Simultaneous kinetic determination of phosphate and silicate based on heteropoly blue formation

Small amounts of phosphate (0.08–1.16 μg ml^-1) and larger amounts of silicate (12–60 μg ml^-1) can be determined simultaneously by a kinetic method based on the difference in the rates of the heteropoly blue formation with molybdenum (V)—molybdenum (VI) mixtures in 0.28 M perchloric acid. The interference of large amounts of iron(III) on the determination of phosphate can be eliminated by masking with sodium hydrogen sulfite; this method is applicable to reagent-grade iron(III) chloride.     

Measurement of total tin in marine organisms by stannane generation and atomic absorption spectrometry

Tin is reduced to stannane by sodium tetrahydroborate solution, passed through a heated silica tube and measured by atomic absorption specirometry at 286.33 nm. The detection limit is 0.9 ng ml^-1 and the r.s.d. is 4.1% at 0.01 μg ml^-1. Interferences are discussed and the sample decomposition procedure evaluated. Typical results obtained for macroalgae. fish and molluscs are given.     

Flow injection spectrophotometric determination of europium using chlortetracycline

A flow injection (FI) spectrophotometric determination of europium (III) is described, based on the complexation between europium (III), and chlortetracycline (CTC) in a Tris-buffer pH 8.0 medium. The resulting yellow-coloured complex is measured at its absorption maximum of 400 nm after 100 μl of sample or standard solution containing europium (III) are injected into the merged streams of CTC and Tris-buffer solutions. Optimum conditions for determining μg amounts of europium (III) are achieved by univariate method. Various types of reactors are also investigated. It is shown that the use of a single bead string reactor gives rise to the enhancement of peak height. A linear calibration curve over the range of 0.10-0.60 μg ml⁻¹ europium (III) is established with the regression equation (n=6) Y=34.93X+0.01 and the correlation coefficient of 0.9994 is obtained. A detection limit (3σ) of 0.01 μg ml⁻¹ of europium (III) and the relative standard deviation (R.S.D.) of 4.32% for determining 1.0 μg ml⁻¹ of europium (III) (n=7) are obtained. The recommended method has been applied to the quantitation of europium (III) in spiked water and stream sediment samples with average recoveries of 99.9 and 97.5%, respectively. The sampling rate is found to be 85 h⁻¹.     

Kinetic determination of traces of manganese(II) by its catalytic effect on the oxidation of acid blue 45 with hydrogen peroxide

A catalytic method is described for the determination of trace amounts of manganese(II) based on its catalytic effect on the hydrogen peroxide oxidation of an anthraquinone dye, Acid blue 45 (C.I. 63010). The reaction is followed spectrophotometrically by measuring the rate of change in absorbance of the dye at 595 nm. The calibration graph (rate constant (tg α) vs. manganese concentration) is linear in the range 4–25 ng Mn ml^?1, the relative standard deviation being 1.9% at the 13 ng Mn ml^?1 level. There are few interferences. The kinetic parameters of the reaction were investigated and the role of hydrogen peroxide and hydrogencarbonate ions is discussed.     

Spectrophotometric determination of L-ascorbic acid in pharmaceutical preparations

The method is based on the oxidation of L-ascorbic acid with potassium hexacyanoferrate (III). Excess of oxidant is determined spectrophotometrically by oxidation of phthalophenone to phenolphthalein in alkaline solution. Linear calibration graphs are obtained for 0–7 μg ml^?1 ascorbic acid at 553 nm, with a detection limit of 0.1 μg ml^?1. Sugars and other organic compounds do not interfere when present in moderate amounts.     

Regeneration of poly-L-lysine modified carbon electrodes in the accumulation and cathodic stripping voltammetric determination of the cromoglycate anion

Cromoglycate is accumulated on a poly-l-lysine (PLL) modified carbon electrode best from pH 4 solution, where it is anionic and the PLL is cationic, and at which pH the cromoglycate gives a good reduction peak at −0.82 V. The PLL film can be regenerated readily by washing the electrode with 3 M sodium hydroxide solution, in which the PLL is deprotonated. Regeneration of the film is not required as frequently when larger amounts of PLL are incorporated into it. This allows standard addition procedures to be carried out without regenerating the electrode. Linear calibration graphs have been obtained typically in the range 0.1-1.5 μg ml⁻¹. Detection limits have been calculated to be 10 ng ml⁻¹. The standard addition method has been applied satisfactorily to diluted urine solutions.     

The determination of chromium(VI) in natural waters by differential pulse polarography.

A method utilizing differential pulse polarography for the determination of chromium(VI) in natural water is described. Additions of 0.62 μg Cu(II) ml^-1 and 0.55 μg Fe(III) ml^-1 did not interfere with the determination of 0.050 μg Cr(VI) ml^-1. The natural water samples containing chromium(VI) were buffered to approximately pH 7 with 0.1 M ammonium acetate and 0.005 M ethylene diamine and analyzed. Natural water samples of chromium content from 0.035 μg ml^-1 to 2.0 μg ml^-1 may be analyzed directly without further preparation. The detection limit is 0.010 μg ml^-1.     

Differential pulse polarographic determination of traces of iron in solar-grade silicon

Iron is determined, after volatilization of the matrix as hexafluorosilicic acid, by means of the polarographic iron(III) wave in a 0.1 M triethanolamine—0.1 M potassium bromate—0.5 M sodium hydroxide medium. Differential pulse polarography provides a detection limit of about 0.15 μg g^-1 with a precision of 1–2% and linear calibration graphs up to 0.5 μg Fe(III) ml^-1.     

Flow-injection extraction-spectrophotometric determination of permanganate with the ethylene-bis(triphenylphosphonium) cation

Permanganate is determined spectrophotometrically at 545 nm after extraction into chloroform of the ion-associate, ethylene -bis (triphenylphosphonium) permanganate. The carrier stream is pH 6 buffer containing 10% (w/v) ammonium fluoride and the reagent stream is 0.25% (w/v) ethylene-bis (triphenylphosphonium) bromide. The injection rate is 24 h^?1. Th calibration graph is linear up to 25 μg ml^?1 and the detection limit is 0.58 μg m^?1 Mn (VII), based on 250- μl injections. The system is applied to the determination of manganese in a range of steels.     

Kinetic-Spectrophotometric Determination of Molybdenum(VI) Based on Its Catalytic Effect on the Thionine-Hydrazine Reaction

Abstract

A kinetic method for the determination of trace amounts of Mo(VI) (0.05-4 μg ml^?1) based on its catalytic effect on the reduction of thionine by hydrazine monochloride in strongly acidic media is reported. The reaction is monitored spectrophotometrically by measuring the decrease in absorbance of thionine at 605 nm after a fixed time (5 min.). The detection limit of the method is 23 ng ml^?1 and the relative standard deviation (RSD) for 0.05 μg ml^?1 of Mo(VI) is 1.2% (n=7). The method is almost free from interferences, especially from large amounts of tungsten. The procedure was successfully applied to the determination of trace amounts of molybdenum in steel.     

Determination of manganese(VII) as 3,3′-Dianisole-4,4′-bis(3,5-diphenyltetrazolium chloride) complex and its application

A simple, rapid, selective and sensitive spectrophotometric method is described for the determination of trace amounts of manganese using Blue tetrazolium chloride as a chromogenic reagent. The method is based on the formation of ion-associate complex between manganese(VII) and the cation of ditetrazolium salt, having an absorption maximum at 255 nm. Beer’s law is obeyed in the range of 0.1–1.6 μg mL^?1. The molar absorptivity and Sandell’s sensitivity were found to be 4.97 × 10⁴ L mol^?1 cm^?1 and 1.11 × 10^?3 μg cm^?2, respectively. Limit of deterction is 6.86 ng mL^?1 Mn(VII) and limit of quantitation is 22.8 ng mL^?1 Mn(VII). Optimum reaction conditions were evaluated. The effect of interfering ions on the determination is described. The extraction, distribution and association constants, and the recovery factor have been calculated.     

On-line preconcentration of trace copper for flame atomic absorption spectrometry using a spherical cellulose sorbent with chemically bound quinolin-8-ol

Preconcentration was effected using a 50 mm × 2 mm i.d. minicolumn packed with a spherical cellulose sorbent with chemically bound quinolin-8-ol function groups (Ostorb Oxin). The column was connected to the nebulizer of the atomic absorption spectrometer and the sample solution and eluent (2 M hydrochloric acid) were sucked through it at a flow-rate of 2–3 ml min^?1 by utilizing the negative pressure of the nebulizer. The experimental design was tested with the determination of traces of copper. Peak-area and peak-height measurements were compared. Owing to the simple calibration, the former method was used for quantification. The dynamic range was from 0.3 ng ml^?1 (detection limit) to 5 μg ml^?1 (breakthrough). The reproducibility in the concentration range 25 ng ml^?1-5 μg ml^?1 was better than 5%. Water-soluble inorganic salts, ammonia and sodium hydroxide were analysed. The accuracy of the results was checked by anodic-stripping voltammetry and by electrothermal AAS.     

Kinetic determination of traces of manganese(II) by its catalytic effect on the autoxidation of 1,4-dihydroxy phthalimide dithiosemicarbazone

A kinetic method is described for the determination of trace amounts of manganese(II) based on its catalytic effect on the aerial oxidation of 1,4-dihydroxyphthalimide dithiosemicarbazone. The reaction is followed spectrophotometrically by measuring the rate of change in absorbance at 594 nm. The calibration graph (rate constant vs. manganese concentration) is linear in the range 10–90 ng Mn ml^-1. The preparation and properties of the reagent are described and the kinetic parameters of the reaction are reported. There are few interferences.     

Quinone—cyanide reactions: their use for the determination of quinones and cyanide

Both quinones and cyanide can be determined in the μg—ng ml^-1 range by measuring the fluorescence of the addition products produced. The yield is low (except for the 2-sulfonic acid of 1,4-naphthoquinone) in aqueous solution and 1:1 DMSO:water is the recommended medium for determinations of quinones. The 2-sulfonic acid of 1,4-naphthoquinone permits the determination of trace amounts of cyanide in aqueous solution; there are few interferences.     

“Stat” methods in continuous flow analysis : Determination of Copper,Iron, Iodide and Hydrochloric Acid

A continuous flow “stat” method is described in which a certain arbitrarily imposed state in the flowing stream is automatically maintained by regulating the rate of flow of one of the components. The electronic system is regulated by measuring a physical phenomenon in the flowing solution. The method is illustrated by the examples of a continuous flow absorptiostat [Fe(III)/S₂O₃^2-/Cu(II)]for determinations of copper(II) (1–10 μg ml^-1), iron(III) (25–250 or 12.5–125 μg ml^-1), as well as for determination of iodide (12.8–128 μg ml^-1). A continuous flow conductostat [HCl/NaOH] for determination of 1–2.5 × 10^-4 M HCl is also described. This analytical technique is intended for automatic continuous monitoring of sample streams.     

An improved spectrophotometric determination of manganese(II) with 1-(2-quinolylazo)-2,4,5-trihydroxybenzene with applications to medicinal plants and chemical reagents

The effects of organic solvent, time and temperature on the colour-forming reaction are described. For nine solvents tested, the molar absorptivities were in the range 2.0×10⁴?6.7×10⁴ mol^?1 cm^?1; best sensitivity was obtained with a 1:1 water/2-propanol solution after a standing time of 35 min; temperature should be controlled to ±2°C. Beer's law was obeyed for 0–1.45 μg ml^?1 Mn(II). The improved method was applied to determinations of manganese(II) in various herbs and chemical reagents; the values found were in the range 5.4–48.4 μg g^?1 in herbs, and 0.001-0.012% (w/w) in reagents.     

Molekülabsorptionsspektrometrie bei elektrothermischer verdampfung in einer graphitrohrküvette: Teil 7. Untersuchung der erdalkali-halogen-molekülabsorptionen,bestimmung von Fluorid- und Chloridspuren durch die molekülabsorption von MgF- und MgCl-molekülen

(Molecular absorption spectrometry with electrothermal volatilization in a graphite tube. Part 7. A study of molecular absorption of alkaline earth halides and determination of traces of fluoride and chloride based on molecular absorption of MgF and MgCl moleculesv)The molecular absorption of alkaline earth halides, generated by volatilization in a normal graphite tube, is reported. Intense absorption bands were found only with MgF and MgCl molecules. These molecules are used for the determination of fluoride and chloride, respectively. Fluoride can be determined at 268.3 nm or 358.2 nm; for 10-μl injections, the linear ranges are, respectively, 0–6 μg ml^-1 and 0–35 μg ml^-1, with sensitivities (0.01 absorbance) of 2.4 ng and 7.5 ng. Chloride can be determined at 376.3 nm; response is linear up to 15 μg ml^-1, with a sensitivity of 5.8 ng if copper ions are added. Optimal conditions, interferences and mechanisms are discussed.     

Extraction and Spectrophotometric Determination of Manganese(VII) with N1-Hydroxy-N1,N2-Diphenylbenzamidine

Abstract

Spectrophotometric determination of manganese(VII) at 614 nm after its extraction with N¹ -hydroxy-N¹,N²-diphenylbenzamidine into amyl alcohol at pH 7–8 is described. Beer's law was obeyed for 0.1–10 μg ml^?1 Mn(VII). The effects of experimental variables and of several diverse ions on the determination of manganese(VII) have been studied. The method has been applied to the determination of manganese in steels and in water extracts of a commercial tea and is found to be simple, precise and highly selective.     

Simultaneous First-Derivative Spectrophotometric Determination of Nickel and Manganese Complexes with 2-(2-Pyridylmethyleneamino)phenol

Abstract

A method is proposed for the simultaneous determination of nickel and manganese by first-derivative spectrophotometry based on their reactions with 2-(2-pyridylmethyleneamino)phenol (PMAP) Schiff base. The method allows the determination of Ni and Mn in the concentration range 0.3–3.0 μg ml^?1 in mixtures with their ten-fold concentration ratio. The method has been applied for Ni and Mn determination in bronzes. To optimize the experimental conditions for spectrophotometric determination of Mn with PMAP stability constants at different pH values have been determined. A critical evaluation of the proposed method was performed by statistical analysis of the experimental data.     

Determination of chloramphenicol at ultra-trace levels by high-performance differential pulse polarography: Application to Milk and Meat

High-performance differential pulse polarography (h.p.d.p.p.) is used to determine the antibiotic chloramphenicol. Optimum operating conditions are discussed. Calibration curves are linear from 10 ng ml^-1 to 1 μg ml^-1; the detection limit is about 3 ng ml^-1. Above 1 μg ml^-1, deviations from linearity occur, because of adsorption of chloramphenicol at the mercury electrode. A correction, based on variations in natural drop time, is suggested. Chloramphenicol is readily extracted from milk or minced meat with diethyl ether. The ether is evaporated, and the residue is taken up in acetate buffer pH 4.7 and filtered through a membrane filter. Recoveries from samples fortified at levels of 10–1000 ng ml^-1 are about 60% for milk and 50% for minced meat.