Cloud Point Extraction and Separation of Scandium and Yttrium (III) with Triton X‐114 in the Presence or Absence 8‐Hydroquiloline as an Added Chelate

Abstract

In this paper, the cloud point extraction and separation of scandium and yttrium (III) via use of Triton X‐114 with and without 8‐hydroquiloline (HQ) as an added chelate agent are investigated. The effects of various parameters, such as the aqueous phase pH, HQ concentration, Triton X‐114 concentration, heating temperature, and incubation time, on the cloud point extraction of scandium and yttrium (III) are studied. The results demonstrate that, there are different extraction and separation behaviors for scandium and yttrium (III) with and without HQ as an added chelate. And in contrast to solvent extraction, cloud point extraction is an excellent method to extract and separate scandium and yttrium (III).     

Cloud Point Extraction and Preconcentration for the Determination of Cu and Ni in Natural Water by Flame Atomic Absorption Spectrometry

Abstract

In this work, a new cloud point extraction (CPE) method was developed for the separation and preconcentration of copper and nickel. The analyte was complexed with 3‐[(8‐{[(E)‐2‐hydroxyimino‐1‐methylpropylidene] amino}‐1‐naphthyl) imino]‐2‐butanone oxime (H₂mdo) in the initial aqueous solution and octylphenoxy polyethoxy ethanol (Triton X‐114) was added as a surfactant. After phase separation, based on the cloud point in the mixture, and dilution of the surfactant‐rich phase with methanol containing 0.1 mol l^?1 HNO₃, the enriched analytes were determined by flame atomic absorption spectrometry. After optimization of the complexation and extraction conditions (i.e. pH=8.5, H₂mdo=3×10^?4 mol l^?1, Triton X‐114=0.1% (w/v)) the enhancement factors of 65 and 59 and detection limits of 0.14 and 0.2 ng ml^?1 were obtained for copper and nickel respectively. The proposed method was applied to the determination of copper and nickel in several natural water samples with satisfactory results.     

Temperature‐induced surfactant‐ mediated pre‐concentration of uranium assisted by complexation

Cloud‐point extraction (CPE) was used with lipophilic chelating agent to extract uranium(VI) from aqueous solutions. The methodology used is based on the formation of metal complexes soluble in a micellar phase of a non‐ionic surfactant, Triton X‐114. The metal ions complexes are then extracted into the surfactant‐rich phase at a temperature above the cloud‐point temperature. The influence of surfactant concentration on extraction efficiency was studied and the advantage of adding 8‐hydroxyquinoline (8HQ) as lipophilic chelating agent was evidenced. High extraction efficiency was observed, indicating the feasibility of extracting U(VI) using CPE. This study describes a four‐step process—(1) extraction, (2) thermo‐induced phase splitting, (3) back‐extraction and (4) second phase splitting—for the recovery of uranium from water. In our conditions, the extraction yield is quantitative and the concentration factor obtained is superior to 100. After stripping with a diluted nitric acid solution (pH < 1), the system can be recycled through a new four‐step cycle. Copyright © 2006 Society of Chemical Industry     

Recovery of polyphenols from camu-camu (Myrciaria dubia H.B.K. McVaugh) depulping residue by cloud point extraction

In this study the potential of cloud point extraction formed by a non-ionic surfactant was used in order to separate polyphenols from industrial residues of camu-camu. The effects of operational conditions of the cloud point extraction (CPE) on the polyphenol recovery and volumetric ratio were investigated. The results showed a maximum recovery of 95.71% that was obtained using 7.0 wt% Triton X-114, native pH (3.25), and 80 wt% polyphenol extract at 30 °C. The use of cloud point extraction was successful to recover the polyphenols from agroindustrial residue since it is a simple as well as of low-cost technique.     

Micelle‐Mediated Extraction for Direct Spectrophotometric Determination of Trace Uranium(VI) in Water Samples

Abstract

The possibility of using Dibenzoylmethane (DBM) for uranium(VI) concentrating by the way of micellar extraction at cloud point temperature and later spectrophotometric determination was investigated. Under the optimum conditions, preconcentration of 50 mL of water samples in the presence of 0.2% (w/v) octylphenoxypolyethoxy ethanol (Triton X‐114), 2×10^?4 mol L^?1 DBM and 2×10^?3 mol L^?1 buffer solution (pH=9) gave a limit of detection 11 ng mL^?1, and the calibration graph was linear in the range of 15–300 ng mL^?1. The recovery under optimum working conditions was higher than 98%.

The proposed method has been applied to the spectrophotometric determination of uranium(VI) in natural water samples after cloud point extraction with satisfactory results.     

Cloud Point Extraction of Glycyrrhizic Acid from Licorice Root

Abstract

An attempt has been made to extract glycyrrhizic acid (GA) from licorice root by surfactant mediated cloud point extraction (CPE) using non‐ionic surfactant (Triton X‐100). Almost all of the GA molecules were concentrated in the surfactant‐rich phase (also called coacervate phase) after phase separation. The pH is the most critical factor regulating the distribution of GA in the micelle which related to the ionization form. The other effects of the concentration of GA and the surfactant, the temperature, and the salt concentration on the extraction efficiency of GA in the coacervate phase and aqueous phase have been studied. The mechanism of CPE of GA was explored with transmitting electron microscopy. It was deduced that aggregate GA molecules were adsorbed on micelles' outer poler mantle and inner cross‐linked micelles at high GA concentrations in coacervate phase.     

Aqueous Surfactant Two‐Phase Systems for the Continuous Countercurrent Cloud Point Extraction

Aqueous nonionic surfactant solutions split into two phases if the temperature is increased beyond a certain temperature, the so‐called cloud point temperature. Presently many different types of nonionic surfactants are produced commercially, out of these numerous have been considered as potential solvent for the cloud point extraction. In this work the crucial thermophysical properties of nonionic surfactants are investigated to determine the potential of surfactant systems for extraction processes. Phase equilibria of the binary system Triton X‐114/water and the ternary system Triton X‐114/water/phenol were measured. Based on these data the cloud point extraction was implemented in a continuous stirred extraction column. It was found, that increasing temperature within the column reduces the loss of surfactant and leads to an increasing enrichment factor. This work demonstrates that surfactant/water systems represent a suitable alternative to conventional solvents and can effectively be processed in continuous extraction columns.     

Partitioning equilibria in multicomponent surfactant systems for design of surfactant-based extraction processes

Aqueous biphasic systems based on nonionic surfactants have perspective applications in extraction processes, in particular, cloud point extraction of hazardous compounds or high valued products, especially biomolecules. Additives (e.g., ionic surfactants, salts) and variations in pH can significantly affect the surfactant-based separation processes, representing an additional degree of freedom for their optimization. However, there are few systematic studies of phase and partition behavior for these multicomponent surfactant systems.In this study we examined the clouding, phase compositions and partitioning equilibria for aqueous mixed surfactant systems of a nonionic surfactant (Triton X-114), ionic surfactants (cetyltrimethylammonium bromide or sodium dodecyl sulfate) and NaCl, in order to improve the extraction efficiency. Vanillin was used as a model substance at three different pH values, specifically in (partly) dissociated or non-dissociated states. The partition coefficients obtained in the batch experiments were compared to the predictions by the thermodynamic model COSMO-RS. Based on this knowledge a continuous multistep extraction process was carried out.To the best of our knowledge this is the first demonstration of using a mixed surfactant system for continuous countercurrent cloud point extraction.     

Cloud Point Extraction of Four Triphenylmethane Dyes by Triton X-114 as Nonionic Surfactant

A method for removing four triphenylmethane dyes from wastewater by cloud point extraction with the nonionic surfactant Triton X-114 (TX-114) was developed. The triphenylmethane dyes were crystal violet, ethyl violet, malachite green and brilliant green. The cloud point of TX-114 generally increased in the presence of any of the four dyes. In the cloud point system, these dyes were solubilized into a coacervate phase that left a color-free dilute phase. The extraction efficiency of the dyes increased with the temperature, TX-114 concentration, and salt (NaCl and CaCl₂) concentration. More than 97% TX-114 in the dilute phase was recovered by adjusting the volume ratio of dichloromethane to the dilute phase. The Langmuir-type adsorption isotherm was used to describe the dye solubilization. The Langmuir constants m and n were calculated as functions of temperature. The results showed that the solubilization of the triphenylmethane dyes in the cloud point system was related to the partition coefficient and their molecular structures.     

Separation of Neutral Red and Methylene Blue from Wastewater using Two Aqueous Phase Extraction Methods

Abstract

The aim of this work was the two‐aqueous phase extraction of neutral red and methylene blue from wastewater. This has been achieved on the basis of phase separation properties of non‐ionic surfactants above the so‐called cloud point curve and the solubilization phenomena of coacervate micelles (surfactant rich phase). Three commercial surfactants were used in this work; the Oxo‐C₁₅E₇ which is an ethoxylate fatty alcohol (Dehydol LT 7), Triton X‐114 (iso‐C₈H₁₇‐C₆H₄‐(OCH₂CH₂)_7,5OH), and Triton X‐100 (iso‐C₈H₁₇‐C₆H₄‐(OCH₂CH₂)_9,5OH) which are alkyl phenol ethoxylate surfactants. The phase diagrams of binary water/surfactants systems were drawn and the effect of sodium sulphate on water‐surfactant systems was therefore studied. Oxo‐C₁₅E₇ and Triton X‐114 were used for the cloud point extraction of neutral red and methylene blue from their aqueous solutions at 100 mg/L and 7 mg/L, respectively. The experimental extraction results were expressed by the following three responses: percentage of the extracted dye (E), residual concentrations of dye in the dilute phase (X_s,w), and the volume fraction of coacervate (φ_C) at the equilibrium. The results obtained for each parameter were also represented on three‐dimensional diagrams using an empirical smoothing method. The empirical modelling data were in agreement with the experimental ones. The main advantage was sought between E, which has reached 99% in the case of neutral red, whereas in the case of mehtylene blue 92% was obtained with respect to (φ_C), which should have a minimum value. At the optimal conditions, neutral red and methylene blue concentrations in the effluent were reduced to about 500 times and 7 times, respectively.     

Room temperature ionic liquid,cetyl pyridinium naphthenate,supported cloud point extractive separation and ultra trace determination of copper in blood and environmental samples

A new unconventional room temperature ionic liquid, cetyl pyridinium naphthenate (CPN) was synthesized and was ascertained by IR, NMR and CHN analysis. Cloud point extraction of Cu(II) was carried out by using CPN for a synergistic enhancement effect. Triton X 100 was used as surfactant in cloud point extraction and cloud point temperature was 750 C. Quantification was carried out by FAAS. The mean recovery, enrichment factor, tolerance limit, RSD, LOD and LOQ were found to be 99.8%, 40, 1000 ppm, 0.15%, 27 ppt and 93 ppt respectively. Method was validated by analyzing natural water and blood samples.     

Micelle-Mediated Extraction and Cloud Point Preconcentration of Chlorophylls from Spinach

A micelle-mediated extraction and cloud point preconcentration of chlorophylls method was developed. Non-ionic surfactant (Genapol X-080) was employed as an alternative and effective extraction solvent. The optimal extraction parameters based on the micelle extraction technique were determined. Under optimal conditions, i.e., 5% Genapol X-080 (v/v), pH 9.0, liquid/solid ratio of 10:1 (mL g^?1), ultrasonic-assisted extraction for 30 min, extraction amount reached the highest value. For the preconcentration of chlorophylls by cloud point extraction (CPE), the solution was incubated at 50° for 30 min, and 0.1 g mL^?1 sodium chloride was added to the solution to facilitate the phase separation. The microstructure of coacervate phase after CPE was explored with transmitting electron microscopy. The preconcentration factor for chlorophylls was about 12.5, the extraction recovery approached 99.2%, and the loading capacity was about 1 mg mL^?1. Thus coupling of ultrasonic-assisted micelle extraction and cloud point extraction could be employed as a new and effective technique for the rapid extraction and preconcentration of chlorophylls from plants such as spinach.     

Removal of Copper(II) from a Concentrated Sulphate Medium by Cloud Point Extraction Using an N,N′-Bis(salicylaldehyde)Ethylenediimine Di-Schiff Base Chelating Ligand

Various chelating ligands have been investigated for the cloud point extraction of several metal ions. However, limited studies on the use of the Schiff base ligands have been reported. In this work, cloud point extraction behavior of copper(II) with N,N′‐bis(salicylaldehyde)Ethylenediimine Schiff base chelating ligand, (H₂SALEN), was investigated in aqueous concentrated sulphate medium. The extraction process used is based on the formation of hydrophobic H₂SALEN–copper(II) complexes that are solubilized in the micellar phase of a non‐ionic surfactant, i.e. ethoxylated (9.5EO) tert‐butylphenol. The copper(II) complexes are then extracted into the surfactant‐rich phase above cloud point temperature. Different parameters affecting the extraction process of Cu(II), such as equilibrium pH, extractant concentration, and non‐ionic surfactant concentration were explored. The extraction of Cu(II) was studied in the pH range of 2–11. The results obtained showed that it was profoundly influenced by the pH of the aqueous medium. The concentration factor, C_f, of about 17 with extraction efficiency of E % ≈100 was achieved. The stoichiometry of the extracted complex of copper(II) was ascertained by the Yoe–Jones method to give a composition of 1:1 (Cu:H₂L). The optimum conditions of the extraction‐removal have been established as the following: (1) 1.86 × 10^?3 mol/L ligand; (2) 3 wt% surfactant; (3) pH of 8 (4) 0.5 mol/L Na₂SO₄ and (5) temperature of 60 °C.     

An economic and sensitive method for extracting chromium speciation in airborne inhalable dust,using a green sample treatment coupled with electrothermal atomic absorption

ABSTRACT

A new approach of cloud point extraction CPE procedure is optimized for hexavalent chromium determination in airborne dusts. Triton X-114 is used as a surfactant and 1-(2-pyridylazo)-2-naphthol as a specific complexing agent for the trivalent chromium’s removal from the aqueous phase to isolate hexavalent chromium compounds. The parameters influencing the extraction protocol (pH, surfactant concentration, and temperature are optimized. The obtained detection and quantification limits are 0.1 and 0.4 μg/L, respectively. The linearity is verified, with a regression coefficient close to 0.999 and the extraction recovery exceeds 99%. The method was successfully applied to analyze airborne samples collected from workplaces.     

浊点萃取-分光光度法测定硫酸阿米卡星

文章建立了硫酸阿米卡星的浊点萃取-紫外可见分光光度检测法。在酸性条件下,以溴麝香草酚蓝(BTB)为显色剂,TritonX-100非离子型表面活性剂浊点萃取硫酸阿米卡星。考察了pH、TritonX-100用量、水浴温度和水浴时间对萃取率的影响,优化了浊点萃取条件。在0.5～3.5μg·mL-1范围内线性关系良好,r=0.9996(n=7),高、中、低三个水平的回收率在92.9%～107.8%之间,大多数离子不干扰测定。本方法用于市售注射剂及人体尿液中硫酸阿米卡星含量的测定,结果令人满意。     

Extraction of Parabens from Water Samples Using Cloud Point Extraction with a Non-Ionic Surfactant with β-Cyclodextrin as Modifier

A cloud point extraction process using a silicone non-ionic surfactant to extract selected parabens compounds from water samples was investigated using reversed phase high performance liquid chromatography. The cloud point extraction process, in the presence of β-cyclodextrin (β-CD) as a modifier, is a new extraction process which was optimized with five parameters, i.e. salt concentration, pH of the solution, temperature, surfactant concentration and β-CD concentration. The developed method with the β-CD modifier results in an excellent performance on detection of parabens from water samples with limits of detection in the range of 0.017–0.043 μg/L and percentage recoveries from 90.5 to 98.9 %.     

浊点萃取-FAAS法测定化妆品中六价铬

提出了浊点萃取-火焰原子吸收光谱法测定化妆品中痕量六价铬的方法。考察了溶液pH、APDC用量、Triton X-114用量、平衡温度及时间等条件对浊点萃取率的影响,在优化条件下,对化妆品进行测定。该方法测定铬的检出限为0.026 mg/L,相对标准偏差为1.52%。结果表明：市售多数化妆品中的铬含量超过国家标准,须引起质量监督部门的注意。     

浊点萃取—火焰原子吸收光谱法测定痕量镉

以1-（2-吡啶偶氮）-2-萘酚（PAN）为络合剂、以Triton X—100为表面活性剂进行浊点萃取建立了浊点萃取——火焰原子吸收光谱法测定痕量镉的方法。探讨了络合剂的浓度、溶液的pH,缓冲溶液的浓度、表面活性剂的浓度等影响浊点萃取的因素。该方法用于自来水、湖水、雨水中痕量镉的测定,具有低毒,高效,安全,简便等特点。     

Synthesis of amphiphilic polyurethane nanonetwork particles and their application for the soil‐washing process

Nanosized amphiphilic polyurethane (APU) particles synthesized on the basis of amphiphilic urethane acrylate nonionomers could solubilize phenanthrene within their hydrophobic interiors in the same way that surfactant micelles do in the aqueous phase. At low concentrations of APU or Triton X‐100 in the aqueous phase, APU particles exhibited a greater extraction efficiency of sorbed phenanthrene than did the Triton X‐100 aqueous pseudophase. At higher APU particle and Triton X‐100 doses in aqueous solution, the extraction efficiency of the APU aqueous solution was almost same as that of the Triton X‐100 aqueous solution, even though APU particles exhibited a lower solubilizing efficiency than Triton X‐100 micelles in the absence of aquifer soil. This was because APU particles have a relatively low degree of sorption on aquifer sand because of their chemically crosslinked structure. APU particles could be also recovered at a rate of 100% through an ultrafiltration process at a greater pore size of the separation membrane, which would make soil washing with APU particles more economical and useful in practical applications. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 87: 1666–1677, 2003     

A new method for analysis of sunset yellow in food samples based on cloud point extraction prior to spectrophotometric determination

A simple new micelle mediated preconcentration method was developed for analysis of sunset yellow (SY) prior to its spectrophotometric determination. The method was based upon cloud point extraction of the ion associate of SY and trioctylamine (TOA) in HCl–Triton X-100. In the surfactant phase the SY species react with TOA yielding hydrophobic ion associate of SY^?·TOA⁺. The distribution coefficient of SY between surfactant-rich phase and aqueous phase was approximately 104. Validation was tested by comparing the results with standard HPLC. Isotherm and thermodynamic parameters, chemical equilibrium, extraction constants and stiochiometry of the associate were assigned.