Separation and determination of the sulph-hydryl flotation collectors using ion-interaction chromatography

Summary This paper discusses simple and practical methods for the separation and determination of various sulph-hydryl flotation reagents by ion-interaction chromatography. Physical and chemical parameters such as column length, the support, and the constituents of the mobile phase and their respective concentrations were considered. A set of capacity factors, determined for a given set of conditions, is used to assist in the design of separation methods. The developed methodology enables the determination of various sulph-hydryl compounds in a given mixture of flotation reagents, distinction between compounds with the same functionality, and the separation of structural isomers of a particular compound. The applicability of the methods was demonstrated by the analysis of some commercial flotation reagents, as well as samples generated in an investigation of synergism of the sulp-hydryl collectors.     

Combination collectors in adsorption colloid flotation for multielement determination in waters by neutron activation

A method is described for the collection of small amounts of both anions and cations in water samples by adsorption colloid flotation with a combination collector, prior to quantitation by neutron activation. In the presence of 20 mg of iron(III) and 2 ml of 0.1 M ammonium pyrrolidinedithiocarbamate, As(V), Cd(II), Co(II), Cu(II), Hg(II), Mo(VI), Sn(IV), Sb(III), Te(VI), Ti(IV), U(VI), V(V) and W(VI) are quantitatively collected from 1 -l samples at a pH 5.8 ± 0.1; sodium dodecyl sulfate and sodium oleate are used as surfactant. Recoveries for all the elements tested are greater than 90%. Results for a number of elements in sea waer and an NBS water standard, SRM 1643a, are given.     

Optical sensors for determination of heavy metal ions

A review is given on optical means for single shot testing (probing) as well as continuous monitoring (sensing) of heavy metal ions (HMs). Following an introduction into indicator based approaches, we discuss the types of indicator dyes and polymeric supports used, as well as existing sensing schemes for HMs. The wealth of information is compiled in the form of tables and critically reviewed. Notwithstanding the tremendous work performed so far, it is obvious that still severe limitations do exist in terms of selectivity, limits of detection, dynamic ranges, applicability to specific problems, and reversibility. On the other hand, such sensors have found — and will find — their application whenever rapid and cost-effective testing is required, where personnel is scarce or unskilled, and in field tests. Despite their limitations, the number of such sensors (and of irreversible probes) for HMs is likely to increase in future.     

Nanoparticle flotation collectors II: the role of nanoparticle hydrophobicity

The ability of polystyrene nanoparticles to facilitate the froth flotation of glass beads was correlated to the hydrophobicity of the nanoparticles. Contact angle measurements were used to probe the hydrophobicity of hydrophilic glass surfaces decorated with hydrophobic nanoparticles. Both sessile water drop advancing angles, θ(a), and attached air bubble receding angle measurements, θ(r), were performed. For glass surfaces saturated with adsorbed nanoparticles, flotation recovery, a measure of flotation efficiency, increased with increasing values of each type of contact angle. As expected, the advancing water contact angle on nanoparticle-decorated, dry glass surfaces increased with surface coverage, the area fraction of glass covered with nanoparticles. However, the nanoparticles were far more effective at raising the contact angle than the Cassie-Baxter prediction, suggesting that with higher nanoparticle coverages the water did not completely wet the glass surfaces between the nanoparticles. A series of polystyrene nanoparticles was prepared to cover a range of surface energies. Water contact angle measurements, θ(np), on smooth polymer films formed from organic solutions of dissolved nanoparticles were used to rank the nanoparticles in terms of hydrophobicity. Glass spheres were saturated with adsorbed nanoparticles and were isolated by flotation. The minimum nanoparticle water contact angle to give high flotation recovery was in the range of 51° < θ(np(min)) ≤ 85°.     

Preconcentration and determination of trace metals in synthetic sea water by flotation with inert organic collectors

The preconcentration and separation of copper, cadmium, cobalt and nickel 8-quinolinolates in solutions of high salinity including synthetic sea water is studied with phenolphthalein or 2-naphthol as collector and octadecylamine as surfactant. A simplex optimization is applied. Yields > 90% are achieved for Ni, Co and Cd with both collectors, but the copper yield is low. Flame atomic absorption spectrometry is used for the final measurements.     

Complexing sorbents based on dispersed minerals for recovery of heavy metal ions from aqueous solutions

We have obtained sorbents for recovery of heavy metal ions from aqueous solutions by modification of kaolinite and metakaolinite, aluminum oxyhydroxide and aluminum hydroxide by polyphosphates. Using sorption of Ni²⁺, Co²⁺ and Cr³⁺ as an example, we have shown that the sorbents have high sorption capacity and distribution coefficient with respect to heavy metal ions. We have studied the composition of the complexes formed. We have developed methods for granulation of the sorbents with a binder and for regeneration of the sorbents. A. V. Dumanskii Institute of Colloid Chemistry and Chemistry of Water, National Academy of Sciences of Ukraine, 42 Bul'var Akademika Vernadskogo, Kiev-142 252680, Ukraine. Translated from Teoreticheskaya i éksperimental'naya Khimiya, Vol. 35, No. 3, pp. 167–170, May–June, 1999.     

Catalytic kinetic methods for photometric or fluorometric determination of heavy metal ions

An overview is presented on catalytic kinetic methods for heavy metal determination by photometry or fluorometry reported in recent years. The article summarizes the analytical procedures, the kinetics and reaction mechanisms of some typical methods, and their applications to real sample determination.     

A new microcolumn flotation cell for determining the wettability and floatability of minerals

Flotation is one of the most important physicochemical processes for mineral separations and other recovery operations. Flotation machines have been developed since the beginning of the 19th century and are still under intensive research and development. The cell we devised is a combination of the Canadian column flotation cell and the Partridge-Smith cell. The materials used for the construction of the new cell are cheap and use available laboratory accessories and aquarium materials. The cell functions well in terms of its scale, control, and sample requirement. It can be used both in the laboratory for research and in classrooms for demonstrations of experiments. Some of the data obtained by the flotation method using this cell are in good agreement with data measured independently on the same minerals by the contact angles method. The critical values of surface tension of wetting (gamma(c)) for talc, sulfur, and chemically treated surfaces of calcite and barite obtained by the contact angle measurements were 31, 26, 30.5, and 31.2 mN/m, respectively. On the other hand, the gamma(c) values of those minerals, obtained using our new designed flotation cell, were 30, 28, 31.4, and 34.5 mN/m, respectively. The measurements obtained in our experiment are also comparable to those previously published for the same minerals.     

HPLC determination of non-ionic surfactants used in tertiary oil recovery

Summary Having developed a chromatographic technique with a diol bonded phase for the study of the distribution versus ethylene oxide number (E.O.) for various non-ionic polyoxyethylated surfactants used in enhanced oil recovery (KL 6, ; KM 11, and KM 20, ) we report here the titration of one of these surfactants (KL 6) in the presence of an ionic surfactant (S 385, sulfonated petroleum fraction) and other non-ionic surfactants (KM 11 and/or KM 20) which are the conditions found in enhanced oil recovery. This work has been carried out in brine and in n-decane, as a model for the petroleum phase. Obviously in the case of aqueous phases it was necessary to carry out a thorough dehydration before the chromatographic analyses. We have shown that it is possible, under these conditions, to determine the KL 6 surfactant in the concentration range 500 to 6000 ppm with a precision of 70 ppm without experiencing interference from KM 11 or KM 20 non-ionic surfactants or S 385 ionic surfactant. Furthermore, from some of the samples studied which were in contact with the rock shale, we showed that strong adsorption of the KL 6 occurs. Chromatographic analyses show that this surfactant is only desorbed from the rock shale when employing a non-ionic surfactant such as KM 25 which is much more polar than the KL 6.     

HPLC determination of PAHs in mineral oils used as dispersing agents for herbicides

Summary The representative refined mineral oil samples, crude petroleum straightrun distillates, potentially used in the manufacture of crop protection products were analysed by isocratic and gradient high performance liquid chromatography (HPLC) to investigate their trace polycyclic aromatic hydrocarbon (PAH) content. Liquid-liquid extraction followed by size-exclusion column chromatography was employed to isolate the fraction containing PAHs with more than two fused rings. The identity of individual PAHs was confirmed by comparing their UV and fluorimetric detector signals with those recorded from reference standards. The level of extracted PAHs in the oil samples are discussed with respect to their physical and chemical properties.     

络合吸附伏安法同时测定多种重金属离子

在络合剂亚硝基苯胲 乙醇 乙酸铵体系中,Cr(Ⅵ)、Cd2 、Cu2 、Pb2 、Ni2 等离子都能在汞电极上产生灵敏的阴极络合吸附波,其二次导数伏安峰电流均与离子质量浓度有良好的线性关系,可用于这些离子的定量检测,测定线性范围为Cr(Ⅵ)0.0017～0.67μg mL、Cd2 0.0017～0.117μg mL、Cu2 0.0083～5 8μg mL、Pb2 0.083～1.25μg mL、Ni2 0.17～150μg mL,RSD分别为5.7%、1 3%、1.4%、2 5%和1.6%。方法为工业废水、地表水及生活用水等样品中重金属离子的同时测定提供了可靠、灵敏的检测方法。     

Solid-phase reagent for molecular spectroscopic determination of heavy metal speciation in natural water

A solid-phase reagent based on 1-(4-adamantyl-2-thiasolylazo)-2-naphthol adsorbed onto silica gel was prepared for Co(II) recovery and preconcentration prior to its sorption-spectroscopic detection. The immobilized reagent was applied to the determination of free cobalt ions in natural water. The solid-phase reagent and chemiluminescent method coupled with membrane filtration, gel-permeation and ion-exchange chromatography were applied to the study of the speciation of iron and cobalt in water from the Dnieper reservoirs and lakes of Kyiv City; their predominant forms were complexes of Fe(III) and Co(II) with dissolved organic matter and fulvic acids play a main role in their complexation.     

Spectrophotometric determination of flotation collectors and organic reagents in ore treatment process liquors and effluents with an atomic absorption spectrometer

An atomic absorption spectrometer has been adapted to measure the absorbance of solutions of flotation reagents (e.g. xanthate, mercaptobenzothiazole, dithiophosphate, and Z-200) in the concentration range 0–10 mg l^-1 in aqueous and non-aqueous solvents in the u.v. and visible regions. The absorbance values obtained are similar to those from a u.v.—visible spectrophotometer and straight-line calibration graphs are obtained. Hollow-cathode lamps emitting the desired wavelengths can be selected from wavelength tables of atomic lines. This technique allows a metallurgical analytical laboratory to extend its range of determinations without additional cost by the use of an a.a.s. unit as a u.v.—visible spectrometer.     

QSAR modeling of flotation collectors using principal components extracted from topological indices

Several topological indices were calculated for substituted-cupferrons that were tested as collectors for the froth flotation of uranium. The principal component analysis (PCA) was used for data reduction. Seven principal components (PC) were found to account for 98.6% of the variance among the computed indices. The principal components thus extracted were used in stepwise regression analyses to construct regression models for the prediction of separation efficiencies (Es) of the collectors. A two-parameter model with a correlation coefficient of 0.889 and a three-parameter model with a correlation coefficient of 0.913 were formed. PCs were found to be better than partition coefficient to form regression equations, and inclusion of an electronic parameter such as Hammett sigma or quantum mechanically derived electronic charges on the chelating atoms did not improve the correlation coefficient significantly. The method was extended to model the separation efficiencies of mercaptobenzothiazoles (MBT) and aminothiophenols (ATP) used in the flotation of lead and zinc ores, respectively. Five principal components were found to explain 99% of the data variability in each series. A three-parameter equation with correlation coefficient of 0.985 and a two-parameter equation with correlation coefficient of 0.926 were obtained for MBT and ATP, respectively. The amenability of separation efficiencies of chelating collectors to QSAR modeling using PCs based on topological indices might lead to the selection of collectors for synthesis and testing from a virtual database.     

Adsorption mechanism of mixed cationic/anionic collectors in feldspar-quartz flotation system

The adsorption mechanism of mixed cationic alkyl diamine and anionic sulfonate/oleate collectors at acidic pH values was investigated on microcline and quartz minerals through Hallimond flotation, electrokinetic and diffuse reflectance FTIR studies. In the presence of anionic collectors, neither of the minerals responded to flotation but the diamine flotation of the minerals was observed to be pH and concentration dependent. The presence of sulfonate enhanced the diamine flotation of the minerals by its co-adsorption. The difference in surface charge between the minerals at pH 2 was found to be the basis for preferential feldspar flotation from quartz in mixed diamine/sulfonate collectors. The infrared spectra revealed no adsorption of sulfonate collector when used alone but displayed its co-adsorption as diamine-sulfonate complex when used with diamine. The presence of sulfonate increased the diamine adsorption due to a decrease in the electrostatic head-head repulsion between the adjacent surface ammonium ions and thereby increasing the lateral tail-tail hydrophobic bonds. The mole ratio of diamine/sulfonate was found to be an important factor in the orientation of alkyl chains and thus the flotation response of minerals. The increase in sulfonate concentration beyond diamine concentration leads to the formation of soluble 1:2 diamine-sulfonate complex or precipitate and the adsorption of these species decreased the flotation since the alkyl chains are in chaotical orientation with a conceivable number of head groups directing towards the solution phase.     

Optimization of separation and determination of chloramphenicol in food using aqueous two-phase flotation coupled with HPLC

An aqueous two-phase flotation (ATPF) based on short-chain alcohol and salt was a preconcentration, separation and analysis method of chloramphenicol (CAP) coupled with high-performance liquid chromatography with ultraviolet–visible detector. The influences of salt concentration, flotation time, flow rate and the volume of n-propanol on the flotation efficiency of CAP were discussed. Response surface methodology was employed to optimize the experimental conditions. Under the optimal conditions, this method has been applied to quantitative determination of CAP in food with detection limit of 0.12 ng g^?1 and quantification limit of 0.4 ng g^?1 and the recoveries were in the range of 91.53–103.95 %. This ATPF used low cost of organic solvents, had high concentration coefficient and supplied a moderate and biocompatible environment, which is suitable for biomolecules.