硅胶G基纳米钛酸锶钡吸附富集-火焰原子吸收法对水中Pb~(2+)的测定

采用溶胶-凝胶法制备了硅胶G基纳米钛酸锶钡,并且用X射线衍射(XRD)、扫描电镜(SEM)和傅立叶变换红外光谱(FTIR)进行了表征.系统地研究了该物质对水中铅的吸附性能.提出了硅胶G负载纳米钛酸锶钡分离富集,FAAS法测定水中痕量铅的新方法.结果表明,纳米钛酸锶钡能够负载于硅胶G表面,制成蚕茧状颗粒吸附材料.在pH值为4～6时,该吸附剂对水中的铅离子具有很强的吸附能力,静态吸附容量达到86.28m/g.吸附在硅胶G负载纳米钛酸锶钡上的铅离子可用1mol/L的硝酸完全洗脱下来,经硅胶G负载纳米钛酸锶钡富集10倍后,方法检出限为7.4μg/L.用于河水和自来水中痕量铅的测定,结果满意.     

纳米钛酸锶钡粉体吸附富集-火焰原子吸收光谱法测定水样中锰离子

提出了纳米钛酸锶钡粉体吸附富集,火焰原子吸收光谱法测定水中痕量锰的含量。在pH 6的氨性缓冲介质中,采用纳米钛酸锶钡(0.02 g)对水样(10 mL)中的锰离子振荡吸附15 min。优化条件下吸附容量达5.4 mg.g-1。方法检出限(3s/k)为2.1μg.L-1。用0.15 mg.L-1锰(Ⅱ)标准溶液连续测定6次,求得其相对标准偏差(n=6)为3.4%。用于河水和地下水中痕量锰的测定,用标准加入法测得方法的回收率在93.5%~99.7%之间。     

海带吸附法分离富集水样中痕量铅和镉

研究了用海带吸附法分离富集水中痕量Pb2 和Cd2 的方法.在25℃下,pH4.0～5.0,水样经过预先用海带制成吸附柱后,用10mL 1 mol/L的HCl,流速为1 mL/min对吸附柱进行洗脱,采用原子吸收光谱法测定洗脱液中Pb2 和Cd2 .Pb2 和Cd2 的饱和吸附量分别为164.67和8.73 mg/g,回收率在95.8%～103.1%之间.     

基于秸秆模板法制备多孔纳米钛酸锶钡及其对重金属的吸附性能

以高粱秸秆为模板,采用溶胶-凝胶法制备了纳米钛酸锶钡多孔吸附剂(SPBST),以X射线衍射(XRD)、扫描电子显微镜(SEM)和傅立叶变换红外光谱(FTIR)进行表征.考察了该多孔吸附剂对水中重金属铅、镉和锌的吸附富集性能,探讨了煅烧温度对吸附剂形貌和吸附性能的影响.并以镉离子为例,系统地研究了吸附热力学和动力学.结果表明,各煅烧温度下合成的多孔材料均由钙钛矿结构的纳米钛酸锶钡组成,晶体粒径均不大于20nm,多孔吸附剂对水中铅、镉和锌均有较强的吸附能力,吸附性能与材料的煅烧合成温度和介质的pH值以及吸附时间有关.煅烧温度过高,纳米钛酸锶钡晶体团聚严重,吸附能力降低;温度过低,材料松散易碎,不利于重复使用,750℃煅烧6h合成的材料性能最好.当介质的pH值为5～8时,吸附70min,对铅、镉和锌的静态吸附容量分别为191.51,19.00和19.97mg?g―1.其吸附行为符合Freundlich吸附等温模型和HO准二级动力学方程式,吸附过程焓变(?H)为35.905kJ?mol-1,各温度下的自由能变(?G)均小于零,熵变(?S)均为正值,吸附过程的活化能(Ea)为62.430kJ?mol-1.该吸附过程是自发的吸热物理过程.被吸附的金属离子均可用1mol?L-1的硝酸完全洗脱回收.对铅、镉和锌的富集因子均超过200.将其应用于水中痕量铅、镉和锌的吸附富集和原子吸收测定,回收率分别为90.3%～103.4%,91.5%～103.2%和94.35%～101.1%.     

冠醚壳聚糖多孔微球选择性富集-石墨炉原子吸收法测定雨水中痕量铅的研究

报道用冠醚壳聚糖多孔微球选择性富集雨水中痕量铅并用石墨炉原子吸收法测定.DB-18-crown-6-CTS多孔微球在pH 5.5时,对Pb2+的富集率达到98%.吸附的Pb2+能用5 mL 2 mol·L-1的HCl定量洗脱,洗脱率98.1%.Pb2+被洗脱后,用石墨炉原子吸收法测定.该方法的富集倍数为100倍,检出限(3σ)为0.085 μg·L-1,相对标准偏差小于2.75%,用于分析实际雨水样,回收率为94.5%～102%.     

冠醚壳聚糖多孔微球选择性富集-石墨炉原子吸收法测定绒柄牛肝菌中的痕量铅

报道了用冠醚壳聚糖多孔微球选择性富集绒柄牛肝菌中痕量铅并用石墨炉原子吸收法测定.DB-18-crown-6-CTS多孔微球在pH5.5时,对Pb2+的富集率达到98%.吸附的Pb2+能用5 mL 2 mol/L的HCl定量洗脱,洗脱率98.1%.Pb2+被洗脱后,用石墨炉原子吸收法测定.该方法的富集倍数为100倍,检出限(3σ)为0.085μg/L,相对标准偏差小于2.8%,用于分析绒柄牛肝菌样品,回收率为94.5%～102%.     

纳米SiO_2分离富集-火焰原子吸收法测定水中痕量银

研究了纳米SiO_2分离富集-火焰原子吸收法测定水中痕量银的新方法.考察了溶液pH、吸附时间、洗脱条件和干扰离子等因素对Ag~+分离富集的影响,确定了纳米SiO_2对Ag~+吸附的最佳条件.结果表明:在pH 4.1时,纳米SiO_2能定量吸附银,吸附在纳米SiO_2上的Ag~+可用0.5 mol/L HCl+0.5 mol/L硫脲定量洗脱.该法对银的检出限为0.77 ng/mL(3σ,n=11);线性范围为0.005～1.5μg/mL,对0.5μg/mL的Ag~+标液进行7次测定,RSD为3.6%,回收率在94.0%～101.5%之间;方法可用于环境水样中痕量银的测定.     

聚丙烯腈微球预富集分离微柱与FAAS联用测定痕量Cd(Ⅱ)和Zn(Ⅱ)

将自制的聚合物微球填充到玻璃柱制备了2.5cm×4 mm i.d.预富集分离柱,并将其与火焰原子吸收光谱(FAAS)法联用,测定了其对Cd2和Zn2+的动态吸附,建立了测定溶液中痕量Cd2+和Zn2+的预富集分离-FAAS方法;优化了对Cd2+和Zn2+的吸附富集与洗脱条件,在室温下,溶液pH为5～6,上样和洗脱液流速...     

双硫腙修饰纳米TiO2分离富集石墨炉原子吸收光谱法测定水样中痕量金属离子

建立了双硫腙修饰纳米TiO2分离富集-石墨炉原子吸收光谱法测定水样中痕量镉、铬和铅的新方法,优化了纳米TiO2-双硫腙对试样中这3种痕量物质的吸附和解吸条件。结果表明,在pH 5.0时,镉、铬和铅可被定量吸附,静态饱和吸附容量分别为13.3、5.5、21.8 mg/g。吸附的各种金属离子可用5 mL 0.1mol/L的硝酸完全洗脱。该方法对Cd2+、Cr3+和Pb2+的检出限(3σ,n=11)分别为0.18、0.51、1.92 ng/L,相对标准偏差分别为2.8%、2.3%和1.0%,加标回收率为96%～101%。该方法已成功应用于环境水样中镉、铬和铅的测定。     

流动注射-微柱在线富集/电感耦合等离子发射光谱法测定中成药中痕量铅和镉

采用自制固相萃取材料PTFE-g-GMA-PEI纤维填充微柱预富集和流动注射(FI) 与电感耦合等离子发射光谱仪联用, 测定样品中痕量Pb2+和Cd2+.对Pb2+和Cd2+的富集与洗脱条件进行优化,并给出相应离子的分析特性.结果表明: 本方法Pb2+和Cd2+检出限分别为3.5和0.15 μg/L; 富集倍数分别为30和80; RSD分别为1.5%和0.6%(n=9,单个离子浓度为50 μg/L).本方法应用于几种中成药中的痕量铅和镉的同时测定,样品加标回收率在90%～108% 之间, 结果满意.     

纳米钛酸钙粉体的制备及其对水中铅和镉的吸附行为

采用柠檬酸络合溶胶-凝胶法制备了纳米钛酸钙粉体. 以X射线衍射(XRD)、透射电子显微镜(TEM)和傅立叶变换红外光谱(FTIR)对其进行了表征. 考察了该纳米粉体对水中重金属铅和镉的吸附性能, 并以镉离子为例, 系统地研究了吸附热力学和动力学. 结果表明, 该法合成的钛酸钙为钙钛矿结构的纳米粉体, 粒径大小受灼烧温度的影响, 灼烧温度越高, 粉体平均粒径越大, 600 ℃灼烧2 h条件下, 粉体的平均粒径最小, 约为20 nm. 当介质的pH值为4～8时, 钛酸钙对水中的铅和镉具有很强的吸附能力. 其对镉离子的吸附行为符合Langmuir 吸附等温模型和HO准二级动力学方程式, 吸附过程焓变(ΔH)为39.312 kJ•mol－1, 各温度下的自由能变(ΔG)均小于零, 熵变(ΔS)均为正值, 吸附过程的活化能(Ea)为20.359 kJ•mol－1. 该吸附过程是自发的吸热物理过程. 被吸附的铅和镉均可用1 mol•L－1的硝酸完全洗脱回收. 对铅和镉的富集因子均超过200. 将其应用于水中痕量铅和镉的吸附富集和测定, 回收率分别为96.3%～107.2%和93.5%～104.0%, 与石墨炉原子吸收光谱法测定结果一致.     

双硫腙螯合型树脂同时分离富集-火焰原子吸收光谱法测定痕量铅和镉

以大孔聚苯乙烯树脂为母体,通过-N=N-,与双硫腙键合,合成了双硫腙螯合型树脂,并将其应用于痕量铅和镉的同时分离富集,实验了酸度、流速、共存离子干扰等因素对双硫腙螯合型树脂吸附和洗脱Pb和Cd的影响,建立了双硫腙螯合型树脂同时分离富集-火焰原子吸收光度法测定食品及环境样品中痕量Pb和Cd的方法.对Pb和Cd,方法的检出限分别为0.015和0.0013μg/mL,相对标准偏差(RSD)均优于3.0%.     

Removal of heavy metals and bacteria from aqueous solution by novel hydroxyapatite/zeolite nanocomposite,preparation, and characterization

In this study, a HAp/NaP nanocomposite was prepared by adding a synthesized nano-hydroxyapatite to zeolite NaP gel in the hydrothermal condition and used for the removal of lead(II) and cadmium(II) ions from aqueous solution. HAp/zeolite nanocomposite was then characterized by Fourier transform infrared spectroscopy, X-ray diffraction and Rietveld method, scanning electron microscope, energy-dispersive X-ray analysis, and surface area and thermal analyses. Results suggested that the nanocomposite crystals of HAp were dispersed onto the zeolite external surface and/or encapsulated within the zeolite channels and pores. The potential of the composite in adsorption of heavy metals was investigated by using batch experiment. The metal concentration in the equilibrium C _e (mg/g) after adsorption with nanocomposite of HAp/NaP was analyzed using flame atomic adsorption spectrometry. The adsorption experiments were carried out at pH of 3–9. The influences of contact time, initial concentration, dose, and temperature on the adsorption of lead and cadmium ions were also studied. Results show that these nanocomposites have further adsorption related to NaP and HAp. They have great potential (about 95 %) for Pb(II) and Cd(II) adsorption at room temperature. The equilibrium process was described by Frendlich, Langmuir, Temkin, and Dubinin–Radushkevich (D-R) models. The kinetics data were successfully fitted by a pseudo-second-order model. The in vitro antibacterial activity of these composites was evaluated against Bacillus subtilis (as Gram-positive bacteria) and Pseudomonas aeruginosa (as Gram-negative bacteria) and compared with standard drugs that show inhibition on bacterial growth.     

Coadsorption of Cd(II) and oxalate ions at the TiO2/electrolyte solution interface

The study of the adsorptions of cadmium and oxalate ions at the titania/electrolyte interface and the changes of the electrical double layer (edl) structure in this system are presented. The adsorption of cadmium or oxalate ions was calculated from an uptake of their concentration from the solution. The concentration of Cd(II) or oxalate ions in the solution was determined by radiotracer method. For labeling the solution 14C and 115Cd isotopes were used. Coadsorption of Cd(II) and oxalic ions was determined simultaneously. Besides, the main properties of the edl, i.e., surface charge density and zeta potential were determined by potentiometer titration and electrophoresis measurements, respectively. The adsorption of cadmium ions increases with pH increase and shifts with an increase of the initial concentration of Cd(II) ions towards higher pH values. The adsorption process causes an increase of negatively charged sites on anatase and a decrease of the zeta potential with an increase of initial concentration of these ions. The adsorption of oxalate anions at the titania/electrolyte interface proceeds through the exchange with hydroxyl groups. A decrease of pH produces an increase of adsorption of oxalate ions. The processes of anion adsorption lead to increase the number of the positively charged sites at the titania surface. However, specific adsorption of bidenate ligand as oxalate on one surface hydroxyl group may form inner sphere complexes on the metal oxide surface and may overcharge the compact part of the edl. The presence of oxalate ions in the system affects the adsorption of Cd(II) ions on TiO2, increasing the adsorption at low pH range and decreasing the adsorption at high pH range. Using adsorption as a function of pH data, some characteristic parameters of adsorption envelope were calculated.     

Removal of Pb2+ and Cd2+ ions from aqueous solutions using guanidine modified hydrogels

In this study, experimental measurements have been made on the batch adsorption of cadmium and lead ions from aqueous solutions using poly(guanidine modified 2‐acrylamido‐2‐methylpropan sulfonic acid/acrylic acid/N‐vinylpyrrolidone/2‐Hydroxyethyl methacrylate), P(AMPSG/AAc/NVP/HEMA) hydrogels. The guanidyl end group bearing AMPSG monomer was synthesized from the reaction of AMPS and guanidine. The hydrogels were prepared by UV‐curing technique. The morphology of the dry H10‐hydrogel sample was examined by SEM. The influence of the uptake conditions, such as pH, functional monomer per cent, contact time, initial feed concentration, and foreign metal ions on the metal ion binding capacity of hydrogel, was also tested. The selectivity of the hydrogel toward the different metal ions tested was Hg(II) > Pb(II) > Au(III) > Cd(II). The adsorption isotherm models were applied to the experimental data, and it was seen that the Langmuir isotherm model was the best fit for the adsorption of Cd(II) and Pb(II) ions on P(AMPSG/AAc/NVP/HEMA) hydrogel. It was found that adsorbed lead and cadmium ions on P(AMPSG/AAc/NVP/HEMA) hydrogel can be effectively desorbed by acid leaching and the regenerated P(AMPSG/AAc/NVP/HEMA) hydrogel can be reused almost five times less without any loss of adsorption capacity. Copyright © 2009 John Wiley & Sons, Ltd.     

Adsorption of univalent and bivalent metal nitrates on hydrous lead dioxide Adsorption behaviour of potassium, cupric, zinc, cadmium and nitrate ions

The individual adsorption behaviour of potassium, cupric, zinc, cadmium and nitrate ions on hydrous lead dioxide (HLD) was investigated. HLD was found to be an amphoteric ion-exchanger with an equi-adsorption point in the vicinity of pH 4.6. For bivalent metal ions, the amount of adsorption increased with pH (at pH > 3) and there was almost 100% adsorption at pH > 6. Both the adsorption capacity and the adsorption affinity on HLD were in the order copper(II) > zinc(II) > cadmium(II).     

Simultaneous determination of cadmium(II), lead(II) and copper(II) by using a screen-printed electrode modified with mercury nano-droplets

We are presenting a strategy for the fabrication of disposable screen-printed electrodes modified with mercury nano-droplets and capable of sensing heavy metal ions. They were prepared by coating electrodes with a mixture of multi-walled carbon nanotubes and chitosan, this followed by adsorption of mercury. The resulting sensor was characterized by cyclic voltammetry and impedance spectroscopy. Also the effects caused by adsorption of mercury were investigated. It is shown that square wave anodic stripping voltammetry enables simultaneous determination of cadmium(II), lead(II) and copper(II), for which detection limits of 12, 23 and 20 nM, respectively, are found. Relative standard deviations for ten determinations at 0.6 µM concentrations of these ions are in the range of 3.0 to 5.7%. The applicability was tested by analyzing river water and showed recoveries between 94.1 and 104.6%, thus demonstrating its utility for in-field monitoring of these heavy metal ions.     

Thermal degradation and their kinetics of biodegradable poly(butylene succinate-co-butylene terephthate)s under nitrogen and air atmospheres

In this study, thermal degradation and their related kinetics have been investigated mainly by means of thermal gravimetrical analyzer (TGA) under the dynamic nitrogen and air atmospheres for the chemically prepared biodegradable aliphatic-aromatic copolyesters of poly(butylene succinate-co-butylene terephthalate) (PBST). To further shed new lights on the comonomer molar composition and experimental condition dependences of thermal degradation kinetics, the as-known Friedman model was at first applied to quantitatively evaluate the kinetic parameters in terms of activation energy (E), degradation reaction order (n) and the frequency factor (Z). The results clearly demonstrated that thermal stabilities of these PBST copolyesters were substantially enhanced with the incorporation of more rigid butylene terephthalate comonomer, and tended to be much better in nitrogen than in air. Furthermore, the Friedman, Freeman-Carroll and Chang models were concurrently employed to quantitatively evaluate the thermal degradation kinetic parameters of the PBST copolyesters in nitrogen at different heating rates of 1, 2 and 5 K/min. It was found that the thermal degradation kinetic parameters for the PBST copolyesters were strongly dependent on the heating rate and calculating models. In addition, life-time parameters of the biodegradable PBST copolyesters were first calculated to predict the maximum usable temperatures, and this would be useful for practical application of these new bio-based green plastics.     

Adsorption of heavy metal ions to floc-type biosorbents

Adsorption of cadmium and lead ions to floc-type biosorbents was reported in this work. Two types of biosorbents containing a marine microalga, Heterosigma akashiwo (Hada) Hada, or a purple non-sulfur bacterium, Rhodobacter sphaeroides, were prepared. The micro-organisms inactivated by steam sterilization were immobilized in casein floc and cross-linked with glutaraldehyde. In the present immobilizing method, we obtained the biosorbents comprising as much as 67% of micro-organism on a dry-weight basis. Simple metal-binding models were applied to explain the adsorption mechanism of bivalent metal ions to the biosorbents. The results showed that casein acted as both the immobilizing material and the adsorbent material. The adsorption of bivalent metal ions to the biosorbents was due to bidentate binding to the acidic sites on casein and monodentate binding to the acidic sites on micro-organisms. The metal-binding constants and the binding capacities of micro-organisms were scarcely influenced by immobilization.     

Synthesis of 2-mercaptobenzothiazole/magnetic nanoparticles modified multi-walled carbon nanotubes for simultaneous solid-phase microextraction of cadmium and lead

This study describes the successful sequential modification of multi-walled carbon nanotube (MWCNT) by Fe₃O₄ magnetic nanoparticles and 2-mercaptobenzothiazole (MBT) followed by its application as a novel sorbent for simultaneous magnetic solid phase microextraction of lead and cadmium. Fourier transform infrared spectroscopy and scanning electron microscopy were employed to confirm the chemical surface modification of the MWCNT. The ions retained on the 2-MBT/magnetic nanoparticles modified MWCNTs were eluted with 1.0 mL of nitric acid (0.8 mol L^?1) in methanol solution and determined by the flame atomic absorption spectrometry. All parameters affecting the extraction condition were thoroughly investigated and optimised. Under the optimised condition preconcentration factor of 150.0, enhancement factors of 149.0 and 149.2 and limits of detection of 0.21 and 0.01 µg L^?1 were achieved for lead and cadmium, respectively. Using the prepared magnetic nanocomposite, the possible interference of other common ions associated with lead and cadmium determination was effectively avoided and the method was successfully applied to the simultaneous determination of the target ions in various environmental water samples.