A simple and very sensitive spectrophotometric method for the direct determination of copper ions

A sensitive spectrophotometric method for the direct determination of copper in aqueous samples without a preconcentration step has been developed. It is based on the formation of a yellow complex with the chromogenic reagent di-2-pyridyl ketone benzoylhydrazone (dPKBH) in an alkaline medium. The complex stoichiometry was 1:2 (Cu:dPKBH) and presents maximum absorbance at 370 nm. The influence of chemical variables affecting the behaviour of the system such as pH, concentration of dPKBH, buffer solution and ethanol, order of addition of the reagents and stability of the complex, were evaluated. The molar absorptivity (epsilon) was 3.92x10(4) L mol(-1) cm(-1), and Beer's law was obeyed up to 3 mg L(-1) of copper. The relative standard deviation was 0.46% (n=11) for a sample containing 1 mg L(-1) Cu(II). The limit of detection was 2.5 micro g L(-1) and was therefore more sensitive than the direct methods reported previously. Finally, the method was successfully validated by analysing several real samples with different matrices, such as tap water, natural water or copper alloys, with an average relative error of 2.46%.     

A selective spectrophotometric method for determination of copper with ferron

A selective spectrophotometric determination of copper is based on extraction of the copper-ferron complex with tribenzylamine in chloroform at low acidity, and measurement of the absorbance of the yellow extract at 410 nm. Beer's law is found to hold up to 8 microg/ml copper concentration. Of 30 elements tested, only molybdenum interferes. The ratio copper:ferron:tribenzylamine in the extracted species is 1:2:2.     

A sensitive spectrophotometric method for the determination of dithiocarbamate fungicide and its application in environmental samples

A sensitive spectrophotometric method based on the evolution of CS₂ and colour development by leuco crystal violet is described for the determination of dithiocarbamate fungicides, e.g. thiram, ziram and zineb. Dithiocarbamate fungicides release CS₂ on acid hydrolysis. This CS₂ is absorbed in ethanolic sodium hydroxide and forms xanthate. The xanthate formed is subsequently treated with potassium iodate and N-chlorosuccinimide, during which free iodine is liberated. Crystal violet dye was formed through selective oxidation of leuco crystal violet by liberated iodine, which has an absorbance maxima at 595 nm. The colour systems obey Beer's law in the range of 0.02–0.20, 0.02–0.24 and 0.04–0.32 ppm for thiram, ziram and zineb respectively. The molar absorptivity of the colour system were found to be 9.6×10⁵, 1.1×10⁶ and 6.8×10⁵±100 l mol⁻¹ cm⁻¹ for thiram, ziram and zineb respectively. The method has been successfully applied to the determination of these dithiocarbamate fungicides in various environmental samples.     

A derivative UV spectrophotometric method for the determination of levothyroxine sodium in tablets

A derivative UV (D-UV) spectrophotometric method was developed for the determination of Levothyroxine Sodium (L-T₄) in tablets of different doses. Quantification was performed using the second derivative of the absorption spectrum at 253 nm (²D₂₅₃) in methanol: water (50: 50; v/v) (pH 11.2). The method was validated and compared with an HPLC procedure carried out using a RP-18 column (125 × 4 mm, 5 μm) and methanol: phosphoric acid (0.1%) (70: 30, v/v) (pH 3) as mobile phase. Flow rate was set at 1.5 mL/min, and detection was performed at 225 nm. The proposed D-UV method was linear in the range 3.0–40.0 μg/mL with an appropriate precision and accuracy, and it was selective for the drug under study. On the other hand, results obtained by ²D₂₅₃ analysis were similar to those obtained by HPLC, with no statistically significant differences between them. Therefore, it was concluded that the developed method is suitable for the determination of L-T₄ in tablets at the tested doses.     

New method for the spectrophotometric determination of ultramicro amounts of copper

A deep yellow colour is formed by the reaction with phenol and chloramine-T in the presence of copper, and this reaction is used for the photometric determination of copper. An aqueous solution of copper and the reagents at pH 11.5-11.6 is heated. The molar absorptivity at 410 mmu, is 2.32 x 10(6). The method has been used satisfactorily to determine ultram amounts of copper in high-purity silicon.     

A simple method for the spectrophotometric determination of atrazine using p-aminoacetophenone and its application in environmental and biological samples

A spectrophotometric method is described for the determination of the widely used herbicide, atrazine. Atrazine reacts with pyridine and forms a quaternary halide which adds a hydroxyl group in the presence of alkali to form a carbinol base. The heterocyclic ring of the resulting carbinol breaks forming a glutaconic dialdehyde which is subsequently coupled with p-aminoacetophenone (PMP) to form a yellow orange polymethine dye. Beer's law is obeyed in the range 0.16–1.6 ppm of atrazine at 470 nm. The method is sensitive and free from the interference of most of the foreign species. The analytical parameters have been optimised and the method has been successfully applied to the determination of atrazine in various environmental and biological samples.     

A spectrophotometric method for uranium determination

A very sensitive extraction spectrophotometric method for the analysis of uranium based on the extraction of a uranium—benzoate—crystal violet complex by a mixture of xylene and benzene is described. The absorbance maximum is at 606 nm and molar absorptivity is 4.28·10⁴ l·mol⁻¹·cm⁻¹. The interference due to a number of anions and cations studied without any pre-extraction was found to be within permissible limits. The method has been used for determining uranium in a synthetic solution, i.e., uranium in the presence of various other ions. The interference due to some cations was eliminated by the use of a masking agent (boric acid).     

A spectrophotometric method for the determination of nickel

A photometric method for the determination of nickel using versene is described. Up to 20 mg of nickel can be determined with a maximum deviation of ± 0.10 mg. The effect of interfering elements, concentrations, accuracy and limitations of the method are discussed.     

A spectrophotometric method for the determination of nitrite

Nitrite reacts with dichromate quantitatively under suitable conditions of temperature and acid concentration. A linear relationship was found to exist between nitrite concentration and the absorbance at 580 nm of the chromium (III) species produced. This was used to determine the nitrite. The influence of a number of ions on the determination of nitrite was investigated; up to 100-fold excess nitrate has no influence on the determination of nitrite.     

A highly selective procedure for the spectrophotometric determination of aluminium with 8-hydroxy-quinoline and its application to the determination of

Aluminium, hydroxyquinolate can be quantitatively extracted by chloroform from an ammoniacal solution containing hydroxyquinoline, complexone and cyanide. Likewise extracted are titanium, vanadium, tantalum, niobium, uranium, zirconium, gallium, antimony, bismuth, indium and traces of beryllium. Aluminium can be separated from the first five elements by an extraction in ammoniacal solution containing hydrogen peroxide.Zirconium, gallium, bismuth and antimony can be eliminated by a cupferron extraction and indium by extraction with diethyldithiocarbamate. Beryllium is eliminated by performing an extraction with hydroxyquinoline at pH 5. The proposed method enables a practically specific photometrical determination of aluminium. Applications are given of the determination of trace and higher amounts of aluminium in steels, non-ferrous alloys and in glass.     

乙基紫褪色分光光度法测定七叶皂苷钠

在pH 4.1的BR缓冲溶液中,乙基紫(EV)与七叶皂苷钠(SA)作用,形成离子缔合物,溶液颜色发生明显褪色.其最大褪色波长位于594 nm处,七叶皂苷钠的质量浓度与褪色强度呈正比,七叶皂苷钠的质量浓度在0.15～35.0μg/mL范围内遵守比尔定律,相关系数为R=0.9995,摩尔吸光系数为2.5×104L·mol-1·cm-1,检出限为45.8 ng/mL.该方法已用于片剂和尿样中七叶皂苷钠的测定.     

A simple spectrophotometric method for the determination of minoxidil

A simple and sensitive method for the determination of minoxidil using 3-methyl-2-benzothiazolinone hydrazone (MBTH) and Fe(III) as the coloring agent is described. The method is sensitive to permit the determination of 0.5–4.5 μg ml⁻¹ of minoxidil at 500 nm. The accuracy and precision of the method were checked by high-performance liquid chromatography.     

A spectrophotometric method for the determination of nitric oxide

In dimethylsulfoxide, nitric oxide reduces copper(II) to copper(I) in the presence of p-chloroaniline. The resulting copper(I) is determined spectrophotometrically with 2,2′-biquinoline. The reactions are reproducible and the absorbance is proportional to the concentration of nitric oxide over the range 1.8–108 ppm (mg dm^?3. Most other atmospheric contaminants are without effect.     

A solid-phase spectrophotometric method for the determination of sulphathiazole

A spectrophotometric method for the determination of sulphathiazole (ST) has been developed, based on solid-phase spectrophotometry. The influence of experimental variables on fixation on Sephadex SP C-25 is discussed. The applicable concentration range is 0.10-10.00 mg/l., with a relative standard deviation of 0.62% and a detection limit of 0.02 mg/l. The accuracy and precision of the method are reported. The proposed method has been satisfactorily applied to the determination of sulphathiazole in pharmaceuticals.     

A new spectrophotometric method for the determination of nadolol

A new spectrophotometric method has been developed for the assay of nadolol in pure form and in tablets. The assay procedure is based on a derivatization methodology employing 4-carboxyl-2,6-dinitrobenzene diazonium ion (CDNBD) as a diazo coupling reagent. The azo dye formed between nadolol and CDNBD absorbed visible light at the wavelength maximum of 416 nm (λ_max) demonstrating a bathochromic shift from the absorption maximum of nadolol. Optimization studies established an optimal reaction time of 10 min at 60 °C. The assays were linear over 1.25–10 μg ml^?1 of nadolol, and the reaction occurred by a 3:1 reagent/drug stoichiometric ratio. The method is found to be selective and has a lower detection limit of 0.29 μg ml^?1. Recovery studies over three days gave mean recovery of 101.4% (RSD 3.0%). This new method has been successfully applied in the determination of nadolol and nadolol/bendroflumethiazide tablets with accuracy and precision similar to the official (USP) HPLC procedure (p > 0.05). The new procedure has the advantages of high sensitivity, lower limit of detection and could find application as an in-process quality control method for nadolol.     

A co-precipitation and spectrophotometric determination of micro-quantities of iron in Japanese brewing water and liquor

Summary Co-precipitation and spectrophotometric determination of microquantities of iron in the Japanese brewing water, Miya mizu, and in the Japanese liquor, Saké, have been investigated. Iron was collected from brewing water by co-precipitation with manganese dioxide, and was then determined spectrophotometrically witho-phenanthroline. The error of the method was about 0.1 g Fe in 500 ml, or 0.0002 ppm Fe, which corresponds to a relative error of about 20%. The brewing water Miya mizu investigated contains a very small quantity of iron, e. g., from 0.0001 to 0.0006 ± 0.0002 ppm of iron. Samples of Saké were ashed with sulphuric and nitric acids, and the procedure as for brewing water was followed. Pyrophosphate had no effect. The error in this case was about 0.005 ppm Fe, which corresponds to 0.25 g Fe in 50 ml or to a relative error of 2%. Saké contains, for example, 0.263 ±0.005 ppm of iron.

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Zusammenfassung Die Mitfällung und spektrophotometrische Bestimmung von Mikromengen Eisen in dem japanischen Brauereiwasser Miya mizu und in dem japanischen Reisbier Saké wurde untersucht. Das Eisen wurde durch Mitfällung mit Mangandioxyd aus Miya mizu angereichert und dann mit o-Phenanthrolin spektrophotometrisch bestimmt. Der Fehler dieses Verfahrens betrug etwa 0,1 g Fe für 500 ml bzw. 0,0002 ppm. Dies entspricht einer relativen Abweichung von etwa 20%. Das untersuchte Miya mizu enthält nur sehr kleine Eisenmengen in der Größenordnung von 0,0001 bis 0,0006 ± 0,0002 ppm. Die Saké-Proben wurden mit Schwefelsäure und Salpetersäure verascht und weiter in gleicher Weise aufgearbeitet. Die Anwesenheit von Pyrophosphat hatte keinen störenden Einfluß auf das Verfahren. Der Fehler betrug in diesem Fall etwa 0,005 ppm Fe; dies entspricht 0,25 g Fe in 50 ml bzw. einer relativen Abweichung von 2%. Saké enthält beispielsweise 0,263 ± 0,005 ppm Fe.

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Résumé On a étudié le dosage par co-précipitation et par spectrophotométrie de microquantités de fer dans l'eau de brasserie japonaise »Miya mizu« et dans la liqueur japonaise » Saké«. On a recueilli le fer de l'eau de brasserie par co-précipitation avec le bi-oxyde de manganèse et on l'a dosé par spectrophotométrie avec l'o-phénanthroline. L'erreur de la méthode est d'environ 0,1 g Fe pour 500 ml, soit 0,0002 p. p. m. Fe, ce qui correspond à une erreur relative d'environ 20%. L'eau de brasserie »Miya mizu« étudiée contient une très petite quantité de fer, environ 0,0001 à 0,0006 ± 0,0002 p. p. m. de fer. On a fait les cendres sulfuriques et nitriques avec les échantillons de »Saké« et l'on a ensuite suivi le même processus que pour l'eau de brasserie. Les pyrophosphates étaient sans effet. Dans ce cas, l'erreur était d'environ 0,005 p. p. m. de fer, ce qui correspond à 0,25 g Fe dans 50 ml, soit une erreur relative de 2%. Le »Saké« contient par exemple 0,263 ± 0,005 p. p. m. de fer.

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Work done under the auspices of the Nadagogo Brewing Guild.     

A facile spectrophotometric method for cobalt determination using alpha-benzilmonoxime in sodium dodecylsulfate micellar solutions.

Alpha-benzilmonoxime in sodium dodecylsulfate micellar media has been used for the spectrophotometric determination of cobalt at pH 9.0. The linear range of calibration is 0.05-1.50 microg cm(-3) of cobalt at 380 nm with molar absorptivity of 3.72 x 10(4) dm3 mol(-1) cm(-1), which is about 1.5-times greater than that of the alpha-benzilmonoxime extraction based method. The relative standard deviations, recoveries, detection limit and effects of diverse ions on the determination of cobalt were studied. These analytical results were satisfactory. The method was successfully applied to the determination of cobalt in the various samples.