Determination of Arsenic and Mercury in Soil by Microwave Digestion and Hidride GenerationAtomic Fluorescence Spectrometry

[Objective] The aim was to develop a rapid, simple method for determina- tion of arsenic and mercury in soil samples by atomic fluorescence spectrometry. [Method] The method for determination of As and Hg in soil by combined atomic fluorescence spectrometry and microwave digestion was used. [Result] The concentration curve was linear within the range of 0-80.0μg/L of As and 0-8.0 μg/L of Hg, and the detection limits of As and Hg was 0.036 μg/L and 0.015 μg/L, respectively. The precision for elevenfold determination of As at 40.0 ug/L level and Hg at 4.0μg/L level were 1.1% and 2.2%（RSD）, respectively. Recoveries of 103.0%-106.6% for As and 90.0%-95.0% for Hg were obtained for there soil samples. [Conclusion] The proposed method has the advantages of simple operation, high sensitivity, and high efficiency; it was successfully used for determination of As and Hg in soil samples.

Geochemical analysis of marine sediments using fused glass disc by X-ray fluorescence spectrometry

A method was developed for content determination of Na, Mg, A1, Si, P,S, C1, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Nb, Zr, Y, Sr, Rb, Ba, La and Ce etc. covering 26 major, minor, and trace elements in marine sediment samples using fused glass disc by X-ray Fluorescence spectrometry. Calibration was made using marine sediment certified reference materials and the synthetic standard samples prepared by mixing several marine sediments with stream sediment and carbonate standard samples in different proportions. The matrix effect was corrected using theoretical alpha coefficients, experience coefficients and the scattered radiation as the internal standard （for the trace elements）. The accuracy of the method was evaluated by analysis of certified reference materials GBW07314, GBW07334 and GSMS6. The results are in good agreement with the certified values of the standards with RSD less than 2.60%, except for Y, Cr, Ga, Ce, La, Nb, Rb, and V with RSD less than 9.0% （n=12）.

Speciation Analysis of Arsenic Compounds in Seafood by Ion Chromatography-Atomic Fluorescence Spectrometry

Ion chromatography-ultra violet-hydride generation-Atomic Florescence Spectrometry was applied to detect 5 arsenic species in seafoods. The arsenic species studied include arsenobetaine(As B), arsenite(As(III)), dimethylarsinic acid(DMA), monomethylarsonic acid(MMA), and arsenate(As(V)), which were extracted from samples using 2% formic acid. Gradient elution using 33 mmol L^(-1) CH_3COONH_4 and 15 mmol L^(-1) Na_2CO_3 with 10 mL CH_3CH_2OH at pH 8.4 allowed the chromatographic separation of all the species on a Hamilton PRP-X100 anion-exchange column in less than 8 min. In this study, an ultrasound extraction method was used to extract arsenic species from seafood. The extraction efficiency was good and the recoveries from spiked samples were in the range of 72.6%–109%; the precision between sample replicates was higher than 3.6% for all determinations. The detection limits were 3.543 μg L^(-1) for As B, 0.4261 μg L^(-1) for As(III), 0.216 μg L^(-1) for DMA, 0.211 μg L^(-1) for MMA, and 0.709 μg L^(-1) for As(V), and the linear coefficients were greater than 0.999. We also developed an application of this method for the determination of arsenic species in bonito, Euphausia superba, and Enteromorpha with satisfactory results. Therefore, it was confirmed that this method was appropriate for the detection of arsenic species in seafood.

Determination of Trace Germanium in Marine Sediments by Hydride Generation-Atomic Fluorescence Spectrometry (HG-AFS)

A method for the analysis of trace germanium in marine sediments by HG-AFS has been investigated. The experimental conditions such as the acidity of reduction reaction, the amount of sodium boro-hydride, the carrier gas flow rate, etc., were tested and optimized by using a kind of orthogonal design. The detection limit of the presented method is 0.95 μg L -1 for germanium. The calibration curve shows a satisfactory line in the concentration range 0-320 μg L -1 Ge with a variation coefficient of ±2.1%.

EVALUATON OF MICROWAVE PLASMA TORCH FOR ATOMIC FLUORESCENCE SPECTROMETRY WITH AN ULTRASONIC NEBULIZATION SAMPLE INTRODUCTION SYSTEM

In this paper, a new MPT(microwave plasma torch) device has been used as a atomizer for atomic fluorescence spectrometry. Spme elements, such as Zn, Cd, Hg, Pb, As, Co, Mg, Cu, Ag, Mn, Fe have been investigated in detail.

Determination of Selenium in Marine Aquatic Products by Hydride Generation-atomic Fluorescence Spectrometry (HG-AFS)

A method for the analysis of selenium in marine aquatic products by HG-AFS has been investigated. The method is based on the reduction of inorganic selenium to volatile SeH2 which is bubbled out by carrier gas of pure argon, and then swept to Ar-H2 flame quarts atomizer to measure its fluorescence intensity. The hydride generation, transportation, atomization and some instrumental parameters were studied by a kind of orthogonal design. The optimum conditions selected are as follows： reactive acidity, 20% HC1; the amount of NaBH4, 4.9mL; gas flow of argon, 600mLmin^-1; atomizing temperature, 200 ℃ ; negative high voltage, - 300V; light current, 100 mA; integral time, 7s. The detection limit of the presented method is 0.072μgL^-1 for selenium. The calibration curve shows a satisfactory line inthe concentration range from 0.000 to 1.000μgL^-1 Se. The recovery is 95.8%-102.2%.

X-ray fluorescence spectrometry determination of open-hearth furnace slag by pressed powder briquetting

A rapid analysis method of determining content of eight compounds of open-hearth furnace slag was developed using X-ray fluorescence spectrometry and pressed powder briquettes. Matrix effect was corrected using theoretical alpha coefficient. Grains-size effect was eliminated by optimized sample preparation technique parameters. Mineral effect was corrected with standard curve of specially made standard samples. The analysis results of TiO2, TFe, SiO2, MgO, Al2O3, CaO, MnO and P2O5 in slag samples showed that both precision and accuracy are comparable with that of chemical method.

Evaluation of Atomic Fluorescence Spectrometry for Determination of Mercury Using a Low-Powered Argon Microwave Plasma Torch (MPT)

The Microwave-Induced Plasma (MIP) has received considerable attention during the past decade since theintroduction of the Becnakker Cavity. It has been commonly used as an atomization cell for atomic emission spectrometry (AES) and atomic absorption spectrometry (AAS), and a great success was achieved for both techniques. More

Determination of Ultra Trace Level of Uranium in Electronic Materials by Fluorescence Spectrometry

Using ultra high purity NaF-NaKCO3 in the Fluorescence spectrometry, determination of sub ppb levels of Uranium in the electronic materials has been achieved. The method could be applied to determination of Uranium in any electronic materials.

Determination of Hg in soil by ultrasonic slurry sampling hydride generation atomic fluorescence spectrometry

Ultrasonic aided slurry sampling hydride generation atomic fluorescence spectrometry （USS-HG-AFS） was developed for the determination of Hg in soil samples from a sewage-irrigated farm. 500 mg grounded soil was suspended in agar solution by an ultrasound water bath before the HG-AFS determination. The results for the reference material of soil （serial number GBW-07411） agreed satisfactorily with the certified values. Results obtained by the developed procedure compared well with those after traditional acid digestion of samples. The detection limit are 6.7ngL-1 for Hg respectively, with average relative standard deviation values of 6.4% for analysis of a series of soil samples of different origin. The recoveries of the anatytes varied in the range from 95 to 107%. This observation has stimulated interest in fast, accurate and sensitive analytical methods for determination of metals in soil.

Determination of trace lead and mercury in airborne particles by hydride generation atomic fluorescence spectrometry

A new method for determination of trace lead and mercury by hydride generation atomic fluorescence spectrometry （HG-AFS） was established. Lead was determined in the medium of citric acid using potassium ferricyanide （K3Fe（CN）6） as oxidant. Ni enhanced the fluorescence signals in this system. Mercury was determined in the medium of nitric acid using mixture of thiourea and ascorbic acid as masking reagent, sodium dioctylsulphosuccinate （SDSS） as enhancing reagent. The working mechanism of the hydride generation of lead and mercury was discussed. Interferences of some coexisting ions were studied systematically and the determination conditions were optimized. Under the optimized conditions, the detection limits of the method were 0.31μg.L^-1 for lead and 0.023 μg·L^-1 for mercury, and the relative standard deviations based on eleven determinations of 5.00 μg·L^-1 standard of Pb and Hg, were 2.6% for Pb and 2.2 % for Hg. This method was applied to the analysis of lead and mercury in four different diameter airborne particles after microwave digestion. Results suggested heavy metal elements easily concentrated in smaller particles.

Determination of Cadmium in TSP, PM10 in urban areas by hydride generation atomic fluorescence spectrometry

In this paper, two different diameter particles （TSP, PM10） were collected by TH-16A four-channels classification air sampler. The samples were treated by HNO3. Analysis of cadmium was carried out by hydride generation atomic fluorescence spectrometry （HG-AFS） method, and distribution proportions of elements in four phases were calculated. This method was based on the reaction of cadmium with 1.5% （m/v） KBH4 solution and 0.5% KOH（m/v） solution to form the hydride gas in medium of 2% （v/v） HCl. The detection limit for cadmium as low as 0.008μg/L was obtained. The lineally correlation coefficient was 0.99992. The relative standard deviation （n=5, C=1.00μg/L） was 3.26%. The proposed method was applied for the determination of cadmium in atmosphere aerosol samples and the recoveries in the range of 95-102.2% were obtained. This method was simple, rapid, less matrix interference and high sensitivity.

Microwave Digestion Sample Hydride Generation-Atomic Fluorescence Spectrometry Determines Trace Selenium of Mogroside

0.2000g mogroside sample is digested by 7.0ml nitric acid and 3.0ml hydrogen peroxide, and generated by coprecipitation enrichment hydride - atomic fluorescence spectrometry determines trace selenium in it. Under optimum experiment conditions, a standard curve was produced using selenium standard solution, the linear equation is Ise=2890.6c＋0.0012,compared wish the linear relaticnship is not by coprecipitation direct determination of standard series Ise=82.56c＋0.0018 Selenium detection sensitivity was increased by 35.01 times,the correlation coefficient of obtained linear regression equation is 0.9996, the detection limit is 0.0012~tg/L and the relative standard deviation is 0.76% （n=5）. Containing 0.1808pg.g-1 Se Luo Han Shen samples. Based on mogroside sample, add a certain of standard solution to do recovery experiment, the obtained recovery rate is in 95.8%-103.6% and the result is satisfactory.

Elemental and proximate analysis of coal by x-ray fluorescence assisted laser-induced breakdown spectroscopy

Although laser-induced breakdown spectroscopy(LIBS),as a fast on-line analysis technology,has great potential and competitiveness in the analysis of chemical composition and proximate analysis results of coal in thermal power plants,the measurement repeatability of LIBS needs to be further improved due to the difficulty in controlling the stability of the generated plasmas at present.In this paper,we propose a novel x-ray fluorescence(XRF) assisted LIBS method for high repeatability analysis of coal quality,which not only inherits the ability of LIBS to directly analyze organic elements such as C and H in coal,but also uses XRF to make up for the lack of stability of LIBS in determining other inorganic ash-forming elements.With the combination of elemental lines in LIBS and XRF spectra,the principal component analysis and the partial least squares are used to establish the prediction model and perform multi-elemental and proximate analysis of coal.Quantitative analysis results show that the relative standard deviation(RSD) of C is 0.15%,the RSDs of other elements are less than 4%,and the standard deviations of calorific value,ash content,sulfur content and volatile matter are 0.11 MJ kg,0.17%,0.79% and 0.41%respectively,indicating that the method has good repeatability in determination of coal quality.This work is helpful to accelerate the development of LIBS in the field of rapid measurement of coal entering the power plant and on-line monitoring of coal entering the furnace.

Interaction of Carbofuran and Bovine Serum Albumin by Spectrometry

[Objective]The aim was to study the interaction characteristic of bovine serum albumin （BSA） and carbofuran. [ Method]With synchronous fluorescence spectrometry adopted, the interaction of carbofuran and BSA in Tris-HCI buffer system （pH 7.40） was investigated. The binding constants at different temperatures were calculated and the interaction types between carbofuran and BSA were discussed. [ Result] Under normal physiological conditions, higher quenching effect of carbofuran on BSA was electrostatic interaction. The changes of different drug concentrations and temperature proved a static quenching of carbofuran with BSA. The binding constants （KSV） at 25 ℃, 37 ℃ and 50 ℃ were 1.17 × 10^4, 1.07 × 10^4 and 0. 99 × 10^4 L/mol respectively with ratio of carbofuran and BSA at 1 ： 1. [ Conclusion ] The research is of guiding significance for learning transport and metabolism of carbofuran at molecular level.

Synthesis and photo activity of phenylazonaphthalene peptide nucleic acid monomers

Phenylazonaphthalene peptide nucleic acid （PNA） monomers were successfully synthesized, and their photoisomerization was examined. The new PNA monomers showed reversible trans-cis isomerization with UVand visible light irradiation, which might be the foundation of photo-regulating the hybridization between PNA containing phenylazonaphthalene unit and DNA. Simultaneously, the fluorescence of the new PNA monomers might make them especially useful as structural probes.

Structural Description of Polyaromatic Nucleus in Residue

The proton nuclear magnetic resonance spectroscopy （1H-NMR）, the synchronous fluorescence spectrometry （SFS） and the ruthenium ions catalyzed oxidation （RICO） method were used to determine the chemical structure of polyaromatic nucleus in Oman residue fractions. The results of 1H-NMR analyses showed that the average numbers of aromatic rings in the aromatics, resins and asphaltenes units were 3.2, 5.6 and 8.2, respectively. SFS was used to investigate the distribution of aromatic rings in residue fractions, the main distribution range of aromatic rings in aromatics, resins and asphaltenes were 3 4 rings, 3--5 rings and more than 5 rings, respectively. The aromatic network in residue fractions was oxidized to produce numerous carboxylic acids. The types and content of benzenepolycarboxylic acids, such as phthalic acid, benzenetricarboxylic acids, benzenetetracarboxylic acids, benzenepentacarboxylic acid and benzenehexacarboxylic acid disclosed the condensed types of aromatic nuclei in the core. The biphenyl fraction （BIPH）, the cata-condensed fraction （CATA）, the peri-condensed fraction （PERI） and the condensed index （BCI） were calculated based on the benzenepolycarboxylic acids formed. The results implied that there was less biphenyl type structures in all residue fractions. The aromatics fraction was almost composed of the cata-condensed type system, and the asphaltenes fraction was wholly composed of the peri-condensed type system, while in the resins fraction co-existed the two types, herein the peri-con- densed type was predominant over the cata-condensed type. Based on the analytical results obtained in the study, the components --aromatics, resins and asphaltenes -- were given the likely structural models.

Investigation and Analysis of Soil Pollution of Heavy Metals(Hg,As) in Duanzhou District,Zhaoqing City

The soil heavy metals(Hg and As)in Duanzhou District of Zhaoqing City were determined by AFS200 T atomic fluorescence spectropho-tometer,and the soil environment in Duanzhou District was evaluated by several evaluation methods of soil heavy metal pollution,such as single factor index method,pollution load index method and Nemerow comprehensive pollution index method.Finally,according to the data and conclu-sions,the soil pollution situation in Duanzhou District of Zhaoqing was analyzed.The results will let more people pay attention to the changes of the environment and realize the harm of the environment,and the government can formulate a new plan conducive to the coordinated development of the environment and economy.

Geochemical Characterization and Mineralogy of Babouri-Figuil Oil Shale,North-Cameroon

Organic geochemistry methods such as high temperature combustion, Rock-Eval pyrolysis and gas analysis were used to analyze oil shale from Babouri-Figuil Basin. Results show that the average content of organic matter is 36.25 %wt, while that of mineral matter is 63.75 %wt. The total organic carbon (TOC) is between 15.93 %wt and 26.82 %wt. The HI vs. Tmax diagram indicates an immature Type I kerogen. The average value of the oil potential (S2b) is 149.95 mg HC/g rock. The gases obtained by retort process are H2, CO2, CO and CnH2n, CnH2n+2. Finally, it emerges that, the organic matter of Babouri-Figuil shales was immature or has just reached the beginning of the oil window. The mineralogical study of Babouri-Figuil oil shale has been carried out by means of XRD (X-Ray Diffractometry) and XRF (X-Ray Fluorescence spectrometry). The results show that mineral matrix contains silica, carbonates, sulphates, oxides and clay minerals. Besides, compounds contain metals and metalloids like Fe, In, Ca. The main oxides are SiO2 (majority), CaO, Fe2O3, Al2O3, SO3, and K2O.

Chemical Characterization of Auriferous Ores from the Brazilian State of Paraiba

One of the most important problems facing the gold industry is that the placer and free milling gold ores are almost terminating. Hence, the use of refractory ores has been increased during the recent years. In general, gold refractory ores occurs in various types of deposits associated with a range of minerals. Among the refractory ores, the sulfide type is the most common. The methodology employed in the mining process depends on the mode of occurrence of the ore and on the particle size, shape and degree of purity of the auriferous species. We have undertaken a mineralogical investigation of a representative sample of a complex gold mining ore collected in the municipality of Princesa Isabel, Paraiba, Brazil, using X-ray fluorescence spectrometry, X-ray diffractometry, infrared spectroscopy, inductively coupled plasma-atomic emission spectrometry and the Fire Assay. The results showed that the arsenic content of the ore was closely related to the gold content, and that the occurrence of “invisible gold” was associated primarily with pyrite and secondarily with arsenopyrite. The sulfur content of the ore was directly related to its refractoriness. It is concluded that gold mineralization in the study area is mainly of the gold-quartz-sulfide veins (lode gold), while the gold found in the mini-fractures of the deposits is probably associated with the hydrothermal processes that occurred in the region.