Spectrophotometric determination of acetone in acetic acid

A sensitive and selective spectrophotometric method for the determination of acetone in acetic acid has been worked out. It is based on the reaction of acetone with diazotized p-aminobenzoic acid in a strongly alkaline medium to form a purple color with maximum absorption at 540 nm. Beer's law holds up in the range 20–140 μg of acetone in a final volume of 20 ml, with a molar absorptivity of 8.1 × 10³ liters mol^?1 cm^?1, sensitivity index of 0.0072 μg cm^?2, relative error of ?1.9 to +0.6%, and relative standard deviation of 0.7–3.5, depending on the concentration level. Furthermore, the color reaction is fast, and the procedure is simple, and avoids the use of an extraction.     

Spectrophotometric determination of formaldehyde,furfural, and vanillin in bisulfite solutions

Formaldehyde, furfural, and vanillin are determined in solutions containing bisulfite. The interference of bisulfite is eliminated by oxidation with iodine before furfural and vanillin are determined spectrophotometrically in ultraviolet light. Formaldehyde is determined with chromotropic acid by a slightly modified procedure; bisulfite is not destroyed previously.     

Chemiluminometric determination of vanillin in commercial vanillin products

Vanillin, ethylvanillin and 4-hydroxy-3-methoxy-benzylalcohol have been found to chemiluminesce by the action of potassium permanganate in sulphuric or polyphosphoric acid media. Both acid media have been compared and sulphuric acid allows the sensitive determination of 0.15-10.0, 0.010-1.0 and 0.0030-0.30 μg mL⁻¹ of vanillin, ethylvanillin and 4-hydroxy-3-methoxy-benzylalcohol with limits of detection equal to 0.045, 0.0030 and 0.00090 μg mL⁻¹, respectively. Recoveries of vanillin from commercial vanillin products are within the range of 95-109%. Comparison with results from the official method shows differences within the range of 0.5-3.0%. The chemiluminogenic reaction mechanism is also discussed.     

Spectrophotometric determination of indium using gallion

Summary The formation of violet coloured chelate of indium with Gallion has been studied. Indium forms only one chelate with Gallion at p_H 4.5 having _max 610 nm. The composition of the complex formed has been determined by various methods and is found to be 11 (MR). The values of stability constant have been calculated by three methods and the average value of logK obtained is 5.6 ± 0.1. A procedure for the spectrophotometric determination of indium has been suggested.

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Zusammenfassung Die Bildung eines violetten Chelates von Indium mit dem Reagens Gallion wurde studiert. In bildet damit ein einziges Chelat bei p_H=4,5 und _max=610 nm. Die Zusammensetzung des entstandenen Komplexes wurde nach verschiedenen Methoden ermittelt und gleich 11 (MetallReagens) gefunden. Die Stabilitätskonstante wurde nach drei Verfahren berechnet, wobei sich als Mittelwert logK=5,6±0,1 ergab. Eine Arbeitsvorschrift für die spektrophotometrische Bestimmung des In wird vorgeschlagen.

     

Spectrophotometric determination of hydralazine using p-dimethylaminobenzaldehyde

A new spectrophotometric method for the assay of hydralazine hydrochloride in bulk and dosage forms has been developed. The procedure is based on a condensation reaction between alcoholic solution of hydralazine and acidic solution of p-dimethylaminobenzaldehyde to generate an instant greenish-yellow coloured product. The hydrazone formed absorbed visible light strongly and optimal detector response was obtained at a wavelength of 470 nm with a molar absorptivity of 3.652 × 10³ l mol^?1 cm^?1. Optimization of temperature and time revealed 30 °C and 10 min as the best conditions for optimal color formation, while methanol was found to be the most suitable alcohol as diluting solvent. The reaction product is stable for at least 24 h. Beer’s law was obeyed in the concentration range of 2–10 μg ml^?1. Recovery studies over three days gave a mean recovery of 101.87% with a relative standard deviation of 1.29%. There was no interference from commonly used tablet excipients. There was no significant difference between the results obtained with the new method and the BP iodimetric method (p > 0.05). The proposed method is simple, sensitive, rapid and economical, and could find application as an in-process quality control method for hydralazine.     

Spectrophotometric determination of osmium using o-hydroxythiobenzhydrazide

Summary Osmium(VI) forms a violet complex witho-hydroxythiobenzhydrazide in the pH range 5.4–6.4. The complex is readily extractable in chloroform to give a violet solution which can be employed for the photometry of osmium. The extract shows maximal absorption at 540–550 nm and obeys Beer's law over the concentration range 1.44–14.40g Os ml^–1.g amounts of osmium can be determined witho-hydroxythiobenzhydrazide in the presence of considerable amounts of diverse ions commonly associated with the metal using EDTA as the masking agent. However, gold should be removed prior to the determination of osmium with the reagent. The molar extinction coefficient of the complex and the Sandell sensitivity are 1.18×10⁴ l mole^–1 cm^–1 and 0.016g cm^–2 respectively.

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Zusammenfassung Osmium(VI) bildet mit o-Hydroxythiobenzhydrazid zwischen pH 5,4 und 6,4 eine violette Komplexverbindung. Diese läßt sich mit Chloroform gut extrahieren. Die violette Lösung eignet sich für die photometrische Bestimmung des Osmiums, zeigt maximale Absorption bei 540–550 nm und entspricht zwischen 1,44 und 14,40g Os/ml dem Beerschen Gesetz. Mikrogrammengen Osmium können so neben erheblichen Mengen verschiedener anderer Begleitionen nach deren Maskierung mit ÄDTA bestimmt werden. Gold jedoch muß vorher entfernt werden. Der molare Extinktionskoeffizient beträgt 1,18×10⁴ l · Mol^–1 · cm^–1, die Empfindlichkeit nach Sandell 0,016g · cm^–2.

     

Spectrophotometric determination of zirconium using robinetin

Summary The complex formation between zirconium and robinetin has been spectrophotometrically investigated and made use of in the determination of zirconium. The complex has been found to contain zirconium and the flavonol in the molar ratio of 12. It obeys Beer's law up to 3.0 ppm of Zr and its stability constant has been calculated to be l.5×10⁹. The reaction is quite sensitive and selective at high concentrations of hydrochloric acid (sensitivity 0.0045 g/cm²).

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Zusammenfassung Zur spektrophotometrischen Bestimmung von Zirkonium wird als Reagens Robinetin empfohlen, das mit Zr einen Komplex im Verhältnis 12 (ZrRobinetin) bildet. Die Stabilitätskonstante wurde zu 1,5 · 10⁹ bestimmt. Das Beersche Gesetz wird bis zu 3,0 ppm Zr befolgt. In stark Salzsauren Lösungen ist die Reaktion empfindlich und selektiv (Empfindlichkeit: 0,0045 g Zr/cm²).

     

Spectrophotometric determination of palladium using arsenazo I

A new simple rapid method for the spectrophotometric determination of palladium using arsenazo I is given. The optimum conditions favoring the formation of the complex are extensively investigated; the molecular structure was found to be 1:1. Beer's law is obeyed for the ranges 1.0–10.6 or 0.64–6.39 ppm of Pd.     

Spectrophotometric determination of phosphate using lanthanum chloranilate

The spectrophotometric determination of phosphate using lanthanum chloranilate has been investigated. It is possible to determine 3–300 ppm of phosphate with an accuracy of ±2%, if suitable conditions are chosen. Chloride or nitrate ions do not interfere up to 400 ppm. Interference from sulphate ion can be compensated for by adding a large amount of sulphate both to the sample and to the standard solutions. This method is simpler, has less critical reaction conditions, and develops a much more stable coloration than the conventional heteropolyacid methods.     

液相色谱串联四极杆质谱法同时测定婴幼儿配方食品中甲基香兰素和乙基香兰素

建立了混合阴离子交换固相萃取柱净化,液相色谱串联四极杆质谱法测定婴幼儿配方食品中甲基香兰素和乙基香兰素的方法.样品经水和乙腈提取,CuSO4溶液沉淀蛋白,NaOH调节pH,增加样品溶解性,阴离子交换固相萃取柱净化.目标化合物在梯度洗脱条件下经C18柱分离后采用ESI源负离子多反应监测模式进行检测.分别选取了婴幼儿配方乳...     

Spectrophotometric determination of nitrate using chromotropic acid

A spectrophotometric method is described for the determination of nitrate in the 0.5 to 50μg range using chromotropic acid as the reagent and masking agents for the elimination of possible critical interferences due to chloride, chlorine, iron(III) and oxidants. The method can be applied directly for the determination of 0.2–20 mg of nitrate/l in 2.5-ml samples of water. Over 4000 mg of chloride/l can be tolerated. The method is simple, rapid and reliable. At the 1 mg/l level for nitrate the coefficient of variation at the 95% confidence limit is 4% There are no interferences.     

Spectrophotometric determination of formaldehyde by using formaldehyde dehydrogenase

A new method for the determination of formaldehyde by using formaldehyde dehydrogenase is described. The method is based on the quantitative oxidation of formaldehyde with oxidized nicotinamide adenine dinucleotide (NAD⁺), in the presence of formaldehyde dehydrogenase, to form the reduced dinucleotide (NADH). This enzyme does not require glutathione as a co-factor and the NADH produced, which is directly proportional to the concentration of formaldehyde in the assay solution, is then measured spectrophotometrically at 340 nm. Formaldehyde can be determined in the range 0.3–8.0 μg ml^?1 (1.0×10^?5–2.7× 10^?4 M) with a sensitivity of 0.216 absorbance/ μg ml^?1 (0.0065 absorbance/μM). Optimal conditions and the selectivity of this enzyme toward formaldehyde are described.     

Spectrophotometric determination of rhenium using 2-pyridyl thiourea

The reagent 2-pyridyl thiourea produces a reddish brown complex with rhenium in hydrochloric acid medium in the presence of tin(II) chloride. The complex shows absorption maxima at 405 nm, obeys Beer's law for a range of 1–16 ppm of rhenium. The sensitivity and molar absorptivity is found to be 0.0115g cm^–2 and 1.603×10⁴ 1 mol^–1 cm^–1 respectively showing an improvement over other sulphur-nitrogen bearing ligands. Composition found by Job's and mole ratio method, indicates that the complex contains metal and reagent in the ratio 12. Stability constant and stepwise formation constants of the complex have been evaluated by Harvey-Manning's method (logK _overall=8.825), Leden's method (logK _overall=8.3096), Rossotti-Rossotti's method (logK _overall=8.653) and Yatsimirskii's method (logK _overall=8.740). The relative error per 1% absolute photometric error is found to be 2.7%.     

Spectrophotometric determination of copper in alloys using naphthazarin

Naphthazarin (5,8-dihydroxy-1,4-naphthoquinone; Naph) is proposed as a chromogenic reagent for the spectrophotometric determination of copper(II). The polynuclear complex has a mole ratio of Cu:Naph=4:6 in a 50% v/v ethanol/water medium containing 0.1 M ammonium acetate and 1.5% (w/v) sodium dodecyl sulfate. The copper-naphthazarin complex shows an absorption maximum at 330 nm with a molar absorptivity of 1.84x10(4) l mol(-1) cm(-1). Beer's law is obeyed up to 4.5 ppm of copper(II). The method was applied for copper determination in alloy samples with satisfactory results.