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1.
Dispersive liquid-liquid microextraction and liquid chromatographic determination of pentachlorophenol in water 总被引:1,自引:0,他引:1
Khalil Farhadi Mir A. Farajzadeh Amir A. Matin Paria Hashemi 《Central European Journal of Chemistry》2009,7(3):369-374
A simple and sensitive dispersive liquid-liquid microextraction method for extraction and preconcentration of pentachlorophenol
(PCP) in water samples is presented. After adjusting the sample pH to 3, extraction was performed in the presence of 1% W/V
sodium chloride by injecting 1 mL acetone as disperser solvent containing 15 μL tetrachloroethylene as extraction solvent.
The proposed DLLME method was followed by HPLC-DAD for determination of PCP. It has good linearity (0.994) with wide linear
dynamic range (0.1–1000 μg L−1) and low detection limit (0.03 μg L−1), which makes it suitable for determination of PCP in water samples.
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2.
Jaromíra Chýlková Renáta Šelešovská-Fadrná Jaroslava Machalíková 《Central European Journal of Chemistry》2007,5(2):479-495
The optimal process of pre-treatment and activation of gold rotating disc electrode (AuRDE) before voltammetric determination
of mercury is proposed. This treatment encompasses polishing of the electrode surface, electrochemical cycling, and activation.
This procedure both increases determination sensitivity as well as improves determination reproducibility. The detection limit
on the working electrode achieved using this approach amounted to 8.26·10−10 mol L−1for direct mercury determination in water solution (applying 200 s running accumulation). The procedure of the quantitative
mercury isolation from complicated sample matrix was developed as well. It provides better selectivity and significant increase
of sensitivity of mercury determination. In case of mercury isolation from one liter of water the detection limit is 6.23·10−11 mol L−1 (analyzing a greater sample volume the determined concentration could be lower).
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3.
Qingyang Liu 《Central European Journal of Chemistry》2010,8(2):326-330
This work presents a nano-Al2O3 solid phase extraction technique for the determination of ultra-trace amounts of inorganic selenium species in aqueous systems
using ion chromatography inductively coupled plasma-mass spectrometry (IC-ICP-MS). In this experiment, the inorganic selenium
species were successfully extracted on a nano-Al2O3 solid phase column and then quantitative eluted with a 100 mmol L−1 NaOH solution. Extraction conditions such as solvent identity, solvent concentration, solvent volume, solvent pH and salt
addition were optimized. Under the optimum extraction conditions (elute solvent: 100 mmol L−1 NaOH, solvent volume: 4 mL, pH: 7.0), low detection limits (Se (IV): 6 ng L−1, Se (VI): 11 ng L−1; RSD<5.0%) and good linear range (0.5–100 ng mL−1, R2 > 0.999) were obtained for all of the analytes. Good spiked recoveries over the range of 80–98% were obtained by applying
the proposed method on real environmental water samples. These results indicated that this method is very sensitive and reliable
when monitoring trace levels of inorganic selenium species in aqueous samples.
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4.
Aleksandra Prichodko Kristina Jonusaite Vida Vickackaite 《Central European Journal of Chemistry》2009,7(3):285-290
A hollow fibre liquid phase microextraction for gas chromatographic determination of some p-hydroxybenzoic acid esters has
been developed. Chlorobenzene containing tetradecane as internal standard was used for the extraction. Optimized extraction
was carried out at room temperature for 40 min in the presence of 0.4 g mL−1 NaCl in the sample solution. Calibration was linear up to 30 mg L−1. Correlation coefficients were 0.996–0.998. Enrichment factors were 21, 95 and 154, and detection limits were 0.20, 0.03
and 0.01 μg mL−1 for methylparaben, ethylparaben and propylparaben, respectively. Reproducibility was acceptable with relative standard deviations
up to 11.7%. The technique was tested for water and urine analysis.
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5.
In the present paper, an off-line preconcentration procedure for the determination of cadmium and lead by flame atomic absorption
spectrometry (FAAS) is proposed. Polyurethane foam (PUF) functionalized with o-aminophenol (o-AP) followed by Pyrazolone (Pyr)
packed in a minicolumn was used as a sorbent material. The metals were retained on the modified PUF, from which it could be
eluted and effectively preconcentrated. The detection limits were 0.072 and 0.016 μg L−1 for Pb and Cd respectively. Enrichment factors were 250 and 319 for lead and cadmium respectively. The procedure has been
applied successfully to metal determination in water samples, fish liver and reference material.
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6.
Jinzhang Gao Yingying Zhang Jie Ren Ming Li Wu Yang 《Central European Journal of Chemistry》2010,8(3):602-606
A sensitive and convenient method for the determination of trace europium ions using an oscillating chemical reaction involving
Ce(IV) - KBrO3 - acetone - oxalic acid - H2SO4 was proposed. The results indicated that the changes in oscillating period (T) was linearly proportional to the negative
logarithmic concentration of Eu3+ (-log C) in the range of 1.41 × 10−8 ˜ 1.41 × 10−4 mol L−1 (r = 0.9982) with a detection limit of 1.04 × 10−9 mol L−1. The recoveries were limited to the range of 99.5% to 100.8%. Under the same conditions, other rare earth ions did not interfere
with the determination of Eu3+. In addition, a perturbation mechanism was also discussed briefly.
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7.
Ardeshir Shokrollahi Mojtaba Shamsipur Fahimeh Jalali Hamid Nomani 《Central European Journal of Chemistry》2009,7(4):938-944
A simple, sensitive and selective flotation method is described for the preconcentration and atomic absorption spectrometric
determination of zinc ion in water and blood samples. At a solution pH of 5.2, 4-(2-pyridylazo-resorcinol) and Triton X-114
were used as hydrophobic ligand and non-ionic surfactant, respectively. The chemical variables affecting the preconcentration
process were optimized. Under the optimized experimental conditions, the selective preconcentration and determination of as
low zinc concentration as 6.5 μg L−1 can be made. The proposed method was successfully applied to the preconcentration and low-level determination of zinc in
different water and blood serum samples.
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8.
Hossein Abdolmohammad-Zadeh Elnaz Ebrahimzadeh 《Central European Journal of Chemistry》2010,8(3):617-625
A rapid dispersive liquid-liquid micro-extraction (DLLME) methodology based on the application of 1-hexylpyridinium hexafluorophosphate
[C6py][PF6] ionic liquid (IL) as an extractant solvent was applied for the pre-concentration of trace levels of cobalt prior to determination
by flame atomic absorption spectrometry (FAAS). 1-Phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP) was employed as a chelator
forming a Co-PMBP complex to extract cobalt ions from aqueous solution into the fine droplets of [C6py][PF6]. Some effective factors that influence the micro-extraction efficiency include the pH, the PMBP concentration, the amount
of ionic liquid, the ionic strength, the temperature and the centrifugation time which were investigated and optimized. In
the optimum experimental conditions, the limit of detection (3s) and the enrichment factor were 0.70 μg L−1 and 60, respectively. The relative standard deviation (RSD) for six replicate determinations of 50 μg L−1 Co was 2.36%. The calibration graph using the pre-concentration system was linear at levels 2–166 μg L−1 with a correlation coefficient of 0.9982. The applicability of the proposed method was evaluated by the determination of
trace amounts of cobalt in several water samples.
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9.
M. H. Sorouraddin M. Iranifam A. Imani-Nabiyyi 《Central European Journal of Chemistry》2009,7(1):143-147
A simple and selective method for penicillin V potassium (PVK) determination by chemiluminescence (CL) was developed. Oxidation
of PVK by alkaline hydrogen peroxide produces CL, which is greatly enhanced by N, N-dimethyl formamide (DMF) and N-cetyl-N,N,N-trimethylammonium
bromide (CTMAB). Optimum conditions were established using luminometry. There is a linear relationship between the chemiluminescent
peak height and the amount of PVK within the range 0.5–129.5 mg L−1, with a detection limit of 0.2 mg L−1. The coefficient of variation was 1.2% for 40 mg L−1 PVK solution (n = 7). The method is very simple, has high sensitivity and good selectivity, and is usable for process control.
It was successfully utilized for the determination of PVK in pharmaceuticals and spiked human urine.
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10.
Joanna Lenik Cecylia Wardak Barbara Marczewska 《Central European Journal of Chemistry》2008,6(4):513-519
Naproxen membrane electrodes based on different plasticizers and the quaternary ammonium salts (QASs) dimethyldidecylammonium
bromide, methyltrioctylammonium chloride, or tetraoctylammonium chloride, were prepared. The following basic parameters were
investigated for the optimal electrode: measurement range (10−4 − 10−1 mol L−1), slope of the linear range of the calibration curve (−58.3 mV decade−1), limit of detection (6.0 × 10−5 mol L−1), lifetime (2.5 months), dependence of the electrode potential on pH (5.5 − 9.0), reproducibility of potential (1.2 mV) and
selectivity coefficients in relation to selected organic and inorganic anions. The electrode was utilized for determination
of naproxen in tablets by the calibration curve method and the standard addition method.
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11.
Hana Dejmkova Candan Dag Jiri Barek Jiri Zima 《Central European Journal of Chemistry》2012,10(4):1310-1317
New methods for the determination of metoclopramide, antiemetic and gastroprokinetic pharmaceutical, were developed, using
differential pulse voltammetry (DPV) and flow injection analysis (FIA) with amperometric detection on a boron-doped diamond
film electrode. Electrode pretreatment necessary to ensure the stable results was investigated and it was found, that while
DPV requires frequent electrode cleaning, FIA with a sufficiently high flow rate can maintain a stable signal with no signs
of electrode passivation. The calculated quantification limits of the DPV and FIA with amperometric detection were 0.13 μmol
L−1 and 0.015 mmol L−1, respectively. The applicability of the new methods was verified by the determination of metoclopramide in a pharmaceutical
preparation. FIA with amperometic detection proved to be sensitive, accurate and, due to the resistance of the electrode to
the passivation, also simple to handle.
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12.
Elisaveta K. Mladenova Ivanka G. Dakova Dimiter L. Tsalev Irina B. Karadjova 《Central European Journal of Chemistry》2012,10(4):1175-1182
A sorbent L-cysteine grafted silica gel has been evaluated for separation and enrichment of dissolved inorganic i-Hg(II) and methylmercury CH3Hg(I) from surface waters at sub-μg L−1 concentrations. Chemical parameters for mercury species enrichment and separation have been optimized. Analytical schemes for the determination of Hg species, using selective column solid phase extraction (SPE) with continuous flow chemical vapor generation atomic absorption spectrometry (CF-CVG-AAS) or inductively coupled plasma-mass spectrometry (ICP-MS) were developed. Possibilities for on-site SPE enrichment were demonstrated as well. The limits of quantification were 1.5 and 5 ng L−1 for dissolved i-Hg(II) and CH3Hg(I) by CF-CVG-AAS and 1 and 2.5 ng L−1 by ICP-MS with relative standard deviations between 7–12% and 7–14%, respectively. The chemically modified SPE sorbent has demonstrated high regeneration ability, chemical and mechanical stability, acceptable capacity and good enrichment factors. Results for total dissolved mercury were in reasonable agreement with those from independent analyses by direct ICP-MS determinations for river waters and for estuarine water certified reference material. 相似文献
13.
Ibuprofen membrane electrodes based on different plasticizers: diisobutyl phthalate (DIBP), o-nitrophenyloctyl ether (o-NPOE),
dioctyl sebacate (DOS) and tetraoctylammonium 2-(4-isobutylphenyl)propionate were prepared. All electrodes show: a near Nernstian
slope of characteristic (58.3–60.9 mV decade−1) in the measurement range (10−4–10−1 mol L−1), limit of detection (5.0×10−5 mol L−1), really long lifetime (12 months), dependence of the electrode potential on pH (5.5–9.0), reproducibility of potential (0.6–1.2
mV) and selectivity coefficients in relation to some organic and inorganic anions. The electrodes were applied for the determination
of ibuprofen in tablets by the calibration curve method and the standard addition method.
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14.
Issac A. Ololade Labunmi Lajide Isiaka A. Amoo 《Central European Journal of Chemistry》2009,7(1):83-89
Seasonal changes in petroleum hydrocarbons in water and streambed sediment from selected oil-related areas of Ondo State,
Nigeria have been examined using gravimetric and infrared methods. The highest and lowest total petroleum hydrocarbon concentrations
(TPH) in water (sediments in brackets) gravimetrically were 3.49 mg L−1 (199.3) mg kg−1 and 0.003 mg L−1 (81.0) mg kg−1 while the concentrations found by IR were 24.0 mg L−1 (135.0 mg kg−1) and 14.0 mg L−1 (33.0 mg kg−1) respectively. The two seasons were positively correlated (α = 0.01) by both methods. The TPH level was well correlated with
the sediment organic carbon (OC) during both seasons. The characteristic carbonyl (C=O) vibrations at 1650 cm−1 and 1700 cm−1 indicate oxidation of the oil residue. The study recommends further investigation into the type of organics present to evaluate
their toxicity and appropriate remediation.
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15.
Saman Azodi-Deilami Majid Abdouss Seyed Alireza Hasani 《Central European Journal of Chemistry》2010,8(4):861-869
In this paper, a highly selective molecularly imprinted polymer (MIP) for tramadol hydrochloride, a drug used to treat moderate
to severe pain, was prepared and its use as solid-phase extraction (SPE) sorbent was demonstrated. The molecularly imprinted
solid-phase extraction procedure followed by high performance liquid chromatography with ultraviolet detector (MISPE-HPLC)
was developed for selective extraction and determination of tramadol in human plasma and urine. The optimal conditions for
molecularly imprinted solid-phase extraction (MISPE) consisted of conditioning with 1 mL methanol and 1 mL of deionized water
at neutral pH, loading of tramadol sample (50 μg L−1) at pH 7.5, washing using 1 mL acetone and elution with 3 × 1 mL of 10% (v/v) acetic acid in methanol. The MIP selectivity
was evaluated by checking several substances with similar molecular structures to that of tramadol. Results from the HPLC
analyses showed that the calibration curve of tramadol (using MIP from human plasma and urine) is linear in the ranges of
6–100 and 3–120 μg L−1 with good precisions (1.9% and 2.9% for 5.0 μg L−1), respectively. The recoveries for plasma and urine samples were higher than 81%.
相似文献
16.
Paraskevas D. Tzanavaras Theano D. Karakosta Pantelis G. Rigas Demetrius G. Themelis Anastasia Zotou 《Central European Journal of Chemistry》2012,10(5):1459-1463
The first HPLC method for the separation of three paraben preservatives (methyl-, ethyl- and propyl parabens) using a core-shell analytical column is reported in this study. The separation was completed in less than 8 min at a low flow rate of 0.4 mL min−1 and an isocratic mobile phase containing 20% acetonitrile as organic modifier. The backpressure was < 200 bar in all cases, enabling the usage of conventional HPLC equipment. The proposed analytical procedure was validated for linearity (0.5–20 μg L−1), limits of detection (15–43 μg L−1) and quantification (50–142 μg L−1), selectivity, within day (1.3–1.5%) and day-to-day (3.4–4.6%) precision and accuracy. The proposed method has been applied to the determination of the selected paraben preservatives in commercially available hygiene wipes. The mean percent recoveries were found to be in the range of 98.0–98.4%. 相似文献
17.
Mónica Díaz-Pérez Manuel Aboal-Somoza Pilar Bermejo-Barrera Adela Bermejo-Barrera 《Central European Journal of Chemistry》2008,6(4):520-525
Preliminary results of development of a direct and fast method of determination of antimony in samples of tap water using
GFAAS are presented. The found levels of antimony were lower than permitted for human consumption. A mixture of Pd and Mg(NO3)2 (concentrations in the injected solution: 8.6 μg mL−1 and 5.8 μg mL−1 respectively) was used as the chemical modifier. The pyrolysis and atomization temperatures were 1000 and 1700°C, respectively
and the mean analytical recovery 98.2%.
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18.
Ismail M. M. Rahman Yoshiaki Furusho Zinnat A. Begum Akhmad Sabarudin Shoji Motomizu Teruya Maki Hiroshi Hasegawa 《Central European Journal of Chemistry》2011,9(6):1019-1026
A simple flow-based method was developed for the simultaneous separation of certain transition metal ions (Co, Ni, Cu, Zn,
Cd) from aqueous systems, which ions show ecotoxic effects when present at elevated concentrations. A silica-gel-bonded macrocycle
system, commonly known as molecular recognition technology (MRT) gel, was used for solid phase extraction (SPE) of the target
analytes. The collection behavior of the MRT-SPE system was studied based on pH. Fortified deionized water samples containing
250 μg L−1 of each of the elements were treated at the flow rate of 1 mL min−1. The collected analytes were then eluted by 3 M HNO3 and analyzed using inductively coupled plasma spectrometry. Detection limits of the proposed technique were in the range
of 0.004–0.040 μg L−1 for the studied metal ions. The validity of this separation technique was checked with spiked ‘real’ water samples, which
produced satisfactory recoveries of 96–102%. The non-destructive nature and highly selective ion-extraction capability of
the SPE material are the most important aspects of the proposed method and they are the main focus of this paper.
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19.
The construction and optimization of five new types of miniaturized flow-through electrolytic cells with lead cathode and
platinum anode for electrochemical hydride generation in atomic absorption spectrometry (HG-QFAAS) were achieved during this
research study. The ion-exchange membrane was not part of these cells and only one carrying electrolyte for both electrode
chambers was used. Hydride generation efficiency achieved was either comparable or higher than the one recorded for the classic
thin-layer generation cell. The inner volume of the cathode chamber was reduced to a quarter of the classic thin-layer flow-through
cell. Compared to the commonly used thin-layer flow-through cell, higher sensitivity (7.32×103 dm3 μg−1) and better limit of detection (0.32 μg dm−3) were obtained for selenium determination using two of these new generators.
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20.
Nagwa Burham Sami A. Azeem Mohamed F. El-Shahat 《Central European Journal of Chemistry》2009,7(4):945-954
A new solid — phase extraction sorbent was developed based on stepwise anchoring of two ligand molecules for the determination
of copper, zinc, lead and cadmium in drinking water by flame AAS. Amberlite XAD-2 functionalized with 4′-(2-hydroxyphenylazo)-3′-methyl-1′-phenyl-2′-pyrazolin-5′-one
(HPAPyr) was utilized for preconcentration/separation of these elements. The sorbent was prepared by two successive azo coupling
reactions. First, 2-aminophenol was anchored to the amino groups in the resin resulted from nitration followed by reduction.
Then, the resulted 2-aminophenol functionalized resin was further diazotized and coupled to the pyrazolone compound and the
final product HPAPyr-XAD-2 was characterized by IR and elemental analysis. The optimum pH range for sorption, shaking time,
exchange capacity, sample flow rate, preconcentration factor and interference from co-existing ions were investigated. All
metal ions were quantitatively desorbed from the resin by 4.5 mol L−1 nitric acid solution. The sorbent provides limit of detection within the range 0.9–3.3 μg L−1 and concentration factor up to 250. The procedure was validated by analysis of certified material NIST-SRM 1577b. Application
to drinking water showed satisfactory results with relative standard deviation RSD ≤ 8.5%.
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