Sensitized spectrophotometric determination of Cr(III) ion for speciation of chromium ion in surfactant media using alpha-benzoin oxime

A simple and accurate micellanized spectrophotometric method for determination of trace amounts of Cr(III) ion in tab and top water and a synthetic mixture has been described. The micellar method is based on effect of organized molecular assemblies such as micelles in spectrophotometric measurement due to their effect on the systems of interest. The ability of micellar system in solubilizing of sparingly soluble ligand or complexes has been used for increasing figures of merit of an analytical method. Due to solubility increasing in aqueous media requirement for a primary extraction can be eliminated. Using the alpha-benzoin oxime (alpha-BO) spectrophotometric determination of Cr(III) ion has been performed and results are compared. The spectrophotometric determination of Cr(III) ion using alpha-BO in the presence of non-ionic surfactant Triton X-100 has been performed. The influence of type and amount of surfactant, pH, complexation time and amount of ligand were examined. Finally, the repeatability, accuracy and the effect of interfering ions on the determination of Cr(III) ion was evaluated. The proposed methods successfully with recovery yield of almost 100% have been applied to the rapid and simple determination of Cr(III) ion in the real samples. There is a good agreement between methods and atomic absorption spectrometry. The Beers law is obeyed over the concentration range of 0.1-13.7 microg mL(-1) for micellar media. The detection limit is 0.8 ng mL(-1). The molar absorptivity of complex is 5350 L mol(-1) cm(-1).     

镉试剂与银显色反应体系中乙醇的超分子作用及其应用

金属离子、有机溶剂与偶氮类试剂之间存在一定的超分子作用,有机溶剂及缓冲介质的浓度对显色反应的灵敏度有很大的影响。据此建立了乙醇存在下的镉试剂与银的显色反应新体系。在pH9.5的硼砂-NaOH缓冲介质中,表面活性剂吐温-80的存在下,镉试剂与银反应生成2:1稳定配合物。络合物的λmax=518nm,摩尔吸光系数7.01×104L.mol-1.cm-1,银质量浓度0～1.0μg/mL范围内符合比尔定律。方法用于环境水样中银的测定,取得满意效果。     

Solid phase extraction and spectrophotometric determination of trace amounts of thiocyanate in real samples

A simple, selective and rapid method for solid phase extraction and spectrophotometric determination of thiocyanate using a manganese (III) tetrakis (p-sulfonatophenyl) porphyrin, [Mn (TPPS) OAC] bound to Amberlite IR-400 has been developed. The influence of pH, amount of solid phase, sample matrix, type and amount of eluting agent and flow rates i.e. variables affecting the efficiency of the extraction system were evaluated and conditions of the sample, eluting solution and active phase were optimized. The maximal capacity was found to be as 1.16 microg mL(-1) for 1200 mL. Thiocyanate ions can be eluted quantitatively with 8 mL 0.3 M ferric chloride. The enrichment factor was 150. The linear range of the determination is between 0.4-2.0 microg mL(-1) for preconcentration method with a limit of detection of 2.8 ng mL(-1). The method has been successfully applied for determination of trace amounts of thiocyanate in tap water, saliva sample and a synthetic mixture.     

Catalytic determination of traces of silver(I) using the oxidation of Janus Green with peroxodisulfate.

A method for sensitive and selective determination of silver based on the catalytic effect of silver(I) ion on the oxidation of Janus Green by peroxodisulfate is described. o-Phenanthroline is used as an activator. The rate of the decrease in absorbance of Janus Green (at 615 nm) is proportional to the concentration of silver in the range of 0.3-4.0 ng mL(-1) and 4.0-500.0 ng mL(-1). The theoretical limit of detection was 0.25 ng mL(-1). The method is free from most interferences. The method was applied to the determination of silver in plants (the uptake of silver by plants), in photographic solutions, lake water and several synthetic samples.     

Studies and application of catalytic kinetic spectrophotometric determination of trace chromium(VI) sensitized by microemulsion medium

A new catalytic kinetic spectrophotometric method for the determination of trace amount of chromium (VI) in microemulsion medium has been developed. The method is based on the catalytic effect of chromium (VI) on the oxidation of nuclear fast red in the presence of Tween-80 microemulsion and HAc-NaAc buffer solution (pH = 5.2). The linear ranges are in the range of 0 approximately 0.0480 microg mL(-1) of Cr (VI) at 528 nm and the detection limit is 1.56x10(-9)g mL(-1). The method has been applied in determination of Cr (VI) in water and food samples with satisfactory results. The relative standard deviation is less than 4.6 % and the recovery is 93.5 approximately 104 %.     

增效试剂在动力学分析法中的应用研究Ⅱ: 锰(Ⅱ)-氨三乙酸-十二烷基硫酸钠-高碘酸钾-罗丹明B催化体系

基于存在活化剂氨三乙酸和增敏剂十二烷基硫酸钠, 锰(Ⅱ)催化高碘酸钾氧化罗丹明B的反应, 拟定了测定痕量锰的新催化光度法。讨论了有关的反应机理。本法由于添加了表面活性剂, 灵敏度提高3.4倍。测定锰含量线性范围为10-120ng·25mL^-^1, 相对标准偏差为2.6%(n=9), 检出限为8.0×10^-^1^1g·mL^-^1。用于测定水样和酒样中锰。     

Silver-enhanced reduction of 2,3,5-triphenyl-2H-tetrazolium by semicarbazide for the spectrophotometric determination of traces of silver(I).

A sensitive spectrophotometric method for the determination of silver is described. The reaction involves a silver-enhanced reduction of 2,3,5-triphenyl-2H-tetrazolium chloride by semicarbazide hydrochloride to yield a pink-colored product with maximum absorption at 510 nm. Beer's law is obeyed in the concentration range of 0.02-0.34 microg cm(-3) of silver, and the molar absorptivity is 4.51 x 10(5) l mol(-1) cm(-1). The optical parameters, optimum reaction conditions and interference studies have been described. The method has been applied to the determination of silver in photographic film waste water and in synthetic samples.     

Derivative spectrophotometry in the determination of phenyl-beta-naphthylamine used as an antioxidant in rubber mixtures

A method for the determination of phenyl-beta-naphthylamine (PBN) in ternary mixtures by second-derivative spectrophotometry is described. The procedure works without any separation step of PBN from the other polymer additives. By applying the second-derivative spectrophotometry, Beer's law was valid over the range 0.25-10 micro g mL(-1). The proposed method has been applied to the determination PBN in synthetic ternary mixtures and rubber samples. A comparative study of the results obtained using the second and the third-derivative spectrophotometric methods is presented and evaluated. The derivative spectrophotometric method indicated that the amount of PBN found after extraction from the rubber samples was 0.97+/-0.02 g/100 g of sample.     

meso-四(4-磺酸基苯基)卟啉与银(Ⅰ)高灵敏显色反应的研究与应用

本文提出以meso-四(4-磺酸基苯基)卟啉(TPPS_4)为显色剂和CTMAB、β-CD为辅助配合剂,在酸性条件下灵敏度最高的测定痕量银的分光光度新体系。实验发现在此显色反应进行完全后,以适量H_2SO_4溶液(2+3)酸化,将过量的显色剂转化为质子化H_4P~(2+)形体,其最大吸收波长红移,而配合物稳定且最大吸收峰不变,增大了对比度(Δλ=66nm);同时提高了方法的灵敏度和选择性,表观摩尔吸光系数ε=5.21×10~5L/mol·cm。应用本法于相纸、定影废液和矿石等试样中银的测定,与AAS法结果一致。     

Highly selective and sensitized spectrophotometric determination of iron (III) following potentiometric study

A simple, selective and sensitized spectrophotometric method for determination of trace amounts of Fe3+ ion in tap and waste water solutions has been described. The spectrophotometric determination of Fe3+ ion using Ferron in the presence of N,N-Dodecytrimethylammonium bromide (DTAB) has been carried out. The Beer's law is obeyed over the concentration range of 0.05-2.6 microg mL(-1) of Fe3+ ion with the relative standard deviation (RSD %) <0.2% and the molar absorptivity of complexes in pH 3.5 is 3.8 x 10(3) L mol(-1) cm(-1). Potentiometric pH titration has been used for prediction of protonation constants of ferron, and evaluating its stoichiometry and respective stability constant with Fe3+ ion. As it is obvious the most likely species of ferron alone and its complexes are LH (log = 7.64), LH2 (logK = 10.52), LH3 (logK = 11.74) and ML2 (logbeta = 23.68), ML3 (logbeta = 23.68), ML3H (logbeta = 23.68), ML3H2 (logbta = 23.68) and ML(OH)2 (logbeta = 23.68) respectively.     

Kinetic spectrophotometric determination of famotidine in commercial dosage forms.

A simple kinetic spectrophotometric method is described for the determination of famotidine. The method is based on the oxidation of the drug with alkaline potassium permanganate. The reaction is followed spectrometrically by measuring the rate of change of the absorbance at 610 nm. The initial-rate and fixed-time (at 12 min) methods are adopted for determining the drug concentration. The calibration graphs are linear in the ranges of 2-10 microg mL(-1) and 1-8 microg mL(-1) using the initial-rate and fixed-time methods, respectively. The method has been applied to the determination of famotidine in tablet formulations. The obtained results are compared statistically with those given by a reference spectrophotometric method.     

KBrO3氧化甲基紫褪色动力学光度法测定食品中痕量钒

基于0.004 mol/L的柠檬酸介质中,痕量V(Ⅴ)催化KBrO3氧化甲基紫的褪色反应,建立了测定痕量V(Ⅴ)的动力学光度法。方法的检出限为1.23μg/L,线性范围为0～0.16μg/mL。讨论了酸度、反应物浓度、温度、反应时间、干扰离子等因素的影响,确定了该体系反应的最佳条件。在25 mL溶液中,测定2.0μg V(Ⅴ)的RSD为1.9%(n=11)。方法可用于测定小麦和苹果中的痕量V(Ⅴ),RSD为1.1%～2.7%,标准加入回收率为97.6%～99.0%。     

Spectrophotometric determination of formaldehyde

A new spectrophotometric method for the determination of micro amounts of formaldehyde in aqueous and methanol solutions is based on the oxidation of formaldehyde by hydrous silver oxide at pH 11-12.5 and oxidation of the metallic silver produced, with iron(III) in the presence of Ferrozine. The absorbance of the resulting iron(II)-Ferrozine complex at 562 nm is proportional to the amount of formaldehyde and corresponds to an apparent molar absorptivity of 5.58 x 10(4) 1.mole(-1).cm(-1).     

过硫酸钾氧化偶氮荧光桃红催化光度法测定痕量银

以过硫酸盐氧化偶氮类试剂催化动力学法测定银,多数线性范围较窄、选择性欠佳。本文建立了以偶氮荧光桃红作指示物质、α,α′-联吡啶作活化剂的催化光度法,测定痕量银检出限为1.0×10^-4μg/mL,线性范围2.0×10^-4～4.0×10^-2μg/mL,灵敏度高,选择性好。用于测定鄂铜矿中银,结果满意。采用自装的微机动力学数据处理系统,测试简便、准确。     

Kinetic spectrophotometric determination of traces of sulfide in nonionic micellar medium

A sensitive kinetic spectrophotometric method for the determination of ng amounts of sulfide has been developed based on the reduction of Azure A by sulfide in the presence of Brij-35 at pH 7. The decrease in absorbance of Azure A at 600 nm is proportional to the concentration of sulfide over the range 25-1,400 ng mL(-1). The variables affecting the rate of the reaction were investigated and the optimum conditions were established. The method is simple, rapid, precise, sensitive, and widely applicable. The limit of detection is 17 ng mL(-1), and the relative standard deviation of seven determinations of 500 ng mL(-1) sulfide was 2.1%. The method was applied to the determination of sulfide in spring water.     

Spectrophotometric determination of silver with 2-(2-quinolylazo)-5-diethylaminophenol as chromogenic reagent

A new chromogenic reagent, 2-(2-quinolylazo)-5-diethylaminophenol (QADEAP) was synthesized. A highly sensitive, selective and rapid method for the determination of silver based on the rapid reaction of silver(I) with QADEAP has been developed. In the presence of citric acid-sodium hydroxide buffer solution (pH=5.0) and sodium dodecyl sulfonate (SDS) medium, QADEAP reacts with silver to form a violet complex of a molar ratio 1:2 (silver to QADEAP). The molar absorptivity of the complex is 1.33x10(5) L mol(-1) cm(-1)at 590 nm. Beer' s law is obeyed in the range of 0.01-0.6 micro g mL(-1). The relative standard deviations for eleven replicate samples of 0.2 microg mL(-1) is 1.38%. This method was applied to the determination of silver in water with satisfactory results.     

Spectrophotometric determination of silver with cadion 2B and triton X-100

A highly sensitive and selective procedure for spectrophotometric determination of silver has been developed. At pH 9.2, in the presence of Triton X-100, silver forms a dark red-violet complex with cadion 2B which has an absorption maximum at 565 nm. The molar absorptivity is 1.0 x 10(5) l.mole(-1).cm(-1). Beer's law is obeyed for silver in the range 0.02-0.8 mug ml . The colour reaction, if EDTA is used as a masking agent, is free from interference by the 20 cations and 19 anions investigated. Only Cl(-), Br(-), I(-), S(2-) and CN(-) interfere and must be absent. This method has been used to determine silver in waste-water.     

Analysis of Thiabendazole Via its Metal Complexes

Abstract

A new spectrophotometric method for the determination of thiabendazole has been developed. The method depends on the reaction of thiabendazole with copper (II), mercury (II) and silver (I) to form 1:1 complexes having maximum absorption at 317 nm, 318 nm and 324 nm, respectively. These absorption bands were used for the spectrophotometric determination of thiabendazole in pure form, in raw material and in pharmaceutical formulations.     

Kinetic-spectrophotometric determination of trace amounts of silver using the oxidation of thionine with peroxodisulfate.

A simple, rapid and sensitive method has been developed for determination of traces of silver(I) (0.2 - 13 ng mL(-1)) based on its catalytic effect on the oxidation of thionine by peroxodisulfate in the presence of 1 - 10 phenanthroline as an activator. The reaction is monitored spectrophotometrically by measuring the decrease in absorbance of thionine at 600 nm by the fixed time method. The detection limit is 0.098 ng mL(-1) and the relative standard deviation for 0.5, 3.0, 5.0 and 10 ng ml(-1) Ag(I) are 4.1, 1.37, 1.06 and 0.64%, respectively. The method is free from most interferences and it was applied to determination of silver in photographic solutions and well-water samples.     

阳离子表面活性剂增敏催化光度法测定痕量铬(Ⅵ)

基于存在增敏剂十六烷基三甲基溴化铵,铬（Ⅵ）催化过氧化氢氧化胭脂红酸的反应,拟定了测定痕量铬（Ⅵ）的新催化光度法。本法由于添加了十六烷基三甲基溴化铵,灵敏度提高３．３倍,测定铬（Ⅵ）含量的线性范围为０．００５～０．１６μｇ／ｍＬ,检出限为１．０×１０－３μｇ／ｍＬ,相对标准偏差为０．５％（ｎ＝９）,可用于测定水样中的铬（Ⅵ）。