Determination of some carbonyl carboxylic acids using chemiluminescent reaction of Ru(bipy)3 2+−Ce(IV)

A coupled chemiluminescence method for the determination of some carboxylic acids was developed, based on their enhancement the chemiluminescence light emission of the reaction of tirs (2,2′-bipyridine) ruthenium(II) and Ce(IV) in sulfuric acid medium. The conditions for their determination were optimized. The following detection limits were obtained: oxalic acid, 2.67×10⁻⁸ mol/L; propandioic acid, 1.20×10⁻⁶ mol/L; pyruvic acid, 1.35×10⁻⁸ mol/L; citric acid, 5.10×10⁻⁸ mol/L; barbituric acid, 2.48×10⁻⁷ mol/L. The proposed method was successfully applied to determination of oxalic acid. The coupled chemiluminescent reaction mechanism and rate equation are proposed. Foundation item: Supported by the National Natural Science Foundation of China and the Natural Science Foundation of Hubei Province Biography: HAN He-you (1962-), male, Associate professor, phD, graduate candidate     

HPLC determination of ascorbic acid using luminol-Cu (II) chemiluminescence-application to the analysis of Juice beverage

The chemiluminescence (CL) of luminol-Cu (II) was applied to HPLC determination of ascorbic acid, which was separated by a C₁₈ reverse-phase column with a mobile phase of 0.25 mol/L HAc. The eluted ascorbic acid was mixed with 0.3 mmol/L luminol and 0.05 mol/L CuSO₄. The light emission from the reaction of Cu(II) oxidized ascorbic acid and luminol was detected by a modified luminometer. The detection limit was 3.6×10⁻⁶ mol/L for ascorbic acid at aS/N ratio of 3, and the linear calibration range was 2×10⁻⁴–2×10⁻³ mol/L. The relative standard deviation for 5 replicate injections of 1×10⁻³ mol/L ascorbic acid was calculated as 4.3%. The method was successfully applied to determination of ascorbic acid in juice beverage. Foundation item: National Natural Science Foundation of China (29605001) Biography: Wu Feng-wu(1963-), male, research direction: analytical chemistry.     

Electrocatalytic oxidation of H<Subscript>2</Subscript>O<Subscript>2</Subscript> at a carbon paste electrode modified with a nickel (II)-5, 11, 17, 23-tetra-tert-butyl-25, 27-bis(Diethylcarbamoylmethoxy) calix[4] arene complex and its application

Electrochemical behavior of a carbon paste electrode (CPE) modified with nickel(II)-5, 11, 17, 23-tetra-tert-butyl-25, 27-bis(diethylcarbamoylmethoxy) calix[4]arene (Ni (II)-L) complex and its electrocatalytic activity towards the oxidation of hydrogen peroxide were investigated by cyclic voltammetric technique in a 5.0×10⁻² mol/L NaClO₄+1.0×10⁻³ mol/L NaOH solution. It was found that Ni(II)-L acts as an effective catalyst for the oxidation of hydrogen peroxide. The modified electrode exhibited a linear response over a hydrogen peroxide concentrations in the range of 2.0×10⁻⁵−1.0×10⁻⁴ mol/L with a detection limit as low as 1.0×10⁻⁶ mol/L. The relative standard deviation was 3.5% for 5 successive determinations of H₂O₂ at 1.0×10⁻⁵ mol/L. The modified electrode was used successfully in rainwater analysis. Foundation item: Supported by the Natural Science Foundation of Hubei Province (98J040). Biography: Li Chun ya(1972-), Ph. D. candidate, research direction: electroanalysis and electrosynthesis.     

Compression behavior and equation of state of Ni77P23 amorphous alloy

The compression behavior of Ni77P23 amorphous alloy is investigated at room temperature in a diamond-anvil cell instrument using insitu high pressure energy dispersive X-ray diffraction with a syn- chrotron radiation source. The equation of state is determined by fitting the experimental data accord- ing to Birch-Murnaghan equation: -ΔV/V0=0.08606P-3.2×10-4P2 5.7×10-6P3. It is found that the structure of Ni77P23 amorphous alloy is stable under pressures up to 30.5 GPa.     

电沉积Ni-S合金析氢阴极的研究

以硫脲作为硫源,在瓦特浴体系中通过电沉积方法获得NiS合金电极·系统地讨论了电沉积过程中各工艺条件(硫脲浓度、电流密度、pH值及温度)对镀层中S含量的影响,确定了硫脲浓度和电流密度为NiS合金镀层中S含量的主要影响因素;以恒电流极化方法测试不同S含量的合金电极的析氢过电位,得到了析氢过电位仅为90mV的非晶态NiS合金析氢阴极;以稳态极化方法测定该电极的稳态极化曲线,并通过计算得出其电化学参数(b,i0)·结果表明,该电极具有极高的电化学活性·     

The electrochemical properties of thionine adsorbed monolayer on gold electrode

A gold electrode modified with adsorbed thionine monolayer was investigated with ac impedance and cyclic voltammetry method. It was found there were some different redox properties for the adsorbed thionine depended on the different potential scanning rate. At the slower potential scanning rate (10 mV· s⁻¹), the dimer of thionine appeared and possessed the catalytic activity for the oxidation of ascorbic acid. The underpotential deposition (UPD) and the bulk deposition of Cu²⁺ were also employed to investigate the monolayer of adsorbed thionine. Biography: Fang Cheng (1971-), male, Ph. D candidate, research direction: electroanalysis.     

Synthesis and X-ray crystal structure of a new manganese 18-metallacrown-6

0　IntroductionThemetalionsinmetallamacrocylesformedbysupramolecularself assemblycantaketrigonal,square planar,andtetrahe dralconfiguration[1 ,2 ] .Metallacrownisaspecialclassofmetalla macrocyle,theyareanalogoustocrownethersinbothstructureandfunctionexceptthatthemetalionsarenowtakingthepositionsofcoordinationatomsincrownether[3,4] .Themetallacrownswithdifferentnumberof [M—N—O]repeatunithavedifferentcavitysizes,suchas 9 MC 3[5 7] ,12 MC 4 [4,8 1 4 ] and 15 MC 5 [1 5] .Thereportedazameta…     

Chemiluminescence determination of tetracycline and oxytetracycline in pharmaceutical preparations using Ru (bipy)3 2+-cerium (IV) system

A new chemiluminescence (CL) method for the determination of tetracycline and oxytetracycline is developed, based on the CL reaction of tetracycline and oxytetracycline with Ru (bipy)₃ ²⁺ and Ce (IV). In sulfuric acid medium, the CL emission is generated upon continuous oxidtion of Ru(bipy)₃ ²⁺ by cerium (IV). The emission intensity is greatly enhanced when tetracycline and oxytetracycline are introduced into the reaction system after acid degradation. Under the optimum conditions, the calibration curves are linear over the range of 8.0×10⁻⁸∼4.0×10⁻⁶ mol/L for tetracycline and of 2.0×10⁻⁷∼4.0×10⁻⁵ mol/L for oxytetracycline, with the detection limits are 4.2×10⁻⁸ mol/L for tetracycline and 1.5×10⁻⁷ mol/L for oxytetracycline, respectively. The proposed method was used for the determination of tetracycline and oxytetracycline in pharmaceutical formulations with good results. Foundation item: Supported by the National Natural Science Foundation of China and the Natural Science Foundation of Hubei Province. Biography: HAH He-you (1962), male, Associate profeddor, Ph.D graduate candidate. Present address, Department of Chemistry, Huainan Teacher's College, Huainan.     

Voltammetric determination of estrogens based on the enhancement effect of surfactant at carbon paste electrode

Highly sensitive voltammetric method for the determination of estrogens, based on the enhancement effect of cetyltrimethylammonium bromide (CTAB) has been described. In the presence of CTAB, the oxidation peak currents of estrogens (estradiol, estrone, estriol, estradiol valerate and diethylstilbestrol) as the carbon paste electrode (CPE) increased significantly after open-circuit accumulation. The peak current was proportional to the concentration of estradiol over the range from 5×10⁻⁹ to 2.5×10⁻⁶ mol·L⁻¹. The detection limit was 8×10⁻¹⁰ mol·L⁻¹ at 6 min of accumulation. The total amounts of estrogens in the blood serums were determined and the average recovery was 104.92%. Under the conditions used, the electrode process of estradiol was examined the mechanism for peak current enhancement was also discussed. Foundation item: Supported by the National Natural Science Foundation of China (60171023) and the Natural Science Foundation of Hubei Province (99J060) Biography: Wu Kang-bing(1977-), male, Ph.D. candidate. research direction: bioelectrochemistry.     

Synthesis, conductivity and photosensitivity of 2-D conjugated polymers of metalporphyrazine with sulfur bridges

The title polymers PMS₈Pz, M=Mn^II, Fe^II, Co^II, Ni^II, Cu^II, Zn^II, were synthesized by reaction of 2, 3, 5, 6-tetracyano-1, 4-dithiin with corresponding metal salts, respectively. The structure and properties of these polymers were characterized by elemental analysis, transmission electron microscope, DTA, IR, UV-Vis, fluorescence and EPR spectra. It has been found that these conjugated polymers have the property of intrinsic semiconductor. The conductivity σ_298K of these polymers is in the range of 10⁻⁹≈10⁻³ S·cm⁻¹ under pressure 10.63 MPa and incrementals in the metal order Mn<Co<Fe<Zn<Cu<Ni. The photosensitivity of the MS₈Pz to the CdS-PVA films is incrementals in the metal order Zn<Mn<Co<Fe<Cu<Ni. Supported by the National Natural Science Foundation of China and by the Approach Fund of State Key Laboratory of Coordination Chemistry in Nanjing University Peng Zhenghe: born in Apr. 22, 1945, Professor     

The synthesis and characterisation of polyaniline catalysed and doped by squaric acid

Aniline was polymerized in dilute aqueous squaric acid and the polyaniline (PAn) was doped with 10⁻¹–10⁻³ mol/L of squaric acid. The corresponding electrical conductivity of the PAn is 10⁻¹–10⁻² S ⊙ cm⁻¹. The solubility of the doped PAn has been improved in common polar organic solvents. The FTIR and UV—Vis spectra show that the PAn has the structure of both quinone and imine. Supported by the National Natural Sciences Foundation of China Zhan Caimao: born in 1948, Associate professor     

Cellulose-hydrogen production from corn stalk biomass by anaerobic fermentation

Cellulose-hydrogen production from corn stalk by lesser panda manure was carried out in batch tests and a 5 L scale-up continuously stirred anaerobic bioreactor(CSABR),respectively.The bio-pretreatment of corn stalk was found most effective at 25℃ using microbe additive of 7.5 g/kg,in which the yields of soluble saccharides(SS) and lactic acid were 212 mg/g-TS and 21 mg/g-TS,respectively.The maximum cumulative H2 yield(176 ml/g-TS) and H2 production rate(14.5 ml/g-TS h-1) were obtained at pH 5.5,36℃ by trea...     

Spectrofluorimetric method for the determination of triamcinolone acetonide

0　IntroductionTriamcinoloneAcetonide,9 fluoro 11β,2 1 dihydroxy 16α,17[(1 methylethylidene)bis (oxy) ] pregn 1,4 diene 3,2 0 dione,Mris 4 34.4 8(abr.TA ) .Itbelongstoaclassofadrenalcortexhormonedrug ,whosefunctionsareaffectionofsugarmetabolism ,anti inflammationandresistancehypersusceptibilityetc.TAcanbesuitabletorheumatoidarthritisanddermatosissuchashypersusceptibilityandneuropathicdermatitis .ThefunctionsofTAisstrongerandlongerthantriamcinolone[1 ,2 ] .ThecommonmethodsofdetectingTAm…     

Application of Nanometer-Size Titanium Dioxide in Extreme-Trace V（Ⅴ） Analysis

0Introduction Vanadiumplaysanimportantroleinmodernindustry,es peciallyinsteelandchemicalindustry.Forinstance,itscompoundsarewidelyappliedintheproceduresofvitrioland petroleumchemicalmanufactureascatalyzers[14].Vanadium hasseveralvalences,butgenerallyitslowvalencesturnintohighoneseasilyinenvironment[5].BecauseV(Ⅴ)isthemost stableandpoisonousone,weoftenlayemphasisonitinenvi ronmentalpollutioncontrol.Vanadiumexistsinenvironmentalwaterwithextremelylowconcentration.Inseawateritscontentislessthan…     

Organic media enhanced spectrofluorimetric determination of L-ascorbic acid

A novel spectrofluorimetric method for the determination of L-ascorbic acid is proposed. It is based on the inhibition of L-ascorbic acid on the formation of 2,3-diaminophenazine, which is an oxidation product ofo-phenylenediamine catalyzed by laccase. The fluorescence (at λ_cx/λ_cm=464 nm /530 nnm) was enhanced strongly in the presence of organic media. The mechanism ofo-phenylenediamine oxidation reaction catalyzed by laccase in the presence of L-ascorbic acid is discussed. L-ascorbic acid is determined in the ethanol, 1,4-dioxane and acetone over the linear range of 4.0×10⁻⁷≈1.2×10⁻⁴ mol/L, 4.0×10⁻⁷≈8.0×10⁻⁵ mol/L and 4.0×10⁻⁷≈1.0×10⁻⁴ mol/L with a detection limit of 1.20×10⁻⁵ mol/L, 1.19×10⁻⁵ mol/L and 1.24×10⁻⁸ mol/L, respectively. The method has been successfully applied to the simple and rapid determination of L-ascorbic acid in pharmaceuticals and milk powder. Supported by National Natural Science Foundation of China and the Special Funds of State Education Committe for Doctorate Research Huang Zuyun: born in Aug. 1963. Ph.D     

Spectrofluorimetric determination of magnesium (II) with 7-(8-Hydroxy-3, 6-disulfonaphthylazo)-8-hydroxyquinoline-5-sulfonic acid

A new fluorescent reagent, 7-(8-hydroxy-3, 6-disulfonaphthylazo)-8-hydroxyquinoline-5-sulfonic acid (HDNHQ) for the determination of magnesium has been developed. It reacted with magnesium to form a 1∶1 fluorescent complex withλ _ex/λ _em immediately at room temperature in ammonia-ammonium chloride buffer (pH 10.7). A linear relationship was obtained in the magnesium concentration range of 0–160 ng·mL⁻¹ with the detection limit of 0.04 ng·mL⁻¹. The proposed method was simple, rapid and sensitive. It has been successfully applied to the determination of trace magnesium in blood serum with recoveries of 103.75% and 98.16%, respectively. Foundation item: Supported by the Zi-Qiang Foundation of Wuhan University Biography: Zhang Xian (1975-), female, Ph. D candidant, research direction: organic reagent synthesis and analysis.     

Synthesis, Characterization and Properties of LiFePO4/C Cathode Material

Lithium iron phosphate coated with carbon (LiFePO₄/C) was synthesized by improved solid-state reaction using comparatively lower temperature and fewer sintering time. The carbon came from citric acid, which acted as a new carbon source. It was characterized by thermogravimetry and differential thermal analysis (TG/DTA), X ray diffractometer (XRD), Element Analysis (EA) and Scanning electron microscope (SEM). We also studied the electrochemical properties of the material. The first discharge capacity of the LiFePO₄/C is 121 mAh·g⁻¹ at 10 mA·g⁻¹, at room temperature. When the current density increased to 100 mA·g⁻¹, the first discharge capacity decreased to 110 mAh·g⁻¹ and retained 95% of the initial capacity after 100 cycles. The LiFePO₄/C obtained shows a good electrochemical capacity and cycle ability at a large current density. Foundation item: Supported by the National Natural Science Foundation of China (20071026) Biography: ZHOU Xin-wen (1980-), male, Master, research direction: inorganic material chemistry.     

Effects of gravity on the electrodeposition and characterization of nickel foils

The effects of gravity on nickel electrodeposition, the morphology and mechanical properties of deposits were studied in a super gravity field. Predictions in a microgravity field were also presented based on the obtained experimental tendency. Linear sweep voltammetry reveals that the nickel electrodeposition process is enhanced by increasing the gravity coefficient (G). The limiting current density changes from 10.2 to 293.0 mA·cm-2 with the increase of the G value from 10-4 to 354. The morphology of deposits was analyzed by scanning electron microscopy (SEM) and atomic force microscopy (AFM). The images show that the morphology deposited in the super gravity field has finer grain sizes and denser and smoother surfaces. The roughness reduces from 48.3 to 4.9 nm with the increase of the G value from 10-4 to 354. Meanwhile, mechanical tests indicate that the mechanical properties of nickel foils are greatly improved due to introducing a super gravity field during electrodeposition.     

Fluorescence Determination of Artemisinin Using Hemoglobin as Catalyst and Pyronine B as Substrate

0 IntroductionMaalnadria siusb atr ompajicosr .he aAltrthe pmrisoibnlienmi (n qtihneghtraoopsiucs,QHS,Fig.1) is a sesquiterpene endoperoxide isola-ted fromArtemisia annuaL., an ancient Chineseherbal medicine usedfor treatment of fever and ma-laria.Studies of the structure and activity relation-ship have shownthat endoperoxide groupis essentialfor anti malarial activity of QHS and absence of thismoiety lead to completely loss in activity of thedrug. Many techniques have been developed to de…