乳状液膜法分离水中镉

本文报道了用乳状液膜法分离镉的研究。在此分离体系中,以煤油作为膜溶剂,span80为表面活性剂,磷酸三丁酯(TBP)为载体,液体石蜡为膜增强剂。详细讨论了制乳时间、混合时间、搅拌速度,span80、TBP以及液体石蜡的浓度,乳水比和油内比,内相氨水和外相HCl溶液的浓度对分离的影响,确立了最佳分离条件。     

液膜法分离钴和镍

钻、镍的分离一直受到关注，人们先后利用离子交换法［’‘、色谱法［’‘、苹取法「’‘等方法对它们在水溶液中共存时进行了分离．本文利用液膜法将共存的微量钻、镍一步分离开，同时富集了钻离子．利用液膜富集和分离钻、镍，大量工作是针对它们的富集；对其实施分离，报道甚少［‘·’‘，且分离效果不够满意．将EDTA作为掩蔽剂应用于钻、镍的分离，尚未见报道·仪器为721型分光光度计（上海第三分析仪器厂），PHS－ZC精密酸度计（上海雷磁仪器厂）．试剂为2一乙基已基单2一乙基己基磷酸酯（P507，中国科学院上海有机化学研究所），…     

微晶三苯甲烷分离富集和测定痕量镉

镉是一种广泛分布于环境中并严重危及生物体健康的有毒重金属元素之一[1].但由于环境水样中Cd(II)的含量低而难于直接测定.浊点萃取法[2]、液膜法[3]及固相萃取法[4]等被用来分离富集Cd(II).但这些方法不能直接用于大体积(如1L)水样中痕量金属离子的分离与富集,且萃取相 (浊点相[2],有机膜相[3],固相萃取剂[4])的制备程序较为复杂.本文建立了负载氯化十四烷基二甲基苄基铵(Zeph)的微晶三苯甲烷分离富集痕量Cd(II)的新方法.     

液膜预富集水相痕量镍的分析研究

研究了液膜体系对水相中痕量镍离子的富集方法,镍离子从外相水溶液被膜相载体通过液膜运进含有反萃取剂的内相,从而达到富集效果,液膜富集一次回收率达98％,二闪富集倍数250倍,试验了载体,表面活性剂,液体石蜡,膜与内相水的水／油比,乳化液与外相水的乳／水比,内相酸度,外相PH值,富集时间的破乳剂用量等因素的影响,利用正交分析试验选出了最佳试验条件,并比较在相同条件下液膜法与萃取法提取镍的效果,通过液膜富集,使原子吸收法测定痕量镍达到了10^-9级。     

离子液体[Bmim]PF6萃取-火焰原子吸收法测定水中痕量镉

1引言化学工业排放的废水含有大量金属镉,对环境产生严重危害,因而环境水样中痕量镉的准确测定具有重要意义。目前,常用原子吸收光谱法[1]测定痕量的镉,但由于环境水样中镉的含量低且样品复杂,为了提高分析方法的灵敏度和选择性,样品的预分离与富集至关重要。液-液萃取是一种常用的预分离与富集方法,但常用有机溶剂作萃取剂,易带来二     

准液膜-火焰原子吸收光谱法测定水中痕量铬

用选择性好,富集倍数高的液膜法处理含铬废水已有报道[1]。本文在文献[2,3]的基础上,进一步探讨了准液膜的富集行为,确立了以液膜体系富集铬的最佳试验条件,并用于废水中铬的测定,得到了满意的结果。1　试验部分1.1　主要仪器与试剂WYX 402A型原子吸收分光光度计(沈阳分析仪器厂),准液膜体系富集装置(自制,见图1)。　　　　图1　准液膜体系富集装置Fig.1　Preconcentrationinstallationofthequasi 　　　　　　liquid membrane　　1.料液池(Cellforsamplesolution)　　2.分离柱(Separationcolumn)　　3.解吸剂池(Cellforabsorbent)…     

微量Cu2+的乳化液膜法富集分离及原子吸收光谱测定

微量Cu2+的乳化液膜法富集分离及原子吸收光谱测定;Cu2+; 乳状液膜; 分离; 富集; 原子吸收光谱     

微晶酚酞-乙基紫分离富集镉(Ⅱ)

微晶酚酞-乙基紫分离富集镉(Ⅱ);微晶酚酞;乙基紫;分离富集;镉(Ⅱ)     

印迹壳聚糖/凹土分离富集-FAAS测定水中痕量镉

建立了用离子印迹壳聚糖/凹土(ⅡGA)分离富集-火焰原子吸收光谱(FAAS)测定痕量镉的新方法.在动态吸附条件下,系统地研究了溶液pH值、流速、洗脱条件和干扰离子对痕量镉分离富集的影响;在pH4.5、上样流速为0.60 mL/min的条件下,镉能被ⅡCA定量富集;吸附的镉可用1.0 mol/L HCl-0.1 mol/...     

壳聚糖富集火焰原子吸收法测定天然水口痕量镉

提出了壳聚糖分离富集火焰原子吸收法检测水中痕量镉的新方法，研究了富集的最佳条件及洗脱方法。回收率达９８％，灵敏度０．０２１μｇ．Ｌ＾－１。方法灵敏度高，选择性好，用于天然水中痕量镉的测定，获得满意结果。     

Solid-phase extraction and determination of ultra trace amounts of lead,mercury and cadmium in water samples using octadecyl silica membrane disks modified with 5,5′-dithiobis(2-nitrobenzoic acid) and atomic absorption spectrometry

A simple and fast method for preconcentration and determination of ultra trace amounts of lead(II), mercury(II) and cadmium(II) in water samples is presented. Lead, mercury and cadmium adsorbed quantitatively during passage of water samples (pH?=?7, flow rate?=?20 mL min^?1) through octadecyl silica membrane disks modified with 5,5′-dithiobis(2-nitrobenzoic acid). The retained lead, mercury and cadmium are then stripped from the disk with a minimal amount of 1 M hydrochloric acid solution as eluent, and determined by atomic absorption spectrometry. The influence of flow rates of the eluent and sample solution, the amount of ligand, type and least amount of eluent, pH of sample, effect of other ions and breakthrough volume are determined. The breakthrough volume of the method is greater than 2000 mL for lead and greater than 1500 mL for mercury and cadmium, which results in an enrichment factor of 200 for lead and an enrichment factor of 150 for both mercury and cadmium. The limit of detection of the proposed method is 177, 2 and 13 ng l^?1 for lead, mercury and cadmium, respectively.     

Direct spectrophotometric measurements of acid-catalyzed complexation of palladium(II) with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol at the heptane/water interface by a centrifugal liquid membrane method.

The centrifugal liquid membrane (CLM) method, designed for the rapid sample injection, was applied to the kinetic study of the complexation of palladium(II) with 2-(5-bromo-2-pyridylazo)-5-diethyaminophenol (5-Br-PADAP) in the heptane/water system. The formation rates of Pd(II)-5-Br-PADAP complex, which existed only at the heptane/water interface, could be directly measured by the CLM method combined with transmission spectrophotometry. We found that the formation rates of Pd(II)-5-Br-PADAP complex were accelerated by the protonation of 5-Br-PADAP at the diethylamino-group that did not coordinate to Pd(II) ion and that the rate constant for the reaction of protonated 5-Br-PADAP at the interface was close to that in the aqueous phase. The present study demonstrated that the CLM method was easily applicable for the measurements of relatively fast interfacial reactions.     

Determination of lead, cadmium and mercury in microwave-digested foodstuffs by RP-HPLC with an on-line enrichment technique.

A new method for the simultaneous determination of lead, cadmium and mercury ions in microwave-digested foodstuffs by reversed-phase high-performance liquid chromatography combined with on-line enrichment technique has been developed. The foodstuff samples were digested by microwave digestion. The lead, cadmium and mercury ions can be precolumn derivatized with 5,10,15,20-tetrakis(3-aminophenyl)porphine (T3APP) to form color chelates; then, the Hg-T3APP, Cd-T3APP and Pb-T3APP chelates can be enriched and separated on a valve switching HPLC system combined with on-line enrichment technique. The linearity ranges are 0.01-120 microg/l for each metal ion. The detection limits (S/N = 3) of lead, cadmium and mercury are 1.2 ng/l, 0.5 ng/l and 0.8 ng/l, respectively. This method was applied to the determination of lead, cadmium and mercury in foodstuffs with good results.     

Measurement of circular dichroism spectra of liquid/liquid interface by centrifugal liquid membrane method.

The direct measurement of the circular dichroism (CD) spectra of liquid/liquid interface has been achieved for the first time by the centrifugal liquid membrane (CLM) method combined with a conventional CD spectropolarimetry. In the sample chamber of the CD spectropolarimeter, a cylindrical glass cell containing small amounts of organic and aqueous phases was rotated at ca. 7000 rpm to generate a two-phase liquid membrane with a high specific interfacial area. The CD spectra of the J-aggregate of protonated 5,10,15,20-tetraphenylporphyrin formed at the toluene/sulfuric acid interface in the rotating cell have been measured. The results demonstrated the novelty and advantages of this method.     

Simultaneous determination of four heavy metal ions in tobacco and tobacco additive by online enrichment followed by RP-HPLC and microwave digestion

A new method for the simultaneous determination of tin, lead, cadmium, and mercury in tobacco and tobacco additive by reversed-phase high-performance liquid chromatography combined with microwave digestion and an online enrichment technique is developed. The tin, lead, cadmium, and mercury ions are precolumn derivatized with tetra-(4-dimethylaminophenyl)-porphyrin (T(4)-DMAPP) to form color chelates. The Sn-T(4)-DMAPP, Hg-T(4)-DMAPP, Cd-T(4)-DMAPP, and Pb-T(4)-DMAPP chelates are absorbed onto the front of the enrichment column using a buffer solution of 0.05 mol/L pyrrolidine-acetic acid (pH = 10.0) as the mobile phase. After the concentration is finished (by switching the six-port switching valve) the retained chelates are back-flushed by the mobile phase and move to the analytical column. The chelate separation on the analytical column is satisfactory using gradient elution with methanol (containing 0.05 mol/L pyrrolidine-acetic acid buffer salt, pH = 10.0) and tetrahydrofuran (containing 0.05 mol/L pyrrolidine-acetic acid buffer salt, pH = 10.0). The linearity range is 0.01-120 micro g/L for each metal ion. The detection limits (S/N = 3) of tin, lead, cadmium, and mercury are 0.6, 0.8, 0.5, and 0.6 ng/L, respectively. This method is applied to the determination of tin, lead, cadmium, and mercury in tobacco and it's additive with good results.     

Solidified floating organic drop microextraction for pre-concentration and trace monitoring of cadmium ions in environmental food and water samples

In this research, solidified floating organic drop microextraction as an efficient sample preparation method was used for trace monitoring of cadmium ions in environmental samples. In this method, a free microdroplet of 1-undecanol is floated on the surface of aqueous solution and agitated by a stirring bar placed on the bottom of the sample vial. Cadmium ions were complexed with neocuproine to obtain hydrophobic complex and extracted to extraction solvent. The extracted target ions were determined by flow injection–flame atomic absorption spectrometry. The effect of important factors on the extraction of target ions by the proposed sample preparation method was evaluated and optimized. The limit of detection, relative standard deviation (%) and enrichment factor of the method were 0.02, 3.7 and 98.5%, respectively. The validation of the method was examined by the analysis of cadmium ions in the certified reference material (sea food mix), and the obtained data can proof the reliability of the method for trace detection of cadmium ions. The method was successfully applied for determination of cadmium in the real food and water samples, and satisfactory relative recoveries (97–102%) were achieved.     

混合金属络合物羟基镍铝交联蒙托土的表面酸性及催化性能

用NH_3-TPD,IR技术研究了混合金属络合物羟基镍铝交联蒙托土的表面羟基和表面酸性。考察了制备方法、Al/Ni比对其表面酸性的影响,同时用异丙苯裂解反应表征了其催化性能。结果表明,交联蒙托土存在L酸和B酸,其中以L酸为主。表面酸性可能来源于柱子和表面羟基,柱子的热稳定性对表面羟基,表面酸性均有较大影响。Ni的引入增加了L酸和B酸,取代法制备的样品具有比共聚法的样品更强的酸性。交联蒙托土具有较好的异丙苯裂解性能,Ni的引入使其活性有较大的增加。     

Determination of trace lead, cadmium and mercury by on-line column enrichment followed by RP-HPLC as metal-tetra-(4-bromophenyl)-porphyrin chelates

This paper reports the utilization of tetra-(4-bromophenyl)-porphyrin (T(4)BPP) as a chelating reagent using Waters Xterratrade mark RP(18) column for the on-line column enrichment and the separation of trace lead, cadmium and mercury ions by reversed-phase high-performance liquid chromatography (RP-HPLC) with photodiode array detector. When the Hg-T(4)BPP, Pb-T(4)BPP and Cd-T(4)BPP chelates were injected into the injector and sent to the enrichment column with 0.05 mol l(-1) of pH 10.0 pyrrolidine-phosphoric acid buffer solution (containing 10% of tetrahydrofuran (THF)) as mobile phase. The chelates were retained on the top of the enrichment column. After the enrichment is finished, by switching the valve of six-ports switching valve, the retained metal-T(4)BPP chelates will be eluted by mobile phase in reverse direction and will travel towards analytical column. With THF (containing 0.05 mol l(-1), pH 10.0 pyrrolidine-phosphoric acid buffer salt) and 0.05 mol l(-1), pH 10.0 pyrrolidine-phosphoric acid buffer solution (containinging 10% THF) gradient elution as mobile phase, the chelates separation on the analytical column was satisfactory. The linearity ranges are 0.01-120 mug l(-1) for each metal ion. The detection limits (S/N=3) of lead, cadmium and mercury are 1.0, 0.5 and 1.0 ng l(-1), respectively. This method can be applied to the determination (mug l(-1)) level of lead, cadmium and mercury in drinking water with satisfactory results.     

Ionic liquid-based hollow fiber supported liquid membrane extraction combined with thermospray flame furnace AAS for the determination of cadmium

We have developed a simple and effective method for hollow fiber liquid-phase microextraction of cadmium. It is based on the use of a room temperature ionic liquid (RTIL) and was coupled to thermospray flame furnace AAS. The RTIL was placed in the pores of a polypropylene hollow fiber (acting as a liquid membrane) and also used as the acceptor solution. Ammonium pyrrolidinedithiocarbamate (APDC) was used as the chelating agent. The effects of the concentration of APDC, the pH of samples, stirring rates, extraction time, and potential interferences were optimized to result in a detection limit of 9?ng?L^?1 and an enrichment factor of 90. The relative standard deviation is 4.7% (at 0.5?ng?mL^?1, for n?=?5). The method was successfully applied to the determination of cadmium.