Spectrophotometric determination of phenol and resorcinol by reaction with p-aminophenol

Based on the reaction with p-aminophenol, a series of procedures have been developed for the spectrophotometric determination of phenol and resorcinol. Three basic approaches have been studied: (i) a batch procedure, using the dissolved oxygen as oxidant, (ii) a stopped-flow procedure by use of KIO(4) as oxidant and (iii) a flow injection (FI) procedure developed in the presence of KIO(4). Phenol can be accurately determined at 626 nm, in the stopped-flow mode, after a reaction time of 45 min in 0.005M NaOH, 0.004M KIO(4) and 500 mug/ml of PAP. The development of a manifold, which incorporates a sample parking, is a convenient approach which makes it possible to measure, in the stopped-flow mode, four solutions in one hour. The limit of detection of this method corresponds to 64 ng/ml of phenol Resorcinol can be determined by FI at 540 nm in 0.006M NaOH, 0.0002M KIO(4) and 50 mug/ml PAP with a limit of detection of 6.6 ng/ml and a sample throughput of 300 injections per hour. A combination between the FI procedure for the determination of resorcinol and the stopped-flow procedure for phenol determination provides accurate results in the analysis of spiked samples containing both phenol and resorcinol.     

Spectrophotometric determination of ethiofencarb in waters by reaction with p-aminophenol

Summary An automatized procedure has been developed for the spectrophotometric determination of ethiofencarb in water by reaction with p-aminophenol after alkaline hydrolysis to obtain the corresponding phenol sulphone. The hydrolyzed samples are continuously introduced into different manifolds at the same time as 300 mg/l p-aminophenol, 0.004 mol/l KIO₄ and 0.04 mol/l NaOH solutions. The absorbance is measured at 638 nm after a reaction time of 6 min in stop flow. This absorbance band corresponds to the indo dye obtained from the reaction between the phenol sulphone of ethiofencarb and the quinoneimine form of the p-aminophenol and it permits a matrix-free spectrophotometric determination of ethiofencarb with a limit of detection of 33 g/l. The recovery of ethiofencarb in different water matrices varies from 71 to 126%.     

Spectrophotometric determination of palladium with sulfochlorophenolazorhodanine by flow injection

Sulfochlorophenolazorhodanine (as its sodium salt) has been used in the automated development of a sensitive flow-injection procedure for the spectrophotometric determination of palladium. The resulting method has high sample throughput, good precision, and low consumption of both sample and reagents. The optimum pH for the reaction is 5.0 and the response is constant at pH between 4.7 and 5.3. The sensitivity (calibration slope) of the procedure is 4.4 x 10(3) l./mole. The linear dynamic range is 0.045-30.0 mug/ml. The sample throughput is at least 120/hr. An automated procedure for optimization of analytical variables is described and a two-variable response surface for the system is given. Interference studies on 19 metal ions show that the method has good selectivity.     

Spectrophotometric determination of calcium with a flow injection system

The indirect spectrophotometric determination of 0.8–7.2 ppm calcium in the presence of magnesium, phosphate and sulphate by flow injection analysis (f.i.a.) is described. The method is based on the exchange reaction between the calcium and the zinc complex of ethylene glycol-bis(2-aminoethylether)tetraacetic acid (EGTA) in the presence of 4-(2-pyridylazo)resorcinol (PAR): Ca + Zn(EGTA) + 2 PAR ? Zn(PAR)₂ + Ca(EGTA). A home-made and a commercial flow injection system with a sampling rate of 80 h^?1, are compared. Results for water samples are in good agreement with those obtained by atomic absorption spectrometry.     

Spectrophotometric determination of pH by flow injection

Flow injection is used for the determination of pH over a wide range. Using an appropriate combination of pH-indicating dyes, plots of absorbance vs. pH are linear in the range pH < 1–8 for static measurements and pH 3.6–6.8 in the flow-injection experiment. In the current configuration, the flow-injection method has the capability of measuring approximately 100 samples h^?1 with a precision and accuracy of ±0.2 pH. The reasons for the linear calibration graphs, effects of ionic strength and day to day reproducibility are presented together with results for lake-water samples.     

Spectrophotometric flow injection determination of chloride in ethanol

A flow injection procedure is described for the spectrophotometric determination of chloride in ethanol, based on the mercury(II) thiocyanate—iron(III) reaction. Effects of reagent composition and ethanol content of the sample are investigated in detail. The proposed system can analyse 120 samples of ethanol (94–100% v/v) per hour, with a relative standard deviation lower than 1%, when the chloride content ranges from 0.1–6.0 ppm. Recoveries of ca. 96% are found.     

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.     

Spectrophotometric determination of aluminum in river water with bromopyrogallol red and n-tetradecyltrimethylammonium bromide by flow injection analysis

In the proposed flow injection system, the reagent solution contains bromopyrogallol red, n-tetradecyltrimethylammonium bromide and hexamine in 60% ethanolic solution, and the carrier solution contains acetate buffer, 1,10-phenanthroline and hydroxylammonium chloride. Sample solutions (160 μl) acidified by sulfuric acid are injected and the peak absorbance at 623 nm is recorded. The detection limit is about 0.001 ppm and calibration plots are linear for the ranges 0–0.3 and 0–0.1 ppm aluminum.     

Spectrophotometric determination of dopamine and methyldopa with metaperiodate by flow injection analysis

A flow-injection spectrophotometric method for determining dopamine and methyldopa is described. It is based on the oxidation reaction with metaperiodate. Calibration graphs were linear up to 2 × 10^–4 mol/l catecholamines. The method allows the measurement of 130 samples per hour and was successfully applied to the analyis of pharmaceuticals.     

Spectrophotometric determination of dopamine and methyldopa with metaperiodate by flow injection analysis

A flow-injection spectrophotometric method for determining dopamine and methyldopa is described. It is based on the oxidation reaction with metaperiodate. Calibration graphs were linear up to 2 x 10(-4) mol/l catecholamines. The method allows the measurement of 130 samples per hour and was successfully applied to the analyis of pharmaceuticals.     

Spectrophotometric determination of fluoxetine by batch and flow injection methods

A rapid, simple, and accurate spectrophotometric method is presented for the determination of fluoxetine by batch and flow injection analysis methods. The method is based on fluoxetine competitive complexation reaction with phenolphthalein-beta-cyclodextrin (PHP-beta-CD) inclusion complex. The increase in the absorbance of the solution at 554 nm by the addition of fluoxetine was measured. The formation constant for fluoxetin-beta-CD was calculated by non-linear least squares fitting. Fluoxetine can be determined in the range 7.0 x 10(-6)-2.4 x 10(-4) mol l(-1) and 5.0 x 10(-5)-1.0 x 10(-2) mol l(-1) by batch and flow methods, respectively. The limit of detection and limit of quantification were respectively 4.13 x 10(-6) mol l(-1) and 1.38 x 10(-5) mol l(-1) for batch and 2.46 x 10(-5) mol l(-1) and 8.22 x 10(-5) mol l(-1) for flow method. The sampling rate in flow injection analysis method was 80+/-5 samples h(-1). The method was applied to the determination of fluoxetine in pharmaceutical formulations and after addition to human urine samples.     

Spectrophotometric determination of nitrite in foodstuffs by flow injection analysis

A simple method for the determination of nitrite in foodstuffs by flow injection analysis is described. Nitrite samples are prepared in a microwave oven, treated with a 1 mol/lNH₄Cl solution at a pH of 9 (all under nitrogen atmosphere) and are immediately analysed. Nitrite is diazotised in the FIA system with N-(1-naphthyl) ethylenediammonium dichloride to form the highly coloured azo dye, which is measured at 540 nm. The detection limit is 0.036 mg/kg for sample injections of 400 l. The sampling rate is about 50 samples per hour and the relative standard deviation is 0.67%.     

Spectrophotometric determination of phenylephrine hydrochloride in pharmaceuticals by flow injection analysis exploiting the reaction with potassium ferricyanide and 4-aminoantipyrine

This paper presents a method for the determination of phenylephrine hydrochloride in pharmaceuticals by spectrophotometric flow injection analysis exploiting the reaction with potassium ferricyanide and 4-aminoantipyrine, which leads to the formation of a condensation product with strong absorptivity at 500 nm. The linear dynamic range was between 0.95 and 9 mg/L, with a limit of detection of 0.2 mg/L and a sampling throughput of 120 samples per hour. The method was applied to eyewashes and nasal decongestant liquid medicines.     

Spectrophotometric determination of rare earth elements by flow injection analysis based on their reaction with xylenol orange and cetylpyridinium bromide

Individual rare earth elements (REE) and their mixtures were determined by a FIA method based on the reaction with Xylenol Orange (XO) in the presence of cetylpyridinium bromide (CPB). Volumes of 30 microl of 2.5-25 microM REE solutions were injected into a carrier stream of 0.1M acetate buffer of pH 4.5 or 5.5 that was 0.06 mM in XO and 0.6 mM in CPB. At 1.8 ml/min flow rate, a sampling frequency of up to 100 samples per hour was achieved. The detection limits were in the range of 0.1-0.4 microg/ml REE and relative standard deviation of the measurement was 0.88% rel.     

Spectrophotometric determination of copper by flow injection analysis with an on-line reduction column

A silver reductor minicolumn is used ina flow-injection system for reduction of copper(II) to copper(I), which is detected spectrophotometrically using bathocuproine disulphonic acid. The reductor functions very well at flow rates up to 4 ml min^?1; this allows sample injection ar rates up to 120 h^?1. Linear calibration is achieved for 5 × 10^?7– 1 × 10^?4 M copper. The detection limit is 3.4 ng and the midrange precision is 1%.     

Spectrophotometric determination of trace-level bromate in drinking water after post-column reaction with pararosaniline based on multi-walled carbon nanotubes

A simple and sensitive spectrophotometric method is described for low level determinationof bromate in drinking water. This method is based on the reduction of bromate ions into bromine in the presence of pararosaniline by sodium metabisulphite to form a highly stable pink-red complex measured at 540 nm. Maximum colour formation was obtained at about 45 min. Multi-walled carbon nanotubes, a solid phase extraction sorbent, has been described for the removal of cationic interferences of major elements and heavy metals from water samples prior to conducting the assay. Bear’s law is obeyed in the range of 5–80 µg.L^?1 with limit of detection of 0.44 µg.L^?1 and correlation coefficient of 0.998 (n = 5). The mean relative standard deviation (RSD%) of the results within-day precision and accuracy were ≤1.2% which confirmed the reproducibility of the assay technique. The optimum assay conditions and their applicability to the determination of water samples are described. The method was successfully applied for the determination of bromate in water samples with satisfactory results and recommended to be applied in all desalination plant samples.     

Spectrophotometric determination of fluoride with lanthanum/alizarin complexone by flow injection analysis

Lanthanum/alizarin complexone (1:1) in 70% acetone is used in conjunction with a 500-cm reaction coil at 60°C to determine 0.03–1.2 mg l^?1 fluoride at 24 samples per h. The method is applied to tap-water samples.     

Flow analysis-spectrophotometric determination of L-Dopa in pharmaceutical formulations by reaction with p-aminophenol

A new method has been developed for the spectrophotometric determination of L-Dopa in pharmaceutical formulations. The method is based on the reaction between the open-chain quinone of L-Dopa, obtained in NaOH, and the benzoquinoneimine form of p-aminophenol, in the presence of KIO(4). The reaction product is determined at 574 nm by using both alternately procedures, one based on the stopped-flow and another on a flow injection approach. Under the best experimental conditions L-Dopa can be determined with a limit of detection of 52 ng/ml and a relative standard deviation of 0.2% for three replicate measurements of a solution containing 4 microg/ml.     

Spectrophotometric determination of ascorbic acid in pharmaceuticals by background correction and flow injection

Background correction has been shown to be an effective and indispensable modification in the spectrophotometric determination of ascorbic acid. The decomposition of ascorbic acid in pharmaceutical samples was carried out by incubation with sodium hydroxide to give products that were insensitive to ultraviolet light. The rapid oxidation in air of ascorbic acid, especially in dilute solutions, was avoided by the use of the flow injection principle for spectrophotometric determination and by employing a carrier stream of an anti-oxidizing nature consisting of 6 micrograms ml(-1) of 2-mercaptoethanol in 0.25% sulphuric acid. The optimized method with a single channel manifold made use of a carrier stream flow rate of 1.1 ml min(-1), an injection volume of 50 microl, a delay coil of 50 cm (0.5 mm i.d.) and detection at 245 nm. The throughput was at least 180 injections h(-1). The proposed flow injection method yielded results for the analysis of 0-20 micrograms ml(-1) of ascorbic acid that were 99-102% (relative standard deviation 0.6% or better) in agreement with those produced by comparable methods involving titration with iodine, chloranil or 2,6-dichlorophenolindophenol [4-(2,6-dichloro-4-hydroxyphenylimino)cyclohexa-2,5-dieno ne], and high-performance liquid chromatography. When the agreement was not good (as low as 14% with respect to the method being compared), this was traced to the presence of substances which are known to interfere in one or other of the methods of comparison.