Analytical Approach to Clusters in near Critical CO2

Clusters greatly influence thermophysical properties of near critical gases. The cluster structures of supercritical fluids in general and Carbon Dioxide especially are important for the advanced supercritical fluid technologies and analytics development. The paper extends to near critical densities the developed earlier methods to extract the clusters’ properties from Online Electronic Database of NIST on thermophysical properties of fluids. This Database contains a hidden knowledge of cluster fractions’ properties in real gases. The discovered earlier linear chain clusters dominate at intermediate densities. Their properties can be extrapolated to high density gases, thus opening the way to study large 3D clusters in near critical zone. The potential energy density of a gas, cleared from the chain clusters’ contribution, reflects only the 3D clusters’ characteristics. A series expansion of this value by the Monomer Fraction density discovers properties of n-particle 3D clusters. The paper demonstrates a discrete row of 3D clusters’ particle numbers and gives estimations for bond energies of these clusters.

Recent progress in microbial cell surface display systems and their application on biosensors

Microbial cell surface display technology is a recombinant technology to express target proteins on the cell membrane,which can be used to redesign the cell surface with functional proteins and peptides.Bacterial and yeast surface display systems are the most common cell surface display systems of prokaryotic and eukaryotic proteins,that are widely applied as the core elements in the field of biosensors due to their advantages,including enhanced stability,high yield,good safety,expression of larger and more complex proteins.To further promote the performance of biosensors,the biomineralized microbial surface display technology was proposed.This review summarized the different microbial surface display systems and the biomineralized surface display systems,where the mechanisms of surface display and biomineralization were introduced.Then we described the recent progress of their applications on biosensors for different types of detection targets.Finally,the outlooks and tendencies were discussed and forecasted with the expectation to provide some general functions and enlightenments to this aspect of research.

Spectrofluorimetric determination of terbium(Ⅲ) by fluorescence enhancement system of Tb-TPA-Triton X-100 by La^(3+)

The phenomenon of fluorescence enhancement for the system of terbium(b!) with terephthalic acid (benzene-1,4-dicarboxylic acid (TPA)) in the presence of an excess of La3+ in Triton X-100 aqueous solution has been studied. The fluorescence intensity of Tbb!-TPA system can be greatly increased by La3+. The intermolecular transfer of energy was responsible for the mechanism of the fluorescence enhancement. Triton X-100 plays an important role for the stabilization of the system. The system, having the maximum excitation and emission wavelengths at 256 nm and 546 nm, respectively, shows a constant fluorescence intensity over the pH range between 4-6. The fluorescence intensity is a linear function of Tb3+concentration in the range of 1.00 ?

Catalytic spectrophotometric determination of trace selenium in microemulsion after separation and enrichment by SDG

A new catalytic spectrophotometric method was developed for the determination of trace amount of Se（Ⅳ） in microemulsion medium. The method is based on the catalytic effect of traces of Se（Ⅳ） on the oxidation of 2＇,4＇-dichlorophenylfluomne （p-CPF） by potassium bromate with HNO3 as an activator in the presence of nonionic microemulsion medium. Under optimum conditions, the calibration graph is linear in the range of 0.4-15 μg·L^-1 of Se（Ⅳ） at 480 nm. The detection limit achieved is 9.86 × 10^-10μg·L^-1. Samples were dissolved and the obtained trace Se（Ⅳ） was separated and enriched by sulphydryl dextrane gel （SDG）. The method has been applied for determination of trace selenium with satisfactory results.

Determination of Sub-Trace Sc, Y and Ln in Carbonate by ICP-MS with Inter-Element Matrix-Matched Technique

A simple method for the determination of Sc, Y and Ln in carbonate at sub μg·g -1 levels by ICP MS with inter elements matrix matched technique was developed. A series of matrix matched standard solution were prepared by adopting the normalized concentration values, which were calculated the statistic average compositions of reference values of REEs in carbonate standard reference materials. The matrix effects of Ca and Mg on REEs were studied in detail and the results show that the matrix effect of Ca and Mg can be ignored when the dilution factors are more than 1000. The combination of 115 In and 103 Rh as internal standard was selected to compensate the drift of analytical signals. The method proposed was applied to the analysis of ultra trace REEs in carbonate references materials GSR 6, GSR 12 and real samples.

Analysis of trace mercury in water by solid phase extraction using dithizone modified nanometer titanium dioxide and cold vapor atomic absorption spectrometry

A new method for analysis of trace mercury in water samples was developed, based on the combination of preconcentration/separation using dithizone-modified nanometer titanium dioxide （TiO2） as a solid phase extractant and determination by cold vapor atomic adsorption spectrometry （CVAAS）. Dithizone was dissolved with alcohol and loaded on the surface of nano-sized TiO2 powders by stirring. The static adsorption behavior of Hg^2＋on the dithizone-modified nanoparficles was investigated in detail. It was found that excellent adsorption ratio for Hg^2＋ could be obtained in the pH range of 7-8 with an oscillation time of 15 rain, and a 5 mL of 3.5 mol·L^-1 HCI solution could quantitatively elute Hg^2＋ from nanometer TiO2 powder. Common coexisting ions caused no obvious influence on the determination of mercury. The mechanisms for the adsorption and desorption were discussed. The detection limit （30） for Hg^2＋ was calculated to be 5 ng·L^-1. The proposed method was applied to the determination of Hg^2＋ in a mineral water sample and a Zhujiang River water sample. By the standard addition method, the average recoveries were found to be 94.4%-108.3% with RSD （n = 5） of 2.9%-3.5%.

Minimizing chemical interference errors for the determination of lithium in brines by flame atomic absorption spectroscopy analysis

Chemical interferences （ionization and oxide/hydroxide formation） on the atomic absorbance signal of lithium in FAAS analysis of brine samples are elaborated in this article. It is suggested that inadequate or overaddition of deionization buffers can lead to loss of sensitivities under particular operating conditions. In the analysis of brine samples, signal enhancing and oxide/hydroxide formation inducing signal reduction resulting from overaddition of deionization buffers can be seen with varying amounts of chemical buffers. Based on experimental results, the authors have arrived at the optimized operating conditions for the detection of lithium, under which both ionization and stable compound formation can be suppressed. This is a simplified and quick method with adequate accuracy and precision for the determination of lithium in routine brine samples from chemical plants or R＆D laboratories, which contain comparable amounts of lithium with some other components.

Fluorescence enhancement and cofluorescence in complexes of terbium(III) with trimellitic acid

The fluorescence of terbium （Ⅲ） was enhanced by about three orders of magnitude in the presence of trimellitic acid （benzene-1, 2, 4-tricarboxylic acid （TLA）） in aqueous solution at pH 6. The fluorescence intensity could be greatly increased when the system of Tb^3＋-TLA was treated with La^3＋ （or Gd^3＋） and TritonX- 100. The addition of La^3＋ （or Gd^3＋） enhanees the fluorescence of the system by about two orders of magnitude due to cofluorescenee, and the TritonX-100 micellar medium plays an important role for stabilization of the system. Both the intermolecular energy transfer mode and intramolecular energy transfer mode are responsible for the mechanism of fluorescence enhancement. In the optimum condi- tions, the fluorescence intensity is a linear function of Tb3~ concentration in the range of 7.8 × 10^-9-3.6 × 10^4 mol/L for the system Tb^3＋-La^3＋-TLA and 1.0 × 10^-8-4.7 × 10^-5 mol/L for the system Tb^3＋-Gd^3＋-TLA, and the limits of detection are 4.6 × 10^-10 mol/L and 6.0 × 10^-10 mol/L, respectively.

Catalytic spectrophotometric determination of trace vanadium in fly ash and coal gangue by Triton X-100 enhancing effect

Trace Ⅴ(Ⅴ) catalyzes mightily the decolorization reaction of arsenazo Ⅲ(AsA Ⅲ) by oxidizing with H_2O_2 in a pH 4.0 HAc-NaAc buffer solution, and the addition of TritonX-100 can further increase the sensitivity of the reaction and its catalytic extent is linear withthe content of Ⅴ(Ⅴ). A catalytic spectrophotometric procedure for determining trace Ⅴ(Ⅴ)wasdeveloped. The results show that the maximun absorption of the color solution is at 560 nm and thedetection limit of the method for Ⅴ(Ⅴ) is 0.014 mg·L^(-1). Beer's law is obeyed for Ⅴ(Ⅴ) in therange of 0.00-0.20 mg·L^(-1). The recoveries are 99.0%-104.6%, and the relative standarddeviations (RSD) are 2.7%-3.7%. Combined with ion-exchange resin, the method has been applied to thedetermination of trace vanadium in fly ash and coal gangue with satisfactory results.

Simultaneous determination of some trace metal impurities in high-purity sodium tungstate using coprecipitation and inductively coupled plasma atomic emission spectrometry

A method based on the combination of coprecipitation with inductively coupledplasma atomic emission spectrometry (ICP-AES) was developed for the determination of impurities inhigh-purity sodium tungstate. Six elements (Co, Cu, Fe, Mn, Ni, and Pb) were coprecipitated bylanthanum hydroxide so as to be concentrated and separated from the tungsten matrix. Effects of somefactors on the recoveries of the analytes and on the residual amount of sodium tungstate wereinvestigated, and the optimum conditions for the coprecipitation were proposed. Matrix-matchingcalibration curve method was used for the analysis. It is shown that the elements mentioned abovecan be quantitatively recovered. The detection limits for Co, Cu, Fe, Mn, Ni, and Pb are 0.07, 0.4,0.2, 0.1, 0.6, and 1.3 μg·g^(-1), respectively. The recoveries vary from 92.5% to 108%, and therelative standard deviations (RSDs) are in the range of 3.1%-5.5%.

Determination of micro yttrium in an ytterbium matrix by inductively coupled plasma atomic emission spectrometry and wavelet transform

In the determination of trace yttrium (Y) in an ytterbium (Yb) matrix byinductively coupled plasma atomic emission spectrometry (ICP-AES), the most prominent line ofyttrium, Y 371.030 nm line, suffers from strong interference due to an emission line of ytterbium.In mis work, a method based on wavelet transform was proposed for the spectral interferencecorrection. Haar wavelet was selected as the mother wavelet. The discrete detail after the thirddecomposition, D3, was chosen for quantitative analysis based on the consideration of bothseparation degree and peak height. The linear correlation coefficient between the height of the leftpositive peak in D3 and the concentration of Y was calculated to be 0.9926. Six synthetic sampleswere analyzed, and the recovery for yttrium varied from 96.3 percent to 110.0 percent. The amountsof yttrium in three ytterbium metal samples were determined by the proposed approach with an averagerelative standard deviation (RSD) of 2.5 percent, and the detection limit for yttrium was 0.016percent. This novel correction technique is fast and convenient, since neither complicated modelassumption nor time-consuming iteration is required. Furthermore, it is not affected by thewavelength drift inherent in monochromators that will severely reduce the accuracy of resultsobtained by some chemometric methods.

Solid-phase extraction of trace Au(Ⅲ) with SDG and determination by the catalytic spectrophotometric method

The new catalytic kinetic spectrophotometric method for Au（III） determination was developed and validated. It was based on the catalytic effect of gold on the oxidation of sudan red III by ammonium peroxodisulfate （（NH4）2S2O8） with nitrilo triacetic acid as an activator in microemulsion and H2SO4 medium. Under optimum conditions, there was the linearity of the calibration curve in the concentration range from 0 to 20 μg/L Au（Ⅲ） at 520 nm. The relative standard deviation was 3.0% with a correlation coefficient of 0.9986. The detection limit achieved was 9.75 × 10^-5 μg/mL. A new method using a column packed with sulfhydryl dextrose gel （SDG） as a solid-phase extractant has been developed for the preconcentration and separation of Au（Ⅲ） ions. The method has been applied to the determination of trace gold with satisfactory results.

Application and research advancement on the microwave-assisted extraction

This paper summarized application and research advancement of the microwave-assisted extraction in the agriculture, food industry, environmental analytical chemistry, traditional Chinese medicine industry, and so on. The microwave-assisted extraction was manifested to be a simple device, wide area of application, high extraction efficiency, good reproducibility and low consumption of agent and time as well as low environmental pollution. At present, industrialization question of the microwave-assisted extraction technology has been attached importance, which will impel the microwave-assisted extraction technology to more development in the future

Spectrofluorimetric determination of gallium with calon-carboxyli cacid

A simple and sensitive spectrofluorimetric procedure for the analysis ofmicroquantities of gallium in alloy was described. The method is based on the formation ofGa(III)-CCA (calon-carboxylic acid) complex. The emission of the fluorescent complex was measured atlambda = 620 nm with excitation at lambda = 584 nm. A good linearity was found in the gallium rangeof 0.7-280 ng/mL. The precision of the method is good and the relative standard deviation is 1.9percent for a gallium standard solution of 70 ng/mL. The procedure was proved to be suitable interms of accuracy and selectivity for the microamount of gallium in alloy.

Fluorescence determination of platinum with dibromohydroxyphenyl-fluorone in microemulsion after separation and enrichment by sulfhydryl dextrose gel

A new fluorescence quenching method has been developed for the determination of platinum in nonionic microemulsion medium.This method is based on the fact that platinum can form a stable chelate with dibromohydroxyphenyl-fluorine（DBHPF） when they are in the molar ratio of 1：2 in the nonionic microemulsion medium.Under optimum conditions,the system,having the maximum excitation and emission wavelengths at 468 nm and 532 nm,respectively,shows constant fluorescence intensity in the pH range of 3.5-4.0 and high selectivity and sensitivity as well as low interference from foreign ions.Furthermore,this fluorescence intensity is a linear function of Pt（IV） concentration in the range of 0.002-1.00 μg·mL^-1 and the limit of detection is 2.90 ng·mL^-1.

The ultra-sonication of minerals in swine feed

A sample preparation method based on ultrasound assisted-extraction （UAE） of Ca, Mg and P from swine feed has been described. The experiment was performed to cover the variables influencing the sonication process and, the method validation using standard reference material. Final solutions obtained upon sonication were analyzed by flame atomic absorption spectrometry （for Ca and Mg） and by UV-vis spectrophotometry （for P）. The best conditions for metal extraction were as follows： sample mass： 100 mg in 20 mL 0.10 mol/L HCI, a particle size： 〈60 lam, sonication time： 5 cycles of 10 s and ultrasound power： 102 W. The UAE method was applied in digestibility assays in different piglet feeds and their results showed that it is highly comparable （P 〉 0.05） to the other methods used for such purposes, as block digestion, and offered a Ca, Mg and P method of quantification limit of 10.6, 12.4 and 14 mg/kg, respectively. The major advantages of the UAE method compared to other methods are the high treatment rate, low reagent usage in the extracts and, it does not generate toxic residues that might negatively affect human health and the environment, accompanied by good precision and accuracy.

Analysis of rare earth elements in high purity europium oxide

Five trace impurities as Ce, Pr, Sm, Gd, and Dy are separated from europium oxide with P507 extraction resin by extraction chromatography. When determined simultaneously by ICP-AES, the impurities show their recovery ratios between 88% and 105%. A lower than 10% relative standard deviation of these elements is obtained when their contents in europium oxide are 5μg/g. The satisfactory results indicate this simple method is sensitive and accurate. It has been employed in the analysis of these five rare earth elements in 99.99% europium oxide.

Quantitative Analysis of Components in OC-CS Sprays by High Performance Liquid Chromatography with Double Wavelength UV Detection

The method of reversed-phase high performance liquid chromatography was established for the determination of effective components in OC-CS spray using double wavelength UV detection.The method was utilized under following conditions:a column of Kromasil C18(250 mm × 4.6 mm,5 μm),mobile phase consisting of methanol/water(80 /20) at a flow rate of 0.8 mL/min,column temperature of 25 ℃,and the UV detection at 227 nm and 300 nm.Three key components in OC-CS spray could be distinguished clearly,including o-chlorobenzalmalononitrile(CS),oleoresin capsicum(OC) and dihydrocapsaicin(DC).This method has the advantages of fast,simple and satisfactory linear relationship between UV absorption and concentration.It may be considered to turn into a standard method for detection of related components in the spray.

Studies on Determination of Ge in Au Alloys by Potassium Iodate Potentiometric Titration Method

The paper presents a new method of determining Ge in gold alloys by potassium iodate potentiometric titration rather than by traditional distillation separation. The influences of conditions such as the reduction acidity, dosage of sodium hypophosphite and reduction time on the determination of Ge were studied. Comparison was made between the influences of end-point indication for potential method and starch method on accruracy and precision of the analysed results, stability and sensitivity of end-point, selectivity of method and so on. The possibility of reaction in an electrochemical way was discussed. Ge in the alloys such as AuGe 12 , AuGeNi 12 2 , AuAgGe 18.8 12.5 and AuAgGeNi 43.8 6 0.2 was measured, respectively, with the relative standard deviation of 0.10%~0.31% and the recoveries of added standard Ge in sample of 99.40%～100.40% when the reduction acidity was 0.40~0.80 mol/L HCl and 3.3 mol/L H 3 PO 4, 15 g sodium hypophosphite and reduction time 40 min. The new method presented is high accuracy and precision in results, good stability and sensibility in end point, easy operation and strong selectivity of determination. When it is applied to analyse actual samples, satisfactory results are achieved.

Trace Determination of Scandium Using Adsorption Voltammetry of Mix-Polynuclear Complex of Scandium-Calcium-Alizarin Red S at Carbon Paste Electrode

A novel method was described for the determination of ultra trace amount of scandium based on the cathodic adsorptive voltammetry of the mix-polynuclear complex of scandium-calcium-alizarin red S at a carbon paste electrode (CPE). The 2nd-order derivative linear scan voltammograms of the adsorbed complex were recorded by model JP-303 polarographic analyzer from 0.0 to -1.0 V (vs. SCE). The experimental conditions of the working procedure were optimized. The results show that the complex can be adsorbed on the surface of the CPE, yielding one peak at -0.61 V, corresponding to the reduction of the alizarin red S in the mix-polynuclear complex at the electrode. The detection limit of Sc^(3+) is 1.0×10^(-10) mol·L^(-1) for 3 min of accumulation time. The procedure was successfully applied to the determination of trace amount of scandium in the sample ores.