基于局域表面等离子体增强的NaYF_4:Yb,Er荧光上转换及其应用

阐述了局域表面等离子体共振增强荧光上转换的相关机制,并以此为基础总结了三种调节机制和四种上转换/金属复合材料结构。具有明显增强效果的上转换/金属结构复合材料大致分为四种:掺入Au和Ag纳米颗粒的稀土掺杂基质;core/shell结构;稀土掺杂的NaYF_4靠近金属颗粒或金属纳米线所形成的gap结构;周期性金属阵列结构。最后介绍了它们在生物医学和光电子器件领域的应用进展。

The Determination of Heavy Metal Elements in Honey by MWD-ICP-AES

In order to build method for measuring of elements in honey, the contents of Ba, Cu, Pb, Cd, As, Hg, Cr, Mn, Se had been determined by microwave diges- tion （MWD） and actively coupled plasma atomic emission spectrometry （ICP-AES）. The results show that, the range of heavy metal elements were in the range of 0- 10.0 mg/L, with good linear relationship. In addition, all correlation coefficients kept higher than 0.999, and the recovery rate of ample added with standard solution was in 94.1%-110%. By comparison with the result of chemical experiment, the method was quickly accessible and convenient, widely used in the measurement of elements in honey, with satisfactory results.

The Determination of Heavy Metal Elements in Sipunculs nudus by MWD-ICP-AES

In order to develop a method for measuring of elements in Sipunculus nudus, the contents of Cu, Pb, Cd, Cr, Mn, As, Hg and Ba were determined by actively coupled plasma atomic emission spectrometry （MWD） and microwave digestion （ICP-AES）. The results showed that correlation coefficients al kept higher than 0.999 and the recovery rates of sample added standard solutions were in 98%-114%. The results indicated that the contents of Cu, Pb, Cd, Cr, Mn, As, Hg and Ba were 17.119, 3.781, 0.695, 7.351, 1997.982, 0.620, 0.144, 4.249 mg/kg respectively. The contents of Mn exceeded national limit by hundredfold, Cd sevenfold, Pd fourfold, Cd three-and-a-half-fold, and As onefold. Sipunculs nudus became seriously pol uted. Therefore, it is necessary to formulate robust policies to fol ow closely and pay close attention to coastal areas pol ution around Dongfang City.

药用滑石粉酸中可溶物中杂质元素的分析及探讨

目的:通过能谱扫描电镜与ICP-AES的联合应用,考察滑石粉酸中可溶物项目控制的必要性与可行性。方法:通过扫描电子显微镜/X-射线能谱仪(SEM/EDS)对滑石粉酸中可溶物的主要金属元素构成进行分析,并采用电感耦合等离子体原子发光光谱法(ICP-AES)定量测定酸中可溶物中的钙、镁、铁等主要金属元素杂质。结果:扫描电子显微镜/X-射线能谱仪(SEM/EDS)发现滑石粉酸中可溶物普遍存在镁元素,但现行各国药典中均未对可能存在的酸溶性镁盐进行控制。增加ICP-AES测定法,对滑石粉酸中可溶的钙、镁、铁进行考察,并经方法学验证,方法可行。结论:(1)不同来源的滑石粉,酸中可溶物的金属元素含量构成比例有所不同,有必要对酸中可溶物进行控制;(2)ICP-AES可对滑石粉酸中可溶物的钙、镁、铁等主要金属元素杂质进行质量控制及评价。

ICP-AES法测定硅钢中铌的不确定度评定

分析了电感耦合等离子体发射光谱法(ICP-AES)测定硅钢中铌的检测过程,讨论了该检测过程中不确定度的主要来源,建立了该方法的定量的数学模型,并根据这一模型计算出了检测结果的合成标准不确定度和扩展不确定度。

Construction of Inorganic Elemental Fingerprint and Multivariate Statistical Analysis of Marine Traditional Chinese Medicine Meretricis concha from Rushan Bay

Meretricis concha is a kind of marine traditional Chinese medicine(TCM), and has been commonly used for the treatment of asthma and scald burns. In order to investigate the relationship between the inorganic elemental fingerprint and the geographical origin identification of Meretricis concha, the elemental contents of M. concha from five sampling points in Rushan Bay have been determined by means of inductively coupled plasma optical emission spectrometry(ICP-OES). Based on the contents of 14 inorganic elements(Al, As, Cd, Co, Cr, Cu, Fe, Hg, Mn, Mo, Ni, Pb, Se, and Zn), the inorganic elemental fingerprint which well reflects the elemental characteristics was constructed. All the data from the five sampling points were discriminated with accuracy through hierarchical cluster analysis(HCA) and principle component analysis(PCA), indicating that a four-factor model which could explain approximately 80% of the detection data was established, and the elements Al, As, Cd, Cu, Ni and Pb could be viewed as the characteristic elements. This investigation suggests that the inorganic elemental fingerprint combined with multivariate statistical analysis is a promising method for verifying the geographical origin of M. concha, and this strategy should be valuable for the authenticity discrimination of some marine TCM.

Inorganic Elemental Determinations of Marine Traditional Chinese Medicine Meretricis concha from Jiaozhou Bay:The construction of Inorganic Elemental Fingerprint Based on Chemometric Analysis

The goal of this paper is to explore the relationship between the inorganic elemental fingerprint and the geographical origin identification ofMeretricis concha, which is a commonly used marine traditional Chinese medicine （TCM） for the treatment of asthma and scald bums. For that, the inorganic elemental contents ofMeretricis concha from five sampling points in Jiaozhou Bay have been determined by means of inductively coupled plasma optical emission spectrometry, and the comparative investigations based on the contents of 14 inorganic elements （A1, As, Cd, Co, Cr, Cu, Fe, Hg, Mn, Mo, Ni, Pb, Se and Zn） of the samples from Jiaozhou Bay and the previous reported Rushan Bay were performed. It has been found that the samples from the two bays are ap- proximately classified into two kinds using hierarchical cluster analysis, and a four-factor model based on principle component analysis could explain approximately 75% of the detection data, also linear discriminant analysis can be used to develop a prediction model to distinguish the samples from Jiaozhou Bay and Rushan Bay with accuracy of about 93%. The results of the present investi- gation suggested that the inorganic elemental fingerprint based on the combination of the measured elemental content and chemom- etric analysis is a promising approach for verifying the geographical origin ofMeretricis concha, and this strategy should be valuable for the authenticity discrimination of some marine TCM.

Preparation and Characterization of High Purity Enriched 10B Boric Acid via Anti-Solvent Recrystallization

Self-made enriched IUB boric acid as raw material was purified by recrystallization. The effects of final crystallization temperature, crystallization time, stirring speed, crystallization frequency and other factors on the purity were investigated. The appropriate operating condition was that the final crystallization temperature and time were 5 ℃ and 10 h respectively under a low-speed stirring for crystallizing twice, which would make the purity and yield of boric acid reach 99.94% and 95.36%, respectively. Taking this as foundation, recrystallization process was optimized with acetone as anti-solvent, whose amount was the most important index. The boric acid solution was added into acetone and recrystallized under the same condition, and the purity and yield of boric acid would reach 99.98% and 99.61%, respectively. The product detected by XRD was confirmed as boric acid crystal. Main ion concentration in the product was detected by ICP, which basically met the national standard of high purity. Crystal morphology of boric acid was observed by SEM.

Effect and mechanism of dolomite with different size fractions on hematite flotation using sodium oleate as collector

The effect of dolomite with different particle size fractions on hematite flotation was studied using sodium oleate as collector at p H of about 9. The effect mechanism of dolomite on hematite flotation was investigated by means of solution chemistry, ultraviolet spectrophotometry(UV), inductively coupled plasma atomic emission spectrometry(ICP-AES) and X-ray photoelectron spectroscopy(XPS). It is observed that dolomite with different size fractions has depressing effect on hematite flotation using sodium oleate as collector, and dolomite could be the "mineral depressant" of hematite using sodium oleate as collector. The reasons for that are concerned with sodium oleate consumption and the adsorption onto hematite of dissolved species of dolomite.

Distribution,fractionation,and contamination assessment of heavy metals in offshore surface sediments from western Xiamen Bay,China

Surface sediment samples were collected at 21 offshore sites in western Xiamen Bay, Southeast China. Total concentrations of Li, V, Cr, Co, Ni, Cu, Zn, St, Mn, Pb, Ba, Fe, and Ti were determined by inductively coupled plasma-optical emission spectrometry; Hg was determined by atomic fluorescence spectrometry. A modified BCR sequential extraction procedure was used to extract fractions of the above elements. Concentrations of Pb, Cr, and Hg at most sites met the primary standard criteria of Marine Sediment Quality except site S12 for Pb and S7 for Cr, while concentrations of Zn at 17 sites and Cu at seven sites exceeded the criteria. The mean concentration of Hg was three times higher than the background, with a possible source being the Jiulong River. Fe, Ti, Ba, Co, V, and Li dominated the residual phase, mainly from terrestrial input. Ni, Cr, Pb, and Hg in the non-residual phase varied largely between sites. Sr, Mn, Cu, and Zn were mainly in the non- residual fraction. Most sites showed considerable ecological risk; exceptions were site S7 （very high） and sites S10, S11, and S14 （moderate）. Cu showed moderate-to-high pollution and Pb exhibited no-to-low pollution, while other metals had a non-pollution status according to their ratios of secondary phase to primary phase （RSP）. Results of two assessment methods showed moderate pollution and a very high ecological risk for Cu, Zn, Ni, and Cr at site S7, which might be due to the local sewage treatment plant.

Ghezeljeh nanoclay as a new natural adsorbent for the removal of copper and mercury ions: Equilibrium, kinetics and thermodynamics studies

Heavy metal determination was carried out by applying the solid phase extraction （SPE） method in batch mode followed by atomic absorption spectroscopy （AAS） and inductively coupled plasma atomic emission spectrosco py （ICP-AES） from aqueous solutions using Ghezeljeh montmorillonite nanoclay as a new natural adsorbent. The Ghezeljeh clay is characterized by using Fourier Transform Infrared （FT-IR） Spectroscopy, Scanning Electron Mi- croscopy-Energy Dispersive Spectrometry （SEM-EDS） and X-ray Diffractometry （XRD） and X-ray Fluorescence （XRF）. The results of XRD and FT-IR of nanoclay confirm that montmorillonite is the dominant mineral phase. Based on SEM images of Ghezeljeh clay, it can be seen that the distance between the plates is Nano. The effects of varying parameters such as initial concentration of metal ions, pH and type of buffer solutions, amount of ad- sorbent, contact time, and temperature on the adsorption process were examined. The effect of various interfer- ing ions was studied. The adsorption data correlated with Freundlich, Langmuir, Dubinin-Radushkevich （D-R）, and Temkin isotherms. The Langmuir and Freundlich isotherms showed the best fit to the equilibrium data for Hg（II）, but the equilibrium nature of Cu（ll） adsorption has been described by the Langmuir isotherm. The kinetic data were described with pseudo-first-order, pseudo-second-order and double-exponential models, The adsorp- tion process follows a pseudo-second-order reaction scheme, Calculation of AGσ, △Hσ and ASσ showed that tilenature of Hg（II） ion sorption onto the Ghezeljeh nanoclay was endothermic and was favored at higher temper- attire, and the nature of Cu（II） ion sorption was exothermic and was favored at lower temperature,

E-pH diagram of ZnS-H_2O system during high pressure leaching of zinc sulfide

The values of GΘ,EΘ or pH from 110 to 160℃ were calculated and the relevant potential expressions were obtained.E-pH diagrams of ZnS-H2O system at oxygen partial pressure of 0.8 MPa,ionic activity of 1.0 and different temperatures were drawn through thermodynamical calculation.With the temperature increasing,the stable regions of S and Zn(Ⅱ) in the E-pH diagrams become gradually larger,but the amplification decreases over 150℃.The impacts of leaching parameters,such as temperature,liquid to solid ratio,initial acidic concentration,leaching time,oxygen partial pressure and stirring speed on the leaching rate of Zn(Ⅱ) and conversion rate of S in the single factor of high pressure leaching experiment of ZnS in autoclave,were studied.The leaching residue was examined by X-ray fluorescence(XRF) chemical composition identification and X-ray diffraction(XRD) phase identification,and the content of the leaching solution was tested by inductively coupled plasma-atomic emission spectrometry(ICP).The experimental results indicate that the leaching rate of zinc increases from 60.05% to 97.85% and the conversion rate of sulfur increases from 38.90% to 80.92% with the temperature increasing from 110℃ to 150℃,5:1 of liquid-to-solid ratio,150 g/L of initial acidic concentration,120 min of leaching time,0.8 MPa of oxygen partial pressure,and 480 r/min of stirring speed,which tend to be stable over 150℃.The experimental results correspond with theoretical calculation.

Preparation and Characterization of Tungsten-substituted Molybdophosphoric Acids and Catalytic Cyclodehydration of 1,4-Butanediol to Tetrahydrofuran

A series of tungsten-substituted molybdophosphoric acids(H3PMo12-nWnO40·xH2O) were synthesized and characterized by inductive coupled plasma atomic emission spectroscopy(ICPAES),thermal gravimetry and differential scanning calorimetry(TG-DSC),Fourier transform infrared spectroscopy(FTIR),X-ray diffraction(XRD),and FTIR pyridine adsorption.The as-prepared heteropoly acids have a Keggin type structure.The synthesis of tetrahydrofuran by reactive distillation and cyclodehydration of 1,4-butanediol was studied using the tungsten-substituted molybdophosphoric acids as catalysts.The results of catalytic test indicated that the catalytic activity increased with the increase in the substitution number(n) of tungsten atom in H3PMo12-nWnO40·xH2O and was constant as the substitution number(n) was more than 8.The catalytic activity increased with the increase in the catalyst loading and the selectivity of tetrahydrofuran was nearly 100%.

Enhancing Effect of Fe^(2+) on the Formaldehyde Production from Trimethylamine N-oxide Decomposition Catalyzed by the Extract of Harpadon nehereus Kidney

The effects of Fe2+ on the trimethylamine N-oxide (TMAO) demethylating activity of the Harpadon nehereus kidney extract were studied in this research.The activity of the kidney extract was presumably inhibited by ethylene diamine tetra-acetic acid (EDTA),which indicates that the kidney extract contains an enzyme or enzyme system with metal cations as activator.Activity of the kidney extract was enhanced significantly when Fe2+ was added into the model system in vitro.As the concentration of Fe2+ increased,the decomposing rate of TMAO increased rapidly until TMAO decomposed completely.The activity of the kidney extract was also enhanced by reductant such as ascorbic acid.Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) was employed to determine the content of total iron in a number of fishery products.Significant positive correlation between the contents of total iron and endogenous formaldehyde (FA) was found,especially in marine products.

A Novel γ-Alumina Supported Fe-Mo Bimetallic Catalyst for Reverse Water Gas Shift Reaction

In reverse water gas shift （RWGS） reaction COa is converted to CO which in turn can be used to pro- duce beneficial chemicals such as methanol. In the present study, Mo/AlaO3, Fe/AlaO3 and Fe-Mo/Al2O3 catalysts were synthesised using impregnation method. The structures of catalysts were studied using X-ray diffraction （XRD）, Brunauer-Emmett-Teller （BET） method, inductively coupled plasma atomic emission spectrometer （ICP-AES）, temperature programmed reduction （H2-TPR）, CO chemisorption, energy dispersive X-ray （EDX） and scanning electron microscopy （SEM） techniques. Kinetic properties of all catalysts were investigated in a batch re- actor for RWGS reaction. The results indicated that Mo existence in structure of Fe-Mo/AlzO3 catalyst enhances its activity as compared to Fe/AlaO3. This enhancement is probably due to better Fe dispersion and smaller particle size of Fe species. Stability test of Fe-Mo/AlzO3 catalyst was carried out in a fixed bed reactor and a high CO yield for 60 h of time on stream was demonstrated. Fez（MoO4）3 phase was found in the structures of fresh and used catalysts. TPR results also indicate that Fez（MoO4）3 phase has low reducibility, therefore the Fe2（MoO4）3 phase significantly inhibits the reduction of the remaining Fe oxides in the catalyst, resulted in high stability of Fe-Mo/Al2O3 catalyst. Overall, this study introduces Fe-Mo/Al2O3 as a novel catalyst with high CO yield, almost no by-products and fairly stable for RWGS reaction.

The Influence of Seafloor Hydrothermal Activity on Major and Trace Elements of the Sediments From the South Mid-Atlantic Ridge

Sediment samples obtained from the South Mid-Atlantic Ridge were analyzed for the major and trace elements by inductively coupled plasma atomic emission spectroscopy and inductively coupled plasma mass spectrometry. Results revealed that the contents of elements(e.g., Fe, Mn, Cu, Zn, V, Co) were high in samples 22V-TVG10 and 26V-TVG05 from the sites near the hydrothermal areas, and low in sample 22V-TVG14, which was collected far from the hydrothermal areas. The contents of Ca, Sr and Ba in the samples showed opposite trends. A positive correlation between the concentrations of metallic elements(Cu, Zn, Co, Ni, Pb, V) and Fe in the samples were observed. These results are consistent with chemical evolution of the dispersing hydrothermal plume.

Influence factors on activity of Ru–Zn catalysts in selective hydrogenation of benzene

Selective hydrogenation of benzene is an atom economic green route to produce cyclohexene. The control of Zn species is the key to the catalytic performance of Ru–Zn catalysts. The influences of ZnO crystals on selective hydrogenation of benzene were explored. A series of Ru–Zn catalysts with different Zn contents and ZnO morphologies were prepared by changing the amount of NaOH in the co-precipitation process. The catalysts were characterized by N_2 physisorption, X-ray powder diffraction(XRD), inductively coupled plasma optical emission spectrometer(ICP-OES), scanning electron microscope(SEM), temperature-programmed reduction(H_2-TPR)and Malvern laser particle size analyzer. It is found that with increasing the amount of NaOH, the Zn content first increased then decreased, and the ZnO crystals changed from relatively thicker pyramidal-shaped crystals to slimmer needle-shaped crystals. The catalyst had the highest Zn content(22.1%) and strongest interaction between ZnO crystals and Ru particles at pH 10.6 of the solution after reduction. As a result, it had the lowest activity. The activity of Ru–Zn catalysts is affected by both the Zn content and the interaction between ZnO crystals and Ru particles. The effect of reduction time was also investigated. Prolonging the reduction time caused no significant growth of ZnO crystals but the aggregation of catalyst particles and growth of Ru nanocrystals, thus resulting in the decrease of catalytic activity.

Silica-gel Supported V Complexes： Preparation, Characterization and Catalytic Oxidative Desulfunzation

In this manuscript, a series of catalyst SG n-[VVO2-PAMAM-MSA] (SG silica gel, PAMAM polyamidoamine, MSA 5-methyl salicylaldehyde, n=0, 1, 2, 3) was prepared and their structures were fully characterized by Fourier transform-infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS) and inductive coupled plasma emission spectrometer (ICP) etc. XPS revealed that the metal V and SG n-PAMAM-MSA combined more closely after the formation of Schiff base derivatives. Their catalytic activities for oxidation of dibenzothiophene were evaluated using tert-butyl hydroperoxide as oxidant. The results showed that the catalyst SG 2.0-[VVO2-PAMAM-MSA] presented good catalytic activity and recycling time. Meanwhile, the optimal condition for the catalytic oxidation of SG 2.0-[VVO2-PAMAM-MSA] was also investigated, which showed that when the oxidation temperature was 90 °C, time was 60 min, the O/S was 3:1, and the mass content of catalyst was 1%, the rate of desulfurization could reach 85.2%. Moreover, the catalyst can be recycled several times without significant decline in catalytic activity.

Adsorption of Chromium （Ⅵ） from Aqueous Solution Using Zeolite/Chitosan Hybrid Composite

This study investigated the adsorption ability of ZCHC （zeolite/chitosan hybrid composite） as adsorbent for chromium （Cr（Ⅵ））, ZCHC was prepared with sol-gel method by mixing zeolite and chitosan. Adsorption experiment from aqueous solutions containing known amount of Cr（Ⅵ） using zeolite, chitosan and ZCHC was explored to evaluate the efficiency of ZCHC as adsorbent for Cr in a batch system. The amount of Cr（Ⅵ） adsorbed at different pH values, initial concentrations, adsorbent dosages, and contact times were determined by ICP-AES （inductively coupled plasma-atomic emission spectrometry） in order to determine the optimum conditions for Cr（Ⅵ） adsorption. Furthermore, the adsorption mechanism of Cr（Ⅵ） by zeolite, chitosan and ZCHC was investigated by applying Langmuir and Freundlich isotherm equations to the data obtained. In addition, the rates of adsorption were found to conform to pseudo-second order kinetics.

Heavy metals accumulation effect in rabbit body fluids after smoking

Concentration of heavy metals in blood and urine of rabbit after inhaling three different kinds of cigarette was studied through the animal passive smoking pattern. The samples were prepared by nitric acid solution digestion and determination of seven kinds of heavy metals including Hg, Se, Sn, Pb, Cd, Ni and Cr was performed by inductively coupled plasma-atomic emission spectrometry （ICP-AES）. The ICP-AES method was established with good precision and accuracy, relative standard deviation （n=6） was between 2.9% and 5.9%, and the recovery was in the range of 95.0%-104.2%. Concentration of six heavy metals increases in some extent in blood and urine after period of smoking and the increasing of heavy metals in blood and urine all shows time dependence. Significantly higher heavy metal levels are observed in the blood and urine of the cigarette inhaling rabbits in the exposed group. The concentration of six kinds of heavy metals in the blood of the rabbit increases after 16 weeks exposing to cigarette smoking. Three times of rig, ten times of Se and trace amount ofPb, Cd, Ni and Cr are detected in the blood after 16 weeks of smoking. For urine samples, about three times of Hg, two times of Se, five times of Pb and trace amount of Cd are detected after 16 weeks of inhalation of cigarette. Comparatively, higher concentration of heavy metals are detected after inhaling of Nise cigarette.