Certification of total mercury and methylmercury concentrations in mussel homogenate (Mytilus edulis) reference material, IAEA-142

Due to the increased demand for new reference materials certified for total and methylmercury (MeHg) a sample of mussel homogenate (IAEA-142) has been prepared. Thirteen experienced laboratories reported results for total Hg of which 9 laboratories also reported results for MeHg content. Laboratories reporting MeHg results used various isolation techniques (solvent extraction, saponification, acid leaching, ion-exchange separation, and distillation) and detection systems (cold vapour atomic absorption spectrometry (CV AAS), cold vapour atomic fluorescence spectrometry (CV AFS), gas chromatography with electron capture detector (GC/ECD) and HPLC with CV AAS detector). In the case of total Hg, most of the laboratories used acid digestion, only two used alkaline dissolution, followed either by CV AAS or CV AFS. One laboratory used neutron activation analyses with radiochemical separation. The data received were in good agreement. The value for total Hg was certified to be 126 ng/g, with a 95% confidence interval from 119 to 132 ng/g. For MeHg the certified value of 47 ng/g expressed as Hg was assigned, with a 95% confidence interval from 43 to 51 ng/g. Stability testing has shown that both total and MeHg are stable if samples are stored in a dry and dark place at room temperature. The sample is now available as a certified reference material and is, in particular, useful for quality control measurements of Hg and MeHg in mussel samples at low concentration levels.     

Synthesis of 5-fluoro-2-methyl-3-(2-trifluoromethyl-1,3,4-thiadiazol-5-yl)-4(3H)-quinazolinone and related compounds with potential antiviral and anticancer activity

The synthesis of ten new substituted 1,3,4-thiadiazolyl-4(3H)-quinazolinones 8–11, 13, 17 , and 20–23 is reported. Compounds 8–11 were prepared by condensation of 5-fluoro-2-methyl-3,1-benzoxazin-4-one (3) and 5-substituted 2-amino-1,3,4-thiadiazoles 4–7. Compound 13 was obtained by condensation of 5-fluoro-2-methyl-3,1-benzoxazin-4-one (3) with DL-α-amino-?-caprolactam (12) . Compound 17 was synthesized by condensation of 6-bromo-2-methyl-3,1-benzoxazin-4-one (16) and 2-amino-5-t-butyl-1,3,4-thiadiazole (5) . Compounds 20–23 were obtained by condensation of 5-chloro-6,8-dibromo-2-methyl-3,1-benzoxazin-4-one (19) and 5-substituted 2-amino-1,3,4-thiadiazoles 4–7, respectively. The substituted 3,1-benzoxazin-4-ones 3, 16, and 19 were obtained in good yield by refluxing the appropriate anthranilic acid, 1,15 , and 18 with acetic anhydride (2) .     

SDS/n－C5H11OH/n－C7H16/H2O体系中W/O－BI微乳液界面电性质

In the system of SDS/n-C5H11OH/n-C7H16/H2O with the weight ratio of SDS/n-C5H11OH/H2O system at5.0/47.5/47.5, the upper phase of the system was W/O microemulsion, and the lower phase was the bicontinuous microemulsion. When the n-heptane content was less than 1%, with the increase of the n-heptane content, the capacitance (Co, Cod) in the upper phase (W/O) dropped, the capacitance (CB1, CBld) in the lower phase (BI) raised. At the same time, the W/O-BI inteffacial potential (ΔE), capacitance (Ci), and charge-transfer current (ict) decreased.After the n-heptane content reached 1%, with the increase of the n-heptane content, ΔE, Ci and ict demonstrated no significant change.     

Are the pyrazolines formed from the reaction of [60]fullerene with alkyl diazoacetates unstable?

[60]Fullerene-fused pyrazolines 1 were prepared by the reaction of C₆₀ with alky diazoacetates under the solid-state high-speed vibration milling conditions as well as in toluene solution. Pyrazolines 1 were stable in refluxing toluene and its thermolysis process in 1,2-dichlorobenzene was investigated, the decomposition rates and activation energies of pyrazolines 1 were obtained. The current work demonstrated that the liquid-phase reaction of C₆₀ with alkyl diazoacetates undergoes via 1,3-dipolar cycloaddition pathway at room temperature, or proceeds via carbene mechanism at a temperature of refluxing toluene, thus clarifies the previous ambiguity of its reaction mechanism.     

Die Benzonitril‐Addukte [Ho2Cl6(PhCN)6] und [HoCl3(PhCN)]: Synthese,Kristallstrukturen, FIR‐ und MIR‐Spektroskopische Untersuchungen

The Benzonitrile Adducts [Ho₂Cl₆(PhCN)₆] and equation/tex2gif-stack-4.gif [HoCl₃(PhCN)]: Syntheses, Crystal Structures, FarIR and MIR Spectroscopy Investigations Transparent light pink crystals of the compound [Ho₂Cl₆(PhCN)₆] were obtained by the reaction of a mixture of HoCl₃ and AlCl₃ with benzonitrile at 150μ °C. Transparent pink crystals of the compound equation/tex2gif-stack-5.gif[HoCl₃(PhCN)] were obtained by the same reaction under solvothermal conditions at 200μ °C. [Ho₂Cl₆(PhCN)₆] exhibits a dimeric structure of linked pentagonal bipyramids whereas equation/tex2gif-stack-6.gif[HoCl₃(PhCN)] forms a layer structure of trigonal Cl prisms around Ho, linked via corners and separated by coordinating PhCN molecules.     

PA.FPNS: its synthesis and use in spectrophotometric determination of magnesium

A new polymeric chromogenic reagent PA.FPNS has been synthesized by condensing polyallylamine (PA) with 3-(4-formylphenylazo)-4,5-dihydroxynaphthalene-2,7-disulfonic acid (FPNS) and its properties studied. In alkaline media, PA.FPNS reacts with magnesium to form a water-soluble blue complex, whose absorption maximum is at 604 nm. The molar absorptivity (varepsilon) of the complex is 5.2 x 10(4)l mol(-1) cm(-1), which is four times that of the FPNS-Mg complex, and Beer's law is obeyed over the range 0-0.35 mug ml(-1) magnesium. Compared to the corresponding low-molecular-weight FPNS and other chromogenic reagents, PA.FPNS offers considerably improved sensitivity and selectivity for magnesium, which may be attributed to incorporating FPNS into a water-soluble polymer and the effect of the polymeric chain on the reaction microenvironment. Also, a simple and sensitive spectrophotometric method for the determination of magnesium has been developed and applied to water and human fluid samples with satisfactory results.     

New many fold 1,2,3‐selenadiazole aromatic derivatives

The many fold aromatic ketones 2a‐d are versatile compounds for the synthesis of the many fold 1,2,3‐selenadiazole aromatic derivatives 5a‐d . The preparation starts with the reaction between the many fold bromomethylene benzene derivatives 1a‐d and 4‐hydroxyacetophenone, which are transformed through the reaction with semicarbazide hydrochloride or ethylhydrazine carboxylate into the corresponding semicarbazones derivatives 3a‐d or hydrazones 4a‐d . The reaction with selenium dioxide leads to regiospecific ring closure of semicarbazones or hydrazones to give the many fold 1,2,3‐selenadiazole aromatic derivatives in high yield.     

The Henicosaphosphide Iodides of Potassium and Rubidium,K4P21I and Rb4P21I

The novel ternary polyphosphides M₄P₂₁I (M = K, Rb) have been synthesized from the elements in single crystalline form, representing further examples for the formation of mixed crystals between simple salts and binary phosphides. They form as ruby‐red platelets and dark‐red prisms, respectively, and are only slightly sensitive to moisture and oxygen. The compounds are isotypic (Ccmm (no 63); Z = 4; oP104; K₄P₂₁I: a = 12.853Å; b = 21.795Å; c = 9.748Å; 1168 hkl, R = 0.033; Rb₄P₂₁I: a = 13.281Å; b = 21.868Å; c = 9.771Å; 777 hkl, R = 0.053) and feature corrugated 2D networks formed from two different types of polymerized P₇ units. The networks form large cavities filled by M⁺ and I^‐ ions. Zigzag chains of condensed trigonal M₆ prisms, centered by the I^‐ anions, separate the polyphosphide nets. The mean homoatomic P‐P bond length (d = 2.216Å) corresponds to a P‐P single bond. However, the individual P‐P distances vary with position and function (2.126 ‐ 2.247Å) and these are compared with those of the isolated P₂₁^‐3 anion.     

Fabrication, Characterization and Electrocatalysis of an Ordered Carbon Nanotube Electrode

A method for fabrication of ordered carbon nanotube (CNT) film,which was template-synthesized within the highly ordered pores of a commercially available alumina template membrane,modified glassy carbon(CNT/GC) electrode was established.The CNT/GC electrode showed excellent electrocatalytic activity toward dopamine electrochemical reaction without introducing any electrochemically active group into CNT film or activating any electrochemically active group into CNT film or activating the electrode electrochemically.DA undergoes ideal reversible electrochemical reaction on CNT/GC electrode at low scan rate(≤20mV/s) with an excellent reproducibility and stability.The CNT/GC electrode might be used in biosensors because the highly ordered CNT may present a steric effect on more efficient redox reactions of biomolecules.     

Selective determination of uric acid in the presence of ascorbic acid using a penicillamine self-assembled gold electrode

The electrochemical behaviors of uric acid (UA) at the penicillamine (Pen) self-assembled monolayers modified gold electrode (Pen/Au) have been studied. The Pen/Au electrode is demonstrated to promote the electrochemical response of UA by cyclic voltammetry (CV). The diffusion coefficient D of UA is 6.97 × 10⁻⁶ cm² s⁻¹. In differential pulse voltammetric (DPV) measurements, the Pen/Au electrode can separate the UA and ascorbic acid (AA) oxidation potentials by about 120 mV and can be used for the selective determination of UA in the presence of AA. The detection limit was 1 × 10⁻⁶ mol L⁻¹. The modified electrode shows excellent sensitivity, good selectivity and antifouling properties.