Application of multiwalled carbon nanotubes treated by potassium permanganate for determination of trace cadmium prior to flame atomic absorption spectrometry

In this study we investigated the enrichment ability of oxidized multiwalled carbon nanotubes （MWCNTs） and established a new method for the determination of trace cadmium in environment with flame atomic absorption spectrometry. The MWCNTs were oxidized by potassium permanganate under appropriate conditions before use as preconcentration packing. Parameters influencing the recoveries of target analytes were optimized. Under optimal conditions, the target analyte exhibited a good linearity （R^2=0.9992） over the concentration range 0.5-50 ng/ml. The detection limit and precision of the proposed method were 0.15 ng/ml and 2.06%, respectively. The proposed method was applied to the determination of cadmium in real-world environmental samples and the recoveries were in the range of 91.3%-108.0%. All these experimental results indicated that this new procedure could be applied to the determination of trace cadmium in environmental waters.

Preconcentration of copper with multi-walled carbon nanotubes pretreated by potassium permanganate cartridge for solid phase extraction prior to flame atomic absorption spectrometry

A procedure for the preconcentration of copper was described in this paper using multi-walled carbon nanotubes (MWCNTs) oxidized by potassium permanganate as the adsorbent for the enrichment of trace copper in water samples. Important parameters, such as the sample pH, the concentration and volume of eluent, sample flow rate and volume, and interference of coexisting ions, were investigated. The obtained results indicated that proposed method possessed an excellent analytical performance. The linear range, the detection limit, and precison (RSD) were 1–100 ng/mL (R(2) = 0.9993), 0.32 ng/mL and 2.88%, respectively. The results showed that copper could be adsorbed quantitatively on the pretreated MWCNTs with potassium permanganate, and proposed method was very useful in the monitoring of copper in the environment.

Preconcentration of Lead in Sugar Samples by Solid Phase Extraction and Its Determination by Flame Atomic Absorption Spectrometry

A simple and sensitive solid phase extraction utilizing C18 filled cartridges incorporated with dithizone for preconcentration of lead and its subsequent determination by flame atomic absorption spectrometry (FAAS) was developed. Several parameters such as type, concentration and volume of eluent, pH of the sample solution, flow rate of extraction and volume of the sample were evaluated. The effect of a variety of ions on preconcentration and recovery was also investigated. At pH = 7.4 and 1.0 mol?L–1 HCl eluting them, lead ions were recovered quantitatively. The limit of detection (LOD) defined as 3Sbl was determined to be 8.1 μg L–1 for 500 mL of sample solution and eluted with 5 mL of 1.0 mol?L–1 HCl under optimum conditions. The accuracy and precision (RSD %) of the method were >90% and <10%, respectively. In the end, the proposed method was applied to a number of real sugar samples and the amount of lead was determined by spiking a known concentration of lead into the solution.

The Use of Multiwalled Carbon Nanotubes Mini Column for Preconcentration of Trace Metal Ions in Tap Water of Khartoum City and Their Determination by Flame Atomic Absorption Spectrometry （FAAS）

The adsorption behavior of multiwalled carbon nanotubes （MWNTs） toward heavy elements has been investigated systemically, and a new method has been developed for the determination of trace elements in water samples based on preconcentration with mini-column packed with MWNTs prior to its determination by flame atomic absorption spectrometry （FAAS） The recommended parameters of proposed method influencing the preconcentration of the analytes, such as pH of the sample, sample flow rate and volume, elute solution and interfering ions, have been used. Under the optimized conditions, the calibration graphs were linear with the correlation coefficient range 0.9981-0.9995. According to the results, the metals were found 0.019-0.051, 0.011-0.031, 0.00-0.081, 0.00-0.0002, 0.007-0.0925, 0.00-0.0104 μg/L in water samples for Pb, Mn, Zn, Cd, Fe, Cu respectively. The percentage relative standard deviation （%RSD） for five replicate samples were 〈 5% in all cases. The method has been successfully applied to the determination of trace elements in some environmental samples with satisfactory results.

Preconcentration of Cadmium in Environmental Samples by Cloud Point Extraction and Determination by FAAS

Cloud point extraction (CPE) has been used for the preconcentration of cadmium, after the formation of a complex with 1, 5-bis(di-2-pyridylmethylene) thiocarbonohydrazide (DPTH), and further determination by flame atomic absorption spectrometry (FAAS) using Triton X-114 as surfactant. The main factors affecting the CPE, such as concentration of Triton X-114 and DPTH, pH, equilibration temperature and incubation time, were optimized for the best extract efficiency. Under the optimum conditions i.e., pH 5.4, [DPTH] = 6x10-3%, [Triton X-114] = 0.25% (v/v), an enhancement factor of 10.5 fold was reached. The lower limit of detection (LOD) obtained under the optimal conditions was 0.95 μg L?1. The precision for 8 replicate deter- minations at 20 and 100 μgL?1 Cd were 2.4 % and 2 % relative standard deviation (R.S.D.). The calibration graph using the preconcentration method was linear with a correlation coefficient of 0,998 at levels close to the detection limit up to at least 200 μgL?1. The method was successfully applied to the determination of cadmium in water, environmental and food samples and in a BCR-176 standard reference material.

Preconcentration and Determination of Trace Amounts of Heavy Metals in Water Samples Using Membrane Disk and Flame Atomic Absorption Spectrometry

A fast and simple method for preconcentration of Ni^2＋, Cd^2＋, Pb^2＋, Zn^2＋, Cu^2＋ and Co^2＋ from natural water samples was developed. The metal ions were complexed with sodium diethyldithiocarbamate （Na-DDTC）, then adsorbed onto octadecyl silica membrane disk, recovered and determined by FAAS. Extraction efficiency, influence of sample volume and eluent flow rates, effects of pH, amount of Na-DDTC, nature and amount of eluent for elution of metal ions from membrane disk, break through volume and limit of detection have been evaluated. The effect of foreign ions on the percent recovery of heavy metal ions has also been studied. The limit of detection of the proposed method for Ni^2＋, Cd^2＋, Pb^2＋, Zn^2＋, Cu^2＋ and Co^2＋was found to be 2.03, 0.47, 3.13, 0.44, 1.24 and 2.05 ng·mL^-1, respectively. The proposed （DDTC） method has been successfully applied to the recovery and determination of heavy metal ions in different water samples.

Determination of Trace Amounts of Zinc, Iron and Copper by Flame Atomic Absorption after Their Preconcentration Using Sodium Dodecyl Sulfate (SDS) Coated Alumina Nanoparticles Modified with 3-Mercapto-D-Valin from Environmental Samples

A sensitive and simple solid phase extraction method for the simultaneous determination of trace and toxic metals in environmental samples has been reported. The method is based on the adsorption of Zinc, Iron and Copper on SDS-coated alumina nanoparticles, which is also modified with 3-mercapto-D-valine. The retained analyte ions on modified solid phase were eluted using 5 mL of 4 mol·L﹣1 HNO3. The analyte determination was carried out by flame atomic absorption spectrometry. The influences of some metal ion and anions on the recoveries of understudy analyte ion were investigated. The influences of the analytical parameters including pH, ligand and SDS amount, eluting solution (type and concentrations) and sample volume on metal ions recoveries were investigated. The extraction efficiency was > 98% with relative standard deviation lower than 3% the method has been successfully applied for the extraction and determination of these ions content in some real samples. Prepared adsorbent was characterized by SEM and FT-IR measurements.

Preconcentration and Determination of Chromium Species Using Octadecyl Silica Membrane Disks and Flame Atomic Absorption Spectrometry

A novel and selective method for the fast determination of trace amounts of chromium species in water samples has been developed. The procedure is based on the selective formation of chromium diethyldithiocarbamate complexes at different pH in the presence of Mn（Ⅱ） as an enhancement agent of chromium signals followed by elution with organic eluents and determination by atomic flame absorption spectrometry. The maximum capacity of the employed disks was found to be （396±3） pg and （376±2） pg for Cr（Ⅲ） and Cr（Ⅵ）, respectively. The detection limit of the proposed method is 49 and 43 ng·L^-1 for Cr（Ⅲ） and Cr（Ⅵ）, respectively. The proposed method was successfully applied for determination of chromium species Cr（Ⅲ） and Cr（Ⅵ） in different water samples.

无机-有机复合材料沸石@聚丙烯酰胺的制备及对Pb^(2+)的吸附研究

重金属污染会引起严峻的环境问题。因此,必须对重金属离子进行测定,但由于重金属离子的含量低并受基体效应影响,检测前需要先将其分离富集。利用一锅法制备沸石@聚丙烯酰胺复合材料,将其作为分离富集材料,结合火焰原子吸收光谱仪,研究对Pb^(2+)的吸附性能。为了得到最佳的吸附性能,对制备条件中的沸石用量进行了优化,并对优化后的复合材料进行了扫描电镜、热重分析和比表面积表征。利用单一变量法,对固相萃取条件中的溶液pH值和振荡时间进行了优化。研究了复合材料在吸附Pb^(2+)过程中的动力学模型、等温线模型和热力学参数。结果表明:在沸石用量为333 mg/g,溶液pH值为5和振荡时间为80 min时,复合材料的吸附效率最佳;沸石@聚丙烯酰胺复合材料吸附Pb^(2+)的过程符合二级动力学和Freundlich模型,且在298.15 K时,热力学参数ΔH=15614.18 J/mol、ΔS=65.2 J/(mol·K)、ΔG=-1878.059 J/mol,是一个吸热且熵增的自发过程;此外,复合材料经过连续三次吸附和解吸实验,对Pb^(2+)的吸附量基本不变,且解吸率保持在89.7%以上,说明沸石@聚丙烯酰胺复合材料具有较好的再生性能。

Preconcentration and Determination of Copper（Ⅱ） Using Octadecyl Silica Membrane Disks Modified by 1,5-Diphenylcarhazide and Flame Atomic Absorption Spectrometry

A simple and reproducible method for the rapid extraction and determination of trace amounts of copper（Ⅱ） ions using octadecyl-bonded silica membrane disks modified by 1,5-diphenylcarbazide （DPC） and atomic absorption spectrometry was presented, which was based on complex formation on the surface of the ENVI-18 DISK^TM disks followed by stripping of the retained species by minimum amounts of appropriate organic solvents. The elution was efficient and quantitative. The effect of potential interfering ions, pH, ligand amount, stripping solvent, and sample flow rate were also investigated. Under the optimal experimental conditions, the break-through volume was found to be about 1000 mL providing a preconcentration factor of 400. The maximum capacity of the disks was found to be （255±5） lag for Cu^2＋, and the limit of detection of the proposed method was 5 ng per 1000 mL. The method was applied to the extraction and recovery of copper in different water samples.

沸石改性聚丙烯酰胺复合材料对铜的吸附性能研究

重金属污染是严峻的问题,其难以被生物降解,会进入动植物体,传播至生态系统,最终危及人类健康。因此,必须对重金属离子进行测定,但由于重金属离子的含量低并受基质效应影响,需要先将其分离和富集。固相萃取是一种简单、成本低、环保的方法。本论文合成了沸石改性聚丙烯酰胺复合材料,将其作为铜分离富集材料,结合火焰原子分光光度计,对铜进行了测定;为了得到最佳的吸附性能,优化了固相萃取条件,包括pH值和吸附时间;研究了沸石改性聚丙烯酰胺复合材料在吸附铜过程中的动力学、等温线和热力学模型。

Solid Phase Extraction of Trace Copper（Ⅱ） Using Octadecyl Silica Membrane Disks Modified with N,N′-Disalicylideneethylenediamine

A simple and reproducible method for the rapid extraction and determination of trace amounts of copper（Ⅱ） ions using octadecyl-bonded silica membrane disks modified by N,N′-disalicylideneethylenediamine （DESDA） and atomic absorption spectrometry was presented. The method is based on complex formation on the surface of the ENVI-18 DISK^TM disks followed by stripping of the retained species by minimum amounts of appropriate organic solvents. The elution is efficient and quantitative. The effects of potential interfering ions, pH, ligand amount, stripping solvent, and sample flow rate were also investigated. Under the optimal experimental conditions, the break-through volume was found to about be 1000 mL providing a preconcentration factor of 500. The maximum capacity of the disks was found to be （389±4） μg for Cu^2＋. The limit of detection of the proposed method is 5 ng per liter. The method was applied to the extraction and recovery of copper in different water samples.

乙醇-硫酸铵双水相萃取-火焰原子吸收光谱法测定镉

建立了萃取镉的乙醇-硫酸铵双水相体系。以火焰原子吸收光谱法(FAAS)为检测手段,研究了乙醇-硫酸铵双水相萃取镉的主要影响因素,并且利用FT-IR光谱,对其萃取机理进行了初步的探讨。实验结果表明,Cd2+与I-、结晶紫在pH5.0～6.0的乙醇-硫酸铵双水相体系中形成稳定的紫色络合物,在最佳萃取条件下,镉能很好地与其他常见的金属离子分离,萃取率达到100%。该方法测定镉的线性范围为0～0.50μg/mL,相关线性系数为0.9993,方法检出限为0.012μg/mL。用于环境水样中镉量的测定,相对标准偏差为为2.8%～3.6%,加标回收率大于95%。

浊点萃取-火焰原子吸收光谱法测定大米样品中的痕量镉

以Triton X-114为表面活性剂,基于甲基绿（MG）与CdI42-形成疏水性离子缔合物的浊点萃取新体系.详细考察了pH值、KI及MG溶液浓度、Triton X-114体积分数等因素对浊点萃取的影响,建立了浊点萃取-火焰原子吸收光谱法测定大米样品中痕量镉的新方法.在最佳条件下,该法检测限（3σ）为0.90 ng/mL,相对标准偏差RSD为4.2%（c=50.0 ng/mL,n=7）.将该法成功应用于大米样品中痕量镉的测定,其回收率在91.0%~107.0%.

析相萃取富集火焰原子吸收法测定矿样中的金

提出了析相萃取火焰原子吸收光谱法测定矿样中金的新方法 ,讨论在TritonX -10 0体系中、在辛醇及无机盐存在下的析相萃取条件 ,方法检出限为 0 0 0 6 4μg/ml。用于岩矿中金的测定 。

以负载5-(2-羟基-5-硝基苯偶氮)-硫代若丹宁石墨化碳黑作吸附剂的固相萃取-火焰原子吸收光谱法测定金

制备了负载5-（2-羟基-5-硝基苯偶氮）-硫代若丹宁（HNATR）的多孔石墨化碳黑并用作分离金的固相萃取柱填充剂。含金样品以1.0 mol/L的磷酸介质过柱，金定量吸附在小柱上，用0.1 mol/L的硫代硫酸钠洗脱小柱上富集的金，可实现样品中低浓度金的高倍数富集和与大部分干扰离子的分离。用火焰原子吸收光谱法测定洗脱液中的金，在选定实验条件下，吸光度与Au（Ⅲ）含量在0.05-3.0μg/mL范围内呈线性关系，线性回归方程的相关系数r=0.999 6；方法用于矿石和环境水样中金的测定，相对标准偏差在2.2%-3.2%之间，加入标准回收率在88%-104%之间。

磁性固相萃取-火焰原子吸收光谱法测定工业废水中的Cu^(2+)

以Fe_3O_4/多壁碳纳米管/壳聚糖(Fe_3O_4/MWCNTs/CS)磁性纳米粒子为吸附剂填装于固相萃取柱中,用于分离工业废水中的Cu^(2+),采用火焰原子吸收光谱法测定Cu^(2+)。当吸附剂用量为30mg,样品溶液体积为40.0mL,样品溶液pH 7.0,流量为30μL·s^(-1)时,用0.5mol·L^(-1)HCl以10μL·s^(-1)的流量进行洗脱,Cu^(2+)的富集倍数达40。Cu^(2+)的线性范围为0.1~30.0μg·L^(-1),检出限(3s/k)为0.012μg·L^(-1)。方法应用于实际样品的分析,加标回收率在98.9%~102%之间,测定值的相对标准偏差(n=3)小于4%。

浊点萃取-火焰原子吸收光谱法测定水样中的痕量镉

研究了以二乙胺基二硫代甲酸钠（DDTC）为配位剂、Triton X-114为表面活性剂的浊点萃取-火焰原子吸收光谱法测定痕量镉的实验方法。探讨了溶液pH值、试剂质量浓度、平衡温度等实验条件对浊点萃取效率的影响。在最优条件下，镉的检测限为0.238μg／L，富集倍数为55，加标回收率为98％-102％。方法用于水样中痕量镉的测定，结果令人满意。

固相萃取富集-火焰原子吸收分光光度法测定水中的镉

强阴离子交换固相萃取柱萃取富集 ,火焰原子吸收分光光度法测定环境水样中镉 ,方法相对标准偏差在 2 .5 %— 3.5 %之间 ,加标回收率在 97%— 1 0 4 %之间 。

析相萃取火焰原子吸收光谱法测定水样中痕量铁

研究了析相萃取火焰原子吸收光谱法测定水样中铁的方法 ,在酸性条件下 ,Fe3 + 与SCN- 生成络合物 ,在适当的温度下 ,被TritonX 10 0 正辛醇 水体系萃取富集。析出相用火焰原子吸收进行测定。方法检出限为 0 .0 0 4 μg·ml- 1,用于水样中痕量铁的测定 。