Fluorimetric sensor for the determination of fluoride at the nanograms per millilitre level

A rapid, sensitive and selective method is described for the determination of traces of fluoride in real samples based on the integration of retention and fluorescence detection (λ_ex = 335 nm, λ_em 405 nm) of a ternary complex [zirconium(IV)-Calcein Blue-fluoride) using a conventional flow cell packed with an anion-exchange resin. A study of a large number of experimental variables (flow-injection configuration, type of support, eluting carrier, sample pH, etc.) allowed the development of an optimized, highly selective determination of fluoride with an analytical concentration range of 1–40 ng ml^?1 (r.s.d. 1%) with a sampling frequency of 30 h^?1. A critical comparison with a probe sensor using the same chemical system showed the described flow-through sensor to be clearly superior.     

Kinetic photometric determination of copper at the nanograms per millilitre level in real samples

A highly sensitive and selective kinetic method is proposed for the determination of nanogram amounts of copper(II) based on its catalytic effect on the oxidation of 3-hydroxybenzaldehyde azine by potassium peroxydisulphase in an ammoniacal medium. The rate of the reaction is monitored spectrophotometrically at 465 nm and the method allows the determination of copper concentrations in the range 0.5–18 ng ml^?1 with a relative standard deviation of about 2%. The proposed method is virtually specific to copper and has been applied satisfactorily to its determination in a variety of food and industrial samples. A possible mechanism for the catalysed reaction is proposed.     

Selective kinetic spectrophotometric determination of copper at nanograms per milliliter level

A sensitive and selective kinetic method is proposed for the determination of nanogram amounts of copper. The method is based on the catalytic effect of copper on the reduction of Ponceau S by sodium sulfide in an alkaline media. The rate of the reaction is monitored spectrophotometrically at 560 nm. The method allows determination of copper concentrations in the range 2-400 ng ml(-1) with a relative standard deviation of approximately 2%. The proposed method, which is highly selective to copper, has been applied satisfactory to its determination in real samples.     

Extractive spectrophotometric determination of cobalt using Cyanex-272

Cyanex-272 forms a blue-colored complex with Co(II) in the organic phase. The complex shows three absorption maxima. The peak at 635 nm has been used for developing a spectrophotometric procedure for cobalt determination. Beer's law was found to be obeyed in the range 0.295-2.36 mg of cobalt. The nature of the extracted species was found to be CoR(2).HR. The molar absorptivity was found to be 3.07 x 10(2) l. mol(-1). cm(-1) at 635 nm. The method was applied for cobalt determination in solutions obtained from Beta Cake and a super alloy and was found to give values close to the actual ones. Easy regeneration of the reagent (Cyanex-272) for re-use is the main advantage of the present method.     

Selective spectrophotometric determination of TNT using a dicyclohexylamine-based colorimetric sensor

Because of the extremely heterogeneous distribution of explosives in contaminated soils, on-site colorimetric methods are efficient tools to assess the nature and extent of contamination. To meet the need for rapid and low-cost chemical sensing of explosive traces or residues in soil and post-blast debris, a colorimetric absorption-based sensor for trinitrotoluene (TNT) determination has been developed. The charge-transfer (CT) reagent (dicyclohexylamine, DCHA) is entrapped in a polyvinylchloride (PVC) polymer matrix plasticised with dioctylphtalate (DOP), and moulded into a transparent sensor membrane sliced into test strips capable of sensing TNT showing an absorption maximum at 530 nm when placed in a 1-mm spectrophotometer cell. The sensor gave a linear absorption response to 5-50 mg L⁻¹ TNT solutions in 30% aqueous acetone with limit of detection (LOD): 3 mg L⁻¹. The sensor is only affected by tetryl, but not by RDX, pentaerythritoltetranitrate (PETN), dinitrotoluene (DNT), and picric acid. The proposed method was statistically validated for TNT assay against high performance liquid chromatography (HPLC) using a standard sample of Comp B. The developed sensor was relatively resistant to air and water, was of low-cost and high specificity, gave a rapid and reproducible response, and was suitable for field use of TNT determination in both dry and humid soil and groundwater with a portable colorimeter.     

Extraction spectrophotometric determination of cobalt and nickel using ethylthioxanthate

A spectrophotometric method for the determination of cobalt and nickel using a new reagent sodium ethylthioxanthate has been described. The yellow-colored cobalt complex and red-colored nickel complex have been extracted quantitatively using carbon tetrachloride in the pH ranges 4.0–11 and 4.0–6.7, respectively. The colors of these complexes are stable and absorbances have been measured at 389 nm for cobalt and 495 nm for the nickel complexes. Few ions interfere but the method has been applied successfully for the determination of these metal ions in various complex materials.     

Rapid spectrophotometric determination of cobalt after extraction using oximidobenzotetronic acid

A spectrophotometric method based on the extraction of cobalt with benzene solutions of oximidobenzotetronic acid (OBTA) is proposed for the estimation of 0.2-3.0 ppm of cobalt. The 3:1 OBTA : Co complex containing cobalt(III) has its absorption maximum at 430 nm; its molar absorptivity in benzene is 1.82 x 10(3)L. mole(-1). mm(-1). Since the blue iron(II) complex is not extracted into benzene, iron(II) and cobalt(II) can be separated and determined spectrophotometrically.     

Extraction and spectrophotometric determination of cobalt with dithizone

Cobalt(II) in acetate-tartrate buffer (pH 6.0-7.3) is extracted quantitatively as cobalt(III) dithizonate with excess of dithizone in CCl(4). The molar absorptivity in the CCl(4) phase is 4.6 x 10(4) 1.mole(-1).cm(-1) at the absorption maximum 550 nm. The calibration graph is linear for 1-10 mug of cobalt in 10 ml of CCl(4) when excess of dithizone is removed by back-extraction with 0.01M aqueous ammonia. Most interferences can be overcome by (a) initial extraction with dithizone at pH 1.3, (b) selective back-extraction into hydrochloric acid (pH 1 to 2), (c) oxidation of iron and tin to iron(III) and tin(IV) and addition of fluoride to complex the former, and (d) selective reaction of nickel dithizonate with 1,10-phenanthroline in the CCl(4) phase followed by back-extraction of nickel into 0.1M acid. The method has been applied to determination of cobalt in a copper-nickel-zinc alloy and a nimonic alloy.     

亚硝基R盐分光光度法测定合金钢中钴

本文改进了亚硝基R盐分光光度法测定合金钢中钴的分析方法,并详细探讨了该方法中吸收波长、缓冲溶液、氧化剂、消解酸种类、加热时间、共存离子等测定条件对结果准确度和精密度的影响.结合示差光度法,在不需分离铁、铜、镍、铬等干扰元素的条件下,可适用于测定合金钢中高含量钴,相对误差在3%以下,相对标准偏差小于1%.测定高含量钴标准...     

Spectrofluorimetric determination of submicrogram amounts of aluminium using salicylidene-o-aminophenol

Salicylidene-o-aminophenol provides a sensitive spectrofluorimetric reagent for the determination of aluminium down to 27 ng (or 2.7 x 10(-4) ppm in the final solution). The most suitable conditions of pH (5.6), reagent concentration and development time (>20 min) have been established. Extraction with sodium diethyldithiocarbamate into ethyl acetate at the pH of the determination renders the method highly selective; out of 46 foreign cations examined only chromium(III), scandium and thorium interfere. Anions which form complexes with aluminium, such as citrate, tartrate and fluoride, also cause interference, but none of the common anions interferes. A 1:1 stoichiometry of the complex has been established and some conclusions have been drawn concerning its nature.     

Rapid spectrophotometric determination of cobalt with 2,2'-dipyridyl ketoxime

A rapid spectrophotometric method for the determination of low levels of cobalt(III) with 2,2 -dipyridyl ketoxime is proposed. A 3:1 water-soluble complex which is easily extractable into chloroform and has an absorption maximum at 388 mmicro forms instantaneously. Beer's law is obeyed and the molar absorptivity is 19.5 x 10(3). An investigation of the interference of 60 cations and anions shows the method to be widely applicable; it is simple, convenient and reproducible.     

Detection and spectrophotometric determination of cobalt with dimedone dioxime

Dimedone dioxime forms coloured complexes only with cobalt, nickel and copper ions in alkaline solution. Acidification and solvent extraction enables cobalt (1-50 mug) to be determined spectrophotometrically without interference. A specific spot test for cobalt is based on the same reaction.