Ligand-less in situ surfactant-based solid phase extraction for preconcentration of silver from natural water samples prior to its determination by atomic absorption spectroscopy

A simple and rapid ligand-less in situ surfactant-based solid phase extraction method for preconcentration of silver from water samples is developed. In this method, a cationic surfactant containing a proper alkyl group (n-dodecyltrimethylammonium bromide) is dissolved in the aqueous sample and then a proper ion-pairing agent (ClO₄^?) is added. Due to the interaction between surfactant and ion-pairing agent, solid particles are formed and used for adsorption of silver carbonate. After centrifugation, the sediment is dissolved in 2.0 mL 1 M HNO₃ in ethanol and then aspirated directly into the flame atomic absorption spectrometer. Variables affecting the extraction efficiencies such as pH, concentrations of surfactant and CO₃^2?, ion pair concentration, and extraction time, are optimized. Under such conditions, the calibration curve is linear from 3 to 700 μg L^?1. Detection limit is 1.1 μg L^?1 with an enrichment factor of 37. The relative standard deviation for eight replicate measurements of 100 μg L^?1 is 2.1%. The method has been applied for the determination of silver in water samples.     

Preconcentration of samarium with modified yeast cells for its determination by atomic emission spectroscopy

A chelating-modified biosorbent is produced by coupling of a dye, procion red, to yeast cells. The resulting modified cells have been characterized by Fourier transform infrared, elemental analysis and thermogravimetric analysis and studied for preconcentration and determination of trace Sm(III). The optimum pH value for sorption of the samarium ions is 6.2. The sorption capacity of functionalized modified yeast cells is 7.2 mg g^?1. Recovery was 99% when Sm(III) was eluted with an aqueous solution of 0.1 mol L^?1 ethylenediaminetetraacetic acid. Scatchard analysis suggested that binding sites were homogeneous. The equilibrium data were analyzed using Langmuir, Freundlich, Temkin, and Redlich–Peterson isotherm models, and the respective constants were determined as 1.0 (L mg^?1), 2.9 [(mg g^?1) (L mg^?1)^1/n], 2.4 × 10⁸ (L g^?1), and 30 (dm³ g^?1) at 20 °C. The method was applied for an Sm(III)-containing sample of ceramic industry effluent.     

Removal of textile dyes from aqueous solution using PEG based aqueous biphasic system

Aqueous biphasic systems (ABSs) composed of polyethylene glycol (PEG) and salt have been examined for the removal of textile dyes from textile effluent. The partitioning of four dyes namely Cibacron Scarlet LS 2G, Rhodamine B, Brown ERN and Astacryl Red 3B was investigated. All the dyes studied were found to partition into the upper PEG rich layer. Sodium carbonate was found to be the most efficient salt for extraction of dyes. Sodium sulphate was found to be marginally less efficient. Sodium chloride did not cause partitioning at all. Partitioning occurred at all pH and was almost pH independent. The partitioning of these dyes in larger volume (100?mL) ABS was also demonstrated. Studies using dye bath effluent were also conducted. In all cases very high efficiencies consistently above 98% were obtained.     

Solid phase extraction of trace metals from environmental samples using Amberlite XAD-7 loaded with 2-hydroxy-propiophenone-4-phenyl-3-thiosemicarbazone and determination by inductively coupled plasma–atomic emission spectrometry

A method for the solid phase extraction of trace metals, namely Co, Cu, Pb, Ni and Zn, from environmental and biological samples using column Amberlite XAD-7 loaded with 2-hydroxy-propiophenone-4-phenyl-3-thiosemicarbazone (HPPPTSC) and determination by inductively coupled spectrometry (ICP–AES) has been developed. The reagent has the capacity to form chelate complexes with the metals because of three binding sites in the reagent molecule. The optimum experimental conditions for the quantitative sorption of five metals, pH, effect of flow rate, concentration of eluent, sorption capacity and the effect of diverse ions on the preconcentration of analytes have been investigated. The sorption capacity of the resin has 83, 127, 35, 88 and 85?µmol?g^?1 for Co²⁺, Cu²⁺, Pb²⁺, Ni²⁺ and Zn²⁺, respectively. The preconcentration factors for Co²⁺, Cu²⁺, Pb²⁺, Ni²⁺ and Zn²⁺ were 100, 110, 120, 140 and 150, respectively. The accuracy of the proposed procedure was evaluated by standard reference materials. The achieved results were in good agreement with certified values. The proposed method was applied for the determination of trace metals in river water and plant leaves.     

Study of atrazine degradation in soil from Kenyan sugarcane-cultivated fields in controlled laboratory conditions

A study to compare the extent of atrazine mineralization in soils from Kenyan sugarcane-cultivated fields with and without history of atrazine use was carried out in the laboratory under controlled conditions. The study was testing the hypothesis that repeated atrazine application to soil will not result in enhanced atrazine mineralization. The study was carried out with ¹⁴C-uniformly ring-labeled atrazine in a laboratory under controlled conditions. Atrazine mineralization to ¹⁴CO₂ in soil with no history of atrazine use was negligible (0.16%) after 163 days of soil incubation. The three metabolites hydroxyatrazine, desisopropylatrazine, and desethylatrazine in the proportion of 17.7%, 1.3%, and 2.6%, respectively, were in the soil after 75 days. In the soil from the sugarcane-cultivated field with history of atrazine use, atrazine mineralization was 89.9% after 98 days. The same soil, amended with mature compost, showed a lag phase of eight days before rapid atrazine mineralization was observed.     

干扰素生产废水处理试验及生物相分析

采用水解酸化与生物接触氧化组合工艺对干扰素生产废水进行试验研究,并考察其处理效果,观察生物接触氧化工艺中生物相。结果表明：该组合工艺对出水COD的去除率大于90%,出水COD低于40 mg/L,且运行稳定后生物接触氧化槽中污泥浓度较低。对生物相的显微镜观察可知生物接触氧化槽中生物相种类以藻类为主。     

稻田样品中丁虫腈及其代谢产物的残留分析方法

建立了固相萃取-气相色谱法同时测定稻田环境样品中丁虫腈及其代谢产物的残留分析方法,即:稻田水样品以二氯甲烷萃取,水稻土样品以丙酮提取后再经乙酸乙酯萃取,稻株样品以乙腈提取后用CarbonNH2固相萃取小柱净化,然后均用气相色谱-电子捕获检测器(GC-ECD)检测。结果表明,稻田水中丁虫腈及其代谢产物的最低检测质量浓度均为0.01 mg·L-1,土壤和水稻植株中目标物最低检测质量含量为0.015 mg·kg-1。在该方法条件下,当添加水平为0.05～1.0 mg·L-1(或mg·kg-1)时,稻田水、土壤和水稻植株中丁虫腈及其代谢产物的平均回收率为75.1%～109.2%,变异系数为1.0%～7.9%。     

矿井瓦斯液相催化氧化制甲醇的理论初探

提出了以瓦斯气中的氧气作为氧化剂,选用适当的催化剂对瓦斯气中的甲烷进行直接催化氧化合成甲醇的研究思路。从甲烷液相催化氧化反应机理入手,围绕着矿井瓦斯部分氧化制甲醇的热力学、甲烷液相部分氧化制甲醇的研究基础、瓦斯中氮气的防爆惰化作用及构建的实验系统几个方面对矿井瓦斯液相催化氧化制甲醇的可行性进行了探讨。     

基于改进极端学习机的混沌时间序列瓦斯涌出量预测

为更准确地预测瓦斯涌出量,预防瓦斯灾害,有必要建立和应用基于改进极端学习机(IELM)的混沌时间序列预测模型。首先,对瓦斯涌出量监测数据构成的多变量时间序列进行相空间重构,采用互信息法与虚假邻点法得到每一变量的延迟时间和最佳嵌入维数;然后,通过最小二乘方法和误差反馈原理计算出最优的网络输入层到隐含层的学习参数,对极端学习机(ELM)进行改进;最后,借助IELM建立瓦斯混沌时间序列的预测模型。通过仿真试验,运用该预测模型预测的最大相对误差为3.290 2%,最小相对误差为0.898 2%,平均相对误差为1.952 8%。     

液相色谱-电喷雾质谱法测定污水和污泥中壬基酚聚氧乙烯醚的参数优化

在液相色谱-电喷雾质谱法测定壬基酚聚氧乙烯醚的过程中,对壬基酚聚氧乙烯醚加合离子的形成影响因素进行分析,优化了关键参数,建立了测定污水和污泥中壬基酚聚氧乙烯醚的高分辨高灵敏的液相色谱-电喷雾质谱方法.流动相A为0.1mmol·l~(-1)乙酸钠缓冲液,流动相B为甲醇,各聚合度壬基酚聚氧乙烯醚的加合离子响应值达到最大;锥孔电压没为60V能最大程度上避免[NPnEO+2Na]~(2+)对测定的干扰.NP1EO,NP2EO和NPnEOs(n=3-15)的仪器检出限分别为10pg,1pg和0.1pg.该方法成功用于污水和污泥中壬基酚聚氧乙烯醚的测定.