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Standard Addition Method (standard + addition_method)

Distribution by Scientific Domains

Chemistry	84%

Selected Abstracts

Simultaneous Determination of Copper and Bismuth by Anodic Stripping Voltammetry Using H-Point Standard Addition Method with Simultaneous Addition of Analytes

ELECTROANALYSIS, Issue 17 2005
Esmaeil Shams
Abstract Simultaneous determination of bismuth and copper by anodic stripping voltammetry using H-point standard addition method (HPSAM) with simultaneous addition of analytes is described. The effect of various parameters including acid concentration, accumulation time, accumulation potential and concentration ratio of analytes in the standard solution on the sensitivity and accuracy of method were investigated. The results of applying the H-point standard addition method showed that Cu2+ and Bi3+ could be determined simultaneously with the concentration ratios of Cu2+ to Bi3+ varying from 1,:,15 to 16,:,1 in the mixed sample. The method was successfully applied to the simultaneous determination of copper and bismuth in some synthetic mixtures. [source]

A New Indirect Electroanalytical Method to Monitor the Contamination of Natural Waters with 4-Nitrophenol Using Multiwall Carbon Nanotubes

ELECTROANALYSIS, Issue 9 2009
Cruz Moraes, Fernando
Abstract The electrochemical detection of the hazardous pollutant 4-nitrophenol (4-NP) at low potentials, in order to avoid matrix interferences, is an important research challenge. This study describes the development, electrochemical characterization and utilization of a multiwall carbon nanotube (MWCNT) film electrode for the quantitative determination of 4-NP in natural water. Electrochemical impedance spectroscopy measurements showed that the modified surface exhibits a decrease of ca. 13 times in the charge transfer resistance when compared with a bare glassy carbon (GC) surface. Voltammetric experiments showed the possibility to oxidize a hydroxylamine layer (produced by the electrochemical reduction of 4-NP on the GC/MWNCT surface) in a potential region which is approximately 700,mV less positive than that needed to oxidize 4-NP, thus minimizing the interference of matrix components. The limit of detection for 4-NP obtained using square-wave voltammetry (0.12,,mol L,1) was lower than the value advised by EPA. A natural water sample from a dam located in São Carlos (Brazil) was spiked with 4-NP and analyzed by the standard addition method using the GC/MWCNT electrode, without any further purification step. The recovery procedure yielded a value of 96.5% for such sample, thus confirming the suitability of the developed method to determine 4-NP in natural water samples. The electrochemical determination was compared with that obtained by HPLC with UV-vis detection. [source]

Quantitative Analysis of Prometrine Herbicide by Liquid,Liquid Extraction Procedures Coupled to Electrochemical Measurements

ELECTROANALYSIS, Issue 6 2009
V. Juarez
Abstract A sensitive method is proposed for the preconcentration and quantification of the herbicide Prometrine (PROM) at a liquid-liquid interface employing square-wave voltammetry. The preconcentration stage was based on liquid-liquid extraction methodology and the PROM quantification was carried out from the peak current of square-wave voltammograms. Under the experimental conditions employed, linear calibration curves in the concentration range 1.0×10,6,M,5.0×10,5,M, with detection limit equal to 1.5×10,6,M were obtained without pretreatment of the samples. This linear range, as well as detection limit could be extended towards lower concentrations when a pretreatment procedure was employed. In this way, linearity of calibration curves between 8.0×10,8,M and 2.4×10,7,M and detection limit of 1.0×10,7,M, were observed. On the other hand, the standard addition method was also used as an alternative and an appropriated quantification technique for this system. A linear concentration range between 1.0×10,6,M and 2.7×10,5,M, with a correlation coefficient of 0.997, was obtained. This procedure has also a promising application in the separation of herbicides from other interferents, present in real samples, previous to their quantification. [source]

Electrocatalytic Oxidation and Voltammetric Determination of Hydrazine on the Tetrabromo- p -Benzoquinone Modified Carbon Paste Electrode

ELECTROANALYSIS, Issue 5 2007
Jahan-Bakhsh Raoof
Abstract The electrochemical properties of hydrazine studied at the surface of a carbon paste electrode spiked with p -bromanil (tetrabromo- p -benzoquinone) using cyclic voltammetry (CV), double potential-step chronoamperometry and differential pulse voltammetry (DPV) in aqueous media. The results show this quinone derivative modified carbon paste electrode, can catalyze the hydrazine oxidation in an aqueous buffered solution. It has been found that under the optimum conditions (pH,10.00), the oxidation of hydrazine at the surface of this carbon paste modified electrode occurs at a potential of about 550,mV less positive than that of a bar carbon paste electrode. The electrocatalytic oxidation peak current of hydrazine showed a linear dependent on the hydrazine concentrations and linear analytical curves were obtained in the ranges of 6.00×10,5 M,8.00×10,3 M and 7.00×10,6 M,8.00×10,4 M of hydrazine concentration with CV and differential pulse voltammetry (DPV) methods, respectively. The detection limits (3,) were determined as 3.6×10,5 M and 5.2×10,6 M by CV and DPV methods. This method was also used for the determination of hydrazine in the real sample (waste water of the Mazandaran wood and paper factory) by standard addition method. [source]

Simultaneous Determination of Copper and Bismuth by Anodic Stripping Voltammetry Using H-Point Standard Addition Method with Simultaneous Addition of Analytes

Evaluation of Cu,Ethylenediamine Metal Ion Buffers as Calibrants for Ion-Selective Electrode Measurement of Copper in Fresh Water Systems

ELECTROANALYSIS, Issue 10 2005
Ling Zeng
Abstract An investigation was made into the accuracy of cupric ion selective electrode (ISE) measurement of Cu in solutions approximating acidic freshwaters with Cu-ethylenediamine buffers used as the calibrants. This method overestimates the free Cu compared with calibration using Cu(NO3)2 standards, the standard addition method, and speciation modelling calculations. Statistical tests showed a small, but significant, difference between the intercepts of the linear Nernstian regressions of the calibration plots of Cu-en buffer standardisation and direct calibration with Cu(NO3)2 standards in matrix that matches the samples. The difference in the intercepts, which corresponds with Eo values of the electrode, is not well understood, but is possibly caused by potentially interfering cations such as Fe2+. The results of this study showed that down to 10,8,M Cu2+, where a linear Nernstian response is possible, the Cu ISE is probably better calibrated using Cu standards prepared in the same matrix as the sample solutions to avoid potential matrix effects. [source]

Heavy Metals in Matrices of Food Interest: Sequential Voltammetric Determination at Trace and Ultratrace Level of Copper, Lead, Cadmium, Zinc, Arsenic, Selenium, Manganese and Iron in Meals

ELECTROANALYSIS, Issue 18 2004
Clinio Locatelli
Abstract The voltammetric methods are very suitable and versatile techniques for the simultaneous metal determination in complex matrices. The present work, regarding the sequential determination of Cu(II), Pb(II), Cd(II), Zn(II) by square-wave anodic stripping voltammetry (SWASV), As(III), Se(IV) by square-wave cathodic stripping voltammetry (SWCSV) and Mn(II), Fe(III) by square-wave voltammetry (SWV) in matrices involved in foods and food chain as wholemeal, wheat and maize meal, are an interesting example of the possibility to sequentially determine each single element in real samples. Besides the set up of the analytical method, particular attention is aimed either at the problem of possible signal interference or to show that, using the peak area Ap as instrumental datum, it is possible to achieve lower limits of detection. The analytical procedure was verified by the analysis of the standard reference materials: Wholemeal BCR-CRM 189, Wheat Flour NIST-SRM 1567a and Rice Flour NIST-SRM 1568a. Precision, as repeatability, and accuracy, expressed as relative standard deviation and relative error, respectively, were lower than 6% in all cases. In the presence of reciprocal interference, the standard addition method considerably improved the resolution of the voltammetric technique. Once set up on the standard reference materials, the analytical procedure was transferred and applied to commercial meals sampled on market for sale. A critical comparison with spectroscopic measurements is also discussed. [source]

Voltammetric Determination of ,-Tocopheryl Acetate in Pharmaceutical Dosage Forms

ELECTROANALYSIS, Issue 11 2004
Slawomir Michalkiewicz
Abstract A simple and rapid voltammetric method has been developed for the quantitative determination of ,-tocopheryl acetate (,-TOAc) in pharmaceutical preparations. Studies with linear scan (LSV), square-wave (SQWV) and differential pulse voltammetry (DPV) were carried out using platinum microelectrodes. A well-defined, irreversible oxidation wave/peak was obtained at 1.30,V (vs. Ag/AgCl reference electrode.) The use of SQWV or DPV technique provides a precise determination of ,-tocopheryl acetate using the multiple standard addition method. The statistical parameters and the recovery study data clearly indicate good reproducibility and accuracy of the method. Accuracy of the results assessed by recovery trials was found within the 99.3% to 103.5%, and 99.1% to 101.4%, for SQWV and DPV, respectively. The quantification limits for the both voltammetric techniques were found to be 6×10,5,M (SQWV) and 7×10,5,M (DPV). Analysis of the authentic samples containing ,-TOAc showed no interference with common additives and excipients, such as unsaturated fatty acids (co-formulated as glycerine esters) and vitamin A (as retinol or ,-carotene). The method proposed does not require any pretreatment of the pharmaceutical dosage forms. A gas chromatography determination of ,-TOAc in real samples was also performed for comparison. [source]

Substances with estrogenic activity in effluents of sewage treatment plants in southwestern Germany.

ENVIRONMENTAL TOXICOLOGY & CHEMISTRY, Issue 10 2001

Abstract A gas chromatography/mass spectrometry method for the simultaneous quantitative determination of natural and synthetic estrogens (17,-estradiol, estrone, 17,-ethinylestradiol, and mestranol), phytoestrogens (genistein and ,-sitosterol), and xenoestrogens (benzyl butyl phthalate, dibutyl phthalate, bisphenol A, 4-nonylphenol [NP], 4-nonylphenoxyacetic acid [NP1EC], 4-nonyl-phenol diethoxylate [NP2EO], and ,-endosulfan) in effluents of sewage treatment plants (STPs) was developed. Identification and quantification were carried out with the standard addition method using analyte-specific and, in some cases, deuterium-labeled internal standards. The effluents of 18 STPs were investigated. Apart from ,-endosulfan and mestranol, all selected substances were detected in the majority of samples. The median concentrations of steroidal estrogens were between 0.4 ng/L (17,-ethiny-lestradiol) and 1.6 ng/L (17,-estradiol). The metabolites of the nonylphenol polyethoxylates, NP, NP1EC, and NP2EO were found in concentrations ranging from the upper-ng/L-range (NP) to the lower-,g/L range (NP1EC). For all substances except mestranol and ,-endosulfan, median values were calculated and compared to the results of other investigations in Europe and the United States. Possible dependencies of measured concentrations on the geographical location, the capacity, the influent composition, and the technical fitting of the STPs are discussed. [source]

Determination of Ti, K, Sm and Gd Values in Geological Survey of Japan Reference Materials by Prompt Gamma Neutron Activation Analysis

GEOSTANDARDS & GEOANALYTICAL RESEARCH, Issue 1 2006
Takashi Sano
activation neutronique et comptage gamma; GSJ; roches ignées; samarium gadolinium Prompt gamma neutron activation analysis was applied to the determination of the titanium, potassium, samarium and gadolinium contents of nine Geological Survey of Japan (GSJ) reference materials (JB-1, 1a, 2, 3; JA-1, 2, 3; JR-1, 2). Firstly, the values in JB-1 were determined by the standard addition method: pressed powder disks of JB-1 were used for neutron irradiation and gamma-ray measurements, after known quantities of standard reagents had been added. Secondly, the contents of eight other reference materials were determined by comparison methods using JB-1 as the comparative standard. The precision of analyses were obtained by replicate determinations on these samples. The relative standard deviation was generally less than 5%. For most samples, analysed values agreed well (< 5%) with the recommended values. L'analyse par activation neutronique et comptage des particules gamma rapide a été appliquée à la détermination des concentrations en titane, potassium, samarium et gadolinium de neuf matériaux de référence du Service Géologique du Japon (GSJ) : (JB-1, 1a, 2, 3; JA-1, 2, 3; JR-1, 2). Tout d'abord les teneurs dans JB-1 ont été déterminées par la technique de l'addition de standard : des pastilles de poudre compressée de JB-1 ont été irradiées par un flux neutronique puis la mesure des émissions gamma, a été effectuée après que des quantités connues de réactifs standards aient été ajoutées. Ensuite les teneurs dans les huit autres ont été déterminées en utilisant JB-1 comme standard de calibration. La précision des analyses a été déterminée en dupliquant les analyses de ces échantillons. Les déviations standard relatives étaient généralement de moins de 5%. Pour la plupart des échantillons les teneurs déterminées sont en bon accord (< 5%) avec les valeurs recommandées. [source]

Analysis of aromatic amines in cigarette smoke,

RAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 18 2003
Regina Stabbert
A method for the analysis of o -toluidine, o -anisidine, 2-naphthylamine, and 4-aminobiphenyl in cigarette mainstream smoke has been developed, which combines the sensitivity of their pentafluoropropionyl (PFP) derivatives in negative ion chemical ionization (NICI) mode with the selectivity of the gas chromatography/tandem mass spectrometry (GC/MS/MS) technique. The use of four deuterated analogues as internal standards along with the application of the standard addition method results in accurate and precise results; the interday precision for the aromatic amines was 3,10% and the accuracy ranged from 97,100%. This method was applied to two American-blend University of Kentucky reference cigarettes, eight American-blend market cigarettes, a bright (flue-cured) tobacco cigarette, and an electrically heated cigarette smoking system (EHCSS). For the American-blend cigarettes there was a linear correlation between aromatic amine yields and mainstream smoke ,tar' (,tar',=,total particulate matter , (nicotine,+,water)), whereas the bright tobacco cigarette and the EHCSS demonstrated significantly lower aromatic amine yields on an equal ,tar' basis. The results support the hypothesis that the nitrogen content of the tobacco, and above all the cigarette combustion temperature, are determining factors for the yields of aromatic amines in smoke. Copyright © 2003 John Wiley & Sons, Ltd. [source]

Differential Kinetic Spectrophotometric Determination of Methamidophos and Fenitrothion in Water and Food Samples by Use of Chemometrics

CHINESE JOURNAL OF CHEMISTRY, Issue 3 2010
Na Deng
Abstract A spectrophotometric method for simultaneous analysis of methamidophos and fenitrothion was proposed by application of chemometrics to the spectral kinetic data, which was based upon the difference in the inhibitory effect of the two pesticides on acetylcholinesterase (AChE) and the use of 5,5,-dithiobis(2-nitrobenzoic acid) (DTNB) as a chromogenic reagent for the thiocholine iodide (TChI) released from the acetylthiocholine iodide (ATChI) substrate. The absorbance of the chromogenic product was measured at 412 nm. The different experimental conditions affecting the development and stability of the chromogenic product were carefully studied and optimized. Linear calibration graphs were obtained in the concentration range of 0.5,7.5 ng·mL,1 and 5,75 ng·mL,1 for methamidophos and fenitrothion, respectively. Synthetic mixtures of the two pesticides were analysed, and the data obtained processed by chemometrics, such as partial least square (PLS), principal component regression (PCR), back propagation-artificial neural network (BP-ANN), radial basis function-artificial neural network (RBF-ANN) and principal component-radial basis function-artificial neural network (PC-RBF-ANN). The results show that the RBF-ANN gives the lowest prediction errors of the five chemometric methods. Following the validation of the proposed method, it was applied to the determination of the pesticides in several commercial fruit and vegetable samples; and the standard addition method yielded satisfactory recoveries. [source]

Voltametric and Flow Injection Determination of Oxytetracycline Residues in Food Samples Using Carbon Fiber Microelectrodes

ELECTROANALYSIS, Issue 7 2003
L. Agüí
Abstract A voltammetric method for the determination of the antibiotic oxytetracycline (OTC) in food samples is reported. Carbon fiber microelectrodes (CFMEs), which allow voltammetric measurements to be performed in a small volume (1,mL) of the analyte extract from the samples, are employed. Repeatable electroanalytical responses were obtained with no need of applying cleaning treatments to the CFME. Under the optimized square-wave conditions, a linear calibration plot for OTC was obtained in the 1.0×10,6,1.0×10,4,mol,L,1 range, with a detection limit of 2.9×10,7,mol,L,1 (150,ng,mL,1) OTC. The determination of OTC by a flow-injection method with amperometric detection using a homemade flow cell specially designed to work with CFMEs, was also evaluated using pure acetonitrile as the carrier. The SW voltammetric method was applied to the determination of OTC in spiked milk and eggs samples, at 100,ng,mL,1 and 200,ng g,1 levels, respectively. The procedure involved the extraction of the analyte in ethyl acetate, evaporation of the solvent and reconstitution of the residue in acetonitrile ,5.0×10,4,mol,L,1 tetrabutylammonium perchlorate medium. Recoveries of 96±8 and 91±8% were obtained for milk and eggs, respectively, by applying the standard additions method. [source]