浊点萃取-石墨炉原子吸收光谱法同时测定生物样品中痕量铅和镉

提出了石墨炉原子吸收光谱法同时测定小鼠肝中痕量Pb和Cd的方法。以8-羟基喹啉为络合剂,在pH 9.0时,用Triton X-100浊点萃取富集样品中的Pb和Cd。用NH4H2PO4作为基体改进剂测定Pb和Cd,Pb和Cd的检出限(3s/k)分别为0.103μg/L和0.0136μg/L,相对标准差(n=6)分别为1.4%,0.73%。对于10 mL样品溶液的富集倍数分别为7.1,9.3。利用该法分别测定了小鼠肝中的Pb和Cd的含量,加标回收率分别为96.4%～97.1%和101.3%～103.2%。     

三乙烯四胺修饰β-环糊精交联树脂分离富集/原子吸收法测定大米中的铅、镉

该文制备了一种新型吸附材料三乙烯四胺修饰β-环糊精交联树脂(TETA-β-CDP),并对其进行红外光谱表征,优化了该吸附材料对痕量铅、镉的吸附和解析条件,建立了动态条件下同时分离富集/原子吸收光谱测定大米中铅和镉的新方法。在p H 5.5时,样品溶液以1.0 m L/min流速过柱,试液中的Pb2+和Cd2+可被该树脂定量富集,其动态饱和吸附容量分别为22.8,31.3 mg/g,吸附在TETA-β-CDP上的Pb2+和Cd2+可用0.1 mol/L HCl以0.8 m L/min流速完全洗脱。该方法对铅、镉的检出限(3σ,n=11)分别为0.038 mg/L和0.016 mg/L;线性范围分别为0.2~20 mg/L和0.05~2.5 mg/L;相对标准偏差(RSD)分别为2.8%和1.7%;加标回收率分别为97.5%~101.0%和95.0%~102.5%。该方法用于大米样品中痕量铅、镉的测定,结果满意。     

反相高效液相色谱法同时测定镉、铅、铜和锌

 研究了meso-四（对羟基苯基）卟啉为柱前衍生化试剂与Cd2+,Pb2+,Cu2+和Zn2+离子的配合反应条件及配合物在C18色谱柱上的分离条件,建立了反相高效液相色谱快速分离光度检测Cd2+,Pb2+,Cu2+和Zn2+的新方法。配合物和试剂在15 min内出峰完毕。4种离子的检出限为: Cd2+0.02 ng,Pb2+0.02 ng, Cu2+0.02 ng,Zn2+0.12 ng;线性范围为:Cd2+0.8 μg/L～150 μg/L,Pb2+0.8 μg/L～300 μg/L,Cu2+0.8 μg/L～500 μg/L,Zn2+5.0 μg/L～1 000 μg/L;方法的日内相对标准偏差为:2.8%～4.8%,测定低、中、高3个浓度的日间相对标准偏差为3.7%～9.7%。     

氢化物发生-原子荧光光谱法测定化妆品中痕量砷和铅

建立了氢化物发生-原子荧光光谱法测定化妆品中痕量As、Pb的方法,研究了样品前处理及实验条件对As、Pb测定的影响.本方法可同时用于固态、液态等各类样品处理的优点.测量As、Pb的线性范围分别为0～100 μg/L和0～120 μg/L,方法的检出限分别为0.94和1.22 μg/L,回收率分别为91.67%～102.67%和91.60%～98.80%,相对标准偏差(n=3)分别在1.7%～7.3%和2.2%～6.8%范围内.     

预镀铋膜修饰碳糊电极差分脉冲伏安法测定废水中铅和镉

采用预镀铋膜法制得铋膜修饰碳糊电极,当沉积时间为540s得到最优铋膜。采用差分脉冲伏安法(DPV)实现了对痕量Pb2+、Cd2+的同时测定。优化了DPV测定条件,当富集时间为150s、富集电位为-1.25V、HAc-NaAc缓冲底液的pH为4.5时,Pb2+、Cd2+的峰电流最大。在最优的实验条件下,Pb2+和Cd2+的峰电流与其浓度呈良好的线性关系,线性相关系数R分别为0.9912和0.9937,线性范围分别为1~10μmol/L和5~50μmol/L,Pb2+和Cd2+的检出限分别为0.32μmol/L和2.01μmol/L。对实际废水样品进行了加标回收实验,其中Pb2+和Cd2+的回收率分别为98.4%~102.6%和95.4%~104.6%。     

球形立方相纳米二氧化铈-ICP-MS法同时测定痕量铅和镉

采用室温固相法合成球形立方相纳米CeO2,建立了纳米CeO2富集分离,ICP-M S同时测定痕量Pb(Ⅱ)和Cd(Ⅱ)的方法。在pH 7.0,10 mg CeO2,吸附15min后,纳米CeO2对Pb(Ⅱ),Cd(Ⅱ)的吸附率均可达100%;以2mL 0.05 mol/L HCl溶液为洗脱剂、洗脱20 min后,对Pb(Ⅱ)和Cd(Ⅱ)的洗脱率可分别达到98%和95%以上;纳米CeO2对Pb(Ⅱ),Cd(Ⅱ)的最大静态吸附容量分别为496.9μg/g和243.1μg/g,富集倍数均可达250倍,共存离子影响小。优化ICP-MS仪器工作条件,选择205Bi和115In为在线内标进行Pb(Ⅱ)和Cd(Ⅱ)的测定,检出限分别为1.7 pg/mL和9.2 pg/mL,RSD分别为4.8%和0.94%。方法应用于实际水样,回收率分别为Pb(Ⅱ)93.6%~106.4%,Cd(Ⅱ)96.2%~108.9%。     

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%.     

手控注射式钛酸锶钡多孔球富集器分离富集-火焰原子吸收法测定水中铅和镉

以D311树脂为模板,采用溶胶-凝胶法制备了纳米钛酸锶钡多孔球,用X射线衍射仪(XRD)、扫描电子显微镜(SEM)和傅立叶变换红外光谱仪(FTIR)进行了表征.考察了Pd2+和Cd2+的吸附和解脱条件.将微球装柱,制成注射式富集器,研究了此富集器对水中痕量Pd2+和Cd2+的富集性能.结果表明: 此法合成的多孔球,由钙钛矿结构的纳米钛酸锶钡组成,晶体平均粒径为21 nm,球体表面布满了不规则的纳米孔洞.当pH 4～7时,此多孔球对水中的Pd2+和Cd2+具有很强的吸附能力,静态吸附容量分别为61.9和14.8 mg/g.由多孔球装柱制成的手控注射式富集器,可成功实现对水中Pd2+和Cd2+的同时吸附.用2 mol/L HNO3洗脱后,火焰原子吸收测定.建立了手控注射式纳米钛酸锶钡富集器分离富集、FAAS法测定水中痕量Pd2+和Cd2+的新方法.此方法对Pd2+和Cd2+的检出限分别为0.099和0.0034 μg/L.用于水样中痕量Pd2+和Cd2+的富集和原子吸收测定,回收率分别为97.8%～106.5%和93.0%～100.7%.     

预镀铋膜修饰铂电极差分脉冲溶出伏安法测定痕量铅、镉

采用预镀铋膜法修饰铂电极,用该电极对痕量Pd、Cd同时进行了差分脉冲溶出伏安法测定,Pd、Cd在富集中和铋形成类似于汞齐的合金,溶出峰良好。讨论了在不同沉积液和沉积时间下得到的铋膜电极的性能和富集时间、富集电位及底液pH对金属离子测定的影响。在优化的实验条件下,分别对10~100μg/L、20~200μg/L和50~500μg/L3个不同浓度系列的Pb2 、Cd2 进行了同时测定,Pb、Cd溶出峰电流与Pb2 、Cd2 浓度呈良好的线性关系(r≥0.999),Pb2 、Cd2 浓度的线性范围均为10~500μg/L;富集时间为180 s时,Pb2 、Cd2 的检出限分别为0.38μg/L和0.82μg/L。利用本方法测定了蔬菜中Pb的含量,并与原子荧光分析法做了对比,结果令人满意。     

固相萃取-离子色谱法测定地下水中痕量高氯酸根离子

建立了测定地下水中痕量高氯酸根（ClO~4）的固相萃取-离子色谱(SPE-IC)分析方法。0.7 L水样经预处理降低主要干扰离子Cl~、CO2~3和SO2~4的干扰后,使用Cleanert PWAX弱阴离子交换固相萃取小柱对地下水中痕量(μg/L级)的ClO~4进行富集,用6 mL 1%NaOH溶液洗脱,富集液经0.45 μm水膜过滤后,用IonPac AS20阴离子分离柱、50 μL进样环、40 mmol/L KOH溶液淋洗、抑制电导检测分离分析。结果表明,地下水样品中ClO~4的方法检出限和测定下限分别为0.15 μg/L和0.60 μg/L,进样质量浓度在1～15 μg/L范围内有很好的线性关系,线性相关系数为0.9992,回收率为99.7%～100.5%;该方法经济有效,可用于地下水中痕量ClO~4的检测。利用该方法测定了哈尔滨周边部分地区地下水中ClO~4浓度,检测结果与离子色谱-质谱联用法的检测结果的相对误差为1.85%～9.24%。     

响应面法优化巴旦木壳对废水中Pb、Cu和Cd的吸附及同时测定

研究废弃巴旦木壳对模拟废水中Pb、Cu和Cd的去除率。在单因素实验的基础上,采用响应面法对吸附剂投加量、吸附时间和pH值3因素进行优化。实验结果表明,Pb、Cu和Cd分别在最佳吸附吸附剂投加量0.4 g,吸附时间49.38 min,pH值为9.96;吸附剂投加量0.4 g,吸附时间49.91 min,pH值为10.13;吸附剂投加量0.4 g、吸附时间49.83 min、pH值为10.42的条件下,去除率分别为87.42%、73.49%和85.11%。采用偏最小二乘法(PLS)对Pb、Cu和Cd模拟混合试样吸附后的溶液测定的曲线进行拟合回归,计算得出吸附剂对Pb、Cu和Cd的去除率分别为83.2%、66.0%和83.3%。用PLS对吸附后的模拟废水样品进行计算分析,并间接得出巴旦木壳对Pb、Cd和Cu的去除率和建立Pb、Cd、Cu三组分同时测定的多元校正分析方法。     

Preparation and characterization of porous calcium titanate-based coated glass fiber filter material and its application in determination of lead and cadmium ion concentrations in water

Glass fiber filter coated with a porous block adsorption agent of calcium titanate (GPCTO) was prepared by the citric acid sol-gel method, and characterized by X-ray diffraction, scanning electron microscopy, and FTIR spectrophotometry. Its Pb2+ and Cd2+ adsorption properties from water were studied. Adsorption and elution were investigated under different conditions, as were the thermodynamics and kinetics of adsorption, using Cd ion as representative. Calcium titanate may react with glass fiber, forming Si-O-Ti and B-O-Ti bonds and becoming a composite adsorbent. The Pb and Cd ions were quantitatively retained at pH 4-9; their adsorption capacities by the GPCTO were 199.72 and 19.68 mg/g, respectively. The isothermal data were described by the Langmuir equation. The dynamic data followed the pseudo-second-order kinetic model well. The enthalpy change (AH) of the adsorption process was 37.160 kJ/mol. At various temperatures, Gibbs free energy changes (delta G) were negative, and entropy changes (delta S) were positive. The activation energy (Ea) was 38.127 kJ/mol for the adsorption. Cd ion adsorption by the GPCTO was endothermic and spontaneous. The adsorbed Pb and Cd ions were completely recovered by elution with 2 M HNO3. The Pb+ and Cd2+ concentration factors were up to 200. The method has been applied to the preconcentration for flame atomic absorption spectrometric determinations of trace Pb and Cd ions in water samples. The recoveries were 95.2 to 102.4% for Pb and 92.2 to 98.0% for Cd.     

Adsorption properties of the double-imprinted electrospun crosslinked chitosan nanofibers

Pb(II)-Cd(II) double-imprinted electrospun crosslinked chitosan nanofibers (Pd/Cd-DIECCNs) were prepared by combining electrospinning and ion-imprinting methods, which showed excellent adsorption capacity for both Pb(II) and Cd(II).     

三乙烯四胺改性榴莲壳吸附水溶液中的Cd~(2+)、Pb~(2+)

采用三乙烯四胺改性榴莲壳,制备新型的改性榴莲壳吸附剂,研究其对Cd2+、Pb2+的吸附性能。结果表明,吸附Cd2+、Pb2+的适宜条件为:pH 6.0,吸附时间120 min。改性后榴莲壳吸附剂对Cd2+、Pb2+的吸附容量有了很大程度的提高,Cd2+、Pb2+最大吸附量分别达到39.30、53.76 mg/g。吸附过程可以很好地用准二级动力学方程描述,吸附等温线用Langmuir方程的拟合效果优于Freundlich方程。     

Comparison of Pb, Cd Adsorption to Surface Coatings Developed in Natural Waters with that in Plant Effluents

The comparative studies of Pb and Cd adsorption to the surface coatings (Fe, Mn, AI oxides, organic materials, and associated minerals), which were developed on glass slides in five natural and two technical waters (plant effluents), were carried out under controlled |aboratory conditions(mineral salts solution with defined speciation, ionic strength 0.05 mol/L, 25 ℃ and pH 6. 0). The classical Langmuir adsorption isotherm was applied to estimating the equilibrium coefficients of Pb and Cd adsorption to the surface coat-ings. The results show that the maximum adsorption of Pb and Cd to the surface coatings mentioned above varied widely. There was a systemic increase in the maximum adsorption of Pb and Cd to the surface coatings with increasing the contents of Mn and Fe oxides in the surface coatings in significant correlation, respective-ly, not only highlighting the relative importance of the metal oxide fraction for Pb and Cd adsorption to the surface coatings developed in natural and technical water samples, but also implying the same adsorption mechanisms of Pb and Cd to the surface coatings developed both in natural and technical water samples.     

Preparation of silicon-doped ferrihydrite for adsorption of lead and cadmium: Property and mechanism

In this study, Si-doped ferrihydrite (Si-Fh) was successfully synthesized by a simple coprecipitation method for removal of heavy metals in water. Subsequently, the physicochemical properties of Si-Fh before and after adsorption were further studied using several techniques. The Si-Fh exhibited good adsorption capacity for heavy metal ions such as Pb(II) and Cd(II). The maximum adsorption capacities of lead and cadmium are respectively 105.807, 37.986 mg/g. The distribution coefficients of the materials for Pb(II) and Cd(II) also showed a great affinity (under optimal conditions). Moreover, it was found that the adsorption fit well with the Freundlich isotherm and pseudo-second-order kinetic model which means this was a chemical adsorption process. It can be conducted from both characterization and model results that adsorption of Pb(II) and Cd(II) was mainly through the complexation interaction of abundance oxygen functional groups on the surface of Si-Fh. Overall, the Si-Fh adsorbents with many superiorities have potential for future applications in the removal of Pb(II) and Cd(II) from wastewater.     

Removal of Cd(II) and Pb(II) from aqueous solution by modified attapulgite clay

Three low-cost adsorbents (purified raw attapulgite (A-ATP), high-temperature-calcined attapulgite (T-ATP), and hydrothermal loading of MgO (MgO-ATP)) were prepared as adsorbents for the removal of Cd(II) and Pb(II). By evaluating the effect of the initial solution pH, contact time, initial solution concentration, temperature and coexistence of metal ions on Cd(II) and Pb(II) adsorption, the experimental results showed that MgO-ATP was successfully prepared by hydrothermal reaction and calcination as well as appearing to be a promising excellent adsorbent. At an initial pH of 5.0, A-ATP, T-ATP and MgO-ATP reached maximum adsorption amounts of 43.5, 53.9 and 127.6 mg/g for Pb(II) and 10.9, 11.2, and 25.3 mg/g for Cd(II) at 298 K, respectively. The Cd(II) adsorption on A-ATP was fitted by the Freundlich model, while the adsorption of Pb(II) and Cd(II) on T-ATP and MgO-ATP as well as Pb(II) adsorption on A-ATP agreed with the Langmuir model. All kinetic experimental data favored pseudo second-order model. The calculated thermodynamic parameters suggested that Pb(II) adsorption onto MgO-ATP was spontaneous and exothermic. When considering foreign metal ions, the three adsorbents all presented preferential adsorption for Pb (II). Chemical adsorption had a high contribution to the removal of Cd(II) and Pb(II) by modified attapulgite. In summary, the adsorption was greatly enhanced by the hydrothermal loading of MgO. It aimed to provide insights into the MgO-ATP, which could be able to efficiently remove Cd(II) and Pb(II) and serve as an economic and promising adsorbent for heavy metal-contaminated environmental remediation.     

黄孢展齿革菌菌丝球同时吸附铅镉离子的动力学

采用间歇法，利用黄孢展齿革菌菌丝球吸附溶液中的Pb^2 和Cd^2 ，研究Pb^2 和Cd^2 共存体系中吸附初速率随初始浓度的变化规律。实验结果表明，少量Cd^2 的存在促进其对Pb^2 的吸附，并提高吸附初速率，但随着Cd^2 初始浓度的增加，促进作用逐渐减弱并转为抑制作用；Cd^2 的吸附初速率随着Pb^2 初始浓度增大而减小；Pb^2 和Cd^2 的吸附初速率都随自身初始浓度的增加而增大。     

磁性纳米粒子富集-电感耦合等离子体发射光谱法测定食具中铬、镍、镉、铅、砷的迁移量

采用氩电弧等离子体法制备磁性碳包铁纳米粒子,考察了其对水溶液中Cr,Ni,Cd,Pb和As的富集能力,建立电感耦合等离子体原子发射光谱同时测定食具中Cr,Ni,Cd,Pb和As迁移量的分析方法。研究了纳米粒子表面经H2O2处理后,pH值、吸附时间、吸附剂用量等因素对各元素富集效率的影响。结果表明,H2O2表面处理可有效提高纳米粒子对待检元素的吸附率。在pH 8.0～9.5范围内,选用30 mg碳包铁纳米粒子定量富集,振荡3 min后,Cr,Ni,Cd,Pb和As均可被磁性碳包铁纳米粒子定量富集,酸性溶液(pH 1～2)可洗脱吸附离子。采用本方法测定了实际样品,各元素回收率在87%～106%之间。     

Lead and Cadmium Adsorption onto Iron Oxides and Manganese Oxides in the Natural Surface Coatings Collected on Natural Substances in the Songhua River of China

Natural surface coatings collected from natural substances(NSCsNS)were employed to study the roles of the main chemical components(iron oxides,manganese oxides,and other components)in controlling the adsorption of lead(Pb)and cadmium(Cd)in aquatic environments.The selective chemical extraction followed by the adsorption of Pb and Cd experiments and statistical analysis,were used to investigate the adsorption property of each component.Hydroxylamine hydrochloride was used to remove manganese oxides selectively,and sodium dithionite was used to extract iron oxides and manganese oxides.The result indicated that iron oxides and manganese oxides played an important role in the adsorption of Pb and Cd on NSCsNS,and the relative contribution was about two-thirds.The contribution of manganese oxides was the greatest,with a lesser role indicated for other components.The adsorption ability of manganese oxides for Pb and Cd was greater than that of iron oxides or other components for Pb and Cd.The Pb adsorption observed in each component was greater than Cd adsorption.