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.     

Kinetic-Spectrophotometric Determination of Tellurium (IV) by Its Catalytic Effect on the Reduction of Thionine by Sodium Sulfide in Cationic Micellar Medium

A simple and highly sensitive method is proposed for the determination of Te(IV) by its catalytic effect on the reduction of thionine by sodium sulfide in the presence of cetyl trimethyl ammonium bromide as a micelle media. The reaction was monitored spectrophotometrically by measuring the decrease in absorbance of thionine at 600 nm with a fixed time of 0.5-2.5 min from initiation of the reaction. Tellurium can be measured in the concentration range of 0.6-500.0 ng/mL, with a limit of detection of 0.3 ng/mL Te(IV). The influence of more than thirty potential interfering ions was studied on the determination of tellurium. The relative standard deviation for ten replicate measurements of 0.020 and 50.0 ng/mL Te(IV) was 2.1 and 1.9%, respectively. The method was applied for the determination of tellurium in synthetic samples.     

Determination of proteins at nanogram levels by their quenching effect on large particle scattering of colloidal silver chloride

A novel quantitative method for the determination of proteins in aqueous solutions has been based on the quenching of the resonance scattering light of colloidal silver chloride in the presence of proteins. The detection limits for eight kinds of proteins (BSA, HSA, egg albumin, human gamma-IgG,alpha-chymotrypsin, E. Coli. alpsase, myoglobin, alpha-casein) were at about 8 ng/mL; the linear ranges of the calibration curves were 10-400 ng/mL under optimal conditions,except for human gamma-IgG (20-400 ng/mL), myoglobin (10-300 ng/mL), and alpha-casein (10-300 ng/mL). Three wavelengths (398 nm, 475 nm, 499 nm) were all suitable for the determination and any acidity from pH 3.0 to pH 9.0 could be chosen. A few non-protein substances at high concentration levels interfered with this method, but this problem could simply be overcome by diluting the samples before the assay. Mechanism studies showed that the quenching effect of proteins on the scattering light of colloidal silver chloride was mainly due to the coagulation of AgCl particles retarded by protein. The method was employed for the determination of total protein in human serum with satisfactory results.     

A simple thermometric technique for reaction-rate determination of inorganic species, based on the iodide-catalysed cerium(IV)-arsenic(III) reaction

A very simple reaction-rate thermometric technique is used for determination of iodide (5-20 ng ml ), based on its catalytic action on the cerium(IV)-arsenic(III) reaction, and for determination of mercury(II) (1.5-10 ng ml ) and silver(I) (2-10 ng ml ), based on their inhibitory effect on this reaction. The reaction is followed by measuring the rate of temperature increase. The method suffers from very few interferences and is applied to determination of iodide in biological and inorganic samples, and Hg(II) and Ag(I) in pharmaceutical products.     

萃取富集-火焰原子吸收光谱法测定食品中痕量银

建立了萃取富集-火焰原子吸收法测定食品中痕量银的新方法.在硫氰酸钾、十六烷基三甲基溴化铵和氯化钠溶液体系中,银离子能被定量萃取到乙酸乙酯中,从而起到富集作用,取乙酸乙酯于火焰原子吸收光谱仪测定其中的银元素含量,提高了测定灵敏度和选择性.结果显示:银在0-200ng/mL内线性良好,r=0.999 3,测定银的灵敏度(特...     

Kinetic Spectrophotometric Determination of Vanadium (V) Based on its Inhibitory Effect on the Thionine – Ascorbic Acid Reaction

ABSTRACT

A simple and sensitive kinetic method for the determination of vanadium(V) based on its inhibitory effect on the reduction of thionine by ascorbic acid at pH=5 is described. The reaction rate is monitored spectrophotometrically by measuring the decrease in absorbance of thionine at 598 nm after a fixed time (10 min). The calibration graph is linear in the range of 10 ? 120 ng ml^?1 of vanadium(V) and the detection limit is 6 ng ml^?1. The relative standard deviation (RSD) for 80 ng ml^?1 of V(V) was 0.96% (n=10). The method was successfully applied to the determination of vanadium in a certified reference sample.     

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.     

Fabrication of a new multi-walled carbon nanotube paste electrode for stripping voltammetric determination of Ag(I)

A new modified carbon paste electrode based on multi-walled carbon nanotubes and a synthesized Schiff base of N,N'-bis(2-hydroxybenzylidene)-2,2'(aminophenylthio) ethane, acting as a chelating agent for Ag(I) ions, is described. The electroanalytical procedure for the determination of Ag(I) was comprised of two steps: the chemical accumulation of the analyte under open-circuit conditions followed by replacing the medium with a 0.1 M HCl solution where the accumulated Ag(I) was reduced for 20 s in -0.7 V. The potential was then scanned from -0.2 to +0.2 V to obtain the voltammetric peak. The effective parameters in the sensor response were examined. Under optimized operational conditions, a linear response range from 0.5-200 ng mL(-1) was obtained. The detection limit for silver determination was 0.092 ng mL(-1). For 7 successive determinations of 15.0 and 60.0 ng mL(-1) of Ag(I), relative standard deviations of 2.2% and 1.2% were obtained, respectively. The procedure was applied in determining Ag(I) in X-ray photographic films and water samples.     

Highly selective and sensitive spectrophotometric determination of trace amounts of silver ion in surfactant media using 2-mercaptobenzoxazole

A simple and accurate spectrophotometric method for determination of trace amounts of silver ion in tap and wastewater solution and photographic solutions has been described. The spectrophotometric determination of silver ion using 2-mercaptobenzoxazole (MBO) in the presence of Triton X-100 as nonionic surfactant has been carried out. The Beer's law is obeyed over the concentration range of 0.1-9.0 microg mL(-1) of Ag+ ion with the detection limits of 1.6 ng mL(-1). The influence of type and amount of surfactant, pH, complexation time and amount of ligand on sensitivity of method were optimized. Finally the repeatability, accuracy and the effect of interfering ions on the determination of silver ion were evaluated. There is a good agreement between results of proposed method and atomic absorption spectrometry.     

Determination of proteins at nanogram levels by their quenching effect on large particle scattering of colloidal silver chloride

A novel quantitative method for the determination of proteins in aqueous solutions has been based on the quenching of the resonance scattering light of colloidal silver chloride in the presence of proteins. The detection limits for eight kinds of proteins (BSA, HSA, egg albumin, human γ-IgG,α-chymotrypsin, E. Coli. alpsase, myoglobin, α-casein) were at about 8 ng/mL; the linear ranges of the calibration curves were 10–400 ng/mL ¶under optimal conditions,except for human γ-IgG (20–¶400 ng/mL), myoglobin (10–300 ng/mL), and α-casein (10–300 ng/mL). Three wavelengths (398 nm, 475 nm, 499 nm) were all suitable for the determination and any acidity from pH 3.0 to pH 9.0 could be chosen. A few non-protein substances at high concentration levels interfered with this method, but this problem could simply be overcome by diluting the samples before the assay. Mechanism studies showed that the quenching effect of proteins on the scattering light of colloidal silver chloride was mainly due to the coagulation of AgCl particles retarded by protein. The method was employed for the determination of total protein in human serum with sactifactory results.     

基于纳米金与碳纳米管-纳米铂-壳聚糖纳米复合物固定癌胚抗原免疫传感器的研究

采用纳米金(nano-Au)、多壁碳纳米管-纳米铂-壳聚糖的纳米复合物(MWNT-Pt-CS)及电子媒介体硫堇(Th)固载抗体制得高灵敏癌胚抗原免疫传感器．首先, 于壳聚糖溶液中用NaBH4还原H2PtCl6, 并将多壁碳纳米管分散于其中制得碳纳米管-纳米铂-壳聚糖纳米复合物, 并将其滴涂在玻碳电极上成膜; 然后, 吸附电子媒介体硫堇制得硫堇/碳纳米管-纳米铂-壳聚糖(Th/MWNT-Pt-CS)修饰电极．利用壳聚糖和硫堇分子中大量的氨基固定纳米金并吸附癌胚抗体(anti-CEA); 最后, 用辣根过氧化物酶(HRP)封闭活性位点从而制得高灵敏电流型免疫传感器．在优化的实验条件下, 该传感器响应的峰电流值与癌胚抗原(carcinoembryonic antigen)浓度在0.5～10和10～120 ng/mL的范围内保持良好的线性关系, 检测限为0.2 ng/mL．     

Separation of trace amount of silver using dispersive liquid-liquid based on solidification of floating organic drop microextraction

In the present work, dispersive liquid-liquid microextraction based on solidification of floating organic drop was developed as a simple and rapid technique for separation of silver ions from aqueous samples. In this technique, 700 μL 0.02% of 5-(4'-dimethylamino benzyliden)-rhodanine (chelating agent) was added into the 10 mL analyte sample in a test tube and 30.0 μL 1-undecanol (extraction solvent) was injected shortly thereafter. The test tubes were sonicated, centrifuged and then some effective parameters on extraction and complex formation, such as type and volume of extraction and disperser solvent, pH, the amount of chelating agent and extraction time were optimized. The effect of the interfering ions on the analytes recovery was also investigated. The calibration graph was linear in the range of 0.10-10.0 ng mL(-1) with detection limit of 0.056 ng mL(-1) (n=8). The relative standard deviation (RSD) was ±4.3% (n=8, C=5.0 ng mL(-1)) and the enrichment factor was 250.0. The proposed method was applied for extraction and determination of silver in different water samples.     

Katalytische bestimmung von silberspuren in wabetariger lösung und nach extraktion

The application of the catalysed oxidation of Bromopyrogallol Red by potassium per- sulphate for silver determination is discussed. In aqueous solution silver concentrations of 0.5- 1 mug/ml can be determined and 1- 13 ng/ml in the presence of 1, 10-phenanthroline as activator. In combination with solvent extraction, catalytic determination of the extracted silver is possible even in presence of 200 mug of iron(III), cobalt(II) and palladium(II). By means of an automatic variant of the simultaneous comparison method a more sensitive determination (0.2-20 ng/ml) was achieved.     

Nucleic acids determination using the complex of eriochrome black T and silver nanoparticles in a resonance light scattering technique

A novel method for the determination of nucleic acids by using silver nanoparticle (AgNPs)-eriochrome black T (EBT) as a resonance light scattering (RLS) probe has been developed. Under optimum conditions, there are linear relationships between the quenching extent of RLS intensity and the concentration of nucleic acids in the range of 4.0×10(-9)-4.0×10(-7), 4.0×10(-7)-1.6×10(-6) g mL(-1) for fish sperm DNA (fsDNA) and 4.0×10(-8)-2.0×10(-6) g mL(-1) for yeast RNA (yRNA). Their detection limits (S/N=3) are 2.0 ng mL(-1) and 21 ng mL(-1), respectively. The results indicate that AgNPs can form wirelike aggregates and nanoslices in the presence of the EBT. Whereas, when nucleic acids are added into the AgNPs-EBT system, the dynamic balance of AgNPs-EBT system is destroyed and the nanoparticles undergo dispersion again, leading to the RLS intensity of AgNPs-EBT system quenching. Meanwhile, the conformation of fsDNA is changed by the synergistic effect of AgNPs and EBT.     

On-line separation and preconcentration of silver ion on amidino-thiourea immobilized glass beads packing in flow injection analysis with atomic absorption spectrometric detection.

Amidino-thiourea immobilized glass beads (AGB I) were prepared and used as the microcolumn packing for the flow injection (FI) on-line separation and preconcentration of Ag(I) coupled with atomic absorption spectrometry (AAS) determination. Base metal ions and anions with a concentration of 2.0 mg mL(-1) had no interference with the determination of Ag(I). The limit of detection (LOD) of Ag(I) for a preconcentration time of 60 s with a sampling flow rate of 5.0 mL min(-1) for 40.0 ng mL(-1) of Ag(I) were 0.50 ng mL(-1) with the peak-height absorbance mode and 1.26 ng mL(-1) with the peak-area absorbance mode, respectively. The relative standard deviations (RSD) of 7 replicate determinations were 0.9% and 0.7% for the peak-height absorbance (H) and the peak-area absorbance (A), respectively. The method was successfully applied to the determination of Ag(I) in ore samples.     

Determination of Utratrace Silver Using Surfactant As Sensitizer by Catalytic Near Field Laser Thermal Lens Spectrometry

Thermal lens spectrometry (TLS) is an excellent tool for trace analysis1. TLS allows the detection of absorbances of 10-7～10-8, concentration of ≈ 10-11 mol稬-1 and the analysis of 10-15 L volumes with ≈10-2 absorbing molecules2. Kinetic analysis is playing an increasingly important part in modern analytical chemistry. Therefore, TLS shows much promise in combination with kinetic analysis. However, there are few data on TLS applications in kinetic analysis method so far3～4. A ne…     

Kinetic spectrofluorimetric determination of silver, based on its catalytic effect on the oxidation of pyrocatechol-1-aldehyde 2-pyridylhydrazone by peroxodisulphate in the presence of 1,10-phenanthroline as activator

A kinetic fluorimetric method for the determination of silver is described, based on its catalytic effect on the oxidation of pyrocatechol-1-aldehyde 2-pyridylhydrazone by peroxodisulphate. In aqueous solution silver concentrations of 0.2-0.8 mug ml can be determined, and 10-80 ng ml in the presence of 1,10-phenanthroline as activator. The fluorescent species obtained (lambda(ex) 357 nm, lambda(em) 445 nm) results from oxidation of the reagent. The kinetic parameters and the interferences are reported, and the method is applied to the determination of silver in developed panchromatic plates.     

Flow injection spectrophotometric determination of trace amounts of selenium

A simple, rapid and sensitive flow injection spectrophotometric method for determination of selenium (0.005-1.5 mug ml(-1)) is described. The method is based on the catalytic effect of Se(IV) on the reduction reaction of thionine (TN) with sulphide ion, monitored spectrophotometrically at 598 nm. The detection limit is 5 ng ml(-1) the relative standard deviation for eight replicate measurements is 1.1% for 1 mug ml(-1) of selenium. The sampling rate is 25-30 samples h(-1). The procedure was applied successfully to the determination of selenium in real samples.     

Kinetic-Spectrophotometric Determination of Molybdenum(VI) Based on Its Catalytic Effect on the Thionine-Hydrazine Reaction

Abstract

A kinetic method for the determination of trace amounts of Mo(VI) (0.05-4 μg ml^?1) based on its catalytic effect on the reduction of thionine by hydrazine monochloride in strongly acidic media is reported. The reaction is monitored spectrophotometrically by measuring the decrease in absorbance of thionine at 605 nm after a fixed time (5 min.). The detection limit of the method is 23 ng ml^?1 and the relative standard deviation (RSD) for 0.05 μg ml^?1 of Mo(VI) is 1.2% (n=7). The method is almost free from interferences, especially from large amounts of tungsten. The procedure was successfully applied to the determination of trace amounts of molybdenum in steel.     

Study on the Color Reaction of Silver with 2‐(2‐Quinolylazo)‐5‐Dimethylaminoaniline and its Application

A new chromogenic reagent, 2‐(2‐quinolylazo)‐5‐dimethylaminoaniline (QADMAA) was synthesized. A highly sensitive, selective and rapid method for the determination of silver based on the rapid reaction of silver(I) with QADMAA was developed. In the presence of pH = 6.5 sodium citrate‐sodium hydroxide buffer solution and sodium dodecyl sulfonate (SDS) medium, QADMAA reacts with silver to form a violet complex of a molar ratio 1:2 (silver to QADMAA). The molar absorptivity of the complex is 1.26 × 10⁵ L. mol^?1.cm^?1 at 570 nm. Beer's law is obeyed in the range of 0.01–0.6 μg/mL. The relative standard deviation for eleven replicate samples of 0.2 μg/mL silver is 1.76%. This method was applied to the determination of silver in water with good results.