微晶酚酞预富集-分光光度法测定痕量Co(Ⅱ)

建立了一种以微晶酚酞作为固态吸附剂对样品中痕量的Co（Ⅱ）分离富集的新方法,富集后的co（Ⅱ）可直接用光度法测定。控制一定条件,Co（Ⅱ）能与常见阳离子Ni（Ⅱ）、Cd（Ⅱ）、Al（Ⅲ）、Ca（Ⅱ）、Mg（Ⅱ）、Pb（Ⅱ）、Mn（Ⅱ）、Fe（Ⅲ）、Bi（Ⅲ）等完全分离,且富集时基本不受SO4^2-、NO3^-、Br^-、Cl^-、I^-等阴离子影响。微晶酚酞对Co（Ⅱ）的吸附容量为23．5mg／g;富集因数可达200倍,回收率在97．6％以上,RSD为1．1％～2．3％。已用于环境水样及日常用水中Co（Ⅱ）的富集测定。     

微晶酚酞分离富集分光光度法测定铊(Ⅲ)

建立了利用无毒的微晶酚酞作为固相萃取剂分离富集溶液中痕量Tl(Ⅲ)的方法。在H3PO4介质中,Tl(Ⅲ)在水相中与I-和结晶紫(CV+)形成离子缔合物而被微晶酚酞定量吸附,富集后的Tl(Ⅲ)可直接用光度法测定。控制一定的条件,Tl(Ⅲ)能与常见离子Na+,K+,Al3+,Cu2+,Pb2+,Zn2+,Ba2+,Mn2+,Ca2+,Cd2+,Fe2+等完全分离,且基本不受Cl-,Br-,SO42-,NO3-等阴离子的影响。方法可直接应用于环境水样中痕量Tl3+的测定,富集倍数可达100倍,回收率95.6%~101.8%,检出限为13 ng/L。     

甲基紫修饰的微晶酚酞分离富集-光度法测定痕量铋(Ⅲ)的研究

建立了以修饰有甲基紫(MV)的微晶酚酞作为固相吸附剂分离富集和测定环境样品中痕量Bi(Ⅲ)的新方法.研究表明,Bi(Ⅲ)与I-、 MV 形成三元离子缔合物[BiI6] (MV)3能定量吸附在微晶酚酞上,在适当条件下,Bi(Ⅲ)能与Co(Ⅱ)、 Ni(Ⅱ)、 Mn(Ⅱ)、 Fe(Ⅱ)、 Al(Ⅲ)、 Zn(Ⅱ)等常见阳离子分离,且基本不受Br-、 SCN-、 SO42-、 NO3-、 Cl-、 ClO4-等阴离子影响.Bi(Ⅲ)的静态吸附容量为0.81 mmol/g,富集因数可达200倍,回收率在97.2%以上,RSD 1.3%～2.2%之间.已应用于环境水样中Bi(Ⅲ)的测定.     

负载乙基紫的微晶酚酞吸附富集-分光光度法测定水中痕量钒

建立了以微晶酚酞作为吸附剂分离富集环境水样中痕量钒的新方法。研究表明,当pH值在3.7～7.0时,溶液中以V3O39-存在形式为主的钒,与乙基紫阳离子(EV )形成的离子缔合物(V3O93-).(EV )3能被微晶酚酞定量吸附,在钒被富集的同时并能使其与常见阳离子Co(Ⅱ)、Ni(Ⅱ)、Zn(Ⅱ)、Cd(Ⅱ)、Al(Ⅲ)、Cu(Ⅱ)、Hg(Ⅱ)、Pb(Ⅱ)、Mn(Ⅱ)、Fe(Ⅲ)、Cr(Ⅲ)等完全分离,且基本不受能与EV 形成离子缔合物的阴离子SO24-、NO3-、Br-、Cl-、I-、ClO4-的影响。分别在1.0L不同环境水样中加入5.00mL1.0×10-3mol/LEV 及1.0mL0.10mol/LHCl(调溶液pH值约为4.0)和5.00mL15.8%的酚酞乙醇溶液,搅拌约50min,能够使水样中的痕量钒得到很好的富集。富集因数达100～200倍,回收率在98.0%以上,RSD为1.1%～2.3%。     

微晶酚酞富集-分光光度法测定痕量Zn(II)

建立了一种利用修饰有结晶紫(CV^＋)的微晶酚酞作为固态吸附剂分离富集溶液中痕量Zn(II)的新方法, 富集后的Zn(II)含量可直接用光度法测定. 控制一定条件, Zn(II)能与常见阳离子Ni(II), Cd(II), Al(III), Ca(II), Mg(II), Co(II), Mn(II), Cu(II), Pb(II), Fe(III)等完全分离, 且富集时基本不受, , Br^－, Cl^－, I^－,等阴离子影响. 微晶酚酞对Zn(II)的吸附容量为25.8 mg/g; 富集因数可达200倍, 回收率在97.7%～102%之间, RSD小于2.7%. 该方法已成功应用于实际水样中Zn(II)的富集测定, 结果令人满意.     

微晶酚酞富集-分光光度法测定痕量Zn(II)

建立了一种利用修饰有结晶紫(CV^＋)的微晶酚酞作为固态吸附剂分离富集溶液中痕量Zn(II)的新方法, 富集后的Zn(II)含量可直接用光度法测定. 控制一定条件, Zn(II)能与常见阳离子Ni(II), Cd(II), Al(III), Ca(II), Mg(II), Co(II), Mn(II), Cu(II), Pb(II), Fe(III)等完全分离, 且富集时基本不受, , Br^－, Cl^－, I^－,等阴离子影响. 微晶酚酞对Zn(II)的吸附容量为25.8 mg/g; 富集因数可达200倍, 回收率在97.7%～102%之间, RSD小于2.7%. 该方法已成功应用于实际水样中Zn(II)的富集测定, 结果令人满意.     

硫酸铵-碘化钾-乙基紫体系浮选分离Pb(Ⅱ)

铅;硫酸铵-碘化钾-乙基紫体系浮选分离Pb(Ⅱ)     

无机盐存在下双水相体系萃取分离碘-乙基紫-镉(Ⅱ)缔合物

研究了在丙醇-水体系中加入表面活性剂乙基紫(EV)后,影响Cd2 分离的酸度、无机盐、卤离子种类等条件。实验表明,(NH4)2SO4存在下,无表面活性剂EV,一定量的I-,在酸性条件下,Cd2 的萃取率为68%,而同样条件下,加入mg级表面活性剂EV后,Cd2 与EV、г形成三元缔合物,被均相萃取、异相分离;缔合物进入丙醇相,Cd2 被完全萃取分离;在pH 1.0时,试验了Cd2 加入量为5μg/mL时与Fe3 、Co2 、Ni2 、Zn2 、Mn2 、Zn2 、Cr3 的二元或多元离子混合液的分离试验,分离完全。     

负载十四烷基二甲基苄基铵的微晶三苯甲烷分离富集痕量Cu(Ⅱ)

在SCN-存在下,Cu(Ⅱ)与SCN-形成的Cu(SCN)42-可被吸附在负载氯化十四烷基苄基铵(Zeph)的微晶三苯甲烷(TPM)上。在最佳条件下,Cu(Ⅱ)能与常见阳离子Fe(Ⅲ)、Ni(Ⅱ)、Cr(Ⅲ)、Al(Ⅲ)、Mn(Ⅱ)、Pb(Ⅱ)、Cd(Ⅱ)等完全分离,且富集时基本不受SO24-、NO3-、SCN-、Br-、Cl-、ClO4-的影响。富集因子可达100倍,回收率在91%以上。该方法已成功用于环境水样中Cu(Ⅱ)的富集与测定。     

碘化钾-乙基紫-水体系固相浮选分离镉的研究

研究了碘化钾 乙基紫 水体系固相浮选分离镉的行为及与常见金属离子分离的最佳条件。试验表明,将碘化钾溶液、乙基紫溶液和盐酸溶液混合稀释,生成稳定的CdI2-4·(EV+)2三元缔合物可很快浮于水相,使Cd(Ⅱ)被定量浮选。控制适当条件,可实现Cd(Ⅱ)与常见金属离子Mn(Ⅱ)、Al(Ⅲ)、Ni(Ⅱ)、Zn(Ⅱ)之间的分离。对合成水样进行了浮选分离测定,结果满意。     

Cadmium Preconcentration from Aqueous Environmental Samples Using Microcrystalline Phenolphthalein Modified by Crystal Violet

Abstract

The present work describes a novel method for cadmium preconcentration and separation with microcrystalline phenolphthalein. Phenolphthalein as an extractant modified by crystal violet was originally applied to cadmium extraction from aqueous solution. Cadmium(II) as CdI₃ ^? and CdI₄ ^2? can associate with the cationic crystal violet (CV⁺) forming water‐insoluble ion‐association complexes (CdI₃ ^?) · (CV⁺) and (CdI₄ ^2?) · (CV⁺)₂, which are quantitatively adsorbed on microcrystalline phenolphthalein over the pH range from 1.0 to 6.0. All experimental parameters necessary for successful preconcentration and separation have been investigated and optimized. The study shows that common metal ions, such as Zn(II), Fe(II), Co(II), Ni(II), Mn(II), Cr(III) and Al(III), cannot interfere with cadmium extraction in this microcrystalline system by controlling acidity. The extraction can be accomplished in 15 min. The interaction between CdI₃ ^?and CdI₄ ^2? and CV⁺ plays an important role in the extraction process. The reported method was successfully applied to the preconcentration and separation of cadmium in synthetic samples and real samples with satisfactory results. The results proved that it is an efficient and attractive technique for cadmium preconcentration and separation at trace level.     

用硫酸铵-碘化钾-结晶紫体系浮选分离镉

研究了硫酸铵－碘化钾－结晶紫体系浮选分离镉的行为及其与常见离子分离的条件,该体系能使Cd(Ⅱ）与常见离子Zn(Ⅱ）、Fe（Ⅲ）、Co(Ⅱ）、Ni(Ⅱ）、Mn(Ⅱ）、Al（Ⅲ）分离。     

Separation of Mercury with an Ammonium Sulfate‐Ammonium Thiocyanate‐Ethyl Violet Flotation System

The separation behavior of mercury by a flotation system consisting of ammonium sulfate, ammonium thiocyanate and ethyl violet, and the conditions for the separation of Hg(II) with other common metal ions have been studied. The studies show that in aqueous solutions, Hg(II) combines with NH₄SCN and ethyl violet(EV) into dissoluble ternary ion‐association complex [Hg(SCN)4^2?]?(EV)₂. In the presence of ammonium sulfate, the precipitate is floats well on the surface of the water phase and separates from water thoroughly. It shows that Hg(II) can be separated completely from Cd(II), Fe(II), Co(II), Ni(II), Mn(II) and Al(III) by flotation at pH1.0. The flotation mechanism of Hg(II) is described in this paper.     

硫酸铵存在下碘化物—结晶紫—丙醇体系萃取分离镉

研究了硫酸铵存在下，碘化物－结晶紫－丙醇体系萃取镉的行为以及丙醇水溶液的分相条件，试验表明，丙醇作为萃取溶剂，能萃取中性离子缔合物，调节溶液ｐＨ＝１．０或ｐＨ＝４．０，该体系使能Ｃｄ＾２＋，从常见过渡元素Ｆｅ＾３＋，Ｃｏ＾２＋，Ｎｉ＾２＋，Ｍｎ＾２＋，Ｚｎ＾２＋，Ｃｒ＾３＋的混合液中分离出来。     

Study on Determination of Trace Nickel in Water Samples after Separation/enrichment using Microcrystalline Phenolphthalein Loaded with Chelate

The paper presents a novel method for the separation/enrichment of trace Ni²⁺ using microcrystalline phenolphthalein loaded with chelate prior to the determination by spectrophotometry. The effects of different parameters, such as the dosages of phenolphthalein and sodium diethyldithiocarbamate (DDTC), various salts and acidity on the enrichment yield of Ni²⁺ have been investigated to select the experimental conditions. The possible enrichment mechanism of Ni²⁺ was discussed. The results showed that under the optimum conditions, Ni²⁺ could be quantificationally adsorbed on the surface of microcrystalline phenolphthalein in the form of the chelate precipitate of Ni(DDTC)₂, while K⁺, Na⁺, Ca²⁺, Mg²⁺, Zn²⁺, Fe²⁺, Al²⁺, Pb²⁺ and Cd²⁺ could not be adsorbed at all. Therefore, Ni²⁺ was completely separated from the above metal ions in the solution. A new method for the separation/enrichment and determination of trace nickel using microcrystalline phenolphthalein loaded with chelate was established. The proposed method has been successfully applied to the determination of Ni²⁺ in various water samples, and the results agreed well with those obtained by FAAS method.     

Study of the concentration and separation of cadmium with microcrystalline phenolphthalein modified by crystal violet

A new method for cadmium separation and concentration with microcrystalline phenolphthalein modified by crystal violet (CV) was developed in the paper. In the presence of potassium iodide (KI) and CV, cadmium are quantitatively absorbed on microcrystalline phenolphthalein in the pH range 1.0-6.0 as the forms of water-insoluble ion-associated complexes (CdI₃⁻)·(CV⁺) and (CdI₄²⁻)·(CV⁺)₂. Effect of different parameters such as phenolphthalein amount, stirring time, the concentration of CV and KI, various salts and metal ions was studied in detail. During the present study, a significant enhancement of the extraction of cadmium was observed. Cd(II) can be completely separated from Zn(II), Fe(II), Co(II), Ni(II), Mn(II), Cr(III) and Al(III) in this microcrystalline system and well concentrated without the interference of these metal ions at high level. The possible reactive mechanism of cadmium concentration has been discussed. Analytical results obtained by this new method were very gratifying.     

硝酸钠-碘化钾/孔雀绿-水体系浮选分离镉

硝酸钠-碘化钾/孔雀绿-水体系浮选分离镉