Flow-injection spectrophotometric determination of fluoride by using the zirconium/alizarin red S complex

A spectrophotometric flow-injection procedure is described for fluoride in aqueous samples. The method is based on the decrease in absorbance of the zirconium/alizarin red S complex at 520 nm; linear response is obtained for the range 0.1–10 mg l^?1 fluoride at a sampling rate of 100 h^?1. Aluminum(III), iron(III) and phosphate interfere.     

The automatic determination of fluoride in sea water and other natural waters

A Technicon AutoAnalyzer has been used for the determination of 0–1.5 μg fluoride/ml in sea water and other natural waters. Photometric measurement is made on the blue complex formed by reaction with the chelate formed between lanthanum and alizarin fluorine blue, The method has a coefficient of variation of ca. 0.9% at a fluoride level of 1.5 μm/ml.     

Spectrophotometric determination of zirconium with alizarin red S in the presence of polyvinylpyrrolidone

The absorbance of the microcolloidal zirconium/alizarin red S/polyvinylpyrrolidone complex is measured at 525 nm in acetate buffered medium at pH 4.75. The molar absorptivity is 3.8 × 10⁴ l mol^?1 cm^?1, which is much greater than that of the classical method. Sulphate and fluoride do not interfere.     

Flow-injection spectrophotometric determination of fluoride based on alizarin fluorine blue in the presence of sodium dodecyl sulphate

The stopped-flow reagent-injection method proposed for the spectrophotometric determination of fluoride with lanthanum (III)/alizarin fluorine blue in the presence of sodium dodecyl sulphate at pH 4.6 (λ_max=574 nm) provides a linear calibration graph for 0.08–1.2 mg l^?1 fluoride. The relative standard deviation (n=10) was 0.2% at 0.60 mg l^?1 fluoride. The sampling rate was 60 h^?1. The method is applied to sea and bottled mineral waters with satisfactory results.     

Die bestimmung von alizarin s nach der anreicherung am stationären quecksilbertropfen und ihre anwendung zur fluoridanalyse

Traces of alizarin S can be concentrated on the stationary mercury electrode. The lower limit for the production of d.c. voltammograms is 5·10^-9M. The voltammetric spectrum of the dyestuff was examined by means of d.c. and a.c. polarographic techniques. An indirect voltammetric method for the determination of fluoride in the range 5·10^-7–5·10^-6M is suggested.     

Indirect determination of fluoride in waters with lanthanum alizarin complexone and inductively-coupled plasma emission spectrometry

Fluoride is determined indirectly by measurement of the La II 333.75-nm line in the lanthanum/alizarin complexone/fluoride complex. The ternary complex is extracted into hexanol containing N,N-diethylaniline and the extract is introduced directly into the plasma. Related to water samples, the detection limit (3σ, concentration factor 5) is 0.59 ng ml^?1 fluoride, calibration is linear up to 1.2 μg ml^?1 and the relative standard deviation for 0.04 μg ml^?1 is 2.6%. Alkali, alkali elements and most anions do not interfere. The method is applied in the analysis of river water, coastal seawater and drinking water.     

Determination of Fluoride in Water by Reversed-Phase High-Performance Liquid Chromatography using F−-La3+-Alizarin Complexone Ternary Complex

A method for the determination of fluoride by reversed-phase, high-performance liquid chromatography (RP-HPLC) is described. Fluoride, La³⁺ and alizarin complexone form F-La³⁺-alizarin complexone ternary complex, which is separated from the matrix on a RP, Ultrasphere C₁₈ column (250 × 4.6 mm, 5 μm) using methanol-water (19:81, v/v) mobile phase at 1.00 mL min^?1; detection at 568 nm. The calibration graph was linear from 1.0–150 ng mL^?1 for fluoride with a correlation coefficient: 0.9993 (n=6). The detection limit was 0.2 ng mL^?1. The method was successfully applied to the determination of fluoride in river and tap water. Recovery was: 94–102%, RSD in the range: 1.9 –3.6%.     

Liquid membrane transportation of fluoride ions with alizarin based azacrown ether Zr-complex

A new alizarin based azacrown ether N-(alizarin-4-methylene)-4-azadibenzo-18-crown-6 (AMADCE) was synthesized, for the transportation of fluoride ions, by reacting 4-aza dibenzo 18-crown-6 with alizarin in the presence of formaldehyde. The compound forms a stable purple-red coloured complex with Zr(IV) in 0.5-1.0 M hydrochloric acid and gets quantitatively extracted into diphenyl ether. This diphenyl ether extract of the Zr(IV) complex instantaneously transfers fluoride ions from the aqueous phase, which was utilised for the sensitive determination and transportation of fluoride ions through the liquid membrane. The conditions like concentration of membrane phase, acidity of the source phase and the receiving phase, and the transportation time were optimized. The continuous transportation of fluoride ions was achieved by adding receptor ions like La³⁺ and Ca²⁺ in the receiving phase. The rate constant K and t_1/2 for the transportation were determined. The studies were extended for the removal of fluoride ions through the liquid membrane from the ground water samples and industrial effluent.     

The determination of trace amounts of zirconium,hafnium, thorium and cerium in silicate rocks

A method is described for the determination of traces of zirconium, hafnium, cerium and thorium in rocks. After the sample has been opened up, these elements are separated from the major component elements by extraction from 10 N nitric acid with a 40% solution of tri-n-butyl phosphate, cerium being oxidised with bro-mate. After back-extraction the elements are separated from each other and from other extracted elements by cation exchange. Zirconium is determined photometrically with quinalizarin sulphonic acid which gives about twice the sensitivity of alizarin red S. Thorium is determined photometrically with thorin, and cerium by utilizing its bleaching action on iron(II) phenanthroline. Hf is determined spectro-graphically.     

茜素红S-硼酸体系对单糖的双光谱识别

利用硼酸与茜素红S和糖中的邻二羟基可逆结合的特点,以硼酸为中介运用竞争结合作用机理构建单糖分析法.在pH7.4的KH2PO4-NaOH缓冲溶液中,茜素红S作为指示剂与硼酸结合生成ARS-BA配合物,其结合常数为5.09×102L/mol.糖与指示剂ARS竞争结合硼酸使指示剂游离出来,产生明显的颜色变化,据此建立糖的识别方法.考察了D-葡萄糖、D-山梨醇、D-半乳糖、D-甘露糖、D-果糖、D-阿拉伯糖和L-阿拉伯糖对上述ARS-BA体系光谱的影响.结果显示:该体系对D-山梨醇和D-果糖有较好的光谱响应,其光谱变化灵敏度依D-山梨醇＞D-果糖＞D-阿拉伯糖～D-半乳糖＞D-葡萄糖＞D-甘露糖＞L-阿拉伯糖之序.     

Use of alizarin red S as a chromogenic agent for the colorimetric determination of dothiepin hydrochloride in pharmaceutical formulations

The present study describes two simple, rapid, selective and cost-effective spectrophotometric methods for the determination of dothiepin hydrochloride (DOTH), an antidepressant drug, in bulk drug and pharmaceutical formulations. The first method (method A) is based on the formation of yellow colored ion-pair complex between DOTH and alizarin red S (ARS) in acid medium which was extracted into dichloromethane and the absorbance was measured at 445 nm. The second method (method B) is based on the breaking of the yellow DOTH–ARS ion-pair complex in alkaline medium followed by the measurement of the violet color free dye at 570 nm. Under the optimized conditions, Beer’s law is obeyed over the concentration ranges of 2.50–55.0 and 1.00–35.0 μg ml⁻¹ DOTH for method A and method B, respectively. The molar absorptivity, Sandell’s sensitivity, detection and quantification limits are also calculated. The methods were validated for intra-day and inter-day accuracy and precision; selectivity and robustness and ruggedness. The proposed methods were applied successfully to the determination of DOTH in pure drug and commercial formulations. The accuracy and reliability of the proposed methods were further established by parallel determination by the official method and also by recovery studies via standard addition technique.     

Adsorption voltammetry of the zirconium-alizarin red S complex at a multi-walled carbon nanotubes modified carbon paste electrode

We used a carbon paste electrode modified with multi-walled carbon nanotubes as a working electrode and studied the electrochemical behavior of zirconium-alizarin red S complex on it. It was found that the modified electrode exhibited a significant catalytic effect toward the reduction of free alizarin red S and the complex. The second derivative linear scan voltammograms of the complex were recorded by a polarographic analyser from 0 to −1000 mV (vs. SCE), and it was found that the complex can be adsorbed on the surface of the modified electrode, yielding a peak at about −470 mV, corresponding to the reduction of alizarin red S in the complex. The linear range was found to be 2.0 × 10⁻¹¹–8.0 × 10⁻⁷ mol L⁻¹, and the detection limit was 1.0 × 10⁻¹¹ mol L⁻¹ (S/N = 3) for 3 min accumulation. The procedure was successfully applied to the determination of trace amounts of zirconium in the ore samples. Correspondence: Pei-Hong Deng, Department of Chemistry and Material Science, Hengyang Normal University, Hengyang Hunan 421008, P.R. China     

Polarographic determination of fluoride using the adsorption wave of the Ce(III)-alizarin complexone-fluoride complex

A very sensitive electrochemical method for trace measurement of fluoride in water is discussed. The complex of cerium(III) with alizarin complexone (ALC) and fluoride ion is adsorbed at the dropping mercury electrode. In cathodic sweeps, the peak height is directly proportional to the concentration of fluoride over the range 8 x 10(-8)-5 x 10(-6)M (1.5 x 10(-9)-9.5 x 10(-8) g/ml), and the detection limit is 5 x 10(-8)M (9.5 x 10(-10) g/ml). The proposed method was applied to the determination of fluoride in water.     

Molecular recognition by a novel boronate-containing CTG derivative for hydroxyanthraquinones

C₃-functionalized cyclotriguaiacylene (CTG) derivatives were employed in the development of highly selective recognition compounds due to their unique molecular structures. Here, a novel C₃-functionalized CTG containing boronate (PPB-CTG) was synthesized and its molecular recognition ability for hydroxyanthraquinones was investigated by fluorescence spectroscopy. The addition of the synthesized PPB-CTG led to a large increase in the fluorescence intensity of only alizarin and not 1-hydroxyanthraquinone, 2-hydroxyanthraquinone nor quinizarin. It was, thus, suggested that the cyclotriveratrylene (CTV) structure plays an important role in the recognition ability toward alizarin since the mono-phenyl boronate compound (m-TPBAP) showed poor fluorescence properties toward alizarin. Moreover, it was found that the 1:1 mixture of PPB-CTG and alizarin was effective as a fluorescence-enhanced probe toward fluoride ions.     

Spectrophotometric study of a ternary zirconium/fluoride/alizarin complex with application to the determination of zirconium

A ternary zirconium/fluoride/alizarin complex is extracted into methyl isobutyl ketone. The apparent molar absorptivity at 556 nm is 1.52 × 10⁵ 1 mol^?1 cm^?1. The r.s.d. is 1.3% for 10 μg Zr (n = 12). There are several interferences, some of which can be masked with EDTA.     

Spectrophotometric determination of fluoride with lanthanum/alizarin complexone by flow injection analysis

Lanthanum/alizarin complexone (1:1) in 70% acetone is used in conjunction with a 500-cm reaction coil at 60°C to determine 0.03–1.2 mg l^?1 fluoride at 24 samples per h. The method is applied to tap-water samples.     

An improved method for the spectrophotometric determination of fluoride by addition of sodium dodecyl sulphate to the fluoride/lanthanum (III)/Alizarin fluorine blue system

The conventional spectrophotometric method for the determination of fluoride, based on the fluoride/lanthanum(III)/alizarin fluorine blue ternary complex, is improved by addition of sodium dodecyl sulphate. In 15% (v/v) acetone medium, the absorbance of the binary reagent complex is decreased and the reaction time is only 3 min under sonication. Beer's Law is obeyed at 574 nm for fluoride concentrations in the ranges 0.075–0.30 and 0.20–1.2 mg 1^?1; the apparent molar absorptivities are (1.6 ± 0.1) × 10⁴ and (1.5 ± 0.1) × 10⁴ mol^?1 cm^?1 fluoride levels, respectively. This method is applied to the determination of fluoride in bottled mineral waters.     

Gas diffusion with preconcentration for the determination of fluoride in water samples by flow injection

The preconcentration of fluoride is achieved on-line by converting it to trimethylsilane which then diffuses through a gas permeable membrane to be absorbed in a stationary sodium hydroxide acceptor stream. This stream is enclosed in the sample loop of an injection valve and after preconcentration, the fluoride sample is flushed into a flow injection manifold for spectrophotometric analysis by the zirconium/alizarin S procedure at 520 nm. The method is suitable for fluoride analysis in the range 0.1-10 mg/l at a sampling rate of 17/hr. Phosphate does not interfere and aluminium and iron can be tolerated at 200 and 500 times the fluoride concentration, respectively. The LOD was calculated to be 0.055 mg/l and LOQ was found to be 0.18 mg/l.     

茜素与β-胡萝卜素自由基抗氧化和一氧化氮释放 的研究

在均相体系中利用紫外吸收光谱法,研究了偶氮二异丁睛(AIBN)引发的亚油酸(LH)过氧化反应,发现茜素(Alz)和β-胡萝卜素(β-C)对LH过氧化均有抑制作用,并表现出协同效应。膨胀计法研究表明Alz和β-C对AIBN引发的苯乙烯自由基聚合有阻滞作用,发现Alz与β-C间存在明显的协同阻、缓聚作用。通过在培养的人脐静脉内皮细胞中的研究表明,Alz可促使内皮细胞释放一氧化氮(NO),其作用比乙酰胆碱(Ach)更为显著。     

Spectrophotometric microdetermination of nefopam, mebevrine and phenylpropanolamine hydrochloride in pharmaceutical formulations using alizarins

Simple and rapid spectrophotometric procedures have been established for quantitation of nefopam hydrochloride (NF) mebevrine hydrochloride (MB) and phenylpropanolamine hydrochloride (PP). The procedures are based on the reaction between the examined drugs (NF, MB and PP) and alizarin (I), alizarin red S (II), alizarin yellow G (III) and quinalizarin (IV) producing ion-pair complexes which can be measured at the optimum wavelength. The optimization of the reaction conditions is investigated. Beer's law is obeyed in the concentration ranges 0.5-30.0 microg ml(-1). The molar absorptivity, Sandell sensitivity, detection and quantification limits are also calculated. The correlation coefficient was > or =0.9988 (n=6) with a relative standard deviation (R.S.D.) of < or =1.3, for six determinations of 20 microg ml(-1). The methods are successfully applied to the determination of NF, MB and PP in their pharmaceutical formulations.