电感耦合等离子体原子发射光谱(ICP-AES)测定米粉、饼干、粉条、油条中的铝

铝是一种低毒的金属元素,不会导致人体急性中毒,但是食品中铝元素含量超过一定量就会对人体造成危害。

电感耦合等离子体原子发射光谱分析仪器与方法的新进展

电感耦合实现的等离子体发射广谱技术,实现了数字化垂直感应检测应用。通过高新能的计算分析,强化功能的图谱拟定设计。在高通量自动化配置技术分析中,通过高效节能环保设计理念,确定图谱的分辨率和稳定分析,提高整体应用性能水平。

微波消解-ICP-AES同时测定黄芪中10种微量元素

用硝酸和过氧化氢作为消解剂,微波消解技术处理黄芪样品,建立了微波消解-电感耦合等离子体发射光谱法(ICP-AES)同时测定黄芪中K、P、Ca、Mg、Fe、Sn、Mn、Cu、Zn和Cr等10种微量元素含量的方法。通过对样品微波消解条件和ICP-AES工作参数进行了优化,测定了各元素的分析线性、检出限、精密度和回收率等。各测试元素的校准曲线均具有良好的线性关系,检出限符合分析要求;以西红柿叶标准样品EPS-1验证,测得方法回收率为89.7%—112.8%,相对标准偏差(RSD)<5.0%;黄芪样品的加标回收率为90.4%—107.0%,RSD<5.0%。该方法具有良好的准确度和精密度,且具有快速、高效等特点。测定结果表明,黄芪中富含有K、P、Ca、Mg、Fe和Sn等元素,并据此对黄芪中富含的各元素与其特殊药理功效的关系做了初步讨论。

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.

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.

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%.

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.

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.

Facile synthesis of Zn_2GeO_4 nanorods toward improved photocatalytic reduction of CO_2 into renewable hydrocarbon fuel

Zn2GeO4 nanorods were prepared by a surfactant-assisted solution phase route.The as-prepared products were characterized by X-ray powder diffraction(XRD),scanning electron microscopy(SEM),high-resolution transmission electron microscopy(HRTEM),inductively coupled plasma atomic emission spectrometer(ICP-AES),UV-vis diffuse reflection spectroscopy and photoluminescence(PL) spectroscopy.The possible formation mechanism of Zn2GeO4 nanorods was discussed.It was supposed that the CTA+ cations preferentially adsorb on the planes of Zn2GeO4 nanorods,leading to preferential growth along the c-axis to form the Zn2GeO4 rods with larger aspect ratio and higher surface area,which showed the improved photocatalytic activity for photoreduction of CO2.The photoluminescence(PL) property of Zn2GeO4 nanorods was investigated through the emission spectra.

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.

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.

Preparation and Characterization of Magnetic Resin Made from Chitosan and Cerium

In this study, the water-based ferromagnetic fluid and magnetic resin made from chitosan and cerium complex （MRCCC） were successfully prepared by using the chemical co-precipitation technique and by the reversed-phase suspension cross-linking polymerization. MRCCC presented uniform and narrow panicle size distribution as determined by the Laser Panicles Sizer. The Inductively Coupled Plasma-Atomic Emission Spectrometry （ICP-AES）, Fourier transform infrared spectroscopy （FT-IR）, differential scanning calorimetry （DSC） and X-ray powder diffraction （XRD） study demonstrated that there were iron and cerium existing in MRCCC. The movement of MRCCC under magnetic field proved its magnetic property. The swelling kinetics in water or solutions with different pH indicated that MRCCC could be applied in solutions with pH greater than 1.0. The ferromagnetic fluid particles were stable in MRCCC soaked in solutions with pH 〉2.0. In view of these results, MRCCC can be used as material for separation, clarification, adsorption, sustained release and hydrolysis activity.

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.

Dissolution behavior of calcium-magnesium-silicate glass fiber

The dissolution behavior of CaO-MgO-SiO2 glass fiber was investigated by scanning electron microscopy （SEM）, Fourier-transform infrared spectrometer （FTIR） and inductively coupled plasma atomic emission spectroscopy （ICP-AES） using in-vitro tests. The results show that the soaked fiber is surrounded by an outer calcium-magnesium silicate hydrated layer, and there exists a balancing fimction between the formation and abscission of the hydrated layer during the dissolution process. The concentrations of leached ions increase constantly, and the mass loss of the fibers and pH changes of the solution are found to rise rapidly during the initial dissolution process, then their increasing rates are controlled by the balancing function of the hydrated layer at the subsequent dissolution stages. The dissolution rate constant and time for complete dissolution are estimated to be 274 ng/（cm2.h） and 15.2 d, respectively, presenting preferable biosolubilities.

Analysis of Cadmium in Water Extracts from Contaminated Soils with High Arsenic and Iron Concentration Levels

Cadmium （Cd） concentrations in the water extracts of ten contaminated soils by arsenic （As） with various iron （Fe） contents were measured using inductively coupled plasma atomic emission spectrometry （ICP-AES） and electrothermal atomic absorption spectrometry （ETAAS）, Due to the potential spectral interferences of As and Fe in the quantification of Cd, two methods were used for the background compensation. The first method was based on the use of a deuterium lamp （BGCD2 mode）. The second one required a Cd hollow cathode lamp pulsated with a current for which the intensity varies in the course of time （BGCSR mode）. The results showed that the choices of the analytical technique and the method used for the background compensation depend on the Cd, As and Fe concentrations in the solution and the concentration ratios As/Cd or/and Fe/Cd. In comparison with the ICP-AES and the ETAAS in combination with the BGCD2 mode, it was shown that the high-speed self-reversal method （HSSR） was a more appropriate method to correct As and Fe spectral interferences during the Cd measurements. On the other hand, depending on the Cd concentration, it was established that no significant Fe interference occurred during the Cd determination even if Fe concentration was 50 mg/L, reflecting the efficiency of the HSSR method to overcome the Fe interferences in the determination of Cd concentration by ETAAS without any matrix modifier in water extracts.

Composition of Pig Manures and Wastewaters under the Gan Qing Fen System in China

A large scale pig farm located in the North West of Beijing that applies the gan qing fen manure management system was selected and a continuous sampling of manures and wastewaters was performed from June to October 2009. Samples were collected once a week based on the pig production cycle, namely gestation, farrowing, weaning and fattening. Analysis of nutrients and heavy metals were determined by means of Inductively Coupled Plasma Atomic Emission Spectroscopy （ICP）. Total Nitrogen （TN） was determined by the Kjeldahl method. The main results showed that pig manures were characterized by high nutrients and heavy metals contents that might be due to the solid fraction separation from the liquid fraction under the gan qing fen manure management system. Further, piggery wastewaters were characterized by very low concentrations of nutrients and heavy metals as result of their dilution with flushing water mainly used for cleaning the pigsties. Manure and wastewaters samples from weaning pigs contained the highest concentrations of nutrients and heavy metals that could be due to high supplementation rates of these minerals in the weaner diets. In general, it seems that the manual daily collection of pig manures in the gan qing fen system is an efficient practice in order to maintain nutrient contents in pig manures but the use of flushing water should be reduced as it can lead to further environmental pollution.

Structure Analysis of Polyacrylonitrile Polymerized in Ionic Liquids

Polyacrylonitriles （PANs） ware synthesized both by atom transfer radical polymerization （ATRP） anti free radical polymerization in ionic liquid 1 - buty - 3 - methylimidazolium chloride （[bmim]Cl）. [bmim]Cl demonstrates to be a preferable solvent for ATRP of acrylonitrile （AN）. The polymerization maintains the usual advantages of ATRP with molecular weight agrees well with theoretical value and low polydispersity （PDI = 1.15）. It is also shown the higher conversion and lower molecular weight dispersion in ionic liquid than in dimethylformamide （DMF）. From FTIR and NMR analysis, it is confirmed that the chemical structures of PANs synthesized in [bmim]Cl were identical with that obtained in DMF. In atom transfer radical polymerization, the methine and cyan carbon atoms in isotactic configuration for PAN produced in [bmim] Cl have a configuration consisting of about 55.5% isotactic diads. It is higher than that obtained in DMF which is 52.2%. So, ionic liquid has effect on the stereostructure of PANs. Further analysis of ^13C NMR spectra indicated that the isotacticity of PAN synthesized by free radical polymerization was lower than that of PAN prepared by ATRP, although both of them were random in stereoregularity. Besides the pentad tacticities of PANs also suggested that the sequence distributions of them all obey Bernoulli statistics.

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,

Mineral Constituents in Common Chanterelles and Soils Collected from a High Mountain and Lowland Sites in Poland

This paper reported the results of the determination of Ag, A1, Ba, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, P, Pb, Rb, Sr and Zn in Common Chanterelles （Cantharellus cibarius） Fr. and surface soil layer （o-io cm） underneath the fruiting bodies. Mushrooms and soils were collected from a lowland site in the Hel Peninsula （Baltic Sea coast） and a high mountain site in the Tatra Mountains. The trace elements were determined using validated method and inductively coupled plasma - atomic emission spectroscopy （ICP-AES）. Common Chanterelles that emerged at sites poor in mineral nutrients podzols of the Hel Peninsula forests efficiently bioeoncentrated several essential trace elements （K, P, Co, Cu, Mn, Na, Zn）, while the abundance of those elements in carpophores was around half less compared to specimens from Zakopane region and which emerged in soils much richer in minerals. Common Chanterelles collected at two spatially distant background areas in Poland were only weakly contaminated with metals such as Ag, Cd, Hg and Pb. The maximum tolerable Cd and Pb contents of certain cultivated mushrooms are regulated in the European Union by law and these hazardous metals in C. cibarius were far below tolerance limits set.

Synthesis, characterization of triphenyltin grafted on SBA-15mesoporous silica and its catalytic performance for the synthesis of 4-methylacetophenone

The production of Ph3Sn–O–SBA-15(Ph3Sn SBA)was achieved by heating triphenyltin chloride and SBA-15in N-methylpyrrolidone at 190°C for 5 h using triethylamine as a catalyst.The composition,structure,and surface physical and chemical properties of Ph3Sn SBA were characterized using inductively coupled plasma-atomic emission spectroscopy(ICP-AES),13C,119Sn and29Si solid-state nuclear magnetic resonance(NMR)spectroscopy in situ pyridine infrared spectroscopy(Py-IR),N2adsorption–desorption isotherms,X-ray diffraction(XRD)and transmission electron microscopy(TEM).The results of ICP-AES and organic elemental analysis showed that the grafting yield of Sn was 17%(by mass)for Ph3Sn SBA.The elemental analysis and solid-state NMR results for Ph3Sn SBA were consistent with grafting of triphenyltin on SBA-15.The N2adsorption–desorption,XRD and TEM analyses showed that Ph3Sn SBA retained an ordered hexagonal mesoporous structure,resulting in decreases in the surface area,pore size and mesopore volume,and an increase in acidity as compared with SBA-15.The Hammett acidity function(H0)value and the number of acid sites for Ph3Sn SBA,obtained by the Hammett methods,were 2.77–3.30 and 2.07 mmol·g-1,respectively.The Friedel–Crafts acylation of toluene and acetic anhydride over Ph3Sn SBA was investigated.The yield of methylacetophenone(MAP)and the selectivity for 4-methylacetophenone(PMAP)were 79.56%and 97.12%,respectively,when the conditions were n(toluene):n(anhydride)=2.0:1.0 with 6%(by mass)catalyst,and heating under reflux for 5 h.The PMAP selectivity still reached 93.11%when Ph3Sn SBA was used for the fifth time under the same reaction conditions.