A procedure, depending on the derivatization and determination of aniline was depicted andvalidated in this study. 8-hydroxyquinoline (8-HQ) was used as the derivatizing agent for thedetermination of aniline. An optimization study was performed for the derivatization reaction, i.e.,the diazonium coupling reaction, the optimum parameters were as follows: 22 mM of hydrochloricacid, 54mM of sodium hydroxide, and 1.8mM of sodium nitrate. The optimization study of themethod of cloud point extraction (CPE) revealed that the extraction solvent was 0.5 ml of Triton X-100, the optimum temperature was 90 °C, and the incubation time was 25 min. The linearity,correlation coefficients, molar absorptivities, and limits of detection were improved using the CPEmethod. The extraction product was injected into HPLC. The chromatographic conditions were asfollows: the mobile phase was acetonitrile:water 60:40, the stationary phase was C18 RP column,the detection was at visible wavelength of 420 nm, flow rate 1ml/min. The proposed method wasapplied for the trace detection in environmental application of wastewater. The concentration ofaniline in wastewater was in range of 0.2-7 μg/l. (PDF) DETERMINATION OF ANILINE IN WASTEWATER BY CLOUD POINT EXTRACTION FOLLOWED BY HPLC USING 8- HYDROXYQUINOLINE AS A DERIVATIZATION AGENT. Available from: https://www.researchgate.net/publication/358078777_DETERMINATION_OF_ANILINE_IN_WASTEWATER_BY_CLOUD_POINT_EXTRACTION_FOLLOWED_BY_HPLC_USING_8-_HYDROXYQUINOLINE_AS_A_DERIVATIZATION_AGENT [accessed Mar 08 2025].
A procedure for the mutual derivatization and determination of thymol and Dapsone was developed and validated in this study. Dapsone was used as the derivatizing agent for the determination of thymol, and thymol was used as the derivatizing agent for the determination of Dapsone. An optimization study was performed for the derivatization reaction; i.e., the diazonium coupling reaction. Linear regression calibration plots for thymol and Dapsone in the direct reaction were constructed at 460 nm, within the concentration range of 0.3-7 μg ml-1 for thymol and 0.3-4 μg ml-1 for Dapsone, with limits of detection 0.086 and 0.053 μg ml-1, respectively. Corresponding plots for the cloud point extraction of thymol and Dapsone were constructed
... Show MoreUltrasonic Extraction method followed by gradient HPLC was carried out for the simultaneous determination of four insecticides are [imidacloprid (Imi), thiamethoxam (Thi), indoxacarb (Ind) and abamectin (Aba)] used to combat the major insect pests in Iraq, whitefly, Dubas Bug, worms fruits as well as to combat the spiders – dream respectively in eco-soil samples. The extraction recovery was in the range of 99.77 to 109.1 %. The dissipation kinetics and residual levels of these insecticides in soil sample was studied under field ecosystem. The half-life of the mix insecticides was determined. The half-life was in range of 0.38 to 4.06 days with the soil samples were brought from the Agricultural Land called Nahrawan located in th
... Show MoreA solid Phase Extraction (SPE) cartridges followed by HPLC-UV method is described for the simultaneous quantitative determination of benzidine (BZ) and its substituted 3, 3’-dichlorobenzidine (DCB) and 3, 3’-Dimethylbenzidine (DMB). The Benzidines were separated by liquid chromatography using a C-18 column with UV detector at wave length of 280nm. The mode of Flow was isocratic. The mobile phase was consisted of 75:25 methanol: water, column temperature 50C°, and Flow Rate 1.8ml/min. Calibration curves were linear (R2 = 0.9979-0.9995). LOD (26.36-33.67) µg/L, LOQ (109.98-186.11) µg/L, the Robustness (2.99-4.35), Ruggedness (2.93-3.65).Conditions of extraction by (SPE) cartridges were optimized, the resin used is Octadecyl silica (ODS
... Show MoreThis work reports the development of an analytical method for the simultaneous analysis of three fluoroquinolones; ciprofloxacin (CIP), norfloxacin (NOR) and ofloxacin (OFL) in soil matrix. The proposed method was performed by using microwave-assisted extraction (MAE), solid-phase extraction (SPE) for samples purification, and finally the pre-concentrated samples were analyzed by HPLC detector. In this study, various organic solvents were tested to extract the test compounds, and the extraction performance was evaluated by testing various parameters including extraction solvent, solvent volume, extraction time, temperature and number of the extraction cycles. The current method showed a good linearity over the concentration ranging from
... Show MoreA solid Phase Extraction (SPE) followed by HPLC-UV method is described for the simultaneous quantitative determination of nine priority pollutant phenols : Phenol, 2- and 4-Nitrophenol, 2,4-Dimethylphenol, 2-, 2,4-Di-, 2,4,6-Tri-, and Penta- chlorophenol, 4 Chloro-3-methylphenol. The phenols were separated using a C-18 column with UV detector at wave length of 280nm. The Flow of mobile phase was isocratic consisted of 50:50 Acetonitrile: phosphate buffer pH=7.1, column temperature 45 C°, Flow Rate 0.7 ml/min. Calibration curves were linear (R2 = 0.9961-0.9995). The RSDs (1.301-5.805)%, LOD(39.1- 412.4) µg/L, LOQ(118.5-1250.8) µg/L, the Robustness (1.55-4.89), Ruggedness (2.82-4.00), Repeatability (2.1-4.95), Recoveries%
... Show MoreTwo simple methods for the determination of eugenol were developed. The first depends on the oxidative coupling of eugenol with p-amino-N,N-dimethylaniline (PADA) in the presence of K3[Fe(CN)6]. A linear regression calibration plot for eugenol was constructed at 600 nm, within a concentration range of 0.25-2.50 μg.mL–1 and a correlation coefficient (r) value of 0.9988. The limits of detection (LOD) and quantitation (LOQ) were 0.086 and 0.284 μg.mL–1, respectively. The second method is based on the dispersive liquid-liquid microextraction of the derivatized oxidative coupling product of eugenol with PADA. Under the optimized extraction procedure, the extracted colored product was determined spectrophotometrically at 618 nm. A l
... Show MoreA simple, accurate and rapid method for separation and determination of most commonly usedinsecticides in Iraq [thiamethoxam (Thi), imidacloprid (Imi), indoxacarb (Ind), and abamectin (Aba)] ispresented. The separation was performed by gradient reversed-phase high performance liquidchromatography on a C18 stationary phase column. The method was developed and validated. The-1mobile phase was a mixture of acetonitrile and water using gradient flow. The flow rate was 1.0 mL min .The optimum temperature of separation was 25 ºC. The detection was performed at multiple wavelengths.The analysis time was up to 10.5 minutes with retention times of 3.221, 3.854, 6.385, and 9.452 min for-1the studied insecticides. The linearity was in the range of 0.
... Show MoreA method is developed for the determination of iron (III) in pharmaceutical preparations by coupling cloud point extraction (CPE) and UV-Vis spectrophotometry. The method is based on the reaction of Fe(III) with excess drug ciprofloxacin (CIPRO) in dilute H2SO4, forming a hydrophobic Fe(III)- CIPRO complex which can be extracted into a non-ionic surfactant Triton X-114, and iron ions are determined spectrophotometrically at absorption maximum of 437 nm. Several variables which impact on the extraction and determination of Fe (III) are optimized in order to maximize the extraction efficiency and improve the sensitivity of the method. The interferences study is also considered to check the accuracy of the procedure. The results hav
... Show MoreA sensitive and environmentally benign spectrometric method was developed for quantifying Meprobamate (MEP). The analyzed MEP was derivatized into a colored complex and determined spectrometrically. The colorimetric analytical parameters were optimized and validated. Low limit of detection (LOD) was achieved down to 1.88×10-6 mol/l while the limit of quantification (LOQ) was extended over the range of 1.97×10-6 - 1.35×10-3 mol/l. The high precision has been denoted by the 1.54% value of the coefficient of variation. The recovery was 96.07%, while the RSD (n=3) was 1.05 - 1.19%. The apparent molar absorptivity (Æ) obtained within 1154.7 - 1691.9 L.mol-1.cm
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