Solid phase extraction and spectrophotometric determination of Au(III) with 5-(2-hydroxy-5-nitrophenylazo)thiorhodanine.

A new chromogenic reagent, 5-(2-hydroxy-5-nitrophenylazo)thiorhodanine (HNATR) was synthesized. A highly sensitive, selective and rapid method for the determination microg l(-1) level of Au(III) based on the rapid reaction of Au(III) with HNATR and the solid phase extraction of the colored complex with a reversed phase polymer-based C(18) cartridge have been developed. The HNATR reacted with Au(III) to form a red complex of a molar ratio 1:2 (Au(III) to HNATR) in the presence of 0.05 - 0.5 mol l(-1) of phosphoric acid solution and emulsifier-OP medium. This complex was enriched by the solid phase extraction with a polymer-based C(18) cartridge. The enrichment factor of 100 was achieved. The molar absorptivity of the complex is 1.37 x 10(5) l mol(-1) cm(-1) at 520 nm in the measured solution. The system obeys Beer's law in the range of 0.01 - 3 microg ml(-1). The relative standard deviation for eleven replicates sample of 0.5 microg l(-1) level is 2.18%. The detection limit, based on the three times of standard deviation is 0.02 microg l(-1) in the original sample. This method was applied to the determination of gold in water and ore with good results.     

Highly selective ionic liquid-based microextraction method for sensitive trace cobalt determination in environmental and biological samples

A simple and rapid dispersive liquid-liquid microextraction procedure based on an ionic liquid (IL-DLLME) was developed for selective determination of cobalt (Co) with electrothermal atomic absorption spectrometry (ETAAS) detection. Cobalt was initially complexed with 1-nitroso-2-naphtol (1N2N) reagent at pH 4.0. The IL-DLLME procedure was then performed by using a few microliters of the room temperature ionic liquid (RTIL) 1-hexyl-3-methylimidazolium hexafluorophosphate [C₆mim][PF₆] as extractant while methanol was the dispersant solvent. After microextraction procedure, the Co-enriched RTIL phase was solubilized in methanol and directly injected into the graphite furnace. The effect of several variables on Co-1N2N complex formation, extraction with the dispersed RTIL phase, and analyte detection with ETAAS, was carefully studied in this work. An enrichment factor of 120 was obtained with only 6 mL of sample solution and under optimal experimental conditions. The resultant limit of detection (LOD) was 3.8 ng L⁻¹, while the relative standard deviation (RSD) was 3.4% (at 1 μg L⁻¹ Co level and n = 10), calculated from the peak height of absorbance signals. The accuracy of the proposed methodology was tested by analysis of a certified reference material. The method was successfully applied for the determination of Co in environmental and biological samples.     

Highly selective and sensitive spectrophotometric determination of trace amounts of silver ion in surfactant media using 2-mercaptobenzoxazole

A simple and accurate spectrophotometric method for determination of trace amounts of silver ion in tap and wastewater solution and photographic solutions has been described. The spectrophotometric determination of silver ion using 2-mercaptobenzoxazole (MBO) in the presence of Triton X-100 as nonionic surfactant has been carried out. The Beer's law is obeyed over the concentration range of 0.1-9.0 microg mL(-1) of Ag+ ion with the detection limits of 1.6 ng mL(-1). The influence of type and amount of surfactant, pH, complexation time and amount of ligand on sensitivity of method were optimized. Finally the repeatability, accuracy and the effect of interfering ions on the determination of silver ion were evaluated. There is a good agreement between results of proposed method and atomic absorption spectrometry.     

A sensitive spectrophotometric method for the determination of trace amounts of uranium(VI) using 2-hydroxy-1-naphthaldehyde isonicotinoyl hydrazone

The reaction between uranium(VI) and 2-hydroxy-1-naphthaldehyde isonicotinoyl hydrazone (2HNAINH) has been investigated in HCl-sodium acetate buffers and a highly sensitive and simple procedure for the determination of uranium(VI) is suggested. The orange red colored complex showed maximum absorption at 430 nm in buffer solutions of pH 3. Beer's law is obeyed in the range of 0.2 to 33 g ml^–1. The molar absorptivity and Sandell's sensitivity are found to be 9.6×10³ mol·l^–1 and 0.025 g cm^–2, respectively. The composition of the complex between metal and reagent is found to be 11. The effect of diverse ions is also studied and the method is successfully applied for the determination of uranium in synthetic mixtures.     

An improved spectrophotometric method for the determination of silver with 5-[p-(dimethylamino)benzylidene]rhodanine

The proposed spectrophotometric determination of Ag(+) with 5-[p(dimethylamino)benzyl-idene]rhodanine has the following improvements: (1) more effective control of pH; (2) use of poly(vinyl alcohol)-200 as the protective colloid to enhance the molar absorptivity to 3.5 x 10(-4) l.mole(-1).cm(-1) and to lengthen the period of stable absorbance to 50 min; (3) use of lactic and hydrofluoric acids as maskants to improve the selectivity. Beer's law is obeyed over the range 10-40 mug of Ag. The standard deviation is 0.39 mug of Ag (n = 14).     

1,5-二(2-羟基-5-氯苯基)-3-氰基甲 催化动力学光度法测定痕量锰(II)

The aerial oxidation of 1, 5-bis (2-hydroxy-5-chlorophenyl)- 3-cyanoformazan (HCPCF) in ammoniacal medium catalyzed by Mn(II) has been investigated and used for spectrophotometric determination of trace Mn(II) in water. The effect of various experimental factors was studied and the optimal conditions for Mn(II) determination were found. It has been shown that the reaction follows the rate expression:     

A sensitive and selective spectrophotometric method for the determination of chromium (III)

Microchimica Acta - Chromium (III) forms a golden yellow colour with tropolone on heating on a boiling water-bath, and is extractable into chloroform. The complex absorbs maximum at 400 nm. The...     

A new sensitive method for the spectrophotometric determination of molybdenum using 3-hydroxy-2-(2'-thienyl)-4H-chromen-4-one

A spectrophotometric method has been developed for the determination of Molybdenum (VI) using 3-hydroxy-2-(2'-thienyl)-4H-chromen-4-one as a complexing agent. The complex formed was dissolved in water in the presence of Triton X-100 and exhibits an absorption maximum at 410 nm. A large number of metal ions like Co(II), Ni(II), Mn(II), Cr(III), Zn(II), Cu(II), Hg(II), Bi(III), Fe(II), Fe(III), Zr(IV), V(V) can be tolerated at an appreciable concentrations. Molar absorptivity and Sandell's sensitivity of the method is 2.80 x 10(5) l mol-1cm-1 and 3.42 x 10(-4) micrograms cm-2, respectively. Beer's law is obeyed in the concentration range of 0.01-0.4 ppm Mo(VI). Aliquots containing 0.2 ppm of Mo(VI) give a mean absorbance of 0.56 with a relative standard deviation of 1.3%.     

Extraction and sensitive spectrophotometric determination of ytterbium with 2-(3,5-dichloro-2-pyridylazo)-5-dimethylaminophenol

The operating conditions for the absorptiometric determination of Yb(III) with the reagent 2-(3,5-dichloro-2-pyridylazo)-5-dimethylaminophenol (3,5-diClDMPAP) by a liquid—liquid extraction technique are presented. The complex yields a molar absorptivity of 1.54 × 10⁵l.mole⁻¹.cm⁻¹ (λ_max = 588 nm) and an optimum concentration range of 0.025–1.360n mg/l., at pH = 10. The method developed has been applied to the determination of Yb(III) in synthetic and concrete mixtures.     

一种简单灵敏的光度法测定环境水样中痕量对苯二酚

在SCN -存在下,控制溶液pH5.0,对苯二酚使Cu(Ⅱ)还原生成的Cu(Ⅰ)与SCN -反应生成CuSCN沉淀,通过测定溶液中剩余Cu(Ⅱ)的量,可以测定对苯二酚的含量.吸光度与对苯二酚含量之间存在良好线性关系.线性方程:A =4.567 +0.9726ρ(μg/mL),线性范围为0.16～4.0μg/mL,相关系...     

Kinetic spectrophotometric method for gold(III) determination

The kinetic spectrophotometric method for Au(III) determination was developed and validated. It was based on the catalytic effect of gold on the oxidation of methylene blue B (3,7di-(dimethyl amino)-10-dehydro-phenotiazin chloride) by ammonium peroxo-disulfate in citric buffer solution. There was the linearity of the calibration curve in the concentration range from 0.09 to 2.90 μg ml⁻¹ Au(III). The relative standard deviation was 2.50% and correlation coefficient of 0.9999. The limit of detection was determined as signal to noise ratio (3:1) and it was 5.5 ng ml⁻¹. The limit of quantification, based on signal to noise ratio 10:1 was 19.25 ng ml⁻¹. The selectivity was tested on the basis of influence of known amounts of different ions in the reaction mixture, upon the reaction rate. Kinetic and thermodynamic parameters were reported for both catalytic and non-catalytic reactions. The method was verified by Au(III) determination in anti-rheumatic drug “Tauredon” and in human urine samples, using ICP-AES as the comparative method. As the method is accurate, reliable, quick and simple it could be useful for clinical and toxicological practice.     

Highly sensitive spectrophotometric determination of trace amounts of platinum(IV) with the molybdate-basic dyes-poly(vinyl alcohol) system

Three highly sensitive spectrophotometric methods for the determination of platinum(IV) have been developed, based on its colour reactions with molybdate and basic dyes (BD) in aqueous solution in the presence of poly(vinyl alcohol). Platinum(IV) reacts with molybdate and BD to form ion — association complexes of composition (BD)₂[Pt (MoO₄)₃]. The molar absorptivities are between 6.83 × 10⁵ and 9.51 × 10⁵ dm³mol^–1cm^–1, the highest value being found with nile blue. Suitable conditions for the reactions and the effects of foreign ions were investigated. The methods can be applied to the spectrophotometric determination of trace amounts of platinum(IV) in some catalysts and ores.     

Combined extraction/multiwavelength spectrophotometric method for quantification of gold in geological samples

The capabilities of a combined liquid-liquid extraction/spectrophotometric method for the trace determination of gold in geological samples are presented. After extraction with ethyl acetate, gold in the extracts is quantified as tetrachloroaurate with the multicomponent data-processing programs inherent in a diode-array u.v.-visible spectrophotometer. This method has an overall detection limit of 0.4 μg Au g^?1 sample and a combined extraction/measurement imprecision of less than ± 12%.     

Catalytic spectrophotometric determination of trace amounts of copper(II) with 3-hydroxy-2-naphthoic acid

A very sensitive catalytic spectrophotometric method for the determination of copper(II) concentrations as low as 0.06 ng/ml is described. This method is based on the oxidation of 3-hydroxy-2-naphthoic acid by hydrogen peroxide in ammoniacal medium, catalysed by copper(II). The results of an exhaustive study of interferences are given. The new method is applied to determination of copper in atmospheric aerosol samples. A qualitative study of the mechanism by means of electron paramagnetic resonance spectroscopy is also included.     

Highly sensitive and selective assay method for iodide ion determination based on gold nanoparticles conjugated with glycol chitosan

A sensitive colorimetric method for the determination of iodide ions was developed using gold nanoparticles (AuNPs) functionalised with glycol chitosan (GCS). The iodide ions were at the centre of the O–I^––O coordination structure, formed with the GCS-AuNPs, reducing their interparticle distance and inducing aggregation. Time-of-flight secondary ion mass spectrometry analyses showed that the bound iodide ions were coordinated to the oxygen atoms of the ethylene glycol in GCS, with this aggregation leading to a considerable variation in colour from light red to dark violet. Using this GCS-AuNP probe, the iodide ion concentration in environmental, biological and pharmaceutical samples could be determined by both the naked eye and UV-Vis spectroscopy. Additionally, the sensitivity of the detection was found to be markedly enhanced at pH 6, where a more pronounced colour change was observed. The absorption ratio A₇₀₀/A₅₂₁ of the functionalised AuNP solution correlated linearly with the iodide ion concentration within the range 0.0–10.0 mg/L, and the limits of detection in tap water, pond water, and bovine serum solution were 3.5, 3.6, and 3.4 μg/L, respectively. The present assay method can thus be utilised to rapidly measure the concentration of iodide ions in aqueous samples.     

A sensitive spectrophotometric determination of niobium(V) with the reagent 5-chloro-8-hydroxy-7-iodoquinoline

Summary The determination of niobium at levels of 0.02% and above is required in certain types of stainless steels and niobium stabilized steels. A method has been developed for the determination of microgram amounts of niobium in stainless steels with the reagent 5-chloro-8-hydroxy-7-iodoquinoline in citric acid medium. The effects of heating time, pH, reagent concentration and other variables have been studied. The system obeyes Beer's law over the concentration range investigated. The optimum concentration range for measurements in 10-mm cells is 1.0–10.0g of niobium ml^–1. The molar absorptivity of the complex is 5.143 x 10³l·moli–1·cm^–1. The interferences from foreign ions have been evaluated. The stoichiometry of the complex ML₂ (metal:ligand) was confirmed by Job's continuous variations and mole ratio methods.

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Empfindliche spektrophotometrische Bestimmung von Niob(V) mit S-Chlor-8-hydroxy-7-jodchinolin

Zusammenfassung Die Bestimmung von Niob in der Größenordnung von 0,02% und darüber ist in der Stahlanalyse nötig. Ein Verfahren zur Bestimmung von Mikrogrammengen Niob in rostfreien Stählen mit 5-Chlor-8-hydroxy-7-jodchinolin in zitronensaurem Medium wurde ausgearbeitet. Der Einfluß von Temperatur, Zeit, pH, Reagenskonzentration u. a. wurde untersucht. In dem angegebenen Bereich folgt die Reaktion dem Beerschen Gesetz. Bei Verwendung von 10-mm-Küvetten ist die Menge von 1,0–10,0g/ml optimal. Die molare Absorptivität des Komplexes beträgt 5,143 x 10,0³l·mol^–1·cm^–1. Fremdioneneinflüsse wurden untersucht. Die Stöchiometrie des Komplexes (Metall:Ligand=12) wurde bestätigt.

     

Highly sensitive and selective spectrophotometric and spectrofluorimetric methods for the determination of ropinirole hydrochloride in tablets

Three sensitive, selective, accurate spectrophotometric and spectrofluorimetric methods have been developed for the determination of ropinirole hydrochloride in tablets. The first method was based on measuring the absorbance of drug solution in methanol at 250 nm. The Beer's law was obeyed in the concentration range 2.5-24 microg ml(-1). The second method was based on the charge transfer reaction of drug, as n-electron donor with 7,7,8,8-tetracyanoquinodimethane (TCNQ), as pi-acceptor in acetonitrile to give radical anions that are measured at 842 nm. The Beer's law was obeyed in the concentration range 0.6-8 microg ml(-1). The third method was based on derivatization reaction with 4-chloro-7-nitrobenzofurazan (NBD-Cl) in borate buffer of pH 8.5 followed by measuring the fluorescence intensity at 525 nm with excitation at 464 nm in chloroform. Beer's law was obeyed in the concentration range 0.01-1.3 microg ml(-1). The derivatization reaction product of drug with NBD-Cl was characterized by IR, 1H NMR and mass spectroscopy. The developed methods were validated. The following analytical parameters were investigated: the molar absorptivity (epsilon), limit of detection (LOD, microg ml(-1)) and limit of quantitation (LOQ, microg ml(-1)), precision, accuracy, recovery, and Sandell's sensitivity. Selectivity was validated by subjecting stock solution of ropinirole to acidic, basic, oxidative, and thermal degradation. No interference was observed from common excipients present in formulations. The proposed methods were successfully applied for determination of drug in tablets. The results of these proposed methods were compared with each other statistically.     

Simultaneous determination of palladium, platinum, rhodium and gold by on-line solid phase extraction and high performance liquid chromatography with 5-(2-hydroxy-5-nitrophenylazo)thiorhodanine as pre-column derivatization regents

In this paper, 5-(2-hydroxy-5-nitrophenylazo)thiorhodanine (HNATR) was synthesized. A new method for the simultaneous determination of palladium, platinum, rhodium and gold ions as metal-HNATR chelates was developed using a rapid analysis column high performance liquid chromatography equipped with on-line solid phase extraction technique. The samples (Water, human urine, geological samples and soil) were digested by microwave acid-digestion. The palladium, platinum, rhodium and gold ions in the digested samples were pre-column derivatized with HNATR to form colored chelates. The Pd-HNATR, Pt-HNATR, Rh-HNATR and Au-HNATR chelates can be absorbed onto the front of the enrichment column when they were injected into the injector and sent to the enrichment column [Zorbax Stable Bound, 10 mm x 4.6 mm, 1.8 microm] with a buffer solution of 0.05 mol L(-1) phosphoric acid as mobile phase. After the enrichment had finished, by switching the six ports switching valve, the retained chelates were back-flushed by mobile phase and travelling towards the analytical column. These chelates separation on the analytical column [Zorbax Stable Bound, 10 mm x 4.6 mm, 1.8 microm] was satisfactory with 72% acetonitrile (containing 0.05 mol L(-1) of phosphoric acid and 0.1% of Triton X-100) as mobile phase. The palladium, platinum, rhodium and gold chelates were separated completely within 2.5 min. Compared to the routine chromatographic method, more then 80% of separation time was shortened. By on-line solid phase extraction system, a large volume of sample (10 mL) can be injected, and the sensitivity of the method was greatly improved. The detection limits (S/N=3, the sample injection volume is 10 mL) of palladium, platinum, rhodium and gold in the original samples reaches 1.4, 1.8, 2.0 and 1.2 ng L(-1), respectively. The relative standard deviations for five replicate samples were 2.4-3.6%. The standard recoveries were 88-95%. This method was applied to the determination of palladium, platinum, rhodium and gold in human urine, water and geological samples with good results.     

Sensitive spectrophotometric determination of vanadium with 2-(5-bromo-2-pyridylazo)-5-diethyl-aminophenol (5-Br-PADAP)

A new sensitive and highly selective method is described for the spectrophotometric determination of microgram amounts of vanadium(V). First, vanadium is isolated by extraction withN-benzoyl-N-phenylhydroxylamine (BPHA) in chloroform from about 4M hydrochloric acid medium. Then, chloroform is evaporated and the residue mineralized with mixture of cone. perchloric and nitric acid. Finally, a colour reaction of vanadium(V) separated with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) in an acetate buffer (pH 4.5) gives a molar absorptivity of 5.48×10⁴l·mol^–1·cm^–1 at 585 nm. The proposed method was applied for the determination of traces of vanadium in aluminium samples. The results obtained show a good precision and accuracy of the method.