Determination of Traces Of Bismuth in Water with Polyurethane Foak Thin-Layer Spectrophotometry

Abstract

A method for the spectrophotometric determination of bismuth is described. The method is based on using polyether polyurethane foam sorbent as a favourable matrix. Sorption of the bismuth iodide complex into the foam thin layer contributed into substantial improvement of the measured absorbance value of the coloured species. In this way quite satisfactory results were achieved, the average recovery amounts to 105.25%.     

Sensitive Synchronous Spectrofluorimetric Methods for the Determination of 1- and 2-Naphthol in Micellar Media

Abstract

The interaction of 1-naphthol and 2-naphthol with several quaternary ammonium salts was studied. Spectrofluorimetric methods were developed for the determination of both naphthols in hexadecyltrimethylammonium bromide micellar medium. The detection limits are 1.4 and 10.2 ng/ml for 1-naphthol, and 6.2 and 5.1 ng/ml for 2-naphthol employing the conventional and synchronous spectrofluorimetric methods, respectively. The use of the first-derivative spectrum allows for the simultaneous determination of both naphthols. The recoveries of 1-naphthol and 2-naphthol in natural waters are acceptable.     

Two-stage extraction preconcentration and HPLC determination of phenol and 1-naphthol in aqueous solutions

The extraction of phenol and 1-naphthol with isomolar mixtures of ethyl acetate and hexane under batch conditions and with tributyl phosphate impregnated into a polyurethane foam under batch and dynamic conditions was studied. A procedure for determining phenol and 1-naphthol in aqueous samples was developed including their dynamic recovery on a column packed with polyurethane foam impregnated with tributyl phosphate, elution with a 0.1 M NaCl solution of pH 12.5–13.0, extraction with a mixture of ethyl acetate and hexane, and separation by normal-phase high-performance liquid chromatography (HPLC) with UV-detection. The overall preconcentration coefficient was 250. The detection limits were 2.5 μg/L. The relative error of determination was lower than 18%. The time of one determination was 2–2.5 h.     

Semiquantitative and Quantitative Determination of Trace Amount of Phosphate Ion in Water Using Polyurethane Foam Thin -Layer Colorimetry

Abstract

A simple, sensitive and fast method for the colorimetric determination of phosphate ion in water is described.

The method is based on spectrophotometric measurement of the blue molybdoantimony phosphoric acid species sorbed in a polyurethane foam thin-layer for quantitative determination of phosphate ion, or the visual color comparison technique for rapid semiquantitative determination.

The detection limit for the quantitative procedure is 5 μg/1 and for semiquantitative procedure 20 μg/1 for sample volumes of 100 ml and 25 ml, respectively.     

Pulsating column separation and preconcentration of radioiodine on hydrophobic organic reagent loaded resilient open-cell polyurethane foam

The method is based on the resiliency of the open-cell polyurethane foam filling used in a pulsing bed column. A liquid anion exchanger containing I₂ has been used as a hydrophobic organic phase immobilized in the polyurethane foam matrix. Forced flow of the mobile phase during successive pulsing of the column bed results in high preconcentration factors with practically quantitative separation yields. The pulsated column technique may also be conveniently automated. It can be utilized most advantageously for the rapid determination of low activity radioiodine in environmental waters mainly in routine field analysis.     

Test method for the determination of hydrogen peroxide in atmospheric precipitation and water using indicator papers

A test method is proposed for the determination of hydrogen peroxide based on the oxidation of 4-chloro-1 -naphthol oro-tolidine catalyzed with horseradish peroxidase on cellulose or aldehydecellulose papers. The concentration of H₂O₂ is determined by the length of the colored zone on a test strip (3 x 80 mm) sealed into adhesive polymer film after its contact with the test solution. The analytical range of H₂O₂ is 0.1–300 mg/L. For the determination of H₂O₂ by the color intensity of indicator paper after passing 20 mL of a test solution, the analytical range is 0.005-1 mg/L. Rapid test procedures for the determination of hydrogen peroxide in atmospheric precipitation and in waste and natural waters are developed and tested (RSD ≤ 30%).     

Synergistic Spectrophotometric and Atomic Absorption Spectrometric Analysis of Zinc in Alloys and Environmental Samples with N-p-MEthoxyphenyl-2-Furylacrylohydroxamic Acid and Pyridylazo Reagents

Abstract

Zinc (II) was selectively extracted from aqueous solutions of pH 7.8–8.5 into chloroform with N-p-methoxyphenyl-2-furylacrylohydroxamic acid (MFHA). 1-(2-pyridylazo)-2-naphthol (PAN) or 2-[(5-nitro-2-pyridyl)azo]-1-naphthol (NPAN) were added to the extract to form intensely coloured ternary complexes measurable spectrophotometrically at 550 nm (? = 6.03 × 10⁴ 1 mol^?1 cm^?1) and 625 nm (? = 8.15 × 10⁴ mol^?1 cm^?1) respectively. For atomic absorption spectrometric analysis, methyl isobutyl ketone (MIBK) was used as extracting solvent instead of chloroform and the zinc-MFHA-MIBK extract was aspirated directly into an air-acetylene flame. The absorbance was measured at the 213.9 nm resonance line with a detection limit of 0.05 ppb, which was significantly better than the limit of 1.0 ppb achieved for zinc previously with flame AAS. The method tolerated a large number of anions and cations normally occurring with zinc in environmental samples, and was applied to the trace analysis of zinc in alloys, coal, plant tissues, animal tissues and natural waters. The combinations of MFHA and PAN/NPAN were chosen from eleven hydroxamic acids and nine pyridylazo reagents as detailed in the paper.     

Spectrophotometric simultaneous determination of creatinine and creatine by flow injection with reagent injection

The reactions of creatinine with picric acid and of creatine with 1-naphthol and biacetyl, both in an alkaline medium, have been used to develop a flow injection method for the simultaneous determination of creatinine and creatine, respectively. The sample containing both analytes is continuously merged with a picrate stream and mixed through the reactors; the coloured stream passes through a flow cell in a spectrophotometer set at 520 nm, recording a continuous signal proportional to the creatinine concentration. The mixture of the reagents 1-naphthol and biacetyl is inserted into the stream by use of the injection valve, which results in a peak (superimposed on the continuous signal), proportional to the creatine concentration. Linear calibration graphs for both analytes were obtained up to 30 mg l^–1 with relative standard deviations <2%, and a sampling rate of 42 measurements h^–1. The method was applied to the determination of creatinine and creatine in broth cube samples.     

Thick-target PIGE analysis of plant materials preconcentrated by dry ashing

An analytical methodology has been developed for the UV-spectrophotometric determination of carbaryl in waters after its preconcentration onto a polyether type polyurethane foam followed by on-line elution. The aforementioned strategy offers an easy way for in-field sampling and to improve the analytical sensitivity. Several chemical and flow variables (mass of sorbent, sample flow rate, sample volume and carrier flow rate) were studied to ensure the best performance of the system. Recovery studies, carried out on natural water samples spiked with known amounts of carbaryl at concentration levels between 250 and 500 mug l(-1), provided recovery percentages between 94 and 105%. A detection limit of 12 mug l(-1) was achieved and a variation coefficient of 3.4% was obtained at 0.50 mug ml(-1).     

Determination of Traces of Mercury (II) and Phenylmercury by Direct Polyurethane foam Thin-Layer Spectrophotometry

Abstract

The determination of mercury and phenylmercury in the ppb concentration range using polyurethane foam (PUF) thin-layer spectrophotometry has been described. Sorption of mercury and phenylmercury into foam parallepiped loaded with diphenylthiocarbazone (dithizone) contributed to considerable improvement in the absorbance value of the colored species, being concentrated about 140 times.

The method allowed the achievement of satisfactory results, the detection limits are 5 and 10 μg per litre for mercury and phenylmercury, respectively, for 100ml sample volume. The average recovery from tap water amounts to 100% for mercury and 96.6% for phenylmercury.     

Ultrasonic-assisted supramolecular solvent-based liquid phase microextraction of mercury as 1-(2-pyridylazo)-2-naphthol complexes from water samples

A separation-preconcentration method based on supramolecular solvent ultrasonic-assisted liquid-phase microextraction (Ss-USA-LPME) for spectrophotometric determination of mercury as 1-(2-pyridylazo)-2-naphthol (PAN) chelates has been established. Red coloured Hg(II)-PAN hydrophobic complex was extracted into the supramolecular phase (1-decanol/THF) at pH 9.5. The extract was separated from aqueous phase by centrifugation, diluted with ethanol and determined by UV–Vis spectrophotometer at λ_max = 560 nm. The influences of important analytical parameters such as pH, amount of PAN, 1-decanol and THF, sample volume and matrix effects for the quantitative recoveries were examined and optimised. Under the optimised experimental conditions, the amount of ligand, 1-decanol and THF were 1.0 × 10^–4 M, 200 µL and 300 µL, respectively. The optimum time of ultrasonic bath and centrifugation were found as 2 min and 5 min. A linear calibration graph was obtained linearly in the concentration ranges of 8.3–1000 µg L^?1. The preconcentration factor was obtained as 20. The limit of detection (LOD) was 2.6 µg L^?1 with the relative standard deviation (RSD) of 2.4% for mercury (C = 100 µg L^?1, n = 7). The validity of the developed Ss-USA-LPME technique was checked with a certified reference material of NIST 1641d. The presented method has been successfully applied to the determination of mercury in water samples.     

Determination of Lithium in Pharmaceutical preparations with 1-(2-Arsenophenylazo)-2-Hydroxy 3, 6-Naphthalendisulfonic Acid

Abstract

This paper reports the characteristics, in acetonic medium, of the lithium complex with 1-(2-arsenophenylazo)2-hydroxy 3,6-naphthalenedisulfonic acid (APHNDS).The analytical optimization is also reported. The coloured product was measured spectrophotometrically at 468 nm. The Beer's law was realized at 0.1–4.0 μg ml^?1. The method was used for the determination of lithium in pharmaceutical preparation. The reproducibility of the described method was efficient. The accuracy of the procedure was evaluated measuring the recovery, between 86.0–97.9 %.     

X-ray fluorescence and atomic emission determination of cobalt in water using polyurethane foam sorbents

The conditions of analytical signal formation during direct X-ray fluorescence and arc atomic emission determination of metals using polyurethane foam sorbents were studied. A sorption spectroscopic technique of cobalt determination in water with preconcentration in the form of thiocyanate complexes based on simple ethers using polyurethane foam sorbents was developed. The linear calibration range was two orders of magnitude. With a cobalt concentration from 25 ml of water in the static mode, the lower limit of the metal content was 3 and 9 μg/l for X-ray fluorescence and atomic emission methods, respectively.     

Chemical Recycling and Liquefaction of Rigid Polyurethane Foam Wastes through Microwave Assisted Glycolysis Process

Glycolysis of polyurethane rigid foams (PUFs) was performed utilizing microwave irradiation at atmospheric pressure. The effects of various metal hydroxide and acetate catalysts as well as different microwave powers were investigated. All reactions were monitored by FTIR spectroscopy. The recovered liquid product containing OH functional groups was applied as a portion of the polyol in formulation of a new polyurethane rigid foam product. The reactivity factors and densities were compared with the foam produced from totally virgin polyol.     

Spectrophotometric determination of uranium in natural waters after preconcentration on TBP-plasticized dibenzoylmethane-loaded polyurethane foams

A method is presented for the spectrophotometric determination of uranium in natural waters after a preconcentration step involving percolation of a suitable aliquot of the water sample whose pH is adjusted to 6.0–6.5 through a TBP-plasticized dibenzoylmethane-loaded polyurethane foam bed. Uranium on the foam is eluted with 0.6M HCl solution and then determined spectrophotometrically using arsenazo III as a chromogenic reagent.     

Indirect Determination of Phosphate by X-ray Fluorescence Spectrometry Using Polyurethane Foam

Abstract

An indirect X-ray fluorescence method for phosphate has been established based on the extraction of phosphomolybdate by polyurethane foam. The molybdenum, which is associated in a fixed ratio with phosphorus, is determined directly on foam, by X-ray fluorescence spectrometry.     

Determination of Copper by Atomic Absorption Spectrophotometry After Solid-Liquid Separation by Adsorption of its 1-Nitroso-2-Naphthol Complex onto Microcrystalline Benzophenone

ABSTRACT

A sensitive method for the determination of trace copper by preconcentration and adsorption of its 1-nitroso-2-naphthol complex onto the microcrystalline benzophenone has been developed. Several experimental conditions such as the pH of the solution, the quantities of 1-nitroso-2-naphthol and benzophenone, and the stirring time were optimized for effective separation. Trace copper in a 100 ml water sample was chelated with 2.0 ml of 0.050 M 1-nitroso-2-naphthol at pH 8.0. The solution was heated to 30 °C, stirred vigorously for 10 minutes to adsorb the copper complex quantitatively onto 0.20 g benzophenone. After the microcrystalline benzophenone adsorbed copper complex was filtered and dissolved in acetone, the content of copper was determined by flame atomic absorption spectrophotometry. The interfering effects of concomitant ions were investigated and almost eliminated. The detection limit and the determination limit of this method were 6.9 ngml^?1 and 22.9 ngml^?1, respectively. Recoveries of 103.7 % and 94.2 % were obtained in a tap water and a brass sample, respectively. In the determination of copper in real samples, the values obtained by this proposed method were close to those by GF-AAS.

Based on these experimental results, it is supposed that this method can be applied to the determination of copper in real samples.     

A Routine Method for the Quantitative Determination of Polycyclic Aromatic Hydrocarbons (PAHs) in Urban Air

Abstract

We have developed a method for the quantitative determination of polycyclic aromatic hydrocarbons (PAHs) present in urban air, which can be performed rather quickly, and which uses a minimal amount of solvents.

Air samples were collected using a home-made low-volume air sampler equipped with glass fibre filter and polyurethane foam plugs. After Soxhlet extraction a liquid-liquid partition was carried out to isolate the PAH fraction. This liquid-liquid partition was performed in micro-scale, enabling us to use small quantities of the solvents and to separate the solution layers very rapidly using a centrifuge. Sample clean-up was accomplished on a high performance liquid chromatograph equipped with two normal phase silica columns. The losses of all investigated PAHs occurring during the various steps of sample clean-up have been determined. The qualitative and quantitative determination of the PAHs was carried out by capillary gas chromatography; the results were confirmed by GC/MS measurements.

The analytical procedure described was applied over a period of one year to measure the concentrations of 21 PAHs in the city of Vienna at a site with high traffic density. The concentrations of the four more volatile PAHs were determined on a semi-quantitative basis. The ratio of two selected PAHs was used to estimate the respective contribution of traffic and domestic heating to the total PAH level at the sampling site.     

On The Analysis of Procaine Hydrochloride By Diazotisation and Coupling Reaction

Abstract

N-(1-naphthyl) ethylene diamine dihydrochloride, thymol, α-naphthol and β-naphthol are used as coupling agents for the determination of diazotised procaine hydrochloride in pure form and in pharmaceutical preparations. All the experimental conditions have been adjusted, the effect of interferring substances, sensitivity and the validity of the procedure have been studied.     

Spectrofluorimetric determination of carbaryl and 1-naphthol in micellar media

The interaction of 1-naphthol-N-methyl-carbamate (carbaryl) and its degradation product, 1-naphthol, with the surfactant hexadecyl-trimethylammonium bromide has been studied. The micellar medium allows the direct spectrofluorimetric determination of carbaryl, with 6.2 ng/ml as detection limit in acidic medium, or indirectly, after hydrolysis, as 1-naphthol at pH 11.0 or pH 3.0 with detection limits of 0.4 and 1.6 ng/ml, respectively. The recoveries of carbaryl and 1-naphthol from natural waters are acceptable.