scholarly journals Dimercaptosuccinic Acid Functionalized Polystyrene Column for Trace Concentration Determination of Heavy Metal Ions: Experimental and Theoretical Calculation Studies

Water ◽  
2021 ◽  
Vol 13 (21) ◽  
pp. 3056
Author(s):  
Uzma Haseen ◽  
Syed Ghazanfar Ali ◽  
Khalid Umar ◽  
Abuzer Ali ◽  
Hilal Ahmad ◽  
...  
Keyword(s):  
Metal Ion ◽  
Density Functional ◽  
Solid Phase ◽  
Standard Addition ◽  
Dimercaptosuccinic Acid ◽  
Stable Complex ◽  
Ligand Stabilization ◽  
Preconcentration Factor ◽  
Method Accuracy

Metal ion studies in wastewater are required on a regular basis for environmental monitoring and assessment. Less metal ion concentrations and the interference from complex sample matrices remains challenging for instrumental quantification. Herein, we proposed a fix-bed solid phase extraction method, consisting of a newly prepared dimercaptosuccinic acid functionalized polystyrene beads. The ligand forms stable complex with Hg(II), Pb(II), and Cd(II), evident by experimental as well as density functional theory. The metal-ligand stabilization energy calculations, suggested the higher selectivity of polystyrene dimercaptosuccinic acid (PSDMSA) toward Pb(II) compared to Cd(II) and Hg(II). The prepared adsorbent was utilized to enrich Hg(II), Pb(II), and Cd(II) ions from environmental samples. Column parameters were studied in detail and optimized accordingly. The preconcentration factor for Hg(II), Pb(II), and Cd(II) were found to be 900, with the preconcentration limit of 0.74 µg L−1. The detection limit for Pb(II), Cd(II), and Hg(II) ions was found to be 1.3 ± 0.2, 1.5 ± 0.3, and 1.8 ± 0.3 ng L−1, respectively. The method accuracy was tested against systematic and continuous errors by standard addition method (<5% RSD). Real samples was successfully analyzed following the proposed method.

Solid Phase Extraction and Preconcentration of Trace Gallium, Indium, and Thallium Using New Modified Amino Silica

2016 ◽  
Vol 71 (2) ◽  
pp. 288-299 ◽  
Author(s):  
Mohamed M. Hassanien ◽  
Wael I. Mortada ◽  
Ibrahim M. Kenawy ◽  
Heba El-Daly
Keyword(s):  
Solid Phase ◽  
Liquid Crystal Display ◽  
Absorption Spectrometry ◽  
Separation Process ◽  
Phase Extraction ◽  
Flame Atomic Absorption ◽  
Adsorption Capacities ◽  
Experimental Parameters ◽  
Preconcentration Factor

Amino silica gel functionalized with 2-hydroxy-5 -(2-hydroxybenzylideneamino)benzoic acid was synthesized, characterized and used as adsorbent for the removal of Ga3+, In3+ and Tl3+ from aqueous solution prior to their determination by flame atomic absorption spectrometry. Experimental parameters that affect the separation process were investigated in both batch and column modes. The maximum adsorption capacities of the sorbent are 61.7 mg g−1, 81.3 mg g−1 and 133.0 mg g−1 for Ga3+, In3+ and Tl3+, respectively. The preconcentration factor is 200 and the limits of detection of Ga3+, In3+ and Tl3+ are 4.10 μg L−1, 1.55 μg L−1 and 1.21 μg L−1, respectively. Interference by Al3+ can be masked by the addition of F−; and that of Fe3+ by its reduction to Fe2+ using 10% ascorbic acid. The method was successfully applied for the determination of these ions in water, sediments and liquid crystal display samples.

Computational Determination of Heats of Formation of Energetic Compounds

1995 ◽  
Vol 418 ◽  
Author(s):  
Peter Politzer ◽  
Jane S. Murray ◽  
M. Edward Grice
Keyword(s):  
Gas Phase ◽  
Density Functional ◽  
Functional Group ◽  
Solid Phase ◽  
Heats Of Formation ◽  
Energetic Compounds ◽  
Phase Data ◽  
Heats Of Vaporization ◽  
Group Effects

AbstractA recently-developed density functional procedure for computing gas phase heats of formation is briefly described and results for several categories of energetic compounds are summarized and discussed. Liquid and solid phase values can be obtained by combining the gas phase data with heats of vaporization and sublimation estimated by means of other relationships. Some observed functional group effects upon heats of formation are noted.

Magnetic Solid-Phase Extraction Based on Fe3O4/g-C3N4 Nanocomposite for the Determination of Polychlorinated Biphenyls and Polychlorinated Diphenyl Ethers in Environmental Waters

2020 ◽  
Vol 20 (12) ◽  
pp. 7469-7479
Author(s):  
Dongliang Ji ◽  
Meixing Zhang ◽  
Xinxiang Geng ◽  
Zhenxing Zha ◽  
Ying Li ◽  
...  
Keyword(s):  
Polychlorinated Biphenyls ◽  
Solid Phase ◽  
Magnetic Solid Phase Extraction ◽  
Environmental Water ◽  
Environmental Waters ◽  
Diphenyl Ethers ◽  
Preconcentration Factor ◽  
Magnetic Solid ◽  
Polychlorinated Diphenyl Ethers

The graphitic carbon nitride (g-C3N4) and the Fe3O4/g-C3N4 magnetic materials were synthesized in this paper. The structures of the materials were confirmed by a series of analysis. The Fe3O4/g-C3N4 was then used as a sorbent to adsorb polychlorinated diphenyl ethers and polychlorinated biphenyls. Different extraction conditions were examined, including adsorbent amount, salinity, pH of the sample matrix, adsorption time, reaction temperature, elution solvent and preconcentration factor. The maximum recoveries were obtained by employing methanol to desorb pollutants on 40.0 mg Fe3O4/g-C3N4 in 120.0 mL environmental water with a salinity of 5% (w/v) at a pH of 7 at 25 °C within 10 min. Using the optimized parameters, the detection limits of the method are between 0.01 and 0.04 μ · L−1 with a satisfying linear relationship. The adsorbent can be recycled at least 10 times with no significant reduction in the extraction efficiency.

scholarly journals Determination of Trace Metal Ions in Common Salt by Stripping Voltammetry

1999 ◽  
Vol 82 (6) ◽  
pp. 1413-1418 ◽  
Author(s):  
Azza M M Ali
Keyword(s):  
Metal Ion ◽  
Supporting Electrolyte ◽  
Standard Addition ◽  
Stripping Voltammetry ◽  
Differential Pulse ◽  
Ion Concentration ◽  
Common Salt ◽  
Trace Metal Ions

Abstract Sensitive voltammetric methods using cathodic and anodic differential pulse stripping techniques were applied for determination of trace ions cadmium(II), cobalt(II), copper(II), lead(II), manganese(II), nickel(II), and zinc(II), which are usually found in different grades of common salt as contaminants. The optimal conditions, i.e., deposition time, preconcentration potential, supporting electrolyte, and ionic strength, were investigated for each metal ion. Concentration of the metal ion was determined by the standard addition method. Metal content varied according to the quality of the table salt.

Single-Laboratory Evaluation of Method 8060 for the Determination of Phthalates in Environmental Samples

1991 ◽  
Vol 74 (5) ◽  
pp. 793-808 ◽  
Author(s):  
Viorica Lopez Avila ◽  
June Milanes ◽  
Werner F Beckert
Keyword(s):  
Solid Phase ◽  
Sandy Loam ◽  
Internal Standard ◽  
Fused Silica ◽  
Laboratory Evaluation ◽  
Column Method ◽  
Sample Extract ◽  
Method Accuracy ◽  
Single Laboratory

Abstract Method 8060 of the SW-846 methods manual for the determination of phthalates In aqueous and solid matrixes was modified and evaluated in a single laboratory. The range of compounds of interest was expanded to 16 phthalates. The results of a study to determine the extent and the sources of phthalate contamination in the laboratory and ways to minimize background contamination, conducted as part of this work, were reported elsewhere. The packed columns specified in Method 8060 for the gas chromatographic analysis were replaced with 2 fused-silica open-tubular columns of dissimilar stationary phases. These columns were connected to an inlet splitter and 2 electron capture detectors; this dual-column/ dual-detector setup allowed the primary and confirmatory analyses to be conducted simultaneously. Extracts were cleaned up by column chromatography on 10 g Florisil or alumina. Of the 16 target compounds, only 13 were recovered from the Florisil column (Method 3620), but all 16 were recovered from the alumina column (Method 3610). The use of commercially available Florisil and alumina solid-phase extraction cartridges for sample extract cleanup was evaluated, and a method that uses such cartridges (Florisil or alumina) was developed. This latter method gave quantitative recoveries for all 16 compounds. The effects of interferences represented by corn oil, dlesel hydrocarbons, and elemental sulfur were evaluated, and an internal standard and 3 surrogate compounds were identified and proposed for use with this method. The revised method was tested with samples of an estuarine water, a leachate, a groundwater, an estuarine sediment, a municipal sludge, and a sandy loam soil, each spiked with the 16 phthalates. For the aqueous samples spiked at 20 and 60 μg/L, the method accuracy ranged from 60 to 117% and method precision was better than 28%. The method accuracy and precision for solid samples extracted by Method 3550 were highly dependent on matrix type and on analyte concentration.

Simultaneous Spectrophotometric Determination of Brilliant Blue and Tartrazine in Diverse Sample Matrices after Solid Phase Extraction

2020 ◽  
Vol 103 (6) ◽  
pp. 1478-1485
Author(s):  
Abdullah Taner Bişgin
Keyword(s):  
Spectrophotometric Determination ◽  
Solid Phase ◽  
Brilliant Blue ◽  
Liquid Samples ◽  
Quantitative Extraction ◽  
Relative Standard ◽  
Separation And Preconcentration ◽  
Preconcentration Factor ◽  
Experienced Operator

Abstract Background Brilliant blue (BB) and tartrazine (TZ) are manufactured from petroleum and its products. These are the most popular consumed food dyes and are widely used in foodstuffs. Therefore, overuse of these dyes in foodstuffs and consumption of excessive amounts of these dyes can lead to health problems in humans. Objective The aim of this study was to develop a simple separation and preconcentration method for simultaneous spectrophotometric determination of BB and TZ dyes. Methods A column solid-phase separation extraction method combined with UV-Vis spectrophotometry was preferred and developed for single and simultaneous determination of BB and TZ dyes. Results The preconcentration factor was obtained as 80. Relative standard deviations were below than 4%. Detection limits of the method were determined as 0.29 and 1.21 µg/L for BB and TZ, respectively. Recovery values were obtained between 95–99% and 96–100% for BB and TZ, respectively. 10.9–235.7 µg/g and 1.7–8.0 µg/mL of BB contents of real samples were determined for solid and liquid samples, respectively. TZ concentrations of solid and liquid samples were ranged between 18.7–220.7 µg/g and 5.9–7.5 µg/mL, respectively. Conclusions Quantitative extraction results and satisfactory recovery values showed that method was successful and applicable for determination of BB and TZ concentrations in real pharmaceutical, industrial, and foodstuff samples. Highlights The method has exhibited a high preconcentration factor and effective separation against to matrix ions. The method did not need an experienced operator with high operation experience. Elution solvent can be chosen according to the availability of the chemicals in the laboratory and cheapness of the chemicals.

Experimental Design Methodology Applied to Mercury Determination: Hair Samples as a Mercury Bioindicator

2015 ◽  
Vol 98 (1) ◽  
pp. 176-182
Author(s):  
Mohammad Karimi ◽  
Forouzan Aboufazeli ◽  
Hamid Reza Lotfi Zadeh Zhad ◽  
Omid Sadeghi ◽  
Ezzatollah Najafi
Keyword(s):  
Magnetic Nanoparticles ◽  
Design Methodology ◽  
Solid Phase ◽  
Mercury Determination ◽  
Hair Samples ◽  
Preconcentration Factor ◽  
Modified Magnetic Nanoparticles ◽  
Surface Response Design ◽  
Experimental Design Methodology

Abstract The application of modified magnetic nanoparticles in extraction of trace Hg was investigated. For this purpose, surfaces of magnetic nanoparticles were modified by 2-picolamine and then utilized as a solid-phase sorbent for Hg(II) extraction. A statisticalmethod, based on surface response design, has been used for the optimization of Hg ion elution from the magnetic nanoparticles. The sorbed Hg ions were eluted quantitatively with 5.5 mL of a solution containing 0.8 M HCl and 0.08 M EDTA after 12 min. The recovery value in this method was 98.6% with RSD of 1.4%,and the obtained LOD was 0.01 ng/mL. The preconcentration factor was calculated to be 179. The method was applied to the determination of hair Hg content for biomonitoring purposes.

scholarly journals SPECTROMETRIC INVESTIGATION OF CEFPROZIL IN BULK POWDER AND IN PHARMACEUTICAL FORMULATIONS

2002 ◽  
Vol 70 (1) ◽  
pp. 67-76 ◽  
Author(s):  
EI-Adl Sobhy M. ◽  
Saleh Hanaa M.
Keyword(s):  
Metal Ion ◽  
Hydrolysis Product ◽  
Reference Method ◽  
Standard Addition ◽  
Pharmaceutical Formulations ◽  
Dosage Forms ◽  
Pharmaceutical Dosage Forms ◽  
Bulk Powder ◽  
Ion Contents

Three accurate methods were developed for the quantitative determination of cefprozil in pure form and in its dosage forms. The first method was based upon the interaction of the drug with 3-methyl-benzothiazolinone-2-hydrazone (MBTH) in the presence of ceric ammonium sulfate or ferric chloride as an oxidizing agent, where the formed color was measured at λ 521 nm or 624 nm, respectively. The second inethod was based on the chelate formation with palladium (II) chloride (PdCl2) in the presence of buffered medium, where the formed complex was determined at λ 345 nm. The third method was based upon the reaction of the neutral solution of the hydrolysis product of drug with each of silver nitrate & lead acetate standard solutions, forming drug-metal complex and the metal ion contents were determined directly or indirectly by atomic absorption spectroscopy (AAS). The reaction conditions of the proposed methods were studied and optimized. The precision of the proposed methods was achieved by determining different samples of bulk powder and pharmaceutical dosage forms. The validity of the methods was assessed by applying the standard addition technique and the results were compared with those obtained by the reference method showing a great agreement

scholarly journals Pipette Tip Solid-Phase Extraction Combined with Fluorescence Spectroscopy for Determination of Selenium in Green Tea Samples

2021 ◽  
Vol 913 (1) ◽  
pp. 012064
Author(s):  
S R Kamali ◽  
C H Tsai ◽  
C N Chen
Keyword(s):  
Solid Phase Extraction ◽  
Green Tea ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Standard Addition ◽  
Phase Extraction ◽  
Addition Method ◽  
The Matrix ◽  
Pipette Tip

Abstract In this study, the custom-built pipette-tip solid phase extraction (PT-SPE), was used for pre-concentrating the selenium (Se) in green tea samples. The PT-SPE was prepared using a pipette tip and C18 as the adsorbent that was placed between glass wool. This method afforded several advantages in terms of efficiency of extraction time (8 min), sample (2 mL), and solvent (1 mL) volumes with less wastage of solvent. Under optimal conditions of extraction, this method yielded good linearity (r2=0.998) for the Se calibration curve and good limit of detection (0.2 μg/L) and quantification (0.6 μg/L). The standard addition method was used to remove the matrix effect. The recovery percentages of tea samples spiked with different Se concentrations ranged from 97.7 to 106.0%, indicating that the proposed method would be suitable for the determination of Se in green tea samples.

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