电感耦合等离子体发射光谱法测定生物样品中铁、钙、镁、磷、钾、钠

本文介绍了电感耦合等离子体发射光谱法测定生物样品中Fe、Ca、Mg、K、Na、P等元素的分析方法,参加了国家植物标准物质定值,结果令人满意。

含云母铁尾矿的工艺矿物学研究

铁尾矿储量大,长期堆放会造成环境污染,但是铁尾矿中有价金属含量多,具有重要的回收利用价值。本研究针对某含云母铁尾矿,采用HYDRO2000M-MU激光粒度仪、XRF、XRD、MLA、电子探针等,系统地研究了其中铁、钾的赋存状态。粒度、成分及嵌布特性等分析结果表明:矿物中含有氧化物、硫化物、硅酸盐和磷酸盐,矿物中铁的含量为12.48%,有两种赋存状态,一种是以独立矿物的形式存在,另一种是以类质同象的形式存在。矿物中钾的含量为0.62%,主要以独立矿物的形式存在。本工艺矿物学研究可为含云母铁尾矿的后续处理与回收利用提供参考。

Relationship and effect of redox potential,jarosites and extracellular polymeric substances in bioleaching chalcopyrite by acidithiobacillus ferrooxidans

The changes of pH,redox potential,concentrations of soluble iron ions and Cu^2＋ with the time of bioleaching chalcopyrite concentrates by acidithiobacillus ferrooxidans were investigated under the different conditions of initial total-iron amount as well as mole ratio of Fe（III） to Fe（II） in the solutions containing synthetic extracellular polymeric substances （EPS）.When the solution potential is lower than 650 mV （vs SHE）,the inhibition of jarosites to bioleaching chalcopyrite is not vital as EPS produced by bacteria can retard the contamination through flocculating jarosites even if concentration of Fe（III） ions is up to 20 g/L but increases with increasing the concentration of Fe（III） ions;jarosites formed by bio-oxidized Fe3＋ ions are more easy to adhere to outside surface of EPS space on chalcopyrite;the EPS layer with jarosites acts as a weak diffusion barrier to further rapidly create a high redox potential of more than 650 mV by bio-oxidizing Fe^2＋ ions inside and outside EPS space into Fe^3＋ ions,resulting in a rapid deterioration of ion diffusion performance of the EPS layer to inhibit bioleaching chalcopyrite severely and irreversibly.

Control method of chalcopyrite passivation in bioleaching

Passivation is a common phenomenon on the surface of chalcopyrite in the process of bioleaching. The ordinary leaching and strengthening leaching by adding glass beads were carried out. The results show that the passivation of chalcopyrite was greatly weakened in strengthening leaching due to the change of leaching conditions. The copper leaching efficiency was increased from 50% to 89.8% through adding beads. The SEM and X-ray diffraction （XRD） analyses illustrate that there are few jarosite precipitates and weak passivation on the surface of chalcopyrite in strengthening leaching. In contrast, there are thick and compact jarosite precipitate and obvious passivation in ordinary leaching, which hinders further dissolution of chalcopyrite.

Environmentally benign and economic synthesis of covalent triazine-based frameworks

Covalent triazine-based frameworks（CTFs） are important microporous materials with a wide range of applications.Here,we demonstrate an environmentally benign and economic synthetic pathway to CTFs.The monomers used for CTFs,aromatic nitriles,were obtained by cyanation using nontoxic potassium hexacyanoferrate（Ⅱ） in place of commonly used toxic cyanides.Then,the CTFs were synthesized by trimerization of the corresponding cyano monomers in molten zinc chloride.A series of CTFs was synthesized,and the highest Brunauer-Emmett-Teller surface area measured in this series was 2404 m^2/g.Among the synthesized CTFs,CTF_（DCP） exhibited excellent CO_2 adsorption properties,with a CO_2 uptake of 225 mg/g at 0℃.

Preparation of potassium chromate by roasting of carbon ferrochrome

The oxidizing roasting process of carbon ferrochrome to prepare potassium chromate in the presence of potassium carbonate and air was investigated. The effects of reaction temperature, reaction time, mole ratio of potassium carbonate to carbon ferrochrome were studied, and thermodynamics and kinetics were also discussed. It was observed that the reaction temperature and reaction time had a significant influence on the roasting reaction of carbon ferrochrome. The reaction mechanism changed greatly as the temperature varied. A two-stage roasting process was favorable for the roasting reaction, and a chromium recovery rate of 97.06% was obtained through this two-stage roasting method. The chromium residue yielded from this method was only 1/3 of the product. Moreover, the component of Fe in the residue was as high as 55.04%. Therefore, it can be easily recovered to produce sponge iron, realizing complete detoxication and zero-emission of chromium residue.

Bioleaching and electrochemical property of marmatite by Sulfobacillus thermosulfidooxidans

Bioleaching and electrochemical experiments were conducted to evaluate marmatite dissolution in the presence of pure S.thermosulfidooxidans.The effects of particle size,p H controlling and external addition of Fe^3＋ ions on the zinc extraction were investigated.The results show that in the bioleaching process the best particle size range is 0.043-0.074 mm and adjusting p H regularly to the initial value has a profound effect on obtaining high leaching rate.External addition of Fe^3＋ ions could accelerate the bioleaching,while the concentration of additional Fe^3＋ over 2.5 g/L weakens the positive effect,and even hinders the dissolution of marmatite.SEM and XRD analyses of the leaching residues reveal that a product layer composed of elemental sulfur and jarosite is formed on the mineral surface,which results in a low leaching speed at later phase.The results of electrochemical measurements illustrate that additional Fe^3＋ ions could increase the corrosion current density,which is favorable to zinc extraction.The EIS spectra show that rate-limiting step does not change when Fe^3＋ ions are added.

Determination of Ca,K,Mg and Fe in Four Fish Species by FAAS

A method for determining calcium （Ca）, potassium （K）, magnesium （Mg） and iron （Fe） in four fish species was opti- mized and validated. It included microwave mineralization of the samples and subsequent quantification by flame atomic absorption spectroscopy （FAAS） with Zeeman-effect background correction. Using HNO3 （65%） and H202 （33%） as extraction solutions, the optimal conditions of extraction were established as follows： 0.5 g of sample mass; microwave time program of 300 W/5 min and 600 W/5 min. The method was free of matrix interferences. The linear correlation coefficients were ≥0.9991, the recovery percentage of analytes was from 99.31% to 103.70% and the RSD （relative standard deviation） was lower than 2.06%. The detection limits obtained were 32.3, 43.2, 14.0 and 68.6ng mL^-1 for Ca, K, Mg and Fe in FAAS respectively. It is shown that the method is rapid, simple, sensitive and accurate. The method was applied to the studies of digestibility and measurement of these nutrients in samples of fish collected from Norway, Japan and China.

Transformation of iron in pure culture process of extremely acidophilic microorganisms

Jarosite and extracellular polymer substance generated during pure culture and bioleaching process have been widely accepted the main transformation of decreasing iron in the medium.In the present work,acidophilus bioleaching organisms Ferroplasma thermophilum,Leptospirillum ferriphilum and Acidithioobacillus ferrooxidans were cultured.It was found that they can live in low pH environment,and more than10particles in each cell intracellular nano-particles are synthesized in the cells.By analyzing the morphology and chemical composition of nano-particles,they were found to contain iron,and the three microorganisms belonged to high-yielding strains.The results show that the transformation of the decreasing iron ions is not only generating jarosite,but also taken into cells and synthesizing ferruginous nano-particles.

Physical Properties and Electrochemical Performance of Solid K_2FeO_4 Samples Prepared by Ex-situ and in-situ Electrochemical Methods

K2FeO4 powders were synthesized by the ex-situ and in-situ electrochemical methods, respectively, and characterized by infrared spectrum （IR）, scanning electron microscopy （SEM）, X-ray powder diffraction （XRD） and BET. Their electrochemical performances were investigated by means of galvanostatic discharge and electrochemi-cal impedance spectroscopy （EIS）. The results of physical characterization showed that the two samples have simi-lar structural features, but their surface morphologies and oriented growth of the crystals are different, which results in smaller specific surface area and lower solubility of the ex-situ electrosynthesized K2FeO4 sample. The results of discharge experiments indicated that the ex-situ electrosythesized K2FeO4 electrode has much larger discharge ca-pacity and lower electrode polarization than the in-situ electrosynthesized K2FeO4 electrode. It was found from the results of EIS that lower electrochemical polarization might be responsible for the improvement on the discharge performance of the ex-situ electrosynthesized K2FeO4 electrode.

Formation of jarosite and its effect on important ions for Acidithiobacillus ferrooxidans bacteria

The precipitation of jarosite adversely affects the bio-leaching of copper sulfides in the Sarcheshmeh heap bio-leaching process. The variables of the initial concentration of ferrous iron in the growth medium, pH, and temperature were examined in the laboratory to determine how they affect the precipitation of jarosite in the presence of Acidithiobacillus ferrooxidans bacteria. It was found that the maximum ferric precipitate occurred at a ferrous sulfate concentration of 50 g/L, a temperature of 32 ℃, and an initial pH value of 2.2. The effects of the precipitation of ferric iron on the quantities of ions that are important for A. ferrooxidans bacteria in aqueous phase, i.e., ferric, sulfate, potassium, phosphate, and magnesium ions, also were assessed. The results showed relatively similar patterns for the ferric and potassium ions, and then reason might have been the co-precipitation of these ions as constituent elements of jarosite mineral. At pH values greater than 1.6, the solubility of phosphate ions decreased dramatically due to the co-precipitation of phosphate ions with the jarosite precipitate and due to the significant growth rate of A. ferrooxidans bacteria in this pH range. Due to the dissolution of a gangue constituent in the ore, the magnesium levels increased in the first few days of the bio-leaching process;thereafter, it decreased slightly.

Benzohydroxamic acid to improve iron removal from potash feldspar ores

The technological mineralogy of the potash feldspar was investigated and a new collector named Yb105 was adopted to remove iron from potash feldspar ores.The technological mineralogy results indicate that the main components of the ore were feldspar,sericite,quartz and kaolinite,and iron mainly existed in limonite and hematite,most of which can be removed by beneficiation.The results show the benzohydroxamic acid can not only increase the recovery of iron and reduce the consumption of oleic acid collector,but also enhance the collecting performance of oleic acid at low temperature,which can realize the flotation of the ores at a low temperature and play an important role in saving energy to some extent.Compared with oleic oil,the benzohydroxamic acid had a great advantage in removing iron from potash feldspar,a potash feldspar concentrate with Fe grade of 0.23%,K2O grade of 12.59%and Na2O grade of 0.26%was obtained by flotation with Yb105 as collector,and the yield of the concentrate was 82.55%.

Acid Release from an Acid Sulfate Soil Sample Under Successive Extractions with Different Extractants

An acid sulfate soil sample was successively extracted with deionized water, 1 mol L-1 KCl and 0.000 5 mol L-l Ca(OH)2 solutions. The results showed that only very small amounts of acidity were extracted by deionized water, possibly through slow jarosite hydrolysis. Acid release through jarosite hydrolysis was greatly enhanced by Ca(OH)2 extraction at the expense of the added OH- being neutralized by the acid released. Successive extraction of the sample with KCl removed the largest amounts of acidity from the sample. However, it is likely that the major form of acidity released by KCl extraction was exchangeable acidity. The results also show the occurrence of low or non charged Al and Fe species in water and Ca(OH)2 extracts after first a few extractions. It appears that such a phenomenon was related to a decreasing EC value with increasing number of extractions.

Bioleaching of pyrrhotite by Sulfobacillus thermosulfidooxidans

The bioleaching of pyrrhotite was investigated using Sulfobacillus thermosulfidooxidans.The effects of pH,pulp concentration,inoculation amount,external addition of ferrous and ferric ions were examined.The pH is found to exert a profound effect on the leaching process for controlling the bacterial activity and precipitation of ferric ions mainly as jarosite.The results show that low pulp content increases the leaching rate of iron.The inoculation amount from 1×107 cell/mL to 1×108 cell/mL has positive effects on the leaching rate.The results also imply that addition of ferrous sulfate(1 g/L) is required for the bacteria to efficiently drive the extraction of iron,however,the leaching efficiency has no obvious enhancement when 2 g/L ferrous sulfate was added.Comparatively,addition of ferric sulfate(2 g/L) significantly inhibits the bioleaching process.At the end of bioleaching,jarosite and sulfur are observed on the surface of pyrrhotite residues by using XRD and SEM.With the passivation film formed by jarosite and sulfur,the continuous iron extraction is effectively blocked.

Oxidative Desulfurization of Model Sulfur Compound by Potassium Ferrate in the Presence of Phosphomolybdic Acid Catalyst

In this work, the removal of thiophene from simulated oil has been studied by using the adsorption, extraction and oxidation/adsorption methods, respectively. In the adsorptive desulfurization process, different commercial adsorbents were used to eliminate thiophene at ambient pressure and mild temperature, and the results showed that carbon powder had the best adsorption ability. In the extractive desulfurization process, the best desulfurization result was obtained when DMF is used. In the oxidative/adsorptive desulfurization procedure using synthesized potassium ferrate as the oxidant and phosphomolybdic acid solution as the catalyst, thiophene was oxidized and removed from hydrocarbons in combination with active carbon adsorption, and the residual sulfur content of simulated oil could be reduced to 15.3mg/L from the original level of 200mg/L, with the desulfurization rate reaching 92.3%.

Thermal Decomposition of Potassium Titanium Hexacyanoferrate(Ⅱ) Loaded with Cesium in a Fixed Bed Calciner

The thermal decomposition of potassium titanium hexacyanoferrate（ Ⅱ ） （KTiFC） loaded with cesium （referred to as Used Exchanger,or UE） was-studied at different flow rate of air in a fixed bed calciner. The calcina t ign processconsisted of four stages：ambient temperature- 180℃ （stageⅠ ）, 180-250℃（stage Ⅱ）, 250-400℃ （stage Ⅲ）, and constant 400℃ （stage Ⅳ）.The most intense reaction occurred in stage .Ⅱ. The rate of thermal decomposition was controlled, depending on the O2 flux, by O2 or CN concentration in ditterent stages. Results from differential thermal analysis （DTA） showed that the calcination reaction of the anhydrous UE was exothermic, with an approximate heat output of 4.6kJ·g^-1, which was so large to cause the possible agglomeration of calcined residues. The agglomeration could be avoided by enhancing heat transfer and controlling the O2 flux. It was found that there was no cyanides in the calcined residues and no CN-bearing gases such as HCN and （CN）2 in the off-gas. It seemed that the catalytic oxidation furnace behind the fixed bed calciner could be cancelled.

电感耦合等离子体发射光谱法同时测定无机复混肥料中的7种元素

本文建立了稀盐酸分解、电感耦合等离子体发射光谱法(ICP-OES)同时测定无机复混肥料样品中7种元素的分析方法。各元素检出限结果为:磷0.036μg/mL、钙0.104μg/mL、镁0.116μg/mL、钾0.097μg/mL、钠0.107μg/mL、铁0.115μg/mL、硫0.050μg/mL。该方法快速且操作简单,准确度、精密度均满足要求,适合推广运用于大批量无机复混肥料样品中磷、钙、镁、钾、钠、铁和硫元素的快速分析。

Bioleaching of chalcopyrite by Leptospirillum ferriphilum

Chalcopyrite oxidation rates were examined under various conditions in the presence of Leptospirillum ferriphilum,in which the effects of different pulp content,inoculation amount,external addition of Fe3+ and initial pH value were studied.The bioleaching residues were investigated by X-ray diffractograms(XRD),scanning electron microscopy(SEM) and energy dispersion spectrum(EDS) analysis.The results show that low pulp concentration increases the leaching rate of copper,and external addition of Fe3+ is also beneficial to leaching chalcopyrite.The changes of inoculation amount and initial pH from 1.6 to 2.5 have a little effect on the final leaching rate.The results also imply that Fe3+ ions are important for bioleaching of chalcopyrite.At the end of bioleaching,jarosite and sulfur are observed on the surface of chalcopyrite residues by using XRD,SEM and EDS.With the passivation layer formed by jarosite and sulfur,the continuous copper extraction is effectively blocked.

Spatial Differentiation of Elements in Soils on Red-Earthy Hill Landscape of Central China

Samples of 21 soil profiles and 165 top soils from an area of approximate 1.5km^2 on red-earthy hill landscape were collected and analysed.The content of Ca,Mg,K,P,Fe,Mn,Zn and Cu in soils relate with the kind of parent material and the position of topography,however,there is great variation due to the local difference of the form of soil utilization.From the difference in spatial distribution of elements content,it is believed that eight kinds of elements are lost by chemical leaching and physical translocation,meanwhile some are added (such as Ca,P,K,Mg) and some mobilized (such as Fe,Mn,Zn,Cu and P) through cultivation,fertilization and irrigation in the soils on the landscape investigated.The sectional differentiation in abundance or deficiency of elements in top soils on the landscape investigated is distinct,which is important for carrying out agricultural management and reasonable fertilization according to local conditions.

Preparation of jarosite by Acidithiobacillus ferrooxidans oxidation

The formation ofjarosite in the presence of Acidithiobacillusferrooxidans （A. ferrooxidans） was researched to ascertain the conditions of producing minimum precipitation. The effects of salt concentration and pH on the characteristics ofjarosite formed in K2SO4/（NHa）2SOa-FeSO4 inorganic salt solution and 9K medium were studied by using the measurements of scanning electron microscope, X-ray diffraction, Fourierism transform infrared analysis, thermogravity/differential thermogravity analysis and particle size analysis to evaluate the product. The results indicate that the formation of jarosite begins when A. ferrooxidans reaches logarithmic growth phase in 9K medium, and a higher pH value is beneficial to the formation of jarosite. The jarosite formed in 9K medium has smaller and more concentrative particle size and smoother surface than that formed in inorganic salt solution.