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A sweeping-micellar electrokinetic chromatography method for the detection of three chlorophenols in cosmetic samples

Zheng Zhihan, Li Xiaobin, Gao Fangfang, Liu Huitao, Gao Yuan

Acta Chromatographica

2021

Vol. 33, no. 4

387--393

A sweeping micellar electrokinetic chromatography (sweeping-MEKC) enrichment model was established for the determination of three chlorophenols (CPs) in cosmetics, namely, bithionol, pentachlorophenol (PCP), and 2,4,6-trichlorophenol (2,4,6-TCP). The optimum electrophoretic conditions were 20 mM NaH2PO4-80 mM sodium dodecyl sulfate (SDS) and 30% (v/v) acetonitrile (pH 2.3). The optimum on-line concentration conditions were as follows: sample matrix, 100 mM NaH2PO4; pressure injection at 20.67 kPa (3 psi) for 25 s. The linear range of bithionol, PCP, and 2,4,6-TCP are 0.20–4.00 μg mL−1, 0.10–2.00 μg mL−1, and 0.05–2.00 μg mL−1 respectively, with correlation coefficient (r) over 0.9972. The limits of detection (LOD) based on three times the signal-to-noise ratio (S/N = 3) are in the range of 0.0061–0.024 μg mL−1. Recoveries for the three CPs in powder and lotion samples are between 79.7 and 110.2% with relative standard deviation (RSD) of 1.38–5.54% and 92.2–121.3% with RSD of 0.72–6.09%, respectively. The proposed method can provide reference for the determination of trace CPs in different sample matrix.

Adsorpcja 2,4,6-trichlorofenolu na węglu aktywnym z roztworów wodno-metanolowych

Dąbek L., Kuśmierek K, Świątkowski A.

Inżynieria i Ochrona Środowiska

2013

T. 16, nr 3

313--321

W pracy zbadano adsorpcję 2,4,6-trichlorofenolu na węglu aktywnym Norit R3-ex z wody, metanolu oraz roztworów woda/metanol o różnym składzie procentowym. Rozpatrywano zarówno kinetykę procesu, jak i adsorpcję w stanie równowagi. Badania kinetyczne pokazały, że 2,4,6-trichlorofenol adsorbował się szybciej z metanolu niż z wody, równowaga ustalała się odpowiednio po 3 i 5 godzinach. Kinetyka przebiegała zgodnie z modelem pseudo II rzędu, o czym świadczą wyższe wartości współczynników korelacji (> 0,99). Zbadano również adsorpcję w stanie równowagi z wody, metanolu oraz roztworów wodno- -metanolowych, zawierających 25, 50 i 75% rozpuszczalnika organicznego. Izotermy adsorpcji były dobrze opisane równaniem Freundlicha. Wartości stałych Freundlicha KF zmniejszały się wraz ze wzrostem zawartości metanolu w roztworze (od 1,533 dla wody do 0,288 dla czystego metanolu). Pokazuje to, że metanol wpływa negatywnie na adsorpcję 2,4,6-trichlorofenolu na węglu aktywnym. Zwiększenie zawartości rozpuszczalnika organicznego w roztworze powoduje pogorszenie adsorpcji.

Adsorption of chlorophenols on activated carbon is one of the most popular methods for their removal from water. The adsorption process is affected by the adsorbate and adsorbent properties, temperature, and solution properties (e.g. ionic strength, pH). The influence of these parameters on the adsorption of chlorophenols on activated carbon is well documented, but to our knowledge there is no information on the effect of organic solvents. The purpose of this study was to examine the adsorption of the 2,4,6-trichlorophenol on activated carbon Norit R3-ex from water, methanol, and from water/methanol mixtures of different composition (25/75, 50/50 and 75/25%). Both, the kinetics and adsorption equilibria were investigated. The adsorbate concentrations in the solutions were measured by high- -performance liquid chromatography with ultraviolet detection. The kinetic studies were conducted for initial concentration of chlorophenol 0.25 mmol/dm3 from water and methanol. It was observed that 2,4,6-trichlorophenol was adsorbed more rapidly from the methanol than from the water, but nevertheless effective adsorption was much worse (41 vs. 93%). Adsorption equilibrium was achieved after 5 hours for water and after about 3 hours for methanol, respectively. In order to investigate the kinetics of adsorption the constant of adsorption were determined in terms of the pseudo-first-order and pseudo-second-order equations. The results showed that the pseudo-first-order model gives poor fitting with low R2 values, whereas the pseudo-second order model fits the experimental data quite well with correlation coefficients better than 0.99. Adsorption equilibrium data were also analyzed and were fitted well using Freundlich isotherm in the studied concentration range (from 0.05 to 0.5 mmol/dm3). The values of KF determined from the Freundlich plots decreased with increasing amount of methanol in a solution (from 1.533 for water to 0.288 for pure methanol). This suggests that methanol has a negative effect on the adsorption on activated carbon. Increasing of the methanol concentration in the solution results in deterioration of the 2,4,6-trichlorophenol adsorption.