A simple, rapid, sensitive and inexpensive approach is described in this work based on a combination of solid‐phase extraction of 8‐hydroxyquinoline (8HQ), for speciation and preconcentration of Cr(III) and Cr(VI) in river water, and the direct determination of these species using a flow injection system with chemiluminescence detection (FI–CL) and a 4‐diethylamino phenyl hydrazine (DEAPH)–hydrogen peroxide system. At different pH, the two forms of chromium [Cr(III) and Cr(VI)] have different exchange capacities for 8HQ, therefore two columns were constructed; the pH of column 1 was adjusted to pH 3 for retaining Cr(III) and column 2 was adjusted to pH 1 for retaining of Cr(VI). The sorbed Cr(III) and Cr(VI) species were eluted from columns using 3.0 ml of 0.1 N of HCl and 3.0 ml of 0.1 N of NaOH, respectively. The flow injection–chemiluminescence (FI–CL) method is based on light emitted due to the oxidation of DEAPH by the H2O2 in the presence of Cr(III), which catalyzes the reaction. The flow cell is a transparent coiled tube made from glass (2.0 × 4.0, inner and outer diameter) and located close to the photodetector. The flow parameters: flow rate, sample volume, flow cell length, and distance to the CL detector were studied and optimized. Under optimum flow conditions, the Cr(III) concentration can be determined over the range 5–350 μg L−1 with a limit of detection of 1.2 μg L−1, as the Cr(III) concentration is proportional to the intensity of the CL signal. The relative standard deviations (%) for 10 and 50 μg L−1 Cr(III) were 1.2% and 3.2%, respectively. The effects of Al(III), Cd(II), Zn(II), Hg(II), Pb(II), Co(II), Cu(II), Ni(II), Mn(II), Ca(II), and Fe(III) were investigated. The proposed method is highly selective and sensitive, enabling a rapid determination of the Cr(III) amount in the presence of other interfering metals. Finally, the FI–CL method was examined in five river water samples with excellent recoveries.
Azo-ligand-(HL) ([4- ((2-hydroxyquinolin-3-yl) diazenyl) -N- (5-methylisoxazol-3yl) benzenesulfonamide]), (2- hydroxy quinolin derivative),reacts with the next metal ions (Cr (III), Fe (III),Co (II) and Cu(II)) forming stable complexes with unique geometries such as(tetrahedral for bothCo (II) and Cu (II), octahedral for both Cr (III) and Fe (III)). The creation of such complexes was detected by employing spectroscopic means involving ultraviolet-visible which proved the obtained geometries, Fourier transfer proved the involvement of coordinated water molecule in all complexes besides the pyrolysis (TGA & DSC) studies proved the coordination of water residues with metal ions inside the coordination sphere as well as chlorine atoms. Moreover
... Show MoreNew, simple and sensitive batch and reverse FIA spectrophotometric methods for the determination of doxycycline hyclate in pure form and in pharmaceutical preparations were proposed. These methods based on oxidative coupling reaction between doxycycline hyclate and 3-methylbenzothiazolinone-2-hydrazone hydrochloride (MBTH) in the presence ammonium ceric sulfate in acidic medium, to form green water-soluble dye that is stable and has a maximum absorbance at 626 nm. A calibration graph shows that a Beer's law is obeyed over the concentration range of 1-80 and 0.5-110 ?g.mL-1 of DCH for the batch and rFIA respectively with detection limit of 0.325 ?g.mL-1 of DCH for r-FIA methods. All different chemicals and physical experimental paramete
... Show MoreA new, simple and sensitive method was used forevaluation of propranolol withphosphotungstic acidto prove the efficiency, reliability and repeatability of the long distance chasing photometer (NAG-ADF-300-2) using continuous flow injection analysis. The method is based on reaction between propranolol and phosphotungstic acid in an aqueous medium to obtain a yellow precipitate. Optimum parameters was studied to increase the sensitivity for developed method. A linear range for calibration graph was 0.007-13 mmol/L for cell A and 5-15 mmol/L for cell B, and LOD 207.4792 ng/160 µL and 1.2449 µg/160 µL respectively to cell A and cell B with correlation coefficient (r) 0.9988 for cell A, 0.9996 for cell B, RSD% was lower than 1%, (n=8) for the
... Show MoreThis study was done to evaluate a new technique to determine the presence of methamphetamine in the hair using nano bentonite-based adsorbent as the filler of extraction column. The state of the art of this study was based on the presence of silica in the nano bentonite that was assumed can interact with methamphetamine. The hair used was treated using methanol to extract the presence of methamphetamine, then it was continued by sonicating the hair sample. Qualitative analysis using Marquish reagent was performed to confirm the presence of methamphetamine in the isolate.The hair sample that has been taken in a different period confirmed that this current developing method can be used to analyzed methamphetamine. This m
... Show MoreIn this research, an organobentonite (HDTMA-BT) was prepared by modifying a jordanian bentonite (BT) with hexadecyltrimethylammonium bromide. By means of in situ free radical polymerization in THF with AIBN as the initiator, this organobentonite is used to prepare the polymethylmethacrylate-bentonite (PMA-HDTMA-BT) nanocomposite. Scanning electron microscopy (SEM), x-ray diffraction (XRD), energy dispersive spectrometer (EDS) and Fourier transform infrared (FTIR) spectroscopy were used to characterize both HDTMA-BT and PMA-HDTMA-BT. Those adsorbents were used in a batch process to remove Pb(II), Cr(III) ions, and p-chlorophenol (PCP) from aqueous solution. Investigated factors included adsorbent dosage, initial pH solution, contact time, an
... Show Moreأجريت هذه الدراسة في محافظة النجف بالعراق لتحليل عينات بيولوجية من المدخنين وغير المدخنين. تم استخدام العينات، بما في ذلك مصل الدم والبول والشعر والأظافر، كمؤشرات حيوية لتحديد تركيزات اليورانيوم (UC) ونظائره (238U، 235U، و234U). وباستخدام طريقة التعرض الطبيعي، تم استخدام كاشف المسار النووي (CR-39، المملكة المتحدة) لقياس تركيزات اليورانيوم في العينات. تم جمع خمسة وسبعين عينة من مصل الدم والبول والشعر والأظافر للمد
... Show MoreThis study was aimed to develop an optimized Dy determination method using differential pulse voltammetry (DPV). The Plackett-Burman (PB) experimental design was used to select significant factors that affect the electrical current response, which were further optimized using the response surface method-central composite design (RSM-CCD). The type of electrolyte solution and amplitude modulation were found as two most significant factors, among the nine factors tested, which enhance the current response based on PB design. Further optimization using RSM-CCD shows that the optimum values for the tw
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