A study on nitroimidazole-99mTc(CO)3 complexes as hypoxia marker: Some observations towards possible improvement in in vivo efficacy

International Nuclear Information System (INIS)

Mallia, Madhava B.; Subramanian, Suresh; Mathur, Anupam; Sarma, H.D.; Banerjee, Sharmila

2014-01-01

Introduction: Hypoxia plays a negative role in the clinical management of cancer. Detection of hypoxic status of a cancer is important for selecting patients for hypoxia directed therapy. Though [ 18 F]fluoromisonidazole ([ 18 F]FMISO), a PET radiopharmaceutical, is presently being used in the clinic for the detection of hypoxia, considering the logistical advantages of 99m Tc and wider availability of SPECT scanners, a radiopharmaceutical based on this isotope may find wider applicability. Methods: Nine nitroimidazole (2-, 4- and 5-nitroimidazole) ligands were synthesized and radiolabeled using [ 99m Tc(CO) 3 (H 2 O) 3 ] + precursor to obtain a group of complexes possessing different single electron reduction potential (SERP), overall charge and lipophilicity, the three attributes which decide the efficacy of the complex to detect hypoxic cells in vivo. The nitroimidazole- 99m Tc(CO) 3 complexes as well as [ 18 F]FMISO were evaluated in fibrosarcoma tumor bearing mice. Results: The 99m Tc(CO) 3 complexes of nitroimidazole iminodiacetic acid (IDA) showed better tumor uptake and retention than nitroimidazole diethylenetriamine (DETA) and nitroimidazole aminoethylglycine (AEG) complexes. Tumor uptake observed with [ 18 F]FMISO was higher than any of the nitroimidazole-IDA- 99m Tc(CO) 3 complexes. However, [ 18 F]FMISO clearance from tumor was found to be faster compared to 2-nitroimidazole-IDA- 99m Tc(CO) 3 complex. Observed tumor uptake and retention of the radiotracers evaluated could be correlated to its blood clearance pattern and SERP. Conclusions: Results of the present study indicated that uptake of the radiotracer in tumor is closely associated with its rate of clearance from blood. The study also indicated that along with SERP, clearance of radiotracer from blood (net effect of charge and lipophilicity) is a critical factor which decides the in vivo efficacy of the hypoxia detecting radiopharmaceutical

Cytotoxic properties of a 4-nitroimidazole (NSC 38087): a radiosensitizer of hypoxic cells in vitro

International Nuclear Information System (INIS)

Stratford, I.J.; Williamson, C.; Hardy, C.

1981-01-01

5-Phenoxysulphonyl-1-methyl-4-nitroimidazole (NSC 38087) can act as a sensitizer of hypoxic mammalian cells to radiation in vitro. The degree of sensitization achieved is greater than would be predicted from the drug's electron affinity. Cytotoxicity studies have shown that 5sub(μM) NSC 38087 can reduce the surviving fraction of log-phase V79 cells in air at 37 0 C to 10 -2 after 2 h exposure. This toxicity is considerably increased by small rises in temperature. In contrast to other nitroheterocyclic radiosensitizers, NSC 38087 and related 5-substituted 4-nitroimidazoles show greater toxicity towards aerobic than to hypoxic cells. Log-phase cells show the highest sensitivity to the toxic action of NSC 38087, with plateau-phase cells, cells with a history of chronic hypoxia, and thermotolerant cells showing greater resistance. These toxicity data are compared to those for the 2-nitroimidazole hypoxic-cell sensitizer misonidazole. (author)

A rapid-mix study on the effect of lipophilicity of nitroimidazoles on the radiosensitization of mammalian cells in vitro

International Nuclear Information System (INIS)

Watts, M.E.; Hodgkiss, R.J.; Jones, N.R.; Sehmi, D.S.; Woodcock, M.

1983-01-01

A liquid flow rapid-mixing apparatus has been used to study the role of lipophilicity (octanol: water partition coefficient, P) in the sensitization of hypoxic V79 cells by nitroimidazoles. Sensitization by seven neutral 2-nitroimidazoles of similar reduction potential but widely differing partition (0.11-77) and one basic 2-nitroimidazole (pKsub(a) = 8.9; p = 8.5 (of free base)) was studied as a function of pre-irradiated contact time ca. 3-40 ms. With increasing P, sensitization occurs at increasingly shorter pre-irradiated contact times. The results suggest that even though factors other than passive diffusion control the sensitization observed with the base Ro 03-8799 it is able to diffuse to the target site faster than misonidazole. (author)

An experimental study of 99Tcm-PnAO-nitroimidazole and 99Tcm-HL91 in detection of myocardial hypoxia

International Nuclear Information System (INIS)

Yao Zhiming; Liu Xiujie; Shi Rongfang; Guo Feng; Liu Yunzhong; Wang Qi; Wei Hongxing; Zhu Lin

1999-01-01

Objective: To investigate the biological characteristics of two hypoxic-avid imaging agents, 99 Tc m -PnAO-nitroimidazole and 99 Tc m -HL91, and the experimental myocardial hypoxia, low perfusion and ischemic reperfusion were performed. Methods: Isolated rat hearts were retrograde perfused with Kerbs-Henscleit buffer (KH) in four phantoms: control, low perfusion, ischemic reperfusion and hypoxia. Control hearts were perfused with 95% O 2 and 5% CO 2 balanced KH at 9∼10 mL/min rate. Low perfusion hearts were perfused with the same KH at 1 mL/min rate, and ischemic reperfusion rat hearts were discontinued perfusion for 20 min then reperfused with the same KH. Hypoxic hearts were perfused with 100% N 2 balanced KH. Results: 1) At 30 and 60 min, the radioactivity ratio of liver to heart (L/H) was 11.6 and 6.9 ( 99 Tc m -PnAO-nitroimidazole), and 5.7 and 6.2 ( 99 Tc m -HL91), respectively. The lung to heart ratios at 60 min of 99 Tc m -PnAO-nitroimidazole and 99 Tc m -HL91 were 1.8 and 2.1, respectively 2) The accumulation of 99 Tc m -PnAo-nitroimidazole in the hypoxic, low perfusion and ischemic hearts was 4.8, 3.7 and 2.8 times that in the control hearts. At 60 min after starting washout, the retentions of 99 Tc m -PnAO-nitroimidazole in hypoxic, low flow and ischemic reperfusion myocardium were much higher than that of control hearts [(23.7 +- 9.1)%]. The accumulation of 99 Tc m -HL91 in the hypoxic and low perfusion hearts was also significantly higher than that in the control and ischemic reperfusion hearts, P 99 Tc m -HL91 in the low perfusion heart was 5.34, 3.43 and 1.23 times those of control, ischemic reperfusion and hypoxic hearts, respectively. Conclusions: 99 Tc m -PnAO-nitroimidazole can be accumulated in low perfusion, ischemic reperfusion and hypoxic hearts, while 99 Tc m -HL91 is mainly accumulated in hypoxic, specially low perfusion hearts. Since there is a high L/H in perfusions with either agent, the detecting of inferoposterior wall may be

Radiosynthesis and evaluation of two novel 123I-labeled 2-methyl-4-nitroimidazole derivatives as potential infection imaging agents.

Science.gov (United States)

Rossouw, Daniel D; Lötter, Mattheus G; du Raan, Hanlie; Jansen, Susara E; Höhn, Alexander; Burger, Ben V

2005-05-01

The inflammation- and infection-seeking properties of (131)I-labeled ornidazole, a 5-nitroimidazole derivative, have recently been reported. Whole-body images in rabbits showed a more rapid uptake in inflamed areas compared to (67)Ga. In the present study, two novel (123)I-labeled 2-methyl-4-nitroimidazole derivatives were synthesized and their infection-seeking properties compared with those of (67)Ga and (123)I-labeled ornidazole. Radiolabeling was carried out by means of iodide-for-tosylate, triflate or halogen exchange. Various methods were utilized in order to synthesize the labeling precursors for the (123)I-labeled novel compounds. Serum stability studies on all of the (123)I-labeled tracers were followed by gamma camera imaging studies on rabbits artificially infected with Escherichia coli bacteria. The (123)I-labeled tracers were obtained in moderate to good radiochemical yields (34-80%) and acceptable radiochemical purities (93-99%). In contrast to (123)I-labeled ornidazole, 1-[(1-hydroxy-3-[(123)I]iodoprop-2-yloxy)methyl]-2-methyl-4-nitroimidazole (2) and 1-[(1-[(123)I]iodoprop-2-yloxy)methyl]-2-methyl-4-nitroimidazole (3) showed high serum stability. Compared to noninfected controls, all of the (123)I-labeled tracers showed increased uptake at the area of induced infection after 6 and 24 h, but the uptake was significantly lower than in the case of (67)Ga over the same period. Tracer 3 showed a slightly superior uptake after 6 h than the other (123)I-labeled tracers over the same period. The advantage of the initially slightly faster rate at which nitroimidazole tracers appear to accumulate in the infection area in comparison to (67)Ga might not outweigh the advantage of the eventual higher target to nontarget ratio displayed by (67)Ga.

Validation of a method for simultaneous determination of nitroimidazoles, benzimidazoles and chloramphenicols in swine tissues by ultra-high performance liquid chromatography-tandem mass spectrometry.

Science.gov (United States)

Xia, Xi; Wang, Yuanyuan; Wang, Xia; Li, Yun; Zhong, Feng; Li, Xiaowei; Huang, Yaoling; Ding, Shuangyang; Shen, Jianzhong

2013-05-31

This paper presents a sensitive and confirmatory multi-residue method for the analysis of 23 veterinary drugs and metabolites belonging to three classes (nitroimidazoles, benzimidazoles, and chloramphenicols) in porcine muscle, liver, and kidney. After extracted with ethyl acetate and basic ethyl acetate sequentially, the crude extracts were defatted with hexane and further purified using Oasis MCX solid-phase extraction cartridges. Rapid determination was carried out by ultra-high performance liquid chromatography-electrospray ionization tandem mass spectrometry. Data acquisition was performed under positive and negative mode simultaneously. Recoveries based on matrix-matched calibrations for meat, liver, and kidney ranged from 50.6 to 108.1%. The method quantification limits were in the range of 3-100ng/kg. Copyright © 2012 Elsevier B.V. All rights reserved.

Effect of the nitroimidazole Ro 03-8799 on the activity of chemotherapeutic agents against a murine tumour in vivo.

OpenAIRE

Sheldon, P. W.; Gibson, P.

1984-01-01

The effect of the 2-nitroimidazole Ro 03-8799 (8799) on the activity of 11 chemotherapeutic agents against the anaplastic MT tumour in mice has been determined by soft agar cloning. The 8799, whilst producing little cytotoxicity by itself, potentiated the cytotoxic actions of the alkylating agents melphalan and cyclophosphamide, and the nitrosoureas BCNU, CCNU and MeCCNU. This potentiation was influenced by the time interval between the administration of 8799 and the chemotherapeutic agents, ...

In vivo click reaction between Tc-99m-labeled azadibenzocyclooctyne-MAMA and 2-nitroimidazole-azide for tumor hypoxia targeting.

Science.gov (United States)

Sun, Wenjing; Chu, Taiwei

2015-10-15

The bioactivity of nitroimidazole in Tc-99m-labeled 2-nitroimidazole, a traditional solid tumor hypoxia-imaging agent for single photon emission computed tomography (SPECT), is reduced by the presence of large ligand and metallic radionuclide, exhibiting lower tumor-to-nontumor ratios. In an effort to solve this general problem, a pretargeting strategy based on click chemistry (strain-promoted cyclooctyne-azide cycloaddition) was applied. The functional click synthons were synthesized as pretargeting components: an azide group linked to 2-nitroimidazole (2NIM-Az) serves for tumor hypoxia-targeting and azadibenzocyclooctyne conjugated with monoamine monoamide dithiol ligand (AM) functions as radiolabeling and binding group to azides in vivo. 2NIM-triazole-MAMA was obtained from in vitro click reaction with a reaction rate constant of 0.98M(-1)s(-1). AM and 2NIM-triazole-MAMA were radiolabeled with Tc-99m. The hypoxia-pretargeting biodistribution was studied in Kunming mice bearing S180 tumor; (99m)Tc-AM and (99m)Tc-triazole-2NIM were used as blank control and conventional control. Compared to the control groups, the pretargeting experiment exhibits the best radio-uptake and retention in tumor, with higher tumor-to-muscle and tumor-to-blood ratios (up to 8.55 and 1.44 at 8h post-(99m)Tc-complex-injection, respectively). To some extent, the pretargeting strategy protects the bioactivity of nitroimidazole and therefore provides an innovative approach for the development of tumor hypoxia-SPECT imaging agents. Copyright © 2015 Elsevier Ltd. All rights reserved.

Neuropathy of nitroimidazole radiosensitizers: clinical and pathological description

International Nuclear Information System (INIS)

Wasserman, T.H.; Nelson, J.S.; VonGerichten, D.

1984-01-01

The dose limiting toxicity of the nitroimidazole radiosensitizers is peripherial neuropathy. Improved pharmacology of newer drugs has eliminated the encephalopathy. Peripheral neuropathies are predominently mild to moderate paresthesias of both hands and feet. Subjective changes occur with or without minimal objective changes on neurologic exam. All of the neuropathies occurred within 30 days of the last drug dose and are of varible duration. Sural nerve biopsies from patients indicate progressive axonal degeneration affecting both large and small caliber myelinated fibers. Axonal damage appears to be more severe in the distal portion of the nerves. More data are needed for correlation of clinical and pathological changes

99mTcO(BAT-NI), a novel nitroimidazole tracer: in vivo uptake studies in ischaemic myocardium

International Nuclear Information System (INIS)

Hoffend, J.; Linke, G.; Mohammed, A.; Haberkorn, U.; Tiefenbacher, C.P.; Eisenhut, M.

2003-01-01

Myocardial perfusion single-photon emission tomography (SPET) performed with cationic technetium-99m complexes indicates ischaemic areas as cold lesions. By contrast, nitroimidazole derivatives labelled with fluorine-18 or 99m Tc have recently shown promising results for hot spot imaging of ischaemic myocardium. This study evaluates 99m TcO(BAT-NI), a new 99m Tc complex comprising the nitroimidazole ligand, 2,10-dimercapto-2, 10-dimethyl-4, 8-diaza-6-[4-(2-nitroimidazolyl)butyl]undecane, in a low-flow in vivo model of myocardial ischaemia in thoracotomised rats. To elucidate the influence of the 2-nitroimidazole group on ischaemia-induced uptake, comparisons with ligand derivatives were performed where (a) the 2-nitro group was deleted [ 99m TcO(BAT-I)], (b) the 2-nitroimidazole functionality was replaced by a Br atom [ 99m TcO(BAT-Br)] and (c) the 99m TcO(BAT) moiety was replaced by an iodine-125 iodophenoxybutyl ligand ( 125 IP-NI). The radiolabelled compounds were i.v. injected 15 min after reducing resting myocardial blood flow by 50-60% and the uptake of radioactivity was assessed 90 min post injection. Autoradiography of left ventricular short-axis slices showed median uptake ratios of ischaemic/non-ischaemic myocardium (I/N) of 3.4, 4.5 and 3.4 for 99m TcO(BAT-NI), 99m TcO(BAT-I) and 99m TcO(BAT-Br), respectively. In contrast, 125 IP-NI was not preferentially taken up by ischaemic myocardium. Accumulation of 99m TcO(BAT-NI) in ischaemic heart regions was comparable to that in the liver. Biodistribution studies showed a median uptake of 0.65% ID/g of 99m TcO(BAT-NI) in ischaemic tissue and an I/N of 3.3. On planar images of the thorax and upper abdomen the ischaemic hearts were visualised faintly; the median heart to lung count ratio for 99m TcO(BAT-NI) was 1.7, and the median heart to liver count ratio was 1.0. We conclude that uptake of 99m TcO(BAT-NI) in ischaemic myocardium does not depend on the nitroimidazole moiety but is intrinsic to the BAT complex

In vitro and in vivo activities of the nitroimidazole TBA-354 against Mycobacterium tuberculosis.

Science.gov (United States)

Upton, A M; Cho, S; Yang, T J; Kim, Y; Wang, Y; Lu, Y; Wang, B; Xu, J; Mdluli, K; Ma, Z; Franzblau, S G

2015-01-01

Nitroimidazoles are a promising new class of antitubercular agents. The nitroimidazo-oxazole delamanid (OPC-67683, Deltyba) is in phase III trials for the treatment of multidrug-resistant tuberculosis, while the nitroimidazo-oxazine PA-824 is entering phase III for drug-sensitive and drug-resistant tuberculosis. TBA-354 (SN31354[(S)-2-nitro-6-((6-(4-trifluoromethoxy)phenyl)pyridine-3-yl)methoxy)-6,7-dihydro-5H-imidazo[2,1-b][1,3]oxazine]) is a pyridine-containing biaryl compound with exceptional efficacy against chronic murine tuberculosis and favorable bioavailability in preliminary rodent studies. It was selected as a potential next-generation antituberculosis nitroimidazole following an extensive medicinal chemistry effort. Here, we further evaluate the pharmacokinetic properties and activity of TBA-354 against Mycobacterium tuberculosis. TBA-354 is narrow spectrum and bactericidal in vitro against replicating and nonreplicating Mycobacterium tuberculosis, with potency similar to that of delamanid and greater than that of PA-824. The addition of serum protein or albumin does not significantly alter this activity. TBA-354 maintains activity against Mycobacterium tuberculosis H37Rv isogenic monoresistant strains and clinical drug-sensitive and drug-resistant isolates. Spontaneous resistant mutants appear at a frequency of 3 × 10(-7). In vitro studies and in vivo studies in mice confirm that TBA-354 has high bioavailability and a long elimination half-life. In vitro studies suggest a low risk of drug-drug interactions. Low-dose aerosol infection models of acute and chronic murine tuberculosis reveal time- and dose-dependent in vivo bactericidal activity that is at least as potent as that of delamanid and more potent than that of PA-824. Its superior potency and pharmacokinetic profile that predicts suitability for once-daily oral dosing suggest that TBA-354 be studied further for its potential as a next-generation nitroimidazole. Copyright © 2015, American

ORF Alignment: NC_003030 [GENIUS II[Archive

Lifescience Database Archive (English)

Full Text Available NC_003030 gi|15895740 >1w3oA 13 174 5 153 2e-30 ... ref|NP_349089.1| Possible 5-Nitroimidazole antibiotics... ... gb|AAK80429.1| Possible 5-Nitroimidazole antibiotics ... resistance protein, NimA-family [Clost...ridium ... acetobutylicum ATCC 824] pir||B97205 probable ... 5-Nitroimidazole antibiotics

Contribution of the nitroimidazoles PA-824 and TBA-354 to the activity of novel regimens in murine models of tuberculosis.

Science.gov (United States)

Tasneen, Rokeya; Williams, Kathy; Amoabeng, Opokua; Minkowski, Austin; Mdluli, Khisimuzi E; Upton, Anna M; Nuermberger, Eric L

2015-01-01

New regimens based on two or more novel agents are sought in order to shorten or simplify the treatment of both drug-susceptible and drug-resistant forms of tuberculosis. PA-824 is a nitroimidazo-oxazine now in phase II trials and has shown significant early bactericidal activity alone and in combination with the newly approved agent bedaquiline or with pyrazinamide with or without moxifloxacin. While the development of PA-824 continues, a potential next-generation derivative, TBA-354, has been discovered to have in vitro potency superior to that of PA-824 and greater metabolic stability than that of the other nitroimidazole derivative in clinical development, delamanid. In the present study, we compared the activities of PA-824 and TBA-354 as monotherapies in murine models of the initial intensive and continuation phases of treatment, as well as in combination with bedaquiline plus pyrazinamide, sutezolid, and/or clofazimine. The monotherapy studies demonstrated that TBA-354 is 5 to 10 times more potent than PA-824, but selected mutants are cross-resistant to PA-824 and delamanid. The combination studies revealed that TBA-354 is 2 to 4 times more potent than PA-824 when combined with bedaquiline, and when administered at a dose equivalent to that of PA-824, TBA-354 demonstrated superior sterilizing efficacy. Perhaps most importantly, the addition of either nitroimidazole significantly improved the sterilizing activities of bedaquiline and sutezolid, with or without pyrazinamide, confirming the value of each agent in this potentially universally active short-course regimen. Copyright © 2015, American Society for Microbiology. All Rights Reserved.

5-Nitroimidazole Derivatives and their Antimicrobial Activity

International Nuclear Information System (INIS)

Khan, K.M.; Salar, U.; Yousuf, S.; Naz, F.

2016-01-01

5-Nitroimidazole derivatives 2-8 were synthesized from secnidazole. The syntheses were accomplished in two steps which start from the oxidation of secnidazole to the secnidazolone 1. Secnidazolone 1 was converted into its hydrazone derivative 2-8 by treating with different substituted acid hydrazide. Compounds 2-8 were evaluated for their antimicrobial activity against Gram-positive and Gram-negative bacteria, compounds 3 and 4 showed the significant activity against Staphylococcus epidermidis, however, compound 2 showed good inhibitions against Corynebacterium diphtheria when compared with the standard. Compound 3 showed good inhibitory potential against tested Gram-negative bacterial strains i.e. Enterobacter aerogene, Escherichia coli, Salmonella typhi, Salmonella paratyphi A, Shigella flexeneri and Vibrio choleriae. All synthetic derivatives were also tested against eight fungal stains, however, they were weekly active against Aspergillus flavus and Candida albican. The synthesized compounds were characterized by different spectroscopy techniques. (author)

Screening and confirmation of steroids and nitroimidazoles in urine, blood, and food matrices: Sample preparation methods and liquid chromatography tandem mass spectrometric separations.

Science.gov (United States)

Tölgyesi, Ádám; Barta, Enikő; Simon, Andrea; McDonald, Thomas J; Sharma, Virender K

2017-10-25

Veterinary drugs containing synthetic anabolic steroid and nitroimidazole active agents are not allowed for their applications in livestock of the European Union (EU). This paper presents analyses of twelve selected steroids and six nitroimidazole antibiotics at low levels (1.56μg/L-4.95μg/L and 0.17μg/kg-2.14μg/kg, respectively) in body fluids and egg incurred samples. Analyses involved clean-up procedures, high performance liquid chromatography (HPLC) separation, and tandem mass spectrometric screening and confirmatory methods. Target steroids and nitroimidazoles in samples were cleaned by two independent supported liquid extraction and solid phase extraction procedures. Separation of the selected compounds was conducted on Kinetex XB C-18 HPLC column using gradient elution. The screening methods utilised supported liquid extraction that enabled fast and cost effective clean-up. The confirmatory methods were improved by extending the number of matrices and compounds, and by introducing an isotope dilution mass spectrometry for nitroimidazoles. The new methods were validated according to the recommendation of the European Union Reference Laboratories and the performance characteristics evaluated met fully the criteria. The methods were applied to incurred samples in the proficiency tests. The obtained results of Z-scores demonstrated the applicability of developed protocols of the methods to real samples. The confirmatory methods were applied to the national monitoring program and natural contamination of prednisolone could be detected in urine at low concentration in few samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Simple and rapid determination of 5-nitroimidazoles and metabolites in fish roe samples by salting-out assisted liquid-liquid extraction and UHPLC-MS/MS.

Science.gov (United States)

Hernández-Mesa, Maykel; Cruces-Blanco, Carmen; García-Campaña, Ana M

2018-06-30

A novel multiresidue method is proposed for the determination of 12 5-nitroimidazoles and their metabolites in fish roe samples using UHPLC-MS/MS. A salting-out assisted liquid-liquid extraction procedure was performed prior to sample analysis. The separation of compounds was accomplished using a C18 Zorbax Eclipse Plus column (50 mm × 2.1 mm, 1.8 µm) at 25 °C and a mobile phase consisting of 0.025% (v/v) aqueous formic acid and pure MeOH at a flow rate of 0.5 mL/min. Parameters involved in ionization and fragmentation were also optimized. The method was characterized in terms of linearity (R 2  ≥ 0.9992), extraction efficiency (≥68.9%), repeatability (RSD ≤ 9.8%), reproducibility (RSD ≤ 13.9%) and trueness (recoveries ≥81.4%). Decision limits (CCα) and detection capabilities (CCβ) were obtained in the ranges 0.1-1.0 and 0.2-1.7 µg/kg, respectively. Copyright © 2018 Elsevier Ltd. All rights reserved.

Effect of nitroimidazoles on glucose utilization and lactate accumulation in mouse brain

International Nuclear Information System (INIS)

Chao, C.F.; Subjeck, J.R.; Brody, H.; Shen, J.; Johnson, R.J.R.

1984-01-01

The radiation sensitizers misonidazole (MISO) and desmethylmisonidazole (DMM) can produce central and peripheral neuropathy in patients and laboratory animals. Nitroimidazoles can also interfere with glycolysis in vitro under aerobic and anaerobic conditions. In the present work, the authors studied the effect of MISO or DMM on lactate production and glucose utilization in mouse brain. It is observed that these compounds result in a 25% inhibition of lactate production in brain slices relative to the control at a 10 mM level. Additionally, MISO (1.0 mg/g/day) or DMM (1.4 mg/g/day) were administered daily (oral) for 1, 4, 7, or 14 days to examine the effect of these two drugs on the regional glucose utilization in C3Hf mouse brain. Five microcuries of 2-deoxy[ 14 C]glucose was given following the last drug dose and autoradiographs of serial brain sections were made and analyzed by a densitometer. Following a single dose of either MISO or DMM, no significant differences in glucose uptake were observed when compared with controls. However, following 4, 7, and 14 doses the rate of glucose utilization was significantly reduced in the intoxicated animals. Larger reductions were measured in specific regions including the posterior colliculus, cochlear nuclei, vestibular nuclei, and pons with increasing effects observed at later stages. These results share a degree of correspondence with the regional brain pathology produced by these nitroimidazoles

A new look into the quantum chemical and spectroscopic investigations of 5-chloro-1-methyl-4-nitroimidazole.

Science.gov (United States)

Arjunan, V; Raj, Arushma; Anitha, R; Mohan, S

2014-05-05

Optimised geometrical structural parameters, harmonic vibrational frequencies, natural bonding orbital analysis and frontier molecular orbitals are determined by B3LYP and B3PW91 methods. The exact geometry of 5-chloro-1-methyl-4-nitroimidazole is determined through conformational analysis. The experimentally observed infrared and Raman bands have been assigned and analysed. The (13)C and (1)H NMR chemical shifts of the compound are investigated. The total electron density and molecular electrostatic potentials are determined. The electrostatic potential (electron+nuclei) distribution, molecular shape, size and dipole moments of the molecule have been displayed. The energies of the frontier molecular orbitals and LUMO-HOMO energy gap are measured. The possible electronic transitions of the molecule are studied by TD-DFT method along with the UV-Visible spectrum. The structure-activity relationship of the compound is also investigated by conceptual DFT methods. Copyright © 2014 Elsevier B.V. All rights reserved.

Interaction of nitroimidazole sensitizers and oxygen in the radiosensitization of mammalian cells at ultrahigh dose rates

International Nuclear Information System (INIS)

Michaels, H.B.; Ling, C.C.; Epp, E.R.; Peterson, E.C.

1981-01-01

When CHO cells, equilibrated with 0.44% oxygen, are irradiated with single 3-nsec pulses of electrons from a 600-kV-field emission source, a breaking survival curve is observed. The breaking behavior, believed to be the result of radiolytic oxygen depletion, can be prevented by the presence of a relatively low concentration of the hypoxic cell sensitizer misonidazole; similar results are obtained with metronidazole and Ro-05-9963. The resulting survival curves exhibit a sensitized response similar to that obtained with conventional dose rate radiation for CHO cells under this oxygen concentration. This degree of sensitization is greater than that observed for CHO cells irradiated at ultrahigh dose rates under the same concentration of sensitizer in nitrogen. The data suggest that the nitroimidazole compounds interfere with the radiation chemical oxygen depletion process and that the radiosensitization observed in the nonbreaking survival curve is the consequence of sensitization by both the nitroimidazole and, primarily, the oxygen rather than a direct subsitution for oxygen by the sensitizer. This conclusion is also supported by data obtained in double-pulse experiments. The results are discussed with regard to the mechanisms of the oxygen depletion process and radiosensitization

ESR spectroscopy applied to the study of drugs radiosterilization: case of three nitroimidazoles

International Nuclear Information System (INIS)

Duroux, J.L.; Bernard, M.; Basly, J.P.; Penicaut, B.

1996-01-01

The use of ionizing radiation for sterilization of pharmaceuticals is now a well established technology. In this paper, we examined the time stability at ambient conditions and higher temperatures of free radicals produced after the gamma irradiation of three nitroimidazoles: metronidazole, ornidazole and ternidazole. The bi-exponential model used to fit the decay curves showed, in major cases, two simultaneous phases: the first corresponding to a fast 'pure' exponential decay; and, a second corresponding to a slowly 'quasi linear' decay, possibly due to a solid diffusion mechanism. (author)

Factors influencing intracellular uptake and radiosensitization by 2-nitroimidazoles in vitro

International Nuclear Information System (INIS)

Brown, D.M.; Gonzalez-Mendez, R.; Brown, J.M.

1983-01-01

In this study it is shown that the radiosensitization of hypoxic Chinese hamster ovary (HA-1) cells in vitro by misonidazole (MIS) and other 1-substituted 2-nitroimidazoles depends on the rate and extent of intracellular uptake of these radiosensitizers, which in turn is governed by their lipophilicity [expressed as the octanol:water partition coefficient (P)]. As the lipophilicity of the compounds decreased, the rate of drug entry into the cells was slower, and below P values of approximately 0.05, peak intracellular drug concentrations were found to be lower than that of MIS (P=0.43). In addition, the number of hydroxyl groups on the side chain of the nitroimidazole molecule influenced the uptake of drug into the cells. For compounds of similar P, but differing in the number of side-chain hydroxyl groups, the addition of a single hydroxyl group to the molecule decreased the amount of drug entering the cell by a factor of approximately 2. These compounds enter the cell by nonmediated passive diffusion since altering the energy (ATP) capacity of the cell by 2-deoxyglucose did not affect uptake. It is also shown that increases in temperature or decreases in pH can increase the intracellular uptake of MIS. For example, equal intracellular and extracellular concentrations (100% uptake) of MIS were obtained if cells were heated to 44-45 0 C for 15 min compared to 20-40% uptake at 37 0 C. Increases in MIS uptake by factors of 2 to 3 could be demonstrated within 30 min when cells were incubated in Hanks' balanced salt solution at pH between 6.0 and 6.3 without loss of cell viability. In addition, MIS uptake in aerobic cultured cells varied from 15 to 60% depending on the cell line and culure conditions used

Radiosensitization, mutagenicity, and toxicity of Escherichia coli by several nitrofurans and nitroimidazoles. [X radiation

Energy Technology Data Exchange (ETDEWEB)

Chessin, H.; McLaughlin, T.; Mroczkowski, Z.; Rupp, W.D.; Low, K.B.

1978-08-01

Representative nitrofurans (nitrofurantoin, nifuroxime, NF-167, NF-269) and nitroimidazoles (metronidazole, misonidazole) were found to sensitize hypoxic RecA/sup -/ Escherichia coli cells to X irradiation. These compounds were also mutagenic to E. coli using a UvrA/sup -/ strain as a test system, and toxic at high concentrations, using several strains differing in their repair capacity. However, the relative degrees of radiosensitization, mutagenicity, and toxicity, for the various compounds, were not simply correlated, suggesting that potential radiosensitizers with fewer side effects could be screened using bacteria.

Facile and efficient synthesis of [{sup 18}F]fluoromisonidazole using novel 2-nitroimidazole derivatives

Energy Technology Data Exchange (ETDEWEB)

Kwon, Young-Do; Lim, Seok Tae; Sohn, Myung-Hee; Kim, Hee-Kwon, E-mail: hkkim717@jbnu.ac.kr [Department of Nuclear Medicine, Chonbuk National University Medical School and Hospital, Jeonju (Korea, Republic of); Jung, Yongju [Department of Chemical Engineering, Korea University of Technology and Education, Cheonan (Korea, Republic of)

2016-07-01

[{sup 18}F]Fluoromisonidazole ([{sup 18}F]FMISO) is a hypoxia imaging marker utilized in positron emission tomography. Novel FMISO precursors were prepared from a commercially available material, and several reaction factors that affect synthesis of [{sup 18}F]FMISO were examined to achieve a higher fluorination yield. [{sup 18}F]FMISO was obtained from radiosynthesis, followed by the hydrolysis of protecting groups with HCl. New 2-nitroimidazole precursor showed a higher [{sup 18}F]fluorination and a higher synthetic yield. This result provided alternative guidelines for the preparation of hypoxia imaging marker. (author)

Preclinical validation of the hypoxia tracer 2-(2-nitroimidazol-1-yl)-N-(3,3,3-[18F]trifluoropropyl)acetamide, [18F]EF3

International Nuclear Information System (INIS)

Mahy, P.; De Bast, M.; Gregoire, V.; Leveque, P.H.; Gillart, J.; Labar, D.; Marchand, J.

2004-01-01

The 2-nitroimidazole derivative 2-(2-nitroimidazol-1-yl)-N-(3,3,3-trifluoropropyl)acetamide (EF3) is a marker which forms adducts into hypoxic cells. Radiosynthesis of [ 18 F]EF3 was recently performed by our group. Our aim was to study the pharmacokinetics, biodistribution, metabolism and specificity for hypoxia of [ 18 F]EF3. MCa-4, SCC VII, NFSA, FSA, FSA II or Sa-NH tumour-bearing C3H mice were injected intravenously with [ 18 F]EF3 and allowed to breathe air, 10% O 2 or carbogen until sacrifice 5-770 min after injection. Radioactivity was measured ex vivo in various organs, including urine and faeces. Selected organs were additionally processed to measure tracer metabolites with high-performance liquid chromatography. The half-life in blood was 73.9 min. [ 18 F]EF3 was eliminated mainly via the kidneys, with 75% of the injected activity found in the urine by 12 h 50 min. The biodistribution was fast and homogeneous except in the brain and the bone, where it was significantly lower, and in the liver and the kidney, where it was significantly higher. In most organs, the exceptions being the gastrointestinal and urinary tract, tissue-to-blood ratios were below or close to unity. In tumours, a relative accumulation of the tracer was observed with time, which, at 220 min after injection, depended on tumour strain and oxygenation conditions, i.e. 10% O 2 significantly increased the tumour-to-muscle ratio whereas carbogen decreased it. [ 18 F]EF3 was rapidly metabolised in the kidney and the liver. [ 18 F]EF3 is a promising tracer for detection of tumour hypoxia. A phase I study in head and neck cancer patients is in progress at our institution. (orig.)

Labelled compounds of interest as antitumour agents. Pt. 4: Deuteration and tritiation of a nitroimidazole-carborane designed for BNCT

International Nuclear Information System (INIS)

Scobie, Martin; Bew, S.P.; Threadgill, M.D.

1994-01-01

Quenching the anion generated from a 2-(ω-carboranylalkyl)dithiane with 2 H 2 O at -78 o C and at 0 o C introduced deuterium exclusively at C-2 of the carborane. Extension of this model reaction to a bioreductively-targetted carborane allowed the synthesis of 2-[ 2 H]- and 2-[ 3 H]-isotopomers of a nitroimidazole-carborane which is of interest in boron neutron capture therapy (BNCT) of cancer. (author)

Synthesis and Electrochemistry of 2-Ethenyl and 2-Ethanyl Derivatives of 5-Nitroimidazole and Antimicrobial Activity against Giardia lamblia

Science.gov (United States)

Valdez, Carlos A.; Tripp, Jonathan C.; Miyamoto, Yukiko; Kalisiak, Jaroslaw; Hruz, Petr; Andersen, Yolanda S.; Brown, Sabrina E.; Kangas, Karina; Arzu, Leo V.; Davids, Barbara J.; Gillin, Frances D.; Upcroft, Jacqueline A.; Upcroft, Peter; Fokin, Valery V.; Smith, Diane K.; Sharpless, K. Barry; Eckmann, Lars

2009-01-01

Infections with the diarrheagenic pathogen, Giardia lamblia, are commonly treated with the 5-nitroimidazole (5-NI) metronidazole (Mz), and yet treatment failures and Mz resistance occur. Using a panel of new 2-ethenyl and 2-ethanyl 5-NI derivatives, we found that compounds with a saturated bridge between the 5-NI core and a pendant ring system exhibited only modestly increased antigiardial activity and could not overcome Mz resistance. By contrast, olefins with a conjugated bridge connecting the core and a substituted phenyl or heterocyclic ring showed greatly increased antigiardial activity without toxicity, and several overcame Mz resistance and were more effective than Mz in a murine giardiasis model. Determination of the half-wave potential of the initial one-electron transfer by cyclic voltammetry revealed that easier redox activation correlated with greater antigiardial activity and capacity to overcome Mz resistance. These studies show the potential of combining systematic synthetic approaches with biological and electrochemical evaluations in developing improved 5-NI drugs. PMID:19480409

In vivo radiosensitizing effect of nitroimidazole derivative KIN-804

International Nuclear Information System (INIS)

Tada, Takuhito; Nakajima, Toshifumi; Onoyama, Yasuto; Murayama, Chieko; Mori, Yomoyuki; Nagasawa, Hideko; Hori, Hitoshi; Inayama, Seiichi

1994-01-01

In vivo characteristics of 2-nitroimidazole-1-methylacetohydroxamate (KIN-804), which is a newly developed hypoxic cell radiosensitizer, are presented. The toxicity, pharmacokinetics, and radiosensitizing effect of KIN-804 were studied by in vivo experiments using C3H/He mice bearing the SCCVII tumor. Results were compared with misonidazole (MISO). LD 50 7 of KIN-804 and MISO were 3200 mg/kg and 2000 mg/kg, respectively. The peak concentration of KIN-804 in the tumor occurred 20 min after intraperitoneal injection and reached about 62% of the maximum concentration in the blood. The concentrations in brain and sciatic nerve were very low and clearance from sciatic nerve was rapid. Enhancement ratios of KIN-804 calculated using the growth delay method were 1.22, 1.50, and 1.71 at doses of 50, 100, and 200 mg/kg, respectively, compared with 1.36 for MISO at a dose of 100 mg/kg. In the TCD 50 assay, enhancement ratios at a dose of 200 mg/kg were 1.69 for KIN-804 and 1.52 for MISO, respectively. KIN-804 is a promising radiosensitizer since it shows less toxicity and higher radiosensitizing activity than MISO. 10 refs., 5 figs

How does methylation suppress the electron-induced decomposition of 1-methyl-nitroimidazoles?

Science.gov (United States)

Kossoski, F.; Varella, M. T. do N.

2017-10-01

The efficient decomposition of nitroimidazoles (NIs) by low energy electrons is believed to underlie their radiosensitizing properties. Recent dissociative electron attachment (DEA) measurements showed that methylation at the N1 site unexpectedly suppresses the electron-induced reactions in 4(5)-NI. We report theoretical results that provide a clear interpretation of that astounding finding. Around 1.5 eV, DEA reactions into several fragments are initiated by a π* resonance, not considered in previous studies. The autoionization lifetime of this anion state, which limits the predissociation dynamics, is considerably shorter in the methylated species, thereby suppressing the DEA signals. On the other hand, the lifetime of the π* resonance located around 3 eV is less affected by methylation, which explains why DEA is still observed at these energies. Our results demonstrate how even a simple methylation can significantly modify the probabilities for DEA reactions, which may be significant for NI-based cancer therapy.

Radiosensitizing efficacy of iso-metronidazole after intravesical application in bladder cancer. A clinical phase II study

International Nuclear Information System (INIS)

Kob, D.; Lilienthal, A.; Bauhardt, H.; Merkle, K.; Schroeder, E.; Schroeder, E.; Hentschel, M.

1991-01-01

The radiosensitizing efficacy of iso-Metronidazole, a 4-Nitroimidazole derivative, was evaluated in a prospective clinical phase II study. The results of combined radiotherapy of 25 patients with bladder cancer were compared with those of a control group of 25 patients treated with radiotherapy only. Tumor regression six months after radiotherapy was used as an endpoint. The surgical procedure was performed as double TUR. Evaluating the local tumor control after additional application of iso-Metronidazole a gain factor of 1.2 is obtained. (orig.) [de

Syntheses of 2-nitroimidazole derivatives conjugated with 1,4,7-triazacyclononane-N,N'-diacetic acid labeled with F-18 using an aluminum complex method for hypoxia imaging.

Science.gov (United States)

Hoigebazar, Lathika; Jeong, Jae Min; Lee, Ji-Youn; Shetty, Dinesh; Yang, Bo Yeun; Lee, Yun-Sang; Lee, Dong Soo; Chung, June-Key; Lee, Myung Chul

2012-04-12

Hypoxia imaging is important for diagnosis of ischemic diseases, and thus various (18)F-labeled radiopharmaceuticals have been developed. However, (18)F-labeling requires multistep procedures including azeotropic distillation, which is complicated and difficult to automate. Recently, (18)F-labeling method using Al-F complex in aqueous solution was devised that offered a straightforward (18)F-labeling procedure. We synthesized nitroimidazole derivatives conjugated with 1,4,7-triazacyclononane-1,4-diacetic acid (NODA) that can be labeled with (18)F using Al-F complex and examined their radiochemistries, in vitro and in vivo biological properties, and animal PET imaging characteristics. We found that the synthesized derivatives have excellent (18)F-labeling efficiencies, high stabilities, specific uptakes in cultured hypoxic tumor cells, and high tumor to nontumor ratios in xenografted mice. Furthermore, the derivatives were labeled with (18)F in a straightforward manner within 15 min at high labeling efficiencies and radiochemical purities. In conclusion, (18)F-labeled NODA-nitroimidazole conjugates were developed and proved to be promising hypoxia PET agents. © 2012 American Chemical Society

Targeting carbonic anhydrase IX by nitroimidazole based sulfamides enhances the therapeutic effect of tumor irradiation: A new concept of dual targeting drugs

International Nuclear Information System (INIS)

Dubois, Ludwig; Peeters, Sarah G.J.A.; Kuijk, Simon J.A. van; Yaromina, Ala; Lieuwes, Natasja G.; Saraya, Ruchi; Biemans, Rianne; Rami, Marouan; Parvathaneni, Nanda Kumar; Vullo, Daniela; Vooijs, Marc; Supuran, Claudiu T.; Winum, Jean-Yves

2013-01-01

Background and purpose: Carbonic anhydrase IX (CAIX) plays an important role in pH regulation processes critical for tumor cell growth and metastasis. We hypothesize that a dual targeting bioreductive nitroimidazole based anti-CAIX sulfamide drug (DH348) will reduce tumor growth and sensitize tumors to irradiation in a CAIX dependent manner. Material and methods: The effect of the dual targeting anti-CAIX (DH348) and its single targeting control drugs on extracellular acidification and radiosensitivity was examined in HT-29 colorectal carcinoma cells. Tumor growth and time to reach 4× start volume (T4×SV) was monitored for animals receiving DH348 (10 mg/kg) combined with tumor single dose irradiation (10 Gy). Results: In vitro, DH348 reduced hypoxia-induced extracellular acidosis, but did not change hypoxic radiosensitivity. In vivo, DH348 monotherapy decreased tumor growth rate and sensitized tumors to radiation (enhancement ratio 1.50) without systemic toxicity only for CAIX expressing tumors. Conclusions: A newly designed nitroimidazole and sulfamide dual targeting drug reduces hypoxic extracellular acidification, slows down tumor growth at nontoxic doses and sensitizes tumors to irradiation all in a CAIX dependent manner, suggesting no “off-target” effects. Our data therefore indicate the potential utility of a dual drug approach as a new strategy for tumor-specific targeting

Synthesis of 2-nitroimidazole-glycopeptide 68Ga-labeled for identification of areas of hypoxia in the tumor microenvironment

International Nuclear Information System (INIS)

Pérez Nario, Arian; Leiria Campo, Vanessa; Soares Bernardes, Emerson

2016-01-01

Introduction: Hypoxia is a pathological condition characterized by a reduction in oxygen delivery to a tissue or cell specific. It is estimated that 60% of solid tumors in advanced stages have areas of hypoxia and anoxia (almost complete absence of oxygen). It is now known that hypoxia in the tumor microenvironment is closely related to: 1) increased tumor aggressiveness; 2) increased relapse rate; 3) increased resistance to chemotherapy and radiotherapy; 4) poor prognosis of the disease. Therefore the use of non-invasive methods for the identification and quantification of areas of hypoxia in the tumor are extremely important for treating various types of cancers, allowing the use of individualized treatment strategies. Gallium-68 is a radionuclide widely used for positron emission tomography due to the availability of the generator 68 Ge / 68 Ga. With the aim of developing a new potential radiopharmaceutical 68 Ga-labeled for imaging hypoxia, it has been synthesized a new derivative of 2-nitroimidazole. Methods: The new glycopeptide derivative of 2-nitroimidazole was obtained by coupling the derivative of acetic acid 2-nitroimidazole with a glycopeptide obtained by solid phase synthesis, was subsequently conjugated with the chelating agent DOTA-NHS for labeling with the radionuclide 68 Ga . preparation and 68 Ga-labeled glycopeptide optimization marking with respect to solvent, time and temperature was made; also the radiochemical purity was assessed by reversed phase HPLC. Comparison with 18 F-FAZA, radiopharmaceutical used worldwide is also presented. Results: The new glycopeptide conjugate DOTA was conducted successfully synthesized and analyzed by mass spectrometry. Labeling with 68 Ga reached a maximum radiochemical purity of 96.6 ± 0.4% when 15μg glycopeptide was dissolved in 0.2 mL of acetonitrile, chloride 68Ga (5mCi) was evaporated to dryness and reconstituted in 0.1 mL of sterile water at room temperature, followed by heating to 95 ° C for 15 min. In

Nitroimidazoles as hypoxic cell radiosensitizers and hypoxia probes: misonidazole, myths and mistakes.

Science.gov (United States)

Wardman, Peter

2018-03-20

Nitroimidazoles have been extensively explored as hypoxic cell radiosensitizers but have had limited clinical success, with efficacy restricted by toxicity. However, they have proven clinically useful as probes for tumour hypoxia. Both applications, and probably much of the dose-limiting toxicities, reflect the dominant chemical property of electron affinity or ease of reduction, associated with the nitro substituent in an aromatic structure. This single dominant property affords unusual, indeed extraordinary flexibility in drug or probe design, suggesting further development is possible in spite of earlier limitations, in particular building on the benefit of hindsight and an appreciation of errors made in earlier studies. The most notable errors were: the delay in viewing cellular thiol depletion as a likely common artefact in testing in vitro; slow recognition of pH-driven concentration gradients when compounds were weak acids and bases; and a failure to explore the possible involvement of pH and ascorbate in influencing hypoxia probe binding. The experience points to the need to involve a wider range of expertise than that historically involved in many laboratories when studying the effects of chemicals on radiation response or using diagnostic probes.

Crystal structure of di-μ-chlorido-bis[chloridobis(1,2-dimethyl-5-nitro-1H-imidazole-κN3copper(II] acetonitrile disolvate

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Patrick J. Quinlivan

2016-11-01

Full Text Available 1,2-Dimethyl-5-nitroimidazole (dimetridazole, dimet is a compound that belongs to a class of nitroimidazole drugs that are effective at inhibiting the activity of certain parasites and bacteria. However, there are few reports that describe structures of compounds that feature metals complexed by dimet. Therefore, we report here that dimet reacts with CuCl2·H2O to yield a chloride-bridged copper(II dimer, [Cu2Cl4(C5H7N3O24] or [Cu(μ-ClCl(dimet2]2. In this molecule, the CuII ions are coordinated in an approximately trigonal–bipyramidal manner, and the molecule lies across an inversion center. The dihedral angle between the imidazole rings in the asymmetric unit is 4.28 (7°. Compared to metronidazole, dimetridazole lacks the hydroxyethyl group, and thus cannot form intermolecular O...H hydrogen-bonding interactions. Instead, [Cu(μ-ClCl(dimet2]2 exhibits weak intermolecular interactions between the hydrogen atoms of C—H groups and (i oxygen in the nitro groups, and (ii the terminal and bridging chloride ligands. The unit cell contains four disordered acetonitrile molecules. These were modeled as providing a diffuse contribution to the overall scattering by SQUEEZE [Spek (2015. Acta Cryst. C71, 9–18], which identified two voids, each with a volume of 163 Å3 and a count of 46 electrons, indicative of a total of four acetonitrile molecules. These acetonitrile molecules are included in the chemical formula to give the expected calculated density and F(000.

Emodin (1,3,8-trihydroxy-6-methylanthraquinone): a spectrophotometric reagent for the determination of beryllium(II), magnesium(II) and calcium(II)

International Nuclear Information System (INIS)

Pal, T.; Jana, N.R.

1993-01-01

The individual determination of Be II , Mg II or Ca II by conventional spectrophotometry and simultaneous determination of Mg II and Ca II in mixtures by first-derivative spectrophotometry are possible at trace levels, using emodin (1,3,8-trihydroxy-6-methylanthraquinone) as spectrophotometric reagent. Interference from other metal species, application of these methods to rock samples and statistical analysis of the results are discussed. (author)

Imaging Mass Spectrometry Revealed the Accumulation Characteristics of the 2-Nitroimidazole-Based Agent "Pimonidazole" in Hypoxia.

Directory of Open Access Journals (Sweden)

Yukiko Masaki

Full Text Available Hypoxia, or low oxygen concentration, is a key factor promoting tumor progression and angiogenesis and resistance of cancer to radiotherapy and chemotherapy. 2-Nitroimidazole-based agents have been widely used in pathological and nuclear medicine examinations to detect hypoxic regions in tumors; in particular, pimonidazole is used for histochemical staining of hypoxic regions. It is considered to accumulate in hypoxic cells via covalent binding with macromolecules or by forming reductive metabolites after reduction of its nitro group. However, the detailed mechanism of its accumulation remains unknown. In this study, we investigated the accumulation mechanism of pimonidazole in hypoxic tumor tissues in a mouse model by mass spectrometric analyses including imaging mass spectrometry (IMS. Pimonidazole and its reductive metabolites were observed in the tumor tissues. However, their locations in the tumor sections were not similar to the positively stained areas in pimonidazole-immunohistochemistry, an area considered hypoxic. The glutathione conjugate of reduced pimonidazole, a low-molecular-weight metabolite of pimonidazole, was found in tumor tissues by LC-MS analysis, and our IMS study determined that the intratumor localization of the glutathione conjugate was consistent with the area positively immunostained for pimonidazole. We also found complementary localization of the glutathione conjugate and reduced glutathione (GSH, implying that formation of the glutathione conjugate occurred in the tumor tissue. These results suggest that in hypoxic tumor cells, pimonidazole is reduced at its nitro group, followed by conjugation with GSH.

Energy determination at BEPC-II

International Nuclear Information System (INIS)

Achasov, M.N.; Blinov, V.E.; Bogomyagkov, A.V.; Fu ChengDong; Harris, F.A.; Kaminsky, V.V.; Liu, Q.; Mo Xiaohu; Muchnoi, N.Yu.; Nikitin, S.A.; Nikolaev, I.B.; Qin Qing; Qu Huamin; Olsen, S.L.; Pyata, E.E.; Shamov, A.G.; Shen, C.P.; Varner, G.S.; Wang Yifang; Xu Jinqiang

2009-01-01

The BEPC-II collider beam energy calibration system is discussed. The system is based on the Compton backscattering method. The expected precision of the electron and positron beam energy ε determination is δε/ε∼3.10 -5 .

Optimization of simultaneous electrochemical determination of Cd(II), Pb(II), Cu(II) and Hg(II) at carbon nanotube-modified graphite electrodes.

Science.gov (United States)

Pikna, L'ubomír; Heželová, Mária; Kováčová, Zuzana

2015-01-01

The health of the environment is worsening every day. Monitoring of potentially toxic elements and remediation of environmental pollution are necessary. Therefore, the research and development of simple, inexpensive, portable and effective sensors is important. Electrochemistry is a useful component of the field of environment monitoring. The present study focuses on evaluating and comparing three types of electrodes (PIGE, PIGE/MWCNT/HNO3 and PIGE/MWCNT/EDTA/HNO3) employed for the simultaneous electrochemical determination of four potentially toxic elements: Cd(II), Pb(II), Cu(II) and Hg(II). Cyclic voltammograms were measured in an acetate buffer. The LOD, LOQ, the standard and relative precisions of the method and a prediction intervals were calculated (according to the technical procedure DIN 32 645) for the three electrodes and for each measured element. The LOD for PIGE/CNT/HNO3 (the electrode with narrowest calculated prediction intervals) was 2.98 × 10(-7) mol L(-1) for Cd(II), 4.83 × 10(-7) mol L(-1) for Pb(II), 3.81 × 10(-7) mol L(-1) for Cu(II), 6.79 × 10(-7) mol L(-1) for Hg(II). One of the benefits of this study was the determination of the amount of Hg(II) in the mixture of other elements.

Radiosensitization of hypoxic bacterial cells by nitroimidazoles of low lipophilicity: steady-state and rapid-mix studies

International Nuclear Information System (INIS)

Anderson, R.F.; Patel, K.B.; Sehmi, D.S.

1981-01-01

Radiosensitization of hypoxic bacterial cells by five 2-nitroimidazoles, with similar reduction potentials to misonidazole but having lower lipophilicites, has been measured in Escherichia coli AB 1157 and Streptococcus lactis 712. Sensitization efficiency progressively decreased with decreasing lepophilicity in E. coli but not in S. lactis. This difference is discussed in terms of the differing membrane properties of the two bacteria; E. coli resembled a multicompartment model, as would also be expected with mammalian cells. Rapid-mix experiments are described which show that the radiosensitization observed after experiments are described which show that the radiosensitization observed after preirradiation contact times between ca. 3 and 30 msec is dependent on the lipophilicity of the sensitizer, higher lipophilicity resulting in a lower contact time being required for radiosensitization. This result and the observation that a highly lipophilic compound affects only half the full oxygen enhancement level after short contact times suggest that part of the sensitization process occurs in a lipophilic compartment of the cell

Spectrophotometric determination of cobalt(II), nickel(II) and copper (II) with 1-(2 pyridylazo)-2-naphthol in micellar medium

International Nuclear Information System (INIS)

Shar, G.A.; Soomro, G.A.

2004-01-01

Spectrophotometric determination of cobalt(II), nickel(II) and copper(II) is carried out with 1-(2 pyridylazo)-2-naphthol as a complexing reagent in aqueous phase using non-ionic surfactant Tween 80. Beer's law is obeyed for Co(II), Ni(II) and Cu(II) over the range 0.5 - 4.0, 0.5 - 4.0 and 0.5 - 3.0 ngmL/sup -1/ with detection limit (2 σ) of 6.7, 3.2 and 3.9 ngmL/sup -1/. The max molar absorption, molar absorptivity, Sandell's sensitivity of Co(II), Ni(II) and Cu(II) are 580 nm, 570 nm and 555 nm; max (104 mol/sup -1/ cm /sup -1/) is 0.87, 1.8 and 1.6 and 6.8, 3.3 and 3.9 ng cm-2 respectively. The pH at which complex is formed for Co(II), Ni(II) and Cu(II) is 5, 5.5 and 6.5 respectively. The critical micelle concentration (CMC) of Tween 80 is 5%. The present method is compared with that of atomic absorption spectroscopy and no significant difference is noted between the two methods at 95% confidence level. The method has been applied to the determination of Co(II), Ni(II) and Cu(II) in industrial waste water and pharmaceutical samples. (author)

Determination of activities of human carbonic anhydrase II inhibitors ...

African Journals Online (AJOL)

Purpose: To evaluate the activities of new curcumin analogs as carbonic anhydrase II (CA-II) inhibitor. Methods: Carbonic anhydrase II (CA-II) inhibition was determined by each ligand capability to inhibit the esterase activity of CA-II using 4-NPA as a substrate in 96-well plates. Dimethyl sulfoxide was used to dissolve each ...

Hydrothermal synthesis of polyethylenimine-protected high luminescent Pt-nanoclusters and their application to the detection of nitroimidazoles

International Nuclear Information System (INIS)

Xu, Na; Li, Hong-Wei; Wu, Yuqing

2017-01-01

A novel one-step hydrothermal synthesis of highly fluorescent platinum nanoclusters protected by polyethylenimine (Pt-NCs@PEI) is described. The products are characterized well by UV–vis absorption, fluorescence spectra, X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM) imaging. The Pt-NCs@PEI possess high quantum yield at 28%, which is the relatively high one among the reported Pt-NCs; especially, the synthesis is in one-step and the reaction time is much shorter (<1 h) than the related methods. In addition, the Pt-NCs@PEI have large Stocks-shift (∼150 nm), high tolerability to the extreme pH and high ionic strengths, and excellent photo-stability under UV–vis irradiation, lay the foundation for the practical bio-applications. Finally, the obtained Pt-NCs@PEI are used to determine trace amount of metronidazole (MTZ) in buffer solution in showing a linear response over a concentration range of 0.25–300 μM and a low detection limit of 0.1 μM. Furthermore, the related investigation on response mechanism will be helpful to design and synthesize new metal nanoclusters as fluorescent probe to detect the trace amount of harmful medicine residuum as nitroimidazoles in human body. - Highlights: • This paper provides the first hydrothermal synthesis of platinum nanoclusters. • The prepared polyethylenimine-protected platinum nanoclusters possess high quantum yield of 28%. • A new method to detect trace amount of metronidazole in urine is proposed.

Hydrothermal synthesis of polyethylenimine-protected high luminescent Pt-nanoclusters and their application to the detection of nitroimidazoles

Energy Technology Data Exchange (ETDEWEB)

Xu, Na [State Key Laboratory of Supramolecular Structure and Materials, College of Chemistry, Jilin University, Changchun, 130012 (China); College of Materials Science and Engineering, Jilin Institute of Chemical Technology, Jilin, 132022 (China); Li, Hong-Wei, E-mail: lihongwei@jlu.edu.cn [State Key Laboratory of Supramolecular Structure and Materials, College of Chemistry, Jilin University, Changchun, 130012 (China); Wu, Yuqing, E-mail: yqwu@jlu.edu.cn [State Key Laboratory of Supramolecular Structure and Materials, College of Chemistry, Jilin University, Changchun, 130012 (China)

2017-03-15

A novel one-step hydrothermal synthesis of highly fluorescent platinum nanoclusters protected by polyethylenimine (Pt-NCs@PEI) is described. The products are characterized well by UV–vis absorption, fluorescence spectra, X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM) imaging. The Pt-NCs@PEI possess high quantum yield at 28%, which is the relatively high one among the reported Pt-NCs; especially, the synthesis is in one-step and the reaction time is much shorter (<1 h) than the related methods. In addition, the Pt-NCs@PEI have large Stocks-shift (∼150 nm), high tolerability to the extreme pH and high ionic strengths, and excellent photo-stability under UV–vis irradiation, lay the foundation for the practical bio-applications. Finally, the obtained Pt-NCs@PEI are used to determine trace amount of metronidazole (MTZ) in buffer solution in showing a linear response over a concentration range of 0.25–300 μM and a low detection limit of 0.1 μM. Furthermore, the related investigation on response mechanism will be helpful to design and synthesize new metal nanoclusters as fluorescent probe to detect the trace amount of harmful medicine residuum as nitroimidazoles in human body. - Highlights: • This paper provides the first hydrothermal synthesis of platinum nanoclusters. • The prepared polyethylenimine-protected platinum nanoclusters possess high quantum yield of 28%. • A new method to detect trace amount of metronidazole in urine is proposed.

Iodometric determination of peroxydiphosphate in the presence of copper(II) or iron(II) as catalyst.

Science.gov (United States)

Kapoor, S; Sharma, P D; Gupta, Y K

1975-09-01

Peroxydiphosphate can be determined iodometrically in the presence of a large excess of potassium iodide with copper(II) or iron(II) as catalyst through the operation of the Cu(II)/Cu(I) or Fe(II)/Fe(III) cycle. The method is applicable in HClO(4), H(2)SO(4), HCl and CH(3)COOH acid media in the range 0.1-1.0M studied. Nickel, manganese(II), cobalt(II), silver, chloride and phosphate are without effect.

Synthesis of hypoxia imaging agent 1-(5-deoxy-5-fluoro-α-D-arabinofuranosyl)-2-nitroimidazole using microfluidic technology

International Nuclear Information System (INIS)

Bouvet, Vincent R.; Wuest, Melinda; Wiebe, Leonard I.; Wuest, Frank

2011-01-01

Introduction: Microfluidic technology allows fast reactions in a simple experimental setup, while using very low volumes and amounts of starting material. Consequently, microfluidic technology is an ideal tool for radiolabeling reactions involving short-lived positron emitters. Optimization of the complex array of different reaction conditions requires knowledge of the different reaction parameters linked to the microfluidic system as well as their influence on the radiochemical yields. 1-(5-Deoxy-5-fluoro-α-D-arabinofuranosyl)-2-nitroimidazole ([ 18 F]FAZA) is a frequently used radiotracer for PET imaging of tumor hypoxia. The present study describes the radiosynthesis of [ 18 F]FAZA by means of microfluidic technology and subsequent small animal PET imaging in EMT-6 tumor-bearing mice. Methods: Radiosyntheses were performed using the NanoTek Microfluidic Synthesis System (Advion BioSciences, Inc.). Optimal reaction conditions were studied through screening different reaction parameters like temperature, flow rate, residency time, concentration of the labeling precursor (1-(2,3-di-O-acetyl-5-O-tosyl-α-D-arabinofuranosyl)-2-nitroimidazole) and the applied volume ratio between the labeling precursor and [ 18 F]fluoride. Results: Optimized reaction conditions at low radioactivity levels (1 to 50 MBq) afforded 63% (decay-corrected) of HPLC-purified [ 18 F]FAZA within 25 min. Higher radioactivity levels (0.4 to 2.1 GBq) gave HPLC-purified [ 18 F]FAZA in radiochemical yields of 40% (decay-corrected) within 60 min at a specific activity in the range of 70 to 150 GBq/μmol. Small animal PET studies in EMT-6 tumor-bearing mice showed radioactivity accumulation in the tumor (SUV 20min 0.74 ± 0.08) resulting in an increasing tumor-to-muscle ratio over time. Conclusions: Microfluidic technology is an ideal method for the rapid and efficient radiosynthesis of [ 18 F]FAZA for preclinical radiopharmacological studies. Careful analysis of various reaction parameters is an

Covalent triazine framework-1 as adsorbent for inline solid phase extraction-high performance liquid chromatographic analysis of trace nitroimidazoles in porcine liver and environmental waters.

Science.gov (United States)

Zhong, Cheng; Chen, Beibei; He, Man; Hu, Bin

2017-02-03

In this study, covalent triazine framework-1 (CTF-1) was adopted as solid phase extraction (SPE) sorbents, and a method of SPE inline coupled with high performance liquid chromatography-ultraviolet (HPLC-UV) detection was developed for trace analysis of three nitroimidazolaes (including metronidazole, ronidazole and dimetridazole) in porcine liver and environmental water samples. CTF-1 has rich π-electron and N containing triazine, thus can form π-π interaction and intermolecular hydrogen bond with three target polar nitroimidazoles, resulting in high extraction efficiency (87%-98%). Besides, CTF-1 has large specific area, which benefits rapid mass transfer and low column pressure, leading to fast adsorption/desorption dynamics. Several parameters affecting inline SPE including pH, sample flow rate, sample volume, desorption reagents, elution flow rate, elution volume, and ionic strength were investigated. Under the optimal experimental conditions, the limits of detection (S/N=3) were found to be in the range of 0.11-0.13μg/L. The enrichment factors (EFs) ranged from 52 to 59 fold (theoretical EF was 60-fold). The relative standard deviations were in the range of 4.3-9.4% (n=7, c=1μg/L), and the linear range was 0.5-500μg/L for three target analytes. The sample throughput is 7/h. The proposed method was successfully applied to the analysis of nitroimidazoles in porcine liver and environmental water samples with good recoveries for the spiked samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Expanded therapeutic potential in activity space of next-generation 5-nitroimidazole antimicrobials with broad structural diversity

Science.gov (United States)

Miyamoto, Yukiko; Kalisiak, Jarosław; Korthals, Keith; Lauwaet, Tineke; Cheung, Dae Young; Lozano, Ricardo; Cobo, Eduardo R.; Upcroft, Peter; Upcroft, Jacqueline A.; Berg, Douglas E.; Gillin, Frances D.; Fokin, Valery V.; Sharpless, K. Barry; Eckmann, Lars

2013-01-01

Metronidazole and other 5-nitroimidazoles (5-NI) are among the most effective antimicrobials available against many important anaerobic pathogens, but evolving resistance is threatening their long-term clinical utility. The common 5-NIs were developed decades ago, yet little 5-NI drug development has since taken place, leaving the true potential of this important drug class unexplored. Here we report on a unique approach to the modular synthesis of diversified 5-NIs for broad exploration of their antimicrobial potential. Many of the more than 650 synthesized compounds, carrying structurally diverse functional groups, have vastly improved activity against a range of microbes, including the pathogenic protozoa Giardia lamblia and Trichomonas vaginalis, and the bacterial pathogens Helicobacter pylori, Clostridium difficile, and Bacteroides fragilis. Furthermore, they can overcome different forms of drug resistance, and are active and nontoxic in animal infection models. These findings provide impetus to the development of structurally diverse, next-generation 5-NI drugs as agents in the antimicrobial armamentarium, thus ensuring their future viability as primary therapeutic agents against many clinically important infections. PMID:24101497

Keynote address: cellular reduction of nitroimidazole drugs: potential for selective chemotherapy and diagnosis of hypoxic cells

International Nuclear Information System (INIS)

Chapman, J.D.; Lee, J.; Meeker, B.E.

1989-01-01

Nitroimidazole drugs were initially developed as selective radiosensitizers of hypoxic cells and, consequently, as adjuvants to improve the local control probabilities of current radiotherapies. Misonidazole (MISO), the prototype radiosensitizing drug, was found in Phase I clinical studies to cause dose-limiting neurotoxicities (mainly peripheral neuropathies). MISO was also found to be cytotoxic in the absence of radiation and to covalently bind to cellular molecules, both processes demonstrating rates much higher in hypoxic compared with oxygenated cells. It is likely that neurotoxicity, cellular cytotoxicity and adduct formation results from reactions between reduction intermediates of MISO and cellular target molecules. Spin-offs from radiosensitizer research include the synthesis and characterization of more potent hypoxic cytotoxins and the exploitation of sensitizer-adducts as probes for measuring cellular and tissue oxygen levels. Current developments in hypoxic cell cytotoxin and hypoxic cell marker research are reviewed with specific examples from studies which characterize the cellular reduction of TF-MISO, (1-(2-nitro-1-imidazolyl)-3[2,2,2-trifluoroethoxy]-2-propanol). 45 references

Colorimeter determination of Fe(II)/Fe(III) ratio in glass

International Nuclear Information System (INIS)

Baumann, E.W.; Coleman, C.J.; Karraker, D.G.; Scott, W.H.

1987-01-01

A colorimetric method has been developed to determine the Fe(II)/Fe(III) ratio in glass containing nuclear waste. Fe(II) is stabilized with pentavalent vanadium during dissolution in sulfuric and hydrofluoric acids. The chromogen is FerroZine (Hach Chemical Company), which forms a magenta complex with Fe(II). The two-step color development consists of determining the Fe(II) by adding FerroZine, followed by determining total Fe after the Fe(III) present is reduced with ascorbic acid. The method was validated by analyzing mixtures of ferrous/ferric solutions and nonferrous glass frit, and by comparison with Moessbauer spectroscopy. The effect of gamma radiation was established. The procedure is generally applicable to nonradioactive materials such as minerals and other glasses

Antibacterianos de acción sistémica: Parte II. Otros grupos de antibióticos

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Manuel Cué Brugueras

1998-08-01

Full Text Available Se presenta la segunda parte de una revisión bibliográfica sobre los antibacterianos de acción sistémica, la cual incluye grupos de antibióticos tan importantes como aminociclitoles, aminoglucósidos, diaminopirimidinas, estreptograminas, fosfomicinas, fusidanos, glicopéptidos, lincosamidas, macrólidos, nitrofuranos, nitroimidazoles, polipéptios, quinolonas y rifamicinasThe second part of the literature review on systemic antibacterial drugs is presented. It deals with such important groups of antibiotics as aminociclitol, aminoglycosides, diaminopirimidine, streptogramin, fosfomycin, fusidane, glycopeptides, lincosamides, macrolides, nitrofurans, nitroimidazols, polypeptides, quinolones, and rifamycins

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

Science.gov (United States)

Berber, Hale; Alpdogan, Güzin

2017-01-01

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

High-sensitivity determination of Zn(II) and Cu(II) in vitro by fluorescence polarization

Science.gov (United States)

Thompson, Richard B.; Maliwal, Badri P.; Feliccia, Vincent; Fierke, Carol A.

1998-04-01

Recent work has suggested that free Cu(II) may play a role in syndromes such as Crohn's and Wilson's diseases, as well as being a pollutant toxic at low levels to shellfish and sheep. Similarly, Zn(II) has been implicated in some neural damage in the brain resulting from epilepsy and ischemia. Several high sensitivity methods exist for determining these ions in solution, including GFAAS, ICP-MS, ICP-ES, and electrochemical techniques. However, these techniques are generally slow and costly, require pretreatment of the sample, require complex instruments and skilled personnel, and are incapable of imaging at the cellular and subcellular level. To address these shortcomings we developed fluorescence polarization (anisotropy) biosensing methods for these ions which are very sensitivity, highly selective, require simple instrumentation and little pretreatment, and are inexpensive. Thus free Cu(II) or Zn(II) can be determined at picomolar levels by changes in fluorescence polarization, lifetime, or wavelength ratio using these methods; these techniques may be adapted to microscopy.

Radioimmunologic determination of plasmapepsinogen II

International Nuclear Information System (INIS)

Patzschke, C.; Berg, U.

1979-01-01

Within the frame of this study the pepsinogen II concentration could be determined for the first time with a radioimmunoassay in the plasma. In our normal study group the mean value was 13.91 ng/ml with a variation between 4.08 and 36.19 ng/ml. With increasing patient age a continuous increase of this concentration could be observed. The mean value of 14.99 ng/ml for male patients was by 4.75 ng/ml higher than the mean value of 10.24 ng/ml for female patients. The 24 hour profiles represented for the pepsinogen plasma concentration daily physiologic fluctuations and a stabilisation at night. The effects of meals could not be defined unambiguously. In stimulation tests Pentagastrin provoked in 4 of 9 test persons an increase of the concentration of up to 70% of the basic value. In short-term stress-tests the Pg II concentrations found in the test subjects presented an increase or a decrease. In investigations before or after the same patient underwent an operative procedure, an expressive Pg II decrease (up to 33.74 ng/ml) could be detected. Patients with a total resection of the stomach had only a very low Pg II concentration (less than 3.1 ng/ml). In patients with gastric pathologies a significant difference of the confidence limits was found for the Pg II concentration between superficial gastritis (m = 16.04 ng/ml) and atrophic gastritis (m = 27.38 ng/ml). Compared with various gastric diseases the normal patient group presents a significant difference with reference to the atrophic gastritis or the cancerous stomach. The mean values found in atrophic gastritis or the cancerous stomach. The mean values found in atrophic gastritis and in gastric carcinoma are close to each other and are increased, compared to those measured in the normal patient group. (orig./MG) [de

Methods of humidity determination Part II: Determination of material humidity

OpenAIRE

Rübner, Katrin; Balköse, Devrim; Robens, E.

2008-01-01

Part II covers the most common methods of measuring the humidity of solid material. State of water near solid surfaces, gravimetric measurement of material humidity, measurement of water sorption isotherms, chemical methods for determination of water content, measurement of material humidity via the gas phase, standardisation, cosmonautical observations are reviewed.

Determination of tin (II) in radiopharmaceutical kits by polarographic method

International Nuclear Information System (INIS)

Aungurarat, A.; Thuntawewadthananon, T.

1996-01-01

Radiopharmaceutical kit is a diagnostic compound which contains Stannous (II) as a reducing agent. The quantity of Stannous (II) is depended on the type of kits. So the quantity of Stannous (II) is determined by polarographic method with Differential Pulse Voltammetry (D P Mode) in which a saturated calomel electrode is used as anode and a dropping mercury electrode is used as cathode. Both of electrodes are immerged in the premixed solution of supporting electrolyte and analytical Stannous (II). The Stannous (II) is determined by direct method Stannous (II) is analyzed in the form of Stannous; Sn 2 + itself, and indirect method Stannous (II) is analyzed in the form of S tannic; Sn 4+ (Sn 2+ , + N H 4 + ----> Sn 4+ ). Both methods are done at polarographic half wave potential -470 and -520 mV respectively. The Limit of Detection (LOD) of the direct method is 1.9445 micro g and indirect method is 1.3018 micro g. The result received from indirect method is much more accurate than the direct method (Sn 2+ ). The accuracy of the direct method is about 97.5-102.5% recovery

Simultaneous Determination of Cobalt (II and Nickel (II By First Order Derivative Spectrophotometry in Micellar Media

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Rajni Rohilla

2012-01-01

Full Text Available A first-derivative spectrophotometry method for the simultaneous determination of Co (II and Ni (II with Alizarin Red S in presence of Triton X-100 is described. Measurements were made at the zero-crossing wavelengths at 549.0 nm for Co (II and 546.0 nm for Ni (II. The linearity is obtained in the range of 0.291- 4.676 μg/ml of Ni (II and 0.293- 4.124 μg/ml of Co (II in the presence of each other by using first derivative spectrophotometric method. The possible interfering effects of various ions were studied. The validity of the method was examined by using synthetic mixtures of Co (II and Ni (II. The developed derivative procedure, using the zero crossing technique, has been successfully applied for the simultaneous analysis of Co (II and Ni (II in spiked water samples.

Complexometric determination, Part II: Complexometric determination of Cu2+-ions

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Rajković Miloš B.

2002-01-01

Full Text Available A copper-selective electrode of the coated wire type based on sulphidized copper wire was applied successfully for determining Cu(II ions by complexometric titration with the disodium salt of EDTA (complexon III. By the formation of internal complex compounds with the Cu(II ion, the copper concentration in the solution decreases, and all this is followed by a change of potential of the indicator system Cu-DWISE (or Cu-EDWISE/SCE. At the terminal point of titration, when all the Cu(II ions are already utilized for the formation of the complex with EDTA, there occurs a steep rise of potential, thus enabling us, through the first or second derivative to note the quantity of copper that is present in the solution. Copper-selective electrode showed a responsivity towards titration with EDTA as a complexing agent, with the absence of "fatigue" due to a great number of repeated measurings. Errors occurring during quantitative measurements were more a characteristic of the overall procedure which involve, because of the impossibility of the complete absence of subjectivity, a constant error, and the reproducibility of the results confirmed this fact. The disodium salt of EDTA appeared as a very efficient titrant in all titrations and with various concentrations ot Cu(II ions in the solution, with somewhat weaker response at lower concentrations in the solution.

PVC Based Membrane of Ti(IV Iodovanadate for Pb(II Determination

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Mu. Naushad

2008-08-01

Full Text Available Ti(IV iodovanadate has been synthesized by mixing a mixture of aqueous solutions of 0.1 M sodium vanadate and 0.1 M potassium iodate with 0.1 M solution of Ti(IV chloride at pH 1.0. Distribution coefficients (Kd of various metal ions were determined on the column of Ti(IV iodovanadate which showed the selectivity of Pb(II ions by this cation exchange material. So Ti(IV iodovanadate has been used as an electoactive material for the construction of Pb(II selective electrode. The main purpose of this study is to develop an inexpensive, simple and reliable ion-selective electrode for Pb(II determination. The sensor exhibit Nernstian response for Pb(II ions over a wide concentration range of 1 x 10-7 M to 1 x 10-1 M with a slope of 30±0.4 mV per decade of activity. The electrode is suitable for use in aqueous solution in a pH range of 2-7.2 with a response time of 10 second. The membrane electrode can be used at least for 4 months without any divergence in potential. The selectivity coefficients were determined by the mixed solution method and revealed that the electrode was selective for Pb(II ions in the presence of interfering cations. The sensor could be used as an indicator electrode in the potentiometric titration of Pb(II ions with EDTA. The practical applicability of the proposed sensor has been reported for Pb(II determination in a standard rock sample and water sample. The results are found to be in good agreement with those obtained by using conventional methods.

Determination of kinetic and equilibrium parameters of the batch adsorption of Mn(II), Co(II), Ni(II) and Cu(II) from aqueous solution by black carrot (Daucus carota L.) residues

International Nuclear Information System (INIS)

Guezel, Fuat; Yakut, Hakan; Topal, Giray

2008-01-01

In this study, the effect of temperature on the adsorption of Mn(II), Ni(II), Co(II) and Cu(II) from aqueous solution by modified carrot residues (MCR) was investigated. The equilibrium contact times of adsorption process for each heavy metals-MCR systems were determined. Kinetic data obtained for each heavy metal by MCR at different temperatures were applied to the Lagergren equation, and adsorption rate constants (k ads ) at these temperatures were determined. These rate constants related to the adsorption of heavy metal by MCR were applied to the Arrhenius equation, and activation energies (E a ) were determined. In addition, the isotherms for adsorption of each heavy metal by MCR at different temperatures were also determined. These isothermal data were applied to linear forms of isotherm equations that they fit the Langmuir adsorption isotherm, and the Langmuir constants (q m and b) were calculated. b constants determined at different temperatures were applied to thermodynamic equations, and thermodynamic parameters such as enthalpy (ΔH), free energy (ΔG), and entropy (ΔS) were calculated and these values show that adsorption of heavy metal on MCR was an endothermic process and process of adsorption was favoured at high temperatures

Fluorescent sensing and determination of mercury (II) ions in water ...

African Journals Online (AJOL)

In this study we report on a fluorescent sensing probe based on a naphthyl azo dye modified dibenzo-18-crown-6-ether (DB18C6) for the detection and determination of mercury (II) ions in water. The probe showed high sensitivity and selectivity towards the mercury (II) ion among various alkali, alkaline earth, and transition ...

Penicillamine-modified sensor for the voltammetric determination of Cd(II) and Pb(II) ions in natural samples.

Science.gov (United States)

Pérez-Ràfols, Clara; Serrano, Núria; Díaz-Cruz, José Manuel; Ariño, Cristina; Esteban, Miquel

2015-11-01

A new penicillamine-GCE was developed based on the immobilization of d-penicillamine on aryl diazonium salt monolayers anchored to the glassy carbon electrode (GCE) surface and it was applied for the first time to the simultaneous determination of Cd(II) and Pb(II) ions by stripping voltammetric techniques. The detection and quantification limits at levels of µg L(-1) suggest that the penicillamine-GCE could be fully suitable for the determination of the considered ions in natural samples. Copyright © 2015 Elsevier B.V. All rights reserved.

The determination of 800 to 30 μg lead(II) by potentiometric titration with molybdate

International Nuclear Information System (INIS)

Campiglio, A.

1985-01-01

The determination of 800 to 30 μg Pb(II) by potentiometric titration with molybdate by using a lead(II)-selective electrode was investigated. Under suitable conditions, 800 to 300 μg Pb(II) in aqueous solution by automatic or manual titration with 4x10 -3 M molybdate can be determined with an accuracy of +-0.57% and +-0.45% and a precision of +-0.43% and 0.30% (standard deviation = 0.25% and 0.17%, resp.). For determining amounts of Pb(II) below 300 μg, a 2x10 -3 M molybdate solution has to be used. Although 300 to 100μg Pb(II) are determinable again in water with satisfactory results, the titration in 40% ethanol is however more reliable: in this medium, amounts of 300 to 30μg Pb(II) can be determined with an accuracy of +-1% and a precision of +-2% (standard deviation from 20 titrations of 100μg Pb(II)=0.60%). The titration of 300-800μg Pb(II) in water and of 30-300μg Pb(II) in 40% ethanol is also possible in 0.1 M NaNO 3 sub- snd 0.1 M NaClO 4 sub- medium and can be used in the lead determination in organic compounds after mineralization with HNO 3 sub-HClO 4 sub-H 2 O 2 . (Author)

Determination of Proton Relaxivities of Mn(II, Cu(II and Cr(III added to Solutions of Serum Proteins

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Ali Yilmaz

2009-04-01

Full Text Available Relaxometric studies are still of scientific interest due to their use in medicine and biology. In this study, proton T1 and T2 relaxivities of Mn(II, Cu(II and Cr(III in water were determined in the presence and absence of various proteins (albumin, α-globulin, γ-globulin, lysozyme, fibrinogen. The 1/T1 and 1/T2 in all solutions are linearly proportional to the concentration of the paramagnetic ions. Mn(II has the great influence to alter relaxations in all protein solutions, while Cu(II and Cr(III have a poor influence on the relaxations. In addition, Mn(II and Cu(II are bound to each protein, but Cr(III is not bound to any protein.

A High Sensitivity Micro Format Chemiluminescence Enzyme Inhibition Assay for Determination of Hg(II

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Kanchanmala Deshpande

2010-06-01

Full Text Available A highly sensitive and specific enzyme inhibition assay based on alcohol oxidase (AlOx and horseradish peroxidase (HRP for determination of mercury Hg(II in water samples has been presented. This article describes the optimization and miniaturization of an enzymatic assay using a chemiluminescence reaction. The analytical performance and detection limit for determination of Hg(II was optimized in 96 well plates and further extended to 384 well plates with a 10-fold reduction in assay volume. Inhibition of the enzyme activity by dissolved Hg(II was found to be linear in the range 5–500 pg.mL−1 with 3% CVin inter-batch assay. Due to miniaturization of assay in 384 well plates, Hg(II was measurable as low as 1 pg.mL−1 within15 min. About 10-fold more specificity of the developed assay for Hg(II analysis was confirmed by challenging with interfering divalent metal ions such as cadmium Cd(II and lead Pb(II. Using the proposed assay we could successfully demonstrate that in a composite mixture of Hg(II, Cd(II and Pb(II, inhibition by each metal ion is significantly enhanced in the presence of the others. Applicability of the proposed assay for the determination of the Hg(II in spiked drinking and sea water resulted in recoveries ranging from 100–110.52%.

Spectrophotometric Determination of Iron(II and Cobalt(II by Direct, Derivative, and Simultaneous Methods Using 2-Hydroxy-1-Naphthaldehyde-p-Hydroxybenzoichydrazone

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V. S. Anusuya Devi

2012-01-01

Full Text Available Optimized and validated spectrophotometric methods have been proposed for the determination of iron and cobalt individually and simultaneously. 2-hydroxy-1-naphthaldehyde-p-hydroxybenzoichydrazone (HNAHBH reacts with iron(II and cobalt(II to form reddish-brown and yellow-coloured [Fe(II-HNAHBH] and [Co(II-HNAHBH] complexes, respectively. The maximum absorbance of these complexes was found at 405 nm and 425 nm, respectively. For [Fe(II-HNAHBH], Beer’s law is obeyed over the concentration range of 0.055–1.373 μg mL−1 with a detection limit of 0.095 μg mL−1 and molar absorptivity ɛ, 5.6 × 104 L mol−1 cm−1. [Co(II-HNAHBH] complex obeys Beer’s law in 0.118–3.534 μg mL−1 range with a detection limit of 0.04 μg mL−1 and molar absorptivity, ɛ of 2.3 × 104 L mol−1 cm−1. Highly sensitive and selective first-, second- and third-order derivative methods are described for the determination of iron and cobalt. A simultaneous second-order derivative spectrophotometric method is proposed for the determination of these metals. All the proposed methods are successfully employed in the analysis of various biological, water, and alloy samples for the determination of iron and cobalt content.

Cacotheline as an oxidimetric reagent. Determination of Sn(II), Cu(I), Ti(III), Fe(II), V(II) and V(III)

International Nuclear Information System (INIS)

Nemani Murty, K.; Yedluri Rao, P.; Geddada Chalam, K.

1982-01-01

Sn(II), Ti(III), Cu(I),Fe(II), V(III) and V(II) can be titrated potentiometrically with cacotheline in 1-4 M hydrochloric acid, 0.5-2 M hydrochloric acid, 0.5-1.5 M sulphuric acid in presence of 4 ml of 10% EDTA solution in a total volume of 50 ml, 9-10 M phosphoric acid, 4-8 M acetic acid and 3-8 M acetic acid respectively. Cacotheline can be used for the assay of tin plate and solder. The cacotheline undergoes a 2-electron reduction reaction. A cacotheline solution (0.005 M) in 0.02 M hydrochloric acid is fairly stable for several months. The conditional redox potentials of cacotheline have been determined in sulphuric, phosphoric and acetic acid medium. (Author)

Synchronous determination of mercury (II) and copper (II) based on quantum dots-multilayer film

International Nuclear Information System (INIS)

Ma Qiang; Ha Enna; Yang Fengping; Su Xingguang

2011-01-01

Graphical abstract: We developed a sensitive sensor for synchronous detection of Hg (II) and Cu (II) based on the quenchedand recovered PL intensity of QDs-multilayer films. Solutions containing Hg (II) or Cu (II) were used to quench the fluorescence of the QDs-multilayer films firstly. Then, glutathione (GSH) was used to remove Hg (II) or Cu (II) from the QDs-multilayer films due to stronger affinity of GSH-metal ions than that of QDs metal ions. Thus, the fluorescence of QDs-multilayer films was recovered. Highlights: → QDs-multilayer films were developed for synchronous detection of Hg (II) and Cu (II). → Hg (II) and Cu (II) could quench the photoluminescence of the QDs-multilayer films. → Glutathione was used to remove metal ions and recovery photoluminescence of QDs-multilayer films. - Abstract: A sensitive sensor for mercury (II) and copper (II) synchronous detection was established via the changed photoluminescence of CdTe quantum dots (QDs) multilayer films in this work. QDs were deposited on the quartz slides to form QDs-multilayer films by electrostatic interactions with poly(dimethyldiallyl ammonium chloride) (PDDA). Hg 2+ or Cu 2+ could quench the photoluminescence of the QDs-multilayer films, and glutathione (GSH) was used to remove Hg 2+ or Cu 2+ from QDs-multilayer films due to strong affinity of GSH-metal ions, which resulted in the recovered photoluminescence of QDs-multilayer films. There are good linear relationships between the metal ions concentration and the photoluminescence intensity of QDs in the quenched and recovered process. It was found that the Stern-Volmer constants for Hg 2+ are higher than that for Cu 2+ . Based on different quenching and recovery constant between Hg 2+ and Cu 2+ , the synchronous detection of Hg 2+ and Cu 2+ can be achieved. The linear ranges of this assay were obtained from 0.005 to 0.5 μM for Hg 2+ and from 0.01 to 1 μM for Cu 2+ , respectively. And the artificial water samples were determined by this

Rapid-mix studies on the anomalous radiosensitization of mammalian cells by 5-chloro-1-methyl-4-nitroimidazole

International Nuclear Information System (INIS)

Watts, M.E.; Hodgkiss, R.J.; Sehmi, D.S.; Woodcock, M.

1980-01-01

It has been suggested that the anomalously high radiosensitization shown by 5-chloro-1-methyl-4-nitroimidazole (CMNI) arises from dissociation of the CMNI radical-anion, yielding Cl - and an arylating free radical, and that the importance of this dehalogenation process could be investigated by irradiating hypoxic mammalian cells in vitro in the presence of CMNI, followed by the rapid addition of oxygen to prevent the dehalogenation process. 0.1 mmol dm -3 CMNI gave a sensitizer enhancement ratio (SER) of 1.7 when irradiated under steady-state conditions with 250 kVp X-rays (dose rate 3.93 Gymin -1 ) using V79 379A cells. Irradiation with 2.5 MeV electrons in the rapid-mix apparatus with 0.15 mmol dm -3 CMNI flowing through both tubes gave a slightly lower value, SER=1.5, in hypoxia. When air- or oxygen saturated 0.15 mmol dm -3 CMNI in Eagle's MEM were added to cells irradiated in hypoxic 0.15 mmol dm -3 CMNI solution 17 ms after irradiation, no change in SER was observed. Control experiments without CMNI also confirmed that the addition of oxygen at this time has no influence on radiosensitization. It was concluded that since a significant reduction in SER was not observed, the elimination of the ortho-substituted 'leaving group' is not responsible for the anomalously high radiosensitization efficiency. (U.K.)

[Sensitivity of microbial associations of periodontal lesions to antibacterial agents].

Science.gov (United States)

Makeeva, I M; Daurova, F Yu; Byakova, S F; Ippolitov, E V; Gostev, M S; Polikushina, A O; Shubin, E V

2016-01-01

The aim of the study was the development of approaches to improve the effectiveness of antibiotic therapy in dental practice on the basis of determining the sensitivity of pathogenic microorganisms to antibiotics of different groups. The study included determination of the sensitivity of the microbial complexes from wound exudate of periodontal pocket and apical abscess to macrolides, quinolones, penicillins, lincosamides and 5-nitroimidazole. A survey of dentists and dental clinics patients to identify the cause and frequency of use of antibiotics and to identify possible adverse reactions was also conducted. Dentists prefer macrolide antibiotics, protected penicillins, and fluoroquinolone combined with 5-nitroimidazole. All patients have taken antibiotics themselves at least once a year. Microbial complexes in patients with acute and exacerbated apical periodontitis in 79% of cases are susceptible to amoxicillin/clavulanic acid, to azithromycin - 52%, lincomycin - 36%, 5-nitroimidazole - 68%, ciprofloxacin - 73.7%. In patients with apical abscess high rates of resistance of microbial complexes to all types of antibiotics was revealed (33% for lincomycin 76,1% for ciprofloxacin, 28,6% for 5-nitroimidazole). Patients with moderate to severe periodontitis in 90.5% are sensitive to amoxicillin/clavulanic acid and azithromycin, in 62.4% to lincomycin. Sensitivity to ciprofloxacin was detected in 85.7% of patients, in 14.3% - moderate resistance.

Artificial neural networks study of the catalytic reduction of resazurin: stopped-flow injection kinetic-spectrophotometric determination of Cu(II) and Ni(II)

International Nuclear Information System (INIS)

Magni, Diana M.; Olivieri, Alejandro C.; Bonivardi, Adrian L.

2005-01-01

An artificial neural network (ANN) procedure was used in the development of a catalytic spectrophotometric method for the determination of Cu(II) and Ni(II) employing a stopped-flow injection system. The method is based on the catalytic action of these ions on the reduction of resazurin by sulfide. ANNs trained by back-propagation of errors allowed us to model the systems in a concentration range of 0.5-6 and 1-15 mg l -1 for Cu(II) and Ni(II), respectively, with a low relative error of prediction (REP) for each cation: REP Cu(II) = 0.85% and REP Ni(II) = 0.79%. The standard deviations of the repeatability (s r ) and of the within-laboratory reproducibility (s w ) were measured using standard solutions of Cu(II) and Ni(II) equal to 2.75 and 3.5 mg l -1 , respectively: s r [Cu(II)] = 0.039 mg l -1 , s r [Ni(II)] = 0.044 mg l -1 , s w [Ni(II)] = 0.045 mg l -1 and s w [Ni(II)] = 0.050 mg l -1 . The ANNs-kinetic method has been applied to the determination of Cu(II) and Ni(II) in electroplating solutions and provided satisfactory results as compared with flame atomic absorption spectrophotometry method. The effect of resazurin, NaOH and Na 2 S concentrations and the reaction temperature on the analytical sensitivity is discussed

Simultaneous determination of Cd(II) and Pb(II) by differential pulse anodic stripping voltammetry based on graphite nanofibers-Nafion composite modified bismuth film electrode.

Science.gov (United States)

Li, Dongyue; Jia, Jianbo; Wang, Jianguo

2010-12-15

A bismuth-film modified graphite nanofibers-Nafion glassy carbon electrode (BiF/GNFs-NA/GCE) was constructed for the simultaneous determination of trace Cd(II) and Pb(II). The electrochemical properties and applications of the modified electrode were studied. Operational parameters such as deposition potential, deposition time, and bismuth ion concentration were optimized for the purpose of determination of trace metal ions in 0.10 M acetate buffer solution (pH 4.5). Under optimal conditions, based on three times the standard deviation of the baseline, the limits of detection were 0.09 μg L(-1) for Cd(II) and 0.02 μg L(-1) for Pb(II) with a 10 min preconcentration. In addition, the BiF/GNFs-NA/GCE displayed good reproducibility and selectivity, making it suitable for the simultaneous determination of Cd(II) and Pb(II) in real sample such as river water and human blood samples. Copyright © 2010 Elsevier B.V. All rights reserved.

Determining the Amount of Copper(II) Ions in a Solution Using a Smartphone

Science.gov (United States)

Montangero, Marc

2015-01-01

When dissolving copper in nitric acid, copper(II) ions produce a blue-colored solution. It is possible to determine the concentration of copper(II) ions, focusing on the hue of the color, using a smartphone camera. A free app can be used to measure the hue of the solution, and with the help of standard copper(II) solutions, one can graph a…

Determination of static and dynamic reactivity effects in KNK II

International Nuclear Information System (INIS)

Essig, C.

1987-11-01

In the frame of a pre-study of the KNK II test program two series of experiments related to inherent safety characteristics of sodium cooled breeder reactors have been elaborated, which are one basis for the performance of experiments of the Loss Of Flow (LOF) type and the Loss Of Heat Sink (LOHS) type. Tests of this type at KNK II would -different from the earlier tests at RAPSODIE and EBR-II- provide a demonstration of the inherently safe performance in case of a significantly non-zero Doppler effect. With a suitable execution, the foreseen series of experiments allow, as explained in this report, a substantial separation of the reactivity contributions and the determination of reactivity effects, i.e. the time constants of the recouplings. The performance and evaluation of these experiments with respect to the inherent safety potential will once more underline the distinguished role of KNK II for the development of fast breeders [de

Synthesis and preclinical characterization of 1-(6'-deoxy-6'-[18F]fluoro-β-d-allofuranosyl)-2-nitroimidazole (β-6'-[18F]FAZAL) as a positron emission tomography radiotracer to assess tumor hypoxia.

Science.gov (United States)

Wanek, Thomas; Kreis, Katharina; Križková, Petra; Schweifer, Anna; Denk, Christoph; Stanek, Johann; Mairinger, Severin; Filip, Thomas; Sauberer, Michael; Edelhofer, Patricia; Traxl, Alexander; Muchitsch, Viktoria E; Mereiter, Kurt; Hammerschmidt, Friedrich; Cass, Carol E; Damaraju, Vijaya L; Langer, Oliver; Kuntner, Claudia

2016-11-01

Positron emission tomography (PET) using fluorine-18 ( 18 F)-labeled 2-nitroimidazole radiotracers has proven useful for assessment of tumor oxygenation. However, the passive diffusion-driven cellular uptake of currently available radiotracers results in slow kinetics and low tumor-to-background ratios. With the aim to develop a compound that is actively transported into cells, 1-(6'-deoxy-6'-[ 18 F]fluoro-β-d-allofuranosyl)-2-nitroimidazole (β-[ 18 F]1), a putative nucleoside transporter substrate, was synthetized by nucleophilic [ 18 F]fluoride substitution of an acetyl protected labeling precursor with a tosylate leaving group (β-6) in a final radiochemical yield of 12±8% (n=10, based on [ 18 F]fluoride starting activity) in a total synthesis time of 60min with a specific activity at end of synthesis of 218±58GBq/μmol (n=10). Both radiolabeling precursor β-6 and unlabeled reference compound β-1 were prepared in multistep syntheses starting from 1,2:5,6-di-O-isopropylidene-α-d-allofuranose. In vitro experiments demonstrated an interaction of β-1 with SLC29A1 and SLC28A1/2/3 nucleoside transporter as well as hypoxia specific retention of β-[ 18 F]1 in tumor cell lines. In biodistribution studies in healthy mice β-[ 18 F]1 showed homogenous tissue distribution and excellent metabolic stability, which was unaffected by tissue oxygenation. PET studies in tumor bearing mice showed tumor-to-muscle ratios of 2.13±0.22 (n=4) at 2h after administration of β-[ 18 F]1. In ex vivo autoradiography experiments β-[ 18 F]1 distribution closely matched staining with the hypoxia marker pimonidazole. In conclusion, β-[ 18 F]1 shows potential as PET hypoxia radiotracer which merits further investigation. Copyright © 2016 Elsevier Ltd. All rights reserved.

Determination of cobalt(II) and nickel(II) with isoamylxanthate as a complexing reagent in micellar media

International Nuclear Information System (INIS)

Shar, G.A.; Soomro, G.A.

2008-01-01

Cobalt(II) and nickel(II) were determined spectrophotometrically using sodium isoamyl xanthate as a complexing reagent in aqueous phase in the presence of anionic surfactant sodium dodecylsulphate (SDS). Beer's law was obeyed for Co(ll) and Ni(ll) over the concentration range 3.0-35 and 2.0-37 micro gmL/sup -1/ respectively. The lambda/sub max/ molar absorptivity and Sandell's sensitivity of Co(ll) and Ni(ll) were 360 nm and 416 nm; is 0.19 and 0.2 (x 10/sup 4/ mol/sup -1/ cm/sup -1/) 31.1 and 29.3 ng cm/sup -2/ respectively. Maximum absorbance at 1:2 (M: L) molar ratio suggested the formation of M(C/sub 6/H/sub 11/ OS/sub 2/)/sub 2/ where M = Co(II) and Ni(II). The complex remained stable for more than 2 h. The optimized reagent concentration 0.5% was used throughout the study. Surfactant concentration of 1.0% SDS caused significant enhancement in absorbance. Maximum absorption was observed at 360 nm and 416 nm for Co and Ni complexes, respectively. The absorption maxima were obtained at optimized pH of 7.0. Validation of method has been made by comparing the results with Atomic Absorption Spectrometry, no significant difference was obtained between the two methods at 95% confidence interval. The method is simple, accurate, economical and has been applied to the determination of cobalt(ll) and nickel(ll) in industrial wastewater, pharmaceutical and edible oil samples. (author)

Fluorimetric determination of copper(II) in aqueous solution using lucifer yellow CH as selective metal reagent

Energy Technology Data Exchange (ETDEWEB)

Mayr, T.; Wencel, D.; Werner, T. [Univ. of Regensburg (Germany) Inst. of Analytical Chemistry, Chemo- and Biosensors

2001-09-01

Lucifer yellow CH is shown to be a highly selective fluorescent reagent for the determination of Cu(II) in the {mu}g L{sup -1} concentration range. The fluorophore is statically quenched by Cu(II); the carbohydrazide group was assigned as the complexing part of the dye molecule. A total range of Cu(II) determination from 0.06 mg L{sup -1} (1 {mu}mol L{sup -1}) to 6.3 mg L{sup -1} (100 {mu}mol L{sup -1}) with a limit of detection of 0.019 mg L{sup -1} (0.3 {mu}mol L{sup -1}) was obtained, along with surprisingly high selectivity. There was no interference from alkaline and earth alkaline metal ions. The cross sensitivity to heavy metal ions was evaluated by the separate solution method and by competitive binding experiments. Calibration plots are shown for Cu(II) determination at different pH and the dissociation constant was determined. The application of the reagent was demonstrated by the determination of the Cu(II) content of tap water samples. (orig.)

Potentiometric determination of the tungsten content of tantalum-tungsten alloys with chromium II

International Nuclear Information System (INIS)

Gavra, Z.; Ronen, S.; Levin, R.

1977-05-01

A method was developed for the potentiometric determination of the tungsten content of tantalum-tungsten alloys of different compositions. These were dissolved under conditions that enabled the tungsten content to be determined with chromium (II). Phosphoric acid was selected as a suitable complexing agent for the prevention of the precipitation of tungsten and tantalum compounds. The use of chromium (II) required an oxygen-tight system and therefore the work was carried out in suitable vessels for storage and tritation

Determination of tin(II) in reagents for radiopharmaceuticals

International Nuclear Information System (INIS)

Morosanova, E.I.; Loginova, K. A.; Epstein, N.B.

2003-01-01

The goal of this work is to elaborate a procedure for rapid and simple determination of tin(II) in reagents for preparation of radiopharmaceuticals based on a system albumin-Tc-99m. Original test tools for the determination of various analytes have been suggested in our lab based on the use of small glass tubes (1-2 mm i.d. - 50-70 mm) filled with indicator powders containing suitable immobilized chromogenic reagents. An analytical signal (a length of colored zone which is proportional to the concentration of an analyte) is detected after a sample passing through the indicator tube. Heteropoly compounds are well-known analytical reagents for a photometric determination of various reductants. For elaboration of indicator tubes abilities of Mo,P-heteropoly compounds to give deeply colored blue compounds after reduction were used. (authors)

Simultaneous determination of Hg(II)-Ag(I)-Cd(II) by conductometric titration using the formation of ternary complex

International Nuclear Information System (INIS)

Hayashida, Ichiro; Yoshida, Hitoshi; Taga, Mitsuhiko; Hikime, Seiichiro

1979-01-01

A conductometric determination of Hg(II), Ag(I) and Cd(II) was carried out by using the insoluble ternary complex formation of the metal ions with iodide ion in the presence of 1,10-phenanthroline (phen). Recommended procedure is as follows; An aliquot of sample solution containing (14 -- 29) mg of Hg(II), (8 -- 16) mg of Ag(I), and (9 -- 17) mg of Cd(II) transfered into a 100 ml beaker. Add to acetate buffer and stoichiometric amounts of phen (40% ethanol-water solution). Amounts of nitrate ion which was estimated separately by other titration with 0.1 M Ag(phen) 2 complex (40% ethanol-water solution) are adjusted in the range of (4.0 -- 6.0) mM. The sample solution is titrated with 0.1 M KI standard solution at the rate of 0.20 ml/min or less. The titration curve showed three end-points corresponding to the formation of (1) Hg(phen) 2 I 2 , (2) Ag(phen)I, and (3) Cd(phen) 2 I 2 . The relative standard deviation was less than 0.8%, when the pH value was controlled at 4.0 -- 4.5 (acetate buffer) and the nitrate concentration was adjusted in the range of (4.0 -- 6.0)mM. The effect of diverse ions on the determination was also investigated in detail. (author)

Determination of subnanomolar levels of mercury (II) by using a graphite paste electrode modified with MWCNTs and Hg(II)-imprinted polymer nanoparticles.

Science.gov (United States)

Alizadeh, Taher; Hamidi, Negin; Ganjali, Mohamad Reza; Rafiei, Faride

2017-12-05

Mercury ion-imprinted polymer nanoparticles (Hg-IP-NPs) were synthesized via precipitation polymerization by using itaconic acid as a functional monomer. A carbon paste electrode was impregnated with the synthesized Hg-IP-NPs and MWCNTs to obtain a highly sensitive and selective electrode for determination of Hg(II). Mercury ion is first accumulated on the electrode surface via an open circuit procedure. After reduction of Hg(II) ions to its metallic form at a negative pre-potential, square wave anodic stripping voltammetry was applied to generate the electrochemical signal. The high affinity of the Hg-IP-NPs for Hg(II) was substantiated by comparing of the signals of electrodes with imprinted and non-imprinted polymer. The beneficial effect of MWCNTs on the voltammetric signal is also demonstrated. Under the optimized conditions and at a typical working potential of +0.05 V (vs. Ag/AgCl), the electrode has a linear response in the 0.1-20 nmol L -1 Hg(II) concentration range and a 29 pM detection limit. The electrochemical sensitivity is as high as 1441 A·M -1 ·cm -2 which is among the best values known. The electrode was applied to the determination of Hg(II) in water samples. Graphical abstract Schematic representation of the sensor electrode modified with mercury-imprinted polymer nanoparticles, and the recognition and voltammetric determination steps.

SDSS-II: Determination of shape and color parameter coefficients for SALT-II fit model

Energy Technology Data Exchange (ETDEWEB)

Dojcsak, L.; Marriner, J.; /Fermilab

2010-08-01

In this study we look at the SALT-II model of Type IA supernova analysis, which determines the distance moduli based on the known absolute standard candle magnitude of the Type IA supernovae. We take a look at the determination of the shape and color parameter coefficients, {alpha} and {beta} respectively, in the SALT-II model with the intrinsic error that is determined from the data. Using the SNANA software package provided for the analysis of Type IA supernovae, we use a standard Monte Carlo simulation to generate data with known parameters to use as a tool for analyzing the trends in the model based on certain assumptions about the intrinsic error. In order to find the best standard candle model, we try to minimize the residuals on the Hubble diagram by calculating the correct shape and color parameter coefficients. We can estimate the magnitude of the intrinsic errors required to obtain results with {chi}{sup 2}/degree of freedom = 1. We can use the simulation to estimate the amount of color smearing as indicated by the data for our model. We find that the color smearing model works as a general estimate of the color smearing, and that we are able to use the RMS distribution in the variables as one method of estimating the correct intrinsic errors needed by the data to obtain the correct results for {alpha} and {beta}. We then apply the resultant intrinsic error matrix to the real data and show our results.

Solid phase extraction of Cd(II) and Pb(II) using a magnetic metal-organic framework, and their determination by FAAS

International Nuclear Information System (INIS)

Sohrabi, Mahmoud Reza; Matbouie, Zahra; Asgharinezhad, Ali Akbar; Dehghani, Ali

2013-01-01

We describe a novel magnetic metal-organic framework (MOF) for the preconcentration of Cd(II) and Pb(II) ions. The MOF was prepared from the Fe 3 O 4 -pyridine conjugate and the copper(II) complex of trimesic acid. The MOF was characterized by IR spectroscopy, elemental analysis, SEM and XRD. A Box-Behnken design through response surface methodology and experimental design was used to identify the optimal parameters for preconcentration. Extraction time, amount of magnetic MOF and pH value were found to be critical factors for uptake, while type, volume, concentration of eluent, and elution time are critical in the elution step. The ions were then determined by FAAS. The limits of detection are 0.2 and 1.1 μg L −1 for Cd(II), and Pb(II) ions, respectively, relative standard deviations are −1 of Cd(II) and Pb(II) ions), and the enrichment capacity of the MOF is at around 190 mg g −1 for both ions which is higher than the conventional Fe 3 O 4 -pyridine material. The magnetic MOF was successfully applied to the rapid extraction of trace quantities of Cd(II) and Pb(II) ions in fish, sediment, and water samples. (author)

Indirect complexometric determination of mercury(II) using potassium bromide as selective masking agent

International Nuclear Information System (INIS)

Sreekumar, N.V.; Nazareth, R.A.; Narayana, B.; Hegde, P.; Manjunatha, B.R.

2002-01-01

A complexometric method for the determination of mercury in presence of other metal ions based on the selective masking ability of potassium bromide towards mercury is described. Mercury(II) present in a given sample solution is first complexed with a known excess of EDTA and the surplus EDTA is titrated against zinc sulfate solution at pH 5-6 using xylenol orange as the indicator. A known excess of 10 % solution of potassium bromide is then added and the EDTA released from Hg-EDTA complex is titrated against standard zinc sulfate solution. Reproducible and accurate results are obtained for 8 mg to 250 mg of mercury(II) with a relative error ±0.28 % and standard deviations /leg 0.5 mg. The interference of various ions is studied. This method was applied to the determination of mercury(II) in its alloys. (author)

Voltammetric determination of Zn(II in Zn-Fe alloy electroplating baths using square-wave voltammetry

Directory of Open Access Journals (Sweden)

Favaron Regiane

2001-01-01

Full Text Available A routine analytical method for zinc (II determination in Zn-Fe alloy galvanic baths was developed employing square-wave voltammetry with the static mercury drop electrode (SMDE as working electrode. Real alloy bath samples were analyzed by the standard addition method and recovery tests were undertaken. The supporting electrolytes used in the analyses were 1.0 mol L-1 NH3 / 0.2 mol L-1 NH4Cl or 0.1 mol L-1 citric acid (pH=3, presenting peak potentials for zinc (II, respectively, at -1.30 V and -0.99 V vs. Ag|AgCl (saturated KCl. The proposed voltammetric method showed a linear response range at 25 °C between 1.0 x 10-5 and 2.2 x 10-4 mol L-1 for zinc (II, in both electrolytes studied. The interference levels for some metals, such as Cu (II, Pb (II, Cr (III and Mn (II, which could prejudice Zn-Fe alloy deposition, were evaluated. These ions did not present significant degrees of interference in the zinc (II determination. The zinc (II recovery tests for the proposed method exhibited a good agreement with the reference method, showing relative errors lower than 3.0%.

Synthesis and application of surface-imprinted activated carbon sorbent for solid-phase extraction and determination of copper (II)

Science.gov (United States)

Li, Zhenhua; Li, Jingwen; Wang, Yanbin; Wei, Yajun

2014-01-01

A new Cu(II)-imprinted amino-functionalized activated carbon sorbent was prepared by a surface imprinting technique for selective solid-phase extraction (SPE) of Cu(II) prior to its determination by inductively coupled plasma atomic emission spectrometry (ICP-AES). Experimental conditions for effective adsorption of Cu(II) were optimized with respect to different experimental parameters using static and dynamic procedures in detail. Compared with non-imprinted sorbent, the ion-imprinted sorbent had higher selectivity and adsorption capacity for Cu(II). The maximum static adsorption capacity of the ion-imprinted and non-imprinted sorbent for Cu(II) was 26.71 and 6.86 mg g-1, respectively. The relatively selectivity factor values (αr) of Cu(II)/Zn(II), Cu(II)/Ni(II), Cu(II)/Co(II) and Cu(II)/Pb(II) were 166.16, 50.77, 72.26 and 175.77, respectively, which were greater than 1. Complete elution of the adsorbed Cu(II) from Cu(II)-imprinted sorbent was carried out using 2 mL of 0.1 mol L-1 EDTA solution. The relative standard deviation of the method was 2.4% for eleven replicate determinations. The method was validated for the analysis by two certified reference materials (GBW 08301, GBW 08303), the results obtained is in good agreement with standard values. The developed method was also successfully applied to the determination of trace copper in natural water samples with satisfactory results.

Complexo-potentiometric determination of mercury (II) in chlormerodrin and mercuric chloride labelled with radioactive mercury

International Nuclear Information System (INIS)

Duek, E.E.

1976-09-01

A method is described for determining the amount of mercury (II) in radioactively labelled chlormerodrin and mercuric chloride. By measuring the absolute activity in an ionization chamber, the specific activity is therefore immediately obtained. The determination of Hg (II) is based on a complexometric titration. Because of method characteristics and speed convenience, the end point is observed by means of a pH-meter. A comparison is made with a determination performed by detecting the end point with color-change indicators. The error is estimated, and the results are statistically interpreted. (author) [es

Determination of Ni(II) crystal structure by powder x-ray diffraction ...

African Journals Online (AJOL)

X-ray powder diffraction pattern was used to determine the length of the unit cell, “a”, the lattice structure type, and the number of atoms per unit cell of Ni(II) crystal. The “a” value was determined to be 23.66 ± 0.005 Å, particle size of 34.87 nm, volume 13.24 Å and Strain value ε = 9.8 x 10-3. The cell search on PXRD patterns ...

3-Mercaptopropyltrimethoxysilane Modified Diatomite: Preparation and Application for Voltammetric Determination of Lead (II and Cadmium (II

Directory of Open Access Journals (Sweden)

Dinh Quang Khieu

2017-01-01

Full Text Available In this study, functionalized diatomite was prepared by grafting of 3-mercaptopropyltrimethoxysilane (MPTMS to diatomite (MPTMS-diatomite. The diatomite with thermal treatment from 100 to 700°C was functionalized by MPTMS under dry and humid conditions. The obtained MPTMS-diatomite was characterized by X-ray diffraction (XRD, thermal gravity-differential scanning calorimeter (TG-DSC, and Fourier transformation infrared (FT-IR. The results showed that an increase in treatment temperature seems to reduce the loading of MPTMS onto diatomite. The humidity of diatomite was favorable for the grafting of functional groups on the surface. The possible mechanisms of MPTMS loading to diatomite (MPTMS-diatomite were also proposed. The performance of a carbon paste electrode (CPE modified with MPTMS-diatomite in the simultaneous determination of Cd(II and Pb(II ions was addressed.

Application of Carrier Element-Free Co-precipitation Method for Ni(II), Cu(II) and Zn(II) Ions Determination in Water Samples Using Chrysin

International Nuclear Information System (INIS)

Layth Imad Abd Ali; Wan Aini Wan Ibrahim; Azli Sulaiman; Mohd Marsin Sanagi

2015-01-01

A co-precipitation method was developed to separate and pre-concentrate Ni(II), Cu(II) and Zn(II) ions using an organic co precipitant, chrysin without adding any carrier element termed as carrier element-free co-precipitation (CEFC). Analytes were determined using flame atomic absorption spectrometry (FAAS). The influence of analytical conditions, such as pH of the solution, quantity of co-precipitant, standing time, centrifugation rate and time, sample volume, and interference of concomitant ions were investigated over the recovery yields of the trace metals. The limit of detection, the limit of quantification and linearity range obtained from the FAAS measurements were found to be in the range of 0.64 to 0.86 μg L -1 , 2.13 to 2.86 μg L -1 and 0.9972 to 0.9989 for Ni(II), Cu(III) and Zn(II) ions, respectively. The precision of the method, evaluated as the relative standard deviation (RSD) obtained after analyzing a series of 10 replicates, was between 2.6 % to 3.9 % for the trace metal ions. The proposed procedure was applied and validated by analyzing river water reference material for trace metals (SLRS-5) and spiking trace metal ions in some water samples. The recoveries of the analyte metal ions were between 94.7-101.2 %. (author)

A cephalometric analysis of Class II dentate subjects to establish a formula to determine the occlusal plane in Class II edentate subjects: A neo adjunct

OpenAIRE

Nikita Sinha; K Mahendranadh Reddy; Nidhi Gupta; Y M Shastry

2017-01-01

Purpose: Occlusal plane (OP) differs considerably in participants with skeletal Class I and Class II participants. In this study, cephalometrics has been used to help in the determination of orientation of the OP utilizing the nonresorbable bony anatomic landmarks in skeletal Class II participants and an attempt has been made to predict and examine the OP in individuals with skeletal class II jaw relationship. Materials and Methods: One hundred dentulous participants with skeletal Class II...

Determination of Mercury (II Ion on Aryl Amide-Type Podand-Modified Glassy Carbon Electrode

Directory of Open Access Journals (Sweden)

Sevgi Güney

2011-01-01

Full Text Available A new voltammetric sensor based on an aryl amide type podand, 1,8-bis(o-amidophenoxy-3,6-dioxaoctane, (AAP modified glassy carbon electrode, was described for the determination of trace level of mercury (II ion by cyclic voltammetry (CV and differential pulse voltammetry (DPV. A well-defined anodic peak corresponding to the oxidation of mercury on proposed electrode was obtained at 0.2 V versus Ag/AgCl reference electrode. The effect of experimental parameters on differential voltammetric peak currents was investigated in acetate buffer solution of pH 7.0 containing 1 × 10−1 mol L−1 NaCl. Mercury (II ion was preconcentrated at the modified electrode by forming complex with AAP under proper conditions and then reduced on the surface of the electrode. Interferences of Cu2+, Pb2+, Fe3+, Cd2+, and Zn2+ ions were also studied at two different concentration ratios with respect to mercury (II ions. The modified electrode was applied to the determination of mercury (II ions in seawater sample.

Extractive Spectrophotometric Determination of Nortriptyline Hydrochloride Using Sudan II, IV and Black B.

Science.gov (United States)

Amin, A S; Saleh, H M

2017-08-17

A simple spectrophotometric methods has been developed for the determination of nortriptyline hydrochloride in pure and in pharmaceuticalformulations based on the formation of ion-pair complexes with sudun II (S II ), sudan (IV) (S IV ) and sudan black B (S BB ). The selectivity of the method was improved through extraction with chloroform. The optimum conditions for complete extracted colour development were assessed. The absorbance measurements were made at 534, 596 and 649 nm for S II , S IV and S BB complexes, respectively. The calibration graph was linear in the ranges 0.5- 280. 0.5- 37.5 and 0.5 - 31.0 μg ml -1 of the drug usiny the same reagents, respectively. The precision of the procedure was checked by calculating the relative standard deviation of ten replicate determinations on 15 μg ml -1 of nortriptyline HCI and was found to be 1.7, 1.3 and 1.55% using S II , S IV , and S BB complexes, respectively. The molar absorptivity and Sandell sensitivity for each ion-pair were calculated. The proposed methods were successfully applied to the deterniination of pure nortriptyline HCI and in pharmaceutical formulations, and the results demonstrated that the method is equally accurate, precise and reproducible as the official method.

Amalgam Electrode-Based Electrochemical Detector for On-Site Direct Determination of Cadmium(II and Lead(II from Soils

Directory of Open Access Journals (Sweden)

Lukas Nejdl

2017-08-01

Full Text Available Toxic metal contamination of the environment is a global issue. In this paper, we present a low-cost and rapid production of amalgam electrodes used for determination of Cd(II and Pb(II in environmental samples (soils and wastewaters by on-site analysis using difference pulse voltammetry. Changes in the electrochemical signals were recorded with a miniaturized potentiostat (width: 80 mm, depth: 54 mm, height: 23 mm and a portable computer. The limit of detection (LOD was calculated for the geometric surface of the working electrode 15 mm2 that can be varied as required for analysis. The LODs were 80 ng·mL−1 for Cd(II and 50 ng·mL−1 for Pb(II, relative standard deviation, RSD ≤ 8% (n = 3. The area of interest (Dolni Rozinka, Czech Republic was selected because there is a deposit of uranium ore and extreme anthropogenic activity. Environmental samples were taken directly on-site and immediately analysed. Duration of a single analysis was approximately two minutes. The average concentrations of Cd(II and Pb(II in this area were below the global average. The obtained values were verified (correlated by standard electrochemical methods based on hanging drop electrodes and were in good agreement. The advantages of this method are its cost and time effectivity (approximately two minutes per one sample with direct analysis of turbid samples (soil leach in a 2 M HNO3 environment. This type of sample cannot be analyzed using the classical analytical methods without pretreatment.

Preconcentration of Sn (II) using the methylene blue on the activated carbon and its determination by spectrophotometry method.

Science.gov (United States)

Khodadoust, Saeid; Cham Kouri, Narges

2014-04-05

A simple and accurate spectrophotometric method for determination of trace amounts of Sn (II) ion in soil sample was developed by using the methylene blue (MB) in the presence of activated carbon (AC) as the adsorbent Solid Phase Extraction (SPE) of Sn (II) and then determined by UV-Vis. The Beer's law is obeyed over the concentration range of 1-80ngmL(-1) of Sn (II) with the detection limits of 0.34ngmL(-1). The influence of type and volume of eluent, concentration of MB, pH, and amount of AC on sensitivity of spectrophotometric method were optimized. The method has been successfully applied for Sn (II) ion determination in soil sample. Copyright © 2013 Elsevier B.V. All rights reserved.

Electrochemically modified sulfisoxazole nanofilm on glassy carbon for determination of cadmium(II) in water samples

International Nuclear Information System (INIS)

Gupta, Vinod Kumar; Yola, Mehmet Lütfi; Atar, Necip; Solak, Ali Osman; Uzun, Lokman; Üstündağ, Zafer

2013-01-01

Highlights: • Sulfisoxazole was grafted onto glassy carbon electrode. • The electrode was characterized by spectroscopic and electrochemical methods. • It has been used for the determination of Cd(II) ions in real samples in very low concentrations. -- Abstract: Sulfisoxazole (SO) was grafted to glassy carbon electrode (GCE) via the electrochemical oxidation of SO in acetonitrile solution containing 0.1 M tetrabutylammoniumtetra-fluoroborate (TBATFB). The prepared electrode was characterized by using cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), reflection–absorption infrared spectroscopy (RAIRS) and X-ray photoelectron spectroscopy (XPS). The ellipsometric thickness of SO nanofilm at the glassy carbon surface was obtained as 14.48 ± 0.11 nm. The stability of the SO modified GCE was studied. The SO modified GCE was also utilized for the determination of Cd(II) ions in water samples in the presence of Pb(II) and Fe(II) by adsorptive stripping voltammetry. The linearity range and the detection limit of Cd(II) ions were 1.0 × 10 −10 to 5.0 × 10 −8 M and 3.3 × 10 −11 M (S/N = 3), respectively

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

International Nuclear Information System (INIS)

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

2009-01-01

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

Novel and validated titrimetric method for determination of selected angiotensin-II-receptor antagonists in pharmaceutical preparations and its comparison with UV spectrophotometric determination

Directory of Open Access Journals (Sweden)

Shrikant H. Patil

2012-12-01

Full Text Available A novel and simple titrimetric method for determination of commonly used angiotensin-II-receptor antagonists (ARA-IIs is developed and validated. The direct acid base titration of four ARA-IIs, namely eprosartan mesylate, irbesartan, telmisartan and valsartan, was carried out in the mixture of ethanol:water (1:1 as solvent using standardized sodium hydroxide aqueous solution as titrant, either visually using phenolphthalein as an indicator or potentiometrically using combined pH electrode. The method was found to be accurate and precise, having relative standard deviation of less than 2% for all ARA-IIs studied. Also, it was shown that the method could be successfully applied to the assay of commercial pharmaceuticals containing the above-mentioned ARA-IIs. The validity of the method was tested by the recovery studies of standard addition to pharmaceuticals and the results were found to be satisfactory. Results obtained by this method were found to be in good agreement with those obtained by UV spectrophotometric method. For UV spectrophotometric analysis ethanol was used as a solvent and wavelength of 233 nm, 246 nm, 296 nm, and 250 nm was selected for determination of eprosartan mesylate, irbesartan, telmisartan, and valsartan respectively. The proposed titrimetric method is simple, rapid, convenient and sufficiently precise for quality control purposes. Keywords: Angiotensin-II-receptor antagonists, Titrimetric assay, UV spectrophotometry, Validation

Sol-gel based optical sensor for determination of Fe (II): a novel probe for iron speciation.

Science.gov (United States)

Samadi-Maybodi, Abdolraouf; Rezaei, Vida; Rastegarzadeh, Saadat

2015-02-05

A highly selective optical sensor for Fe (II) ions was developed based on entrapment of a sensitive reagent, 2,4,6-tri(2-pyridyl)-s-triazine (TPTZ), in a silica sol-gel thin film coated on a glass substrate. The thin films fabricated based on tetraethoxysilane (TEOS) as precursor, sol-gel pH∼3, water:alkoxyde ratio of 4:1 and TPTZ concentration of 0.112 mol L(-1). The influence of sol-gel parameters on sensing behavior of the fabricated sensor was also investigated. The fabricated sensor can be used for determination of Fe (II) ion with an outstanding high selectivity over a dynamic range of 5-115 ng mL(-1) and a detection limit of 1.68 ng mL(-1). It also showed reproducible results with relative standard deviation of 3.5% and 1.27% for 10 and 90 ng mL(-1) of Fe (II), respectively, along with a fast response time of ∼120 s. Total iron also was determined after reduction of Fe (III) to Fe (II) using ascorbic acid as reducing agent. Then, the concentration of Fe (III) was calculated by subtracting the concentration of Fe (II) from the total iron concentration. Interference studies showed a good selectivity for Fe (II) with trapping TPTZ into sol-gel matrix and appropriately adjusting the structure of doped sol-gel. The sensor was compared with other sensors and was applied to determine iron in different water samples with good results. Copyright © 2014 Elsevier B.V. All rights reserved.

Dead layer and active volume determination for GERDA Phase II detectors

Energy Technology Data Exchange (ETDEWEB)

Lehnert, Bjoern [TU Dresden (Germany); Collaboration: GERDA-Collaboration

2013-07-01

The GERDA experiment investigates the neutrinoless double beta decay of {sup 76}Ge and is currently running Phase I of its physics program. Using the same isotope as the Heidelberg Moscow (HDM) experiment, GERDA aims to directly test the claim of observation by a subset of the HDM collaboration. For the update to Phase II of the experiment in 2013, the collaboration organized the production of 30 new Broad Energy Germanium (BEGe) type detectors from original 35 kg enriched material and tested their performance in the low background laboratory HADES in SCK.CEN, Belgium. With additional 20 kg of detectors, GERDA aims to probe the degenerated hierarchy scenario. One of the crucial detector parameters is the active volume (AV) fraction which directly enters into all physics analysis. This talk presents the methodology of dead layer and AV determination with different calibration sources such as {sup 241}Am, {sup 133}Ba, {sup 60}Co and {sup 228}Th and the results obtained for the new Phase II detectors. Furthermore, the AV fraction turned out to be the largest systematic uncertainty in the analysis of Phase I data which makes it imperative to reduce its uncertainty for Phase II. This talk addresses the major contributions to the AV uncertainty and gives an outlook for improvements in Phase II analysis.

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

Energy Technology Data Exchange (ETDEWEB)

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

2009-09-15

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

Radiosensitizing and cytotoxic properties of DNA targeted phenanthridine-linked nitroheterocycles of varying electron affinities

International Nuclear Information System (INIS)

Cowan, D.S.M.; Rauth, A.M.; Toronto Univ., ON; Matejovic, J.F.; McClelland, R.A.; Wardman, P.

1994-01-01

2-Nitroimidazoles targeted to DNA via intercalation have previously been shown to be as much as 10-100 times more efficient on a molar basis than the untargeted nitroimidazole, misonidazole, in vitro as hypoxic cell selective radiosensitizers and cytotoxins based on extracellular concentrations. In this work the effect of varying the nitroaromatic group has been examined through the preparation of a DNA-targeted 4-nitroimidazole (4-MeNLP-3), a 5-nitroimidazole (5-NLP-3) and a 5-nitrofuran (FEP-2) linked to phenanthridinium ions. With the previously synthesized 2-nitroimidazoles, this provides a series of DNA targeted compounds of varying electron affinity as well as structure at the nitroaromatic position. The present series of compounds was tested for partition coefficient, DNA binding ability, reduction potentials and in vitro radiosensitizing and cytotoxic abilities. The results obtained indicate that targeting such compounds to DNA diminishes the dependency of radiosensitizing and cytotoxic properties on reduction potential and may allow significant uncoupling of toxicity from radiosensitizing ability. (author)

HTLV-I/II and blood donors: determinants associated with seropositivity in a low risk population

Directory of Open Access Journals (Sweden)

Bernadette Catalan Soares

2003-08-01

Full Text Available OBJECTIVE: Blood donors in Brazil have been routinely screened for HTLV-I/II since 1993. A study was performed to estimate the prevalence of HTLV-I/II infection in a low risk population and to better understand determinants associated with seropositivity. METHODS: HTLV-I/II seropositive (n=135, indeterminate (n=167 and seronegative blood donors (n=116 were enrolled in an open prevalence prospective cohort study. A cross-sectional epidemiological study of positive, indeterminate and seronegative HTLV-I/II subjects was conducted to assess behavioral and environmental risk factors for seropositivity. HTLV-I/II serological status was confirmed using enzyme-linked immunosorbent assay (EIA and Western blot (WB. RESULTS: The three groups were not homogeneous. HTLV-I/II seropositivity was associated to past blood transfusion and years of schooling, a marker of socioeconomic status, and use of non-intravenous illegal drugs. CONCLUSIONS: The study results reinforce the importance of continuous monitoring and improvement of blood donor selection process.

Simultaneous trace-levels determination of Hg(II) and Pb(II) ions in various samples using a modified carbon paste electrode based on multi-walled carbon nanotubes and a new synthesized Schiff base

International Nuclear Information System (INIS)

Afkhami, Abbas; Bagheri, Hasan; Khoshsafar, Hosein; Saber-Tehrani, Mohammad; Tabatabaee, Masoumeh; Shirzadmehr, Ali

2012-01-01

Highlights: ► A new chemically modified carbon paste electrode was constructed and used. ► A new Schiff base and multi-walled carbon nanotube was used as a modifier. ► The electrochemical properties of the modified electrode were studied. ► The electrode was used to the simultaneous determination of Pb 2+ and Hg 2+ . - Abstract: A modified carbon paste electrode based on multi-walled carbon nanotubes (MWCNTs) and 3-(4-methoxybenzylideneamino)-2-thioxothiazolodin-4-one as a new synthesized Schiff base was constructed for the simultaneous determination of trace amounts of Hg(II) and Pb(II) by square wave anodic stripping voltammetry. The modified electrode showed an excellent selectivity and stability for Hg(II) and Pb(II) determinations and for accelerated electron transfer between the electrode and the analytes. The electrochemical properties and applications of the modified electrode were studied. Operational parameters such as pH, deposition potential and deposition time were optimized for the purpose of determination of traces of metal ions at pH 3.0. Under optimal conditions the limits of detection, based on three times the background noise, were 9.0 × 10 −4 and 6.0 × 10 −4 μmol L −1 for Hg(II) and Pb(II) with a 90 s preconcentration, respectively. In addition, the modified electrode displayed a good reproducibility and selectivity, making it suitable for the simultaneous determination of Hg(II) and Pb(II) in real samples such as sea water, waste water, tobacco, marine and human teeth samples.

Application of determination of PRA, Ang II and IGF-1 levels in the study of typing of essential hypertension

International Nuclear Information System (INIS)

Lu Yongyi; Chen Qun; Yang Yongqing

2010-01-01

Objective: To study the clinical application of determination of plasma renin activity (PRA), Angiotensin II (Ang II ) and insulin-like growth factor-1 (IGF-1) levels in typing of essential hypertension (EH). Methods: Determined the levels of PRA and Aug II in 256 patients with EH and 70 healthy volunteers (as control group) by radioimmunoassay, and measured IGF-1 level by enzyme immunoassay. Research on the typing of EH and the difference between the groups. Results: The PRA and Ang II in control group was (0.432±0.236) μg·L -1 ·h -1 and (31.7±7.4) μg/L respectively. In 256 patients with EH, PRA was increased, normal and decreased in 18.0%, 71.8% and 10.2% respectively, while the level of Ang II was increased, normal and decreased in 12.9%, 76.2% and 10.9% respectively. The IGF-1 levels in 256 patients with EH were increased following the increase of blood pressure. Conclusion: Typing of EH patients with PRA and Ang II as well as the determination of IGF-1 were useful in treating and following up the patients with EH. (authors)

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

Directory of Open Access Journals (Sweden)

Şerife Tokalıoğlu

2017-01-01

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

Chloroplatinum(II) complex-modified MWCNTs paste electrode for electrochemical determination of mercury in skin lightening cosmetics

International Nuclear Information System (INIS)

Isa, Illyas Md; Saidin, Mohamad Idris; Ahmad, Mustaffa; Hashim, Norhayati; Bakar, Suriani Abu; Ali, Noorshida Mohd; Si, Suyanta M.

2017-01-01

The chemically modified multiwalled carbon nanotubes (MWCNTs) paste electrode with chloroplatinum(II) complex for the determination of mercury is presented. The chloroplatinum(II) complex was characterized by nuclear magnetic resonance spectroscopy (NMR), Fourier transforms infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), energy-dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), scanning electron microscope (SEM), and transmission electron microscope (TEM). The capability of the electron transfer rate on the surface of modified electrode evaluated is by electrochemical impedance spectroscopy (EIS). The square wave stripping voltammetry (SWSV) technique was employed to investigate the performance of chloroplatinum(II) complex-MWCNTs paste electrode for determination of mercury. Several operational parameters such as the composition ratios of the electrode, type of supporting electrolyte, pH of the solution, and the SWSV parameters were thoroughly investigated. Under optimal conditions, the linear range obtained was from 5.0 μM to 0.1 mM with limit detection of 3.7 μM. The interference from other heavy metals such as Ca 2+ , Mg 2+ , Ni 2+ , Zn 2+ , Cd 2+ , Co 2+ , Ba 2+ , Mn 2+ , and Ce 3+ did not influence the electrochemical response. The chloroplatinum(II) complex-MWCNTs paste electrode was successfully applied to determine mercury in skin lightening cosmetics with a good recovery (98.9%–101.1%).

Determination of serum insulinlike growth factor II levels in coronary heart disease patient and its significance

International Nuclear Information System (INIS)

Fan Bifu; Ji Naijun; Mei Yibin; Wang Chengyao; Zhao Junfei; Guan Lihua; Gao Meiying; Li Jiangao

2002-01-01

Objective: To explore the changes and clinical significance of serum insulinlike growth factor II (IGF II) levels in coronary heart disease (CHD) patients. Methods: The serum IGF II levels were determined by radioimmunoassay in 68 patients with coronary heart disease (CHD) and 30 controls with only mild non-cardiac diseases. Results: Compared with the controls, the serum IGF II level in CHD patients were increased significantly (0.66 ± 0.13 μg/L vs 0.51 ± 0.11 μg/L; t = 5.506, p 0.05). Level in patients dies in hospital (n = 9) were much higher than those in patients recovered (n = 59) (t = 2.402, p < 0.05). Conclusion: Serum IGF II levels seems to be related to the seriousness of CHD; the actual mechanism remains to be defined

An alternative method for determination of oscillator strengths: The example of Sc II

International Nuclear Information System (INIS)

Ruczkowski, J.; Elantkowska, M.; Dembczyński, J.

2014-01-01

We describe our method for determining oscillator strengths and hyperfine structure splittings that is an alternative to the commonly used, purely theoretical calculations, or to the semi-empirical approach combined with theoretically calculated transition integrals. We have developed our own computer programs that allow us to determine all attributes of the structure of complex atoms starting from the measured frequencies emitted by the atoms. As an example, we present the results of the calculation of the structure, electric dipole transitions, and hyperfine splittings of Sc II. The angular coefficients of the transition matrix in pure SL coupling were found from straightforward Racah algebra. The transition matrix was transformed into the actual intermediate coupling by the fine structure eigenvectors obtained from the semi-empirical approach. The transition integrals were treated as free parameters in the least squares fit to experimental gf values. For most transitions, the experimental and the calculated gf-values are consistent with the accuracy claimed in the NIST compilation. - Highlights: • The method of simultaneous determination of all the attributes of atomic structure. • The semi-empirical method of parameterization of oscillator strengths. • Illustration of the method application for the example of Sc II data

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

Energy Technology Data Exchange (ETDEWEB)

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

2007-07-19

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

A solid phase extraction procedure for the determination of Cd(II) and Pb(II) ions in food and water samples by flame atomic absorption spectrometry.

Science.gov (United States)

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

2015-05-01

A relatively rapid, accurate and precise solid phase extraction method is presented for the determination of cadmium(II) and lead(II) in various food and water samples. Quantitation is carried out by flame atomic absorption spectrometry (FAAS). The method is based on the retention of the trace metal ions on Dowex Marathon C, a strong acid cation exchange resin. Some important parameters affecting the analytical performance of the method such as pH, flow rate and volume of the sample solution; type, concentration, volume, flow rate of the eluent; and matrix effects on the retention of the metal ions were investigated. Common coexisting ions did not interfere on the separation and determination of the analytes. The detection limits (3 σb) for Cd(II) and Pb(II) were found as 0.13 and 0.18 μg L(-1), respectively, while the limit of quantification values (10 σb) were computed as 0.43 and 0.60 μg L(-1) for the same sequence of the analytes. The precision (as relative standard deviation was lower than 4% at 5 μg L(-1) Cd(II) and 10 μg L(-1) Pb(II) levels, and the preconcentration factor was found to be 250. The accuracy of the proposed procedure was verified by analysing the certified reference materials, SPS-WW2 Batch 108 wastewater level 2 and INCT-TL-1 tea leaves, with the satisfactory results. In addition, for the accuracy of the method the recovery studies (⩾ 95%) were carried out. The method was applied to the determination of the analytes in the various natural waters (lake water, tap water, waste water with boric acid, waste water with H2SO4) and food samples (pomegranate flower, organic pear, radish leaf, lamb meat, etc.), and good results were obtained. While the food samples almost do not contain cadmium, they have included lead at low levels of 0.13-1.12 μg g(-1). Copyright © 2014 Elsevier Ltd. All rights reserved.

Type I and type II residual stress in iron meteorites determined by neutron diffraction measurements

Science.gov (United States)

Caporali, Stefano; Pratesi, Giovanni; Kabra, Saurabh; Grazzi, Francesco

2018-04-01

In this work we present a preliminary investigation by means of neutron diffraction experiment to determine the residual stress state in three different iron meteorites (Chinga, Sikhote Alin and Nantan). Because of the very peculiar microstructural characteristic of this class of samples, all the systematic effects related to the measuring procedure - such as crystallite size and composition - were taken into account and a clear differentiation in the statistical distribution of residual stress in coarse and fine grained meteorites were highlighted. Moreover, the residual stress state was statistically analysed in three orthogonal directions finding evidence of the existence of both type I and type II residual stress components. Finally, the application of von Mises approach allowed to determine the distribution of type II stress.

Determining decoupling points in a supply chain networks using NSGA II algorithm

Energy Technology Data Exchange (ETDEWEB)

Ebrahimiarjestan, M.; Wang, G.

2017-07-01

Purpose: In the model, we used the concepts of Lee and Amaral (2002) and Tang and Zhou (2009) and offer a multi-criteria decision-making model that identify the decoupling points to aim to minimize production costs, minimize the product delivery time to customer and maximize their satisfaction. Design/methodology/approach: We encounter with a triple-objective model that meta-heuristic method (NSGA II) is used to solve the model and to identify the Pareto optimal points. The max (min) method was used. Findings: Our results of using NSGA II to find Pareto optimal solutions demonstrate good performance of NSGA II to extract Pareto solutions in proposed model that considers determining of decoupling point in a supply network. Originality/value: So far, several approaches to model the future have been proposed, of course, each of them modeled a part of this concept. This concept has been considered more general in the model that defined in follow. In this model, we face with a multi-criteria decision problem that includes minimization of the production costs and product delivery time to customers as well as customer consistency maximization.

Determining decoupling points in a supply chain networks using NSGA II algorithm

International Nuclear Information System (INIS)

Ebrahimiarjestan, M.; Wang, G.

2017-01-01

Purpose: In the model, we used the concepts of Lee and Amaral (2002) and Tang and Zhou (2009) and offer a multi-criteria decision-making model that identify the decoupling points to aim to minimize production costs, minimize the product delivery time to customer and maximize their satisfaction. Design/methodology/approach: We encounter with a triple-objective model that meta-heuristic method (NSGA II) is used to solve the model and to identify the Pareto optimal points. The max (min) method was used. Findings: Our results of using NSGA II to find Pareto optimal solutions demonstrate good performance of NSGA II to extract Pareto solutions in proposed model that considers determining of decoupling point in a supply network. Originality/value: So far, several approaches to model the future have been proposed, of course, each of them modeled a part of this concept. This concept has been considered more general in the model that defined in follow. In this model, we face with a multi-criteria decision problem that includes minimization of the production costs and product delivery time to customers as well as customer consistency maximization.

Characterization of Angiotensin II Molecular Determinants Involved in AT1 Receptor Functional Selectivity.

Science.gov (United States)

Domazet, Ivana; Holleran, Brian J; Richard, Alexandra; Vandenberghe, Camille; Lavigne, Pierre; Escher, Emanuel; Leduc, Richard; Guillemette, Gaétan

2015-06-01

The octapeptide angiotensin II (AngII) exerts a variety of cardiovascular effects through the activation of the AngII type 1 receptor (AT1), a G protein-coupled receptor. The AT1 receptor engages and activates several signaling pathways, including heterotrimeric G proteins Gq and G12, as well as the extracellular signal-regulated kinases (ERK) 1/2 pathway. Additionally, following stimulation, βarrestin is recruited to the AT1 receptor, leading to receptor desensitization. It is increasingly recognized that specific ligands selectively bind and favor the activation of some signaling pathways over others, a concept termed ligand bias or functional selectivity. A better understanding of the molecular basis of functional selectivity may lead to the development of better therapeutics with fewer adverse effects. In the present study, we developed assays allowing the measurement of six different signaling modalities of the AT1 receptor. Using a series of AngII peptide analogs that were modified in positions 1, 4, and 8, we sought to better characterize the molecular determinants of AngII that underlie functional selectivity of the AT1 receptor in human embryonic kidney 293 cells. The results reveal that position 1 of AngII does not confer functional selectivity, whereas position 4 confers a bias toward ERK signaling over Gq signaling, and position 8 confers a bias toward βarrestin recruitment over ERK activation and Gq signaling. Interestingly, the analogs modified in position 8 were also partial agonists of the protein kinase C (PKC)-dependent ERK pathway via atypical PKC isoforms PKCζ and PKCι. Copyright © 2015 by The American Society for Pharmacology and Experimental Therapeutics.

Determination of Lead(II), Cadmium(II) and Copper(II) in Waste-Water and Soil Extracts on Mercury Film Screen-Printed Carbon Electrodes Sensor

International Nuclear Information System (INIS)

Mohd Fairulnizal Md Noh; Tothill, I.E.

2011-01-01

A sensor incorporating a three electrodes configuration have been fabricated using low cost screen-printing technology. These electrodes couples with Square Wave Stripping Voltammetry (SWSV) has provided a convenient screening tool for on-site detection of trace levels of Pb(II), Cd(II) and Cu(II). Modification of the graphite carbon surface based on in situ deposition of mercury film has been carried out. By appropriate choice of supporting medium and optimized parameters setting such as amount of mercury used the deposition potential, deposition time, frequency and scan rate, well resolved and reproducible response for Pb(II), Cd(II) and Cu(II) were obtained. The performance characteristics of the developed mercury film screen printed carbon electrode (MFSPCE) for 120 s deposition time showed that the linear range for Cd(II), Pb(II) and Cu(II) were 10 to 200 μg L -1 . The detection limit recorded for Cd(II), Pb(II) and Cu(II) were 2, 1 and 5 μg L -1 with relative standard deviation (RSD) of 6.5 %, 6.9 % and 7.5 %, respectively. Successful applications of the sensing device to waste-water and extracted soil samples were demonstrated. (author)

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

Energy Technology Data Exchange (ETDEWEB)

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

2010-01-15

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

Air-assisted Liquid Liquid Microextraction Combined with Graphite Furnace Atomic Absorption Spectrometry for Preconcentration and Determination of Trace Amount of Co(II and Ni(II Ions in Water Samples

Directory of Open Access Journals (Sweden)

Saeed Mohammad Sorouraddin

2017-12-01

Full Text Available A simple, rapid and efficient method has been developed for the extraction, preconcentration and determination of cobalt (II and nickel (II ions in water samples by air-assisted liquid-liquid microextraction (AALLME coupled with graphite furnace atomic absorption spectrometry (GFAAS. In the proposed method, much less volume of an organic solvent was used as the extraction solvent in the absence of disperser solvent. Fine organic droplets were formed by sucking and injecting of the mixture of aqueous sample solution and extraction solvent with a syringe for several times in a conical test tube. After extraction, phase separation was performed by centrifugation and the enriched analytes in the sedimented phase were determined by GFAAS. Several variables that could affect the extraction efficiency were investigated and optimized. Calibration graphs were linear in the range of 6.5-100 ng L-1. Detection limits for Co and Ni were 2.3 ng L-1 and 3 ng L-1, respectively. The accuracy of the developed procedure was checked by analyzing NRCC-SLRS4 Riverine water as a certified reference material. Finally, the proposed method has been successfully applied for the determination of cobalt (II and nickel (II ions in tap, surface and river water samples.

The use of a polymer inclusion membrane in a paper-based sensor for the selective determination of Cu(II).

Science.gov (United States)

Jayawardane, B Manori; Coo, Lilibeth dlC; Cattrall, Robert W; Kolev, Spas D

2013-11-25

A disposable paper-based sensor (PBS) is described for the determination of Cu(II) in natural and waste waters at approximately 2 cents per measurement. The device makes use of a polymer inclusion membrane (PIM) to provide the selectivity for Cu(II). The PIM consists of 40 wt% di(2-ethlyhexyl) phosphoric acid (D2EHPA) as the carrier, 10 wt% dioctyl phthalate (DOP) as a plasticizer, 49.5 wt% poly(vinyl chloride) (PVC) as the base polymer and 0.5 wt% (mm(-1)) 1-(2'-pyridylazo)-2-naphthol (PAN) as the colourimetric reagent. High selectivity under mildly acidic conditions (HCl, pH 2.0) is achieved for Cu(II) in the presence of frequently encountered metal ions in natural and waste waters such as Fe(III), Al(III), Zn(II), Cd(II), Pb(II), Ca(II), Mg(II), and Ni(II). The laminated PBS consists of a PIM sensing disc (2mm in diameter) attached to the centre of a circular hydrophilic zone (7 mm in diameter) pretreated with 0.01 M HCl. This hydrophilic zone separates the sample port (a circular hole in the plastic cover) from the PIM sensing disc. After introducing 19.2 μL of a sample/standard solution to the sample port, Cu(II) diffuses across the hydrophilic zone and is extracted into the PIM disc as the Cu(II)-D2EHPA complex which subsequently reacts with PAN to produce the red-purple coloured Cu(II)-PAN complex. The colour intensity of the PIM disc is measured 15 min after sample/standard introduction by scanning using a flatbed scanner. Under optimal conditions the device is characterized by a limit of detection (LOD) and limit of quantitation (LOQ) of 0.06 and 0.21 mg L(-1) Cu(II), respectively, with two linear ranges together covering the Cu(II) concentration range from 0.1 to 30.0 mg L(-1). The PBS was successfully applied to the determination of Cu(II) in hot tap water and mine tailings water. Copyright © 2013 Elsevier B.V. All rights reserved.

A nanosized cadmium(II)-imprinted polymer for use in selective trace determination of cadmium in complex matrices

International Nuclear Information System (INIS)

Behbahani, Mohammad; Bagheri, Akbar; Barati, Mozhgan; Pourali, Ali Reza; Tapeh, Nasim Akbari Ghareh; Bojdi, Majid Kalate

2013-01-01

We describe a nanosized Cd(II)-imprinted polymer that was prepared from 4-vinyl pyridine (the functional monomer), ethyleneglycol dimethacrylate (the cross-linker), 2,2′-azobisisobutyronitrile (the radical initiator), neocuproine (the ligand), and Cd(II) (the template ion) by precipitation polymerization in acetonitrile as the solvent. The imprinted polymer was characterized by X-ray diffraction, thermogravimetric analysis, differential thermal analysis, and scanning electron microscopy. The maximum adsorption capacity of the nanosized sorbent was calculated to be 64 mg g −1 . Cadmium(II) was then quantified by FAAS. The relative standard deviation and limit of detection are 4.2 % and 0.2 μg L −1 , respectively. The imprinted polymer displays improve selectivity for Cd(II) ions over a range of competing metal ions with the same charge and similar ionic radius. This nanosized sorbent is an efficient solid phase for selective extraction and preconcentration of Cd(II) in complex matrices. The method was successfully applied to the trace determination of Cd(II) in food and water samples. (author)

Common molecular determinants of tarantula huwentoxin-IV inhibition of Na+ channel voltage sensors in domains II and IV.

Science.gov (United States)

Xiao, Yucheng; Jackson, James O; Liang, Songping; Cummins, Theodore R

2011-08-05

The voltage sensors of domains II and IV of sodium channels are important determinants of activation and inactivation, respectively. Animal toxins that alter electrophysiological excitability of muscles and neurons often modify sodium channel activation by selectively interacting with domain II and inactivation by selectively interacting with domain IV. This suggests that there may be substantial differences between the toxin-binding sites in these two important domains. Here we explore the ability of the tarantula huwentoxin-IV (HWTX-IV) to inhibit the activity of the domain II and IV voltage sensors. HWTX-IV is specific for domain II, and we identify five residues in the S1-S2 (Glu-753) and S3-S4 (Glu-811, Leu-814, Asp-816, and Glu-818) regions of domain II that are crucial for inhibition of activation by HWTX-IV. These data indicate that a single residue in the S3-S4 linker (Glu-818 in hNav1.7) is crucial for allowing HWTX-IV to interact with the other key residues and trap the voltage sensor in the closed configuration. Mutagenesis analysis indicates that the five corresponding residues in domain IV are all critical for endowing HWTX-IV with the ability to inhibit fast inactivation. Our data suggest that the toxin-binding motif in domain II is conserved in domain IV. Increasing our understanding of the molecular determinants of toxin interactions with voltage-gated sodium channels may permit development of enhanced isoform-specific voltage-gating modifiers.

Spectrophotometric Determination of Metoprolol Tartrate in Pharmaceutical Dosage Forms on Complex Formation with Cu(II

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Mustafa Cesme

2011-06-01

Full Text Available A new, simple, sensitive and accurate spectrophotometric method has been developed for the assay of metoprolol tartrate (MPT, which is based on the complexation of drug with copper(II [Cu(II] at pH 6.0, using Britton-Robinson buffer solution, to produce a blue adduct. The latter has a maximum absorbance at 675 nm and obeys Beer’s law within the concentration range 8.5-70 mg/mL. Regression analysis of the calibration data showed a good correlation coefficient (r = 0.998 with a limit of detection of 5.56 mg/mL. The proposed procedure has been successfully applied to the determination of this drug in its tablets. In addition, the spectral data and stability constant for the binuclear copper(II complex of MPT (Cu2MPT2Cl2 have been reported.

Clinical significance of determination of changes of serum IGF-II, CRP levels after treatment in pediatric patients with broncho-pneumonia

International Nuclear Information System (INIS)

Chen Chuanbin

2006-01-01

Objective: To investigate the changes of serum insulin-like growth factor-II (IGF-II), CRP levels after treatment in pediatric patients with bronchopneumonia. Methods: Serum IGF-II levels were measured with RIA and serum CRP levels with immune method both before and after treatment in 33 pediatric patients with bronchopneumonia and 35 controls. Results: Before treatment the serum levels of IGF-II, CRP were significantly higher in the patients than those in controls (P 0.05). Conclusion: Determination of serum IGF-II, CRP levels is clinically useful in the management of pediatric patients with bronchopneumonia. (authors)

Levels of Cd (II, Mn (II, Pb (II, Cu (II, and Zn (II in Common Buzzard (Buteo buteo from Sicily (Italy by Derivative Stripping Potentiometry

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P. Licata

2010-01-01

Full Text Available The purpose of this study was to determine the concentrations of heavy metals (Cd, Pb, Cu, Mn, and Zn in different organs (liver, kidney, muscle, lung, skin, and feathers of buzzards (Buteo buteo, utilized as a “biological indicator” for environmental contamination, from different areas of Sicily and to investigate the relationships between birds sex, age, and weight and metal levels in these samples. All samples of common buzzards were collected at the “Recovery Center of Wild Fauna” of Palermo, through the Zooprophilactic Institute. Potentiometric stripping analysis (PSA was used to determine the content of Cd(II, Cu(II, Mn(II, Pb(II, and Zn(II in bird tissues. For toxic metals, the highest levels of Pb were in liver and those of Cd in lung; Zn levels were higher than Cu and Mn in all tissues analyzed. The concentrations in liver, lung, kidney, and muscle could be considered as an indicative of chronic exposure to metals while the presence of metals in skin could be consequential to storing and elimination processes. The found concentrations of metals in the studied matrices required a highly sensitive method for their determination and a simple sample preparation procedure, and the proposed method was well suited for this purpose.

Performance Evaluation of Monolith Based Immobilized Acetylcholinesterase Flow-Through Reactor for Copper(II Determination with Spectrophotometric Detection

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Parawee Rattanakit

2014-01-01

Full Text Available A monolith based immobilized acetylcholinesterase (AChE flow-through reactor has been developed for the determination of copper(II using flow injection spectrophotometric system. The bioreactor was prepared inside a microcapillary column by in situ polymerization of butyl methacrylate, ethylene dimethacrylate, and 2,2-dimethoxy-1,2-diphynyletane-1-one in the presence of 1-decanol, followed by vinyl azlactone functionalization and AChE immobilization. The behavior of AChE before and after being immobilized on the monolith was evaluated by kinetic parameters from Lineweaver and Burk equation. The detection was based on measuring inhibition effect on the enzymatic activity of AChE by copper(II using Ellman’s reaction with spectrophotometric detection at 410 nm. The linear range of the calibration graph was obtained over the range of 0.02–3.00 mg L−1. The detection limit, defined as 10% inhibition (I10, was found to be 0.04 mg L−1. The repeatability was 3.35 % (n=5 for 1.00 mg L−1 of copper(II. The proposed method was applied to the determination of copper(II in natural water samples with sampling rate of 4 h−1.

CATALYTIC SPECTROPHOTOMETRIC DETERMINATION OF Mn(II ...

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method is based on the catalytic effect of Mn(II) with the oxidation of Celestine blue .... water samples were filtered through a 0.45 μm pore size membrane filter to remove suspended .... slope of the calibration graph as the optimization criterion. ..... In presence of Phen as stability enhancement agent in indicator system. ( ) +.

Determination of Cu(III) and Cu(II)+Cu(III) in superconducting copper ceramics

International Nuclear Information System (INIS)

Nedelcheva, T.; Kostadinova, L.; Stoyanova-Ivanova, A.; Ivanova, I.

1992-01-01

Copper(III) and total copper in superconducting Y-Ba-Cu oxide and related compounds can be determinated by two successive iodimetric titrations after the sample has been dissolved under Ar in HCl/KI medium. First, the iodine equivalent to copper(III) is titrated with Na 2 S 2 O 3 solution at pH 4.8, copper(II) being masked with EDTA. The total copper is then determined in the same solution by demasking with acid and iodide, followed by iodimetric titration. The method is both accurate and reproducible. The relative standard deviations for 1.074% copper(III) and 23.37% total copper are 0.8% and 0.3%, respectively. (orig.)

Straightforward grafting approach for cyclam-functionalized screen-printed electrodes for selective Cu(II) determination

International Nuclear Information System (INIS)

Jasmin, Jean-Philippe; Ouhenia-Ouadahi, Karima; Miserque, Frédéric; Dumas, Eddy; Cannizzo, Caroline; Chaussé, Annie

2016-01-01

We report in this paper an original way to covalently bind the macrocyclic ligand, 1,4,8,11-tetraazacyclotetradecane (cyclam), through diazonium salt chemistry, on the surface of carbon screen-printed electrodes (SPEs). The in situ synthesis of the diazonium salt obtained from the amine precursor derived from the cyclam and its electrografting are described. X-ray Photoelectron Spectroscopy was used to characterize this functionalized surface. Owing to the strong cyclam–Cu(II) affinity, the so called SPE-cyclam can be used as electrochemical sensors for Cu(II) determination at trace levels. The influence of electroanalysis parameters such as the accumulation time and the pH of the medium were investigated. An interference study was carried out with numerous metallic cations and few interference was found for Cu(II) quantification. The described method provided a limit of detection and a limit of quantification of 1.3 × 10"−"8 M and 4.0 × 10"−"8 M, respectively. Interference study and performances show that SPE-cyclam could be considered as efficient sensors for environmental analysis.

Clinical significance of determination of serum insulin-like growth factor II levels in patients with chronic obstructive pulmonary diseases (COPD)

International Nuclear Information System (INIS)

Wu Changming

2006-01-01

Objective: To explore the clinical significance of the changes of serum insulinlike growth factor II (IGF-II) levels in patients with chronic obstruive pulmonary diseases (COPD). Methods: The serum IGF-II levels was determined with radioimmunoassay in 60 patients with COPD and 30 controls. Results: The serum IGF-II levels in patients with COPD were significantly higher than those in controls (0.65 ± 0.22μg/L vs 0.51±0.18μg/L, P<0.01). There were no significant differences among the levels in patients of different stages (stages I, II, III). Levels of IGF-II were significantly higher in patients succumbed to the dis- ease than those in patients recoverd (P<0.05). Conclusion: Serum IGF-II levels were significantly increased in patients with COPD, especially in those succumbed. (authors)

Sequence variation of functional HTLV-II tax alleles among isolates from an endemic population: lack of evidence for oncogenic determinant in tax.

Science.gov (United States)

Hjelle, B; Chaney, R

1992-02-01

Human T-cell leukemia-lymphoma virus type II (HTLV-II) has been isolated from patients with hairy cell leukemia (HCL). We previously described a population with longstanding endemic HTLV-II infection, and showed that there is no increased risk for HCL in the affected groups. We thus have direct evidence that the endemic form(s) of HTLV-II cause HCL infrequently, if at all. By comparison, there is reason to suspect that the viruses isolated from patients with HCL had an etiologic role in the disease in those patients. One way to reconcile these conflicting observations is to consider that isolates of HTLV-II might differ in oncogenic potential. To determine whether the structure of the putative oncogenic determinant of HTLV-II, tax2, might differ in the new isolates compared to the tax of the prototype HCL isolate, MO, four new functional tax cDNAs were cloned from new isolates. Sequence analysis showed only minor (0.9-2.0%) amino acid variation compared to the published sequence of MO tax2. Some codons were consistently different from published sequences of the MO virus, but in most cases, such variations were also found in each of two tax2 clones we isolated from the MO T-cell line. These variations rendered the new clones more similar to the tax1 of the pathogenic virus HTLV-I. Thus we find no evidence that pathologic determinants of HTLV-II can be assigned to the tax gene.

Removal of nickel(II and palladium(II from surface waters

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V. Sharifzade

2013-04-01

Full Text Available A new sorbent was prepared using alumina and 5-Br-PADAP, and its adsorption ability for the removal of Ni(II and Pd(II from different waters was investigated. The procedure is based on retention of the analytes on the alumina load with 5-Br-PADAP at pH ~ 6. The separation/preconcentration conditions for the quantitative recoveries were investigated. The limit of detections (LOD based on three times the standard deviations of the blank, were 0.187 and 0.253 ng mL-1 for Ni(II and Pd(II, respectively. Obtained sorption capacities for 1 g sorbent were 6.0 mg Ni(II and 11.0 mg Pd(II. The linearity was maintained in the concentration range of 0.625 to 6.0 ng mL-1 for Ni(II and 0.416 to 7.0 ng mL-1 for Pd(II in the original solution. Eight replicate determinations of a mixture containing 2.0 µg mL-1 each of the elements in the final solution gave relative standard deviation of ±0.82 and ±1.12% for Ni(II and Pd(II, respectively. The proposed method was successfully applied to the determination trace amounts of Ni(II and Pd(II in the surface water samples.DOI: http://dx.doi.org/10.4314/bcse.v27i1.2

Clinical significance of determination of changes of serum IGF-II, GM-CSF and TNF-α levels after treatment in children with acute nephritis

International Nuclear Information System (INIS)

Xu Xiaoyan; Zhou Hong; Xu Weiqin; Li Xinghua

2008-01-01

Objective: To explore the clinical significance of determination of changes of serum IGF-II, GM-CSF and TNF- α levels after treatment in children with acute nephritis. Methods: Serum IGF-II, GM-CSF and TNF-α levels (with RIA) were measured in 31 pediatric patients with acute nephritis and 35 controls. Results: Before treatment, the serum IGF-II, GM-CSF and TNF-α levels in the patients were significantly higher than those in controls (P< O.01). After treatment for 3 months, the serum IGF-II, GM-CSF and TNF-α levels, though markedly corrected, remained significantly higher than those in controls (P<0.05). Conclusion: Determination of changes of serum IGF-II, GM-CSF and TNF-α contents after treatment might be of prognostic importance in pediatric patients with acute nephritis. (authors)

Speciative Determination of Dissolved Inorganic Fe(II), Fe(III) and Total Fe in Natural Waters by Coupling CPE with FAAS

International Nuclear Information System (INIS)

Gurkan, R.; Altunay, N.

2013-01-01

A new cloud point extraction (CPE) method for the preconcentration of trace iron speciation in natural waters prior to determination by flame atomic absorption spectrometry (FAAS) was developed in the present study. In this method, Fe(II) sensitively and selectively reacts with Calcon carboxylic acid (CCA) in presence of cetylpyridinium chloride (CPC) yielding a hydrophobic complex at pH 10.5, which is then entrapped in surfactant-rich phase. Total Fe was accurately and reliably determined after the reduction of Fe(III) to Fe(II) with sulfite. The amount of Fe(III) in samples was determined from the difference between total Fe and Fe(II). CPC was used not only as an auxiliary ligand in CPE, but also as sensitivity enhancement agent in FAAS. The nonionic surfactant, polyethylene glycol tert-octylphenyl ether (Triton X-114) was used as an extracting agent. The analytical variables affecting CPE efficiency were investigated in detail. The preconcentration/enhancement factors of 50 and 82 respectively, were obtained for the preconcentration of Fe(II) with 50 mL solution. Under the optimized conditions, the detection limit of Fe(II) in linear range of 0.2-60 μg L/sup -1/ was 0.06 μg L/sup -1/. The relative standard deviation was 2.7 percentage (20 μg L/sup -1/, N: 5), recoveries for Fe(II) were in range of 99.0-102.0 percentage for all water samples including certified reference materials (CRMs). In order to verify its accuracy, two CRMs were analyzed and the results obtained were statistically in good agreement with the certified values. (author)

Insulin-like growth factor I and II in 14 animal species and man as determined by three radioligand assays and two bioassays

Energy Technology Data Exchange (ETDEWEB)

Zangger, I.; Zapf, J.; Froesch, E.R.

1987-01-01

Insulin-like growth factor I and II (IGF I and II) were determined by five different assays in human serum, in the sera of ten mammalian species and in chicken, turtle, and frog serum. Sera of all tested mammals contain two different IGFs corresponding to human immunoreactive IGF I and receptor reactive IGF II. Receptor reactive IGF II of most animal species does not show significant cross-reactivity in the RIA for human IGF II. IGF activity was also detected in sera of non-mammals, such as chicken and turtles, but not in frog serum. The IGF values obtained with the different assay system corresponded rather well: there is a good correlation between the values obtained in the protein binding and the fat cell assay, and between the results of the latter assays and the sum of immunoreactive IGF I and receptor reative IGF II. The results suggest that those regions in the IGF I and II molecules which are responsible for reactivity with the type I IGF and the insulin receptor have not essentially changed during evolution. Similarly, the C-region, which mainly determines the immunological properties of IGFs, appears to have remained relatively constant in the IGF I, but not in the IGF II molecule.

Indirect spectrophotometric determination of sodium ceftriaxone with n-propyl alcohol-ammonium sulfate-water system by extraction flotation of copper(II).

Science.gov (United States)

Zhao, Wei; Zhang, Yan; Li, Quanmin

2008-05-01

Although the determination methods of sodium ceftriaxone has been increasingly reported, these methods have their inherent limits preventing them from being broadly applied in common laboratories. In order to circumvent this problem, a rapid and simple method for the indirect spectrophotometric determination of sodium ceftriaxone is reported. Sodium ceftriaxone was degraded completely in the presence of 0.20 mol/l sodium hydroxide in boiling water bath for 20 min. The thiol group (-SH) of the degradation product (I) of sodium ceftriaxone could reduce cupric to cuprous ions, and the resulting which was precipitated with the thiol group (-SH) of the degradation product (II) at pH 4.0. By determining the residual amount of copper (II), the indirect determination of sodium ceftriaxone can be achieved. Standard curve of sodium ceftriaxone versus the flotation yield of copper(II) showed that sodium ceftriaxone could be determined in low concentrations. The linear range of sodium ceftriaxone was 0.70-32 microg/ml and the detection limit evaluated by calibration curve (3sigma/k) was found to be 0.60 microg/ml. A simple and efficient method was developed and it has been successfully applied to the determination of sodium ceftriaxone in human serum and urine samples, respectively. It is expected that this method will find broad applications in the detection of cephalosporin derivatives with similar structure.

Single peak parameters technique for simultaneous measurements: Spectrophotometric sequential injection determination of Fe(II) and Fe(III).

Science.gov (United States)

Kozak, J; Paluch, J; Węgrzecka, A; Kozak, M; Wieczorek, M; Kochana, J; Kościelniak, P

2016-02-01

Spectrophotometric sequential injection system (SI) is proposed to automate the method of simultaneous determination of Fe(II) and Fe(III) on the basis of parameters of a single peak. In the developed SI system, sample and mixture of reagents (1,10-phenanthroline and sulfosalicylic acid) are introduced into a vessel, where in an acid environment (pH≅3) appropriate compounds of Fe(II) and Fe(III) with 1,10-phenanthroline and sulfosalicylic acid are formed, respectively. Then, in turn, air, sample, EDTA and sample again, are introduced into a holding coil. After the flow reversal, a segment of air is removed from the system by an additional valve and as EDTA replaces sulfosalicylic acid forming a more stable colorless compound with Fe(III), a complex signal is registered. Measurements are performed at wavelength 530 nm. The absorbance measured at minimum of the negative peak and the area or the absorbance measured at maximum of the signal can be used as measures corresponding to Fe(II) and Fe(III) concentrations, respectively. The time of the peak registration is about 2 min. Two-component calibration has been applied to analysis. Fe(II) and Fe(III) can be determined within the concentration ranges of 0.04-4.00 and 0.1-5.00 mg L(-1), with precision less than 2.8% and 1.7% (RSD), respectively and accuracy better than 7% (RE). The detection limit is 0.04 and 0.09 mg L(-1) for Fe(II) and Fe(III), respectively. The method was applied to analysis of artesian water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Polarographic determination of Sn (II) and total Sn in PYRO and MDP radiopharmaceutical kits

International Nuclear Information System (INIS)

Sebastian, Maria V.A.; Lugon, Marcelo Di M.V.; Silva, Jose L. da; Fukumori, Neuza T.O.; Pereira, Nilda P.S. de; Silva, Constancia P.G. da; Matsuda, Margareth M.N.

2007-01-01

A sensitive, alternative method to atom absorption spectrometry, fluorimetry or potentiometry for the evaluation of tin(II) ions (0.1- 10 mg) and total tin in radiopharmaceutical kits was investigated. Differential pulse polarography was chosen. The supporting electrolyte was H 2 SO 4 3 mol L -1 and HCl 3 mol L -1 solution. The potential was swept from -250 to -800 mV vs Ag/AgCl/saturated KCl, using a dropping mercury electrode with 1 s drop time, 50 mV s -1 scan rate, -50 mV pulse amplitude, 40 ms pulse time and 10 mV step amplitude. Pure nitrogen was used to deaerate the polarographic cell solution for 5 min, before and after each sample introduction. Oxidation of Sn(II) was made in the same sample vial by adding H 2 O 2 (hydrogen peroxide) 10 mol L -1 , at 37 deg C, in order to quantify the total Sn. The calibration curve for Sn(II) and Sn(IV) was obtained in the concentration range of 0-10 ppm from a 1000 ppm standard solution. The detection limit of Sn(II) is 0.5 ppm and for Sn(IV) is 0.6 ppm. Differential pulse polarography was performed in the pyrophosphate (PYRO) and methylenediphosphonic acid (MDP) radiopharmaceutical kits, containing 2 mg and 1 mg of SnCl 2 .2H 2 O per vial, respectively. The described method for determination of stannous ion (Sn(II)), is selective, reproducible and adequate to be used in the quality control of lyophilized reagents and it shall be performed for other cold kits produced at IPEN. (author)

Flame atomic absorption spectrometric determination of heavy metals in aqueous solution and surface water preceded by co-precipitation procedure with copper(II) 8-hydroxyquinoline

Science.gov (United States)

Ipeaiyeda, Ayodele Rotimi; Ayoade, Abisayo Ruth

2017-12-01

Co-precipitation procedure has widely been employed for preconcentration and separation of metal ions from the matrices of environmental samples. This is simply due to its simplicity, low consumption of separating solvent and short duration for analysis. Various organic ligands have been used for this purpose. However, there is dearth of information on the application of 8-hydroxyquinoline (8-HQ) as ligand and Cu(II) as carrier element. The use of Cu(II) is desirable because there is no contamination and background adsorption interference. Therefore, the objective of this study was to use 8-HQ in the presence of Cu(II) for coprecipitation of Cd(II), Co(II), Cr(III), Ni(II) and Pb(II) from standard solutions and surface water prior to their determinations by flame atomic absorption spectrometry (FAAS). The effects of pH, sample volume, amount of 8-HQ and Cu(II) and interfering ions on the recoveries of metal ions from standard solutions were monitored using FAAS. The water samples were treated with 8-HQ under the optimum experimental conditions and metal concentrations were determined by FAAS. The metal concentrations in water samples not treated with 8-HQ were also determined. The optimum recovery values for metal ions were higher than 85.0%. The concentrations (mg/L) of Co(II), Ni(II), Cr(III), and Pb(II) in water samples treated with 8-HQ were 0.014 ± 0.002, 0.03 ± 0.01, 0.04 ± 0.02 and 0.05 ± 0.02, respectively. These concentrations and those obtained without coprecipitation technique were significantly different. Coprecipitation procedure using 8-HQ as ligand and Cu(II) as carrier element enhanced the preconcentration and separation of metal ions from the matrix of water sample.

Thiopental and Phenytoin as Novel Ionophores for Potentiometric Determination of Lead (II Ions

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Yasser M. Abd EL-Karem

2009-03-01

Full Text Available Two novel polymeric membrane sensors for the analysis of Pb(II have been developed based ontwo therapeutic drugs, thiopental (TP and phenytoin (PT as two new ionophores and potassium tetrakis(p-chlorophenyl borate (KTpClPB as a lipophilic additive, in plasticized PVC membranes. The sensors show a Nernstian response for Pb(II ions over the wide concentration ranges of 1×10-2 - 7×10-6 M and 1×10-2 - 8×10-6 M for the sensors based on thiopental and phenytoin, respectively. The proposed sensors have a fast response time and can be used for more than nine weeks without any considerable divergence in potentials. The sensors exhibit comparatively good selectivity with respect to alkaline, alkaline earth and some transition and heavy metal ions. They were employed for direct determination of lead in solder alloys and in galena rocks with a good agreement with the obtained results by atomic absorption spectroscopy.

SPE coupled to AAS trace determination of Cd(II) and Zn(II) in food samples using amine functionalized GMA-MMA-EGDMA terpolymer: Isotherm and kinetic studies.

Science.gov (United States)

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

2016-12-15

An ethylenediamine functionalized glycidyl methacrylate (GMA) based terpolymeric chelating resin was synthesized for the separation and preconcentration of Cd(II) and Zn(II) by SPE from bread, rice and fruit juice prior to FAAS determination. The resin was characterized by FT-IR, TGA/DTA, SEM, BET analysis and EDS. Synthesized resin shows a good capacity of 53.96mgg(-1) for Cd(II) and 24.19mgg(-1) for Zn(II) at pH 8.0. Five isotherm equilibrium models were studied to explain the sorption phenomenon out of which Langmuir, Dubinin-Radushkevich, Scatchard and Temkin models were found to be the best fitted. The limit of detection (LOD) and limit of quantification (LOQ) were observed to be 1.5 and 5.1μgL(-1) for Cd and 1.2 and 4.1μgL(-1) for Zn. The reliability of the method was investigated by the analysis of SRM and the recovery of analytes from various spiked food samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

Sensitive stripping voltammetric determination of Cd(II) and Pb(II) by a Bi/multi-walled carbon nanotube-emeraldine base polyaniline-Nafion composite modified glassy carbon electrode

International Nuclear Information System (INIS)

Zhao, Guo; Yin, Yuan; Wang, Hui; Liu, Gang; Wang, Zhiqiang

2016-01-01

Highlights: • A MWCNT-EBP-NA composite film modified GCE was fabricated and characterized. • The GCE modified with the MWCNT-EBP-NA composite film exhibited excellent performance in the analysis of Cd(II) and Pb(II) by SWASV. • The Cd(II) and Pb(II) detection limits of the developed electrode were approximately 0.06 μg/L and 0.08 μg/L, respectively. • Bi/MWCNT-EBP-NA/GCE was successfully used to determine metal ions in soil samples. - Abstract: In this study, a multi-walled carbon nanotube (MWCNT)-emeraldine base polyaniline (EBP)-Nafion (NA) composite modified glassy carbon electrode (MWCNT-EBP-NA/GCE) was prepared and used for the sensitive detection of trace Pb(II) and Cd(II), with a detection limit of 0.06 μg/L for Cd(II) and 0.08 μg/L for Pb(II) (S/N = 3), by square wave anodic stripping voltammetry (SWASV). A bismuth film was prepared through the in situ plating of bismuth on the MWCNT-EBP-NA/GCE. The morphologies and electrochemical properties of the modified electrode were characterized by SWASV, scanning electron microscopy (SEM), electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). The parameters affecting the stripping current response were investigated and optimized. The formed MWCNTs in the composite film enlarged the specific surface area of the electrode and significantly promoted electron transferring, and the formed polyaniline (PANI) enhanced the ion-exchange capacity and prevented the macromolecules in real samples from absorbing onto the surface of the electrode. The presence of NA effectively increased the stability and adhesion of the composite film, enhanced the cation-exchange capacity and improved the ability to preconcentrate metal ions. Under the optimized conditions, a linear range of 1.0 to 50.0 μg/L was achieved for both metal ions, with a detection limit of 0.06 μg/L for Cd(II) and 0.08 μg/L for Pb(II) (S/N = 3), offering good repeatability. Finally, the Bi/MWCNT-EBP-NA/GCE was used for the

Selective and sensitized spectrophotometric determination of trace amounts of Ni(II) ion using α-benzyl dioxime in surfactant media

Science.gov (United States)

Ghaedi, Mehrorang

2007-02-01

Highly sensitive and interference-free sensitized spectrophotometric method for the determination of Ni(II) ions is described. The method is based on the reaction between Ni(II) ion and benzyl dioxime in micellar media in the presence of sodium dodecyl sulfate (SDS). The absorbance is linear from 0.1 up to 25.0 μg mL -1 in aqueous solution with repeatability (RSD) of 1.0% at a concentration of 1 μg mL -1 and a detection limit of 0.12 ng mL -1 and molar absorption coefficient of 68,600 L mol -1 cm -1. The influence of reaction variables including type and amount of surfactant, pH, and amount of ligand and complexation time and the effect of interfering ions are investigated. The proposed procedure was applied to the determination of trace amounts of Ni(II) ion in tap water, river water, chocolate and vegetable without separation or organic solvent extraction.

Multisensor system for determination of iron(II), iron(III), uranium(VI) and uranium(IV) in complex solutions

International Nuclear Information System (INIS)

Legin, A.V.; Seleznev, B.L.; Rudnitskaya, A.M.; Vlasov, Yu.G.; Tverdokhlebov, S.V.; Mack, B.; Abraham, A.; Arnold, T.; Baraniak, L.; Nitsche, H.

1999-01-01

Development and analytical evaluation of a multisensor system based on the principles of 'electronic tongue' for the determination of low contents of uranium(VI), uranium(IV), iron(II) and iron(III) in complex aqueous media have been carried out. A set of 29 different chemical sensors on the basis of all- solid-state crystalline and vitreous materials with enhanced electronic conductivity and redox and ionic cross-sensitivity have been incorporated into the sensor array. Multidimensional data have been processed by pattern recognition methods such as artificial neural networks and partial least squares. It has been demonstrated that Fe(II) and Fe(III) contents in the range from 10 -7 to 10 -4 mol L -1 of total iron concentration can be determined with the average precision of about 25 %. U(VI) and U(IV) contents can been determined with the average precision of 10-40% depending on the concentration. The developed multisensor system can be applied in future for the analysis of mining and borehole waters as well other contaminated natural media, including on-site measurements. (author)

A cephalometric analysis of Class II dentate subjects to establish a formula to determine the occlusal plane in Class II edentate subjects: A neo adjunct.

Science.gov (United States)

Sinha, Nikita; Reddy, K Mahendranadh; Gupta, Nidhi; Shastry, Y M

2017-01-01

Occlusal plane (OP) differs considerably in participants with skeletal Class I and Class II participants. In this study, cephalometrics has been used to help in the determination of orientation of the OP utilizing the nonresorbable bony anatomic landmarks in skeletal Class II participants and an attempt has been made to predict and examine the OP in individuals with skeletal class II jaw relationship. One hundred dentulous participants with skeletal Class II malocclusion who came to the hospital for correcting their jaw relationship participated in the study. Their right lateral cephalogram was taken using standardized procedures, and all the tracings were manually done by a single trained examiner. The cephalograms which were taken for the diagnostic purpose were utilized for the study, and the patient was not exposed to any unnecessary radiation. The numerical values obtained from the cephalograms were subjected to statistical analysis. Pearson's correlation of orientation of the OP in Class II edentulous participants. Pearson's correlation coefficient and linear regression analysis were performed, and a high correlation was found between A2 and (A2 + B2)/(B2 + C2) with " r " value of 0.5. A medium correlation was found between D2 and (D2 + E2)/(E2 + F2) with " r " value of 0.42. The formula obtained for posterior reference frame through linear regression equation was y = 0.018* × +0.459 and the formula obtained for anterior reference frame was y1 = 0.011* × 1 + 0.497. It was hypothesized that by substituting these formulae in the cephalogram obtained from the Class II edentate individual, the OP can be obtained and verified. It was concluded that cephalometrics can be useful in examining the orientation of OP in skeletal Class II participants.

Determination of metallothioneins by fluorescence and resonance light scattering strategies based on ciprofloxacin–Cu(II) system

Energy Technology Data Exchange (ETDEWEB)

Liu, Lu [College of Public Health, University of South China, Hengyang 421001 (China); Wang, Yong-Sheng, E-mail: yongsheng.w@tom.com [College of Public Health, University of South China, Hengyang 421001 (China); Xue, Jin-Hua; Yang, Hui-Xian; Li, Qiu; Zhou, Bin; Wang, Jia-Cheng; Yin, Ji-Cheng; Wang, Yong-Song [College of Public Health, University of South China, Hengyang 421001 (China); Xiao, Xi-Lin [College of Chemistry and Chemical Engineering, University of South China, Hengyang 421001 (China)

2013-06-15

Based on ciprofloxacin (CIP)–Cu(II) system, the novel methods for the detection of metallothioneins (MTs) have been developed by fluorescence (FL) and resonance light scattering (RLS) strategies. The FL strategy avoids the label and derivatization steps in common methods, while the RLS strategy can be applied for determining bio-macromolecules and small molecules without native fluorescence. The response signals linearly correlated with the concentration of MTs over the ranges of 1.03×10{sup −8}–1.23×10{sup −6} mol L{sup −1} for FL, and of 2.56×10{sup −7}–1.54×10{sup −6} mol L{sup −1} for RLS. The limits of detection (LOD) are 3.1×10{sup −9} mol L{sup −1} for FL and 7.68×10{sup −8} mol L{sup −1} for RLS. This study represents the comparison of these two methods using the same CIP–Cu{sup 2+}–MTs system. They not only allow practical application for MTs detection but also serve as a potential choice for the operators according to their concrete needs. In addition, the mechanisms for FL and RLS enhancement of the system were also discussed. -- Highlights: ► Determination of MTs was developed based on CIP–Cu(II) system by FL and RLS strategies. ► FL strategy provides lower limit of detection and wider linear range, and avoids the label and derivatization steps. ► RLS strategy can be applied for determining bio-macromolecules and small molecules. ► The mechanism of interaction of MTs with CIP–Cu(II) chelate was discussed.

Determination of copper (II) in foodstuffs based on its quenching effect on the fluorescence of N,N'-bis(pyridoxal phosphate)-o-phenylenediamine.

Science.gov (United States)

Xu, Canhui; Liao, Lifu; He, Yunfei; Wu, Rurong; Li, Shijun; Yang, Yanyan

2015-01-01

A Schiff base-type fluorescence probe was prepared for the detection of copper (II) in foodstuffs. The probe is N,N'-bis(pyridoxal phosphate)-o-phenylenediamine (BPPP). It was synthesized by utilizing the Schiff base condensation reaction of pyridoxal 5-phosphate with 1,2-phenylenediamine. BPPP has the properties of high fluorescence stability, good water solubility and low toxicity. Its maximum excitation wavelength and maximum fluorescence emission wavelength are at 389 and 448 nm, respectively. When BPPP coexists with copper (II), its fluorescence is dramatically quenched. Under a certain condition, the fluorescence intensity decreased proportionally to the concentration of copper (II) by the quenching effect. Based on this fact, we established a fluorescence quenching method for the determination of copper (II). Under optimal conditions a linear range was found to be 0.5-50 ng/mL with a detection limit of 0.2 ng/mL. The method has been applied to determine copper (II) in foodstuff samples and the analytical results show good agreement with that obtained from atomic absorption spectrometry method. Copyright © 2015 Elsevier B.V. All rights reserved.

Multisensor system for determination of iron(II), iron(III) and uranium(VI) in complex solutions

International Nuclear Information System (INIS)

Legin, A.V.; Seleznev, B.L.; Rudnitskaya, A.M.; Vlasov, Yu.G.

1998-01-01

The aim of the present paper is the development and analytical evaluation of a multisensor system for determination of low content of iron(II), iron(III) and uranium(VI) in complex aqueous media. Sensor array included sensors on the basis of chalcogenide vitreous materials with redox and ionic cross-sensitivities, crystalline silver sulphide electrode, noble metal electrodes Pt, Au, Ag and redox sensor on the basis of oxide glass. Potentiometric measurements have been taken in a conventional electrochemical cell vs. a standard Ag/AgCl reference electrode. All measurements have been taken at room temperature. Calibration solutions contained UO 2 (NO 3 ) 2 in concentration range 10 -6 -1,610 -5 mol/L, K 3 Fe(CN) 6 and K 4 Fe(CN) 6 or FeSO 4 (NH 4 ) 2 SO 4 and FeCl 3 , with the ratio of Fe(II)/Fe(III) concentration from 100:1 to 1:100, the total concentration of Fe was 10 -4 and 10 -5 mol/L. All solutions have been made on the background electrolyte of calcium and magnesium chlorides and sulphates with the fixed content of 5-27 mmol/L of each component which is a typical one for groundwater or mining water. Sensor potentials have been processed by a back-propagation artificial neural net. Average error of determination of Fe(II) and Fe(III) is about 20 %, of uranium(VI) - 40 %. It was found that sensitivity of the sensor array to iron and uranium is irrespective of the chemical form of these species

Indirect complexometric determination of mercury(II in synthetic alloys and complexes using ethanethiol as a selective masking agent

Directory of Open Access Journals (Sweden)

J. KARTHIKEYAN

2006-03-01

Full Text Available Acomplexometric method for the determination of mercury(II in presence of other metal ions, based on the selective masking action of ethanethiol towards mercury(II is described. Mercury(II present in a given sample solution is first complexed with an excess of EDTAand the unreacted EDTAis titrated against zinc sulphate solution at pH 5–6 (hexamine buffer using xylenol orange as the indicator. An excess of a 0.3 % solution of ethanethiol is then added to displace EDTA from the Hg(II–EDTA complex. The released EDTAis titrated with a standard zinc sulphate solution. Reproducible and accurate results are obtained for 4–85 mg of mercury(II with a relative error of less than ± 0.46 % and coefficient of variation of not more than 0.47 %. The effects of the presence of various ions were studied. The method can be used for the analysis of mercury in its synthetic alloy mixtures and also in complexes.

Selective flotation-spectrophotometric determination of trace copper(II) in natural waters, human blood and drug samples using phenanthraquinone monophenylthiosemicarbazone.

Science.gov (United States)

Khalifa, M E; Akl, M A; Ghazy, S E

2001-06-01

Copper(II) forms 1:1 and 1:2 intense red complexes with phenanthraquinone monophenylthiosemicarbazone (PPT) at pH 3-3.5 and > or =6.5, respectively. These complexes exhibit maximal absorbance at 545 and 517 nm, the molar absorptivity being 2.3 x 10(4) and 4.8 x 10(4) l mol(-1) cm(-1), respectively. However, the 1:1 complex was quantitatively floated with oleic acid (HOL) surfactant in the pH range 4.5-5.5, providing a highly selective and sensitive procedure for the spectrophotometric determination of CuII. The molar absorptivity of the floated Cu-PPT complex was 1.5 x 10(5) l mol)(-1) cm(-1). Beer's law was obeyed over the range 3-400 ppb at 545 nm. The analytical parameters affecting the flotation process and hence the determination of copper traces were reported. Also, the structure of the isolated solid complex and the mechanism of flotation were suggested. Moreover, the procedure was successfully applied to the analysis of CuII in natural waters, serum blood and some drug samples.

Preparation and Spectral Properties of Mixed-Ligand Complexes of VO(IV, Ni(II, Zn(II, Pd(II, Cd(II and Pb(II with Dimethylglyoxime and N-acetylglycine

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Shayma A. Shaker

2010-01-01

Full Text Available A number of mixed-ligand complexes of the general formula [M(D(G] where D=dimethylglyoximato monoanion, G=N-acetylglycinato and M=VO(IV, Ni(II, Zn(II, Pd(II, Cd(II and Pb(II were prepared. Each complex was characterized by elemental analysis, determination of metal, infrared spectra, electronic spectra, (1H and 13C NMR spectra, conductivity and magnetic moments. All these complexes were not soluble in some of the organic solvent but highly soluble in dimethylformamide. The conductivity data showed the non-electrolytic nature of the complexes. The electronic spectra exhibited absorption bands in the visible region caused by the d-d electronic transition such as VO(IV, Ni(II and Pd(II. The IR and (1H, 13C NMR spectra which have indicate that the dimethylglyoxime was coordinated with the metal ions through the N and O atoms of the oxime group and N-acetylglycine was coordinated with metal ions through the N atom and terminal carboxyl oxygen atom.

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

Energy Technology Data Exchange (ETDEWEB)

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

2008-02-15

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

Clinical significance of determination of changes of serum IGF-II, IL-6, IL-8 and hs-CRP levels after treatment in pediatric patients with bronchopneumonia

International Nuclear Information System (INIS)

Wang Guanghui; Chen Chuanbing; Wang Xianwu

2009-01-01

Objective: To explore the clinical significance of changes of serum IGF-II, IL-6, IL-8 and hs-CRP levels after treatment in pediatric patients with bronchopneumonia. Methods: Serum IGF-II, IL-6, IL-8 (with RIA) and hs-CRP (with immunoturbidity method) levels were determined in 36 pediatric patients with bronchopneumonia both before and after treatment as well as in 35 controls. Results: Before treatment, serum IGF-II, IL-6, IL-8 and hs-CRP levels in the patients were significantly higher than those in the controls (P 0.05). Conclusion: Determination of serum IGF-II, IL-6, IL-8 and hs-CRP levels in pediatric patients with bronchopneumonia was important for diagnosis and outcome prediction. (authors)

A convenient method for determination of quizalofop-p-ethyl based on the fluorescence quenching of eosin Y in the presence of Pd(II)

Science.gov (United States)

Wu, Huan; Zhao, Yanmei; Tan, Xuanping; Zeng, Xiaoqing; Guo, Yuan; Yang, Jidong

2017-03-01

A convenient fluorescence quenching method for determination of Quizalofop-p-ethyl(Qpe) was proposed in this paper. Eosin Y(EY) is a red dye with strong green fluorescence (λex/λem = 519/540 nm). The interaction between EY, Pd(II) and Qpe was investigated by fluorescence spectroscopy, resonance Rayleigh scattering(RRS) and UV-Vis absorption. Based on changes in spectrum, Pd(II) associated with Qpe giving a positively charged chelate firstly, then reacted with EY through electrostatic and hydrophobic interaction formed ternary chelate could be demonstrated. Under optimum conditions, the fluorescence intensity of EY could be quenched by Qpe in the presence of Pd(II) and the RRS intensity had a remarkable enhancement, which was directly proportional to the Qpe concentration within a certain concentration range, respectively. Based on the fluorescence quenching of EY-Pd(II) system by Qpe, a novel, convenient and specific method for Qpe determination was developed. To our knowledge, this is the first fluorescence method for determination of Qpe was reported. The detection limit for Qpe was 20.3 ng/mL and the quantitative determination range was 0.04-1.0 μg/mL. The method was highly sensitive and had larger detection range compared to other methods. The influence of coexisting substances was investigated with good anti-interference ability. The new analytical method has been applied to determine of Qpe in real samples with satisfactory results.

Spectrophotometric determination of palladium (II) with rubeanic acid (RA) in presence of pyridine, piperidine and 3-picoline

International Nuclear Information System (INIS)

Hassiruzzaman, M.; Hossain, M.A.; Rahman, G.M.M.; Kamal, A.S.M.; Kabir, M.H.; Mustafa, A.I.

1999-01-01

Unpretentious and exclusive methods for the spectrophotometric determination of trace amount of divalent palladium (II) have been developed with rubeanic acid (dithio-oxamide) in presence of secondary ligands like pyridine, piperidine and 3-picoline. Both direct and extraction spectrophotometry showed that coloured rubeanates are only stable in acidic medium. The violent yellow coloured products are formed below ph 5.0 with an absorption maxima at 416.0 and 422.0 (pyridine), 405.0 and 416.5 (piperidine) and 418.0 and 422.0 (3-picoline) both in direct and isoamyl alcohol (IAA) extracted system, respectively. Results indicate that the highest sensitivity and molar absorptivity of Pd-RA pyridine system in direct spectrophotometry were 0.01497 mu g Pd(II) cm/sup -2/ and 7107.89 L mol sup -1/ cm/sup -1/ respectively. IAA extracted Pd-RA-piperidine system was found to give a sensitivity of 0.01087 mu g(Pd(II) cm /sup -2/ and molar absorptivity of 9788.80 L mol /sup -1/ cm/sup -1/ which were the highest of all the system. The effects due to variation of pH, reagent concentrations, order of addition of reagents, time, temperature and solvent media on the absorption spectra have been investigated and the optimum conditions determined. The effects of diverse ions and their tolerance limit have also been studies. (author)

Stability constants of glutarate complexes of copper(II), zinc(II), cobalt(II) and uranyl(II) by paper electrophoresis

International Nuclear Information System (INIS)

Singh, R.K.P.; Yadava, J.R.; Yadava, K.L.

1981-01-01

Stability constants of Copper(II), Zinc(II), Cobalt(II) and Uranyl(II) glutarates have been determined by paper electrophoresis. Glutaric acid (0.005 mol dmsup(-3)) was added to the background electrolyte : 0.1 mol dmsup(-3) HClO 4 . The proportions of (CH 2 ) 3 COOH COO - and (CH 2 ) 3 C 2 O 4 2- were varied by changing the pH of the electrolyte. These anions yielded the complexes Cu(CH 2 ) 3 C 2 O 4 , [Zn(CH 2 ) 3 COOH COO] + [Co(CH 2 ) 3 COOH COO] + and UO 2 (CH 2 ) 3 C 2 O 4 whose stability constants are found to be 10sup(3.9), 10sup(2.9), 10sup(2.7) and 10sup(13.5) respectively. (author)

Solvation structure determination of nickel(II) ion in six nitriles using extended X-ray absorption fine structure spectroscopy

International Nuclear Information System (INIS)

Inada, Yasuhiro; Funahashi, Shigenobu

1997-01-01

The solvation structures of the nickel(II) ion in six nitriles have been determined using X-ray absorption fine structure spectroscopy. The coordination number and the Ni-N bond length are 6 and 206.9 ± 0.6 pm in acetonitrile, 5.9 ± 0.2 and 206.9 ± 0.6 pm in propionitrile, 6.0 ± 0.2 and 206.8 ± 0.6 pm in butyronitrile, 6.0 ± 0.2 and 206.8 ± 0.6 pm in isobutyronitrile, 6.0 ± 0.2 and 206.8 ± 0.6 pm in valeronitrile, and 6.0 ± 0.2 and 206.5 ± 0.7 pm in benzonitrile, respectively. The structure parameters around the nickel(II) ion in all the nitriles are not affected by the bulkiness of the nitrile molecules. On the basis of the obtained structure parameters, we have discussed the structural characteristics around the nickel(II) ion with nitrogen and oxygen donor solvents and the reaction mechanisms for nitrile exchange on the nickel(II) ion. (author)

Extraction studies of Cd(II), Cu(II), Mn(II), Ni(II) and Zn(II) using N, N', N, N' -Bis((2-hydroxy-3,5-di-tert-butylbenzyl) (2-pyridylmethyl)) -ethylenediamine as a novel ligand

International Nuclear Information System (INIS)

Laus, R.; Anjos, A.D.; Naves, A.

2008-01-01

In the present study, the use of N,N',N,N'-bis((2-hydroxy-3,5-di-tert-butylbenzyl) (2- pyridylmethyl))-ethylenediamine (H2L) as ligand was evaluated in the liquid-liquid (water- chloroform) extraction of Cd(II), Cu(II), Mn(II), Ni(II) and Zn(II). Experiments were carried out to determine the pH for maximum extraction for each metal ion by ligand, maximum extraction capacity, extraction kinetics and extraction selectivity. The results revealed that the extraction of metal ions is dependent on the pH: maximum extraction maximum was obtained in the pH range of 4.5 - 6.0 for Cu(II) and 8.0 - 9.0 for Zn(II). Cd(II) and Mn(II) were best extracted at pH 9.0 and Ni(II) at 10.0. The ligand H2L was effective for the extraction of Cd(II), Cu(II) and Zn(II) (extraction efficient, %E equal 100%), whereas %E of 76% and 23.5% were observed for Mn(II) and Ni(II), respectively. The ligand presented high selectivity for the extraction of Cu(II) at pH 4.0. (author)

Synthesis and biodistribution of 18F-labeled fluoronitroimidazoles: Potential in vivo markers of hypoxic tissue

International Nuclear Information System (INIS)

Jerabek, P.A.; Kilbourn, M.R.; Dischino, D.D.; Welch, M.J.; Patrick, T.B.; Southern Illinois University, Edwardsville

1986-01-01

Three 18 F labeled fluoronitroimidazoles have been prepared as potential in vivo markers of hypoxic cells in tumors, and ischemic areas of the heart and brain. 1-(2-Nitroimidazolyl)-3-[ 18 F]fluoro-2-hydroxy-propanol ([ 18 F]fluoro-normethoxymisonidazole 4, 1-(2-[ 18 F]fluoroethyl)-2-nitroimidazole 7, and 1-(2-[ 18 F]-fluoroethyl)-2-methyl-5-nitromidazole ([ 18 F]fluoro-norhydroxymetronidazole) 10 were prepared in average radiochemical yields of 18 F labeled fluoronitroimidazoles. At 1 and 3 h after administration, the tissue distribution of each of the 18 F labeled nitroimidazoles was quite uniform and consistent with that of nitroimidazoles previously studied. These results suggest the need for a suitable animal model to evaluate their potential as in vivo markers of hypoxic tissue in the brain. (author)

Synthesis and Voltammetric Determination of Pb(II Using a ZIF-8-Based Electrode

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Dinh Quang Khieu

2018-01-01

Full Text Available Zeolite imidazole framework-8 (ZIF-8 was prepared by the hydrothermal process. The obtained ZIF-8 was a characteristic of X-ray-diffraction (XRD, transmission electron microscope (TEM, thermal gravity-differential thermal analysis (TG-DTA, and dynamic light scattering (DLS. The obtained ZIF-8 possessed large specific area and was highly dispersed. Its morphology consisted of nanospherical particles with 30–50 nm in diameter. Chemical stability of ZIF-8 in different conditions was studied. The ZIF-8 was used as an electrode modifier for the determination of trace levels of lead. The parameters including solvents and solution pH were investigated. The repeatability, reproducibility, accuracy, linear range, limit of detection, and limit of quantitation were also addressed. The results showed that ZIF-8 is a potential electrode modifier for differential pulse anodic stripping method to determine Pb(II in aqueous solution.

Experimental and numerical determination of the dynamic properties of the reactor building of Atucha II NPP

International Nuclear Information System (INIS)

Ceballos, M.A.; Car, E.J.; Prato, T.A.; Prato, C.A.; Alvarez, L.M.; Godoy, A.R.

1995-01-01

Determination of the dynamic properties of the reactor building of Atucha II NPP is carried out in order to: i) Obtain valuable information for seismic qualification of the plant, and ii) Assess some procedures for testing and analysis that are used in the process of seismic evaluation of existing nuclear facilities founded on Quaternary soil deposits. Both steady state and impulsive dynamic tests were performed but attention is centered here in tile techniques used to determine natural frequencies and modal damping ratios with impulsive tests. Numerical analyses were performed by means of a 3-D model model of the superstructure together with foundation stiffness coefficients derived in a separate paper from steady state vibration tests, and also from analysis with a 2-D F.E. model of the soil layers capable of approximating the 3-D features of the problem. The computed foundation stiffness coefficients are compared both with those obtained from the tests and from an axisymmetric F.E. model; results indicate that foundation stiffness coefficients calculated with F.E. models with soil parameters given by laboratory tests performed on cored samples are significantly lower than those given by the steady state vibration tests. (author)

Application of 1- (3,4-dimenthylphenyl)-dodecanedione-1,2-dioxime (MFDDO) to substoichiometris extraction and determination of nickel(II) by the isotope dilution method

Energy Technology Data Exchange (ETDEWEB)

Gorski, Z.; Goraczko, W. [Technical University Poznan, Poznan (Poland). Radio and Photo Chemistry Department

1997-10-01

The conditions for use of 1-3,4-dimenthylphenyl-dodecanedione-1,2-dioxime (MFDDO) in toluene solution for substoichiometric extraction of Ni(II) from aqueous phases are described. This procedure allows the determination of 0.006-0.06 g/ml of nickel(II) in human urine and blood`s serum samples by the isotope dilution method using {sup 63}Ni(II) 9 refs., 5 figs.

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

International Nuclear Information System (INIS)

Soylak, Mustafa; Cay, Rukiye Sungur

2007-01-01

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

A dip-and-read test strip for the determination of mercury(II) ion in aqueous samples based on urease activity inhibition.

Science.gov (United States)

Shi, Guo-Qing; Jiang, Guibin

2002-11-01

A sensitive dip-and-read test strip for the determination of mercury in aqueous samples based on the inhibition of urease reaction by the ion has been developed. The strip has a circular sensing zone that containing two layers: the top layer is a cellulose acetate membrane where urease is immobilized on it; the bottom layer is a pH indicator wafer that is impregnated with urea. The principle of the measurement is based on the disappearance of a yellow spot on the pH indicator wafer. The elapsing time until the disappearance of the spot which depends on the concentration of mercury(II) ion is measured with a stopwatch. Under the experimental conditions, as low as 0.2 ng/ml mercury can be observed with the detection range from 0.2 to 200 ng/ml in water. Organomercury compounds give essentially the same response as inorganic mercury. Heavy-metal ions such as Ag(I), Cu(II), Cd(II), Ni(II), Zn(II), and Pb(II) as well as other sample matrixes basically do not interfere with the mercury measurement.

Effects of imidazole derivatives in the survival of 60Co irradiated mice

International Nuclear Information System (INIS)

Villavicencio, A.L.C.H.; Mastro, N.L. del.

1988-07-01

The presence of hypoxic and radioresistant cells is considered the main reason of failure in radiotherapy of neoplasms. Hypoxic cell radiosensitizers, as nitroimidazole derivatives, have an advantage over other alternative methods for improving the effects of radiotherapy since hypoxic cells exist in considerable concentration in tumours and only in small concentration in normal tissues. Its show also a direct cytotoxicity over the hypoxic cell population. In this work, studies on combining ip administered drugs and single dose radiation treatments in healthy albino mice are presented. It was compared the action of 2-nitroimidazole, levamisole and cysteine, the latest considered as radioprotector for several biological systems. The results showed some radioprotective action for 2 - nitroimidazole (MISO), sensitizer capacity for levamisole and in those conditions, cysteine failed to produce any effects on the survival of 9 Gy 60 Co irradiated mice. (author) [pt

Boron doped diamond sensor for sensitive determination of metronidazole: Mechanistic and analytical study by cyclic voltammetry and square wave voltammetry

International Nuclear Information System (INIS)

Ammar, Hafedh Belhadj; Brahim, Mabrouk Ben; Abdelhédi, Ridha; Samet, Youssef

2016-01-01

The performance of boron-doped diamond (BDD) electrode for the detection of metronidazole (MTZ) as the most important drug of the group of 5-nitroimidazole was proven using cyclic voltammetry (CV) and square wave voltammetry (SWV) techniques. A comparison study between BDD, glassy carbon and silver electrodes on the electrochemical response was carried out. The process is pH-dependent. In neutral and alkaline media, one irreversible reduction peak related to the hydroxylamine derivative formation was registered, involving a total of four electrons. In acidic medium, a prepeak appears probably related to the adsorption affinity of hydroxylamine at the electrode surface. The BDD electrode showed higher sensitivity and reproducibility analytical response, compared with the other electrodes. The higher reduction peak current was registered at pH 11. Under optimal conditions, a linear analytical curve was obtained for the MTZ concentration in the range of 0.2–4.2 μmol L"−"1, with a detection limit of 0.065 μmol L"−"1. - Highlights: • SWV for the determination of MTZ • Boron-doped diamond as a new electrochemical sensor • Simple and rapid detection of MTZ • Efficiency of BDD for sensitive determination of MTZ

Solid phase selective separation and preconcentration of Cu(II) by Cu(II)-imprinted polymethacrylic microbeads.

Science.gov (United States)

Dakova, Ivanka; Karadjova, Irina; Ivanov, Ivo; Georgieva, Ventsislava; Evtimova, Bisera; Georgiev, George

2007-02-12

Ion-imprinted polymer (IIP) particles are prepared by copolymerization of methacrylic acid as monomer, trimethylolpropane trimethacrylate as crosslinking agent and 2,2'-azo-bis-isobutyronitrile as initiator in the presence of Cu(II), a Cu(II)-4-(2-pyridylazo)resorcinol (Cu(II)-PAR) complex, and PAR only. A batch procedure is used for the determination of the characteristics of the Cu(II) solid phase extraction from the IIP produced. The results obtained show that the Cu(II)-PAR IIP has the greatest adsorption capacity (37.4 micromol g(-1) of dry copolymer) among the IIPs investigated. The optimal pH value for the quantitative preconcentration is 7, and full desorption is achieved by 1 M HNO(3). The selectivity coefficients (S(Cu/Me)) for Me=Ni(II), Co(II) are 45.0 and 38.5, respectively. It is established that Cu(II)-PAR IIPs can be used repeatedly without a considerable adsorption capacity loss. The determination of Cu(II) ions in seawater shows that the interfering matrix does not influence the preconcentration and selectivity values of the Cu(II)-PAR IIPs. The detection and quantification limits are 0.001 micromol L(-1) (3sigma) and 0.003 micromol L(-1) (6sigma), respectively.

New method for simultaneous determination of Fe(II) and Fe(III) in water using flow injection technique

International Nuclear Information System (INIS)

Kozak, J.; Gutowski, J.; Kozak, M.; Wieczorek, M.; Koscielniak, P.

2010-01-01

The method exploits the possibilities of flow injection gradient titration in a system of reversed flow with spectrophotometric detection. In the developed approach a small amount of titrant (EDTA) is injected into a stream of sample containing a mixture of indicators (sulfosalicylic acid and 1,10-phenanthroline). In acid environment sulfosalicylic acid forms a complex with Fe(III), whereas 1,10-phenanthroline forms a complex with Fe(II). Measurements are performed at wavelength λ = 530 nm when radiation is absorbed by both complexes. After injection EDTA replaces sulfosalicylic acid and forms with Fe(III) more stable colourless complex. As a result, a characteristic 'cut off' peak is registered with a width corresponding to the Fe(III) concentration and with a height corresponding to the Fe(II) concentration. Calibration was performed by titration of four two-component standard solutions of the Fe(II)/Fe(III) concentrations established in accordance with 2 2 factorial plan. The method was tested with the use of synthetic samples and then it was applied to the analysis of water samples taken from artesian wells. Under optimized experimental conditions Fe(II) and Fe(III) were determined with precision less than 0.8 and 2.5% (RSD) and accuracy less than 3.2 and 5.1% (relative error) within the concentration ranges of 0.1-3.0 and 0.9-3.5 mg L -1 of both analytes, respectively.

Flow injection determination of hydrogen peroxide using catalytic effect of cobalt(II) ion on a dye formation reaction.

Science.gov (United States)

Kurihara, Makoto; Muramatsu, Miyuki; Yamada, Mari; Kitamura, Naoya

2012-07-15

A novel flow injection photometric method was developed for the determination of hydrogen peroxide in rainwater. This method is based on a cobalt(II)-catalyzed oxidative coupling of 3-methyl-2-benzothiazolinone hydrazone (MBTH) with N-ethyl-N-(2-hydroxy-3-sulfopropyl)-3,5-dimethoxyaniline (DAOS) as a modified Trinder's reagent to produce intensely colored dye (λ(max)=530nm) in the presence of hydrogen peroxide at pH 8.4. In this method, 1,2-dihydroxy-3,5-benzenedisulfonic acid (Tiron) acted as an activator for the cobalt(II)-catalyzed reaction and effectively increased the peak height for hydrogen peroxide. The linear calibration graphs were obtained in the hydrogen peroxide concentration range 5×10(-8) to 2.2×10(-6)mol dm(-3) at a sampling rate of 20h(-1). The relative standard deviations for ten determinations of 2.2×10(-6) and 2×10(-7)mol dm(-3) hydrogen peroxide were 1.1% and 3.7%, respectively. The proposed method was successfully applied to the determination of hydrogen peroxide in rainwater samples and the analytical results agreed fairly well with the results obtained by different two reference methods; peroxidase method and hydrogen peroxide electrode method. Copyright © 2012 Elsevier B.V. All rights reserved.

Clinical significance of determination of changes of serum IGF-II, IL-6, IL-8, TNF-α levels after treatment in children with bronchopneumonia

International Nuclear Information System (INIS)

Feng Yue

2011-01-01

Objective: To explore the clinical significance of changes of serum IGF-II, IL-6, IL-8 and TNF-α levels after treatment in children with bronchopneumonia. Methods: Serum IGF-II, IL-6, IL-8 and TNF-α levels with RIA were detected both before and after treatment in 33 patients with children bronchopneumonia as well as in 35 controls. Results: Before treatment, serum IGF-II, IL-6, IL-8 and TNF-α levels were significantly higher in the patients than those in the controls (P 0.05). Conclusions: Serum IGF-II, IL-6, IL-8 and TNF-α could take part in the pathogenesis of children bronchopneumonia in various ways and determination of these levels was clinically important. (authors)

Fluorometric determination of aluminium (III) and cadmium (II) by solvent extraction of the ternary complex composed of metal ion, 8-hydroxy-5-quinolinesulfonic acid, and methyltrioctylammonium ion

International Nuclear Information System (INIS)

Kondoh, Yukihiro; Kataoka, Masamitsu; Kambara, Tomihito

1982-01-01

A fluorometric micro determination of aluminium (III) and cadmium (II) using the formation of metal-8-hydroxy-5-quinolinesulfonic acid-capriquat (methyltrioctylammonium) ternary complex is described. These complexes are easily extracted into chloroform phase and the extract emits a strong fluorescence. Spectra of aluminium (III) and cadmium (II) ternary complexes have the excitation maximum at 396 nm and 400 nm, and emission maximum at 501 nm and 524 nm, respectively. Fluorescence intensity of the aluminium (III) and cadmium (II) ternary complexes extracted into chloroform showed the constant and maximum values in the pH range of aqueous phase from 5.3 to 8.5 and 8.1 to 8.5, respectively. The calibration curves for aluminium (III) and cadmium (II) show good proportionality int the concentration range from 0.5 to 5.0 and 1.0 to 50.0 μg, respectively. The relative standard deviation observed with four measurements was found to be 1.8% for 0.5 μg of aluminium (III) and 1.1% for 10.0 μg of cadmium (II). The effect of diverse ions is studied and a 25-fold amount of Cu(II), Ni(II), Fe(II), Fe(III) in weight gave errors, however, the interferences were easily eliminated by the addition of appropriate masking agent. In the determination of cadmium (II), an equal amount of Co(II), Ni(II), Mn(II), Fe(III) and twice amount of Al(III) gave negative errors, however, the interference of Fe(III) and Al(III) were also eliminated as above. (author)

Novel zinc(II)phthalocyanines bearing azo-containing schiff base: Determination of pKa values, absorption, emission, enzyme inhibition and photochemical properties

Science.gov (United States)

Kantar, Cihan; Mavi, Vildan; Baltaş, Nimet; İslamoğlu, Fatih; Şaşmaz, Selami

2016-10-01

Azo-containing schiff bases are well known and there are many studies about their various properties in literature. However, phthalocyanines bearing azo-containing schiff bases, their spectral, analytical and biological properties are unknown. Therefore, new zinc (II) phthalocyanines bearing azo-containing schiff base were synthesized and investigated to determine pKa values, absorption, emission, enzyme inhibition and photochemical properties. Emission spectra were reported and large Stokes shift values were determined for all compounds, indicating that all molecules exhibit excited state intramolecular proton transfer. These phthalocyanines were the first examples of phthalocyanine showing excited state intramolecular proton transfer. Singlet oxygen quantum yields of zinc (II) phthalocyanines were determined. pKa values and indicator properties of all compounds were investigated by potentiometry. All compounds were assayed for inhibitory activity against bovine milk xanthine oxidase and acetylcholinesterase enzyme in vitro. Compound 2 showed the high inhibitory effect against xanthine oxidase (IC50 = 0.24 ± 0.01 μM). However, phthalocyanine compounds did not show enzyme inhibitor behavior.

Spectrophotometric Determination of Iron(II after Solid Phase Extraction of Its 2,2′ Bipyridine Complex on Silica Gel-Polyethylene Glycol

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Nahid Pourreza

2013-01-01

Full Text Available A new solid phase extraction procedure was developed for preconcentration of iron(II using silica gel-polyethylene glycol (silica-PEG as an adsorbent. The method is based on retention of iron(II as 2,2′ bipyridine complex on silica-PEG. The retained complex is eluted by 1.0 mol L−1 of sulfuric acid-acetone mixture (1:2 and its absorbance is measured at 518 nm, spectrophotometrically. The effects of different parameters such as pH, concentration of the reagent, eluting reagent, sample volume, amount of adsorbent, and interfering ions were investigated. The calibration graph was linear in the range of 1–60 ng mL−1 of iron(II. The limit of detection based on 3Sb was 0.57 ng mL−1 and relative standard deviations (R.S.D for ten replicate measurements of 12 and 42 ng mL−1 of iron(II were 2.4 and 1.7%, respectively. The method was applied to the determination of of iron(II in water, multivitamin tablet, and spinach samples.

Chelation of Cu(II, Zn(II, and Fe(II by Tannin Constituents of Selected Edible Nuts

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Magdalena Karamać

2009-12-01

Full Text Available The tannin fractions isolated from hazelnuts, walnuts and almonds were characterised by colorimetric assays and by an SE-HPLC technique. The complexation of Cu(II and Zn(II was determined by the reaction with tetramethylmurexide, whereas for Fe(II, ferrozine was employed. The walnut tannins exhibited a significantly weaker reaction with the vanillin/HCl reagent than hazelnut and almond tannins, but the protein precipitation capacity of the walnut fraction was high. The SE-HPLC chromatogram of the tannin fraction from hazelnuts revealed the presence of oligomers with higher molecular weights compared to that of almonds. Copper ions were most effectively chelated by the constituents of the tannin fractions of hazelnuts, walnuts and almonds. At a 0.2 mg/assay addition level, the walnut tannins complexed almost 100% Cu(II. The Fe(II complexation capacities of the tannin fractions of walnuts and hazelnuts were weaker in comparison to that of the almond tannin fraction, which at a 2.5 mg/assay addition level, bound Fe(II by ~90%. The capacity to chelate Zn(II was quite varied for the different nut tannin fractions: almond tannins bound as much as 84% Zn(II, whereas the value for walnut tannins was only 8.7%; and for hazelnut tannins, no Zn(II chelation took place at the levels tested.

Voltammetric determination of sudan ii in food samples at graphene modified glassy carbon electrode based on the enhancement effect of sodium dodecyl sulfate

International Nuclear Information System (INIS)

Ma, X.; Chen, M.; Chao, M.

2013-01-01

Summary: Herein, a novel electrochemical method was de veloped for the determination of Sudan II based on the electrochemical catalytic activity of graphene modified glassy carbon electrode (GME) and the enhancement effect of sodium dodecyl sulfate (SDS). In a pH 6.0 phosphate buffer solution, Sudan II exhibited a pair of well-defined quasi reversible redox peaks at the GME in the presence of 5.0x10/sup -5/ mol L/sup 1/ SDS. The oxidation peak current of Sudan II was linearly proportional to its concentration in a range from 4.0x10/sup -8/ to 4.0x10/sup -6/ mol L/sup 1/, with a linear regression equation of ipa (A) = 3.35 c + 5.96 x 10/sup -6/, r = 0.9988 and a detection limit of 8.0x10/sup -9/ mol L/sup 1/. The recoveries from the standards fortified blank samples were in the range of 94.7% to 97.5% with RSD lower than 4.0%. The novel method has been successfully used to determine Sudan II in food products with satisfactory results. (author)

Determination of mixed stability constants of lead(II/uranyl(II-NTA-cysteine complexes by paper electrophoresis

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Brij Bhushan Tewari

2005-12-01

Full Text Available A method involving the use of paper ionophoresis is described for the study of equilibria in mixed – ligand complex systems in solution. The technique is based on the movement of a spot of metal ion under an electric field with the complexants added to the background electrolyte at pH 8.5. The stability constants of the complexes Pb(II – nitrilotriacetate – cysteine and UO2(II – nitrilotriacetate – cysteine are found to be 5.35 plus or minus 0.02 and 6.27 plus or minus 0.07 (logarithm of stability constant values at ionic strength 0.1 M and a temperature of 35 0C.

Experimental and molecular docking investigation on metal-organic framework MIL-101(Cr) as a sorbent for vortex assisted dispersive micro-solid-phase extraction of trace 5-nitroimidazole residues in environmental water samples prior to UPLC-MS/MS analysis.

Science.gov (United States)

Lu, Nan; Wang, Ting; Zhao, Pan; Zhang, Lianjun; Lun, Xiaowen; Zhang, Xueli; Hou, Xiaohong

2016-11-01

In the presented work, metal-organic framework (MOF) material MIL-101(Cr) (MIL, Matérial Institute Lavoisier) was used as a sorbent for vortex assisted dispersive micro-solid-phase extraction (VA-D-μ-SPE) of trace amount of metronidazole (MNZ), ronidazole (RNZ), secnidazole (SNZ), dimetridazole (DMZ), tinidazole (TNZ), and ornidazole (ONZ) in different environmental water samples. Ultra-high-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS) was used to quantify the target analytes. The extraction conditions, including type of sorbents, amount of MIL-101(Cr), solution pH, extraction method, extraction time, effect of salt, and elution conditions were investigated. Upon the optimal conditions, the developed method showed an excellent extraction performance with the average recovery ranging from 75.2 to 98.8 %. Good sensitivity levels were achieved with the detection limits of 0.03∼0.06 μg/L and the quantitation limits of 0.09∼0.20 μg/L. The linear ranges were varied from 0.1 to 20 for SNZ and ONZ and from 0.2 to 40 μg/L for MNZ, RNZ, DMZ, and TNZ (r 2  > 0.992), and repeatability of the method was satisfactory with the relative standard deviations (RSD) extraction and determination of 5-nitroimidazoles (5-NDZs) in 12 real water samples, showing the positive findings of MNZ and TNZ ranging from 0.3 to 1.0 μg/L. Furthermore, molecular docking was applied to explain the molecular interactions and free binding energies between MIL-101(Cr) and 5-NDZs, providing a deep insight into the adsorption mechanism. The proposed method exhibited the advantages of simplicity, rapidly, less solvent consumption, ease of operation, higher sensitivity, and lower matrix effect. Graphical abstract Schematic diagram of the extraction process and molecular docking investigation.

Initial results of hypoxia imaging using 1-α-d-(5-deoxy-5-[18F]-fluoroarabinofuranosyl)-2-nitroimidazole (18F-FAZA)

International Nuclear Information System (INIS)

Postema, Ernst J.; McEwan, Alexander J.B.; Riauka, Terence A.; Kumar, Piyush; Richmond, Dacia A.; Abrams, Douglas N.; Wiebe, Leonard I.

2009-01-01

Tumour hypoxia is thought to play a significant role in the outcome of solid tumour therapy. Positron emission tomography (PET) is the best-validated noninvasive technique able to demonstrate the presence of hypoxia in vivo. The locally developed PET tracer for imaging hypoxia, 1-α-d-(5-deoxy-5-[ 18 F]-fluoroarabinofuranosyl)-2-nitroimidazole ( 18 F-FAZA), has been shown to accumulate in experimental models of tumour hypoxia and to clear rapidly from the circulation and nonhypoxic tissues. The safety and general biodistribution patterns of this radiopharmaceutical in patients with squamous cell carcinoma of the head and neck (HNSCC), small-cell lung cancer (SCLC) or non-small-cell lung cancer (NSCLC), malignant lymphoma, and high-grade gliomas, were demonstrated in this study. Patients with known primary or suspected metastatic HNSCC, SCLC or NSCLC, malignant lymphoma or high-grade gliomas were dosed with 5.2 MBq/kg of 18 F-FAZA, then scanned 2-3 h after injection using a PET or PET/CT scanner. Images were interpreted by three experienced nuclear medicine physicians. The location and relative uptake scores (graded 0 to 4) of normal and abnormal 18 F-FAZA biodistribution patterns, the calculated tumour-to-background (T/B) ratio, and the maximum standardized uptake value were recorded. Included in the study were 50 patients (32 men, 18 women). All seven patients with high-grade gliomas showed very high uptake of 18 F-FAZA in the primary tumour. In six out of nine patients with HNSCC, clear uptake of 18 F-FAZA was observed in the primary tumour and/or the lymph nodes in the neck. Of the 21 lymphoma patients (15 with non-Hodgkin's lymphoma and 6 with Hodgkin's disease), 3 demonstrated moderate lymphoma-related uptake. Of the 13 lung cancer patients (12 NSCLC, 1 SCLC), 7 had increased 18 F-FAZA uptake in the primary lung tumour. No side effects of the administration of 18 F-FAZA were observed. This study suggests that 18 F-FAZA may be a very useful radiopharmaceutical

Dynamic adsorption of mixtures of Rhodamine B, Pb (II), Cu (II) and Zn(II) ions on composites chitosan-silica-polyethylene glycol membrane

Science.gov (United States)

Mahatmanti, F. W.; Rengga, W. D. P.; Kusumastuti, E.; Nuryono

2018-04-01

The adsorption of a solution mixture of Rhodamine B, Pb (II), Cu (II) and Zn(II) was studied using dynamic methods employing chitosan-silica-polyethylene glycol (Ch/Si/P) composite membrane as an adsorptive membrane. The composite Ch/Si/P membrane was prepared by mixing a chitosan-based membrane with silica isolated from rice husk ash (ASP) and polyethylene glycol (PEG) as a plasticizer. The resultant composite membrane was a stronger and more flexible membrane than the original chitosan-based membrane as indicated by the maximum percentage of elongation (20.5 %) and minimum Young’s Modulus (80.5 MPa). The composite membrane also showed increased mechanical and hydrophilic properties compared to the chitosan membranes. The membrane was used as adsorption membrane for Pb (II), Cu (II), Cd (II) ions and Rhodamine B dyes in a dynamic system where the permeation and selectivity were determined. The permeation of the components was observed to be in the following order: Rhodamine B > Cd (II) > Pb (II) > Cu (II) whereas the selectivity was shown to decrease the order of Cu (II) > Pb (II) > Cd (II) > Rhodamine B.

Selective separation, preconcentration and determination of Pd(II ions in environmental samples by coprecipitation with a 1,2,4-triazole derivative

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D. Ozdes

2015-01-01

Full Text Available A simple, sensitive, facile and low cost methodology, combined with flame atomic absorption spectrometry (FAAS, was employed to evaluate the selective separation and preconcentration of Pd(II ions in environmental samples by using a triazole derivative as an organic coprecipitating agent without a carrier element. The developed method was systematically investigated in different set of experimental parameters that influence the quantitative recovery of Pd(II ions. The accuracy of the method was tested by analyzing certified reference material and spike tests. The developed coprecipitation procedure has been applied to road dust, anodic slime, industrial electronic waste materials and water samples to determine their Pd(II levels. DOI: http://dx.doi.org/10.4314/bcse.v29i1.1

Application of Box-Behnken designs in parameters optimization of differential pulse anodic stripping voltammetry for lead(II) determination in two electrolytes.

Science.gov (United States)

Yu, Xiao-Lan; He, Yong

2017-06-05

Box-Behnken design was advantageous to parameters optimization of differential pulse anodic stripping voltammetry (DPASV) for the analysis of lead(II) with its high efficiency and accuracy. Five Box-Behnken designs were designed and conducted in the electrolyte of 0.1 mol/L acetate buffer and 0.1 mol/L HCl without the removal of oxygen. Significant parameters and interactions in each electrolyte were found (P-value Box-Behnken designs in parameters optimization of DPASV for lead(II) determination regardless of the electrolyte kinds.

Determination of activities of human carbonic anhydrase II inhibitors ...

African Journals Online (AJOL)

the esterase activity of CA-II using 4-NPA as a substrate in 96-well plates. Dimethyl sulfoxide was used ... intensive search for novel drugs is ongoing, through synthesis of new ..... License (http://creativecommons.org/licenses/by/. 4.0) and the ...

Determination of plutonium by secondary coulometric titration with internally generated iron(II) Pt. 2

International Nuclear Information System (INIS)

Chitnis, R.T.; Talnikar, S.G.; Thakur, V.A.; Paranjape, A.H.

1979-01-01

Determination of plutonium by secondary coulometry involving the controlled potential technique for the generation of an iron(II) mediator, is reported in Part I. In this paper, the same determination is reported using constant current coulometry for the generation of the mediator, and zero current potentiometry for end-point detection. The factors affecting the current efficiency, viz. current density and supporting electrolyte composition have been checked in order to define the appropriate conditions for obtaining 100% current efficiency. The original method of Carson et al. suffers from the disadvantage that it involves complicated sample treatment. Introduction of perchloric acid treatment as a method for the oxidation of plutonium and the pretitration of the supporting electrolyte to the end-point potential prior to sample addition, have considerably helped to improve the precision and accuracy of the method. Exhaustive analytical data are reported covering plutonium quantities ranging from 25 micrograms to 5 milligrams, which establishes the scope of the method. (author)

Determination of lead in water by electrothermal atomic absorption spectrometry with a nickel(II)-ammonium tartrate modifier

International Nuclear Information System (INIS)

Sekerka, I.; Lechner, J.F.

1991-01-01

A method is described for the determination of low concentrations of lead in water samples. Atomic absorption spectrometry is used with a tungsten ribbon furnace and Zeeman background correction. Interferences are eliminated by the addition of ammonium tartrate and nickel(II) nitrate to the samples to act as a matrix modifier and adjust the pH. The results show the superior performance of this modifier over other types used conventionally. The detection limit is 1 μg l -1 relative standard deviation of -1 can be obtained. The instrumentation is simple and the method is efficient for the determination of lead in various water samples. 25 refs.; 7 figs.; 6 tabs

Clinical significance of determination of changes of serum NSE, IGF-II and TNF-α levels after chemotherapy in patients with lung cancer

International Nuclear Information System (INIS)

Ji Yajun; Yang Chengxi; Bian Baoxiang; Song Ziyan

2008-01-01

Objective: To detect the changes of serum NSE, IGF-II and TNF-α levels after chemotherapy in patients with lung cancer. Methods: Serum NSE, IGF-II and TNF-α levels were determined with RIA in 38 patients with lung cancer both be- fore and after chemotherapy as well as in 35 controls. Results: Before chemotherapy, serum NSE, IGF-II and TNF-α levels in the patients were significantly higher than those in the controls (P<0.01), After chemotherapy, in 25 cases without recurrence at 6 months, the levels were remained dropped markedly and approached those in controls. However in the 5 patients with recurrence, the levels increased again, approaching those before chemotherapy. Conclusion: Serum levels of NSE, IGF-II and TNF-α might be useful for diagnosis and predicting therapeutic effects after chemotherapy in patients with lung cancer. (authors)

Biosorption characteristics of copper (II), chromium (III), nickel (II), and lead (II) from aqueous solutions by Chara sp. and Cladophora sp.

Science.gov (United States)

Elmaci, Ayşe; Yonar, Taner; Ozengin, Nihan

2007-09-01

The aim of this research was to expose individual removals of copper, chromium, nickel, and lead from aqueous solutions via biosorption using nonliving algae species, Chara sp. and Cladophora sp. Optimum pH values for biosorption of copper (II), chromium (III), nickel (II), and lead (II) from aqueous solutions were determined to be 6, 7, 7, and 3 for Cladophora sp. and 5, 3, 5, and 4 for Chara sp. respectively. Maximum adsorption capacities of Chara sp. [10.54 for chromium (III) and 61.72 for lead (II)] and Cladophora sp. [6.59 for chromium (III) and 16.75 and 23.25 for lead (II)] for chromium (III) and lead (II) are similar. On the other hand, copper (II) and nickel (II) biosorption capacity of Cladophora sp. [14.28 for copper (II) and 16.75 for nickel (II)] is greater than Chara sp. [6.506 for copper (II) and 11.76 for nickel (II)]. Significantly high correlation coefficients indicated for the Langmuir adsorption isotherm models can be used to describe the equilibrium behavior of copper, chromium, nickel, and lead adsorption onto Cladophora sp. and Chara sp.

Synthesis and characterization of aspartic acid-capped CdS/ZnS quantum dots in reverse micelles and its application to Hg(II) determination

Energy Technology Data Exchange (ETDEWEB)

Hosseini, Mohammad Saeid, E-mail: mshosseini1336@yahoo.com; Kamali, Mohsen

2015-11-15

In this work, CdS/ZnS quantum dots (QDs) coated with aspartic acid (AsA) were synthesized in reverse micelles. The synthesized QDs were characterized by XRD, TEM, IR and photoluminescence (PL) spectroscopy. It was found that the intensity of CdS/ZnS QDs coated with AsA is much greater than CdS, and CdS/ZnS QDs. The interaction of some heavy metal ions with CdS/ZnS/AsA QDs was investigated at different buffering pH media. Based on the PL quenching of the QDs in the presence of each one of the metal ions, the feasibility of their determinations was examined according to the Stern–Volmer equation. The investigations showed that Hg(II) ions can be easily determined in contaminated atmospheric environments with the detection limit of 0.05 mg m{sup −3}. The results were satisfactorily confirmed by cold vapor atomic absorption spectrometric method. - Highlights: • A new CdS/ZnS quantum dot capped with aspartic acid (DDBA) was prepared. • The prepared QDs benefit from a favorable fluorescence. • Interaction of some metal ions with the QDs was examined according to the Stern–Volmer equation. • The determination of Hg(II) is feasible in the present of many co-existence metal ions. • The method benefits from a high-speed and considerable simplicity for Hg(II) determination.

Clinical significance of determination of serum NSE and plasma ET, IGF-II, CNP levels in patients with acute brain injury

International Nuclear Information System (INIS)

Chen Bo

2010-01-01

Objective: To investigate the clinical significance of changes of plasma ET, IGF-II, CNP and serum NSE contents in patients with acute brain injury. Methods: Serum contents of neuron specific enolase (NSE) were measured with chemiluminescence immunoassay and plasma endothelin (ET), insulin-like growth factor-II (IGF-II) and C-type natriuretic peptide (CNP) were measured with radioimmunoassay in 30 patients with acute brain injury and 35 controls. Results: Serum contents of NSE and plasma IGF-II, CNP were not much different in patients with mild brain injury from those in controls (P >0.05), but plasma contents of ET were already significantly higher in patients with mild brain injury than those in controls(P < 0.01). The serum NSE and plasma ET levels in patients with moderate and severe brain injury were significantly higher than those in patients with mild brain injury and controls (P < 0.01). Decrease of plasma levels of IGF-II and CNP was not significant in patients with mild brain injury (vs controls). However, the plasma levels of IGF-II and CNP were significantly lower in patients with moderate and severe brain injury than those in patients with mild brain injury and controls (P <0.01). As a whole, the magnitude of changes of these parameters was proportional to the severity of the injury. Conclusion: Changes of serum NSE and plasma IGF-II, ET and CNP levels were closely related to the pathological process of brain injury. Determination of these parameters was of clinical importance for evaluation of the severity of injury and outcome prediction. (authors)

Nuclear fuel technology - Determination of uranium in solutions, uranium hexafluoride and solids - Part 2: Iron(II) reduction/cerium(IV) oxidation titrimetric method

International Nuclear Information System (INIS)

2004-01-01

This first edition of ISO 7097-1 together with ISO 7097-2:2004 cancels and replaces ISO 7097:1983, which has been technically revised, and ISO 9989:1996. ISO 7097 consists of the following parts, under the general title Nuclear fuel technology - Determination of uranium in solutions, uranium hexafluoride and solids: Part 1: Iron(II) reduction/potassium dichromate oxidation titrimetric method; Part 2: Iron(II) reduction/cerium(IV) oxidation titrimetric method. This part 2. of ISO 7097 describes procedures for determination of uranium in solutions, uranium hexafluoride and solids. The procedures described in the two independent parts of this International Standard are similar: this part uses a titration with cerium(IV) and ISO 7097-1 uses a titration with potassium dichromate

Nuclear fuel technology - Determination of uranium in solutions, uranium hexafluoride and solids - Part 1: Iron(II) reduction/potassium dichromate oxidation titrimetric method

International Nuclear Information System (INIS)

2004-01-01

This first edition of ISO 7097-1 together with ISO 7097-2:2004 cancels and replaces ISO 7097:1983, which has been technically revised, and ISO 9989:1996. ISO 7097 consists of the following parts, under the general title Nuclear fuel technology - Determination of uranium in solutions, uranium hexafluoride and solids: Part 1: Iron(II) reduction/potassium dichromate oxidation titrimetric method; Part 2: Iron(II) reduction/cerium(IV) oxidation titrimetric method. This part 1. of ISO 7097 describes procedures for the determination of uranium in solutions, uranium hexafluoride and solids. The procedures described in the two independent parts of this International Standard are similar: this part uses a titration with potassium dichromate and ISO 7097-2 uses a titration with cerium(IV)

Separation and preconcentration of lead(II), cobalt(II), and nickel(II) on EDTA immobilized activated carbon cloth prior to flame atomic absorption spectrometric determination in environmental samples

OpenAIRE

ALOTHMAN, ZEID ABDULLAH; YILMAZ, ERKAN; HABİLA, MOHAMED; SOYLAK, MUSTAFA

2015-01-01

The synthesis and characterization of ethylenediaminetetraacetic acid immobilized activated carbon cloth was performed in the present work. It was used for preconcentration-separation of lead(II), cobalt(II), and nickel(II) at trace levels as an adsorbent. Factors including pH, concentration and volume of eluent, sample and eluent flow rates, sample volume, and effect of coexisting ions on the solid phase extraction of analytes were examined. The preconcentration factor was 50. The detection ...

DNA binding and biological activity of mixed ligand complexes of Cu(II, Ni(II and Co(II with quinolones and N donor ligand

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S.M M Akram

2015-10-01

Full Text Available  AbstractMixed ligand complexes of  Cu(II, Ni(II and Co(II have been synthesized by using levofloxacin and bipyridyl and characterized using spectral and analytical techniques. The binding behavior of the Ni(II and Cu(II complexes with herring sperm DNA(Hs-DNA were determined using electronic absorption titration, viscometric measurements and cyclic voltammetry measurements. The binding constant calculated  for Cu(II and Ni(II complexes are 2.0 x 104 and 4.0 x 104 M-1 respectively. Detailed analysis reveals that these metal complexes interact with DNA through intercalative binding mode. The nuclease activity of  Cu(II and Ni(II complexes with ct-DNA was carried out using agarose gel electrophoresis technique. The antioxidant activities for the synthesized complexes have been tested and the antibacterial activity for Ni(II complex was also checked.Key words: Intercalation, hypochromism, red shift and  peak potential.

New Mn(II, Ni(II, Cd(II, Pb(II complexes with 2-methylbenzimidazole and other ligands. Synthesis, spectroscopic characterization, crystal structure, magnetic susceptibility and biological activity studies

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Shayma A. Shaker

2016-11-01

Full Text Available Synthesis and characterization of Mn(II, Ni(II, Cd(II and Pb(II mixed ligand complexes of 2-methylbenzimidazole with other ligands have been reported. The structure of the ligands and their complexes was investigated using elemental analysis, IR, UV–Vis, (1H, 13C NMR spectroscopy, molar conductivity and magnetic susceptibility measurements. In all the studies of complexes, the 2-methylbenzimidazole behaves as a neutral monodentate ligand which is coordinated with the metal ions through the N atom. While benzotriazole behaves as a neutral bidentate ligand which is coordinated with the Ni(II ion through the two N atoms. Moreover, the N-acetylglycine behaves as a bidentate ligand which is coordinated with the Mn(II, Ni(II and Pb(II ions through the N atom and the terminal carboxyl oxygen atom. The magnetic and spectral data indicate the tetrahedral geometry for Mn(II complex, irregular tetrahedral geometry for Pb(II complex and octahedral geometry for Ni(II complex. The X-ray single crystal diffraction method was used to confirm a centrosymmetric dinuclear Cd(II complex as each two metal ions are linked by a pair of thiocyanate N = S bridge. Two 2-methylbenzimidazole N-atom donors and one terminal thiocyanate N atom complete a highly distorted square pyramid geometry around the Cd atom. Besides, different cell types were used to determine the inhibitory effect of Mn(II, Ni(II, Cd(II and Pb(II complexes on cell growth using MTT assay. Cd(II complex showed cytotoxic effect on various types of cancer cell lines with different EC50 values.

Determination of radiocesium in environmental water samples using copper ferro(II)cyanide and sodium tetraphenylborate

International Nuclear Information System (INIS)

Popov, L.; Kuleff, I.; Djingova, R.

2006-01-01

A procedure for the radiochemical separation and radiochemical purification of radiocesium ( 134 Cs and 137 Cs) in bulk environmental water samples is proposed. Radiocesium was removed from the water by cation-exchange with copper ferro(II)cyanide and was purified by precipitation with sodium tetraphenylborate. The influence of the concentration of potassium in the water sample on the chemical yield was investigated. The validation of the proposed method was carried out by analyzing reference materials. The application of the method was demonstrated with the determination of the concentration of radiocesium in water samples from rivers around NPP 'Kozloduy', Bulgaria, Danube and Ogosta. (author)

A method for the determination of ascorbic acid using the iron(II)-pyridine-dimethylglyoxime complex

International Nuclear Information System (INIS)

Arya, S. P.; Mahajan, M.

1998-01-01

A simple and rapid spectrophotometric method for the determination of ascorbic acid is proposed. Ascorbic acid reduces iron (III) to iron (II) which forms a red colored complex with dimethylglyoxime in the presence of pyridine. The absorbance of the resulting solution is measured at 514 nm and a linear relationship between absorbance and concentration of ascorbic acid is observed up to 14 μg ml -1 . Studies on the interference of substances usually associated with ascorbic acid have been carried out and the applicability of the method has been tested by analysing pharmaceutical preparations of vitamin C [it

Titrimetric application of 2-bromo-bis-1,10-phenanthroline-copper (II) bromide as a titrant in determination of ascorbic acid in pure form, fruits and vegetables

International Nuclear Information System (INIS)

Oladeji, O.

2016-01-01

Ascorbic acid is very important to man and the consumption has been linked to the prevention of degenerative diseases such as scurvy and serves as an antioxidants. There have been different approaches in the determination of ascorbic acid in fruits and vegetable. In recent times, new methods were introduced by scientists. Therefore, in order to prove the authenticity of these methods, the concentrations obtained were compared with the conventional methods. The results show that orange has maximum ascorbic acid content when compared to cashew and in vegetables Vermonia baldwinii has maximum and Solanium incanum has low ascorbic acid content. The amount of ascorbic acid determined by 2, 6-dichlorophenol-indophenol and copper (II) complex (2-bromo-bis-1, 10 phenanthroline-copper (II) bromide) are comparable.Therefore, 2-bromo-bis-1, 10-phenanthroline-copper (II) bromide can serve as a titrant in titrimetric determination of ascorbic acid in pure form, fruits and vegetables. (author)

ETA-II experiments for determining advanced radiographic capabilities of induction linacs

International Nuclear Information System (INIS)

Weir, J.T.; Caporaso, G.J.; Clark, J.C.; Kirbie, H.C.; Chen, Y.J.; Lund, S.M.; Westenskow, G.A.; Paul, A.C.

1997-05-01

LLNL has proposed a multi-pulsed, multi-line of sight radiographic machine based on induction linac technology to be the core of the advanced hydrotest facility (AHF) being considered by the Department of Energy. In order to test the new technologies being developed for AHF we have recommissioned the Experimental Test Accelerator (ETA II). We will conduct our initial experiments using kickers and large angle bending optics at the ETA II facility. Our current status and our proposed experimental schedule will be presented

New complexes of Co(II, Ni(II, Cu(II with Schiff base N,N’-bis-(3-methoxy-saliciliden-3,3’-dimethylbenzidine

Directory of Open Access Journals (Sweden)

Alan Ionela

2013-01-01

Full Text Available The new N,N’-bis-(3-methoxy-saliciliden-3,3’-dimetilbenzidine (H2L Schiff base and complexes with Co(II, Ni(II and Cu(II of type [M(HLCl(H2O] (M=Co(II, Cu(II [M2L(H2O4]X2 (M=Co(II, X=ClO4 and M=Cu(II, X=NO3 and [M2L(CH3COO2] (M=Co(II, Ni(II, Cu(II were synthesised. The ligand and complexes were characterized by elemental analysis, conductibility measurements, magnetic moments at room temperature, IR, NMR, UV-VIS-NIR, EPR spectra and thermogravimetric analysis. A molar ratio of 1:1 or 1:2 between ligand and metal was determined from the elemental analysis. Except for perchlorate complex that behave as electrolyte, the rest of complexes are non-electrolytes. The spectral data suggest a tetrahedral, pseudo-tetrahedral or square-planar stereochemistry respectively, data confirmed by magnetic behaviour of complexes. The antimicrobial tests indicate a fungicide effect both for ligand and complexes.

Resistance of Gram-positive bacteria to nisin is not determined by Lipid II levels

NARCIS (Netherlands)

Kramer, NE; Smid, EJ; Kok, J; de Kruijff, B; Kuipers, OP; Breukink, E; Kramer, Naomi E.; Smid, Eddy J.

2004-01-01

Lipid II is essential for nisin-mediated pore formation at nano-molar concentrations. We tested whether nisin resistance could result from different Lipid II levels, by comparing the maximal Lipid II pool in Micrococcus flavus (sensitive) and Listeria monocytogenes (relatively insensitive) and their

Flow-injection chemiluminescent determination of estrogen benzoate using the tris(1,10-phenanthroline) ruthenium(II)-permanganate system.

Science.gov (United States)

Ma, Yan; Cao, Wei; Qiao, Shuang; Liu, Wenwen; Yang, Jinghe

2011-01-01

Chemiluminescence (CL) detection for the determination of estrogen benzoate, using the reaction of tris(1,10-phenanthroline)ruthenium(II)-Na(2)SO(3)-permanganate, is described. This method is based on the CL reaction of estrogen benzoate (EB) with acidic potassium permanganate and tris(1,10-phenanthroline)ruthenium(II). The CL intensity is greatly enhanced when Na(2)SO(3) is added. After optimization of the different experimental parameters, a calibration graph for estrogen benzoate is linear in the range 0.05-10 µg/mL. The 3 s limit of detection is 0.024 µg/mL and the relative standard deviation was 1.3% for 1.0 µg/mL estrogen benzoate (n = 11). This proposed method was successfully applied to commercial injection samples and emulsion cosmetics. The mechanism of CL reaction was also studied. Copyright © 2011 John Wiley & Sons, Ltd.

Study of new rubber to steel adhesive systems based on Co(II and Cu(II sulphides coats

Directory of Open Access Journals (Sweden)

Labaj Ivan

2018-01-01

Full Text Available The presented paper deals with the preparation of new rubber to steel adhesive systems using the steel surface treatment with deposition of adhesive coats based on Co(II and Cu(II sulphides. Efficiency of new prepared adhesive systems containing Co(II and Cu(II sulphides has been compared with the efficiency of double layer adhesive system commonly used in industry. The chemical composition of prepared adhesive systems was determined using the EDX analysis. Scanning Electron Microscopy (SEM was used for study of topography and microstructure of prepared rubber to steel adhesive systems (Co(II, Cu(II sulphide, double layer adhesive system. For determination of adhesion strength between rubber blends and metal pieces with various adhesive systems deposited on these pieces, the test according to ASTM D429 standard relating to Rubber to metal adhesion, method A was used. For all test samples, the same type of rubber blend and the same curing conditions have been used.

A method for the determination of ascorbic acid using the iron(II)-pyridine-dimethylglyoxime complex

Energy Technology Data Exchange (ETDEWEB)

Arya, S. P.; Mahajan, M. [Haryana, Kurukshetra Univ. (India). Dept. of Chemistry

1998-05-01

A simple and rapid spectrophotometric method for the determination of ascorbic acid is proposed. Ascorbic acid reduces iron (III) to iron (II) which forms a red colored complex with dimethylglyoxime in the presence of pyridine. The absorbance of the resulting solution is measured at 514 nm and a linear relationship between absorbance and concentration of ascorbic acid is observed up to 14 {mu}g ml{sup -1}. Studies on the interference of substances usually associated with ascorbic acid have been carried out and the applicability of the method has been tested by analysing pharmaceutical preparations of vitamin C. [Italiano] Si propone un rapido e semplice metodo spettrofotometrico per la determinazione dell`acido ascorbico. L`acido ascorbico riduce il ferro(III) a ferro(II) che forma con la dimetilgliossima, in presenza di piridina, un complesso colorato in rosso. L`assorbanza della soluzione risultante e` misurata a 514 nm e si ottiene una relazione lineare tra assorbanza e concentrazione dell`acido ascorbico fino a 14 {mu}g ml{sup -1}. Si sono condotti studi sugli interferenti usualmente associati all`acido ascorbico ed e` stata valutata l`applicabilita` del metodo all`analisi di preparati farmaceutici di vitamina C.

Significance of determination of the serum levels of homocysteine (Hcy) and insulin-like growth factor-II (IGF-II) in patients with cerebrovascular diseases

International Nuclear Information System (INIS)

Tong Haijiang; Wang Yaling; Wang Lin; Xia Weiren; Shi Min; Lu Yaling

2006-01-01

Objective: To investigate the clinical significance of the changes of homocysteine (Hcy) and insulin-like growth factor H (IGF-II) in patients with cerebrovascular diseases (CVD). Methods: The serum Hcy (with CLIA) and IGF-II (with RIA) levels were measured in 123 patients with CVD (cerebral infarction 69 and cerebral hemorrhage 54) and 43 controls. Results: The levels of Hcy and IGF-II in patients with CVD were significantly higher than those in the controls (P 0.05). Conclusion: The serum Hcy and IGF-II levels in patients with CVD are elevated, Hcy and IGF-II may be involved in the development and pathogenesis of CVD. (authors)

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

Science.gov (United States)

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

2013-01-01

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

Luminescence properties of copper(I), zinc(II) and cadmium(II) coordination compounds with picoline ligands

Energy Technology Data Exchange (ETDEWEB)

Małecki, Jan Grzegorz, E-mail: gmalecki@us.edu.pl; Maroń, Anna

2017-06-15

Mononuclear coordination compounds of copper(I) – [Cu(PPh{sub 3}){sub 2}(picoline)(NO{sub 3})], zinc(II) – [ZnCl{sub 2}(picoline){sub 2}] (picoline=3– and 4–methylpyridine) and polymeric cadmium(II) – [CdCl{sub 2}(β-picoline){sub 2}]{sub n} were prepared and their luminescence properties in solid state and acetonitrile solutions were determined. Single crystal X-ray crystallography revealed distorted tetrahedral geometry around the central ions of the compounds. The compounds exhibit green photoluminescence in solid state and in acetonitrile solutions. The emission of copper(I) compounds originated from metal-to-ligand charge transfer state combined with nitrato-to-picoline charge transfer state i.e. ({sup 1}(M+X)LCT). The presence of nitrato ligand in the coordination sphere of copper(I) compounds quenches the emission. Luminescence of zinc(II) and cadmium(II) compounds results from chloride-to-picoline charge transfer state and the quantum efficiency in the case of the polymeric Cd(II) compound reaches 39%. The photoluminescence quantum yields of the mononuclear zinc(II) compounds vary from 10 to 16% depending on the conditions (solid state, solution). - Graphical abstract: Coordination compounds of copper(I), zinc(II) and polymeric cadmium(II) with picoline ligands were prepared and their luminescence properties in solid state and acetonitrile solutions were determined. The compounds exhibit green photoluminescence in solid state and in acetonitrile solutions. Emission of copper(I) compounds originated from {sup 1}(M+X)LCT state. Luminescence of zinc(II) and cadmium(II) compounds results from chloride-to-picoline charge transfer state and the quantum efficiency in the case of the polymeric Cd(II) compound reaches 39%. The photoluminescence quantum yields of the mononuclear zinc(II) compounds vary from 10 to 16% depending on the conditions (solid state, solution).

Boron doped diamond sensor for sensitive determination of metronidazole: Mechanistic and analytical study by cyclic voltammetry and square wave voltammetry

Energy Technology Data Exchange (ETDEWEB)

Ammar, Hafedh Belhadj, E-mail: hbelhadjammar@yahoo.fr; Brahim, Mabrouk Ben; Abdelhédi, Ridha; Samet, Youssef

2016-02-01

The performance of boron-doped diamond (BDD) electrode for the detection of metronidazole (MTZ) as the most important drug of the group of 5-nitroimidazole was proven using cyclic voltammetry (CV) and square wave voltammetry (SWV) techniques. A comparison study between BDD, glassy carbon and silver electrodes on the electrochemical response was carried out. The process is pH-dependent. In neutral and alkaline media, one irreversible reduction peak related to the hydroxylamine derivative formation was registered, involving a total of four electrons. In acidic medium, a prepeak appears probably related to the adsorption affinity of hydroxylamine at the electrode surface. The BDD electrode showed higher sensitivity and reproducibility analytical response, compared with the other electrodes. The higher reduction peak current was registered at pH 11. Under optimal conditions, a linear analytical curve was obtained for the MTZ concentration in the range of 0.2–4.2 μmol L{sup −1}, with a detection limit of 0.065 μmol L{sup −1}. - Highlights: • SWV for the determination of MTZ • Boron-doped diamond as a new electrochemical sensor • Simple and rapid detection of MTZ • Efficiency of BDD for sensitive determination of MTZ.

Emulsification based dispersive liquid microextraction prior to flame atomic absorption spectrometry for the sensitive determination of Cd(II) in water samples

International Nuclear Information System (INIS)

Rahimi-Nasrabadi, Mehdi; Banan, Alireza; Zahedi, Mir Mahdi; Pourmortazavi, Seied Mahdi; Nazari, Zakieh; Asghari, Alireza

2013-01-01

We report on the application of emulsification-based dispersive liquid micro extraction (EB-DLME) to the preconcentration of Cd(II). This procedure not only possesses all the advantages of routine DLLME, but also results in a more stable cloudy state which is particularly useful when coupling it to FAAS. In EB-DLME, appropriate amounts of the extraction solvent (a solution of dithizone in chloroform) and an aqueous solution of sodium dodecyl sulfate (SDS; acting as a disperser) are injected into the samples. A stable cloudy microemulsion is formed and Cd(II) ion is extracted by chelation. After phase separation, the sedimented phase is subjected to FAAS. Under optimized conditions, the calibration curve for Cd(II) is linear in the range from 0.1 to 25 μg L −1 , the limit of detection (at S/N = 3) is 30 pg L −1 , the relative standard deviations for seven replicate analyses (at 0.56 μg L −1 of Cd(II)) is 4.6 %, and the enrichment factor is 151. EB-DLME in our opinion is a simple, efficient and rapid method for the preconcentration of Cd(II) (and most likely of many other ions) prior to FAAS determination. (author)

Preparation of phenacylchloride, morpholinophenacyl and N-Piperidinophenacyl oximes and study of their complexation with Copper (II) and Cobalt (II) ions

International Nuclear Information System (INIS)

Ali, Kamal Eldin Ahmed

1999-01-01

The aim of the present work is to prepare phenacyl chloride oxime and phenacyl of N-Piperidine and morpholine derivatives, and mainly to study their complexes with Cu(II) and Co(II) ions with objective ascertaining that one of these ligands can be used in quantitative extraction of these metal ions from the aqueous solution. Copper (II) salts form 1:1 complexes with the phenyacyl oximes of N-piperidine and morpholine and 1:2 complex with phenacyl chloride oxime. However, cobalt(II) salts form 1:2 complexes with phenacyl oxime of N-piperidine and morpholine but does not complex with phenacyl chloride oxime. The stoichiometry of these complexes were determined by UV/VIS spectrophotometry using the mole ratio, continuous variation and slope ratio methods.The stability constants of the five complexes were calculated from aberrances using Job's method. They showed that the copper (II) and cobalt (II) complexes with N-piperidinophenacy oxime are more stable than those with morpholinophenacyl oxime. Copper (II) complexes with any of these two ligands are more stable than those of cobalt (II). IR spectra of the complexes of copper (II) and cobalt (II) with phenacyl oxime of N-piperidine and morpholine show diminished peaks of hydrogen bonds between N and O atoms of the ligand. Specific extractabilities using amylalcohol of copper (II) complexes with the three ligands increase from PH4 to reach its maximum at PH8. The high value for N-piperidinophenacyl oxime ligand (96%-97%) indicates that, this ligand can be used as analytical reagent for the quantitative spectrophotometric determination of copper (II) salts in aqueous media. Cobalt (II) complexes were formed and extracted from solution only at PH6 (specific PH). The extractabilities ranging from 81.6-87.2% warrants the use of these ligands in quantitative spectrophotometric determination of cobalt (II).(Author)

Better prognostic marker in ICU - APACHE II, SOFA or SAP II!

Science.gov (United States)

Naqvi, Iftikhar Haider; Mahmood, Khalid; Ziaullaha, Syed; Kashif, Syed Mohammad; Sharif, Asim

2016-01-01

This study was designed to determine the comparative efficacy of different scoring system in assessing the prognosis of critically ill patients. This was a retrospective study conducted in medical intensive care unit (MICU) and high dependency unit (HDU) Medical Unit III, Civil Hospital, from April 2012 to August 2012. All patients over age 16 years old who have fulfilled the criteria for MICU admission were included. Predictive mortality of APACHE II, SAP II and SOFA were calculated. Calibration and discrimination were used for validity of each scoring model. A total of 96 patients with equal gender distribution were enrolled. The average APACHE II score in non-survivors (27.97+8.53) was higher than survivors (15.82+8.79) with statistically significant p value (discrimination power than SAP II and SOFA.

Disposable biosensor based on cathodic electrochemiluminescence of tris(2,2-bipyridine)ruthenium(II) for uric acid determination

International Nuclear Information System (INIS)

Ballesta-Claver, J.; Rodríguez-Gómez, R.; Capitán-Vallvey, L.F.

2013-01-01

Highlights: ► Cathodic ECL offers conventional and non-aggressive analysis conditions. ► The ECL hydrogen peroxide/ruthenium complex system for uric acid determination is novel. ► The ruthenium complex is electrochemically immobilized on graphite screen-printed electrodes. ► The quantification of the uric acid is based on a Stern–Volmer type equation. ► The use of the cathodic ECL working methodology reduces interferences during analysis. -- Abstract: A new method for uric acid (UA) determination based on the quenching of the cathodic ECL of the tris(2,2-bipyridine)ruthenium(II)–uricase system is described. The biosensor is based on a double-layer design containing first tris(2,2-bipyridine)ruthenium(II) (Ru(bpy) 3 2+ ) electrochemically immobilized on graphite screen-printed cells and uricase in chitosan as a second layer. The uric acid biosensing is based on the ECL quenching produced by uric acid over the cathodic ECL caused by immobilized Ru(bpy) 3 2+ in the presence of uricase. The use of a −1.1 V pulse for 1 s with a dwelling time of 10 s makes it possible to estimate the initial enzymatic rate, which is used as the analytical signal. The Stern–Volmer type calibration function shows a dynamic range from 1.0 × 10 −5 to 1.0 × 10 −3 M with a limit of detection of 3.1 × 10 −6 M and an accuracy of 13.6% (1.0 × 10 −4 M, n = 5) as relative standard deviation. Satisfactory results were obtained for urine samples, creating an affordable alternative for uric acid determination

Structural characterization and antioxidant properties of Cu(II) and Ni(II) complexes derived from dicyandiamide

Science.gov (United States)

Kertmen, Seda Nur; Gonul, Ilyas; Kose, Muhammet

2018-01-01

New Cu(II) and Ni(II) complexes derived from dicyandiamide were synthesized and characterised by spectroscopic and analytical methods. Molecular structures of the complexes were determined by single crystal X-ray diffraction studies. In the complexes, the Cu(II) or Ni(II) ions are four-coordinate with a slight distorted square planar geometry. The ligands (L-nPen and L-iPen) derived from dicyandiamide formed via nucleophilic addition of alcohol solvent molecule in the presence Cu(II) or Ni(II) ions. Complexes were stabilised by intricate array of hydrogen bonding interactions. Antioxidant activity of the complexes was evaluated by DPPH radical scavenging and CUPRAC methods. The complexes exhibit antioxidant activity, however, their activities were much lower than standard antioxidants (Vitamin C and trolox).

Determination of trace amounts of nickel(II) with α-(2-Benzimidazolyl)-α',α''-(N-5-nitro-2-pyridyl hydrazone) toluene in the presence of triton X-100 by fluorescence method

International Nuclear Information System (INIS)

Park, Chan Il; Kim, Hyun Soo; Cha, Ki Won

2000-01-01

A method is described for the fluorimetric determination of nicke, based on the formation of Ni(II)-α-(2-Benzimidazolyl)-α',α''-(N-5-nitro-2-pyridyl hydrazone)-toluene complex in the presence of a non-ionic surfactant. The complex has practically no fluorescence in the absence of surfactant, but the addition of Triton X-100 makes possible the fluorimetric determination of low concentrations of Ni(II) as it enhances the fluorescence intensity of the complex by up to about 5-fold. This method is very sensitive and selective for the direct determination of nickel ion. The optimum conditions are a Triton X-100 concentration of 2.0 mL (5.0%, v/v) and pH 9.0 ± 0.2 (ammonium chloride-ammonia buffer). The fluorescence is measured at 337 nm of emission wavelength under 300 nm of excitation wavelength. The fluorescence intensity is a linear function of the concentration of Ni(II) in the range 5-70 ng/mL, and the detection limit is 2.0 ng/mL. The proposed method has been successfully applied to the determination of trace amounts of Ni(II) in food and human hair samples

Fexinidazole--a new oral nitroimidazole drug candidate entering clinical development for the treatment of sleeping sickness.

Directory of Open Access Journals (Sweden)

Els Torreele

2010-12-01

Full Text Available Human African trypanosomiasis (HAT, also known as sleeping sickness, is a fatal parasitic disease caused by trypanosomes. Current treatment options for HAT are scarce, toxic, no longer effective, or very difficult to administer, in particular for the advanced, fatal stage of the disease (stage 2, chronic HAT. New safe, effective and easy-to-use treatments are urgently needed. Here it is shown that fexinidazole, a 2-substituted 5-nitroimidazole rediscovered by the Drugs for Neglected Diseases initiative (DNDi after extensive compound mining efforts of more than 700 new and existing nitroheterocycles, could be a short-course, safe and effective oral treatment curing both acute and chronic HAT and that could be implemented at the primary health care level. To complete the preclinical development and meet the regulatory requirements before initiating human trials, the anti-parasitic properties and the pharmacokinetic, metabolic and toxicological profile of fexinidazole have been assessed.Standard in vitro and in vivo anti-parasitic activity assays were conducted to assess drug efficacy in experimental models for HAT. In parallel, a full range of preclinical pharmacology and safety studies, as required by international regulatory guidelines before initiating human studies, have been conducted. Fexinidazole is moderately active in vitro against African trypanosomes (IC₅₀ against laboratory strains and recent clinical isolates ranged between 0.16 and 0.93 µg/mL and oral administration of fexinidazole at doses of 100 mg/kg/day for 4 days or 200 mg/kg/day for 5 days cured mice with acute and chronic infection respectively, the latter being a model for the advanced and fatal stage of the disease when parasites have disseminated into the brain. In laboratory animals, fexinidazole is well absorbed after oral administration and readily distributes throughout the body, including the brain. The absolute bioavailability of oral fexinidazole was 41% in mice

Study of the interference of uranium, vanadium, aluminium and molebdenum in the determination of FeII, FeIII in Syrian phosphoric acid by spectrophotometry

International Nuclear Information System (INIS)

Zaizafoun, Ghadir; Elian, Nazha

1991-04-01

The spectrophotometric determination of the ratio of iron I I to iron I II in crude phosphoric acid is of great importance because of its influence on the redox potential in the different stages which lead to the extraction of uranium from crude phosphoric acid. The suitability of a number of reagents for this determination was examined and only 1,10-phenanthroline, 5-sulfosalicylic acid and 2,2'-bipyridine were selected for further experimentation. 1-10-phenanthroline can give a deep red complex with Fe I I, in phosphoric acid medium at PH 4-6, absorbs at λ = 510 nm. The total iron was determined by reducing Fe I II to Fe I I using hydroxylamine hydrochloride. The second reagent was found capable of forming a yellow complex absorbs light at λ = 430 nm in amonia medium at PH 8.5 - 11 with Fe I II. The adopted procedure was to determine total iron first by oxidation with nitric acid. Then iron I I was determined in a second test at PH 1.5 and at λ = 500 nm. The third reagent i.e. 2-2' bipyridine is capable of forming a red complex with iron I I absorbs at λ = 522 nm. The interference of U, V, Al, and Mo was investigated. These elements were selected because of their presence in considerable amounts in Syrian commercial phosphoric acid. The work was designed so that the effect of the presence of each element as well as the presence of all possible combinations of these elements can be estimated. The investigation revealed that the interference is very high in the case of 2-2' bipyridine in addition to the instability of the complex. In the case of 1,10-phenanthroline the interference was also found high. Thus these two reagents were disregarded. The 5-sulfosalicylic reagent was found satisfactory when determining iron I II, However when Fe I I is considered the error resulting from interference ranges between 17.5 - 50%. This error was found very dependent on the PH of the medium and further work is in progress in order to lower the value of interferences

Synthesis, characterization and biological studies of metal complexes of Co (II), Ni (II), Cu (II), Zn (II) with sulphadimidine-benzylidene

International Nuclear Information System (INIS)

Tahira, F.; Imran, M.; Iqbal, J.

2009-01-01

Some novel complexes of Co (II), Ni (II), Cu (II), and Zn (II) have been synthesized with a Schiff base ligand derived from sulphadimidine and benzaldehyde. The structural features of the complexes have been determined by elemental analysis, magnetic susceptibility, conductance measurement, UV/ Vis. and infrared spectroscopy. IR studies revealed that the Schiff base ligand Sulphadimidine-benzylidene has monoanionic bidendate nature and coordinate with metal ions through nitrogen atom of azomethine (>C = N) and deprotonated -NH group. All the complexes were assigned octahedral geometry on the basis of magnetic moment and electronic spectroscopic data. Low value of conductance supports their non-electrolytic nature. The ligand, as well as its complexes were checked for their in vitro antimicrobial activities against two gram positive bacterial strains, Bacillus subtillus. Staphylococcus aureus and one gram negative Salmonella typhae and five fungal strains, Nigrospora oryzae, Curvularia lunata, Drechslera rostrata, Aspergillus niger and Candida olbicans by disc diffusion method and agar plate technique, respectively. Both the antibacterial and antitungal activities of the synthesized metal complexes were found to be more as compared to parent drug and uncomplexed ligand. All the complexes contain coordinated water, which is lost at 141-160 degree C. (author)

Role of dust in H II regions

International Nuclear Information System (INIS)

Sarazin, C.L.

1975-01-01

The purpose of this dissertation is to determine quantitatively the effects of U.V. absorbing dust on H II regions, and compare these effects with observations. Many observations indicate that dust grains are present within H II regions. An analytic theory is presented which describes all three of the effects of dust in H II regions. Although this model is relatively crude, it is useful in determining the approximate size of the modifications due to dust. In order to explore this problem more carefully, detailed numerical models of H II regions with dust were constructed. The ionization and thermal structure of these model H II regions is discussed. The observational consequences of the presence of dust are explored; the optical line intensities, radio continuum and line fluxes, and infrared emission of model H II regions with dust are given. These numerical models are compared with observations of diffuse nebulae. The optical line ratios are compared to several nearby bright H II regions, and it is found that the dust models may explain several anomalies in their spectrum

Selective dispersive liquid–liquid microextraction and preconcentration of Ni(II) into a micro droplet followed by ETAAS determination using a yellow Schiff's base bisazanyl derivative

International Nuclear Information System (INIS)

Alizadeh, Kamal; Nemati, Hadi; Zohrevand, Somaieh; Hashemi, Payman; Kakanejadifard, Ali; Shamsipur, Mojtaba; Ganjali, Mohammad Reza; Faridbod, Farnoush

2013-01-01

A simple, rapid and sensitive method was developed for the selective separation and preconcentration of Ni(II) using dispersive liquid–liquid microextraction, by a yellow Schiff's base bisazanyl derivative, as a selective complexing agent. In this method, a mixture of 45 μL chloroform (extraction solvent) and 450 μL tetrahydrofuran (dispersive solvent) is rapidly injected by syringe into a 5 mL aqueous sample containing 3% (w/v) sodium chloride and an appropriate amount of the Schiff's base. As a result, a cloudy solution is formed by entire dispersion of the extraction solvent into the aqueous phase. After centrifuging for 5 min at 5000 rpm, the sedimented phase is directly injected into the electrothermal atomic absorption spectrometry for Ni(II) determination. Some important parameters, such as kind and volume of extraction and dispersive solvents, extraction time, salt effect, pH and concentration of the chelating agent have been optimized. Under the optimum conditions, the enrichment factor for the presented method is 138. The calibration curve was linear over a nickel concentration range of 10–50 ng mL −1 . The detection limit and relative standard deviation were 0.04 ng mL −1 and 2.1%, respectively. The method was successfully applied to the extraction and determination of Ni(II) in different water samples. - Highlights: ► A new synthesized schiff's base was used for selective separation of Ni(II) ions. ► The method based on DLLME was successfully applied to the determination of Ni(II). ► A cloudy solution is formed by entire dispersion of the extraction solvent into the aqueous phase. ► In this work, the response surface analysis was used for the optimization purpose. ► The curvature of response surface reflects the interactive effect of the variables.

Determination of mercury (II) ions based on silver-nanoparticles-assisted growth of gold nanostructures: UV-Vis and surface enhanced Raman scattering approaches

Science.gov (United States)

Chen, Jun-Liang; Yang, Pei-Chia; Wu, Tsunghsueh; Lin, Yang-Wei

2018-06-01

Innovative dual detection methods for mercury(II) ions (Hg(II)) have been developed based on the formation of gold nanostructures (AuNSs) following the addition of mercury-containing solution to a mixture containing an optimized amount of Au(III), H2O2, HCl, and silver nanoparticles (AgNPs). In the absence of Hg(II), the addition of Au(III), H2O2, and HCl to the AgNP solution changes the solution's color from yellow to red, and the absorption peak shifts from 400 to 526 nm, indicating the dissolution of AgNPs and the formation of gold nanoparticles (AuNPs). Because of the spontaneous redox reaction of Hg(II) toward AgNPs, the change in the amount of remaining AgNP seed facilitates the generation of irregular AuNSs, resulting in changes in absorption intensity and shifting the peak within the range from 526 to 562 nm depending on the concentration of Hg(II). Under optimal conditions, the limit of detection (LOD) for Hg(II) at a signal-to-noise ratio (S/N) of 3 was 0.3 μM. We further observed that AgNP-assisted catalytic formation of Au nanomaterials deposited on a surface enhanced Raman scattering active substrate significantly reduced the Raman signal of 4-mercaptobenzoic acid, dependent on the Hg(II) concentration. A linear relationship was observed in the range 0.1 nM-100 μM with a LOD of 0.05 nM (S/N 3.0). As a simple, accurate and precise method, this SERS-based assay has demonstrated its success in determining levels of Hg(II) in real water samples.

QM/MM simulations identify the determinants of catalytic activity differences between type II dehydroquinase enzymes.

Science.gov (United States)

Lence, Emilio; van der Kamp, Marc W; González-Bello, Concepción; Mulholland, Adrian J

2018-05-16

Type II dehydroquinase enzymes (DHQ2), recognized targets for antibiotic drug discovery, show significantly different activities dependent on the species: DHQ2 from Mycobacterium tuberculosis (MtDHQ2) and Helicobacter pylori (HpDHQ2) show a 50-fold difference in catalytic efficiency. Revealing the determinants of this activity difference is important for our understanding of biological catalysis and further offers the potential to contribute to tailoring specificity in drug design. Molecular dynamics simulations using a quantum mechanics/molecular mechanics potential, with correlated ab initio single point corrections, identify and quantify the subtle determinants of the experimentally observed difference in efficiency. The rate-determining step involves the formation of an enolate intermediate: more efficient stabilization of the enolate and transition state of the key step in MtDHQ2, mainly by the essential residues Tyr24 and Arg19, makes it more efficient than HpDHQ2. Further, a water molecule, which is absent in MtDHQ2 but involved in generation of the catalytic Tyr22 tyrosinate in HpDHQ2, was found to destabilize both the transition state and the enolate intermediate. The quantification of the contribution of key residues and water molecules in the rate-determining step of the mechanism also leads to improved understanding of higher potencies and specificity of known inhibitors, which should aid ongoing inhibitor design.

Selective enrichment and determination of monoamine neurotransmitters by CU(II) immobilized magnetic solid phase extraction coupled with high-performance liquid chromatography-fluorescence detection.

Science.gov (United States)

He, Maofang; Wang, Chaozhan; Wei, Yinmao

2016-01-15

In this paper, iminodiacetic acid-Cu(II) functionalized Fe3O4@SiO2 magnetic nanoparticles were prepared and used as new adsorbents for magnetic solid phase extraction (MSPE) of six monoamine neurotransmitters (MNTs) from rabbit plasma. The selective enrichment of MNTs at pH 5.0 was motivated by the specific coordination interaction between amino groups of MNTs and the immobilized Cu(II). The employed weak acidic extraction condition avoided the oxidation of MNTs, and thus facilitated operation and ensured higher recoveries. Under optimal conditions, the recoveries of six MNTs from rabbit plasma were in the range of 83.9-109.4%, with RSD of 2.0-10.0%. When coupled the Cu(II) immobilized MSPE with high-performance liquid chromatography-fluorescence detection, the method exhibited relatively lower detection limits than the previously reported methods, and the method was successfully used to determine the endogenous MNTs in rabbit plasma. The proposed method has potential application for the determination of MNTs in biological samples. Also, the utilization of coordination interaction to improve the selectivity might open another way to selectively enrich small alkaloids from complex samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Pharmacokinetics and toxicology of continuously infused nitroimidazoles

International Nuclear Information System (INIS)

Eifel, P.J.; Brown, J.M.

1984-01-01

The pharmacokinetics and toxicology of misonidazole (MISO) and SR-2508 given by continuous intraperitoneal infusion were studied in female C 3 H mice. The survival (time to death) of animals receiving continuous infusions of SR-2508 and MISO was compared and related to plasma concentration, rate of infusion and total amount of drug delivered. Brain and plasma concentrations were determined by HPLC. For SR-2508, plasma concentration was directly proportional to the infusion rate. However, as the infusion rate of MISO was doubled, the plasma concentration of MISO increased approximately 6-fold, reflecting a substantial increase in the apparent half-life. The brain/plasma concentration ratio in animals infused for up to 6 days with SR-2508 remained constant, at approximately 0.09. At plasma concentrations of 0.08-1.5 mM, animals receiving SR-2508 survived approximately 3 times as long as animals exposed to a comparable plasma concentration of MISO. Even at the lowest infusion rates employed in this study, the survival of mice receiving SR-2508 was much shorter than would have been predicted if the toxicity of these two drugs were solely related to the integral brain exposure. The low brain/plasma concentration ratio of SR-2508 was maintained throughout long continuous exposures

Use of the cation exchange equilibrium method for the determination of stability constants of Co(II) with soil humic and fulvic acids

International Nuclear Information System (INIS)

Du, J.Z.; Zhou, C.Y.; Dong, W.M.; Tao, Z.Y.

1999-01-01

The stability constants for tracer concentrations of Co(II) complexes with both the red earth humic and fulvic acids were determined at pH 5.9 and ionic strength 0.010 mol/l by using the ARDAKANI-STEVENSON cation exchange equilibrium method and the radiotracer 60 Co. It was found that the 1:1 complexes of Co(II) with the red earth humic and fulvic acids were formed and that the average values of logβ (stability constant) of humic and fulvic acid complexes were 5.76±0.19 and 4.42±0.03, respectively. (author)

Analytical Evaluation to Determine Selected PAHs in a Contaminated Soil With Type II Fuel

International Nuclear Information System (INIS)

Garcia Alonso, S.; Perez Pastor, R. M.; Sevillano Castano, M. L.; Garcia Frutos, F. J.

2010-01-01

A study on the optimization of an ultrasonic extraction method for selected PAHs determination in soil contaminated by type II fuel and by using HPLC with fluorescence detector is presented. The main objective was optimize the analytical procedure, minimizing the volume of solvent and analysis time and avoiding possible loss by evaporation. This work was carried out as part of a project that investigated a remediation process of agricultural land affected by an accidental spillage of fuel (Plan Nacional I + D + i, CTM2007-64 537). The paper is structured as: Optimization of wavelengths in the chromatographic conditions to improve resolution in the analysis of fuel samples. Optimization of the main parameters affecting in the extraction process by sonication. Comparison of results with those obtained by accelerated solvent extraction. (Author) 3 refs.

Disposable biosensor based on cathodic electrochemiluminescence of tris(2,2-bipyridine)ruthenium(II) for uric acid determination

Energy Technology Data Exchange (ETDEWEB)

Ballesta-Claver, J.; Rodríguez-Gómez, R. [ECsens, Department of Analytical Chemistry, Campus Fuentenueva, Faculty of Sciences, University of Granada, E-18071 Granada (Spain); Capitán-Vallvey, L.F., E-mail: lcapitan@ugr.es [ECsens, Department of Analytical Chemistry, Campus Fuentenueva, Faculty of Sciences, University of Granada, E-18071 Granada (Spain)

2013-04-03

Highlights: ► Cathodic ECL offers conventional and non-aggressive analysis conditions. ► The ECL hydrogen peroxide/ruthenium complex system for uric acid determination is novel. ► The ruthenium complex is electrochemically immobilized on graphite screen-printed electrodes. ► The quantification of the uric acid is based on a Stern–Volmer type equation. ► The use of the cathodic ECL working methodology reduces interferences during analysis. -- Abstract: A new method for uric acid (UA) determination based on the quenching of the cathodic ECL of the tris(2,2-bipyridine)ruthenium(II)–uricase system is described. The biosensor is based on a double-layer design containing first tris(2,2-bipyridine)ruthenium(II) (Ru(bpy){sub 3}{sup 2+}) electrochemically immobilized on graphite screen-printed cells and uricase in chitosan as a second layer. The uric acid biosensing is based on the ECL quenching produced by uric acid over the cathodic ECL caused by immobilized Ru(bpy){sub 3}{sup 2+} in the presence of uricase. The use of a −1.1 V pulse for 1 s with a dwelling time of 10 s makes it possible to estimate the initial enzymatic rate, which is used as the analytical signal. The Stern–Volmer type calibration function shows a dynamic range from 1.0 × 10{sup −5} to 1.0 × 10{sup −3} M with a limit of detection of 3.1 × 10{sup −6} M and an accuracy of 13.6% (1.0 × 10{sup −4} M, n = 5) as relative standard deviation. Satisfactory results were obtained for urine samples, creating an affordable alternative for uric acid determination.

Synthesis and characterisation of Cu(II), Ni(II), Mn(II), Zn(II) and VO(II ...

Indian Academy of Sciences (India)

Unknown

Synthesis and characterisation of Cu(II), Ni(II), Mn(II), Zn(II) and VO(II) Schiff base complexes derived from o-phenylenediamine and acetoacetanilide. N RAMAN*, Y PITCHAIKANI RAJA and A KULANDAISAMY. Department of Chemistry, VHNSN College, Virudhunagar 626 001, India e-mail: ra_man@123india.com.

Initial results of hypoxia imaging using 1-{alpha}-d-(5-deoxy-5-[{sup 18}F]-fluoroarabinofuranosyl)-2-nitroimidazole ({sup 18}F-FAZA)

Energy Technology Data Exchange (ETDEWEB)

Postema, Ernst J.; McEwan, Alexander J.B.; Riauka, Terence A.; Kumar, Piyush; Richmond, Dacia A.; Abrams, Douglas N. [University of Alberta, Department of Oncology, Edmonton, Alberta (Canada); Wiebe, Leonard I. [University of Alberta, Faculty of Pharmacy and Pharmaceutical Sciences, Edmonton, Alberta (Canada)

2009-10-15

Tumour hypoxia is thought to play a significant role in the outcome of solid tumour therapy. Positron emission tomography (PET) is the best-validated noninvasive technique able to demonstrate the presence of hypoxia in vivo. The locally developed PET tracer for imaging hypoxia, 1-{alpha}-d-(5-deoxy-5-[{sup 18}F]-fluoroarabinofuranosyl)-2-nitroimidazole ({sup 18}F-FAZA), has been shown to accumulate in experimental models of tumour hypoxia and to clear rapidly from the circulation and nonhypoxic tissues. The safety and general biodistribution patterns of this radiopharmaceutical in patients with squamous cell carcinoma of the head and neck (HNSCC), small-cell lung cancer (SCLC) or non-small-cell lung cancer (NSCLC), malignant lymphoma, and high-grade gliomas, were demonstrated in this study. Patients with known primary or suspected metastatic HNSCC, SCLC or NSCLC, malignant lymphoma or high-grade gliomas were dosed with 5.2 MBq/kg of {sup 18}F-FAZA, then scanned 2-3 h after injection using a PET or PET/CT scanner. Images were interpreted by three experienced nuclear medicine physicians. The location and relative uptake scores (graded 0 to 4) of normal and abnormal {sup 18}F-FAZA biodistribution patterns, the calculated tumour-to-background (T/B) ratio, and the maximum standardized uptake value were recorded. Included in the study were 50 patients (32 men, 18 women). All seven patients with high-grade gliomas showed very high uptake of {sup 18}F-FAZA in the primary tumour. In six out of nine patients with HNSCC, clear uptake of {sup 18}F-FAZA was observed in the primary tumour and/or the lymph nodes in the neck. Of the 21 lymphoma patients (15 with non-Hodgkin's lymphoma and 6 with Hodgkin's disease), 3 demonstrated moderate lymphoma-related uptake. Of the 13 lung cancer patients (12 NSCLC, 1 SCLC), 7 had increased {sup 18}F-FAZA uptake in the primary lung tumour. No side effects of the administration of {sup 18}F-FAZA were observed. This study suggests

Characterization of NIES CRM No. 23 Tea Leaves II for the determination of multielements.

Science.gov (United States)

Mori, Ikuko; Ukachi, Miyuki; Nagano, Kimiyo; Ito, Hiroyasu; Yoshinaga, Jun; Nishikawa, Masataka

2010-05-01

A candidate environmental certified reference material (CRM) for the determination of multielements in tea leaves and materials of similar matrix, NIES CRM No. 23 Tea Leaves II, has been developed and characterized by the National Institute for Environmental Studies (NIES), Japan. The origin of the material was tea leaves, which were ground, sieved through a 106-microm mesh, homogenized, and then subdivided into amber glass bottles. The results of homogeneity and stability tests indicated that the material was sufficiently homogeneous and stable for use as a reference material. The property values of the material were statistically determined based on chemical analyses by a network of laboratories using a wide range of methods. Sixteen laboratories participated in the characterization, and nine certified values and five reference values were obtained. These property values of the candidate CRM, which are expressed as mass fractions, were close to the median and/or mean values of the mass fractions of elements in various tea products. The candidate CRM is appropriate for use in analytical quality control and in the evaluation of methods used in the analysis of tea and materials of similar matrix.

MHC class II+ (HLA-DP-like) cells in the cow reproductive tract: II. Immunolocalization of MHC class II+ cells in oviduct and vagina.

Science.gov (United States)

Eren, U; Kum, S; Sandikçi, M; Eren, V; Ilhan, F

2009-08-01

The aim of this study was to determine and examine the distribution of major frequency MHC II+ cells in the oviduct and vagina of cows during the oestrous and dioestrus phases. Right oviduct (ampulla, isthmus) and vaginal samples taken from a total of twenty seven multiparous cows were used. Tissue samples were processed to obtain both cryostat and paraffin sections. Sections were stained immunocytochemically using StreptABC method using a specific monoclonal antibody to MHC II+ cell population. Intra-epithelial and subepithelial areas along with lamina propria, muscularis mucosae and serosa of both ampulla and isthmus and intra-epithelial/subepithelial areas and mucosae of vagina were examined for the presence of MHC II+ cells. The density of immune positive cells was determined using a subjective scoring system. MHC II+ cells were demonstrated in all areas examined in both oestrus and dioestrus. In oestrus, the density of MHC II+ cells decreased in subepithelial areas (in between the epithelial cells and the basal membrane) of isthmus, whereas the density of immune positive cells was increased in muscularis mucosae of isthmus (P < 0.05), lamina propria and muscularis mucosae of ampulla (P < 0.05) as well as in the mucosae of vagina (P II+ cells observed in the oviduct and vagina increases in the majority of areas examined due to the effect of oestrogen.

Stability constants of salicylate of zinc(II), cobalt(II), uranyl(II) and thorium(IV) by paper electrophoresis

International Nuclear Information System (INIS)

Singh, R.K.P.; Yadava, J.R.; Yadava, P.C.; Yadava, K.L.

1983-01-01

Stability constants of zinc(II), cobalt(II), uranyl(II) and thorium(IV) have been determined by paper electrophoresis. Salicylic acid (0.005 mol dm - 3 ) was added to the background electrolyte: 0.1 mol dm - 3 HClO 4 . The proportions of C 6 H 4 OHCOO - and C 6 H 4 OCOO/sup =/ were varied by changing the pH of the electrolyte. These anions yielded the complexes, ZnC 6 H 4 OHCOO + , CoC 6 H 4 OHCOO + , Th(C 6 H 4 OHCOO) 4 and UO 2 (C 6 H 4 OCOO) 2 /sup =/ whose stability constants are found to be 10/sup 3.1/, 10/sup 3.2/, 10/sup 11.6/ and 10/sup 22.2/, respectively (μ = 0.1, temp. 40 0 C). (author)

Biologically active new Fe(II, Co(II, Ni(II, Cu(II, Zn(II and Cd(II complexes of N-(2-thienylmethylenemethanamine

Directory of Open Access Journals (Sweden)

C. SPÎNU

2008-04-01

Full Text Available Iron(II, cobalt(II, nickel (II, copper (II, zinc(II and cadmium(II complexes of the type ML2Cl2, where M is a metal and L is the Schiff base N-(2-thienylmethylenemethanamine (TNAM formed by the condensation of 2-thiophenecarboxaldehyde and methylamine, were prepared and characterized by elemental analysis as well as magnetic and spectroscopic measurements. The elemental analyses suggest the stoichiometry to be 1:2 (metal:ligand. Magnetic susceptibility data coupled with electronic, ESR and Mössbauer spectra suggest a distorted octahedral structure for the Fe(II, Co(II and Ni(II complexes, a square-planar geometry for the Cu(II compound and a tetrahedral geometry for the Zn(II and Cd(II complexes. The infrared and NMR spectra of the complexes agree with co-ordination to the central metal atom through nitrogen and sulphur atoms. Conductance measurements suggest the non-electrolytic nature of the complexes, except for the Cu(II, Zn(II and Cd(II complexes, which are 1:2 electrolytes. The Schiff base and its metal chelates were screened for their biological activity against Escherichia coli, Staphylococcus aureus and Pseudomonas aeruginosa and the metal chelates were found to possess better antibacterial activity than that of the uncomplexed Schiff base.

Spectrophotometric determination of some metal ions using hydrazones

International Nuclear Information System (INIS)

Mohammed, M. S.

2000-05-01

In this research many starting materials were prepared, like methyl salicylate and salicylic acid hydrazide from which different derivatives of hydrazones were synthesized by coupling with carbonyl compounds like benzil monoxime and benzil mono hydrazone which are prepared and others like salicylaldehyde and benzoin. The hydrazones that were synthesized are salicylaldehyde salicylic acid hydrazone, benzoin salicylic acid hydrazone, benzil mono hydrazone salicylic acid hydrazone and benzil monoxime salicylic acid hydrazone. These reagents were determined by different methods, IR spectrophotometric determination, the nitrogen content method and melting point determination. These hydrazones act as ligands for determination of some metal ions by making different coloured complexes that were prepared for eight hydrazones with eight metal ions U (VI), Fe (II), Fe (III), Co (II), V (II), Mo (VI), Ni (II) and Cu (II). These complexes were determined by ultraviolet and visible spectrophotometer (UV/VIS) to detect their absorbance and wavelengths (λ max). The two hydrazones salicylaldehyde salicylic acid-hydrazone and benzoin salicylic acid hydrazone, were selected for determination of five metal ions (Fe (II), Fe (III), U (VI), Ni (II) and Cu (II)), using two micelles sodium n-dodecyl sulphate and pyridinium hexa decyl bromide mono hydrate. Their absorbance and wavelengths were detected using UV/VIS spectrophotometer. (Author)

Synthesis, characterisation and electrochemical behaviour of Cu(II)

Indian Academy of Sciences (India)

Neutral tetradentate N2O2 type complexes of Cu(II), Ni(II), Co(II) and Zn(II) have been synthesised using the Schiff base formed by the condensation of acetylacetone and p-anisidine. Microanalysis, molar conductance, magnetic susceptibility, IR, UV-Vis, 1H NMR, CV and EPR studies have been carried out to determine the ...

Method for the determination of technical specifications limiting temperature in EBR-II operation

International Nuclear Information System (INIS)

Chang, L.K.; Hill, D.J.; Ku, J.Y.

1994-01-01

The methodology and analysis procedure to qualify the Mark-V and Mark-VA fuels for the Experimental Breeder Reactor II are summarized in this paper. Fuel performance data and design safety criteria are essential for thermal-hydraulic analysis and safety evaluations. Normal and off-normal operation duty cycles and transient classifications are required for the safety assessment of the fuels. The temperature limits of subassemblies were first determined by a steady-state thermal-structural and fuel damage analysis, in which a trial-and-error approach was used to predict the maximum allowable fuel pin temperature that satisfies the design criteria for steady-state normal operation. The steady-state temperature limits were used as the basis of the off-normal transient analysis to assess the safety performance of the fuel for anticipated, unlikely and extremely unlikely events. If the design criteria for the off-normal events are not satisfied, then the subassembly temperature limit is reduced and an iterative procedure is employed until all design criteria are met

Complexes of cobalt(II), nickel(II), copper(II), zinc(II), cadmium(II) and dioxouranium(II) with thiophene-2-aldehydethiosemicarbazone

International Nuclear Information System (INIS)

Singh, Balwan; Misra, Harihar

1986-01-01

Metal complexes of thiosemicarbazides have been known for their pharmacological applications. Significant antitubercular, fungicidal and antiviral activities have been reported for thiosemicarbazides and their derivatives. The present study describes the systhesis and characterisation of complexes of Co II , Cu II , Zn II ,Cd II and UO II with thiosemicarbazone obtained by condensing thiophene-2-aldehyde with thiosemicarbazide. 17 refs., 2 tables. (author)

Extraction and Determination of Pb(II by Organic Functionalisation of Graphenes Adsorbed on Surfactant Coated C18 in Environmental Sample

Directory of Open Access Journals (Sweden)

A. Moghimi

2013-11-01

Full Text Available A novel, simple, sensitive and effective method has been developed for preconcentration of lead. This solid-phase extraction adsorbent was synthesized by functionalization of graphenes with covalently linked N-methyl-glycine and 3, 4-dihydroxybenzaldehyde onto the surfaces of graphite. The method is based on selective chelation of Pb (II on surfactant coated C18, modified with functionalization of graphenes (graphene-f-OH. The adsorbed ions were then eluted with 4 ml of 4 M nitric acid and determined by flame atomic absorption spectrometry (FAAS at 283.3 for Pb. The influence of flow rates of sample and eluent solutions, pH, breakthrough volume, effect of foreign ions were investigated on chelation and recovery. 1.5 g of surfactant coated C18 adsorbs 40 mg of the functionalization of graphenes (graphene-f-OH base which in turn can retain15.2±0.8mg of each of the two ions. The limit of detection (3σ for Pb(II was found to be 3.20 ng l -1. The enrichment factor for both ions is 100. The mentioned method was successfully applied on the determination of Pb in different water samples.

Extraction and Determination of Pb(II by Organic Functionalisation of Graphenes Adsorbed on Surfactant Coated C18 in Environmental Sample

Directory of Open Access Journals (Sweden)

A. Moghimi

2014-05-01

Full Text Available A novel, simple, sensitive and effective method has been developed for preconcentration of lead. This solidphase extraction adsorbent was synthesized by functionalization of graphenes with covalently linked N-methyl-glycine and 3, 4-dihydroxybenzaldehyde onto the surfaces of graphite. The method is based on selective chelation of Pb (II on surfactant coated C18, modified with functionalization of graphenes (graphene-f-OH. The adsorbed ions were then eluted with 4 ml of 4 M nitric acid and determined by flame atomic absorption spectrometry (FAAS at 283.3 for Pb. The influence of flow rates of sample and eluent solutions, pH, breakthrough volume, effect of foreign ions were investigated on chelation and recovery. 1.5 g of surfactant coated C18 adsorbs 40 mg of the functionalization of graphenes (graphene-f-OH base which in turn can retain15.2±0.8mg of each of the two ions. The limit of detection (3σ for Pb(II was found to be 3.20 ng l -1. The enrichment factor for both ions is 100. The mentioned method was successfully applied on the determination of Pb in different water samples

IMPROVED log(gf ) VALUES OF SELECTED LINES IN Mn I AND Mn II FOR ABUNDANCE DETERMINATIONS IN FGK DWARFS AND GIANTS

International Nuclear Information System (INIS)

Den Hartog, E. A.; Lawler, J. E.; Sobeck, J. S.; Sneden, C.; Cowan, J. J.

2011-01-01

The goal of the present work is to produce transition probabilities with very low uncertainties for a selected set of multiplets of Mn I and Mn II. Multiplets are chosen based upon their suitability for stellar abundance analysis. We report on new radiative lifetime measurements for 22 levels of Mn I from the e 8 D, z 6 P, z 6 D, z 4 F, e 8 S, and e 6 S terms and six levels of Mn II from the z 5 P and z 7 P terms using time-resolved laser-induced fluorescence on a slow atom/ion beam. New branching fractions for transitions from these levels, measured using a Fourier-transform spectrometer, are reported. When combined, these measurements yield transition probabilities for 47 transitions of Mn I and 15 transitions of Mn II. Comparisons are made to data from the literature and to Russell-Saunders (LS) theory. In keeping with the goal of producing a set of transition probabilities with the highest possible accuracy and precision, we recommend a weighted mean result incorporating our measurements on Mn I and II as well as independent measurements or calculations that we view as reliable and of a quality similar to ours. In a forthcoming paper, these Mn I/II transition probability data will be utilized to derive the Mn abundance in stars with spectra from both space-based and ground-based facilities over a 4000 A wavelength range. With the employment of a local thermodynamic equilibrium line transfer code, the Mn I/II ionization balance will be determined for stars of different evolutionary states.

NMR investigation of dynamic processes in complexes of nickel(II) and zinc(II) with iminodiacetate, n-methyliminodiacetate and n-ethyliminodiacetate

International Nuclear Information System (INIS)

Wagner, M.R.

1985-11-01

Analysis of oxygen-17 bulk water relaxation rates with an aqueous solution of 1:1 Ni(II):ida reveals that two rate-limiting processes are involved with solvent exchange. Analysis of carbon-13 longitudinal relaxation rates of the bis-ligand complexes with zinc(II) are used to determine molecular tumbling rates and methyl rotation rates. The carbon-13 transverse relaxation rates for the carbons in the bis-ligand complex with Ni(II) are adequately fitted to the Solomon-Bloembergen equation. Three carboxylate carbon peaks are seen with the 13 C spectrum of the 1:2 Ni(II):ida complex, which coalesce into a single peak above about 360 K. The mechanism and rate of ligand exchange are determined for the complexes Zn(II)L 2 -2 (L = mida, eida) in aqueous solution by total lineshape analysis of the proton spectrum at 500 MHz

Impact determination of strength and resistance training on Glycoside hemoglobin and blood sugar on patients with type II diabetes”

OpenAIRE

Bahman Hasanvand; Kobra Karami; Abdollah Khodadi; Mehdi Valipour

2011-01-01

Background : This study determined the impact of strength and resistance training on hemoglobin Glycoside and glucose in type II diabetic patients in Khorramabad in 2009. Materials and Methods: This quasi-experimental study was carried out on 30 men with type 2 diabetes referred to laboratories in Khorramabad, selected by screening and interview and purposeful sampling . After the subjects completed questionnaires of medical records and written consent, they were randomly divided into th...

Intrafibrillar Mineral May be Absent in Dentinogenesis Imperfecta Type II (DI-II)

Energy Technology Data Exchange (ETDEWEB)

Pople, John A

2001-03-29

High-resolution synchrotron radiation computed tomography (SRCT) and small angle x-ray scattering (SAXS) were performed on normal and dentinogenesis imperfecta type II (DI-II) teeth. Three normal and three DI-II human third molars were used in this study. The normal molars were unerupted and had intact enamel; donors were female and ranged in age from 18-21y. The DI-II specimens, which were also unerupted with intact enamel, came from a single female donor age 20y. SRCT showed that the mineral concentration was 33% lower on average in the DI-II dentin with respect to normal dentin. The SAXS spectra from normal dentin exhibited low-angle diffraction peaks at harmonics of 67.6 nm, consistent with nucleation and growth of the apatite phase within gaps in the collagen fibrils (intrafibrillar mineralization). In contrast, the low-angle peaks were almost nonexistent in the DI-II dentin. Crystallite thickness was independent of location in both DI-II and normal dentin, although the crystallites were significantly thicker in DI-II dentin (6.8 nm (s.d. = 0.5) vs 5.1 nm (s.d. = 0.6)). The shape factor of the crystallites, as determined by SAXS, showed a continuous progression in normal dentin from roughly one-dimensional (needle-like) near the pulp to two-dimensional (plate-like) near the dentin-enamel junction. The crystallites in DI-II dentin, on the other hand, remained needle-like throughout. The above observations are consistent with an absence of intrafibrillar mineral in DI-II dentin.

Validity of transcobalamin II-based radioassay for the determination of serum vitamin B12 concentrations

International Nuclear Information System (INIS)

Paltridge, G.; Rudzki, Z.; Ryall, R.G.

1980-01-01

A valid radioassay for the estimation of serum vitamin B 12 in the presence of naturally occurring vitamin B 12 (= cobalamin) analogues can be operated if serum transcobalamin II (TC II) is used as the binding protein. Serum samples that gave diagnostically discrepant results when their vitamin B 12 content was analysed (i) by a commercial radioassay known to be susceptible to interference from cobalamin analogues, and (ii) by microbiological assay, were further analysed by an alternative radioassay which uses the transcobalamins (principally TC II) of diluted normal serum as the assay binding protein. Concordance between the results from microbiological assay and the TC II-based radioassay was found in all cases. In an extended study over a three-year period, all routine serum samples sent for vitamin B 12 analysis that had a vitamin B 12 content of less than 320 ng/l by the TC II-based radioassay (reference range 200-850 ng/l) were reanalysed using an established microbiological method. Over 1000 samples were thus analysed. The data are presented to demonstrate the validity of the TC II-based radioassay results in this group of patients, serum samples from which are most likely to produce diagnostically erroneous vitamin B 12 results when analysed by a radioassay that is less specific for cobalamins. (author)

Electrochemical Microsensors for the Detection of Cadmium(II and Lead(II Ions in Plants

Directory of Open Access Journals (Sweden)

Olga Krystofova

2010-05-01

Full Text Available Routine determination of trace metals in complex media is still a difficult task for many analytical instruments. The aim of this work was to compare three electro-chemical instruments [a standard potentiostat (Autolab, a commercially available miniaturized potentiostat (PalmSens and a homemade micropotentiostat] for easy-to-use and sensitive determination of cadmium(II and lead(II ions. The lowest detection limits (hundreds of pM for both metals was achieved by using of the standard potentiostat, followed by the miniaturized potentiostat (tens of nM and the homemade instrument (hundreds of nM. Nevertheless, all potentiostats were sensitive enough to evaluate contamination of the environment, because the environmental limits for both metals are higher than detection limits of the instruments. Further, we tested all used potentiostats and working electrodes on analysis of environmental samples (rainwater, flour and plant extract with artificially added cadmium(II and lead(II. Based on the similar results obtained for all potentiostats we choose a homemade instrument with a carbon tip working electrode for our subsequent environmental experiments, in which we analyzed maize and sunflower seedlings and rainwater obtained from various sites in the Czech Republic.

Mn(II), Zn(II) and VO(II) Schiff

Indian Academy of Sciences (India)

Home; Journals; Journal of Chemical Sciences; Volume 113; Issue 3. Synthesis and characterisation of Cu(II), Ni(II), Mn(II), Zn(II) and VO(II) Schiff base complexes derived from o-phenylenediamine and acetoacetanilide. N Raman Y Pitchaikani Raja A Kulandaisamy. Inorganic Volume 113 Issue 3 June 2001 pp 183-189 ...

Voltammetric determination of zirconium using azo compounds

International Nuclear Information System (INIS)

Orshulyak, O.O.; Levitskaya, G.D.

2008-01-01

The optimum conditions for zirconium complexation with azo compounds are found. The applicability of Eriochrome Red B, Calcon, and Calcion to the voltammetric determination of zirconium, total Zr(IV) and Hf(IV), and Zr(IV) in the presence of Zn(II), Cu(II), Cd(II), Ni(II), or Ti(IV) is demonstrated. The developed procedures are used to determine zirconium in a terbium alloy and in an alloy for airplane wheel drums [ru

Chemically modified activated carbon with 1-acylthiosemicarbazide for selective solid-phase extraction and preconcentration of trace Cu(II), Hg(II) and Pb(II) from water samples.

Science.gov (United States)

Gao, Ru; Hu, Zheng; Chang, Xijun; He, Qun; Zhang, Lijun; Tu, Zhifeng; Shi, Jianping

2009-12-15

A new sorbent 1-acylthiosemicarbazide-modified activated carbon (AC-ATSC) was prepared as a solid-phase extractant and applied for removing of trace Cu(II), Hg(II) and Pb(II) prior to their determination by inductively coupled plasma optical emission spectrometry (ICP-OES). The separation/preconcentration conditions of analytes were investigated, including effects of pH, the shaking time, the sample flow rate and volume, the elution condition and the interfering ions. At pH 3, the maximum static adsorption capacity of Cu(II), Hg(II) and Pb(II) onto the AC-ATSC were 78.20, 67.80 and 48.56 mg g(-1), respectively. The adsorbed metal ions were quantitatively eluted by 3.0 mL of 2% CS(NH2)2 and 2.0 mol L(-1) HCl solution. Common coexisting ions did not interfere with the separation. According to the definition of IUPAC, the detection limits (3sigma) of this method for Cu(II), Hg(II) and Pb(II) were 0.20, 0.12 and 0.45 ng mL(-1), respectively. The relative standard deviation under optimum conditions is less than 4.0% (n=8). The prepared sorbent was applied for the preconcentration of trace Cu(II), Hg(II) and Pb(II) in certified and water samples with satisfactory results.

Oxidation of Fe(II) in rainwater.

Science.gov (United States)

Willey, J D; Whitehead, R F; Kieber, R J; Hardison, D R

2005-04-15

Photochemically produced Fe(II) is oxidized within hours under environmentally realistic conditions in rainwater. The diurnal variation between photochemical production and reoxidation of Fe(II) observed in our laboratory accurately mimics the behavior of ferrous iron observed in field studies where the highest concentrations of dissolved Fe(ll) occur in afternoon rain during the period of maximum sunlight intensity followed by gradually decreasing concentrations eventually returning to early morning pre-light values. The experimental work presented here, along with the results of kinetics studies done by others, suggests thatthe primary process responsible for the decline in photochemically produced Fe(II) concentrations is oxidation by hydrogen peroxide. This reaction is first order with respect to both the concentrations of Fe(II) and H2O2. The second-order rate constant determined for six different authentic rain samples varied over an order of magnitude and was always less than or equal to the rate constant determined for this reaction in simple acidic solutions. Oxidation of photochemically produced ferrous iron by other oxidants including molecular oxygen, ozone, hydroxyl radical, hydroperoxyl/superoxide radical, and hexavalent chromium were found to be insignificant under the conditions present in rainwater. This study shows that Fe(II) occurs as at least two different chemical species in rain; photochemically produced Fe(II) that is oxidized over time periods of hours, and a background Fe(II) that is protected against oxidation, perhaps by organic complexation, and is stable against oxidation for days. Because the rate of oxidation of photochemically produced Fe(II) does not increase with increasing rainwater pH, the speciation of this more labile form of Fe(II) is also not controlled by simple hydrolysis reactions.

Biosorption of Cd(II), Ni(II) and Pb(II) from aqueous solution by dried biomass of aspergillus niger: application of response surface methodology to the optimization of process parameters

Energy Technology Data Exchange (ETDEWEB)

Amini, Malihe; Younesi, Habibollah [Department of Environmental Science, Faculty of Natural Resources and Marine Sciences, Tarbiat Modares University, Noor (Iran)

2009-10-15

In this study, the biosorption of Cd(II), Ni(II) and Pb(II) on Aspergillus niger in a batch system was investigated, and optimal condition determined by means of central composite design (CCD) under response surface methodology (RSM). Biomass inactivated by heat and pretreated by alkali solution was used in the determination of optimal conditions. The effect of initial solution pH, biomass dose and initial ion concentration on the removal efficiency of metal ions by A. niger was optimized using a design of experiment (DOE) method. Experimental results indicated that the optimal conditions for biosorption were 5.22 g/L, 89.93 mg/L and 6.01 for biomass dose, initial ion concentration and solution pH, respectively. Enhancement of metal biosorption capacity of the dried biomass by pretreatment with sodium hydroxide was observed. Maximal removal efficiencies for Cd(II), Ni(III) and Pb(II) ions of 98, 80 and 99% were achieved, respectively. The biosorption capacity of A. niger biomass obtained for Cd(II), Ni(II) and Pb(II) ions was 2.2, 1.6 and 4.7 mg/g, respectively. According to these observations the fungal biomass of A. niger is a suitable biosorbent for the removal of heavy metals from aqueous solutions. Multiple response optimization was applied to the experimental data to discover the optimal conditions for a set of responses, simultaneously, by using a desirability function. (Abstract Copyright [2009], Wiley Periodicals, Inc.)

Comparison of the performance of different modified graphene oxide nanosheets for the extraction of Pb(II) and Cd(II) from natural samples

International Nuclear Information System (INIS)

Sayar, Omid; Mehrani, Kheirollah; Mehrani, Azadeh; Hoseinzadeh, Fatemeh; Sadeghi, Omid

2014-01-01

Graphene nanosheets were modified with amino groups and the resulting material was used as a sorbent for the extraction of cadmium and lead ions. The nanosheets were characterized by IR spectroscopy, transmission electron microscopy, thermal gravimetric analysis and elemental analysis. The effects of sample pH, eluent parameters (type, concentration and volume of eluent), flow rates (of both sample and eluent), and of a variety of other ions on the efficiency of the extraction of Cd(II) and Pb(II) were optimized. Following solid phase extraction, the elements were determined by FAAS. The limits of detection are <0.9 μg L −1 for Pb(II) and <5 ng L −1 for Cd(II). The relative standard deviations are <2.2 %. The method was validated by analyzing several certified reference materials and was then used for Pb(II) and Cd(II) determination in natural waters and vegetables. (author)

Validity of the Mania Subscale of the Diagnostic Assessment for the Severely Handicapped-II (DASH-II).

Science.gov (United States)

Matson, Johnny L.; Smiroldo, Brandi B.

1997-01-01

A study tested the validity of the Diagnostic Assessment for the Severely Handicapped-II (DASH-II) for determining the presence of mania (bipolar disorder) in 22 individuals with severe mental retardation. Results found the mania subscale to be internally consistent and able to be used to classify manic and control subjects accurately. (Author/CR)

Adsorption of Pb(II), Cu(II), Cd(II), Zn(II), Ni(II), Fe(II), and As(V) on bacterially produced metal sulfides.

Science.gov (United States)

Jong, Tony; Parry, David L

2004-07-01

The adsorption of Pb(II), Cu(II), Cd(II), Zn(II), Ni(II), Fe(II) and As(V) onto bacterially produced metal sulfide (BPMS) material was investigated using a batch equilibrium method. It was found that the sulfide material had adsorptive properties comparable with those of other adsorbents with respect to the specific uptake of a range of metals and, the levels to which dissolved metal concentrations in solution can be reduced. The percentage of adsorption increased with increasing pH and adsorbent dose, but decreased with increasing initial dissolved metal concentration. The pH of the solution was the most important parameter controlling adsorption of Cd(II), Cu(II), Fe(II), Ni(II), Pb(II), Zn(II), and As(V) by BPMS. The adsorption data were successfully modeled using the Langmuir adsorption isotherm. Desorption experiments showed that the reversibility of adsorption was low, suggesting high-affinity adsorption governed by chemisorption. The mechanism of adsorption for the divalent metals was thought to be the formation of strong, inner-sphere complexes involving surface hydroxyl groups. However, the mechanism for the adsorption of As(V) by BPMS appears to be distinct from that of surface hydroxyl exchange. These results have important implications to the management of metal sulfide sludge produced by bacterial sulfate reduction.

Oxidative generation of guanine radicals by carbonate radicals and their reactions with nitrogen dioxide to form site specific 5-guanidino-4-nitroimidazole lesions in oligodeoxynucleotides.

Science.gov (United States)

Joffe, Avrum; Mock, Steven; Yun, Byeong Hwa; Kolbanovskiy, Alexander; Geacintov, Nicholas E; Shafirovich, Vladimir

2003-08-01

A simple photochemical approach is described for synthesizing site specific, stable 5-guanidino-4-nitroimidazole (NIm) adducts in single- and double-stranded oligodeoxynucleotides containing single and multiple guanine residues. The DNA sequences employed, 5'-d(ACC CG(1)C G(2)TC CG(3)C G(4)CC) and 5'-d(ACC CG(1)C G(2)TC C), were a portion of exon 5 of the p53 tumor suppressor gene, including the codons 157 (G(2)) and 158 (G(3)) mutation hot spots in the former sequence with four Gs and the codon 157 (G(2)) mutation hot spot in the latter sequence with two Gs. The nitration of oligodeoxynucleotides was initiated by the selective photodissociation of persulfate anions to sulfate radicals induced by UV laser pulses (308 nm). In aqueous solutions, of bicarbonate and nitrite anions, the sulfate radicals generate carbonate anion radicals and nitrogen dioxide radicals by one electron oxidation of the respective anions. The guanine residue in the oligodeoxynucleotide is oxidized by the carbonate anion radical to form the neutral guanine radical. While the nitrogen dioxide radicals do not react with any of the intact DNA bases, they readily combine with the guanine radicals at either the C8 or the C5 positions. The C8 addition generates the well-known 8-nitroguanine (8-nitro-G) lesions, whereas the C5 attack produces unstable adducts, which rapidly decompose to NIm lesions. The maximum yields of the nitro products (NIm + 8-nitro-G) were typically in the range of 20-40%, depending on the number of guanine residues in the sequence. The ratio of the NIm to 8-nitro-G lesions gradually decreases from 3.4 in the model compound, 2',3',5'-tri-O-acetylguanosine, to 2.1-2.6 in the single-stranded oligodeoxynucleotides and to 0.8-1.1 in the duplexes. The adduct of the 5'-d(ACC CG(1)C G(2)TC C) oligodeoxynucleotide containing the NIm lesion in codon 157 (G(2)) was isolated in HPLC-pure form. The integrity of this adduct was established by a detailed analysis of exonuclease digestion

Determination of UO2(II), and Ce(III) complexes formed with halogen and nitro derivatives of 8-hydroxyquinoline

International Nuclear Information System (INIS)

Teksoez, S.; Uenak, P.

2001-01-01

Proton-ligand stability constants for some iodo and nitro derivatives of 8-hydroxyquinoline were determined by Calvin Bjerrum potantiometrical method. The stability constants of the corresponding chelates with UO 2 (II), Th(IV) and Ce(III) were studied potentiometrically at 25 degree Celsius by applying Irving-Rossotti computing method. The complexes of the nitro-substituted ligands were less stable than the corresponding complexes of the unsubstituted ligands. The stability constants of metal-ligands depend on the ionic radii and ionic charge of metals and also they decrease with steric repulsions of the nitro groups

Effect of KNO3 to remove silver interferences in the determination of mercury(II: Application in milk and breast milk samples

Directory of Open Access Journals (Sweden)

A. Farahi

2015-06-01

Full Text Available Mercury determination was performed at rotating silver electrode (RSE using square wave voltammetry (SWV in electrolytic mixture of HCl (0.1 mol L−1 and KNO3 (0.2 mol L−1. The reproducibility, sensitivity and accuracy are good, provided the proper instrumental parameters and supporting electrolyte are used. The relationship between the peak current of mercury(II and its concentration is linear with regression equation: I(μA = 0.784 [Hg(II] + 49.5 (r2 = 0.9878 in the dynamic range from 1.0 × 10−7 to 8.0 × 10−4 mol L−1. The detection limit (DL,3σ and quantification limit (QL,10σ were 4.61 × 10−8 mol L−1 and 15.3 × 10−8 mol L−1, respectively. The relative standard deviation (RSD for seven replicate analysis of a solution containing 5.0 × 10−5 mol L−1 was 2.19%. Possible effects of Cu, Co, Fe, MnO4, Zn, were investigated but did not cause any significant interferences. Immobilization of mercury(II on the surface of rotating silver electrode obeyed to the Langmuir adsorption isotherm. The calculated ΔG°ads value showed that the interaction between mercury and silver electrodes is mainly controlled by a chemisorption process. This methodology was potentially applied for mercury determination in milk and breast milk samples.

Cobalt(II), nickel(II), copper(II), and zinc(II) complexes with [3(5)]adamanzane, 1,5,9,13-tetraazabicyclo[7.7.3]nonadecane and [(2.3)(2).2(1)]adamanzane, 1,5,9,12-tetraazabicyclo[7.5.2]hexadecane

DEFF Research Database (Denmark)

Broge, Louise; Pretzmann, Ulla; Jensen, Nicolai

2001-01-01

) and of three cobalt(II), four nickel(II), one copper(II), and two zinc(II) complexes with [3(5)]adamanzane. For nine of these compounds (2-8, 10b, and 12) the single-crystal X-ray structures were determined. The coordination geometry around the metal ion is square pyramidal in [Cu([(2.3)(2).2(1)]adz)Br]ClO4 (2......) and trigonal bipyramidal in the isostructural structures [Cu([3(5)]adz)Br]Br (3), [Ni-([3(5)]adz)Cl]Cl (5), [Ni([3(5)]adz)Br]Br (6), and [Co([3(5)]adz)Cl]Cl (8). In [Ni([3(5)]adz)(NO3)]NO3 (4) and [Ni([3(5)]-adz)(ClO4)]ClO4 (7) the coordination geometry around nickel(II) is a distorted octahedron...... with the inorganic ligands at cis positions. The coordination polyhedron around the metal ion in [Co([3(5)]adz)][ZnCl4] (10b) and [Zn([3(5)]adz)][ZnCl4] (12) is a slightly distorted tetrahedron. Anation equilibrium constants were determined spectrophotometrically for complexes 2-6 at 25 and 40 degreesC and fall...

Intrafibrillar Mineral May be Absent in Dentinogenesis Imperfecta Type II (DI-II); TOPICAL

International Nuclear Information System (INIS)

Pople, John A.

2001-01-01

High-resolution synchrotron radiation computed tomography (SRCT) and small angle x-ray scattering (SAXS) were performed on normal and dentinogenesis imperfecta type II (DI-II) teeth. Three normal and three DI-II human third molars were used in this study. The normal molars were unerupted and had intact enamel; donors were female and ranged in age from 18-21y. The DI-II specimens, which were also unerupted with intact enamel, came from a single female donor age 20y. SRCT showed that the mineral concentration was 33% lower on average in the DI-II dentin with respect to normal dentin. The SAXS spectra from normal dentin exhibited low-angle diffraction peaks at harmonics of 67.6 nm, consistent with nucleation and growth of the apatite phase within gaps in the collagen fibrils (intrafibrillar mineralization). In contrast, the low-angle peaks were almost nonexistent in the DI-II dentin. Crystallite thickness was independent of location in both DI-II and normal dentin, although the crystallites were significantly thicker in DI-II dentin (6.8 nm (s.d.= 0.5) vs 5.1 nm (s.d.= 0.6)). The shape factor of the crystallites, as determined by SAXS, showed a continuous progression in normal dentin from roughly one-dimensional (needle-like) near the pulp to two-dimensional (plate-like) near the dentin-enamel junction. The crystallites in DI-II dentin, on the other hand, remained needle-like throughout. The above observations are consistent with an absence of intrafibrillar mineral in DI-II dentin

The interaction of platinum complexes with low doses of X-rays in hypoxic cells

International Nuclear Information System (INIS)

Skov, K.A.

1992-01-01

It is not clear why electron affinic compounds (O2, nitroimidazoles) should be more effective sensitizers at high doses (modify double events, 6, 16) while platinum complexes interact to a greater extent at low doses (modification of single-events). The possibility that crosslinks are involved requires further consideration. While DNA intrastrand crosslinks do not appear essential, future low dose experiments are planned to determine the role of interstrand and DNA-protein crosslinks in modifying response at clinical doses. (author). 31 refs., 2 tabs

Characteristics of fluorinated nitroazoles as hypoxic cell radiosensitizers

International Nuclear Information System (INIS)

Shibamoto, Y.; Nishimoto, S.; Shimokawa, K.

1989-01-01

Types of 2-nitroimidazoles and 3-nitro-1,2,4-triazoles bearing one or two fluorine atoms on their side chains were synthesized to evaluate their physicochemical properties, radiosensitizing effects, and toxicity. The reduction potential of the compounds containing one fluorine was similar to that of misonidazole (MISO), whereas that of the difluorinated compounds was slightly higher. Both mono- and difluorinated compounds had an in vitro sensitizing activity comparable to or slightly higher than that of MISO. The fluorinated 3-nitrotriazoles were almost as efficient as the 2-nitroimidazoles with the same substituent. In vivo, some of the compounds were up to twice more efficient than MISO, whereas others were as efficient as MISO. Toxicity in terms of LD50/7 in mice was quite variable depending on the side-chain structure; the amide derivatives were less toxic than MISO, whereas the alcohol and ether derivatives were more toxic. In view of the radiosensitizing effect and toxicity in vivo, at least one compound, KU-2285 (a 2-nitroimidazole with an N1-substituent of: CH2CF2CONHCH2CH2OH) has been found to be as useful a hypoxic cell sensitizer as SR-2508

Synthesis and spectroscopic studies of biologically active tetraazamacrocyclic complexes of Mn(II, Co(II, Ni(II, Pd(II and Pt(II

Directory of Open Access Journals (Sweden)

Monika Tyagi

2014-01-01

Full Text Available Complexes of Mn(II, Co(II, Ni(II, Pd(II and Pt(II were synthesized with the macrocyclic ligand, i.e., 2,3,9,10-tetraketo-1,4,8,11-tetraazacycoletradecane. The ligand was prepared by the [2 + 2] condensation of diethyloxalate and 1,3-diamino propane and characterized by elemental analysis, mass, IR and 1H NMR spectral studies. All the complexes were characterized by elemental analysis, molar conductance, magnetic susceptibility measurements, IR, electronic and electron paramagnetic resonance spectral studies. The molar conductance measurements of Mn(II, Co(II and Ni(II complexes in DMF correspond to non electrolyte nature, whereas Pd(II and Pt(II complexes are 1:2 electrolyte. On the basis of spectral studies an octahedral geometry has been assigned for Mn(II, Co(II and Ni(II complexes, whereas square planar geometry assigned for Pd(II and Pt(II. In vitro the ligand and its metal complexes were evaluated against plant pathogenic fungi (Fusarium odum, Aspergillus niger and Rhizoctonia bataticola and some compounds found to be more active as commercially available fungicide like Chlorothalonil.

The CDF SVX II upgrade for the Tevatron Run II

International Nuclear Information System (INIS)

Bortoletto, Daniela

1997-01-01

A microstrip silicon detector SVX II has been proposed for the upgrade of CDF to be installed in 1999 for Run II of the Tevatron. Three barrels of five layers of double-sided silicon microstrip detectors will cover the interaction region. A description of the project status will be presented. Emphasis will be given to the R and D program for silicon sensors which includes capacitance minimization, the study of coupling capacitor integrity, the operation of the detectors in conjunction with the SVXH and SVX2 readout chips in two beam tests and the determination of the detectors performance deterioration due to radiation damage

Biosorption of copper(II), lead(II), iron(III) and cobalt(II) on Bacillus sphaericus-loaded Diaion SP-850 resin

International Nuclear Information System (INIS)

Tuzen, Mustafa; Uluozlu, Ozgur Dogan; Usta, Canan; Soylak, Mustafa

2007-01-01

The biosorption of copper(II), lead(II), iron(III) and cobalt(II) on Bacillus sphaericus-loaded Diaion SP-850 resin for preconcentration-separation of them have been investigated. The sorbed analytes on biosorbent were eluted by using 1 mol L -1 HCl and analytes were determined by flame atomic absorption spectrometry. The influences of analytical parameters including amounts of pH, B. sphaericus, sample volume etc. on the quantitative recoveries of analytes were investigated. The effects of alkaline, earth alkaline ions and some metal ions on the retentions of the analytes on the biosorbent were also examined. Separation and preconcentration of Cu, Pb, Fe and Co ions from real samples was achieved quantitatively. The detection limits by 3 sigma for analyte ions were in the range of 0.20-0.75 μg L -1 for aqueous samples and in the range of 2.5-9.4 ng g -1 for solid samples. The validation of the procedure was performed by the analysis of the certified standard reference materials (NRCC-SLRS 4 Riverine Water, SRM 2711 Montana soil and GBW 07605 Tea). The presented method was applied to the determination of analyte ions in green tea, black tea, cultivated mushroom, boiled wheat, rice and soil samples with successfully results

Determination of tumour hypoxia with the PET tracer [18F]EF3: improvement of the tumour-to-background ratio in a mouse tumour model

International Nuclear Information System (INIS)

Christian, Nicolas; Bol, Anne; Bast, Marc de; Labar, Daniel; Lee, John; Mahy, Pierre; Gregoire, Vincent

2007-01-01

The 2-(2-nitroimidazol-1-yl)-N-(3,3,3-trifluoropropyl)acetamide (EF3) is a 2-nitroimidazole derivative which undergoes bioreductive activation under hypoxic conditions. Using the PET tracer [ 18 F]EF3 in mice, tumour-to-muscle ratios ranging from 1.3 to 3.5 were observed. This study investigated the impact of various interventions aimed at increasing [ 18 F]EF3 elimination, thus potentially increasing the tumour-to-noise ratio in mice, by increasing the renal filtration rate (spironolactone, furosemide), decreasing tubular re-absorption (metronidazole, ornidazole, amino acid solution) or stimulating gastro-intestinal elimination (phenobarbital). C3H mice were injected i.v. with an average of 12.95 MBq of [ 18 F]EF3. Drugs were injected i.v. 15 min before the tracer or daily 4 days prior to the experiment (phenobarbital). Anaesthetised mice were imaged from 30 to 300 min with a dedicated animal PET (Mosaic, Philips). Regions of interest were delineated around the tumour, bladder, heart, liver and leg muscle. Radioactivity was expressed as a percentage of injected activity per gram of tissue. Ornidazole decreased the urinary excretion and increased the liver uptake of [ 18 F]EF3, but without causing any changes in the other organs. Phenobarbital significantly increased the liver concentration and decreased radioactivity in blood and muscle without affecting the tracer uptake in tumour. Consequently, a small but non-significant increase in tumour-to-noise ratio was observed. Although some effects were observed with other drugs, they did not modify the tumour-to-noise ratio. Only phenobarbital induced a trend toward an increased tumour-to-noise ratio that could possibly be tested in the clinical situation. (orig.)

Immunosuppression by hypoxic cell radiosensitizers: a phenomenon of potential clinical importance

International Nuclear Information System (INIS)

Rockwell, S.; Kapp, D.S.

1982-01-01

The nitroimidazoles metronidazole, misonidazol, and desmethyl misonidazole are currently undergoing clinical trials as possible adjuncts to radiotherapy. Ongoing clinical trials are evaluating the effectiveness of these agents and also documenting the pharmacokinetics and toxicities of radiosensitizing doses of these drugs in man. A variety of toxic effects have been noted in man, including anorexia, nausea and vomiting, peripheral neuropathy, central nervous system symptoms, ototoxicity, allergy, and fear. Laboratory studies have also suggested that these agents have potential to be mutagenic, carcinogenic, and teratogenic. In the editorial presented, the author attempts to draw attention to an additional toxic effect of nitroimidazoles - the inhibition of cell-mediated immune responses

Adsorption and thermodynamic studies of Cu(II) and Zn(II) on organofunctionalized-kaolinite

International Nuclear Information System (INIS)

Guerra, Denis Lima; Airoldi, Claudio; Sousa, Kaline S. de

2008-01-01

Kaolinite-bearing clay samples from Perus, Sao Paulo state, Brazil, were used for chemical modification process with dimethyl sulfoxide and organofunctionalized with the silyating agent (RO) 3 Si(CH 2 ) 3 NH(CH 2 ) 2 NH 2 in the present study. The resulting material and natural kaolinite were subjected adsorpion process with Cu(II) and Zn(II) from aqueous solution at pH 6.0 and controlated temperature of 298 K. The Langmuir adsorption isotherm model has been applied to fit the experimental data. The results showed that the chemical modification process increases the basal spacing of the natural kaolinite from 0.711 to 0.955 nm. The energetic effects caused by Cu(II) and Zn(II) interactions were determined through calorimetric titration at the solid-liquid interface and gave a net thermal effect that enabled the calculation of the exothermic values and the equilibrium constant

Effectively simultaneous naked-eye detection of Cu(II), Pb(II), Al(III) and Fe(III) using cyanidin extracted from red cabbage as chelating agent

Science.gov (United States)

Khaodee, Warangkhana; Aeungmaitrepirom, Wanlapa; Tuntulani, Thawatchai

Simultaneous determination of Cu(II), Pb(II), Al(III) and Fe(III) using cyanidin as a chelating agent was investigated in terms of both quantitative and qualitative detections. Cyanidin was extracted and purified from red cabbage which is a local plant in Thailand. The selectivity of this method was examined by regulating the pH of cyanidin solution operated together with masking agents. It was found that Cu(II), Pb(II), Al(III) and Fe(III) simultaneously responded with the color change at pH 7, pH 6, pH 5 and pH 4, respectively. KF, DMG and the mixture of KF and DMG were used as masking agents for the determination of Fe(III), Al(III) and Pb(II), respectively. Results from naked-eye detection were evaluated by comparing with those of inductively coupled plasma (ICP), and there was no significant difference noticed. Cyanidin using as a multianalyte reagent could be employed for simultaneous determination of Cu(II), Pb(II), Al(III) and Fe(III) at the lowest concentration at 50, 80, 50 and 200 μM, respectively, by slightly varying pHs. Moreover, the proposed method could be potentially applied for real water samples with simplicity, rapidity, low cost and environmental safety.

Synthesis, spectroscopic and DNA binding ability of Co{sup II}, Ni{sup II}, Cu{sup II} and Zn{sup II} complexes of Schiff base ligand (E)-1-(((1H-benzo[d]imidazol-2-yl)methylimino)methyl)naphthalen-2-ol. X-ray crystal structure determination of cobalt (II) complex

Energy Technology Data Exchange (ETDEWEB)

Yarkandi, Naeema H. [Chemistry Department, Faculty of Applied Science, Umm Al–Qura University, Makkah (Saudi Arabia); El-Ghamry, Hoda A., E-mail: helghamrymo@yahoo.com [Chemistry Department, Faculty of Applied Science, Umm Al–Qura University, Makkah (Saudi Arabia); Chemistry Department, Faculty of Science, Tanta University, Tanta (Egypt); Gaber, Mohamed [Chemistry Department, Faculty of Science, Tanta University, Tanta (Egypt)

2017-06-01

A novel Schiff base ligand, (E)-1-(((1H-benzo[d]imidazol-2-yl)methylimino)methyl)naphthalen-2-ol (HL), has been designed and synthesized in addition to its metal chelates [Co(L){sub 2}]·l2H{sub 2}O, [Ni(L)Cl·(H{sub 2}O){sub 2}].5H{sub 2}O, [Cu(L)Cl] and [Zn(L)(CH{sub 3}COO)]. The structures of the isolated compounds have been confirmed and identified by means of different spectral and physicochemical techniques including CHN analysis, {sup 1}H &{sup 13}C NMR, mass spectral analysis, molar conductivity measurement, UV–Vis, infrared, magnetic moment in addition to TGA technique. The infrared spectral results ascertained that the ligand acts as monobasic tridentate binding to the metal centers via deprotonated hydroxyl oxygen, azomethine and imidazole nitrogen atoms. The UV–Vis, magnetic susceptibility and molar conductivity data implied octahedral geometry for Co(II) & Ni(II) complexes, tetrahedral for Zn(II) complex and square planar for Cu(II) complex. X-ray structural analysis of Co(II) complex 1 has been reported and discussed. Moreover, the type of interaction between the ligand & its complexes towards salmon sperm DNA (SS-DNA) has been examined by the measurement of absorption spectra and viscosity which confirmed that the ligand and its complexes interact with DNA via intercalation interaction as concluded from the values of binding constants (K{sub b}). - Highlights: • Synthesis of Co{sup II}, Ni{sup II}, Cu{sup II} and Zn{sup II} complexes of the Schiff base ligand based on 2-(aminomethyl)benzimidazole moiety. • The constitutions and structures of the ligand and complexes were elucidated. • Molecular structure of Co{sup II} complex was confirmed by single crystal X-ray diffraction method. • The ligand and its complexes interact with SS-DNA via intercalation mods.

EBR-II [Experimental Breeder Reactor-II] system surveillance using pattern recognition software

International Nuclear Information System (INIS)

Mott, J.E.; Radtke, W.H.; King, R.W.

1986-02-01

The problem of most accurately determining the Experimental Breeder Reactor-II (EBR-II) reactor outlet temperature from currently available plant signals is investigated. Historically, the reactor outlet pipe was originally instrumented with 8 temperature sensors but, during 22 years of operation, all these instruments have failed except for one remaining thermocouple, and its output had recently become suspect. Using pattern recognition methods to compare values of 129 plant signals for similarities over a 7 month period spanning reconfiguration of the core and recalibration of many plant signals, it was determined that the remaining reactor outlet pipe thermocouple is still useful as an indicator of true mixed mean reactor outlet temperature. Application of this methodology to investigate one specific signal has automatically validated the vast majority of the 129 signals used for pattern recognition and also highlighted a few inconsistent signals for further investigation

Adsorption of lead(II) and copper(II) on activated carbon by complexation with surface functional groups

International Nuclear Information System (INIS)

Pesavento, Maria; Profumo, Antonella; Alberti, Giancarla; Conti, Fabio

2003-01-01

The adsorption of lead(II) and copper(II) on an activated carbon (Filtrasorb 300, Chemviron) was characterized assuming that it takes place by formation of complexes with functional groups, present in the activated carbon. Their concentration and conditional adsorption coefficients were determined for each metal by titration of the carbon in suspension in aqueous phase, at constant acidity, with the metal itself. For each titration point, the concentration of the metal in the solution phase after equilibration was determined, and the data were processed by the Ruzic linearization method, to obtain the concentration of the active sites involved in the sorption, and the conditional constant. The effect of the pH was also examined, in the range 4-6, obtaining that the adsorption increases at increasing pH. The protonation and adsorption constants were determined from the conditional adsorption coefficients obtained at the different acidities. The concentration of the active sites is 0.023 and 0.042 mmol g -1 , and the protonation constants are 1.0x10 6 and 4.6x10 4 M -1 for Pb(II) and Cu(II). The corresponding adsorption constants are respectively 1.4x10 5 and 6.3x10 3 M -1 . All the parameters are affected by a large uncertainty, probably due to the heterogeneity of the active groups in the activated carbon. Even if so, these parameters make it possible a good prediction of the adsorption in a wide range of conditions. Other sorption mechanism can be set up at different conditions, in particular at different pH, as it has been demonstrated in the case of copper(II)

Adsorption of lead(II) and copper(II) on activated carbon by complexation with surface functional groups

Energy Technology Data Exchange (ETDEWEB)

Pesavento, Maria; Profumo, Antonella; Alberti, Giancarla; Conti, Fabio

2003-03-17

The adsorption of lead(II) and copper(II) on an activated carbon (Filtrasorb 300, Chemviron) was characterized assuming that it takes place by formation of complexes with functional groups, present in the activated carbon. Their concentration and conditional adsorption coefficients were determined for each metal by titration of the carbon in suspension in aqueous phase, at constant acidity, with the metal itself. For each titration point, the concentration of the metal in the solution phase after equilibration was determined, and the data were processed by the Ruzic linearization method, to obtain the concentration of the active sites involved in the sorption, and the conditional constant. The effect of the pH was also examined, in the range 4-6, obtaining that the adsorption increases at increasing pH. The protonation and adsorption constants were determined from the conditional adsorption coefficients obtained at the different acidities. The concentration of the active sites is 0.023 and 0.042 mmol g{sup -1}, and the protonation constants are 1.0x10{sup 6} and 4.6x10{sup 4} M{sup -1} for Pb(II) and Cu(II). The corresponding adsorption constants are respectively 1.4x10{sup 5} and 6.3x10{sup 3} M{sup -1}. All the parameters are affected by a large uncertainty, probably due to the heterogeneity of the active groups in the activated carbon. Even if so, these parameters make it possible a good prediction of the adsorption in a wide range of conditions. Other sorption mechanism can be set up at different conditions, in particular at different pH, as it has been demonstrated in the case of copper(II)

Effect of Cu(II), Cd(II) and Zn(II) on Pb(II) biosorption by algae Gelidium-derived materials.

Science.gov (United States)

Vilar, Vítor J P; Botelho, Cidália M S; Boaventura, Rui A R

2008-06-15

Biosorption of Pb(II), Cu(II), Cd(II) and Zn(II) from binary metal solutions onto the algae Gelidium sesquipedale, an algal industrial waste and a waste-based composite material was investigated at pH 5.3, in a batch system. Binary Pb(II)/Cu(II), Pb(II)/Cd(II) and Pb(II)/Zn(II) solutions have been tested. For the same equilibrium concentrations of both metal ions (1 mmol l(-1)), approximately 66, 85 and 86% of the total uptake capacity of the biosorbents is taken by lead ions in the systems Pb(II)/Cu(II), Pb(II)/Cd(II) and Pb(II)/Zn(II), respectively. Two-metal results were fitted to a discrete and a continuous model, showing the inhibition of the primary metal biosorption by the co-cation. The model parameters suggest that Cd(II) and Zn(II) have the same decreasing effect on the Pb(II) uptake capacity. The uptake of Pb(II) was highly sensitive to the presence of Cu(II). From the discrete model it was possible to obtain the Langmuir affinity constant for Pb(II) biosorption. The presence of the co-cations decreases the apparent affinity of Pb(II). The experimental results were successfully fitted by the continuous model, at different pH values, for each biosorbent. The following sequence for the equilibrium affinity constants was found: Pb>Cu>Cd approximately Zn.

SPITZER ANALYSIS OF H II REGION COMPLEXES IN THE MAGELLANIC CLOUDS: DETERMINING A SUITABLE MONOCHROMATIC OBSCURED STAR FORMATION INDICATOR

International Nuclear Information System (INIS)

Lawton, B.; Gordon, K. D.; Meixner, M.; Sewilo, M.; Shiao, B.; Babler, B.; Bracker, S.; Meade, M.; Block, M.; Engelbracht, C. W.; Misselt, K.; Bolatto, A. D.; Carlson, L. R.; Hora, J. L.; Robitaille, T.; Indebetouw, R.; Madden, S. C.; Oey, M. S.; Oliveira, J. M.; Vijh, U. P.

2010-01-01

H II regions are the birth places of stars, and as such they provide the best measure of current star formation rates (SFRs) in galaxies. The close proximity of the Magellanic Clouds allows us to probe the nature of these star forming regions at small spatial scales. To study the H II regions, we compute the bolometric infrared flux, or total infrared (TIR), by integrating the flux from 8 to 500 μm. The TIR provides a measure of the obscured star formation because the UV photons from hot young stars are absorbed by dust and re-emitted across the mid-to-far-infrared (IR) spectrum. We aim to determine the monochromatic IR band that most accurately traces the TIR and produces an accurate obscured SFR over large spatial scales. We present the spatial analysis, via aperture/annulus photometry, of 16 Large Magellanic Cloud (LMC) and 16 Small Magellanic Cloud (SMC) H II region complexes using the Spitzer Space Telescope's IRAC (3.6, 4.5, 8 μm) and MIPS (24, 70, 160 μm) bands. Ultraviolet rocket data (1500 and 1900 A) and SHASSA Hα data are also included. All data are convolved to the MIPS 160 μm resolution (40 arcsec full width at half-maximum), and apertures have a minimum radius of 35''. The IRAC, MIPS, UV, and Hα spatial analysis are compared with the spatial analysis of the TIR. We find that nearly all of the LMC and SMC H II region spectral energy distributions (SEDs) peak around 70 μm at all radii, from ∼10 to ∼400 pc from the central ionizing sources. As a result, we find the following: the sizes of H II regions as probed by 70 μm are approximately equal to the sizes as probed by TIR (∼70 pc in radius); the radial profile of the 70 μm flux, normalized by TIR, is constant at all radii (70 μm ∼ 0.45TIR); the 1σ standard deviation of the 70 μm fluxes, normalized by TIR, is a lower fraction of the mean (0.05-0.12 out to ∼220 pc) than the normalized 8, 24, and 160 μm normalized fluxes (0.12-0.52); and these results are the same for the LMC and the

The tetracycline resistance determinant Tet 39 and the sulphonamide resistance gene sulII are common among resistant Acinetobacter spp. isolated from integrated fish farms in Thailand

DEFF Research Database (Denmark)

Agersø, Yvonne; Petersen, Andreas

2007-01-01

Objectives: To determine the genetic basis for tetracycline and sulphonamide resistance and the prevalence of class I and II integrons in oxytetracycline-resistant Acinetobacter spp. from integrated fish farms in Thailand. Methods: A total of 222 isolates were screened for tetracycline resistance...... and Southern blots with sulII and tet(39) probes were performed on selected isolates. Results: The recently identified tetracycline resistance gene tet(39) was demonstrated in 75% (166/222) of oxytetracycline-resistant Acinetobacter spp. from integrated fish farms in Thailand. Isolates that were also...

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

Science.gov (United States)

Ensafi, Ali A; Shiraz, A Zendegi

2008-02-11

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

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

International Nuclear Information System (INIS)

Ensafi, Ali A.; Shiraz, A. Zendegi

2008-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2008-02-11

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

Power and power-to-flow reactivity transfer functions in EBR-II [Experimental Breeder Reactor II] fuel

International Nuclear Information System (INIS)

Grimm, K.N.; Meneghetti, D.

1989-01-01

Reactivity transfer functions are important in determining the reactivity history during a power transient. Overall nodal transfer functions have been calculated for different subassembly types in the Experimental Breeder Reactor II (EBR-II). Steady-state calculations for temperature changes and, hence, reactivities for power changes have been separated into power and power-to-flow-dependent terms. Axial nodal transfer functions separated into power and power-to-flow-dependent components are reported in this paper for a typical EBR-II fuel pin. This provides an improved understanding of the time dependence of these components in transient situations

A simple and low cost dual-wavelength β-correction spectrophotometric determination and speciation of mercury(II) in water using chromogenic reagent 4-(2-thiazolylazo) resorcinol

Science.gov (United States)

Al-Bagawi, A. H.; Ahmad, W.; Saigl, Z. M.; Alwael, H.; Al-Harbi, E. A.; El-Shahawi, M. S.

2017-12-01

The most common problems in spectrophotometric determination of various complex species originate from the background spectral interference. Thus, the present study aimed to overcome the spectral matrix interference for the precise analysis and speciation of mercury(II) in water by dual-wavelength β-correction spectrophotometry using 4-(2-thiazolylazo) resorcinol (TAR) as chromogenic reagent. The principle was based on measuring the correct absorbance for the formed complex of mercury(II) ions with TAR reagent at 547 nm (lambda max). Under optimized conditions, a linear dynamic range of 0.1-2.0 μg mL- 1 with correlation coefficient (R2) of 0.997 were obtained with lower limits of detection (LOD) of 0.024 μg mL- 1 and limit of quantification (LOQ) of 0.081 μg mL- 1. The values of RSD and relative error (RE) obtained for β-correction method and single wavelength spectrophotometry were 1.3, 1.32% and 4.7, 5.9%, respectively. The method was validated in tap and sea water in terms of the data obtained from inductively coupled plasma-optical emission spectrometry (ICP-OES) using student's t and F tests. The developed methodology satisfactorily overcomes the spectral interference in trace determination and speciation of mercury(II) ions in water.

Removal of Ni(II), Zn(II) and Pb(II) ions from single metal aqueous solution using rice husk-based activated carbon

Energy Technology Data Exchange (ETDEWEB)

Taha, Mohd F., E-mail: faisalt@petronas.com.my; Shaharun, Maizatul S. [Fundamental and Applied Sciences Department, Universiti Teknologi PETRONAS, Bandar Seri Iskandar, 31750, Perak Darul Ridzuan (Malaysia); Shuib, Anis Suhaila, E-mail: anisuha@petronas.com.my; Borhan, Azry [Chemical Engineering Department, Universiti Teknologi PETRONAS, Bandar Seri Iskandar, 31750, Perak Darul Ridzuan (Malaysia)

2014-10-24

An attempt was made to investigate the potential of rice husk-based activated carbon as an alternative low-cost adsorbent for the removal of Ni(II), Zn(II) and Pb(II) ions from single aqueous solution. Rice husk-based activated carbon was prepared via treatment of rice husk with NaOH followed by the carbonization process at 400°C for 2 hours. Three samples, i.e. raw rice husk, rice husk treated with NaOH and rice husk-based activated carbon, were analyzed for their morphological characteristics using field-emission scanning electron microscope/energy dispersive X-ray (FESEM/EDX). These samples were also analyzed for their carbon, hydrogen, nitrogen, oxygen and silica contents using CHN elemental analyzer and FESEM/EDX. The porous properties of rice husk-based activated carbon were determined by Brunauer-Emmett-Teller (BET) surface area analyzer, and its surface area and pore volume were 255 m{sup 2}/g and 0.17 cm{sup 2}/g, respectively. The adsorption studies for the removal of Ni(II), Zn(II) and Pb(II) ions from single metal aqueous solution were carried out at a fixed initial concentration of metal ion (150 ppm) with variation amount of adsorbent (rice husk-based activated carbon) as a function of varied contact time at room temperature. The concentration of each metal ion was analyzed using atomic absorption spectrophotometer (AAS). The results obtained from adsorption studies indicate the potential of rice husk as an economically promising precursor for the preparation of activated carbon for removal of Ni(II), Zn(II) and Pb(II) ions from single aqueous solution. Isotherm and kinetic model analyses suggested that the experimental data of adsorption studies fitted well with Langmuir, Freundlich and second-order kinetic models.

Physicochemical properties of 3,4,5-trimethoxybenzoates of Mn(II, Co(II, Ni(II and Zn(II

Directory of Open Access Journals (Sweden)

W. FERENC

2005-09-01

Full Text Available The complexes of Mn(II, Co(II, Ni(II, Cu(II and Zn(II with 3,4,5-trimethoxybenzoic acid anion of the formula: M(C10H11O52·nH2O, where n = 6 for Ni(II, n = 1 for Mn(II, Co(II, Cu(II, and n = 0 for Zn, have been synthesized and characterized by elemental analysis, IR spectroscopy, X–ray diffraction measurements, thermogravimetry and magnetic studies. They are crystalline compounds characterized by various symmetry. They decompose in various ways when heated in air to 1273 K. At first, they dehydrate in one step and form anhydrous salts. The final products of decomposition are oxides of the respective metals (Mn2O3, Co3O4, NiO, CuO, ZnO. The solubilities of the analysed complexes in water at 293 K are in the orders of 10-2 – 10-4 mol dm-3. The magnetic susceptibilities of the Mn(II, Co(II, Ni(II and Cu(II complexes were measured over the range of 76–303 K and the magnetic moments were calculated. The results show that the 3,4,5-trimethoxybenzoates of Mn(II, Co(II and Ni(II are high-spin complexes but that of Cu(II forms a dimer [Cu2(C10H11O54(H2O2]. The carboxylate groups bind as monodentate or bidentate chelating or bridging ligands.

Photosystem II electron flow as a measure for phytoplankton gross primary production = [Fotosysteem II elektronentransport als een maat voor de bruto primaire produktie van fytoplankton

NARCIS (Netherlands)

Geel, C.

1997-01-01

Saturating pulse fluorescence measurements, well known from studies of higher plants for determination of photosystem II (PS II) characteristics, were applied to cultures of the green alga Dunaliella teitiolecta (Chapter 2). The actual efficiency of PS II (φ _PS

Extractive Spectrophotometric Determination of Nortriptyline Hydrochloride Using Sudan II, IV and Black B

Directory of Open Access Journals (Sweden)

A. S. Amin

2017-08-01

formulations based on the formation of ion-pair complexes with sudun II (SII, sudan (IV (SIV and sudan black B (SBB. The selectivity of the method was improved through extraction with chloroform. The optimum conditions for complete extracted colour development were assessed. The absorbance measurements were made at 534, 596 and 649 nm for SII, SIV and SBB complexes, respectively. The calibration graph was linear in the ranges 0.5- 280. 0.5- 37.5 and 0.5 – 31.0 μg ml−1 of the drug usiny the same reagents, respectively. The precision of the procedure was checked by calculating the relative standard deviation of ten replicate determinations on 15 μg ml−1 of nortriptyline HCI and was found to be 1.7, 1.3 and 1.55% using SII, SIV, and SBB complexes, respectively. The molar absorptivity and Sandell sensitivity for each ion-pair were calculated. The proposed methods were successfully applied to the deterniination of pure nortriptyline HCI and in pharmaceutical formulations, and the results demonstrated that the method is equally accurate, precise and reproducible as the official method.

Synthesis and spectral studies of manganese(II), cobalt(II), nickel(II), copper(II), zinc(II), cadmium(II) and mercury(II) complexes of 4-oxo-4H-1-benzopyran-3-carboxaldehyde hydrazone derivatives

International Nuclear Information System (INIS)

Nawar, N.; Khattab, M.A.; Bekheit, M.M.; El-Kaddah, A.H.

1996-01-01

A few complexes of Mn(II), Co(II), Ni(II), Cu(II), Zn(II), Cd(II) and Hg(II) with 4-oxo-4H-1-benzopyran-3-(carboxaldehyde-4-chlorobenzylhydrazone) (BCBH) and 4-oxo-4H-1-benzopyran-3-(carboxaldehyde-4-methylbenzylhydrazone) (BMBH) have been synthesised and characterized by elemental analysis, molar conductivities, magnetic measurements and infrared (IR) and visible spectral studies. The IR spectra show that BCBH and BMBH behave as bidentate ligands either in the keto or enol form. (author). 24 refs., 2 tabs

Synthesis, Characterization, and Biological Activity of Mn(II, Fe(II, Co(II, Ni(II, Cu(II, Zn(II, and Cd(II Complexes of N-Thiophenoyl-N′-Phenylthiocarbohydrazide

Directory of Open Access Journals (Sweden)

M. Yadav

2013-01-01

Full Text Available Mn(II, Fe(II, Co(II, Ni(II, Cu(II, Zn(II, and Cd(II complex of N-thiophenoyl -N′-phenylthiocarbohydrazide (H2 TPTH have been synthesized and characterized by elemental analysis, magnetic susceptibility measurements, infrared, NMR, electronic, and ESR spectral studies. The complexes were found to have compositions [Mn(H TPTH2], [Co(TPTH (H2O2], [Ni(TPTH (H2O2], [Cu(TPTH], [Zn(H TPTH], [Cd(H TPTH2], and [Fe(H TPTH2(EtOH]. The magnetic and electronic spectral studies suggest square planar geometry for [Cu(TPTH], tetrahedral geometry for [Zn(TPTH] and [Cd(H TPTH2], and octahedral geometry for rest of the complexes. The infrared spectral studies of the 1 : 1 deprotonated complexes suggest bonding through enolic oxygen, thiolato sulfur, and both the hydrazinic nitrogens. Thus, H2TPTH acts as a binegative tetradentate ligand. H2 TPTH and its metal complexes have been screened against several bacteria and fungi.

TYPE II-P SUPERNOVAE FROM THE SDSS-II SUPERNOVA SURVEY AND THE STANDARDIZED CANDLE METHOD

International Nuclear Information System (INIS)

D'Andrea, Chris B.; Sako, Masao; Dilday, Benjamin; Jha, Saurabh; Frieman, Joshua A.; Kessler, Richard; Holtzman, Jon; Konishi, Kohki; Yasuda, Naoki; Schneider, D. P.; Sollerman, Jesper; Wheeler, J. Craig; Cinabro, David; Nichol, Robert C.; Lampeitl, Hubert; Smith, Mathew; Atlee, David W.; Bassett, Bruce; Castander, Francisco J.; Goobar, Ariel

2010-01-01

We apply the Standardized Candle Method (SCM) for Type II Plateau supernovae (SNe II-P), which relates the velocity of the ejecta of a SN to its luminosity during the plateau, to 15 SNe II-P discovered over the three season run of the Sloan Digital Sky Survey-II Supernova Survey. The redshifts of these SNe-0.027 0.01) as all of the current literature on the SCM combined. We find that the SDSS SNe have a very small intrinsic I-band dispersion (0.22 mag), which can be attributed to selection effects. When the SCM is applied to the combined SDSS-plus-literature set of SNe II-P, the dispersion increases to 0.29 mag, larger than the scatter for either set of SNe separately. We show that the standardization cannot be further improved by eliminating SNe with positive plateau decline rates, as proposed in Poznanski et al. We thoroughly examine all potential systematic effects and conclude that for the SCM to be useful for cosmology, the methods currently used to determine the Fe II velocity at day 50 must be improved, and spectral templates able to encompass the intrinsic variations of Type II-P SNe will be needed.

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

Directory of Open Access Journals (Sweden)

Jameel Ahmed Baig

2013-01-01

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

Effect of diabetes and insulin on the turnover of hexokinase II in the skeletal muscle

International Nuclear Information System (INIS)

Frank, S.K.

1985-01-01

An ELISA procedure was developed to determine the amount of hexokinase II protein in the skeletal muscle extracts of rats, and immunoprecipitation was utilized to determine the hexokinase II activity. Both hexokinase II activity and the amount of hexokinase II protein decreased in the diabetic rat. Both increased toward normal treatment with insulin. The rate of synthesis of hexokinase II in the skeletal muscle was determined by the rate of incorporation of [ 3 H] leucine into hexokinase II. This rate was compared to that of the total cytosolic proteins to determine if the rate of hexokinase II synthesis was specifically affected by insulin. This relative rate of synthesis of hexokinase II was found to be approximately two times greater in the normal as compared to the diabetic rat. The apparent rate constants of degradation were determined using a double-isotope technique and from these constants it was possible to calculate the apparent half-lives. The apparent half-life was approximately 2.3 times greater in the normal compared to the diabetic rat and 2 times greater in the insulin-treated compared to the diabetic

Radioiodination of melagenine-II with I-125 (preliminary study)

International Nuclear Information System (INIS)

Caso, R.; Ruiz, M.

1996-01-01

Radioiodination of Melagenine-II with I-125 farmacokinetic studies was made, using Chloramine-T method. Radiochemical purity and stability of the labelled product were determined by radiochromatography. The labelled Melagenine-II showed two radioactive fractions

Chemical speciation of Pb(II, Cd(II, Hg(II, Co(II, Ni(II, Cu(II and Zn(II binary complexes of l-methionine in 1,2-propanediol-water mixtures

Directory of Open Access Journals (Sweden)

M. Padma Latha

2007-04-01

Full Text Available Chemical speciation of Pb(II, Cd(II, Hg(II, Co(II, Ni(II, Cu(II and Zn(II complexes of L-methionine in 0.0-60 % v/v 1,2-propanediol-water mixtures maintaining an ionic strength of 0.16 M at 303 K has been studied pH metrically. The active forms of ligand are LH2+, LH and L-. The predominant species detected are ML, MLH, ML2, ML2H, ML2H2 and MLOH. Models containing different numbers of species were refined by using the computer program MINIQUAD 75. The best-fit chemical models were arrived at based on statistical parameters. The trend in variation of complex stability constants with change in the dielectric constant of the medium is explained on the basis of electrostatic and non-electrostatic forces.

Study of physicochemical parameters for cadmium (II) and mercury (II) phytoremediation using the specie Eichhornia Crassipes (water hyacinth)

International Nuclear Information System (INIS)

Poma Llantoy, Victor R.; Valderrama Negron, Ana C.

2014-01-01

In this work, the studies were performed to measure the sorption capacity of metal ions Cd (II) and Hg (II) using the specie Eichhornia crassipes (water hyacinth). This study includes assays where the nutrient concentration, the pH and the metal ion concentration were optimized. These tests were carried out at room temperature and with aqueous solutions of Cd (II), Hg (II), in which the samples of Eichhornia crassipes were placed. To confirm the removal of these metals, the waste solutions after the treatment with the Water Hyacinth species were treated using the method APHA 3030-e. However, Eichhornia crassipes samples were treated using the EPA 200.3 method. The concentration of Cd (II) was determined by an ICP-OES spectrometer and Hg (II), by an atomic absorption spectrophotometer. The results showed: Optimal dosage 1 mL of A and 0,5 mL of B, optimum pH 5, optimum concentration of Cd (II) and Hg (II) 5 mg/L for each ion. With these parameters, it was started the removal of 5 mg/L of the metal ions contained in 1 L of solution. Being the percentages of sorption 16,56% for Cd (II) and 15,6% for Hg (II) after a period of 7 days. (author)

Boletus edulis loaded with γ-Fe2O3 nanoparticles as a magnetic sorbent for preconcentration of Co(II) and Sn(II) prior to their determination by ICP-OES.

Science.gov (United States)

Ozdemir, Sadin; Serkan Yalcin, M; Kilinc, Ersin; Soylak, Mustafa

2017-12-20

The authors show that the fungus Boletus edulis loaded with γ-Fe 2 O 3 nanoparticles is a viable sorbent for magnetic solid phase extraction of trace levels of Co(II) and Sn(II). The surface structure of immobilized magnetized B. edulis was characterized by FT-IR, SEM and EDX. Experimental parameters were optimized. Following elution with 1 M HCl, the ions were quantified by ICP-OES. The limits of detection are 21 pg·mL -1 for Co(II), and 19 pg·mL -1 for Sn(II). The preconcentration factors are 100 for both ions. The sorption capacities of the sorbent are 35.8 mg·g -1 for Co(II) and 29.6 mg·g -1 for Sn(II). The method was applied to the analysis of certificated reference materials and gave ≥95% recoveries with low RSDs. It was also successfully applied to the quantification of Co(II) and Sn(II) in spiked environmental and food samples. Graphical abstract The fungus Boletus edulis loaded with γ-Fe 2 O 3 nanoparticles is a viable biosorbent for magnetic solid phase extraction (MSPE) of trace levels of Co(II) and Sn(II). The surface structure of immobilized magnetized B. edulis was characterized by FT-IR, SEM and EDX. Experimental parameters were optimized.

DNA methyltransferase inhibitor CDA-II inhibits myogenic differentiation

International Nuclear Information System (INIS)

Chen, Zirong; Jin, Guorong; Lin, Shuibin; Lin, Xiumei; Gu, Yumei; Zhu, Yujuan; Hu, Chengbin; Zhang, Qingjiong; Wu, Lizi; Shen, Huangxuan

2012-01-01

Highlights: ► CDA-II inhibits myogenic differentiation in a dose-dependent manner. ► CDA-II repressed expression of muscle transcription factors and structural proteins. ► CDA-II inhibited proliferation and migration of C2C12 myoblasts. -- Abstract: CDA-II (cell differentiation agent II), isolated from healthy human urine, is a DNA methyltransferase inhibitor. Previous studies indicated that CDA-II played important roles in the regulation of cell growth and certain differentiation processes. However, it has not been determined whether CDA-II affects skeletal myogenesis. In this study, we investigated effects of CDA-II treatment on skeletal muscle progenitor cell differentiation, migration and proliferation. We found that CDA-II blocked differentiation of murine myoblasts C2C12 in a dose-dependent manner. CDA-II repressed expression of muscle transcription factors, such as Myogenin and Mef2c, and structural proteins, such as myosin heavy chain (Myh3), light chain (Mylpf) and MCK. Moreover, CDA-II inhibited C1C12 cell migration and proliferation. Thus, our data provide the first evidence that CDA-II inhibits growth and differentiation of muscle progenitor cells, suggesting that the use of CDA-II might affect skeletal muscle functions.

Clinical significance of combined determination of the changes of serum IGF-II, CA19-9 and AFP levels after intervention therapy in patients with primary hepatic cancer

International Nuclear Information System (INIS)

Wang Zhong

2007-01-01

Objective: To investigate the clinical significance of changes of serum IGF-II, CA19-9 and AFP levels after intervention therapy in patients with primary hepatic cancer. Methods: Serum levels of IGF-II, CA19-9 and AFP (with RIA) were repeatedly determined in 35 patients with primary hepatic cancer before intervention therapy, 1 month after intervention therapy and 6 months after intervention therapy as well as in 30 controls. Results: Before intervention therapy, serum levels of IGF-II, CA19-9 and AFP in the patients were significantly higher than those in the controls (P <0.01 ). One month after intervention therapy, all the serum levels were approaching normal. Six months later, the levels in the patients without recurrence remained normal. However, the levels in the 6 patients with recurrence returued to those before intervention therapy again. Conclusion: Changes of serum IGF-II, CA19-9 and AFP levels are closely related to the tumor burden and may reflect the presence of recurrence. (authors)

Adsorptive stripping voltammetric determination of nitroimidazole derivative on multiwalled carbon nanotube modified electrodes: influence of size and functionalization of nanotubes

Energy Technology Data Exchange (ETDEWEB)

Jara-Ulloa, Paola; Canete-Rosales, Paulina; Nunez-Vergara, Luis J; Squella, Juan A., E-mail: asquella@ciq.uchile.c [University of Chile, Santiago (Chile). Chemical and Pharmaceutical Sciences Faculty. Bioelectrochemistry Lab.

2011-07-01

1-Methyl-4-nitro-2-bromine methylimidazole (4-NimMeBr), was electrochemically reduced on mercury, glassy carbon and multiwalled carbon nanotubes (MWCNT) modified electrodes. 4-NimMeBr was adsorbed on the MWCNT modified electrode thus permitting the implementation of an adsorptive stripping voltammetric (ASV) method. We have used 4-NimMeBr as a prototype electroactive nitro compound to study the effect of both the size of the nanotubes and its functionalization by oxidation. The oxidized MWCNT forms better dispersions than the non-oxidized, producing electrode surface with higher density of MWCNT as was determined by electrochemical mapping using scanning electrochemical microscopy (SECM). Under the optimized conditions, the peak current was proportional to the concentration of 4-NimMeBr in the range of 10{sup -6} mol L{sup -1} to 10{sup -4} mol L{sup -1} with detection and quantification limits of 4.41 x 10{sup -6} mol L{sup -1} and 6.21 x 10{sup -6} mol L{sup -1}, respectively. The sensibility of bare electrode was 0.01 {mu}A per mmol L{sup -1}, which was lower than the value of 5.34 and 6.97 mA per mmol L{sup -1} obtained using short and large oxidized MWCNT, respectively. (author)

cobalt (ii), nickel (ii)

African Journals Online (AJOL)

DR. AMINU

Department of Chemistry Bayero University, P. M. B. 3011, Kano, Nigeria. E-mail: hnuhu2000@yahoo.com. ABSTRACT. The manganese (II), cobalt (II), nickel (II) and .... water and common organic solvents, but are readily soluble in acetone. The molar conductance measurement [Table 3] of the complex compounds in.

Inhibition of X-ray-induced potentially lethal damage (PLD) repair in aerobic plateau-phase Chinese hamster cells by misonidazole

International Nuclear Information System (INIS)

Brown, D.M.

1984-01-01

The effect of the 2-nitroimidazole radiosensitizer misonidazole (MISO) and the hydrophilic analog SR-2508 on the repair of X-ray-induced potentially lethal damage (PLD) was studied in plateau-phase Chinese Hamster ovary (HA-1) cells. It was found that although MISO does not radiosensitize aerobic cells, it inhibits the repair of PLD. However, under hypoxic conditions, MISO has no effect on PLD repair. The major portion of the inhibition of PLD repair in aerobic cells requires the presence of MISO only during irradiation; little or no additional inhibition occurs when MISO is present during the postirradiation repair period. Also, treatment of aerobic cells with 5 mM MISO for either 5 or 30 min prior to irradiation is equally inhibitory. This suggests that the presence of MISO in some way modifies the initial lesion under aerobic conditions since it does not increase cell killing as determined by immediate plating but inhibits subsequent repair. The inhibition is concentration dependent; 0.5 mM MISO inhibits PLD repair by one-half while 5-10 mM totally inhibits the repair measured 6 hr postirradiation. This phenomenon suggests that radiosensitization of tissue in vivo by MISO and other 2-nitroimidazoles may not be unequivocal proof of the presence of hypoxic cells

Colorimetric determination of reducing normality in the Purex process

International Nuclear Information System (INIS)

Baumann, E.W.

1983-07-01

Adjustment of the valence state of plutonium from extractable Pu(IV) to nonextractable Pu(III) in the Purex process is accomplished by addition of reductants such as Fe(II), hydroxylamine nitrate (HAN), or U(IV). To implement on-line monitoring of this reduction step for improved process control at the Savannah River Plant, a simple colorimetric method for determining excess reductant (reducing normality) was developed. The method is based on formation of a colored complex of Fe(II) with FerroZine (Hach Chemical Company). The concentration of Fe(II) is determined directly. The concentration of HAN or U(IV), in addition to Fe(II), is determined indirectly as Fe(II), produced through reduction of Fe(III). Experimental conditions for a HAN-Fe(III) reaction of known stoichiometry were established. The effect of hydrazine, which stabilizes U(IV), was also determined. Real-time measurements of color development were made that simulated on-line performance. A laboratory analytical procedure is included. 5 references, 8 figures

Synthesis, spectroscopic and DNA binding ability of CoII, NiII, CuII and ZnII complexes of Schiff base ligand (E)-1-(((1H-benzo[d]imidazol-2-yl)methylimino)methyl)naphthalen-2-ol. X-ray crystal structure determination of cobalt (II) complex.

Science.gov (United States)

Yarkandi, Naeema H; El-Ghamry, Hoda A; Gaber, Mohamed

2017-06-01

A novel Schiff base ligand, (E)-1-(((1H-benzo[d]imidazol-2-yl)methylimino)methyl)naphthalen-2-ol (HL), has been designed and synthesized in addition to its metal chelates [Co(L) 2 ]·l2H 2 O, [Ni(L)Cl·(H 2 O) 2 ].5H 2 O, [Cu(L)Cl] and [Zn(L)(CH 3 COO)]. The structures of the isolated compounds have been confirmed and identified by means of different spectral and physicochemical techniques including CHN analysis, 1 H & 13 C NMR, mass spectral analysis, molar conductivity measurement, UV-Vis, infrared, magnetic moment in addition to TGA technique. The infrared spectral results ascertained that the ligand acts as monobasic tridentate binding to the metal centers via deprotonated hydroxyl oxygen, azomethine and imidazole nitrogen atoms. The UV-Vis, magnetic susceptibility and molar conductivity data implied octahedral geometry for Co(II) & Ni(II) complexes, tetrahedral for Zn(II) complex and square planar for Cu(II) complex. X-ray structural analysis of Co(II) complex 1 has been reported and discussed. Moreover, the type of interaction between the ligand & its complexes towards salmon sperm DNA (SS-DNA) has been examined by the measurement of absorption spectra and viscosity which confirmed that the ligand and its complexes interact with DNA via intercalation interaction as concluded from the values of binding constants (K b ). Copyright © 2017 Elsevier B.V. All rights reserved.

A Survey of Optometry Graduates to Determine Practice Patterns: Part II: Licensure and Practice Establishment Experiences.

Science.gov (United States)

Bleimann, Robert L.; Smith, Lee W.

1985-01-01

A summary of Part II of a two-volume study of optometry graduates conducted by the Association of Schools and Colleges of Optometry is presented. Part II includes the analysis of the graduates' licensure and practice establishment experiences. (MLW)

CATALYTIC KINETIC SPECTROPHOTOMETRIC DETERMINATION ...

African Journals Online (AJOL)

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acetylchlorophosphonazo(CPApA) by hydrogen peroxide in 0.10 M phosphoric acid. A novel catalytic kinetic-spectrophotometric method is proposed for the determination of copper based on this principle. Copper(II) can be determined spectrophotometrically ...

A Novel Potentiometric Sensor Based on 1,2-Bis(N’-benzoylthioureido)benzene and Reduced Graphene Oxide for Determination of Lead (II) Cation in Raw Milk

International Nuclear Information System (INIS)

Abraham, Abigail Asha; Rezayi, Majid; Manan, Ninie S.A.; Narimani, Leila; Rosli, Ahmad Nazmi Bin; Alias, Yatimah

2015-01-01

We have developed a highly sensitive and selective potentiometric PVC-membrane sensor for lead (II) cation. A glassy carbon electrode (GCE) was modified with synthesized 1,2-Bis(N’-benzoylthioureido) benzene (BBTB) as an ionophore and reduced graphene oxide (RGO), and this material was characterized by scanning electron microscopy. The sensor shows sensitive and highly selective response to Pb(II) ion with a linear range from 6.31 × 10 −8 to 3.98 × 10 −2 M, Nernstian slope of 30.37 ± 0.62 mV per decade and a detection limit of 2.51 × 10 −8 M. The proposed sensor could be used in a pH range of 4.0–8.0. Selectivity coefficients were determined for known common cations by applying the match potential method (MPM). The sensor was successfully applied to monitor Pb(II) in raw milk and in potentiometric titration of Pb 2+ ions. The structure of BBTB ligand and its complexation with some common cations were investigated by using quantum mechanical DFT calculations. Lead (II) cation showed prominent affinity to the BBTB carrier

Synthesis and structural characterisation of iron(II) and copper(II) diphosphates containing flattened metal oxotetrahedra

Energy Technology Data Exchange (ETDEWEB)

Keates, Adam C. [School of Chemistry, University of Southampton, Southampton, Hampshire SO17 1B,. UK (United Kingdom); Wang, Qianlong [Department of Chemistry, University of Bath, Claverton Down, Bath, BA2 7AY (United Kingdom); Weller, Mark T., E-mail: m.t.weller@bath.ac.uk [Department of Chemistry, University of Bath, Claverton Down, Bath, BA2 7AY (United Kingdom)

2014-02-15

Single crystal and bulk polycrystalline forms of K{sub 2}MP{sub 2}O{sub 7} (M=Fe(II), Cu(II)) have been synthesised and their structures determined from single crystal X-ray diffraction data. Both compounds crystallize in the tetragonal system, space group P-42{sub 1}m. Their structures are formed from infinite sheets of linked oxopolyhedra of the stoichiometry [MP{sub 2}O{sub 7}]{sup 2−} with potassium cations situated between the layers. The MO{sub 4} tetrahedra share oxygen atoms with [P{sub 2}O{sub 7}]{sup 4−} diphosphate groups and the potassium ions have KO{sub 8} square prismatic geometry. In both compounds the M(II) centre has an unusual strongly flattened, tetrahedral coordination to oxygen, as a result of the Jahn–Teller (JT) effect for the high spin d{sup 6} Fe(II) and p-orbital mixing or a second order JT effect for d{sup 9} Cu(II) centres in four fold coordination. The uncommon transition metal ion environments found in these materials are reflected in their optical absorption spectra and magnetism data. - Graphical abstract: The structures of the tetragonal polymorphs of K{sub 2}MP{sub 2}O{sub 7}, M=Cu(II), Fe(II), consist of infinite sheets of stoichiometry [MP{sub 2}O{sub 7}]{sup 2−}, formed from linked pyrophosphate groups and MO{sub 4} tetrahedra, separated by potassium ions. In both compounds the unusual tetrahedral coordination of the M(II) centre is strongly flattened as a result of Jahn–Teller (JT) effects for high spin, d{sup 6} Fe(II) and p-orbital mixing and second-order JT effects for d{sup 9} Cu(II). Display Omitted - Highlights: • Tetrahedral copper and iron(II) coordinated by oxygen. • New layered phosphate structure. • Jahn–Teller and d{sup 10} distorted coordinations.

Synthesis and structural characterisation of iron(II) and copper(II) diphosphates containing flattened metal oxotetrahedra

International Nuclear Information System (INIS)

Keates, Adam C.; Wang, Qianlong; Weller, Mark T.

2014-01-01

Single crystal and bulk polycrystalline forms of K 2 MP 2 O 7 (M=Fe(II), Cu(II)) have been synthesised and their structures determined from single crystal X-ray diffraction data. Both compounds crystallize in the tetragonal system, space group P-42 1 m. Their structures are formed from infinite sheets of linked oxopolyhedra of the stoichiometry [MP 2 O 7 ] 2− with potassium cations situated between the layers. The MO 4 tetrahedra share oxygen atoms with [P 2 O 7 ] 4− diphosphate groups and the potassium ions have KO 8 square prismatic geometry. In both compounds the M(II) centre has an unusual strongly flattened, tetrahedral coordination to oxygen, as a result of the Jahn–Teller (JT) effect for the high spin d 6 Fe(II) and p-orbital mixing or a second order JT effect for d 9 Cu(II) centres in four fold coordination. The uncommon transition metal ion environments found in these materials are reflected in their optical absorption spectra and magnetism data. - Graphical abstract: The structures of the tetragonal polymorphs of K 2 MP 2 O 7 , M=Cu(II), Fe(II), consist of infinite sheets of stoichiometry [MP 2 O 7 ] 2− , formed from linked pyrophosphate groups and MO 4 tetrahedra, separated by potassium ions. In both compounds the unusual tetrahedral coordination of the M(II) centre is strongly flattened as a result of Jahn–Teller (JT) effects for high spin, d 6 Fe(II) and p-orbital mixing and second-order JT effects for d 9 Cu(II). Display Omitted - Highlights: • Tetrahedral copper and iron(II) coordinated by oxygen. • New layered phosphate structure. • Jahn–Teller and d 10 distorted coordinations

Application of Zr/Ti-Pic in the adsorption process of Cu(II), Co(II) and Ni(II) using adsorption physico-chemical models and thermodynamics of the process; Aplicacao de Zr/Ti-PILC no processo de adsorcao de Cu(II), Co(II) e Ni(II) utilizando modelos fisico-quimicos de adsorcao e termodinamica do processo

Energy Technology Data Exchange (ETDEWEB)

Guerra, Denis Lima; Airoldi, Claudio [Universidade Estadual de Campinas (UNICAMP), SP (Brazil). Inst. de Quimica. Dept. de Quimica Inorganica]. E-mail: dlguerra@iqm.unicamp.br; Lemos, Vanda Porpino; Angelica, Romulo Simoes [Universidade Federal do Para (UFPa), Belem (Brazil); Viana, Rubia Ribeiro [Universidade Federal do Mato Grosso (UFMT), Cuiaba (Brazil). Inst. de Ciencias Exatas e da Terra. Dept. de Recursos Minerais

2008-07-01

The aim of this investigation is to study how Zr/Ti-Pic adsorbs metals. The physico-chemical proprieties of Zr/Ti-Pic have been optimized with pillarization processes and Cu(II), Ni(II) and Co(II) adsorption from aqueous solution has been carried out, with maximum adsorption values of 8.85, 8.30 and 7.78 x-1 mmol g{sup -1}, respectively. The Langmuir, Freundlich and Temkin adsorption isotherm models have been applied to fit the experimental data with a linear regression process. The energetic effect caused by metal interaction was determined through calorimetric titration at the solid-liquid interface and gave a net thermal effect that enabled the calculation of the exothermic values and the equilibrium constant. (author)

Validation of an HPLC method for determination of chemical purity of [18F]fluoromisonidazole ([18F]FMISO)

International Nuclear Information System (INIS)

Nascimento, Natalia C.E.S.; Oliveira, Mércia L.; Lima, Fernando R.A.; Silveira, Marina B.; Ferreira, Soraya Z.; Silva, Juliana B.

2017-01-01

[ 18 F]Fluoromisonidazole ([ 18 F]FMISO) is a nitroimidazole derivative labelled with fluorine-18 that selectively binds to hypoxic cells. It has been shown to be a suitable PET tracer for imaging hypoxia in tumors as well as in noncancerous tissues. [ 18 F]FMISO was prepared using a TRACERlabMX FDG ® module (GE) with cassettes, software sequence and reagents kits from ABX. In this work, we aimed to develop and to validate a new high performance liquid chromatography (HPLC) method for determination of chemical purity of [ 18 F]FMISO. Analyses were performed with an Agilent chromatograph equipped with radioactivity and UV detectors. [ 18 F]FMISO and impurities were separated on a C18 column by gradient elution with water and acetonitrile. Selectivity, linearity, detection limit (DL), quantification limit (LQ), precision, accuracy and robustness were assessed to demonstrate that the HPLC method is adequate for its intended purpose. The HPLC method showed a good precision, as all RSD values were lower than 5%. Robustness was evaluated considering a variation on parameters such mobile phase gradient and flow rate. Results evidenced that the HPLC method is validated and is suitable for radiochemical purity evaluation of [ 18 F]FMISO, considering operational conditions of our laboratory. As an extension of this work, other analytical methods used for [ 18 F]FMISO quality control should be evaluated, in compliance with good manufacture practice. (author)

Determination of tumour hypoxia with the PET tracer [{sup 18}F]EF3: improvement of the tumour-to-background ratio in a mouse tumour model

Energy Technology Data Exchange (ETDEWEB)

Christian, Nicolas; Bol, Anne; Bast, Marc de; Labar, Daniel; Lee, John; Mahy, Pierre; Gregoire, Vincent [Universite Catholique de Louvain, Center for Molecular Imaging and Experimental Radiotherapy, Brussels (Belgium)

2007-09-15

The 2-(2-nitroimidazol-1-yl)-N-(3,3,3-trifluoropropyl)acetamide (EF3) is a 2-nitroimidazole derivative which undergoes bioreductive activation under hypoxic conditions. Using the PET tracer [{sup 18}F]EF3 in mice, tumour-to-muscle ratios ranging from 1.3 to 3.5 were observed. This study investigated the impact of various interventions aimed at increasing [{sup 18}F]EF3 elimination, thus potentially increasing the tumour-to-noise ratio in mice, by increasing the renal filtration rate (spironolactone, furosemide), decreasing tubular re-absorption (metronidazole, ornidazole, amino acid solution) or stimulating gastro-intestinal elimination (phenobarbital). C3H mice were injected i.v. with an average of 12.95 MBq of [{sup 18}F]EF3. Drugs were injected i.v. 15 min before the tracer or daily 4 days prior to the experiment (phenobarbital). Anaesthetised mice were imaged from 30 to 300 min with a dedicated animal PET (Mosaic, Philips). Regions of interest were delineated around the tumour, bladder, heart, liver and leg muscle. Radioactivity was expressed as a percentage of injected activity per gram of tissue. Ornidazole decreased the urinary excretion and increased the liver uptake of [{sup 18}F]EF3, but without causing any changes in the other organs. Phenobarbital significantly increased the liver concentration and decreased radioactivity in blood and muscle without affecting the tracer uptake in tumour. Consequently, a small but non-significant increase in tumour-to-noise ratio was observed. Although some effects were observed with other drugs, they did not modify the tumour-to-noise ratio. Only phenobarbital induced a trend toward an increased tumour-to-noise ratio that could possibly be tested in the clinical situation. (orig.)

The effect of 3'- methyl-N,N-dimethylaminoasobenzene and gamma rays on the serum level of deoxyribonuclease II of the rat and the isolation of deoxyribonuclease II from the human spleen

International Nuclear Information System (INIS)

Jansen van Rensburg, E.

1979-01-01

The purpose of this investigation was twofold, viz.: 1. To determine the influence of ionising radiation (physical carcinogen) on deoxyribonuclease II in serum. 2. To develop a sensitive method for determining deoxyribonuclease II, viz. a radioimmunoassay (RlA). With this object in view, the influence of a strong physical carcinogen, viz. 60 Co gamma rays, on the activity of DNase II in rat serum was studied. For comparative studies, the influence of a strong chemical carcinogen (3'-methyl-N,N-dimethylaminoasobenzene) on rat serum DNase II was determined. In addition, attempts were made to isolate, purify and characterise DNase II from human spleen. These attempts were made as the first step in the development of a RlA. The in vivo studies of the influence of 3'MeDAB over a long period (40 weeks) showed that the DNase II activity increased in the serum and liver nuclei of rats during the pre-cancer phase. This increase may, together with other parameters, be useful in the early diagnosis of liver cancer. The most important contribution of this investigation is the possible use of a serum DNase II RlA together with a battery RlAs for other indicators (biochemical) for the determination of radiation exposure in man [af

Development of a Novel Cu(II Complex Modified Electrode and a Portable Electrochemical Analyzer for the Determination of Dissolved Oxygen (DO in Water

Directory of Open Access Journals (Sweden)

Salvatore Gianluca Leonardi

2016-04-01

Full Text Available The development of an electrochemical dissolved oxygen (DO sensor based on a novel Cu(II complex-modified screen printed carbon electrode is reported. The voltammetric behavior of the modified electrode was investigated at different scan rates and oxygen concentrations in PBS (pH = 7. An increase of cathodic current (at about −0.4 vs. Ag/AgCl with the addition of oxygen was observed. The modified Cu(II complex electrode was demonstrated for the determination of DO in water using chronoamperometry. A small size and low power consumption home-made portable electrochemical analyzer based on custom electronics for sensor interfacing and operating in voltammetry and amperometry modes has been also designed and fabricated. Its performances in the monitoring of DO in water were compared with a commercial one.

The Physiological Functions and Structural Determinants of Catalytic Bias in the [FeFe]-Hydrogenases CpI and CpII of Clostridium pasteurianum Strain W5

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Jesse B. Therien

2017-07-01

capturing excess reducing equivalents under nitrogen fixation conditions. Comparison of the primary sequences of CpI and CpII and their homologs provides an initial basis for identifying key structural determinants that modulate hydrogen production and hydrogen oxidation activities.

The Physiological Functions and Structural Determinants of Catalytic Bias in the [FeFe]-Hydrogenases CpI and CpII of Clostridium pasteurianum Strain W5

Science.gov (United States)

Therien, Jesse B.; Artz, Jacob H.; Poudel, Saroj; Hamilton, Trinity L.; Liu, Zhenfeng; Noone, Seth M.; Adams, Michael W. W.; King, Paul W.; Bryant, Donald A.; Boyd, Eric S.; Peters, John W.

2017-01-01

reducing equivalents under nitrogen fixation conditions. Comparison of the primary sequences of CpI and CpII and their homologs provides an initial basis for identifying key structural determinants that modulate hydrogen production and hydrogen oxidation activities. PMID:28747909

Predictive value of SAPS II and APACHE II scoring systems for patient outcome in a medical intensive care unit

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Amina Godinjak

2016-11-01

Full Text Available Objective. The aim is to determine SAPS II and APACHE II scores in medical intensive care unit (MICU patients, to compare them for prediction of patient outcome, and to compare with actual hospital mortality rates for different subgroups of patients. Methods. One hundred and seventy-four patients were included in this analysis over a oneyear period in the MICU, Clinical Center, University of Sarajevo. The following patient data were obtained: demographics, admission diagnosis, SAPS II, APACHE II scores and final outcome. Results. Out of 174 patients, 70 patients (40.2% died. Mean SAPS II and APACHE II scores in all patients were 48.4±17.0 and 21.6±10.3 respectively, and they were significantly different between survivors and non-survivors. SAPS II >50.5 and APACHE II >27.5 can predict the risk of mortality in these patients. There was no statistically significant difference in the clinical values of SAPS II vs APACHE II (p=0.501. A statistically significant positive correlation was established between the values of SAPS II and APACHE II (r=0.708; p=0.001. Patients with an admission diagnosis of sepsis/septic shock had the highest values of both SAPS II and APACHE II scores, and also the highest hospital mortality rate of 55.1%. Conclusion. Both APACHE II and SAPS II had an excellent ability to discriminate between survivors and non-survivors. There was no significant difference in the clinical values of SAPS II and APACHE II. A positive correlation was established between them. Sepsis/septic shock patients had the highest predicted and observed hospital mortality rate.

Cu(II AND Zn(II COMPLEX COMPOUNDS WITH BIGUANIDES AROMATIC DERIVATIVES. SYNTHESIS, CHARACTERIZATION, BIOLOGICAL ACTIVITY

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Ticuţa Negreanu-Pîrjol

2011-05-01

Full Text Available In this paper we report the synthesis, physical-chemical characterization and antimicrobial activity of some new complex compounds of hetero-aromatic biguanides ligands, chlorhexidine base (CHX and chlorhexidine diacetate (CHXac2 with metallic ions Cu(II and Zn(II, in different molar ratio. The synthesized complexes were characterized by elemental chemical analysis and differential thermal analysis. The stereochemistry of the metallic ions was determined by infrared spectra, UV-Vis, EPR spectroscopy and magnetic susceptibility in the aim to establish the complexes structures. The biological activity of the new complex compounds was identified in solid technique by measuring minimum inhibition diameter of bacterial and fungal culture, against three standard pathogen strains, Escherichia coli ATCC 25922, Staphilococcus aureus ATCC 25923 and Candida albicans ATCC 10231. The results show an increased specific antimicrobial activity for the complexes chlorhexidine:Cu(II 1:1 and 1:2 compared with the one of the Zn(II complexes.

Norepinephrine metabolism in neuronal cultures is increased by angiotensin II

International Nuclear Information System (INIS)

Sumners, C.; Shalit, S.L.; Kalberg, C.J.; Raizada, M.K.

1987-01-01

In this study the authors have examined the actions of angiotensin II (ANG II) on catecholamine metabolism in neuronal brain cell cultures prepared from the hypothalamus and brain stem. Neuronal cultures prepared from the brains of 1-day-old Sprague-Dawley rats exhibit specific neuronal uptake mechanisms for both norepinephrine (NE) and dopamine (DA), and also monoamine oxidase (MAO) and catechol O-methyltransferase (COMT) activity. Separate neuronal uptake sites for NE and DA were identified by using specific neuronal uptake inhibitors for each amine. In previous studies, they determined that ANG II (10 nM-1 μM) stimulates increased neuronal [ 3 H]NE uptake by acting as specific receptors. They have confirmed these results here and in addition have shown that ANG II has not significant effects on neuronal [ 3 H]DA uptake. These results suggest that the actions of ANG II are restricted to the NE transporter in neuronal cultures. It is possible that ANG II stimulates the intraneuronal metabolism of at least part of the NE that is taken up, because the peptide stimulates MAO activity, an effect mediated by specific ANG II receptors. ANG II had no effect on COMT activity in neuronal cultures. Therefore, the use of neuronal cultures of hypothalamus and brain stem they have determined that ANG II can specifically alter NE metabolism in these areas, while apparently not altering DA metabolism

Determinants of aortic stiffness: 16-year follow-up of the Whitehall II study.

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Nanna B Johansen

Full Text Available Aortic stiffness is a strong predictor of cardiovascular disease endpoints. Cross-sectional studies have shown associations of various cardiovascular risk factors with aortic pulse wave velocity, a measure of aortic stiffness, but the long-term impact of these factors on aortic stiffness is unknown.In 3,769 men and women from the Whitehall II cohort, a wide range of traditional and novel cardiovascular risk factors were determined at baseline (1991-1993 and aortic pulse wave velocity was measured at follow-up (2007-2009. The prospective associations between each baseline risk factor and aortic pulse wave velocity at follow-up were assessed through sex stratified linear regression analysis adjusted for relevant confounders. Missing data on baseline determinants were imputed using the Multivariate Imputation by Chained Equations.Among men, the strongest predictors were waist circumference, waist-hip ratio, heart rate and interleukin 1 receptor antagonist, and among women, adiponectin, triglycerides, pulse pressure and waist-hip ratio. The impact of 10 centimeter increase in waist circumference on aortic pulse wave velocity was twice as large for men compared with women (men: 0.40 m/s (95%-CI: 0.24;0.56; women: 0.17 m/s (95%-CI: -0.01;0.35, whereas the opposite was true for the impact of a two-fold increase in adiponectin (men: -0.30 m/s (95%-CI: -0.51;-0.10; women: 0.61 m/s (95%-CI: -0.86;-0.35.In this large prospective study, central obesity was a strong predictor of aortic stiffness. Additionally, heart rate in men and adiponectin in women predicted aortic pulse wave velocity suggesting that strategies to prevent aortic stiffening should be focused differently by sex.

Synthesis and Characterization of Some New Cu(II, Ni(II and Zn(II Complexes with Salicylidene Thiosemicarbazones: Antibacterial, Antifungal and in Vitro Antileukemia Activity

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Tudor Rosu

2013-07-01

Full Text Available Thirty two new Cu(II, Ni(II and Zn(II complexes (1–32 with salicylidene thiosemicarbazones (H2L1–H2L10 were synthesized. Salicylidene thiosemicarbazones, of general formula (XN-NH-C(S-NH(Y, were prepared through the condensation reaction of 2-hydroxybenzaldehyde and its derivatives (X with thiosemicarbazide or 4-phenylthiosemicarbazide (Y = H, C6H5. The characterization of the new formed compounds was done by 1H-NMR, 13C-NMR, IR spectroscopy, elemental analysis, magnetochemical, thermoanalytical and molar conductance measurements. In addition, the structure of the complex 5 has been determined by X-ray diffraction method. All ligands and metal complexes were tested as inhibitors of human leukemia (HL-60 cells growth and antibacterial and antifungal activities.

Cr(III,Mn(II,Fe(III,Co(II,Ni(II,Cu(II and Zn(II Complexes with Diisobutyldithiocarbamato Ligand

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Mohammad Tarique

2011-01-01

Full Text Available The synthesis of sulphur and nitrogen containing dithiocarbamato ligand derived from diisobutylamine as well as its coordination compounds with 3d series transition metals is presented. These synthesized compounds were characterized on the basis of elemental analysis, conductometric measurements and IR spectral studies. The analytical data showed the stoichiometry 1:2 and 1:3 for the compounds of the types ML2 {M=Mn(II, Co(II, Ni(II, Cu(II and Zn(II} and M'L3{M'=Cr(III and Fe(III} respectively. The conductometric measurements proved the non-electrolytic behaviour of all the compounds. The bidentate nature of dithiocarbamato moiety was confirmed on the basis of IR spectral data.

Crystal structures of copper(II) chloride, copper(II) bromide, and copper(II) nitrate complexes with pyridine-2-carbaldehyde thiosemicarbazone

Science.gov (United States)

Chumakov, Yu. M.; Tsapkov, V. I.; Jeanneau, E.; Bairac, N. N.; Bocelli, G.; Poirier, D.; Roy, J.; Gulea, A. P.

2008-09-01

The crystal structures of chloro-(2-formylpyridinethiosemicarbazono)copper dimethyl sulfoxide solvate ( I), bromo-(2-formylpyridinethiosemicarbazono)copper ( II), and (2-formylpyridinethiosemicarbazono)copper(II) nitrate dimethyl sulfoxide solvate ( III) are determined using X-ray diffraction. In the crystals, complexes I and II form centrosymmetric dimers in which the thiosemicarbazone sulfur atom serves as a bridge and occupies the fifth coordination site of the copper atom of the neighboring complex related to the initial complex through the center of symmetry. In both cases, the coordination polyhedron of the complexing ion is a distorted tetragonal bipyramid. Complex III in the crystal structure forms polymer chains in which the copper atom of one complex forms the coordination bond with the thicarbamide nitrogen atom of the neighboring complex. In this structure, the coordination polyhedron of the central atom is an elongated tetragonal bipyramid. It is established that complexes I III at a concentration of 10-5 mol/l selectively inhibit the growth of 60 to 90 percent of the cancer tumor cells of the human myeloid leukemia (HL-60).

Crystal structures of copper(II) chloride, copper(II) bromide, and copper(II) nitrate complexes with pyridine-2-carbaldehyde thiosemicarbazone

International Nuclear Information System (INIS)

Chumakov, Yu. M.; Tsapkov, V. I.; Jeanneau, E.; Bairac, N. N.; Bocelli, G.; Poirier, D.; Roy, J.; Gulea, A. P.

2008-01-01

The crystal structures of chloro-(2-formylpyridinethiosemicarbazono)copper dimethyl sulfoxide solvate (I), bromo-(2-formylpyridinethiosemicarbazono)copper (II), and (2-formylpyridinethiosemicarbazono)copper(II) nitrate dimethyl sulfoxide solvate (III) are determined using X-ray diffraction. In the crystals, complexes I and II form centrosymmetric dimers in which the thiosemicarbazone sulfur atom serves as a bridge and occupies the fifth coordination site of the copper atom of the neighboring complex related to the initial complex through the center of symmetry. In both cases, the coordination polyhedron of the complexing ion is a distorted tetragonal bipyramid. Complex III in the crystal structure forms polymer chains in which the copper atom of one complex forms the coordination bond with the thicarbamide nitrogen atom of the neighboring complex. In this structure, the coordination polyhedron of the central atom is an elongated tetragonal bipyramid. It is established that complexes I-III at a concentration of 10 -5 mol/l selectively inhibit the growth of 60 to 90 percent of the cancer tumor cells of the human myeloid leukemia (HL-60).

Crystal structures of copper(II) chloride, copper(II) bromide, and copper(II) nitrate complexes with pyridine-2-carbaldehyde thiosemicarbazone

Energy Technology Data Exchange (ETDEWEB)

Chumakov, Yu. M., E-mail: chumakov.xray@phys.asm.md [Academy of Sciences of Moldova, Institute of Applied Physics (Moldova, Republic of); Tsapkov, V. I. [State University of Moldova (Moldova, Republic of); Jeanneau, E. [Universite Claude Bernard, Laboratoire des Multimateriaux et Interfaces (France); Bairac, N. N. [State University of Moldova (Moldova, Republic of); Bocelli, G. [National Research Council (IMEM-CNR), Institute of Materials for Electronics and Magnetism (Italy); Poirier, D.; Roy, J. [Centre Hospitalier Universitaire de Quebec (CHUQ) (Canada); Gulea, A. P. [State University of Moldova (Moldova, Republic of)

2008-09-15

The crystal structures of chloro-(2-formylpyridinethiosemicarbazono)copper dimethyl sulfoxide solvate (I), bromo-(2-formylpyridinethiosemicarbazono)copper (II), and (2-formylpyridinethiosemicarbazono)copper(II) nitrate dimethyl sulfoxide solvate (III) are determined using X-ray diffraction. In the crystals, complexes I and II form centrosymmetric dimers in which the thiosemicarbazone sulfur atom serves as a bridge and occupies the fifth coordination site of the copper atom of the neighboring complex related to the initial complex through the center of symmetry. In both cases, the coordination polyhedron of the complexing ion is a distorted tetragonal bipyramid. Complex III in the crystal structure forms polymer chains in which the copper atom of one complex forms the coordination bond with the thicarbamide nitrogen atom of the neighboring complex. In this structure, the coordination polyhedron of the central atom is an elongated tetragonal bipyramid. It is established that complexes I-III at a concentration of 10{sup -5} mol/l selectively inhibit the growth of 60 to 90 percent of the cancer tumor cells of the human myeloid leukemia (HL-60).

Computer augumented modelling studies of Pb(II, Cd(II, Hg(II, Co(II, Ni(II, Cu(II and Zn(II complexes of L-glutamic acid in 1,2-propanediol–water mixtures

Directory of Open Access Journals (Sweden)

MAHESWARA RAO VEGI

2008-12-01

Full Text Available Chemical speciation of Pb(II, Cd(II, Hg(II, Co(II, Ni(II, Cu(II and Zn(II complexes of L-glutamic acid was studied at 303 K in 0–60 vol. % 1,2-propanediol–water mixtures, whereby the ionic strength was maintained at 0.16 mol dm-3. The active forms of the ligand are LH3+, LH2 and LH–. The predominant detected species were ML, ML2, MLH, ML2H and ML2H2. The trend of the variation in the stability constants with changing dielectric constant of the medium is explained based on the cation stabilizing nature of the co-solvents, specific solvent–water interactions, charge dispersion and specific interactions of the co-solvent with the solute. The effect of systematic errors in the concentrations of the substances on the stability constants is in the order alkali > > acid > ligand > metal. The bioavailability and transportation of metals are explained based on distribution diagrams and stability constants.

Determination of the O/M ratios of polynary uranium oxides by Ce(IV)-Fe(II) back titration after dissolution in mixed sulphuric and phosphoric acids.

Science.gov (United States)

Fujino, T; Sato, N; Yamada, K

1996-01-01

Uranium (IV) in polynary uranium oxides is determined after the solid has been dissolved in a warm mixed solution of sulphuric and phosphoric acids containing excess Ce(IV). The latter is titrated with a Fe(II) standard solution using ferroin as indicator. This method is especially effective for (mixed) uranium oxides which are difficult to dissolve in hot Ce(IV) sulphuric acid. The standard deviation of the determined x value in polynary oxides is estimated to be below +/- 0.004 for samples of 10-30 mg.

The speciation of aqueous zinc(II) bromide solutions to 500 °C and 900 MPa determined using Raman spectroscopy

Science.gov (United States)

Mibe, Kenji; Chou, I-Ming; Anderson, Alan J.; Mayanovic, Robert A.; Bassett, William A.

2009-01-01

A Raman spectral study was carried out on 3 solutions of varying concentration and bromide/zinc ratios. Spectra were collected at 11 different temperature-pressure conditions ranging from ambient to 500????C-0.9??GPa. Raman band assignments for zinc(II) bromide species reported in previous studies were used to determine the relative concentrations of ZnBr42-, ZnBr3-, ZnBr2, and ZnBr+ species at various temperatures and pressures. Our results are in close agreement with X-ray absorption spectroscopic (XAS) data, and confirm that the tetrabromo zinc(II) complex, ZnBr42-, is the predominant species up to 500????C in solutions having high Zn concentrations (1??m) and high bromide/zinc molar ratios ([Br]/[Zn] = 8). In agreement with previous solubility and Raman spectroscopic experiments, our measurements indicate that species with a lower number of halide ligands and charge are favored with increasing temperature in dilute solutions, and solutions with low bromide/zinc ratios ([Br]/[Zn] Raman technique provides an independent experimental means of evaluating the quality of XAS analyses of data obtained from high temperature disordered systems. The combination of these two techniques provides complementary data on speciation and the structure of zinc(II) bromide complexes. The preponderance of the ZnBr42- species in highly saline brines at high temperature is consistent with the predominance of ZnCl42- in chloride-rich brines reported in previous XAS studies. Knowledge of Zn complexing in metal-rich highly saline brines is important for numerical models of ore deposition in high temperature systems such as skarns and porphyry-type deposits. ?? 2008 Elsevier B.V.

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

Science.gov (United States)

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.

Synthesis and characterization of heterobimetallic complexes of the type [Cu(pn2][MCl4] where M = Co(II, Ni(II, Cu(II, Zn(II, Cd(II, and Hg(II

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Seema Yadav

2016-11-01

Full Text Available A series of new bimetallic transition metal complexes of the type [Cu(pn2] [MCl4] have been synthesized (where M = Co(II, Ni(II, Cu(II, Zn(II, Cd(II and Hg(II, pn = 1,3-diaminopropane and characterized by elemental analysis, molar conductance, TGA, IR and electronic spectra. All the compounds are 1:1 electrolyte in DMF. The Cu(II ion is square-planar while metal ions in the anionic moiety acquire their usual tetrahedral arrangement. On the basis of these studies it is concluded that anionic moiety is electrically stabilized by its cationic counterpart.

7 CFR 1430.606 - Determination of losses incurred.

Science.gov (United States)

2010-01-01

... 7 Agriculture 10 2010-01-01 2010-01-01 false Determination of losses incurred. 1430.606 Section... Disaster Assistance Payment Program II (DDAP-II) § 1430.606 Determination of losses incurred. (a) Eligible payable losses are calculated on a dairy operation by dairy operation basis and are limited to those...

Indirect spectrophotometric determination of trace cyanide with cationic porphyrins.

Science.gov (United States)

Ishii, H; Kohata, K

1991-05-01

Three highly sensitive methods for the determination of cyanide have been developed, based on the fact that the complexation of silver ions with three cationic porphyrins, 5,10,15,20-tetrakis-(1-methyl-2-pyridinio)porphine [T(2-MPy)P], 5,10,15,20-tetrakis(1-methyl-3-pyridinio)porphine [T(3-MPy)P] and 5,10,15,20-tetrakis(1-methyl-4-pyridinio)porphine [T(4-MPy)P], in alkaline media is inhibited by cyanide and the decrease in absorbance of the silver(II) complex is proportional to the cyanide concentration. Sensitivities of the procedures developed are 0.133, 0.126 and 0.234 ng/cm(2), respectively for an absorbance of 0.001. Cadmium(II), copper(II), mercury(II), zinc(II), iodide and sulfide interfere with the cyanide determination. One of the proposed methods was applied to the determination of cyanide in waste-water samples, with satisfactory results.

Synthesis, characterization, spectroscopic and theoretical studies of new zinc(II), copper(II) and nickel(II) complexes based on imine ligand containing 2-aminothiophenol moiety

Science.gov (United States)

Shafaatian, Bita; Mousavi, S. Sedighe; Afshari, Sadegh

2016-11-01

New dimer complexes of zinc(II), copper(II) and nickel(II) were synthesized using the Schiff base ligand which was formed by the condensation of 2-aminothiophenol and 2-hydroxy-5-methyl benzaldehyde. This tridentate Schiff base ligand was coordinated to the metal ions through the NSO donor atoms. In order to prevent the oxidation of the thiole group during the formation of Schiff base and its complexes, all of the reactions were carried out under an inert atmosphere of argon. The X-ray structure of the Schiff base ligand showed that in the crystalline form the SH groups were oxidized to produce a disulfide Schiff base as a new double Schiff base ligand. The molar conductivity values of the complexes in dichloromethane implied the presence of non-electrolyte species. The fluorescence properties of the Schiff base ligand and its complexes were also studied in dichloromethane. The products were characterized by FT-IR, 1H NMR, UV/Vis spectroscopies, elemental analysis, and conductometry. The crystal structure of the double Schiff base was determined by single crystal X-ray diffraction. Furthermore, the density functional theory (DFT) calculations were performed at the B3LYP/6-31G(d,p) level of theory for the determination of the optimized structures of Schiff base complexes.

Small Diameter Bomb Increment II (SDB II)

Science.gov (United States)

2015-12-01

Selected Acquisition Report (SAR) RCS: DD-A&T(Q&A)823-439 Small Diameter Bomb Increment II (SDB II) As of FY 2017 President’s Budget Defense... Bomb Increment II (SDB II) DoD Component Air Force Joint Participants Department of the Navy Responsible Office References SAR Baseline (Production...Mission and Description Small Diameter Bomb Increment II (SDB II) is a joint interest United States Air Force (USAF) and Department of the Navy

Synthesis and structural characterization of nickel(II), cobalt(II), Zinc(II), manganese(II), cadmium(II) and uranium(VI) complexes of α-oximinoacetoacet-o/p-anisidide thiosemicarbazone

International Nuclear Information System (INIS)

Patel, P.S.; Patel, M.M.; Ray, R.M.

1993-01-01

A few metal complexes of α-oximinoacetoacet-o/p-anisidide thiosemicarbazones (OAOATS)/(OAPATS) with Ni(II), Co(II), Zn(II), Mn(II), Hg(II), Cd(II) and UO 2 (II) have been prepared and characterized by elemental analyses, conductivity, differential scanning calorimetry study, thermogravimetric analyses and infrared and electronic spectral measurements in conjunction with magnetic susceptibility measurements at room temperature. They have also been tested for their antimicrobial activities. (author). 24 refs., 2 tabs

Competitive adsorption of copper(II), cadmium(II), lead(II) and zinc(II) onto basic oxygen furnace slag

International Nuclear Information System (INIS)

Xue Yongjie; Hou Haobo; Zhu Shujing

2009-01-01

Polluted and contaminated water can often contain more than one heavy metal species. It is possible that the behavior of a particular metal species in a solution system will be affected by the presence of other metals. In this study, we have investigated the adsorption of Cd(II), Cu(II), Pb(II), and Zn(II) onto basic oxygen furnace slag (BOF slag) in single- and multi-element solution systems as a function of pH and concentration, in a background solution of 0.01 M NaNO 3 . In adsorption edge experiments, the pH was varied from 2.0 to 13.0 with total metal concentration 0.84 mM in the single element system and 0.21 mM each of Cd(II), Cu(II), Pb(II), and Zn(II) in the multi-element system. The value of pH 50 (the pH at which 50% adsorption occurs) was found to follow the sequence Zn > Cu > Pb > Cd in single-element systems, but Pb > Cu > Zn > Cd in the multi-element system. Adsorption isotherms at pH 6.0 in the multi-element systems showed that there is competition among various metals for adsorption sites on BOF slag. The adsorption and potentiometric titrations data for various slag-metal systems were modeled using an extended constant-capacitance surface complexation model that assumed an ion-exchange process below pH 6.5 and the formation of inner-sphere surface complexes at higher pH. Inner-sphere complexation was more dominant for the Cu(II), Pb(II) and Zn(II) systems

Competitive adsorption of copper(II), cadmium(II), lead(II) and zinc(II) onto basic oxygen furnace slag

Energy Technology Data Exchange (ETDEWEB)

Xue Yongjie [School of Resource and Environment Science, Wuhan University, Hubei, Wuhan (China); Wuhan Kaidi Electric Power Environmental Protection Co. Ltd., Hubei, Wuhan (China)], E-mail: xueyj@mail.whut.edu.cn; Hou Haobo; Zhu Shujing [School of Resource and Environment Science, Wuhan University, Hubei, Wuhan (China)

2009-02-15

Polluted and contaminated water can often contain more than one heavy metal species. It is possible that the behavior of a particular metal species in a solution system will be affected by the presence of other metals. In this study, we have investigated the adsorption of Cd(II), Cu(II), Pb(II), and Zn(II) onto basic oxygen furnace slag (BOF slag) in single- and multi-element solution systems as a function of pH and concentration, in a background solution of 0.01 M NaNO{sub 3}. In adsorption edge experiments, the pH was varied from 2.0 to 13.0 with total metal concentration 0.84 mM in the single element system and 0.21 mM each of Cd(II), Cu(II), Pb(II), and Zn(II) in the multi-element system. The value of pH{sub 50} (the pH at which 50% adsorption occurs) was found to follow the sequence Zn > Cu > Pb > Cd in single-element systems, but Pb > Cu > Zn > Cd in the multi-element system. Adsorption isotherms at pH 6.0 in the multi-element systems showed that there is competition among various metals for adsorption sites on BOF slag. The adsorption and potentiometric titrations data for various slag-metal systems were modeled using an extended constant-capacitance surface complexation model that assumed an ion-exchange process below pH 6.5 and the formation of inner-sphere surface complexes at higher pH. Inner-sphere complexation was more dominant for the Cu(II), Pb(II) and Zn(II) systems.

Competitive adsorption of copper(II), cadmium(II), lead(II) and zinc(II) onto basic oxygen furnace slag.

Science.gov (United States)

Xue, Yongjie; Hou, Haobo; Zhu, Shujing

2009-02-15

Polluted and contaminated water can often contain more than one heavy metal species. It is possible that the behavior of a particular metal species in a solution system will be affected by the presence of other metals. In this study, we have investigated the adsorption of Cd(II), Cu(II), Pb(II), and Zn(II) onto basic oxygen furnace slag (BOF slag) in single- and multi-element solution systems as a function of pH and concentration, in a background solution of 0.01M NaNO(3). In adsorption edge experiments, the pH was varied from 2.0 to 13.0 with total metal concentration 0.84mM in the single element system and 0.21mM each of Cd(II), Cu(II), Pb(II), and Zn(II) in the multi-element system. The value of pH(50) (the pH at which 50% adsorption occurs) was found to follow the sequence Zn>Cu>Pb>Cd in single-element systems, but Pb>Cu>Zn>Cd in the multi-element system. Adsorption isotherms at pH 6.0 in the multi-element systems showed that there is competition among various metals for adsorption sites on BOF slag. The adsorption and potentiometric titrations data for various slag-metal systems were modeled using an extended constant-capacitance surface complexation model that assumed an ion-exchange process below pH 6.5 and the formation of inner-sphere surface complexes at higher pH. Inner-sphere complexation was more dominant for the Cu(II), Pb(II) and Zn(II) systems.

Preparation of Schiff s base complexes of Mn(II), Co(II), Ni(II), Cu(II), Zn(II), and Cd(II) and their spectroscopic, magnetic, thermal, and antifungal studies

International Nuclear Information System (INIS)

Parekh, H.M.; Patel, M.N.

2006-01-01

The potassium salt of salicylidene-DL-alanine (KHL), bis(benzylidene)ethylenediamine (A 1 ), thiophene-o-carboxaldene-p-toluidine (A 2 ), and its metal complexes of the formula [(M II (L)(A)(H 2 O)] (M=Mn(II), Co(II), Ni(II), Cu(II), Zn(II), and Cd(II); A = A 1 or A 2 ) are prepared. They are characterized by elemental analysis, magnetic susceptibility measurements, thermogravimetric analysis, and infrared and electronic spectral studies. The electronic spectral and magnetic moment data suggest an octahedral geometry for the complexes. All of these complexes, metal nitrates, fungicides (bavistin and emcarb), and ligands are screened for their antifungal activity against Aspergillus niger, Fusarium oxysporum, and Aspergillus flavus using a plate poison technique. The complexes show higher activity than those of the free ligands, metal nitrate, and the control (DMSO) and moderate activity against bavistin and emcarb [ru

Removal of mercury (II) from aqueous solution by activated carbon obtained from furfural.

Science.gov (United States)

Yardim, M F; Budinova, T; Ekinci, E; Petrov, N; Razvigorova, M; Minkova, V

2003-08-01

The adsorption of Hg(II) from aqueous solution at 293 K by activated carbon obtained from furfural is studied. The carbon is prepared by polymerization of furfural following carbonization and activation of the obtained polymer material with water vapor at 800 degrees C. Adsorption studies of Hg(II) are carried out varying some conditions: treatment time, metal ion concentration, adsorbent amount and pH. It is determined that Hg(II) adsorption follows both Langmuir and Freundlich isotherms. The adsorption capacity of the carbon is 174 mg/g. It is determined that Hg(II) uptake increases with increasing pH. Desorption studies are performed with hot water. The percent recovery of Hg(II) is 6%.

Determination of the O/M ratios of polynary uranium oxides by Ce(IV)-Fe(II) back titration after dissolution in mixed sulphuric and phosphoric acids

International Nuclear Information System (INIS)

Fujino, T.; Sato, N.; Yamada, K.

1996-01-01

Uranium (IV) in polynary uranium oxides is determined after the solid has been dissolved in a warm mixed solution of sulphuric and phosphoric acids containing excess Ce(IV). The latter is titrated with a Fe(II) standard solution using ferroin as indicator. This method is especially effective for (mixed) uranium oxides which are difficult to dissolve in hot Ce(IV) sulphuric acid. The standard deviation of the determined x value in polynary oxides is estimated to be below ± 0.004 for samples of 10-30 mg. (orig.)

Cu(II) AND Zn(II)

African Journals Online (AJOL)

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SYNTHESIS OF 2,2-DIMETHYL-4-PHENYL-[1,3]-DIOXOLANE USING ZEOLITE. ENCAPSULATED Co(II), Cu(II) AND Zn(II) COMPLEXES. B.P. Nethravathi1, K. Rama Krishna Reddy2 and K.N. Mahendra1*. 1Department of Chemistry, Bangalore University, Bangalore-560001, India. 2Department of Chemistry, Government ...

Anodic stripping voltammetry with carbon paste electrodes for rapid Ag(I) and Cu(II) determinations.

Science.gov (United States)

Labar, C; Lamberts, L

1997-05-01

The simultaneous determination of silver(I) and copper(II) is realized for the routine analysis of trace levels of these elements by anodic stripping voltammetry (ASV) at the carbon paste electrode (CPE). The electrochemical response is studied in 14 different supporting electrolytes, ranging from acidic solutions (pH 0.1) to neutral and basic (pH 9.7) media, and the parameters governing electrodeposition and stripping steps are characterized for each medium by the use of pseudo-voltammograms. Comparison between different modes of matter transport mechanisms is also given. The dynamic range of the method is 0.05 to 150 mug 1(-1) Ag(I) in the majority of the media studied and can be extended to 400 mug l(-1) in selected media, with a general reproducibility in the +/- 2% range for five replicate measurements. The total analysis time lies between approximately 30 s and 10 min. Activation of the CPE surface has been studied, but this pretreatment is demonstrated to be unfavourable and is replaced by a simpler unique 'cleaning' procedure of dipping the CPE in diluted nitric acid.

Column Chromatography Of Co(II), Zn(II) And Eu(III) Using Pistachio Shell And Different Mobile Phases

International Nuclear Information System (INIS)

Abdel-Fattah, A.A.

2009-01-01

Pistachio shell particles (0.5-1 mm) have been applied as the stationary phase for studying the column chromatography of Co(II), Zn(II) and Eu(III) at room temperature; 26 + - 1 oC. This solid sorbent has been characterized by thermogravimetric analysis, infra-red spectroscopy and X-ray diffraction. Its surface area and percent of swelling have been also determined. Different eluting agents have been used for eluting the sorbed elements. The elution curves have been done from which the distribution coefficients (K d ), number of theoretical plates (N) and heights equivalent to theoretical plates (H) have been determined. Column performance studies have been conducted for a representative system under certain experimented conditions and Van Deemter equation has been applied. Thermodynamic studies have been applied and thermodynamic functions ( δG 0 ,δH 0 andδ S 0 ) have been calculated for this representative system by determining K d at three different room temperatures (18, 26 and 37 + - 1o C).

Template synthesis of poly aza macrocyclic copper(II) and nickel(II) complexes: Spectral characterization and antimicrobial studies

Energy Technology Data Exchange (ETDEWEB)

Gurumoorthy, P.; Ravichandran, J.; Kaliur Rahiman, A. [The New College, Chennai (India); Karthikeyan, N.; Palani, P. [Univ. of Madras, Chennai (India)

2012-07-15

The template synthesis of copper(II) and nickel(II) complexes derived from 2,6-diformyl-4-methylphenol with diethylenetriamine or 1,2-bis(3-amino propylamino)ethane produce the 12-membered N{sub 3}O and 17-membered N{sub 4}O macrocyclic complexes, respectively. The geometry of the complexes has been determined with the help of electronic and EPR spectroscopic values and found to be five coordinated square pyramidal and, six coordinated distorted tetragonal for 12-membered and 17-membered macrocyclic complexes, respectively. Electrochemical studies of the mononuclear N{sub 3}O and N{sub 4}O copper(II) complexes show one irreversible one electron reduction wave at E{sup pc} = .1.35 and .1.15 V respectively, and the corresponding nickel(II) complexes show irreversible one-electron reduction wave at E{sup pc} = .1.25 and .1.22 V, respectively. The nickel(II) complexes show irreversible one-electron oxidation wave at Epa = +0.84 and +0.82 V, respectively. All the complexes were evaluated for in vitro antimicrobial activity against the human pathogenic bacteria and fungi.

Spectroscopic and thermal degradation behavior of Mg(II, Ca(II, Ba(II and Sr(II complexes with paracetamol drug

Directory of Open Access Journals (Sweden)

Moamen S. Refat

2017-05-01

Full Text Available Complexes of Mg(II, Ca(II, Ba(II and Sr(II with paracetamol drug were synthesized and characterized by elemental analysis, conductivity, UV–Vis, IR, and 1H NMR spectroscopy and thermal analysis, as well as screened for antimicrobial activity. The IR spectral data suggested that the ligand behaves as paracetamol behaves as a neutral bidentate ligand coordinated to the metal ions via the lone pair of electrons of nitrogen and carbonyl-O atoms of the amide group. From the microanalytical data, the stoichiometry of the complexes reacts with Mg(II, Ca(II, Ba(II and Sr(II by molar ratios (2:1 (paracetamol:metal ion. The thermal behavior (TG/DTG of the complexes was studied. The ligand and their metal complexes were screened against both of antibacterial and fungicidal activities.

ETAAS determination of thallium and silver from water matrix after colloidal precipitate flotation using lead(II hexamethylenedithiocarbamate

Directory of Open Access Journals (Sweden)

TRAJCE STAFILOV

2001-10-01

Full Text Available Afast method for the preconcentration of thallium and silver in nanogram quantities in fresh drinking waters (source, well, tap and waters for irrigation using colloidal precipitate flotation is described. Lead(II hexamethylenedithiocarbamate, Pb(HMDTC2 played the role of flotation collector. The experimental conditions for the successful separation of thallium and silver (mass of Pb, amount ofHMDTC-, pHof the system, induction time, type of surfactant etc. were optimized. After flotation separation from the mother liquor, the solid sublate containing traces of thallium and silver was dissolved and the analytes were determined by electrothermal atomic absorption spectrometry (ETAAS. The results of the ETAAS analysis are compared with those obtained by inductively coupled plasma-atomic emission spectrometry. The detection limit for thallium by this method is 0.027 mg/l, and for silver 0.005 microg/l.

Carbonate-mediated Fe(II) oxidation in the air-cathode fuel cell: a kinetic model in terms of Fe(II) speciation.

Science.gov (United States)

Song, Wei; Zhai, Lin-Feng; Cui, Yu-Zhi; Sun, Min; Jiang, Yuan

2013-06-06

Due to the high redox activity of Fe(II) and its abundance in natural waters, the electro-oxidation of Fe(II) can be found in many air-cathode fuel cell systems, such as acid mine drainage fuel cells and sediment microbial fuel cells. To deeply understand these iron-related systems, it is essential to elucidate the kinetics and mechanisms involved in the electro-oxidation of Fe(II). This work aims to develop a kinetic model that adequately describes the electro-oxidation process of Fe(II) in air-cathode fuel cells. The speciation of Fe(II) is incorporated into the model, and contributions of individual Fe(II) species to the overall Fe(II) oxidation rate are quantitatively evaluated. The results show that the kinetic model can accurately predict the electro-oxidation rate of Fe(II) in air-cathode fuel cells. FeCO3, Fe(OH)2, and Fe(CO3)2(2-) are the most important species determining the electro-oxidation kinetics of Fe(II). The Fe(II) oxidation rate is primarily controlled by the oxidation of FeCO3 species at low pH, whereas at high pH Fe(OH)2 and Fe(CO3)2(2-) are the dominant species. Solution pH, carbonate concentration, and solution salinity are able to influence the electro-oxidation kinetics of Fe(II) through changing both distribution and kinetic activity of Fe(II) species.

Sorption Mechanisms of Cesium on Cu II2Fe II(CN) 6and Cu II3[Fe III(CN) 6] 2Hexacyanoferrates and Their Relation to the Crystalline Structure

Science.gov (United States)

Ayrault, S.; Jimenez, B.; Garnier, E.; Fedoroff, M.; Jones, D. J.; Loos-Neskovic, C.

1998-12-01

CuII2FeII(CN)6·xH2O and CuII3[FeIII(CN)6]2·xH2O can be prepared with reproducible chemical compositions and structures after careful washing. They have cubicFmoverline3mstructures with iron vacancies. In CuII2FeII(CN)6, copper occupies two different sites: Cu1 in position 4blinked to Fe through the CN groups, and Cu2 not linked to the CN groups and partially occupying the interstitial 24epositions. The second type of site is not present in CuII3[FeIII(CN)6]2. Sorption kinetics and isotherms were determined for cesium on both hexacyanoferrates by batch experiments. On CuII3[FeIII(CN)6]2, the maximum uptake is only 0.073 Cs/Fe (at./at.). On CuII2FeII(CN)6, the uptake reaches 1.5 Cs/Fe. The sorption kinetics include at least two steps: at1/2variation until approximately 72 h and then a slow evolution studied up to 6 months. The sorption mechanism is complex. The main process seems to be diffusion of ion pairs, followed by a reorganization of the solid, resulting in one or more new solid phases. The presence of the Cu2 site seems to play a favorable role in the sorption. Owing to its good midterm stability and the first rapid step of exchange, CuII2FeII(CN)6·xH2O seems to be one of the most promising compounds for the recovery of cesium from nuclear liquid wastes.

The n-propyl 3-azido-2,3-dideoxy-β-D-arabino-hexopyranoside: Syntheses, crystal structure, physical properties and stability constants of their complexes with Cu(II), Ni(II) and VO(II)

Science.gov (United States)

Barabaś, Anna; Madura, Izabela D.; Marek, Paulina H.; Dąbrowska, Aleksandra M.

2017-11-01

The structure, conformation and configuration of the n-propyl 3-azido-2,3-dideoxy-β-D-arabino-hexopyranoside (BAra-nPr) were determined by 1H NMR, 13C NMR, and IR spectroscopy, as well as by optical rotation. The crystal structure was confirmed by single-crystal X-ray diffraction studies at room temperature. The compound crystallizes in P21 space group symmetry of the monoclinic system. The molecule has a 4C1 chair conformation with azide group in the equatorial position both in a solution as well as in the crystal. The spatial arrangement of azide group is compared to other previously determined azidosugars. The hydrogen bonds between the hydroxyl group of sugar molecules lead to a ribbon structure observed also for the ethyl homolog. The packing of ribbons is dependent on the alkyl substituent length and with the elongation changes from pseudohexagonal to lamellar. Acidity constants for the n-propyl 3-azido-2,3-dideoxy-β-D-arabino-hexopyranoside (BAra-nPr) in an aqueous solution were evaluated by the spectrophotometric and potentiometric titrations methods. Title compound exhibit blue absorption with the maximum wavelengths in the range of 266 nm and 306 nm. Based on these measurements we showed equilibria existing in a particular solution and a distribution of species which have formed during the titration. We also investigated interactions between Cu(II), Ni(II) and VO(II) and title compound (as ligand L) during complexometric titration. On these bases we identified that in [CuII-BAra-nPr]2+ the ratio of the ligand L to metal ion M(II) was 3:1, while in [NiII-BAra-nPr]2+ and [VOII-BAra-nPr]2+ complexes 2:1 ratios were found. The cumulative stability constants (as log β) occurring in an aqueous solution for the complexes of BAra-nPr with Cu(II), Ni(II) and VO(IV) were 14.57; 11.71 and 4.20, respectively.

Reduced plasma noradrenaline during angiotensin II-induced acute hypertension in man

DEFF Research Database (Denmark)

Henriksen, J H; Kastrup, J; Christensen, N J

1985-01-01

1. Plasma noradrenaline and adrenaline concentrations were measured in ten subjects before, during and after intravenous infusion of angiotensin II (ANG II) in order to determine the sympathoadrenal response of ANG II challenge in man. In five subjects ganglionic blockade was additionally performed...... by intravenous infusion of trimethaphan. 2. During ANG II infusion mean arterial blood pressure increased by 30% (P adrenaline decreased less. 3. During ganglionic blockade plasma noradrenaline decreased significantly (P

The prevalence of microalbuminuria among patients with type II ...

African Journals Online (AJOL)

This cross-sectional community-based study was carried out to determine the prevalence of microalbuminuria among patients with type II diabetes mellitus in a primary care setting, and to study the association between various risk factors and the presence of microalbuminuria. All patients with type II diabetes mellitus who ...

Solar photocatalytic removal of Cu(II), Ni(II), Zn(II) and Pb(II): Speciation modeling of metal-citric acid complexes

International Nuclear Information System (INIS)

Kabra, Kavita; Chaudhary, Rubina; Sawhney, R.L.

2008-01-01

The present study is targeted on solar photocatalytic removal of metal ions from wastewater. Photoreductive deposition and dark adsorption of metal ions Cu(II), Ni(II), Pb(II) and Zn(II), using solar energy irradiated TiO 2 , has been investigated. Citric acid has been used as a hole scavenger. Modeling of metal species has been performed and speciation is used as a tool for discussing the photodeposition trends. Ninety-seven percent reductive deposition was obtained for copper. The deposition values of other metals were significantly low [nickel (36.4%), zinc (22.2%) and lead (41.4%)], indicating that the photocatalytic treatment process, using solar energy, was more suitable for wastewater containing Cu(II) ions. In absence of citric acid, the decreasing order deposition was Cu(II) > Ni(II) > Pb(II) > Zn(II), which proves the theoretical thermodynamic predictions about the metals

Dual repressive effect of angiotensin II-type 1 receptor blocker telmisartan on angiotensin II-induced and estradiol-induced uterine leiomyoma cell proliferation.

Science.gov (United States)

Isobe, Aki; Takeda, Takashi; Sakata, Masahiro; Miyake, Asako; Yamamoto, Toshiya; Minekawa, Ryoko; Nishimoto, Fumihito; Oskamoto, Yoko; Walker, Cheryl Lyn; Kimura, Tadashi

2008-02-01

Although uterine leiomyomas or fibroids are the most common gynecological benign tumor and greatly affect reproductive health and well-being, the pathophysiology and epidemiology of uterine leiomyomas are poorly understood. Elevated blood pressure has an independent, positive association with risk for clinically detected uterine leiomyoma. Angiotensin II (Ang II) is a key biological peptide in the renin-angiotensin system that regulates blood pressure. In this study, we investigated the potential role of Ang II (1-1000 nM) in the proliferation of rat ELT-3 leiomyoma cells in vitro. RT-PCR and western blot analysis with cell proliferation and DNA transfection assays were performed to determine the mechanism of action of Ang II. Ang II induced ELT-3 leiomyoma cell proliferation (P estradiol-induced cell proliferation (P < 0.01). AT(1)R, but not AT(2)R, plays a role in Ang II-induced ELT-3 cell proliferation. These experimental findings in vitro highlight the potential role of Ang II in the proliferation of leiomyoma cells.

Cd(II), Cu(II)

African Journals Online (AJOL)

user

Depending on the way goethite was pretreated with oxalic acid, affinity for Cd(II) varied ...... Effects and mechanisms of oxalate on Cd(II) adsorption on goethite at different ... precipitation, surfactant mediation, hydrothermal and micro-emulsion.

Sequestration of Cu(II), Ni(II), and Co(II) by ethyleneimine immobilized on silica

International Nuclear Information System (INIS)

Arakaki, Luiza N.H.; Alves, Ana Paula M.; Silva Filho, Edson C. da; Fonseca, Maria G.; Oliveira, Severino F.; Espinola, Jose Geraldo P.; Airoldi, Claudio

2007-01-01

Thermodynamic data on interaction of Cu(II), Ni(II), and Co(II) with silica modified with ethyleneimine are obtained by calorimetric titration. The amount of ethyleneimine anchored on silica surface was estimated to be 0.70 mmol g -1 . The enthalpies of binding Ni(II), Cu(II) and Co(II), are -3.59 ± 0.001, -4.88 ± 0.001, and -7.75 ± 0.003 kJ mol -1 , respectively

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

International Nuclear Information System (INIS)

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

2011-01-01

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

Direct determination of bulk etching rate for LR-115-II solid state ...

Indian Academy of Sciences (India)

The thickness of the removed layer of the LR-115-II solid state nuclear track detector during etching is measured directly with a rather precise instrument. Dependence of bulk etching rate on temperature of the etching solution is investigated. It has been found that the bulk etching rate is 3.2 m/h at 60°C in 2.5 N NaOH of ...

Opposing motor activities of dynein and kinesin determine retention and transport of MHC class II-containing compartments

NARCIS (Netherlands)

Wubbolts, R.; Fernandez-Borja, M.; Jordens, I.; Reits, E.; Dusseljee, S.; Echeverri, C.; Vallee, R. B.; Neefjes, J.

1999-01-01

MHC class II molecules exert their function at the cell surface by presenting to T cells antigenic fragments that are generated in the endosomal pathway. The class II molecules are targetted to early lysosomal structures, termed MIIC, where they interact with antigenic fragments and are subsequently

Effects of binding metronidazole to a copper-acetate compound on radiosensitizer properties

International Nuclear Information System (INIS)

Negron, Ana C. Valderrama; Silva, Denise de Oliveira; Cruz, Aurea S.

2009-01-01

Copper compounds exhibit interesting biological properties. Nitroimidazoles show radiosensitizer properties for radiotherapy tumor treatment. In the present work, the effect of binding metronidazole (1-(2-hydroxyethyl)-2-methyl-5-nitroimidazole = MTZ) to copper-acetate on the radiosensitizer properties has been investigated. A compound of copper-acetate-MTZ was prepared and characterized. The experiments were carried out by gamma-irradiation of Hep2 (human larynx cancer) cells under hypoxic conditions. The radiation doses for 50% cell survival in the presence of radiosensitizer were about 8.2 Gy for CuAcMTZ or free MTZ. The effect of binding metronidazole to copper acetate on radiosensitizer properties is mainly related to the radiosensitizer process which involves two events for CuAcMTZ in contrast to one event observed for the MTZ free drug. (author)

Effect of hepatocyte growth factor and angiotensin II on rat cardiomyocyte hypertrophy

Energy Technology Data Exchange (ETDEWEB)

Chen, Ai-Lan [Department of Cardiology, The First Affiliated Hospital of Guangzhou Medical University, Guangzhou (China); Ou, Cai-Wen [The Fourth Affiliated Hospital of Guangzhou Medical University, Guangzhou (China); He, Zhao-Chu [Department of Cardiology, The First Affiliated Hospital of Guangzhou Medical University, Guangzhou (China); Liu, Qi-Cai [Experimental Medical Research Center, Guangzhou Medical University, Guangzhou (China); Dong, Qi [Department of Physiology, Guangzhou Medical University, Guangzhou (China); Chen, Min-Sheng [Guangzhou Key Laboratory of Cardiovascular Disease, Guangzhou Institute of Cardiovascular Disease, The Second Affiliated Hospital of Guangzhou Medical University, Guangzhou (China)

2012-10-15

Angiotensin II (Ang II) plays an important role in cardiomyocyte hypertrophy. The combined effect of hepatocyte growth factor (HGF) and Ang II on cardiomyocytes is unknown. The present study was designed to determine the effect of HGF on cardiomyocyte hypertrophy and to explore the combined effect of HGF and Ang II on cardiomyocyte hypertrophy. Primary cardiomyocytes were isolated from neonatal rat hearts and cultured in vitro. Cells were treated with Ang II (1 µM) alone, HGF (10 ng/mL) alone, and Ang II (1 µM) plus HGF (10 ng/mL) for 24, 48, and 72 h. The amount of [{sup 3}H]-leucine incorporation was then measured to evaluate protein synthesis. The mRNA levels of β-myosin heavy chain and atrial natriuretic factor were determined by real-time PCR to evaluate the presence of fetal phenotypes of gene expression. The cell size of cardiomyocytes was also studied. Ang II (1 µM) increased cardiomyocyte hypertrophy. Similar to Ang II, treatment with 1 µM HGF promoted cardiomyocyte hypertrophy. Moreover, the combination of 1 µM Ang II and 10 ng/mL HGF clearly induced a combined pro-hypertrophy effect on cardiomyocytes. The present study demonstrates for the first time a novel, combined effect of HGF and Ang II in promoting cardiomyocyte hypertrophy.

Determination of quercetin using a photo-electrochemical sensor modified with titanium dioxide and a platinum(II)-porphyrin complex

International Nuclear Information System (INIS)

Tian, Li; Wang, Binbin; Chen, Ruizhan; Gao, Ye; Chen, Yanling; Li, Tianjiao

2015-01-01

A glassy carbon electrode (GCE) was modified with a film containing titanium dioxide and a Pt(II)-porphyrin complex, and its response to quercetin was investigated employing cyclic voltammetry and chronoamperometry. The oxidation current caused by quercetin is largely enhanced under UV illumination. The effects of pH value, mass of TiO 2 in the film, UV illumination time and applied potential were studied. Under optimized conditions, the peak current at a typically applied voltage of +0.4 V depends linearly on the concentration of quercetin in the 0.002 to 50 mg L −1 range. The detection limit (at an SNR of 3) is 0.8 μg L −1 . The method was successfully applied to the determination of quercetin in (spiked) samples of tea and apple juice. (author)

Differential association of the N-propeptide of collagen IIA (PIIANP) and collagen II C-telopeptide (CTX-II) with synovitis and erosions in early and longstanding rheumatoid arthritis

DEFF Research Database (Denmark)

Christensen, A F; Lottenburger, T; Lindegaard, H

2009-01-01

OBJECTIVES: To determine the N-terminal propeptide of collagen IIA (PIIANP) in early and established rheumatoid arthritis (RA) and to study the association with collagen II degradation assessed by its C-telopeptide (CTX-II), x-ray status and disease activity measures. METHODS: Two cohorts of RA......-ray progression (p=0.84). There was no correlation between PIIANP and CTX-II. CONCLUSION: Declining PIIANP with increasing RA duration and persistently increased CTX-II indicate that cartilage anabolic and degradative pathways are unbalanced from clinical RA onset. Furthermore, that collagen II depletion in RA...... is both mediated by anti-anabolic effects unassociated with synovitis (decreased PIIANP) and by excess collagen II degradation linked to synovitis (increased CTX-II)....

EBR-II: summary of operating experience

International Nuclear Information System (INIS)

Perry, W.H.; Leman, J.D.; Lentz, G.L.; Longua, K.J.; Olson, W.H.; Shields, J.A.; Wolz, G.C.

1978-01-01

Experimental Breeder Reactor II (EBR-II) is an unmoderated, sodium-cooled reactor with a design power of 62.5 MWt. The primary cooling system is a submerged-pool type. The early operation of the reactor successfully demonstrated the feasibility of a sodium-cooled fast breeder reactor operating as an integrated reactor, power plant, and fuel-processing facility. In 1967, the role of EBR-II was reoriented from a demonstration plant to an irradiation facility. Many changes have been made and are continuing to be made to increase the usefulness of EBR-II for irradiation and safety tests. A review of EBR-II's operating history reveals a plant that has demonstrated high availability, stable and safe operating characteristics, and excellent performance of sodium components. Levels of radiation exposure to the operating and maintenance workers have been low; and fission-gas releases to the atmosphere have been minimal. Driver-fuel performance has been excellent. The repairability of radioactive sodium components has been successfully demonstrated a number of times. Recent highlights include installation and successful operation of (1) the hydrogen-meter leak detectors for the steam generators, (2) the cover-gas-cleanup system and (3) the cesium trap in the primary sodium. Irradiations now being conducted in EBR-II include the run-beyond-cladding breach fuel tests for mixed-oxide and carbide elements. Studies are in progress to determine EBR-II's capability for conducting important ''operational safety'' tests. These tests would extend the need and usefulness of EBR-II into the 1980's

Morphological caracteristics of malocclusion class II

Directory of Open Access Journals (Sweden)

Pavlović J.

2015-01-01

Full Text Available Class II malocclusion are complex anomalies of the skeletal and dental systems. The aim of this study is that the rengenkefalometrics analysis closer determine the morphological characteristics of this malocclusion. For this study were used 30 patients aged 18-30, previously clinically diagnosed class II, before the planned orthodontic treatment. The results analisis lateral cephalometric radiographs were compared with the 30 patients with class I malocclusion. Analyzed three linear and two angular cranial base dimensions and nine angular and four linear measures from the facial skeleton. The Results show: No statistically significant differensis in cranial base angle (SNBa and anterior cranial base length (S-N between class II and control Class I. Angle maxillar prognathism ( SNA is no signifikant different between class I and Class II but SNB angle were signifikant smaller. The length of maxillary base (A'-SnP is longer and the length of mandibule (Pg'-MT1/MT is signifficantly smaller. The gonial angle (ArGo-Me was smaller with open articular angle (GoArSN. Morphological characteristics of class II malocclusion are , retrognathic and smaller mandibular ligth, normognathic and longer maxilla, open articular angle with vertical tendency of the craniofacial growth pattern.

Ca II H and K emission from late-type stars

International Nuclear Information System (INIS)

Middlekoop, F.

1982-01-01

This thesis is based on a study of the Ca II H and K emission features of late main-sequence stars. In Chapter II it is shown that rotation periods can be determined from a modulation in the Ca II H and K signal for many stars in a broad range of spectral types. In Chapter III it is shown that a clear correlation exists between Ca II H and K emission and rotational velocity in active main-sequence stars. There is an indication for a (probably colour-dependent) critical velocity at which the Ca II H and K emission suddenly drops. Chapter IV discusses the dependence of Ca II H and K emission on the rotation rate for evolved stars. (Auth./C.F.)

Drug: D00409 [KEGG MEDICUS

Lifescience Database Archive (English)

Full Text Available moniasis [DS:H00812] Intestinal amebiasis (amebic dysentery) [DS:H00360] Anaerobic bacterial infections [DS:H01410] Bacterial endocar...ditis [DS:H00334] ... Nitroimidazole derivative Trichomonas infection ... Enzyme: CYP2A6

Belle II silicon vertex detector

Energy Technology Data Exchange (ETDEWEB)

Adamczyk, K. [H. Niewodniczanski Institute of Nuclear Physics, Krakow 31-342 (Poland); Aihara, H. [Department of Physics, University of Tokyo, Tokyo 113-0033 (Japan); Angelini, C. [Dipartimento di Fisica, Università di Pisa, I-56127 Pisa (Italy); INFN Sezione di Pisa, I-56127 Pisa (Italy); Aziz, T.; Babu, V. [Tata Institute of Fundamental Research, Mumbai 400005 (India); Bacher, S. [H. Niewodniczanski Institute of Nuclear Physics, Krakow 31-342 (Poland); Bahinipati, S. [Indian Institute of Technology Bhubaneswar, Satya Nagar (India); Barberio, E.; Baroncelli, Ti.; Baroncelli, To. [School of Physics, University of Melbourne, Melbourne, Victoria 3010 (Australia); Basith, A.K. [Indian Institute of Technology Madras, Chennai 600036 (India); Batignani, G. [Dipartimento di Fisica, Università di Pisa, I-56127 Pisa (Italy); INFN Sezione di Pisa, I-56127 Pisa (Italy); Bauer, A. [Institute of High Energy Physics, Austrian Academy of Sciences, 1050 Vienna (Austria); Behera, P.K. [Indian Institute of Technology Madras, Chennai 600036 (India); Bergauer, T. [Institute of High Energy Physics, Austrian Academy of Sciences, 1050 Vienna (Austria); Bettarini, S. [Dipartimento di Fisica, Università di Pisa, I-56127 Pisa (Italy); INFN Sezione di Pisa, I-56127 Pisa (Italy); Bhuyan, B. [Indian Institute of Technology Guwahati, Assam 781039 (India); Bilka, T. [Faculty of Mathematics and Physics, Charles University, 121 16 Prague (Czech Republic); Bosi, F. [INFN Sezione di Pisa, I-56127 Pisa (Italy); Bosisio, L. [Dipartimento di Fisica, Università di Trieste, I-34127 Trieste (Italy); INFN Sezione di Trieste, I-34127 Trieste (Italy); and others

2016-09-21

The Belle II experiment at the SuperKEKB collider in Japan is designed to indirectly probe new physics using approximately 50 times the data recorded by its predecessor. An accurate determination of the decay-point position of subatomic particles such as beauty and charm hadrons as well as a precise measurement of low-momentum charged particles will play a key role in this pursuit. These will be accomplished by an inner tracking device comprising two layers of pixelated silicon detector and four layers of silicon vertex detector based on double-sided microstrip sensors. We describe herein the design, prototyping and construction efforts of the Belle-II silicon vertex detector.

Analytical applications of some macro-schiff's bases for spectrophotometric determination of some metal ions

International Nuclear Information System (INIS)

Ahmed, N. A. M.

2005-06-01

In this research three schiff's bases PAD, N, NBPAD and N, NBHPAD were synthesized by condensation of o-phenylenediamine with p-aminoacetophenone, to give an intermediate which then further condensed with benzil, and 2,5 hexanedione, respectively, in ethanol to give macro schiff's bases. These schiff's bases were identified using I.R spectra, UV/VIS spectrophotometer, elemental analyzer, and melting point. Their applications as analytical reagents were studied using UV/VIS spectrophotometer with Pb(II), Cr(VI), Cu(II), Cd(II), V(V), Ni(II), Hg(II), Zn(II), Co(II), Fe(II) and Fe(III). Various parameters were investigated in order to find their optimum conditions for the analytical application of these schiff's bases. These include the effect of solvent, the effect of micelle as well as the presence of foreign metal ions. Good results were obtained for determination of Cr(VI), and V(V) with N, NBPAD in terms of linearity detection limit, and interference, and for the determination of Fe(II) with N, NBHPAD. The stoichiometry of some these complexes was determined. The study also showed a good results for the determination of Hg(II), and Pb(II) (two serious environmental pollutants) if interference is removed.(Author)

potentiometric studies of the complexes formed by copper (ii) and zinc

African Journals Online (AJOL)

MBI

, P. M. B. 3011, Kano, Nigeria e-mail: jnaaliya@yahoo.com. ABSTRACT. The overall stability constants of copper (II) and zinc (II) ions with some polar uncharged amino acids including proline, threonine and asparagines were determined by ...

Removal of Ca(II) and Mg(II) from potassium chromate solution on Amberlite IRC 748 synthetic resin by ion exchange

International Nuclear Information System (INIS)

Yu Zhihui; Qi Tao; Qu Jingkui; Wang Lina; Chu Jinglong

2009-01-01

Experimental measurements have been made on the batch ion exchange of Ca(II) and Mg(II) from potassium chromate solution using cation exchanger of Amberlite IRC 748 as K + form. The ion exchange behavior of two alkaline-earth metals on the resin, depending on contact time, pH, temperature and resin dosage was studied. The adsorption isotherms were described by means of the Langmuir and Freundlich isotherms. For Ca(II) ion, the Langmuir model represented the adsorption process better than the Freundlich model. The maximum ion exchange capacity was found to be 47.21 mg g -1 for Ca(II) and 27.70 mg g -1 for Mg(II). The kinetic data were tested using Lagergren-first-order and pseudo-second-order kinetic models. Kinetic data correlated well with the pseudo-second-order kinetic model, indicating that the chemical adsorption was the rate-limiting step. Various thermodynamic parameters such as Gibbs free energy (ΔG o ), enthalpy (ΔH o ) and entropy (ΔS o ) were also calculated. These parameters showed that the ion exchange of Ca(II) and Mg(II) from potassium chromate solution was feasible, spontaneous and endothermic process in nature. The activation energy of ion-exchange (E a ) was determined as 12.34 kJ mol -1 for Ca(II) and 9.865 kJ mol -1 for Mg(II) according to the Arrhenius equation.

Syntheses, structural characterization and spectroscopic studies of cadmium(II)-metal(II) cyanide complexes with 4-(2-aminoethyl)pyridine

Science.gov (United States)

Karaağaç, Dursun; Kürkçüoğlu, Güneş Süheyla; Şenyel, Mustafa; Hökelek, Tuncer

2017-02-01

Three new cadmium(II)-metal(II) cyanide complexes, [Cd(4aepy)2(H2O)2][Ni(CN)4] (1), [Cd(4aepy)2(H2O)2][Pd(CN)4] (2) and [Cd(4aepy)2(H2O)2][Pt(CN)4] (3) [4aepy = 4-(2-aminoethyl)pyridine], have been synthesized and characterized by elemental, thermal, FT-IR and Raman spectral analyses. The crystal structures of 1 and 2 have been determined by single crystal X-ray diffraction technique, in which they crystallize in the monoclinic system and C2/c space group. The M(II) [M(II) = Ni(II), Pd(II) and Pt(II)] ions are coordinated with the carbon atoms of the four cyanide groups in the square planar geometries and the [M(CN)4]2- ions act as counter ions. The Cd(II) ions display an N4O2 coordination sphere with a distorted octahedral geometry, the nitrogen donors belonging to four molecules of the organic 4aepy that act as unidentate ligands and two oxygen atoms from aqua ligands. 3D supramolecular structures of 1 and 2 were occurred by M⋯π and hydrogen bonding (Nsbnd H⋯N and Osbnd H⋯N) interactions. Vibrational assignments of all the observed bands were given and the spectral properties were also supported the crystal structures of the complexes. A possible decompositions of the complexes were investigated in the temperature range 30-800 °C in the static atmosphere.

Synthesis and characterization of a surface-grafted Cd(II) ion-imprinted polymer for selective separation of Cd(II) ion from aqueous solution

Energy Technology Data Exchange (ETDEWEB)

Li, Min [State Key Laboratory of Explosion Science and Technology, Beijing Institute of Technology, Beijing 100081 (China); Feng, Changgen, E-mail: cgfeng@cast.org.cn [State Key Laboratory of Explosion Science and Technology, Beijing Institute of Technology, Beijing 100081 (China); Li, Mingyu; Zeng, Qingxuan; Gan, Qiang [State Key Laboratory of Explosion Science and Technology, Beijing Institute of Technology, Beijing 100081 (China); Yang, Haiyan [Research Institute of Tsinghua University in Shenzhen, Shenzhen 518057 (China)

2015-03-30

Highlights: • Cd(II) ion-imprinted polymer (Cd(II)-IIP) is prepared. • Cd(II)-IIP shows high stability, good selectivity and reusability. • Cd(II)-IIP can be used as a sorbent for selective removal of Cd(II) ion. - Abstract: A novel Cd(II) ion-imprinted polymer (Cd(II)-IIP) was prepared with surface imprinting technology by using cadmium chloride as a template and allyl thiourea (ATU) as a functional monomer for on-line solid-phase extraction of trace Cd(II) ion and selective separation Cd(II) ion in water samples. The Cd(II)-IIP exhibited good chemical performance and thermal stability. Kinetics studies showed that the equilibrium adsorption was achieved within 8.0 min and the adsorption process can be described by pseudo-second-order kinetic model. Compared to the Cd(II) non-imprinted polymer (Cd(II)-NIP), the Cd(II)-IIP had a higher adsorption capacity and selectivity for Cd(II) ion. The maximum adsorption capacities of the Cd(II)-IIP and Cd(II)-NIP for Cd(II) were 38.30 and 13.21 mg g{sup −1}, respectively. The relative selectivity coefficients of the adsorbent for Cd(II) in the presence of Cu{sup 2+}, Ni{sup 2+}, Co{sup 2+}, Pb{sup 2+} and Zn{sup 2+} were 2.86, 6.42, 11.50, 9.46 and 3.73, respectively. In addition, the Cd(II) ion adsorbed was easy to remove from sorbent and the Cd(II)-IIP exhibited good stability and reusability. The adsorption capacity had no obvious decrease after being used six times. The accuracy of this method was verified by the standard reference material, it was then applied for cadmium ion determination in different types of water samples.

Average [O II] nebular emission associated with Mg II absorbers: dependence on Fe II absorption

Science.gov (United States)

Joshi, Ravi; Srianand, Raghunathan; Petitjean, Patrick; Noterdaeme, Pasquier

2018-05-01

We investigate the effect of Fe II equivalent width (W2600) and fibre size on the average luminosity of [O II] λλ3727, 3729 nebular emission associated with Mg II absorbers (at 0.55 ≤ z ≤ 1.3) in the composite spectra of quasars obtained with 3 and 2 arcsec fibres in the Sloan Digital Sky Survey. We confirm the presence of strong correlations between [O II] luminosity (L_{[O II]}) and equivalent width (W2796) and redshift of Mg II absorbers. However, we show L_{[O II]} and average luminosity surface density suffer from fibre size effects. More importantly, for a given fibre size, the average L_{[O II]} strongly depends on the equivalent width of Fe II absorption lines and found to be higher for Mg II absorbers with R ≡W2600/W2796 ≥ 0.5. In fact, we show the observed strong correlations of L_{[O II]} with W2796 and z of Mg II absorbers are mainly driven by such systems. Direct [O II] detections also confirm the link between L_{[O II]} and R. Therefore, one has to pay attention to the fibre losses and dependence of redshift evolution of Mg II absorbers on W2600 before using them as a luminosity unbiased probe of global star formation rate density. We show that the [O II] nebular emission detected in the stacked spectrum is not dominated by few direct detections (i.e. detections ≥3σ significant level). On an average, the systems with R ≥ 0.5 and W2796 ≥ 2 Å are more reddened, showing colour excess E(B - V) ˜ 0.02, with respect to the systems with R < 0.5 and most likely trace the high H I column density systems.

Syntheses, crystal structures and spectroscopic properties of copper(II)-tetracyanometallate(II) complexes with nicotinamide and isonicotinamide ligands

Science.gov (United States)

Sayın, Elvan; Kürkçüoğlu, Güneş Süheyla; Yeşilel, Okan Zafer; Hökelek, Tuncer

2015-09-01

Four new one dimensional (1D) cyanide complexes, namely {[Cu(NH3)4(μ-na)][M‧(CN)4]}n and {[Cu(NH3)2(ina)2M‧(μ-CN)2(CN)2]}n (M‧(II) = Pd (1 and 3) or Pt (2 and 4), na:nicotinamide and ina:isonicotinamide) have been synthesized and characterized by elemental, spectral (FT-IR and Raman), and thermal (TG, DTG and DTA) analyses. The crystal structures of complexes 1-3 have been determined by single crystal X-ray diffraction technique. In complexes 1 and 2, na ligand is coordinated to the adjacent Cu(II) ions as a bridging ligand, giving rise to 1D linear cationic chain and the [M‧(CN)4]2- anionic complex acts as a counter ion. Complexes 3 and 4 are also 1D linear chain in which two cyanide ligands bridged neighboring M‧(II) and Cu(II) ions, while ina ligand is coordinated Cu(II) ion through nitrogen atom of pyridine ring. In the complexes, the Cu(II) ions adopt distorted octahedral geometries, while M‧(II) ions are four coordinated with four carbon atoms from cyanide ligands in square-planar geometries. The adjacent chains are further stacked through intermolecular hydrogen bond, Nsbnd Hṡṡṡπ, Csbnd H⋯M‧ and M‧⋯π interactions to form 3D supramolecular networks. Vibration assignments are given for all the observed bands. In addition, thermal stabilities of the compounds are also discussed.

An efficient, cost effective, sensing behaviour liquid-liquid extraction and spectrophotometric determination of copper(II) incorporated with 4-(4'-chlorobenzylideneimino)-3-methyl-5-mercapto-1, 2, 4-triazole: Analysis of food samples, leafy vegetables, fertilizers and environmental samples.

Science.gov (United States)

Barache, Umesh B; Shaikh, Abdul B; Lokhande, Tukaram N; Kamble, Ganesh S; Anuse, Mansing A; Gaikwad, Shashikant H

2018-01-15

The aim of the present work is to develop an efficient, simple and selective moreover cost-effective method for the extractive spectrophotometric determination of copper(II) by using the Schiff base 4-(4'-chlorobenzylideneimino)-3-methyl-5-mercapto-1, 2, 4-triazole [CBIMMT]. This chromogenic reagent forms a yellow coloured complex with copper(II) in acetate buffer at pH4.2. The copper(II) complex with ligand is instantly extracted into chloroform and shows a maximum absorbance at 414nm which remains stable for >48h. The composition of extracted complex is found to be 1:2 [copper(II): reagent] which was ascertained using Job's method of continuous variation, mole ratio method and slope ratio method. Under optimal conditions, the copper(II) complex in chloroform adheres to Beer's law up to 17.5μgmL -1 of copper(II). The optimum concentration range obtained from Ringbom's plot is from 5μgmL -1 to 17.5μgmL -1 . The molar absorptivity, Sandell's sensitivity and enrichment factor of the extracted copper(II) chelate are 0.33813×10 4 Lmol -1 cm -1 , 0.01996μgcm -2 and 2.49 respectively. In the extraction of copper(II), several affecting factors including the solution pH, ligand concentration, equilibrium time, effect of foreign ions are optimized. The interfering effects of various cations and anions were also studied and use of masking agents enhances the selectivity of the method. The chromogenic sulphur containing reagent, 4-(4'-chlorobenzylideneimino)-3-methyl-5-mercapto-1, 2, 4-triazole has been synthesized in a single step with high purity and yield. The synthesized reagent has been successfully applied first time for determination of copper(II). The reagent forms stable chelate with copper(II) in buffer medium instantly and quantitatively extracted in chloroform within a minute. The method is successfully applied for the determination of copper(II) in various synthetic mixtures, complexes, fertilizers, environmental samples such as food samples, leafy

Adsorption efficiencies of calcium (II ion and iron (II ion on activated carbon obtained from pericarp of rubber fruit

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Orawan Sirichote

2008-03-01

Full Text Available Determination of adsorption efficiencies of activated carbon from pericarp of rubber fruit for calcium (II ion and iron (II ion has been performed by flowing the solutions of these ions through a column of activated carbon. The weights of activated carbon in 500 mL buret column (diameter 3.2 cm for flowing calcium (II ion and iron (II ion solutions were 15 g and 10 g, respectively. The initial concentration of calcium ion was prepared to be about eight times more diluted than the true concentration found in the groundwater from the lower part of southern Thailand. Calcium (II ion concentrations were analysed by EDTA titration and its initial concentration was found to be 23.55 ppm. With a flow rate of 26 mL/min, the adsorption efficiency was 11.4 % with passed through volume 4.75 L. Iron (II ion concentrations were analysed by spectrophotometric method; its initial concentration was found to be 1.5565 ppm. At a flow rate of 22 mL/min, the adsorption efficiency was 0.42 % with passed through volume of 34.0 L.

Microcephalic osteodysplastic primordial dwarfism type II (MOPD II) with multiple vascular complications misdiagnosed as Dubowitz syndrome.

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Dieks, Jana-Katharina; Baumer, Alessandra; Wilichowski, Ekkehard; Rauch, Anita; Sigler, Matthias

2014-09-01

To date, the genetic basis of Dubowitz syndrome (short stature, microcephaly, facial abnormalities, eczema) is unknown and vascular complications are not known to be associated with this syndrome. In microcephalic osteodysplastic primordial dwarfism type II (MOPD II; disproportionate short statue, microcephaly, facial abnormalities), however, cerebral aneurysms and other vascular abnormalities are frequent complications. MOPD II is a genetic disorder caused by mutations in the pericentrin (PCNT) gene (21q22). We report on a patient who came to our attention as a 22-year-old with subarachnoid bleeding due to a ruptured cranial aneurysm. Until then, the patient was thought and published to have Dubowitz syndrome; previously, he was treated with coronary bypass surgery for extensive coronary angiopathy. Consecutive genetic testing revealed MOPD II. After clinical stabilization, the patient was discharged to a specialized rehabilitation center where he died due to re-rupture of a cranial aneurysm. In patients with short stature-especially when clinical features are accompanied by vascular complications-MOPD II should be considered as a differential diagnosis leading to consecutive genetic testing. After detection of mutations in the PCNT gene, a full vascular status including cerebral imaging and cardiac evaluation needs to be determined in order to analyze vascular abnormalities and initiate prophylactic treatment.

Method for the determination of technical specifications limiting temperature in EBR-II operation

International Nuclear Information System (INIS)

Chang, L.K.; Hill, D.J.; Ku, J.Y.

2004-01-01

The methodology and analysis procedure to qualify the Mark-V and Mark-VA fuels for the Experimental Breeder Reactor II are summarized in this paper. Fuel performance data and design safety criteria are essential for thermal-hydraulic analyses and safety evaluations. Normal and off-normal operation duty cycles and transient classifications are required for the safety assessment of the fuels. Design safety criteria for steady-state normal and transient off-normal operations were developed to ensure structural integrity of the fuel pin. The maximum allowable coolant outlet temperatures and powers of subassemblies for steady-state normal operation conditions were first determined in a row-by-row basis by a thermal-hydraulic and fuel damage analysis, in which a trial-and-error approach was used to predict the maximum subassembly coolant outlet temperatures and powers that satisfy the design safety criteria for steady-state normal operation conditions. The limiting steady-state temperature and power were then used as the initial subassembly thermal conditions for the off-normal transient analysis to assess the safety performance of the fuel pin for anticipated, unlikely and extremely unlikely events. If the design safety criteria for the off-normal events are not satisfied, then the initial steady-state subassembly temperatures and/or powers are reduced and an iterative procedure is employed until the design safety criteria for off-normal conditions are satisfied, and the initial subassembly outlet coolant temperature and power are the technical specification limits for reactor operation. (author)

New Cu (II), Co(II) and Ni(II) complexes of chalcone derivatives: Synthesis, X-ray crystal structure, electrochemical properties and DFT computational studies

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Tabti, Salima; Djedouani, Amel; Aggoun, Djouhra; Warad, Ismail; Rahmouni, Samra; Romdhane, Samir; Fouzi, Hosni

2018-03-01

The reaction of nickel(II), copper(II) and cobalt(II) with 4-hydroxy-3-[(2E)-3-(1H-indol-3-yl)prop-2-enoyl]-6-methyl-2H-pyran-2-one (HL) leads to a series of new complexes: Ni(L)2(NH3), Cu(L)2(DMF)2 and Co(L)2(H2O). The crystal structure of the Cu(L)2(DMF)2 complex have been determined by X-ray diffraction methods. The Cu(II) lying on an inversion centre is coordinated to six oxygen atoms forming an octahedral elongated. Additionally, the electrochemical behavior of the metal complexes were investigated by cyclic voltammetry at a glassy carbon electrode (GC) in CH3CN solutions, showing the quasi-reversible redox process ascribed to the reduction of the MII/MI couples. The X-ray single crystal structure data of the complex was matched excellently with the optimized monomer structure of the desired compound; Hirschfeld surface analysis supported the packed crystal lattice 3D network intermolecular forces. HOMO/LUMO energy level and the global reactivity descriptors quantum parameters are also calculated. The electrophilic and nucleophilic potions in the complex surface are theoretically evaluated by molecular electrostatic potential and Mulliken atomic charges analysis.

Structural information on the coordination compounds formed by manganese(II), cobalt(II), nickel(II), zinc(II), cadmium(II) and mercury(II) thiocyanates with 4-cyanopyridine N-oxide from their magnetic moments, electronic and infrared spectra

Science.gov (United States)

Ahuja, I. S.; Yadava, C. L.; Singh, Raghuvir

1982-05-01

Coordination compounds formed by the interaction of 4-cyanopyridine. N-oxide (4-CPO), a potentially bidentate ligand, with manganese(II), cobalt(II), nickel(II), zinc(II), cadmium(II) and rnercury(II) thiocyanates have been prepared and characterized from their elemental analyses, magnetic susceptibilities, electronic and infrared spectral studies down to 200 cm -1 in the solid state. The compounds isolated are: Mn(4-CPO) 2(NCS) 2, Co(4-CPO) 2(NCS) 2,Ni(4-CPO) 2(NCS) 2,Zn(4-CPO) 2(NCS) 2, Cd(4-CPO)(NCS) 2 and Hg(4-CPO) 2(SCN) 2. It is shown that 4-CPO acts as a terminal N-oxide oxygen bonded monodentate ligand in all the metal(II) thiocyanate complexes studied. Tentative stereochemistries of the complexes in the solid state are discussed. The ligand field parameters 10 Dq, B, β and λ calculated for the manganese(II), cobalt(II) and nickel(II) complexes are consistent with their proposed stereochemistries.

Column Chromatography Of Co(II), Zn(II) And Eu(III) Using Pistachio Shell And Different Mobile Phases

Energy Technology Data Exchange (ETDEWEB)

Abdel-Fattah, A A [Nuclear Chemistry Department, Radioisotopes Production Division, Hot Laboratories Centre, Atomic Energy Authority, Cairo (Egypt)

2009-07-01

Pistachio shell particles (0.5-1 mm) have been applied as the stationary phase for studying the column chromatography of Co(II), Zn(II) and Eu(III) at room temperature; 26{sup +}-{sup 1}oC. This solid sorbent has been characterized by thermogravimetric analysis, infra-red spectroscopy and X-ray diffraction. Its surface area and percent of swelling have been also determined. Different eluting agents have been used for eluting the sorbed elements. The elution curves have been done from which the distribution coefficients (K{sub d}), number of theoretical plates (N) and heights equivalent to theoretical plates (H) have been determined. Column performance studies have been conducted for a representative system under certain experimented conditions and Van Deemter equation has been applied. Thermodynamic studies have been applied and thermodynamic functions ( {delta}G{sup 0} ,{delta}H{sup 0} and{delta} S{sup 0}) have been calculated for this representative system by determining K{sub d} at three different room temperatures (18, 26 and 37{sup +}-{sup 1o}C)

Macrocyclic receptor showing extremely high Sr(II)/Ca(II) and Pb(II)/Ca(II) selectivities with potential application in chelation treatment of metal intoxication.

Science.gov (United States)

Ferreirós-Martínez, Raquel; Esteban-Gómez, David; Tóth, Éva; de Blas, Andrés; Platas-Iglesias, Carlos; Rodríguez-Blas, Teresa

2011-04-18

Herein we report a detailed investigation of the complexation properties of the macrocyclic decadentate receptor N,N'-Bis[(6-carboxy-2-pyridil)methyl]-4,13-diaza-18-crown-6 (H(2)bp18c6) toward different divalent metal ions [Zn(II), Cd(II), Pb(II), Sr(II), and Ca(II)] in aqueous solution. We have found that this ligand is especially suited for the complexation of large metal ions such as Sr(II) and Pb(II), which results in very high Pb(II)/Ca(II) and Pb(II)/Zn(II) selectivities (in fact, higher than those found for ligands widely used for the treatment of lead poisoning such as ethylenediaminetetraacetic acid (edta)), as well as in the highest Sr(II)/Ca(II) selectivity reported so far. These results have been rationalized on the basis of the structure of the complexes. X-ray crystal diffraction, (1)H and (13)C NMR spectroscopy, as well as theoretical calculations at the density functional theory (B3LYP) level have been performed. Our results indicate that for large metal ions such as Pb(II) and Sr(II) the most stable conformation is Δ(δλδ)(δλδ), while for Ca(II) our calculations predict the Δ(λδλ)(λδλ) form being the most stable one. The selectivity that bp18c6(2-) shows for Sr(II) over Ca(II) can be attributed to a better fit between the large Sr(II) ions and the relatively large crown fragment of the ligand. The X-ray crystal structure of the Pb(II) complex shows that the Δ(δλδ)(δλδ) conformation observed in solution is also maintained in the solid state. The Pb(II) ion is endocyclically coordinated, being directly bound to the 10 donor atoms of the ligand. The bond distances to the donor atoms of the pendant arms (2.55-2.60 Å) are substantially shorter than those between the metal ion and the donor atoms of the crown moiety (2.92-3.04 Å). This is a typical situation observed for the so-called hemidirected compounds, in which the Pb(II) lone pair is stereochemically active. The X-ray structures of the Zn(II) and Cd(II) complexes show that

Transport of Zn (II by TDDA-Polypropylene Supported Liquid Membranes and Recovery from Waste Discharge Liquor of Galvanizing Plant of Zn (II

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Hanif Ur Rehman

2017-01-01

Full Text Available The facilitated passage of Zn (II across flat sheet supported liquid membrane saturated with TDDA (tri-n-dodecylamine in xylene membrane phase has been investigated. The effect of acid and metal ion concentration in the feed solution, the carrier concentration in membrane phase, stripping agent concentration in stripping phase, and coions on the extraction of Zn (II was investigated. The stoichiometry of the extracted species, that is, complex, was investigated on slope analysis method and it was found that the complex (LH2·Zn(Cl2 is responsible for transport of Zn (II. A mathematical model was developed for transport of Zn (II, and the predicted results strongly agree with experimental ones. The mechanism of transport was determined by coupled coion transport mechanism with H+ and Cl− coupled ions. The optimized SLM was effectively used for elimination of Zn (II from waste discharge liquor of galvanizing plant of Zn (II.

Evaluation of dentoskeletal effects of Farmand functional appliance (Fa II on class II malocclusion

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Yassaei S.

2007-07-01

Full Text Available Background and Aim: Functional appliances refer to a variety of removable or fixed appliances designed to alter the mandibular position both sagitally and vertically, resulting in orthodontic and orthopedic changes. Despite the long history of functional appliances, there is still much controversy related to their effectiveness and mode of action. The aim of this study was to evaluate dental and skeletal effects of Fa II in patients with class II malocclusion due to mandibular deficiency.Materials and Methods: In this before-after clinical trial, 35 patients with class II div I malocclusion were selected. These samples were under treatment with Fa II appliance for 11 months. The range of age of females was 10-13 years and males 11-14 years. Combination analysis was used to determine skeletal and dental effects. Paired t-test was used to compare the differences of mean value pre and post treatment. P<0.05 was considered as the level of significance. Results: There was significant difference between pre and post treatment in respect to posterior and anterior facial height, eruption of upper and lower posterior teeth, eruption of upper anterior teeth, mandibular body length, ANB angle, IMPA and 1 to SN. No significant difference was observed between pre and post treatment regarding facial growth.Conclusion: Treatment with Fa II functional appliance leads to significant alterations in dental and skeletal elements of craniofacial complex and improvement of dental and jaws relationship.

Solving multiobjective optimal reactive power dispatch using modified NSGA-II

Energy Technology Data Exchange (ETDEWEB)

Jeyadevi, S.; Baskar, S.; Babulal, C.K.; Willjuice Iruthayarajan, M. [Department of Electrical and Electronics Engineering, Thiagarajar College of Engineering, Madurai, Tamilnadu 625 015 (India)

2011-02-15

This paper addresses an application of modified NSGA-II (MNSGA-II) by incorporating controlled elitism and dynamic crowding distance (DCD) strategies in NSGA-II to multiobjective optimal reactive power dispatch (ORPD) problem by minimizing real power loss and maximizing the system voltage stability. To validate the Pareto-front obtained using MNSGA-II, reference Pareto-front is generated using multiple runs of single objective optimization with weighted sum of objectives. For simulation purposes, IEEE 30 and IEEE 118 bus test systems are considered. The performance of MNSGA-II, NSGA-II and multiobjective particle swarm optimization (MOPSO) approaches are compared with respect to multiobjective performance measures. TOPSIS technique is applied on obtained non-dominated solutions to determine best compromise solution (BCS). Karush-Kuhn-Tucker (KKT) conditions are also applied on the obtained non-dominated solutions to substantiate a claim on optimality. Simulation results are quite promising and the MNSGA-II performs better than NSGA-II in maintaining diversity and authenticates its potential to solve multiobjective ORPD effectively. (author)

Selective solid-phase extraction of Ni(II) by an ion-imprinted polymer from water samples

International Nuclear Information System (INIS)

Saraji, Mohammad; Yousefi, Hamideh

2009-01-01

A new ion-imprinted polymer (IIP) material was synthesized by copolymerization of 4-vinylpyridine as monomer, ethyleneglycoldimethacrylate as crosslinking agent and 2,2'-azobis-sobutyronitrile as initiator in the presence of Ni-dithizone complex. The IIP was used as sorbent in a solid-phase extraction column. The effects of sampling volume, elution conditions, sample pH and sample flow rate on the extraction of Ni ions form water samples were studied. The maximum adsorption capacity and the relative selectivity coefficients of imprinted polymer for Ni(II)/Co(II), Ni(II)/Cu(II) and Ni(II)/Cd(II) were calculated. Compared with non-imprinted polymer particles, the IIP had higher selectivity for Ni(II). The relative selectivity factor (α r ) values of Ni(II)/Co(II), Ni(II)/Cu(II) and Ni(II)/Cd(II) were 21.6, 54.3, and 22.7, respectively, which are greater than 1. The relative standard deviation of the five replicate determinations of Ni(II) was 3.4%. The detection limit for 150 mL of sample was 1.6 μg L -1 using flame atomic absorption spectrometry. The developed method was successfully applied to the determination of trace nickel in water samples with satisfactory results.

The spectrum of singly ionized oxygen, O II

International Nuclear Information System (INIS)

Wenaker, I.

1990-01-01

The spectrum of singly ionized oxygen, O II, emitted by a spark-generated, electrodeless discharge light source, has been investigated in the wavelength range 2100-11700 A. About 740 lines, 359 of which have not been reported earlier, were measured. As a result the energies of about 50 new levels have been determined, and the O II term system now presented includes 254 levels. The quartet system is firmly connected to the doublet system by 56 identified intersystem lines. The ionization limits have been determined by applying the polarization formula to the 4f, 5f, 5g and 6g levels. The experimentally determined value for the lowest limit, 2s 2 2p 2 3 P 0 , is 283270.9±0.5 cm -1 above the 2s 2 2p 3 4 S 3/2 ground state. (orig.)

Determination of formal redox potentials in aqueous solution of copper(II) complexes with ligands having nitrogen and oxygen donor atoms and comparison with their EPR and UV-Vis spectral features.

Science.gov (United States)

Tabbì, Giovanni; Giuffrida, Alessandro; Bonomo, Raffaele P

2013-11-01

Formal redox potentials in aqueous solution were determined for copper(II) complexes with ligands having oxygen and nitrogen as donor atoms. All the chosen copper(II) complexes have well-known stereochemistries (pseudo-octahedral, square planar, square-based pyramidal, trigonal bipyramidal or tetrahedral) as witnessed by their reported spectroscopic, EPR and UV-visible (UV-Vis) features, so that a rough correlation between the measured redox potential and the typical geometrical arrangement of the copper(II) complex could be established. Negative values have been obtained for copper(II) complexes in tetragonally elongated pseudo-octahedral geometries, when measured against Ag/AgCl reference electrode. Copper(II) complexes in tetrahedral environments (or flattened tetrahedral geometries) show positive redox potential values. There is a region, always in the field of negative redox potentials which groups the copper(II) complexes exhibiting square-based pyramidal arrangements. Therefore, it is suggested that a measurement of the formal redox potential could be of great help, when some ambiguities might appear in the interpretation of spectroscopic (EPR and UV-Vis) data. Unfortunately, when the comparison is made between copper(II) complexes in square-based pyramidal geometries and those in square planar environments (or a pseudo-octahedral) a little perturbed by an equatorial tetrahedral distortion, their redox potentials could fall in the same intermediate region. In this case spectroscopic data have to be handled with great care in order to have an answer about a copper complex geometrical characteristics. © 2013.

Equilibrium modeling of mono and binary sorption of Cu(II and Zn(II onto chitosan gel beads

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Nastaj Józef

2016-12-01

Full Text Available The objective of the work are in-depth experimental studies of Cu(II and Zn(II ion removal on chitosan gel beads from both one- and two-component water solutions at the temperature of 303 K. The optimal process conditions such as: pH value, dose of sorbent and contact time were determined. Based on the optimal process conditions, equilibrium and kinetic studies were carried out. The maximum sorption capacities equaled: 191.25 mg/g and 142.88 mg/g for Cu(II and Zn(II ions respectively, when the sorbent dose was 10 g/L and the pH of a solution was 5.0 for both heavy metal ions. One-component sorption equilibrium data were successfully presented for six of the most useful three-parameter equilibrium models: Langmuir-Freundlich, Redlich-Peterson, Sips, Koble-Corrigan, Hill and Toth. Extended forms of Langmuir-Freundlich, Koble-Corrigan and Sips models were also well fitted to the two-component equilibrium data obtained for different ratios of concentrations of Cu(II and Zn(II ions (1:1, 1:2, 2:1. Experimental sorption data were described by two kinetic models of the pseudo-first and pseudo-second order. Furthermore, an attempt to explain the mechanisms of the divalent metal ion sorption process on chitosan gel beads was undertaken.

Comparison of adsorption of Cd(II and Pb(II ions on pure and chemically modified fly ashes

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Sočo Eleonora

2016-06-01

Full Text Available The study investigates chemical modifications of coal fly ash (FA treated with HCl or NH4HCO3 or NaOH or Na2edta, based on the research conducted to examine the behaviour of Cd(II and Pb(II ions adsorbed from water solution on treated fly ash. In laboratory tests, the equilibrium and kinetics were examined applying various temperatures (293 - 333 K and pH (2 - 11 values. The maximum Cd(II and Pb(II ions adsorption capacity obtained at 293 K, pH 9 and mixing time 2 h from the Langmuir model can be grouped in the following order: FA-NaOH > FA-NH4HCO3 > FA > FA-Na2edta > FA-HCl. The morphology of fly ash grains was examined via small-angle X-ray scattering (SAXS and images of scanning electron microscope (SEM. The adsorption kinetics data were well fitted by a pseudo-second-order rate model but showed a very poor fit for the pseudofirst order model. The intra-particle model also revealed that there are two separate stages in the sorption process, i.e. the external diffusion and the inter-particle diffusion. Thermodynamics parameters such as free energy, enthalpy and entropy were also determined. A laboratory test demonstrated that the modified coal fly ash worked well for the Cd(II and Pb(II ion uptake from polluted waters.

A fluorescent DNA based probe for Hg(II) based on thymine-Hg(II)-thymine interaction and enrichment via magnetized graphene oxide.

Science.gov (United States)

Li, Meng-Ke; Hu, Liu-Yin; Niu, Cheng-Gang; Huang, Da-Wei; Zeng, Guang-Ming

2018-03-03

The authors describe a fluorometric assay for the determination of Hg(II). A naphthalimide derivative is used as a label for a thymine (T) rich ssDNA, and graphene oxide magnetized with Fe 3 O 4 nanoparticles acts as a quencher and preconcentrators. In the absence of Hg(II), the labeled ssDNA does not separate from the magnetized graphene oxide. As a result, fluorescence is fully quenched. In the presence of Hg(II), a T-Hg(II)-T link is formed dues to the highly affinity between T and Hg(II). Hence, fluorescence is restored. The assay has a linear response in the 1.0 to 10.0 nM Hg(II) concentration range, and a 0.65 nM detection limit. The method is selective and sensitive. It was applied to the analysis of spiked environmental water samples, and data agreed well with those obtained by atomic fluorescence spectrometry. Graphical abstract Strategy of a fluorescent probe for detecting Hg(II). The method has a 0.65 nM detection limit and is selective. MGO: magnetized graphene oxide, AHN: a fluorescent derivative of naphthalimide.

Studies of the labelling of human serum albumin with 99mTc using Sn(II) tartrate and Sn(II)Cl2 as reducing agents

International Nuclear Information System (INIS)

El-Kolaly, M.T.; El-Asrag, H.A.; El-Wetery, A.S.; El-Mohty, A.A.

1990-01-01

A comparative study has been carried out on the effect of Sn(II) tartrate and Sn(II)Cl 2 on the labelling efficiency and tissue distribution of 99m Tc-human serum albumin. The effect of reductant content, reaction time (incubation time), albumin content, pH, and ascorbic acid on the efficiency of labelling and the tissue distribution of the labelled albumin has been investigated. The percentage of labelling was determined by paper and thin layer radiochromatography. Ascorbic acid shows no effect on either labelling efficiency or tissue distribution of 99m Tc-HSA prepared by Sn(II) tartrate or Sn(II)Cl 2 . (author)

Highly selective potentiometric and colorimetric determinations of cobalt (II) ion using thiazole based ligands.

Science.gov (United States)

Singhal, Divya; Singh, Ashok Kumar; Upadhyay, Anjali

2014-12-01

New PVC-membrane electrodes were prepared by using 2-((thiazol-2-ylimino)methyl)phenol (L1) and 2-((thiazol-2-ylamino)methyl)phenol (L2) and explored as Co(II) selective electrodes. The effect of various plasticizers and anion excluder was studied in detail and improved performance was observed. It was found that the electrode based on L1 shows better response characteristics in comparison to L2. Optimum performance was observed for the membrane electrode having a composition of L1:NaTPB:DBP:PVC≡2:8:78:62 (w/w, mg). The performance of PME based on L1 was compared with that of CGE. The electrodes exhibit Nernstian slope for Co(II) ions with a limit of detection of 6.91×10(-7) mol L(-1) for PME and 7.94×10(-8) mol L(-1) for CGE. The response time for PME and CGE was found to be 15s and 12 s respectively. The potentiometric responses are independent in the pH range 3.0-9.0 for CGE. The CGE could be used for a period of 90 days. The CGE was used as an indicator electrode in potentiometric titration of EDTA with Co(2+) ion. Further the selectivity of the L1 and L2 was also confirmed by the UV-vis and colorimetric studies and found that L1 is more selective for Co(II) ion. Copyright © 2014 Elsevier B.V. All rights reserved.

Highly selective determination of methylmercury with methylmercury-imprinted polymers

Energy Technology Data Exchange (ETDEWEB)

Liu Yongwen [Department of Chemistry, Shanxi Datong University, Datong 037009 (China)]. E-mail: dtlyw@263.net; Zai Yunhui [School of Chemistry and Chemical Engineering of Lanzhou University, Lanzhou 730000 (China); Chang Xijun [School of Chemistry and Chemical Engineering of Lanzhou University, Lanzhou 730000 (China); Guo Yong [Department of Chemistry, Shanxi Datong University, Datong 037009 (China); Meng Shuangming [Department of Chemistry, Shanxi Datong University, Datong 037009 (China); Feng Feng [Department of Chemistry, Shanxi Datong University, Datong 037009 (China)

2006-08-11

Methylmercury-imprinted and non-imprinted polymers were prepared by formation monomer complex of methylmercury with (4-ethenylphenyl)-4-formate-6-phenyl-2,2'-bipyridine and thermally polymerizing with divinylbenzene (crosslinker) in the presence of 2,2'-azobisisobutyronitrile as initiator and subsequently leached with the acidic thiourea solution (1.0 mol L{sup -1} of thiourea and 4.0 mol L{sup -1} of HCl). In the same way, non-imprinted copolymers were prepared without methylmercury chloride added. The separation and preconcentration characteristics of the polymers for methylmercury were investigated by batch and column procedures. The results demonstrated that the methylmercury-imprinted polymers had higher adsorption capacity (170 {mu}mol g{sup -1} of dry microbeads) and good selectivity for methylmercury compared to non-imprinted polymers. The distribution ratio (D) values of the methylmercury-imprinted polymers increased for methylmercury with respect to both D values of Hg(II), Cu(II), Zn(II), Cd(II) and non-imprinted polymers. The relatively selective factor ({alpha} {sub r}) values of CH{sub 3}Hg{sup +}/Hg(II), CH{sub 3}Hg{sup +}/Cu(II), CH{sub 3}Hg{sup +}/Zn(II), and CH{sub 3}Hg{sup +}/Cd(II) are 24.0, 46.7, 50.7, and 40.2, which are greater than 1. The methylmercury-imprinted polymers can be used at least twenty times with recoveries no less than 95%. Based on the packed columns with methylmercury-imprinted polymers, a highly selective solid-phase extraction (SPE) and preconcentration method for methylmercury was developed. The metal ion imprinted polymer solid-phase extraction (MIIP-SPE) preconcentration procedure showed a linear calibration curve within concentration range from 0.093 to 22 {mu}g L{sup -1}. The detection limit and quantification limit were 0.041 and 0.093 {mu}g L{sup -1} (3{sigma}) for cold vapor atomic absorption spectrometry (CVAAS). The relative standard deviation of the 10 replicate determinations was 3.5% for the

An efficient, cost effective, sensing behaviour liquid-liquid extraction and spectrophotometric determination of copper(II) incorporated with 4-(4‧-chlorobenzylideneimino)-3-methyl-5-mercapto-1, 2, 4-triazole: Analysis of food samples, leafy vegetables, fertilizers and environmental samples

Science.gov (United States)

Barache, Umesh B.; Shaikh, Abdul B.; Lokhande, Tukaram N.; Kamble, Ganesh S.; Anuse, Mansing A.; Gaikwad, Shashikant H.

2018-01-01

The aim of the present work is to develop an efficient, simple and selective moreover cost-effective method for the extractive spectrophotometric determination of copper(II) by using the Schiff base 4-(4‧-chlorobenzylideneimino)-3-methyl-5-mercapto-1, 2, 4-triazole [CBIMMT]. This chromogenic reagent forms a yellow coloured complex with copper(II) in acetate buffer at pH 4.2. The copper(II) complex with ligand is instantly extracted into chloroform and shows a maximum absorbance at 414 nm which remains stable for > 48 h. The composition of extracted complex is found to be 1:2 [copper(II): reagent] which was ascertained using Job's method of continuous variation, mole ratio method and slope ratio method. Under optimal conditions, the copper(II) complex in chloroform adheres to Beer's law up to 17.5 μg mL- 1 of copper(II). The optimum concentration range obtained from Ringbom's plot is from 5 μg mL- 1 to 17.5 μg mL- 1. The molar absorptivity, Sandell's sensitivity and enrichment factor of the extracted copper(II) chelate are 0.33813 × 104 L mol- 1 cm- 1, 0.01996 μg cm- 2 and 2.49 respectively. In the extraction of copper(II), several affecting factors including the solution pH, ligand concentration, equilibrium time, effect of foreign ions are optimized. The interfering effects of various cations and anions were also studied and use of masking agents enhances the selectivity of the method. The chromogenic sulphur containing reagent, 4-(4‧-chlorobenzylideneimino)-3-methyl-5-mercapto-1, 2, 4-triazole has been synthesized in a single step with high purity and yield. The synthesized reagent has been successfully applied first time for determination of copper(II). The reagent forms stable chelate with copper(II) in buffer medium instantly and quantitatively extracted in chloroform within a minute. The method is successfully applied for the determination of copper(II) in various synthetic mixtures, complexes, fertilizers, environmental samples such as food samples

Validating the Beck Depression Inventory-II in Indonesia's general population and coronary heart disease patients

NARCIS (Netherlands)

Ginting, H.; Näring, G.W.B.; Veld, W.M. van der; Srisayekti, W.; Becker, E.S.

2013-01-01

This study assesses the validity and determines the cut-off point for the Beck Depression Inventory-II (the BDI-II) among Indonesians. The Indonesian version of the BDI-II (the Indo BDI-II) was administered to 720 healthy individuals from the general population, 215 Coronary Heart Disease (CHD)

High-resolution structure of the antibiotic resistance protein NimA from Deinococcus radiodurans

International Nuclear Information System (INIS)

Leiros, Hanna-Kirsti S.; Tedesco, Consiglia; McSweeney, Seán M.

2008-01-01

In this paper, the 1.2 Å atomic resolution crystal structure of the 5-nitroimidazole antibiotic resistance protein NimA from Deinococcus radiodurans (DrNimA) is presented. Many anaerobic human pathogenic bacteria are treated using 5-nitroimidazole-based (5-Ni) antibiotics, a class of inactive prodrugs that contain a nitro group. The nitro group must be activated in an anaerobic one-electron reduction and is therefore dependent on the redox system in the target cells. Antibiotic resistance towards 5-Ni drugs is found to be related to the nim genes (nimA, nimB, nimC, nimD, nimE and nimF), which are proposed to encode a reductase that is responsible for converting the nitro group of the antibiotic into a nonbactericidal amine. A mechanism for the Nim enzyme has been proposed in which two-electron reduction of the nitro group leads to the generation of nontoxic derivatives and confers resistance against these antibiotics. The cofactor was found to be important in the mechanism and was found to be covalently linked to the reactive His71. In this paper, the 1.2 Å atomic resolution crystal structure of the 5-nitroimidazole antibiotic resistance protein NimA from Deinococcus radiodurans (DrNimA) is presented. A planar cofactor is clearly visible and well defined in the electron-density map adjacent to His71, the identification of the cofactor and its properties are discussed

The extraction constant of mercury(II) o-o'-dimethyldithizonate into toluene

NARCIS (Netherlands)

Jütte, B.A.H.G.; Agterdenbos, J.; Welle, R.A. van der

An attempt was made to determine spectrophotometrically the extraction constant of mercury(II) o-o'-dimethyldithizonate into toluene by means of a known excess of iodide as a masking agent. The results found, however, could not be explained by a simple reaction between mercury(II)

Electrochemiluminescent determination of methamphetamine based on tris(2,2'-bipyridine)ruthenium(II) ion-association in organically modified silicate films

International Nuclear Information System (INIS)

Yi Changqing; Tao Yin; Wang Bo; Chen Xi

2005-01-01

Tetramethoxysilane (TMOS) and dimethyldimethoxysilane (DiMe-DiMOS) were used as co-precursor to immobilize poly(p-styrenesulfonate) (PSS), then tris(2,2'-bipyridine)ruthenium(II) (Ru(bpy) 3 2+ ) was successfully immobilized on a glass carbon electrode via ion-association. The immobilized Ru(bpy) 3 2+ shows good electrochemical and photochemical activities. Electrochemical and electrochemiluminescence (ECL) characterizations of the organically modified silicates (ORMOSILs) modified film electrodes were made by means of cyclic voltammetry and chronocoulometry. The ORMOSIL films were investigated by atomic force microscopy, scanning electrochemical microscope, tunnelling electrochemical microscope, X-ray photoelectron spectroscopy (XPS), UV-vis spectroscopy and fluorescence spectroscopy. XPS in-depth profiles revealed a homogeneous distribution of Ru(bpy) 3 2+ inside the silica thin layers. The modified electrode was used for the ECL determination of methamphetamine (METH) and showed high sensitivity. Detection limit was 2.0 x 10 -7 mol l -1 for METH (S/N = 3) with a linear range from 5.0 x 10 -7 to 1.0 x 10 -3 mol l -1 (R = 0.986). The relative standard deviation (n = 6) was 1.1% for the determination of 1.0 x 10 -5 mol l -1 METH. Furthermore, the Ru(bpy) 3 2+ immobilized modified electrode was applied in the ECL determination of methamphetamine (METH) in scout cases

Fragment Screening of Human Kynurenine Aminotransferase-II.

Science.gov (United States)

Jayawickrama, Gayan S; Nematollahi, Alireza; Sun, Guanchen; Church, W Bret

2018-03-01

Kynurenine aminotransferase-II (KAT-II) is a pyridoxal 5'-phosphate (PLP)-dependent enzyme that acts in the tryptophan metabolic pathway by catalyzing the transamination of kynurenine into kynurenic acid (KYNA). It is one of four isoforms in the KAT family, of which it is the primary homologue responsible for KYNA production in the mammalian brain. KAT-II is targeted for inhibition as KYNA is implicated in diseases such as schizophrenia, where it is found in elevated concentrations. Previously, many different approaches have been taken to develop KAT-II inhibitors, and herein fragment-based drug design (FBDD) approaches have been exploited to provide further lead compounds that can be designed into novel inhibitors. Surface plasmon resonance (SPR) was used to screen a fragment library containing 1000 compounds, of which 41 hits were identified. These hits were further evaluated with SPR, and 18 were selected for inhibition studies. From these hits, two fragments, F6037-0164 and F0037-7280, were pursued and determined to have an IC 50 of 524.5 (± 25.6) μM and 115.2 (± 4.5) μM, respectively. This strategy shows the viability of using FBDD in gleaning knowledge about KAT-II inhibition and generating leads for the production of KAT-II inhibitors.

Complexes in the Ni2+-imidazole-RN(CH2COO-)2 systems. The crystal structures of tris(imidazole)iminodiacetatonickel(II) monohydrate, hexa(imidazole)nickel(II) bis(N-methyliminodiacetato)nickelate(II) hexahydrate, and tetra(aqua)bis(imidazole)nickel(II) bis(N-benzyliminodiacetato)nickelate(II)

International Nuclear Information System (INIS)

Polyakova, I.N.; Sergienko, V.S.; Poznyak, A.L.

2000-01-01

Crystals of different compositions, namely, [Ni(Ida)(Im) 3 ] · H 2 O (I), [Ni(Im) 6 ][Ni(Mida) 2 ] · 6H 2 O (II), and [Ni(Im) 2 (H 2 O) 4 ][Ni(Bida) 2 ] (III), have been precipitated from aqueous solutions of the Ni 2+ -Lig 2- Im systems, where Lig 2- is Ida, Mida, and Bida, respectively. The crystal structures of I-III are determined by X-ray diffraction analysis (R = 0.0307, 0.0348, and 0.0302 for 3061, 4706, and 2882 reflections, respectively). Crystals I are built of monomeric mixed-ligand complexes and molecules of crystallization water, which are interlinked by hydrogen bonds into a three-dimensional framework. In II and III, the ligands Lig 2- and Im form charged complexes separately. In II, the cationic and anionic layers of the complexes alternate along the c-axis. Numerous hydrogen bonds involving molecules of crystallization water link the layers into a three-dimensional framework. In III, the cationic and anionic complexes, which serve as proton donors and acceptors, respectively, are bound into layers parallel to the xy plane

Selective solid-phase extraction of Hg(II) using silica gel surface - imprinting technique

International Nuclear Information System (INIS)

Zheng, H.; Geng, T.; Hu, L.

2008-01-01

A new ion-imprinted amino-functionalized silica gel sorbent was synthesized by surface-imprinting technique for preconcentration and separation of Hg(II) prior to its determination by inductively coupled plasma optical emission spectrometry (ICP-OES). Compared to the traditional solid sorbents and non-imprinted polymer particles, the ion-imprinted polymers (IIPs) have higher adsorption capacity and selectivity for Hg(II). The maximum static adsorption capacity of the imprinted and non-imprinted sorbent for Hg(II) was 29.89 mg g -1 and 11.21 mg g -1 , respectively. The highest selectivity coefficient for Hg(II) in the presence of Zn(II) exceeded 230. The detection limit (3σ) of the method was 0.25 μg L -1 . The relative standard deviation of the method was 2.5% for eight replicate determinations of 10 μg of Hg 2+ in 200 mL-in-volume water sample. The procedure was validated by performing the analysis of the certified river sediment sample (GBW 08603, China) using the standard addition method. The developed method was also successfully applied to the determination of trace mercury in Chinese traditional medicine and water samples with satisfactory results. (authors)

Removal of pharmaceutical compounds from water by adsorption on activated carbon and degradation with ozone; Eliminacion de compuestos farmaceuticos de las aguas por adsorcion en carbon activado y degradacion con ozono

Energy Technology Data Exchange (ETDEWEB)

Sanchez Polo, M.; Prado Joya, G.; Rivera Utrilla, J.; Ferro Garcia, M. A.; Bautista Toledo, M. I.; Lopez Penalver, J. J.; Gomez Merlo de la fuente, C.

2007-07-01

The removal of pharmaceutical compounds from water, using nitroimidazoles as model compounds, by means of both adsorption on activated carbon and ozonization has been studied. The results obtained have shown that activated carbon presents a great efficiency to remove these contaminants from waters because: the adsorption kinetics is very fast, and it is not affected by diffusion problems; the maximum adsorption capacity is very high (400-96 mg/g); and the nitroimidazole adsorption capacity is enhanced in natural waters. Regarding to the ozonization process, a low reactivity of these compounds with ozone has been observed (k{sub 0}3{approx_equal}100 M{sup -}1 s{sup -}1) although, nevertheless, they present a high affinity to the hydroxyl radicals (k{sub O}H{approx_equal}10{sup 1}0 M{sup -}1s{sup -}1). (Author) 13 refs.

Relative frequency of Human T-cell Lymphotropic Virus I/II in HIV/AIDS patients

Directory of Open Access Journals (Sweden)

Mohsen Meidani

2014-01-01

Conclusion: In our survey, relative frequency of HTLV-I/II was 1.8% in HIV+ patients. This study reveals that relative frequency of HTLV-I/II in HIV positive patients is considerable but determining the need for screening of HTLV-I/II requires further investigation.

Synthesis, characterization and thermal studies of nickel (II), copper (II), zinc (II) and cadmium (II) complexes with some mixed ligands

International Nuclear Information System (INIS)

Mitra, Samiran; Kundu, Parimal; Singh, Rajkumar Bhubon

1998-01-01

Dichloro-(DCA) and trichloroacetate(TCA) -cyclic ligand morpholine (Morph)/thiomorpholine (Tmorph)/methylmorpholine (Mmorph)/dimethyl-piperazine (DMP) complexes of nickel (II), copper (II), zinc (II) and cadmium (II) with the compositions [Ni(tmorph) 2 (DCA) 2 ], [Ni(tmorph) 2 (TCA) 2 ].2H 2 O, [Cu(DMP) 2 (TCA) 2 ],[ML 2 X 2 ].nH 2 O where M=Zn II or Cd II , L=Morph, DMP or tmorph and X=DCA or TCA and n=O except in case of [Cd (Morph) 2 (TCA) 2 ] where n=1 have been synthesised. Some intermediate complexes have been isolated by temperature arrest technique (pyrolysis) and characterised. Configurational and conformational changes have been studied by elemental analyses, IR and electronic spectra, magnetic moment data (in the case of Ni(II) and Cu(II) complexes) and thermal analysis. E a * , ΔH, and ΔS for the decomposition reaction of these complexes are evaluated and the stability of the complexes with respect to activation energy has also been compared. The linear correlation has been found between E a * and ΔS for the decomposition of the complexes. (author)

An independent determination of the local Hubble constant

Science.gov (United States)

Fernández Arenas, David; Terlevich, Elena; Terlevich, Roberto; Melnick, Jorge; Chávez, Ricardo; Bresolin, Fabio; Telles, Eduardo; Plionis, Manolis; Basilakos, Spyros

2018-02-01

The relationship between the integrated H β line luminosity and the velocity dispersion of the ionized gas of H II galaxies and giant H II regions represents an exciting standard candle that presently can be used up to redshifts z ˜ 4. Locally it is used to obtain precise measurements of the Hubble constant by combining the slope of the relation obtained from nearby (z ≤ 0.2) H II galaxies with the zero-point determined from giant H II regions belonging to an `anchor sample' of galaxies for which accurate redshift-independent distance moduli are available. We present new data for 36 giant H II regions in 13 galaxies of the anchor sample that includes the megamaser galaxy NGC 4258. Our data are the result of the first 4 yr of observation of our primary sample of 130 giant H II regions in 73 galaxies with Cepheid determined distances. Our best estimate of the Hubble parameter is 71.0 ± 2.8(random) ± 2.1(systematic) km s- 1Mpc- 1. This result is the product of an independent approach and, although at present less precise than the latest SNIa results, it is amenable to substantial improvement.

Competition from Cu(II), Zn(II) and Cd(II) in Pb(II) binding to Suwannee River Fulvic Acid

NARCIS (Netherlands)

Chakraborty, P.; Chakrabarti, C.L.

2008-01-01

This is a study of trace metal competition in the complexation of Pb(II) by well-characterized humic substances, namely Suwannee River Fulvic Acid (SRFA) in model solutions. It was found that Cu(II) seems to compete with Pb(II) for strong binding sites of SRFA when present at the same concentration