Spectrophotometric determination of paracetamol with microwave assisted alkaline hydrolysis

A novel and rapid spectrophotometric method for the determination of paracetamol is proposed in this paper. The proposed method is based on the microwave assisted alkaline hydrolysis of paracetamol to p-aminophenol that reacts with S2- in the presence of Fe3+ as oxidant to produce a methylene blue-like dye having an absorptivity maximum at 540 nm. The experiment showed that paracetamol could be hydrolysed quantitatively to p-aminophenol in only 1.5 min under radiation power 640 W using a microwave in NaOH medium. The system obeys Beer's law in the range of 0-3.0 x 10(-4) mol l(-1) paracetamol. The molar absorptivity and Sandell's sensitivity were found to be 3.2 x 10(-3) l mol(-1) cm(-1) and 0.047 microg cm(-2), respectively. The relative standard deviation (n=11) was 1.7% for 8.0 x 10(-5) mol l(-1) paracetamol. The method has been applied successfully to analysis of paracetamol in pharmaceutical preparation.     

Spectrophotometric determination of zirconium with 9-methyl-2,3,7-trihydroxy-6-fluorone

Summary 9-Methyl-2.3.7-trihydroxy-6-fluorone has been used as a new colorimetric reagent for zirconium. The rose-red complex shows maximum absorption, against the reagent blank, at 500 nm and obeys Beer's law from 0.1 to 2.5 ppm. The optimum concentration range is from 0.66 to 2.5 ppm, where the per cent relative analysis error is 2.96. The composition of the complex, obtained from Job's method, indicates that the complex in solution contains the metal and the reagent in a ratio of 11. The instability constant of the complex is 1.07 · 10^–6.     

Spectrophotometric determination of molybdenum with 9-methyl-2,3,7-trihydroxy-6-fluorone

9-Methyl-2,3,7-trihydroxy-6-fluorone is proposed as a highly sensitive reagent for molybdenum. Thc rose-red complex shows maximum absorption at 510 mμ and obeys Beer's law from 0.2 to 3 p.p.m. of molybdenum, the optimum range being 08 to 3 p p m. where the percent relative analysis error is only 28. In solution the complex contains molybdenum and the reagent in the ratio 1:1. The instability constant of the complex is about 2.09·10^-6.     

9-Substituted acridines. Demethoxylation of 9-methoxyacridine and dechlorination of 9-chloroacridine in hydroxylic solvents

In methanol-water mixtures containing sodium or potassium hydroxide (up to 2.00M) the demethoxylation of 9-methoxyacridine to 9-acridone is of first order in both the free form of 9-methoxyacridine and the hydroxyl ion. The rate of the reaction is increased with an increase in the concentration of water. Sodium perchlorate has a small retarding effect on the reaction. In methanol-water mixtures containing perchloric or hydrochloric acid (up to 3.45M) the demethoxylation is of first order with respect to the protonated form of 9-methoxyacridine. The rate of the reaction decreases with an increase in the concentration of the acid or of sodium perchlorate, but when the concentration of water is increased (≈?1.7 to 50M) and that of the acid is not changed, it reaches a maximum value in mixtures containing 8 to 10M-water. The dechlorination of 9-chloroacridine to 9-methoxyacridine in methanol containing sodium hydroxide or methoxide (up to 0.31 M) is of first order in both the 9-chloroacridine and the hydroxyl or methoxyl ions.     

Spectrophotometric determination of osmium

Summary m-Amino benzoic acid in large excess reacts with tetra-, hexa- and octavalent osmium at theph range 4.5–6 to give a purple complex having absorption maximum at 500 nm. Beer's law is obeyed for 0.5 to 8 ppm of osmium(VI) and osmium(VIII) with optimum concentration range of 2 to 8 ppm of osmium(VI) and 3 to 8 ppm for osmium(VIII). The per cent relative error per 1% absolute photometric error is 2.8 for both osmium(VI) and osmium(VIII). Ions such as Pd²⁺, Rh³⁺, Ir⁴⁺, W⁶⁺, U⁶⁺, Co²⁺, Hg²⁺, Mg²⁺, Ca²⁺, Ba²⁺, Sr²⁺, Th⁴⁺ and Zr⁴⁺ do not interfere in the determination.Molar ratio method indicates that the reagent first reduces osmium (VIII) and osmium(VI) to osmium(IV), which then probably forms a 11 complex with the excess unoxidised reagent.Part III.: Anal. chim. Acta 22, 306 (1960); cf. Z. analyt. Chem. 177, 291 (1960).     

Spectrophotometric determination of bromide

A Spectrophotometric method for bromide determination has been developed. Bromide is converted to tribromide which absorbs at 267 nm. The detection limit is 0.01 g/ml bromide. As little as 0.4 g of bromide can be determined in an excess of chloride and sulfate with a coefficient of variation of 4%.     

Spectrophotometric determination of crotonaldehyde

Summary A spectrophotometric method for determining crotonaldehyde witho-tolidine in glacial acetic acid medium is described. Aromatic aldehydes interfere.

---

Zusammenfassung Ein spektrophotometrisches Verfahren zur Bestimmung von Krotonal-dehyd in Eisessiglösung unter Verwendung vono-Tolidin wurde beschrieben. Aromatische Aldehyde stören.

     

Spectrophotometric determination of phenylephrine

This paper describes a spectrophotometric assay procedure for the determination of small amounts of phenylephrine in the presence of a variety of foreign substances including ascorbic acid. This method is based on the formation of a blue colored indophenol derivative from the reaction of phenylephrine with N,2,6-trichloro-p-benzoquinoneimine.     

Spectrophotometric determination of peucedanin

Conclusions A spectrophotometric method has been proposed for determining peucedanin in a crystalline powder and in the roots ofPeucedanum Morisoni Bess.Khimiya Prirodnykh Soedinenii, Vol. 6, No. 1, pp. 3–6, 1970     

Spectrophotometric determination of piroxicam

The possibility of the spectrophotometric determination of piroxicam based on the extraction of its ion associate (IA) with the polymethine dye, 5-thiocyanate-1,3,3-trimethyl-2[(1E)-3-[(2E)-1,3,3-trime-thyl-1-H-indol-2-ilidine]-propenyl]-3H-indolium chloride. The maximal recovery of IA with toluene is achieved when pH of the aqueous phase is 8.0–12.0 and the concentration of the dye is (1.0–2.0) × 10⁻⁴. The molar absorption coefficient of IA is 8 × 10⁴, the detection limit of piroxicam is 0.49 μg/mL. A procedure has been developed for the extraction-spectrophotometric determination of piroxicam in the concentration range 1.0–20.0 μg/mL.     

电荷转移络合物分光光度法测定磺胺脒的研究

研究了电子给体磺胺脒与电子受体对苯醌之间的荷移反应。结果表明 ,在乙醇介质中磺胺脒与对苯醌能形成橙红色电荷转移络合物 ,且反应体系的pH范围较宽。络合物的最大吸收波长λmax=497.6nm ,表观摩尔吸光系数为 2 .3 5× 1 0 3L·mol- 1 ·cm- 1 ,比耳定律的线性范围是 0～ 5 0mg/L ,络合比为 1∶2。应用拟定的方法测定磺胺脒制剂的含量 ,平均回收率为 1 0 0 .4% ,可用于磺胺脒制剂的分析。     

Spectrophotometric determination of fusicoccin

Fusicoccin incubated for 17 h in 6 M HCl at 37°C gives rise to a chromophoric system having an absorption maximum at 555 nm. A colorimetric method for the determination of pure fusicoccin and of fusicoccin in fermentation liquors and infected plant tissues is described. The method is useful for 50–800 μg of fusicoccin.     

Spectrophotometric determination of ruthenium

Zusammenfassung Es wurde festgestellt, daß die Mehrzahl der Amidoxime mit folgenden Ionen reagiert: Hg²⁺, Cu²⁺, Fe³⁺, Co²⁺, UO₂ ²⁺, Cd²⁺, Ag^+;, Pb²⁺, Pd²⁺, Ni²⁺. Von den Malonsäure-bis-amidoximen wurden hergestellt die Silber-, Blei-, Cadmium-, Kupfer- und zwei Quecksilbersalze, von den Amidoximen der Nicotin- und Isonicotinsäure Palladium-, Kupfer-, Cadmium- und Bleisalze. Die Salzbildungsfähigkeit der Amidoximgruppe ist vom Radikal, von den Substituenten an der Amidgruppe und vom Reagens-medium abhängig. Die braunrote Färbung mit Fe³⁺-Ionen ist für alle Amidoxime typisch, diese Reaktion kann zum Nachweis der am Amidstickstoff nichtsubstituierten Amidoxime angewandt werden.IX. Mitteilung: Collect. czechoslov. chem. Commun. 24, 1720 (1959). — X. Mitteilung: Collect. czechoslov. chem. Commun. (im Druck).     

Spectrophotometric determination of EDTA

Both iron(III) and its EDTA complex in 0-1N H(2)SO(4) medium absorb in the ultraviolet region of the spectrum, with absorption maxima at 305 and 258 nm respectively. EDTA can thus be determined by addition of excess of Fe(III) and measurement of the absorbance at the two wavelengths. An EDTA concentration as low as 10(-6)M can be determined with a fair degree of accuracy. The method is free from interferences from most common metal ions, and is simple and rapid.     

Spectrophotometric determination of peucedanin

Chemistry of Natural Compounds - A spectrophotometric method has been proposed for determining peucedanin in a crystalline powder and in the roots ofPeucedanum Morisoni Bess.     

Spectrophotometric determination of aspidin

Chemistry of Natural Compounds - A spectrophotometric method is proposed for determining the content of aspidin in a crystalline powder and in the rhizomes of the fernsDryopteris spinulosa (M),D....     

Spectrophotometric determination of muzolimine

Five simple, rapid and sensitive spectrophotometric procedures for the determination of muzolimine in bulk samples and pharmaceutical dosage forms are described. The methods are based on the formation of coloured species when muzolimine is reacted with 3-methyl-2-benzothiazolinone hydrazone hydrochloride, p-N,N-dimethylphenylenediamine dihydrochloride or p-N-methylaminophenol sulphate and a suitable oxidant or with 2,6-dichloroquinone chlorimide. The results obtained are reproducible with a coefficient of variation of less than 1.5%.