共查询到20条相似文献,搜索用时 62 毫秒
1.
Ashraf A. Mohamed 《Monatshefte für Chemie / Chemical Monthly》2001,56(2):919-928
A new selective, sensitive, and simple kinetic method is developed for the determination of trace amounts of iodide. The method is based on the catalytic effect of iodide on the reaction of triflupromazine (TFP) with H2O2. The reaction is followed spectrophotometrically by tracing the oxidation product at 498 nm within 1 min after addition of H2O2. The optimum reaction conditions are TFP (0.4 × 10−3 M), H2SO4 (1.0M), H3PO4 (2.0M), and H2O2 (1.6M) at 30°C. Following this procedure, iodide can be determined with a linear calibration graph up to 4.5 ng ċ cm−3 and a detection limit of 0.04 ng ċ cm−3, based on the 3 Sb criterion. The method can also be applied to the determination of iodate and periodate ions. Determination of as little as 0.2, 1.0, 2.0, and 4.0 ng ċ cm−3 of I−, IO3 -, or IO4 - in aqueous solutions gave an average recovery of 98% with relative standard deviations below 1.6% (n = 5). The method was applied to the determination of iodide in Nile river water and ground waters as well as in various food samples after alkaline ashing treatment. The method is compared with other catalytic spectrophotometric procedures for iodide determination. 相似文献
2.
Ashraf A. Mohamed Saleh A. Ahmed Mohamed F. El-Shahat 《Monatshefte für Chemie / Chemical Monthly》2002,133(1):31-40
Summary. A highly selective, sensitive, and simple catalytic method for the determination of molybdenum in natural and waste waters
was developed. It is based on the catalytic effect of Mo(VI) on the oxidation of 2-aminophenol with H2O2. The reaction is monitored spectrophotometrically by tracing the oxidation product at 430 nm after 10 min of mixing the reagents.
Addition of 800 μg · cm−3
EDTA conferred high selectivity; however, interfering effects of Au(III), Cr(III), Cr(VI), and Fe(III) had to be eliminated by
a reduction and co-precipitation procedure with SnCl2 and Al(OH)3. Mo(VI) shows a linear calibration graph up to 11.0 ng · cm−3; the detection limit, based on the 3S
b-criterion, is 0.10 ng · cm−3. The unique selectivity and sensitivity of the new method allowed its direct application to the determination of Mo(VI) in
natural and waste waters.
Received April 11, 2001. Accepted (revised) June 18, 2001 相似文献
3.
Vesna Kuntić Dusěan Malesěev Zorica Radović Vladana Vukojević 《Monatshefte für Chemie / Chemical Monthly》2000,131(7):769-777
Summary. In the present work, rutin (3,3′ ,4′ ,5,7-pentahydrohyflavone-3-rhamnoglucoside) was determinated via a complexing reaction with a titanyloxalate anion. K2[TiO(C2O4)2] and rutin react in 50% ethanol forming a 1:2 complex in a pH range from 4.00 to 11.50, in which the TiO(C2O4)2
2− ion is linked to rutin through the 4-carbonyl and 5-hydroxyl group. The thermodynamic stability constant log β2
0 of the complex is determined to 10.80 at pH = 6.50. The change of the standard Gibbs free energy Δ G0 amounts to −61 kJċ mol−1, indicating that the process of complex formation is spontaneous. The optimal conditions for the spectrophotometric determination
of microconcentrations of rutin are at pH=6.40 and λ= 430 nm, where the complex shows an absorption maximum with a molar absorption coefficient a
430=(60±2)ċ103 dm3ċ mol−1ċ cm−1. The method is applied rutin determination from tablets.
Received January 4, 2000. Accepted (revised) February 17, 2000 相似文献
4.
Vesna Kunti? Dusěan Malesěev Zorica Radovi? Vladana Vukojevi? 《Monatshefte für Chemie / Chemical Monthly》2000,18(5):769-777
In the present work, rutin (3,3′ ,4′ ,5,7-pentahydrohyflavone-3-rhamnoglucoside) was determinated via a complexing reaction with a titanyloxalate anion. K2[TiO(C2O4)2] and rutin react in 50% ethanol forming a 1:2 complex in a pH range from 4.00 to 11.50, in which the TiO(C2O4)2 2− ion is linked to rutin through the 4-carbonyl and 5-hydroxyl group. The thermodynamic stability constant log β2 0 of the complex is determined to 10.80 at pH = 6.50. The change of the standard Gibbs free energy Δ G0 amounts to −61 kJċ mol−1, indicating that the process of complex formation is spontaneous. The optimal conditions for the spectrophotometric determination of microconcentrations of rutin are at pH=6.40 and λ= 430 nm, where the complex shows an absorption maximum with a molar absorption coefficient a 430=(60±2)ċ103 dm3ċ mol−1ċ cm−1. The method is applied rutin determination from tablets. 相似文献
5.
Samuel Melaku Ilse Gelaude Frank Vanhaecke Luc Moens Richard Dams 《Mikrochimica acta》2003,142(1-2):7-12
Microwave digestion reduction-aeration and pyrolysis combined with cold vapour atomic absorption and cold vapour atomic fluorescence
are compared for the determination of total mercury in several biological and environmental matrices. The biological samples
were digested in a mixture of HNO3/H2O2, the environmental samples in a mixture of HNO3/HClO4. After reduction with SnCl2, the mercury was collected by two-stage gold amalgamation. After microwave digestion reduction-aeration, detection limits
of 1.4 ng g−1 and 0.6 ng g−1 were obtained for cold vapour atomic absorption spectrometry (CVAAS) and cold vapour atomic fluorescence spectrometry (CVAFS),
respectively, for 250 mg of environmental samples. For biological samples (500 mg) the detection limits were 0.7 ng g−1 (CVAAS) and 0.4 ng g−1 (CVAFS). After pyrolysis, detection limits of 3.5 ng g−1 and 1.6 ng g−1 for CVAAS and CVAFS, respectively, were obtained for a 10 mg sample. Pyrolysis can only be applied when the organic content
of the sample is not too high. Accurate results were obtained for 8 certified reference materials of both environmental and
biological origin. In addition, a real sludge sample was analysed.
Author for correspondence. E-mail: richard.dams@rug.ac.be
Received September 18, 2002; accepted December 3, 2002
Published online May 5, 2003 相似文献
6.
A new spectrofluorimetric method was developed for the determination of trace amounts of coenzyme A (CoA). In the presence
of periodic acid (H5IO6), CoA can remarkably enhance the fluorescence intensity of the Tb3+–ciprofloxacin (CIP) complex at 545 nm in a buffer solution at pH 5.4; the enhanced fluorescence intensity of the Tb3+ ion is proportional to the concentration of CoA. The optimal conditions for the determination of CoA were also investigated.
The linear range and the detection limit for the determination of CoA were 6.08 × 10−6–1.64 × 10−5 and 2.1 × 10−8 mol L−1, respectively. This method is simple, practical and relatively free of interference from coexisting substances, and can be
successfully applied to assess CoA in injection and biological samples. Moreover, the enhancement mechanism of the fluorescence
intensity of the CoA–Tb3+–CIP system in the presence of H5IO6 is also discussed. 相似文献
7.
A new H2O2 biosensor was fabricated on the basis of nanocomposite films of hemoglobin (Hb), silver nanoparticles (AgNPs), and multiwalled
carbon nanotubes (MWNTs)–chitosan (Chit) dispersed solution immobilized on glassy carbon electrode (GCE). The immobilized
Hb displayed a pair of well-defined and reversible redox peaks with a formal potential (E
θ′) of −22.5 mV in 0.1 M pH 7.0 phosphate buffer solution. The apparent heterogeneous electron transfer rate constants (k
s) in the Chit–MWNTs film was evaluated as 2.58 s−1 according to Laviron’s equation. The surface concentration (Γ*) of the electroactive Hb in the Chit–MWNTs film was estimated to be (2.48 ± 0.25) × 10−9 mol cm−2. Meanwhile, the Chit–MWNTs/Hb/AgNPs/GCE demonstrated excellently electrocatalytical ability to H2O2. Its apparent Michaelis–Menten constant (K
Mapp) for H2O2 was 0.0032 mM, showing a good affinity. Under optimal conditions, the biosensors could be used for the determination of H2O2 ranging from 6.25 × 10−6 to 9.30 × 10−5 mol L−1 with a detection limit of 3.47 × 10−7 mol L−1 (S/N = 3). Furthermore, the biosensor possessed rapid response to H2O2 and good stability, selectivity, and reproducibility. 相似文献
8.
Günter Grampp Stephan Landgraf Tomasz Wesierski Beata Jankowska Ewa Kalisz Dana-Maria Sabou Boryana Mladenova 《Monatshefte für Chemie / Chemical Monthly》2002,133(10):1363-1372
Summary. The kinetics of the CrO(O2)2 formation by H2O2 and Cr2O7
2− in aqueous acidic media was measured at 293 ± 2 K in a pH range between 2.5 and 3.3. Using the stopped-flow method with rapid scan UV-VIS detection, the rate law of the formation
of CrO(O2)2 was determined. For the media HClO4, HNO3 and CH3COOH, the reaction order in the Cr2O7
2− concentration was found to be 0.5. For [H2O2] as well as for [H+], the reaction was first order in all acids used. In HCl and H2SO4 media the reaction was first order in Cr2O7
2−. At T = 293 ± 2 K the rate constant for the formation of Cr(O)(O2)2 was found to be (7.3 ± 1.9) · 102 M−3/2 s−1 in HClO4.
Corresponding author. E-mail: grampp@ptc.tu-graz.ac.at
Received January 30, 2002; accepted (revised) June 5, 2002 相似文献
9.
Peter Švančárek Peter Schwendt Jozef Tatiersky Ivana Smatanová Jaromír Marek 《Monatshefte für Chemie / Chemical Monthly》2000,131(2):145-154
Summary. Oxo peroxo glycolato complexes of vanadium(V) (M
2[V2O2(O2)2(C2H2O3)2]ċnH2O (n=0, 1; M=NBu4
+ (1), K+ (2), NH4
+ (3), Cs+ (4), NPr4
+ (5)) as well as (NBu4)2[V2O4(C2H2O3)2]ċ H2O (6) have been prepared and characterized by spectroscopic methods. X-Ray structure analysis of 1 revealed the presence of dinuclear [V2O2(O2)2(C2H2O3)2]2− anions with a (chemical structure) bridging core and six coordinated vanadium(V) atoms in a distorted pentagonal pyramidal
array.
Received July 12, 1999. Accepted (revised) October 28, 1999 相似文献
10.
Sensitive fluorescent probes for determination of hydrogen peroxide and glucose based on enzyme-immobilized magnetite/silica nanoparticles 总被引:2,自引:0,他引:2
Qing Chang Lihua Zhu Guodong Jiang Heqing Tang 《Analytical and bioanalytical chemistry》2009,395(7):2377-2385
Sensitive fluorescent probes for the determination of hydrogen peroxide and glucose were developed by immobilizing enzyme
horseradish peroxidase (HRP) on Fe3O4/SiO2 magnetic core–shell nanoparticles in the presence of glutaraldehyde. Besides its excellent catalytic activity, the immobilized
enzyme could be easily and completely recovered by a magnetic separation, and the recovered HRP-immobilized Fe3O4/SiO2 nanoparticles were able to be used repeatedly as catalysts without deactivation. The HRP-immobilized nanoparticles were able
to activate hydrogen peroxide (H2O2), which oxidized non-fluorescent 3-(4-hydroxyphenyl)propionic acid to a fluorescent product with an emission maximum at 409 nm.
Under optimized conditions, a linear calibration curve was obtained over the H2O2 concentrations ranging from 5.0 × 10−9 to 1.0 × 10−5 mol L−1, with a detection limit of 2.1 × 10−9 mol L−1. By simultaneously using glucose oxidase and HRP-immobilized Fe3O4/SiO2 nanoparticles, a sensitive and selective analytical method for the glucose detection was established. The fluorescence intensity
of the product responded well linearly to glucose concentration in the range from 5.0 × 10−8 to 5.0 × 10−5 mol L−1 with a detection limit of 1.8 × 10−8 mol L−1. The proposed method was successfully applied for the determination of glucose in human serum sample. 相似文献
11.
The chemiluminescence (CL) of peracetic acid (PAA) in alkaline medium is very weak but is strongly enhanced after the addition
of dihydralazine sulfate (DHZS). Based on this phenomenon, a simple, rapid and highly sensitive flow-injection CL method for
the determination of DHZS was developed. The CL emission was linearly related to the DHZS concentration in the range of 20–4000 ng mL−1 with a detection limit (3σ) of 1.2 ng mL−1. As a preliminary application, the proposed method was successfully applied to the determination of DHZS in pharmaceutical
preparations; the recovery of DHZS in human urine was between 96.5% and 102.2%. A detailed CL mechanism was proposed and singlet
molecular oxygen (1O2) was suggested to be produced in the CL reaction process. 相似文献
12.
Günter Grampp Stephan Landgraf Tomasz Wesierski Beata Jankowska Ewa Kalisz Dana-Maria Sabou Boryana Mladenova 《Monatshefte für Chemie / Chemical Monthly》2002,212(4):1363-1372
The kinetics of the CrO(O2)2 formation by H2O2 and Cr2O7
2− in aqueous acidic media was measured at 293 ± 2 K in a pH range between 2.5 and 3.3. Using the stopped-flow method with rapid scan UV-VIS detection, the rate law of the formation
of CrO(O2)2 was determined. For the media HClO4, HNO3 and CH3COOH, the reaction order in the Cr2O7
2− concentration was found to be 0.5. For [H2O2] as well as for [H+], the reaction was first order in all acids used. In HCl and H2SO4 media the reaction was first order in Cr2O7
2−. At T = 293 ± 2 K the rate constant for the formation of Cr(O)(O2)2 was found to be (7.3 ± 1.9) · 102 M−3/2 s−1 in HClO4. 相似文献
13.
Valéria Guzsvány Mihály Kádár Ferenc Gaál Klára Tóth Luka Bjelica 《Mikrochimica acta》2006,154(3-4):321-328
The polarographic behavior of thiamethoxam (a neonicotinoid insecticide) was studied by direct current and differential pulse
polarography. Depending on the pH thiamethoxam exhibited one or two well-defined cathodic polarographic waves. The characteristics
of the electrode reaction were investigated and it was found that at pH > 5.0 the target molecule captures four electrons
in the first step, and two in the second. Based on the reduction behavior of the target molecule on the mercury electrode,
a differential pulse polarographic method was elaborated for the rapid determination of thiamethoxam at pH 8.0. With the optimized
method, a linear response for thiamethoxam was found in the concentration range of 31.1 − 470 ng cm−3, the relative standard deviation did not exceed 1.6%, and the detection and quantitation limits were found to be 9.3 ng cm−3 and 31.1 ng cm−3, respectively. The method was applied to the determination of thiamethoxam in commercial formulations and real samples (potato
and maize). The procedure is simple, fast, sensitive, and compares well with comparative spectrophotometric and chromatographic
(HPLC/DAD) methods. 相似文献
14.
Fadila Balegroune Pierre Braunstein Jérôme Durand Thierry Faure Daniel Grandjean Michael Knorr Maurizio Lanfranchi Chiara Massera Xavier Morise Antonio Tiripicchio 《Monatshefte für Chemie / Chemical Monthly》2001,132(8):885-896
Summary. Iodo derivatives of diphosphine-bridged heterobimetallic Fe—Pd and Fe—Pt complexeshave been prepared in which an alkoxysilyl
ligand bridges the two metals in a μ2−η2-SiO manner. In the course of their synthesis by halide exchange from (dppx = dppm (Ph2 PCH2 PPh2) or dppa (Ph2PNHPPh2); M = Pd or Pt), loss of the alkoxysilyl ligand occurred resulting in the formation of complexes in which a bridging iodide has
replaced, as a 3e−-donor, the bridging alkoxysilyl ligand. These complexes of formula (M = Pd, Pt are better prepared by reaction of with [MI2(cod)]. The crystal structures of (2a), (2b), and · CH2Cl2 (3b · CH2Cl2) have been determined by X-ray diffraction.
Received January 24, 2001. Accepted February 12, 2001 相似文献
15.
Timothy J. Johnson Robert L. Sams Sarah D. Burton Thomas A. Blake 《Analytical and bioanalytical chemistry》2009,395(2):377-386
We report quantitative infrared spectra of vapor-phase hydrogen peroxide (H2O2) with all spectra pressure-broadened to atmospheric pressure. The data were generated by injecting a concentrated solution
(83%) of H2O2 into a gently heated disseminator and diluting it with pure N2 carrier gas. The water vapor lines were quantitatively subtracted from the resulting spectra to yield the spectrum of pure
H2O2. The results for the ν6 band strength (including hot bands) compare favorably with the results of Klee et al. (J Mol. Spectrosc. 195:154, 1999) as well as with the HITRAN values. The present results are 433 and 467 cm-2 atm−1 (±8 and ±3% as measured at 298 and 323 K, respectively, and reduced to 296 K) for the band strength, matching well the value
reported by Klee et al. (S = 467 cm−2 atm−1 at 296 K) for the integrated band. The ν1 + ν5 near-infrared band between 6,900 and 7,200 cm−1 has an integrated intensity S = 26.3 cm−2 atm−1, larger than previously reported values. Other infrared and near-infrared bands and their potential for atmospheric monitoring
are discussed. 相似文献
16.
Nashwa M. H. Rizk 《Mikrochimica acta》2002,138(1-2):53-58
The construction and electrochemical response characteristics of poly(vinyl) chloride matrix membrane sensors for menadione
(vitamin K3) are described. Membranes incorporating the ion association complexes of menadione anion with bathophenanthroline nickel(II)
and iron(II) as electroactive materials show linear response for menadione over the range 10−1–10−5 M with anionic slopes of 58.2–51.4 mV per concentration decade. Both sensors exhibit fast response time (20–30 s), low detection
limit (2 × 10−5 M), good stability (4–6 weeks) and selectivity coefficient (10−1–10−3). Direct potentiometric determination of menadione under static and hydrodynamic mode of operations shows average accuracies
of 98.8 and 98.5% with relative standard deviations of 0.6% and 1.3%, respectively. Application of the method for the determination
of menadione in human plasma gives favourable results compared with those obtained by the standard spectrophotometric method.
Received February 26, 2001. Revision October 1, 2001. 相似文献
17.
Radhey M. Naik Raj K. Tiwari Pradeep K. Singh Shiv Bali S. Yadav Abhas Asthana 《Transition Metal Chemistry》2008,33(5):615-623
It is observed that Ag(I) catalyzes the rate of substitution of phenylhydrazine (PhNHNH2) into hexacyanoferrate(II), producing a cherry red colored complex, [Fe(CN)5PhNHNH2]3−. The reaction was monitored at 488 nm leading to the formation of the complex under the conditions: [Fe(CN)6]4− (5.0 × 10−3 mol dm−3), PhNHNH2 (2.0 × 10−3 mol dm−3), temperature (25 ± 0.1 °C), pH (2.8 ± 0.02), and ionic strength, I (0.02 mol dm−3), (KNO3). Under optimum conditions, absorbance at fixed times (A
t
) is linearly related to Ag(I) in the concentration range 10.79–97.08 ng cm−3, in the presence of several diverse ions. The highest percentage error and relative standard deviations in the entire range
of Ag(I) determination are found to be 2.5% and 0.16, with a detection limit of 8.75 ng cm−3 of silver(I). The experimental accuracies expressed in terms of percentage recoveries are in the range of 97.87–102.50. The
method was successfully applied for the determination of Ag(I) in a few synthetic samples and found to be in good agreement
with those obtained from atomic absorption spectrophotometry (AAS). The validity of the proposed method has also been tested
for Ag(I) determination in spiked drinking water samples. The present catalytic kinetic method (CKM) is highly sensitive,
selective, reproducible, and inexpensive. A review of recently published catalytic spectrophotometric methods for determination
of Ag(I) has also been presented for comparison. 相似文献
18.
A novel catalytic procedure for zirconium was proposed based on Zr(IV) catalyzed oxidation of gallocyanine by hydrogen peroxide
in hexamethylene tetramine-hydrochloric acid buffer medium. The calibration graph is linear for 0–110 ngċml−1, and the detection limit is 0.4 ngċml−1 Zr(IV). Most foreign ions do not interfere with the determination, except for Cu2+, Fe3+ and Cr(VI). The interferences of Cu2+ and Fe3+ could be eliminated by masking with EDTA and mannitol, and that of Cr(VI) by reducing to Cr(III) with ascorbic acid. The
typical features of this procedure are that it is sensitive for zirconium, and the determination could be carried out at room
temperature. It had been used to the determination of zirconium in zirconium bronze, simulated samples and a certified reference
material. The recoveries were 98.6 ∼ 102%, and relative standard deviations (R.S.D.) were 0.9 ∼ 1.5%, respectively.
Received September 12, 1999. Revision April 10, 2000. 相似文献
19.
Summary. A new simple, rapid, sensitive, and selective method is proposed for the microdetermination of mercury. Mercury(II) forms
insoluble complexes with 2,3-dichloro-6-(2-hydroxy-3,5-dinitrophenylazo)-quinoxaline (1), 2,3-dichloro-6-(5-amino-3-carboxy-2-hydroxy-phenylazo)-quinoxaline (2), 2,3-dichloro-6-(2,7-dihydroxynaphth-1-ylazo)-quinoxaline (3), and 2,3-dichloro-6-(3-carboxy-2-hydroxy-naphth-1-ylazo)-quinoxaline (4) in aqueous acidic medium; the complexes can be made soluble by the action of an anionic surfactant. The solution of the
pink coloured compounds is stable for at least 24 h. Beer’s law is obeyed over the concentration range from 0.1 to 2.8 μg · cm−3 of mercury. For a more accurate analysis, Ringbom optimum concentration ranges were found to be 0.25–2.5 μg · cm−3. The molar absorpitivity, Sandell sensitivity, and relative standard deviations were also calculated. A slight interference from Pd2+ and Cd2+ is exhibited by the first three ligands, whereas the last one is only negligibly affected by these metal ions. Strong interference
from Ag(I) is evident for all ligands, whereas alkali, alkaline earth, and other transition metals tested posed negligible
interference. 15 μg · cm−3 of Cd2+ and Pd2+ or 10 μg · cm−3 of Ag+ can be tolerated if 1.0 mg of potassium bromide and 2.0 mg of citrate as masking agents are added for the determination of
1.5 μg · cm−3 of mercury(II). The method was applied to the determination of methyl- and ethylmercury chloride and the analysis of environmental
water samples.
Received August 7, 2000. Accepted (revised) October 18, 2000 相似文献
20.
Mohammad Mazloum Ardakani Payam Ebrahimi Karami Hamid Reza Zare Mohammad Hamzehloo 《Mikrochimica acta》2007,159(1-2):165-173
The preparation and electrochemical characterization of glassy carbon electrodes modified with plumbagin were investigated
by employing cyclic voltammetry, chronoamperometry and rotating disc electrode techniques. The cyclic voltammograms of the
electroreduction of oxygen showed an enhanced current peak at approximately −0.289 V in air-saturated phosphate buffer pH
= 7 and scan rate 10 mV s−1. The thermodynamic and kinetic parameters of the reduction of oxygen at glassy carbon have been evaluated using cyclic voltammetry.
The experimental parameters were optimized and the mechanism of the catalytic process was discussed. The obtained values of
E°′ (V vs. Ag/AgCl), the apparent electron transfer rate constant ks (s−1), heterogeneous rate constant for the reduction of O2 at the surface of the modified electrode kh (M−1 s−1) and α (charge transfer coefficient of oxygen) were as follows: −0.146, 23.4, 9.9 × 103 and 0.57, respectively. In addition, plumbagin exhibited strong catalytic activity toward the reduction of H2O2. 相似文献