STUDY ON THE DETERMINATION OF TRACE Fe（III） BY THIN LAYER RESIN PHASE SPECTROPHOTOMETRY

A method to determine Fe（Ⅲ） by thin layer resin phase spectrophotometry has been developed in this paper. The colored complex formed by Fe（Ⅲ） and 1,2-benzendiol is concentrated on the 717^# resin, then Fe（Ⅲ） can be determined directly by making thin layer. The method is sensitive with a apparent molar absorption of 4.8×10^4L/mol.cm, which is 16 times higher than that of liquid phase spectrophotornetry, most coexisting ions do not influence the determination. The detection limit for Fe（Ⅲ） is 1.47μg/L with the precision of 3.3% [n=6, 7μg/50mL Fe（Ⅲ）]. The calibration curve is linear in the range of 0-25μg/50mL. The preposed method was applied to the determination of Fe（Ⅲ） in water sample with satisfactory results.     

STUDY ON THE DETERMINATION OF TRACE BISMUTH(Ⅲ) BY THIN-LAYER RESIN PHASE SPECTROPHOTOMETRY

In this paper, a new thin-layer ion-exchange resin phase analytical method is introduced. It is based on that, the bismuthous cation can associate with iodic anions, so as to formed an anioncomplex [BiI-4] in a strong acidic environments. This anion complex can also exchanges with a weaker anions on the surface active site of anion exchange resin, so that a [R+] [BiI-4] solid phase binary associational system is produced. Owing to the solid system is a great many dispersive particulates, it can be pressed to a thin-layer by press tools of the so called "thin-layer resin phase"or "resin phase ", and using this solid association system spectrophotometry for the determination of trace metals. So it can increase the analytical sensitivity. This association system exhibits maximum absorbance at 460nm, and obeys Beer's law over the concentration range 0. 01ug/ml～1.20ug/ml of bismuthous(Ⅲ). It has a molar absorptivity of 7.1 ×105 [L/mol cm]. It indicated the resin phase spectrophotometry is a sensitive analytical method for trace bismuthous. It is 18 times higher than routine aqueous spectrophotometry. The relative standard deviations is 1.82% (n=6) for the measurements of 0. 5ug/ml Bi(Ⅲ). The detection limit of Bismuthous(Ⅲ) is 1.4 ×10-8mol/L. The method has applied to the analysis Bi(Ⅲ) in environmental water samples.     

Application of potassium ferricyanide in the spectrophotometric determination of captopril

A novel method for the determination of captopril by speetrophotometer is described in this paper. The experiment is based on the fact that Fe(Ⅲ) is reduced to Fe(Ⅱ) by captopril, then the in situ formed Fe(Ⅱ) reacts with potassium ferricyanide to give the soluble prussian blue at pH 4.00, and its maximal adsorption wavelength (λmax) is 735 nm. Good linear relationship is obtained between the absorbance and the concentration of captopril in the wide range of 0.05-20 μg/mL. The linear regression equation is A = -0.04314 + 0.11423C (μg/mL) with a correlation coefficient R = 0.9998. The detection limit (3a/k) is 0.04 μg/mL, the molar absorption coefficient is 2.5×104 L/mol cm. By mensurating the absorbance of soluble prussian blue, the indirect determination of eaptopril can be obtained. This method has been successfully applied to determination of captopril in pharmaceutical samples.Analytical results obtained are satisfactory.     

STUDY ON THE DETERMINATION OF TRACE BISMUTH（III） BY THIN-LAYER RESIN PHASE S PECTROPHOTOME TRY

In this paper, a new thin-layer ion-exchange resin phase analytical method is introduced. It is based on that, the bismuthous cation can associate with iodic anions, so as to formed an anion complex [BiI4-_] in a strong acidic environments. This anion complex can also exchanges with a weaker anions on the surface active site of anion exchange resin, so that a[R+] [Bil4-] solid phase binary associational system is produced. Owing to the solid system is a great many dispersive particulates, it can be pressed to a thin-layer by press tools of the so called “thin-layer resin phase “ or “resin phase “, and using this solid association system spectrophotometry for the determination of trace metals. So it can increase the analytical sensitivity. This association system exhibits maximum absorbance at 460nm, and obeys Beer‘s law over the concentration range 0.0lug/ml-l.20ug/ml of bismuthous(lll), h has a molar absorptivity of 7.1×l^5 [L/mol.cm]. it indicated the resin phase spectrophotometry is a sensitive analytical method for trace bismuthous. It is 18 times higher than routine aqueous spectrophotometry. The relative standard deviations is 1.82% (n=6) for the F fmeasurements of 0.Sug/ml Bi(llO. The detection limit of Bismuthous(lll) is 1.4 XlO~mol/L. The method has applied to the analysis Bi(lll) in environmental water samples.     

Kinetic spectrophotometric method for the determination of selenium(IV) by its catalytic effect on the reduction of spadns by sulphide in micellar media

A simple kinetic spectrophotometric method was developed for the determination of ultratrace amounts of Se(IV). The method is based on the reduction of spadns by sulphide in micellar media. The reaction was monitored spectrophotometrically by measuring the decrease in the absorbance of spadns at 515 nm with a fixed-time method. The decrease in the absorbance of spadns is proportional to the concentration of Se(IV) in the range 0.5–100 ng/mL with a fixed time of 2.5–7.0 min from the initiation of the reaction. The limit of detection is 0.3 ng/mL Se(IV). The relative standard deviation for the determination of 0.02 and 0.10 μg/mL Se(IV) was 2.10 and 1.95%, respectively. The method was applied to the determination of Se(IV) in water. The text was submitted by the authors in English.     

Flow injection spectrophotometric determination of vitamin E in pharmaceuticals,milk powder and blood serum using potassium ferricyanide-Fe(Ⅲ) detection system

<正>A simple and sensitive flow injection spectrophotometric method is reported for the determination of vitamin E using potassium ferricyanide-Fe(Ⅲ) detection system.In the presence of vitamin E,Fe(Ⅲ)/ferricyanide reduces.The in situ reduced ions are then reacted with unreduced portion of ferricyanide/Fe(Ⅲ) to make soluble Prussian blue,which is monitored at absorption wavelength of 735 nm.Linear calibration graph was obtained in the concentration range of 0.1-40μg mL~(-1).The relative standard deviations (n=4) were in the range of 1.1-3.6%,with limits of detection(3 s blank) of 0.04μg mL~(-1).The proposed method allowed 12 injections h~(-1).The method is applied to determine vitamin E in pharmaceuticals,infant milk and blood serum samples using hexane extraction with the recoveries in the range of 93±3 to 97.5±4%.The method is validated using certified reference materials SRM 968c for blood serum samples.     

Kinetic spectrophotometric determination of bromide in clidinium-c drug

A simple,rapid and sensitive method has been described for the determination of the trace amounts of bromide.The method is based on the catalytic effect of bromide ion on the oxidation of methylene blue by bromate in sulfuric acid media.The reaction is monitored spectrophotometrically by measuring the decrease in the absorbance of methylene blue at 665 nm. Bromide was determined in the range of 0.05-1.90μg/mL with the detection limit of 0.03μg/mL.The relative standard deviations of five replicate determinations of 0.20 and 10.0μg/mL of bromide were 2.4%and 1.8%,respectively.The influence of potential interfering ions and substances was studied.The method is applied to the analysis of bromide in clidinium-c tablet as a real sample.     

A novel method for the spectrophotometric determination of cefradine by using sodium nitroprusside as chromogenic reagent

A novel method is developed for the determination of cefradine by using sodium nitroprusside as chromogenic reagent. The experiment indicates that a russety product is formed by the reaction of cefradine with sodium nitroprusside in basic solution, and the maximum absorption wavelength （λmax） of russety product is 505 rim. And the sensitization of tetradecyl benzyl dimethyl ammonium chloride for the reaction of cefradine with sodium nitroprusside is remarkable, The apparent molar absorption coefficient （5505） is 2.81 × 103 L/mol cm. The linear equation isA = 0.0657 ＋ 0.00804C （μg/mL） in the range of 1.50-55.0μg/mL of cefradine with a correlation coefficient r = 0.9992, and the detection limit is 1.38 p,g/mL. This method has been applied to determine cefradine in capsule and tablet samples.     

基于聚酰胺高效吸附剂和高效液相色谱-紫外检测的抗干扰方法用于同时测定番红花和尿液中3种苏丹染料(英文)

With polyamide(PA)as an efficient sorbent for solid phase extraction(SPE)of Sudan dyes II,III and Red 7B from saffron and urine,their determination by HPLC was performed.The optimum conditions for SPE were achieved using 7 mL methanol/water(1∶9,v/v,pH 7)as the washing solvent and 3 mL tetrahydrofuran for elution.Good clean-up and high(above 90%)recoveries were observed for all the analytes.The optimized mobile phase composition for HPLC analysis of these compounds was methanol-water(70∶30,v/v).The SPE parameters,such as the maximum loading capacity and breakthrough volume,were also determined for each analyte.The limits of detection(LODs),limits of quantification(LOQs),linear ranges and recoveries for the analytes were 4.6-6.6μg/L,13.0-19.8μg/L,13.0-5 000μg/L(r20.99)and 92.5%-113.4%,respectively.The precisions(RSDs)of the overall analytical procedure,estimated by five replicate measurements for Sudan II,III and Red 7B in saffron and urine samples were 2.3%,1.8%and 3.6%,respectively.The developed method is simple and successful in the application to the determination of Sudan dyes in saffron and urine samples with HPLC coupled with UV detection.     

Simultaneous Laser Thermal Lens Spectrometric Determination of Trace Platinum and Palladium in an Aquesous Solution

A selective and sensitive method for determination of platinum and palladium(Ⅱ）in an aqueous solution simultaneously by laser thermal lens spectrometry,based on the complex reaction of 2-(3,5-dichloropyridylazo)-5-dimethylaminoamiline(3,5-diCl-PADMA) with platinum and palladium,has been developed.It is shown that the palladium complex can be fromed at room temperature, while the platinum complex can be only formed after being heated in a boiling water bath.By using this difference of reaction temperature and the characteristic of the complexes mentioned above,the method for simultaneous determination of platinum and palladium was established in an aqueous solution without a pre-separation.The results show that the dynamic linear ranges of determination for platinum and palladium are 0.005-0.04μg/mL and 0.005-0.25μg/mL respectively,and that the detection limits are both 0.002/μg/mL.The method has been applied to the determination of platinum and palladium simultaneously in alloy and catalyst samples with satisfactory results.     

Determination of Sulpiride by Linear Sweep Stripping Voltammetry at a Mercury Electrode

This paper reports the electrochemical properties of sulpiride at a mercury electrode,especially its adsorptive characteristic,Sulpiride dissolved in a supporting electrolyte of a McIlvaine buffer at pH 6.8 represents a sensitive and well defined reduction wave by linear sweep stripping voltammetry.This method is based on the pre-concentration and the reduction of sulpiride at a hung mercury drop electrode.The reduction peak potential is -1.72V(vs.Ag-AgCl) and the peak current is proportional to the concentration of sulpiride in the range of 0.1-0.6 μg/mL.The detection limit is 0.0250μg/mL obtained under the experimental conditions selected in this work.The electrochemical properties of this system were investigated.and the proposed method was applied to the determination of sulpiride in pharmaceutical tablets with satisfactory results,It was compared well with the UV spectrophotometric method,showing a superior sensitivity.     

Spectrophotometric determination of cationic surfactants by formation of ternary complexes with Fe(Ⅲ) and chrome azurol S

An extraction-free spectrophotometric method for the determination of cationic surfactants, such as cetylpyridinium chloride, cetyltrimethylammonium bromide and zephiramine is proposed, which is based on the formation of ternary complexes with Fe(Ⅲ) and chrome azurol S. The molar ratio of the complex is 2:1:1 (Fe(Ⅲ):chrome azurol S:cationic surfactant). The method is simple, rapid and sensitive, giving an apparent molar absorptivity of 4.5×104 L.mol-1.cm-1 and a linear range of 0.1-6.0 umol/L cationic surfactants. The total cationic surfactant content can be determined directly in aqueous solutions by measuring the absorbance at 680 nm (pH 5.8). The method has been successfully applied to water samples.     

The study of preconcentration and separation of vanadium(V) using microcrystalline triphenylmethane loaded with crystal violet and the determination of vanadium(V) in water samples by spectrophotometry

The paper describes a novel method for vanadium(V) preconcentration using microcrystalline triphenylmethane loaded with crystal violet (CV) prior to the determination by spectrophotometry. The effects of different parameters, such as the amounts of crystal violet and triphenylmethane, acidity, stirring time, various salts and metal ions etc on the enrichment yield of V(V) have been investigated to select the experimental conditions. V(V) can be completely separated from Cd(II), Pb(II), Mn(II), Co(II), Cu(II), Fe(III), Ni(II), Al(III), Zn(II) and Hg(II) by controlling acidity. Under the optimum conditions, V(V) can be totally adsorbed on the surface of microcrystalline triphenylmethane. The possible reaction mechanism of the enrichment of V(V) is discussed in detail in this paper. The detection limit of this proposed method is 0.023 μg L⁻¹ with the preconcentration factor of 200. The recovery is in a range of 96.0–104%. The proposed method has been successfully applied to the determination of trace vanadium in various water samples with satisfactory results.     

FLAME ATOMIC ABSORPTION DETERMINATION OF COPPER IN CEREALS FOOD SAMPLES WITH THE PRECONCENTRATION OF POTASSIUM TETRATITANATE WHISKER

A simple and reliable method has been developed for separation and preconcentration of trace amounts of copper ions in cereals food for subsequent measurement by flame atomic absorption spectrometry （FAAS）. The Cu^2＋ ions are adsorbed selectively and quantitatively during the passage. The retained copper ions were desorbed from the potassium tetratitanate whisker with 10.0mL of 2mol/L sulphuric acid solutions as eluent and were determined by FAAS. The linear range was 0.05μg/mL-0.20μg/mL in the original solution with a correlation coefficient of 0.9998. The detection limit of the proposed method is 2. lng/mL in the original solution （3σ, n=9）. Determination of copper in standard ions showed that the proposed method has good accuracy （recovery was more than 95%）. The method was successfully applied for recovery and determination of copper in cereals food samples     

高效液相色谱法测定火药包复层迁移组分

A method based on reversed phase HPLC is used to determine migrated components of propellant coa-tings, The stationary phase is YQG-C_(18)H_(37),and mobile phase is methanol/water,50:50(V/V),with flowrate of 0. 5mL/min. Detector wavelength is set on UV 230nm. Standard deviations of TEGN and NG areboth in 0.01.Coefficients of variafion are 1.19 and 1.86 respectively, The method can meet the requirementsfor the determination of migrated components.     

Incoporation of Fe(Ⅲ) in framework of zeolite L

Zeolite L with Fe in lattice position is prepared from the gel with Fe/(Fe+Al) ratio up to 0.4 using ferric nitrate as Fe source. The incorporation of Fe(Ⅲ) in framework is characterized by XRD, IR, TG/DTA, BET and Mossbauer spectroscopy. Zeolite L is destabilized by Fe(Ⅲ) in framework and the reduction of Fe(Ⅲ) in framework of (Al,Fe )KL was first reported.     

异丙肾上腺素在硅酸铋离子交换薄层上的选择性分离与测定（英文）

A simple and sensitive method for the separation and determination of isoproterenol from other doping drugs has been developed on thin layers of bismuth silicate,a synthetic inorganic ion exchanger as adsorbent in thin layer chromatography(TLC).A mixture of methanol and 0.1 mol/L formic acid(3∶7,v/v)was employed as the mobile phase.The development time was 32 min.The quantitative measurement were performed with a Camag TLC Scanner-3 at wavelength(λ)of 410 nm.The isoproterenol recovery in this procedure was 98.9%.The linear correlation coefficient was greater than 0.987 1 and the relative standard deviation(RSD)was less than 0.94.The limit of detection(LOD)and limit of quantification(LOQ)were 7.7×10-7mol/L and 3.85×10-6mol/L,respectively.This method has been applied in the determination of isoproterenol in dosage forms and in biological fluids.     

Synthesis of Polyacrylaminothiourea Chelating Fiber and Properties of Concentration and Separation of Trace Noble Metal Ions from Samples

A novel polyacrylaminothiourea chelating fiber was synthesized simply and rapidly from nitrilon (an acrylonitrile-based synthetic fiber), which was applied to preconcentrate and separate of trace amount of Au(Ⅲ）,Pt(Ⅳ）,Pd(Ⅳ） and Ir (Ⅳ） ions from solution of samples.The analyzed ions can be quantitatively concentrated by the fiber up to a flow rate of 20.0mL/min at pH2, and can also be desorbed with 15 mL of 4mol/L HCl 3% thiourea from the fiber column with recoveries of 96.5%-100%.The chelating fiber can be reused for ten times,the recoveries of these ions are still over 92%,and hundred to thousand times of excess of Fe(Ⅲ）,Al（Ⅲ）,Ca(Ⅱ），Mg（Ⅱ）,Ni(Ⅱ）,Mn（Ⅱ),Cu(Ⅱ），Zn(Ⅱ），and Cd(Ⅱ） cause no interference on the determination of the analyzed ions by inductively-coupled plasma atomic emission spectrometry (ICP-AES).The static saturation adsorption capacities of the fiber for the analytes are in the range of 1.15-2.80mmol/g.The relative standard deviations for the determination of 20.0ng/mL each of Au(Ⅲ）,Pt(Ⅳ）,Pd(Ⅳ）and Ir(Ⅳ） are in the range of 0.7%-3.0%.The recoveries for test from standard additions to real solution samples are between 96% and 100%.The concentration of each ion in powder sample detected by the method is in good agreement with the certified value.     

SPECTROPHOTOMETRIC STUDY OF BIMETALLIC TERNARY COMPLEX OF LANTHANUM——COPPER WITH ALIZARIN FLUORINE BLUE

The bimetallic ternary complex formation in the aqueous solution of La and Cu with alizarin fluorine blue (AFB) was studied by spectrophotometry.The ternary complex LaCu3(AFB)3 has maximum light absorption at 550nm.The colour reaction selectivity is fairly good and the method can be applied to the direct photometric determination of copper in lanthanum or some pure metals.A new mathematical approach to the treatment of spectrophotometric data for differentiation between mononuclear and polynuclear in solution is presented.The improvable fixed logarithm method is for complexes of the type MmBn(m=n) or MmBn(m=n).We report that La(Ⅲ) combines with AFB at pH 4.5 to form a single complex,withm=n=2,La2(AFB)2.     

Direct and Derivative Spectrophotometric Determination of Zinc with 2,4-Dihydroxybenzaldehyde Isonicotinoyl Hydrazone in Potable Water and Pharmaceutical Samples

A simple and sensitive spectrophotometric method is developed for the determination of zinc in aqueous solutions. The metal ion forms a greenish-yellow colored complex with 2,4-dihydroxybenzaldehyde isonicotinoyl hydrazone (2,4-DHBINH) in the pH range of 4–10. The complex shows maximum absorbance at 390 nm and in the pH range of 6–8. Beer's law is obeyed in the range 0.10–1.50 μg/mL of Zn(II). The molar absorptivity and Sandell's sensitivity are 3.55 × 10⁴ mol⁻¹ cm⁻¹ and 0.0016 μg/cm², respectively. The composition of the complex is 1 : 1. The effect of interfering ions has been studied, and the method was applied to the determination of zinc(II) in potable water and pharmaceutical samples. A fast derivative spectrophotometry method is also proposed for the determination of zinc in the range 0.06–1.60 μg/mL, which is more sensitive than the zero order method. __________ Translated from Zhurnal Analiticheskoi Khimii, Vol. 60, No. 9, 2005, pp. 933–937. Original Russian Text Copyright ? 2005 by Sivaramaiah, Raveendra Reddy. The text was submitted by the authors in English.