Separation/preconcentration of trace heavy metals in urine, sediment and dialysis concentrates by coprecipitation with samarium hydroxide for atomic absorption spectrometry

Multi-element determination of trace elements in urine and dialysis solutions by atomic absorption spectrometry has been investigated. Coprecipitation with samarium hydroxide was used for preconcentration of trace elements and elimination of matrix elements. To 10 ml of each sample was added 500 μl of 2 mg ml⁻¹ samarium solutions; the pH was then adjusted to 12.2 in order to collect trace heavy metals on samarium hydroxide. The precipitate was separated by centrifugation and dissolved in 1 ml of 1 mol l⁻¹ HNO₃. Coprecipitation parameters and matrix effects are discussed. The precision, based on replicate analysis, is around 5% for the analytes, and recovery is quantitative, based on analysis of spiked samples and solutions including matrix components. The time required for the coprecipitation and determination was about 30 min.     

碳酸钙共沉淀原子吸收法测定天然水中锶

采用CaCO3共沉淀富集天然水中痕量锶后，再用空气-乙缺焰原子吸收法测定，使方法灵敏度提高一个数量级。本法简便，准确，最低检出限达0.0012mg/L。对0.10mg/L的锶水样，十次测定的标准偏差为0.0082，相对标准偏差为8.2%。     

Solid phase extraction vis-à-vis coprecipitation preconcentration of cadmium and lead from soils onto 5,7-dibromoquinoline-8-ol embedded benzophenone and determination by FAAS

This article compares the solid phase extraction (SPE) and coprecipitative preconcentration of cadmium and lead from dilute aqueous solutions as a function of pH and weight of chelating agent. SPE enriches cadmium and lead over a wider pH range (6.0-8.0) and requires lower weight of DBQ chelate embedded benzophenone. Among the quinoline-8-ol and its dihaloderivatives, DBQ embedded benzophenone allows quantitative enrichment over a wide pH range (6.0-8.0) for both cadmium and lead unlike DCQ (∼6.5 for Cd and 6.5-7.0 for Pb), DBQ was preferred. The calibration plots were rectilinear over the concentration range of 0.1-50 and 2.5-200 μg l⁻¹ of cadmium and lead with detection limits of 0.1 and 2.0 μg l⁻¹, respectively, which are 400 times lower than the direct FAAS method. The precision of the developed procedure is good as it provides relative standard deviation values of 2.20 and 2.45% during five replicate determinations of 2 and 25 μg l⁻¹ of cadmium and lead, respectively. The accuracy of the developed procedure was tested by analyzing certified reference materials (CRM's) of soil and marine sediment samples supplied by IAEA, Italy and NRC, Canada, respectively. Furthermore, the developed procedure has been successfully used for the speciative determination of cadmium and lead in soil samples collected from the vicinity of industries in India.     

镁铝氢氧化物正电溶胶结构研究

镁铝氢氧化物正电溶胶结构研究韩书华，张春光，侯万国，孙德军，王果庭（山东大学胶体与界面化学研究所，济南，２５０１００）关键词镁铝氢氧化物，正电溶胶，共沉淀镁铝氢氧化物是一种层状的氢氧化物。Ｂｕｒｂａ等［１］提出将镁铝氢氧化物与钠质蒙脱土作用可得到抑制...     

Sintering behavior and apatite formation of diopside prepared by coprecipitation process

Sintering behavior and bioactivity of diopside, CaMgSi₂O₆, prepared by a coprecipitation process were examined for its biomedical applicability. As-prepared powder was synthesized by adding aqueous ammonia to an ethanol solution containing Ca(NO₃)₂·4H₂O, Mg(NO₃)₂·6H₂O, and Si(OC₂H₅)₄ and characterized by means of TG–DTA, XRD, and TG–MS. The dried powder was X-ray amorphous and crystallized into diopside at 845.5 °C. The glass network formation by SiO₄ tetrahedra was almost completed below 800 °C. The bioactivity of the diopside prepared by sintering the compressed powder at 1100 °C for 2 h was evaluated by immersion of the sintered body in a simulated body fluid (SBF) at 36.5 °C. Leaf-like apatite particles were found to be formed on the surface of the sintered body and grew with passage of soaking time. This apatite-forming behavior in the SBF is related to the dissolution of Ca(II) ions from the sintered body in the early stage of immersion. Thus, diopside prepared by the coprecipitation process using the metal alkoxide and the metal salts was found to have an apatite-forming ability.     

Synthesis of coprecipitated strontium hexaferrite nanoparticles in the presence of polyvinyl alcohol

Strontium hexaferrite (SrFe₁₂O₁₉) nanoparticles were synthesized by the chemical coprecipitation method and using polyvinyl alcohol (PVA) as a protective agent. The synthesized samples were characterized by differential thermal analysis, X-ray diffraction, scanning and transmission electron microscopy, particle size analyzer, sedimentation test and vibrating sample magnetometer. In the presence of PVA, the single-phase SrFe₁₂O₁₉ nanoparticles were obtained at low temperature of 650 °C. The average particle size of SrFe₁₂O₁₉ precursor was 15 nm, which increased to 61 nm after calcination at 650 °C. The magnetic measurements indicated that PVA decreased coercivity from 4711 to 3216 Oe with particle size reduction. The results showed that PVA as a protective agent could be effective in decreasing the particle size, calcination temperature and coercivity of SrFe₁₂O₁₉ nanoparticles.     

Investigations on structural and magnetic properties of cobalt ferrite/silica nanocomposites prepared by the coprecipitation method

Magnetic nanocomposites consisting of cobalt ferrite nanoparticles embedded in silica matrix were prepared by the coprecipitation method using metallic chlorides as precursors for ferrite. Subsequently composites were annealed at 100, 200 and 300 °C for 2 h. The samples were structurally characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and transmission electron microscopy (TEM). The magnetic properties were measured in the temperature range of 10-300 K using vibrating sample magnetometer (VSM). The effects of thermal treatment on structural and magnetic properties of nanocomposites were investigated. When the samples were annealed, CoFe₂O₄ nanocrystallites were observed in the SiO₂ matrix, whose size increases with increase in annealing temperature. The coercivity and saturation magnetization of nanocomposite (annealed at 300 °C for 2 h) are much higher than that of bulk cobalt ferrite. The realization of adjustable particle sizes and controllable magnetic properties makes the applicability of the CoFe₂O₄ nanocomposite more versatile.     

Fabrication of N-(Amino-Ethyl)-Amino-Propyl Functionalized Magnetite Nanoparticles for Oil–Water Separation of Wastewater From Tertiary Oil Recovery

N-(amino-ethyl)-amino-propyl trimethoxy silane (AEAPTMS) is used to modify Fe₃O₄ with a one-pot coprecipitation method. Powder X-ray diffraction measurements show the spinel structure of magnetite nanoparticles. A high positive charge of +33.96 mV was obtained on the surfaces of modified magnetic nanoparticles, with the diameter ranging from 6.5 to 22.5 nm. The modified Fe₃O₄ was first applied to the treatment of wastewater from tertiary oil recovery. The obtained results indicated that the oil removal rate increased with the dosage of modified Fe₃O₄ and slightly increased with the separation time. The mechanism of modified Fe₃O₄ toward wastewater from tertiary oil recovery was attributed to the electrostatic interaction between negatively charged microemulsion oil in wastewater and the positively charged surfaces of magnetic nanoparticles.     

铕掺杂纳米氧化锌晶体结构和荧光光谱的研究

以醋酸锌、氧化铕、氢氧化钠为主要原材料,利用共沉淀法制备ZnO∶Eu3+纳米晶体.在X射线衍射谱中,只观察到氧化锌的峰,没有观察到氧化铕的特征峰.比较了ZnO和ZnO∶Eu3+拉曼光谱,在ZnO∶Eu3+样品拉曼光谱中观察到新的局部振动模.这些现象表明铕离子已经进入氧化锌晶格中.SEM形貌显示Eu3+离子掺入使ZnO晶...     

T形微反应器共沉淀法制备Mg-Al层状双金属氢氧化物及其粒径可控性

采用T形微反应器通过共沉淀法制备了Mg-Al层状双金属氢氧化物(LDHs)纳米颗粒, 考察了流速、混合盐溶液浓度和温度等对产物粒径及其分布的影响. 实验结果表明, 所制备的LDHs样品的形貌和晶体结构与传统共沉淀法结果一致, 但本方法制备的样品粒径小、分布窄. 随着流速增大, 温度升高, 所合成的LDHs样品平均粒径减小, 分布变窄; 而随着混合盐溶液浓度的增大, 所得LDHs样品粒径增大, 分布变宽.