HPLC-FLD determination of 4-nonylphenol and 4-<Emphasis Type="Italic">tert</Emphasis>-octylphenol in surface water samples

A simple, sensitive and reliable HPLC-FLD method for the routine determination of 4-nonylphenol, 4-NP and 4-tert-octylphenol, 4-t-OP content in water samples was developed. The method consists in a liquid–liquid extraction of the target analytes with dichloromethane at pH  3.0–3.5 followed by the HPLC-FLD analysis of the organic extract using a Zorbax Eclipse XDB C8 column, isocratic elution with a mixed solvent acetonitrile/water 65:35, at a flow rate of 1.0 mL/min and applying a column temperature of 40°C. The method was validated and then applied with good results for the determination of 4-NP and 4-t-OP in Ialomi?a River water samples collected each month during 2006. The concentration levels of 4-NP and 4-t-OP vary between 0.08–0.17 μg/L with higher values of 0.24–0.37 μg/L in the summer months for 4-NP, and frequently <0.05 μg/L but also between 0.06–0.09 μg/L with higher values of 0.12–0.16 μg/L in July and August for 4-t-OP and were strongly influenced by sesonial and anthropic factors. The method was also applied on samples collected over 2 years 2007 and 2008 from urban wastewaters discharged into sewage or directly into the rivers by economic agents located in 30 Romanian towns. Good results were obtained when the method was used for analysis of effluents discharged into surface waters by 16 municipal wastewater treatment plants, during the year 2008.     

Monitoring of aminophenol isomers in surface water samples using a new HPLC method

A new HPLC method was developed for the simultaneous determination of aminophenol isomers by means of a mixed-mode stationary phase containing both SCX and C18 moieties. All factors influencing the separation were discussed and optimized. The chromatographic conditions for the separation of aminophenols are the stationary phase duet SCX/C18, the mobile phase of aqueous phosphate buffer (pH 4.85):methanol?=?85:15 (v/v) delivered with a flow rate of 1 mL/min and a detection at 285 nm. The method proposed was validated in terms of linearity, limits of detection and quantification, accuracy and precision. The HPLC method elaborated here was applied with good results on river water samples. In order to survey the quality of surface rivers entered in treatment plants which deliver water for Bucharest, two major rivers were included in a monitoring program which last more than 1 year.     

Valorization of titanium metal wastes as tanning agent used in leather industry

The development of new tanning agents and new technologies in the leather sector is required to cope with the increasingly higher environmental pressure on the current tanning materials and processes such as tanning with chromium salts. In this paper, the use of titanium wastes (cuttings) resulting from the process of obtaining highly pure titanium (ingots), for the synthesis of new tanning agent and tanning bovine hides with new tanning agent, as alternative to tanning with chromium salts are investigated. For this purpose, Ti waste and Ti-based tanning agent were characterized for metal content by inductively coupled plasma mass spectrometry (ICP-MS) and chemical analysis; the tanned leather (wet white leather) was characterized by Scanning Electron Microscope/Energy Dispersive Using X-ray (Analysis). SEM/EDX analysis for metal content; Differential scanning calorimetric (DSC), Micro-Hot-Table and standard shrinkage temperature showing a hydrothermal stability (ranged from 75.3 to 77 °C) and chemical analysis showing the leather is tanned and can be processed through the subsequent mechanical operations (splitting, shaving). On the other hand, an analysis of major minor trace substances from Ti-end waste (especially vanadium content) in new tanning agent and wet white leather (not detected) and residue stream was performed and showed that leachability of vanadium is acceptable. The results obtained show that new tanning agent obtained from Ti end waste can be used for tanning bovine hides, as eco-friendly alternative for chrome tanning.     

Determination of three alkylphenol isomers in various water samples using a new HPLC method based on a duet stationary phase

The level of three alkylphenols (APs) 4-nonylphenol, 4-octylphenol and 4-tert-octylphenol was monitored in various water samples using a new developed and validated HPLC method. The HPLC method employed a column with a mixed-mode stationary phase (C18/SCX) using a mobile phase of water to methanol?=?15:85 (v/v) delivered at a flow rate of 1 mL/min at room temperature. Both diode array, DAD and fluorescence, FLD detectors were employed. The method is linear when APs concentration ranged from 0.025 to 0.5 μg/mL with a DAD detection at 279 nm and between 0.0008 and 0.1 μg/mL when the detection was made by FLD (excitation at 220 nm, emission at 315 nm). The limit of detection and limit of quantitation for alkylphenols were found to be 5 and 15 ng/mL, respectively (detection by DAD). The method was employed with good results for the determination of APs in the presence of polycyclic aromatic hydrocarbons in various water samples.