosemicarbazone derivatives form coordination complex with various metals such as Zn, Cu, Fe, Co, Ni, Pt, Pd, etc., and these complexes provide better activities than the free thiosemicarbazones. Recent patents show that the controlled or sustained release dosage form of the thiosemicarbazone derivatives along with ionizing radiations is used for the treatment of proliferative diseases (US20110152281, US20110245304, US20120172217). PMID:22963201

  13. Synthesis, characterization and biological evaluation of paeonol thiosemicarbazone analogues as mushroom tyrosinase inhibitors.

    PubMed

    Zhu, Tian-Hua; Cao, Shu-Wen; Yu, Yan-Ying

    2013-11-01

    A series of hydroxy- and methoxy-substituted paeonol thiosemicarbazone analogues were synthesized as potential tyrosinase inhibitors and their inhibitory effects on mushroom tyrosinase and inhibitory mechanism were evaluated. Paeonol thiosemicarbazone analogues have been found exhibiting more remarkable inhibition than their indexcompounds on mushroom tyrosinase. Among them, compound 2,4-dihydroxy acetophenone-4-phenyl-3-thiosemicarbazone (d1) had the most potent inhibition activity with the IC50 value of 0.006 ± 0.001 mM, displayed as a reversible competitive inhibitor. The inhibitory ability of o- or p-substituted acetophenone thiosemicarbazones was: di-substituted acetophenone thiosemicarbazones>mono-substituted acetophenone thiosemicarbazones>non-substituted acetophenone thiosemicarbazones. Copper ions chelation assay explained that compound d1 exhibited competitive inhibition by forming a chelate with the copper ions at the catalytic domain of tyrosinase as well as indicate a 1.5:1 binding ratio of compound d1 with copper ions. In the fluorescence spectrum study, compound d1 behaved stronger fluorescence quenching on tyrosinase towards d1-Cu(2+) complex, inhibiting tyrosinase mainly by means of chelating the two copper ions in the active site. The newly synthesized compounds may serve as structural templates for designing and developing novel tyrosinase inhibitors. PMID:24120880

  14. The antimicrobial activity of lapachol and its thiosemicarbazone and semicarbazone derivatives

    PubMed Central

    Souza, Marina Azevêdo; Johann, Susana; Lima, Luciana Alves Rodrigues dos Santos; Campos, Fernanda Fraga; Mendes, Isolda Castro; Beraldo, Heloisa; de Souza-Fagundes, Elaine Maria; Cisalpino, Patrícia Silva; Rosa, Carlos Augusto; Alves, Tânia Maria de Almeida; de Sá, Nívea Pereira; Zani, Carlos Leomar

    2013-01-01

    Lapachol was chemically modified to obtain its thiosemicarbazone and semicarbazone derivatives. These compounds were tested for antimicrobial activity against several bacteria and fungi by the broth microdilution method. The thiosemicarbazone and semicarbazone derivatives of lapachol exhibited antimicrobial activity against the bacteria Enterococcus faecalis and Staphylococcus aureus with minimal inhibitory concentrations (MICs) of 0.05 and 0.10 µmol/mL, respectively. The thiosemicarbazone and semicarbazone derivatives were also active against the pathogenic yeast Cryptococcus gattii (MICs of 0.10 and 0.20 µmol/mL, respectively). In addition, the lapachol thiosemicarbazone derivative was active against 11 clinical isolates of Paracoccidioides brasiliensis, with MICs ranging from 0.01-0.10 µmol/mL. The lapachol-derived thiosemicarbazone was not cytotoxic to normal cells at the concentrations that were active against fungi and bacteria. We synthesised, for the first time, thiosemicarbazone and semicarbazone derivatives of lapachol. The MICs for the lapachol-derived thiosemicarbazone against S. aureus, E. faecalis, C. gattii and several isolates of P. brasiliensis indicated that this compound has the potential to be developed into novel drugs to treat infections caused these microbes. PMID:23778660

  15. 40 CFR 440.90 - Applicability; description of the antimony ore subcategory.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... antimony ore subcategory. 440.90 Section 440.90 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) EFFLUENT GUIDELINES AND STANDARDS (CONTINUED) ORE MINING AND DRESSING POINT SOURCE CATEGORY Antimony Ore Subcategory § 440.90 Applicability; description of the antimony ore subcategory....

  16. 40 CFR 440.90 - Applicability; description of the antimony ore subcategory.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... antimony ore subcategory. 440.90 Section 440.90 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) EFFLUENT GUIDELINES AND STANDARDS (CONTINUED) ORE MINING AND DRESSING POINT SOURCE CATEGORY Antimony Ore Subcategory § 440.90 Applicability; description of the antimony ore subcategory....

  17. 40 CFR 440.90 - Applicability; description of the antimony ore subcategory.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... antimony ore subcategory. 440.90 Section 440.90 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) EFFLUENT GUIDELINES AND STANDARDS ORE MINING AND DRESSING POINT SOURCE CATEGORY Antimony Ore Subcategory § 440.90 Applicability; description of the antimony ore subcategory. The provisions of...

  18. 40 CFR 440.90 - Applicability; description of the antimony ore subcategory.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... antimony ore subcategory. 440.90 Section 440.90 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) EFFLUENT GUIDELINES AND STANDARDS ORE MINING AND DRESSING POINT SOURCE CATEGORY Antimony Ore Subcategory § 440.90 Applicability; description of the antimony ore subcategory. The provisions of...

  19. 40 CFR 440.90 - Applicability; description of the antimony ore subcategory.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... antimony ore subcategory. 440.90 Section 440.90 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) EFFLUENT GUIDELINES AND STANDARDS (CONTINUED) ORE MINING AND DRESSING POINT SOURCE CATEGORY Antimony Ore Subcategory § 440.90 Applicability; description of the antimony ore subcategory....

  20. Preparation of zinc sulfide nanocrystallites from single-molecule precursors

    NASA Astrophysics Data System (ADS)

    Palve, Anil M.; Garje, Shivram S.

    2011-07-01

    Zinc sulfide nanocrystallites were prepared using Zinc(II) thiosemicarbazone complexes of the types Zn(L) 2 and ZnCl 2(LH) 2 (where, LH=thiosemicarbazones of cinnamaldehyde, 4-chlorobenzaldehyde, indol-3-carboxaldehyde and thiophene-2-carboxaldehyde) as single source precursors by solvothermal decomposition in ethylene glycol and ethylene diamine in few cases. The materials were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction, energy dispersive X-ray analysis and UV-vis and IR spectroscopy. Solvothermal decomposition in ethylene glycol resulted in the formation of hexagonal ZnS (JCPDS: 36-1450) as evident from the XRD patterns. However, XRD shows formation of hybrid material, ZnS 0.5EN in case of solvothermal decomposition in ethylenediamine. Infrared spectra authenticate the capping of ethylene glycol and ethylenediamine on ZnS and ZnS 0.5EN, respectively. TEM images showed formation of spherical nanoparticles for the materials obtained from ethylene glycol, whereas plate-like morphology is observed in case of materials obtained from ethylene diamine. The blue shift of absorption bands compared to bands of bulk materials in the UV-vis spectra supports the formation of smaller particles.

  1. Isatin based thiosemicarbazone derivatives as potential bioactive agents: Anti-oxidant and molecular docking studies

    NASA Astrophysics Data System (ADS)

    Haribabu, J.; Subhashree, G. R.; Saranya, S.; Gomathi, K.; Karvembu, R.; Gayathri, D.

    2016-04-01

    A new series of isatin based thiosemicarbazones has been synthesized from benzylisatin and unsubstituted/substituted thiosemicarbazides (1-5). The synthesized compounds were characterized by elemental analyses, and UV-Visible, FT-IR, 1H &13C NMR and mass spectroscopic techniques. Three dimensional molecular structure of three compounds (1, 3 and 4) was determined by single crystal X-ray crystallography. Anti-oxidant activity of the thiosemicarbazone derivatives showed their excellent scavenging effect against free radicals. In addition, all the compounds showed good anti-haemolytic activity. In silico molecular docking studies were performed to screen the anti-inflammatory and anti-tuberculosis properties of thiosemicarbazone derivatives.

  2. Technetium-99m antimony colloid for bone-marrow imaging

    SciTech Connect

    Martindale, A.A.; Papadimitriou, J.M.; Turner, J.H.

    1980-11-01

    Technetium-99m antimony colloid was prepared in our laboratory for bone-marrow imaging. Optimal production of colloid particles of size range 1 to 13 nm was achieved by the use of polyvinylpyrrolidone of mol. wt. 44,000. Electron microscopy was used to size the particles. Studies in rabbits showed exclusive concentration in the subendothelial dendritic phagocytes of the bone marrow. Pseudopods from these cells were found to traverse interendothelial junctions and concentrate colloid from the sinusoids. Imaging studies of bone marrow in rabbits showed the superiority of the Tc-99m antimony colloid over the much larger colloidal particle of Tc-99m sulfur colloid. Tissue distribution studies in the rat confirmed that bone-marrow uptake of Tc-99m antimony colloid was greater than that of Tc-99m sulfur colloid, although blood clearance was much slower.

  3. Possible Links between Sickle Cell Crisis and Pentavalent Antimony

    PubMed Central

    Garcerant, Daniel; Rubiano, Luisa; Blanco, Victor; Martinez, Javier; Baker, Nancy C.; Craft, Noah

    2012-01-01

    For over 60 years, pentavalent antimony (Sbv) has been the first-line treatment of leishmaniasis. Sickle cell anemia is a disease caused by a defect in red blood cells, which among other things can cause vasooclusive crisis. We report the case of a 6-year-old child with leishmaniasis who during treatment with meglumine antimoniate developed a sickle cell crisis (SCC). No previous reports describing the relationship between antimonial drugs and sickle cell disease were found. Reviews of both the pathophysiology of SCC and the mechanism of action of Sbv revealed that a common pathway (glutathione) may have resulted in the SCC. ChemoText, a novel database created to predict chemical-protein-disease interactions, was used to perform a more expansive and systematic review that was able to support the association between glutathione, Sbv, and SCC. Although suggestive evidence to support the hypothesis, additional research at the bench would be needed to prove Sbv caused the SCC. PMID:22665619

  4. Antimony Based III-V Thermophotovoltaic Devices

    SciTech Connect

    CA Wang

    2004-06-09

    Antimony-based III-V thermophotovoltaic (TPV) cells are attractive converters for systems with low radiator temperature around 1100 to 1700 K, since these cells potentially can be spectrally matched to the thermal source. Cells under development include GaSb and the lattice-matched GaInAsSb/GaSb and InPAsSb/InAs quaternary systems. GaSb cell technology is the most mature, owing in part to the relative ease in preparation of the binary alloy compared to quaternary GaInAsSb and InPAsSb alloys. Device performance of 0.7-eV GaSb cells exceeds 90% of the practical limit. GaInAsSb TPV cells have been the primary focus of recent research, and cells with energy gap E{sub g} ranging from {approx}0.6 to 0.49 eV have been demonstrated. Quantum efficiency and fill factor approach theoretical limits. Open-circuit voltage factor is as high as 87% of the practical limit for the higher-E{sub g} cells, but degrades to below 80% with decreasing E{sub g} of the alloy, which might be due to Auger recombination. InPAsSb cells are the least studied, and a cell with E{sub g} = 0.45-eV has extended spectral response out to 4.3 {micro}m. This paper briefly reviews the main contributions that have been made for antimonide-based TPV cells, and suggests additional studies for further performance enhancements.

  5. Reductive precipitation of metals photosensitized by tin and antimony porphyrins

    DOEpatents

    Shelnutt, John A.; Gong, Weiliang; Abdelouas, Abdesselam; Lutze, Werner

    2003-09-30

    A method for reducing metals using a tin or antimony porphyrin by forming an aqueous solution of a tin or antimony porphyrin, an electron donor, such as ethylenediaminetetraaceticacid, triethylamine, triethanolamine, and sodium nitrite, and at least one metal compound selected from a uranium-containing compound, a mercury-containing compound, a copper-containing compound, a lead-containing compound, a gold-containing compound, a silver-containing compound, and a platinum-containing compound through irradiating the aqueous solution with light.

  6. Lattice dynamics of femtosecond laser-excited antimony

    NASA Astrophysics Data System (ADS)

    Abdel-Fattah, Mahmoud Hanafy; Bugayev, Aleksey; Elsayed-Ali, Hani E.

    2016-07-01

    Ultrafast electron diffraction is used to probe the lattice dynamics of femtosecond laser-excited antimony thin film. The temporal hierarchies of the intensity and position of diffraction orders are monitored. The femtosecond laser excitation of antimony film was found to lead to initial compression after the laser pulse, which gives way to tension vibrating at new equilibrium displacement. A damped harmonic oscillator model, in which the hot electron-blast force contributes to the driving force of oscillations in lattice spacing, is used to interpret the data. The electron-phonon energy-exchange rate and the electronic Grüneisen parameter were obtained.

  7. Barium and antimony distributions on the hands of nonshooters.

    PubMed

    Havakost, D G; Peters, C A; Koons, R D

    1990-09-01

    Barium and antimony levels from selected areas of the left and right hands of 269 nonshooters provide a database for interpretation of gunshot residue swab analysis results. The database represents a variety of activities of individuals sampled by collectors throughout the United States. Nonshooting exposure to barium and antimony can generally be distinguished from firearms-associated exposure by considering the relative levels of the elements, location on the hands, and condition of the swabs. Consistent definition of sampling procedures and accurate analytical results make this database applicable for interpretation of data generated by most gunshot residue swab examiners. PMID:2230685

  8. Antimony recycling in the United States in 2000

    USGS Publications Warehouse

    Carlin, James F.

    2006-01-01

    The importance of recycling has become more obvious as concerns about the environment and import dependence have grown in recent years. When materials are recycled, fewer natural resources are consumed, and less waste products go to landfills or pollute the water and air. This study, one of a series of reports on metals recycling in 2000, discusses the flow of antimony from mining through its uses and disposal with emphasis on recycling. In 2000, the recycling efficiency for antimony was estimated to be 89 percent, and the recycling rate was about 20 percent.

  9. Reinvestigation of growth of urea thiosemicarbazone monohydrate crystal

    NASA Astrophysics Data System (ADS)

    Srinivasan, Bikshandarkoil R.; Raghavaiah, Pallepogu; Nadkarni, V. S.

    2013-08-01

    The reaction of urea with thiosemicarbazide in 1:1 mole ratio in aqueous solution does not result in the formation of urea thiosemicarbazone monohydrate crystal, as reported by Hanumantharao, Kalainathan and Bhagavannarayana [Spectrochim. Acta A91 (2012) 345-351]. A reinvestigation of the reported reaction reveals that the crystal obtained is the starting material namely thiosemicarbazide, which has been unambiguously confirmed with the aid of infrared and 1H NMR spectra and single crystal X-ray structure determination. Analysis of 1H NMR spectrum reveals that thiosemicarbazide exhibits thione-thiol tautomerism in solution. In contrast, thiosemicarbazide exists as the thione tautomer in the solid state.

  10. ESR, electrochemical and reactivity studies of antitrypanosomal palladium thiosemicarbazone complexes

    NASA Astrophysics Data System (ADS)

    Otero, Lucía; Folch, Christian; Barriga, Germán; Rigol, Carolina; Opazo, Lucia; Vieites, Marisol; Gambino, Dinorah; Cerecetto, Hugo; Norambuena, Ester; Olea-Azar, Claudio

    2008-08-01

    Cyclic voltammetry (CV) and electron spin resonance (ESR) techniques were used in the investigation of novel palladium complexes with bioactive thiosemicarbazones derived from 5-nitrofurane or 5-nitrofurylacroleine. Sixteen palladium complexes grouped in two series of the formula [PdCl 2HL] or [PdL 2] were studied. ESR spectra of the free radicals obtained by electrolytic reduction were characterized and analyzed. The ESR spectra showed two different hyperfine patterns. The stoichiometry of the complexes does not seem to affect significantly the hyperfine constants however we observed great differences between 5-nitrofurane and 5-nitrofurylacroleine derivatives. The scavenger properties of this family of compounds were lower than Trolox.

  11. A spectral study of 2-formylimidazole 4N-substituted thiosemicarbazones and their copper(II) complexes

    NASA Astrophysics Data System (ADS)

    West, Douglas X.; Lockwood, Mark A.; Albert, Julyan N.; Liberta, Anthony E.

    1993-11-01

    Copper(II) complexes of 2-formylimidazole 4N-methyl-, 4N-dimethyl- 4N-ethyl- and 3-hexa-methyleneiminylthiosemicarbazone, along with two nickel(II) complexes of the latter thiosemicarbazone, have been synthesized. Infrared, electronic, NMR and ESR spectra have been used to characterize the complexes and the uncomplexed thiosemicarbazones. None of the complexes or thiosemicarbazones possess growth inhibitory activity against Aspergillus niger and Paecilomyces variotii.

  12. Structural studies of six and four coordinate zinc(II), nickel(II) and dioxovanadium(V) complexes with thiosemicarbazones

    NASA Astrophysics Data System (ADS)

    Sreekanth, A.; Sivakumar, S.; Prathapachandra Kurup, M. R.

    2003-07-01

    Three Zn(II) complexes of di-2-pyridyl ketone thiosemicarbazone, an octahedral Ni(II) complex of 2-acetylpyridine hexamethyleneiminyl-3-thiosemicarbazone, and a V(V) complex of 2-acetylpyridine morpholyl-3-thiosemicarbazone were prepared and characterized. Crystal structure of Ni(II) and V(V) complexes are reported. The ligand in the nickel complex is found to coordinate in the thione form with a pseudo octahedral geometry and the vanadium(V) complex has trigonal bipyramidal geometry.

  13. Influence of anthraquinone scaffold on E/Z isomer distribution of two thiosemicarbazone derivatives. 2D NMR and DFT studies

    NASA Astrophysics Data System (ADS)

    Marković, Violeta; Joksović, Milan D.; Marković, Svetlana; Jakovljević, Ivan

    2014-01-01

    A distribution of possible isomeric and tautomeric forms of two tautomerizable anthraquinone-thiosemicarbazones with pronounced cytotoxic potential was investigated using 2D NMR and DFT studies. Conformational analysis of the E and Z isomers of both thiosemicarbazones was performed to find out the most stable conformation for each molecule. It was found that superior stability of E-isomers results from ten-membered intramolecular hydrogen bond between thiosemicarbazone N2H and anthraquinone carbonyl group. This hydrogen bond is stronger than that between thiosemicarbazone N2H and ester oxygen, owing to the large partial negative charge on the anthraquinone oxygen.

  14. Cyclopalladated organosilane-tethered thiosemicarbazones: novel strategies for improving antiplasmodial activity.

    PubMed

    Adams, Muneebah; Barnard, Linley; de Kock, Carmen; Smith, Peter J; Wiesner, Lubbe; Chibale, Kelly; Smith, Gregory S

    2016-04-01

    Two series of ferrocenyl- and aryl-derived cyclopalladated organosilane thiosemicarbazone complexes were synthesised via C-H bond activation. Selected compounds were evaluated for in vitro antiplasmodial activity against the chloroquine-sensitive (NF54) and chloroquine-resistant (Dd2) strains of the human malaria parasite Plasmodium falciparum. Cyclopalladation of the thiosemicarbazones resulted in antiplasmodial activities in the low micromolar range. PMID:26911403

  15. Acid-base properties of titanium-antimony oxides catalysts

    SciTech Connect

    Zenkovets, G.A.; Paukshtis, E.A.; Tarasova, D.V.; Yurchenko, E.N.

    1982-06-01

    The acid-base properties of titanium-antimony oxide catalysts were studied by the methods of back titration and ir spectroscopy. The interrelationship between the acid-base and catalytic properties in the oxidative ammonolysis of propylene was discussed. 3 figures, 1 table.

  16. Discovery of palladium, antimony, tellurium, iodine, and xenon isotopes

    SciTech Connect

    Kathawa, J.; Fry, C.; Thoennessen, M.

    2013-01-15

    Currently, thirty-eight palladium, thirty-eight antimony, thirty-nine tellurium, thirty-eight iodine, and forty xenon isotopes have been observed and the discovery of these isotopes is described here. For each isotope a brief synopsis of the first refereed publication, including the production and identification method, is presented.

  17. Antimony tartrate corrosion inhibitive composition for coolant systems

    SciTech Connect

    Payerle, N.E.

    1987-08-11

    An automobile coolant concentrate is described comprising (a) a liquid polyhydric alcohol chosen from the group consisting of ethylene glycol, propylene glycol, diethylene glycol and mixtures thereof, and (b) corrosion inhibitors in a corrosion inhibitory amount with respect to corrosion of lead-containing solders, the corrosion inhibitors comprising (i) an alkali metal antimony tartrate, and (ii) an azole compound.

  18. Antimony to Cure Visceral Leishmaniasis Unresponsive to Liposomal Amphotericin B

    PubMed Central

    Morizot, Gloria; Jouffroy, Romain; Faye, Albert; Chabert, Paul; Belhouari, Katia; Calin, Ruxandra; Charlier, Caroline; Miailhes, Patrick; Siriez, Jean-Yves; Mouri, Oussama; Yera, Hélène; Gilquin, Jacques; Tubiana, Roland; Lanternier, Fanny; Mamzer, Marie-France; Legendre, Christophe; Peyramond, Dominique; Caumes, Eric; Lortholary, Olivier; Buffet, Pierre

    2016-01-01

    We report on 4 patients (1 immunocompetent, 3 immunosuppressed) in whom visceral leishmaniasis had become unresponsive to (or had relapsed after) treatment with appropriate doses of liposomal amphotericin B. Under close follow-up, full courses of pentavalent antimony were administered without life-threatening adverse events and resulted in rapid and sustained clinical and parasitological cure. PMID:26735920

  19. Antimony to Cure Visceral Leishmaniasis Unresponsive to Liposomal Amphotericin B.

    PubMed

    Morizot, Gloria; Jouffroy, Romain; Faye, Albert; Chabert, Paul; Belhouari, Katia; Calin, Ruxandra; Charlier, Caroline; Miailhes, Patrick; Siriez, Jean-Yves; Mouri, Oussama; Yera, Hélène; Gilquin, Jacques; Tubiana, Roland; Lanternier, Fanny; Mamzer, Marie-France; Legendre, Christophe; Peyramond, Dominique; Caumes, Eric; Lortholary, Olivier; Buffet, Pierre

    2016-01-01

    We report on 4 patients (1 immunocompetent, 3 immunosuppressed) in whom visceral leishmaniasis had become unresponsive to (or had relapsed after) treatment with appropriate doses of liposomal amphotericin B. Under close follow-up, full courses of pentavalent antimony were administered without life-threatening adverse events and resulted in rapid and sustained clinical and parasitological cure. PMID:26735920

  20. The structure-activity relationships of the antiviral chemotherapeutic activity of isatin β-thiosemicarbazone

    PubMed Central

    Bauer, D. J.; Sadler, P. W.

    1960-01-01

    As part of an investigation devoted to the development of new antiviral agents a compound of established antiviral activity has been subjected to systematic structural modification. The structure-activity data so obtained have been used in the design of new compounds, some of which are described. The compound chosen was isatin β-thiosemicarbazone, which has high activity against neurovaccinia infection in mice, and a 4-point parallel-line assay of in vivo chemotherapeutic activity has been developed, which has enabled the activity of the derivatives to be determined against isatin β-thiosemicarbazone as a standard. The overall dimensions of the isatin β-thiosemicarbazone molecule appear to be nearly maximal for the retention of high activity, as all substituents in the aromatic ring decrease the activity irrespective of their nature or position. The projection of the -CS.NH2 group in relation to the ring nitrogen was found to be critical, as the α-thiosemicarbazone was inactive. A number of modifications of the side-chain were investigated:all led to reduction or loss of antiviral activity. The antiviral activity showed a positive correlation with chloroform solubility over a considerable range. The most active compound encountered was 1-ethylisatin β-thiosemicarbazone, with an activity of 286 (isatin β-thiosemicarbazone≡100). Isatin β-thiosemicarbazone showed no activity against 15 other viruses, and 20 related compounds showed on activity against ectromelia. PMID:13797622

  1. Antimony and arsenic biogeochemistry in the East China Sea

    NASA Astrophysics Data System (ADS)

    Ren, Jing-Ling; Zhang, Xu-Zhou; Sun, You-Xu; Liu, Su-Mei; Huang, Daji; Zhang, Jing

    2016-02-01

    The biogeochemical cycles of the metalloid elements arsenic and antimony in the East China Sea (ECS), one of the most important marginal seas for western Pacific, were examined in May 2011. Dissolved inorganic arsenic (As(V) and As(III)) and antimony (Sb(V) and Sb(III)) species were determined by selective hydride generation-atomic fluorescence spectrometry (HG-AFS). Results show that total dissolved inorganic arsenic (TDIAs; [TDIAs]=[As(V)]+[As(III)]) were moderately depleted in the surface water and enriched in the deep water. Arsenite (As(III)) showed different vertical profiles with that of TDIAs, with significant surface enrichment in the middle shelf region where the concentrations of phosphate were extremely low. Speciation of dissolved arsenic was subtly controlled by the stoichiometric molar ratio of arsenate (As(V)) to phosphate. The average As(V)/P ratio for the ECS in spring 2011 was 10.8×10-3, which is higher than previous results and indicates the arsenate stress. The concentrations of total dissolved inorganic antimony (TDISb; [TDISb]=[Sb(V)]+[Sb(III)]) were high near the Changjiang Estuary and the coastal area of Hangzhou Bay and decreased moderately off the coast. TDISb displayed moderate conservative behavior in the ECS that confirms by the correlations with salinity and dissolved aluminum. Different with that of As(III), antimonite (Sb(III)) concentrations were extremely lower in the ECS, with relative higher concentration appeared at the bottom layer which indicates the contribution from sediment-water interface. A preliminary box model was established to estimate the water-mass balance and antimony budgets for the ECS. Compared with other areas in the world, the concentrations of dissolved inorganic arsenic and antimony in the ECS remain at natural levels.

  2. Transition metal quinone-thiosemicarbazone complexes 3: Spectroscopic characterizations of spin-mixed iron (III) of naphthoquinone-thiosemicarbazones

    NASA Astrophysics Data System (ADS)

    Chikate, Rajeev C.; Padhye, Subhash B.

    2007-04-01

    An interesting series of iron (III) complexes with naphthoquinone-thiosemicarbazones are synthesized and physico-chemically characterized by elemental analysis, UV-vis, IR, EPR and magnetic susceptibility measurements. They possess a cationic octahedral [FeL 2] + species and a tetrahedral [FeCl 4] - anion and exhibit unusual spin-mixed states involving high-spin and low-spin ferric centers as revealed from magnetic behavior with significant amount of exchange interactions mediated by intermolecular associations. The magnetic susceptibility data is fitted with S=5/2 and S=1/2 Heisengberg's exchange coupled model; Hˆ=-2JSS and the magnetic exchange interactions are found to be of the order of -13.6 cm -1 indicating the moderate coupling between two paramagnetic centers present in different chemical and structural environment. The presence of spin-paired iron (III) cation having dxz2dxz2dxz1 ground state is revealed from the EPR spectra with three prominent peaks while the high-spin tetrahedral iron (III) anion exhibits characteristics g = 4 signal whose intensity increases with lowering the temperature suggesting its influence on the magnetic properties of the complex molecule. FTIR measurements indicate tridentate ONS donor systems involving quinone/hydroxyl oxygen, imine/hydrazinic nitrogen and thione/thiol sulfur atoms as binding sites for naphthoquinone-thiosemicarbazones.

  3. BioGeochemistry of antimony, Sources, Transfers, Impacts and Assessment

    NASA Astrophysics Data System (ADS)

    Le Roux, Gael; Pinelli, Eric; Hedde, Mickael; Guiresse, Maritxu; De Vleeschouwer, François; Silvestre, Jérôme; Enrico, Maxime; Gandois, Laure; Monna, Fabrice; Gers, Charles; Probst, Anne

    2013-04-01

    BioGeoSTIB is a project funded by ADEME (French Environmental Protection Agency). Its aim is to provide a better understanding of biogeochemical cycle disturbances of antimony by man. Specifically, it is focused on the atmosphere-soil-organism interfaces. Based on a multi-scale approach, the impact of antimony on organisms and organism communities and the factors of Sb dispersion in the environment aim to better characterized. This report gives the main results of 2 and 1 -2 years of research. Using peat bogs as environmental archives, we show that Sb contamination in soils date back to the beginning of the metallurgy. Atmospheric deposition of Sb largely increased by 100 times during the Industrial Revolution compared to natural levels (~0,001-0,01 mg m-2 an-1) estimated in the deepest peat layers. This disturbance in the antimony geochemical cycle modified its concentrations in soils. One main source of present Sb contamination is automotive traffic due to Sb in braking lines. This emerging contamination was characterized close to a roundabout. This additional source of Sb does not seem to impact soil fauna but Sb concentrations in soil solutions exceed 1 μg L-1. Genotoxicity tests have been performed on the model plant Vicia faba and show that antimony is genotoxic at its lowest concentrations and that there is a synergistic effect lead, a trace metal frequently found in association with antimony in the environment. It is a main issue to determine Sb critical loads in the environment but main identified lacks are thermodynamic data, which are not available yet, to model the behavior of Sb in soil solutions and the fact the antimony is always associated with other anthropogenic trace metals like lead. Critical thresholds of Sb have been determined for the first time based on genotoxicity experiment. Simulations show that these thresholds can be exceeded in the future, whereas present limits for invertebrates (US-EPA) are and will not be reached. However

  4. Determination of fluorine in antimony catalysts for the liquid-phase production of freons

    SciTech Connect

    Shchavelev, V.B.

    1986-08-01

    In order to reduce the solubility of lanthanum fluoride and to improve the precision of fluorine determination, (ILLEGIBLE) recommend (ILLEGIBLE) organic solvents (ethanol, acetone, etc.) to the titrated solution. It is shown that fluoride can be determined in the presence of antimony without preparation only when all antimony is present in the tervalent state. The results obtained in the determination of fluoride ion in synthetic mixtures at a fluorine:antimony molar ratio of 2, which approximates the composition of the antimony catalyst, are shown in tables. It can be seen that hydrobromic acid is the only suitable of the agents tested, whereby its concentration in the analyzed sample must not be less than 7.6. The relatively high reproducibility of the proposed procedure allows the authors to recommend it for the determination of fluorine in antimony catalysts or other analogous compositions when fluorine and pentavalent antimony are present simultaneously.

  5. Antimony-assisted carbonization of Si(111) with solid source molecular beam epitaxy

    SciTech Connect

    Hackley, Justin; Richardson, Christopher J. K.; Sarney, Wendy L.

    2013-11-15

    The carbonization of an antimony-terminated Si (111) surface in a solid source molecular beam epitaxy system is presented. Reflection high-energy electron diffraction, atomic force microscopy, x-ray photoelectron spectroscopy, and cross-sectional transmission electron microscopy are used to characterize samples grown with and without antimony termination. It is shown that the antimony-terminated surface promotes the formation of thin, smooth and continuous SiC films at a relatively low temperature of 800 °C.

  6. States of antimony and tin atoms in lead chalcogenides

    SciTech Connect

    Bordovsky, G. A.; Nemov, S. A.; Marchenko, A. V.; Zaiceva, A. V.; Kozhokar, M. Yu.; Seregin, P. P.

    2011-04-15

    It is shown by Moessbauer spectroscopy of the {sup 119}Sb({sup 119m}Sn) isotope that impurity antimony atoms in PbS, PbSe, and PbTe lattices are distributed between cation and anion sublattices. In n-type samples, the greatest part of antimony is located in the anion sublattice; in hole ones, in the cation sublattice. The tin atoms formed as a result of radioactive decay of {sup 119}Sb (antisite state) are electrically inactive in the anion sub-lattice of PbS and PbSe, while, in the cation sublattice, they form donor U{sup -} centers. Electron exchange between the neutral and doubly ionized tin U{sup -} centers via the allowed band states is observed. The tin atoms formed after radioactive decay of {sup 119}Sb are electrically inactive in the anion and cation sublattices of PbTe.

  7. Transmission Potential of Antimony-Resistant Leishmania Field Isolates

    PubMed Central

    Seblova, Veronika; Oury, Bruno; Eddaikra, Naouel; Aït-Oudhia, Khatima; Pratlong, Francine; Gazanion, Elodie; Maia, Carla; Volf, Petr

    2014-01-01

    We studied the development of antimony-resistant Leishmania infantum in natural vectors Lutzomyia longipalpis and Phlebotomus perniciosus to ascertain the risk of parasite transmission by sand flies. All three resistant strains produced fully mature late-stage infections in sand flies; moreover, the resistant phenotype was maintained after the passage through the vector. These results highlight the risk of circulation of resistant Leishmania strains and question the use of human drugs for treatment of dogs as Leishmania reservoirs. PMID:25049256

  8. Solid solutions based on bismuth and antimony tellurides andbismuth selenides

    SciTech Connect

    Abrikosov, N.K.; Stasova, M.M.

    1986-05-01

    The phase diagrams of the systems Bi-Te, Bi-Se, and Sb-Te serve as a basis for constructing multiphase diagrams of ternary semiconductor systems. This paper studies layered structures with large unit-cell parameters in the regions of the solid solutions to explain the ordering processes in the solid solutions of semiconductor and intermetallic systems. The laws governing the formation and structral features of bismuth and antimony chalcogenides are studied to obtain thermoelectric materials and identification of minerals.

  9. Transmission potential of antimony-resistant leishmania field isolates.

    PubMed

    Seblova, Veronika; Oury, Bruno; Eddaikra, Naouel; Aït-Oudhia, Khatima; Pratlong, Francine; Gazanion, Elodie; Maia, Carla; Volf, Petr; Sereno, Denis

    2014-10-01

    We studied the development of antimony-resistant Leishmania infantum in natural vectors Lutzomyia longipalpis and Phlebotomus perniciosus to ascertain the risk of parasite transmission by sand flies. All three resistant strains produced fully mature late-stage infections in sand flies; moreover, the resistant phenotype was maintained after the passage through the vector. These results highlight the risk of circulation of resistant Leishmania strains and question the use of human drugs for treatment of dogs as Leishmania reservoirs. PMID:25049256

  10. [Successful treatment of cutaneous leishmaniasis with amphotericin B; a case of unresponsive to pentavalent antimony therapy].

    PubMed

    Yeşilova, Yavuz; Turan, Enver; Sürücü, Hacer Altın; Aksoy, Mustafa; Özbilgin, Ahmet

    2015-03-01

    Cutaneous Leishmaniasis (CL) is a skin infection caused by various species of Leishmania parasites, which is transmitted by infected Phlebotomus sandfly bites. Pentavalent antimonials (meglumine antimoniate and sodium stibogluconate) are used for the treatment of adult CL patients as an effective and safe method. Liposomal amphotericin B is an alternative for the treatment of choice in cutaneous leishmaniasis cases which pentavalan antimony contraindicated or unresponsive to pentavalent antimony therapy. In this study, successful treatment with systemic liposomal amphotericin B of a cutaneous leishmaniasis case developing local side effects related both systemic and intralesional meglumine antimonate treatment was presented. PMID:25917587

  11. Correlation of CsK{sub 2}Sb photocathode lifetime with antimony thickness

    SciTech Connect

    Mamun, M. A. Elmustafa, A. A.; Hernandez-Garcia, C.; Poelker, M.

    2015-06-01

    CsK{sub 2}Sb photocathodes with quantum efficiency on the order of 10% at 532 nm, and lifetime greater than 90 days at low voltage, were successfully manufactured via co-deposition of alkali species emanating from an effusion source. Photocathodes were characterized as a function of antimony layer thickness and alkali consumption, inside a vacuum chamber that was initially baked, but frequently vented without re-baking. Photocathode lifetime measured at low voltage is correlated with the antimony layer thickness. Photocathodes manufactured with comparatively thick antimony layers exhibited the best lifetime. We speculate that the antimony layer serves as a reservoir, or sponge, for the alkali.

  12. Correlation of CsK2Sb photocathode lifetime with antimony thickness

    SciTech Connect

    Mamun, M. A.; Hernandez-Garcia, C.; Poelker, M.; Elmustafa, A. A.

    2015-06-01

    CsK2Sb photocathodes with quantum efficiency on the order of 10% at 532 nm, and lifetime greater than 90 days at low voltage, were successfully manufactured via co-deposition of alkali species emanating from an effusion source. Photocathodes were characterized as a function of antimony layer thickness and alkali consumption, inside a vacuum chamber that was initially baked, but frequently vented without re-baking. Photocathode lifetime measured at low voltage is correlated with the antimony layer thickness. Photocathodes manufactured with comparatively thick antimony layers exhibited the best lifetime. We speculate that the antimony layer serves as a reservoir, or sponge, for the alkali.

  13. Possible links between sickle cell crisis and pentavalent antimony.

    PubMed

    Garcerant, Daniel; Rubiano, Luisa; Blanco, Victor; Martinez, Javier; Baker, Nancy C; Craft, Noah

    2012-06-01

    For over 60 years, pentavalent antimony (Sb(v)) has been the first-line treatment of leishmaniasis. Sickle cell anemia is a disease caused by a defect in red blood cells, which among other things can cause vasooclusive crisis. We report the case of a 6-year-old child with leishmaniasis who during treatment with meglumine antimoniate developed a sickle cell crisis (SCC). No previous reports describing the relationship between antimonial drugs and sickle cell disease were found. Reviews of both the pathophysiology of SCC and the mechanism of action of Sb(v) revealed that a common pathway (glutathione) may have resulted in the SCC. ChemoText, a novel database created to predict chemical-protein-disease interactions, was used to perform a more expansive and systematic review that was able to support the association between glutathione, Sb(v), and SCC. Although suggestive evidence to support the hypothesis, additional research at the bench would be needed to prove Sb(v) caused the SCC. PMID:22665619

  14. Antimony nanoparticles anchored on interconnected carbon nanofibers networks as advanced anode material for sodium-ion batteries

    NASA Astrophysics Data System (ADS)

    Hou, Hongshuai; Jing, Mingjun; Yang, Yingchang; Zhang, Yan; Song, Weixin; Yang, Xuming; Chen, Jun; Chen, Qiyuan; Ji, Xiaobo

    2015-06-01

    Interconnected carbon nanofibers networks (ICNNs) prepared through the carbonization of polypyrrole (PPy) precursor are utilized as conductive pathways and buffer to improve the Na storage performance of antimony (Sb) as anode for sodium-ion batteries (SIBs). The as-obtained Sb/ICNNs composite exhibits excellent cycle stability. The reversible capacity can remain 542.5 mAh g-1 with a high capacity retention of 96.7% after 100 cycles at a current density of 100 mA g-1. And the superior rate performance is also observed, the reversible capacity can still reach 325 mAh g-1 at a high current density of 3200 mA g-1. These great electrochemical performances observed above suggest that this type of composite can be a nice option for advanced SIBs anode materials and may be extended to other active materials/ICNNs composite electrode.

  15. Spectral, thermal, electrochemical and analytical studies on Cd(II) and Hg(II) thiosemicarbazone complexes

    NASA Astrophysics Data System (ADS)

    El-Asmy, A. A.; El-Gammal, O. A.; Saleh, H. S.

    2008-11-01

    The coordination characteristic of the investigated thiosemicarbazones towards hazard pollutants, Cd(II) and Hg(II), becomes the first goal. Their complexes have been studied by microanalysis, thermal, electrochemical and spectral (electronic, IR and MS) studies. The substitutent (salicylaldehyde, acetophenone, benzophenone, o-hydroxy- p-methoxybenzophenone or diacetylmonoxime) plays an important role in the complex formation. The coordination sites were the S for thiosemicarbazide (HTS); NN for benzophenone thiosemicarbazone (HBTS); NS for acetophenone thiosemicarbazone (HATS) and salicylaldehyde thiosemicarbazone (H 2STS); NNS or NSO for diacetylmonoxime thiosemicarbazone (H 2DMTS). The stability constants of Hg(II) complexes were higher than Cd(II). The kinetic and thermodynamic parameters for the different thermal decomposition steps in the complexes have been evaluated. The activation energy values of the first step ordered the complexes as: [Cd(H 2STS)Cl 2]H 2O > [Cd(H 2DAMTS)Cl 2] > [Cd(HBTS) 2Cl 2]2H 2O > [Cd(HATS) 2Cl 2]. The CV of [Cd(H 2STS)Cl 2]H 2O and [Hg(HBTS)Cl 2] were recorded. The use of H 2DMTS as a new reagent for the separation and determination of Cd(II) ions from water and some synthetic samples using flotation technique is aimed to be discussed.

  16. Structural, optical and charge generation properties of chalcostibite and tetrahedrite copper antimony sulfide thin films prepared from metal xanthates† †Electronic supplementary information (ESI) available: Chemical structures of the used metal xanthates, additional XRD, SEM-EDX and UV-vis data. See DOI: 10.1039/c5ta05777a Click here for additional data file.

    PubMed Central

    MacLachlan, Andrew J.; Brown, Michael D.

    2015-01-01

    Herein, we report on a solution based approach for the preparation of thin films of copper antimony sulfide, an emerging absorber material for third generation solar cells. In this work, copper and antimony xanthates are used as precursor materials for the formation of two different copper antimony sulfide phases: chalcostibite (CuSbS2) and tetrahedrite (Cu12Sb4S13). Both phases were thoroughly investigated regarding their structural and optical properties. Moreover, thin films of chalcostibite and tetrahedrite were prepared on mesoporous TiO2 layers and photoinduced charge transfer in these metal sulfide/TiO2 heterojunctions was studied via transient absorption spectroscopy. Photoinduced charge transfer was detected in both the chalcostibite as well as the tetrahedrite sample, which is an essential property in view of applying these materials as light-harvesting agents in semiconductor sensitized solar cells. PMID:27019713

  17. Ruthenium(II) complexes of 2-benzoylpyridine-derived thiosemicarbazones with cytotoxic activity against human tumor cell lines

    NASA Astrophysics Data System (ADS)

    Graminha, Angelica E.; Rodrigues, Cláudia; Batista, Alzir A.; Teixeira, Letícia R.; Fagundes, Elaine S.; Beraldo, Heloisa

    2008-04-01

    Reaction of [RuCl 3(dppb)H 2O] (dppb = 1,4 bis(diphenylphospine)butane) with 2-benzoylpyridine thiosemicarbazone (H2Bz4DH) and its N(4)-methyl (H2Bz4M) and N(4)-phehyl (H2Bz4Ph) derivatives gave [RuCl(dppb)(H2Bz4DH)]Cl ( 1), [RuCl(dppb)(H2Bz4M)]Cl ( 2) and [RuCl(dppb)(H2Bz4Ph)]Cl ( 3). The cytotoxic activity of the studied compounds was tested against the MCF-7, TK-10 and UACC-62 human tumor cell lines. The precursor [RuCl 3(dppb)H 2O] exhibits cytocidal activity against the tree cell lines. H2BzDH, H2Bz4M, and [RuCl(dppb)(H2Bz4M)]Cl ( 2) show a selective cytocidal effect against the UACC-62 cell line which makes them the most promising compounds.

  18. Facile synthesis of antimony-doped tin oxide nanoparticles by a polymer-pyrolysis method

    SciTech Connect

    Li, Yuan-Qing; Wang, Jian-Lei; Fu, Shao-Yun; Mei, Shi-Gang; Zhang, Jian-Min; Yong, Kang

    2010-06-15

    In this article, antimony-doped tin oxide (ATO) nanoparticles was synthesized by a facile polymer-pyrolysis method. The pyrolysis behaviors of the polymer precursors prepared via in situ polymerization of metal salts and acrylic acid were analyzed by simultaneous thermogravimetric and differential scanning calorimetry (TG-DSC). The structural and morphological characteristics of the products were studied by powder X-ray diffraction (XRD) and transmission electron microscope (TEM). The results reveal that the ATO nanoparticles calcined at 600 {sup o}C show good crystallinity with the cassiterite structure and cubic-spherical like morphology. The average particle size of ATO decreases from 200 to 15 nm as the Sb doping content increases from 5 mol% to 15 mol%. Electrical resistivity measurement shows that the resistivity for the 10-13 mol% Sb-doped SnO{sub 2} nanoparticles is reduced by more than three orders compared with the pure SnO{sub 2} nanoparticles. In addition, due to its versatility this polymer-pyrolysis method can be extended to facile synthesis of other doped n-type semiconductor, such as In, Ga, Al doped ZnO, Sn doped In{sub 2}O{sub 3}.

  19. Enhanced hematite water electrolysis using a 3D antimony-doped tin oxide electrode.

    PubMed

    Moir, Jonathon; Soheilnia, Navid; O'Brien, Paul; Jelle, Abdinoor; Grozea, Claudia M; Faulkner, Daniel; Helander, Michael G; Ozin, Geoffrey A

    2013-05-28

    We present herein an example of nanocrystalline antimony-doped tin oxide (nc-ATO) disordered macroporous "inverse opal" 3D electrodes as efficient charge-collecting support structures for the electrolysis of water using a hematite surface catalyst. The 3D macroporous structures were created via templating of polystyrene spheres, followed by infiltration of the desired precursor solution and annealing at high temperature. Using cyclic voltammetry and electrochemical impedance spectroscopy, it was determined that the use of this 3D transparent conducting oxide with a hematite surface catalyst allowed for a 7-fold increase in active surface area for water splitting with respect to its 2D planar counterpart. This ratio of surface areas was evaluated based on the presence of oxidized trap states on the hematite surface, as determined from the equivalent circuit analysis of the Nyquist plots. Furthermore, the presence of nc-ATO 2D and 3D "underlayer" structures with hematite deposited on top resulted in decreased charge transfer resistances and an increase in the number of available active surface sites at the semiconductor-liquid junction when compared to hematite films lacking any nc-ATO substructures. Finally, absorption, transmission, and reflectance spectra of all of the tested films were measured, suggesting the feasibility of using 3D disordered structures in photoelectrochemical reactions, due to the high absorption of photons by the surface catalyst material and trapping of light within the structure. PMID:23581965

  20. In vitro evaluation of the activity of thiosemicarbazone derivatives against mycotoxigenic fungi affecting cereals.

    PubMed

    Degola, Francesca; Morcia, Caterina; Bisceglie, Franco; Mussi, Francesca; Tumino, Giorgio; Ghizzoni, Roberta; Pelosi, Giorgio; Terzi, Valeria; Buschini, Annamaria; Restivo, Francesco Maria; Lodi, Tiziana

    2015-05-01

    With a steadily increasing world population, a more efficient system of food production is of paramount importance. One of the major causes of food spoilage is the presence of fungal pathogens and the production and accumulation of mycotoxins. In the present work we report a study on the activity of a series of functionalized thiosemicarbazones (namely cuminaldehyde, trans-cinnamaldehyde, quinoline-2-carboxyaldehyde, 5-fluoroisatin thiosemicarbazone and 5-fluoroisatin N(4)-methylthiosemicarbazone), as antifungal and anti-mycotoxin agents, against the two major genera of cereal mycotoxigenic fungi, i.e. Fusarium and Aspergillus. These thiosemicarbazones display different patterns of efficacy on fungal growth and on mycotoxin accumulation depending on the fungal species. Some of the molecules display a greater effect on mycotoxin synthesis than on fungal growth. PMID:25702884

  1. Spectral studies of copper(II) complexes of 6-(3-thienyl) pyridine-2-thiosemicarbazone

    NASA Astrophysics Data System (ADS)

    Mahjoub, Omima Abdalla; Farina, Yang

    2014-09-01

    Two novel copper(II) complexes [Cu(HL)Cl]Cl˙H2O (1) and [Cu(L)NO3]˙H2O (2) of the three NNS donor thiosemicarbazone ligand 6-(3-thienyl) pyridine-2-thiosemicarbazone have been synthesized. The ligand and its copper(II) complexes were characterized by elemental analysis (C, H, N, and S), FT-IR, UV-visible, magnetic susceptibility and molar conductance. The thiosemicarbazone is present either as the thione form in complex 1 or as thiol form in complex 2 and is coordinated to copper(II) atom via the pyridine nitrogen atom, the azomethine nitrogen atom and the sulfur atom. The physicochemical and spectral data suggest square planar geometry for copper(II) atoms.

  2. Spectral studies of copper(II) complexes of 6-(3-thienyl) pyridine-2-thiosemicarbazone

    SciTech Connect

    Mahjoub, Omima Abdalla; Farina, Yang

    2014-09-03

    Two novel copper(II) complexes [Cu(HL)Cl]Cl.H{sub 2}O (1) and [Cu(L)NO{sub 3}]Ðœ‡H{sub 2}O (2) of the three NNS donor thiosemicarbazone ligand 6-(3-thienyl) pyridine-2-thiosemicarbazone have been synthesized. The ligand and its copper(II) complexes were characterized by elemental analysis (C, H, N, and S), FT-IR, UV-visible, magnetic susceptibility and molar conductance. The thiosemicarbazone is present either as the thione form in complex 1 or as thiol form in complex 2 and is coordinated to copper(II) atom via the pyridine nitrogen atom, the azomethine nitrogen atom and the sulfur atom. The physicochemical and spectral data suggest square planar geometry for copper(II) atoms.

  3. 78 FR 59679 - Antimony Trioxide TSCA Chemical Risk Assessment; Notice of Public Meetings and Opportunity To...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2013-09-27

    ... AGENCY Antimony Trioxide TSCA Chemical Risk Assessment; Notice of Public Meetings and Opportunity To... review of EPA's draft Toxic Substances Control Act (TSCA) chemical risk assessment, ``TSCA Workplan Chemical Risk Assessment for Antimony Trioxide.'' EPA will hold three peer review meetings by web...

  4. Corrosion of low-antimony lead-cadmium alloys in conditions of long-term polarization

    NASA Astrophysics Data System (ADS)

    Nuzhny, Alex

    Nowadays, lead-acid battery grids are manufactured mostly from low-antimony and lead-calcium alloys. A variable corrosion resistance of battery grids is caused by either battery operation conditions, purity of used alloy components, an alloy makeup, and the castings quality. Such compositions as usual lead-antimony alloy, low-antimony lead-arsenious alloy and lead-calcium alloy with moderate content of tin today may be regarded as the most studied ones. A significant share of published works has been devoted to low-antimony lead-tin alloys. In the present article, results of corrosion tests of the samples made with application of cadmium as the second component of low-antimony alloy, has been represented. Several samples were extra-alloyed by selenium and silver. Samples of lead-calcium and usual antimony alloys as well as pure lead samples were being tested simultaneously. Upon termination of polarization, weight of anodic films referred to a unit of the sample surface has been determined. Thus, the film covering lead-antimony alloy sample has the maximal weight, whereas the oxidation products on the pure lead surface have the lowest one. Among low-antimony alloys, the highest corrosion resistance has been found out with the samples alloyed by a low amount of silver. The microstructure of the castings surface has been analysed. Process of corrosion has been considered in connection with size of grains.

  5. Oxidation and mobilization of metallic antimony in aqueous systems with simulated groundwater

    NASA Astrophysics Data System (ADS)

    Ilgen, A. G.; Majs, F.; Barker, A. J.; Douglas, T. A.; Trainor, T. P.

    2014-05-01

    Antimony (Sb) is a contaminant of concern that can be present in elevated concentrations in shooting range soils due to mobilization from spent lead/antimony bullets. Antimony in shooting range soils has been observed as either metallic Sb(0) or as Sb(V) immobilized by iron (hydr)oxides. The absence of Sb(III) in soils is indicative of rapid Sb(III) oxidation to Sb(V) under surface soil conditions. However, the major controls on antimony oxidation and mobility are poorly understood. To better understand these controls we performed multiple batch experiments under oxic conditions to quantify the oxidation and dissolution of antimony in systems where Sb(0) is oxidized to Sb(III) and further to Sb(V). We also tested how variations in the aqueous matrix composition and the presence of metallic lead (Pb) affect the dissolution, solid phase speciation, and oxidation of antimony. We monitored changes in the aqueous antimony speciation using liquid chromatography inductively coupled plasma mass spectrometry (LC-ICP-MS). To test which solid phases form as a result of Sb(0) oxidation, and therefore potentially limit the mobility of antimony in our studied systems, we characterized the partially oxidized Sb(0) powders by means of extended X-ray absorption fine structure (EXAFS) spectroscopy and powder X-ray diffraction (XRD).

  6. Intermolecular interaction of thiosemicarbazone derivatives to solvents and a potential Aedes aegypti target

    NASA Astrophysics Data System (ADS)

    da Silva, João Bosco P.; Hallwass, Fernando; da Silva, Aluizio G.; Moreira, Diogo Rodrigo; Ramos, Mozart N.; Espíndola, José Wanderlan P.; de Oliveira, Ana Daura T.; Brondani, Dalci José; Leite, Ana Cristina L.; Merz, Kenneth M.

    2015-08-01

    DFT calculations were used to access information about structure, energy and electronic properties of series of phenyl- and phenoxymethyl-(thio)semicarbazone derivatives with demonstrated activity against the larvae of Aedes aegypti in stage L4. The way as the thiosemicarbazone derivatives can interact with solvents like DMSO and water were analyzed from the comparison between calculated and experimental 1H NMR chemical shifts. The evidences of thiosemicarbazone derivatives making H-bond interaction to solvent have provide us insights on how they can interact with a potential A. aegypti's biological target, the Sterol Carrier Protein-2.

  7. Spectroscopic evaluation of manganese(II) complexes derived from semicarbazones and thiosemicarbazones

    NASA Astrophysics Data System (ADS)

    Chandra, Sulekh; Gupta, Lokesh Kumar

    2005-09-01

    Manganese(II) complexes having the general composition Mn(L) 2X 2 [where L = isopropyl methyl ketone semicarbazone (LLA), isopropyl methyl ketone thiosemicarbazone (LLB), 4-aminoacetophenone semicarbazone (LLC) and 4-aminoacetophenone thiosemicarbazone (LLD) and X = Cl -, 1/2SO 42-] have been synthesized. All the complexes were characterized by elemental analyses, molar conductance, magnetic moment susceptibility, EI-mass, 1H NMR, IR, EPR and electronic spectral studies. All the complexes show magnetic moments corresponding to five unpaired electrons. The possible geometries of the complexes were assigned on the basis of EPR, electronic and infrared spectral studies.

  8. EPR, mass, IR, electronic, and magnetic studies on copper(II) complexes of semicarbazones and thiosemicarbazones

    NASA Astrophysics Data System (ADS)

    Chandra, Sulekh; Gupta, Lokesh Kumar

    2005-01-01

    Copper(II) complexes having the general composition Cu(L) 2X 2 [where L = isopropyl methyl ketone semicarbazone (LLA), isopropyl methyl ketone thiosemicarbazone (LLB), 4-aminoacetophenone semicarbazone (LLC), and 4-aminoacetophenone thiosemicarbazone (LLD) and X = Cl -, 1/2SO 42-] have been synthesized. All the Cu(II) complexes reported here have been characterized by elemental analyses, molar conductance, magnetic moment susceptibility, EI mass, 1H NMR, IR, EPR, and electronic spectral studies. All the complexes were found to have magnetic moments corresponding to one unpaired electrons. The possible geometries of the complexes were assigned on the basis of EPR, electronic, and infrared spectral studies.

  9. Manganese(II) complexes of substituted di-2-pyridyl ketone thiosemicarbazones: Structural and spectral studies

    NASA Astrophysics Data System (ADS)

    Philip, Varughese; Suni, V.; Kurup, Maliyeckal R. Prathapachandra; Nethaji, Munirathinam

    2006-05-01

    The reaction between manganese(II) acetate and two substituted thiosemicarbazones derived from di-2-pyridyl ketone (HL) in 1:2 molar ratio produces new complexes of general formula [MnL 2]. The thiosemicarbazone moiety in HL deprotonates and gets coordinated to Mn(II) through the azomethine nitrogen, one of the pyridyl nitrogens, and the thiolate sulfur in both the complexes. The crystal structure of [ MnL21] was established by single crystal X-ray diffraction and the compound crystallizes into a monoclinic lattice with P2 1/ c space group. Manganese(II) exists in a distorted octahedral geometry in the complexes.

  10. Testing of antimony selective media for treatment of liquid radwaste

    SciTech Connect

    Yarnell, P.A.

    2007-07-01

    Nuclear power plants have sought radiation source term reduction and reduced discharge of radioactive constituents for many years. In the case of pressurized water reactors (PWRs), the latter efforts have been directed toward capture and immobilization of recalcitrant (ubiquitous radionuclides with long half-lives) species such as Cs-134 and Cs-137 and Co-58 and Co-60. As these plants resolved, or at least mitigated, the problems with radiocesium and radio-cobalt, antimony radionuclides (Sb-122, Sb-124, and Sb-125) have become a primary concern in liquid liquid radwaste systems Graver Technologies developed a granular composite metal oxide media with good selectivity for radio-antimony. Initial laboratory data were collected using non-radioactive salts of antimony, cesium, and cobalt to judge efficacy of selective removal of antimony. Based on success of those trials, the media, designated Gravex GX187, was tested in partnership with Energy Solutions (nee Duratek) using actual liquid liquid radwaste in two PWR plants. One of these plants performed extensive slip-stream trials comparing the GX187 with strong base anion resins. With more than 2500 bed volumes of throughput, the GX187 outperformed the other competitors by reducing both Sb-124 and Sb-125 radionuclides below minimum detectable activity (MDA) with average decontamination factors (DF's) of 170, even when subjected to high levels of borate. Based on these favorable results, Energy Solutions installed the GX187 in a layered bed in their ALPS liquid radwaste processing system at this plant in August 2005. After one year of intermittent, batchwise operation including an outage, the GX187 processed more than 2.25 million liters (>600,000 gallons) of liquid liquid radwaste while reducing the Sb-125 activity to 2.9 E-08 Bq/L (DF=111) on average. This evaluation is ongoing and will continue at least until the fall 2006 outage at this plant. Concurrently, Graver developed a second generation antimony selective

  11. New antimony substituted Mg-Al layered double hydroxides.

    PubMed

    Kim, Jin A; Hwang, Seong-Ju; Choy, Jin-Ho

    2008-10-01

    No antimony hydroxide has been previously reported not only in solid state but also in aqueous solution, surely due to the fact that the formation of antimony oxide, Sb2O3, is thermodynamically more favorable than that of the hydroxide phase, Sb(OH)3. According to the pH dependent solubility diagram of Sb2O3, antimony (III) hydroxide may not exist as a definite compound but be proposed as a hydrated monomeric molecular species, Sb(OH)3(aq), which is in equilibrium with Sb2O3, under a condition of very small ionic strength. This is probably the reason why no Sb(3+)-containing layered double hydroxide, LDH, has been reported as yet. In the present study, an attempt has been made to prepare new Sb(3+)-LDH by substituting the Al3+ in octahedral site partially with Sb3+ up to approximately 10%. From the X-ray diffraction analysis, we found that the lattice constants (a = 3.075 angstroms, c = 23.788 angstroms) of the pristine, Mg-Al LDH, increased gradually upto those (a = 3.087 angstroms, c = 24.167 angstroms) of Sb-LDH (8%-substituted). Beyond 10%, the Sb substitution does not lead to any further increases of lattice constants but the impurity Sb2O3 phase is formed. It is, therefore, concluded that the solubility limit of Sb3+ in LDH would be around 10%. In addition, we were able to determine the chemical formula of Sb-substituted LDHs as follows, Mg4Al(1-x)Sb(x)OH10(CO3)(1/2) x H2O (x = 0 approximately 0.08) on the basis of energy dispersive X-ray spectroscopy. PMID:19198414

  12. The Hydrothermal Chemistry of Gold, Arsenic, Antimony, Mercury and Silver

    SciTech Connect

    Bessinger, Brad; Apps, John A.

    2003-03-23

    A comprehensive thermodynamic database based on the Helgeson-Kirkham-Flowers (HKF) equation of state was developed for metal complexes in hydrothermal systems. Because this equation of state has been shown to accurately predict standard partial molal thermodynamic properties of aqueous species at elevated temperatures and pressures, this study provides the necessary foundation for future exploration into transport and depositional processes in polymetallic ore deposits. The HKF equation of state parameters for gold, arsenic, antimony, mercury, and silver sulfide and hydroxide complexes were derived from experimental equilibrium constants using nonlinear regression calculations. In order to ensure that the resulting parameters were internally consistent, those experiments utilizing incompatible thermodynamic data were re-speciated prior to regression. Because new experimental studies were used to revise the HKF parameters for H2S0 and HS-1, those metal complexes for which HKF parameters had been previously derived were also updated. It was found that predicted thermodynamic properties of metal complexes are consistent with linear correlations between standard partial molal thermodynamic properties. This result allowed assessment of several complexes for which experimental data necessary to perform regression calculations was limited. Oxygen fugacity-temperature diagrams were calculated to illustrate how thermodynamic data improves our understanding of depositional processes. Predicted thermodynamic properties were used to investigate metal transport in Carlin-type gold deposits. Assuming a linear relationship between temperature and pressure, metals are predicted to predominantly be transported as sulfide complexes at a total aqueous sulfur concentration of 0.05 m. Also, the presence of arsenic and antimony mineral phases in the deposits are shown to restrict mineralization within a limited range of chemical conditions. Finally, at a lesser aqueous sulfur

  13. Growth and Characterization of Bismuth and Antimony Thin Films

    NASA Astrophysics Data System (ADS)

    Martinez, A.; Berrios, A. R.; Collazo, R.; Garcia, J. L.; Ducoudray, G. O.

    1996-03-01

    We have grown thin films of bismuth and antimony using hot wall epitaxy. The polycrystalline films were grown onto (111)-silicon substrates. The chemical integrity of the films was established using Auger electron spectroscopy. The crystallographical properties of the films were assessed using x-ray diffraction techniques. We will report on the results of these characterization efforts, as well as, on the growth apparatus and process. Work supported in part by NSWC-CRADA 93-01 and EPSCoR-NSF Grant EHR-9108775

  14. A novel series of thiosemicarbazone drugs: from synthesis to structure.

    PubMed

    Ebrahimi, Hossein Pasha; Hadi, Jabbar S; Alsalim, Tahseen A; Ghali, Thaer S; Bolandnazar, Zeinab

    2015-02-25

    A new series of thiosemicarbazones (TSCs) and their 1,3,4-thiadiazolines (TDZs) containing acetamide group have been synthesized from thiosemicarbazide compounds by the reaction of TSCs with cyclic ketones as well as aromatic aldehydes. The structures of newly synthesized 1,3,4-thiadiazole derivatives obtained by heterocyclization of the TSCs with acetic anhydride were experimentally characterized by spectral methods using IR, (1)H NMR, (13)C NMR and mass spectroscopic methods. Furthermore, the structural, thermodynamic, and electronic properties of the studied compounds were also studied theoretically by performing Density Functional Theory (DFT) to access reliable results to the experimental values. The molecular geometry, the highest occupied molecular orbital (HOMO), the lowest unoccupied molecular orbital (LUMO) and Mulliken atomic charges of the studied compounds have been calculated at the B3LYP method and standard 6-31+G(d,p) basis set starting from optimized geometry. The theoretical (13)C chemical shift results were also calculated using the gauge independent atomic orbital (GIAO) approach and their respective linear correlations were obtained. PMID:25291504

  15. A novel series of thiosemicarbazone drugs: From synthesis to structure

    NASA Astrophysics Data System (ADS)

    Ebrahimi, Hossein Pasha; Hadi, Jabbar S.; Alsalim, Tahseen A.; Ghali, Thaer S.; Bolandnazar, Zeinab

    2015-02-01

    A new series of thiosemicarbazones (TSCs) and their 1,3,4-thiadiazolines (TDZs) containing acetamide group have been synthesized from thiosemicarbazide compounds by the reaction of TSCs with cyclic ketones as well as aromatic aldehydes. The structures of newly synthesized 1,3,4-thiadiazole derivatives obtained by heterocyclization of the TSCs with acetic anhydride were experimentally characterized by spectral methods using IR, 1H NMR, 13C NMR and mass spectroscopic methods. Furthermore, the structural, thermodynamic, and electronic properties of the studied compounds were also studied theoretically by performing Density Functional Theory (DFT) to access reliable results to the experimental values. The molecular geometry, the highest occupied molecular orbital (HOMO), the lowest unoccupied molecular orbital (LUMO) and Mulliken atomic charges of the studied compounds have been calculated at the B3LYP method and standard 6-31+G(d,p) basis set starting from optimized geometry. The theoretical 13C chemical shift results were also calculated using the gauge independent atomic orbital (GIAO) approach and their respective linear correlations were obtained.

  16. Targeting Iron in Colon Cancer via Glycoconjugation of Thiosemicarbazone Prochelators.

    PubMed

    Akam, Eman A; Tomat, Elisa

    2016-08-17

    The implication of iron in the pathophysiology of colorectal cancer is documented at both the biochemical and epidemiological levels. Iron chelators are therefore useful molecular tools for the study and potential treatment of this type of cancer characterized by high incidence and mortality rates. We report a novel prochelation strategy that utilizes a disulfide redox switch to connect a thiosemicarbazone iron-binding unit with carbohydrate moieties targeting the increased expression of glucose transporters in colorectal cancer cells. We synthesized three glycoconjugates (GA2TC4, G6TC4, and M6TC4) with different connectivity and/or carbohydrate moieties, as well as an aglycone analog (ATC4). The sugar conjugates present increased solubility in neutral aqueous solutions, and the ester-linked conjugates M6TC4 and G6TC4 compete as effectively as d-glucose for transporter-mediated cellular uptake. The glycoconjugates show improved selectivity compared to the aglycone analog and are 6-11 times more toxic in Caco-2 colorectal adenocarcinoma cells than in normal CCD18-co colon fibroblasts. PMID:27471913

  17. Synthesis, spectroscopic studies and crystal structure of ( E)-2-(2,4-dihydroxybenzylidene)thiosemicarbazone and ( E)-2-[(1 H-indol-3-yl)methylene]thiosemicarbazone

    NASA Astrophysics Data System (ADS)

    Yıldız, Mustafa; Ünver, Hüseyin; Erdener, Diğdem; Kiraz, Aşkın; İskeleli, Nazan Ocak

    2009-02-01

    Thiosemicarbazone Schiff bases ( 1 and 2) derived from 2,4-dihydroxybenzaldehyde, indoline-3-carbaldehyde and thiosemicarbazone have been synthesized and their structures were elucidated by elemental analysis, FT-IR, 1H NMR, 13C NMR and UV-visible spectroscopic techniques. The structures of compounds 1 and 2 have also been examined cyrstallographically. The title compounds 1 and 2 crystallize in the monoclinic space group C2/ c and triclinic space group P1¯, with unit cell parameters: a = 21.421(1) and 7.233(1), b = 4.131(1) and 11.166(1), c = 24.942(2) and 13.648(1) Å, V = 1856.1(2) and 1019.5(1) Å 3, D x = 1.512 and 1.422 g cm -3 and Z = 8 and 4, respectively.

  18. Anti-HIV activity of thiosemicarbazone and semicarbazone derivatives of (+/-)-3-menthone.

    PubMed

    Mishra, Vibha; Pandeya, S N; Pannecouque, Christophe; Witvrouw, Myriam; De Clercq, E

    2002-05-01

    A series of thiosemicarbazones and semicarbazone derivatives of (+/-)-3-menthone have been synthesized and their anti-HIV activity evaluated against HIV-1(III(B))and HIV-2 (ROD). The studies revealed that maximum protection is offered by chloro-substituted derivatives 2 and 7 against HIV-1 (III(B)) and HIV-2 (ROD). PMID:12210774

  19. The wide pharmacological versatility of semicarbazones, thiosemicarba-zones and their metal complexes.

    PubMed

    Beraldo, Heloisa; Gambino, Dinorah

    2004-01-01

    The more significant bioactivities of a variety of semicarbazones (anti-protozoa, anticonvulsant) and thiosemicarbazones (antibacterial, antifungal, antitumoral, antiviral) and their metal complexes are reviewed together with proposed mechanisms of action and structure-activity relationships. Clinical or potential pharmacological applications of these versatile compounds are discussed. PMID:14754441

  20. Insights into the binding of thiosemicarbazone derivatives with human serum albumin: spectroscopy and molecular modelling studies.

    PubMed

    Karthikeyan, Subramani; Bharanidharan, Ganesan; Kesherwani, Manish; Mani, Karthik Ananth; Srinivasan, Narasimhan; Velmurugan, Devadasan; Aruna, Prakasarao; Ganesan, Singaravelu

    2016-06-01

    4-[(1Z)-1-(2-carbamothioylhydrazinylidene)ethyl]phenyl acetate [Ace semi],4-[(1Z)-1-(2-carbamothioylhydrazinylidene)ethyl]phenyl propanoate [Pro semi] from the family of thiosemicarbazones derivative has been newly synthesized. It has good anticancer activity as well as antibacterial and it is also less toxic in nature, its binding characteristics are therefore of huge interest for understanding pharmacokinetic mechanism of the drug. The binding of thiosemicarbazone derivative to human serum albumin (HSA) has been investigated by studying its quenching mechanism, binding kinetics and the molecular distance (r) between donor (HSA) and acceptor (thiosemicarbazone derivative) was estimated according to Forster's theory of non-radiative energy transfer using fluorescence spectroscopy. The binding dynamics has been elaborated using synchronous fluorescence spectroscopy, and the feature of thiosemicarbazone derivative induced structural changes of HSA has been studied by circular dichorism, Fourier transform infrared spectroscopy. Molecular modelling simulations explore the hydrophobic interaction and hydrogen bonding which stabilizes the interaction. PMID:26368536

  1. Antimony sulphide, an absorber layer for solar cell application

    NASA Astrophysics Data System (ADS)

    Ali, N.; Hussain, Arshad; Ahmed, R.; Shamsuri, W. N. Wan; Shaari, A.; Ahmad, N.; Abbas, S. M.

    2016-01-01

    Replacement of the toxic, expensive and scarce materials with nontoxic, cheap and earth-abundant one, in solar cell absorber layer, is immensely needed to realize the vision of green and sustainable energy. Two-micrometre-thin antimony sulphide film is considered to be adequate as an absorbing layer in solar cell applications. In this paper, we synthesize antimony sulphide thin films on glass substrate by physical vapour deposition technique, and the obtained films were then annealed at different temperatures (150-250 °C). The as-deposited and annealed samples were investigated for structural and optoelectronic properties using different characterization techniques. The X-ray diffraction analysis showed that the annealed samples were polycrystalline with Sb2S3 phase, while the as-deposited sample was amorphous in nature. The optical properties are measured via optical ellipsometric techniques. The measured absorbance of the film is adequately high, and every photon is found to be absorbed in visible and NIR range. The conductivity type of the films measured by hot-point probe technique is determined to be p-type. The optical band gap of the resulted samples was in the range (2.4-1.3 eV) for the as-deposited and annealed films.

  2. Alkali oxide-tantalum, niobium and antimony oxide ionic conductors

    NASA Technical Reports Server (NTRS)

    Roth, R. S.; Brower, W. S.; Parker, H. S.; Minor, D. B.; Waring, J. L.

    1975-01-01

    The phase equilibrium relations of four systems were investigated in detail. These consisted of sodium and potassium antimonates with antimony oxide and tantalum and niobium oxide with rubidium oxide as far as the ratio 4Rb2O:llB2O5 (B=Nb, Ta). The ternary system NaSbO3-Sb2O4-NaF was investigated extensively to determine the actual composition of the body centered cubic sodium antimonate. Various other binary and ternary oxide systems involving alkali oxides were examined in lesser detail. The phases synthesized were screened by ion exchange methods to determine mobility of the mobility of the alkali ion within the niobium, tantalum or antimony oxide (fluoride) structural framework. Five structure types warranted further investigation; these structure types are (1) hexagonal tungsten bronze (HTB), (2) pyrochlore, (3) the hybrid HTB-pyrochlore hexagonal ordered phases, (4) body centered cubic antimonates and (5) 2K2O:3Nb2O5. Although all of these phases exhibit good ion exchange properties only the pyrochlore was prepared with Na(+) ions as an equilibrium phase and as a low porosity ceramic. Sb(+3) in the channel interferes with ionic conductivity in this case, although relatively good ionic conductivity was found for the metastable Na(+) ion exchanged analogs of RbTa2O5F and KTaWO6 pyrochlore phases.

  3. Antimony contamination and its effect on Trifolium plants

    NASA Astrophysics Data System (ADS)

    Corrales, Isabel; Barceló, Juan; Bech, Jaume; Poschenrieder, Charlotte

    2014-05-01

    Antimony is not an essential element and soil Sb contents usually are low.However, soil contamination by Sb has increased in the last years due to the human activities (combustion of fossil fuels, mining, waste incineration, smelting, shooting and road traffic). The main objective of this work was to study the effect of different concentrations of antimony (KSb(OH)6) in order to evaluate the effect on growth and Sb uptake on Trifolium pratense cv. Milvus and Trifolium repens. Our results show that Sb accumulated both in roots and shoots of clover without any negative effect on root growth, cellular viability and lipid peroxidation. This absence of toxicity sympthoms in clover plants could be very dangerous because Sb can be inadvertedly incorporated into the trophic chain causing toxic effects both in animals and humans. The absence of toxic effects on plants does not seem to be due to detoxification by phytochelatins because the use of the gamma-glutamylcysteine synthetase inhibitor, L-buthionine-[S,R]-sulphoximine (BSO) did not enhance Sb toxicity to plants. (Supported by the Spanish MICINN project BFU2010-14873)

  4. Electronic band structure calculations of bismuth-antimony nanowires

    NASA Astrophysics Data System (ADS)

    Levin, Andrei; Dresselhaus, Mildred

    2012-02-01

    Alloys of bismuth and antimony received initial interest due to their unmatched low-temperature thermoelectric performance, and have drawn more recent attention as the first 3D topological insulators. One-dimensional bismuth-antimony (BiSb) nanowires display interesting quantum confinement effects, and are expected to exhibit even better thermoelectric properties than bulk BiSb. Due to the small, anisotropic carrier effective masses, the electronic properties of BiSb nanowires show great sensitivity to nanowire diameter, crystalline orientation, and alloy composition. We develop a theoretical model for calculating the band structure of BiSb nanowires. For a given crystalline orientation, BiSb nanowires can be in the semimetallic, direct semiconducting, or indirect semiconducting phase, depending on nanowire diameter and alloy composition. These ``phase diagrams'' turn out to be remarkably similar among the different orientations, which is surprising in light of the anisotropy of the bulk BiSb Fermi surface. We predict a novel direct semiconducting phase for nanowires with diameter less than ˜15 nm, over a narrow composition range. We also find that, in contrast to the bulk and thin film BiSb cases, a gapless state with Dirac dispersion cannot be realized in BiSb nanowires.

  5. Periodic macroporous nanocrystalline antimony-doped tin oxide electrode.

    PubMed

    Arsenault, Eric; Soheilnia, Navid; Ozin, Geoffrey A

    2011-04-26

    Optically transparent and electrically conductive electrodes are ubiquitous in the myriad world of devices. They are an indispensable component of solar and photoelectrochemical cells, organic and polymer light emitting diodes, lasers, displays, electrochromic windows, photodetectors, and chemical sensors. The majority of the electrodes in such devices are made of large electronic band-gap doped metal oxides fashioned as a dense low-surface-area film deposited on a glass substrate. Typical transparent conducting oxide materials include indium-, fluorine-, or antimony-doped tin oxides. Herein we introduce for the first time a transparent conductive periodic macroporous electrode that has been self-assembled from 6 nm nanocrystalline antimony-doped tin oxide with high thermal stability, optimized electrical conductivity, and high quality photonic crystal properties, and present an electrochemically actuated optical light switch built from this electrode, whose operation is predicated on its unique combination of electrical, optical, and photonic properties. The ability of this macroporous electrode to host active functional materials like dyes, polymers, nanocrystals, and nanowires provides new opportunities to create devices with improved performance enabled by the large area, spatially accessible and electroactive internal surface. PMID:21391718

  6. Exploring antimony isotope ratio variations for provenancing purposes

    NASA Astrophysics Data System (ADS)

    Lobo, L.; Degryse, P.; Vanhaecke, F.

    2012-04-01

    Production sites and trade routes of Roman glass have received much attention over the past decade. It is assumed that raw glass was produced in primary workshops near the raw material sources used, to be transported to secondary glass houses. Colourless glass was a particularly prestigious material in this process, difficult to make. It has been looked at from the perspective of the provenance of its sand and flux, but rarely from the perspective of the origin of the decolourizing material. In effect, for the production of early Roman colourless glass, antimony was used, deliberately added under the form of Sb-bearing minerals. Isotopic analysis of Sb ores could help identify the origin of the decolorizing agent present in Roman glasses and, consequently, to reconstruct how such material was traded and transported, and how this can be integrated in the network of primary and secondary glass producers. In this work, variations in the isotopic composition of Sb in different ore sources (stibnites) are explored using multi-collector ICP - mass spectrometry. A new method is proposed, where Sb is directly analysed for its isotopic composition using MC-ICP-MS after chromatographic isolation of the target element from a sample digest. The isotopic composition of the selected materials shows variations up to 6 ?-units relative to an antimony standard solution. Indium was used as internal standard for correction for instrumental mass discrimination and an external precision for the 123Sb/121Sb ratio of 0.01% RSD was obtained

  7. Polyimide Precursor Solid Residuum

    NASA Technical Reports Server (NTRS)

    Weiser, Erik S. (Inventor); St.Clair, Terry L. (Inventor); Echigo, Yoshiaki (Inventor); Kaneshiro, Hisayasu (Inventor)

    2001-01-01

    A polyimide precursor solid residuum is an admixture of an aromatic dianhydride or derivative thereof and an aromatic diamine or derivative thereof plus a complexing agent, which is complexed with the admixture by hydrogen bonding. The polyimide precursor solid residuum is effectively employed in the preparation of polyimide foam and the fabrication of polyimide foam structures.

  8. Antimony in the environment: A review focused on natural waters. III. Microbiota relevant interactions

    NASA Astrophysics Data System (ADS)

    Filella, Montserrat; Belzile, Nelson; Lett, Marie-Claire

    2007-02-01

    Antimony is ubiquitously present in the environment as a result of natural processes and human activities. Antimony is not considered to be an essential element for plants or animals. In this third review paper on the occurrence of antimony in natural waters, the interactions of antimony with microbiota are discussed in relation to its fate in natural waters. This paper covers the following aspects: occurrence in microbiota, uptake transport mechanisms, pathways of Sb(III) removal from cells involved in antimony tolerance, oxidation and reduction of antimony by living organisms, phytochelatin induction and biomethylation. This review is based on a careful and systematic examination of a comprehensive collection of papers on the above mentioned aspects of the subject. All data are quoted from the original sources. Relatively little existing information falls within the strict scope of this review and, when relevant, discussion on the interactions of antimony with reference microorganisms, such as Escherichia coli, Saccharomyces cerevisiae and different protozoan parasites of the genus Leishmania, has been included.

  9. Immobilization of antimony waste slag by applying geopolymerization and stabilization/solidification technologies.

    PubMed

    Salihoglu, Güray

    2014-11-01

    During the processing of antimony ore by pyrometallurgical methods, a considerable amount of slag is formed. This antimony waste slag is listed by the European Union as absolutely hazardous waste with a European Waste Catalogue code of 10 08 08. Since the levels of antimony and arsenic in the leachate of the antimony waste slag are generally higher than the landfilling limits, it is necessary to treat the slag before landfilling. In this study, stabilization/solidification and geopolymerization technologies were both applied in order to limit the leaching potential of antimony and arsenic. Different combinations ofpastes by using Portland cement, fly ash, clay, gypsum, and blast furnace slag were prepared as stabilization/solidification or geopoljymer matrixes. Sodium silicate-sodium hydroxide solution and sodium hydroxide solution at 8 M were used as activators for geopolymer samples. Efficiencies of the combinations were evaluated in terms of leaching and unconfined compressive strength. None of the geopolymer samples prepared with the activators yielded arsenic and antimony leaching below the regulatory limit at the same time, although they yielded high unconfined compressive strength levels. On the other hand, the stabilization/solidification samples prepared by using water showed low leaching results meeting the landfilling criteria. Use of gypsum as an additive was found to be successful in immobilizing the arsenic and antimony. PMID:25509550

  10. Removal of arsenic and antimony from anode slime by vacuum dynamic flash reduction.

    PubMed

    Lin, Deqiang; Qiu, Keqiang

    2011-04-15

    Anode slime is an important material of recycling precious metals. Up to now, treating the arsenic- and antimony-rich anode slime by conventional processes has the following problems: its economic and environmental effect is less than satisfactory, and the removal effect of arsenic and antimony from anode slime in present processes is not all that could be desired. Therefore, vacuum dynamic flash reduction, a new process for treating arsenic- and antimony-rich anode slime, was investigated in this work. During vacuum dynamic flash reduction, silver from the arsenic- and antimony-rich anode slime was left behind in the distilland as the silver alloy, and trivalent oxides of arsenic and antimony were evaporated in the distillate. The experimental results showed that the evaporation percent of the arsenic- and antimony-rich anode slime was 65.6%. Namely, 98.92% by weight of arsenic and 93.67% by weight of antimony can be removed under the following experimental conditions: temperature of 1083 K, vacuum evaporation time of 60 min, and air flow rate of 400 mL/min corresponding to the residual gas pressure of 250 Pa. Moreover, vacuum treatment eliminates much of the air pollution and material losses associated with other conventional treatment methods. PMID:21446728

  11. A green synthesis route for the phase and size tunability of copper antimony sulfide nanocrystals with high yield.

    PubMed

    Chen, Keqiang; Zhou, Jing; Chen, Wen; Chen, Qiao; Zhou, Peng; Liu, Yueli

    2016-03-01

    Until now, it is a great challenge for the controllable synthesis of copper antimony sulfide (CAS) nanocrystals (NCs), as the reactivity of precursors is quite difficult to be controlled during the synthesis process. In the present work, a novel solution-based method is proposed to synthesize CAS NCs by choosing N,N'-diphenylthiourea as the sulfide precursor, which is favorable for balancing the relative reactivity of Cu and Sb ions. It is found that three phases (CuSbS2, Cu12Sb4S13 and Cu3SbS4) of CAS NCs with size tunability were successfully synthesized for the first time. To the best of our knowledge, the lowest reaction temperature of 110 °C and the highest yield over 90% for CAS NCs were also achieved for the first time, which may be considered to be a green synthesis route compared with other conventional methods. Optical properties indicate that the as-prepared CAS NCs have strong optical absorption in the visible light region of the solar spectrum, and we also observed the band gap tunability of CuSbS2 and Cu3SbS4 materials for the first time. PMID:26875832

  12. Growth and Characterization of Co-Doped Fluorine and Antimony in Tin Oxide Thin Films Obtained by Ultrasonic Spray Pyrolysis

    NASA Astrophysics Data System (ADS)

    Gaewdang, Thitinai; Wongcharoen, Ngamnit

    Fluorine (F)-doped, antimony (Sb)-doped, fluorine and antimony co-doped tin oxide (SnO2) thin films were prepared by ultrasonic spray pyrolysis technique using SnCl2, NH4F and SbCl3 as precursors of Sn, F and Sb elements respectively. F and Sb doping concentrations carried out from 1 to 20 wt% and 1 to 4 wt% in F-doped and Sb-doped SnO2 films respectively. In F and Sb co-doped SnO2 films, the proportions of F and Sb to Sn in starting solution were 15 and 2 wt% respectively. XRD patterns showed that the preferred orientation of SnO2:F, SnO2:Sb and SnO2:F, Sb is dependent on the doping concentration. The variation of doping concentration and preferred orientation of the films was reflected in their morphology as investigated by SEM. The electrical properties of the films were performed by Hall effect measurements in van der Pauw configuration. The minimum resistivity values of SnO2:F and SnO2:Sb were found in the films doped with 15 wt% of F and 2 wt% of Sb. However, The minimum of resistivity value of F and Sb co-doped SnO2 films is not better than neither the one of F-doped nor the one of Sb-doped SnO2 films. The optical transmission of SnO2:F films was found to increase with increasing in F doping concentration. Whereas the optical transmission of SnO2:Sb was found to decrease with increasing in Sb concentration. The F and Sb co-doped SnO2 films annealed in three different conditions at 500°C show the lower transmission values than the value obtained in the as-prepared SnO2:F, Sb films.

  13. [Differentiation activity of pyridoxal thiosemicarbazone and its copper and cobalt complexes on Friend erythroleukemia cells].

    PubMed

    Albertini, R; Gasparri Fava, G; Pinelli, S; Tarasconi, P; Starcich, B

    1991-07-01

    Thiosemicarbazones are a wide group of organic derivatives whose biological activities are a function of the parent aldehyde or ketone and of the coordination metal type. Some thiosemicarbazones possess a broad spectrum of potentially useful chemotherapeutic properties (antitumor, antibacterial, antiviral, antimalarial). The present study reports the biological effects of pyridoxal thiosemicarbazone, H2L, and relative complexes with copper, [(Cu(HL)(OH2))2]++ and with cobalt, [Co(III)(L)(HL)] on the differentiation of Friend erythroleukemia cells (FLC). They are murine proerythroblasts chronically infected by a producing Friend leukemia virus complex; their exposure to dimethylsulfoxide (Me2SO) or other chemical agents induces these cells to terminal erythroid differentiation, therefore these cells represent a good model of differentiation in vitro. Here we describe induction differentiation experiment of pyridoxal thiosemicarbazone and relative complexes of copper and cobalt on FLC performed with concentrations of 50 ug/ml (ligand), 2 ug/ml (complexes). These have little effects on cell proliferation at doses used in these experiments. Higher doses have evident cytotoxic effects. The treatment with the copper complex induces a moderate differentiation of FLC and enhances effects on erythroid differentiation of Me2SO-induced FLC. On the contrary H2L and [Co(III)(L)(HL)] haven't inducing effects or enhancing effects on Me2SO-induced FLC hemopoietic differentiation. In conclusion, the present study shows that copper complexes of pyridoxal thiosemicarbazone exert action of inducing agent and are able to enhance Me2SO-induced FLC hemopoietic differentiation. PMID:1818592

  14. Structural and optical characterization of thermally evaporated bismuth and antimony films for photovoltaic applications

    NASA Astrophysics Data System (ADS)

    Srimathy, N.; Ruban Kumar, A.

    2016-05-01

    In this present study, the thin film of bismuth and antimony is coated by thermal evaporation system equipped with the inbuilt ultra high vacuum system. XRD analysis confirmed the rhombohedral structure of Bismuth and Antimony on the prepared film. The surface roughness and physical appearance is analyzed by Atomic force microscopy. The results of Raman Spectroscopy show the wave functions and the spectrum of electrons. The preparation technique and conditions strongly influence the crystalline structure and the phase composition of bismuth and antimony thin films. The electrical and optical properties for the prepared film are analyzed. The results show a great interest and promising applications in Photovoltaic devices.

  15. Thiosemicarbazone modification of 3-acetyl coumarin inhibits Aβ peptide aggregation and protect against Aβ-induced cytotoxicity.

    PubMed

    Ranade, Dnyanesh S; Bapat, Archika M; Ramteke, Shefali N; Joshi, Bimba N; Roussel, Pascal; Tomas, Alain; Deschamps, Patrick; Kulkarni, Prasad P

    2016-10-01

    Aggregation of amyloid β peptide (Aβ) is an important event in the progression of Alzheimer's disease. Therefore, among the available therapeutic approaches to fight with disease, inhibition of Aβ aggregation is widely studied and one of the promising approach for the development of treatments for Alzheimer's disease. Thiosemicarbazone compounds are known for their variety of biological activities. However, the potential of thiosemicarbazone compounds towards inhibition of Aβ peptide aggregation and the subsequent toxicity is little explored. Herein, we report synthesis and x-ray crystal structure of novel compound 3-acetyl coumarin thiosemicarbazone and its efficacy toward inhibition of Aβ(1-42) peptide aggregation. Our results indicate that 3-acetyl coumarin thiosemicarbazone inhibits Aβ(1-42) peptide aggregation up to 80% compared to the parent 3-acetyl coumarin which inhibits 52%. Further, 3-acetyl coumarin thiosemicarbazone provides neuroprotection against Aβ-induced cytotoxicity in SH-SY5Y cell line. These findings indicate that thiosemicarbazone modification renders 3-acetyl coumarin neuroprotective properties. PMID:26232353

  16. Coordination- and Redox-Noninnocent Behavior of Ambiphilic Ligands Containing Antimony.

    PubMed

    Jones, J Stuart; Gabbaï, François P

    2016-05-17

    Stimulated by applications in catalysis, the chemistry of ambiphilic ligands featuring both donor and acceptor functionalities has experienced substantial growth in the past several years. The unique opportunities in catalysis offered by ambiphilic ligands stem from the ability of their acceptor functionalities to play key roles via metal-ligand cooperation or modulation of the reactivity of the metal center. Ligands featuring group 13 centers, most notably boranes, as their acceptor functionalities have undoubtedly spearheaded these developments, with remarkable results having been achieved in catalytic hydrogenation and hydrosilylation. Motivated by these developments as well as by our fundamental interest in the chemistry of heavy group 15 elements, we became fascinated by the possibility of employing antimony centers as Lewis acids within ambiphilic ligands. The chemistry of antimony-based ligands, most often encountered as trivalent stibines, has historically been considered to mirror that of their lighter phosphorus-based congeners. There is growing evidence, however, that antimony-based ligands may display unique coordination behavior and reactivity. Additionally, despite the diverse Lewis acid and redox chemistry that antimony exhibits, there have been only limited efforts to explore this chemistry within the coordination sphere of a transition metal. By incorporation of antimony into the framework of polydentate ligands in order to enforce the main group metal-transition metal interaction, the effect of redox and coordination events at the antimony center on the structure, electronics, and reactivity of the metal complex may be investigated. This Account describes our group's continuing efforts to probe the coordination behavior, reactivity, and application of ambiphilic ligands incorporating antimony centers. Structural and theoretical studies have established that both Sb(III) and Sb(V) centers in polydentate ligands may act as Z-type ligands toward late

  17. Earthquakes: hydrogeochemical precursors

    USGS Publications Warehouse

    Ingebritsen, Steven E.; Manga, Michael

    2014-01-01

    Earthquake prediction is a long-sought goal. Changes in groundwater chemistry before earthquakes in Iceland highlight a potential hydrogeochemical precursor, but such signals must be evaluated in the context of long-term, multiparametric data sets.

  18. Calcium metal as a scavenger for antimony from aluminum alloys

    SciTech Connect

    Bonsignore, P.V.; Daniels, E.J.; Wu, C.T.

    1994-10-04

    Previous work has shown that trace amounts of antimony (Sb) can affect the mechanical properties of strontium (Sr) modified aluminum castings. ANL has been investigating technology to remove or neutralize Sb to reduce its negative effect on the physical properties of those alloys. Review of past work on processing and recovery of scrap aluminum inferred that calcium (Ca) is an effective scavenger of Sb, bismuth, lead and cadmium. Following up on that lead, we have found that Ca is, indeed, effective for removing Sb from molten aluminum alloys although its effectiveness can be compromised by a wide range of processing conditions. A minimum ratio of about four to one, by weight, of Ca to Sb appears necessary to insure an effective scavenging of contained Sb.in 356 aluminum alloys.

  19. Diameter Dependence of the Transport Properties of Antimony Telluride Nanowires

    NASA Astrophysics Data System (ADS)

    Zuev, Yuri; Lee, Jin Sook; Park, Hongkun; Kim, Philip

    2010-03-01

    We report measurements of electronic, thermoelectric, and galvanometric properties of individual semimetallic single crystal antimony telluride (Sb2Te3) nanowires. Microfabricated heater and thermometer electrodes were used to probe the transport properties of the nanowires with diameters in the range of 22 - 95nm and temperatures in the range of 2 - 300K. Temperature dependent resistivity varies depending on nanowire diameter. Thermoelectric power (TEP) measurements indicate hole dominant diffusive thermoelectric generation, with an enhancement of the TEP for smaller diameter wires. The large surface-to-volume ratio of Sb2Te3 nanowires makes them an excellent platform to explore novel phenomena in this predicted topological insulator. We investigate mesoscopic magnetoresistance effects in magnetic fields both parallel and perpendicular to the nanowire axis.

  20. Copper, lead, zinc, antimony, and arsenic in Pakistan

    USGS Publications Warehouse

    White, Max Gregg

    1975-01-01

    Copper localities that merit geological investigation are found in the western Chasai District, in North Waziristan Agency, and in the Salt Range in Mianwali and Sargodha Districts. No high-grade deposits have been .reported from these ,areas and if deposits are developed they will likely be low-grade, high-tonnage, disseminated deposits. Those localities reported from Chitral State are too remote and inaccessible to be of interest now. All lead localities found to date are of minor importance; there has been small production at one .locality in Chasai District and in the southern part of the Hazara District. Zinc, antimony, and arsenic are sparse in Pakistan and no important localities of these metals are reported.

  1. Magnesium-Antimony Liquid Metal Battery for Stationary Energy Storage

    SciTech Connect

    Bradwell, DJ; Kim, H; Sirk, AHC; Sadoway, DR

    2012-02-01

    Batteries are an attractive option for grid: scale energy storage applications because of their small footprint and flexible siting. A high-temperature (700 degrees C) magnesium antimony (MgllSb) liquid metal battery comprising a negative electrode of Mg, a molten salt electrolyte (MgCL2-KCl-NaCl), and a positive electrode of Sb is proposed and characterized. Because of the immiscibility of the contiguous salt and metal phases, they stratify by density into three distinct layers. Cells were cycled at rates ranging from 50 to 200 mA/cm(2) and demonstrated up to 69% DC-DC energy efficiency. The self-segregating nature of the battery components and the use Of low-cost materials results in a promising technology for stationary energy storage applications.

  2. Atomistic mechanisms governing structural stability change of zinc antimony thermoelectrics

    SciTech Connect

    Yang, Xiaolong; Lin, Jianping; Qiao, Guanjun; Wang, Zhao

    2015-01-05

    The structural stability of thermoelectric materials is a subject of growing importance for their energy harvesting applications. Here, we study the microscopic mechanisms governing the structural stability change of zinc antimony at its working temperature, using molecular dynamics combined with experimental measurements of the electrical and thermal conductivity. Our results show that the temperature-dependence of the thermal and electrical transport coefficients is strongly correlated with a structural transition. This is found to be associated with a relaxation process, in which a group of Zn atoms migrates between interstitial sites. This atom migration gradually leads to a stabilizing structural transition of the entire crystal framework, and then results in a more stable crystal structure of β–Zn{sub 4}Sb{sub 3} at high temperature.

  3. Silicon quantum dots with counted antimony donor implants

    NASA Astrophysics Data System (ADS)

    Singh, Meenakshi; Pacheco, Jose; Perry, Daniel; Wendt, Joel; Manginell, Ronald; Dominguez, Jason; Pluym, Tammy; Luhman, Dwight; Bielejec, Edward; Lilly, Michael; Carroll, Malcolm

    Antimony donor implants next to silicon quantum dots have been detected with integrated solid-state diode detectors with single ion precision. Devices with counted number of donors have been fabricated and low temperature transport measurements have been performed. Charge offsets, indicative of donor ionization and coupling to the quantum dot, have been detected in these devices. The number of offsets corresponds to 10-50% of the number of donors counted. We will report on tunneling time measurements and spin readout measurements on the donor offsets. This work was performed, in part, at the Center for Integrated Nanotechnologies, a U.S. DOE Office of Basic Energy Sciences user facility. The work was supported by Sandia National Laboratories Directed Research and Development Program. Sandia National Laboratories is a multi-program laboratory operated by Sandia Corporation, a Lockheed-Martin Company, for the U. S. Department of Energy under Contract No. DE-AC04-94AL85000.

  4. Antimony toxicity in the lichen Xanthoria parietina (L.) Th. Fr.

    PubMed

    Paoli, L; Fiorini, E; Munzi, S; Sorbo, S; Basile, A; Loppi, S

    2013-11-01

    In this paper we tested if treating the lichen Xanthoria parietina with Sb-containing solutions causes Sb bioaccumulation as well as physiological and ultrastructural changes. Total and intracellular antimony content in Sb-treated samples increased progressively with increasing concentration in the treatment solutions. Incubation of X. parietina thalli with Sb at concentrations as low as 0.1mM caused a decrease in sample viability, measured as intensity of respiratory activity, and damage to cell membranes, expressed in terms of membrane lipid peroxidation, as well as ultrastructural changes such as plasmolysis, impairment of the thylakoid system of the alga and cytoplasmic lipid droplets. The photosynthetic system hardly responded, at least under the tested experimental conditions. PMID:24001672

  5. Geochemistries of arsenic, antimony, mercury, and related elements in sediments of puget sound

    USGS Publications Warehouse

    Crecelius, E.A.; Bothner, Michael H.; Carpenter, R.

    1975-01-01

    The natural distributions of arsenic, antimony mercury, chromium, cobalt, iron, aluminum, and carbon in the surface sediments of Puget Sound are perturbed by two major anthropogenic sources of trace metals: a copper smelter near Tacoma, Wash., that discharges large amounts of arsenic and antimony, and a chlor-alkali plant in Bellingham, Wash., which, in the recent past, discharged significant amounts of mercury. Arsenic and antimony inputs from the smelter over the past 80 years are evident in sediment cores whose accumulation rates have been determined by the lead-210 technique. An arsenic budget for Puget Sound reveals the importance of atmospheric input resulting from smokestack emissions of the smelter. Chemical extraction studies of sediments showed that more than 82% of the mercury was associated with easily oxidizable organic matter, whereas about 50% of both arsenic and antimony was associated with extractable iron and aluminum compounds.

  6. Concentrations of arsenic, antimony, and boron in steam and steam condensate at The Geysers, California

    USGS Publications Warehouse

    Smith, C.L.; Ficklin, W.H.; Thompson, J.M.

    1987-01-01

    Studies at The Geysers Geothermal Field, California indicate that under some circumstances elements that are transported in the vapor phase can become enriched in the liquid phase. Waters from two condensate traps (steam traps) on steam lines at The Geysers are enriched with arsenic, antimony, and boron compared to the concentrations of these elements in coexisting steam. Concentrations of boron in condensate-trap waters were as high as 160 mg/L, arsenic as high as 35 mg/L, and antimony as high as 200 ??g/L. Enrichment of arsenic, antimony, and boron is at least partially controlled by the partitioning of these elements into the liquid phase, according to their vapor-liquid distribution coefficients, after they are transported in steam. Several of the elements that are most soluble in steam, including arsenic and antimony, are part of the trace-element suite that characterizes precious-metal epithermal ore deposits. ?? 1987.

  7. One-step synthesis and flame retardancy of sheaf-like microcrystal antimony oxychloride.

    PubMed

    Zhou, Jing; Zhao, Hewei; Li, Lidong; Tian, Ming; Han, Jibing; Zhang, Liqun; Guo, Lin

    2011-10-01

    A mild and facile solution route has been developed for large-scale synthesis of sheaf-like antimony oxychloride Sb8O11CI2 (H2O)6 microcrystal at room temperature. The morphologies and structures of the as-prepared products were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). A mechanism for the formation of the sheaf-like microstructure was tentatively proposed. The shape regulation was attributed to the capping mode of the PVP-directed antimony oxychloride crystal. The thermogravimetric and differential thermal analysis (TG/DTA) were employed to investigate thermal decomposition mechanism and temperature-dependent phase transition of antimony oxychloride Sb8O11CI2 (H2O)6 in the air. The flammable property determined by the cone calorimeter showed excellent flame retardancy when applied this antimony oxychloride in poly (vinyl chloride) (PVC) polymer. PMID:22400215

  8. New low-antimony alloy for straps and cycling service in lead-acid batteries

    NASA Astrophysics Data System (ADS)

    Prengaman, R. David

    Lead-antimony alloys used for the positive grids in lead-acid batteries for cycling service have generally used antimony contents of 4.5 wt.% and above. Tubular batteries for cycling service that impart high compression of the active material to the grid surface via gauntlet use alloys with antimony contents as low as 1.5 wt.%. These batteries are generally employed in less-severe cycling service. Value-regulated lead-acid (VRLA) batteries can give good cycling service without lead-antimony in the positive grid, but require a high tin content and high compression. The change in automotive battery positive grid alloys to lead-calcium-tin and the tin contents of VRLA positive grids and straps have dramatically increased the tin content of the recycled grid and strap lead in the USA, Europe, and Australia. The higher tin contents can contaminate the lead used for lead-antimony battery grids and generally must be removed to low levels to meet the specifications. This study describes a low-antimony alloy that contains a substantial amount of tin. The high tin content reduces the rate of corrosion of low-antimony positive grid alloys, improves conductivity, increases the bond between the grid and the active material, and cycles as well as the traditional 5-6 wt.% antimony alloys employed in conventional flat-plate batteries. The alloy is also used as a corrosion-resistant cast-on strap alloy for automotive batteries for high temperature service, as well as for posts, bushings, and connectors for all wet batteries.

  9. Neutron-activation analysis by standard addition and solvent extraction Determination of traces of antimony.

    PubMed

    Alian, A; Shabana, R; Sanad, W; Allam, B; Khalifa, K

    1968-02-01

    The application of neutron activation analysis by standard addition and solvent extraction to the determination of traces of antimony in aluminium and rocks is reported. Three simple extraction procedures, using isopropyl ether, hexone, and tributyl phosphate, are described for the selective separation of radioantimony from interfering radionuclides. Antimony concentration is measured by counting the activities of the (122)Sb and (124)Sb photopeaks at 0.564 and 0.603 MeV. PMID:18960289

  10. Synthesis and Structure-Activity Correlation Studies of Metal Complexes of α-N-heterocyclic Carboxaldehyde Thiosemicarbazones in Shewanella oneidensis

    PubMed Central

    Wilson, Barbara A.; Venkatraman, Ramaiyer; Whitaker, Cedrick; Tillison, Quintell

    2005-01-01

    This investigation involved the synthesis of metal complexes to test the hypothesis that structural changes and metal coordination in pyridine thiosemicarbazones affect cell growth and cell proliferation in vitro. Thiosemicarbazones are well known to possess antitumor, antiviral, antibacterial, antimalarial, and other activities. Extensive research has been carried out on aliphatic, aromatic, heterocyclic and other types of thiosemicarbazones and their metal complexes. Due to the pronounced reactivity exhibited by metal complexes of heterocyclic thiosemicarbazones, synthesis and structural characterization of di-2-pyridylketone 4N-phenyl thiosemicarbazone and diphenyl tin (Sn) and platinum (Pt) complexes were undertaken. Shewanella oneidensis MR-1, a metal ion-reducing bacterium, was used as a model organism to explore the biological activity under aerobic conditions. A comparision of the cytotoxic potential of selected ligand and metal-complex thiosemicarbazones on cell growth in wild type MR-1 and mutant DSP-010 Shewanella oneidensis strains at various concentrations (0, 5, 10, 15, 20 or 25 ppm) was performed. The wild type (MR-1) grown in the presence of increasing concentrations of Sn- thiosemicarbazone complexes was comparatively more sensitive (mean cell number = 4.8 × 108 ± 4.3 × 107 SD) than the DSP-010, a spontaneous rifampicillin derivative of the parent strain (mean cell number = 5.6 × 108 ± 6.4 × 107 SD) under comparable aerobic conditions (p=0.0004). No differences were observed in the sensitivity of the wild and mutant types when exposed to various concentrations of diphenyl Pt- thiosemicarbazone complex (p= 0.425) or the thiosemicarbazone ligand (p=0.313). Growth of MR-1 in the presence of diphenyl Sn- thiosemicarbazone was significantly different among treatment groups (p=0.012). MR-1 cell numbers were significantly higher at 5ppm than at 10 to 20ppm (p = 0.05). The mean number of DSP-010 variant strain cells also differed among diphenyl Sn

  11. Synthesis and structure-activity correlation studies of metal complexes of alpha-N-heterocyclic carboxaldehyde thiosemicarbazones in Shewanella oneidensis.

    PubMed

    Wilson, Barbara A; Venkatraman, Ramaiyer; Whitaker, Cedrick; Tillison, Quintell

    2005-04-01

    This investigation involved the synthesis of metal complexes to test the hypothesis that structural changesand metal coordination in pyridine thiosemicarbazones affect cell growth and cell proliferation in vitro. Thiosemicarbazones are well known to possess antitumor, antiviral, antibacterial, antimalarial, and other activities. Extensive research has been carried out on aliphatic, aromatic, heterocyclic and other types of thiosemicarbazones and their metal complexes. Due to the pronounced reactivity exhibited by metal complexes of heterocyclic thiosemicarbazones, synthesis and structural characterization of di-2-pyridylketone 4N-phenyl thiosemicarbazone and diphenyl tin (Sn) and platinum (Pt) complexes were undertaken. Shewanella oneidensis MR-1, a metal ion-reducing bacterium, was used as a model organism to explore the biological activity under aerobic conditions. A comparision of the cytotoxic potential of selected ligand and metal-complex thiosemicarbazones on cell growth in wild type MR-1 and mutant DSP-010 Shewanella oneidensis strains at various concentrations (0, 5, 10, 15, 20 or 25 ppm) was performed. The wild type (MR-1) grown in the presence of increasing concentrations of Sn- thiosemicarbazone complexes was comparatively more sensitive (mean cell number = 4.8 X 10(8) +/- 4.3 X 10(7) SD) than the DSP-010, a spontaneous rifampicillin derivative of the parent strain (mean cell number = 5.6 x 10(8) +/- 6.4 X 10(7) SD) under comparable aerobic conditions (p = 0.0004). No differences were observed in the sensitivity of the wild and mutant types when exposed to various concentrations of diphenyl Pt- thiosemicarbazone complex (p = 0.425) or the thiosemicarbazone ligand (p = 0.313). Growth of MR-1 in the presence of diphenyl Sn-thiosemicarbazone was significantly different among treatment groups (p = 0.012). MR-1 cell numbers were significantly higher at 5ppm than at 10 to 20ppm (p = 0.05). The mean number of DSP-010 variant strain cells also differed among

  12. A comprehensive global inventory of atmospheric Antimony emissions from anthropogenic activities, 1995-2010.

    PubMed

    Tian, Hezhong; Zhou, JunRui; Zhu, Chuanyong; Zhao, Dan; Gao, Jiajia; Hao, Jiming; He, Mengchang; Liu, Kaiyun; Wang, Kun; Hua, Shenbing

    2014-09-01

    Antimony (Sb) and its compounds are considered as global pollutants due to their health risks and long-range transport characteristics. A comprehensive global inventory of atmospheric antimony emissions from anthropogenic activities during the period of 1995-2010 has been developed with specific estimation methods based on the relevant data available for different continents and countries. Our results indicate that the global antimony emissions have increased to a peak at about 2232 t (t) in 2005 and then declined gradually. Global antimony emissions in 2010 are estimated at about 1904 t (uncertainty of a 95% confidence interval (CI): -30% ∼ 67%), with fuel combustion as the major source category. Asia and Europe account for about 57% and 24%, respectively, of the global total emissions, and China, the United States, and Japan rank as the top three emitting countries. Furthermore, global antimony emissions are distributed into gridded cells with a resolution of 1° × 1°. Regions with high Sb emissions are generally concentrated in the Southeastern Asia and Western Europe, while South Africa, economically developed regions in the eastern U.S., and Mexico are also responsible for the high antimony emission intensity. PMID:25110938

  13. Urinary antimony and leukocyte telomere length: An analysis of NHANES 1999-2002.

    PubMed

    Scinicariello, Franco; Buser, Melanie C

    2016-10-01

    Telomeres are repetitive DNA sequences (TTAGGG) at the end of chromosomes. Cells with critically short telomeres enter replicative senescence and apoptosis. Several in vitro studies report that antimony causes cell apoptosis in human leukocyte cell lines. The goal of this analysis was to investigate whether there is an association between antimony exposure and leukocyte telomere length (LTL) among US adults aged 20 and older based on the National Health and Nutrition Examination Survey (NHANES) 1999-2002. We used multivariate linear regression to analyze the association of urinary antimony with LTL. LTL was log-natural transformed and the results were re-transformed and presented as percent differences. After adjustment for potential confounders, individuals in the 3rd and 4th quartiles of urinary antimony had statistically significantly shorter LTL (-4.78%, 95% CI: -8.42,-0.90; and -6.11%, 95% CI: -11.04,-1.00, respectively) compared to the lowest referent quartile, with evidence of a dose-response relationship (p-value for trend =0.03). Shorter LTL with antimony was driven by middle aged (40-59 years) and older (60-85 years) adult groups. The association may be biologically plausible because of reported oxidative stress and apoptosis effects of antimony on blood cells, effects known to shorten telomere length. PMID:27423705

  14. Nano-titania-crosslinked chitosan composite as a superior sorbent for antimony (III) and (V).

    PubMed

    Nishad, Padala Abdul; Bhaskarapillai, Anupkumar; Velmurugan, Sankaralingam

    2014-08-01

    Removal of radioactive antimony, especially at low levels, is a difficult problem faced by nuclear power plants all over the world. Further, antimony is classified as a pollutant of priority importance by the United States and the European environmental protection agencies. Chitosan, a biopolymer well known for its sorption properties, can also serve as a stable matrix for inorganic sorbents such as titania on crosslinking. A robust high performing sorbent for antimony, in the form of stable beads, has been prepared using nano-TiO2 and chitosan. Raman spectra of the beads confirmed the incorporation of nano-TiO2 in the chitosan matrix. The sorbent exhibited complete sorption of antimony from aqueous solutions with antimony concentrations ranging from as low as 150 ppb to as high as 120 ppm. The sorption dependence on equilibrium pH has been investigated. The beads have been shown to be effective sorbent of antimony in both +3 and +5 oxidation states. The sorption properties of the beads were attributed to the TiO2 component present in the beads, while the crosslinked chitosan provided strong matrix and influenced the formation of much needed stable spherical beads suitable for real life large scale applications. The beads exhibited high sorption efficiency in the column mode, and were found to be physically stable at a flow rate of one bed volume per minute. PMID:24751261

  15. Antimony: an unlikely confounder in the relationship between well water arsenic and health outcomes in Bangladesh.

    PubMed Central

    McCarty, Kathleen M; Senn, David B; Kile, Molly L; Quamruzzaman, Quazi; Rahman, Mahmuder; Mahiuddin, Golam; Christiani, David C

    2004-01-01

    Recent in vitro studies have suggested a potential role for antimony as a confounder in human health studies related to arsenic in drinking water. We measured tube-well water concentrations of antimony and arsenic in the Pabna region of Bangladesh, where arsenic concentrations are known to be elevated and the concentrations of antimony have not yet been thoroughly documented. Two hundred forty-five tube-well water samples were collected from various regions in Pabna, Bangladesh, as part of an ongoing case-control study. Water samples were analyzed for arsenic and antimony concentrations by inductively coupled plasma-mass spectrometry using U.S. Environmental Protection Agency method 200.8. The arsenic concentrations in the tube-well water samples ranged from < 1 microg/L to 747 microg/L. All 245 water samples had antimony concentrations < 1 microg/L. Based on consideration of the concentrations used the in vitro studies compared with field-observed concentrations, our results do not support the hypothesis that antimony would be a significant confounder in observed relationships between arsenic exposure through drinking water and potential health outcomes in Pabna, Bangladesh. PMID:15175164

  16. Monitoring cellular uptake and cytotoxicity of copper(II) complex using a fluorescent anthracene thiosemicarbazone ligand.

    PubMed

    Kate, Anup N; Kumbhar, Anupa A; Khan, Ayesha A; Joshi, Pranaya V; Puranik, Vedavati G

    2014-01-15

    The thiosemicarbazone derivative of anthracene (ATSC, anthracene thiosemicarbazone 1) and its copper(II) complex (CuATSC, 2) were synthesized and characterized by spectroscopic, electrochemical, and crystallographic techniques. Interaction of 1 and 2 with calf thymus (CT) DNA was explored using absorption and emission spectral methods, and viscosity measurements reveal a partial-intercalation binding mode. Their protein binding ability was monitored by the quenching of tryptophan emission using bovine serum albumin (BSA) as a model protein. Furthermore, their cellular uptake, in vitro cytotoxicity testing on the HeLa cell line, and flow cytometric analysis were carried out to ascertain the mode of cell death. Cell cycle analysis indicated that 1 and 2 cause cell cycle arrest in sub-G1 phase. PMID:24328322

  17. Design, synthesis and biological evaluation of new aryl thiosemicarbazone as antichagasic candidates.

    PubMed

    Blau, Lorena; Menegon, Renato Farina; Trossini, Gustavo H G; Molino, João Vitor Dutra; Vital, Drielli Gomes; Cicarelli, Regina Maria Barretto; Passerini, Gabriela Duó; Bosquesi, Priscila Longhin; Chin, Chung Man

    2013-09-01

    The present work reports on the synthesis, biological assaying and docking studies of a series of 12 aryl thiosemicarbazones, which were planned to act over two main enzymes, cruzain and trypanothione reductase. These enzymes are used as targets of trypanocidal activity in Chagas disease control with a minimal mutagenic profile. Three p-nitroaromatic thiosemicarbazones showed high activity against Trypanosoma cruzi in in vitro assays (IC50 < 57 μM), and no mutagenic profile was observed in micronucleous tests. Although the in vitro inhibition test showed that 10-μM doses of eight compounds inhibited cruzain activity, no correlation was found between cruzain inhibition and trypanocidal activity. PMID:23851115

  18. Spectroscopic, thermal and electrochemical studies on some nickel(II) thiosemicarbazone complexes

    NASA Astrophysics Data System (ADS)

    El-Shazly, R. M.; Al-Hazmi, G. A. A.; Ghazy, S. E.; El-Shahawi, M. S.; El-Asmy, A. A.

    2005-01-01

    Several complexes of thiosemicarbazone derivatives with Ni(II) have been prepared. Structural investigation of the ligands and their complexes has been made based on elemental analysis, magnetic moment, spectral (UV-Vis, i.r., 1H NMR, ms), and thermal studies. The i.r. spectra suggest the bidentate mononegative and tridentate (neutral, mono-, and binegative) behavior of the ligands. Different stereochemistries were suggested for the isolated complexes. The thermogravimetry (TG) and derivative thermogravimetry (DTG) have been used to study the thermal decomposition and kinetic parameters of some ligands and complexes using the Coats-Redfern and Horowitz-Metzger equations. The redox properties and stability of the complexes toward oxidation waves explored by cyclic voltammetry are related to the electron withdrawing or releasing ability of the substituent of thiosemicarbazone moiety. The samples displayed Ni II/Ni I couples irreversible waves associated with Ni III/Ni II process.

  19. Synthesis, molecular modeling, and biological evaluation of novel chiral thiosemicarbazone derivatives as potent anticancer agents.

    PubMed

    Taşdemir, Demet; Karaküçük-İyidoğan, Ayşegül; Ulaşli, Mustafa; Taşkin-Tok, Tuğba; Oruç-Emre, Emİne Elçİn; Bayram, Hasan

    2015-02-01

    A series of new chiral thiosemicarbazones derived from homochiral amines in both enantiomeric forms were synthesized and evaluated for their in vitro antiproliferative activity against A549 (human alveolar adenocarcinoma), MCF-7 (human breast adenocarcinoma), HeLa (human cervical adenocarcinoma), and HGC-27 (human stomach carcinoma) cell lines. Some of compounds showed inhibitory activities on the growth of cancer cell lines. Especially, compound exhibited the most potent activity (IC50 4.6 μM) against HGC-27 as compared with the reference compound, sindaxel (IC50 10.3 μM), and could be used as a lead compound to search new chiral thiosemicarbazone derivatives as antiproliferative agents. PMID:25399965

  20. Synthesis and Antiproliferative Activity of Steroidal Thiosemicarbazone Platinum (Pt(II)) Complexes.

    PubMed

    Huang, Yanmin; Kong, Erbin; Gan, Chunfang; Liu, Zhiping; Lin, Qifu; Cui, Jianguo

    2015-01-01

    Steroidal compounds exhibit particular physiological activities. In this paper, some steroidal thiosemicarbazones platinum (Pt(II)) complexes were synthesized by the condensation of steroidal ketones with thiosemicarbazide using estrone, chenodeoxycholic acid, and 7-deoxycholic acid as starting materials and complexation of steroidal thiosesemicarbazones with Pt(II). The complexes were characterized by IR, NMR, and MS, and their antiproliferative activities were evaluated. The results showed that some steroidal thiosemicarbazones platinum (Pt(II)) complexes displayed moderate cytotoxicity to HeLa and Bel-7404 cells. Thereinto, complex 6 showed an excellent inhibited selectivity to HeLa cells with an IC50 value of 9.2 μM and SI value of 21.7. At the same time, all compounds were almost inactive to HEK293T (normal kidney epithelial cells). The information obtained from the studies may be useful for the design of novel chemotherapeutic drugs. PMID:26635511

  1. Human topoisomerase IB is a target of a thiosemicarbazone copper(II) complex.

    PubMed

    Vutey, Venn; Castelli, Silvia; D'Annessa, Ilda; Sâmia, Luciana B P; Souza-Fagundes, Elaine M; Beraldo, Heloisa; Desideri, Alessandro

    2016-09-15

    The human topoisomerase IB inhibition and the antiproliferative activity of 3-(4-bromophenyl)-1-pyridin-2-ylprop-2-en-1-one thiosemicarbazone HPyCT4BrPh alone and its copper(II) complex [Cu(PyCT4BrPh)Cl] was investigated. [Cu(PyCT4BrPh)Cl] inhibits both the DNA cleavage and religation step of the enzyme, whilst the ligand alone does not display any effect. In addition we show that coordination to copper(II) improves the cytotoxicity of HPyCT4BrPh against THP-1 leukemia and MCF-7 breast cancer cells. The data indicate that the copper(II) thiosemicarbazone complex may hit human topoisomerase IB and that metal coordination can be useful to improve cytotoxicity of this versatile class of compounds. PMID:27431056

  2. Synthesis and Antiproliferative Activity of Steroidal Thiosemicarbazone Platinum (Pt(II)) Complexes

    PubMed Central

    Huang, Yanmin; Kong, Erbin; Gan, Chunfang; Liu, Zhiping; Lin, Qifu; Cui, Jianguo

    2015-01-01

    Steroidal compounds exhibit particular physiological activities. In this paper, some steroidal thiosemicarbazones platinum (Pt(II)) complexes were synthesized by the condensation of steroidal ketones with thiosemicarbazide using estrone, chenodeoxycholic acid, and 7-deoxycholic acid as starting materials and complexation of steroidal thiosesemicarbazones with Pt(II). The complexes were characterized by IR, NMR, and MS, and their antiproliferative activities were evaluated. The results showed that some steroidal thiosemicarbazones platinum (Pt(II)) complexes displayed moderate cytotoxicity to HeLa and Bel-7404 cells. Thereinto, complex 6 showed an excellent inhibited selectivity to HeLa cells with an IC50 value of 9.2 μM and SI value of 21.7. At the same time, all compounds were almost inactive to HEK293T (normal kidney epithelial cells). The information obtained from the studies may be useful for the design of novel chemotherapeutic drugs. PMID:26635511

  3. Structural studies on acetophenone- and benzophenone-derived thiosemicarbazones and their zinc(II) complexes

    NASA Astrophysics Data System (ADS)

    Ferraz, Karina S. O.; Silva, Nayane F.; Da Silva, Jeferson G.; Speziali, Nivaldo L.; Mendes, Isolda C.; Beraldo, Heloisa

    2012-01-01

    In the present work N(3)- meta-chlorophenyl-(HAc3 mCl, 1) and N(3)- meta-fluorphenyl-(HAc3 mF, 2) acetophenone thiosemicarbazone, and N(3)- meta-chlorophenyl-(HBz3 mCl, 3) and N(3)- meta-fluorphenyl-(HBz3 mF, 4) benzophenone thiosemicarbazone were obtained, as well as their zinc(II) complexes [Zn(Ac3 mCl) 2] ( 5), [Zn(Ac3 mF) 2] ( 6), [Zn(Bz3 mCl) 2] ( 7) and [Zn(Bz3 mF) 2] ( 8). Upon re-crystallization in DMSO:acetone conversion of 8 into [Zn(Bz3 mF) 2]·(DMSO) ( 8a) occurred. The crystal structures of 2, 5 and 8a were determined.

  4. Synthesis, biological evaluation and molecular docking of N-phenyl thiosemicarbazones as urease inhibitors.

    PubMed

    Hameed, Abdul; Khan, Khalid Mohammed; Zehra, Syeda Tazeen; Ahmed, Ramasa; Shafiq, Zahid; Bakht, Syeda Mahwish; Yaqub, Muhammad; Hussain, Mazhar; de la Vega de León, Antonio; Furtmann, Norbert; Bajorath, Jürgen; Shad, Hazoor Ahmad; Tahir, Muhammad Nawaz; Iqbal, Jamshed

    2015-08-01

    Urease is an important enzyme which breaks urea into ammonia and carbon dioxide during metabolic processes. However, an elevated activity of urease causes various complications of clinical importance. The inhibition of urease activity with small molecules as inhibitors is an effective strategy for therapeutic intervention. Herein, we have synthesized a series of 19 benzofurane linked N-phenyl semithiocarbazones (3a-3s). All the compounds were screened for enzyme inhibitor activity against Jack bean urease. The synthesized N-phenyl thiosemicarbazones had varying activity levels with IC50 values between 0.077 ± 0.001 and 24.04 ± 0.14 μM compared to standard inhibitor, thiourea (IC50 = 21 ± 0.11 μM). The activities of these compounds may be due to their close resemblance of thiourea. A docking study with Jack bean urease (PDB ID: 4H9M) revealed possible binding modes of N-phenyl thiosemicarbazones. PMID:26119990

  5. Spectroscopic and biological studies on newly synthesized nickel(II) complexes of semicarbazones and thiosemicarbazones

    NASA Astrophysics Data System (ADS)

    Chandra, Sulekh; Gupta, Lokesh Kumar

    2005-12-01

    Nickel(II) complexes, having the general composition Ni(L) 2X 2, have been synthesized [where L: isopropyl methyl ketone semicarbazone (LLA), isopropyl methyl ketone thiosemicarbazone (LLB), 4-aminoacetophenone semicarbazone (LLC) and 4-aminoacetophenone thiosemicarbazone (LLD) and X = Cl -, 1/2SO 42-]. All the Ni(II) complexes reported here have been characterized by elemental analyses, magnetic moments, IR, electronic and mass spectral studies. All the complexes were found to have magnetic moments corresponding to two unpaired electrons. The possible geometries of the complexes were assigned on the basis of electronic and infrared spectral studies. Newly synthesized ligand and its nickel(II) complexes have been screened against different bacterial and fungal growth.

  6. Simulation of antimony adsorption on nano-zero valent iron and kaolinite and analyzing the influencing parameters.

    PubMed

    Saeidnia, Setareh; Asadollahfardi, Gholamreza; Darban, Ahmad Khodadadi; Mohseni, Mehdi

    2016-01-01

    Antimony is one of the most toxic pollutants in industrial and mineral wastewaters threatening the life of humans and other creatures. We simulated the adsorption of antimony in the presence of nano-zero valent iron (nZVI) adsorbent, on kaolinite and in the presence of nZVI coated on kaolinite from mineral wastewater using VISUAL MINTEQ 3.1 software. Our aim was to determine the factors affecting the adsorption of antimony by applying simulation. The simulation was performed using an adsorption model of a diffuse layer model. The results of the simulation indicated that the nZVI concentration, initial concentrations of antimony and pH factor are effective on the adsorption of antimony. In the conducted stimulation, the optimum pH was 2-5 and the highest adsorption occurred in an acidic state. With increasing initial concentrations of antimony in the simulation, we concluded that nZVI had absorbed various concentrations above 90% and, by increasing the concentration of nZVI, antimony adsorption rate increased. The increased surface area of nZVI and the expansion of more interchangeable surfaces available for reaction with antimony ions causes more antimony ions to be adsorbed. In all cases, the coefficient of determination between the laboratory results and the model predictions that was obtained was more than 0.9. PMID:27191572

  7. Novel "hybrid" iron chelators derived from aroylhydrazones and thiosemicarbazones demonstrate selective antiproliferative activity against tumor cells.

    PubMed

    Lovejoy, David B; Richardson, Des R

    2002-07-15

    We previously demonstrated that 2-hydroxy-1-naphthylaldehyde isonicotinoyl hydrazone (311) and other aroylhydrazone chelators possess potent antineoplastic activity because of their ability to bind iron (Fe). From these studies, we identified structural components of the hydrazones that provide antineoplastic activity, namely the salicylaldehyde and 2-hydroxy-1-naphthylaldehyde moieties. A related group of chelators known as the thiosemicarbazones also show pronounced antitumor activity because of their ability to inhibit ribonucleotide reductase. Considering this, we designed a new series of "hybrid ligands" by condensation of the aldehydes described above with a range of thiosemicarbazides. The parent compound of these ligands is 2-hydroxy-1-naphthylaldehyde thiosemicarbazone (NT). Of 8 NT analogues, 3 chelators, namely NT, N4mT (2-hydroxy-1-naphthylaldehyde-4-methyl-3-thiosemicarbazone), and N44mT (2-hydroxy-1-naphthylaldehyde-4,4-dimethyl-3-thiosemicarbazone), showed high antiproliferative activity against SK-N-MC neuroepithelioma cells (50% inhibitory concentration [IC(50)] = 0.5-1.5 microM). Indeed, their activity was significantly (P <.0001) greater than that of desferrioxamine (DFO) (IC(50) = 22 microM). We demonstrate that 311, a 311 analogue (311m), and several NT-series chelators have significantly (P <.001) greater antiproliferative activity against tumor cells than against a range of normal cell types. For example, the IC(50) values of NT and N4mT in SK-N-MC neuroepithelioma cells were 0.5 microM, whereas for fibroblasts the IC(50) values were greater than 25 microM. Further, the effect of one of the most potent chelators (311m) on preventing the growth of bone marrow stem cell cultures was far less than that of doxorubicin and similar to that of cisplatin. These studies support the further development of these chelators as antiproliferative agents. PMID:12091363

  8. 1-Methylisatin 3-Thiosemicarbazone Treatment of NZB × NZW Hybrid Mice

    PubMed Central

    Gabriel, R.

    1971-01-01

    Female B/W mice have been treated with the anti-viral agent 1-Methylisatin 3-Thiosemicarbazone. The drug was given upon the day of birth and weekly until death. There was a delay in the development of proteinuria and positive antinuclear factor. The mean survival of the group was prolonged; eventually all mice died from nephritis within a 6 week period. The results are interpreted as a suppression of viral activity in these animals. PMID:5314564

  9. Spectroscopic characterization of copper(II) complexes of indoxyl N(4)-methyl thiosemicarbazone

    NASA Astrophysics Data System (ADS)

    Chandra, Sulekh; Kumar, Umendra

    2004-10-01

    New copper(II) complexes of indoxyl thiosemicarbazone (ITSC) of general composition CuL 2X 2 (where L: ITSC; X: Cl -, NO 3-, ClO 4-, NCS -) have been synthesized and characterized by elemental analysis, molar conductance, magnetic susceptibility measurements and spectral (electronic, IR, EPR, 1H NMR , Mass) studies. Cyclic voltammetry measurements show quasi-reversible Cu 2+/Cu 1+ couple. Various physico-chemical techniques suggest a tetragonal structure for these copper(II) complexes.

  10. Investigation of the salicylaldehyde thiosemicarbazone scaffold for inhibition of influenza virus PA endonuclease.

    PubMed

    Rogolino, Dominga; Bacchi, Alessia; De Luca, Laura; Rispoli, Gabriele; Sechi, Mario; Stevaert, Annelies; Naesens, Lieve; Carcelli, Mauro

    2015-10-01

    The influenza virus PA endonuclease is an attractive target for the development of novel anti-influenza virus therapeutics, which are urgently needed because of the emergence of drug-resistant viral strains. Reported PA inhibitors are assumed to chelate the divalent metal ion(s) (Mg²⁺ or Mn²⁺) in the enzyme's catalytic site, which is located in the N-terminal part of PA (PA-Nter). In the present work, a series of salicylaldehyde thiosemicarbazone derivatives have been synthesized and evaluated for their ability to inhibit the PA-Nter catalytic activity. Compounds 1-6 have been evaluated against influenza virus, both in enzymatic assays with influenza virus PA-Nter and in virus yield assays in MDCK cells. In order to establish a structure-activity relationship, the hydrazone analogue of the most active thiosemicarbazone has also been evaluated. Since chelation may represent a mode of action of such class of molecules, we studied the interaction of two of them, one with and one without biological activity versus the PA enzyme, towards Mg²⁺, the ion that is probably involved in the endonuclease activity of the heterotrimeric influenza polymerase complex. The crystal structure of the magnesium complex of the o-vanillin thiosemicarbazone ligand 1 is also described. Moreover, docking studies of PA endonuclease with compounds 1 and 2 were performed, to further analyse the possible mechanism of action of this class of inhibitors. PMID:26323352

  11. Bivalent transition metal complexes of coumarin-3-yl thiosemicarbazone derivatives: Spectroscopic, antibacterial activity and thermogravimetric studies

    NASA Astrophysics Data System (ADS)

    Refat, Moamen S.; El-Deen, Ibrahim M.; Anwer, Zeinab M.; El-Ghol, Samir

    2009-02-01

    Schiff base complexes of Cu(II), Co(II) and Ni(II) with two coumarin-3-yl thiosemicarbazone derivatives (1E)-1-(1-(2-oxo-2H-chromen-3-yl)ethylidene)thiosemicarbazide (OCET) and (1E)-1-(1-(6-bromo-2-oxo-2H-chromen-3-yl)ethylidene)thiosemicarbazide (BOCET) were synthesized by the reaction of Cu(II), Co(II) and Ni(II) chlorides with each mentioned ligand with molar ratio 1:2 metal-to-ligand. Both ligands and their metal complexes were characterized by different physicochemical methods, elemental analysis, molar conductivity, (UV-vis, Mass, Infrared, 1H NMR spectra) and also thermal analysis (TG and DTG) techniques. The discussion of the outcome data of the prepared complexes indicate that the coumarin-3-yl thiosemicarbazone derivatives ligands behave as a bidentate ligand through both thione sulphur and azomethine nitrogen with 1:2 (metal:ligand) stoichiometry for all complexes. The molar conductance measurements proved that the complexes are electrolytes. The kinetic thermodynamic parameters such as: E∗, Δ H∗, Δ S∗and Δ G∗are calculated from the DTG curves, all complexes are more ordered except Ni(II) complexes. The antibacterial activity of the coumarin-3-yl thiosemicarbazone derivatives and their metal complexes was evaluated against some kinds of Gram positive and Gram negative bacteria.

  12. Zinc(II)-Thiosemicarbazone Complexes Are Localized to the Lysosomal Compartment Where They Transmetallate with Copper Ions to Induce Cytotoxicity.

    PubMed

    Stacy, Alexandra E; Palanimuthu, Duraippandi; Bernhardt, Paul V; Kalinowski, Danuta S; Jansson, Patric J; Richardson, Des R

    2016-05-26

    As the di-2-pyridylketone thiosemicarbazone (DpT) and 2-acetylpyridine thiosemicarbazone (ApT) series show potent antitumor activity in vitro and in vivo, we synthesized their fluorescent zinc(II) complexes to assess their intracellular distribution. The Zn(II) complexes generally showed significantly greater cytotoxicity than the thiosemicarbazones alone in several tumor cell-types. Notably, specific structure-activity relationships demonstrated the importance of the di-2-pyridyl pharmacophore in their activity. Confocal fluorescence imaging and live cell microscopy showed that the Zn(II) complex of our lead compound, di-2-pyridylketone 4-cyclohexyl-4-methyl-3-thiosemicarbazone (DpC), which is scheduled to enter clinical trials, was localized to lysosomes. Under lysosomal conditions, the Zn(II) complexes were shown to transmetallate with copper ions, leading to redox-active copper complexes that induced lysosomal membrane permeabilization (LMP) and cytotoxicity. This is the first study to demonstrate direct lysosomal targeting of our novel Zn(II)-thiosemicarbazone complexes that mediate their activity via transmetalation with copper ions and LMP. PMID:27023111

  13. Microwave synthesis of mixed ligand diimine–thiosemicarbazone complexes of ruthenium(ii): biophysical reactivity and cytotoxicity†

    PubMed Central

    Beckford, Floyd A.; Shaloski, Michael; Leblanc, Gabriel; Thessing, Jeffrey; Lewis-Alleyne, Lesley C.; Holder, Alvin A.; Li, Liya; Seeram, Navindra P.

    2010-01-01

    A novel microwave-assisted synthetic method has been used to synthesise a series of mixed ligand ruthenium(ii) compounds containing diimine as well as bidentate thiosemicarbazone ligands. The compounds contain the diimine 1,10-phenanthroline (phen) or 2,2′-bipyridine (bpy) and the thiosemicarbazone is derived from 9-anthraldehyde. Based on elemental analyses and spectroscopic data, the compounds are best formulated as [(phen)2Ru(thiosemicarbazone)](PF6)2 and [(phen)2Ru(thiosemicarbazone)](PF6)2 where thiosemicarbazone = 9-anthraldehydethiosemicarbazone, 9-anthraldehyde-N(4)-methylthiosemicarbazone, and 9-anthraldehyde-N(4)-ethylthiosemicarbazone. Fluorescence competition studies with ethidium bromide, along with viscometric measurements suggests that the complexes bind calf thymus DNA (CTDNA) relatively strongly via an intercalative mode possibly involving the aromatic rings of the diimine ligands. The complexes show good cytotoxic profiles against MCF-7 and MDA-MB-231 (breast adenocarcinoma) as well as HCT 116 and HT-29 (colorectal carcinoma) cell lines. PMID:20023905

  14. New Antimony Lanthanide Disulfide Dibromides LnSbS

    SciTech Connect

    Gout, D.; Jobic, S.; Evain, M.; Brec, R.

    2001-05-01

    CeSbS{sub 2}Br{sub 2} (I), Ce{sub 1/2}La{sub 1/2}SbS{sub 2}Br{sub 2} (II), and LaSbS{sub 2}Br{sub 2} (III) have been synthesized at 700 C from a mixture of LnBr{sub 3}, Ln{sub 2}S{sub 3}, Sb, and S and characterized by single-crystal X-ray diffraction. The three phases are isostructural (space group P2{sub 1}/c, Z=4) and crystallize in a novel, dense, bidimensional structure with cell parameters a=8.709(3) {angstrom}, b=9.187(2) {angstrom}, c=17.397(5) {angstrom} {beta}=104.26(3) for I, a=8.739(7) {angstrom}, b=9.219(7) {angstrom}, c=17.41(2) {angstrom}, =104.3(1) for II, and a=8.785(1) {angstrom}, b=9.236(2) {angstrom}, c=17.372(3) {angstrom}, {beta}=104.09(2) for III. In these compounds, [Ln S{sub 5}Br{sub 4}] and [Ln S{sub 3}Br{sub 6}] (Ln=Ce, La) distorted tricapped trigonal prisms define infinite {sub {infinity}}{sup 2}[LnS{sub 2}Br{sub 2}] layers counterbalanced and capped by antimony cations. In good accordance with the structural features, the charge balance in these materials is to be written Ln{sup III}Sb{sup III}S{sup -II}{sub 2}Br{sup -I}{sub 2}. These compounds exhibit a yellow hue with a measured absorption threshold of 2.42(1), 2.55(1), and 2.72(1) eV for I, II, and III, respectively. In the two cerium containing bromothioantimonates I and II, the origin of the color is assigned to a Ce-4f{yields}Ce-5d electronic transition, which shifts to higher energy from I to II due either to a matrix effect (increase of the mean Ln-S distances under the substitution of Ce for La) or to an atomic ordering between Ce and La cations on the Ln(1) and Ln(2) crystallographic sites. In contrast, the electronic transition at play in III involves a charge transfer from the bromine and sulfur ions to the antimony ions, the latter contributing substantially to the lowermost levels of the conduction band.

  15. MAPK1 of Leishmania donovani Modulates Antimony Susceptibility by Downregulating P-Glycoprotein Efflux Pumps

    PubMed Central

    Garg, Mansi

    2015-01-01

    Emergence of resistance to pentavalent antimonials has become a severe obstacle in the treatment of visceral leishmaniasis (VL) in the Indian subcontinent. Mitogen-activated protein kinases (MAPKs) are well-known mediators of signal transduction of eukaryotes, regulating important processes, like proliferation, differentiation, stress response, and apoptosis. In Leishmania, MAPK1 has been shown to be consistently downregulated in antimony-resistant field isolates, suggesting that it has a role in antimony resistance. The present work investigates the molecular mechanism of MAPK1 in antimony resistance in Leishmania donovani. The L. donovani MAPK1 (LdMAPK1) single-allele replacement mutants exhibited increased resistance to Sb(III) (5.57-fold) compared to wild-type promastigotes, while overexpressing parasites became much more susceptible to antimony. The LdMAPK1-mediated drug sensitivity was directly related to antimony-induced apoptotic death of the parasite, as was evidenced by a 4- to 5-fold decrease in cell death parameters in deletion mutants and a 2- to 3-fold increase in MAPK1-overexpressing cells. LdMAPK1-underexpressing parasites also exhibited increased P-glycoprotein (P-gp)-mediated efflux pump activity, while a significant decrease in pump activity was observed in overexpressing cells. This change in efflux pump activity was directly related to expression levels of P-gp in all cell lines. However, episomal complementation of the gene restored normal growth, drug sensitivity, P-gp expression, and efflux pump activity. The data indicate that LdMAPK1 negatively regulates the expression of P-glycoprotein-type efflux pumps in the parasite. The decrease in efflux pump activity with an increase in LdMAPK1 expression may result in increased antimony accumulation in the parasite, making it more vulnerable to the drug. PMID:25870075

  16. The MRP1-mediated effluxes of arsenic and antimony do not require arsenic-glutathione and antimony-glutathione complex formation.

    PubMed

    Salerno, Milena; Petroutsa, Maria; Garnier-Suillerot, Arlette

    2002-04-01

    Arsenic trioxide is an effective treatment for acute promyelocytic leukemia, but resistance to metalloid salts is found in humans. Using atomic absorption spectroscopy, we have measured the rate of uptake of arsenic trioxide and of antimony tartrate in GLC4 and GLC4/ADR cells overexpressing MRP1 and the rate of their MRP1-mediated effluxes as a function of the intracellular GSH concentration. In sensitive cells, after 1 h, a pseudosteady state is reached where intra- and extracellular concentrations of metalloid are the same. This precludes the formation, at short term, of complexes between arsenic or antimony with GSH. In resistant cells reduced intracellular accumulation of arsenic (or antimony), reflecting an increased rate of arsenic (or antimony) efflux from the cells, is observed. No efflux of the metalloid is observed in GSH depleted cells. The two metalloids and GSH are pumped out by MRP1 with the same efficiency. Moreover for the three compounds 50% of the efflux is inhibited by 2 microM MK571. This led us to suggest that As- and Sb-containing species could be cotransported with GSH. PMID:12018890

  17. OXIDANT-PRECURSOR RELATIONSHIPS

    EPA Science Inventory

    New methods of ambient air analysis were used to define more clearly the relationships between oxidants and their precursors. Non-methane hydrocarbons, NOx, O2, and oxidants were measured at the same time and location (Riverside, California). The ambient air data presented in thi...

  18. Untangling ENSO Precursors

    NASA Astrophysics Data System (ADS)

    Pegion, K.; Alexander, M. A.

    2014-12-01

    There are several proposed precursors to the El Nino-Southern Oscillation (ENSO) that may provide the ability to predict ENSO as much as one year in advance. Some of these precursors are associated with stochastic forcing from extratropical atmospheric variability. Two examples are the seasonal footprinting mechanism (SFM) and the Pacific meridional mode (PMM). Both of these ENSO precursors are thought to be forced by the North Pacific Oscillation (NPO), a north-south sea level pressure dipole in the north Pacific. Additionally, both the PMM and SFM are thought to impact the tropics through wind evaporation SST feedbacks and have a correlation with ENSO up to one year in advance. These two precursors are discussed interchangeably throughout the literature and various indices used to define them co-mingle them. As a result, whether they are independent of each other or are part of the same process has not been investigated. The research presented is focused on untangling the relationship between the PMM, SFM, NPO, and ENSO using observational datasets and model simulations. Observational results demonstrate that these two mechanisms are different, are forced by different atmospheric circulations, and result in different manifestations of ENSO. Modeling results highlight the extent to which climate models can simulate these relationships and their impact on the simulation of ENSO.

  19. Simultaneous lead and antimony immobilization in shooting range soil by a combined application of hydroxyapatite and ferrihydrite.

    PubMed

    Ogawa, Shouhei; Katoh, Masahiko; Sato, Takeshi

    2015-01-01

    This study investigated whether a combined application of hydroxyapatite and ferrihydrite could immobilize lead and antimony in shooting range soil in which the level of lead contamination is markedly higher than that of antimony. In addition, we evaluated the stability of lead and antimony immobilized by the combined application with varying soil pH. The levels of water-soluble lead and antimony for the combined application were lower than those of single applications of hydroxyapatite or ferrihydrite, indicating that the combined application could suppress the levels of water-soluble lead and antimony by 99.9% and 95.5%, respectively, as compared with the levels in shooting range soil without immobilization material. The amounts of residual lead and amorphous Fe/Al oxide-bound antimony fractions in sequential extraction increased with a decrease in the exchangeable and carbonate lead fractions as well as in non-specifically bound and specifically bound antimony fractions. The alteration of lead and antimony phases to chemically more stable ones as a result of the combined application would result in the suppression of their mobility. The stability of immobilized lead and antimony in the combined application was equal to that of lead with a single application of hydroxyapatite and that of antimony with a single application of ferrihydrite within neutral to alkaline pH conditions, respectively. Therefore, this study suggests that the combined application of hydroxyapatite and ferrihydrite can simultaneously immobilize lead and antimony in shooting range soil with neutral to alkaline pH. PMID:25894550

  20. Calcium-Antimony Alloys as Electrodes for Liquid Metal Batteries

    SciTech Connect

    Ouchi, T; Kim, H; Ning, XH; Sadoway, DR

    2014-08-08

    The performance of a calcium-antimony (Ca-Sb) alloy serving as the positive electrode in a Ca vertical bar vertical bar Sb liquid metal battery was investigated in an electrochemical cell, Ca(in Bi) vertical bar LiCl-NaCl-CaCl2 vertical bar Ca(in Sb). The equilibrium potential of the Ca-Sb electrode was found to lie on the interval, 1.2-0.95 V versus Ca, in good agreement with electromotive force (emf) measurements in the literature. During both alloying and dealloying of Ca at the Sb electrode, the charge transfer and mass transport at the interface are facile enough that the electrode potential varies linearly from 0.95 to 0.75 V vs Ca(s) as current density varies from 50 to 500 mA cm(-2). The discharge capacity of the Ca vertical bar vertical bar Sb cells increases as the operating temperature increases due to the higher solubility and diffusivity of Ca in Sb. The cell was successfully cycled with high coulombic efficiency (similar to 100%) and small fade rate (<0.01% cycle(-1)). These data combined with the favorable costs of these metals and salts make the Ca vertical bar vertical bar Sb liquid metal battery attractive for grid-scale energy storage. (C) The Author(s) 2014. Published by ECS. All rights reserved.

  1. Single-layer crystalline phases of antimony: Antimonenes

    NASA Astrophysics Data System (ADS)

    Aktürk, O. Üzengi; Ã-zçelik, V. Ongun; Ciraci, S.

    2015-06-01

    The pseudolayered character of 3D bulk crystals of antimony has led us to predict its 2D single-layer crystalline phase named antimonene in a buckled honeycomb structure like silicene. Sb atoms also form an asymmetric washboard structure like black phospherene. Based on an extensive analysis comprising ab initio phonon and finite-temperature molecular dynamics calculations, we show that these two single-layer phases are robust and can remain stable at high temperatures. They are nonmagnetic semiconductors with band gaps ranging from 0.3 eV to 1.5 eV, and are suitable for 2D electronic applications. The washboard antimonene displays strongly directional mechanical properties, which may give rise to a strong influence of strain on the electronic properties. Single-layer antimonene phases form bilayer and trilayer structures with wide interlayer spacings. In multilayers, this spacing is reduced and eventually the structure changes to 3D pseudolayered bulk crystals. The zigzag and armchair nanoribbons of the antimonene phases have fundamental band gaps derived from reconstructed edge states and display a diversity of magnetic and electronic properties depending on their width and edge geometry. Their band gaps are tunable with the widths of the nanoribbons. When grown on substrates, such as germanene or Ge(111), the buckled antimonene attains a significant influence of substrates.

  2. Yb3+/Ho3+-codoped antimony-silicate optical fiber

    NASA Astrophysics Data System (ADS)

    Żmojda, Jacek; Dorosz, Dominik; Kochanowicz, Marcin; Miluski, Piotr; Dorosz, Jan

    The emission properties of Yb3+/Ho3+-codoped antimony-silicate optical fiber has been investigated. Luminescence at 2.1 μm corresponding to 5I7--> 5I8 transition in holmium was obtained by energy transfer between Yb3+ and Ho3+ ions. According to the Dexter-Miyakawa model, the parameters of energy migration CDD of the 2F5/2 (Yb3+) <--> 2F5/2 (Yb3+) transition and direct energy transfer CDA of the 2F5/2 (Yb3+) --> 5I6 (Ho3+) transition was calculated. The optimization of the activator content and the concentration ratio were conducted with the purpose of maximizing the efficiency of energy transfer. It made possible to select best-suited glass which was used to manufacture double-clad optical fiber. Strong and narrow bands of spontaneous emission which formed as a result of energy transfer between ytterbium and holmium ions were observed in the fiber under exciting with radiation at 978 nm wavelength.

  3. Yb3+/Ho3+-codoped antimony-silicate optical fiber

    NASA Astrophysics Data System (ADS)

    Żmojda, Jacek; Dorosz, Dominik; Kochanowicz, Marcin; Miluski, Piotr; Dorosz, Jan

    2012-05-01

    The emission properties of Yb3+/Ho3+-codoped antimony-silicate optical fiber has been investigated. Luminescence at 2.1 μm corresponding to 5I7--> 5I8 transition in holmium was obtained by energy transfer between Yb3+ and Ho3+ ions. According to the Dexter-Miyakawa model, the parameters of energy migration CDD of the 2F5/2 (Yb3+) <--> 2F5/2 (Yb3+) transition and direct energy transfer CDA of the 2F5/2 (Yb3+) --> 5I6 (Ho3+) transition was calculated. The optimization of the activator content and the concentration ratio were conducted with the purpose of maximizing the efficiency of energy transfer. It made possible to select best-suited glass which was used to manufacture double-clad optical fiber. Strong and narrow bands of spontaneous emission which formed as a result of energy transfer between ytterbium and holmium ions were observed in the fiber under exciting with radiation at 978 nm wavelength.

  4. Antimony-Based III-V Thermophotovoltaic Materials and Devices

    NASA Astrophysics Data System (ADS)

    Wang, C. A.

    2004-11-01

    Antimony-based III-V thermophotovoltaic (TPV) cells are attractive converters for systems with low radiator temperature of around 1100 to 1700 K, since these cells can be spectrally matched to the thermal source. Cells under development include GaSb and lattice-matched GaInAsSb/GaSb and InPAsSb/InAs. GaSb cell technology is the most mature, owing in part to the relative ease in preparation of the binary alloy compared to the quaternary alloys. Cell performance of 0.7-eV GaSb devices is at ˜90% of the practical limit. GaInAsSb cells with energy gap Eg ranging from ˜0.6 to 0.49 eV have been demonstrated with quantum efficiency and fill factor approaching practical limits. InPAsSb cells are the least studied, and a 0.45-eV cell has spectral response out to 4.3 μm. This paper briefly reviews the main efforts in Sb-based TPV cells.

  5. Antimony as an amphoteric dopant in lead telluride

    SciTech Connect

    Jaworski, Christopher M.; Tobola, Janusz; Levin, E.M.; Schmidt-Rohr, Klaus; Heremans, Joseph P.

    2009-09-24

    We elucidate the amphoteric nature of antimony as a dopant in PbTe. Band-structure calculations show that Sb substituting for Pb is a donor and that Sb on the Te site is an acceptor giving rise to a large excess density of states (DOS). Experimentally, in Te-rich Pb{sub 1-x}Sb{sub x}Te samples, {sup 125}Te NMR spectroscopy shows that Sb substitutes for Pb and transport data reveal that it then acts as a simple donor. In Pb-rich PbSb{sub x}Te{sub 1-x} samples, {sup 125}Te NMR shows that little Sb substitutes for Te when samples are prepared above 770 K and then quenched; {sup 207}Pb NMR shows four types of charge carriers, but only a majority hole and a minority electron contribute to transport. Sb acts as an acceptor in PbSb{sub x}Te{sub 1-x}, but the large DOS calculated must correspond to a large concentration of localized holes and the Seebeck coefficient is not enhanced.

  6. Electrochemical antimony removal from accumulator acid: results from removal trials in laboratory cells.

    PubMed

    Bergmann, M E Henry; Koparal, A Savas

    2011-11-30

    Regeneration of spent accumulator acid could be an alternative process for crystallization, neutralisation and disposal. Therefore, for the first time in a study of the possibilities of electrochemical removal of antimony and accumulator acid regeneration on a laboratory scale, two synthetic and several real systems containing sulfuric acid of concentrations ranging between 28% and 36%, and antimony species were tested. Discontinuous electrochemical reactors with anion exchange membranes were successfully used in these experiments, which were conducted at a temperature of 35°C. Removal of antimony using cells that were not divided by a separator, however, was not possible. In selected experiments, by varying the electrode material, type of electrolyte, and cell current, the concentration of antimony could be reduced from the range of 5 ppm to 0.15 ppm. This resulted in current efficiencies between 0.00002% and 0.001%, and in specific electroenergy demands between 100 Wh L(-1) and 2000 Wh L(-1). In other experiments on substances with antimony contents up to 3500 mg L(-1), the current efficiencies obtained were more than a thousandfold higher. In contrast to the formally high relative energy consumption parameters absolute demand parameters are relatively small and favour the electrochemical method in small scale application. Besides plate electrodes, 3D-cathodes were used. Copper- and graphite cathodes produced the best results. PMID:21978586

  7. Copper-promoted cementation of antimony in hydrochloric acid system: A green protocol.

    PubMed

    Wu, Lian-Kui; Li, Ying-Ying; Cao, Hua-Zhen; Zheng, Guo-Qu

    2015-12-15

    A new method of recovering antimony in hydrochloric acid system by cementation with copper powder was proposed and carried out at laboratory scale. Thermodynamic analysis and cyclic voltammetry test were conducted to study the cementation process. This is a novel antimony removal technology and quite meets the requirements of green chemistry. The main cement product Cu2Sb is a promising anodic material for lithium and sodium ion battery. And nearly all consumed copper powder are transformed into CuCl which is an important industrial material. The effect of reaction temperature, stoichiometric ratio of Cu to Sb(III), stirring rate and concentration of HCl on the cementation efficiency of antimony were investigated in detail. Optimized cementation condition is obtained at 60 °C for 120 min and stirring rate of 600 rpm with Cu/Sb(III) stoichiometric ratio of 6 in 3 mol L(-1) HCl. At this time, nearly all antimony can be removed by copper powder and the cementation efficiency is over 99%. The structure and morphologies of the cement products were characterized by X-ray diffraction and scanning electron microscopy, respectively. Results show that the reaction temperature has little influence on the morphology of the cement products which consist of particles with various sizes. The activation energy of the cementation antimony on copper is 37.75 kJ mol(-1), indicating a chemically controlled step. Inductively coupled plasma mass spectrometry results show that no stibine generates during the cementation process. PMID:26252996

  8. Inactivation of lambda phage infectivity and lambda deoxyribonucleic acid transfection by N-methyl-isatin beta-thiosemicarbazone-copper complexes.

    PubMed

    Levinson, W; Helling, R

    1976-01-01

    The infectivity of intact lambda phage and transfection by lambda deoxyribonucleic acid were inactivated by exposure to the copper complexes of N-methyl-isatin beta-thiosemicarbazone, thiosemicarbazide, and semicarbazide, but not methyl-isatin. No inactivation was observed when these compounds were used in the absence of copper sulfate. This confirms our previous observation that the activity of N-methyl-isatin beta-thiosemicarbazone is mediated by its thiosemicarbazone moiety and that the presence of copper is required for action. This represents the first time, to our knowledge, that semicarbazide has been found to possess antiviral activity. It is clear that these compounds act directly on deoxyribonucleic acid; whether the compounds also act on proteins has not been determined. PMID:769669

  9. On the verification of binding modes of p-dimethylaminobenzaldehyde thiosemicarbazone with mercury(II). The solid state studies

    NASA Astrophysics Data System (ADS)

    Trzesowska-Kruszynska, Agata

    2014-08-01

    Two coordination compounds of p-dimethylaminobenzaldehyde thiosemicarbazone, fluorescent chemosensor, have been synthesised from the mercury(II) nitrate and mercury(II) chloride, and subsequently characterised by IR spectroscopy, thermal analysis, as well as single crystal X-ray diffraction technique. The inorganic anion has a distinct influence on binding mode of thiosemicarbazone ligand to Hg(II) ion. In both compounds the metal to ligand stoichiometry is 1:2 and the organic ligands coordinate to Hg ion in the neutral thione form, but they differ in a ligand binding mode and the conformation of the ligand. The crystal packing of mercury(II) nitrate complex with thiosemicarbazone is controlled by the mercury chelate ring-phenylene ring π···π stacking interactions.

  10. Synthesis, characterization and binding affinities of rhenium(I) thiosemicarbazone complexes for the estrogen receptor (α/β).

    PubMed

    Núñez-Montenegro, Ara; Carballo, Rosa; Vázquez-López, Ezequiel M

    2014-11-01

    The binding affinities towards estrogen receptors (ERs) α and β of a set of thiosemicarbazone ligands (HL(n)) and their rhenium(I) carbonyl complexes [ReX(HL(n))(CO)3] (X=Cl, Br) were determined by a competitive standard radiometric assay with [(3)H]-estradiol. The ability of the coordinated thiosemicarbazone ligands to undergo deprotonation and the lability of the ReX bond were used as a synthetic strategy to obtain [Re(hpy)(L(n))(CO)3] (hpy=3- or 4-hydroxypyridine). The inclusion of the additional hpy ligand endows the new thiosemicarbazonate complexes with an improved affinity towards the estrogen receptors and, consequently, the values of the inhibition constant (Ki) could be determined for some of them. In general, the values of Ki for both ER subtypes suggest an appreciable selectivity towards ERα. PMID:25061691

  11. Antimony leaching in plastics from waste electrical and electronic equipment (WEEE) with various acids and gamma irradiation

    SciTech Connect

    Tostar, Sandra; Stenvall, Erik; Boldizar, Antal; Foreman, Mark R. St. J.

    2013-06-15

    Highlights: • We have proposed a method to recover antimony from electronic plastics. • The most efficient acid solution was sodium hydrogen tartrate in dimethyl sulfoxide. • Gamma irradiation did not influence the antimony leaching ability. - Abstract: There has been a recent interest in antimony since the availability in readily mined areas is decreasing compared to the amounts used. It is important in many applications such as flame retardants and in the production of polyester, which can trigger an investigation of the leachability of antimony from plastics using different acids. In this paper, different types of acids are tested for their ability to leach antimony from a discarded computer housing, made of poly(acrylonitrile butadiene styrene), which is a common plastic type used in electrical and electronic equipment. The acid solutions included sodium hydrogen tartrate (0.5 M) dissolved in either dimethyl sulfoxide or water (at ca. 23 °C and heated to ca. 105 °C). The metal content after leaching was determined by inductively coupled plasma optical emission spectroscopy. The most efficient leaching medium was the heated solution of sodium hydrogen tartrate in dimethyl sulfoxide, which leached almost half of the antimony from the poly(acrylonitrile butadiene styrene). Gamma irradiation, which is proposed to improve the mechanical properties in plastics, was used here to investigate the influence of antimony leaching ability. No significant change in the amount of leached antimony could be observed.

  12. Strong effect of copper(II) coordination on antiproliferative activity of thiosemicarbazone-piperazine and thiosemicarbazone-morpholine hybrids.

    PubMed

    Bacher, Felix; Dömötör, Orsolya; Chugunova, Anastasia; Nagy, Nóra V; Filipović, Lana; Radulović, Siniša; Enyedy, Éva A; Arion, Vladimir B

    2015-05-21

    In this study, 2-formylpyridine thiosemicarbazones and three different heterocyclic pharmacophores were combined to prepare thiosemicarbazone–piperazine mPip-FTSC (HL1) and mPip-dm-FTSC (HL2), thiosemicarbazone–morpholine Morph-FTSC (HL3) and Morph-dm-FTSC (HL4), thiosemicarbazone–methylpyrrole-2-carboxylate hybrids mPyrr-FTSC (HL5) and mPyrr-dm-FTSC (HL6) as well as their copper(II) complexes [CuCl(mPipH-FTSC-H)]Cl (1 + H)Cl, [CuCl(mPipH-dm-FTSC-H)]Cl (2 + H)Cl, [CuCl(Morph-FTSC-H)] (3), [CuCl(Morph-dm-FTSC-H)] (4), [CuCl(mPyrr-FTSC-H)(H2O)] (5) and [CuCl(mPyrr-dm-FTSC-H)(H2O)] (6). The substances were characterized by elemental analysis, one- and two-dimensional NMR spectroscopy (HL1–HL6), ESI mass spectrometry, IR and UV–vis spectroscopy and single crystal X-ray diffraction (1–5). All compounds were prepared in an effort to generate potential antitumor agents with an improved therapeutic index. In addition, the effect of structural alterations with organic hybrids on aqueous solubility and copper(II) coordination ability was investigated. Complexation of ligands HL2 and HL4 with copper(II) was studied in aqueous solution by pH-potentiometry, UV–vis spectrophotometry and EPR spectroscopy. Proton dissociation processes of HL2 and HL4 were also characterized in detail and microscopic constants for the Z/E isomers were determined. While the hybrids HL5, HL6 and their copper(II) complexes 5 and 6 proved to be insoluble in aqueous solution, precluding antiproliferative activity studies, the thiosemicarbazone–piperazine and thiosemicarbazone–morpholine hybrids HL1–HL4, as well as copper(II) complexes 1–4 were soluble in water enabling cytotoxicity assays. Interestingly, the metal-free hybrids showed very low or even a lack of cytotoxicity (IC50 values > 300 μM) in two human cancer cell lines HeLa (cervical carcinoma) and A549 (alveolar basal adenocarcinoma), whereas their copper(II) complexes were cytotoxic showing IC50 values from 25.5 to 65.1

  13. Effect of antimony nano-scale surface-structures on a GaSb/AlAsSb distributed Bragg reflector

    SciTech Connect

    Husaini, S.; Shima, D.; Ahirwar, P.; Rotter, T. J.; Hains, C. P.; Dang, T.; Bedford, R. G.; Balakrishnan, G.

    2013-02-11

    Effects of antimony crystallization on the surface of GaSb during low temperature molecular beam epitaxy growth are investigated. The geometry of these structures is studied via transmission electron and atomic force microscopies, which show the surface metal forms triangular-shaped, elongated nano-wires with a structured orientation composed entirely of crystalline antimony. By depositing antimony on a GaSb/AlAsSb distributed Bragg reflector, the field is localized within the antimony layer. Polarization dependent transmission measurements are carried out on these nano-structures deposited on a GaSb/AlAsSb distributed Bragg reflector. It is shown that the antimony-based structures at the surface favor transmission of light polarized perpendicular to the wires.

  14. SESPE-FRAZIER, DIABLO, MATILIJA, DRY LAKES, SAWMILL-BADLANDS, CUYAMA, ANTIMONY, AND QUATAL ROADLESS AREAS, CALIFORNIA.

    USGS Publications Warehouse

    Frizzell, Virgil A., Jr.; Hale, William N.

    1984-01-01

    The study area, consisting of the Sespe-Frazier, Diablo, Matilija, Dry Lakes, Sawmill-Badlands, Cuyama, Antimony, and Quatal Roadless Areas, occupies about 872 sq mi in the Los Padres National Forest, California. Studies indicate that the Sespe-Frazier Roadless Area contains demonstrated resources of gold, gypsum, phosphate and bentonite; deposits in the Cuyama Roadless Area have demonstrated resources of gypsum; mines in the Antimony Roadless Area have demonstrated resources of antimony, gold, silver, and marble; and the Quatal Roadless Area has demonstrated resources of bentonite. The Sespe-Frazier Roadless Area has substantiated potential for geothermal resources suitable for direct-heat purposes, probable and substantiated potential for oil and gas resources, and probable potential for gold resources. Small areas of probable resource potential for antimony and gold were identified in Antimony Roadless Area.

  15. Process for treating spent catalyst including antimony halides from chlorofluorocarbon production

    SciTech Connect

    Kalcevic, V.; McGahan, J.F.

    1988-06-14

    A process for treating spent catalyst from chlorofluorocarbon production is described wherein the catalyst includes antimony halides and undergoes hydrolysis in an aqueous medium to produce insoluble antimony compounds and fluoride ions. The process comprises hydrolyzing the catalyst in an aqueous solution of ferric chloride having a sufficient concentration of ferric ions to complex substantially all of the fluoride ions produced upon hydrolysis of the catalyst, neutralizing the reaction mass present following hydrolysis of the catalyst and complexing of the fluoride ions by contacting the reaction mass with an aqueous suspension of a compound selected from the class consisting of calcium hydroxide and magnesium hydroxide, and separating the insoluble antimony compounds from the neutralized reaction mass.

  16. The influence of nitrogen and antimony on the optical quality of InNAs(Sb) alloys

    NASA Astrophysics Data System (ADS)

    Latkowska, M.; Baranowski, M.; Linhart, W. M.; Janiaka, F.; Misiewicz, J.; Segercrantz, N.; Tuomisto, F.; Zhuang, Q.; Krier, A.; Kudrawiec, R.

    2016-03-01

    In this work we present detailed studies of the influence of nitrogen and antimony on the optical quality of InNAs(Sb) alloys. We employed photoluminescence, photoreflectance and positron annihilation spectroscopy to reveal the role of antimony and nitrogen on the improvement/degradation of the optical qualities of InNAs(Sb) alloys. A series of 1 μm-thick InNAs(Sb) layers with different nitrogen and antimony concentrations were grown by molecular beam epitaxy. The results of these investigations show that Sb atoms serve as a surfactant which effectively improves the optical quality of InNAsSb alloys. The influence of nitrogen on the optical quality however is not the same as to what has been reported for other dilute nitrides. We observed an improvement of the optical quality for some nitrogen contents. These issues are comprehensively examined and explained.

  17. Use of Antimony in the Treatment of Leishmaniasis: Current Status and Future Directions

    PubMed Central

    Haldar, Arun Kumar; Sen, Pradip; Roy, Syamal

    2011-01-01

    In the recent past the standard treatment of kala-azar involved the use of pentavalent antimonials Sb(V). Because of progressive rise in treatment failure to Sb(V) was limited its use in the treatment program in the Indian subcontinent. Until now the mechanism of action of Sb(V) is not very clear. Recent studies indicated that both parasite and hosts contribute to the antimony efflux mechanism. Interestingly, antimonials show strong immunostimulatory abilities as evident from the upregulation of transplantation antigens and enhanced T cell stimulating ability of normal antigen presenting cells when treated with Sb(V) in vitro. Recently, it has been shown that some of the peroxovanadium compounds have Sb(V)-resistance modifying ability in experimental infection with Sb(V) resistant Leishmania donovani isolates in murine model. Thus, vanadium compounds may be used in combination with Sb(V) in the treatment of Sb(V) resistance cases of kala-azar. PMID:22091408

  18. Antimony mediated growth of high-density InAs quantum dots for photovoltaic cells

    SciTech Connect

    Tutu, F. K.; Wu, J.; Lam, P.; Tang, M.; Liu, H.; Miyashita, N.; Okada, Y.; Wilson, J.; Allison, R.

    2013-07-22

    We report enhanced solar cell performance using high-density InAs quantum dots. The high-density quantum dot was grown by antimony mediated molecular beam epitaxy. In-plane quantum dot density over 1 × 10{sup 11} cm{sup −2} was achieved by applying a few monolayers of antimony on the GaAs surface prior to quantum dot growth. The formation of defective large clusters was reduced by optimization of the growth temperature and InAs coverage. Comparing with a standard quantum dot solar cell without the incorporation of antimony, the high-density quantum dot solar cell demonstrates a distinct improvement in short-circuit current from 7.4 mA/cm{sup 2} to 8.3 mA/cm{sup 2}.

  19. Spectrophotometric procedure using rhodamine B for determination of submicrogram quantities of antimony in rocks

    USGS Publications Warehouse

    Schnepfe, M.M.

    1973-01-01

    A spectrophotometric procedure using Rhodamine B is given for the determination of antimony in mineralized rocks after its separation as stibine. A study of the Rhodamine B reaction points to the importance of the order of addition of reagents in enhancing sensitivity and increasing the stability of the system. The tolerance of some 26 elements is established for the overall procedure. Although the limit of determination is approximately 0??5 ppm Sb in a 0??2-g sample, the procedure is intended primarily for screening samples containing more than 1 ppm Sb. In pure solutions 0??1 ??g of antimony can be determined with a relative standard deviation of 25%. For >0??2 ??g of antimony a relative standard deviation of 15% or less can be expected. ?? 1973.

  20. Response of cutaneous leishmaniasis (chiclero's ulcer) to treatment with meglumine antimoniate in Southeast Mexico.

    PubMed

    Vargas-Gonzalez, A; Canto-Lara, S B; Damian-Centeno, A G; Andrade-Narvaez, F J

    1999-12-01

    Cutaneous leishmaniasis, known as chiclero's ulcer in southeastern Mexico, is characterized by a predominantly single, painless, ulcerated lesion, without lymphangitis or adenopathy. When located on the ear, it tends to become chronic, causing destruction of the pinna and disfigurement. It is caused predominantly by Leishmania (L.) mexicana. Although pentavalent antimonials (Sb5+) are the mainstay of leishmanial therapy and have been used for more than 50 years, dosage regimens have been repeatedly modified and the best one has not been fully identified. The main purpose of the present study was to investigate the response of chiclero's ulcer to treatment with meglumine antimoniate. One hundred five patients were treated with meglumine antimoniate at a daily dose of 1 ampule per day (425 mg of Sb5+) until healing. The lesions healed after a mean of 25 days (range = 5-60 days). PMID:10674678

  1. Concentration transient analysis of antimony surface segregation during Si(100) molecular beam epitaxy

    NASA Technical Reports Server (NTRS)

    Markert, L. C.; Greene, J. E.; Ni, W.-X.; Hansson, G. V.; Sundgren, J.-E.

    1991-01-01

    Antimony surface segregation during Si(100) molecular beam epitaxy (MBE) was investigated at temperatures T(sub s) = 515 - 800 C using concentration transient analysis (CTA). The dopant surface coverage Theta, bulk fraction gamma, and incorporation probability sigma during MBE were determined from secondary-ion mass spectrometry depth profiles of modulation-doped films. Programmed T(sub s) changes during growth were used to trap the surface-segregated dopant overlayer, producing concentration spikes whose integrated area corresponds to Theta. Thermal antimony doping by coevaporation was found to result in segregation strongly dependent on T(sub s) with Theta(sub Sb) values up to 0.9 monolayers (ML): in films doped with Sb(+) ions accelerated by 100 V, Theta(sub Sb) was less than or equal to 4 x 10(exp -3) ML. Surface segregation of coevaporated antimony was kinematically limited for the film growth conditions in these experiments.

  2. The EM Earthquake Precursor

    NASA Astrophysics Data System (ADS)

    Jones, K. B., II; Saxton, P. T.

    2013-12-01

    Many attempts have been made to determine a sound forecasting method regarding earthquakes and warn the public in turn. Presently, the animal kingdom leads the precursor list alluding to a transmission related source. By applying the animal-based model to an electromagnetic (EM) wave model, various hypotheses were formed, but the most interesting one required the use of a magnetometer with a differing design and geometry. To date, numerous, high-end magnetometers have been in use in close proximity to fault zones for potential earthquake forecasting; however, something is still amiss. The problem still resides with what exactly is forecastable and the investigating direction of EM. After the 1989 Loma Prieta Earthquake, American earthquake investigators predetermined magnetometer use and a minimum earthquake magnitude necessary for EM detection. This action was set in motion, due to the extensive damage incurred and public outrage concerning earthquake forecasting; however, the magnetometers employed, grounded or buried, are completely subject to static and electric fields and have yet to correlate to an identifiable precursor. Secondly, there is neither a networked array for finding any epicentral locations, nor have there been any attempts to find even one. This methodology needs dismissal, because it is overly complicated, subject to continuous change, and provides no response time. As for the minimum magnitude threshold, which was set at M5, this is simply higher than what modern technological advances have gained. Detection can now be achieved at approximately M1, which greatly improves forecasting chances. A propagating precursor has now been detected in both the field and laboratory. Field antenna testing conducted outside the NE Texas town of Timpson in February, 2013, detected three strong EM sources along with numerous weaker signals. The antenna had mobility, and observations were noted for recurrence, duration, and frequency response. Next, two

  3. On-line lab-in-syringe cloud point extraction for the spectrophotometric determination of antimony.

    PubMed

    Frizzarin, Rejane M; Portugal, Lindomar A; Estela, José M; Rocha, Fábio R P; Cerdà, Victor

    2016-02-01

    Most of the procedures for antimony determination require time-consuming sample preparation (e.g. liquid-liquid extraction with organic solvents), which are harmful to the environment. Because of the high antimony toxicity, a rapid, sensitive and greener procedure for its determination becomes necessary. The goal of this work was to develop an analytical procedure exploiting for the first time the cloud point extraction on a lab-in-syringe flow system aiming at the spectrophotometric determination of antimony. The procedure was based on formation of an ion-pair between the antimony-iodide complex and H(+) followed by extraction with Triton X-114. The factorial design showed that the concentrations of ascorbic acid, H2SO4 and Triton X-114, as well as second and third order interactions were significant at the 95% confidence level. A Box-Behnken design was applied to obtain the response surfaces and to identify the critical values. System is robust at the 95% confidence level. A linear response was observed from 5 to 50 µg L(-1), described by the equation A=0.137+0.050C(Sb) (r=0.998). The detection limit (99.7% confidence level), the coefficient of variation (n=5; 15 µg L(-1)) and the sampling rate was estimated at 1.8 µg L(-1), 1.6% and 16 h(-1), respectively. The procedure allows quantification of antimony in the concentrations established by environmental legislation (6 µg L(-1)) and it was successfully applied to the determination of antimony in freshwater samples and antileishmanial drugs, yielding results in agreement with those obtained by HGFAAS at the 95% confidence level. PMID:26653503

  4. Amphiphilic Antimony(V) Complexes for Oral Treatment of Visceral Leishmaniasis

    PubMed Central

    Fernandes, Flaviana R.; Ferreira, Weverson A.; Campos, Mariana A.; Ramos, Guilherme S.; Kato, Kelly C.; Almeida, Gregório G.; Corrêa, José D.; Melo, Maria N.; Demicheli, Cynthia

    2013-01-01

    The need for daily parenteral administration is an important limitation in the clinical use of pentavalent antimonial drugs against leishmaniasis. In this study, amphiphilic antimony(V) complexes were prepared from alkylmethylglucamides (L8 and L10, with carbon chain lengths of 8 and 10, respectively), and their potential for the oral treatment of visceral leishmaniasis (VL) was evaluated. Complexes of Sb and ligand at 1:3 (SbL8 and SbL10) were obtained from the reaction of antimony(V) with L8 and L10, as evidenced by elemental and electrospray ionization-tandem mass spectrometry (ESI-MS) analyses. Fluorescence probing of hydrophobic environment and negative-staining transmission electron microscopy showed that SbL8 forms kinetically stabilized nanoassemblies in water. Pharmacokinetic studies with mice in which the compound was administered by the oral route at 200 mg of Sb/kg of body weight indicated that the SbL8 complex promoted greater and more sustained Sb levels in serum and liver than the levels obtained for the conventional antimonial drug meglumine antimoniate (Glucantime [Glu]). The efficacy of SbL8 and SbL10 administered by the oral route was evaluated in BALB/c mice infected with Leishmania infantum after a daily dose of 200 mg of Sb/kg for 20 days. Both complexes promoted significant reduction in the liver and spleen parasite burdens in relation to those in the saline-treated control group. The extent of parasite suppression (>99.96%) was similar to that achieved after Glu given intraperitoneally at 80 mg of Sb/kg/day. As expected, there was no significant reduction in the parasitic load in the group treated orally with Glu at 200 mg of Sb/(kg day). In conclusion, amphiphilic antimony(V) complexes emerge as an innovative and promising strategy for the oral treatment of VL. PMID:23796930

  5. Future trends of global atmospheric antimony emissions from anthropogenic activities until 2050

    NASA Astrophysics Data System (ADS)

    Zhou, Junrui; Tian, Hezhong; Zhu, Chuanyong; Hao, Jiming; Gao, Jiajia; Wang, Yong; Xue, Yifeng; Hua, Shenbin; Wang, Kun

    2015-11-01

    This paper presents the scenario forecast of global atmospheric antimony (Sb) emissions from anthropogenic activities till 2050. The projection scenarios are built based on the comprehensive global antimony emission inventory for the period 1995-2010 which is reported in our previous study. Three scenarios are set up to investigate the future changes of global antimony emissions as well as their source and region contribution characteristics. Trends of activity levels specified as 5 primary source categories are projected by combining the historical trend extrapolation with EIA International energy outlook 2013, while the source-specific dynamic emission factors are determined by applying transformed normal distribution functions. If no major changes in the efficiency of emission control are introduced and keep current air quality legislations (Current Legislation scenario), global antimony emissions will increase by a factor of 2 between 2010 and 2050. The largest increase in Sb emissions is projected from Asia due to large volume of nonferrous metals production and waste incineration. In case of enforcing the pollutant emission standards (Strengthened Control scenario), global antimony emissions in 2050 will stabilize with that of 2010. Moreover, we can anticipate further declines in Sb emissions for all continents with the best emission control performances (Maximum Feasible Technological Reduction scenario). Future antimony emissions from the top 10 largest emitting countries have also been calculated and source category contributions of increasing emissions of these countries present significant diversity. Furthermore, global emission projections in 2050 are distributed within a 1° × 1°latitude/longitude grid. East Asia, Western Europe and North America present remarkable differences in emission intensity under the three scenarios, which implies that source-and-country specific control measures are necessary to be implemented for abating Sb emissions from

  6. A multipoint micro antimony pH electrode for tissue surface measurements.

    PubMed

    Lund, N; Sjöberg, F; Guldbrand, H; Walfridsson, H; Edwall, G

    1984-01-01

    Based on monocrystalline antimony we have developed a multipoint tissue surface pH electrode. The six electrodes were produced by spark cutting from a large antimony single crystal. The electrodes were then cast in epoxy resin in a ring shaped structure which fitted around the MDO oxygen electrode. The antimony electrode was ground and polished to expose an undisturbed closely packed crystal plane of antimony to the measuring solution. Before and after monitoring periods standardization was performed in TRIS buffers of pH 6.72, 7.32 and 7.74 at 37 degrees C. Antimony electrode potential is influenced by oxygen. Therefore, mean tissue oxygen pressure was registered simultaneously with an MDO electrode. The oxygen sensitivity factor used in this study was 18mV/logpO2. The correction factor for the antimony electrode oxygen dependence, measured in vitro, seemed to be correct also for the in vivo state. This, however, needs further investigation. To illustrate the usefulness of the multipoint pH electrode seven normal state rabbits were studied, and thereafter four - one each in a hypoxic, hypocarbic, hypovolemic or hyperoxic situation. In the normal state tissue pH measured on a skeletal muscle surface varied from 7.0 to 7.4. In the case of tissue microcirculation shutdown (in the hypocarbic or the hypovolemic situations), the initial reaction was a scattering of the pH values, and then the development of tissue acidosis. Our conclusion is that the use of a multipoint pH sensor enables improved and more detailed monitoring of the tissue acid-base status. PMID:6546135

  7. Microbial Methylation of Metalloids: Arsenic, Antimony, and Bismuth

    PubMed Central

    Bentley, Ronald; Chasteen, Thomas G.

    2002-01-01

    A significant 19th century public health problem was that the inhabitants of many houses containing wallpaper decorated with green arsenical pigments experienced illness and death. The problem was caused by certain fungi that grew in the presence of inorganic arsenic to form a toxic, garlic-odored gas. The garlic odor was actually put to use in a very delicate microbiological test for arsenic. In 1933, the gas was shown to be trimethylarsine. It was not until 1971 that arsenic methylation by bacteria was demonstrated. Further research in biomethylation has been facilitated by the development of delicate techniques for the determination of arsenic species. As described in this review, many microorganisms (bacteria, fungi, and yeasts) and animals are now known to biomethylate arsenic, forming both volatile (e.g., methylarsines) and nonvolatile (e.g., methylarsonic acid and dimethylarsinic acid) compounds. The enzymatic mechanisms for this biomethylation are discussed. The microbial conversion of sodium arsenate to trimethylarsine proceeds by alternate reduction and methylation steps, with S-adenosylmethionine as the usual methyl donor. Thiols have important roles in the reductions. In anaerobic bacteria, methylcobalamin may be the donor. The other metalloid elements of the periodic table group 15, antimony and bismuth, also undergo biomethylation to some extent. Trimethylstibine formation by microorganisms is now well established, but this process apparently does not occur in animals. Formation of trimethylbismuth by microorganisms has been reported in a few cases. Microbial methylation plays important roles in the biogeochemical cycling of these metalloid elements and possibly in their detoxification. The wheel has come full circle, and public health considerations are again important. PMID:12040126

  8. Mercury, arsenic, antimony, and selenium contents of sediment from the Kuskokwim River, Bethel, Alaska, USA

    USGS Publications Warehouse

    Belkin, H.E.; Sparck, H.M.

    1993-01-01

    The Kuskokwim River at Bethel, Alaska, drains a major mercury-antimony metallogenic province in its upper reaches and tributaries. Bethel (population 4000) is situated on the Kuskokwim floodplain and also draws its water supply from wells located in river-deposited sediment. A boring through overbank and floodplain sediment has provided material to establish a baseline datum for sediment-hosted heavy metals. Mercury (total), arsenic, antimony, and selenium contents were determined; aluminum was also determined and used as normalizing factor. The contents of the heavy metals were relatively constant with depth and do not reflect any potential enrichment from upstream contaminant sources. ?? 1993 Springer-Verlag.

  9. Vascular Precursor Cells

    PubMed Central

    Chaudhury, Hera; Goldie, Lauren C.

    2011-01-01

    Understanding the mechanisms that regulate the proliferation and differentiation of human stem and progenitor cells is critically important for the development and optimization of regenerative medicine strategies. For vascular regeneration studies, specifically, a true “vascular stem cell” population has not yet been identified. However, a number of cell types that exist endogenously, or can be generated or propagated ex vivo, function as vascular precursor cells and can participate in and/or promote vascular regeneration. Herein, we provide an overview of what is known about the regulation of their differentiation specifically toward a vascular endothelial cell phenotype. PMID:22866199

  10. Manganese(II) complexes with thiosemicarbazones as potential anti-Mycobacterium tuberculosis agents.

    PubMed

    Oliveira, Carolina G; da S Maia, Pedro Ivo; Souza, Paula C; Pavan, Fernando R; Leite, Clarice Q F; Viana, Rommel B; Batista, Alzir A; Nascimento, Otaciro R; Deflon, Victor M

    2014-03-01

    Through a systematic variation on the structure of a series of manganese complexes derived from 2-acetylpyridine-N(4)-R-thiosemicarbazones (Hatc-R), structural features have been investigated with the aim of obtaining complexes with potent anti-Mycobacterium tuberculosis activity. The analytical methods used for characterization included FTIR, EPR, UV-visible, elemental analysis, cyclic voltammetry, magnetic susceptibility measurement and single crystal X-ray diffractometry. Density functional theory (DFT) calculations were performed in order to evaluate the contribution of the thiosemicarbazonate ligands on the charge distribution of the complexes by changing the peripheral groups as well as to verify the Mn-donor atoms bond dissociation predisposition. The results obtained are consistent with the monoanionic N,N,S-tridentate coordination of the thiosemicarbazone ligands, resulting in octahedral complexes of the type [Mn(atc-R)2], paramagnetic in the extension of 5 unpaired electrons, whose EPR spectra are consistent for manganese(II). The electrochemical analyses show two nearly reversible processes, which are influenced by the peripheral substituent groups at the N4 position of the atc-R(1-) ligands. The minimal inhibitory concentration (MIC) of these compounds against M. tuberculosis as well as their in vitro cytotoxicity on VERO and J774A.1 cells (IC50) was determined in order to find their selectivity index (SI) (SI=IC50/MIC). The results evidenced that the compounds described here can be considered as promising anti-M. tuberculosis agents, with SI values comparable or better than some commercial drugs available for the tuberculosis treatment. PMID:24188534

  11. Discovery of trypanocidal thiosemicarbazone inhibitors of rhodesain and TbcatB

    PubMed Central

    Mallari, Jeremy P.; Shelat, Anang; Kosinski, Aaron; Caffrey, Conor R.; Connelly, Michele; Zhu, Fangyi; McKerrow, James H.; Guy, R. Kiplin

    2008-01-01

    Human African trypanosomiasis (HAT) is caused by the protozoan parasite Trypanosoma brucei. The cysteine proteases of T.brucei have been shown to be crucial for parasite replication and represent an attractive point for therapeutic intervention. Herein we describe the synthesis of a series of thiosemicarbazones and their activity against the trypanosomal cathepsins TbcatB and rhodesain, as well as human cathepsins L and B. The activity of these compounds was determined against cultured T.brucei, and specificity was assessed with a panel of four mammalian cell lines. PMID:18420405

  12. Spectral studies of coordination compounds of cobalt(II) with thiosemicarbazone of heterocyclic ketone

    NASA Astrophysics Data System (ADS)

    Chandra, Sulekh; Kumar, Umendra

    2005-12-01

    The paper presents the spectral analysis of cobalt(II) complexes with indoxyl thiosemicarbazone (ITSC) of general composition [CoL 2X 2] (where L = ITSC, X = Cl -, NO 3-, (1/2)SO 42-, NCS -). The geometry of the complexes have been characterized by elemental analysis, molar conductance, magnetic susceptibility measurements and spectral (electronic, IR, EPR, 1H NMR, mass) studies. The various physico-chemical techniques suggested a coordination number of six (octahedral) for chloro, nitrato and thiocyanato complexes. Whereas sulfato complex was found to have five coordinate trigonal-bipyramidal geometry. All the complexes are of high spin type showing magnetic moment corresponding to three unpaired electrons.

  13. Microwave assisted synthesis, X-ray crystallography and DFT calculations of selected aromatic thiosemicarbazones

    NASA Astrophysics Data System (ADS)

    Serda, Maciej; Małecki, Jan G.; Mrozek-Wilczkiewicz, Anna; Musioł, Robert; Polański, Jarosław

    2013-04-01

    Series of four benzaldehyde thiosemicarbazones has been synthesized under microwave irradiation and characterized structurally by means of infrared and NMR spectroscopies and mass spectrometry. Their crystal structures were determined by single crystal X-ray analysis followed by DFT calculations. Partial charges on the molecular surface and dipole moments of the structures were calculated. Crystal structures are stabilized by intramolecular hydrogen bonding and stacking interactions. Studied compounds are interesting as antiproliferative and antifungal agents acting through interactions with iron. Thus presented results may be useful in design new more active or specific structures.

  14. Synthesis and spectroscopic study on photochromism of a new thiosemicarbazone compound containing pyrazolone

    NASA Astrophysics Data System (ADS)

    Chai, Hui; Liu, Guangfei; Liu, Lang; Jia, Dianzeng

    2005-09-01

    A new photochromic compound 1,3-diphenyl-4-(4'-fluro)benzal-5-pyrazolone-4-ethyl thiosemicarbazone (DP4FBP-ETSC) was synthesized by direct condensation of 1,3-diphenyl-5-pyrazolone with N(4)-ethyl thiosemicarbazide. The product was characterized by elemental analysis, IR and 1H NMR spectra. The photochromic properties of the compound were studied using time-dependent fluorescence emission spectra, the UV-vis reflection spectra in the solid state and the UV-vis absorption spectroscopy in liquid. The reaction rate constant of compound was also analyzed. The results show that DP4FBP-ETSC can perform photochromism.

  15. The supramolecular chemistry of thiosemicarbazones derived from pyrrole: a structural view

    NASA Astrophysics Data System (ADS)

    Alonso, Ruben; Bermejo, Elena; Carballo, Rosa; Castiñeiras, Alfonso; Pérez, Teresa

    2002-03-01

    Condensation of 2-formylpyrrole or 2-acetylpyrrole with thiosemicarbazide or with N-methyl-, N-ethyl-, N-phenyl- or (for 2-formylpyrrole) N-dimethylthiosemicarbazide afforded nine thiosemicarbazones that were characterized by elemental analysis, mass spectrometry, IR and NMR spectroscopy and, when possible, X-ray-diffractometric structure analysis. N-H⋯S hydrogen bonds (and N-H⋯O and/or O-H⋯S bonds in the structures with water or DMSO of crystallization) give rise to supramolecular structures that in some cases are probably stabilized by π-π interactions.

  16. Coordination Chemistry of Polyaromatic Thiosemicarbazones 2: Synthesis and Biological Activity of Zinc, Cobalt, and Copper Complexes of 1-(Naphthalene-2-yl)ethanone Thiosemicarbazone

    PubMed Central

    LeBlanc, Marc-Andre; Gonzalez-Sarrías, Antonio; Beckford, Floyd A.; Mbarushimana, P. Canisius; Seeram, Navindra P.

    2012-01-01

    A novel thiosemicarbazone from 2-acetonaphthone (represented as acnTSC) has been synthesized and its basic coordination chemistry with zinc(II), cobalt(II), and copper(II) explored. The complexes were characterized by elemental analysis and various spectroscopic techniques and are best formulated as [M(acnTSC)2Cl2] with the metal likely in an octahedral environment. The anticancer activity of the complexes was determined against a panel of human colon cancer cells (HCT-116 and Caco-2). The compounds bind to DNA via an intercalative mode with binding constants of 9.7 × 104 M−1, 1.8 × 105 M−1, and 9.5 × 104 M−1 for the zinc, cobalt, and copper complexes, respectively. PMID:22303515

  17. Synthesis, experimental and theoretical studies on its crystal structure and FT-IR spectrum of new thiosemicarbazone compound E-2-(4-isopropylbenzylidene)thiosemicarbazone

    NASA Astrophysics Data System (ADS)

    Khalaji, Aliakbar Dehno; Mehrani, Sepideh; Eigner, Vaclav; Dusek, Michal

    2013-09-01

    The title compound E-2-(4-isopropylbenzylidene)thiosemicarbazone (1) derived from the reaction of 4-isopropylbenzaldehyde and thiosemicarbazide in ethanol solution has been synthesized and characterized by elemental analyses, FT-IR and 1H NMR spectroscopy and single-crystal X-ray diffraction. Its optimized geometry together with the theoretical assignment of the vibrational frequencies of the title compound has been computed by using density functional theory (DFT) method. In the gas phase the four conformers of the title compound were found and it was found that the conformer Sn1 is the most stable one. The title compound crystallizes in the monoclinic space group P21/c with unit cell parameters: a = 14.4054(4), b = 5.6832(10), c = 14.4337(3) Å, β = 93.306(2)°, V = 1179.70(5) Å3 and Z = 4.

  18. Syntheses and spectroscopic studies on zinc(II) and mercury(II) complexes of isatin-3-thiosemicarbazone

    NASA Astrophysics Data System (ADS)

    Akinchan, N. T.; Drożdżewski, P. M.; Holzer, W.

    2002-10-01

    Zinc(II) and mercury(II) complexes were prepared by reacting isatin-3-thiosemicarbazone (ISTSCH) with zinc(II) acetate or mercury(II) bromide. The complexes were characterized by IR, Raman, diffuse reflectance, 1H and 13C NMR spectra and elemental analysis. Tetrahedral structures for Zn(ISTSC) 2 and Hg(ISTSCH)Br 2 are suggested.

  19. Electrodeposition and device incorporation of bismuth antimony nanowire arrays

    NASA Astrophysics Data System (ADS)

    Keyani, Jennifer

    Thermoelectric materials have the unique property where the application of a potential difference across the material results in the formation of a temperature gradient, and vice versa. There is continued interest in bulk thermoelectric materials for power generation and refrigeration applications, however these materials are not currently in widespread use due to their low conversion efficiency. It has been predicted that nanostructured thermoelectric materials will show enhanced performance over their bulk counterparts. In this study, bismuth antimony (Bi1-xSbx) nanowire arrays have been synthesized and assembled into devices in order to demonstrate an enhanced performance in nanostructured thermoelectric materials. Bi1-xSbx nanowire arrays were fabricated by potentiostatic electrodeposition into porous alumina templates from a dimethyl sulfoxide (DMSO) solution. The nanowire composition and texture were studied as a function of the electrodeposition conditions in order to maximize their thermoelectric performance. Energy dispersive spectrometry and electron microprobe analysis were used to study the nanowire composition as a function of the electroactive and non-electroactive species in solution. Texturing in the nanowire arrays was observed by X-ray diffraction and controlled by the applied voltage and presence of supporting electrolyte. The nanowire arrays were also optimized for device incorporation by maximizing the number of nanowires and minimizing their length distribution. The areal density of nanowire arrays was on the order of 1010 wires/cm2 due to the high density of pores in the alumina and the high degree to which those pores were filled with electrodeposited material. A narrow distribution of nanowire lengths was observed by scanning electron microscopy across millimeter-length portions of the arrays. A hybrid nanowire-bulk thermoelectric device was assembled after electrical contacts were electrodeposited over Bi1-xSbx nanowire arrays. Nickel was

  20. Increased generation of intracellular reactive oxygen species initiates selective cytotoxicity against the MCF-7 cell line resultant from redox active combination therapy using copper-thiosemicarbazone complexes.

    PubMed

    Akladios, Fady N; Andrew, Scott D; Parkinson, Christopher J

    2016-06-01

    The combination of cytotoxic copper-thiosemicarbazone complexes with phenoxazines results in an up to 50-fold enhancement in the cytotoxic potential of the thiosemicarbazone against the MCF-7 human breast adenocarcinoma cell line over the effect attributable to drug additivity-allowing minimization of the more toxic copper-thiosemicarbazone component of the therapy. The combination of a benzophenoxazine with all classes of copper complex examined in this study proved more effective than combinations of the copper complexes with related isoelectronic azines. The combination approach results in rapid elevation of intracellular reactive oxygen levels followed by apoptotic cell death. Normal fibroblasts representative of non-cancerous cells (MRC-5) did not display a similar elevation of reactive oxygen levels when exposed to similar drug levels. The minimization of the copper-thiosemicarbazone component of the therapy results in an enhanced safety profile against normal fibroblasts. PMID:26951232

  1. 78 FR 67141 - Antimony Trioxide (ATO) TSCA Chemical Risk Assessment; Notice of Public Meetings and Opportunity...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2013-11-08

    ... AGENCY Antimony Trioxide (ATO) TSCA Chemical Risk Assessment; Notice of Public Meetings and Opportunity... Substances Control Act (TSCA) chemical risk assessment, ``TSCA Workplan Chemical Risk Assessment for ATO... CONTACT: For technical information contact: Stan Barone, Jr., Risk Assessment Division (7403M), Office...

  2. Thermodynamics for arsenic and antimony in copper matte converting—computer simulation

    NASA Astrophysics Data System (ADS)

    Chaubal, P. C.; Nagamori, M.

    1988-08-01

    Thermodynamic data for arsenic and antimony and their sulfide and oxide gases have been critically reviewed and compiled. The entropy values for AsS(g), SbS(g), and BiS(g) have been recalculated based on a statistical thermodynamic method. The standard heat of formation and entropy of As2O3(g) have been newly assessed to be △H{298/0} = -81,500 cal/mole and S{298/0} = 81.5 cal/deg/mole. Copper matte converting has been mathematically described using the stepwise equilibrium simulation technique together with quadratic approximations of oxygen and magnetite solubilities in molten mattes. A differential equation for the volatilization of arsenic and antimony has been derived and solved for successive reaction microsteps, whereby the volatilization, slagging, and alloying of the minor elements in copper matte converting have been examined as functions of reaction time and other process variables. Only the first (slag-making) stage of converting is responsible for the elimination of arsenic and antimony by volatilization. Arsenic volatilizes mainly as AsS(g) and AsO(g), with As2(g) also contributing when initial mattes are unusually rich in arsenic (above 0.5 pct arsenic). Antimony volatilizes chiefly as SbS(g), and the contributions of other gases such as SbO(g) and Sb(g) always remain negligibly low. The results of the stepwise equilibrium simulation compare favorably with the industrial operating data.

  3. An Insight into Sodiation of Antimony from First-Principles Crystal Structure Prediction

    NASA Astrophysics Data System (ADS)

    Caputo, Riccarda

    2016-02-01

    Elemental antimony has recently become an attractive anode material for potential application in rechargeable sodium-ion batteries. I present a first-principles study of the structure-composition dependence of the Na-Sb system for both sodiation and desodiation processes. The enthalpy of reaction of x moles of sodium with the hexagonal structure of antimony reveals several stable crystal structures for 0 < x ≤ 3, with variable composition states for 1.25 < x < 2.75. The direct and reverse reactions pass through similar states in terms of enthalpy of formation and symmetry representation of the corresponding optimized structures, in particular for x = 1 and x = 3, confirming the two known phases, namely NaSb and Na3Sb. The calculations suggest that the optimal composition range for reversible sodiation of antimony is 1 < x ≤ 3, thus avoiding the global minimum at x = 1. This can help to rationalize the structure-composition dependence of the electrochemical performance of antimony in Na-ion batteries.

  4. Nanostructured Carbon/Antimony Composites as Anode Materials for Lithium-Ion Batteries with Long Life.

    PubMed

    Cheng, Yong; Yi, Zheng; Wang, Chunli; Wang, Lidong; Wu, Yaoming; Wang, Limin

    2016-08-01

    A series of nanostructured carbon/antimony composites have been successfully synthesized by a simple sol-gel, high-temperature carbon thermal reduction process. In the carbon/antimony composites, antimony nanoparticles are homogeneously dispersed in the pyrolyzed nanoporous carbon matrix. As an anode material for lithium-ion batteries, the C/Sb10 composite displays a high initial discharge capacity of 1214.6 mAh g(-1) and a reversible charge capacity of 595.5 mAh g(-1) with a corresponding coulombic efficiency of 49 % in the first cycle. In addition, it exhibits a high reversible discharge capacity of 466.2 mAh g(-1) at a current density of 100 mA g(-1) after 200 cycles and a high rate discharge capacity of 354.4 mAh g(-1) at a current density of 1000 mA g(-1) . The excellent cycling stability and rate discharge performance of the C/Sb10 composite could be due to the uniform dispersion of antimony nanoparticles in the porous carbon matrix, which can buffer the volume expansion and maintain the integrity of the electrode during the charge-discharge cycles. PMID:27310879

  5. Mechanisms of antimony adsorption onto soybean stover-derived biochar in aqueous solutions

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Limited mechanistic knowledge is available to understand how biochar interacts with trace elements that exist predominantly as oxoanions, such as antimony (Sb). Soybean stover biochars were produced at 300 degrees C (SBC300) and 700 degrees C (SBC700), and were characterized by BET, Boehm titration,...

  6. Thermodynamics for arsenic and antimony in copper matte converting; Computer simulation

    SciTech Connect

    Chaubal, P.C. ); Nagamori, M. )

    1989-08-01

    In this paper thermodynamic data for arsenic and antimony and their sulfide and oxide gases have been critically reviewed and compiled. The entropy values for AsS(g), SbS(g), and BiS(g) have been recalculated based on a statistical thermodynamic method. The standard heat of formation and entropy of As/sub 2/O/sub 3/(g) have been newly assessed. Copper matte converting has been mathematically described using the stepwise equilibrium simulation technique together with quadratic approximations of oxygen and magnetite solubilities in molten mattes. A differential equation for the volatilization of arsenic and antimony has been solved for successive reaction microsteps whereby the volatilization, slagging, and alloying of the minor elements have been examined as functions of reaction time and other process variables. Only the first (slag-making) stage of converting is responsible for the elimination of arsenic and antimony by volatilization. Arsenic volatilizes mainly as AsS(g) and AsO(g), with As/sub 2/(g) also contributing when initial mattes are unusually rich in arsenic (above 0.5 pct arsenic). Antimony volatilizes chiefly as SbS(g), and the contributions of other gases such as SbO(g) and Sb(g) remain negligibly low. The results of the simulation compare favorably with industrial operating data.

  7. [Oxidation of gold-antimony ores by a thermoacidophilic microbial consortium].

    PubMed

    Tsaplina, I A; Sorokin, V V; Zhuravleva, A E; Melamud, V S; Bogdanova, T I; Kondrat'eva, T F

    2013-01-01

    Antimony leaching from sulfide ore samples by an experimental consortium of thermoacidophilic microorganisms, including Sulfobacillus, Leptospirillum, and Ferroplasma strains was studied. The ores differed significantly in the content of the major metal sulfides (%): Sb(S), 0.84 to 29.95; Fe(S), 0.47 to 2.5, and As(S), 0.01 to 0.4. Independent on the Sb(S) concentration in the experimental sample, after adaptation to a specific ore and pulp compaction the microorganisms grew actively and leached/oxidized all gold-antimony ores at 39 ± 1 degrees C. The lower was the content of iron and arsenic sulfides, the higher was antimony leaching. For the first time the investigations conducted with the use of X-ray microanalysis research made it possible to conclude that in a natural high-antimony ore Sb inhibits growth of only a part of the cell population and that Ca, Fe, and Sb may compete for the binding centers of the cell. PMID:25509404

  8. Hepatotoxicity of Pentavalent Antimonial Drug: Possible Role of Residual Sb(III) and Protective Effect of Ascorbic Acid

    PubMed Central

    Kato, Kelly C.; Morais-Teixeira, Eliane; Reis, Priscila G.; Silva-Barcellos, Neila M.; Salaün, Pascal; Campos, Paula P.; Dias Corrêa-Junior, José; Rabello, Ana; Demicheli, Cynthia

    2014-01-01

    Pentavalent antimonial drugs such as meglumine antimoniate (Glucantime [Glu; Sanofi-Aventis, São Paulo, Brazil]) produce severe side effects, including cardiotoxicity and hepatotoxicity, during the treatment of leishmaniasis. We evaluated the role of residual Sb(III) in the hepatotoxicity of meglumine antimoniate, as well as the protective effect of the antioxidant ascorbic acid (AA) during antimonial chemotherapy in a murine model of visceral leishmaniasis. BALB/c mice infected with Leishmania infantum were treated intraperitoneally at 80 mg of Sb/kg/day with commercial meglumine antimoniate (Glu) or a synthetic meglumine antimoniate with lower Sb(III) level (MA), in association or not with AA (15 mg/kg/day), for a 20-day period. Control groups received saline or saline plus AA. Livers were evaluated for hepatocytes histological alterations, peroxidase activity, and apoptosis. Increased proportions of swollen and apoptotic hepatocytes were observed in animals treated with Glu compared to animals treated with saline or MA. The peroxidase activity was also enhanced in the liver of animals that received Glu. Cotreatment with AA reduced the extent of histological changes, the apoptotic index, and the peroxidase activity to levels corresponding to the control group. Moreover, the association with AA did not affect the hepatic uptake of Sb and the ability of Glu to reduce the liver and spleen parasite loads in infected mice. In conclusion, our data supports the use of pentavalent antimonials with low residue of Sb(III) and the association of pentavalent antimonials with AA, as effective strategies to reduce side effects in antimonial therapy. PMID:24189251

  9. Human biomonitoring of arsenic and antimony in case of an elevated geogenic exposure.

    PubMed Central

    Gebel, T W; Suchenwirth, R H; Bolten, C; Dunkelberg, H H

    1998-01-01

    Part of the northern Palatinate region in Germany is characterized by elevated levels of arsenic and antimony in the soil due to the presence of ore sources and former mining activities. In a biomonitoring study, 218 residents were investigated for a putative increased intake of these elements. Seventy-six nonexposed subjects in a rural region in south lower Saxony were chosen as the reference group. Urine and scalp hair samples were obtained as surrogates to determine the internal exposures to arsenic and antimony. The analyses were performed using graphite furnace atomic absorption spectrometry except for arsenic in urine, which was determined by the hydride technique. This method does not detect organoarsenicals from seafood, which are not toxicologically relevant. In the northern Palatinate subjects, slightly elevated arsenic contents in urine and scalp hair (presumably not hazardous) could be correlated with an increased arsenic content in the soil. On the other hand, the results did not show a correlation between the antimony contents in the soil of the housing area and those in urine and hair. Except for antimony in scalp hair, age tended to be associated with internal exposures to arsenic and antimony in both study groups. Consumption of seafood had a slight impact on the level of urinary arsenic, which is indicative of the presence of low quantities of inorganic arsenicals and dimethylarsinic acid in seafood. The arsenic and antimony contents in scalp hair were positively correlated with the 24-hr arsenic excretion in urine. However, antimony in scalp hair was not correlated with seafood consumption as was arsenic in scalp hair and in urine. This indicated the existence of unidentified common pathways of exposure contributing to the alimentary body burden. Short time peaks in the 24-hr excretion of arsenic in urine, which could not be assigned to a high consumption of seafood, were detected for six study participants. This suggests that additional factors

  10. Biochemical removal of HAP precursors from coal. Technical progress report, January--March 1996

    SciTech Connect

    1996-08-01

    Shake flask bioleaching tests were conducted with Pittsburgh NO. 8 and Indiana No. 5 coal. Bacteria removed pyritic sulfur from both coals at maximum rates of 5 to 9% per day, which was about 20 times the abiotic rate of pyrite oxidation. Concentrations of inorganic hazardous air pollutant (HAP) precursor elements in starting coal, bioleached coal and in leach solutions were measured. Of the 13 HAP precursors, significant amounts of arsenic, cobalt, cadmium, manganese, and nickel were removed from both coals by bacterial activity and also by the acidic leach solutions in control flasks. Little or no mercury, lead, beryllium, chromium, antimony, fluorine or chlorine was removed from the coals. Selenium was bioleached from both coals as determined by analysis of Se in leach solutions. However, analyses of Se in starting coal and in coal residues remains problematic. With very few exceptions, mass balances for the HAP precursors ranged from 80 to 120%. Improved analytical methods were developed for measuring concentrations of Hg, Se, As, and Sb in coal. Shake flask tests with pyrite oxidizing bacteria were conducted on Pittsburgh No. 8 and Indiana No. 5 coal. Concentrations of HAP precursors in the starting coal, leach solutions, and final coal residues were measured. A column leaching-rotating biological contactor (RBC) unit was assembled and a column leach test with Pittsburgh No. 8 coal was begun.

  11. Synthesis and Characterization of New Palladium(II) Thiosemicarbazone Complexes and Their Cytotoxic Activity against Various Human Tumor Cell Lines

    PubMed Central

    Hernández, Wilfredo; Paz, Juan; Carrasco, Fernando; Spodine, Evgenia; Manzur, Jorge; Sieler, Joachim; Blaurock, Steffen; Beyer, Lothar

    2013-01-01

    The palladium(II) bis-chelate complexes of the type [Pd(TSC1-5)2] (6–10), with their corresponding ligands 4-phenyl-1-(acetone)-thiosemicarbazone, HTSC1 (1), 4-phenyl-1-(2′-chloro-benzaldehyde)-thiosemicarbazone, HTSC2 (2), 4-phenyl-1-(3′-hydroxy-benzaldehyde)-thiosemicarbazone, HTSC3 (3), 4-phenyl-1-(2′-naphthaldehyde)-thiosemicarbazone, HTSC4 (4), and 4-phenyl-1-(1′-nitro-2′-naphthaldehyde)-thiosemicarbazone, HTSC5 (5), were synthesized and characterized by elemental analysis and spectroscopic techniques (IR and 1H- and 13C-NMR). The molecular structure of HTSC3, HTSC4, and [Pd(TSC1)2] (6) have been determined by single crystal X-ray crystallography. Complex 6 shows a square planar geometry with two deprotonated ligands coordinated to PdII through the azomethine nitrogen and thione sulfur atoms in a cis arrangement. The in vitro cytotoxic activity measurements indicate that the palladium(II) complexes (IC50 = 0.01–9.87 μM) exhibited higher antiproliferative activity than their free ligands (IC50 = 23.48–70.86 and >250 μM) against different types of human tumor cell lines. Among all the studied palladium(II) complexes, the [Pd(TSC3)2] (8) complex exhibited high antitumor activity on the DU145 prostate carcinoma and K562 chronic myelogenous leukemia cells, with low values of the inhibitory concentration (0.01 and 0.02 μM, resp.). PMID:24391528

  12. Examination of the Impact of Copper(II) α-(N)-Heterocyclic Thiosemicarbazone Complexes on DNA Topoisomerase IIα.

    PubMed

    Wilson, James T; Jiang, Xiaohua; McGill, Bradley C; Lisic, Edward C; Deweese, Joseph E

    2016-04-18

    Type II DNA topoisomerases resolve topological knots and tangles in DNA that result from routine cellular processes and are effective targets for anticancer therapeutics. To this end, thiosemicarbazones have been identified as having the ability to kill cancer cells from several cell lines. Literature evidence suggests that at least some thiosemicarbazones have an impact on topoisomerase II activity. However, the mechanism is not as clearly defined. Therefore, we set out to analyze the activity of four α-(N)-heterocyclic thiosemicarbazone compounds against topoisomerase IIα. The ligands, acetylpyridine-ethylthiosemicarbazone (APY-ETSC) and acetylpyrazine-methylthiosemicarbazone (APZ-MTSC), and their copper(II) [Cu(II)] complexes [Cu(APY-ETSC)Cl] and [Cu(APZ-MTSC)Cl] were examined for the ability to impact the catalytic cycle of human topoisomerase IIα. Both [Cu(APY-ETSC)Cl] and [Cu(APZ-MTSC)Cl] were more effective at inhibiting DNA relaxation compared with the ligands alone. Further, both [Cu(APY-ETSC)Cl] and [Cu(APZ-MTSC)Cl] increased double-stranded DNA cleavage levels without inhibiting topoisomerase IIα-mediated DNA ligation. The Cu(II) complexes inactivate enzyme activity over time suggesting a critical interaction with the enzyme. Additionally, we found that the Cu(II)-thiosemicarbazone complexes do not significantly impact DNA cleavage by the catalytic core of the enzyme. This evidence is supported by the fact that both [Cu(APY-ETSC)Cl] and [Cu(APZ-MTSC)Cl], and to a lesser extent the ligands, inhibit topoisomerase IIα-mediated ATP hydrolysis. Based upon kinetic analysis, the Cu(II) complexes appear to be noncompetitive inhibitors of the ATPase domain of topoisomerase IIα. Taken together, our results provide evidence that Cu(II) complexes of α-(N)-heterocyclic thiosemicarbazones catalytically inhibit the enzyme through the ATPase domain but also promote double-stranded DNA cleavage by the enzyme. PMID:26982206

  13. An interstellar precursor mission

    NASA Technical Reports Server (NTRS)

    Jaffe, L. D.; Ivie, C.; Lewis, J. C.; Lipes, R. G.; Norton, H. N.; Stearns, J. W.; Stimpson, L.; Weissman, P.

    1977-01-01

    A mission out of the planetary system, with launch about the year 2000, could provide valuable scientific data as well as test some of the technology for a later mission to another star. Primary scientific objectives for the precursor mission concern characteristics of the heliopause, the interstellar medium, stellar distances (by parallax measurements), low energy cosmic rays, interplanetary gas distribution, and mass of the solar system. Secondary objectives include investigation of Pluto. Candidate science instruments are suggested. Individual spacecraft systems for the mission were considered, technology requirements and problem areas noted, and a number of recommendations made for technology study and advanced development. The most critical technology needs include attainment of 50-yr spacecraft lifetime and development of a long-life NEP system.

  14. Identified EM Earthquake Precursors

    NASA Astrophysics Data System (ADS)

    Jones, Kenneth, II; Saxton, Patrick

    2014-05-01

    Many attempts have been made to determine a sound forecasting method regarding earthquakes and warn the public in turn. Presently, the animal kingdom leads the precursor list alluding to a transmission related source. By applying the animal-based model to an electromagnetic (EM) wave model, various hypotheses were formed, but the most interesting one required the use of a magnetometer with a differing design and geometry. To date, numerous, high-end magnetometers have been in use in close proximity to fault zones for potential earthquake forecasting; however, something is still amiss. The problem still resides with what exactly is forecastable and the investigating direction of EM. After a number of custom rock experiments, two hypotheses were formed which could answer the EM wave model. The first hypothesis concerned a sufficient and continuous electron movement either by surface or penetrative flow, and the second regarded a novel approach to radio transmission. Electron flow along fracture surfaces was determined to be inadequate in creating strong EM fields, because rock has a very high electrical resistance making it a high quality insulator. Penetrative flow could not be corroborated as well, because it was discovered that rock was absorbing and confining electrons to a very thin skin depth. Radio wave transmission and detection worked with every single test administered. This hypothesis was reviewed for propagating, long-wave generation with sufficient amplitude, and the capability of penetrating solid rock. Additionally, fracture spaces, either air or ion-filled, can facilitate this concept from great depths and allow for surficial detection. A few propagating precursor signals have been detected in the field occurring with associated phases using custom-built loop antennae. Field testing was conducted in Southern California from 2006-2011, and outside the NE Texas town of Timpson in February, 2013. The antennae have mobility and observations were noted for

  15. Identification of differential anti-neoplastic activity of copper bis(thiosemicarbazones) that is mediated by intracellular reactive oxygen species generation and lysosomal membrane permeabilization.

    PubMed

    Stefani, Christian; Al-Eisawi, Zaynab; Jansson, Patric J; Kalinowski, Danuta S; Richardson, Des R

    2015-11-01

    Bis(thiosemicarbazones) and their copper (Cu) complexes possess unique anti-neoplastic properties. However, their mechanism of action remains unclear. We examined the structure-activity relationships of twelve bis(thiosemicarbazones) to elucidate factors regarding their anti-cancer efficacy. Importantly, the alkyl substitutions at the diimine position of the ligand backbone resulted in two distinct groups, namely, unsubstituted/monosubstituted and disubstituted bis(thiosemicarbazones). This alkyl substitution pattern governed their: (1) Cu(II/I) redox potentials; (2) ability to induce cellular (64)Cu release; (3) lipophilicity; and (4) anti-proliferative activity. The potent anti-cancer Cu complex of the unsubstituted bis(thiosemicarbazone) analog, glyoxal bis(4-methyl-3-thiosemicarbazone) (GTSM), generated intracellular reactive oxygen species (ROS), which was attenuated by Cu sequestration by a non-toxic Cu chelator, tetrathiomolybdate, and the anti-oxidant, N-acetyl-l-cysteine. Fluorescence microscopy suggested that the anti-cancer activity of Cu(GTSM) was due, in part, to lysosomal membrane permeabilization (LMP). For the first time, this investigation highlights the role of ROS and LMP in the anti-cancer activity of bis(thiosemicarbazones). PMID:26335599

  16. A novel zinc bis(thiosemicarbazone) complex for live cell imaging.

    PubMed

    Dayal, Disha; Palanimuthu, Duraippandi; Shinde, Sridevi Vijay; Somasundaram, Kumaravel; Samuelson, Ashoka G

    2011-04-01

    Fluorescent zinc complexes have recently attracted a lot of interest owing to their vast applications in cellular imaging. We report the synthesis as well as physical, chemical and biological studies of a novel zinc glyoxalbis(4-methyl-4-phenyl-3-thiosemicarbazone), [Zn(GTSC)]₃, complex. As compared with the well-studied zinc biacetylbis(4-methyl-3-thiosemicarbazone), Zn(ATSM), complex, which was used as a reference, [Zn(GTSC)]₃ had 2.5-fold higher fluorescence. When cellular fluorescence was measured using flow cytometry, we observed that [Zn(GTSC)]₃ had 3.4-fold to 12-fold higher fluorescence than Zn(ATSM) in various cell lines (n = 9) of different tissue origin. Confocal fluorescence microscopy results showed that [Zn(GTSC)]₃ appeared to have a nuclear localization within 30 min of addition to MCF7 cells. Moreover, [Zn(GTSC)]₃ showed minimal cytotoxicity compared with Zn(ATSM), suggesting that [Zn(GTSC)]₃ may be less deleterious to cells when used as an imaging agent. Our data suggest that the novel [Zn(GTSC)]₃ complex can potentially serve as a biocompatible fluorescent imaging agent for live cells. PMID:21384247

  17. Generating nanoparticles containing a new 4-nitrobenzaldehyde thiosemicarbazone compound with antileishmanial activity.

    PubMed

    Britta, Elizandra Aparecida; da Silva, Cleuza Conceição; Rubira, Adley Forti; Nakamura, Celso Vataru; Borsali, Redouane

    2016-12-01

    Thiosemicarbazones are an important class of compounds that have been extensively studied in recent years, mainly because of their broad profile of pharmacological activity. A new 4-nitrobenzaldehyde thiosemicarbazone compound (BZTS) that was derived from S-limonene has been demonstrated to have significant antiprotozoan activity. However, the hydrophobic characteristic of BZTS limits its administration and results in low oral bioavailability. In the present study, we proposed the synthesis of nanoparticle-based block copolymers that can encapsulate BZTS, with morphological evaluation of the nanoparticle suspensions being performed by transmission and cryo-transmission electronic microscopy. The mean particle sizes of the nanoparticle suspensions were determined by static light and dynamic light scattering (SLS/DLS), and the hydrodynamic radius (Rh) was determined using the Stokes-Einstein equation. The zeta potential (ζ) and polydispersity index (PDI) were also determined. The entrapment encapsulation efficiency of the BZTS nanoparticles was measured by ultraviolet spectrophotometry. In vitro activity of BZTS nanoparticle suspensions against intracellular amastigotes of Leishmania amazonensis and cytotoxic activity were also evaluated. The results showed the production of spherical nanoparticles with varied sizes depending on the hydrophobic portion of the amphiphilic diblock copolymers used. Significant concentration-dependent inhibitory activity against intracellular amastigotes was observed, and low cytotoxic activity was demonstrated against macrophages. PMID:27612813

  18. Synthesis and biological evaluation of some new N4-aryl substituted 5-chloroisatin-3-thiosemicarbazones.

    PubMed

    Pervez, Humayun; Ramzan, Muhammad; Yaqub, Muhammad; Nasim, Faiz-ul-Hassan; Khan, Khalid Mohammed

    2012-05-01

    A new series of sixteen N4-aryl substituted 5-chloroisatin-3-thiosemicarbazones 2a-2p has been synthesized, characterized and tested for selected biological activities i.e. cytotoxicity, phytotoxicity and urease inhibition. In the brine shrimp bioassay, all the synthesized compounds gave LD50 values>2.30x10(-4) M-2.79x10(-4) M and were, therefore, found to be almost inactive, whereas in phytotoxicity assay, regardless of the nature of aryl substituents, they displayed weak to moderate (5-40%) phytotoxic activity at the highest tested concentrations (500 or 1000 μg/mL). In urease inhibition bioassay, compounds 2a, 2c, 2e, 2f, 2k and 2m exhibited relatively a higher degree of urease inhibition with IC50 values ranging from 38.91 μM to 76.65 μM and thus proved to be potent inhibitors of the enzyme. Of these, 2f and 2m displayed pronounced inhibition with IC50 values 38.91 μM and 39.50 μM, respectively, and may act as lead compounds for further studies. Structure-activity relationship (SAR) studies revealed that electronic effects of the substituents about the phenyl ring at N4 of the thiosemicarbazone moiety played an important role in enhancing the urease inhibitory potential of some of the synthesized compounds. PMID:22530899

  19. Cytotoxic gallium complexes containing thiosemicarbazones derived from 9-anthraldehyde: Molecular docking with biomolecules

    NASA Astrophysics Data System (ADS)

    Beckford, Floyd A.; Brock, Alyssa; Gonzalez-Sarrías, Antonio; Seeram, Navindra P.

    2016-10-01

    We have synthesized a trio of gallium complexes bearing 9-anthraldehyde thiosemicarbazones. The complexes were assessed for their anticancer activity and their biophysical reactivity was also investigated. The three complexes displayed good cytotoxic profiles against two human colon cancer cell lines, HCT-116 and Caco-2. The IC50 ranged from 4.7 to 44.1 μM with the complex having an unsubstituted amino group on the thiosemicarbazone being the most active. This particular complex also showed a high therapeutic index. All three complexes bind strongly to DNA via intercalation with binding constants ranging from 7.46 × 104 M-1 to 3.25 × 105 M-1. The strength of the binding cannot be directly related to the level of anticancer activity. The complexes also bind strongly to human serum albumin with binding constants on the order of 104-105 M-1 as well. The complexes act as chemical nucleases as evidenced by their ability to cleave pBR322 plasmid DNA. The binding constants along with the cleavage results may suggest that the extent of DNA interaction is not directly correlated with anticancer activity. The results of docking studies with DNA, ribonucleotide reductase and human serum albumin, however showed that the complex with the best biological activity had the largest binding constant to DNA.

  20. Effect of thiosemicarbazones on corrosion of steel in phosphoric acid produced by wet process

    SciTech Connect

    Khamis, E.; Ameer, M.A.; AlAndis, N.M.; Al-Senani, G.

    2000-02-01

    Corrosion inhibition of steel in phosphoric acid (H{sub 3}PO{sub 4}) by thiosemicarbazide derivatives was studied using different chemical and electrochemical techniques. Protection efficiency up to 99% was obtained with small amounts (10{sup {minus}4} M) of cinnamaldehyde thiosemicarbazone (CTSCN). The order of increasing inhibition efficiency was correlated with the modification of the molecular structure of the inhibitors. Empirical kinetic relationship was obtained describing the experimental data obtained from the different compounds used in this investigation. Potentiodynamic polarization curves indicated that the compounds acted primarily as mixed-type inhibitors. Electrochemical impedance spectroscopy showed that the charge-transfer resistance increased and the capacitance of the double layer decreased with increasing the concentration of the inhibitor in the medium, confirming adsorption process mechanism. At high concentrations (>10{sup 4} M), the capacitance of the double layer leveled off since maximum double-layer thickness was attained. Kinetic-thermodynamic model and Flory-Huggins adsorption isotherm described the experimental findings. Number of active sites, binding constant, and change of free energy were computed for all inhibitors studied. Based on the inhibitor, it was found that each organic molecule replaced one or more adsorbed water molecule from the steel surface. The influence of exposure time on the performance of crotonaldehyde thiosemicarbazone (CrTSCN) was studied. Results showed that the inhibitor performed better with time and at a critical concentration of 5 x 10{sup {minus}4} M.

  1. Lanthanum(III) and praseodymium(III) complexes with isatin thiosemicarbazones

    NASA Astrophysics Data System (ADS)

    Rai, Anita; Sengupta, Soumitra K.; Pandey, Om P.

    2005-09-01

    Ten new lanthanum(III) and praseodymium(III) complexes of the general formula Na[La(L) 2H 2O] (Ln = La(III) or Pr(III); LH 2 = thiosemicarbazones) derived from the condensation of isatin with 4-phenyl thiosemicarbazide, 4-(4-chlorophenyl) thiosemicarbazide, 4-(2-nitrophenyl) thiosemicarbazide, 4-(2-bromophenyl) thiosemicarbazide and 4-(2-methylphenyl) thiosemicarbazide, have been synthesized in methanol in presence of sodium hydroxide. The XRD spectra of the complexes were monitored to verify complex formation. The complexes have also been characterized by elemental analysis, molar conductance, electronic absorption and fluorescence, infrared, far infrared, 1H and 13C NMR spectral studies. Thermal studies of these complexes have been carried out in the temperature range 25-800 °C using TG, DTG and DTA techniques. All these complexes decompose gradually with the formation of Ln 2O 3 as the end product. The Judd-ofelt intensity parameter, oscillator strength, transition probability, stimulated emission cross section for different transitions of Pr 3+ for 4-phenyl thiosemicarbazones have been calculated.

  2. Spectral characterization of iron(III) complexes of 2-benzoylpyridine N(4)-substituted thiosemicarbazones

    NASA Astrophysics Data System (ADS)

    Joseph, Marthakutty; Sreekanth, Anandaram; Suni, V.; Kurup, M. R. Prathapachandra

    2006-06-01

    Three iron(III) complexes (1-3) of 2-benzoylpyridine N(4)-phenyl thiosemicarbazone (HL 1) and one iron(III) complex (4) of 2-benzoylpyridine N(4)-cyclohexyl thiosemicarbazone (HL 2) were synthesized and characterized by means of different physicochemical techniques viz., molar conductivity measurements, magnetic susceptibility studies and electronic, infrared and EPR spectral studies. The analytical data and the molar conductance measurements of the complexes reveal that two molecules of the ligand and the anion are coordinated to the metal atom in all the four complexes. The magnetic moments of the complexes suggest that they are of low spin. From the infrared spectra of the ligands and the complexes it is confirmed that the ligands coordinate to iron(III) as an anion coordinating via the azomethine nitrogen, pyridyl nitrogen, and the thiolate sulphur. The EPR spectra of the complexes in the polycrystalline state at 298 and 110 K and in DMF solution at 110 K were recorded and all the spectra show three g values indicating that these complexes have rhombic distortion. All the iron(III) complexes in DMF solution at 110 K have similar anisotropic spectra with almost the same gav values, indicating that the bonding in all the complexes is similar and is unaffected by the coordination of the anion.

  3. Vanadium(IV/V) complexes of Triapine and related thiosemicarbazones: Synthesis, solution equilibrium and bioactivity.

    PubMed

    Kowol, Christian R; Nagy, Nóra V; Jakusch, Tamás; Roller, Alexander; Heffeter, Petra; Keppler, Bernhard K; Enyedy, Éva A

    2015-11-01

    The stoichiometry and thermodynamic stability of vanadium(IV/V) complexes of Triapine and two related α(N)-heterocyclic thiosemicarbazones (TSCs) with potential antitumor activity have been determined by pH-potentiometry, EPR and (51)V NMR spectroscopy in 30% (w/w) dimethyl sulfoxide/water solvent mixtures. In all cases, mono-ligand complexes in different protonation states were identified. Dimethylation of the terminal amino group resulted in the formation of vanadium(IV/V) complexes with considerably higher stability. Three of the most stable complexes were also synthesized in solid state and comprehensively characterized. The biological evaluation of the synthesized vanadium complexes in comparison to the metal-free ligands in different human cancer cell lines revealed only minimal influence of the metal ion. Thus, in addition the coordination ability of salicylaldehyde thiosemicarbazone (STSC) to vanadium(IV/V) ions was investigated. The exchange of the pyridine nitrogen of the α(N)-heterocyclic TSCs to a phenolate oxygen in STSC significantly increased the stability of the complexes in solution. Finally, this also resulted in increased cytotoxicity activity of a vanadium(V) complex of STSC compared to the metal-free ligand. PMID:26349014

  4. Vanadium Complexes with Hydrazone or Thiosemicarbazone Ligands as Potential Anti-Mycobacterium tuberculosis Agents.

    PubMed

    de Souza, Paula C; Maia, Pedro I S; de Barros, Heloisa B; Leite, Clarice Q F; Deflon, Victor M; Pavan, Fernando R

    2015-01-01

    Tuberculosis (TB) is an infectious disease caused mainly by Mycobacterium tuberculosis (MTB) and still an important public health problem worldwide. Some factors like the emergence of multidrug resistant (MDR) and extensively drug-resistant (XDR) strains make urgent the research of new active compounds. Searching for new inorganic compounds against TB, three new dioxovanadium(V) complexes were obtained upon reaction of [VO(acac)2] with hydrazone and thiosemicarbazone ligands derived from di-2-pyridyl ketone. Spectroscopic studies and X-ray crystallography revealed asymmetrically oxo bridged binuclear complexes of the type [{VO(L(1,2))}2(μ-O)2], involving the hydrazone ligands, while a mononuclear square pyramidal complex of the type [VO2(L(3))] was formed with the thiosemicarbazone ligand. The compounds were tested against M. tuberculosis and three of them, with MICs values between 2.00 and 3.76 μM were considered promising for TB treatment. Such MIC values are comparable or better than those found for some drugs currently used in TB treatment. PMID:24433444

  5. Generation of Nonlinear Vortex Precursors.

    PubMed

    Chen, Yue-Yue; Feng, Xun-Li; Liu, Chengpu

    2016-07-01

    We numerically study the propagation of a few-cycle pulse carrying orbital angular momentum (OAM) through a dense atomic system. Nonlinear precursors consisting of high-order vortex harmonics are generated in the transmitted field due to carrier effects associated with ultrafast Bloch oscillation. The nonlinear precursors survive to propagation effects and are well separated with the main pulse, which provides a straightforward way to measure precursors. By virtue of carrying high-order OAM, the obtained vortex precursors as information carriers have potential applications in optical information and communication fields where controllable loss, large information-carrying capacity, and high speed communication are required. PMID:27447507

  6. Generation of Nonlinear Vortex Precursors

    NASA Astrophysics Data System (ADS)

    Chen, Yue-Yue; Feng, Xun-Li; Liu, Chengpu

    2016-07-01

    We numerically study the propagation of a few-cycle pulse carrying orbital angular momentum (OAM) through a dense atomic system. Nonlinear precursors consisting of high-order vortex harmonics are generated in the transmitted field due to carrier effects associated with ultrafast Bloch oscillation. The nonlinear precursors survive to propagation effects and are well separated with the main pulse, which provides a straightforward way to measure precursors. By virtue of carrying high-order OAM, the obtained vortex precursors as information carriers have potential applications in optical information and communication fields where controllable loss, large information-carrying capacity, and high speed communication are required.

  7. Seebeck and figure of merit enhancement in nanostructured antimony telluride by antisite defect suppression through sulfur doping.

    PubMed

    Mehta, Rutvik J; Zhang, Yanliang; Zhu, Hong; Parker, David S; Belley, Matthew; Singh, David J; Ramprasad, Ramamurthy; Borca-Tasciuc, Theodorian; Ramanath, Ganpati

    2012-09-12

    Antimony telluride has a low thermoelectric figure of merit (ZT < ∼0.3) because of a low Seebeck coefficient α arising from high degenerate hole concentrations generated by antimony antisite defects. Here, we mitigate this key problem by suppressing antisite defect formation using subatomic percent sulfur doping. The resultant 10-25% higher α in bulk nanocrystalline antimony telluride leads to ZT ∼ 0.95 at 423 K, which is superior to the best non-nanostructured antimony telluride alloys. Density functional theory calculations indicate that sulfur increases the antisite formation activation energy and presage further improvements leading to ZT ∼ 2 through optimized doping. Our findings are promising for designing novel thermoelectric materials for refrigeration, waste heat recovery, and solar thermal applications. PMID:22891784

  8. Speciation analysis of inorganic antimony in sediment samples from São Paulo Estuary, Bahia State, Brazil.

    PubMed

    Silva, Mario Marques; Leao, Danilo Junqueira; Moreira, Ícaro Thiago Andrade; de Oliveira, Olívia Maria Cordeiro; de Souza Queiroz, Antônio Fernando; Ferreira, Sergio Luis Costa

    2015-06-01

    This paper proposes an extraction procedure for the speciation analysis of inorganic antimony in sediment samples using slurry sampling and hydride generation atomic absorption spectrometry. The optimization step of extraction of the species was performed employing a full two-level factorial design (2(3)) and a Box-Behnken matrix where the studied factors in both experiments were: extraction temperature, ultrasonic radiation time, and hydrochloric acid concentration. Using the optimized conditions, antimony species can be extracted in closed system using a 6.0 M hydrochloric acid solution at temperature of 70 °C and an ultrasonic radiation time of 20 min. The determination of antimony is performed in presence of 2.0 M hydrochloric acid solution using HG AAS by external calibration technique with limits of detection and quantification of 5.6 and 19.0 ng L(-1) and a precision expressed as relative standard deviation of 5.6 % for an antimony solution with concentration of 6.0 μg L(-1). The accuracy of the method was confirmed by analysis of two certified reference materials of sediments. For a sample mass of sediment of 0.20 g, the limits of detection and quantification obtained were 0.70 and 2.34 ng g(-1), respectively. During speciation analysis, antimony(III) is determined in presence of citrate, while total antimony is quantified after reduction of antimony(V) to antimony(III) using potassium iodide and ascorbic acid. The method was applied for analysis of six sediment samples collected in São Paulo Estuary (Bahia State, Brazil). The antimony contents obtained varied from 45.3 to 89.1 ng g(-1) for total antimony and of 17.7 to 31.4 ng g(-1) for antimony(III). These values are agreeing with other data reported by the literature for this element in uncontaminated sediment samples. PMID:25537284

  9. Electrodeposition of SnSbCu Alloy on Copper from an Electrolyte with Varied Content of Antimony Chloride

    NASA Astrophysics Data System (ADS)

    Valeeva, A. Kh.; Valeev, I. Sh.

    2015-10-01

    The microstructure and chemical composition of electrodeposited alloys of the SnSbCu system with varied concentration of antimony chloride in the electrolyte have been investigated. It is shown that during electrodeposition mechanical-mixture alloys are not formed, but rather intermetallic compounds. It is found that increasing the concentration of antimony chloride in the electrolyte leads to a decrease in the tin content and cracking of the coating.

  10. An interstellar precursor mission

    NASA Technical Reports Server (NTRS)

    Jaffe, L. D.; Ivie, C.; Lewis, J. C.; Lipes, R.; Norton, H. N.; Stearns, J. W.; Stimpson, L. D.; Weissman, P.

    1980-01-01

    A mission out of the planetary system, launched about the year 2000, could provide valuable scientific data as well as test some of the technology for a later mission to another star. Primary scientific objectives for the precursor mission concern characteristics of the heliopause, the interstellar medium, stellar distances (by parallax measurements), low-energy cosmic rays, interplanetary gas distribution, and the mass of the solar system. Secondary objectives include investigation of Pluto. The mission should extend to 400-1000 AU from the sun. A heliocentric hyperbolic escape velocity of 50-100 km/sec or more is needed to attain this distance within a reasonable mission duration (20-50 years). The trajectory should be toward the incoming interstellar gas. For a year 2000 launch, a Pluto encounter and orbiter can be included. A second mission targeted parallel to the solar axis would also be worthwhile. The mission duration is 20 years, with an extended mission to a total of 50 years. A system using one or two stages of nuclear electric propulsion (NEP) was selected as a possible baseline. The most promising alternatives are ultralight solar sails or laser sailing, with the lasers in earth orbit, for example. The NEP baseline design allows the option of carrying a Pluto orbiter as a daughter spacecraft.

  11. Synthesis, characterization, and preliminary in vitro studies of vanadium(IV) complexes with a Schiff base and thiosemicarbazones as mixed-ligands

    PubMed Central

    Lewis, Nerissa A.; Liu, Fange; Seymour, Luke; Magnusen, Anthony; Erves, Travis R.; Arca, Jessa Faye; Beckford, Floyd A.; Venkatraman, Ramaiyer; González-Sarrías, Antonio; Fronczek, Frank R.; VanDerveer, Don G.; Seeram, Navindra P.; Liu, Aimin; Jarrett, William L.; Holder, Alvin A.

    2013-01-01

    [VO(Sal-L-tryp)(H2O)] 1 (where sal-L-tryp = N-salicylidene-L-tryptophanate) was used as a precursor to produce the novel complexes, [VO(Sal-L-tryp)(MeATSC)].1.5C2H5OH 2 (where MeATSC = 9-Anthraldehyde-N(4)-methylthiosemicarbazone), [VO(Sal-L-tryp)(N-Ethhymethohcarbthio)].H2O 3 (where N-Ethhymethohcarbthio = (E)-N-ethyl-2-(4-hydroxy-3-methoxybenzylidene)hydrazinecarbothioamide), and [VO(Sal-L-tryp)(acetylethTSC)].C2H5OH 4 (where acetylethTSC = (E)-N-ethyl-2-(1-(thiazol-2-yl)ethylidene)hydrazinecarbothioamide), by reaction with the respective thiosemicarbazone. The chemical and structural properties of these ligands and complexes were characterised by elemental analysis, ESI MS, FT-IR, UV-visible, ESR, 1H and 13C NMR spectroscopy, and X-ray crystallography. DMSO and DMSO-d6 solutions of compounds 1-4 were oxidised in air to produce vanadium(V) species which were verified by ESI MS and 51V NMR spectroscopy. Anti-cancer properties of compounds 2-4 were examined with three colon cancer cell lines, HTC-116, Caco-2, and HT-29, and also with non-cancerous colonic myofibroblasts, CCD18-Co. Compounds 2-3 exhibited less inhibitory effects in the CCD-18Co cells, indicating a possible cytotoxic selectivity towards colon cancer cells. In general, those compounds which exhibited anti-proliferative activity on cancer cells, but did not affect non-cancerous cells, may have a potential in chemotherapy. PMID:23904789

  12. Synthesis, characterization, and preliminary in vitro studies of vanadium(IV) complexes with a Schiff base and thiosemicarbazones as mixed-ligands.

    PubMed

    Lewis, Nerissa A; Liu, Fange; Seymour, Luke; Magnusen, Anthony; Erves, Travis R; Arca, Jessa Faye; Beckford, Floyd A; Venkatraman, Ramaiyer; González-Sarrías, Antonio; Fronczek, Frank R; Vanderveer, Don G; Seeram, Navindra P; Liu, Aimin; Jarrett, William L; Holder, Alvin A

    2012-02-01

    [VO(Sal-L-tryp)(H2O)] 1 (where sal-L-tryp = N-salicylidene-L-tryptophanate) was used as a precursor to produce the novel complexes, [VO(Sal-L-tryp)(MeATSC)].1.5C2H5OH 2 (where MeATSC = 9-Anthraldehyde-N(4)-methylthiosemicarbazone), [VO(Sal-L-tryp)(N-Ethhymethohcarbthio)].H2O 3 (where N-Ethhymethohcarbthio = (E)-N-ethyl-2-(4-hydroxy-3-methoxybenzylidene)hydrazinecarbothioamide), and [VO(Sal-L-tryp)(acetylethTSC)].C2H5OH 4 (where acetylethTSC = (E)-N-ethyl-2-(1-(thiazol-2-yl)ethylidene)hydrazinecarbothioamide), by reaction with the respective thiosemicarbazone. The chemical and structural properties of these ligands and complexes were characterised by elemental analysis, ESI MS, FT-IR, UV-visible, ESR, (1)H and (13)C NMR spectroscopy, and X-ray crystallography. DMSO and DMSO-d6 solutions of compounds 1-4 were oxidised in air to produce vanadium(V) species which were verified by ESI MS and (51)V NMR spectroscopy. Anti-cancer properties of compounds 2-4 were examined with three colon cancer cell lines, HTC-116, Caco-2, and HT-29, and also with non-cancerous colonic myofibroblasts, CCD18-Co. Compounds 2-3 exhibited less inhibitory effects in the CCD-18Co cells, indicating a possible cytotoxic selectivity towards colon cancer cells. In general, those compounds which exhibited anti-proliferative activity on cancer cells, but did not affect non-cancerous cells, may have a potential in chemotherapy. PMID:23904789

  13. Intrachromosomal Amplification, Locus Deletion and Point Mutation in the Aquaglyceroporin AQP1 Gene in Antimony Resistant Leishmania (Viannia) guyanensis

    PubMed Central

    Monte-Neto, Rubens; Laffitte, Marie-Claude N.; Leprohon, Philippe; Reis, Priscila; Frézard, Frédéric; Ouellette, Marc

    2015-01-01

    Background Antimony resistance complicates the treatment of infections caused by the parasite Leishmania. Methodology/Principal Findings Using next generation sequencing, we sequenced the genome of four independent Leishmania guyanensis antimony-resistant (SbR) mutants and found different chromosomal alterations including aneuploidy, intrachromosomal gene amplification and gene deletion. A segment covering 30 genes on chromosome 19 was amplified intrachromosomally in three of the four mutants. The gene coding for the multidrug resistance associated protein A involved in antimony resistance was also amplified in the four mutants, most likely through chromosomal translocation. All mutants also displayed a reduced accumulation of antimony mainly due to genomic alterations at the level of the subtelomeric region of chromosome 31 harboring the gene coding for the aquaglyceroporin 1 (LgAQP1). Resistance involved the loss of LgAQP1 through subtelomeric deletions in three mutants. Interestingly, the fourth mutant harbored a single G133D point mutation in LgAQP1 whose role in resistance was functionality confirmed through drug sensitivity and antimony accumulation assays. In contrast to the Leishmania subspecies that resort to extrachromosomal amplification, the Viannia strains studied here used intrachromosomal amplification and locus deletion. Conclusions/Significance This is the first report of a naturally occurred point mutation in AQP1 in antimony resistant parasites. PMID:25679388

  14. 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

  15. Treatment of antimony mine drainage: challenges and opportunities with special emphasis on mineral adsorption and sulfate reducing bacteria.

    PubMed

    Li, Yongchao; Hu, Xiaoxian; Ren, Bozhi

    2016-01-01

    The present article summarizes antimony mine distribution, antimony mine drainage generation and environmental impacts, and critically analyses the remediation approach with special emphasis on iron oxidizing bacteria and sulfate reducing bacteria. Most recent research focuses on readily available low-cost adsorbents, such as minerals, wastes, and biosorbents. It is found that iron oxides prepared by chemical methods present superior adsorption ability for Sb(III) and Sb(V). However, this process is more costly and iron oxide activity can be inhibited by plenty of sulfate in antimony mine drainage. In the presence of sulfate reducing bacteria, sulfate can be reduced to sulfide and form Sb(2)S(3) precipitates. However, dissolved oxygen and lack of nutrient source in antimony mine drainage inhibit sulfate reducing bacteria activity. Biogenetic iron oxide minerals from iron corrosion by iron-oxidizing bacteria may prove promising for antimony adsorption, while the micro-environment generated from iron corrosion by iron oxidizing bacteria may provide better growth conditions for symbiotic sulfate reducing bacteria. Finally, based on biogenetic iron oxide adsorption and sulfate reducing bacteria followed by precipitation, the paper suggests an alternative treatment for antimony mine drainage that deserves exploration. PMID:27148704

  16. Antimony leaching in plastics from waste electrical and electronic equipment (WEEE) with various acids and gamma irradiation.

    PubMed

    Tostar, Sandra; Stenvall, Erik; Boldizar, Antal; Foreman, Mark R St J

    2013-06-01

    There has been a recent interest in antimony since the availability in readily mined areas is decreasing compared to the amounts used. It is important in many applications such as flame retardants and in the production of polyester, which can trigger an investigation of the leachability of antimony from plastics using different acids. In this paper, different types of acids are tested for their ability to leach antimony from a discarded computer housing, made of poly(acrylonitrile butadiene styrene), which is a common plastic type used in electrical and electronic equipment. The acid solutions included sodium hydrogen tartrate (0.5M) dissolved in either dimethyl sulfoxide or water (at ca. 23°C and heated to ca. 105°C). The metal content after leaching was determined by inductively coupled plasma optical emission spectroscopy. The most efficient leaching medium was the heated solution of sodium hydrogen tartrate in dimethyl sulfoxide, which leached almost half of the antimony from the poly(acrylonitrile butadiene styrene). Gamma irradiation, which is proposed to improve the mechanical properties in plastics, was used here to investigate the influence of antimony leaching ability. No significant change in the amount of leached antimony could be observed. PMID:23561798

  17. Diphenyllead(IV) chloride complexes with benzilthiosemicarbazones. The first bis(thiosemicarbazone) derivatives.

    PubMed

    Calatayud, David G; López-Torres, Elena; Mendiola, M Antonia

    2007-11-26

    Reactions of diphenyllead(IV) chloride with benzil bis(thiosemicarbazone) (L1H6) and benzil bis(4-methyl-3-thiosemicarbazone) (L1Me2H4) afforded the first complexes containing the diphenyllead(IV) moiety with bis(thiosemicarbazone) ligands. The new complexes show diverse structural characteristics depending on the ligand and the working conditions. Complexes [PbPh2Cl(L1H5)].3H2O (1) and [PbPh2Cl(L1Me2H3)] (3) are mononuclear species in which the ligands are partially deprotonated and the lead atom has a C2N2S2Cl environment in a distorted pentagonal bipyramid coordination geometry. Complex [PbPh(L1Me2H2)](2).2H2O (4) was also obtained, which contains two lead atoms in a binuclear structure with a C2N2S3 coordination sphere for each lead atom, since both dideprotonated ligands act as N2S2 chelate and as sulfur bridge. Reaction from L1H6, in the same conditions in which complex 4 was prepared, gave a mixture of products: the lead (II) complex [Pb(L1H4)]2 (2) and [PbPh3Cl]n. Reactions with the cyclic molecules 5-methoxy-5,6-diphenyl-4,5-dihydro-2H-[1,2,4]-triazine-3-thione (L2H2OCH3) and 5-methoxy-4-methyl-5,6-diphenyl-4,5-dihydro-2H-[1,2,4]-triazine-3-thione (L2MeHOCH3) were also explored. In all the complexes, the ligands are deprotonated. The complexes [PbPh2(L2)2] (5) and [PbPh2(L2MeOCH3)2] (7) present the same characteristics. The X-ray structure of 5 shows a distorted octahedral geometry around the lead atom, with the ligand molecules acting as NS chelates, but the nitrogen bonded to the metal is different; one of the triazines shows a novel behavior, since the nitrogen atom of the new imine group formed is the one that is bonded to the lead center, being a good example of linkage isomerism. The complex [PbPh2Cl(L2)] (6), which was also isolated, could not be crystallized. All the complexes were characterized by elemental analysis, mass spectrometry, IR and 1H, 13C, and 207Pb NMR spectroscopy and some of them by X-ray diffraction studies. PMID:17939655

  18. Electric quadrupole interaction of 100Rh in antimony, hafnium and rhenium

    NASA Astrophysics Data System (ADS)

    Kemp, W. J.; Abiona, A. A.; Kessler, P.; Timmers, H.

    2013-05-01

    Time differential perturbed angular correlation (TDPAC) spectroscopy in beryllium, zinc, rhodium, antimony, hafnium and rhenium was performed with the 100Pd/100Rh probe using four-detector arrays with relative detector orientations of 90° and 180°. The probe was synthesized using the 92Zr(12C,4n)100Pd fusion evaporation reaction, with evaporation residues recoiling into specimens of the metals. The quadrupole coupling constant for 100Rh has been determined for the first time for antimony, hafnium and rhenium, while results for the other elements agree with known values. The coupling constants for the measured hexagonal lattices of the period VI transition metals, hafnium and rhenium, show the same trend with increasing atomic number as those of period V.

  19. Numerical simulation and experimental characterization of the performance evolution of a liquid antimony anode fuel cell

    NASA Astrophysics Data System (ADS)

    Cao, Tianyu; Shi, Yixiang; Wang, Hongjian; Cai, Ningsheng

    2015-06-01

    A solid oxide fuel cell (SOFC) with a liquid antimony anode is fabricated based on a smooth single crystal YSZ electrolyte substrate and a porous Pt cathode. The performance of the liquid antimony anode was tested under "battery mode", with the anode chamber shielded in argon throughout the test and the cathode exposed to air. Polarization curves were taken and a long term constant potential discharging test was carried out afterwards. Taking electrochemical reaction, mass transport and microstructure of the liquid Sb anode into consideration, a one dimensional mathematical model was built and then validated by the polarization curve and the constant potential discharging performance curve obtained during the test. This model analyzes the metallic Sb distribution in the anode during cell operation, explains the cell performance evolution base on the microstructural development of the liquid Sb anode and simulates how the anode microstructure affects the cell performance.

  20. Hot Wall Epitaxy And Characterization Of Bismuth And Antimony Thin Films On Barium Fluoride Substrates

    NASA Astrophysics Data System (ADS)

    Collazo, Ramon; Dalmau, Rafael; Martinez, Antonio

    1998-03-01

    We have grown thin films of bismuth and antimony using hot wall epitaxy. The epitaxial films were grown on (111)-BaF2 substrates. The chemical integrity of the films was established using Auger electron spectroscopy and X ray Photoelectron Spectroscopy. The thickness of the films was measured using an atomic force microscope to establish their growth rate. The crystallographic properties of the films were assessed using x-ray diffraction techniques. Both bismuth and antimony thin films were found to be oriented with the [003] direction perpendicular to the plane of the films. Pole figures of both types of films indicate the epitaxial nature of the films. Bi/Sb multilayer structures were grown using the same growth technique. We will report on the results of the characterization of these films as well as on the growth apparatus and process. Work supported in part by EPSCoR-NSF Grant EHR-9108775 and NCRADA-NSWCDD-92-01.

  1. Reaction of Antimony-Uranium Composite Oxide in the Chlorination Treatment of Waste Catalyst - 13521

    SciTech Connect

    Sawada, Kayo; Hirabayashi, Daisuke; Enokida, Youichi

    2013-07-01

    The effect of oxygen gas concentration on the chlorination treatment of antimony-uranium composite oxide catalyst waste was investigated by adding different concentrations of oxygen at 0-6 vol% to its chlorination agent of 0.6 or 6 vol% hydrogen chloride gas at 1173 K. The addition of oxygen tended to prevent the chlorination of antimony in the oxide. When 6 vol% hydrogen chloride gas was used, the addition of oxygen up to 0.1 vol% could convert the uranium contained in the catalyst to U{sub 3}O{sub 8} without any significant decrease in the reaction rate compared to that of the treatment without oxygen. (authors)

  2. Antimony/Graphitic Carbon Composite Anode for High-Performance Sodium-Ion Batteries.

    PubMed

    Zhao, Xin; Vail, Sean A; Lu, Yuhao; Song, Jie; Pan, Wei; Evans, David R; Lee, Jong-Jan

    2016-06-01

    Although the room-temperature rechargeable sodium-ion battery has emerged as an attractive alternative energy storage solution for large-scale deployment, major challenges toward practical sodium-ion battery technology remain including identification and engineering of anode materials that are both technologically feasible and economical. Herein, an antimony-based anode is developed by incorporating antimony into graphitic carbon matrices using low-cost materials and scalable processes. The composite anode exhibits excellent overall performance in terms of packing density, fast charge/discharge capability and cyclability, which is enabled by the conductive and compact graphitic network. A full cell design featuring this composite anode with a hexacyanometallate cathode achieves superior power output and low polarization, which offers the potential for realizing a high-performance, cost-effective sodium-ion battery. PMID:27172376

  3. Antimony segregation in stressed SiGe heterostructures grown by molecular beam epitaxy

    SciTech Connect

    Drozdov, M. N.; Novikov, A. V.; Yurasov, D. V.

    2013-11-15

    The effects of the growth temperature, composition, and elastic strains in separate layers on the segregation of antimony are studied experimentally for stressed SiGe structures grown by molecular beam epitaxy. It is established that the growth conditions and parameters of the structures exert an interrelated influence on the segregation of Sb: the degree of the influence of the composition and elastic stresses in the SiGe layers on Sb segregation depends on the growth temperature. It is shown that usage of a method previously proposed by us for the selective doping of silicon structures with consideration for the obtained dependences of Sb segregation on the growth conditions and parameters of the SiGe layers makes it possible to form SiGe structures selectively doped with antimony.

  4. Preparation and Characterization of Antimony and Arsenic Tricyanide and Their 2,2'-Bipyridine Adducts.

    PubMed

    Deokar, Piyush; Leitz, Dominik; Stein, Trent H; Vasiliu, Monica; Dixon, David A; Christe, Karl O; Haiges, Ralf

    2016-09-01

    The arsenic(III) and antimony(III) cyanides M(CN)3 (M=As, Sb) have been prepared in quantitative yields from the corresponding trifluorides through fluoride-cyanide exchange with Me3 SiCN in acetonitrile. When the reaction was carried out in the presence of one equivalent of 2,2'-bipyridine, the adducts [M(CN)3 ⋅(2,2'-bipy)] were obtained. The crystal structures of As(CN)3 , [As(CN)3 ⋅(2,2'-bipy)] and [Sb(CN)3 ⋅(2,2'-bipy)] were determined and are surprisingly different. As(CN)3 possesses a polymeric three-dimensional structure, [As(CN)3 ⋅(2,2'-bipy)] exhibits a two-dimensional sheet structure, and [Sb(CN)3 ⋅(2,2'-bipy)] has a chain structure, and none of the structures resembles those found for the corresponding arsenic and antimony triazides. PMID:27492940

  5. Preparation and spectroscopic studies of antimony(III) and bismuth(III) halodithiocarbamate derivatives

    NASA Astrophysics Data System (ADS)

    Giusti, Aleardo; Preti, Carlo; Tosi, Giuseppe; Zannini, Paolo

    1983-04-01

    The complexes of antimony(III) and bismuth(III) with piperidine (Pipdtc), morpholine (Morphdtc) and thiomorpholinedithiocarbamate (Timdtc) of general formula Sb 2-(Rdtc) 3X 3 and M(Rdtc)X 2 (M is antimony or bismuth, X a halogen and Rdtc the dithiocarbamates) have been prepared and characterized by spectroscopic methods. The IR spectra suggest that the dithiocarbamate group coordinates as a bidentate ligand; the metal-sulphur and metal-halide stretching modes have also been assigned. The spectral data are discussed and compared with those of the corresponding trisdithiocarbamate and monohalobisdithiocarbamate derivatives. The molecular weight determinations indicate that all these dithiocarbamate complexes are dimeric. Tentative stereochemistries are proposed and discussed on the basis of the results obtained.

  6. Iron Chelators of the Di-2-pyridylketone Thiosemicarbazone and 2-Benzoylpyridine Thiosemicarbazone Series Inhibit HIV-1 Transcription: Identification of Novel Cellular Targets—Iron, Cyclin-Dependent Kinase (CDK) 2, and CDK9S⃞

    PubMed Central

    Debebe, Zufan; Ammosova, Tatyana; Breuer, Denitra; Lovejoy, David B.; Kalinowski, Danuta S.; Karla, Pradeep K.; Kumar, Krishna; Jerebtsova, Marina; Ray, Patricio; Kashanchi, Fatah; Gordeuk, Victor R.; Richardson, Des R.

    2011-01-01

    HIV-1 transcription is activated by HIV-1 Tat protein, which recruits cyclin-dependent kinase 9 (CDK9)/cyclin T1 and other host transcriptional coactivators to the HIV-1 promoter. Tat itself is phosphorylated by CDK2, and inhibition of CDK2 by small interfering RNA, the iron chelator 2-hydroxy-1-naphthylaldehyde isonicotinoyl hydrazone (311), and the iron chelator deferasirox (ICL670) inhibits HIV-1 transcription. Here we have analyzed a group of novel di-2-pyridylketone thiosemicarbazone- and 2-benzoylpyridine thiosemicarbazone-based iron chelators that exhibit marked anticancer activity in vitro and in vivo (Proc Natl Acad Sci USA 103:7670–7675, 2006; J Med Chem 50:3716–3729, 2007). Several of these iron chelators, in particular 2-benzoylpyridine 4-allyl-3-thiosemicarbazone (Bp4aT) and 2-benzoylpyridine 4-ethyl-3-thiosemicarbazone (Bp4eT), inhibited HIV-1 transcription and replication at much lower concentrations than did 311 and ICL670. Neither Bp4aT nor Bp4eT were toxic after a 24-h incubation. However, longer incubations for 48 h or 72 h resulted in cytotoxicity. Analysis of the molecular mechanism of HIV-1 inhibition showed that the novel iron chelators inhibited basal HIV-1 transcription, but not the nuclear factor-κB-dependent transcription or transcription from an HIV-1 promoter with inactivated SP1 sites. The chelators inhibited the activities of CDK2 and CDK9/cyclin T1, suggesting that inhibition of CDK9 may contribute to the inhibition of HIV-1 transcription. Our study suggests the potential usefulness of Bp4aT or Bp4eT in antiretroviral regimens, particularly where resistance to standard treatment occurs. PMID:20956357

  7. Iron chelators of the di-2-pyridylketone thiosemicarbazone and 2-benzoylpyridine thiosemicarbazone series inhibit HIV-1 transcription: identification of novel cellular targets--iron, cyclin-dependent kinase (CDK) 2, and CDK9.

    PubMed

    Debebe, Zufan; Ammosova, Tatyana; Breuer, Denitra; Lovejoy, David B; Kalinowski, Danuta S; Kumar, Krishna; Jerebtsova, Marina; Ray, Patricio; Kashanchi, Fatah; Gordeuk, Victor R; Richardson, Des R; Nekhai, Sergei

    2011-01-01

    HIV-1 transcription is activated by HIV-1 Tat protein, which recruits cyclin-dependent kinase 9 (CDK9)/cyclin T1 and other host transcriptional coactivators to the HIV-1 promoter. Tat itself is phosphorylated by CDK2, and inhibition of CDK2 by small interfering RNA, the iron chelator 2-hydroxy-1-naphthylaldehyde isonicotinoyl hydrazone (311), and the iron chelator deferasirox (ICL670) inhibits HIV-1 transcription. Here we have analyzed a group of novel di-2-pyridylketone thiosemicarbazone- and 2-benzoylpyridine thiosemicarbazone-based iron chelators that exhibit marked anticancer activity in vitro and in vivo (Proc Natl Acad Sci USA 103:7670-7675, 2006; J Med Chem 50:3716-3729, 2007). Several of these iron chelators, in particular 2-benzoylpyridine 4-allyl-3-thiosemicarbazone (Bp4aT) and 2-benzoylpyridine 4-ethyl-3-thiosemicarbazone (Bp4eT), inhibited HIV-1 transcription and replication at much lower concentrations than did 311 and ICL670. Neither Bp4aT nor Bp4eT were toxic after a 24-h incubation. However, longer incubations for 48 h or 72 h resulted in cytotoxicity. Analysis of the molecular mechanism of HIV-1 inhibition showed that the novel iron chelators inhibited basal HIV-1 transcription, but not the nuclear factor-κB-dependent transcription or transcription from an HIV-1 promoter with inactivated SP1 sites. The chelators inhibited the activities of CDK2 and CDK9/cyclin T1, suggesting that inhibition of CDK9 may contribute to the inhibition of HIV-1 transcription. Our study suggests the potential usefulness of Bp4aT or Bp4eT in antiretroviral regimens, particularly where resistance to standard treatment occurs. PMID:20956357

  8. Genotoxic risk and oxidative DNA damage in workers exposed to antimony trioxide.

    PubMed

    Cavallo, Delia; Iavicoli, Ivo; Setini, Andrea; Marinaccio, Alessandro; Perniconi, Barbara; Carelli, Giovanni; Iavicoli, Sergio

    2002-01-01

    The growing use of antimony (Sb) compounds in industry and the consequent increase in the number of exposed workers make it important to carry out a health risk assessment. The main goal of this study was to assess the genotoxicity of Sb(2)O(3) in occupationally exposed workers. Genotoxicity was evaluated by the sister chromatid exchange (SCE) and micronucleus tests, and the enzyme (Fpg)-modified comet assay. In addition, antimony exposure levels were established by environmental monitoring with personal air samplers. We studied 23 male workers assigned to different fire retardant treatment tasks in the car upholstery industry and a control group of 23 healthy nonexposed males. The exposed workers were divided into two groups on the basis of their tasks and the work cycle: Group A comprised finishing and intermediate inspection operators who directly handled a mixture containing Sb(2)O(3); Group B were jet operators, not directly exposed to the compound. Environmental monitoring detected low Sb exposure levels but significant differences between the two groups, with Group A having the higher exposure level. Cytogenetic analyses showed no difference between exposed workers and controls for micronuclei and SCE. The enzyme-modified comet assay showed a probable relation between moderate levels of oxidative DNA damage and exposure to antimony, with a significantly higher proportion of workers in Group A having oxidative DNA damage compared to controls. The results support the theory that oxidative DNA damage is involved in the genotoxicity of antimony and indicate the need for further research in this field. PMID:12355552

  9. Adsorption of antimony onto iron oxyhydroxides: adsorption behavior and surface structure.

    PubMed

    Guo, Xuejun; Wu, Zhijun; He, Mengchang; Meng, Xiaoguang; Jin, Xin; Qiu, Nan; Zhang, Jing

    2014-07-15

    Antimony is detected in soil and water with elevated concentration due to a variety of industrial applications and mining activities. Though antimony is classified as a pollutant of priority interest by the United States Environmental Protection Agency (USEPA) and Europe Union (EU), very little is known about its environmental behavior and adsorption mechanism. In this study, the adsorption behaviors and surface structure of antimony (III/V) on iron oxides were investigated using batch adsorption techniques, surface complexation modeling (SCM), X-ray photon spectroscopy (XPS) and extended X-ray absorption fine structure spectroscopy (EXAFS). The adsorption isotherms and edges indicated that the affinity of Sb(V) and Sb(III) toward the iron oxides depended on the Sb species, solution pH, and the characteristics of iron oxides. Sb(V) adsorption was favored at acidic pH and decreased dramatically with increasing pH, while Sb(III) adsorption was constant over a broad pH range. When pH is higher than 7, Sb(III) adsorption by goethite and hydrous ferric oxide (HFO) was greater than Sb(V). EXAFS analysis indicated that the majority of Sb(III), either adsorbed onto HFO or co-precipitated by FeCl3, was oxidized into Sb(V) probably due to the involvement of O2 in the long duration of sample preservation. Only one Sb-Fe subshell was filtered in the EXAFS spectra of antimony adsorption onto HFO, with the coordination number of 1.0-1.9 attributed to bidentate mononuclear edge-sharing ((2)E) between Sb and HFO. PMID:24910911

  10. Bi-antimony capped Keggin polyoxometalate modified with Cu-ligand fragment

    SciTech Connect

    Huang, Jiao; Han, Zhangang; Zhang, Heng; Yu, Haitao; Zhai, Xueliang

    2012-10-15

    Three polyoxometalates consisting of bi-antimony capped Keggin-type clusters: [Cu(mbpy){sub 2}]{sub 2}[PMo{sub 12}O{sub 40}Sb{sub 2}]{center_dot}4H{sub 2}O (1), [Cu(mbpy){sub 2}][PMo{sub 12}O{sub 40}Sb{sub 2}] (2) and {l_brace}Cu(mbpy)[Cu(mbpy){sub 2}]{sub 2}{r_brace}[VMo{sub 8}V{sub 4}O{sub 40}Sb{sub 2}]{center_dot}2H{sub 2}O (3) (mbpy=4,4 Prime -dimethyl-2,2 Prime - dipyridyl in 1 and 2; 5,5 Prime -dimethyl-2,2 Prime -dipyridyl in 3) have been synthesized and characterized by IR, X-ray powder diffraction, TG analysis and electrochemical property. Single-crystal analysis revealed that all of three compounds are built upon bi-antimony capped Keggin-type polyoxoanions and Cu-mbpy cations. In 1-3, two Sb{sup III} centers located at the two opposite of anionic surface adopt fundamentally tetragonal pyramidal coordination geometry. Both compounds 1 and 2 consist of P-centered Keggin structure, while compound 3 presents a V-centered Keggin anion. The Keggin-type anions present different structural features: isolated cluster in 1 and Cu-ligand-supported cluster in 2 and 3. - Graphical abstract: Three hybrid compounds consisting of bi-antimony capped Keggin-type clusters modified with Cu-ligand cations have been synthesized and characterized. Highlights: Black-Right-Pointing-Pointer Three hybrid compounds consisting of bi-antimony capped Keggin-type clusters have been synthesized. Black-Right-Pointing-Pointer Two Sb{sup III} centers located at the two opposite of anionic surface adopt tetragonal pyramidal coordination geometry. Black-Right-Pointing-Pointer The anions present different structural features: isolated and Cu-ligand-supported cluster.

  11. Chemically deposited thin films of sulfides and selenides of antimony and bismuth as solar energy materials

    NASA Astrophysics Data System (ADS)

    Nair, M. T.; Nair, Padmanabhan K.; Garcia, V. M.; Pena, Y.; Arenas, O. L.; Garcia, J. C.; Gomez-Daza, O.

    1997-10-01

    Chemical bath deposition techniques for bismuth sulfide, bismuth selenide, antimony sulfide, and antimony selenide thin films of about 0.20 - 0.25 micrometer thickness are reported. All these materials may be considered as solar absorber films: strong optical absorption edges, with absorption coefficient, (alpha) , greater than 104 cm-1, are located at 1.31 eV for Bi2Se3, 1.33 eV for Bi2S3, 1.8 eV for Sb2S3, and 1.35 eV for Sb2Se3. As deposited, all the films are nearly amorphous. However, well defined crystalline peaks matching bismuthinite (JCPDS 17- 0320), paraguanajuatite (JCPDS 33-0214), and stibnite (JCPDS 6-0474) and antimony selenide (JCPDS 15-0861) for Bi2S3, Bi2Se3, Sb2S3 and Sb2Se3 respectively, are observed when the films are annealed in nitrogen at 300 degrees Celsius. This is accompanied by a substantial modification of the electrical conductivity in the films: from 10-7 (Omega) -1 cm-1 (in as prepared films) to 10 (Omega) -1 cm-1 in the case of bismuth sulfide and selenide films, and enhancement of photosensitivity in the case of antimony sulfide films. The chemical deposition of a CuS/CuxSe film on these Vx- VIy films and subsequent annealing at 300 degrees Celsius for 1 h at 1 torr of nitrogen leads to the formation of p-type films (conductivity of 1 - 100 (Omega) -1 cm-1) of multinary composition. Among these, the formation of Cu3BiS3 (JCPDS 9-0488) and Cu3SbS4 (JCPDS 35- 0581), CuSbS2 (JCPDS 35-0413) have been clearly detected. Solar energy applications of these films are suggested.

  12. Cu, Pt, and Pd complexes of the 3-deoxy-1,2-bis(thiosemicarbazone) derived from D-glucose.

    PubMed

    Horton, D; Varela, O

    2000-09-22

    3-Deoxy-D-erythro-hexos-2-ulose bis(thiosemicarbazone) (1) acts as a tetradentate ligand of the N2S2 type which forms stable coordination complexes with metal(II) cations. The Cu(II), Pt(II), and Pd(II) chelates (2, 4, and 6, respectively) of 1 were synthesized and characterized by elemental analysis and NMR spectroscopy. The NMR spectra of the Pt complex (4) showed the coupling of H-1 and C-1, C-2 of the bis(thiosemicarbazone) with 195Pt (33.7% naturally occurring), which supports the structure proposed for the chelate. The complexes 2, 4, and 6 were acetylated to give the corresponding tri-O-acetyl derivatives 3, 5, and 7. Elimination of Cu(II) from 3 with hydrogen sulfide afforded 8, the tri-O-acetyl derivative of 1. Preliminary studies have shown antiviral activity of chelates 2, 4, and 6 against poliovirus type 1. PMID:11072850

  13. Design, synthesis and biological evaluation of thiosemicarbazones, hydrazinobenzothiazoles and arylhydrazones as anticancer agents with a potential to overcome multidrug resistance.

    PubMed

    Pape, Veronika F S; Tóth, Szilárd; Füredi, András; Szebényi, Kornélia; Lovrics, Anna; Szabó, Pál; Wiese, Michael; Szakács, Gergely

    2016-07-19

    There is a constant need for new therapies against multidrug resistant (MDR) cancer. An attractive strategy is to develop chelators that display significant antitumor activity in multidrug resistant cancer cell lines overexpressing the drug efflux pump P-glycoprotein. In this study we used a panel of sensitive and MDR cancer cell lines to evaluate the toxicity of picolinylidene and salicylidene thiosemicarbazone, arylhydrazone, as well as picolinylidene and salicylidene hydrazino-benzothiazole derivatives. Our results confirm the collateral sensitivity of MDR cells to isatin-β-thiosemicarbazones, and identify several chelator scaffolds with a potential to overcome multidrug resistance. Analysis of structure-activity-relationships within the investigated compound library indicates that NNS and NNN donor chelators show superior toxicity as compared to ONS derivatives regardless of the resistance status of the cells. PMID:27161177

  14. Structural and spectral perspectives of a novel thiosemicarbazone synthesized from di-2-pyridyl ketone and 4-phenyl-3-thiosemicarbazide

    NASA Astrophysics Data System (ADS)

    Suni, V.; Prathapachandra Kurup, M. R.; Nethaji, Munirathinam

    2006-01-01

    A new thiosemicarbazone, HL is synthesized from di-2-pyridyl ketone and 4-phenyl-3-thiosemicarbazide and structurally and spectrochemically characterized. 1H NMR, 13C NMR, COSY, HMQC and IR spectra of the compound are studied and the proton magnetic resonance spectrum reveals some unprecedented observations. The thione form is predominant in the solid state, as supported by the crystal structure and IR data, while a thiol-thione equilibrium is proposed in the solution state by NMR studies. The compound crystallizes into a monoclinic lattice with space group C2/c and the ZE conformation is exhibited by the thiosemicarbazone. Intra- and intermolecular hydrogen-bonding interactions give rise to a two-dimensional packing in the crystal lattice.

  15. Antimony retention and release from drained and waterlogged shooting range soil under field conditions.

    PubMed

    Hockmann, Kerstin; Tandy, Susan; Lenz, Markus; Reiser, René; Conesa, Héctor M; Keller, Martin; Studer, Björn; Schulin, Rainer

    2015-09-01

    Many soils polluted by antimony (Sb) are subject to fluctuating waterlogging conditions; yet, little is known about how these affect the mobility of this toxic element under field conditions. Here, we compared Sb leaching from a calcareous shooting range soil under drained and waterlogged conditions using four large outdoor lysimeters. After monitoring the leachate samples taken at bi-weekly intervals for >1.5 years under drained conditions, two of the lysimeters were subjected to waterlogging with a water table fluctuating according to natural rainfall water infiltration. Antimony leachate concentrations under drained conditions showed a strong seasonal fluctuation between 110 μg L(-1) in summer and <40 μg L(-1) in winter, which closely correlated with fluctuations in dissolved organic carbon (DOC) concentrations. With the development of anaerobic conditions upon waterlogging, Sb in leachate decreased to 2-5 μg L(-1) Sb and remained stable at this level. Antimony speciation measurements in soil solution indicated that this decrease in Sb(V) concentrations was attributable to the reduction of Sb(V) to Sb(III) and the stronger sorption affinity of the latter to iron (Fe) (hydr)oxide phases. Our results demonstrate the importance of considering seasonal and waterlogging effects in the assessment of the risks from Sb-contaminated sites. PMID:25592464

  16. Structural, magnetic and dielectric investigations in antimony doped nano-phased nickel-zinc ferrites

    NASA Astrophysics Data System (ADS)

    Lakshmi, Ch. S.; Sridhar, Ch. S. L. N.; Govindraj, G.; Bangarraju, S.; Potukuchi, D. M.

    2015-02-01

    Nanocrystalline Ni-Zn-Sb ferrites synthesized by hydrothermal method are reported. Influence of Sb5+ ions on structural, magnetic and dielectric properties of ferrites is studied. Phase identification, lattice parameter and crystallite size studies are carried out using by X-ray diffraction (XRD). Addition of dopant resulted for decrease in lattice parameter. Crystallite size gets reduced from 62 nm to 38 nm with doping of Antimony. Crystallite size and porosity exhibit similar trends with doping. Morphological study is carried out by Field Emission Scanning Electron Microscopy (FESEM). Strong FTIR absorption bands at 400-600 cm-1 confirm the formation of ferrite structure. Increase of porosity is attributed to the grain size. Doping with Antimony results for decrease in saturation magnetization and increase in coercivity. An initial increase of saturation magnetization for x=0.1 is attributed to the unusually high density. Reversed trend of coercivity with crystallite size are observed. Higher value of dielectric constant ε‧(ω) is attributed to the formation of excess of Fe2+ ions caused by aliovalent doping of Sb5+ ions. Variation of dielectric constant infers hopping type of conductivity mechanism. The dielectric loss factor tanδ attains lower values of ~10-2. High ac resistivity ρ(ω) of 108 Ω cm is witnessed for antimony doped ferrites. Higher saturation magnetization and enhanced dielectric response directs for a possible utility as microwave oscillators and switches.

  17. Studies in atomic-fluorescence spectroscopy-V The fluorescence characteristics and determination of antimony.

    PubMed

    Dagnall, R M; Thompson, K C; West, T S

    1967-10-01

    Atomic-fluorescence of antimony may be generated in an air-propane flame by nebulizing aqueous solutions of antimony salts whilst irradiating the flame by means of a microwave-excited electrode-less discharge tube operating at 30 W. The strongest fluorescence is exhibited by the (4)S(11 2 ) --> (4)P(1 3 ) 2311 A resonance line and weaker signals are observed at the 2068 and 2176 A resonance lines and at four intercombination lines, at 2598, 2671, 2770 and 2878 A. A process of thermally assisted direct-line fluorescence is postulated to account for the otherwise inexplicable intensity of the 2598 A line emission. Atomic-fluorescence spectroscopy at 2176 A permits the determination of antimony in the range 0.1-120 ppm with a detection limit of 0.05 ppm. With the same equipment and source, the range of measurement for atomic-absorption was 6-120 ppm and the detection limit was 1 ppm. No interferences were observed from 100-fold molar amounts of Cd, Co, Cu, Fe, Hg, K, Mg, Mn, Mo, Na, NH(4), Pb and Zn or from arsenate, chloride, nitrate, phosphate and sulphate. PMID:18960212

  18. A new method to reduce false positives due to antimony in detection of gunshot residues.

    PubMed

    Aksoy, Çağdaş; Bora, Taner; Şenocak, Nilgün; Aydın, Fırat

    2015-05-01

    False positives due to the presence of antimony in vehicle seat fabrics are a problem in gunshot residue (GSR) analysis, in particular, when graphite furnace atomic absorption spectrometry (GFAAS) is employed. In this study, we sought to determine the reason for the prevalence of false positive results and to propose a new approach for the analysis of GSR on vehicle seats. GFAAS was used to examine adhesive tape swabs collected from 100 seats of 50 different automobiles. Characterization of seat fabrics was carried out by using Fourier transform infrared (FTIR) spectroscopy and scanning electron microscopy with energy dispersive X-ray (SEM/EDX) spectroscopy. The results of FTIR analysis indicated that all seat covers containing antimony were composed of polyester. Experimental results obtained by SEM/EDX analysis revealed that the fabrics in these seat covers contained evenly distributed antimony within the structure of polyester fibers. This study shows that the type of seat fabric should be determined by FTIR spectroscopy before elemental GSR analysis. In this way, most of the false positives caused by polyester fibers in GSR analysis can be prevented. PMID:25828380

  19. Comparative analysis of the cytotoxicity of substituted (phenylglyoxal bis(4-methyl-3-thiosemicarbazone)) copper (II) chelates.

    PubMed

    Coats, E A; Milstein, S R; Holbein, G; McDonald, J; Reed, R; Petering, H G

    1976-01-01

    Seven para-substituted [phenylglyoxal bis(4-methyl-3-thiosemicarbazone)]copper (II) chelates (12-18) have been designed, synthesized, and tested for their ability to inhibit the respiration of rat liver slices as a normal cell model and Ehrlich ascites cells as a tumor cell model. Relationships between chemical structure and respiratory inhibition are described on a quantitative basis using substituent contants (pi, Es, and sigmap) by computerized multiparameter regression analyses. The correlations indicate that changes in Es have the largest effect on liver slice toxicity of chelates while pi and sigmap account for most of the variation in toxicity to ascites cells. A comparative analysis strongly suggests that electron-donating substituents with greater water solubility should increase cytotoxicity to ascites cells at the expense of cytotoxicity to the rat liver cells. The predictions of the equations were checked by synthesizing and testing an additional derivative. The results strengthen the initial predictions. PMID:1246035

  20. Synthesis of isatin thiosemicarbazones derivatives: In vitro anti-cancer, DNA binding and cleavage activities

    NASA Astrophysics Data System (ADS)

    Ali, Amna Qasem; Teoh, Siang Guan; Salhin, Abdussalam; Eltayeb, Naser Eltaher; Khadeer Ahamed, Mohamed B.; Majid, A. M. S. Abdul

    New derivatives of thiosemicarbazone Schiff base with isatin moiety were synthesized L1-L6. The structures of these compounds were characterized based on the spectroscopic techniques. Compound L6 was further characterized by XRD single crystal. The interaction of these compounds with calf thymus (CT-DNA) exhibited high intrinsic binding constant (kb = 5.03-33.00 × 105 M-1) for L1-L3 and L5 and (6.14-9.47 × 104 M-1) for L4 and L6 which reflect intercalative activity of these compounds toward CT-DNA. This result was also confirmed by the viscosity data. The electrophoresis studies reveal the higher cleavage activity of L1-L3 than L4-L6. The in vitro anti-proliferative activity of these compounds against human colon cancer cell line (HCT 116) revealed that the synthesized compounds (L3, L6 and L2) exhibited good anticancer potency.

  1. Synthesis, Spectroscopic, and Antimicrobial Studies on Bivalent Zinc and Mercury Complexes of 2-Formylpyridine Thiosemicarbazone

    PubMed Central

    Chandra, Sulekh; Parmar, Shikha; Kumar, Yatendra

    2009-01-01

    A series of metal complexes of Zn(II) and Hg(II) having the general composition [M(L)2]X2 [where L = 2-formylpyridine thiosemicarbazone; M = Zn(II) and Hg(II); X = Cl−, NO3− and 1/2SO42−] have been prepared and characterized by elemental chemical analysis, molar conductance, and spectral (IR and mass) studies. The IR spectral data suggests the involvement of sulphur and azomethane nitrogen in coordination to the central metal ion. On the basis of spectral studies, a tetrahedral geometry has been assigned for Zn(II) and Hg(II) complexes. The free ligand and its metal complexes have been tested in vitro against a number of microorganisms in order to assess their antimicrobial properties. PMID:19421419

  2. Vibrational spectroscopic studies and computational study of ethyl methyl ketone thiosemicarbazone

    NASA Astrophysics Data System (ADS)

    Anoop, M. R.; Binil, P. S.; Suma, S.; Sudarsanakumar, M. R.; Y, Sheena Mary.; Varghese, Hema Tresa; Panicker, C. Yohannan

    2010-04-01

    FT-IR and FT-Raman spectra of ethyl methyl ketone thiosemicarbazone were recorded and analyzed. The crystal structure is also described. The vibrational wavenumbers were computed using HF/6-31G(d) and B3LYP/6-31G(d) basis sets and are assigned with the aid of MOLEKEL program. The first hyperpolarizability, infrared intensities and Raman activities are also reported. The calculated first hyperpolarizability is comparable with the reported values of similar derivatives and is an attractive molecule for future applications in non-linear optics. The geometrical parameters of the title compound obtained from XRD studies are in agreement with the calculated values. The red shift of the NH stretching wavenumber in the infrared spectrum compared to the computed wavenumber indicates the weakening of the N-H bond resulting in proton transfer to the neighbouring sulfur atom.

  3. Spectroscopic study one thiosemicarbazone derivative with ctDNA using ethidium bromide as a fluorescence probe.

    PubMed

    Geng, Shaoguang; Wu, Qing; Shi, Lei; Cui, Fengling

    2013-09-01

    In this study, a thiosemicarbazone derivative (E)-2-((1,4-dihydroxy-9,10-anthraquinone-2-yl)methylene)-N-(4-fluorophenyl)hydrazinecarbothioamide (DAFPT) was synthesized, and the interaction of DAFPT with calf thymus DNA (ctDNA) was explored using ethidium bromide (EB) as a fluorescence probe. The binding mode between DAFPT and ctDNA was investigated by UV absorption spectroscopy, fluorescence spectroscopy and molecular docking. The fluorescence quenching mechanism of EB-ctDNA by DAFPT might be a combined quenching type. Thermodynamic parameters showed that the reaction was spontaneous. According to ionic strength, fluorescence polarization and melting temperature (T(m)) curve results, DAFPT-ctDNA interaction was groove binding. The molecular modeling results indicated that DAFPT could slide into the A-T rich region of ctDNA. PMID:23769721

  4. Synthesis and Biochemical Evaluation of Thiochromanone Thiosemicarbazone Analogues as Inhibitors of Cathepsin L

    PubMed Central

    2012-01-01

    A series of 36 thiosemicarbazone analogues containing the thiochromanone molecular scaffold functionalized primarily at the C-6 position were prepared by chemical synthesis and evaluated as inhibitors of cathepsins L and B. The most promising inhibitors from this group are selective for cathepsin L and demonstrate IC50 values in the low nanomolar range. In nearly all cases, the thiochromanone sulfide analogues show superior inhibition of cathepsin L as compared to their corresponding thiochromanone sulfone derivatives. Without exception, the compounds evaluated were inactive (IC50 > 10000 nM) against cathepsin B. The most potent inhibitor (IC50 = 46 nM) of cathepsin L proved to be the 6,7-difluoro analogue 4. This small library of compounds significantly expands the structure–activity relationship known for small molecule, nonpeptidic inhibitors of cathepsin L. PMID:24900494

  5. Synthesis and spectral studies of platinum metal complexes of benzoin thiosemicarbazone

    NASA Astrophysics Data System (ADS)

    Offiong, Offiong E.

    1994-11-01

    The platinum metal chelates of benzoin thiosemicarbazone obtained with Ru(III), Rh(III), Ir(III), Pd(II) and Pt(II) were prepared from their corresponding halide salts. The complexes were characterized by elemental analysis, conductance measurement, IR, Raman, 1H-NMR, 13C-NMR and UV-visible spectra studies. Various ligand field parameters and nephelauxetic parameters were also calculated. The mode of bonding and the geometry of the ligand environment around the metal ion have been discussed in the light of the available data obtained. Complexes of Ru(III), Rh(III) and Ir(III) are six-coordinate octahedral, while Pd(II) and Pt(II) halide complexes are four-coordinated with halides bridging.

  6. Sequential extraction and determination of copper and nickel with 2,4-dihydroxyacetophenone thiosemicarbazone.

    PubMed

    Reddy, A V; Reddy, Y K

    1986-07-01

    2,4-Dihydroxyacetophenone thiosemicarbazone (DAPT) forms a 1:1 complex with copper(II) which can be extracted into n-butanol or ethyl acetate from acetic acid-sodium acetate (pH 5.0) buffer, and a 1:1 nickel(II) complex which can be extracted into n-butanol from ammonium chloride-ammonia (pH 7.5) buffer. The difference between the pH(1 2 ) values for extraction of the two complexes is 3.4 and this has been exploited for their sequential extraction and determination. The molar absorptivities for the copper and nickel complexes are 1.5 x 10(4)l.mole(-1).cm(-1) at 390 nm and 8.2 x 10(3)l.mole(-1).cm(-1) at 385 nm respectively. The procedure has been applied to the analysis of cupronickel. PMID:18964152

  7. Copper complexes of bis(thiosemicarbazones): from chemotherapeutics to diagnostic and therapeutic radiopharmaceuticals.

    PubMed

    Paterson, Brett M; Donnelly, Paul S

    2011-05-01

    The molecules known as bis(thiosemicarbazones) derived from 1,2-diones can act as tetradentate ligands for Cu(II), forming stable, neutral complexes. As a family, these complexes possess fascinating biological activity. This critical review presents an historical perspective of their progression from potential chemotherapeutics through to more recent applications in nuclear medicine. Methods of synthesis are presented followed by studies focusing on their potential application as anti-cancer agents and more recent investigations into their potential as therapeutics for Alzheimer's disease. The Cu(II) complexes are of sufficient stability to be used to coordinate copper radioisotopes for application in diagnostic and therapeutic radiopharmaceuticals. Detailed understanding of the coordination chemistry has allowed careful manipulation of the metal based properties to engineer specific biological activities. Perhaps the most promising complex radiolabelled with copper radioisotopes to date is Cu(II)(atsm), which has progressed to clinical trials in humans (162 references). PMID:21409228

  8. Synthesis, spectral characterization and eukaryotic DNA degradation of thiosemicarbazones and their platinum(IV) complexes

    NASA Astrophysics Data System (ADS)

    Al-Hazmi, G. A.; El-Metwally, N. M.; El-Gammal, O. A.; El-Asmy, A. A.

    2008-01-01

    The condensation products of acetophenone (or its derivatives), salicylaldehyde and o-hydroxy- p-methoxybenzophenone with thiosemicarbazide and ethyl- or phenyl-thiosemicarbazide are the investigated thiosemicarbazones. Their reactions with H 2PtCl 6 produced Pt(IV) complexes characterized by elemental, thermal, mass, IR and electronic spectral studies. The coordination modes were found mononegative bidentate in the acetophenone derivatives and binegative tridentate in the salicylaldehyde derivatives. The complexes were analyzed thermogravimetrically and found highly stable. Some ligands and their complexes were screened against Sarcina sp. and E. coli using the cup-diffusion technique. [Pt( oHAT)(OH)Cl] shows higher activity against E. coli than the other compounds. The degradation power of the tested compounds on the calf thymus DNA supports their selectivity against bacteria and not against the human or related eukaryotic organisms.

  9. Nickel(II) complexes containing thiosemicarbazone and triphenylphosphine: Synthesis, spectroscopy, crystallography and catalytic activity

    NASA Astrophysics Data System (ADS)

    Priyarega, S.; Kalaivani, P.; Prabhakaran, R.; Hashimoto, T.; Endo, A.; Natarajan, K.

    2011-09-01

    Four new Ni(II) complexes of the general formula [Ni(PPh 3)(L)] (L = dibasic tridentate ligand derived from 4-diethylamino-salicylaldehyde and thiosemicarbazide or 4-N-substituted thiosemicarbazide) have been reported. The new complexes have been synthesized and characterized by analytical and spectroscopic (IR, electronic, 1H NMR and 31P NMR) techniques. Molecular structure of one of the complexes has been determined by X-ray crystallography. The complex, [Ni(PPh 3)(L4)] (H 2L4 = thiosemicarbazone prepared from 4-diethylamino-salicylaldehyde and 4-phenylthiosemicarbazide) crystallized in monoclinic space group with two molecules per unit cell and has the dimensions of a = 13.232(6) Å, b = 10.181(5) Å, c = 13.574(7) Å, α = 90°, β = 98.483(2)° and γ = 90°. Catalytic activity of the complexes has been explored for aryl-aryl coupling reaction.

  10. Synthesis and spectral characterization of acetophenone thiosemicarbazone--a nonlinear optical material.

    PubMed

    Santhakumari, R; Ramamurthi, K; Vasuki, G; Yamin, Bohari M; Bhagavannarayana, G

    2010-08-01

    Acetophenone thiosemicarbazone (APTSC) was synthesized. Solubility of APTSC was determined in ethanol and methanol at different temperatures. Single crystals were grown from ethanol by slow evaporation at room temperature. The grown crystal was subjected to FTIR, Laser-Raman and (1)H NMR spectral analyses to confirm the synthesized compound. Thermal properties were investigated by thermogravimetric and differential thermal analyses. High-resolution X-ray diffractometry (HRXRD) was employed to evaluate the perfection of the grown crystal. The range and percentage of optical transmission was ascertained by recording UV-vis-NIR spectrum. The third order nonlinear optical parameters (nonlinear refractive index and nonlinear absorption coefficient) were derived by the Z-scan technique. PMID:20434945

  11. Novel aldehyde and thiosemicarbazone derivatives: Synthesis, spectroscopic characterization, structural studies and molecular docking studies

    NASA Astrophysics Data System (ADS)

    Karakurt, Tuncay; Tahtaci, Hakan; Subasi, Nuriye Tuna; Er, Mustafa; Ağar, Erbil

    2016-12-01

    In this study our purpose is that, synthesis and characterization of compounds containing the aldehyde and thiosemicarbazone groups and comparison of the theoretical results with the experimental results. The structures of all synthesized compounds were elucidated by IR, 1H NMR, 13C NMR, elemental analyses techniques. The structure of compound (4) (C9H8N4O2S) was also elucidated by X-ray diffraction analysis. In addition, the theoretical IR spectrum, 1H NMR and 13C NMR chemical shift values, frontier molecular orbital values (FMO) of these molecules were analyzed by using Becke-3- Lee-Yang-Parr (B3LYP) method with LanL2DZ basis set. Finally, molecular docking studies were performed on synthesized compounds using the 4DKI beta-lactam protein structure to determine the potential binding mode of inhibitors.

  12. Platinum and palladium complexes of thiosemicarbazones derived of 2-acetylthiophene: Synthesis and spectral studies

    NASA Astrophysics Data System (ADS)

    Neto, J. L.; de Lima, G. M.; Beraldo, H.

    2006-03-01

    The reaction of 2-acetylthiophene thiosemicarbazone (2-HATT) and 2-acetylthiophene 4-phenylthiosemicarbazone (2-HAT-4-FT) with Pd(COD)Cl 2 (COD = 1,5-cyclooctadiene) and trans-Pt 2PEt 3Cl 4 yielded four new metal complexes: [Pd(2-HATT)Cl 2] ( 1), [Pd(2-ATT) 2] ( 2), [Pd(2-AT-4-FT)Cl] ( 3) and [Pt(2-ATT)(PEt 3)Cl] ( 4). Apart from compound 3 all the others were characterised by 1H and 13C{ 1H} NMR, infrared spectroscopy, and elemental analysis. Multinuclear NMR experiments of 31P{ 1H} and 195Pt{ 1H} of complex 4 have revealed that the ligand 2-HATT behaves as a bidentate chelating agent towards Pd(COD)Cl 2 and trans-Pt 2PEt 3Cl 4 whereas ligand 2-HAT-4-FT forms a tridentate chelating complex with Pd(COD)Cl 2.

  13. Novel ruthenium(II) cyclopentadienyl thiosemicarbazone compounds with antiproliferative activity on pathogenic trypanosomatid parasites.

    PubMed

    Fernández, Mariana; Arce, Esteban Rodríguez; Sarniguet, Cynthia; Morais, Tânia S; Tomaz, Ana Isabel; Azar, Claudio Olea; Figueroa, Roberto; Diego Maya, J; Medeiros, Andrea; Comini, Marcelo; Helena Garcia, M; Otero, Lucía; Gambino, Dinorah

    2015-12-01

    Searching for new prospective antitrypanosomal agents, three novel Ru(II)-cyclopentadienyl compounds, [Ru(η(5)-C5H5)(PPh3)L], with HL=bioactive 5-nitrofuryl containing thiosemicarbazones were synthesized and characterized in the solid state and in solution. The compounds were evaluated in vitro on the blood circulating trypomastigote form of Trypanosoma cruzi (Dm28c strain), the infective form of Trypanosoma brucei brucei (strain 427) and on J774 murine macrophages and human-derived EA.hy926 endothelial cells. The compounds were active against both parasites with IC50 values in the micromolar or submicromolar range. Interestingly, they are much more active on T. cruzi than previously developed Ru(II) classical and organometallic compounds with the same bioactive ligands. The new compounds showed moderate to very good selectivity towards the parasites in respect to mammalian cells. The global results point at [RuCp(PPh3)L2] (L2=N-methyl derivative of 5-nitrofuryl containing thiosemicarbazone and Cp=cyclopentadienyl) as the most promising compound for further developments (IC50T. cruzi=0.41μM; IC50T. brucei brucei=3.5μM). Moreover, this compound shows excellent selectivity towards T. cruzi (SI>49) and good selectivity towards T. brucei brucei (SI>6). In order to get insight into the mechanism of antiparasitic action, the intracellular free radical production capacity of the new compounds was assessed by ESR. DMPO (5,5-dimethyl-1-pirroline-N-oxide) spin adducts related to the bioreduction of the complexes and to redox cycling processes were characterized. In addition, DNA competitive binding studies with ethidium bromide by fluorescence measurements showed that the compounds interact with this biomolecule. PMID:26275470

  14. Preparation of superconductor precursor powders

    DOEpatents

    Bhattacharya, Raghunath

    1998-01-01

    A process for the preparation of a precursor metallic powder composition for use in the subsequent formation of a superconductor. The process comprises the steps of providing an electrodeposition bath comprising an electrolyte medium and a cathode substrate electrode, and providing to the bath one or more soluble salts of one or more respective metals which are capable of exhibiting superconductor properties upon subsequent appropriate treatment. The bath is continually energized to cause the metallic and/or reduced particles formed at the electrode to drop as a powder from the electrode into the bath, and this powder, which is a precursor powder for superconductor production, is recovered from the bath for subsequent treatment. The process permits direct inclusion of all metals in the preparation of the precursor powder, and yields an amorphous product mixed on an atomic scale to thereby impart inherent high reactivity. Superconductors which can be formed from the precursor powder include pellet and powder-in-tube products.

  15. Bp44mT: an orally active iron chelator of the thiosemicarbazone class with potent anti-tumour efficacy

    PubMed Central

    Yu, Y; Rahmanto, Y Suryo; Richardson, DR

    2012-01-01

    BACKGROUND AND PURPOSE Our previous studies demonstrated that a thiosemicarbazone iron chelator (di-2-pyridylketone-4,4-dimethyl-3-thiosemicarbazone; Dp44mT) possesses potent and selective anti-cancer activity but led to cardiotoxicity at non-optimal doses. In this study, we examined the in vivo anti-tumour efficacy and tolerability of a new-generation 2-benzoylpyridine thiosemicarbazone iron chelator (2-benzoylpyridine-4,4-dimethyl-3-thiosemicarbazone; Bp44mT) administered via the oral or i.v. routes. EXPERIMENTAL APPROACH BpT chelators were tested in vitro against human lung cancer cells (DMS-53) and in vivo in DMS-53 tumour xenografts in mice. The toxicity of Bp44mT in vivo and its effects on the expression of iron-regulated molecules involved in growth and cell cycle control were investigated. KEY RESULTS Administration of Bp44mT by either route resulted in marked dose-dependent inhibition of tumour growth. When administered at 50 mg·kg−1 via oral gavage three times per week for 23 days, the net xenograft growth was inhibited by 75%, compared with vehicle-treated mice. Toxicological examination showed reversible alterations including slight reduction of RBC count, with a decrease of liver and splenic iron levels, which confirmed iron chelation in vivo. Importantly, in contrast to Dp44mT, the chelator-treated mice did not show cardiac histological abnormalities. There was also no significant weight loss in mice, suggesting oral administration of Bp44mT was well tolerated. CONCLUSIONS AND IMPLICATIONS This is the first study to show that Bp44mT can be given orally with potent anti-tumour efficacy. Oral administration of a novel and effective chemotherapeutic agent provides the benefits of convenience for chronic dosing regimens. PMID:21658021

  16. Crystal structure and photochromism of 1-phenyl-3-methyl-4-benzyl-5-one-pyrazole S-methyl thiosemicarbazone

    NASA Astrophysics Data System (ADS)

    Liu, Lang; Jia, Dian-zeng; Ji, Ya-li; Yu, Kai-bei

    2003-07-01

    A new organic photochromic compound containing pyrazolone-ring photochromic functional unit: 1-phenyl-3-methyl-4-benzyl-5-one pyrazole S-methyl thiosemicarbazone (PMBP-smtsc) was synthesized. The photochromic properties and photochemical kinetics of PMBP-smtsc have been studied by UV reflectance spectra under irradiation of 365 nm light. The crystal structure analyses of photocolored product show the photochromism is due to the photoisomerization from enol form to keto form through an intermolecular proton transfer.

  17. Accumulation of antimony and other potentially toxic elements in plants around a former antimony mine located in the Ribes Valley (Eastern Pyrenees)

    NASA Astrophysics Data System (ADS)

    Bech, Jaume; Corrales, Isabel; Duran, Paola; Roca, Núria; Tume, Pedro; Barceló, Juan; Poschenrieder, Charlotte

    2010-05-01

    Soil contamination by antimony is of increasing environmental concern due to the use of this amphoterous p-block element in many industrial applications such as flame retardant, electronics, alloys, rubber and textile industries. However, little is still known about the response of plants to antimony. Here we report on the accumulation of antimony and other potentially toxic elements (mainly As, Pb and Cu) in plants growing around a former antimony mine in the ribes Valley located in the Eastern Pyrenees (424078E, 4686100N alt. 1145 m.a.s.l) that was operating approximately between the years 1870 to 1960. The ore mineral veins are included in quartz gangue. The main ores were: Sulphides: Stibnite (Sb2S3), Pyrite (FeS2), Sphalerite (ZnS), Arsenopyrite (FeAs), Galenite (PbS), Chalcopyrite (CuFeS2), Tetrahydrite (Cu5Sb2S3). Sulphosals: Boulangerite (5PbS•2Sb2S3), Jamesonite (4PbS•FeS•3Sb2S3), Zinckenite (6PbS•7Sb2S3), Plagionite (5PbS•4Sb2S3), Bournonite PbCu (Sb,As)S3, Pyrargirite (Ag3SbS3). Soil and plant samples were taken at five locations with different levels of Sb, As, and polymetallic contamination. Both pseudototal (aqua regia soluble) and extractable (EDTA) concentrations of metals from sites with low (sites 1 and 2), moderate (site 3 and 4) and high (sites 5 and 6) pollutant burdens were studied. The range of agua regia and EDTA values in mgkg-1 is as follows: Sb 8-2904 and 0.88-44; As: 33-16186 and 3.2-167; Pb: 79-4794 and 49-397; Cu: 66-712 and 48-56 mg•kg-1, respectively). While sites 1 to 4 had alkaline soil pH (7.4-8.7), sites 5 and 6 were acidic with values of 6 and 4.6, respectively. Different herbaceous plant species (Poa annua, Echium vulgare, Sonchus asper, Barbera verna among others) at the low and moderately polluted sites were able to efficiently restrict Sb and As transport to shoots showing average concentration ranges between 5.5 and 23 mg/kg As and 1.21 mg/kg and 4.9 mg/kg Sb. However, at the highly polluted acidic sites (5 and

  18. Synthesis, activity and pharmacophore development for isatin-β-thiosemicarbazones with selective activity towards multidrug resistant cellsa

    PubMed Central

    Hall, Matthew D.; Salam, Noeris K.; Hellawell, Jennifer L.; Fales, Henry M.; Kensler, Caroline B.; Ludwig, Joseph A.; Szakacs, Gergely; Hibbs, David E.; Gottesman, Michael M.

    2009-01-01

    We have recently identified a new class of compounds that selectively kill cells that express P-glycoprotein (P-gp, MDR1), the ATPase efflux pump that confers multidrug resistance on cancer cells. Several isatin-β-thiosemicarbazones from our initial study have been validated, and a range of analogs synthesized and tested. A number demonstrated improved MDR1-selective activity over the lead, NSC73306 (1). Pharmacophores for cytotoxicity and MDR1-selectivity were generated to delineate the structural features required for activity. The MDR1-selective pharmacophore highlights the importance of aromatic/hydrophobic features at the N4 position of the thiosemicarbazone, and the reliance on the isatin moiety as key bioisosteric contributors. Additionally, a quantitative structure-activity relationship (QSAR) model that yielded a cross-validated correlation coefficient of 0.85 effectively predicts the cytotoxicty of untested thiosemicarbazones. Together, the models serve as effective approaches for predicting structures with MDR1-selective activity, and aid in directing the search for the mechanism of action of 1. PMID:19397322

  19. G2/M Cell Cycle Arrest and Tumor Selective Apoptosis of Acute Leukemia Cells by a Promising Benzophenone Thiosemicarbazone Compound.

    PubMed

    Cabrera, Maia; Gomez, Natalia; Remes Lenicov, Federico; Echeverría, Emiliana; Shayo, Carina; Moglioni, Albertina; Fernández, Natalia; Davio, Carlos

    2015-01-01

    Anti-mitotic therapies have been considered a hallmark in strategies against abnormally proliferating cells. Focusing on the extensively studied family of thiosemicarbazone (TSC) compounds, we have previously identified 4,4'-dimethoxybenzophenone thiosemicarbazone (T44Bf) as a promising pharmacological compound in a panel of human leukemia cell lines (HL60, U937, KG1a and Jurkat). Present findings indicate that T44Bf-mediated antiproliferative effects are associated with a reversible chronic mitotic arrest caused by defects in chromosome alignment, followed by induced programmed cell death. Furthermore, T44Bf selectively induces apoptosis in leukemia cell lines when compared to normal peripheral blood mononuclear cells. The underlying mechanism of action involves the activation of the mitochondria signaling pathway, with loss of mitochondrial membrane potential and sustained phosphorylation of anti-apoptotic protein Bcl-xL as well as increased Bcl-2 (enhanced phosphorylated fraction) and pro-apoptotic protein Bad levels. In addition, ERK signaling pathway activation was found to be a requisite for T44Bf apoptotic activity. Our findings further describe a novel activity for a benzophenone thiosemicarbazone and propose T44Bf as a promising anti-mitotic prototype to develop chemotherapeutic agents to treat acute leukemia malignancies. PMID:26360247

  20. Preparation and Biodistribution Studies of a Radiogallium-Acetylacetonate Bis (Thiosemicarbazone) Complex in Tumor-Bearing Rodents

    PubMed Central

    Jalilian, Amir Reza; Yousefnia, Hassan; Shafaii, Kamaleddin; Novinrouz, Aytak; Rajamand, Amir Abbas

    2012-01-01

    Various radiometal complexes have been developed for tumor imaging, especially Ga-68 tracer. In the present study, the development of a radiogallium bis-thiosemicarbazone complex has been reported. [67Ga] acetylacetonate bis(thiosemicarbazone) complex ([67Ga] AATS) was prepared starting [67Ga]Gallium acetate and freshly prepared acetylacetonate bis (thiosemicarbazone) (AATS) in 30 min at 90°C. The partition co-efficient and the stability of the tracer were determined in final solution (25°C) and the presence of human serum (37°C) up to 24 h. The biodistribution of the labeled compound in wild-type and fibrosarcoma-bearing rodents were determined up to 72 h. The radiolabled Ga complex was prepared in high radiochemical purity (> 97%, HPLC) followed by initial biodistribution data with the significant tumor accumulation of the tracer in 2 h which is far higher than free Ga-67 cation while the compound wash-out is significantly faster. Above-mentioned pharmacokinetic properties suggest an interesting radiogallium complex while prepared by the PET Ga radioisotope, 68Ga, in accordance with the physical half life, for use in fibrosarcoma tumors, and possibly other malignancies. PMID:24250475

  1. G2/M Cell Cycle Arrest and Tumor Selective Apoptosis of Acute Leukemia Cells by a Promising Benzophenone Thiosemicarbazone Compound

    PubMed Central

    Cabrera, Maia; Gomez, Natalia; Remes Lenicov, Federico; Echeverría, Emiliana; Shayo, Carina; Moglioni, Albertina; Fernández, Natalia; Davio, Carlos

    2015-01-01

    Anti-mitotic therapies have been considered a hallmark in strategies against abnormally proliferating cells. Focusing on the extensively studied family of thiosemicarbazone (TSC) compounds, we have previously identified 4,4’-dimethoxybenzophenone thiosemicarbazone (T44Bf) as a promising pharmacological compound in a panel of human leukemia cell lines (HL60, U937, KG1a and Jurkat). Present findings indicate that T44Bf-mediated antiproliferative effects are associated with a reversible chronic mitotic arrest caused by defects in chromosome alignment, followed by induced programmed cell death. Furthermore, T44Bf selectively induces apoptosis in leukemia cell lines when compared to normal peripheral blood mononuclear cells. The underlying mechanism of action involves the activation of the mitochondria signaling pathway, with loss of mitochondrial membrane potential and sustained phosphorylation of anti-apoptotic protein Bcl-xL as well as increased Bcl-2 (enhanced phosphorylated fraction) and pro-apoptotic protein Bad levels. In addition, ERK signaling pathway activation was found to be a requisite for T44Bf apoptotic activity. Our findings further describe a novel activity for a benzophenone thiosemicarbazone and propose T44Bf as a promising anti-mitotic prototype to develop chemotherapeutic agents to treat acute leukemia malignancies. PMID:26360247

  2. Copper(II) complexes with 2-pyridineformamide-derived thiosemicarbazones: Spectral studies and toxicity against Artemia salina

    NASA Astrophysics Data System (ADS)

    Ferraz, Karina O.; Wardell, Solange M. S. V.; Wardell, James L.; Louro, Sonia R. W.; Beraldo, Heloisa

    2009-07-01

    The copper(II) complexes [Cu(H2Am4DH)Cl 2] ( 1), [Cu(H2Am4Me)Cl 2] ( 2), [Cu(H2Am4Et)Cl 2] ( 3) and [Cu(2Am4Ph)Cl] ( 4) with 2-pyridineformamide thiosemicarbazone (H2Am4DH) and its N(4)-methyl (H2Am4Me), N(4)-ethyl (H2Am4Et) and N(4)-phenyl (H2Am4Ph) derivatives were studied by means of infrared and EPR spectral techniques. The crystal structure of 4 was determined. The studied compounds proved to be toxic to Artemia salina, suggesting that they could present cytotoxic activity against solid tumors. Among the free thiosemicarbazones H2Am4Ph presented higher toxicity than all other compounds, which showed comparable effects. In the case of complexes 2 and 3 toxicity is probably attributable to the complex as an entity or to a synergistic effect involving the thiosemicarbazone and copper. H2Am4Ph and complexes 2 and 3 revealed to be the most promising compounds as potential antineoplasic agents.

  3. Kinetic studies on the oxidation of oxyhemoglobin by biologically active iron thiosemicarbazone complexes: relevance to iron-chelator-induced methemoglobinemia.

    PubMed

    Basha, Maram T; Rodríguez, Carlos; Richardson, Des R; Martínez, Manuel; Bernhardt, Paul V

    2014-03-01

    The oxidation of oxyhemoglobin to methemoglobin has been found to be facilitated by low molecular weight iron(III) thiosemicarbazone complexes. This deleterious reaction, which produces hemoglobin protein units unable to bind dioxygen and occurs during the administration of iron chelators such as the well-known 3-aminopyridine-2-pyridinecarbaldehyde thiosemicarbazone (3-AP; Triapine), has been observed in the reaction with Fe(III) complexes of some members of the 3-AP structurally-related thiosemicarbazone ligands derived from di-2-pyridyl ketone (HDpxxT series). We have studied the kinetics of this oxidation reaction in vitro using human hemoglobin and found that the reaction proceeds with two distinct time-resolved steps. These have been associated with sequential oxidation of the two different oxyheme cofactors in the α and β protein chains. Unexpected steric and hydrogen-bonding effects on the Fe(III) complexes appear to be the responsible for the observed differences in the reaction rate across the series of HDpxxT ligand complexes used in this study. PMID:24317633

  4. Antimony(III) and bismuth(III) amides containing pendant N-donor groups--a combined experimental and theoretical study.

    PubMed

    Vránová, Iva; Jambor, Roman; Růžička, Aleš; Hoffmann, Alexander; Herres-Pawlis, Sonja; Dostál, Libor

    2015-01-01

    N,N- and N,N,N-chelated antimony(III) and bismuth(III) chlorides L(1-3)MCl2 1-4 [for L(1): M = Sb (1), for L(2): M = Sb (2) and for L(3): M = Sb (3) and Bi (4)], containing ligands L(1-3) derived from the pyrrole ring (where L(1) = C4H3N-2-(CH[double bond, length as m-dash]N-2',6'-iPr2C6H3), L(2) = C4H2N-2,5-(CH2NMe2)2, L(3) = C4H2N-2,5-(CH2NC4H8)2), were prepared by the treatment of lithium precursors with SbCl3 or BiCl3. Molecular structures 1-4 of were described both in solution (NMR spectroscopy) and in the solid state (single-crystal X-ray diffraction analysis). Structures of 1-4 were also subjected to a density functional theory study. PMID:25385247

  5. Development of an analytical method for antimony speciation in vegetables by HPLC-hydride generation-atomic fluorescence spectrometry.

    PubMed

    Olivares, David; Bravo, Manuel; Feldmann, Jorg; Raab, Andrea; Neaman, Alexander; Quiroz, Waldo

    2012-01-01

    A new method for antimony speciation in terrestrial edible vegetables (spinach, onions, and carrots) was developed using HPLC with hydride generation-atomic fluorescence spectrometry. Mechanical agitation and ultrasound were tested as extraction techniques. Different extraction reagents were evaluated and optimal conditions were determined using experimental design methodology, where EDTA (10 mmol/L, pH 2.5) was selected because this chelate solution produced the highest extraction yield and exhibited the best compatibility with the mobile phase. The results demonstrated that EDTA prevents oxidation of Sb(III) to Sb(V) and maintains the stability of antimony species during the entire analytical process. The LOD and precision (RSD values obtained) for Sb(V), Sb(III), and trimethyl Sb(V) were 0.08, 0.07, and 0.9 microg/L and 5.0, 5.2, and 4.7%, respectively, for a 100 microL sample volume. The application of this method to real samples allowed extraction of 50% of total antimony content from spinach, while antimony extracted from carrots and onion samples ranged between 50 and 60 and 54 and 70%, respectively. Only Sb(V) was detected in three roots (onion and spinach) that represented 60-70% of the total antimony in the extracts. PMID:22970588

  6. Effect of decabromodiphenyl ether and antimony trioxide on controlled pyrolysis of high-impact polystyrene mixed with polyolefins.

    PubMed

    Mitan, Nona Merry M; Bhaskar, Thallada; Hall, William J; Muto, Akinori; Williams, Paul T; Sakata, Yusaku

    2008-07-01

    The controlled pyrolysis of polyethylene/polypropylene/polystyrene mixed with brominated high-impact polystyrene containing decabromodiphenyl ether as a brominated flame-retardant with antimony trioxide as a synergist was performed. The effect of decabromodiphenyl ether and antimony trioxide on the formation of its congeners and their effect on distribution of pyrolysis products were investigated. The controlled pyrolysis significantly affected the decomposition behavior and the formation of products. Analysis with gas chromatograph with electron capture detector confirmed that the bromine content was rich in step 1 (oil 1) liquid products leaving less bromine content in the step 2 (oil 2) liquid products. In the presence of antimony containing samples, the major portion of bromine was observed in the form of antimony bromide and no flame-retardant species were found in oil 1. In the presence of synergist, the step 1 and step 2 oils contain both light and heavy compounds. In the absence of synergist, the heavy compounds in step 1 oil and light compounds in step 2 oils were observed. The presence of antimony bromide was confirmed in the step 1 oils but not in step 2 oils. PMID:18499216

  7. Thin films of copper antimony sulfide: A photovoltaic absorber material

    SciTech Connect

    Ornelas-Acosta, R.E.; Shaji, S.; Avellaneda, D.; Castillo, G.A.; Das Roy, T.K.; Krishnan, B.

    2015-01-15

    Highlights: • CuSbS{sub 2} thin films were prepared by heating Sb{sub 2}S{sub 3}/Cu layers. • Analyzed the structure, composition, optical, and electrical properties. • PV structures: glass/SnO{sub 2}:F/n-CdS/p-CuSbS{sub 2}/C/Ag were formed at different conditions. • The PV parameters (J{sub sc}, V{sub oc}, and FF) were evaluated from the J–V characteristics. • J{sub sc}: 0.52–3.20 mA/cm{sup 2}, V{sub oc}:187–323 mV, FF: 0.27–0.48 were obtained. - Abstract: In this work, we report preparation and characterization of CuSbS{sub 2} thin films by heating glass/Sb{sub 2}S{sub 3}/Cu layers and their use as absorber material in photovoltaic structures: glass/SnO{sub 2}:F/n-CdS/p-CuSbS{sub 2}/C/Ag. The Sb{sub 2}S{sub 3} thin films of 600 nm were prepared by chemical bath deposition on which copper thin films of 50 nm were thermally evaporated, and the glass/Sb{sub 2}S{sub 3}/Cu multilayers were heated in vacuum at different temperatures. X-ray diffraction analysis showed the formation of orthorhombic CuSbS{sub 2} after heating the precursor layers. Studies on identification and chemical state of the elements were done using X-ray photoelectron spectroscopy. The optical band gap of the CuSbS{sub 2} thin films was 1.55 eV and the thin films were photoconductive. The photovoltaic parameters of the devices using CuSbS{sub 2} as absorber and CdS as window layer were evaluated from the J–V curves, yielding J{sub sc}, V{sub oc}, and FF values in the range of 0.52–3.20 mA/cm{sup 2}, 187–323 mV, and 0.27–0.48, respectively, under illumination of AM1.5 radiation.

  8. Synthesis, structural characterization and antimicrobial activities of 12 zinc(II) complexes with four thiosemicarbazone and two semicarbazone ligands.

    PubMed

    Kasuga, Noriko Chikaraishi; Sekino, Kiyoshi; Ishikawa, Motoki; Honda, Ayano; Yokoyama, Masaki; Nakano, Saori; Shimada, Nobuhiro; Koumo, Chisa; Nomiya, Kenji

    2003-08-01

    Twelve zinc(II) complexes with thiosemicarbazone and semicarbazone ligands were prepared and characterized by elemental analysis, thermogravimetric and differential thermal analysis (TG/DTA), FT-IR and 1H and 13C NMR spectroscopy. Seven three-dimensional structures of zinc(II) complexes were determined by single-crystal X-ray analysis. Their antimicrobial activities were evaluated by MIC against four bacteria (B. subtilis, S. aureus, E. coli and P. aeruginosa), two yeasts (C. albicans and S. cerevisiae) and two molds (A. niger and P. citrinum). The 5- and 6-coordinate zinc(II) complexes with a tridentate thiosemicarbazone ligand (Hatsc), ([Zn(atsc)(OAc)](n) 1, [Zn(Hatsc)(2)](NO(3))(2).0.3H(2)O 2, [ZnCl(2)(Hatsc)] 3 and [Zn(SO(4))(Hatsc)(H(2)O)].H(2)O 4 [Hatsc=2-acetylpyridine(thiosemicarbazone)]), showed antimicrobial activities against test organisms, which were different from those of free ligands or the starting zinc(II) compounds. Especially, complex 2 showed effective activities against P. aeruginosa, C. albicans and moderate activities against S. cerevisiae and two molds. These facts are in contrast to the results that the 5- or 6-coordinate zinc(II) complexes with a tridentate 2-acetylpyridine-4N-morpholinethiosemicarbazone, ([Zn(mtsc)(2)].0.2EtOH 5, the previously reported catena-poly [Zn(mtsc)-mu-(OAc-O,O')](n) and [Zn(NO(3))(2)(Hmtsc)] [Hmtsc=2-acetylpyridine (4N-morpholyl thiosemicarbazone)]), showed no activities against the test microorganisms. The 5- and 6-coordinate zinc(II) complexes with a tridentate 2-acetylpyridinesemicarbazone, ([Zn(OAc)(2)(Hasc)] 6 and [Zn(Hasc)(2)](NO(3))(2) 7 [Hasc=2-acetylpyridine(semicarbazone)]), showed no antimicrobial activities against bacteria, yeasts and molds. Complex [ZnCl(2)(Hasc)] 8, which was isostructural to complex 3, showed modest activity against Gram-positive bacterium, B. subtilis. The 1:1 complexes of zinc(II) with pentadentate thiosemicarbazone ligands, ([Zn(dmtsc)](n) 9 and [Zn(datsc)](n) 10 [H(2)dmtsc=2

  9. Synthesis, characterization, electrochemical studies, and in vitro antibacterial activity of novel thiosemicarbazone and its Cu(II), Ni(II), and Co(II) complexes.

    PubMed

    Khan, Salman A; Asiri, Abdullah M; Al-Amry, Khalid; Malik, Maqsood Ahmad

    2014-01-01

    Metal complexes were prepared by the reaction of thiosemicarbazone with CuCl2, NiCl2, CoCl2, Cu(OAc)2, Ni(OAc)2, and Co(OAc)2. The thiosemicarbazone coordinates to metal through the thionic sulfur and the azomethine nitrogen. The thiosemicarbazone was obtained by the thiosemicarbazide with 3-acetyl-2,5-dimethylthiophene. The identities of these compounds were elucidated by IR, (1)H, (13)C-NMR, and GC-MS spectroscopic methods and elemental analyses. The antibacterial activity of these compounds was first tested in vitro by the disc diffusion assay against two Gram-positive and two Gram-negative bacteria, and then the minimum inhibitory concentration (MIC) was determined by using chloramphenicol as reference drug. The results showed that compound 1.1 is better inhibitor of both types of tested bacteria as compared to chloramphenicol. PMID:24523641

  10. Synthesis, Characterization, Electrochemical Studies, and In Vitro Antibacterial Activity of Novel Thiosemicarbazone and Its Cu(II), Ni(II), and Co(II) Complexes

    PubMed Central

    Khan, Salman A.; Asiri, Abdullah M.; Al-Amry, Khalid; Malik, Maqsood Ahmad

    2014-01-01

    Metal complexes were prepared by the reaction of thiosemicarbazone with CuCl2, NiCl2, CoCl2, Cu(OAc)2, Ni(OAc)2, and Co(OAc)2. The thiosemicarbazone coordinates to metal through the thionic sulfur and the azomethine nitrogen. The thiosemicarbazone was obtained by the thiosemicarbazide with 3-acetyl-2,5-dimethylthiophene. The identities of these compounds were elucidated by IR, 1H, 13C-NMR, and GC-MS spectroscopic methods and elemental analyses. The antibacterial activity of these compounds was first tested in vitro by the disc diffusion assay against two Gram-positive and two Gram-negative bacteria, and then the minimum inhibitory concentration (MIC) was determined by using chloramphenicol as reference drug. The results showed that compound 1.1 is better inhibitor of both types of tested bacteria as compared to chloramphenicol. PMID:24523641

  11. Half-sandwich ruthenium-arene complexes with thiosemicarbazones: Synthesis and biological evaluation of [(η6-p-cymene)Ru(piperonal thiosemicarbazones)Cl]Cl complexes

    PubMed Central

    Dourth, Deidra; Shaloski, Michael; Didion, Jacob; Thessing, Jeffrey; Woods, Jason; Crowell, Vernon; Gerasimchuk, Nikolay; Gonzalez-Sarrías, Antonio; Seeram, Navindra P.

    2011-01-01

    The synthesis and characterization of a number of organometallic ruthenium(II) complexes containing a series of bidentate thiosemicarbazone ligands derived from piperonal is reported. The structure of compounds have been confirmed by spectroscopic analysis (IR and NMR) as well as X-ray crystallographic analysis of [(η6-p-cymene)Ru(pPhTSC)Cl]Cl (4) (pPhTSC is piperonal-N(4)-phenylthiosemicarbazone). The interaction of the complexes ([(η6-p-cymene)Ru(pEtTSC)Cl]Cl) (3) (pEtTSC is piperonal-N(4)-ethylthiosemicarbazone) and 4 with calf thymus DNA, human serum albumin (HSA) and pBR322 plasmid DNA were studied by spectroscopic, gel electrophoresis and hydrodynamic methods. The apparent binding constant for the interaction with DNA was determined to be 3.97 × 103 M−1 and 4.07 × 103 M−1 at 293 K for 3 and 4 respectively. The complexes bind strongly to HSA with binding constants of 2.94 × 104 M−1 and 12.2 × 104 M−1 at 296 K for 3 and 4 respectively. The in vitro anticancer activity of 3 and 4 has been evaluated against two human colon cancer cell line (HCT-116 and Caco-2) with IC50 values in the range 26 – 150 µM. Both 3 and 4 show good activity as a catalytic inhibitor of human topoisomerase II at concentrations as low as 20 µM. The proficiency of 3 and 4 to act as antibacterial agents was also evaluated against six pathogenic bacterial strains with the best activity seen against Gram-positive strains. PMID:21666776

  12. Structure-antiproliferative activity studies on l-proline- and homoproline-4-N-pyrrolidine-3-thiosemicarbazone hybrids and their nickel(ii), palladium(ii) and copper(ii) complexes.

    PubMed

    Dobrova, Aliona; Platzer, Sonja; Bacher, Felix; Milunovic, Miljan N M; Dobrov, Anatolie; Spengler, Gabriella; Enyedy, Éva A; Novitchi, Ghenadie; Arion, Vladimir B

    2016-09-14

    Two water-soluble thiosemicarbazone-proline (H2L(1)) and thiosemicarbazone-homoproline hybrids (H2L(2)) were synthesised. By reaction of H2L(1) with NiCl2·6H2O, PdCl2 and CuCl2·2H2O in ethanol, the series of square-planar complexes [Ni(H2L(1))Cl]Cl·1.3H2O (1·1.3H2O), [Pd(H2L(1))Cl]Cl·H2O (2·H2O) and [Cu(H2L(1))Cl]Cl·0.7H2O (3·0.7H2O) was prepared, and starting from H2L(2) and CuCl2·2H2O in methanol, the complex [Cu(H2L(2))Cl2]·H2O (4·H2O) was obtained. The compounds have been characterised by elemental analysis, spectroscopic methods (IR, UV-vis and NMR spectroscopy), ESI mass spectrometry and single crystal X-ray crystallography (H2L(1), 1, 2 and 4). As a solid, 1 is diamagnetic, while it is paramagnetic in methanolic solution. The effective magnetic moment of 3.26 B.M. at room temperature indicates the change in coordination geometry from square-planar to octahedral upon dissolution. The in vitro anticancer potency of ligand precursors H2L(1) and H2L(2) and metal complexes 1-4 was studied in three human cancer cell lines (A549, CH1 and SW480) and in noncancerous murine embryonal fibroblasts (NIH/3T3), and the mechanism of cell death was also assayed by flow cytometry. Clear-cut structure-activity relationships have been established. The metal ions exert marked effects in a divergent manner: copper(ii) increases, whereas nickel(ii) and palladium(ii) decrease the cytotoxicity of the hybrids. The antiproliferative activity of H2L(1) and metal complexes 1-3 decreases in all three tumour cell lines in the following rank order: 3 > H2L(1) > 1 > 2. The role of square-planar geometry in the underlying mechanism of cytotoxicity of the metal complexes studied seems to be negligible, while structural modifications at the terminal amino group of thiosemicarbazide and proline moieties are significant for enhancing the antiproliferative activity of both hybrids and copper(ii) complexes. PMID:27485263

  13. Precursors of Hypertension: A Review

    PubMed Central

    Thomas, John; Neser, William B.; Thomas, Johniene; Semenya, Kofi; Green, Donald R.

    1983-01-01

    Recent advances in hypertension therapy have been remarkable; however, much less is known about those precursors that facilitate preventive and early intervention measures. This review of the literature indicates that relevant precursors are early elevated casual systolic blood pressures, positive family history, and obesity in females. Additional predisposing or enhancing factors point to high sodium ingestion, heavy smoking, and high socioecologic stress. Evidence for a high-risk hypertensive personality is not conclusive. There is a paucity of longitudinal data on hypertension in the black population. PMID:6864814

  14. Synthesis of antimony complexes of yeast mannan and mannan derivatives and their effect on Leishmania-infected macrophages.

    PubMed Central

    Cantos, G; Barbieri, C L; Iacomini, M; Gorin, P A; Travassos, L R

    1993-01-01

    Antimony(Sb)-yeast mannan complexes were synthesized as a strategy to introduce Sb into macrophages infected with Leishmania amastigotes. The complexes were taken up by endocytosis after specific recognition by alpha-D-mannosyl receptors on the macrophage membrane. About 90% of the intracellular parasites were destroyed by Sb-mannan in vitro, whereas the corresponding Sb concentration used as the pentavalent antimonial drug glucantime destroyed about 60% of the amastigotes. None of the Sb complexes prepared with mannan acid or basic derivatives was as effective as the simple Sb-mannan complex in clearing macrophage infection by Leishmania (L) amazonensis. The leishmanicidal effect of Sb-mannan was also demonstrated in vivo with infected hamsters. The alternative use of Sb-mannan complex in the treatment of human leishmaniasis is envisaged on the basis of parasite-killing efficiency and the use of a low antimony dose. Images Figure 1 PMID:8424752

  15. Role of Metalation in the Topoisomerase IIα Inhibition and Antiproliferation Activity of a Series of α-Heterocyclic-N4-Substituted Thiosemicarbazones and Their Cu(II) Complexes

    PubMed Central

    Zeglis, Brian M.; Divilov, Vadim; Lewis, Jason S.

    2014-01-01

    The topoisomerase-IIα inhibition and antiproliferative activity of α-heterocyclic thiosemicarbazones and their corresponding copper(II) complexes have been investigated. The CuII(thiosemicarbazonato)Cl complexes were shown to catalytically inhibit topoisomerase-IIα at concentrations (0.3–7.2 μM) over an order of magnitude lower than their corresponding thiosemicarbazone ligands alone. The copper complexes were also shown to inhibit the proliferation of breast cancer cells expressing high levels of topoisomerase-IIα (SK-BR-3) at lower concentrations than cells expressing lower levels of the enzyme (MCF-7). PMID:21391686

  16. Hormone Anchored Metal Complexes. 1. Synthesis, Structure, Spectroscopy and In Vitro Antitumor Activity of Testosterone Acetate Thiosemicarbazone and its Metal Complexes

    PubMed Central

    Murugkar, Anupa; Unnikrishnan, Bindu; Bhonde, Ramesh; Teat, Simon; Triantafillou, Evangelia; Sinn, Ekkehard

    1999-01-01

    Testosterone acetate thiosemicarbazone (TATSC, 17-β-hydroxyandrost-4-one acetate thiosemicarbazone) was synthesized and characterized by single crystal X-ray structure determination. The copper and platinum complexes of this steroid derivative were synthesized and characterized by spectroscopy and electrochemiatry. The in vitro activity of these compounds against human breast cancer cell line MCF-7 was tested. The highest activity was found for the [Pt(TATSC)Cl1] followed by [Cu(TATSC)Cl2] and the ligand in compariosn with cisplatin. PMID:18472909

  17. Antimony film sensor for sensitive rare earth metal analysis in environmental samples.

    PubMed

    Makombe, Martin; van der Horst, Charlton; Silwana, Bongiwe; Iwuoha, Emmanuel; Somerset, Vernon

    2016-07-01

    A sensor for the adsorptive stripping voltammetric determination of rare earth elements has been developed. The electrochemical procedure is based on the oxidation of the rare earth elements complexed with alizarin complexone at a glassy carbon electrode that was in situ modified with an antimony film, during an anodic scan from -0.2 V to 1.1 V (vs. Ag/AgCl) and deposition potential of -0.1 V (vs. Ag/AgCl). The factors influencing the adsorptive stripping capability were optimised, including the complexing agent concentration, plating concentration of antimony and deposition time. The detection of rare earth elements (La, Ce and Pr) were realised in 0.08 M sodium acetate (pH = 5.8) solution as supporting electrolyte, with 2 × 10(-6) M alizarin complexone and 1.0 mg L(-1) antimony solution. Under the optimised conditions, a deposition time of 360 s was obtained and a linear response was observed between 1 and 25 µg L(-1). The reproducibility of the voltammetric measurements was found to be within 5.0% RSD for 12 replicate measurements of cerium(III) concentration of 5 µg L(-1) using the same electrode surface. The detection limits obtained using stripping analysis was 0.06, 0.42 and 0.71 μg L(-1) for Ce(III), La(III) and Pr(III), respectively. The developed sensor has been successfully applied for the determination of cerium, lanthanum and praseodymium in municipal tap water samples. PMID:27065049

  18. Silver and Nitrate Oppositely Modulate Antimony Susceptibility through Aquaglyceroporin 1 in Leishmania (Viannia) Species.

    PubMed

    Andrade, Juvana M; Baba, Elio H; Machado-de-Avila, Ricardo A; Chavez-Olortegui, Carlos; Demicheli, Cynthia P; Frézard, Frédéric; Monte-Neto, Rubens L; Murta, Silvane M F

    2016-08-01

    Antimony (Sb) resistance in leishmaniasis chemotherapy has become one of the major challenges to the control of this spreading worldwide public health problem. Since the plasma membrane pore-forming protein aquaglyceroporin 1 (AQP1) is the major route of Sb uptake in Leishmania, functional studies are relevant to characterize drug transport pathways in the parasite. We generated AQP1-overexpressing Leishmania guyanensis and L. braziliensis mutants and investigated their susceptibility to the trivalent form of Sb (Sb(III)) in the presence of silver and nitrate salts. Both AQP1-overexpressing lines presented 3- to 4-fold increased AQP1 expression levels compared with those of their untransfected counterparts, leading to an increased Sb(III) susceptibility of about 2-fold. Competition assays using silver nitrate, silver sulfadiazine, or silver acetate prior to Sb(III) exposure increased parasite growth, especially in AQP1-overexpressing mutants. Surprisingly, Sb(III)-sodium nitrate or Sb(III)-potassium nitrate combinations showed significantly enhanced antileishmanial activities compared to those of Sb(III) alone, especially against AQP1-overexpressing mutants, suggesting a putative nitrate-dependent modulation of AQP1 activity. The intracellular level of antimony quantified by graphite furnace atomic absorption spectrometry showed that the concomitant exposure to Sb(III) and nitrate favors antimony accumulation in the parasite, increasing the toxicity of the drug and culminating with parasite death. This is the first report showing evidence of AQP1-mediated Sb(III) susceptibility modulation by silver in Leishmania and suggests the potential antileishmanial activity of the combination of nitrate salts and Sb(III). PMID:27161624

  19. The LABCG2 Transporter from the Protozoan Parasite Leishmania Is Involved in Antimony Resistance.

    PubMed

    Perea, Ana; Manzano, José Ignacio; Castanys, Santiago; Gamarro, Francisco

    2016-06-01

    Treatment for leishmaniasis, which is caused by Leishmania protozoan parasites, currently relies on a reduced arsenal of drugs. However, the significant increase in the incidence of drug therapeutic failure and the growing resistance to first-line drugs like antimonials in some areas of Northern India and Nepal limit the control of this parasitic disease. Understanding the molecular mechanisms of resistance in Leishmania is now a matter of urgency to optimize drugs used and to identify novel drug targets to block or reverse resistant mechanisms. Some members of the family of ATP-binding cassette (ABC) transporters in Leishmania have been associated with drug resistance. In this study, we have focused our interest to characterize LABCG2's involvement in drug resistance in Leishmania. Leishmania major parasites overexpressing the ABC protein transporter LABCG2 were generated in order to assess how LABCG2 is involved in drug resistance. Assays of susceptibility to different leishmanicidal agents were carried out. Analysis of the drug resistance profile revealed that Leishmania parasites overexpressing LABCG2 were resistant to antimony, as they demonstrated a reduced accumulation of Sb(III) due to an increase in drug efflux. Additionally, LABCG2 was able to transport thiols in the presence of Sb(III) Biotinylation assays using parasites expressing LABCG2 fused with an N-terminal green fluorescent protein tag revealed that LABCG2 is partially localized in the plasma membrane; this supports data from previous studies which suggested that LABCG2 is localized in intracellular vesicles that fuse with the plasma membrane during exocytosis. In conclusion, Leishmania LABCG2 probably confers antimony resistance by sequestering metal-thiol conjugates within vesicles and through further exocytosis by means of the parasite's flagellar pocket. PMID:27021316

  20. Lithium-antimony-lead liquid metal battery for grid-level energy storage

    NASA Astrophysics Data System (ADS)

    Wang, Kangli; Jiang, Kai; Chung, Brice; Ouchi, Takanari; Burke, Paul J.; Boysen, Dane A.; Bradwell, David J.; Kim, Hojong; Muecke, Ulrich; Sadoway, Donald R.

    2014-10-01

    The ability to store energy on the electric grid would greatly improve its efficiency and reliability while enabling the integration of intermittent renewable energy technologies (such as wind and solar) into baseload supply. Batteries have long been considered strong candidate solutions owing to their small spatial footprint, mechanical simplicity and flexibility in siting. However, the barrier to widespread adoption of batteries is their high cost. Here we describe a lithium-antimony-lead liquid metal battery that potentially meets the performance specifications for stationary energy storage applications. This Li||Sb-Pb battery comprises a liquid lithium negative electrode, a molten salt electrolyte, and a liquid antimony-lead alloy positive electrode, which self-segregate by density into three distinct layers owing to the immiscibility of the contiguous salt and metal phases. The all-liquid construction confers the advantages of higher current density, longer cycle life and simpler manufacturing of large-scale storage systems (because no membranes or separators are involved) relative to those of conventional batteries. At charge-discharge current densities of 275 milliamperes per square centimetre, the cells cycled at 450 degrees Celsius with 98 per cent Coulombic efficiency and 73 per cent round-trip energy efficiency. To provide evidence of their high power capability, the cells were discharged and charged at current densities as high as 1,000 milliamperes per square centimetre. Measured capacity loss after operation for 1,800 hours (more than 450 charge-discharge cycles at 100 per cent depth of discharge) projects retention of over 85 per cent of initial capacity after ten years of daily cycling. Our results demonstrate that alloying a high-melting-point, high-voltage metal (antimony) with a low-melting-point, low-cost metal (lead) advantageously decreases the operating temperature while maintaining a high cell voltage. Apart from the fact that this finding

  1. Self-assembled flower-like antimony trioxide microstructures with high infrared reflectance performance

    SciTech Connect

    Ge, Shengsong; Yang, Xiaokun; Shao, Qian; Liu, Qingyun; Wang, Tiejun; Wang, Lingyun; Wang, Xiaojie

    2013-04-15

    A simple hydrothermal process was adopted to self-assembly prepare high infrared reflective antimony trioxide with three-dimensional flower-like microstructures. The morphologies of antimony trioxide microstructures were characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and high resolution transmission electron microscopy (HRTEM) respectively. It is also found that experimental parameters, such as NaOH concentration, surfactant concentration and volume ratio of ethanol–water played crucial roles in controlling the morphologies of Sb{sub 2}O{sub 3} microstructures. A possible growth mechanism of flower-like Sb{sub 2}O{sub 3} microstructure was proposed based on the experimental data. UV–vis–NIR spectra verified that the near infrared reflectivity of the obtained flower-like microstructures could averagely achieve as 92% with maximum reflectivity of 98%, obviously higher than that of other different morphologies of antimony trioxide microstructures. It is expected that the flower-like Sb{sub 2}O{sub 3} nanostructures have some applications in optical materials and heat insulation coatings. - Graphical abstract: Flower-like Sb{sub 2}O{sub 3} microstructures that composed of nanosheets with thickness of ca. 100 nm exhibit high reflectivity under UV–vis–NIR spectra. Highlights: ► Uniform flower-like microstructures were synthesized via simple hydrothermal reaction. ► The flower-like Sb{sub 2}O{sub 3} microstructures exhibited higher reflectivity than other morphologies under the UV–vis–NIR light. ► Influencing parameters on the Sb{sub 2}O{sub 3} morphologies have been discussed in detail. ► Possible mechanism leading to flower-like microstructures was proposed.

  2. Role of Efflux Pumps and Intracellular Thiols in Natural Antimony Resistant Isolates of Leishmania donovani

    PubMed Central

    Rai, Smita; Bhaskar; Goel, Sudhir K.; Nath Dwivedi, Upendra; Sundar, Shyam; Goyal, Neena

    2013-01-01

    Background In view of the recent upsurge in the phenomenon of therapeutic failure, drug resistance in Leishmania, developed under natural field conditions, has become a great concern yet little understood. Accordingly, the study of determinants of antimony resistance is urgently warranted. Efflux transporters have been reported in Leishmania but their role in clinical resistance is still unknown. The present study was designed to elucidate the mechanism of natural antimony resistance in L. donovani field isolates by analyzing the functionality of efflux pump(s) and expression profiles of known genes involved in transport and thiol based redox metabolism Methodology/Principal Findings We selected 7 clinical isolates (2 sensitive and 5 resistant) in addition to laboratory sensitive reference and SbIII resistant mutant strains for the present study. Functional characterization using flow cytometry identified efflux pumps that transported substrates of both P-gp and MRPA and were inhibited by the calmodulin antagonist trifluoperazine. For the first time, verapamil sensitive efflux pumps for rhodamine 123 were observed in L. donovani that were differentially active in resistant isolates. RT-PCR confirmed the over-expression of MRPA in isolates with high resistance index only. Resistant isolates also exhibited consistent down regulation of AQP1 and elevated intracellular thiol levels which were accompanied with increased expression of ODC and TR genes. Interestingly, γ-GCS is not implicated in clinical resistance in L. donovani isolates. Conclusions/Significance Here we demonstrate for the first time, the role of P-gp type plasma membrane efflux transporter(s) in antimony resistance in L. donovani field isolates. Further, decreased levels of AQP1 and elevated thiols levels have emerged as biomarkers for clinical resistance. PMID:24069359

  3. Experimental and theoretical characterization of cationic, neutral, and anionic binary arsenic and antimony azide species.

    PubMed

    Karaghiosoff, Konstantin; Klapötke, Thomas M; Krumm, Burkhard; Nöth, Heinrich; Schütt, Thomas; Suter, Max

    2002-01-28

    Cationic, neutral, and anionic arsenic and antimony halides formed binary arsenic and antimony azide species M(N(3))(4)(+), M(N(3))(4)(-), and M(N(3))(6)(-) (M = As, Sb) upon reaction with trimethylsilyl azide or sodium azide. The compounds were obtained as pure substances or salts, and their identity was established by vibrational spectroscopy and multinuclear NMR spectroscopy and partially by elemental analysis. Attempts to synthesize pentaazides, M(N(3))(5) (M = As, Sb), failed due to spontaneous decomposition of the compounds. Density functional theory (B3LYP) was applied to calculate structural and vibrational data. Vibrational assignments of the normal modes for the isolated azide compounds were made on the basis of their vibrational spectra in comparison with computational results. The molecular structures and vibrational spectra of the arsenic and antimony pentaazides have been investigated theoretically. These calculations (B3LYP) show minima structures (NIMAG = 0) for all reported compounds. It is shown that the M(N(3))(4)(+) (M = As, Sb) cations exhibit ideal S(4) symmetry and the M(N(3))(6)(-) anions (M = As, Sb) ideal S(6) symmetry. The structure of the hexaazidoarsenate(V) has been determined by X-ray diffraction as its pyridinium salt. [py-H][As(N(3))(6)] crystallizes in the triclinic space group P with a = 6.8484(7), b = 7.3957(8), and c = 8.0903(8) A, alpha = 91.017(2), beta = 113.235(2), and gamma = 91.732(2) degrees, V = 376.29(7) A(3), and Z = 1. The structure of the As(N(3))(6)(-) anion exhibits only S(2) symmetry but shows approximately S(6) symmetry. The calculated and experimentally observed structure as well as the calculated and observed IR and Raman frequencies for all azide species (except M(N(3))(5)) are in reasonable agreement. PMID:11800605

  4. Synthesis, characterization and biological studies of new antimony(III) halide complexes with ω-thiocaprolactam.

    PubMed

    Ozturk, Ibrahim I; Banti, Christina N; Manos, Manos J; Tasiopoulos, Anastasios J; Kourkoumelis, Nikolaos; Charalabopoulos, Konstantinos; Hadjikakou, Sotiris K

    2012-04-01

    Three new antimony(III) halide complexes (SbX(3), X=Cl, Br and I) with the heterocyclic thione ω-thiocaprolactam (1-azacycloheptane-2-thione, (Hthcl)) of formulae {[SbCl(2)(μ(2)-Cl)(Hthcl)(2)](n)} (1), {[(SbBr(2)(μ(2)-Br)(Hthcl)(2))(2)]} (2) and {[(SbI(2)(μ(2)-I)(Hthcl)(2))(2)]} (3) were synthesized from the reaction of antimony(III) halides with ω-thiocaprolactam in 1:2 stoichiometry. The complexes were characterized by elemental analysis, FT-IR spectroscopy, (1)H, (13)C NMR spectroscopy and Thermal Gravimetry-Differential Thermal Analysis (TG-DTA). Crystal structures of the ligand ω-thiocaprolactam and its complexes 1-3 were determined with single crystal X-ray diffraction analysis. Complexes 1-3 and ω-thiocaprolactam were evaluated for their in vitro cytotoxic activity against leiomyosarcoma (LMS) and human breast adenocarcinoma (MCF-7) tumor cell lines. Antimony complexes 1-3 exhibit strong antiproliferative activity against both cell lines tested. The higher such activity was found for 3 with IC(50) values of 0.12±0.04 μM (LMS) and 0.76±0.16 μM (MCF-7) which are 60 and 10 times respectively, stronger than that of cisplatin. The influence of these complexes 1-3 and ω-thiocaprolactam upon the catalytic peroxidation of linoleic acid to hyperoxolinoleic acid by the enzyme lipoxygenase (LOX) was kinetically and theoretically studied. The results were shown negligible inhibitory activity of 1-3 against LOX. PMID:22377717

  5. Temperature dependent electrical resistivity of gallium and antimony in a liquid form

    NASA Astrophysics Data System (ADS)

    Prajapati, A. V.; Sonvane, Y. A.; Thakor, P. B.

    2016-05-01

    Present paper deals with the effects of temperature variation on the electrical resistivity (Ω) of liquid Gallium (Ga), and Antimony (Sb). We have used a new parameter free pseudopotential with a Zeeman formula for finding it. To see the effects of screening Farid et al local field correction function is used with the Charged Hard Sphere (CHS) reference system. Analysis and comparison between the plotted graphs, based on present computed data and other experimental data defines and conclude that our newly constructed model potential is an effective one to produce the data for the temperature dependent electrical resistivity of some liquid semiconductors.

  6. Pharmacokinetics of experimental pentavalent antimony after intramuscular administration in adult volunteers*

    PubMed Central

    Vásquez, Laura; Scorza Dagert, José V.; Scorza, José V.; Vicuña-Fernández, Nelson; de Peña, Yaneira Petit; López, Sabrina; Bendezú, Herminia; Rojas, Elina; Vásquez, Libia; Pérez, Belén

    2006-01-01

    Background: Pentavalent antimony (SbV) has demonstrated therapeuticeffectiveness against clinical manifestations of leishmaniasis, an infection caused by Leishmania, a genus of flagellate protozoa comprising parasites of worldwide distribution. Approximately 1.8 million new cases are reported annually. Objective: The aim of this study was to assess the pharmacokinetics of the investigational generic SbV, Ulamina (pentachloride of antimony + N-methylglucamine), in healthy adult volunteers. Methods: In this study, SbV was administered IM as a single 5-mg/kg dose.Blood samples were collected at 0.25, 0.75, 1, 2, 4, 8, 12, and 24 hours after administration; urine samples were collected at 6-hour intervals during the 24-hour postadministration period. Determination of trivalent antimony, SbV, and total antimony concentrations in blood and urine samples was carried out using atomic absorption spectrometry. Clinical history was reviewed and the subjects were monitored before and after administration of SbV using physical examination, weight, and hepatic- and renal-function studies. The pharmacokinetic parameters calculated were Cmax, Tmax, absorption constant (Ka), elimination constant (Kel), AUC2–24h, AUC0-∞, elimination phase (t½β), volume of distribution (Vd), and urinary excretion rate. Results: Five subjects (3 men, 2 women; mean age, 28 years [range, 18–34 years]) were included in the study. One hour after drug administration the following values were obtained: Cmax, 1.1 μg/mL; Tmax, 1.3 hours; Ka, 1.87 hours; Kel, 0.043 hours; AUC0–24h, 12.26 μg/mL · h; AUC0-∞, 19.84 μg/mL · h; t½β, 17.45 hours; Vd, 6.6 L/kg; and urinary excretion rate, 2.8 μg/h; these were mean values for the entire study group. The single dose was well tolerated by all subjects. Conclusions: The investigational generic SbV, Ulamina, was associated with linearelimination after IM administration of a single 5-mg/kg dose. A 2-compartment pharmacokinetic model was observed in

  7. Stable antimony compositions for the passivation of metal contaminated cracking catalysts

    SciTech Connect

    Johnson, M.M.; Tabler, D.C.

    1990-06-12

    This patent describes a stable aqueous metals passivating agent. It comprises: about 10 to about 97 weight percent water, about 1 to about 50 weight percent particulate antimony oxide, and a stabilizing amount of vinyl copolymer in the range of about 0.2 to about 3 weight percent. The weight percentages are based on the total weight of the aqueous metals passivating agent and the vinyl copolymer being the ammonium alt prepared by adding ammonium hydroxide to the hydrolyzed acid form of a poly(methylvinyl ether/maleic anhydride) consisting essentially of repeating units of the formula.

  8. Electromagnetic absorption and shielding behavior of polyaniline-antimony oxide composites

    NASA Astrophysics Data System (ADS)

    Faisal, Muhammad; Khasim, Syed

    2013-02-01

    This work highlights the microwave absorption and electromagnetic interference (EMI) shielding properties of synthesized polyaniline (PAni)-antimony oxide (Sb2O3) composites in the 8-12 GHz (X-band) range. These composites showed absorption dominated EMI shielding effectiveness (EMI SEA) of -34 to -40 dB (> 99 % attenuation), indicating their shielding potential throughout the X-band. Our analyses reveal that the Sb2O3 particles in PAni matrix have key impact in determining the microwave absorption properties of the composites.

  9. Geochemical background of antimony and thallium and its possible relation to soil properties

    NASA Astrophysics Data System (ADS)

    Pérez-Sirvent, C.; Martínez-Sánchez, M. J.; Molina, J.; García-Lorenzo, M. L.; Hernandez-Cordoba, M.

    2009-04-01

    Background value for trace elements in soils can act as a true reference level for estimating the extent of soil pollution with these elements. Background value is highly dependent on the mineralogical composition of the parent material and on the weathering processes that have led to the formation of the soil clay, and organic matter content. In recent years, environmental geochemical mapping has assumed an increasing relevance. Geochemical maps are of great interest because they constitute an effective tool for environmental planning, and for promoting sustainable development. This explains why, in recent years, many governments have promoted research to define geochemical background and baseline levels to serve as a basis for legislation to diagnose, prevent and reduce soil contamination. The objective of this study was to determine the selenium background and baseline values in agricultural soils or abandoned agricultural soils with natural vegetation not subjected to particular point contamination sources, in the Region of Murcia (SE, Spain). Moreover, the purpose of this paper was to study the possible relationship between soil properties, mineralogical composition and selenium content in soil samples. This work seeks to establish the geochemical background for thallium and antimony in the province of Murcia. The possible relationship between soil properties and target metals concentration has been studied. In the present study, background concentrations were established by analysing a large number of samples soils considered unaffected, or at least minimally affected, by human activities. Samples were analysed for antimony content by atomic fluorescence spectrometry (AFS) and by inductively coupled plasma spectrometry (ICP-MS) for thallium content. Other soil characteristics such as electrical conductivity (EC), organic matter (OM), pH, soluble salts, granulometry and calcium carbonate content were also measured to determine their influence on trace element

  10. Facile catalyst-free straightforward thermal evaporation of ultra-long antimony oxide microwires: Synthesis and characterization

    NASA Astrophysics Data System (ADS)

    Qurashi, Ahsanulhaq

    2015-05-01

    Antimony oxide microwires (MWs) were grown on Si/SiO2 substrate by proficient non-catalytic economically promising method based on ambient heating of metallic source materials in crucible in a facile conventional muffle furnace. The produced antimony oxide microwires were 200-300 nm in diameter and tens micron in length. These ultra-long microwires were characterized by FESEM, TEM, XRD and Raman analysis. This approach is useful to develop grams quantities of microwires on Si/SiO2 substrate.

  11. Supramolecular interactions in biologically relevant compounds. 2-Pyrazineformamide thiosemicarbazones and some products of their cyclization

    NASA Astrophysics Data System (ADS)

    Castiñeiras, Alfonso; García-Santos, Isabel; Nogueiras, Silvia; Rodríguez-González, Iria; Rodríguez-Riobó, Raúl

    2014-09-01

    Reaction of 2-cyanopyrazine with thiosemicarbazide or N-methylthiosemicarbazide afforded the (Z)-2-(amino(pyrazin-2-yl)methylene)hydrazinecarbothioamide (HPzAm4DH) and (Z)-2-(amino(pyrazin-2-yl)methylene)-N-methylhydrazine carbothioamide (HPzAm4M), respectively. (2Z,N‧E)-N‧-(4-Oxothiazolidin-2-ylidene)pyrazine-2-carbohydrazonamide (HPzAmot, 5) and (2Z,N‧E)-N‧-(3-methyl-4-oxothiazolidin-2-ylidene)pyrazine-2-carbohydrazonamide (MPzAmot, 7) have been synthesized from these thiosemicarbazones with chloroacetic or bromoacetic acids, using a conventional synthetic methodology and microwave-assisted organic reaction enhancement. The crystal structures of the thiosemicarbazones and their solvates [HPzAm4DHṡ1/2 MeOH (1), HPzAm4DHṡH2O (2), HPzAm4M (3), HPzAm4Mṡ2H2O (4)] and the 1,3-thiazolidin-4-ones (5 and 7) have been studied by X-ray diffractometry. All of the compounds were characterized by elemental analysis, mass spectrometry, FT-IR and 1H and 13C NMR spectroscopy. Several by-products have also been isolated in a crystalline form, namely 3-((Z,E)-N‧-(4-oxothiazolidin-2-ylidene)carbamohydrazonium-yl)pyrazin-1-ium dibromide monohydrate, (H3PzAmot)Br2ṡH2O (6), 2-((5-(pyrazin-2-yl)-1H-1,2,4-triazol-3-yl)thio)acetic acid, (H2Pz124ttAc) (8), 2-amino-5-(pyrazin-2-yl)-1,3,4-thiadiazol-3-ium chloride monohydrate, (HPz134tda)ClṡH2O (9), and 2-(methylamino)-5-(pyrazin-2-yl)-1,3,4-thiadiazol-3-ium chloride N-methyl-5-(pyrazin-2-yl)-1,3,4-thiadiazol-2-amine solvate, (HMPz134tda)Clṡ(MPz134tda) (10). The structures of these compounds were also analyzed by X-ray diffractometry. The microwave-assisted organic reaction method for synthesis is easy, convenient, and ecofriendly when compared to the traditional synthetic methods. Crystal analysis revealed that the compounds have extended 3D supramolecular networks through high levels of H-bonding and weak molecular interactions between the molecular moieties and solvent molecules. The novel synthons, which are

  12. Preparation of superconductor precursor powders

    DOEpatents

    Bhattacharya, R.

    1998-08-04

    A process for the preparation of a precursor metallic powder composition for use in the subsequent formation of a superconductor. The process comprises the steps of providing an electrodeposition bath comprising an electrolyte medium and a cathode substrate electrode, and providing to the bath one or more soluble salts of one or more respective metals which are capable of exhibiting superconductor properties upon subsequent appropriate treatment. The bath is continually energized to cause the metallic and/or reduced particles formed at the electrode to drop as a powder from the electrode into the bath, and this powder, which is a precursor powder for superconductor production, is recovered from the bath for subsequent treatment. The process permits direct inclusion of all metals in the preparation of the precursor powder, and yields an amorphous product mixed on an atomic scale to thereby impart inherent high reactivity. Superconductors which can be formed from the precursor powder include pellet and powder-in-tube products. 7 figs.

  13. Preparation of superconductor precursor powders

    DOEpatents

    Bhattacharya, Raghunath; Blaugher, Richard D.

    1995-01-01

    A process for the preparation of a precursor metallic powder composition for use in the subsequent formation of a superconductor. The process comprises the steps of providing an electrodeposition bath comprising an electrolyte medium and a cathode substrate electrode, and providing to the bath one or more soluble salts of one or more respective metals, such as nitrate salts of thallium, barium, calcium, and copper, which are capable of exhibiting superconductor properties upon subsequent appropriate treatment. The bath is continually energized to cause the metallic particles formed at the electrode to drop as a powder from the electrode into the bath, and this powder, which is a precursor powder for superconductor production, is recovered from the bath for subsequent treatment. The process permits direct inclusion of thallium in the preparation of the precursor powder, and yields an amorphous product mixed on an atomic scale to thereby impart inherent high reactivity. Superconductors which can be formed from the precursor powder include pellet and powder-in-tube products.

  14. Binuclear ruthenium(III) bis(thiosemicarbazone) complexes: synthesis, spectral, electrochemical studies and catalytic oxidation of alcohol.

    PubMed

    Mohamed Subarkhan, M; Ramesh, R

    2015-03-01

    A new series of binuclear ruthenium(III) thiosemicarbazone complexes of general formula [(EPh3)2(X)2Ru-L-Ru(X)2(EPh3)2] (where E=P or As; X=Cl or Br; L=NS chelating bis(thiosemicarbazone ligands) has been synthesized and characterized by analytical and spectral (FT-IR, UV-Vis and EPR). IR spectra show that the thiosemicarbazones behave as monoanionic bidentate ligands coordinating through the azomethine nitrogen and thiolate sulphur. The electronic spectra of the complexes indicate that the presence of d-d and intense LMCT transitions in the visible region. The complexes are paramagnetic (low spin d(5)) in nature and all the complexes show rhombic distortion around the ruthenium ion with three different 'g' values (gx≠gy≠gz) at 77K. All the complexes are redox active and exhibit an irreversible metal centered redox processes (Ru(III)-Ru(III)/Ru(IV)-Ru(IV); Ru(III)-Ru(III)/Ru(II)-Ru(II)) within the potential range of 0.38-0.86V and -0.39 to -0.66 V respectively, versus Ag/AgCl. Further, the catalytic efficiency of one of the complexes [Ru2Cl2(AsPh3)4(L1)] (4) has been investigated in the case of oxidation of primary and secondary alcohols into their corresponding aldehydes and ketones in the presence of N-methylmorpholine-N-oxide(NMO) as co-oxidant. The formation of high valent Ru(V)O species is proposed as catalytic intermediate for the catalytic cycle. PMID:25498823

  15. Binuclear ruthenium(III) bis(thiosemicarbazone) complexes: Synthesis, spectral, electrochemical studies and catalytic oxidation of alcohol

    NASA Astrophysics Data System (ADS)

    Mohamed Subarkhan, M.; Ramesh, R.

    2015-03-01

    A new series of binuclear ruthenium(III) thiosemicarbazone complexes of general formula [(EPh3)2(X)2Ru-L-Ru(X)2(EPh3)2] (where E = P or As; X = Cl or Br; L = NS chelating bis(thiosemicarbazone ligands) has been synthesized and characterized by analytical and spectral (FT-IR, UV-Vis and EPR). IR spectra show that the thiosemicarbazones behave as monoanionic bidentate ligands coordinating through the azomethine nitrogen and thiolate sulphur. The electronic spectra of the complexes indicate that the presence of d-d and intense LMCT transitions in the visible region. The complexes are paramagnetic (low spin d5) in nature and all the complexes show rhombic distortion around the ruthenium ion with three different 'g' values (gx ≠ gy ≠ gz) at 77 K. All the complexes are redox active and exhibit an irreversible metal centered redox processes (RuIII-RuIII/RuIV-RuIV; RuIII-RuIII/RuII-RuII) within the potential range of 0.38-0.86 V and -0.39 to -0.66 V respectively, versus Ag/AgCl. Further, the catalytic efficiency of one of the complexes [Ru2Cl2(AsPh3)4(L1)] (4) has been investigated in the case of oxidation of primary and secondary alcohols into their corresponding aldehydes and ketones in the presence of N-methylmorpholine-N-oxide(NMO) as co-oxidant. The formation of high valent RuVdbnd O species is proposed as catalytic intermediate for the catalytic cycle.

  16. The binding of β-d-glucopyranosyl-thiosemicarbazone derivatives to glycogen phosphorylase: A new class of inhibitors.

    PubMed

    Alexacou, Kyra-Melinda; Tenchiu Deleanu, Alia-Cristina; Chrysina, Evangelia D; Charavgi, Maria-Despoina; Kostas, Ioannis D; Zographos, Spyros E; Oikonomakos, Nikos G; Leonidas, Demetres D

    2010-11-15

    Glycogen phosphorylase (GP) is a promising target for the treatment of type 2 diabetes. In the process of structure based drug design for GP, a group of 15 aromatic aldehyde 4-(β-d-glucopyranosyl)thiosemicarbazones have been synthesized and evaluated as inhibitors of rabbit muscle glycogen phosphorylase b (GPb) by kinetic studies. These compounds are competitive inhibitors of GPb with respect to α-d-glucose-1-phosphate with IC(50) values ranging from 5.7 to 524.3μM. In order to elucidate the structural basis of their inhibition, the crystal structures of these compounds in complex with GPb at 1.95-2.23Å resolution were determined. The complex structures reveal that the inhibitors are accommodated at the catalytic site with the glucopyranosyl moiety at approximately the same position as α-d-glucose and stabilize the T conformation of the 280s loop. The thiosemicarbazone part of the studied glucosyl thiosemicarbazones possess a moiety derived from substituted benzaldehydes with NO(2), F, Cl, Br, OH, OMe, CF(3), or Me at the ortho-, meta- or para-position of the aromatic ring as well as a moiety derived from 4-pyridinecarboxaldehyde. These fit tightly into the β-pocket, a side channel from the catalytic site with no access to the bulk solvent. The differences in their inhibitory potency can be interpreted in terms of variations in the interactions of the aldehyde-derived moiety with protein residues in the β-pocket. In addition, 14 out of the 15 studied inhibitors were found bound at the new allosteric site of the enzyme. PMID:20947361

  17. Spectroscopic analysis, AIM, NLO and VCD investigations of acetaldehyde thiosemicarbazone using quantum mechanical simulations

    NASA Astrophysics Data System (ADS)

    Moorthy, N.; Prabakar, P. C. Jobe; Ramalingam, S.; Govindarajan, M.; Gnanamuthu, S. Joshua; Pandian, G. V.

    2016-08-01

    The prepared Acetaldehyde thiosemicarbazone (ATSC) have been investigated by both the experimental and theoretical methods; through this work, the essentiality of elucidation of molecular fragments source linear and non-linear optical properties was explored. The stability of the structure and entire calculations have been performed on HF and B3LYP methods with 6-311++G(d,p) level of basis set. The Mulliken charge profile, electronic, optical and hyper polarizability analyses have been carried out in order to evaluate nonlinear optical (NLO) performance of the present compound. The exact optical location of the ATSC was determined by executing UV-Visible calculations on TDSCF method. The existence of the molecular group for the inducement and tuning of NLO properties were thoroughly investigated by performing fundamental vibrational investigation. The optical energy transformation among frontier molecular levels has been described in UV-Visible region. The Gibbs energy coefficient of thermodynamic functions was monitored in different temperature and it was found constant irrespective of temperatures. The appearance of different chemical environment of H and C was monitored from the 1H and 13C NMR spectra. The vibrational optical polarization characteristics with respect to molecular composition in the compound have been studied by VCD spectrum. The bond critical point, Laplacian of electron density, electron kinetic energy density and total electron energy density have calculated and analysed using AIM study.

  18. Identification of Semicarbazones, Thiosemicarbazones and Triazine Nitriles as Inhibitors of Leishmania mexicana Cysteine Protease CPB

    PubMed Central

    Schröder, Jörg; Noack, Sandra; Marhöfer, Richard J.; Mottram, Jeremy C.; Coombs, Graham H.; Selzer, Paul M.

    2013-01-01

    Cysteine proteases of the papain superfamily are present in nearly all eukaryotes. They play pivotal roles in the biology of parasites and inhibition of cysteine proteases is emerging as an important strategy to combat parasitic diseases such as sleeping sickness, Chagas’ disease and leishmaniasis. Homology modeling of the mature Leishmania mexicana cysteine protease CPB2.8 suggested that it differs significantly from bovine cathepsin B and thus could be a good drug target. High throughput screening of a compound library against this enzyme and bovine cathepsin B in a counter assay identified four novel inhibitors, containing the warhead-types semicarbazone, thiosemicarbazone and triazine nitrile, that can be used as leads for antiparasite drug design. Covalent docking experiments confirmed the SARs of these lead compounds in an effort to understand the structural elements required for specific inhibition of CPB2.8. This study has provided starting points for the design of selective and highly potent inhibitors of L. mexicana cysteine protease CPB that may also have useful efficacy against other important cysteine proteases. PMID:24146999

  19. Study on the Interaction between Isatin-β-Thiosemicarbazone and Calf Thymus DNA by Spectroscopic Techniques.

    PubMed

    Pakravan, Parvaneh; Masoudian, Shahla

    2015-01-01

    The interaction between isatin-β-thiosemicarbazone (IBT) and calf thymus DNA (CT-DNA) was investigated in physiological buffer (pH 7.4) using Neutral Red (NR) dye as a spectral probe by UV-Vis absorption and fluorescence spectroscopy, as well as viscosity measurements. The IBT is stabilized by intercalation in the DNA (K [IBT -DNA] = 1.03×10(5) M(-1)), and displaces the NR dye from the NR-DNA complex. The binding constants Kf and number of binding sites (n≈1) of IBT with DNA were obtained by fluorescence quenching method at different temperatures. Furthermore, the enthalpy and entropy of the reaction between IBT and CT-DNA showed that the reaction is enthalpy-favored and entropy-disfavored. The changes in the base stacking of CT-DNA upon the binding of IBT are reflected in the circular dichroic (CD) spectral studies. The viscosity increase of CT-DNA solution is another evidence to indicate that, IBT is able to be intercalated in the DNA base pairs. PMID:25561917

  20. Crystal structures of crotonaldehyde semicarbazone and crotonaldehyde thiosemicarbazone from X-ray powder diffraction data.

    PubMed

    Arfan, Atef; Rukiah, Mwaffak

    2015-02-01

    Crotonaldehyde semicarbazone {systematic name: (E)-2-[(E)-but-2-en-1-yl-idene]hydrazinecarboxamide}, C5H9N3O, (I), and crotonaldehyde thio-semi-carba-zone {systematic name: (E)-2-[(E)-but-2-en-1-yldene]hydra-zinecarbo--thio-amide}, C5H9N3S, (II), show the same E conformation around the imine C=N bond. Compounds (I) and (II) were obtained by the condensation of crotonaldehyde with semicarbazide hydro-chloride and thio-semicarbazide, respectively. Each mol-ecule has an intra-molecular N-H⋯N hydrogen bond, which generates an S(5) ring. In (I), the crotonaldehyde fragment is twisted by 2.59 (5)° from the semicarbazide mean plane, while in (II) the corresponding angle (with the thio-semicarbazide mean plane) is 9.12 (5)°. The crystal packing is different in the two compounds: in (I) inter-molecular N-H⋯O hydrogen bonds link the mol-ecules into layers parallel to the bc plane, while weak inter-molecular N-H⋯S hydrogen bonds in (II) link the mol-ecules into chains propagating in [110]. PMID:25878810

  1. Structural, thermal and optical characterization of an organic NLO material—Benzaldehyde thiosemicarbazone monohydrate single crystals

    NASA Astrophysics Data System (ADS)

    Santhakumari, R.; Ramamurthi, K.

    2011-02-01

    Single crystals of the organic NLO material, benzaldehyde thiosemicarbazone (BTSC) monohydrate, were grown by slow evaporation method. Solubility of BTSC monohydrate was determined in ethanol at different temperatures. The grown crystals were characterized by single crystal X-ray diffraction analysis to determine the cell parameters and by FT-IR technique to study the presence of the functional groups. Thermogravimetric and differential thermal analyses reveal the thermal stability of the crystal. UV-vis-NIR spectrum shows excellent transmission in the region of 200-1100 nm. Theoretical calculations were carried out to determine the linear optical constants such as extinction coefficient and refractive index. Further the optical nonlinearities of BTSC have been investigated by Z-scan technique with He-Ne laser radiation of wavelength 632.8 nm. Mechanical properties of the grown crystal were studied using Vickers microhardness tester. Second harmonic generation efficiency of the powdered BTSC monohydrate was tested using Nd:YAG laser and it is found to be ˜5.3 times that of potassium dihydrogen orthophosphate.

  2. 2-Butyl-4-chloroimidazole based substituted piperazine-thiosemicarbazone hybrids as potent inhibitors of Mycobacterium tuberculosis.

    PubMed

    Jallapally, Anvesh; Addla, Dinesh; Yogeeswari, Perumal; Sriram, Dharmarajan; Kantevari, Srinivas

    2014-12-01

    Here a series of 2-butyl-4-chloroimidazole based substituted piperazine-thiosemicarbazone hybrids were designed by combining three different pharmacophoric fragments in single molecular architecture. 2-Butyl-4-chloro-1-(3-(4-substituted)piperazin-1-yl)propyl)-1H-imidazole-5-carbaldehydes (4a-p) prepared by reacting carboxaldehyde 2 with N-alkyl piperazines 3a-p which were condensed with thiosemicarbazine to give desired compounds 5a-p in very good yields. Among all sixteen compounds screened for in vitro antimycobacterial activity against Mycobacterium tuberculosis H37Rv (MTB), two compounds (E)-2-((2-butyl-4-chloro-1-(3-(4-(o-tolyl) piperazin-1-yl)propyl)-1H-imidazol-5-yl)methylene)hydrazinecarbothioamide 5e and (E)-2-((2-butyl-4-chloro-1-(3-(4-(2-methoxyphenyl)piperazin-1-yl)propyl)-1H-imidazol-5-yl)methylene) hydrazine carbothioamide 5f were found to be the most potent antitubercular agents (MIC: 3.13 μg/mL) with low toxicity profile. PMID:25451998

  3. Intracellular reduction/activation of a disulfide switch in thiosemicarbazone iron chelators.

    PubMed

    Akam, Eman A; Chang, Tsuhen M; Astashkin, Andrei V; Tomat, Elisa

    2014-10-01

    Iron scavengers (chelators) offer therapeutic opportunities in anticancer drug design by targeting the increased demand for iron in cancer cells as compared to normal cells. Prochelation approaches are expected to avoid systemic iron depletion as chelators are liberated under specific intracellular conditions. In the strategy described herein, a disulfide linkage is employed as a redox-directed switch within the binding unit of an antiproliferative thiosemicarbazone prochelator, which is activated for iron coordination following reduction to the thiolate chelator. In glutathione redox buffer, this reduction event occurs at physiological concentrations and half-cell potentials. Consistent with concurrent reduction and activation, higher intracellular thiol concentrations increase cell susceptibility to prochelator toxicity in cultured cancer cells. The reduction of the disulfide switch and intracellular iron chelation are confirmed in cell-based assays using calcein as a fluorescent probe for paramagnetic ions. The resulting low-spin Fe(III) complex is identified in intact Jurkat cells by EPR spectroscopy measurements, which also document a decreased concentration of active ribonucleotide reductase following exposure to the prochelator. Cell viability and fluorescence-based assays show that the iron complex presents low cytotoxicity and does not participate in intracellular redox chemistry, indicating that this antiproliferative chelation strategy does not rely on the generation of reactive oxygen species. PMID:25100578

  4. Species Dependence of [64Cu]Cu-Bis(thiosemicarbazone) Radiopharmaceutical Binding to Serum Albumins

    PubMed Central

    Basken, Nathan E.; Mathias, Carla J.; Lipka, Alexander E.; Green, Mark A.

    2008-01-01

    Introduction Interactions of three copper(II) bis(thiosemicarbazone) PET radiopharmaceuticals with human serum albumin, and the serum albumins of four additional mammalian species, were evaluated. Methods 64Cu-labeled diacetyl bis(N4-methylthiosemicarbazonato)copper(II) (Cu-ATSM), pyruvaldehyde bis(N4-methylthiosemicarbazonato)copper(II) (Cu-PTSM), and ethylglyoxal bis(thiosemicarbazonato)copper(II) (Cu-ETS) were synthesized and their binding to human, canine, rat, baboon, and porcine serum albumins quantified by ultrafiltration. Protein binding was also measured for each tracer in human, porcine, rat, and mouse serum. Results The interaction of these neutral, lipophilic copper chelates with serum albumin is highly compound- and species-dependent. Cu-PTSM and Cu-ATSM exhibit particularly high affinity for human serum albumin (HSA), while the albumin binding of Cu-ETS is relatively insensitive to species. At HSA concentrations of 40 mg/mL, “% Free” (non-albumin-bound) levels of radiopharmaceutical were 4.0 ± 0.1%; 5.3 ± 0.2%; and 38.6 ± 0.8% for Cu-PTSM; Cu-ATSM; and Cu-ETS, respectively. Conclusions Species-dependent variations in radiopharmaceutical binding to serum albumin may need to be considered when using animal models to predict the distribution and kinetics of these compounds in humans. PMID:18355683

  5. Synthesis and characterization of some novel antimicrobial thiosemicarbazone O-carboxymethyl chitosan derivatives.

    PubMed

    Mohamed, Nadia A; Mohamed, Riham R; Seoudi, Rania S

    2014-02-01

    Three novel thiosemicarbazone O-carboxymethyl chitosan derivatives were obtained via a condensation reaction of thiosemicarbazide O-carboxymethyl chitosan with o-hydroxybenzaldehyde, p-methoxybenzaldehyde, and p- chlorobenzaldehyde respectively. Their structures were characterized by elemental analysis, FTIR, (13)C NMR and X-ray diffraction. The antimicrobial behaviors of the prepared derivatives against three types of bacteria Staphylococcus aureus (S. aureus, RCMBA 2004), Bacillus subtilis (B. subtilis, RCMBA 6005), and Escherichia coli (E. Coli, RCMBA 5003) and three crops-threatening pathogenic fungi Aspergillus fumigatus (A. fumigatus, RCMBA 06002), Geotrichum candidum (G. candidum, RCMB 05098), and Candida albicans (C. albicans, RCMB 05035) were investigated. The results indicated that the antibacterial and antifungal activities of the investigated derivatives are much higher than those of the parent O-carboxymethyl chitosan. They were more potent in case of Gram-positive bacteria than Gram-negative bacteria. The presence of electron withdrawing chlorine atom on the aryl moiety of the aldehyde portion improved greatly antimicrobial activity to be nearly equivalent to the used standard drugs. PMID:24211430

  6. Synthesis and biological evaluation of new naphthalene substituted thiosemicarbazone derivatives as potent antifungal and anticancer agents.

    PubMed

    Altıntop, Mehlika Dilek; Atlı, Özlem; Ilgın, Sinem; Demirel, Rasime; Özdemir, Ahmet; Kaplancıklı, Zafer Asım

    2016-01-27

    New thiosemicarbazone derivatives (1-10) were obtained via the reaction of 4-(naphthalen-1-yl)thiosemicarbazide with fluoro-substituted aromatic aldehydes. The synthesized compounds were evaluated for their in vitro antifungal effects against pathogenic yeasts and molds using broth microdilution assay. Ames and umuC assays were carried out to determine the genotoxicity of the most effective antifungal derivatives. Furthermore, all compounds were evaluated for their cytotoxic effects on A549 human lung adenocarcinoma and NIH/3T3 mouse embryonic fibroblast cell lines using XTT test. Among these derivatives, 4-(naphthalen-1-yl)-1-(2,3-difluorobenzylidene)thiosemicarbazide (1) and 4-(naphthalen-1-yl)-1-(2,5-difluorobenzylidene)thiosemicarbazide (3) can be identified as the most promising antifungal derivatives due to their notable inhibitory effects on Candida species and no cytotoxicity against NIH/3T3 mouse embryonic fibroblast cell line. According to Ames and umuC assays, compounds 1 and 3 were classified as non-mutagenic compounds. On the other hand, 4-(naphthalen-1-yl)-1-(2,4-difluorobenzylidene)thiosemicarbazide (2) can be considered as the most promising anticancer agent against A549 cell line owing to its notable inhibitory effect on A549 cells with an IC50 value of 31.25 μg/mL when compared with cisplatin (IC50 = 16.28 μg/mL) and no cytotoxicity against NIH/3T3 cells. PMID:26706351

  7. Study on the Interaction between Isatin-β-Thiosemicarbazone and Calf Thymus DNA by Spectroscopic Techniques

    PubMed Central

    Pakravan, Parvaneh; Masoudian, Shahla

    2015-01-01

    The interaction between isatin-β-thiosemicarbazone (IBT) and calf thymus DNA (CT-DNA) was investigated in physiological buffer (pH 7.4) using Neutral Red (NR) dye as a spectral probe by UV–Vis absorption and fluorescence spectroscopy, as well as viscosity measurements. The IBT is stabilized by intercalation in the DNA (K [IBT –DNA] = 1.03×105 M−1), and displaces the NR dye from the NR–DNA complex. The binding constants Kf and number of binding sites (n≈1) of IBT with DNA were obtained by fluorescence quenching method at different temperatures. Furthermore, the enthalpy and entropy of the reaction between IBT and CT-DNA showed that the reaction is enthalpy-favored and entropy-disfavored. The changes in the base stacking of CT-DNA upon the binding of IBT are reflected in the circular dichroic (CD) spectral studies. The viscosity increase of CT-DNA solution is another evidence to indicate that, IBT is able to be intercalated in the DNA base pairs. PMID:25561917

  8. Synthesis, structure and biological activity of nickel(II) complexes of 5-methyl 2-furfural thiosemicarbazone.

    PubMed

    Jouad, E M; Larcher, G; Allain, M; Riou, A; Bouet, G M; Khan, M A; Thanh, X D

    2001-09-01

    5-Methyl 2-furfuraldehyde thiosemicarbazone (M5HFTSC) with nickel(II) leads to three types of complexes: [Ni(M5HFTSC)(2)X(2)], [Ni(M5FTSC)(2)] and [Ni(M5FTSC)(2)] x 2DMF. In the first type the ligand remains in thione form, while in the two other, the anionic thiolato form is involved. The species [Ni(M5HFTSC)(2)X(2)] has been characterized spectroscopically. The structures of [Ni(M5FTSC)(2)] x 2DMF and [Ni(M5FTSC)(2)] have been solved using X-ray diffraction. Biological studies of [Ni(M5HFTSC)(2)Cl(2)] have been carried out in vitro for antifungal activity on human pathogenic fungi, Aspergillus fumigatus and Candida albicans, and in vivo for toxicity on mice. The results are compared to those of the ligand, the metal salt and a similar copper complex [Cu(M5HFTSC)Cl(2)]. PMID:11566328

  9. Structural, thermal and optical characterization of an organic NLO material--benzaldehyde thiosemicarbazone monohydrate single crystals.

    PubMed

    Santhakumari, R; Ramamurthi, K

    2011-02-01

    Single crystals of the organic NLO material, benzaldehyde thiosemicarbazone (BTSC) monohydrate, were grown by slow evaporation method. Solubility of BTSC monohydrate was determined in ethanol at different temperatures. The grown crystals were characterized by single crystal X-ray diffraction analysis to determine the cell parameters and by FT-IR technique to study the presence of the functional groups. Thermogravimetric and differential thermal analyses reveal the thermal stability of the crystal. UV-vis-NIR spectrum shows excellent transmission in the region of 200-1100 nm. Theoretical calculations were carried out to determine the linear optical constants such as extinction coefficient and refractive index. Further the optical nonlinearities of BTSC have been investigated by Z-scan technique with He-Ne laser radiation of wavelength 632.8 nm. Mechanical properties of the grown crystal were studied using Vickers microhardness tester. Second harmonic generation efficiency of the powdered BTSC monohydrate was tested using Nd:YAG laser and it is found to be ∼5.3 times that of potassium dihydrogen orthophosphate. PMID:21186136

  10. β-Cyclodextrin hydrogels for the ocular release of antibacterial thiosemicarbazones.

    PubMed

    Glisoni, Romina J; García-Fernández, María J; Pino, Marylú; Gutkind, Gabriel; Moglioni, Albertina G; Alvarez-Lorenzo, Carmen; Concheiro, Angel; Sosnik, Alejandro

    2013-04-01

    Two types of hydrophilic networks with conjugated beta-cyclodextrin (β-CD) were developed with the aim of engineering useful platforms for the localized release of an antimicrobial 5,6-dimethoxy-1-indanone N4-allyl thiosemicarbazone (TSC) in the eye and its potential application in ophthalmic diseases. Poly(2-hydroxyethyl methacrylate) soft contact lenses (SCLs) displaying β-CD, namely pHEMA-co-β-CD, and super-hydrophilic hydrogels (SHHs) of directly cross-linked hydroxypropyl-β-CD were synthesized and characterized regarding their structure (ATR/FT-IR), drug loading capacity, swelling and in vitro release in artificial lacrimal fluid. Incorporation of TSC to the networks was carried out both during polymerization (DP method) and after synthesis (PP method). The first method led to similar drug loads in all the hydrogels, with minor drug loss during the washing steps to remove unreacted monomers, while the second method evidenced the influence of structural parameters on the loading efficiency (proportion of CD units, mesh size, swelling degree). Both systems provided a controlled TSC release for at least two weeks, TSC concentrations (up to 4000μg/g dry hydrogel) being within an optimal therapeutic window for the antimicrobial ocular treatment. Microbiological tests against P. aeruginosa and S. aureus confirmed the ability of TSC-loaded pHEMA-co-β-CD network to inhibit bacterial growth. PMID:23499082

  11. Synthesis and spectral investigations of Mn(II) complexes of pentadentate bis(thiosemicarbazones)

    NASA Astrophysics Data System (ADS)

    Krishnan, Suja; Laly, K.; Prathapachandra Kurup, M. R.

    2010-02-01

    Five Mn(II) complexes of bis(thiosemicarbazones) which are represented as [Mn(H 2Ac4Ph)Cl 2] ( 1), [Mn(Ac4Ph)H 2O] ( 2), [Mn(H 2Ac4Cy)Cl 2]·H 2O ( 3), [Mn(H 2Ac4Et)Cl 2]·3H 2O ( 4) and [Mn(H 2Ac4Et)(OAc) 2]·3H 2O ( 5) have been synthesized and characterized by elemental analyses, electronic, infrared and EPR spectral techniques. In all the complexes except [Mn(Ac4Ph)H 2O], the ligands act as pentadentate neutral molecules and coordinate to Mn(II) ion through two thione sulfur atoms, two azomethine nitrogens and the pyridine nitrogen, suggesting a heptacoordination. While in compound [Mn(Ac4Ph)H 2O], the dianionic ligand is coordinated to the metal suggesting six coordination in this case. Magnetic studies indicate the high spin state of Mn(II). Conductivity measurements reveal their non-electrolyte nature. EPR studies indicate five g values for [Mn(Ac4Ph)H 2O] showing zero field splitting.

  12. Intracellular reduction/activation of a disulfide switch in thiosemicarbazone iron chelators

    PubMed Central

    Akam, Eman A.; Chang, Tsuhen M.; Astashkin, Andrei V.

    2014-01-01

    Iron scavengers (chelators) offer therapeutic opportunities in anticancer drug design by targeting the increased demand for iron in cancer cells as compared to normal cells. Prochelation approaches are expected to avoid systemic iron depletion as chelators are liberated under specific intracellular conditions. In the strategy described herein, a disulfide linkage is employed as a redox-directed switch within the binding unit of an antiproliferative thiosemicarbazone prochelator, which is activated for iron coordination following reduction to the thiolate chelator. In glutathione redox buffer, this reduction event occurs at physiological concentrations and half-cell potentials. Consistent with concurrent reduction and activation, higher intracellular thiol concentrations increase cell susceptibility to prochelator toxicity in cultured cancer cells. The reduction of the disulfide switch and intracellular iron chelation are confirmed in cell-based assays using calcein as a fluorescent probe for paramagnetic ions. The resulting low-spin Fe(III) complex is identified in intact Jurkat cells by EPR spectroscopy measurements, which also document a decreased concentration of active ribonucleotide reductase following exposure to the prochelator. Cell viability and fluorescence-based assays show that the iron complex presents low cytotoxicity and does not participate in intracellular redox chemistry, indicating that this antiproliferative chelation strategy does not rely on the generation of reactive oxygen species. PMID:25100578

  13. Ruthenium (II) complexes of thiosemicarbazone: synthesis, biosensor applications and evaluation as antimicrobial agents.

    PubMed

    Yildirim, Hatice; Guler, Emine; Yavuz, Murat; Ozturk, Nurdan; Kose Yaman, Pelin; Subasi, Elif; Sahin, Elif; Timur, Suna

    2014-11-01

    A conformationally rigid half-sandwich organoruthenium (II) complex [(η(6)-p-cymene)RuClTSC(N-S)]Cl, (1) and carbonyl complex [Ru(CO)Cl(PPh3)2TSC(N-S)] (2) have been synthesized from the reaction of [{(η(6)-p-cymene)RuCl}2(μ-Cl)2] and [Ru(H)(Cl)(CO)(PPh3)3] with thiophene-2-carboxaldehyde thiosemicarbazon (TSC) respectively and both novel ruthenium (II) complexes have been characterized by elemental analysis, FT-IR and NMR spectroscopy. The peripheral TSC in the complexes acts as an electrochemical coupling unit providing the ability to carry out electrochemical deposition (ED) and to form an electro-deposited film on a graphite electrode surface. The biosensing applicability of complexes 1 and 2 was investigated by using glucose oxidase (GOx) as a model enzyme. Electrochemical measurements at -0.9V versus Ag/AgCl electrode by following the ED Ru(II) reduction/oxidation due to from the enzyme activity, in the presence of glucose substrate. The designed biosensor showed a very good linearity for 0.01-0.5mM glucose. The in vitro antimicrobial activities of complexes 1 and 2 were also investigated against nine bacterial strains and one fungus by the disc diffusion test method. No activity was observed against the Gram-negative strains and fungus, whereas complex 1 showed moderate antibacterial activities against Gram-positive bacterial strains. PMID:25280673

  14. Benzaldehyde Thiosemicarbazone Derived from Limonene Complexed with Copper Induced Mitochondrial Dysfunction in Leishmania amazonensis

    PubMed Central

    Britta, Elizandra Aparecida; Barbosa Silva, Ana Paula; Ueda-Nakamura, Tânia; Dias-Filho, Benedito Prado; Silva, Cleuza Conceição; Sernaglia, Rosana Lázara; Nakamura, Celso Vataru

    2012-01-01

    Background Leishmaniasis is a major health problem that affects more than 12 million people. Treatment presents several problems, including high toxicity and many adverse effects, leading to the discontinuation of treatment and emergence of resistant strains. Methodology/Principal Findings We evaluated the in vitro antileishmanial activity of benzaldehyde thiosemicarbazone derived from limonene complexed with copper, termed BenzCo, against Leishmania amazonensis. BenzCo inhibited the growth of the promastigote and axenic amastigote forms, with IC50 concentrations of 3.8 and 9.5 µM, respectively, with 72 h of incubation. Intracellular amastigotes were inhibited by the compound, with an IC50 of 10.7 µM. BenzCo altered the shape, size, and ultrastructure of the parasites. Mitochondrial membrane depolarization was observed in protozoa treated with BenzCo but caused no alterations in the plasma membrane. Additionally, BenzCo induced lipoperoxidation and the production of mitochondrial superoxide anion radicals in promastigotes and axenic amastigotes of Leishmania amazonensis. Conclusion/Significance Our studies indicated that the antileishmania activity of BenzCo might be associated with mitochondrial dysfunction and oxidative damage, leading to parasite death. PMID:22870222

  15. Structural and biological evaluation of some metal complexes of vanillin-4N-(2-pyridyl) thiosemicarbazone

    NASA Astrophysics Data System (ADS)

    Yousef, T. A.; Abu El-Reash, G. M.; Al-Jahdali, M.; El-Rakhawy, El-Bastawesy R.

    2013-12-01

    The synthesis and characterization of Mn(II), Co(II), Ni(II), Cu(II), Zn(II), Cd(II), Hg(II) and U(VI)O2 complexes of vanillin-4N-(2-pyridyl) thiosemicarbazone (H2PVT) are reported. Theoretical calculations have been performed to obtain IR spectra of ligand and its complexes using AM1, Zindo/1, MM+ and PM3, methods. The Schiff base and its metal complexes have been screened for antibacterial Pseudomonas aeruginosa, Escherichia coli, Bacillus subtilis and Staphylococcus saprophyticus. H2VPT shows no apparent digestion effect on the egg albumin while Mn(II), Hg(II) and Cu(II) complexes exhibited a considerable digestion effect following the order Cu(II) > Mn(II) > Hg(II). Moreover, Ni(II) and Co(II) complexes revealed strong digestion effect. Fe(II), Mn(II), Cu(II), Zn(II) and Ni(II) acted as metal co- SOD enzyme factors, which are located in different compartments of the cell.

  16. Structural and optical study on antimony-silicate glasses doped with thulium ions.

    PubMed

    Dorosz, D; Zmojda, J; Kochanowicz, M; Miluski, P; Jelen, P; Sitarz, M

    2015-01-01

    Structural, spectroscopic and thermal properties of SiO₂-Al₂O₃-Sb₂O₃-Na₂O glass system doped with 0.2 mol% Tm₂O₃ have been presented. Synthesis of antimony-silicate glasses with relatively low phonon energy (600 cm(-1), which implicates a small non-radiative decay rate) was performed by conventional high-temperature melt-quenching methods. The effect of SiO₂/Sb₂O₃ ratio in fabricated Tm(3+) doped glass on thermal, structural and luminescence properties was investigated. On the basis of structural investigations decomposition of absorption bands in the infrared FTIR region was performed, thus determining that antimony ions are the only glass-forming ions, setting up the lattice of fabricated glasses. Luminescence band at the wavelength of 1.8 μm corresponding to (3)F₄→(3)H₆ transition in thulium ions was obtained under 795 nm laser pumping. It was observed that combination of relatively low phonon energy and greater separation of optically active centers in the fabricated glasses influenced in decreasing the luminescence intensity at 1800 nm. PMID:25049172

  17. Antimony(III) complexes with 2-amino-4,6-dimethoxypyrimidines: Synthesis, characterization and biological evaluation.

    PubMed

    Tunç, Turgay; Karacan, Mehmet Sayım; Ertabaklar, Hatice; Sarı, Musa; Karacan, Nurcan; Büyükgüngör, Orhan

    2015-12-01

    Novel pyrimidine compound bearing disulfide bridge, 5,5'-disulfanediylbis(2-amino-4,6-dimetoxypyrimidine) (3) was synthesized by reduction of 2-amino-4,6-dimethoxy-5-thiocyanatopyrimidine for the first time, and its structure was confirmed by X-ray crystallographic analysis. Novel binuclear antimony(III) compound of (3), {Sb[5,5'-disulfanediylbis(2-amino-4,6-dimetoxypyrimidine)]Cl3}2 (4) and mononuclear antimony(III) compounds, SbL2Cl3, [L: 2-amino-5-thiol-4,6-dimethoxy pyrimidine (2) and 2-amino-5-(1H-tetrazol-5-ylthio)-4,6-dimethoxypyrimidine (6)] were synthesized and characterized with the help of elemental analysis, molecular conductivity, FT-IR, (1)H-NMR and LC-MS techniques. The geometrical structures optimized by a DFT/B3LYP/LANL2DZ method of the compounds, indicated that monomeric compounds have square pyramidal shape. Both antileishmanial activity against Leishmania tropica promastigote and glutathione reductase inhibitory activity were determined in vitro. The results showed that (3) has the best biological activity. PMID:26427018

  18. Evaluation of antimony microparticles supported on biochar for application in the voltammetric determination of paraquat.

    PubMed

    Gevaerd, Ava; de Oliveira, Paulo R; Mangrich, Antonio S; Bergamini, Márcio F; Marcolino-Junior, Luiz H

    2016-05-01

    This work describes the construction and application of carbon paste electrodes modified with biochar and antimony microparticles (SbBCPE) for voltammetric determination of paraquat using a simple and sensitive procedure based on voltammetric stripping analysis. Some parameters such as amount of biochar and antimony used in the composition of the carbon paste and instrumental parameters were examined in detail. Under optimized conditions, an analytical curve was obtained for paraquat determination employing SbBCPE, which showed a linear response ranging from 0.2 to 2.9 μmol L(-1), with limit of detection and quantification of 34 nmol L(-1) and 113 nmol L(-1), respectively, after paraquat pre-concentration of 120 s. The repeatability study presented a RSD=2.0% for 10 consecutive measurements using the same electrode surface and the reproducibility study showed a RSD=2.7% for measurements with 10 different electrode surfaces. The proposed sensor was successfully applied for paraquat determination in tap water and citric fruit juice spiked samples and good recoveries were obtained without any sample pre-treatment, showing its promising analytical performance. PMID:26952405

  19. Alkaline reforming of brominated fire-retardant plastics: fate of bromine and antimony.

    PubMed

    Onwudili, Jude A; Williams, Paul T

    2009-02-01

    High-impact polystyrene (HIPS) flame retarded with decabromodiphenyl ether (DDE), has been reacted in supercritical water from 380 to 450 degrees C and 21.5 to 31.0 MPa pressure in a batch reactor. Different concentrations of sodium hydroxide additive were used in situ to neutralize the corrosive inorganic bromine species released during the reactions. It appeared that supercritical water conditions lowered the decomposition temperature of both the fire-retardant DDE and HIPS. The reaction products included oils (up to 76 wt%), char (up to 18 wt%) and gas (up to 2.4 wt%) which was mainly methane. The presence of the alkaline water led to up to 97 wt% debromination of the product oil, producing virtually bromine-free oil feedstock. The removal of antimony from the oil product during processing was of the order of 98 wt%. The oil consisted of many single- and multiple-ringed aromatic compounds, many of which had alkyl substituents and/or aliphatic C(n)-bridges (n=1-4). The major single-ringed compounds included toluene, xylenes, ethylbenzene, propylbenzene and alpha-methylstyrene. Bibenzyl (diphenylethane), stilbene, diphenylmethane, diphenylpropane, diphenylcyclopropane, diphenylpropene, diphenylbutane, diphenylbutene and diphenylbuta-1,3-diene were the major C(n)-bridged compounds. Diphenyl ether and acetophenone were the major oxygenated compounds found. The process thus has the potential to produce bromine-free and antimony-free oils from fire-retardant plastics. PMID:19054543

  20. A Telomeric Cluster of Antimony Resistance Genes on Chromosome 34 of Leishmania infantum.

    PubMed

    Tejera Nevado, Paloma; Bifeld, Eugenia; Höhn, Katharina; Clos, Joachim

    2016-09-01

    The mechanisms underlying the drug resistance of Leishmania spp. are manifold and not completely identified. Apart from the highly conserved multidrug resistance gene family known from higher eukaryotes, Leishmania spp. also possess genus-specific resistance marker genes. One of them, ARM58, was first identified in Leishmania braziliensis using a functional cloning approach, and its domain structure was characterized in L. infantum Here we report that L. infantum ARM58 is part of a gene cluster at the telomeric end of chromosome 34 also comprising the neighboring genes ARM56 and HSP23. We show that overexpression of all three genes can confer antimony resistance to intracellular amastigotes. Upon overexpression in L. donovani, ARM58 and ARM56 are secreted via exosomes, suggesting a scavenger/secretion mechanism of action. Using a combination of functional cloning and next-generation sequencing, we found that the gene cluster was selected only under antimonyl tartrate challenge and weakly under Cu(2+) challenge but not under sodium arsenite, Cd(2+), or miltefosine challenge. The selective advantage is less pronounced in intracellular amastigotes treated with the sodium stibogluconate, possibly due to the known macrophage-stimulatory activity of this drug, against which these resistance markers may not be active. Our data point to the specificity of these three genes for antimony resistance. PMID:27324767

  1. Antimony oxofluorides - a synthesis concept that yields phase pure samples and single crystals.

    PubMed

    Ali, Sk Imran; Johnsson, Mats

    2016-07-26

    The single crystals of the new isostructural compounds Sb3O4F and Y0.5Sb2.5O4F and the two previously known compounds M-SbOF and α-Sb3O2F5 were successfully grown by a hydrothermal technique at 230 °C. The new compound Sb3O4F crystallizes in the monoclinic space group P21/c; a = 5.6107(5) Å, b = 4.6847(5) Å, c = 20.2256(18) Å, β = 94.145(8)°, z = 4. The replacing part of Sb with Y means a slight increase in the unit cell dimensions. The compounds M-SbOF and α-Sb3O2F5 have not been grown as single crystals before and it can be concluded that hydrothermal synthesis has proved to be a suitable technique for growing single crystals of antimony oxofluorides because of the relatively low solubility of such compounds compared to other antimony oxohalides that most often have been synthesised at high temperatures by solid state reactions or gas-solid reactions. PMID:27402498

  2. Effect of indium and antimony doping in SnS single crystals

    SciTech Connect

    Chaki, Sunil H. Chaudhary, Mahesh D.; Deshpande, M.P.

    2015-03-15

    Highlights: • Single crystals growth of pure SnS, indium doped SnS and antimony doped SnS by direct vapour transport (DVT) technique. • Doping of In and Sb occurred in SnS single crystals by cation replacement. • The replacement mechanism ascertained by EDAX, XRD and substantiated by Raman spectra analysis. • Dopants concentration affects the optical energy bandgap. • Doping influences electrical transport properties. - Abstract: Single crystals of pure SnS, indium (In) doped SnS and antimony (Sb) doped SnS were grown by direct vapour transport (DVT) technique. Two doping concentrations of 5% and 15% each were employed for both In and Sb dopants. Thus in total five samples were studied viz., pure SnS (S1), 5% In doped SnS (S2), 15% In doped SnS (S3), 5% Sb doped SnS (S4) and 15% Sb doped SnS (S5). The grown single crystal samples were characterized by evaluating their surface microstructure, stoichiometric composition, crystal structure, Raman spectroscopy, optical and electrical transport properties using appropriate techniques. The d.c. electrical resistivity and thermoelectric power variations with temperature showed semiconducting and p-type nature of the as-grown single crystal samples. The room temperature Hall Effect measurements further substantiated the semiconducting and p-type nature of the as-grown single crystal samples. The obtained results are deliberated in detail.

  3. New approaches to antimony film screen-printed electrodes using carbon-based nanomaterials substrates.

    PubMed

    Pérez-Ràfols, Clara; Serrano, Núria; Díaz-Cruz, José Manuel; Ariño, Cristina; Esteban, Miquel

    2016-04-15

    Three different commercial carbon nanomaterial-modified screen-printed electrodes based on graphene, carbon nanotubes and carbon nanofibers were pioneeringly tested as electrode platforms for the plating with Sb film. They were microscopically and analytically compared to each other and to the most conventional unmodified carbon screen-printed electrode (SPCE). The obtained detection and quantification limits suggest that the in-situ antimony film electrode prepared from carbon nanofibers modified screen-printed electrode (SbSPCE-CNF) produces a better analytical performance as compared to the classical SPCE modified with antimony for Pb(II) and Cd(II) determination, approving its appropriateness for measuring low μg L(-1) levels of the considered metals. In-situ SbSPCE-CNF was successfully used for the simultaneous determination of Pb(II) and Cd(II) ions, by means of differential pulse anodic stripping voltammetry, in a certified reference estuarine water sample with a very high reproducibility and good trueness. PMID:27016434

  4. A Black Phosphate Conversion Coating on Steel Surface Using Antimony(III)-Tartrate as an Additive

    NASA Astrophysics Data System (ADS)

    Li, Feng; Wang, Guiping

    2016-05-01

    A novel black phosphate conversion coating was formed on steel surface through a Zn-Mn phosphating bath containing mainly ZnO, H3PO4, Mn(H2PO4)2, and Ca(NO3)2, where antimony(III)-tartrate was used as the blackening agent of phosphatization. The surface morphology and composition of the coating were characterized by scanning electron microscopy, energy dispersion spectroscopy, and x-ray photoelectron spectroscopy. Corrosion resistance of the coating was studied by potentiodynamic polarization curves and electrochemical impedance spectroscopy. The pH value of the solution had significant influence on the formation and corrosion resistance of the coating. The experimental results indicated that the Sb plays a vital role in the blackening of phosphate conversion coating. The optimal concentration of antimony(III)-tartrate in the phosphating bath used in this experiment was 1.0 g L-1, as higher values reduced the corrosion resistance of the coating. In addition, by saponification and oil seals, the corrosion duration of the black phosphate coating in a copper sulfate spot test can be as long as 20 min.

  5. Sulfur redox chemistry governs diurnal antimony and arsenic cycles at Champagne Pool, Waiotapu, New Zealand

    NASA Astrophysics Data System (ADS)

    Ullrich, Maria K.; Pope, James G.; Seward, Terry M.; Wilson, Nathaniel; Planer-Friedrich, Britta

    2013-07-01

    Champagne Pool, a sulfidic hot spring in New Zealand, exhibits distinct diurnal variations in antimony (Sb) and arsenic (As) concentrations, with daytime high and night-time low concentrations. To identify the underlying mobilization mechanisms, five sites along the drainage channel of Champagne Pool were sampled every 2 h during a 24 h period. Temporal variations in elemental concentrations and Sb, As, and sulfur (S) speciation were monitored in the discharging fluid. Total trace element concentrations in filtered and unfiltered samples were analyzed using ICP-MS, and Sb, As and S species were determined by IC-ICP-MS. Sulfur speciation in the drainage channel was dominated by thiosulfate and sulfide at night, while sulfate dominated during the day. The distinct diurnal changes suggest that the transformations are caused by phototrophic sulfur-oxidizing bacteria. These bacteria metabolize thiosulfate and sulfide in daylight to form sulfate and, as suggested by modeling with PhreeqC, elemental sulfur. Sulfide consumption during the day results in undersaturation of antimony sulfides, which triggers the additional release of dissolved Sb. For As, diurnal cycles were much more pronounced in speciation than in total concentrations, with di- and trithioarsenate forming at night due to excess sulfide, and monothioarsenate forming from arsenite and elemental sulfur during the day. Sulfur speciation was thus found to control Sb and As in terms of both solubility and speciation.

  6. Organically complexed iron enhances bioavailability of antimony to maize (Zea mays) seedlings in organic soils.

    PubMed

    Ptak, Corey; McBride, Murray

    2015-12-01

    Antimony (Sb) is a metalloid belonging to group 15 of the periodic table. Chemical similarities between arsenic (As) and Sb produce concerns about potential health effects of Sb and enrichment in the environment. Antimony is found in oxic environments predominately as an oxyanionic species, antimonite (Sb[OH](6-)). As a result of its net negative charge, Sb[OH](6-) was not initially predicted to have strong interactions with natural organic matter. Oxyanionic species could bind the negatively charged organic matter via a ternary complexation mechanism, in which cationic metals mediate the strong association between organic matter functional groups and oxyanions. However, these interactions are poorly understood in how they influence the bioavailability of oxyanionic contaminants to plants. Iron (Fe) additions to organic soils have been found to increase the number of organically complexed Fe sites suitable for Sb exchange, resulting in a reduced bioavailable fraction of Sb. The bioavailability of Sb to maize seedlings as a function of organically complexed Fe was examined using a greenhouse study. A significant increase in plant tissue Sb was observed as organically complexed Fe increased, which was not predicted by methods commonly used to assess bioavailable Sb. Extraction of soils with organic acids common to the maize rhizosphere suggested that organic acid exudation can readily mobilize Sb bound by organic Fe complexes. PMID:26076768

  7. Morphology-controlled growth of crystalline antimony sulfide via a refluxing polyol process

    NASA Astrophysics Data System (ADS)

    Zhang, Rui; Chen, Xiangying; Mo, Maosong; Wang, Zhenghua; Zhang, Meng; Liu, Xinyuan; Qian, Yitai

    2004-02-01

    By refluxing antimony trichloride (SbCl 3) and thiourea in various solvents at suitable reaction conditions, antimony sulfide (Sb 2S 3) crystallites with a diversity of well-defined morphologies were synthesized. Sb 2S 3 rods with the average diameter of 800 nm and the length of 7 μm, as well as microtubes with the average outer diameter of 1.2 μm, the average inner diameter of 800 nm and the length of 8 μm, were obtained in 1,2-propanediol at 180°C for 10 min. In contrast, a series of experiments under different conditions were carried out to investigate the influencing factors on the reaction. The as-synthesized products were characterized by powder X-ray diffraction, field-emission scanning electron microscopy, transmission electron microscope and X-ray photoelectron spectra. The results indicate Sb 2S 3 crystals with different morphologies, including rod-like, tube-like, bowknot-like, flower-like, straw-bundled-like, taken under different experimental conditions. It is found that the reaction temperature, time, solvent and poly(vinyl pyrrolidone) (as a polymer capping reagent) play important roles in the formation of the final Sb 2S 3 crystallites with different morphologies. Also, the possible growth mechanism is discussed.

  8. Application of Hyphenated Techniques in Speciation Analysis of Arsenic, Antimony, and Thallium

    PubMed Central

    Michalski, Rajmund; Szopa, Sebastian; Jabłońska, Magdalena; Łyko, Aleksandra

    2012-01-01

    Due to the fact that metals and metalloids have a strong impact on the environment, the methods of their determination and speciation have received special attention in recent years. Arsenic, antimony, and thallium are important examples of such toxic elements. Their speciation is especially important in the environmental and biomedical fields because of their toxicity, bioavailability, and reactivity. Recently, speciation analytics has been playing a unique role in the studies of biogeochemical cycles of chemical compounds, determination of toxicity and ecotoxicity of selected elements, quality control of food products, control of medicines and pharmaceutical products, technological process control, research on the impact of technological installation on the environment, examination of occupational exposure, and clinical analysis. Conventional methods are usually labor intensive, time consuming, and susceptible to interferences. The hyphenated techniques, in which separation method is coupled with multidimensional detectors, have become useful alternatives. The main advantages of those techniques consist in extremely low detection and quantification limits, insignificant interference, influence as well as high precision and repeatability of the determinations. In view of their importance, the present work overviews and discusses different hyphenated techniques used for arsenic, antimony, and thallium species analysis, in different clinical, environmental and food matrices. PMID:22654649

  9. Synthesis of silver nanoparticles and antimony oxide nanocrystals by pulsed laser ablation in liquid media

    NASA Astrophysics Data System (ADS)

    Mendivil, M. I.; Krishnan, B.; Sanchez, F. A.; Martinez, S.; Aguilar-Martinez, J. A.; Castillo, G. A.; Garcia-Gutierrez, D. I.; Shaji, S.

    2013-03-01

    Pulsed laser ablation in liquid media (PLALM) is a prominent technique for the controlled fabrication of nanomaterials via rapid reactive quenching of ablated species at the interface between the plasma and liquid. Results on nanoparticles and nanocrystals formed by PLALM of silver (Ag) and antimony (Sb) solid targets in different liquid environments (Sodium Dodecyl Sulfate, distilled water) are presented. These experiments were done by irradiating solid targets of Ag and Sb with a nanosecond pulsed Nd:YAG laser output of wavelength 532 nm. Nanoparticles of silver and nanocrystals of antimony oxide (Sb2O3) obtained were characterized using UV-Vis spectrometry, Scanning Electron Microscopy (SEM), transmission electron microscopy (TEM), X-ray Energy Dispersion Analysis (EDAX) and X-ray diffractometry (XRD). The morphology of nanomaterials formed is studied as a function of surfactant environment. The silver nanoparticles obtained were spherical of size in the order of 10-35 nm in solution of SDS having different concentrations. In case of the Sb target, ablation was performed in two different molarities of SDS solution and distilled water. Nanocrystals of Sb2O3 in powder form having cubic and orthorhombic phases were formed in SDS solution and as fibers of nanocrystals of cubic Sb2O3 in distilled water.

  10. Antimony isotopic composition in river waters affected by ancient mining activity.

    PubMed

    Resongles, Eléonore; Freydier, Rémi; Casiot, Corinne; Viers, Jérôme; Chmeleff, Jérôme; Elbaz-Poulichet, Françoise

    2015-11-01

    In this study, antimony (Sb) isotopic composition was determined in natural water samples collected along two hydrosystems impacted by historical mining activities: the upper Orb River and the Gardon River watershed (SE, France). Antimony isotope ratio was measured by HG-MC-ICP-MS (Hydride Generation Multi-Collector Inductively Coupled Plasma Mass Spectrometer) after a preconcentration and purification step using a new thiol-cellulose powder (TCP) procedure. The external reproducibility obtained for δ(123)Sb measurements of our in-house Sb isotopic standard solution and a certified reference freshwater was 0.06‰ (2σ). Significant isotopic variations were evident in surface waters from the upper Orb River (-0.06‰≤δ(123)Sb≤+0.11‰) and from the Gardon River watershed (+0.27‰≤δ(123)Sb≤+0.83‰). In particular, streams that drained different former mining sites exploited for Sb or Pb-Zn exhibited contrasted Sb isotopic signature, that may be related to various biogeochemical processes occurring during Sb transfer from rocks, mine wastes and sediments to the water compartment. Nevertheless, Sb isotopic composition appeared to be stable along the Gardon River, which might be attributed to the conservative transport of Sb at distance from mine-impacted streams, due to the relative mobile behavior of Sb(V) in natural oxic waters. This study suggests that Sb isotopic composition could be a useful tool to track pollution sources and/or biogeochemical processes in hydrologic systems. PMID:26452900

  11. Migration of antimony from PET containers into regulated EU food simulants.

    PubMed

    Sánchez-Martínez, María; Pérez-Corona, Teresa; Cámara, Carmen; Madrid, Yolanda

    2013-11-15

    Antimony migration from polyethylene terephthalate (PET) containers into aqueous (distilled water, 3% acetic acid, 10% and 20% ethanol) and fatty food simulants (vegetable oil), as well as into vinegar, was studied. Test conditions were according to the recent European Regulation 10/2011 (EU, 2011). Sb migration was assayed by ICP-MS and HG-AFS. The results showed that Sb migration values ranged from 0.5 to 1.2μg Sb/l, which are far below the maximum permissible migration value for Sb, 40μg Sb/kg, (EU, Regulation 10/2011). Parameters as temperature and bottle re-use influence were studied. To assess toxicity, antimony speciation was performed by HPLC-ICP-MS and HG-AFS. While Sb(V) was the only species detected in aqueous simulants, an additional species (Sb-acetate complex) was measured in wine vinegar. Unlike most of the studies reported in the literature, migration tests were based on the application of the EU directive, which enables comparison and harmonisation of results. PMID:23790852

  12. Behavior of antimony(III) during copper electrowinning in chloride solutions

    SciTech Connect

    Lin, H.K.; Wu, X.

    1996-04-01

    Contamination of cathodic copper by Sb during electrowinning in chloride solutions is a surface phenomenon. A digitized scanning electron microscopy (SEM) micrograph indicates that the Sb is concentrated on the surface /of the cathode. Energy-dispersive X-ray (EDX) analysis reveals that the Sb-containing layer is a complex salt of Cu, Sb, Cl, and O. Electrochemical measurements show that the adsorption of Sb or Cu species decreases with the increase of acidity of the solution when the solution contains antimony chloride or cuprous chloride. The adsorption increases with the increase of the acidity when the solution contains both Sb and Cu. The discharge of cuprous ions in the adsorbed complex salt releases antimonious ions and then forms a new layer of the complex salt with cuprous ions from the solution. This newly formed complex salt is readsorbed on the surface of the cathode. Thus, Sb concentrates on the surface of the cathode instead of being evenly distributed throughout the copper product. This suggested mechanism also explains the fact that the presence of Sb in the electrolyte enhances the electrodeposition of Cu.

  13. [Spectroscopic studies on the formation of metal complexes and on the protein binding of antiviral thiosemicarbazone derivatives (author's transl)].

    PubMed

    Heinisch, L; Kramarczyk, K; Tonew, M; Hesse, G

    1981-04-01

    The complexation of some thiosemicarbazones and isothiosemicarbazones of isatin and quinolin-2-aldehydes with Cu2+, Zn2+ and Mn2+ ions was spectrometrically investigated. Semiquantitative data, obtained from extinction values, about the relative complexing tendencies within some groups of homologous substances were brought in relation to their antiviral effects and binding to bovine serum albumin. The complexing tendencies were greatest in compounds with methyl substituents and decreased for higher alkyl substituents. whereas the binding to protein increased in the same order. The well-known maxima of the antiviral observed with medium alkyl groups may be explained by a superposition of these effects. PMID:7255526

  14. Conformation and coordination of 1-phenyl-3-methyl-4-benzal-5-pyrazolone thiosemicarbazone: A density functional study

    NASA Astrophysics Data System (ADS)

    Wu, Dongling; Jia, Dianzeng; Liu, Lang; Liu, Anjie

    Density functional theory method has been employed to study the molecular properties of four tautomers and their deprotonated species of 1-phenyl-3-methyl-4-benzal-5-pyrazolone thiosemicarbazone. The solvent effect has been investigated by applying the polarizable continuum model of the self-consistent reaction field theory. The condensed Fukui functions have been calculated to assess the relative reactivity of different sites in the ligands. Molecular electrostatic potential is obtained as an additional molecular descriptor for revealing the regions of the molecular species to which an electrophile would initially be attracted.

  15. Synthesis and cytotoxic activity of N-substituted thiosemicarbazones of 3-(3,4-methylenedioxy)phenylpropanal.

    PubMed

    Joselice e Silva, M; Alves, A J; Do Nascimento, S C

    1998-03-01

    Five new N-substituted thiosemicarbazones of 3-(3,4-methylenedioxy)phenylpropanal were synthesized. Safrole, a natural product obtained from sassafras oil (Ocotea pretiosa), was oxidized to alcohol using BH3-THF and H2O2, followed by oxidation to aldehyde using pyridinium dichromate (PDC) and condensation with five N-substituted derivatives of thiosemicarbazide. Tests were performed to evaluate the cytotoxic activity with continuous chain KB cells (epidermoide carcinoma of the floor of the mouth). Compounds 5 and 6 showed IC50 values of 1.5 and 4.6 micrograms/ml, respectively. PMID:9639871

  16. Targeting triple negative breast cancer cells by N3-substituted 9,10-Phenanthrenequinone thiosemicarbazones and their metal complexes

    NASA Astrophysics Data System (ADS)

    Afrasiabi, Zahra; Stovall, Preston; Finley, Kristen; Choudhury, Amitava; Barnes, Charles; Ahmad, Aamir; Sarkar, Fazlul; Vyas, Alok; Padhye, Subhash

    2013-10-01

    Novel N3-substituted 9,10-Phenanthrenequinone thiosemicarbazones and their copper, nickel and palladium complexes are structurally characterized and reported along with the single crystal X-ray structures of three ligands and one nickel complex. All compounds were evaluated for their antiproliferative potential against Triple Negative Breast Cancer (TNBC) cells which have poor prognosis and no effective drugs to treat with. All compounds exhibited antiproliferative activity against these cells. Among the metal complexes evaluated, redox active copper complexes were found to be more potent. The possible mechanism for such enhanced activity can be attributed to the generation of oxidative stress, which was amenable for targeting through metal complexation.

  17. The Innate Lymphoid Cell Precursor.

    PubMed

    Ishizuka, Isabel E; Constantinides, Michael G; Gudjonson, Herman; Bendelac, Albert

    2016-05-20

    The discovery of tissue-resident innate lymphoid cell populations effecting different forms of type 1, 2, and 3 immunity; tissue repair; and immune regulation has transformed our understanding of mucosal immunity and allergy. The emerging complexity of these populations along with compounding issues of redundancy and plasticity raise intriguing questions about their precise lineage relationship. Here we review advances in mapping the emergence of these lineages from early lymphoid precursors. We discuss the identification of a common innate lymphoid cell precursor characterized by transient expression of the transcription factor PLZF, and the lineage relationships of innate lymphoid cells with conventional natural killer cells and lymphoid tissue inducer cells. We also review the rapidly growing understanding of the network of transcription factors that direct the development of these lineages. PMID:27168240

  18. Precursor polymer compositions comprising polybenzimidazole

    SciTech Connect

    Klaehn, John R.; Peterson, Eric S.; Orme, Christopher J.

    2015-07-14

    Stable, high performance polymer compositions including polybenzimidazole (PBI) and a melamine-formaldehyde polymer, such as methylated, poly(melamine-co-formaldehyde), for forming structures such as films, fibers and bulky structures. The polymer compositions may be formed by combining polybenzimidazole with the melamine-formaldehyde polymer to form a precursor. The polybenzimidazole may be reacted and/or intertwined with the melamine-formaldehyde polymer to form the polymer composition. For example, a stable, free-standing film having a thickness of, for example, between about 5 .mu.m and about 30 .mu.m may be formed from the polymer composition. Such films may be used as gas separation membranes and may be submerged into water for extended periods without crazing and cracking. The polymer composition may also be used as a coating on substrates, such as metal and ceramics, or may be used for spinning fibers. Precursors for forming such polymer compositions are also disclosed.

  19. Synthetic, structural and kinetic studies on the binding of cyclohexane-1,2-bis(4-methyl-3-thiosemicarbazone) to divalent metal ions (Co, Ni, Cu, Zn or Cd).

    PubMed

    Al-Karawi, Ahmed Jasim M; Clegg, William; Harrington, Ross W; Henderson, Richard A

    2009-01-21

    The reactions of cyclohexane-1,2-bis(4-methyl-3-thiosemicarbazone) (CHMTSC) with MCl2 (M = Co, Ni, Cu or Zn) and Cd(NO3)2 have been shown to produce complexes in which the thiosemicarbazone has been doubly deprotonated [[M(CHMTSC - 2H+)] (M = Co, Ni or Ni)], analogous to those reported earlier with other Schiff base thiosemicarbazones. However, with ZnCl2 and Cd(NO3)2, the complexes isolated are [ZnCl(CHMTSC)]Cl and [Cd(NO3)(CHMTSC)]NO3, containing the protonated forms of the ligand, which have been characterised by X-ray crystallography, as has free CHMTSC. The kinetics of the reactions between CHMTSC and all the various metal salts have been determined by stopped-flow spectrophotometry. In all cases, the reactions are complete on the seconds timescale. The reactions exhibit a first-order dependence on the concentration of metal salt and a first-order dependence on the concentration of CHMTSC. The thermodynamic and kinetic factors influencing the protonation state of the coordinated thiosemicarbazone are discussed. PMID:19122915

  20. Inhibitory effect of synthetic aromatic heterocycle thiosemicarbazone derivatives on mushroom tyrosinase: Insights from fluorescence, (1)H NMR titration and molecular docking studies.

    PubMed

    Xie, Juan; Dong, Huanhuan; Yu, Yanying; Cao, Shuwen

    2016-01-01

    Three structurally similar aromatic heterocyclic compounds 2-thiophenecarboxaldehyde (a), 2-furaldehyde (b), 2-pyrrolecarboxaldehyde (c) were chosen and a series of their thiosemicarbazone derivatives(1a-3a, 1b-3b and 1c-3c) were synthesized to evaluate their biological activities as mushroom tyrosinase inhibitors. The inhibitory effects of these compounds on tyrosinase were investigated by using spectrofluorimetry, (1)H NMR titration and molecular docking techniques. From the results of fluorescence spectrum and (1)H NMR titration, it was found that forming complexes between the sulfur atom from thiourea and copper ion of enzyme center may play a key role for inhibition activity. Moreover, investigation of (1)H NMR spectra further revealed that formation of hydrogen bond between inhibitor and enzyme may be helpful to above complexes formation. The results were well coincident with the suggestion of molecular docking and obviously showed that 2-thiophone N(4)-thiosemicarbazone (1a), 2-furfuran N(4)-thiosemicarbazone (1b) and 2-pyrrole N(4)-thiosemicarbazone (1c) are potential inhibitors which deserves further investigation. PMID:26213029

  1. Spectral and structural studies of copper(II) complexes of thiosemicarbazones derived from salicylaldehyde and containing ring incorporated at N(4)-position

    NASA Astrophysics Data System (ADS)

    Latheef, Leji; Kurup, Maliyeckal R. Prathapachandra

    2008-06-01

    Mononuclear and binuclear copper(II) complexes ( 1- 8) with two ONS donor thiosemicarbazone ligands {salicylaldehyde 3-hexamethyleneiminyl thiosemicarbazone [H 2L 1] and salicylaldehyde 3-tetramethyleneiminyl thiosemicarbazone [H 2L 2]} have been prepared and physico-chemically characterized. IR, electronic and EPR spectra of the complexes have been obtained. The thiosemicarbazones bind to metal as dianionic ONS donor ligands in all the complexes except in [Cu(HL 1) 2] ( 2) and [Cu(HL 2) 2] ( 6). In compounds 2 and 6 the ligands are coordinated as monoanionic HL - ones. The magnetic susceptibility measurements indicate that all the complexes are paramagnetic. In complex [(CuL 1) 2] ( 1), the magnetic moment value is lower than the expected spin only value. In all the complexes g|| > g⊥ > 2.0023 and G values within the range 2.5-3.5 are consistent with d ground state. The complexes were given the formula as [(CuL 1) 2] ( 1); [Cu(HL 1) 2] ( 2); [CuL 1bpy] ( 3); [CuL 1phen] ( 4); [CuL 1γ-pic]·2H 2O ( 5); [Cu(HL 2) 2] ( 6); [CuL 2py]·3H 2O ( 7); [CuL 2bipy] ( 8). The structure of the compound 8 have been solved by single crystal X-ray crystallography and was found to be distorted square pyramid around copper(II) ion.

  2. Improved antiparasitic activity by incorporation of organosilane entities into half-sandwich ruthenium(II) and rhodium(III) thiosemicarbazone complexes.

    PubMed

    Adams, Muneebah; de Kock, Carmen; Smith, Peter J; Land, Kirkwood M; Liu, Nicole; Hopper, Melissa; Hsiao, Allyson; Burgoyne, Andrew R; Stringer, Tameryn; Meyer, Mervin; Wiesner, Lubbe; Chibale, Kelly; Smith, Gregory S

    2015-02-01

    A series of ferrocenyl- and aryl-functionalised organosilane thiosemicarbazone compounds was obtained via a nucleophilic substitution reaction with an amine-terminated organosilane. The thiosemicarbazone (TSC) ligands were further reacted with either a ruthenium dimer [(η(6-i)PrC6H4Me)Ru(μ-Cl)Cl]2 or a rhodium dimer [(Cp*)Rh(μ-Cl)Cl]2 to yield a series of cationic mono- and binuclear complexes. The thiosemicarbazone ligands, as well as their metal complexes, were characterised using NMR and IR spectroscopy, and mass spectrometry. The molecular structure of the binuclear ruthenium(ii) complex was determined by single-crystal X-ray diffraction analysis. The thiosemicarbazones and their complexes were evaluated for their in vitro antiplasmodial activities against the chloroquine-sensitive (NF54) and chloroquine-resistant (Dd2) Plasmodium falciparum strains, displaying activities in the low micromolar range. Selected compounds were screened for potential β-haematin inhibition activity, and it was found that two Rh(iii) complexes exhibited moderate to good inhibition. Furthermore, the compounds were screened for their antitrichomonal activities against the G3 Trichomonas vaginalis strain, revealing a higher percentage of growth inhibition for the ruthenium and rhodium complexes over their corresponding ligand. PMID:25559246

  3. Determination of antimony in environment samples by gas phase chemiluminescence detection following flow injection hydride generation and cryotrapping.

    PubMed

    Ye, Yousheng; Sang, Jianchi; Ma, Hongbing; Tao, Guanhong

    2010-06-15

    A novel method for the determination of antimony in environmental samples was developed with gas phase chemiluminescence detection following flow injection hydride generation and cryotrapping. The stibine, generated from samples by borohydride reduction of antimony using flow injection technique, was separated by using a new gas-liquid separator, dried with an ice-salt cryogenic bath and concentrated in a glass U-tube immersed in liquid nitrogen. Re-vaporization of stibine based on its boiling point was achieved by allowing the tube to warm at room temperature. A gas phase chemiluminescence signal was produced during the ozonation of the hydride in a reflective chamber. Under optimal conditions, the proposed method was characterized by a wide linear calibration range from 1.0microgL(-1) to 10.0mgL(-1) with a detection limit of 0.18microgL(-1) (n=11). The relative standard deviation for 10.0microgL(-1) antimony was 3.56% (n=11) and the sampling rate was 15 samples h(-1). Blank signal was reduced by the purification of reagents and the interference from transition metal ions was eliminated by the addition of L-cysteine into samples. The method was applied to the determination of antimony in environmental samples with satisfactory results. PMID:20441930

  4. Antimony porphyrins as red-light powered photocatalysts for solar fuel production from halide solutions in the presence of air.

    PubMed

    Ertl, M; Wöß, E; Knör, G

    2015-10-01

    Halide ions (X(-)) as cheap and abundant electron donors are oxidized with simulated sunlight in a photocatalytic reaction based on robust antimony porphyrins acting as red-light harvesting multielectron transfer sensitizers. Besides halogen formation (X2/X3(-)) this solar energy storing process under certain conditions also accumulates hydrogen peroxide (H2O2) as a second energy-rich compound. PMID:26360604

  5. STAT4 is critical for immunity but not for antileishmanial activity of antimonials in experimental visceral leishmaniasis

    PubMed Central

    Oghumu, Steve; Gupta, Gaurav; Snider, Heidi M; Varikuti, Sanjay; Terrazas, César A; Papenfuss, Tracey L; Satoskar, Abhay R

    2014-01-01

    Summary We and others have previously shown that IL-12 is indispensable for immunity and is required for optimal antiparasitic activity of antimonials in experimental visceral leishmaniasis caused by Leishmania donovani. In this study we investigated the role of STAT4 in immunity against L. donovani using STAT4 knockout mice and also determined the effect of STAT4 deficiency in response to antimonial therapy. Upon infection with L. donovani, stat4−/− BALB/c and C57BL/6 mice showed enhanced susceptibility to Leishmania during late time points of infection which was associated with a marked reduction in Th1 responses and hepatic immunopathology. Interestingly, these defects in Th1 responses in stat4−/− did not impair the antimonial chemotherapy as both stat4−/− and WT mice showed comparable levels of parasite clearance from the liver and spleen. These findings highlight the role of STAT4 in immunity to L. donovani infection and also provide evidence that STAT4 is dispensable for antimonial based chemotherapy. PMID:24242758

  6. Electrochemical, Structural and Surface Characterization of Nickel/Zirconia Solid Oxide Fuel Cell Anodes in Coal Gas Containing Antimony

    SciTech Connect

    Marina, Olga A.; Pederson, Larry R.; Coyle, Christopher A.; Thomsen, Edwin C.; Nachimuthu, Ponnusamy; Edwards, Danny J.

    2011-02-27

    The interaction of antimony with the nickel-zirconia solid oxide fuel cell (SOFC) anode has been investigated. Tests with both anode-supported and electrolyte-supported button cells were performed at 700 and 800oC in synthetic coal gas containing 10 ppb to 9 ppm antimony. Minor performance loss was observed immediately after Sb introduction to coal gas resulting in ca. 5 % power output drop. While no further degradation was observed during the following several hundred hours of testing, cells abruptly and irreversibly failed after 800-1500 hours depending on Sb concentration and test temperature. Antimony was found to interact strongly with nickel and result in extensive alteration phase formation, consistent with expectations based on thermodynamic properties. Nickel antimonide phases, NiSb and Ni5Sb2, were partially coalesced into large grains and eventually affected electronic percolation through the anode support. Initial degradation was attributed to diffusion of antimony to the active anode/electrolyte interface to form an adsorption layer.

  7. SEATTLE DISTRIBUTION SYSTEM CORROSION CONTROL STUDY. VOLUME III: POTENTIAL FOR DRINKING WATER CONTAMINATION FROM TIN/ANTIMONY SOLDER

    EPA Science Inventory

    This study was conducted to evaluate the potential for leaching of metals into drinking water from tin/antimony solder. The study consisted of five research phases: (1) A theoretical investigation of the corrosion products formed from the solder was conducted using pe-pH diagrams...

  8. Polarographic behavior of copper(II), cerium(IV), and antimony(III) in 2-pyrrolidinone solution

    SciTech Connect

    Puri, B.K.; Kumar, A.; Munshi, T.K.

    1985-04-20

    This paper examines the polarographic characteristics of copper (II), cerium (IV), and antimony (III) using 2-pyrrolidinone alone as the supporting electrolyte. Conditions have been developed for the determination of these metals in various synthetic samples and also in certain alloys. A method has been suggested for the simultaneous determination of these metals when present together.

  9. Nucleation precursors in protein crystallization

    PubMed Central

    Vekilov, Peter G.; Vorontsova, Maria A.

    2014-01-01

    Protein crystal nucleation is a central problem in biological crystallography and other areas of science, technology and medicine. Recent studies have demonstrated that protein crystal nuclei form within crucial precursors. Here, methods of detection and characterization of the precursors are reviewed: dynamic light scattering, atomic force microscopy and Brownian microscopy. Data for several proteins provided by these methods have demonstrated that the nucleation precursors are clusters consisting of protein-dense liquid, which are metastable with respect to the host protein solution. The clusters are several hundred nanometres in size, the cluster population occupies from 10−7 to 10−3 of the solution volume, and their properties in solutions supersaturated with respect to crystals are similar to those in homogeneous, i.e. undersaturated, solutions. The clusters exist owing to the conformation flexibility of the protein molecules, leading to exposure of hydrophobic surfaces and enhanced intermolecular binding. These results indicate that protein conformational flexibility might be the mechanism behind the metastable mesoscopic clusters and crystal nucleation. Investigations of the cluster properties are still in their infancy. Results on direct imaging of cluster behaviors and characterization of cluster mechanisms with a variety of proteins will soon lead to major breakthroughs in protein biophysics. PMID:24598910

  10. American cutaneous leishmaniasis caused by Leishmania (Viannia) braziliensis resistant to meglumine antimoniate, but with good response to pentamidine: a case report.

    PubMed

    Pimentel, Maria Inês Fernandes; Baptista, Cibele; Rubin, Evelyn Figueiredo; Vasconcellos, Erica de Camargo Ferreira e; Lyra, Marcelo Rosandiski; Salgueiro, Mariza de Matos; Saheki, Maurício Naoto; Rosalino, Cláudia Maria Valete; Madeira, Maria de Fátima; Silva, Aline Fagundes da; Confort, Eliame Mouta; Schubach, Armando de Oliveira

    2011-01-01

    This is a case report of a Brazilian soldier with cutaneous leishmaniasis. The lesion relapsed following two systemic treatments with meglumine antimoniate. The patient was treated with amphotericin B, which was interrupted due to poor tolerance. Following isolation of Leishmania sp., six intralesional infiltrations of meglumine antimoniate resulted in no response. Leishmania sp promastigotes were again isolated. The patient was submitted to intramuscular 4 mg/kg pentamidine. Parasites from the first and second biopsies were identified as Leishmania (Viannia) braziliensis; those isolated from the first biopsy were more sensitive to meglumine antimoniate in vitro than those isolated from the second biopsy. No relapse was observed. PMID:21552747

  11. Effects of terminal dimethylation and metal coordination of proline-2-formylpyridine thiosemicarbazone hybrids on lipophilicity, antiproliferative activity, and hR2 RNR inhibition.

    PubMed

    Bacher, Felix; Dömötör, Orsolya; Kaltenbrunner, Maria; Mojović, Miloš; Popović-Bijelić, Ana; Gräslund, Astrid; Ozarowski, Andrew; Filipovic, Lana; Radulović, Sinisa; Enyedy, Éva A; Arion, Vladimir B

    2014-12-01

    The nickel(II), copper(II), and zinc(II) complexes of the proline-thiosemicarbazone hybrids 3-methyl-(S)-pyrrolidine-2-carboxylate-2-formylpyridine thiosemicarbazone (L-Pro-FTSC or (S)-H2L(1)) and 3-methyl-(R)-pyrrolidine-2-carboxylate-2-formylpyridine thiosemicarbazone (D-Pro-FTSC or (R)-H2L(1)), as well as 3-methyl-(S)-pyrrolidine-2-carboxylate-2-formylpyridine 4,4-dimethyl-thiosemicarbazone (dm-L-Pro-FTSC or (S)-H2L(2)), namely, [Ni(L-Pro-FTSC-2H)]2 (1), [Ni(D-Pro-FTSC-2H)]2 (2), [Ni(dm-L-Pro-FTSC-2H)]2 (3), [Cu(dm-L-Pro-FTSC-2H)] (6), [Zn(L-Pro-FTSC-2H)] (7), and [Zn(D-Pro-FTSC-2H)] (8), in addition to two previously reported, [Cu(L-Pro-FTSC-2H)] (4), [Cu(D-Pro-FTSC-2H)] (5), were synthesized and characterized by elemental analysis, one- and two-dimensional (1)H and (13)C NMR spectroscopy, circular dichroism, UV-vis, and electrospray ionization mass spectrometry. Compounds 1-3, 6, and 7 were also studied by single-crystal X-ray diffraction. Magnetic properties and solid-state high-field electron paramagnetic resonance spectra of 2 over the range of 50-420 GHz were investigated. The complex formation processes of L-Pro-FTSC with nickel(II) and zinc(II) were studied in aqueous solution due to the excellent water solubility of the complexes via pH potentiometry, UV-vis, and (1)H NMR spectroscopy. The results of the antiproliferative activity in vitro showed that dimethylation improves the cytotoxicity and hR2 RNR inhibition. Therefore, introduction of more lipophilic groups into thiosemicarbazone-proline backbone becomes an option for the synthesis of more efficient cytotoxic agents of this family of compounds. PMID:25391085

  12. Antimony and arsenic behaviours in soils from three abandoned gold mining areas in northern Portugal

    NASA Astrophysics Data System (ADS)

    Carvalho, Paula; Neiva, Ana; Silva, Maria

    2013-04-01

    The Valongo anticline located 18 km at East of Porto is characterized by the occurrence of several gold deposits, which were exploited until the end of the nineteenth century. This anticline comprises Cambrian to Carboniferous metasediments. The Cambrian schist-graywacke complex crops out in the western limb of the anticline and is intersected by several Sb-Au quartz veins, mainly Montalto and Tapada. At the eastern limb of the anticline, As-Au quartz veins cut Ordovician black slates and were exploited at the Banjas mine. The Sb-Au quartz veins contain mainly quartz, arsenopyrite, pyrrhotite, pyrite, marcasite, sphalerite, chalcophyrite, galena, gold, tetrahedrite, jamesonite, plagionite, berthierite, stibnite, antimony and carbonates. The As-Au quartz veins consist of quartz, arsenopyrite, pyrite, pyrrhotite, cobaltite, glaucodote, sphalerite, boulangerite, tetrahedrite and siderite. Stibnite and arsenopyrite are the most abundant sulphides in Sb-Au and As-Au quartz veins, respectively. Therefore, antimony and arsenic are potential contaminants in the surrounding environments of these old mines. The principal component analysis (PCA) was applied to organic matter, pH, cation exchange capacity, clay size particle and reducible, oxidizable and aqua regia Fe, Mn, As and Sb concentrations obtained by the BCR method in 29 soil samples. The PCA shows a substantial distinction between Sb and As behaviours in soils from the old mining areas of Montalto, Tapada and Banjas. The arsenic concentration ranges between 16.98 mg/kg and 1116 mg/kg, whereas the Sb concentration ranges from 6.4 mg/kg to 21775 mg/kg. The antimony is statistically more correlated with Fe and Mn in the oxides fraction, whereas As in the reducible fraction dependents on pH values. Moreover, Fe and Mn concentrations in the oxidizable fraction are highly correlated with the organic matter, suggesting that pyrite, the main host mineral of Fe, was probably totally altered. However, the As concentration in

  13. Lithium-antimony-lead liquid metal battery for grid-level energy storage.

    PubMed

    Wang, Kangli; Jiang, Kai; Chung, Brice; Ouchi, Takanari; Burke, Paul J; Boysen, Dane A; Bradwell, David J; Kim, Hojong; Muecke, Ulrich; Sadoway, Donald R

    2014-10-16

    The ability to store energy on the electric grid would greatly improve its efficiency and reliability while enabling the integration of intermittent renewable energy technologies (such as wind and solar) into baseload supply. Batteries have long been considered strong candidate solutions owing to their small spatial footprint, mechanical simplicity and flexibility in siting. However, the barrier to widespread adoption of batteries is their high cost. Here we describe a lithium-antimony-lead liquid metal battery that potentially meets the performance specifications for stationary energy storage applications. This Li||Sb-Pb battery comprises a liquid lithium negative electrode, a molten salt electrolyte, and a liquid antimony-lead alloy positive electrode, which self-segregate by density into three distinct layers owing to the immiscibility of the contiguous salt and metal phases. The all-liquid construction confers the advantages of higher current density, longer cycle life and simpler manufacturing of large-scale storage systems (because no membranes or separators are involved) relative to those of conventional batteries. At charge-discharge current densities of 275 milliamperes per square centimetre, the cells cycled at 450 degrees Celsius with 98 per cent Coulombic efficiency and 73 per cent round-trip energy efficiency. To provide evidence of their high power capability, the cells were discharged and charged at current densities as high as 1,000 milliamperes per square centimetre. Measured capacity loss after operation for 1,800 hours (more than 450 charge-discharge cycles at 100 per cent depth of discharge) projects retention of over 85 per cent of initial capacity after ten years of daily cycling. Our results demonstrate that alloying a high-melting-point, high-voltage metal (antimony) with a low-melting-point, low-cost metal (lead) advantageously decreases the operating temperature while maintaining a high cell voltage. Apart from the fact that this

  14. Antimony: a traffic-related element in the atmosphere of Buenos Aires, Argentina.

    PubMed

    Gómez, Darío R; Fernanda Giné, María; Claudia Sánchez Bellato, Ana; Smichowski, Patricia

    2005-12-01

    Vehicular traffic is one of the main sources of antimony in highly populated urban areas like Buenos Aires where an overall traffic density of 1 500 000 vehicles per day (corresponding to 7500 vehicles km(-2)) is estimated. In this context, a study was undertaken to ascertain the levels of Sb and other traffic-related elements (TRE) in the atmosphere of this city. To this end, sixty-seven samples of PM-10 particulate matter were collected during eight days in nine representative sampling sites located downtown Buenos Aires and spread over an area of about 30 km2. The collection of particulate matter was performed on ash-free glass-fibre filters using high volume samplers with PM-10 sampling heads. A combination of aqua regia and perchloric acid was used for leaching metals from filters. The resulting solutions were evaporated and then diluted with 0.1 mol l(-1) HCl. Antimony was determined by inductively coupled plasma-quadrupole mass spectrometry (ICP-QMS) at ng g(-1) levels. Concentrations of Sb varied from 12.9 +/- 0.9 to 375 +/- 23 microg g(-1)(equivalent to 0.87 +/- 0.06 to 15.3 +/- 0.8 ng m(-3)). Statistical analysis was performed on the data set including the measured PM-10 mass and Sb concentrations for the monitored period. Correlations of Sb with other TRE namely, Cu and Mo were also assessed. The highest concentrations of Sb were detected at two sites (Hospital Alemán and Casa Rapallini) located in streets with traffic consisting mostly of passenger cars and showing a "stop-and-go" pattern in peak hours. Antimony levels in the Buenos Aires PM-10 are by far below the level of 0.5 mg m(-3)(for an 8 hour workday, 40 hour work week) set by the US Occupational Safety and Health Administration (OSHA) for occupational exposure. However, monitoring of Sb and other TRE should be carried out in a systematic fashion to detect the possibility of increases in from the present levels. PMID:16307067

  15. Spin dynamics of complex oxides, bismuth-antimony alloys, and bismuth chalcogenides

    NASA Astrophysics Data System (ADS)

    Sahin, Cuneyt

    The emerging field of spintronics relies on the manipulation of electron spin in order to use it in spin-based electronics. Such a paradigm change has to tackle several challenges including finding materials with sufficiently long spin lifetimes and materials which are efficient in generating pure spin currents. This thesis predicts that two types of material families could be a solution to the aforementioned challenges: complex oxides and bismuth based materials. We derived a general approach for constructing an effective spin-orbit Hamiltonian which is applicable to all nonmagnetic materials. This formalism is useful for calculating spin-dependent properties near an arbitrary point in momentum space. We also verified this formalism through comparisons with other approaches for III-V semiconductors, and its general applicability is illustrated by deriving the spin-orbit interaction and predicting spin lifetimes for strained strontium titanate (STO) and a two-dimensional electron gas in STO (such as at the LAO/STO interface). Our results suggest robust spin coherence and spin transport properties in STO related materials even at room temperature. In the second part of the study we calculated intrinsic spin Hall conductivities for bismuth-antimony (BISb) semimetals with strong spin-orbit couplings, from the Kubo formula and using Berry curvatures evaluated throughout the Brillouin zone from a tight-binding Hamiltonian. Nearly crossing bands with strong spin-orbit interaction generate giant spin Hall conductivities in these materials, ranging from 474 ((h/e)O--1cm--1) for bismuth to 96((h/e)O--1cm --1) for antimony; the value for bismuth is more than twice that of platinum. The large spin Hall conductivities persist for alloy compositions corresponding to a three-dimensional topological insulator state, such as Bi0.83Sb0.17. The spin Hall conductivity could be changed by a factor of 5 for doped Bi, or for Bi0.83Sb0.17, by changing the chemical potential by 0.5 e

  16. Precursors of Short Gamma-Ray Bursts

    NASA Technical Reports Server (NTRS)

    Troja, E.; Rosswog, S.; Gehrels, N.

    2010-01-01

    We carried out a systematic search of precursors on the sample of short GRBs observed by Swift. We found that approx. 8-10% of short GRBs display such early episode of emission. One burst (GRB 090510) shows two precursor events, the former approx.13 s and the latter approx. 0.5 s before the GRB. We did not find any substantial difference between the precursor and the main GRB emission, and between short GRBs with and without precursors. We discuss possible mechanisms to reproduce the observed precursor emission within the scenario of compact object mergers. The implications of our results on quantum gravity constraints are also discussed.

  17. Vibrational, NMR and UV-visible spectroscopic investigation and NLO studies on benzaldehyde thiosemicarbazone using computational calculations

    NASA Astrophysics Data System (ADS)

    Moorthy, N.; Prabakar, P. C. Jobe; Ramalingam, S.; Pandian, G. V.; Anbusrinivasan, P.

    2016-04-01

    In order to investigate the vibrational, electronic and NLO characteristics of the compound; benzaldehyde thiosemicarbazone (BTSC), the XRD, FT-IR, FT-Raman, NMR and UV-visible spectra were recorded and were analysed with the calculated spectra by using HF and B3LYP methods with 6-311++G(d,p) basis set. The XRD results revealed that the stabilized molecular systems were confined in orthorhombic unit cell system. The cause for the change of chemical and physical properties behind the compound has been discussed makes use of Mulliken charge levels and NBO in detail. The shift of molecular vibrational pattern by the fusing of ligand; thiosemicarbazone group with benzaldehyde has been keenly observed. The occurrence of in phase and out of phase molecular interaction over the frontier molecular orbitals was determined to evaluate the degeneracy of the electronic energy levels. The thermodynamical studies of the temperature region 100-1000 K to detect the thermal stabilization of the crystal phase of the compound were investigated. The NLO properties were evaluated by the determination of the polarizability and hyperpolarizability of the compound in crystal phase. The physical stabilization of the geometry of the compound has been explained by geometry deformation analysis.

  18. Interaction of Triapine and related thiosemicarbazones with iron(III)/(II) and gallium(III): a comparative solution equilibrium study†

    PubMed Central

    Enyedy, Éva A.; Primik, Michael F.; Kowol, Christian R.; Arion, Vladimir B.; Kiss, Tamás; Keppler, Bernhard K.

    2012-01-01

    Stoichiometry and stability of GaIII, FeIII, FeII complexes of Triapine and five related α-N heterocyclic thiosemicarbazones with potential antitumor activity have been determined by pH-potentiometry, UV-vis spectrophotometry, 1H NMR spectroscopy, and spectrofluorimetry in aqueous solution (with 30% DMSO), together with the characterization of the proton dissociation processes. Additionally, the redox properties of the iron complexes were studied by cyclic voltammetry at various pH values. Formation of high stability bis-ligand complexes was found in all cases, which are predominant at physiological pH with FeIII/FeII, whilst only at the acidic pH range with GaIII. The results show that among the thiosemicarbazones with various substituents the N-terminal dimethylation does not exert a measurable effect on the redox potential, but has the highest impact on the stability of the complexes as well as the cytotoxicity, especially in the absence of a pyridine-NH2 group in the molecule. In addition the fluorescence properties of the ligands in aqueous solution and their changes caused by GaIII were studied. PMID:21523301

  19. Toxic effects of bis(thiosemicarbazone) compounds and its palladium(II) complexes on herpes simplex virus growth.

    PubMed

    Genova, Petia; Varadinova, Tatiana; Matesanz, Ana I; Marinova, Desislava; Souza, Pilar

    2004-06-01

    Here, we present data on the activity of benzyl bis(thiosemicarbazone); 3,5-diacyl-1,2,4-triazole bis(4-methylthiosemicarbazone) and their Pd(II) complexes against the replication of wild type and of acyclovir (ACV)-resistant, herpes simplex virus type 1 (HSV 1) and type 2 (HSV 2) strains. The data were compared to those under the action of acyclovir. The testing of cytotoxic activity suggests that these compounds may be endowed with important antiviral properties. It is interesting to note that the Pd(II)-benzyl bis(thiosemicarbazone) complex, 2, exhibits a significant activity against acyclovir-resistant viruses R-100 (HSV 1) and PU (HSV 2) with an in vitro selectivity index (SI) of 8.0 vs. 0.01 for acyclovir. This complex also negatively influenced the expression of key structural HSV 1 proteins (VP23, gH and gG/gD), thus suppressing simultaneously virus entry, transactivation of virus genome, capsid assembly, and cell-to-cell spread of infectious HSV progeny. PMID:15163546

  20. Synthesis of thiophene-thiosemicarbazone derivatives and evaluation of their in vitro and in vivo antitumor activities.

    PubMed

    de Oliveira, Jamerson Ferreira; da Silva, Anekécia Lauro; Vendramini-Costa, Débora Barbosa; da Cruz Amorim, Cezar Augusto; Campos, Júlia Furtado; Ribeiro, Amélia Galdino; Olímpio de Moura, Ricardo; Neves, Jorge Luiz; Ruiz, Ana Lúcia Tasca Gois; Ernesto de Carvalho, João; Alves de Lima, Maria do Carmo

    2015-11-01

    A series of thiophene-2-thiosemicarbazones derivatives (5-14) was synthesized, characterized and evaluated for their antitumor activity. They were tested in vitro against human tumor cell lines through the colorimetric method. The results revealed that compounds 7 and 9 were the most effective in inhibiting 50% of the cell growth after 48 h of treatment. As compound 7 showed a potent antiproliferative profile, it has been chosen for further studies in 786-0 cell line by flow cytometry. Treatments with compound 7 (50 μM) induced early phosphatidylserine exposure after 18 h of exposure and this process progressed phosphatidylserine exposure with loss of cell membrane integrity after 24 h of treatment, suggesting a time-dependent cell death process. Regarding the cell cycle profile, no changes were observed after treatment with compound 7 (25 μM), suggesting a mechanism of cell death independent on the cell cycle. The in vivo studies show that compound 7 possess low acute toxicity, being the doses of 30-300 mgKg(-1) chosen for studies in Ehrlich solid tumor model in mice. All doses were able to inhibit tumor development being the lowest one the most effective. Our findings highlight thiophene-2-thiosemicarbazones as a promising class of compounds for further studies concerning new anticancer therapies. PMID:26454648

  1. Synthesis, spectroscopic characterization, structural studies and antibacterial and antitumor activities of diorganotin complexes with 3-methoxysalicylaldehyde thiosemicarbazone

    NASA Astrophysics Data System (ADS)

    Khandani, Marzieh; Sedaghat, Tahereh; Erfani, Nasrollah; Haghshenas, Mohammad Reza; Khavasi, Hamid Reza

    2013-04-01

    Three organotin(IV) complexes, Ph2Sn(mstsc) (1), Me2Sn(mstsc) (2) and Bu2Sn(mstsc) (3), have been synthesized from reaction of R2SnCl2 (R = Ph, Me and Bu) with 3-methoxysalicylaldehyde thiosemicarbazone (H2mstsc). The synthesized complexes have been characterized by elemental analysis and FT-IR, 1H, 13C and 119Sn NMR spectroscopy. The structures of 2 and 3 have been also confirmed by X-ray crystallography. On the basis of spectral and structural data thiosemicarbazone acts as a tridentate dianionic ligand and coordinates to tin through phenolic oxygen, the azomethine nitrogen and thiolate sulfur atoms. The metal coordination geometry for 2 and 3 is described as distorted square pyramid and the crystal lattices are stabilized by intermolecular hydrogen bands. On the basis of 119Sn NMR data, coordination number of tin retains five in solution. The in vitro antibacterial activity of ligand and its complexes has been evaluated against one Gram-positive and three Gram-negative bacteria. Complex 2 exhibited good activity along with the standard antibacterial drugs. The in vitro cytotoxicities of the synthesized compounds against Jurkat cells were evaluated by the standard WST-1 assay. The activity decreases in the order 3 > 1 > 2 = H2mstsc.

  2. Comparative evaluation of Bis(thiosemicarbazone)- Biotin and Met-ac-TE3A for tumor imaging.

    PubMed

    Singh, Sweta; Tiwari, Anjani K; Varshney, Raunak; Mathur, R; Shukla, Gauri; Bag, N; Singh, B; Mishra, Anil K

    2016-01-15

    2,2',2″-(11-(2-((4-mercapto-1-methoxy-1-oxobutan-2-yl)amino)-2-oxoethyl)-1,4,8,11-tetraaza cyclotetradecane-1,4,8-triyl)triacetic acid, Met-ac-TE3A and (E)-N-methyl-2-((E)-3-(2-(2-(5-((3aS,4S,6aR)-2-oxohexahydro-1H-thieno[3,4-d]imidazol-4-yl)pentanoyl)hydrazinecarbono-thioyl)hydrazonobutan-2-ylidene)hydrazinecarbothioamide, Bis(thiosemicarbazone)- Biotin were synthesized and evaluated for imaging application. The pharmacokinetics of these ligands were determined by tracer methods. In vitro human serum stability of (99m)Tc Met-ac-TE3A/(99m)Tc Bis(thiosemicarbazone)-Biotin after 24h was found to be 96.5% and 97.0% respectively. Blood kinetics of both ligands in normal rabbits showed biphasic clearance pattern. Ex vivo biodistribution study revealed significant initial tumor uptake and high tumor/muscles ratio which is a pre-requisite condition for a ligand to work as SPECT-radiopharmaceutical for tumor imaging. PMID:26436844

  3. Novel 3,4-methylenedioxyde-6-X-benzaldehyde-thiosemicarbazones: Synthesis and antileishmanial effects against Leishmania amazonensis.

    PubMed

    de Melos, Jorge Luiz R; Torres-Santos, Eduardo Caio; Faiões, Viviane dos S; Del Cistia, Catarina de Nigris; Sant'Anna, Carlos Maurício R; Rodrigues-Santos, Cláudio Eduardo; Echevarria, Aurea

    2015-10-20

    A series of eleven 3,4-methylenedioxyde-6-X-benzaldehyde-thiosemicarbazones (16-27) was synthesised as part of a study to search for potential new drugs with a leishmanicidal effect. The thiosemicarbazones, ten of which are new compounds, were prepared in good yields (85-98%) by the reaction of 3,4-methylenedioxyde-6-benzaldehydes (6-X-piperonal), previously synthesised for this work by several methodologies, and thiosemicarbazide in ethanol with a few drops of H2SO4. These compounds were evaluated against Leishmania amazonensis promastigotes, and derivatives where X = I (22) and X = CN (23) moieties showed impressive results, having IC₅₀ = 20.74 μM and 16.40 μM, respectively. The intracellular amastigotes assays showed IC₅₀ = 22.00 μM (22) and 17.00 μM (23), and selectivity index >5.7 and >7.4, respectively, with a lower toxicity compared to pentamidine (positive control, SI = 4.5). The results obtained from the preliminary QSAR study indicated the hydrophobicity (log P) as a fundamental parameter for the 2D-QSAR linear model. A molecular docking study demonstrated that both compounds interact with flavin mononucleotide (FMN), important binding site of NO synthase. PMID:26375353

  4. Vibrational, NMR and UV-Visible spectroscopic investigation, VCD and NLO studies on Benzophenone thiosemicarbazone using computational calculations

    NASA Astrophysics Data System (ADS)

    Moorthy, N.; Jobe Prabakar, P. C.; Ramalingam, S.; Periandy, S.; Parasuraman, K.

    2016-04-01

    In order to explore the unbelievable NLO property of prepared Benzophenone thiosemicarbazone (BPTSC), the experimental and theoretical investigation has been made. The theoretical calculations were made using RHF and CAM-B3LYP methods at 6-311++G(d,p) basis set. The title compound contains Cdbnd S ligand which helps to improve the second harmonic generation (SHG) efficiency. The molecule has been examined in terms of the vibrational, electronic and optical properties. The entire molecular behavior was studied by their fundamental IR and Raman wavenumbers and was compared with the theoretical aspect. The molecular chirality has been studied by performing vibrational circular dichroism (circularly polarized infrared radiation). The Mulliken charge levels of the compound ensure the perturbation of atomic charges according to the ligand. The molecular interaction of frontier orbitals emphasizes the modification of chemical properties of the compound through the reaction path. The enormous amount of NLO activity was induced by the Benzophenone in thiosemicarbazone. The Gibbs free energy was evaluated at different temperature and from which the enhancement of chemical stability was stressed. The VCD spectrum was simulated and the optical dichroism of the compound has been analyzed.

  5. Synthesis and spectral feature of benzophenone-substituted thiosemicarbazones and their Ni(II) and Cu(II) complexes

    NASA Astrophysics Data System (ADS)

    El-Asmy, A. A.; Al-Hazmi, G. A. A.

    2009-01-01

    The ligational behavior of 2-hydroxybenzophenone and 2-hydroxy-4-methoxybenzophenone N-substituted thiosemicarbazones towards Ni(II) and Cu(II) ions has been investigated. The isolated complexes were identified by elemental analyses, molar conductance, magnetic moment, IR, UV-vis and ESR spectral studies. The IR spectra indicated that the investigated thiosemicarbazones lost the N 2 proton or the N 2 and OH protons and act as mononegative or binegative tridentate ligands. The ligands containing methoxy group facilitate the deprotonation of OH by resonance more than the SH. Most of the Ni(II) complexes measured subnormal magnetic moments due to square-planar + tetrahedral configuration and supported by the electronic spectra. The percentage of square-planar to tetrahedral was calculated and found in agreement with the ligand splitting energy (10Dq). Also, Cu(II) complexes measured subnormal values due to the interaction between copper centers; the lower the value the higher the interaction. It was found that the substitutent has a noticeable effect on the distortion of the complex. The ESR spectra of some solid Cu(II) complexes at room temperature exhibit g|| > g⊥ > 2.0023 confirming a square-planar structure.

  6. New Oxidovanadium Complexes Incorporating Thiosemicarbazones and 1, 10-Phenanthroline Derivatives as DNA Cleavage, Potential Anticancer Agents, and Hydroxyl Radical Scavenger.

    PubMed

    Ying, Peng; Zeng, Pengfei; Lu, Jiazheng; Chen, Hongyuan; Liao, Xiangwen; Yang, Ning

    2015-10-01

    Four novel oxidovanadium(IV) complexes, [VO(hntdtsc)(PHIP)] (1) (hntdtsc = 2-hydroxy-1-naphthaldehyde thiosemicarbazone, PHIP= 2-phenyl-imidazo[4,5-f]1,10-phenanthroline), [VO(hntdtsc)(DPPZ)](2)(DPPZ= dipyrido[3,2-a:2',3'-c]phenazine), [VO(satsc)(PHIP)](3) (satsc=salicylaldehyde thiosemicarbazone), and [VO(satsc)(DPPZ)](4), have been prepared and characterized. The chemical nuclease activities and photocleavage reactions of the complexes were tested. All four complexes can efficiently cleave pBR322 DNA, and complex 1 has the best cleaving ability. The antitumor properties of these complexes were examined with three different tumor cell lines using MTT assay. Their antitumor mechanism has been analyzed using cell cycle analysis, fluorescence microscopy of apoptosis, and Annexin V-FITC/PI assay. The results showed that the growth of human neuroblastoma (SH-SY5Y, SK-N-SH) and human breast adenocarcinoma (MCF-7) cells were inhibited significantly with very low IC50 values. Complex 1 was found to be the most potent antitumor agent among the four complexes. It can cause G0/G1 phase arrest of the cell cycle and exhibited significant induced apoptosis in SK-N-SH cells and displayed typical morphological apoptotic characteristics. In addition, they all displayed reasonable abilities to scavenge hydroxyl radical, and complex 1 was the best inhibitor. PMID:25659415

  7. Comparative evaluation of Bis(thiosemicarbazone)- Biotin and Met-ac-TE3A for tumor imaging

    NASA Astrophysics Data System (ADS)

    Singh, Sweta; Tiwari, Anjani K.; Varshney, Raunak; Mathur, R.; Shukla, Gauri; Bag, N.; Singh, B.; Mishra, Anil K.

    2016-01-01

    2,2‧,2″-(11-(2-((4-mercapto-1-methoxy-1-oxobutan-2-yl)amino)-2-oxoethyl)-1,4,8,11-tetraaza cyclotetradecane-1,4,8-triyl)triacetic acid, Met-ac-TE3A and (E)-N-methyl-2-((E)-3-(2-(2-(5-((3aS,4S,6aR)-2-oxohexahydro-1H-thieno[3,4-d]imidazol-4-yl)pentanoyl)hydrazinecarbono-thioyl)hydrazonobutan-2-ylidene)hydrazinecarbothioamide, Bis(thiosemicarbazone)- Biotin were synthesized and evaluated for imaging application. The pharmacokinetics of these ligands were determined by tracer methods. In vitro human serum stability of 99mTc Met-ac-TE3A/99mTc Bis(thiosemicarbazone)-Biotin after 24 h was found to be 96.5% and 97.0% respectively. Blood kinetics of both ligands in normal rabbits showed biphasic clearance pattern. Ex vivo biodistribution study revealed significant initial tumor uptake and high tumor/muscles ratio which is a pre-requisite condition for a ligand to work as SPECT-radiopharmaceutical for tumor imaging.

  8. In-situ growth of antimony sulfide in carbon nanoparticle matrix: Enhanced electrocatalytic activity as counter electrode in dye-sensitized solar cells

    NASA Astrophysics Data System (ADS)

    Sun, Panpan; Zhang, Ming; Ai, Changzhi; Wu, Zhixin; Lu, Shuang; Zhang, Xintong; Huang, Niu; Sun, Yihua; Sun, Xiaohua

    2016-07-01

    Considering the undesirable electrocatalytic activity toward I-/I3- redox system of prinstine antimony sulfide (Sb2S3) fabricated with the existing conditions, a mesoporous carbon nanoparticle film (CNP) is introduced here for in-situ growth of Sb2S3 to construct a Sb2S3@CNP hybrid catalyst. Based on a Sb-thiourea precursor solution, in-situ growth of Sb2S3 can be achieved via solution deposition (denoted as Sb2S3@CNP-S) as well as atmospheric pressure thermal evaporation (denoted as Sb2S3@CNP-T) in CNP matrix. Structural characterizations indicate that Sb2S3 particles have well dispersed in the pores of CNP matrix. Because of the introduction of porous and conductive CNP matrix to support Sb2S3, the hybrid catalyst exhibits lower charge transfer resistance at the catalyst/electrolyte interface and higher electrocatalytic activity. When used as counter electrode (CE) for dye-sensitized solar cells (DSSCs), devices using Sb2S3@CNP hybrid catalyst as CE produce fill factor of 67.6% and 66.3%, which is significantly higher than that using pristine Sb2S3 fabricated in our previous work (52.8%). Finally, the corresponding power conversion efficiencies reach 6.69% (Sb2S3@CNP-S) and 6.24% (Sb2S3@CNP-T), respectively, which are comparable to that using Pt CE measured under the same conditions (6.74%).

  9. Polymer precursors for ceramic composites

    NASA Technical Reports Server (NTRS)

    Hurwitz, Frances I.

    1986-01-01

    The fiber composite approach to reinforced ceramics provides the possibility of achieving ceramics with high fracture toughness relative to monolithics. Fabrication of ceramic composites, however, demands low processing temperatures to avoid fiber degradation. Formation of complex shapes further requires small diameter fibers as well as techniques for infiltrating the matrix between fibers. Polymers offer low temperature processability, control of rheology not available with ceramic powders, and should serve as precursors to matrix fibers. In recent years, a number of polysilanes and polysilezanes were investigated as potential presursors. A review of candidate polymers is presented, including recent studies of silsesquioxanes.

  10. Antiviral activity of platinum (II) and palladium (II) complexes of pyridine-2-carbaldehyde thiosemicarbazone.

    PubMed

    Varadinova, T; Kovala-Demertzi, D; Rupelieva, M; Demertzis, M; Genova, P

    2001-04-01

    A heterocyclic compound, pyridine-2-carbaldehyde thiosemicarbazone (HFoTsc), and its six metal coordinated bound complexes, three with platinum (II) and three with palladium (II), were studied for their activity against herpes simplex virus 1 (HSV-1) infection in cultured cells. According to their cytotoxicity the compounds were divided into two groups. Group I (cytotoxic compounds) included all three palladium complexes and [Pt(HFoTsc)2] Cl2, with maximum non-toxic concentration (MNC) of 1-10 micromol/l and a 50% cytotoxic concentration (CC50) of 20-100 micromol/l. Group 2 (low cytotoxic compounds) with MNC of 100 micromol/l and CC50 of 548-5820 micromol/l included compounds in the following order: [Pt(HFoTsc)2] Cl2

  11. Evaluation of the Anti-Schistosoma mansoni Activity of Thiosemicarbazones and Thiazoles

    PubMed Central

    de Oliveira, Sheilla Andrade; de Oliveira Filho, Gevânio Bezerra; Moreira, Diogo Rodrigo Magalhaes; Gomes, Paulo André Teixeira; da Silva, Anekécia Lauro; de Barros, Andréia Ferreira; da Silva, Aline Caroline; dos Santos, Thiago André Ramos; Pereira, Valéria Rêgo Alves; Gonçalves, Gabriel Gazzoni Araújo; Brayner, Fábio André; Alves, Luiz Carlos; Wanderley, Almir Gonçalves; Leite, Ana Cristina Lima

    2014-01-01

    Schistosomiasis is a chronic and debilitating disease caused by a trematode of the genus Schistosoma and affects over 207 million people. Chemotherapy is the only immediate recourse for minimizing the prevalence of this disease and involves predominately the administration of a single drug, praziquantel (PZQ). Although PZQ has proven efficacy, there is a recognized need to develop new drugs as schistosomicides since studies have shown that repeated use of this drug in areas of endemicity may cause a temporary reduction in susceptibility in isolates of Schistosoma mansoni. Hydrazones, thiosemicarbazones, phthalimides, and thiazoles are thus regarded as privileged structures used for a broad spectrum of activities and are potential candidates for sources of new drug prototypes. The present study determined the in vitro schistosomicidal activity of 10 molecules containing these structures. During the assays, parameters such motility and mortality, oviposition, morphological changes in the tegument, cytotoxicity, and immunomodulatory activity caused by these compounds were evaluated. The results showed that compounds formed of thiazole and phthalimide led to higher mortality of worms, with a significant decline in motility, inhibition of pairing and oviposition, and a mortality rate of 100% starting from 144 h of exposure. These compounds also stimulated the production of nitric oxide and tumor necrosis factor alpha (TNF-α), thereby demonstrating the presence of immunomodulatory activity. The phthalyl thiazole LpQM-45 caused significant ultrastructural alterations, with destruction of the tegument in both male and female worms. According to the present study, phthalyl thiazole compounds possess antischistosomal activities and should form the basis for future experimental and clinical trials. PMID:24165185

  12. Antibacterial, antifungal and in vitro antileukaemia activity of metal complexes with thiosemicarbazones

    PubMed Central

    Pahontu, Elena; Julea, Felicia; Rosu, Tudor; Purcarea, Victor; Chumakov, Yurie; Petrenco, Petru; Gulea, Aurelian

    2015-01-01

    1-phenyl-3-methyl-4-benzoyl-5-pyrazolone 4-ethyl-thiosemicarbazone (HL) and its copper(II), vanadium(V) and nickel(II) complexes: [Cu(L)(Cl)]·C2H5OH·(1), [Cu(L)2]·H2O (2), [Cu(L)(Br)]·H2O·CH3OH (3), [Cu(L)(NO3)]·2C2H5OH (4), [VO2(L)]·2H2O (5), [Ni(L)2]·H2O (6), were synthesized and characterized. The ligand has been characterized by elemental analyses, IR, 1H NMR and 13C NMR spectroscopy. The tridentate nature of the ligand is evident from the IR spectra. The copper(II), vanadium(V) and nickel(II) complexes have been characterized by different physico-chemical techniques such as molar conductivity, magnetic susceptibility measurements and electronic, infrared and electron paramagnetic resonance spectral studies. The structures of the ligand and its copper(II) (2, 4), and vanadium(V) (5) complexes have been determined by single-crystal X-ray diffraction. The composition of the coordination polyhedron of the central atom in 2, 4 and 5 is different. The tetrahedral coordination geometry of Cu was found in complex 2 while in complex 4, it is square planar, in complex 5 the coordination polyhedron of the central ion is distorted square pyramid. The in vitro antibacterial activity of the complexes against Escherichia coli, Salmonella abony, Staphylococcus aureus, Bacillus cereus and the antifungal activity against Candida albicans strains was higher for the metal complexes than for free ligand. The effect of the free ligand and its metal complexes on the proliferation of HL-60 cells was tested. PMID:25708540

  13. Nickel(ii) radical complexes of thiosemicarbazone ligands appended by salicylidene, aminophenol and aminothiophenol moieties.

    PubMed

    Kochem, Amélie; Gellon, Gisèle; Jarjayes, Olivier; Philouze, Christian; du Moulinet d'Hardemare, Amaury; van Gastel, Maurice; Thomas, Fabrice

    2015-07-28

    The nickel(ii) complexes of three unsymmetrical thiosemicarbazone-based ligands featuring a sterically hindered salicylidene (1), aminophenol (2) or thiophenol (3) moiety were synthesized and structurally characterized. The metal ion lies in an almost square planar geometry in all the complexes. The cyclic voltammetry (CV) curve of 1 shows an irreversible oxidation wave at E = 0.49 V, which is assigned to the phenoxyl/phenolate redox couple. The CV curves of 2 and 3 display a reversible one-electron oxidation wave (E1/2 = 0.26 and 0.22 V vs. Fc(+)/Fc, respectively) and an one-electron reduction wave (E1/2 = -1.55 and -1.46 V, respectively). The cations 2(+) and 3(+) as well as the anions 2(-) and 3(-) were generated. The EPR spectra of the cations in THF show a rhombic signal at g1 = 2.034, g2 = 2.010 and g3 = 1.992 (2(+)) and g1 = 2.069, g2 = 2.018, g3 = 1.986 (3(+)) that is consistent with a main radical character of the complexes. The difference in anisotropy is assigned to the different nature of the radical, iminosemiquinonate vs. iminothiosemiquinonate. The anions display an isotropic EPR signal at giso = 2.003 (2(+)) and 2.006 (3(+)), which is indicative of a main α-diimine radical character of the compounds. Both the anions and cations exhibit charge transfer transitions of low to moderate intensity in their visible spectrum. Quantum chemical calculations (B3LYP) reproduce both the g-values and Vis-NIR spectra of the complexes. The radical anions readily react with dioxygen to give the radical cations. 2(+) catalyzes the aerobic oxidation of benzyl alcohol into benzaldehyde. PMID:26086684

  14. Antibacterial, antifungal and in vitro antileukaemia activity of metal complexes with thiosemicarbazones.

    PubMed

    Pahontu, Elena; Julea, Felicia; Rosu, Tudor; Purcarea, Victor; Chumakov, Yurie; Petrenco, Petru; Gulea, Aurelian

    2015-04-01

    1-phenyl-3-methyl-4-benzoyl-5-pyrazolone 4-ethyl-thiosemicarbazone (HL) and its copper(II), vanadium(V) and nickel(II) complexes: [Cu(L)(Cl)]·C₂H₅OH·(1), [Cu(L)₂]·H₂O (2), [Cu(L)(Br)]·H₂O·CH₃OH (3), [Cu(L)(NO₃)]·2C₂H₅OH (4), [VO₂(L)]·2H₂O (5), [Ni(L)₂]·H₂O (6), were synthesized and characterized. The ligand has been characterized by elemental analyses, IR, (1) H NMR and (13) C NMR spectroscopy. The tridentate nature of the ligand is evident from the IR spectra. The copper(II), vanadium(V) and nickel(II) complexes have been characterized by different physico-chemical techniques such as molar conductivity, magnetic susceptibility measurements and electronic, infrared and electron paramagnetic resonance spectral studies. The structures of the ligand and its copper(II) (2, 4), and vanadium(V) (5) complexes have been determined by single-crystal X-ray diffraction. The composition of the coordination polyhedron of the central atom in 2, 4 and 5 is different. The tetrahedral coordination geometry of Cu was found in complex 2 while in complex 4, it is square planar, in complex 5 the coordination polyhedron of the central ion is distorted square pyramid. The in vitro antibacterial activity of the complexes against Escherichia coli, Salmonella abony, Staphylococcus aureus, Bacillus cereus and the antifungal activity against Candida albicans strains was higher for the metal complexes than for free ligand. The effect of the free ligand and its metal complexes on the proliferation of HL-60 cells was tested. PMID:25708540

  15. Distributions and impact factors of antimony in topsoils and moss in Ny-Ålesund, Arctic.

    PubMed

    Jia, Nan; Sun, Liguang; He, Xin; You, Kehua; Zhou, Xin; Long, Nanye

    2012-12-01

    The distribution of antimony (Sb) in topsoil and moss (Dicranum angustum) in disturbed and undisturbed areas, as well as coal and gangue, in Ny-Ålesund, Arctic was examined. Results show that the weathering of coal bed could not contribute to the increase of Sb concentrations in topsoil and moss in the study area. The distribution of Sb is partially associated with traffic and historical mining activities. The occurrence of the maximum Sb concentration is due to the contribution of human activities. In addition, the decrease of Sb content in topsoil near the coastline may be caused by the washing of seawater. Compared with topsoils, moss could be a useful tool for monitoring Sb in both highly and lightly polluted areas. PMID:22885219

  16. Synthesis and optical properties of antimony oxide glasses doped with holmium trioxide

    NASA Astrophysics Data System (ADS)

    Raghunatha, S.; Eraiah, B.

    2016-05-01

    Holmium doped lithium-antimony-lead borate glasses having 1mol% AgNO3 with composition 50B2O3-20PbO-25Sb2O3-5Li2O have been prepared using single step melt quenching technique. The XRD spectrum confirms amorphous nature of glasses. The optical absorbance studies were carried out on these glasses. The optical direct band gap energies were found to be in the range of 3.10 eV to 3.31 eV and indirect band gap energies were found to be in the range of 2.28 eV to 3.00 eV. The refractive indexes have been calculated by using Lorentz-Lorenz formula and the calculated values in the range of 2.31 to 2.37.

  17. Formation of the properties of antimony matrix alloys for frame-type composite materials

    NASA Astrophysics Data System (ADS)

    Gulevskii, V. A.; Antipov, V. I.; Vinogradov, L. V.; Kolmakov, A. G.; Lazarev, E. M.; Samarina, A. M.; Mukhina, Yu. E.

    2009-12-01

    A frame-type composite material (CM) produced upon impregnation represents a system consisting of a rigid porous frame and a matrix material filling its voids. When metals are used as a matrix material, they bring up specific problems related to melting of a metal, such as the thermal effect of the metal on the frame and the chemical interaction of the matrix and frame with the formation of brittle compounds. A CM that combines the best characteristics of its components can be produced. Since impregnation is, as a rule, performed under vacuum, melting of a matrix metal is accompanied by an increase in the evaporation rate. The evaporation of a matrix metal can be decreased by controlling its chemical composition, decreasing the melting temperature of the melt, and controlling the cooling rate. In this work, antimony alloys are used as a matrix material and their properties are studied.

  18. Sequential solvent extraction for forms of antimony in five selected coals

    SciTech Connect

    Qi, C.C.; Liu, G.J.; Kang, Y.; Chou, C.L.; Wang, R.W.

    2008-03-15

    Abundance of antimony in bulk samples has been determined in five selected coals, three coals from Huaibei Coalfield, Anhui, China, and two from the Illinois Basin in the United States. The Sb abundance in these samples is in the range of 0.11-0.43 {mu} g/g. The forms of Sb in coals were studied by sequential solvent extraction. The six forms of Sb are water soluble, ion changeable, organic matter bound, carbonate bound, silicate bound, and sulfide bound. Results of sequential extraction show that silicate-bound Sb is the most abundant form in these coals. Silicate-plus sulfide-bound Sb accounts for more than half of the total Sb in all coals. Bituminous coals are higher in organic matter bound Sb than anthracite and natural coke, indicating that the Sb in the organic matter may be incorporated into silicate and sulfide minerals during metamorphism.

  19. Antimony vibrations in skutterudites probed by 121Sb nuclear inelastic scattering

    SciTech Connect

    Wille, H. -C.; Hermann, R. P.; Sergueev, I.; Leupold, O.; van der Linden, P.; Sales, Brian C; Grandjean, F.; Long, G. J.; Ruffer, R.; Shvyd'ko, Yu. V.

    2007-01-01

    The antimony specific lattice dynamic properties in the unfilled and filled EuFe4Sb12 skutterudites have been determined by nuclear inelastic scattering at the 121Sb nuclear resonance energy of 37.1298(2) keV with a 4.5 meV high-resolution backscattering sapphire monochromator. The Sb partial vibrational density of states, DOS, shows a maximum centered at 17 and 16 meV in CoSb3 and EuFe4Sb12, respectively. The difference in the Sb DOS of CoSb3 and EuFe4Sb12 reveals that upon filling a transfer of 10% of the vibrational states towards lower energy occurs. Further, a likely indication of the coupling between the guest and the host lattice in rattler systems is observed, a coupling that is required to reduce the lattice thermal conductivity.

  20. Focused ion beam induced synthesis of a porous antimony nanowire network

    SciTech Connect

    Schoendorfer, Christoph; Lugstein, Alois; Hyun, Youn-Joo; Bertagnolli, Emmerich; Bischoff, Lothar; Nellen, Philipp M.; Callegari, Victor; Pongratz, Peter

    2007-08-15

    We present a focused ion beam-based approach for the synthesis of an antimony nanofiber network. The nanofibers, with a homogeneous distribution of diameters of about 25 nm and lengths up to several microns, are synthesized in a self-assembling process without any additional material source at room temperature. It is possible to recrystallize the as-grown amorphous nanofibers by moderate rapid thermal annealing at 473 K. These results have been verified by means of scanning electron microscopy, Auger electron spectroscopy, high-resolution transmission electron microscopy, selected area electron diffraction, and energy dispersive x-ray analysis. As this approach is not limited solely to the material discussed here, other substrates (e.g., GaSb and Ge) and ion sources should extend this method to other materials, which offers a great potential for future nanoscale devices and applications.

  1. Reaction of trimethylsilylacetylenes with antimony pentafluoride under matrix isolation conditions: experimental and computational study.

    PubMed

    Cicak, Helena; Vancik, Hrvoj; Mihalić, Zlatko

    2010-10-15

    Reaction of trimethylsilylacetylenes Me(3)SiC≡CR with SbF(5) in the solid state was investigated using matrix isolation infrared spectroscopy and quantum-mechanical calculations. Two reaction pathways were detected. Replacement of the trimethylsilyl group with SbF(4) produces neutral antimony acetylides F(4)SbC≡CR. Acetylenic bond protonation produces silyl cation 6-R, fully bridged for R = H and SiMe(3). High total charges on the bridging SiMe(3) group and low Me(3)Si-C bond orders to acetylenic moiety, both calculated at the MP4(SDQ)/6-311G(d,p) level of theory, indicate high silyl cation character of these species. PMID:20857942

  2. Sequential solvent extraction for forms of antimony in five selected coals

    USGS Publications Warehouse

    Qi, C.; Liu, Gaisheng; Kong, Y.; Chou, C.-L.; Wang, R.

    2008-01-01

    Abundance of antimony in bulk samples has been determined in five selected coals, three coals from Huaibei Coalfield, Anhui, China, and two from the Illinois Basin in the United States. The Sb abundance in these samples is in the range of 0.11-0.43 ??g/g. The forms of Sb in coals were studied by sequential solvent extraction. The six forms of Sb are water soluble, ion changeable, organic matter bound, carbonate bound, silicate bound, and sulfide bound. Results of sequential extraction show that silicate-bound Sb is the most abundant form in these coals. Silicate- plus sulfide-bound Sb accounts for more than half of the total Sb in all coals. Bituminous coals are higher in organic matterbound Sb than anthracite and natural coke, indicating that the Sb in the organic matter may be incorporated into silicate and sulfide minerals during metamorphism. ?? 2008 by The University of Chicago. All rights reserved.

  3. Microbial diversity and community structure in an antimony-rich tailings dump.

    PubMed

    Xiao, Enzong; Krumins, Valdis; Dong, Yiran; Xiao, Tangfu; Ning, Zengping; Xiao, Qingxiang; Sun, Weimin

    2016-09-01

    To assess the impact of antimony (Sb) on microbial community structure, 12 samples were taken from an Sb tailings pile in Guizhou Province, Southwest China. All 12 samples exhibited elevated Sb concentrations, but the mobile and bioaccessible fractions were small in comparison to total Sb concentrations. Besides the geochemical analyses, microbial communities inhabiting the tailing samples were characterized to investigate the interplay between the microorganisms and environmental factors in mine tailings. In all samples, Proteobacteria and Actinobacteria were the most dominant phyla. At the genus level, Thiobacillus, Limnobacter, Nocardioides, Lysobacter, Phormidium, and Kaistobacter demonstrated relatively high abundances. The two most abundant genera, Thiobacillus and Limnobacter, are characterized as sulfur-oxidizing bacteria and thiosulfate-oxidizing bacteria, respectively, while the genus Lysobacter contains arsenic (As)-resistant bacteria. Canonical correspondence analysis (CCA) indicates that TOC and the sulfate to sulfide ratio strongly shaped the microbial communities, suggesting the influence of the environmental factors in the indigenous microbial communities. PMID:27188777

  4. Properties of antimony doped ZnO thin films deposited by spray pyrolysis technique

    SciTech Connect

    Sadananda Kumar, N. Bangera, Kasturi V.; Shivakumar, G. K.

    2015-07-15

    Antimony (Sb) doped zinc oxide (ZnO) thin films were deposited on the glass substrate at 450°C using spray pyrolysis technique. Effect of Sb doping on surface morphology structural, optical and electrical properties were studied. X-ray diffraction (XRD) analysis showed that both the undoped and doped ZnO thin films are polycrystalline in nature with (101) preferred orientation. SEM analysis showed a change in surface morphology of Sb doped ZnO thin films. Doping results in a marked increase in conductivity without affecting the transmittance of the films. ZnO films prepared with 3 at % Sb shows the lowest resistivity of 0.185 Ohm cm with a Hall mobility of 54.05 cm{sup 2} V{sup –1} s{sup –1}, and a hole concentration of 6.25 × 10{sup 17} cm{sup –3}.

  5. A novel composite material based on antimony(III) oxide and amorphous silica

    SciTech Connect

    Zemnukhova, Ludmila A.; Panasenko, Alexander E.

    2013-05-01

    The composite material nSb₂O₃·mSiO₂·xH₂O was prepared by hydrolysis of SbCl₃ and Na₂SiO₃ in an aqueous medium. It has been shown that the composition of the material is influenced by the ratio of the initial components and the acidity of the reaction medium. The morphology of the material particles and its specific surface area have been determined. The thermal and optic properties were also investigated. - Graphical abstract: Novel composite material containing amorphous silica and crystal antimony(III) oxide has been synthesized by hydrolysis of SbCl₃ and Na₂SiO₃ in an aqueous medium. Highlights: • The composite material nSb₂O₃·mSiO₂·xH₂O was prepared in an aqueous medium. • The composition of the material is controllable by a synthesis conditions. • The morphology of the material and its optic properties have been determined.

  6. Rashba effect in single-layer antimony telluroiodide SbTeI

    SciTech Connect

    Zhuang, Houlong L.; Cooper, Valentino R.; Xu, Haixuan; Ganesh, P.; Hennig, Richard G.; Kent, P. R. C.

    2015-09-04

    Exploring spin-orbit coupling (SOC) in single-layer materials is important for potential spintronics applications. In this paper, using first-principles calculations, we show that single-layer antimony telluroiodide SbTeI behaves as a two-dimensional semiconductor exhibiting a G0W0 band gap of 1.82 eV. More importantly, we observe the Rashba spin splitting in the SOC band structure of single-layer SbTeI with a sizable Rashba coupling parameter of 1.39 eV Å, which is significantly larger than that of a number of two-dimensional systems including surfaces and interfaces. The low formation energy and real phonon modes of single-layer SbTeI imply that it is stable. Finally, our study suggests that single-layer SbTeI is a candidate single-layer material for applications in spintronics devices.

  7. Synthesis of antimony-doped tin oxide (ATO) nanoparticles by the nitrate-citrate combustion method

    SciTech Connect

    Zhang Jianrong; Gao Lian . E-mail: Liangaoc@online.sh.cn

    2004-12-02

    Antimony-doped tin oxide (ATO) nanoparticles having rutile structure have been synthesized by the combustion method using citric acid (CA) as fuel and nitrate as an oxidant, the metal sources were granulated tin and Sb{sub 2}O{sub 3}. The influence of citric acid (fuel) to metal ratio on the average crystallite size, specific surface area and morphology of the nanoparticles has been investigated. X-ray diffraction showed the tin ions were reduced to elemental tin during combustion reaction. The average ATO crystallite size increased with the increase of citric acid (fuel). Powder morphology and the comparison of crystallite size and grain size shows that the degree of agglomeration of the powder decreased with an increase of the ratio. The highest specific surface area was 37.5 m{sup 2}/g when the citric acid to tin ratio was about 6.

  8. The electrical characterizations of selenium (Se) doped gallium antimony (GaSb) single crystal

    NASA Astrophysics Data System (ADS)

    Choudhari, Rashmi; Deshpande, Manisha; Maske, Dilip; Gadkari, Dattatray

    2016-05-01

    The growth of Se doped GaSb bulk crystal is carried out using Vertical directional solidification (VDS) technique. High purity Gallium and Antimony is taken as source material and selenium as doping material. From grown ingot substrate were obtained in wafer form using diamond cutter. The electrical characteristics such as Hall measurement is used to find the carrier concentration and mobility, while Van der pauw for measuring resistivity of the sample The GaSb:Se sample shows high resistivity and mobility. The grown crystal was detached from the ampoule wall with high crystal quality. The measured resistivity of GaSb:Se is 9.9×10-3ohm-cm, the mobility is 1464cm3/Vsec and carrier concentration is 5.08×1017 per cm3.

  9. Focused ion beam induced synthesis of antimony nanowires for gas sensor applications

    NASA Astrophysics Data System (ADS)

    Schoendorfer, Christoph; Hetzel, Martin; Pongratz, Peter; Lugstein, Alois; Bertagnolli, Emmerich

    2012-11-01

    In this paper the formation of antimony (Sb) nanowires (NWs) by a focused Ga ion beam approach and their gas sensing capability is reported. The NWs with uniform diameters of only 25 nm and lengths up to several microns are synthesized at predefined positions at room temperature in an ion beam induced self-assembling process. Then individual Sb-NWs are deposited on insulating substrates and provided with gold electrodes. Subsequently sensing characteristics of individual Sb-NWs are investigated at room temperature for H2O, CO, H2, He, O2 and ethanol over a wide concentration range. The Sb-NWs exhibit selective sensing properties for ethanol and H2O with exceptional sensitivities of more than 17 000 and 60 000, respectively.

  10. Assessment of Hybrid Organic-Inorganic Antimony Sulfides for Earth-Abundant Photovoltaic Applications.

    PubMed

    Yang, Ruo Xi; Butler, Keith T; Walsh, Aron

    2015-12-17

    Hybrid organic-inorganic solar absorbers are currently the subject of intense interest; however, the highest-performing materials contain Pb. Here we assess the potential of three Sb-based semiconductors: (i) Sb2S3, (ii) Cs2Sb8S13, and (iii) (CH3NH3)2Sb8S13. While the crystal structure of Sb2S3 is composed of 1D chains, 2D layers are formed in the ternary cesium and hybrid methylammonium antimony sulfide compounds. In each case, a stereochemically active Sb 5s(2) lone pair is found, resulting in a distorted coordination environment for the Sb cations. The bandgap of the binary sulfide is found to increase, while the ionization potential also changes, upon transition to the more complex compounds. Based on the predicted electronic structure, device configurations are suggested to be suitable for photovoltaic applications. PMID:26624204

  11. Suppression of Grain Growth by Additive in Nanostructured P-type Bismuth Antimony Tellurides

    SciTech Connect

    Zhang, Qian; Zhang, Qinyong; Chen, S.; Liu, W S; Lukas, K; Yan, X; Wang, H; Wang, D.; Opeil, C; Chen, Gang; Ren, Z. F.

    2011-01-01

    Grain growth is a major issue in the preparation of nanostructured bismuth-antimony-tellurides during hot pressing the nanopowders into dense bulk samples. To prevent grain agglomeration during ball milling and growth during hot pressing, organic agent (Oleic Acid, OA) as additive was added into the materials at the beginning of the ball milling process. With different concentrations of OA (0.5, 1.0, 1.5, 2.0, and 2.5 wt%), grains with different sizes are obtained. Structural analysis clearly shows that it is the particle size of the nanopowders that determines the final grain size in the densely compacted bulk samples. A combination of small grains ~200–500 nm and nanopores leads to effective phonon scattering, which results in the decrease of lattice thermal conductivity, and ZT of ~1.3 at 373 K for the sample with 2.0 wt% OA.

  12. Novel fabrication of an electrochromic antimony-doped tin oxide film using a nanoparticle deposition system

    NASA Astrophysics Data System (ADS)

    Kim, Hyungsub; Park, Yunchan; Choi, Dahyun; Ahn, Sung-Hoon; Lee, Caroline Sunyong

    2016-07-01

    Novel deposition method of Antimony-doped tin oxide (ATO) thin films was introduced using a nanoparticle deposition system (NPDS) to fabricate an electrochromic (EC) device. NPDS is a dry deposition method that simplifies the ATO deposition process by eliminating the need for solvents or binders. In this study, an ATO EC layer was deposited using NPDS. The surface morphology and electrochemical and optical transmittance properties were characterized. The optical transmittance change in the ATO EC device was ∼35% over the wavelength range of 350-800 nm, and the cyclic transmittance was stable. The ATO film deposited using NPDS, exhibited a coloration efficiency of 15.5 cm2 C-1. Therefore, our results suggest that ATO EC devices can be fabricated using a simple, cost-effective NPDS, which allows nanoparticles to be deposited directly without pre- or post-processing.

  13. First-Principles Study of Antimony Doping Effects on the Iron-Based Superconductor CaFe(SbxAs1-x)2

    NASA Astrophysics Data System (ADS)

    Nagai, Yuki; Nakamura, Hiroki; Machida, Masahiko; Kuroki, Kazuhiko

    2015-09-01

    We study antimony doping effects on the iron-based superconductor CaFe(SbxAs1-x)2 by using the first-principles calculation. The calculations reveal that the substitution of a doped antimony atom into As of the chainlike As layers is more stable than that into FeAs layers. This prediction can be checked by experiments. Our results suggest that doping homologous elements into the chainlike As layers, which only exist in the novel 112 system, is responsible for rising up the critical temperature. We discuss antimony doping effects on the electronic structure. It is found that the calculated band structures with and without the antimony doping are similar to each other within our framework.

  14. A New ABC Half-Transporter in Leishmania major Is Involved in Resistance to Antimony

    PubMed Central

    Manzano, J. I.; García-Hernández, R.; Castanys, S.

    2013-01-01

    The characterization of ABCI4, a new intracellular ATP-binding cassette (ABC) half-transporter in Leishmania major, is described. We show that ABCI4 is involved in heavy metal export, thereby conferring resistance to Pentostam, to Sb(III), and to As(III) and Cd(II). Parasites overexpressing ABCI4 showed a lower mitochondrial toxic effect of antimony by decreasing reactive oxygen species production and maintained higher values of both the mitochondrial electrochemical potential and total ATP levels with respect to controls. The ABCI4 half-transporter forms homodimers as determined by a coimmunoprecipitation assay. A combination of subcellular localization studies under a confocal microscope and a surface biotinylation assay using parasites expressing green fluorescent protein- and FLAG-tagged ABCI4 suggests that the transporter presents a dual localization in both mitochondria and the plasma membrane. Parasites overexpressing ABCI4 present an increased replication in mouse peritoneal macrophages. We have determined that porphyrins are substrates for ABCI4. Consequently, the overexpression of ABCI4 confers resistance to some toxic porphyrins, such as zinc-protoporphyrin, due to the lower accumulation resulting from a significant efflux, as determined using the fluorescent zinc-mesoporphyrin, a validated heme analog. In addition, ABCI4 has a significant ability to efflux thiol after Sb(III) incubation, thus meaning that ABCI4 could be considered to be a potential thiol-X-pump that is able to recognize metal-conjugated thiols. In summary, we have shown that this new ABC transporter is involved in drug sensitivity to antimony and other compounds by efflux as conjugated thiol complexes. PMID:23716044

  15. Arsenic and antimony determination by on-line flow hydride generation glow discharge optical emission detection

    NASA Astrophysics Data System (ADS)

    Guillermo Orellana-Velado, Néstor; Fernández, Matilde; Pereiro, Rosario; Sanz-Medel, Alfredo

    2001-01-01

    Hollow cathode (HC) and conventional flat cathode (FC) glow discharge (GD) optical emission spectrometry (OES) were used as detectors for the determination of arsenic and antimony by on-line hydride generation (HG) in a flow system. Both radiofrequency (rf) and direct current (dc) sources were investigated to produce the discharge. The design of the HC and FC and also the parameters governing the discharge (pressure, He flow rate, voltage, current and delivered power) and the HG (sodium borohydride concentration and reagent flow rates) were investigated using both cathodes. The analytical performance characteristics of HG-GD-OES with HC and FC were evaluated for some emission lines of arsenic (193.7, 200.3, 228.8 and 234.9 nm). The best detection limit (0.2 μg l -1) was obtained when the emission line of 228.8 nm was used with FC. Under the same arsenic optimized experimental conditions, the system was evaluated to determine antimony at 259.7, 252.7 and 231.1 nm, 252.7 nm being the emission line which produced the best detection limit (0.7 μg l -1). The rf-HC-GD-OES system was applied successfully to the determination of arsenic in freeze-dried urine in the standard reference material 2670 from NIST. Finally, a flow injection system was assayed to determine arsenic at 228.8 nm, using a dc-GD with both FC and HC. The results indicated that for low volumes of sample, the HC discharge allows better analytical signals than the FC.

  16. Optical properties of Eu3+-doped antimony-oxide-based low phonon disordered matrices

    NASA Astrophysics Data System (ADS)

    Som, Tirtha; Karmakar, Basudeb

    2010-01-01

    A new series of monolithic Eu2O3-doped high antimony oxide (40-80 mol%) content disordered matrices (glasses) of low phonon energy (about 600 cm-1) in the K2O-B2O3-Sb2O3 (KBS) system was prepared by the melt-quench technique. Infrared reflection spectroscopy was used to establish the low phonon energy of the glasses. Amorphicity and devitrification of the glasses were confirmed by x-ray diffraction analysis. UV-vis absorption spectra of Eu3+ have been measured and the band positions have been justified with quantitative calculation of the nephelauxetic parameter and covalent bonding characteristics of the host. These Eu2O3-doped glasses upon excitation at 393 nm radiation exhibit six emission bands in the range 500-750 nm due to their low phonon energy. Of these, the magnetic dipole ^{5}\\mathrm {D}_{0} \\to {}^{7} \\mathrm {F_{1}} transition shows small Stark splitting while the electric dipole ^{5}\\mathrm {D}_{0} \\to {}^{7}\\mathrm {F}_{2} transition undergoes remarkable Stark splitting into two components. They have been explained by the crystal field effect. The Judd-Ofelt parameters, Ωt = 2,4,6, were also evaluated and the change of Ωt with the glass composition was correlated with the asymmetric effect at Eu3+ ion sites and the fundamental properties like covalent character and optical basicity. We are the first to report the spectroscopic properties of the Eu3+ ion in KBS low phonon antimony glasses.

  17. The effect of phosphate application on the mobility of antimony in firing range soils.

    PubMed

    Griggs, Christopher S; Martin, W Andy; Larson, Steven L; O'Connnor, Greg; Fabian, Gene; Zynda, Greg; Mackie, David

    2011-05-15

    Chemical and biogenic sources of phosphate are commonly accepted in situ treatment methods for immobilization of lead (Pb) in soil. The metalloid antimony (Sb), commonly associated with Pb in the environment, exists as either a neutral species or a negatively charged oxyanion. Antimony is used in the manufacture of bullets as a hardening agent, constituting approximately 3% of the bullet mass. Technological solutions to reduce the migration of metals from small arms firing range (SAFR) soils for environmental compliance purposes must be robust with respect to multi-component systems containing both cationic and anionic contaminants. The effect of varying physico-chemical soil properties on Sb mobility post-firing was assessed in this study for six soil types using common analytical protocols and methods related to regulatory criteria. The sands (SM and SP) demonstrated the greatest Sb solubility in post-firing leachate samples and therefore were selected to evaluate the effects of five commercially available stabilization amendments on Sb mobility. Enhanced Sb leaching was experimentally confirmed in the phosphate-treated soils compared to both the untreated control soil and the sulfur-based amendment, and thus suggests competition for negative sorption sites between Sb and phosphate. However, the 5% Buffer Block® calcium phosphate amendment did not exhibit the same enhanced Sb release. This can be attributed to the inclusion of aluminum hydroxide in the amendment composition. Technologies are needed that will adequately immobilize Pb without mobilizing oxyanions such as Sb. Further research will be required to elucidate binding mechanisms and redox conditions that govern the mobility of Sb on SAFRs. PMID:21440928

  18. The origin and behavior of lead, cadmium and antimony in MSW incinerator

    SciTech Connect

    Nakamura, Kazuo; Kinoshita, Sayuri; Takatsuki, Hiroshi

    1996-12-31

    The Amendment to the Waste Disposal and Public Cleansing Law in Japan has introduced new regulation of waste requiring strict management. In this regulation, the fly ash generated in the Municipal Solid Waste (MSW) incinerator process was designated as specially controlled solid waste because of relatively high concentrations of lead and cadmium. Furthermore, antimony is a regulated constituent within the Basel Convention on the control of transboundary movements of hazardous wastes and their disposal and was designated a monitor item of environmental standards on water pollution. Thus, in order to understand where the problems lie, the behaviors of these heavy metals in the MSW incinerator was investigated. Also investigated were the kinds of products causing the fly ash to be contaminated. As a result, the amount of lead, cadmium and antimony in household waste was about 120, 3.5 and 7.6 g/T, respectively. The major origins of Pb, Cd and Sb from household waste are small sealed lead batteries, nickel-cadmium batteries and flame-proofed products such as curtains and plastic covers. By incineration treatment, these metals shifted to the fly ash (EP ash); the transfer ratio of Pb, Cd and Sb was about 33, 92 and 45%, respectively. The observed results indicated that the partitioning of metals in the MSW incinerator showed the influence of the vapor pressure of the elements and their compounds. Clearly, to produce precise estimates of this behavior, it will be necessary to determine not only the concentration of the elements in the waste but also the compounds used and the changes these would undergo in the furnace. Finally, several measures which will be helpful in solving these problems are introduced to discuss the future direction of environmentally-friendly social systems.

  19. Speciation of inorganic antimony (III & V) employing polyurethane foam loaded with bromopyrogallol red.

    PubMed

    Vinhal, Jonas O; Gonçalves, Aline D; Cruz, Graziela F B; Cassella, Ricardo J

    2016-04-01

    In this work, the speciation analysis of inorganic antimony (Sb(III) and Sb(V)) is proposed using polyurethane foam loaded with bromopyrogallol red (PUF-BPR) as a selective sorbent for Sb(III). The quantification of Sb in the solutions was performed by graphite furnace atomic absorption spectrometry (GF AAS), and several variables that could affect the performance of the method were carefully evaluated. The best conditions for the sorption of Sb(III) were achieved by shaking 50mg of PUF-BPR with the solutions containing Sb(III) at pH 4.0 for 90 min. In this condition, the retention of Sb(V) was not significant, whereas the removal of Sb(III) from the solution was higher than 95%. The desorption of Sb(III) from loaded PUF-BPR was possible by shaking the loaded foam with 7.5 mL of a 2.5 mol L(-1) HNO3 solution for 30 min. No interference of metal cations was observed on the solid-phase extraction of Sb(III) by PUF-BPR. The developed method was applied in the speciation analysis of antimony in river water samples fortified with different concentrations of Sb(III) and Sb(V). Also, we performed the determination of Sb(III) in a sample of a Sb-based drug utilized in the treatment of leishmaniasis. The results show that Sb(III) can be separated from high concentrations of Sb(V), since recoveries in the range of 81-110% were obtained in the analysis of the samples. The method presented limits of detection and quantification of 0.6 and 2 µg L(-1), respectively, for Sb(III) and 1 and 3 µg L(-1) for Sb(V), respectively. PMID:26838441

  20. Annealing of aromatic polyimide precursors

    NASA Technical Reports Server (NTRS)

    Wakelyn, N. T.

    1975-01-01

    A study has been made of the thermal behavior of polyimide precursors: an isomeric pair of crystals of the complex formed by p-phenylenediamine with the separated isomers of the di-isopropyl ester of pyromellitic acid. Specimens of this material were isothermally annealed in the temperature range 120 C to 170 C for periods of time up to 1 week. Although this temperature range is well below that customarily used for imidizations, the working hypothesis was that it would be more likely that a polymer embodying at least part of the precursor structure could be formed if the molecular motion was minimized to that actually required for the formation of the imide linkage. The progress of the annealing was followed by: infrared spectroscopy, differential thermal analysis, powder X-ray diffraction, and thermal gravimetric analysis. Single crystal X-ray analysis of the meta monomer yields a structure of chains of alternating acid and base and suggests that this monomer is amenable to polymerization with a minimum of geometrical disruption.

  1. Cross-resistance of Leishmania infantum isolates to nitric oxide from patients refractory to antimony treatment, and greater tolerance to antileishmanial responses by macrophages.

    PubMed

    de Moura, Tatiana R; Santos, Micheli Luize Barbosa; Braz, Juciene M; Santos, Luis Felipe V C; Aragão, Matheus T; de Oliveira, Fabricia A; Santos, Priscila L; da Silva, Ângela Maria; de Jesus, Amélia Ribeiro; de Almeida, Roque P

    2016-02-01

    Visceral leishmaniasis is a life-threatening disease characterized by intense parasitism of the spleen, liver, and bone marrow. Antimonials have served as front-line antileishmanial therapeutics for decades, but the increasing failure rates under antimonial treatment have challenged the continued use of these drugs. Pentavalent antimonials are known to reinforce the killing mechanisms of macrophages, although the associated mechanism remains unclear. Here, for the first time, we determined whether Leishmania infantum strains isolated from patients refractory to antimony treatment (relapse cases) were cross-resistant to antimonials, liposomal amphotericin B, and/or nitric oxide, and also whether these strains modulate macrophage infection. We selected four clinical isolates from relapse cases and two clinical isolates from antimony-responsive patients (control group) for the present study. The L. infantum promastigotes from all four relapse cases were resistant to trivalent antimonial treatment and nitric oxide, while only one isolate was resistant to liposomal amphotericin B. We evaluated whether the resistant strains from relapse cases showed enhanced infectivity and amastigote survival in macrophages, or macrophage-killing mechanisms in macrophages activated by lipopolysaccharide plus interferon gamma. Infection indexes calculated using macrophages infected with isolates from relapse were higher than those observed with control strains that were stimulated independently. Macrophage infection was higher with L. infantum isolates from relapse cases and correlated with enhanced interleukin 1-β production but showed similar nitrite production. Our results demonstrate that L. infantum field isolates from relapse cases were resistant to antimonials and nitric oxide and that these parasites stimulated inflammatory cytokines and were resistant to macrophage-killing mechanisms, factors that may contribute to disease severity. PMID:26481489

  2. Decreased antimony uptake and overexpression of genes of thiol metabolism are associated with drug resistance in a canine isolate of Leishmania infantum.

    PubMed

    Gómez Pérez, Verónica; García-Hernandez, Raquel; Corpas-López, Victoriano; Tomás, Ana M; Martín-Sanchez, Joaquina; Castanys, Santiago; Gamarro, Francisco

    2016-08-01

    Visceral leishmaniasis (VL) caused by the protozoan parasite Leishmania infantum, is one of the most important zoonotic diseases affecting dogs and humans in the Mediterranean area. The presence of infected dogs as the main reservoir host of L. infantum is regarded as the most significant risk for potential human infection. We have studied the susceptibility profile to antimony and other anti-leishmania drugs (amphotericin B, miltefosine, paromomycin) in Leishmania infantum isolates extracted from a dog before and after two therapeutic interventions with meglumine antimoniate (subcutaneous Glucantime(®), 100 mg/kg/day for 28 days). After the therapeutic intervention, these parasites were significantly less susceptible to antimony than pretreatment isolate, presenting a resistance index of 6-fold to Sb(III) for promastigotes and >3-fold to Sb(III) and 3-fold to Sb(V) for intracellular amastigotes. The susceptibility profile of this resistant L. infantum line is related to a decreased antimony uptake due to lower aquaglyceroporin-1 expression levels. Additionally, other mechanisms including an increase in thiols and overexpression of enzymes involved in thiol metabolism, such as ornithine decarboxylase, trypanothione reductase, mitochondrial tryparedoxin and mitochondrial tryparedoxin peroxidase, could contribute to the resistance as antimony detoxification mechanisms. A major contribution of this study in a canine L. infantum isolate is to find an antimony-resistant mechanism similar to that previously described in other human clinical isolates. PMID:27317865

  3. Remediation of antimony-rich mine waters: Assessment of antimony removal and shifts in the microbial community of an onsite field-scale bioreactor.

    PubMed

    Sun, Weimin; Xiao, Enzong; Kalin, Margarete; Krumins, Valdis; Dong, Yiran; Ning, Zengping; Liu, Tong; Sun, Min; Zhao, Yanlong; Wu, Shiliang; Mao, Jianzhong; Xiao, Tangfu

    2016-08-01

    An on-site field-scale bioreactor for passive treatment of antimony (Sb) contamination was installed downstream of an active Sb mine in Southwest China, and operated for one year (including a six month monitoring period). This bioreactor consisted of five treatment units, including one pre-aerobic cell, two aerobic cells, and two microaerobic cells. With the aerobic cells inoculated with indigenous mine water microflora, the bioreactor removed more than 90% of total soluble Sb and 80% of soluble antimonite (Sb(III)). An increase in pH and decrease of oxidation-reduction potential (Eh) was also observed along the flow direction. High-throughput sequencing of the small subunit ribosomal RNA (SSU rRNA) gene variable (V4) region revealed that taxonomically diverse microbial communities developed in the bioreactor. Metal (loid)-oxidizing bacteria including Ferrovum, Thiomonas, Gallionella, and Leptospirillum, were highly enriched in the bioreactor cells where the highest total Sb and Sb(III) removal occurred. Canonical correspondence analysis (CCA) indicated that a suite of in situ physicochemical parameters including pH and Eh were substantially correlated with the overall microbial communities. Based on an UPGMA (Unweighted Pair Group Method with Arithmetic Mean) tree and PCoA (Principal Coordinates Analysis), the microbial composition of each cell was distinct, indicating these in situ physicochemical parameters had an effect in shaping the indigenous microbial communities. Overall, this study was the first to employ a field-scale bioreactor to treat Sb-rich mine water onsite and, moreover, the findings suggest the feasibility of the bioreactor in removing elevated Sb from mine waters. PMID:27208755

  4. Premarital precursors of marital infidelity.

    PubMed

    Allen, Elizabeth S; Rhoades, Galena Kline; Stanley, Scott M; Markman, Howard J; Williams, Tamara; Melton, Jessica; Clements, Mari L

    2008-06-01

    Premarital precursors of infidelity were evaluated in a sample of 72 couples (N = 144) who were taking part in a longitudinal study of marriage. Premarital self-report and observational data were compared for couples who experienced infidelity and those who did not experience infidelity in the first years of marriage. Couples in which the male engaged in marital infidelity were characterized, premaritally, by significantly lower male sexual satisfaction, lower male positive communication, and higher female invalidation, whereas couples in which the female went on to engage in infidelity were characterized, premaritally, by significantly lower levels of female positive communication, higher levels of male and female negative communication, and higher levels of male and female invalidation. Implications of the findings for future research on the prediction and prevention of infidelity are discussed. PMID:18605124

  5. Precursors for Carbon Nitride Synthesis

    SciTech Connect

    Prashantha, M.; Gopal, E. S. R.; Ramesh, K.

    2011-07-15

    Nano structured carbon nitride films were prepared by pyrolysis assisted chemical vapour deposition. Pyrrole (C{sub 4}H{sub 5}N), Pyrrolidine (C{sub 4}H{sub 9}N), Azabenzimidazole (C{sub 6}H{sub 5}N{sub 3}) and Triazine (C{sub 6}H{sub 15}N{sub 3}) were used as precursors. The vibrational modes observed for C-N and C = N from FTIR spectra confirms the bonding of nitrogen with carbon. XPS core level spectra of C 1s and N 1s also show the formation of bonding between carbon and nitrogen atoms. The nitrogen content in the prepared samples was found to be around 25 atomic %.

  6. Cyanide and antimony thermodynamic database for the aqueous species and solids for the EPA-MINTEQ geochemical code

    SciTech Connect

    Sehmel, G.A.

    1989-05-01

    Thermodynamic data for aqueous species and solids that contain cyanide and antimony were tabulated from several commonly accepted, published sources of thermodynamic data and recent journal article. The review does not include gases or organic complexes of either antimony or cyanide, nor does the review include the sulfur compounds of cyanide. The basic thermodynamic data, ..delta..G/sub f,298//sup o/, ..delta..H/sub f,298//sup o/, and S/sub f//sup o/ values, were chosen to represent each solid phase and aqueous species for which data were available in the appropriate standard state. From these data the equilibrium constants (log K/sub r,298//sup o/) and enthalpies of reaction (..delta..H/sub r,298//sup o/) at 298 K (25/degree/C) were calculated for reactions involving the formation of these aqueous species and solids from the basic components. 34 refs., 14 tabs.

  7. Antimony incorporation in InAs quantum dots grown on GaAs substrate by molecular beam epitaxy

    NASA Astrophysics Data System (ADS)

    Rihani, J.; Sallet, V.; Christophe, H. J.; Oueslati, M.; Chtourou, R.

    2008-01-01

    We have grown InAs(Sb) quantum dots (QDs) on GaAs (0 0 1) substrates by molecular beam epitaxy (MBE) using two different antimony exposures ( ΦSb). Atomic force microscopy (AFM) and photoluminescence (PL) spectroscopy were carried out to investigate the dot size evolution as function of the incorporated antimony content in InAs/GaAs QDs material. Anomalous asymmetric-band feature was observed in room temperature photoluminescence (RTPL) spectra of the investigated QD samples grown at relatively high temperature (490 °C). From the temperature-dependent PL measurements, it was found that the asymmetric-band feature is associated with the ground-states transitions from QDs with bimodal size distribution. The analysis of the pump power dependent PL spectra allows us to suggest a type II band lineup for the InAsSb/GaAs QDs materials system.

  8. Sensitive spectrophotometric assay for 3-hydroxy-substituted flavonoids, based on their binding with molybdenum, antimony, or bismuth.

    PubMed

    Viswanathan, P; Sriram, V; Yogeeswaran, G

    2000-07-01

    A sensitive spectrophotometric assay has been developed for flavonoids based on their binding with molybdenum, antimony, or bismuth. Acetylation of the hydroxyl group of flavonoids abolished metal binding, thus suggesting a direct role of the hydroxyl groups. From a comparison of several related flavonoids differing in the position of hydroxyl substitutions, the hydroxyl group at position 3 was found to be an important requirement for the formation of a yellow complex. This flavonoid metal complex showed that a specific and significant bathochromic shift in the visible spectrum of the native flavonoid and the corresponding lambda(max) value was used for the colorimetric assays with different metal salts. The molybdenum complex was found to yield higher absorbance compared to antimony and bismuth complexes of various flavonoids. The present method offers a sensitive assay in the 5-25 nM range for these flavonoids and gave comparable results with HPLC quantitative determination. PMID:10898625

  9. Functional analyses and treatment of precursor behavior.

    PubMed

    Najdowski, Adel C; Wallace, Michele D; Ellsworth, Carrie L; MacAleese, Alicia N; Cleveland, Jackie M

    2008-01-01

    Functional analysis has been demonstrated to be an effective method to identify environmental variables that maintain problem behavior. However, there are cases when conducting functional analyses of severe problem behavior may be contraindicated. The current study applied functional analysis procedures to a class of behavior that preceded severe problem behavior (precursor behavior) and evaluated treatments based on the outcomes of the functional analyses of precursor behavior. Responding for all participants was differentiated during the functional analyses, and individualized treatments eliminated precursor behavior. These results suggest that functional analysis of precursor behavior may offer an alternative, indirect method to assess the operant function of severe problem behavior. PMID:18468282

  10. 1994 Accident sequence precursor program results

    SciTech Connect

    Belles, R.J.; Cletcher, J.W.; Copinger, D.A.

    1996-01-01

    The Accident Sequence Precursor (ASP) Program involves the systematic review and evaluation of operational events that have occurred at light-water reactors to identify and categorize precursors to potential severe core damage accident sequences. The results of the ASP Program are published in an annual report. The most recent report, which contains the analyses of the precursors for 1994, is NUREG/CR-4674, Vols. 21 and 22, Precursors to Potential Severe Core Damage Accidents: 1994, A Status Report, published in December 1995. This article provides an overview of the ASP review and evaluation process and a summary of the results for 1994. 12 refs., 2 figs., 4 tabs.

  11. 1995 Accident Sequence Precursor (ASP) Program results

    SciTech Connect

    Muhlheim, M.D.; Belles, R.J.; Cletcher, J.W.; Copinger, D.A.; O`Reilly, P.D.; Dolan, B.W.; Minarick, J.W.

    1997-01-01

    The Accident Sequence Precursor (ASP) Program involves the systematic review and evaluation of operational events that have occurred at light-water reactors to identify and categorize precursors to potential severe core damage accident sequences. The results of the ASP Program are published in an annual report. The most recent report, which contains the precursors for 1995, is NUREG/CR-4674, Volume 23, Precursors to Potential Severe Core Damage Accidents: 1995, A Status Report, published in April 1997. This article provides an overview of the ASP review and evaluation process and a summary of the results for 1995.

  12. Miltefosine and Antimonial Drug Susceptibility of Leishmania Viannia Species and Populations in Regions of High Transmission in Colombia

    PubMed Central

    Fernández, Olga Lucía; Diaz-Toro, Yira; Muvdi, Sandra; Rodríguez, Isabel; Gomez, María Adelaida; Saravia, Nancy Gore

    2014-01-01

    Background Pentavalent antimonials have been the first line treatment for dermal leishmaniasis in Colombia for over 30 years. Miltefosine is administered as second line treatment since 2005. The susceptibility of circulating populations of Leishmania to these drugs is unknown despite clinical evidence supporting the emergence of resistance. Methodology/Principal Findings In vitro susceptibility was determined for intracellular amastigotes of 245 clinical strains of the most prevalent Leishmania Viannia species in Colombia to miltefosine (HePC) and/or meglumine antimoniate (SbV); 163, (80%) were evaluated for both drugs. Additionally, susceptibility to SbV was examined in two cohorts of 85 L. V. panamensis strains isolated between 1980–1989 and 2000–2009 in the municipality of Tumaco. Susceptibility to each drug differed among strains of the same species and between species. Whereas 68% of L. V. braziliensis strains presented in vitro resistance to HePC, 69% were sensitive to SbV. Resistance to HePC and SbV occurred respectively, in 20% y 21% of L. panamensis strains. Only 3% of L. V. guyanensis were resistant to HePC, and none to SbV. Drug susceptibility differed between geographic regions and time periods. Subpopulations having disparate susceptibility to SbV were discerned among L. V. panamensis strains isolated during 1980–1990 in Tumaco where resistant strains belonged to zymodeme 2.3, and sensitive strains to zymodeme 2.2. Conclusions/Significance Large scale evaluation of clinical strains of Leishmania Viannia species demonstrated species, population, geographic, and epidemiologic differences in susceptibility to meglumine antimoniate and miltefosine, and provided baseline information for monitoring susceptibility to these drugs. Sensitive and resistant clinical strains within each species, and zymodeme as a proxy marker of antimony susceptibility for L. V. panamensis, will be useful in deciphering factors involved in susceptibility and the distribution

  13. Co-administration of glycyrrhizic acid with the antileishmanial drug sodium antimony gluconate (SAG) cures SAG-resistant visceral leishmaniasis.

    PubMed

    Bhattacharjee, Amrita; Majumder, Saikat; Majumdar, Suchandra Bhattacharyya; Choudhuri, Soumitra Kumar; Roy, Syamal; Majumdar, Subrata

    2015-03-01

    Since there are very few affordable antileishmanial drugs available, antimonial resistance has crippled antileishmanial therapy, thereby emphasising the need for development of novel therapeutic strategies. This study aimed to evaluate the antileishmanial role of combined therapy with sodium antimony gluconate (SAG) and the triterpenoid glycyrrhizic acid (GA) against infection with SAG-resistant Leishmania (GE1F8R). Combination therapy with GA and SAG successfully limited infection with SAG-resistant Leishmania in a synergistic manner (fractional inhibitory concentration index <1.0). At the same time, mice infected with SAG-resistant Leishmania and co-treated with GA and SAG exhibited a significant reduction in hepatic and splenic parasite burden. In probing the mechanism, it was observed that GA treatment suppressed the expression and efflux activity of P-glycoprotein (P-gp) and multidrug resistance-associated protein 1 (MRP1), two host ABC transporters responsible for antimony efflux from host cells infected with SAG-resistant parasites. This suppression correlated with greater intracellular antimony retention during SAG therapy both in vitro and in vivo, which was reflected in the reduced parasite load. Furthermore, co-administration of GA and SAG induced a shift in the cytokine balance towards a Th1 phenotype by augmenting pro-inflammatory cytokines (such as IL-12, IFNγ and TNFα) and inducing nitric oxide generation in GE1F8R-infected macrophages as well as GE1F8R-infected mice. This study aims to provide an affordable leishmanicidal alternative to expensive antileishmanial drugs such as miltefosine and amphotericin B. Furthermore, this report explores the role of GA as a resistance modulator in MRP1- and P-gp-overexpressing conditions. PMID:25600891

  14. Migration of antimony from PET bottles into beverages: determination of the activation energy of diffusion and migration modelling compared with literature data.

    PubMed

    Welle, F; Franz, R

    2011-01-01

    Plastics bottles made from polyethylene terephthalate (PET) are increasingly used for soft drinks, mineral water, juices and beer. In this study a literature review is presented concerning antimony levels found both in PET materials as well as in foods and food simulants. On the other hand, 67 PET samples from the European bottle market were investigated for their residual antimony concentrations. A mean value of 224 ± 32 mg kg(-1) was found, the median was 220 mg kg(-1). Diffusion coefficients for antimony in PET bottle materials were experimentally determined at different temperature between 105 and 150°C. From these data, the activation energy of diffusion for antimony species from the PET bottle wall into beverages and food simulants was calculated. The obtained value of 189 kJ mol(-1) was found to be in good agreement with published data on PET microwave trays (184 kJ mol(-1)). Based on these results, the migration of antimony into beverages was predicted by mathematical migration modelling for different surface/volume ratios and antimony bottle wall concentrations. The results were compared with literature data as well as international legal limits and guidelines values for drinking water and the migration limit set from food packaging legislation. It was concluded that antimony levels in beverages due to migration from PET bottles manufactured according to the state of the art can never reach or exceed the European-specific migration limit of 40 microg kg(-1). Maximum migration levels caused by room-temperature storage even after 3 years will never be essentially higher than 2.5 microg kg(-1) and in any case will be below the European limit of 5 microg kg(-1) for drinking water. The results of this study confirm that the exposure of the consumer by antimony migration from PET bottles into beverages and even into edible oils reaches approximately 1% of the current tolerable daily intake (TDI) established by World Health Organisation (WHO). Having

  15. Separation of Lead from Crude Antimony by Pyro-Refining Process with NaPO3 Addition

    NASA Astrophysics Data System (ADS)

    Ye, Longgang; Hu, Yuejie; Xia, Zhimei; Chen, Yongming

    2016-04-01

    The main purpose of this study was to separate lead from crude antimony through an oxidation pyro-refining process and by using sodium metaphosphate as a lead elimination reagent. The process parameters that will affect the refining results were optimized experimentally under controlled conditions, such as the sodium metaphosphate charging dosage, the refining temperature and duration, and the air flow rate, to determine their effect on the lead content in refined antimony and the lead removal rate. A minimum lead content of 0.0522 wt.% and a 98.6% lead removal rate were obtained under the following optimal conditions: W_{{{NaPO}_{{3}} }} = 15% W Sb (where W represents weight), a refining temperature of 800°C, a refining time of 30 min, and an air flow rate of 3 L/min. X-ray diffractometry and scanning electron microscopy showed that high-purity antimony was obtained. The smelting operation is free from smoke or ammonia pollution when using monobasic sodium phosphate or ammonium dihydrogen phosphate as the lead elimination reagent. However, this refining process can also remove a certain amount of sulfur, cobalt, and silicon simultaneously, and smelting results also suggest that sodium metaphosphate can be used as a potential lead elimination reagent for bismuth and copper refining.

  16. Separation of Lead from Crude Antimony by Pyro-Refining Process with NaPO3 Addition

    NASA Astrophysics Data System (ADS)

    Ye, Longgang; Hu, Yuejie; Xia, Zhimei; Chen, Yongming

    2016-06-01

    The main purpose of this study was to separate lead from crude antimony through an oxidation pyro-refining process and by using sodium metaphosphate as a lead elimination reagent. The process parameters that will affect the refining results were optimized experimentally under controlled conditions, such as the sodium metaphosphate charging dosage, the refining temperature and duration, and the air flow rate, to determine their effect on the lead content in refined antimony and the lead removal rate. A minimum lead content of 0.0522 wt.% and a 98.6% lead removal rate were obtained under the following optimal conditions: W_{{{NaPO}_{{3}} }} = 15% W Sb (where W represents weight), a refining temperature of 800°C, a refining time of 30 min, and an air flow rate of 3 L/min. X-ray diffractometry and scanning electron microscopy showed that high-purity antimony was obtained. The smelting operation is free from smoke or ammonia pollution when using monobasic sodium phosphate or ammonium dihydrogen phosphate as the lead elimination reagent. However, this refining process can also remove a certain amount of sulfur, cobalt, and silicon simultaneously, and smelting results also suggest that sodium metaphosphate can be used as a potential lead elimination reagent for bismuth and copper refining.

  17. Potential mechanism of the anti-trypanosomal activity of organoruthenium complexes with bioactive thiosemicarbazones.

    PubMed

    Demoro, Bruno; Rossi, Miriam; Caruso, Francesco; Liebowitz, Daniel; Olea-Azar, Claudio; Kemmerling, Ulrike; Maya, Juan Diego; Guiset, Helena; Moreno, Virtudes; Pizzo, Chiara; Mahler, Graciela; Otero, Lucía; Gambino, Dinorah

    2013-06-01

    In the search for new metal-based drugs against diseases produced by trypanosomatid parasites, four organoruthenium(II) compounds [Ru2(p-cymene)2(L)2]X2, where L are bioactive 5-nitrofuryl-containing thiosemicarbazones and X = Cl or PF6, had been previously obtained. These compounds had shown activity on Trypanosoma brucei, the etiological agent of African trypanosomiasis. Because of genomic similarities between trypanosomatides, these ruthenium compounds were evaluated, in the current work, on Trypanosoma cruzi, the parasite responsible of American trypanosomiasis (Chagas disease). Two of them showed significant in vitro growth inhibition activity against the infective trypomastigote form of T. cruzi (Dm28c clone, IC50 = 11.69 and 59.42 μM for [Ru2(p-cymene)2(L4)2]Cl2 and [Ru2(p-cymene)2(L1)2]Cl2, respectively, where HL4 = 5-nitrofuryl-N-phenylthiosemicarbazone and HL1 = 5-nitrofurylthiosemicarbazone), showing fairly good selectivities toward trypanosomes with respect to mammalian cells (J774 murine macrophages). Moreover, [Ru2(p-cymene)2(L2)2]Cl2, where HL2 = 5-nitrofuryl-N-methylthiosemicarbazone, was synthesized in order to evaluate the effect of improved solubility on biological behavior. This new chloride salt showed higher activity against T. cruzi than that of the previously synthesized hexafluorophosphate one (Dm28c clone, IC50 = 14.30 μM for the former and 231.3 μM for the latter). In addition, the mode of antitrypanosomal action of the organoruthenium compounds was investigated. The complexes were not only able to generate toxic free radicals through bioreduction but they also interacted with two further potential parasite targets: DNA and cruzipain, a cysteine protease which plays a fundamental role in the biological cycle of these parasites. The results suggest a "multi-target" mechanism of trypanosomicidal action for the obtained complexes. PMID:23564472

  18. Design and synthesis of novel 5,6-disubstituted pyridine-2,3-dione-3-thiosemicarbazone derivatives as potential anticancer agents.

    PubMed

    Xie, Wenlin; Xie, Shimin; Zhou, Ying; Tang, Xufu; Liu, Jian; Yang, Wenqian; Qiu, Minghua

    2014-06-23

    A series of 5,6-disubstituted pyridine-2,3-dione-3-thiosemicarbazone derivatives(2a-2n) and 5,6-disubstituted pyridine-2,3-dione S-benzyl-3-thiosemicarbazones(3a-3g) were synthesized starting from 2,3-dihydroxypyridine via oxidation-Michael additions, condensations and nucleophilic substitutions. The structures of the compounds were established by IR, (1)H NMR, (13)C NMR, and HRMS. All newly synthesized compounds were screened for their anticancer activity against Breast cancer (MCF-7), Colon cancer (HCT-116) and hepatocellular cancer (BEL7402) cell lines. Bioassay results indicated that most of the prepared compounds exhibited cytotoxicity against various cancer cells in vitro. Some of the compounds exhibited promising antiproliferative activity, which were comparable to the positive control (5-fluorouracil). The structure-activity relationship was discussed. PMID:24819956

  19. Crystal structures of 5-Bromo-2-hydroxybenzaldehyde, 2-hydroxy-3-methoxybenzaldehyde, and 2-hydroxynaphthalene-1-carbaldehyde 4-(2-pyridyl) thiosemicarbazones

    NASA Astrophysics Data System (ADS)

    Chumakov, Yu. M.; Petrenko, P. A.; Codita, T. B.; Tsapkov, V. I.; Poirier, D.; Gulea, A. P.

    2014-03-01

    5-Bromo-2-hydroxybenzaldehyde, 2-hydroxy-3-methoxybenzaldehyde, and 2-hydroxynaphthalene-1-carbaldehyde 4-(2-pyridyl) thiosemicarbazones ( I-III, respectively) were synthesized and their crystal structures were determined by X-ray diffraction. All these molecules are almost planar. The presence of bulky substituents at the terminal nitrogen atoms of these molecules does not lead to changes in the conformation of the thiosemicarbazide moiety. Depending on the nature of substituents in the phenol rings, the crystals are composed of either centrosymmetric dimers ( I) or infinite chains ( II and III). In the concentration range of 10-5-10-7 mol/L, thiosemicarbazones I-III selectively inhibit the growth of human myeloid leukemia HL60 cells.

  20. Synthesis, antioxidant activities of the nickel(II), iron(III) and oxovanadium(IV) complexes with N2O2 chelating thiosemicarbazones

    NASA Astrophysics Data System (ADS)

    Bal-Demirci, Tülay; Şahin, Musa; Özyürek, Mustafa; Kondakçı, Esin; Ülküseven, Bahri

    The nickel(II), iron(III) and oxovanadium(IV) complexes of the N2O2 chelating thiosemicarbazones were synthesized using 4-hydroxysalicyladehyde-S-methylthiosemicarbazone and R1-substitute-salicylaldehyde (R1: 4-OH, H) in the presence of Ni(II), Fe(III), VO(IV) ions by the template reaction. The structures of the thiosemicarbazone complexes were characterized by FT-IR, 1H NMR, elemental, ESI-MS and APCI-MS analysis. The synthesized compounds were screened for their antioxidant capacity by using the cupric reducing antioxidant capacity (CUPRAC) method. Trolox equivalent antioxidant capacity (TEAC) of iron(III) complex, 1c, was measured to be higher than that of the other complexes. Other parameters of antioxidant activity (scavenging effects on rad OH, O2rad - and H2O2) of these compounds were also determined. All the compounds have shown encouraging ROS scavenging activities.

  1. A New Thiosemicarbazone-Based Fluorescence "Turn-on" Sensor for Zn(2+) Recognition with a Large Stokes Shift and its Application in Live Cell Imaging.

    PubMed

    Tang, Lijun; Huang, Zhenlong; Zheng, Zhuxuan; Zhong, Keli; Bian, Yanjiang

    2016-09-01

    Selective fluorescence turn on Zn(2+) sensor with long-wavelength emission and a large Stokes shift is highly desirable in Zn(2+) sensing area. We reported herein the synthesis and Zn(2+) recognition properties of a new thiosemicarbazone-based fluorescent sensor L. L displays high selectivity and sensitivity toward Zn(2+) over other metal ions in DMSO-H2O (1:1, v/v, HEPES 10 mM, pH = 7.4) solution with a long-wavelength emission at 572 nm and a large Stokes shift of 222 nm. Confocal fluorescence microscopy experiments demonstrate that L is cell-permeable and capable of monitoring intracellular Zn(2+). Graphical Abstract We report a new thiosemicarbazone-based fluorescent sensor (L) for selective recognition of Zn(2+) with a long wavelength emission and a large Stokes shift. PMID:27333797

  2. Synthesis, antioxidant activities of the nickel(II), iron(III) and oxovanadium(IV) complexes with N2O2 chelating thiosemicarbazones.

    PubMed

    Bal-Demirci, Tülay; Sahin, Musa; Ozyürek, Mustafa; Kondakçı, Esin; Ulküseven, Bahri

    2014-05-21

    The nickel(II), iron(III) and oxovanadium(IV) complexes of the N2O2 chelating thiosemicarbazones were synthesized using 4-hydroxysalicyladehyde-S-methylthiosemicarbazone and R1-substitute-salicylaldehyde (R1: 4-OH, H) in the presence of Ni(II), Fe(III), VO(IV) ions by the template reaction. The structures of the thiosemicarbazone complexes were characterized by FT-IR, (1)H NMR, elemental, ESI-MS and APCI-MS analysis. The synthesized compounds were screened for their antioxidant capacity by using the cupric reducing antioxidant capacity (CUPRAC) method. Trolox equivalent antioxidant capacity (TEAC) of iron(III) complex, 1c, was measured to be higher than that of the other complexes. Other parameters of antioxidant activity (scavenging effects on •OH, O2(•-) and H2O2) of these compounds were also determined. All the compounds have shown encouraging ROS scavenging activities. PMID:24656797

  3. Structural study of two N(4)-substituted thiosemicarbazones prepared from 1-phenyl-1,2-propanedione-2-oxime and their binuclear nickel(II) complexes

    NASA Astrophysics Data System (ADS)

    Kaminsky, Werner; Jasinski, Jerry P.; Woudenberg, Richard; Goldberg, Karen I.; West, Douglas X.

    2002-05-01

    The crystal structures of the oxime/thiosemicarbazones 1-phenyl-1-{ N(4)-methyl- and 1-phenyl-1-{ N(4)-ethylthiosemicarbazone}-2-oximepropane, H 2Po4M and H 2Po4E, were found to have the oxime and thiosemicarbazone moieties on opposite sides of the carbon-carbon backbone. Intermolecular hydrogen bonding involves the oxime function forming a symmetrical dimer for both compounds. The structures of the binuclear nickel(II) complexes, [Ni(Po4M)] 2 and [Ni(Po4E)] 2, show that bridging by the oximato N-O results in a centrosymmetric arrangement of the two planar nickel centers in each complex. The coordinated thiosemicarbazonato moieties undergo the expected changes in bond distances and angles compared to H 2Po4M and H 2Po4E.

  4. comparative analysis of cellular respiratory inhibition by substituted phenylglyoxal-bis-(4-methyl-3-thiosemicarbazone) zinc chelates.

    PubMed

    Coats, E A; Milstein, S R; Pleiss, M A; Roesener, J A; Schmidt, J; McDonald, J; Reed, R

    1983-03-01

    Fourteen para-substituted phenylglyoxal-bis-(4-methyl-3-thiosemicarbazone) zinc chelates have been synthesized as inhibitors of cellular respiration and therefore as potential antineoplastic agents. Each chelate has been evaluated as an inhibitor of Ehrlich ascites tumor cell and of rat liver slice respiration. The molar I50 values for respiratory inhibition have been subjected to computerized correlation to delineate quantitative relationships between biological activity and chemical structure. Activity against the tumor cell model is characterized by a positive lipophilic and a detrimental steric influence while activity against rat liver slice displays only a weak positive lipophilic effect. Quantitative comparative analysis suggests that selective action against the tumor cell system can be improved by substituents which are electron withdrawing and lipophilic in nature. PMID:6852227

  5. Spectroscopic and biological approach of Ni(II) and Cu(II) complexes of 2-pyridinecarboxaldehyde thiosemicarbazone

    NASA Astrophysics Data System (ADS)

    Chandra, Sulekh; Raizada, Smriti; Tyagi, Monika; Sharma, Praveen Kumar

    2008-03-01

    Ni(II) and Cu(II) complexes having the general composition [M(L) 2X 2] [where L = 2-pyridinecarboxaldehyde thiosemicarbazone, M = Ni(II) and Cu(II), X = Cl -, NO 3- and 1/2 SO 42-] have been synthesized. All the metal complexes were characterized by elemental analysis, molar conductance, magnetic moment, mass, IR, EPR and electronic spectral studies. The magnetic moment measurements of the complexes indicate that all the complexes are of high-spin type. On the basis of spectral studies an octahedral geometry has been assigned for Ni(II) complexes whereas tetragonal geometry for Cu(II) except [Cu(L) 2SO 4] which posseses five coordinated geometry. The ligand and its metal complexes were screened against phytopathogenic fungi and bacteria in vitro.

  6. Cytotoxic and Antitumour Studies of Acetoacetanilide N(4)-methyl(phenyl)thiosemicarbazone and its Transition Metal Complexes.

    PubMed

    Priya, N P; Firdous, A P; Jeevana, R; Aravindakshan, K K

    2015-01-01

    Cytotoxic activities of acetoacetanilide N(4)-methyl(phenyl)thiosemicarbazone (L2H) and its seven different metal complexes were studied. Of these, IC50 value of the copper complex was found to be 46 μg/ml. Antitumour studies of this copper complex was carried out using Daltons Lymphoma Ascites cell-induced solid tumour model and Ehrlich's Ascites Carcinoma cell-induced ascites tumour model. Administration of the copper complex at different concentrations (10, 5 and 1 mg/kg b. wt) inhibited the solid tumour development in mice and increased the mean survival rate and the life span of Ascites tumour bearing mice in a concentration dependent manner. PMID:26997691

  7. Spectroscopic, viscositic and molecular modeling studies on the interaction of 3'-azido-daunorubicin thiosemicarbazone with DNA.

    PubMed

    Cui, Fengling; Liu, Qingfeng; Luo, Hongxia; Zhang, Guisheng

    2014-01-01

    A new daunorubicin has been synthesized and structurally characterized. The interaction of native calf thymus DNA (ctDNA) with 3'-azido-daunorubicin thiosemicarbazone (ADNRT) was investigated under simulated physiological conditions by multi-spectroscopic techniques, viscometric measurements and molecular modeling study. It concluded that ADNRT could intercalate into the base pairs of ctDNA, and the fluorescence quenching by ctDNA was static quenching type. Thermodynamic parameters calculated suggested that the binding of ADNRT to ctDNA was mainly driven by hydrophobic interactions. The relative viscosity of ctDNA increased with the addition of ADNRT, which confirmed the intercalation mode. Furthermore, molecular modeling studies corroborate the above experimental results. PMID:23974700

  8. Spectroscopic evaluation of Co(II), Ni(II) and Cu(II) complexes derived from thiosemicarbazone and semicarbazone

    NASA Astrophysics Data System (ADS)

    Chandra, Sulekh; Kumar, Anil

    2007-12-01

    Co(II), Ni(II) and Cu(II) complexes were synthesized with thiosemicarbazone (L 1) and semicarbazone (L 2) derived from 2-acetyl furan. These complexes were characterized by elemental analysis, molar conductance, magnetic moment, mass, IR, electronic and EPR spectral studies. The molar conductance measurement of the complexes in DMSO corresponds to non-electrolytic nature. All the complexes are of high-spin type. On the basis of different spectral studies six coordinated geometry may be assigned for all the complexes except Co(L) 2(SO 4) and Cu(L) 2(SO 4) [where L = L 1 and L 2] which are of five coordinated square pyramidal geometry.

  9. Cytotoxic and Antitumour Studies of Acetoacetanilide N(4)-methyl(phenyl)thiosemicarbazone and its Transition Metal Complexes

    PubMed Central

    Priya, N. P.; Firdous, A. P.; Jeevana, R.; Aravindakshan, K. K.

    2015-01-01

    Cytotoxic activities of acetoacetanilide N(4)-methyl(phenyl)thiosemicarbazone (L2H) and its seven different metal complexes were studied. Of these, IC50 value of the copper complex was found to be 46 μg/ml. Antitumour studies of this copper complex was carried out using Daltons Lymphoma Ascites cell-induced solid tumour model and Ehrlich's Ascites Carcinoma cell-induced ascites tumour model. Administration of the copper complex at different concentrations (10, 5 and 1 mg/kg b. wt) inhibited the solid tumour development in mice and increased the mean survival rate and the life span of Ascites tumour bearing mice in a concentration dependent manner. PMID:26997691

  10. Synthesis and evaluation of naphthalene-based thiosemicarbazone derivatives as new anticancer agents against LNCaP prostate cancer cells.

    PubMed

    Altintop, Mehlika Dilek; Sever, Belgin; Özdemir, Ahmet; Kuş, Gökhan; Oztopcu-Vatan, Pinar; Kabadere, Selda; Kaplancikli, Zafer Asim

    2016-01-01

    Fourteen new naphthalene-based thiosemicarbazone derivatives were designed as anticancer agents against LNCaP human prostate cancer cells and synthesized. MTT assay indicated that compounds 6, 8 and 11 exhibited inhibitory effect on LNCaP cells. Among these compounds, 4-(naphthalen-1-yl)-1-[1-(4-hydroxyphenyl)ethylidene)thiosemicarbazide (6), which caused more than 50% death on LNCaP cells, was chosen for flow cytometric analysis of apoptosis. Flow cytometric analysis pointed out that compound 6 also showed apoptotic effect on LNCaP cells. Compound 6 can be considered as a promising anticancer agent against LNCaP cells owing to its potent cytotoxic activity and apoptotic effect. PMID:25826149

  11. Synthesis, stereochemical, structural and biological studies of some 2,6-diarylpiperidin-4-one N(4‧)-cyclohexyl thiosemicarbazones

    NASA Astrophysics Data System (ADS)

    Sethukumar, A.; Udhaya Kumar, C.; Agilandeshwari, R.; Arul Prakasam, B.

    2013-09-01

    A new series of 2,6-diarylpiperidin-4-one N(4')-cyclohexyl thiosemicarbazones (13-23) were synthesized by corresponding 2,6-diarylpiperidin-4-ones (1-11) reaction with cyclohexyl thiosemicarbazide (12). The chemical structures were confirmed by means of IR, one and two dimensional NMR, Mass spectra and single crystal X-ray diffraction analysis. Compounds 13-23, exist in chair conformation with equatorial orientation of all the substituents at piperidine ring except the methyl group at C-5 of compounds 21-23 oriented at axial disposition to stabilize the chair conformation. Single crystal X-ray structural analysis of compound 18, evidences that the configuration about Cdbnd N double bond is syn to C-5 carbon (E-form). All the synthesized compounds were screened their biological activity.

  12. Solid-state proton transfer studies on phototautomerization of 1-phenyl-3-methyl-4-furoyl-5-pyrazolone 4-methyl thiosemicarbazone

    NASA Astrophysics Data System (ADS)

    Zhang, Tao; Liu, Guangfei; Liu, Lang; Jia, Dianzeng; Zhang, Li

    2006-08-01

    A novel keto-enol phototautomeric compound of 1-phenyl-3-methyl-4-(-furoyl)-5-pyrazolone 4-methyl thiosemicarbazone was found to undergo phototautomerization in the crystalline state. The reaction rate constant was studied based on the first-order kinetics curve. Crystal structural analysis and theoretical calculations show that the pyrazolone ring stabilizes in the keto form. The conclusion can be made that its phototautomerization in the crystalline state is associated with a photo-induced intermolecular double-proton-transfer reaction along intermolecular hydrogen bonds N sbnd H⋯O and S⋯H sbnd N leading to a colored tautomer as the compound crystallizes in a hydrogen bonded supramolecular configuration.

  13. Synthesis, crystal structures, biological activities and fluorescence studies of transition metal complexes with 3-carbaldehyde chromone thiosemicarbazone.

    PubMed

    Li, Yong; Yang, Zheng-Yin; Wu, Jin-Cai

    2010-12-01

    3-carbaldehyde chromone thiosemicarbazone (L) and its transition metal complexes were synthesized and characterized systematically. Crystal structures of Zn(II) and Ni(II) complexes were determined by single crystal X-ray diffraction analysis. Zn(II) complex exhibits blue fluorescence under UV light and its fluorescent property in solid state was investigated. Interactions of ligand and Cu(II), Zn(II) and Ni(II) complexes with DNA were investigated by spectral and viscosity studies, indicating the compounds bind to DNA via intercalation and Zn(II) complex binds to DNA most strongly. Antioxidant tests in vitro show the compounds possess significant antioxidant activity against superoxide and hydroxyl radicals, and the scavenging effects of Cu(II) complex are stronger than Zn(II), Ni(II) complexes and some standard antioxidants, such as mannitol and vitamin C. PMID:20884087

  14. Microwave gallium-68 radiochemistry for kinetically stable bis(thiosemicarbazone) complexes: structural investigations and cellular uptake under hypoxia.

    PubMed

    Alam, Israt S; Arrowsmith, Rory L; Cortezon-Tamarit, Fernando; Twyman, Frazer; Kociok-Köhn, Gabriele; Botchway, Stanley W; Dilworth, Jonathan R; Carroll, Laurence; Aboagye, Eric O; Pascu, Sofia I

    2016-01-01

    We report the microwave synthesis of several bis(thiosemicarbazones) and the rapid gallium-68 incorporation to give the corresponding metal complexes. These proved kinetically stable under 'cold' and 'hot' biological assays and were investigated using laser scanning confocal microscopy, flow cytometry and radioactive cell retention studies under normoxia and hypoxia. (68)Ga complex retention was found to be 34% higher in hypoxic cells than in normoxic cells over 30 min, further increasing to 53% at 120 min. Our data suggests that this class of gallium complexes show hypoxia selectivity suitable for imaging in living cells and in vivo tests by microPET in nude athymic mice showed that they are excreted within 1 h of their administration. PMID:26583314

  15. Eco-Friendly Synthesis of Some Thiosemicarbazones and Their Applications as Intermediates for 5-Arylazothiazole Disperse Dyes.

    PubMed

    Gaffer, Hatem E; Khalifa, Mohamed E

    2015-01-01

    The solid-solid reactions of thiosemicarbazide with 4-formylantipyrine, 2-acetylpyrrole and camphor were performed to afford the thiosemicarbazones 1-3 which underwent hetero-cyclization with phenacyl bromide to furnish the corresponding thiazole derivatives 4-6. The yields of the reactions are quantitative in all cases and the products do not require further purification. A series of 5-arylazo-2-(substituted ylidene-hydrazinyl)-thiazole dyes 7-9 was then prepared by diazo coupling of thiazole derivatives 4-6 with several diazonium chlorides. The synthesized dyes were applied as disperse dyes for dyeing polyester fabric. The dyed fabrics exhibit good washing, perspiration, sublimation and light fastness properties, with little variation in their moderate to good rubbing fastness. PMID:26690111

  16. Leading time domain seismic precursors

    NASA Astrophysics Data System (ADS)

    Boucouvalas, A. C.; Gkasios, M.; Keskebes, A.; Tselikas, N. T.

    2014-08-01

    The problem of predicting the occurrence of earthquakes is threefold. On one hand it is necessary to predict the date and magnitude of an earthquake, and on the other hand the location of the epicenter. In this work after a brief review of the state of earthquake prediction research, we report on a new leading time precursor for determining time onset of earthquake occurrence. We report the linking between earthquakes of the past with those which happen in the future via Fibonacci, Dual and Lucas numbers (FDL) numbers. We demonstrate it here with two example seed earthquakes at least 100 years old. Using this leading indicator method we can predict significant earthquake events >6.5R, with good accuracy approximately +- 1 day somewhere in the world. From a single seed we produce at least 100 trials simultaneously of which 50% are correct to +- 1day. The indicator is based on Fibonacci, Dual and Lucas numbers (FDL). This result hints that the log periodic FDL numbers are at the root of the understanding of the earthquake mechanism. The theory is based on the assumption that each occurred earthquake discontinuity can be thought of as a generating source of FDL time series. (The mechanism could well be linked to planetary orbits). When future dates are derived from clustering and convergence from previous strong earthquake dates at an FDL time distance, then we have a high probability for an earthquake to occur on that date. We set up a real time system which generates FDL time series from each previous significant earthquake (>7R) and we produce a year to year calendar of high probability earthquake dates. We have tested this over a number of years with considerable success. We have applied this technique for strong (>7R) earthquakes across the globe as well as on a restricted region such as the Greek geographic region where the magnitude is small (>4R-6.5R). In both cases the success of the method is impressive. It is our belief that supplementing this method with

  17. Inhibition of Bovine Viral Diarrhea Virus RNA Synthesis by Thiosemicarbazone Derived from 5,6-Dimethoxy-1-Indanone▿

    PubMed Central

    Castro, Eliana F.; Fabian, Lucas E.; Caputto, María E.; Gagey, Dolores; Finkielsztein, Liliana M.; Moltrasio, Graciela Y.; Moglioni, Albertina G.; Campos, Rodolfo H.; Cavallaro, Lucía V.

    2011-01-01

    In the present work, we described the activity of the thiosemicarbazone derived from 5,6-dimethoxy-1-indanone (TSC), which we previously characterized as a new compound that inhibits bovine viral diarrhea virus (BVDV) infection. We showed that TSC acts at a point of time that coincides with the onset of viral RNA synthesis and that it inhibits the activity of BVDV replication complexes (RCs). Moreover, we have selected five BVDV mutants that turned out to be highly resistant to TSC but still susceptible to ribavirin (RBV). Four of these resistant mutants carried an N264D mutation in the viral RNA-dependent RNA polymerase (RdRp). The remaining mutant showed an A392E mutation within the same protein. Some of these mutants replicated slower than the wild-type (wt) virus in the absence of TSC, whereas others showed a partial reversion to the wt phenotype over several passages in the absence of the compound. The docking of TSC in the crystal structure of the BVDV RdRp revealed a close contact between the indane ring of the compound and several residues within the fingers domain of the enzyme, some hydrophobic contacts, and hydrogen bonds with the thiosemicarbazone group. Finally, in the mutated RdRp from resistant BVDV, these interactions with TSC could not be achieved. Interestingly, TSC inhibited BVDV replication in cell culture synergistically with RBV. In conclusion, TSC emerges as a new nonnucleoside inhibitor of BVDV RdRp that is synergistic with RBV, a feature that turns it into a potential compound to be evaluated against hepatitis C virus (HCV). PMID:21430053

  18. Inhibition of bovine viral diarrhea virus RNA synthesis by thiosemicarbazone derived from 5,6-dimethoxy-1-indanone.

    PubMed

    Castro, Eliana F; Fabian, Lucas E; Caputto, María E; Gagey, Dolores; Finkielsztein, Liliana M; Moltrasio, Graciela Y; Moglioni, Albertina G; Campos, Rodolfo H; Cavallaro, Lucía V

    2011-06-01

    In the present work, we described the activity of the thiosemicarbazone derived from 5,6-dimethoxy-1-indanone (TSC), which we previously characterized as a new compound that inhibits bovine viral diarrhea virus (BVDV) infection. We showed that TSC acts at a point of time that coincides with the onset of viral RNA synthesis and that it inhibits the activity of BVDV replication complexes (RCs). Moreover, we have selected five BVDV mutants that turned out to be highly resistant to TSC but still susceptible to ribavirin (RBV). Four of these resistant mutants carried an N264D mutation in the viral RNA-dependent RNA polymerase (RdRp). The remaining mutant showed an A392E mutation within the same protein. Some of these mutants replicated slower than the wild-type (wt) virus in the absence of TSC, whereas others showed a partial reversion to the wt phenotype over several passages in the absence of the compound. The docking of TSC in the crystal structure of the BVDV RdRp revealed a close contact between the indane ring of the compound and several residues within the fingers domain of the enzyme, some hydrophobic contacts, and hydrogen bonds with the thiosemicarbazone group. Finally, in the mutated RdRp from resistant BVDV, these interactions with TSC could not be achieved. Interestingly, TSC inhibited BVDV replication in cell culture synergistically with RBV. In conclusion, TSC emerges as a new nonnucleoside inhibitor of BVDV RdRp that is synergistic with RBV, a feature that turns it into a potential compound to be evaluated against hepatitis C virus (HCV). PMID:21430053

  19. Ribonucleotide reductase inhibition by metal complexes of Triapine (3-aminopyridine-2-carboxaldehyde thiosemicarbazone): A combined experimental and theoretical study

    PubMed Central

    Popović-Bijelić, Ana; Kowol, Christian R.; Lind, Maria E.S.; Luo, Jinghui; Himo, Fahmi; Enyedy, Éva A.; Arion, Vladimir B.; Gräslund, Astrid

    2012-01-01

    Triapine (3-aminopyridine-2-carboxaldehyde thiosemicarbazone, 3-AP) is currently the most promising chemotherapeutic compound among the class of α-N-heterocyclic thiosemicarbazones. Here we report further insights into the mechanism(s) of anticancer drug activity and inhibition of mouse ribonucleotide reductase (RNR) by Triapine. In addition to the metal-free ligand, its iron(III), gallium(III), zinc(II) and copper (II) complexes were studied, aiming to correlate their cytotoxic activities with their effects on the diferric/tyrosyl radical center of the RNR enzyme in vitro. In this study we propose for the first time a potential specific binding pocket for Triapine on the surface of the mouse R2 RNR protein. In our mechanistic model, interaction with Triapine results in the labilization of the diferric center in the R2 protein. Subsequently the Triapine molecules act as iron chelators. In the absence of external reductants, and in presence of the mouse R2 RNR protein, catalytic amounts of the iron(III)–Triapine are reduced to the iron(II)–Triapine complex. In the presence of an external reductant (dithiothreitol), stoichiometric amounts of the potently reactive iron (II)–Triapine complex are formed. Formation of the iron(II)–Triapine complex, as the essential part of the reaction outcome, promotes further reactions with molecular oxygen, which give rise to reactive oxygen species (ROS) and thereby damage the RNR enzyme. Triapine affects the diferric center of the mouse R2 protein and, unlike hydroxyurea, is not a potent reductant, not likely to act directly on the tyrosyl radical. PMID:21955844

  20. Spectrophotometric determination of Cu(II) in soil and vegetable samples collected from Abraha Atsbeha, Tigray, Ethiopia using heterocyclic thiosemicarbazone.

    PubMed

    Admasu, Daniel; Reddy, Desam Nagarjuna; Mekonnen, Kebede Nigussie

    2016-01-01

    Two selective and sensitive reagents, 2-acetylpyridine thiosemicarbazone (2-APT) and 3-acetylpyridine thiosemicarbazone (3-APT) were used for the spectrophotometric determination of Cu(II). Both reagents gave yellowish Cu(II) complex at a pH range of 8.0-10.0. Beer's law was obeyed for Cu(II)-2-APT and Cu(II)-3-APT in the concentration range of 0.16-1.3 and 0.44-1.05 µg/mL, respectively. The molar absorptivity and of Cu(II)-2-APT and Cu(II)-3-APT were 2.14 × 10(4) at 370 nm, and 6.7 × 10(3) L/mol cm at 350 nm, respectively, while the Sandell's sensitivity were 0.009 and 0.029 µg/cm(2) in that order. The correlation coefficient of the standard curves of Cu(II)-2-APT and Cu(II)-3-APT were 0.999 and 0.998, respectively. The detection limit of the Cu(II)-2-APT and Cu(II)-3-APT methods were 0.053 and 0.147 µg/mL, respectively. The results demonstrated that the procedure is precise (relative standard deviation <2 %, n = 10). The method was tested for Cu(II) determination in soil and vegetable samples. Comparisons of the results with those obtained using a flame atomic absorption spectrophotometer for Cu(II) determination also tested the validity of the method using paired sample t test at the 0.05 level showing a good agreement between them. PMID:27512628