Flotation-spectrophotometric determination of trace of germanium with isochromatic dye ion-pairs formed by rhodamine 6G and tetrabromofluorescein

A flotation spectrophotometric method for the determination of germanium with isochromatic dye ion-pairs is described. The molar ratio of germanium to rhodamine 6G to tetrabromofluorescein is 1:5:5. The apparent molar absorptivity is 5.8 x 10(5) l mol(-1) cm(-1) at 531 nm. Beer's law is obeyed over the concentration range of 5.0 x 10(-8)-1.25 x 10(-6) mol l(-1). The proposed method is sensitive and accuracy and can be applied satisfactorily to the determination of germanium in vegetables.     

Flow injection spectrophotometric analysis of lead in human saliva for monitoring environmental pollution

A new highly sensitive, simple and low-cost methodology for the direct determination of Pb (II) with 2-(5-bromo-2-pyridylazo)-5-dimethylaminophenol in ethanolic medium has been developed. The absorption spectroscopy of the complex has been examined in detail, and the chemical variables affecting the sensitivity of procedure studied, optimized and applied to the determination of trace amounts of lead in human saliva. Under the optimal experimental conditions, a precision of 1.61x10(-4) mug cm(-2) was achieved, the molar absorptivity being (epsilon) 5.6x10(4) l mol(-1) cm(-1). An FI technique is proposed, and it is possible to determine trace levels of lead by injection into a steam buffered at pH 7.15, containing 70% ethanol: 30% Tris buffer 3.5x10(-3) mol l(-1) (pH=7.2), 1x10(-4) mol l(-1) 5-BrDMPAP. The FIA configuration allows the analysis of 45 samples per hour. The lower limit of detection (LOD) was 1x10(-7) mol l(-1). The calibration plot was linear at least within two orders of magnitude of lead concentration. The use of an HPLC pump for the FI analysis led to a substantial improvement in the analytical performance of the method, which clearly satisfies the typical requirements for control processes.     

Simultaneous determination of gallium and indium with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol in cationic micellar medium using derivative spectrophotometry.

A new derivative spectrophotometric method for rapid and selective trace analysis of Ga3+ and In3+ and for their simultaneous determination using 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol in a cationic micellar medium is reported. Molar absorptivity and Sandell's sensitivity of 1:1 Ga+ and In3+ complexes at their lambda(max) 553 nm and 558 nm are: 7.22 x 10(4) l mol(-1) cm(-1) and 5.85 x 10(4) l mol(-1) cm(-1), and 0.96 ng cm(-2) and 1.96 ng cm(-2), respectively. Linearity is observed in the concentration range 0.023-0.700 microg ml(-1) for gallium and 0.076-1.52 microg ml(-1) for indium; IUPAC detection limit is 0.012 and 0.035 ng ml(-1), respectively. These metal ions interfere with the determination of each other. However, 0.07-0.70 microg ml(-1) Ga3+ and 0.115-1.150 microg ml(-1) In3+ could be determined simultaneously when present together by the derivative method without any prior separation. The proposed procedures have been successfully applied for the individual and simultaneous determination of gallium and indium in synthetic binary mixtures, standard reference materials and environmental samples.     

Spectrophotometric determination of nickel with p-acetylarsenazo

A spectrophotometric method for the determination of trace amounts of nickel is described. At pH 6, nickel reacts with p-acetylarsenazo to form a 1:2 coloured complex with an absorption maximum at 630 nm. The apparent molar absorptivity is 6.5 x 10(4) l.mol(-1) . cm(-1) . Beer's law is obeyed over the concentration range of 0-0.8 microg/ml. The proposed method is selective, sensitive and can be applied to the determination of nickel in aluminum alloy.     

Chronoamperometric determination of paracetamol using an avocado tissue (Persea americana) biosensor

A biosensor based on vaseline/graphite modified with avocado tissue (Persea americana) as the source of polyphenol oxidase was developed and used for the chronoamperometric determination of paracetamol in pharmaceutical formulations. This enzyme catalyses the oxidation of paracetamol to N-acetyl-p-benzoquinoneimine whose electrochemical reduction back to paracetamol was obtained at a potential of -0.12 V. After addition of paracetamol reference solutions in glass cell and stirring for 60 s for the accumulation of N-acetyl-p-benzoquinoneimine at the electrode surface under open-circuit conditions, the current response was monitored by 120 s without stirring. The currents obtained at 70 s were proportional to the paracetamol concentration from 1.2x10(-4) to 5.8x10(-3) mol l(-1) (r=0.9927) with a detection limit of 8.8x10(-5) mol l(-1). The recovery of paracetamol from two samples ranged from 97.9 to 100.7% and a relative standard deviation lower than 0.5% for a solution containing 5.0x10(-3) mol l(-1) paracetamol in 0.10 mol l(-1) phosphate buffer solution (pH 7.0; n=10) was obtained. The results obtained for paracetamol in pharmaceutical formulations using the proposed biosensor and those obtained using a pharmacopoeial procedure are in agreement at the 95% confidence level.     

Extraction and spectrophotometric determination of lead(II) with pyridine-2-acetaldehyde salicyloylhydrazone

Lead(II) reacts with pyridine-2-acetaldehyde salicyloylhydrazone (PASH) in the pH range 8.6-9.3 to form a yellow-green, 1:2 chelate which can be extracted into chloroform. Beer's law is obeyed in the concentration range 1.5-6.2 mug ml(-1) of lead(II). The molar absorptivity of the extracted species is 1.93 x 10(4) l mol(-1) cm(-1) at 380 nm. The proposed method is sensitive, simple, rapid, accurate and has been satisfactorily applied for the determination of lead in synthetic mixtures, alloys, water and soil samples.     

Selective flotation-spectrophotometric determination of trace copper(II) in natural waters, human blood and drug samples using phenanthraquinone monophenylthiosemicarbazone.

Copper(II) forms 1:1 and 1:2 intense red complexes with phenanthraquinone monophenylthiosemicarbazone (PPT) at pH 3-3.5 and > or =6.5, respectively. These complexes exhibit maximal absorbance at 545 and 517 nm, the molar absorptivity being 2.3 x 10(4) and 4.8 x 10(4) l mol(-1) cm(-1), respectively. However, the 1:1 complex was quantitatively floated with oleic acid (HOL) surfactant in the pH range 4.5-5.5, providing a highly selective and sensitive procedure for the spectrophotometric determination of CuII. The molar absorptivity of the floated Cu-PPT complex was 1.5 x 10(5) l mol)(-1) cm(-1). Beer's law was obeyed over the range 3-400 ppb at 545 nm. The analytical parameters affecting the flotation process and hence the determination of copper traces were reported. Also, the structure of the isolated solid complex and the mechanism of flotation were suggested. Moreover, the procedure was successfully applied to the analysis of CuII in natural waters, serum blood and some drug samples.     

Determination of submicrogram amounts of Mercury(II) with 5-(2'-carbomethoxyphenyl)azo-8-quinolinol in presence of anionic surfactant by derivative spectrophotometry

A new sensitive, rapid and selective method is proposed for the determination of mercury in submicrogram level. Mercury(II) forms an insoluble complex with 5-(2'-carbomethoxyphenyl)azo-8-quinolinol in aqueous medium at pH 4-4.8 which can be made soluble by the action of anionic surfactant. The dissolution of the complex results in an orange red colour which is stable for at least 20 hr. The molar absorptivity and Sandell's sensitivity are at 512 nm 8.00 x 10(4) l. mol(-1) . cm(-1) and 0.0025 mug/cm(2), respectively. Derivative spectrophotometry is used to achieve selectivity.     

Solvent extraction-spectrophotometric determination of phosphate with molybdate and malachite green in river water and sea-water

Molybdophosphate, formed between orthophosphate and molybdate in sulphuric acid solution, is extracted into a mixture of toluene and 4-methylpentan-2-one (1:3 v v ) with Malachite Green as counter-ion. A single extraction with equal phase volumes gives an apparent molar absorptivity for phosphate of 2.3 x 10(5) l.mole(-1).cm(-1) at 630 nm; the absorbance of the reagent blank is 0.03. With an organic to aqueous phase-volume ratio of 1:10, the molar absorptivity is 2.5 x 10(5) l.mole(-1).cm(-1) and the absorbance of the reagent blank 0.08. By the proposed method, ng ml levels of phosphorus can be determined, and the detection limit is about 0.1 ng ml . The standard deviation and relative standard deviation for the determination of phosphorus in tap water (4.3 ng ml ) are 0.05 ng ml and 1.1%, respectively. The method can also be applied to the determination of phosphorus in river water and sea-water.     

Flotation-spectrophotometric determination of mercury in water samples using iodide and ferroin.

This paper describes a simple and highly selective method for separation, preconcentration and spectrophotometric determination of trace amounts of mercury. The method is based on the flotation of an ion-associate of HgI4(2-) and ferroin between aqueous and n-heptane interface at pH 5. The ion-associate was then separated and dissolved in acetonitrile to measure its absorbance. Quantitative flotation of the ion-associate was achieved when the volume of the water sample containing Hg(II) was varied over 50 - 800 ml. Beer's law was obeyed over the concentration range of 3.2 x 10(-8) - 9.5 x 10(-7) mol l(-1) with an apparent molar absorptivity of 1 x 10(6) l mol(-1) cm(-1) for a 500 ml aliquot of the water sample. The detection limit (n = 25) was 6.2 x 10(-9) mol l(-1), and the RSD (n = 5) for 3.19 x 10(-7) mol l(-1) of Hg(II) was 1.9%. A notable advantage of the method is that the determination of Hg(II) is free from the interference of the almost all cations and anions found in the environmental and waste water samples. The determination of Hg(II) in tap, synthetic waste, and seawater samples was carried out by the present method and a well-established method of extraction with dithizone. The results were satisfactorily comparable so that the applicability of the proposed method was confirmed in encountering with real samples.     

Determination of thallium(I) by flotation-spectrophotometric method using iodide and rhodamine B.

A method for the trace amount determination of Tl(I), via its preconcentration, is proposed. The method is based on the reaction of iodide, Tl(I) and Rhodamine B in a weakly acidic medium. In this process an ion-associated complex is formed, which is floated at the interface of aqueous-cyclohexane layers. Various amounts of Tl(I) by a subsequent separation and dissolution of the floated complex in methanol could be determined, spectrophotometrically. Beer's law was obeyed for the Tl(I) content in the range of (0.8-8.0) x 10(-7) mol l(-1) with a correlation coefficient of 0.9974. The conditional molar absorptivity was found to be 1.0 x 10(6) l mol(-1) cm(-1) at 560 nm, which indicated the considerable sensitivity of the procedure. The detection limit (DL) was 4.7 x 10(-8) mol l(-1) and the RSD (n = 5) for 4 x 10(-7) mol l(-1) of Tl(I) was 3.34%. None of the alkaline cations was interfered, and the interference of many other metal ions was eliminated via ion-exchange separation using a cation-exchanger resin, Amberlite IR-120, before the flotation step. The reliability of the procedure was confirmed by determining the Tl(I) contents of synthetic laboratory waste water by both flotation spectrophotometry and graphite furnace atomic absorption spectrometry (GFAAS). The recovery was 92.3-95.4% for 1 x 10(-7) and 4 x 10(-7) mol l(-1), respectively. The precision and accuracy of the results were comparable via F and t tests at the 95% confidence level.     

Simultaneous determination of beryllium and aluminium in mixtures using derivative spectrophotometry

The spectrophotometric determination of beryllium and aluminium with 5,8-dihydroxy-1,4-naphthoquinone in the presence of a non-ionic surfactant is reported. Absorption maxima, molar absorptivity and Sandell's Sensitivity of 1:2 (M:L) beryllium and aluminium complexes are, 585 nm and 598 nm, 1.63 x 10(4) l.mole(-1).cm(-1) and 2.04 x 10(4) l.mole(-1).cm(-1), and 0.55 ng/cm(2) and 1.32 ng/cm(2) respectively. Beer's law is obeyed between 7.20-3.96 x 10(2) ng/ml beryllium and 1.08 x 10(1)-1.08 x 10(3) ng/ml aluminium. A method for simultaneous determination of beryllium and aluminium in their mixture using derivative spectra is described. The range 3.6 x 10(1)-3.6 x 10(2) ng/ml beryllium could be determined in the presence of 1.08 x 10(2)-1.08 x 10(3) ng/ml aluminium, and vice versa.     

Silver-enhanced reduction of 2,3,5-triphenyl-2H-tetrazolium by semicarbazide for the spectrophotometric determination of traces of silver(I).

A sensitive spectrophotometric method for the determination of silver is described. The reaction involves a silver-enhanced reduction of 2,3,5-triphenyl-2H-tetrazolium chloride by semicarbazide hydrochloride to yield a pink-colored product with maximum absorption at 510 nm. Beer's law is obeyed in the concentration range of 0.02-0.34 microg cm(-3) of silver, and the molar absorptivity is 4.51 x 10(5) l mol(-1) cm(-1). The optical parameters, optimum reaction conditions and interference studies have been described. The method has been applied to the determination of silver in photographic film waste water and in synthetic samples.     

Extraction spectrophotometric determination of selenium(IV) with J acid in environmental samples

A new simple and sensitive method for the extraction and spectrophotometric determination of selenium(IV) is described. Selenium(IV) is reacted with J acid (6-ANSA) to form a butanol extractable complex with maximum absorbance of 520 nm. Beer's law is obeyed in the range of 0.03-0.3 mg/l. of selenium. Molar absorptivity and Sandell's sensitivity are found to be 18.5 +/- (0.1) x 10(3) l. mol(-1). cm(-1) and 0.004 microg/cm(2), respectively. The analytical parameters were optimized and the method applied for the determination of selenium in polluted water, soil, dust, hair and plant materials. The method is compared with other reported methods and found to be superior to many of the reported methods.     

Spectrophotometric determination of thorium in standard samples and monazite sands based on the floated complex of thorium with N-hydroxy-N,N′-diphenylbenzamidine and thorin

A selective and sensitive spectrophotometric method for the determination of Th(IV) has been based on the reaction with thorin and subsequent extraction of the red-orange coloured complex with N-hydroxy-N,N'-diphenylbenzamidine (HDPBA) in benzene as floated complex at pH 2.2. The complex in ethanol exhibits a maximum absorbance at 495 nm, with a molar absorptivity of 6.0x10(4) l mol(-1) cm(-1), with a Sandell's sensitivity of 3.9x10(-3) microg cm(-2). The method follows Beer's law up to 3.0 microg Th(IV) ml(-1). None of the common cations and anions tested interfere. The detection limit of the method is 0.04 microg Th(IV) ml(-1), the RSD (n=10) is 1.4%. The method has been successfully employed for the determination of thorium in various standard and monazite samples.     

Spectrophotometric determination of molybdenum based on charge transfer complex in PVA medium

A very simple, selective and sensitive method was developed for the spectrophotometric determination of Mo in the presence of W. The method was based on the formation of color charge transfer complex, molybdotungstophosphate-3,3',5,5'-tetramethylbezidine anion, which was solubilized and stabilized in PVA medium. Following the recommended procedure, molybdenum could be determined in the linear range of 0.04-2.5 mug ml(-1) and the molar absorptivity was 1.47x10(4) l mol(-1) cm(-1) at 660 nm. The proposed method had been applied to the determination of trace molybdenum in tungsten ore with satisfactory results.     

Sensitive determination of propoxur by spectrophotometry using 3-aminopyridine.

A simple spectrophotometric method for the determination of propoxur, a widely used insecticide, in various environmental samples and pesticide formulations is described. The method is based on the coupling of the hydrolysis product of propoxur with diazotized 3-aminopyridine in an alkaline medium, to form an azo-dye which has a maximum absorbance at 463 nm. Beer's law is obeyed over the concentration range of 0.05 to 1.2 microg ml(-1) of propoxur. The molar absorptivity and Sandell's sensitivity are found to be 3.10 x 10(4) l mol(-1) cm(-1) and 0.007 microg cm(-2), respectively. The important analytical parameters and optimum reaction conditions were evaluated. The method is free from the interference of other commonly used pesticides and inorganic metal ions.     

Spectrophotometric determination of palladium after solid-liquid extraction with 1-(2-Pyridylazo)-2-naphthol at 90 degrees C

An effective spectrophotometric determination of palladium with 1-(2-pyridylazo)-2-naphthol (PAN) using molten naphthalene as a diluent has been studied. A green complex of palladium with PAN is formed at 90 degrees C. In the range of pH 1.5-7.5, the complex is quantitatively extracted into molten naphthalene. The organic phase is anhydrously dissolved in CHCl(3) to be determined spectrophotometrically at 678 nm against the reagent blank. Beer's law is obeyed over the concentration range of 0.5-10 ppm. The molar absorptivity and Sandell's sensitivity are 1.2 x 10(4) l mol(-1) cm(-1) and 0.0070 mg cm(-2), respectively. The optimum conditions for determination are obtained. The interferences of various ions are observed in detail. The method has been applied to the determination of palladium in synthetic samples.     

Rapid and selective method for the spectrophotometric determination of nickel naphthenate in gasoline in a microemulsion

A new method for the spectrophotometric determination of nickel naphthenate in gasoline in a microemulsion was developed. PAN reacts with nickel(II) forming a red complex with composition 1:2 (metal to ligand) nickel(II)-PAN and absorption maximum at 568 nm. Nickel naphthenate in gasoline can be determined with PAN in a microemulsion, in the pH range 3.0 approximately 10.0 with a molar absorptivity of 4.8x10(4) l mol(-1) cm(-1). Beer's law was obeyed up to 0.8 mg l(-1) of nickel(II) in the microemulsion system. The interference of Cu(2+), Fe(3+), Mn(2+), Pb(2+) and Zn(2+) can be eliminated by adding 0.5 ml of a mixed masking agent. The method is rapid, simple and highly selective.     

A simple and sensitive analytical method for the determination of antimony in environmental and biological samples.

The results of a study and application of leucocrystal violet for the determination of antimony in parts per million levels is described here. The proposed method is based on the reaction of antimony(III) with acidified potassium iodate to liberate iodine. The liberated iodine selectively oxidizes leucocrystal violet to crystal violet dye. The formed dye shows maximum absorbance at 590 nm. The color system obeys Beer's law in the concentration range from 0.4 - 3.6 microg antimony per 25 ml of final solution. The molar absorptivity and Sandell's sensitivity were found to be 7.32 x 10(5) l mol(-1) cm(-1) and 0.0016 microg cm(-2), respectively. All variables were studied in order to optimize the reaction. The proposed method is satisfactorily applicable for the analysis of antimony in various environmental and biological samples. The method is simple, highly sensitive, accurate and reliable.