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Sample records for modified titrimetric determination

  1. Titrimetric determination of ruthenium

    International Nuclear Information System (INIS)

    Velichko, V.V.; Belyaeva, T.I.; Kudinova, V.K.; Usatenko, Yu.I.

    1978-01-01

    Titration of ruthenium(4) hydrochloric-acid solutions with Mohr's salt, hydroquinone, and thiourea has been studied with the use of biampero- and potentiometric indication of the titration end point (t.e.p.) Potentiometric and amperometric indication of the t.e.p. is applicable when Ru(4) concentration is from 20 to 6000 mkg in 20 ml of the titrated solution; biamperometric indication can be used at a concentration of 5-1000 mkg in the same volume. It has been established that titration of Ru(4) (in the form of the Na 2 RuCl 6 solution) with Mohr's salt is not hindered by the presence of 1000-fold excess of alkaline and alkali-earth metals, Al, Ti(4), Mn(2), Cr(3), Fe(3), Co, Ni, Cu, Zn, Ga, Ge(4), As, Se, Mo(6), Cd, In, and Te; 100-fold excess of Rh, Pd, W, Bi, and Sn; 10-fold excess of Ag, Au, Pt, Hg, Os. Along with Ru(4) titrated are Ir(4), Te(3), V(5), and Ce(4). Selectivity of hydroquinone and thiourea is lower. Titrimetric procedure of determining ruthenium has been tested for ruthenium alloy containing cobalt tungsten. It cannot be recommended for analysis of the samples which dissolve in aqua regia

  2. Titrimetric determination of uranium

    International Nuclear Information System (INIS)

    Florence, T.M.

    1989-01-01

    Titrimetric methods are almost invariably used for the high precision assay of uranium compounds, because gravimetric methods are nonselective, and not as reliable. Although precipitation titrations have been used, for example with cupferron and ferrocyanide, and chelate titrations with EDTA and oxine give reasonable results, in practice only redox titrations find routine use. With all redox titration methods for uranium a precision of 01 to 02 percent can be achieved, and precisions as high as 0.003 percent have been claimed for the more refined techniques. There are two types of redox titrations for uranium in common use. The first involves the direct titration of uranium (VI) to uranium (IV) with a standard solution of a strong reductant, such as chromous chloride or titanous chloride, and the second requires a preliminary reduction of uranium to the (IV) or (III) state, followed by titration back to the (VI) state with a standard oxidant. Both types of redox titrations are discussed. 4 figs

  3. Modified titrimetric determination of plutonium using photometric end-point detection

    International Nuclear Information System (INIS)

    Baughman, W.J.; Dahlby, J.W.

    1980-04-01

    A method used at LASL for the accurate and precise assay of plutonium metal was modified for the measurement of plutonium in plutonium oxides, nitrate solutions, and in other samples containing large quantities of plutonium in oxidized states higher than +3. In this modified method, the plutonium oxide or other sample is dissolved using the sealed-reflux dissolution method or other appropriate methods. Weighed aliquots, containing approximately 100 mg of plutonium, of the dissolved sample or plutonium nitrate solution are fumed to dryness with an HC1O 4 -H 2 SO 4 mixture. The dried residue is dissolved in dilute H 2 SO 4 , and the plutonium is reduced to plutonium (III) with zinc metal. The excess zinc metal is dissolved with HCl, and the solution is passed through a lead reductor column to ensure complete reduction of the plutonium to plutonium (III). The solution, with added ferroin indicator, is then titrated immediately with standardized ceric solution to a photometric end point. For the analysis of plutonium metal solutions, plutonium oxides, and nitrate solutions, the relative standard deviation are 0.06, 0.08, and 0.14%, respectively. Of the elements most likely to be found with the plutonium, only iron, neptunium, and uranium interfere. Small amounts of uranium and iron, which titrate quantitatively in the method, are determined by separate analytical methods, and suitable corrections are applied to the plutonium value. 4 tables, 4 figures

  4. Titrimetric determination of uranium in tributyl phosphate

    International Nuclear Information System (INIS)

    Sobkowska, A.

    1978-01-01

    The titrimetric method involving the reduction of U(VI) to uranium(IV) by iron(II) in phosphoric acid, selective oxidation of the excess of iron(II) and potentiometric titration with dichromate was directly used for the determination of uranium in tributyl phosphate mixtures. The procedure was applied to solutions containing more than 2 mg of uranium in the sample but the highest precision and accuracy were obtained in the range from 20 to 200 mg of uranium. Dibutyl phosphate and monobutyl phosphate as well as the other radiolysis products of TBP had no influence on the results of determinations. (author)

  5. Joint titrimetric determination of zirconium and hafnium

    International Nuclear Information System (INIS)

    Vazquez, Cristina; Botbol, Moises; Bianco de Salas, G.N.; Cornell de Casas, M.I.

    1980-01-01

    A method for the joint titrimetric determination of zirconium and hafnium, which are elements of similar chemical behaviour, is described. The disodic salt of the ethylendiaminetetracetic acid (EDTA) is used for titration, while xilenol orange serves as final point indicator. Prior to titration it is important to evaporate with sulfuric acid, the solution resulting from the zirconium depolymerization process, to adjust the acidity and to eliminate any interferences. The method, that allows the quick and precise determination of zirconium and hafnium in quantities comprised between 0.01 and mg, was applied to the analysis of raw materials and of intermediate and final products in the fabrication of zirconium sponge and zircaloy. (M.E.L.) [es

  6. Analytical procedure for the titrimetric determination of uranium in concentrates

    International Nuclear Information System (INIS)

    Florence, T.M.; Pakalns, P.

    1989-01-01

    In 1964 Davis and gray published a titrimetric method for uranium which does not require column reductors, electronic instruments or inert atmospheres, and is sufficiently selective to enable uranium to be determined without prior separation. The method involves reduction of uranium (VI) to (IV) by ferrous sulphate in concentrated phosphoric acid medium. The excess ion (II) is then selectively oxidised by nitric acid using molybdenum catalyst. After addition of sulphuric acid and dilution with water, the uranium (IV) is titrated with standard potassium dichromate, using barium diphenylamine sulphonate indicator. This method has been found to be simple, precise and reliable, and applicable to a wide range of uranium-containing materials. The method given here for determining uranium in concentrates is essentially that of Davies and Gray. Its applications, apparatus, reagents, procedures and accuracy and precision are discussed. 10 refs

  7. Titrimetric determination of tungsten in its alloys with tantalum

    International Nuclear Information System (INIS)

    Elinson, S.V.; Nezhnova, T.I.

    1982-01-01

    Titrimetric method of tungsten determination in tantalum base alloys has been developed. The method permits to determine 5-10% tungsten in the alloys with relative standard deviation of 0.013. The conditions are created by application of precipitation from homogeieous solutions or by the method of appearing reagents at pH values, which condition gradual hydrolytic precipitation of tantalum, and sodium tungstate remains in the solution and is not sorbed on tantalum hydroxide. After separation of tantalum oxide tungsten is precipitated in the form of lead tungstate by the excess of ti trated solution of lead salt during boiling and then at the background of lead tungstate precipitate without its separation lead excess is titrated by EDTA in the presence of mixed indicator-4-(2-pyridylazo)resocinol and xylenole orange in acetate buffer solution

  8. Titrimetric and Spectrophotometric Determination of Metaprolol tartrate in Pharmaceuticals Using N-Bromosuccinimide

    OpenAIRE

    K. Basavaiah; B. C. Somashekar

    2007-01-01

    One titrimetric and two spectrophotometric methods are presented for the assay of metaprolol tartrate (MPT) in bulk drug and in tablets. The methods employ N-bromosuccinimide (NBS) as the oxidimetric reagent and two dyes, methyl orange and indigo carmine as spectrophotometric reagents. In titrimetry, an acidified solution of MPT is treated with a known excess amount of NBS and after a definite time, the unreacted oxidant is determined by iodometric back titration. Spectrophotometry involve...

  9. Titrimetric determination of Zr, Hf, Sn, Ta and rare earths in binary oxide systems

    International Nuclear Information System (INIS)

    Flyantikova, G.V.; Chekirda, T.N.; Lasovskaya, O.N.; Migun, N.P.

    1989-01-01

    Proximate method of titrimetric determination of oxides of Zr(4), Hf(4), Sn(4), Ta(5) and rare earths (La, Lu, Nd, Eu, Yb, Y) in binary systems (BS) with high accuracy was developed. A study was made on conditions of decomposition and dissolution of BS by means of their treatment by the mixture of solutions of concentrated sulfuric acid and ammonium sulfate during 2h boiling eith successive complexonometric determination of their components by direct EDTA titration in the presence of xylenol orange. The relative standard deviation when titrating 0.3-9.7mg oxides in BS does not exceed 0.02

  10. Titrimetric determination of thiocyanate in solutions of the hafnium-zirconium separation process

    International Nuclear Information System (INIS)

    Vazquez, Cristina; Botbol, Moises; Hernandez, M.H.

    1980-01-01

    The control of the thiocyanate concentration is necessary during the process of separating hafnium from zirconium by the hexone-thiocyanate method. Said control is carried out by titrimetric determination of thiocyanate in aqueous and organic solutions containing hydrochloric acid and ammonium thiocyanate in presence or absence of zirconium and/or hafnium. The method consists in a redox volumetric analysis using a cerium (IV) salt as titrating agent, and ferroine as the final point indicator. Owing to the instability of thiocyanate in an acid medium it is necessary to know previously if the decomposition of solutions with different concentration of ammonium thiocyanate and hydrochloric acid may have an influence upon the analytic results or may even invalidate them. In order to obtain reliable results, it must be taken into account that the stability of the solutions depends on the thiocyanate concentration, the acidity and the time elapsed from the moment the sample is taken until the test is performed. The decomposition process can be slowed down by cooling the solutions. This method allows to control the plant and does not require any special equipment. (M.E.L) [es

  11. Titrimetric and Spectrophotometric Determination of Metaprolol tartrate in Pharmaceuticals Using N-Bromosuccinimide

    Directory of Open Access Journals (Sweden)

    K. Basavaiah

    2007-01-01

    Full Text Available One titrimetric and two spectrophotometric methods are presented for the assay of metaprolol tartrate (MPT in bulk drug and in tablets. The methods employ N-bromosuccinimide (NBS as the oxidimetric reagent and two dyes, methyl orange and indigo carmine as spectrophotometric reagents. In titrimetry, an acidified solution of MPT is treated with a known excess amount of NBS and after a definite time, the unreacted oxidant is determined by iodometric back titration. Spectrophotometry involves adding a measured excess of NBS to MPT in acid medium followed by determination of residual NBS by reacting with a fixed amount of either methyl orange and measuring the absorbance at 520 nm (Method A or indigo carmine and measuring the absorbance at 610 nm (Method B. In all the methods, the amount of NBS reacted corresponds to the amount of MPT. Reaction conditions have been optimized. Titrimetry allows the determination of 1 - 12 mg of MPT and the calculations are based on a 1: 4 (MPT: NBS reaction stoichiometry. In spectrophotometry, the measured absorbance is found to increase linearly with the concentration of MPT serving as basis for quantitation. The systems obey Beer’s law for 0.5 - 4.0 μg mL-1 and 1.25 - 10.0 μg mL-1 for method A and method B, respectively. The apparent absorptivities are calculated to 1.07 × 105 be and 4.22 × 104 L mol cm-1 for method A and method B, respectively. The methods developed were applied to the assay of MPT in commercial tablet formulations, and the results were compared statistically with those of a reference method. The accuracy and reliability of the methods were further ascertained by performing recovery tests via standard-addition method.

  12. Novel and validated titrimetric method for determination of selected angiotensin-II-receptor antagonists in pharmaceutical preparations and its comparison with UV spectrophotometric determination

    Directory of Open Access Journals (Sweden)

    Shrikant H. Patil

    2012-12-01

    Full Text Available A novel and simple titrimetric method for determination of commonly used angiotensin-II-receptor antagonists (ARA-IIs is developed and validated. The direct acid base titration of four ARA-IIs, namely eprosartan mesylate, irbesartan, telmisartan and valsartan, was carried out in the mixture of ethanol:water (1:1 as solvent using standardized sodium hydroxide aqueous solution as titrant, either visually using phenolphthalein as an indicator or potentiometrically using combined pH electrode. The method was found to be accurate and precise, having relative standard deviation of less than 2% for all ARA-IIs studied. Also, it was shown that the method could be successfully applied to the assay of commercial pharmaceuticals containing the above-mentioned ARA-IIs. The validity of the method was tested by the recovery studies of standard addition to pharmaceuticals and the results were found to be satisfactory. Results obtained by this method were found to be in good agreement with those obtained by UV spectrophotometric method. For UV spectrophotometric analysis ethanol was used as a solvent and wavelength of 233 nm, 246 nm, 296 nm, and 250 nm was selected for determination of eprosartan mesylate, irbesartan, telmisartan, and valsartan respectively. The proposed titrimetric method is simple, rapid, convenient and sufficiently precise for quality control purposes. Keywords: Angiotensin-II-receptor antagonists, Titrimetric assay, UV spectrophotometry, Validation

  13. Ammonium vanadate titrimetric method for determination of micro amount uranium in rock and soil by using vanadate-gold indicator

    International Nuclear Information System (INIS)

    Li Yucheng.

    1990-01-01

    A new vanadate-gold indicator was successfully applied to the ammonium vanadate titrimetric method for determination of micro amount uranium in rock and soil. Uranium in 0.1g of sample is reduced by titanium trichloride in phosphoric acid. Excessive Ti (III) and other low-valent ions are oxidized by sodium nitrite, while the complex of uranium (IV)-phosphate is not oxidized. Excessive nitrite is destroyed by urea. When the concentration of phosphoric acid is 22-24 % , adding two drops of vanadate-gold indicator, uranium (IV) is titrated by standardized ammonium vanadate solution (T = 0.02-20gU/ml) and the end-point is judged by a violet-red color appearance

  14. Nuclear fuel technology - Determination of uranium in solutions, uranium hexafluoride and solids - Part 2: Iron(II) reduction/cerium(IV) oxidation titrimetric method

    International Nuclear Information System (INIS)

    2004-01-01

    This first edition of ISO 7097-1 together with ISO 7097-2:2004 cancels and replaces ISO 7097:1983, which has been technically revised, and ISO 9989:1996. ISO 7097 consists of the following parts, under the general title Nuclear fuel technology - Determination of uranium in solutions, uranium hexafluoride and solids: Part 1: Iron(II) reduction/potassium dichromate oxidation titrimetric method; Part 2: Iron(II) reduction/cerium(IV) oxidation titrimetric method. This part 2. of ISO 7097 describes procedures for determination of uranium in solutions, uranium hexafluoride and solids. The procedures described in the two independent parts of this International Standard are similar: this part uses a titration with cerium(IV) and ISO 7097-1 uses a titration with potassium dichromate

  15. Nuclear fuel technology - Determination of uranium in solutions, uranium hexafluoride and solids - Part 1: Iron(II) reduction/potassium dichromate oxidation titrimetric method

    International Nuclear Information System (INIS)

    2004-01-01

    This first edition of ISO 7097-1 together with ISO 7097-2:2004 cancels and replaces ISO 7097:1983, which has been technically revised, and ISO 9989:1996. ISO 7097 consists of the following parts, under the general title Nuclear fuel technology - Determination of uranium in solutions, uranium hexafluoride and solids: Part 1: Iron(II) reduction/potassium dichromate oxidation titrimetric method; Part 2: Iron(II) reduction/cerium(IV) oxidation titrimetric method. This part 1. of ISO 7097 describes procedures for the determination of uranium in solutions, uranium hexafluoride and solids. The procedures described in the two independent parts of this International Standard are similar: this part uses a titration with potassium dichromate and ISO 7097-2 uses a titration with cerium(IV)

  16. Determination of microamounts of carbon in various metals and alloys by the combustion-nonaqueous titrimetric method

    Energy Technology Data Exchange (ETDEWEB)

    Yoshimori, T; Koike, A [Science Univ. of Tokyo (Japan). Faculty of Engineering; Katoh, N

    1977-12-01

    Microamounts of carbon (7 -- 600 ppm) in ferrous and non-ferrous metals and alloys were determined by the combustion-nonaqueous titrimetric method. The carbon dioxide liberated by the combustion of a sample was absorbed with dimethylformamide (DMF) containing monoethanolamine and then the absorbent was titrated with the standard benzene-methanol solution of tetra-n-butylammonium hydroxide (0.007-0.002 M). The end point of the titration was located either visibly by using thymolphthalein as an indicator or potentiometrically by using a couple of platinum and calomel (containing DMF) electrodes. Pure benzoic acid was used as the standard substance for the standardization. Many improvements were given on both the combustion apparatus and the procedure. Microamounts of carbon in various samples were determined by the proposed method. They are : plain carbon and high purity ferritic stainless steels (0.05 -- 0.002% C), Inconel X-750 (0.027% C), copper alloys (20 -- 30 ppm C), tantalum powder (40 ppm C) and high purity metallic uranium (7 ppm C). All results were quite satisfactory and indicate that the proposed method was adaptable for the determination of carbon less than 100 ppm in various samples without use of any standard samples or calibration curves.

  17. A rapid and specific titrimetric method for the precise determination of plutonium using redox indicator

    International Nuclear Information System (INIS)

    Chitnis, R.T.; Dubey, S.C.

    1976-01-01

    A simple and rapid method for the determination of plutonium in plutonium nitrate solution and its application to the purex process solutions is discussed. The method involves the oxidation of plutonium to Pu(VI) with the help of argentic oxide followed by the destruction of the excess argentic oxide by means of sulphamic acid. The determination of plutonium is completed by adding ferrous ammonium sulphate solution which reduces Pu(VI) to Pu(IV) and titrating the excess ferrous with standard potassium dichromate solution using sodium diphenylamine sulphonate as the internal indicator. The effect of the various reagents add during the oxidation and reduction of plutonium, on the final titration has been investigated. The method works satisfactorily for the analysis of plutonium in the range of 0.5 to 5 mg. The precision of the method is found to be within 0.1%. (author)

  18. Titrimetric and photometric methods for determination of hypochlorite in commercial bleaches.

    Science.gov (United States)

    Jonnalagadda, Sreekanth B; Gengan, Prabhashini

    2010-01-01

    Two methods, simple titration and photometric methods for determination of hypochlorite are developed, based its reaction with hydrogen peroxide and titration of the residual peroxide by acidic permanganate. In the titration method, the residual hydrogen peroxide is estimated by titration with standard permanganate solution to estimate the hypochlorite concentration. The photometric method is devised to measure the concentration of remaining permanganate, after the reaction with residual hydrogen peroxide. It employs 4 ranges of calibration curves to enable the determination of hypochlorite accurately. The new photometric method measures hypochlorite in the range 1.90 x 10(-3) to 1.90 x 10(-2) M, with high accuracy and with low variance. The concentrations of hypochlorite in diverse commercial bleach samples and in seawater which is enriched with hypochlorite were estimated using the proposed method and compared with the arsenite method. The statistical analysis validates the superiority of the proposed method.

  19. Titrimetric determination of uranium in low-grade ores by the ferrous ion-phosphoric acid reduction method

    International Nuclear Information System (INIS)

    Hitchen, A.; Zechanowitsch, G.

    1980-01-01

    The modification and extension of the U.S.A.E.C. ferrous ion-phosphoric acid reduction method for the determination of uranium in high-grade or relatively pure material to a method for the determination of uranium with a high accuracy and precision, in ores containing 0.004 to 7% U is described. It is simple, rapid and requires no prior separations from elements that, in other methods, frequently interfere. For sample materials having very high concentrations of interfering elements, a prior concentration step using extraction with tri-n-octylphosphine oxide is described, but it is shown that, for most low-grade ores, this step is unnecessary. (author)

  20. Contactless, probeless and non-titrimetric determination of acid-base reactions using broadband acoustic resonance dissolution spectroscopy (BARDS).

    Science.gov (United States)

    Ahmed, M Rizwan; McSweeney, Sean; Krüse, Jacob; Vos, Bastiaan; Fitzpatrick, Dara

    2018-02-12

    pH determination is a routine measurement in scientific laboratories worldwide. Most major advances in pH measurement were made in the 19th and early 20th century. pH measurements are critical for the determination of acid base reactions. This study demonstrates how an acid-base reaction can be monitored without the use of a pH probe, indicator and titres of reagent. The stoichiometric reaction between carbonate and HCl acid yields specific quantities of CO 2 , which causes reproducible changes to the compressibility of the solvent. This in turn slows down the speed of sound in solution which is induced by a magnetic follower gently tapping the inner wall of the vessel. As a consequence the frequencies of the acoustic resonances in the vessel are reduced. This approach is called Broadband Acoustic Resonance Dissolution Spectroscopy (BARDS) which harnesses this phenomenon for many applications. The acid-carbonate experiments have also been validated using H 2 SO 4 acid and using both potassium and sodium counterions for the carbonate. This method can be used to interrogate strong acid-base reactions in a rapid and non-invasive manner using carbonate as the base. The data demonstrate the first example of a reactant also acting as an indicator. The applicability of the method to weak acids has yet to be determined. A novel conclusion from the study is that a person with a well-trained ear is capable of determining the concentration and pH of a strong acid just by listening. This brings pH measurement into the realm of human perception.

  1. Titrimetric application of 2-bromo-bis-1,10-phenanthroline-copper (II) bromide as a titrant in determination of ascorbic acid in pure form, fruits and vegetables

    International Nuclear Information System (INIS)

    Oladeji, O.

    2016-01-01

    Ascorbic acid is very important to man and the consumption has been linked to the prevention of degenerative diseases such as scurvy and serves as an antioxidants. There have been different approaches in the determination of ascorbic acid in fruits and vegetable. In recent times, new methods were introduced by scientists. Therefore, in order to prove the authenticity of these methods, the concentrations obtained were compared with the conventional methods. The results show that orange has maximum ascorbic acid content when compared to cashew and in vegetables Vermonia baldwinii has maximum and Solanium incanum has low ascorbic acid content. The amount of ascorbic acid determined by 2, 6-dichlorophenol-indophenol and copper (II) complex (2-bromo-bis-1, 10 phenanthroline-copper (II) bromide) are comparable.Therefore, 2-bromo-bis-1, 10-phenanthroline-copper (II) bromide can serve as a titrant in titrimetric determination of ascorbic acid in pure form, fruits and vegetables. (author)

  2. Gravimetric and titrimetric methods of analysis

    International Nuclear Information System (INIS)

    Rives, R.D.; Bruks, R.R.

    1983-01-01

    Gravimetric and titrimetric methods of analysis are considered. Methods of complexometric titration are mentioned, as well as methods of increasing sensitivity in titrimetry. Gravimetry and titrimetry are applied during analysis for traces of geological materials

  3. Anoxic Activated Sludge Monitoring with Combined Nitrate and Titrimetric Measurements

    DEFF Research Database (Denmark)

    Petersen, B.; Gernaey, Krist; Vanrolleghem, P.A.

    2002-01-01

    was with the carbon source in excess, since excess nitrate provoked nitrite build-up thereby complicating the data interpretation. A conceptual model could quantitatively describe the experimental observations and thus link the experimentally measured proton production with the consumption of electron acceptor......An experimental procedure for anoxic activated sludge monitoring with combined nitrate and titrimetric measurements is proposed and evaluated successfully with two known carbon sources, (-)acetate and dextrose. For nitrate measurements an ion-selective nitrate electrode is applied to allow...... for frequent measurements, and thereby the possibility for detailed determination of the denitrification biokinetics. An internal nitrate electrode calibration is implemented in the experiments to avoid the often-encountered electrode drift problem. It was observed that the best experimental design...

  4. Modeling Aerobic Carbon Source Degradation Processes using Titrimetric Data and Combined Respirometric-Titrimetric Data: Structural and Practical Identifiability

    DEFF Research Database (Denmark)

    Gernaey, Krist; Petersen, B.; Dochain, D.

    2002-01-01

    The structural and practical identifiability of a model for description of respirometric-titrimetric data derived from aerobic batch substrate degradation experiments of a CxHyOz carbon source with activated sludge was evaluated. The model processes needed to describe titrimetric data included su...... the initial substrate concentration S-S(O) is known. The values found correspond to values reported in literature, but, interestingly, also seem able to reflect the occurrence of storage processes when pulses of acetate and dextrose are added. (C) 2002 Wiley Periodicals, Inc....

  5. Modeling Aerobic Carbon Source Degradation Processes using Titrimetric Data and Combined Respirometric-Titrimetric Data: Experimental Data and Model Structure

    DEFF Research Database (Denmark)

    Gernaey, Krist; Petersen, B.; Nopens, I.

    2002-01-01

    Experimental data are presented that resulted from aerobic batch degradation experiments in activated sludge with simple carbon sources (acetate and dextrose) as substrates. Data collection was done using combined respirometric-titrimetric measurements. The respirometer consists of an open aerated....... For acetate, protons were consumed during aerobic degradation, whereas for dextrose protons were produced. For both carbon sources, a linear relationship was found between the amount of carbon source added and the amount of protons consumed (in case of acetate: 0.38 meq/mmol) or produced (in case of dextrose...

  6. Application of titrimetric method in the determination of uranium

    International Nuclear Information System (INIS)

    Cantagallo, M.I.C.; Rodrigues, C.

    1985-01-01

    The analysis of nuclear materials are carried out by Davies-Gray titration. This procedure is evaluated by 'Safeguards Analytical Laboratory - IAEA' for application in safeguards materials. The purpose of this paper is in evaluating the precision and accuracy of the analysis carried out in laboratory by participation in 'IAEA' - Analytical Control Service Program'. The samples SR-50 and SR-60 are analysed and analytical results, the precision and accuracy are presented and discussed. (Author) [pt

  7. TITRIMETRIC AND SENSITIVE SPECTRO-PHOTOMETRIC METHODS FOR THE ASSAY OF QUETIAPINE FUMARATE IN PHARMACEUTICAL FORMULATIONS

    Directory of Open Access Journals (Sweden)

    Nagaraju Rajendraprasad

    2011-03-01

    Full Text Available Quetiapine fumarate (QTF is a selective monoaminergic antagonist with high affinity for the serotonin Type 2 (5HT2, and dopamine type 2 (D2 receptors. Titrimetric and spectrophotometric assay of quetiapine fumarate (QTF using perchloric acid and acetic acid as reagents are described. The first method (method A is a non-aqueous titrimetric method and is based on the titration of QTF in glacial acetic acid with 0.01 M acetous perchloric acid using crystal violet as indicator. In the second method (method B, QTF has been measured in 0.1M acetic acid spectrophotometrically at a wavelength of 222 nm. The titri¬metric method was applicable over the range of 2.0–20.0 mg of QTF. The reac¬tion stoichiometry of 1:3 is obtained which served as the basis for calculation. In spectrophotometry, Beer’s law was obeyed over the concentration range of 1.25–15.0 µg mL-1. The linear regression equation of the calibration graph was A = 0.0115 + 0.0673c with a regression coefficient (r of 0.9986 (n = 7. The apparent molar absorptivity was calculated to be 4.25104 L mol-1cm-1 and the Sandell sensitivity was 0.0145 µg cm-2. The limits of detection (LOD and quantification (LOQ calculated as per the ICH guidelines were 0.07 and 0.21 µg mL-1, respectively. Accuracy and precision of the assays were determined by computing the intra-day and inter-day variations at three different levels of QTF. The intra-day and inter-day relative standard deviation (%RSD were in the range of 0.99–2.88 and 1.65–2.32%, for method A and B, respectively, with an acceptable percentage relative error (%RE < 2%. The methods were successfully applied to the determination of QTF in two different brands of tablets with good accuracy and precision and without detectable interference by excipients. The methods have demonstrated to be simple and easy to apply in routine usage and do not need any costly instrumentation. Therefore, the proposed procedures are advantageous and can be

  8. Ammonium ions determination with polypyrrole modified electrode

    Directory of Open Access Journals (Sweden)

    Luiz Henrique Dall´Antonia

    2007-03-01

    Full Text Available The present work relates the preparation of polypyrrole films (PPy deposited on surfaces of glass carbon, nickel and ITO (tin oxide doped with indium on PET plastic, in order to study the ammonium detection. The popypyrrole films were polymerized with dodecylbenzenesulfonate (DBSA on the electrodes, at + 0,70 V vs. Ag/AgCl, based on a solution containing the pyrrole monomer and the amphiphilic salt. Films deposited on glass carbon presented better performance. Cyclic voltammetries, between – 1,50 to + 0,5 V vs. Ag/AgCl, were repeated adding different concentrations of NH4Cl, in order to observe the behavior of the film as a possible detector of ions NH4+. The peak current for oxidation varies with the concentration of ammonium. A linear region can be observed in the band of 0 to 80 mM, with a sensibility (Sppy approximately similar to 4,2 mA mM-1 cm-2, showing the efficacy of the electrodes as sensors of ammonium ions. The amount of deposited polymer, controlled by the time of growth, does not influence on the sensor sensibility. The modified electrode was used to determine ammonium in grounded waters.

  9. Determination of vanadium

    International Nuclear Information System (INIS)

    Stepin, V.V.; Kurbatova, V.I.; Fedorova, N.D.

    1980-01-01

    Titrimetric and potentiometric methods of vanadium determination in ferrovanadium are developed. The essence of the titrimetric method using phenylanthranilic acid as indicator is in the following. Ferrovanadium weighed amount is dissolved in H 2 SO 4 , vanadium is oxidated by potassium permanganate to V(5) and is titrated by a solution of double salt of sulfuric Fe(2) and ammonium in the presence of indicator. Potentiometric titration is carried out using the same indicator [ru

  10. Nickel hydroxide modified electrodes for urea determination

    Directory of Open Access Journals (Sweden)

    Luiz Henrique Dall´Antonia

    2007-03-01

    Full Text Available Nickel hydroxide films were prepared by electrodeposition from a solution Ni(NO32 0,05 mol L ?¹ on ITO electrodes (Tin oxide doped with Indium on PET-like plastic film, applying a current of - 0,1 A cm ?² during different time intervals between 1800 and 7200 s. The electrochemical behavior of the nickel hydroxide electrode was investigated through a cyclic voltammogram, in NaOH 1,0 mol L ?¹, where it was observed two peaks in the profile in 0,410 and 0,280 V, corresponding to redox couple Ni(II/Ni(III. A sensor for urea presenting a satisfactory answer can be obtained when, after the deposit of the film of Ni(OH2 on the electrode of nickel, it is immersed in a solution of NaOH 1,0 mol L ?¹ and applying a potential of + 0,435 V, where the maximum of the anodic current occurs in the cyclic voltammogram. Analyzing the results it can be observed that, for a range of analite concentration between 5 to 50 m mol L ?¹, the behavior is linear and the sensibility found was of 20,3 mA cm?² (mol L?¹?¹, presenting reproducibility confirming the nickel hydroxide electrodes utilization for the determination of urea.

  11. Description and implementation of acid/base titrimetric techniques for process monitoring; Descripcion e implementacion de tecnicas titrimetricas acido/base para la monitorizacion de procesos

    Energy Technology Data Exchange (ETDEWEB)

    Marcelino Represa, M.; Guisasola i Canudas, A.; Casa Alvero, C.; Lafuente Sancho, F. J.

    2006-07-01

    The basis of titrimetric techniques is that the proton production (or consumption) rate can be indirectly measured with the amount of base (or acid) dosage necessary to maintain the pH at a certain setpoint value. Titrimetric measurements are very useful for the monitoring of any process that influences pH with simple equipment (an accurate pH control loop). This work describes the theoretical basis of titrimetric measurements and shows three examples of the application of titrimetric techniques for the process monitoring: CO{sub 2} absorption, nitrification and biological organic matter removal. (Author)

  12. Copper nanoparticle modified carbon electrode for determination of dopamine

    International Nuclear Information System (INIS)

    Oztekin, Yasemin; Tok, Mutahire; Bilici, Esra; Mikoliunaite, Lina; Yazicigil, Zafer; Ramanaviciene, Almira; Ramanavicius, Arunas

    2012-01-01

    This paper reports the synthesis and characterization of copper nanoparticles (CuNPs) and application of copper nanoparticle-modified glassy carbon electrode for the electrochemical determination of dopamine. Electrochemical measurements were performed using differently modified glassy carbon (GC) electrodes. Bare, oxidized before modification and copper nanoparticle-modified glassy carbon electrodes (bare-GC, ox-GC and CuNP/GC electrodes, respectively) were characterized by cyclic voltammetry and electrochemical impedance spectroscopy in the presence of redox probes. Atomic force microscopy was used for the visualization of electrode surfaces. The CuNP/GC electrode was found to be suitable for the selective determination of dopamine even in the presence of ascorbic acid, uric acid, and p-acetamidophenol. The observed linear range of CuNP/GC for dopamine was from 0.1 nM to 1.0 μM while the detection limit was estimated to be 50 pM. It was demonstrated that here reported glassy carbon electrode modified by copper nanoparticles is suitable for the determination of dopamine in real samples such as human blood serum.

  13. Near infrared spectrometry for faecal fat measurement: comparison with conventional gravimetric and titrimetric methods.

    Science.gov (United States)

    Benini, L; Caliari, S; Guidi, G C; Vaona, B; Talamini, G; Vantini, I; Scuro, L A

    1989-01-01

    This investigation was aimed at comparing a new method for measuring faecal fat excretion, carried out with a semi-automated instrument by using near infrared analysis (NIRA), with the traditional titrimetric (Van de Kamer) and gravimetric (Sobel) methods. Near infrared analysis faecal fat was assayed on the three day stool collection from 118 patients (68 chronic pancreatitis, 19 organic diseases of the gastrointestinal tract, 19 alcoholic liver disease, 12 functional gastrointestinal disorders). A strict linear correlation was found between NIRA and both the titrimetric (r = 0.928, p less than 0.0001) and the gravimetric (r = 0.971, p less than 0.0001) methods. On homogenised faeces, a mean coefficient of variation of 2.1 (SD 1.71)% was found. Before homogenisation (where a mean coefficient of variation of 7% was found) accurate results were obtained when the mean of five measurements was considered. In conclusion, the assay of faecal fat excretion by the near infrared reflessometry appears a simple, rapid and reliable method for measuring steatorrhoea. PMID:2583563

  14. Quantitative Analysis of Tenofovir by Titrimetric, Extractive Ion-pair ...

    African Journals Online (AJOL)

    Methods: Tenofovir disoproxil forms a complex of 1:1 molar ratio with fumaric acid that was employed in its aqueous titration with sodium hydroxide. Non-aqueous titration was also employed for its determination. Extractive ion-pair spectrophotometric technique using methyl orange was similarly employed to evaluate ...

  15. Modified zirconium-eriochrome cyanine R determination of fluoride

    Science.gov (United States)

    Thatcher, L.L.

    1957-01-01

    The Eriochrome Cyanine R method for determining fluoride in natural water has been modified to provide a single, stable reagent solution, eliminate interference from oxidizing agents, extend the concentration range to 3 p.p.m., and extend the phosphate tolerance. Temperature effect was minimized; sulfate error was eliminated by precipitation. The procedure is sufficiently tolerant to interferences found in natural and polluted waters to permit the elimination of prior distillation for most samples. The method has been applied to 500 samples.

  16. Usage of Modified Heuristic Model for Determination of Software Stability

    Directory of Open Access Journals (Sweden)

    Sergey Konstantinovich Marfenko

    2013-02-01

    Full Text Available The subject of this paper is analysis method for determining the stability of software against the attacks on its integrity. It is suggested to use the modified heuristic model of software reliability as mathematic basis of this method. This model is based on classic approach, but it takes into account impact levels of different software errors on system integrity. It allows to define critical characteristics of software: percentage of time in stable working, the possibility of failure.

  17. Evaluation and comparison of two complexometric titration methods for determining of lanthanum in cloridric solutions

    International Nuclear Information System (INIS)

    Menezes, M.F.; Santos, R.L.C. dos; Goes, M.A.C. de

    1994-01-01

    The fast determination of total rare earth concentration in aqueous solutions is based on titrimetric methods using EDTA as complexing agent. This paper evaluates two among several others titrimetric methods used in the determination of lanthanum in hydrochloric acid solutions, using xylenol orange and a mixture of methyl orange and xylenol orange as indicators. The applied statistical evaluation allowed the determination of the stability, accuracy and adequacy of these methods on a given technical specification. (author). 12 refs., 03 tabs., 01 fig

  18. Using the modified sample entropy to detect determinism

    Energy Technology Data Exchange (ETDEWEB)

    Xie Hongbo, E-mail: xiehb@sjtu.or [Department of Health Technology and Informatics, The Hong Kong Polytechnic University, Hung Hom, Kowloon (Hong Kong); Department of Biomedical Engineering, Jiangsu University, Zhenjiang (China); Guo Jingyi [Department of Health Technology and Informatics, Hong Kong Polytechnic University, Hung Hom, Kowloon (Hong Kong); Zheng Yongping, E-mail: ypzheng@ieee.or [Department of Health Technology and Informatics, Hong Kong Polytechnic University, Hung Hom, Kowloon (Hong Kong); Reseach Institute of Innovative Products and Technologies, Hong Kong Polytechnic University (Hong Kong)

    2010-08-23

    A modified sample entropy (mSampEn), based on the nonlinear continuous and convex function, has been proposed and proven to be superior to the standard sample entropy (SampEn) in several aspects. In this Letter, we empirically investigate the ability of the mSampEn statistic combined with surrogate data method to detect determinism. The effects of the datasets length and noise on the proposed method to differentiate between deterministic and stochastic dynamics are tested on several benchmark time series. The noise performance of the mSampEn statistic is also compared with the singular value decomposition (SVD) and symplectic geometry spectrum (SGS) based methods. The results indicate that the mSampEn statistic is a robust index for detecting determinism in short and noisy time series.

  19. Determination of the composition of surface optical layers prepared with the use of rare earth and zirconium oxides

    International Nuclear Information System (INIS)

    Mishchenko, V.T.; Shilova, L.P.; Shkol'nikova, T.M.

    1991-01-01

    Simple titrimetric and gravimetric methods for determination of optical oxide layers (rare earth and zirconium oxides), sputtered on glass or quartz sublayer, have been developed. The minimal determined oxide mass in surface layers is equal to 0.01 mg in titrimetric determination and 0.1 mg - in gravimetric one. It is shown that composition of films and pellets, used for film sputtering, is identical

  20. Colorimetric determination of neomycin using melamine modified gold nanoparticles

    International Nuclear Information System (INIS)

    Xiao, Can; Liu, Junfeng; Yang, Ankang; Zhao, Hong; He, Yujian; Li, Xiangjun; Yuan, Zhuobin

    2015-01-01

    The colorimetric assay for neomycin presented here is based on melamine-modified gold nanoparticles (mel-AuNPs) and the finding that hydrogen bonding between melamine and neomycin results in the aggregation of mel-AuNPs. This results in a change in the color of the solution from wine red to blue and in a red-shift of the absorption maximum of the mel-AuNPs. The concentration of neomycin can be determined by spectrophotometry. The ratio of absorptions at 680 nm and 520 nm is linearly related to the logarithm of the concentration of neomycin in the 0.1 to 5.0 nM range and in the 5 to 100 nM range, with regression coefficients of 0.997 and 0.999, respectively. The detection limit (at an S/N ratio of 3) is 30 pM. This is far below the usual safety limit. The method was applied to the detection of trace levels of neomycin in milk samples and gave recoveries between 98 and 105 %. (author)

  1. Potentiometric end point detection in the EDTA titrimetric determination of gallium

    International Nuclear Information System (INIS)

    Gopinath, N.; Renuka, M.; Aggarwal, S.K.

    2001-01-01

    Gallium is titrated in presence of known amount of Fe (III) with EDTA in HNO 3 solution at pH 2 to 3. The end point is detected potentiometrically employing a bright platinum wire - saturated calomel (SCE) reference electrode system, the redox couple being Fe (III) / Fe (II). Since Fe (III) is also titrated by EDTA, it is, therefore, subtracted from titre value to get the EDTA equivalent to gallium only. Precision and accuracy 0.2 to 0.4% was obtained in the results of gallium in the range of 8 to 2 mg. (author)

  2. Electrochemical determination of mesotrione at organoclay modified glassy carbon electrodes.

    Science.gov (United States)

    Kamga Wagheu, Josephine; Forano, Claude; Besse-Hoggan, Pascale; Tonle, Ignas K; Ngameni, Emmanuel; Mousty, Christine

    2013-01-15

    A natural Cameroonian smectite-type clay (SaNa) was exchanged with cationic surfactants, namely cetyltrimethylammonium (CTA) and didodecyldimethyl ammonium (DDA) modifying its physico-chemical properties. The resulting organoclays that have higher adsorption capacity for mesotrione than the pristine SaNa clay, have been used as modifiers of glassy carbon electrode for the electrochemical detection of this herbicide by square wave voltammetry. The stripping performances of SaNa, SaCTA and SaDDA modified electrodes were therefore evaluated and the experimental parameters were optimized. SaDDA gives the best results in deoxygenated acetate buffer solution (pH 6.0) after 2 min accumulation under open circuit conditions. Under optimal conditions, the reduction current is proportional to mesotrione concentration in the range from 0.25 to 2.5 μM with a detection limit of 0.26 μM. The fabricated electrode was also applied for the commercial formulation CALLISTO, used in European maize market. Copyright © 2012 Elsevier B.V. All rights reserved.

  3. Modified loss coefficients in the determination of optimum generation scheduling

    Energy Technology Data Exchange (ETDEWEB)

    Hazarika, D.; Bordoloi, P.K. (Assam Engineering Coll. (IN))

    1991-03-01

    A modified method has been evolved to form the loss coefficients of an electrical power system network by decoupling load and generation and thereby creating additional fictitious load buses. The system losses are then calculated and co-ordinated to arrive at an optimum scheduling of generation using the standard co-ordination equation. The method presented is superior to the ones currently available, in that it is applicable to a multimachine system with random variation of load and it accounts for limits in plant generations and line losses. The precise nature of results and the economy in the cost of energy production obtained by this method is quantified and presented. (author).

  4. Determinants of public attitudes to genetically modified salmon.

    Directory of Open Access Journals (Sweden)

    Latifah Amin

    Full Text Available The objective of this paper is to assess the attitude of Malaysian stakeholders to genetically modified (GM salmon and to identify the factors that influence their acceptance of GM salmon using a structural equation model. A survey was carried out on 434 representatives from various stakeholder groups in the Klang Valley region of Malaysia. Public attitude towards GM salmon was measured using self-developed questionnaires with seven-point Likert scales. The findings of this study have confirmed that public attitudes towards GM salmon is a complex issue and should be seen as a multi-faceted process. The most important direct predictors for the encouragement of GM salmon are the specific application-linked perceptions about religious acceptability of GM salmon followed by perceived risks and benefits, familiarity, and general promise of modern biotechnology. Encouragement of GM salmon also involves the interplay among other factors such as general concerns of biotechnology, threatening the natural order of things, the need for labeling, the need for patenting, confidence in regulation, and societal values. The research findings can serve as a database that will be useful for understanding the social construct of public attitude towards GM foods in a developing country.

  5. Modified use of Van de Meer method for luminosity determination

    International Nuclear Information System (INIS)

    Palmer, R.B.

    1975-01-01

    Modifications are suggested which should improve the accuracy of the Van de Meer method of determining beam luminosity at the CERN ISR. Four bending magnets would be inserted between the quadrupoles of a given experimental straight section, connected in series, and shimmed so that the machine parameters are not affected. The magnets would be driven with a zigzag current power supply with a uniform rate of current change. Experiments requiring accurate luminosity determination would be run while the deflection magnets are being driven with the oscillatory current pattern. (U.S.)

  6. A modified method to determine biomass concentration as COD in ...

    African Journals Online (AJOL)

    drinie

    2002-10-04

    Oct 4, 2002 ... A modification of the standard VSS technique was also proposed using two membranes in the filtration device; this technique allowed the biomass determination in 1 μm size bacteria cultures that cannot be detected by the standard VSS method because cells are not retained by the 1.5 μm diameter pore ...

  7. Hydrazine determination in presence of uranium by modified spectrophotometric method

    International Nuclear Information System (INIS)

    Velavendan, P.; Pandey, N.K.; Kamachi Mudali, U.; Natarajan, R.

    2011-01-01

    In the present work an indirect, sensitive and accurate method for the determination of hydrazine is described. The method is based on the formation of yellow coloured azine complex by post column derivatization of hydrazine with P-dimethylamino benzaldehyde. The formed yellow coloured complex is stable in acidic medium and has a maximum absorption at 460 nm. Interference due to uranium was studied and the method was applied for the determination of hydrazine in presence of uranium in aqueous stream of nuclear fuel reprocessing. A calibration graph was made for the concentration range of hydrazine from 0.05 ppm to 10 ppm with RSD 0.807% and correlation coefficient of 0.99996. (author)

  8. The Macdonald and Savage titrimetric procedure scaled down to 4 mg sized plutonium samples. P. 1

    International Nuclear Information System (INIS)

    Kuvik, V.; Lecouteux, C.; Doubek, N.; Ronesch, K.; Jammet, G.; Bagliano, G.; Deron, S.

    1992-01-01

    The original Macdonald and Savage amperometric method scaled down to milligram-sized plutonium samples was further modified. The electro-chemical process of each redox step and the end-point of the final titration were monitored potentiometrically. The method is designed to determine 4 mg of plutonium dissolved in nitric acid solution. It is suitable for the direct determination of plutonium in non-irradiated fuel with a uranium-to-plutonium ratio of up to 30. The precision and accuracy are ca. 0.05-0.1% (relative standard deviation). Although the procedure is very selective, the following species interfere: vanadyl(IV) and vanadate (almost quantitatively), neptunium (one electron exchange per mole), nitrites, fluorosilicates (milligram amounts yield a slight bias) and iodates. (author). 15 refs.; 8 figs.; 7 tabs

  9. Determination of hydrogen permeability in commercial and modified superalloys

    Science.gov (United States)

    Bhattacharyya, S.; Peterman, W.

    1983-01-01

    The results of hydrogen permeability measurements on several iron- and cobalt-base alloys as well as on two long-ranged ordered alloys over the range of 705 to 870 C (1300 to 1600 F) are summarized. The test alloys included wrought alloys N-155, IN 800, A-286, 19-9DL, and 19-9DL modifications with aluminum, niobium, and misch metal. In addition, XF-818, CRM-6D, SA-F11, and HS-31 were evaluated. Two wrought long-range ordered alloys, Ni3Al and (Fe,Ni)3(V,Al) were also evaluated. All tests were conducted at 20.7 MPa pressure in either pure and/or 1% CO2-doped H2 for test periods as long as 133 h. Detailed analyses were conducted to determine the relative permeability rankings of these alloys and the effect of doping, exit surface oxidation, specimen design variations, and test duration on permeability coefficient, and permeation activation energies were determined. The two long-range ordered alloys had the lowest permeability coefficients in pure H2 when compared with the eight commercial alloys and their modifications. With CO2 doping, significant decrease in permeability was observed in commercial alloys--no doped tests were conducted with the long-range ordered alloys.

  10. Electrochemical determination of xanthine oxidase inhibitor drug in urate lowering therapy using graphene nanosheets modified electrode

    International Nuclear Information System (INIS)

    Raj, M. Amal; John, S. Abraham

    2014-01-01

    We report the electrochemical determination of urate lowering therapeutic drug, allopurinol (AP) using the electrochemically reduced graphene oxide (ERGO) modified glassy carbon electrode (GCE). The ERGO modified GCE was fabricated by self–assembling graphene oxide (GO) on 1,6-hexadiamine (HDA) modified GCE by the electrostatic interaction between the positively charged amine group and the negatively charged GO layers followed by the electrochemical reduction of GO layers at negative potential. XPS results confirmed the attachment of GO and its electrochemical reduction. The electrochemical behavior of AP was examined at ERGO modified electrode in the presence of ascorbic acid (AA) and uric acid (UA). It was found that ERGO modified electrode not only enhanced the oxidation currents of AP, AA and UA but also showed stable signals for them for repetitive potential cycles. The present modified electrode was successfully used to determine these analytes simultaneously in a mixture. Selective determination of AP in the presence of high concentrations of AA and UA was also demonstrated at ERGO modified GCE. Using amperometry, detections of 40 and 200 nM of UA and AP were achieved and the detection limits were found to be 9.0 × 10 −9 M and 1.1 × 10 −7 M, respectively (S/N = 3). Further, the practical application of the present modified electrode was demonstrated by simultaneously determining the concentrations of AA, UA and AP in human blood serum and urine samples

  11. Copy number determination of genetically-modified hematopoietic stem cells.

    Science.gov (United States)

    Schuesler, Todd; Reeves, Lilith; Kalle, Christof von; Grassman, Elke

    2009-01-01

    Human gene transfer with gammaretroviral, murine leukemia virus (MLV) based vectors has been shown to effectively insert and express transgene sequences at a level of therapeutic benefit. However, there are numerous reports of disruption of the normal cellular processes caused by the viral insertion, even of replication deficient gammaretroviral vectors. Current gammaretroviral and lentiviral vectors do not control the site of insertion into the genome, hence, the possibility of disruption of the target cell genome. Risk related to viral insertions is linked to the number of insertions of the transgene into the cellular DNA, as has been demonstrated for replication competent and replication deficient retroviruses in experiments. At high number of insertions per cell, cell transformation due to vector induced activation of proto-oncogenes is more likely to occur, in particular since more than one transforming event is needed for oncogenesis. Thus, determination of the vector copy number in bulk transduced populations, individual colony forming units, and tissue from the recipient of the transduced cells is an increasingly important safety assay and has become a standard, though not straightforward assay, since the inception of quantitative PCR.

  12. Electrochemical determination of ascorbic acid at p-phenylenediamine film-holes modified glassy carbon electrode

    Directory of Open Access Journals (Sweden)

    Olana Bikila Nagasa

    2015-01-01

    Full Text Available In this work the determination of ascorbic acid (AA at glassy carbon electrode (GCE modified with a perforated film produced by reduction of diazonium generated in situ from p-phenylenediamine (PD is reported. Holes were intentionally created in the modifier film by stripping a pre-deposited gold nanoparticles. The modified electrodes were electrochemically characterized by common redox probes: hydroquinone, ferrocyanide and hexamineruthenium(III. The cyclic voltammetric and amperometric response of AA using the modified electrodes was compared with that of bare GCE. The bare GCE showed a linear response to AA in the concentration range of 5 mM to 45 mM with detection limit of 1.656 mM and the modified GCE showed a linear response to AA in the concentration range of 5 μM to 45 μM with detection limit of 0.123 μM. The effect of potential intereferents on amperometric signal of AA at the modified GCE was examined and found to be minimal. The inter-electrode reproducibility, stability, and accuracy were determined. The modified electrode showed excellent inter-electrode reproducibility, accuracy and stability. The modified electrode reported is a promising candidate for use in electroanalysis of AA.

  13. Determination of Radiographic Healing: An Assessment of Consistency Using RUST and Modified RUST in Metadiaphyseal Fractures.

    Science.gov (United States)

    Litrenta, Jody; Tornetta, Paul; Mehta, Samir; Jones, Clifford; OʼToole, Robert V; Bhandari, Mohit; Kottmeier, Stephen; Ostrum, Robert; Egol, Kenneth; Ricci, William; Schemitsch, Emil; Horwitz, Daniel

    2015-11-01

    To determine the reliability of the Radiographic Union Scale for Tibia (RUST) score and a new modified RUST score in quantifying healing and to define a value for radiographic union in a large series of metadiaphyseal fractures treated with plates or intramedullary nails. Healing was evaluated using 2 methods: (1) evaluation of interrater agreement in a series of radiographs and (2) analysis of prospectively gathered data from 2 previous large multicenter trials to define thresholds for radiographic union. Part 1: 12 orthopedic trauma surgeons evaluated a series of radiographs of 27 distal femur fractures treated with either plate or retrograde nail fixation at various stages of healing in random order using a modified RUST score. For each radiographic set, the reviewer indicated if the fracture was radiographically healed. Part 2: The radiographic results of 2 multicenter randomized trials comparing plate versus nail fixation of 81 distal femur and 46 proximal tibia fractures were reviewed. Orthopaedic surgeons at 24 trauma centers scored radiographs at 3, 6, and 12 months postoperatively using the modified RUST score above. Additionally, investigators indicated if the fracture was healed or not healed. The intraclass correlation coefficient (ICC) with 95% confidence intervals was determined for each cortex, the standard and modified RUST score, and the assignment of union for part 1 data. The RUST and modified RUST that defined "union" were determined for both parts of the study. ICC: The modified RUST score demonstrated slightly higher ICCs than the standard RUST (0.68 vs. 0.63). Nails had substantial agreement, whereas plates had moderate agreement using both modified and standard RUST (0.74 and 0.67 vs. 0.59 and 0.53). The average standard and modified RUST at union among all fractures was 8.5 and 11.4. Nails had higher standard and modified RUST scores than plates at union. The ICC for union was 0.53 (nails: 0.58; plates: 0.51), which indicates moderate

  14. A Palladium-Tin Modified Microband Electrode Array for Nitrate Determination

    Directory of Open Access Journals (Sweden)

    Yexiang Fu

    2015-09-01

    Full Text Available A microband electrode array modified with palladium-tin bimetallic composite has been developed for nitrate determination. The microband electrode array was fabricated by Micro Electro-Mechanical System (MEMS technique. Palladium and tin were electrodeposited successively on the electrode, forming a double-layer structure. The effect of the Pd-Sn composite was investigated and its enhancement of catalytic activity and lifetime was revealed. The Pd-Sn modified electrode showed good linearity (R2 = 0.998 from 1 mg/L to 20 mg/L for nitrate determination with a sensitivity of 398 μA/(mg∙L−1∙cm2. The electrode exhibited a satisfying analytical performance after 60 days of storage, indicating a long lifetime. Good repeatability was also displayed by the Pd-Sn modified electrodes. The results provided an option for nitrate determination in water.

  15. Bismuth Modified Carbon-Based Electrodes for the Determination of Selected Neonicotinoid Insecticides

    Directory of Open Access Journals (Sweden)

    Marko Rodić

    2011-05-01

    Full Text Available Two types of bismuth modified electrodes, a bismuth-film modified glassy carbon (BiF-GCE and a bismuth bulk modified carbon paste, were applied for the determination of selected nitroguanidine neonicotinoid insecticides. The method based on an ex situ prepared BiF-GCE operated in the differential pulse voltammetric (DPV mode was applied to determine clothianidin in the concentration range from 2.5 to 23 μg cm−3 with a relative standard deviation (RSD not exceeding 1.5%. The tricresyl phosphate-based carbon paste electrodes (TCP-CPEs, bulk modified with 5 and 20 w/w% of bismuth, showed a different analytical performance in the determination of imidacloprid, regarding the peak shape, potential window, and noise level. The TCP-CPE with 5% Bi was advantageous, and the developed DPV method based on it allowed the determination in the concentration range from 1.7 to 60 μg cm−3 with an RSD of 2.4%. To get a deeper insight into the morphology of the bismuth-based sensor surfaces, scanning electron microscopic measurements were performed of both the surface film and the bulk modified electrodes.

  16. Schiff Base modified on CPE electrode and PCB gold electrode for selective determination of silver ion

    Science.gov (United States)

    Leepheng, Piyawan; Suramitr, Songwut; Phromyothin, Darinee

    2017-09-01

    The schiff base was synthesized by 2,5-thiophenedicarboxaldehyde and 1,2,4-thiadiazole-3,5-diamine with condensation method. There was modified on carbon paste electrode (CPE) and Printed circuit board (PCB) gold electrode for determination silver ion. The schiff base modified electrodes was characterized by atomic force microscopy (AFM) and scanning electron microscopy (SEM), respectively. The electrochemical study was reported by cyclic voltammetry method and impedance spectroscopy using modified electrode as working electrode, platinum wire and Ag/AgCl as counter electrode and reference electrode, respectively. The modified electrodes have suitable detection for Ag+. The determination of silver ions using the modified electrodes depended linearly on Ag+ concentration in the range 1×10-10 M to 1×10-7 M, with cyclic voltammetry sensitivity were 2.51×108 μAM-1 and 1.88×108 μAM-1 for PCB gold electrode and CPE electrode, respectively, limits of detection were 5.33×10-9 M and 1.99×10-8 M for PCB gold electrode and CPE electrode, respectively. The modified electrodes have high accuracy, inexpensive and can applied to detection Ag+ in real samples.

  17. Modified glassy carbon electrodes based on carbon nanostructures for ultrasensitive electrochemical determination of furazolidone

    Energy Technology Data Exchange (ETDEWEB)

    Shahrokhian, Saeed, E-mail: shahrokhian@sharif.edu [Department of Chemistry, Sharif University of Technology, Tehran 11155-9516 (Iran, Islamic Republic of); Institute for Nanoscience and Nanotechnology, Sharif University of Technology, Tehran (Iran, Islamic Republic of); Naderi, Leila [Department of Chemistry, Sharif University of Technology, Tehran 11155-9516 (Iran, Islamic Republic of); Ghalkhani, Masoumeh [Department of Chemistry, Faculty of Science, Shahid Rajaee Teacher Training University, Lavizan, Tehran (Iran, Islamic Republic of); Institute for advanced technology, Shahid Rajaee Teacher Training University, Lavizan, Tehran, 16788 (Iran, Islamic Republic of)

    2016-04-01

    The electrochemical behavior of Furazolidone (Fu) was investigated on the surface of the glassy carbon electrode modified with different carbon nanomaterials, including carbon nanotubes (CNTs), carbon nanoparticles (CNPs), nanodiamond-graphite (NDG), graphene oxide (GO), reduced graphene oxide (RGO) and RGO-CNT hybrids (various ratios) using linear sweep voltammetry (LSV). The results of voltammetric studies exhibited a considerable increase in the cathodic peak current of Fu at the RGO modified GCE, compared to other modified electrodes and also bare GCE. The surface morphology and nature of the RGO film was thoroughly characterized by scanning electron microscopy (SEM), atomic force microscopy (AFM), electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV) techniques. The modified electrode showed two linear dynamic ranges of 0.001–2.0 μM and 2.0–10.0 μM with a detection limit of 0.3 nM for the voltammetric determination of Fu. This sensor was used successfully for Fu determination in pharmaceutical and clinical preparations. - Highlights: • The electrochemical behavior of Furazolidone (Fu) was investigated on the surface of the modified electrode with different carbon nanomaterials by Linear sweep voltammetry. • Two linear dynamic ranges and a low detection limit were obtained. • The modified electrode was applied for the detection of Fu in pharmaceutical and clinical preparations.

  18. On Dirichlet-to-Neumann Maps and Some Applications to Modified Fredholm Determinants

    OpenAIRE

    Gesztesy, Fritz; Mitrea, Marius; Zinchenko, Maxim

    2010-01-01

    We consider Dirichlet-to-Neumann maps associated with (not necessarily self-adjoint) Schrodinger operators in $L^2(\\Omega; d^n x)$, $n=2,3$, where $\\Omega$ is an open set with a compact, nonempty boundary satisfying certain regularity conditions. As an application we describe a reduction of a certain ratio of modified Fredholm perturbation determinants associated with operators in $L^2(\\Omega; d^n x)$ to modified Fredholm perturbation determinants associated with operators in $L^2(\\partial\\Om...

  19. Chemical modifiers in electrothermal atomic absorption determination of Platinum and Palladium containing preparations in blood serum

    Directory of Open Access Journals (Sweden)

    Аntonina Alemasova

    2012-11-01

    Full Text Available The biological liquids matrixes influence on the characteristic masses and repeatability of Pt and Pd electrothermal atomic absorption spectroscopy (ETAAS determination was studied. The chemical modifiers dimethylglyoxime and ascorbic acid for matrix interferences elimination and ETAAS results repeatability improvement were proposed while bioliquids ETAAS analysis, and their action mechanism was discussed.

  20. Molecularly imprinted electrochemical sensor based on nickel nanoparticle-modified electrodes for phenobarbital determination

    International Nuclear Information System (INIS)

    Yu, Hui Cheng; Huang, Xue Yi; Lei, Fu Hou; Tan, Xue Cai; Wei, Yi Chun; Li, Hao

    2014-01-01

    Highlights: • Uniform Ni nanoparticles were synthesized. • A Ni nanoparticle-modified imprinted sensor was developed to detect phenobarbital. • The modified sensor exhibited high sensitivity for phenobarbital. • The electrochemical properties of the modified sensor were investigated. • The prepared sensor was applied to detect phenobarbital in fish samples. - Abstract: Uniform nickel nanoparticles were applied to improve the sensitivity of sensors for phenobarbital (PB) determination. A Ni nanoparticle-modified imprinted electrochemical sensor was developed by thermal polymerization with the use of methacrylic acid as the functional monomer and ethylene glycol maleic rosinate acrylate as the crosslinking agent. The chemical structures and morphologies of the imprinted films were characterized using Fourier transform infrared spectroscopy and scanning electron microscopy. The success of the fabrication of Ni nanoparticles, as well as the Ni nanoparticle-modified imprinted electrochemical sensor, was confirmed by the analytical results. The electrochemical properties of the modified molecularly imprinted and non-imprinted polymer sensors were investigated by cyclic voltammetry, differential pulse voltammetry, electrochemical impedance spectroscopy, and chronoamperometry. Results showed that the electrochemical properties of the molecularly imprinted sensor were remarkably different from those of the non-imprinted sensor. Linear responses of the imprinted sensor to PB were observed for concentrations ranging from 1.4 × 10 −7 mol L −1 to 1.3 × 10 −4 mol L −1 (r 2 = 0.9976), with a detection limit of 8.2 × 10 −9 mol L −1 (S/N = 3). The imprinted electrochemical sensor was used to determine PB in actual fish samples, in which average recoveries between 95.60% and 104.67% were achieved. The developed Ni nanoparticle-modified electrochemical sensor exhibited high sensitivity, high selectivity, and good recovery

  1. Electrochemical Determination of Caffeine Content in Ethiopian Coffee Samples Using Lignin Modified Glassy Carbon Electrode

    OpenAIRE

    Amare, Meareg; Aklog, Senait

    2017-01-01

    Lignin film was deposited at the surface of glassy carbon electrode potentiostatically. In contrast to the unmodified glassy carbon electrode, an oxidative peak with an improved current and overpotential for caffeine at modified electrode showed catalytic activity of the modifier towards oxidation of caffeine. Linear dependence of peak current on caffeine concentration in the range 6 ? 10?6 to 100 ? 10?6?mol?L?1 with determination coefficient and method detection limit (LoD = 3?s/slope) of 0....

  2. Direct determination of creatinine based on poly(ethyleneimine)/phosphotungstic acid multilayer modified electrode.

    Science.gov (United States)

    Han, Ping; Xu, Shimei; Feng, Shun; Hao, Yanjun; Wang, Jide

    2016-05-01

    In this work, the direct determination of creatinine was achieved using a poly(ethyleneimine)/phosphotungstic acid multilayer modified electrode with the assistance of Copper(II) ions by cyclic voltammetry. The quantity of creatinine were determined by measuring the redox peak current of Cu(II)-creatinine complex/Cu(I)-creatinine complex. Factors affecting the response current of creatinine at the modified electrode were optimized. A linear relationship between the response current and the concentration of creatinine ranging from 0.125 to 62.5μM was obtained with a detection limit of 0.06μM. The proposed method was applied to determine creatinine in human urine, and satisfied results were gotten which was validated in accordance with high performance liquid chromatography. The proposed electrode provided a promising alternative in routine sensing for creatinine without enzymatic assistance. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. Determination of drug lipophilicity by phosphatidylcholine-modified microemulsion high-performance liquid chromatography.

    Science.gov (United States)

    Xuan, Xueyi; Xu, Liyuan; Li, Liangxing; Gao, Chongkai; Li, Ning

    2015-07-25

    A new biomembrane-mimetic liquid chromatographic method using a C8 stationary phase and phosphatidylcholine-modified (PC-modified) microemulsion mobile phase was used to estimate unionized and ionized drugs lipophilicity expressed as an n-octanol/water partition coefficient (logP and logD). The introduction of PC into sodium dodecyl sulfate (SDS) microemulsion yielded a good correlation between logk and logD (R(2)=0.8). The optimal composition of the PC-modified microemulsion liquid chromatography (PC-modified MELC) mobile phase was 0.2% PC-3.0% SDS-6.0% n-butanol-0.8% ethyl acetate-90.0% water (pH 7.0) for neutral and ionized molecules. The interactions between the analytes and system described by this chromatographic method is more similar to biological membrane than the n-octanol/water partition system. The result in this paper suggests that PC-modified MELC can serve as a possible alternative to the shake-flask method for high-throughput unionized and ionized drugs lipophilicity determination and simulation of biological processes. Copyright © 2015 Elsevier B.V. All rights reserved.

  4. Matrix modifiers application during microimpurities determination in complex samples by electrothermal atomic-absorption spectrometry

    International Nuclear Information System (INIS)

    Bejzel', N.F.; Daaman, F.I.; Fuks-Pol', G.R.; Yudelevich, I.G.

    1993-01-01

    The review covers publications of primarily last 5 years and is devoted to the use of matrix modifiers (MM) for the determinations of trace impurities in complex samples by electrothermal atomic-absorption analysis. The role of MM in analytical process has been discussed as well as MM influence on all the elements of analytical system; factors, determining the effectiveness of MM action, the basis types of MM have been described. A great body of information is tabulated on the use of different MM for the determination of particular analysis in geological, medicobiological, technological, ecological samples and in pure materials and chemicals

  5. Modified glassy carbon electrodes based on carbon nanostructures for ultrasensitive electrochemical determination of furazolidone.

    Science.gov (United States)

    Shahrokhian, Saeed; Naderi, Leila; Ghalkhani, Masoumeh

    2016-04-01

    The electrochemical behavior of Furazolidone (Fu) was investigated on the surface of the glassy carbon electrode modified with different carbon nanomaterials, including carbon nanotubes (CNTs), carbon nanoparticles (CNPs), nanodiamond-graphite (NDG), graphene oxide (GO), reduced graphene oxide (RGO) and RGO-CNT hybrids (various ratios) using linear sweep voltammetry (LSV). The results of voltammetric studies exhibited a considerable increase in the cathodic peak current of Fu at the RGO modified GCE, compared to other modified electrodes and also bare GCE. The surface morphology and nature of the RGO film was thoroughly characterized by scanning electron microscopy (SEM), atomic force microscopy (AFM), electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV) techniques. The modified electrode showed two linear dynamic ranges of 0.001-2.0 μM and 2.0-10.0 μM with a detection limit of 0.3 nM for the voltammetric determination of Fu. This sensor was used successfully for Fu determination in pharmaceutical and clinical preparations. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Application of graphene oxide/lanthanum-modified carbon paste electrode for the selective determination of dopamine

    Energy Technology Data Exchange (ETDEWEB)

    Ye, Fengying; Feng, Chenqi; Fu, Ning; Wu, Huihui; Jiang, Jibo, E-mail: jibojiang0506@163.com; Han, Sheng, E-mail: hansheng654321@sina.com

    2015-12-01

    Highlights: • The effective surface area of the modified CPE has been expanded after self-assembly. • The GO–La composite exhibited excellent electrocatalytic activity toward DA. • The GO–La/CPE presented high selectivity, sensitivity, excellent stability and repeatability. - Abstract: A home-made carbon paste electrode (CPE) was reformed by graphene oxide (GO)/lanthanum (La) complexes, and a modified electrode, called GO–La/CPE, was fabricated for the selective determination of dopamine (DA) by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). Several factors affecting the electrocatalytic performance of the modified sensor were investigated. Owning to the combination of GO and La ions, the GO–La/CPE sensor exhibited large surface area, well selectivity, good repeatability and stability in the oxidation reaction of DA. At optimal conditions, the response of the GO–La/CPE electrode for determining DA was linear in the region of 0.01–0.1 μM and 0.1–400.0 μM. The limit of detection was down to 0.32 nM (S/N = 3). In addition, this modified electrode was successfully applied to the detection of DA in real urine and serum samples by using standard adding method, showing its promising application in the electroanalysis of real samples.

  7. Simultaneous voltammetric determination of tramadol and acetaminophen using carbon nanoparticles modified glassy carbon electrode

    International Nuclear Information System (INIS)

    Ghorbani-Bidkorbeh, Fatemeh; Shahrokhian, Saeed; Mohammadi, Ali; Dinarvand, Rassoul

    2010-01-01

    A sensitive and selective electrochemical sensor was fabricated via the drop-casting of carbon nanoparticles (CNPs) suspension onto a glassy carbon electrode (GCE). The application of this sensor was investigated in simultaneous determination of acetaminophen (ACE) and tramadol (TRA) drugs in pharmaceutical dosage form and ACE determination in human plasma. In order to study the electrochemical behaviors of the drugs, cyclic and differential pulse voltammetric studies of ACE and TRA were carried out at the surfaces of the modified GCE (MGCE) and the bare GCE. The dependence of peak currents and potentials on pH, concentration and the potential scan rate were investigated for these compounds at the surface of MGCE. Atomic force microscopy (AFM) was used for the characterization of the film modifier and its morphology on the surface of GCE. The results of the electrochemical investigations showed that CNPs, via a thin layer model based on the diffusion within a porous layer, enhanced the electroactive surface area and caused a remarkable increase in the peak currents. The thin layer of the modifier showed a catalytic effect and accelerated the rate of the electron transfer process. Application of the MGCE resulted in a sensitivity enhancement and a considerable decrease in the anodic overpotential, leading to negative shifts in peak potentials. An optimum electrochemical response was obtained for the sensor in the buffered solution of pH 7.0 and using 2 μL CNPs suspension cast on the surface of GCE. Using differential pulse voltammetry, the prepared sensor showed good sensitivity and selectivity for the determination of ACE and TRA in wide linear ranges of 0.1-100 and 10-1000 μM, respectively. The resulted detection limits for ACE and TRA was 0.05 and 1 μM, respectively. The CNPs modified GCE was successfully applied for ACE and TRA determinations in pharmaceutical dosage forms and also for the determination of ACE in human plasma.

  8. Determination of vanadium in mussels by electrothermal atomic absorption spectrometry without chemical modifiers

    Energy Technology Data Exchange (ETDEWEB)

    Saavedra, Y.; Fernandez, P. [Centro de Control do Medio Marino, Peirao de Vilaxoan s/n, Vilagarcia de Arousa, 36611 Pontevedra (Spain); Gonzalez, A. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Quimica, 15706, Santiago de Compostela (Spain)

    2004-05-01

    A method was developed for the quantitative determination of total vanadium concentration in mussels via electrothermal atomic absorption spectrometry (ETAAS). After the microwave digestion of the samples, a program using temperatures of 1600 C and 2600 C for ashing and atomization respectively, without any matrix modifiers, allowed us to obtain results that were satisfactory since they agreed closely with certified reference material values. The detection limit was 0.03 mg kg{sup -1} (dry weight), indicating that the method is suitable for the analysis of mussel samples. This determination was compared with matrix modifiers that have been reported previously. The method was applied to various cultivated and wild mussels from the Galician coast, yielding levels below 1 mg kg{sup -1} (wet weight). (orig.)

  9. Poly(amidosulfonic acid) modified glassy carbon electrode for determination of isoniazid in pharmaceuticals.

    Science.gov (United States)

    Yang, Gongjun; Wang, Cunxiao; Zhang, Rui; Wang, Chenying; Qu, Qishu; Hu, Xiaoya

    2008-06-01

    Amidosulfonic acid was electropolymerized by cyclic voltammetry onto the surface of glassy carbon electrode (GCE) to fabricate the chemically modified electrode, which showed high stability, good selectivity and reproducibility for determination of isoniazid. The modified electrode showed an excellent electrocatalytical effect on the oxidation of isoniazid. Under the optimum conditions, there was a good linear relationship between anodic peak current and isoniazid concentration in the range of 5.0 x 10(-8)- 1.0 x 10(-5) M, and a detection limit of 1.0 x 10(-8) M (S/N = 3) was obtained after 120 s at the accumulation potential of - 0.2 V (vs. SCE). This developed method had been applied to the direct determination of isoniazid in injection and tablet samples with satisfactory results.

  10. Sensitive determination of buformin using poly-aminobenzoic acid modified glassy carbon electrode

    Directory of Open Access Journals (Sweden)

    Gui-Ying Jin

    2012-12-01

    Full Text Available Glassy carbon electrode, which is used to electrochemically determine the content of buformin, is modified with an electropolymerized film of p-aminobenzoic acid in pH 7.0 acetate buffer solution (ABS. The polymer showed an excellent electrocatalytic activity for the reduction of buformin. In pH 7.0 ABS, the cathodic peak current increased linearly over three concentration intervals of buformin, and the detection limit (S/N=3 was 2.0×10−9 g/mL. The method was successfully applied to directly determine buformin in tablets with standard addition recoveries of 95.8–102.5%. The proposed method is simple, cheap and highly efficient. Keywords: Chemically modified electrode, Aminobenzoic acid, Buformin

  11. Determination of minimum impact parameter by modified touching spheres schemes for intermediate energy Coulomb excitation experiments

    International Nuclear Information System (INIS)

    Kumar, Rajiv; Sharma, Shagun; Singh, Pradeep; Kharab, Rajesh

    2016-01-01

    The energy-independent touching spheres schemes commonly used for the determination of the safe minimum value of the impact parameter for Coulomb excitation experiments are modified through the inclusion of an energy-dependent term. The touching spheres+3fm scheme after modification emerges out to be the best one while touching spheres+4fm scheme is found to be better in its unmodified form. (orig.)

  12. Simultaneous determination of hydroquinone and catechol at gold nanoparticles mesoporous silica modified carbon paste electrode

    Energy Technology Data Exchange (ETDEWEB)

    Tashkhourian, J., E-mail: tashkhourian@susc.ac.ir [Department of Chemistry, College of Sciences, Shiraz University, Shiraz 71456 (Iran, Islamic Republic of); Daneshi, M.; Nami-Ana, F. [Department of Chemistry, College of Sciences, Shiraz University, Shiraz 71456 (Iran, Islamic Republic of); Behbahani, M.; Bagheri, A. [Department of Chemistry, Shahid Beheshti University, G.C., Evin, Tehran (Iran, Islamic Republic of)

    2016-11-15

    Highlights: • An electrochemical sensor based on gold nanoparticles mesoporous silica modified carbon paste electrode was developed. • The electrode provides an accessible surface for simultaneous determination of hydroquinone and catechol. • Hydroquinone and catechol are highly toxic to both environment and human even at very low concentrations. - Abstract: A new electrochemical sensor based on gold nanoparticles mesoporous silica modified carbon paste electrode (AuNPs-MPS) was developed for simultaneous determination of hydroquinone and catechol. Morphology and structure of the AuNPs-MPS were characterized by transmission electron microscopy, X-ray diffraction and Fourier transform infrared spectroscopy. The electrochemical behavior of hydroquinone and catechol were investigated using square wave voltammetry and the results indicate that the electrochemical responses are improved significantly at the modified electrode. The observed oxidative peaks separation of about 120 mV made possible the simultaneous determination of hydroquinone and catechol in their binary-mixture. Under the optimized condition, a linear dynamic range of 10.0 μM–1.0 mM range for hydroquinone with the detection limit of 1.2 μM and from 30.0 μM–1.0 mM for catechol with the detection limit of 1.1 μM were obtained. The applicability of the method was demonstrated by the recovery studies of hydroquinone and catechol in spiked tap water samples.

  13. A modified captive bubble method for determining advancing and receding contact angles

    International Nuclear Information System (INIS)

    Xue, Jian; Shi, Pan; Zhu, Lin; Ding, Jianfu; Chen, Qingmin; Wang, Qingjun

    2014-01-01

    Graphical abstract: - Highlights: • A modified captive bubble method for determining advancing and receding contact angle is proposed. • We have designed a pressure chamber with a pressure control system to the original experimental. • The modified method overcomes the deviation of the bubble in the traditional captive bubble method. • The modified captive bubble method allows a smaller error from the test. - Abstract: In this work, a modification to the captive bubble method was proposed to test the advancing and receding contact angle. This modification is done by adding a pressure chamber with a pressure control system to the original experimental system equipped with an optical angle mater equipped with a high speed CCD camera, a temperature control system and a computer. A series of samples with highly hydrophilic, hydrophilic, hydrophobic and superhydrophobic surfaces were prepared. The advancing and receding contact angles of these samples with highly hydrophilic, hydrophilic, and hydrophobic surfaces through the new methods was comparable to the result tested by the traditional sessile drop method. It is proved that this method overcomes the limitation of the traditional captive bubble method and the modified captive bubble method allows a smaller error from the test. However, due to the nature of the captive bubble technique, this method is also only suitable for testing the surface with advancing or receding contact angle below 130°

  14. A modified captive bubble method for determining advancing and receding contact angles

    Energy Technology Data Exchange (ETDEWEB)

    Xue, Jian; Shi, Pan; Zhu, Lin [Key Laboratory of High Performance Polymer Materials and Technology (Nanjing University), Ministry of Eduction, Nanjing 210093 (China); Ding, Jianfu [Security and Disruptive Technologies, National Research Council Canada, 1200 Montreal Road, Ottawa, K1A 0R6, Ontario (Canada); Chen, Qingmin [Key Laboratory of High Performance Polymer Materials and Technology (Nanjing University), Ministry of Eduction, Nanjing 210093 (China); Wang, Qingjun, E-mail: njuwqj@nju.edu.cn [Key Laboratory of High Performance Polymer Materials and Technology (Nanjing University), Ministry of Eduction, Nanjing 210093 (China)

    2014-03-01

    Graphical abstract: - Highlights: • A modified captive bubble method for determining advancing and receding contact angle is proposed. • We have designed a pressure chamber with a pressure control system to the original experimental. • The modified method overcomes the deviation of the bubble in the traditional captive bubble method. • The modified captive bubble method allows a smaller error from the test. - Abstract: In this work, a modification to the captive bubble method was proposed to test the advancing and receding contact angle. This modification is done by adding a pressure chamber with a pressure control system to the original experimental system equipped with an optical angle mater equipped with a high speed CCD camera, a temperature control system and a computer. A series of samples with highly hydrophilic, hydrophilic, hydrophobic and superhydrophobic surfaces were prepared. The advancing and receding contact angles of these samples with highly hydrophilic, hydrophilic, and hydrophobic surfaces through the new methods was comparable to the result tested by the traditional sessile drop method. It is proved that this method overcomes the limitation of the traditional captive bubble method and the modified captive bubble method allows a smaller error from the test. However, due to the nature of the captive bubble technique, this method is also only suitable for testing the surface with advancing or receding contact angle below 130°.

  15. [Evaluation of fetal lung maturity using a modified lecithin-sphingomyelin determination and Clements' foam test].

    Science.gov (United States)

    Neumann, G; Gartzke, J; Faber, G

    1978-01-01

    The modified thin layer chromatographic method for the determination of the phospholipids lecithin and sphingomyelin from amniotic fluid is useful in estimating fetal pulmonary maturity. The foam test of Clements is a simple rapid method for screening of suspicious cases of pregnancies at risk and of great value as bed side test even performing by the doctor. In comparing Clements-Test with thin layer chromatographic for L/S-Ratio determination we found a good correlation of 81,8% of all cases.

  16. Determination of Burst Pressure of API Steel Pipes using Stress Modified Critical Strain Model

    International Nuclear Information System (INIS)

    Alang, N A; Razak, N A; Sulaiman, A S

    2012-01-01

    This paper presents a technique which can be used to determine the burst pressure of defective steel pipes using non-linear finite element (FE) analysis. The technique uses stress modified critical strain (SMCS) failure criterion to study the effect of gouge defects on maximum working pressure of API X65 steel pipes. The procedures in determining the model parameters using 3-D, homogeneous isotropic elastic-plastic material model with large deformation finite element analyses from notched tensile bars were systematically discussed. The relationship between burst pressure and gouge depth was proposed. The burst pressure estimated then was compared to experimental data from the literature for validation showing overall good agreements.

  17. Modifiable determinants of serum 25-hydroxyvitamin D status in early childhood: opportunities for prevention.

    Science.gov (United States)

    Maguire, Jonathon L; Birken, Catherine S; Khovratovich, Marina; Degroot, Julie; Carsley, Sarah; Thorpe, Kevin E; Mamdani, Muhammad; Parkin, Patricia C

    2013-03-01

    OBJECTIVES To determine the effect of modifiable dietary intake variables (current vitamin D supplementation and daily cow's milk intake) on 25-hydroxyvitamin D level in early childhood and to evaluate the relationship between these modifiable dietary factors and other largely nonmodifiable determinants of vitamin D status including skin pigmentation and season. DESIGN Cross-sectional study. SETTING Primary care pediatric and family medicine practices participating in the TARGet Kids! practice-based research network in Toronto, Ontario, Canada. PARTICIPANTS From December 2008 to June 2011, healthy children 1 to 5 years of age were recruited during a routine physician's visit. INTERVENTIONS Survey, anthropometric measurements, and laboratory data were collected. A multivariable linear regression model was developed to examine the independent effects of vitamin D supplementation and daily volume of cow's milk on 25-hydroxyvitamin D level. MAIN OUTCOME MEASURES 25-Hydroxyvitamin D level. RESULTS Blood was obtained in 1898 children. Two modifiable dietary intake variables, vitamin D supplementation and cow's milk, increased 25-hydroxyvitamin D level by 3.4 ng/mL (95% CI, 2-4 ng/mL) and 1.6 ng/mL per 250-mL cup per day (95% CI, 1-2 ng/mL), respectively. Two nonmodifiable variables reflecting cutaneous vitamin D synthesis (skin pigmentation and season) were also strongly associated with 25-hydroxyvitamin D status but accounted for a much smaller proportion of the explained variation in 25-hydroxyvitamin D level. The effect of vitamin D supplementation and milk intake on 25-hydroxyvitamin D level appeared similar regardless of skin pigmentation or season. CONCLUSION Two modifiable dietary intake variables (vitamin D supplementation and cow's milk intake) are the most important determinants of 25-hydroxyvitamin D status in early childhood.

  18. Graphene-loaded nanofiber-modified electrodes for the ultrasensitive determination of dopamine

    Energy Technology Data Exchange (ETDEWEB)

    Rodthongkum, Nadnudda, E-mail: Nadnudda.R@chula.ac.th [Metallurgy and Materials Science Research Institute, Chulalongkorn University, Pathumwan, Bangkok 10330 (Thailand); Ruecha, Nipapan [Program in Macromolecular Science, Faculty of Science, Chulalongkorn University, Pathumwan, Bangkok 10330 (Thailand); Rangkupan, Ratthapol [Metallurgy and Materials Science Research Institute, Chulalongkorn University, Pathumwan, Bangkok 10330 (Thailand); Center of Innovative Nanotechnology, Chulalongkorn University, Pathumwan, Bangkok 10330 (Thailand); Vachet, Richard W. [Department of Chemistry, University of Massachusetts Amherst, Amherst, MA 01002 (United States); Chailapakul, Orawon, E-mail: corawon@chula.ac.th [Electrochemistry and Optical Spectroscopy Research Unit, Department of Chemistry, Faculty of Science, Chulalongkorn University, Pathumwan, Bangkok 10330 (Thailand)

    2013-12-04

    Graphical abstract: -- Highlights: •A novel electrode based on electrospun graphene/polyaniline/polystyrene nanofibers has been developed. •The proposed system provides ultrahigh sensitivity, good selectivity and wide linearity for the determination of dopamine. •This system was successfully applied to determine dopamine in complex biological environment with excellent reproducibility. -- Abstract: A novel and highly sensitive electrochemical system based on electrospun graphene/polyaniline/polystyrene (G/PANI/PS) nanofiber-modified screen-printed carbon electrodes has been developed for dopamine (DA) determination. A dramatic increase (9 times) in the current signal for the redox reaction of a standard, ferri/ferrocyanide [Fe(CN){sub 6}]{sup 3−/4−} couple was found when compared to an unmodified electrode. This modified electrode also exhibited favorable electron transfer kinetics and excellent electrocatalytic activity toward the oxidation of DA. When used together with square wave voltammetry (SWV), DA can be selectively determined in the presence of the common interferents (i.e. ascorbic acid and uric acid). Under optimal conditions, a very low limit of detection (0.05 nM) and limit of quantification (0.30 nM) were achieved for DA. In addition, a wide dynamic range of 0.1 nM to 100 μM was found for this electrode system. Finally, the system can be successfully applied to determine DA in complex biological environment (e.g. human serum, urine) with excellent reproducibility.

  19. Electrochemical sensor for ranitidine determination based on carbon paste electrode modified with oxovanadium (IV) salen complex.

    Science.gov (United States)

    Raymundo-Pereira, Paulo A; Teixeira, Marcos F S; Fatibello-Filho, Orlando; Dockal, Edward R; Bonifácio, Viviane Gomes; Marcolino, Luiz H

    2013-10-01

    The preparation and electrochemical characterization of a carbon paste electrode modified with the N,N-ethylene-bis(salicyllideneiminato)oxovanadium (IV) complex ([VO(salen)]) as well as its application for ranitidine determination are described. The electrochemical behavior of the modified electrode for the electroreduction of ranitidine was investigated using cyclic voltammetry, and analytical curves were obtained for ranitidine using linear sweep voltammetry (LSV) under optimized conditions. The best voltammetric response was obtained for an electrode composition of 20% (m/m) [VO(salen)] in the paste, 0.10 mol L(-1) of KCl solution (pH 5.5 adjusted with HCl) as supporting electrolyte and scan rate of 25 mV s(-1). A sensitive linear voltammetric response for ranitidine was obtained in the concentration range from 9.9×10(-5) to 1.0×10(-3) mol L(-1), with a detection limit of 6.6×10(-5) mol L(-1) using linear sweep voltammetry. These results demonstrated the viability of this modified electrode as a sensor for determination, quality control and routine analysis of ranitidine in pharmaceutical formulations. Copyright © 2013. Published by Elsevier B.V.

  20. Electrocatalytic Determination of Isoniazid by a Glassy Carbon Electrode Modified with Poly (Eriochrome Black T

    Directory of Open Access Journals (Sweden)

    Karim Asadpour-Zeynali

    2017-06-01

    Full Text Available In this work poly eriochrome black T (EBT was electrochemically synthesized on the glassy carbon electrode as electrode modifier. On the modified electrode, voltammetric behavior of isoniazid (INH was investigated. The poly (EBT-modified glassy carbon electrode has excellent electrocatalytic ability for the electrooxidation of isoniazid. This fact was appeared as a reduced overpotential of INH oxidation in a wide operational pH range from 2 to 13. It has been found that the catalytic peak current depends on the concentration of INH and solution pH. The number of electrons involved in the rate determining step was found 1. The diffusion coefficient of isoniazid was also estimated using chronoamperometry technique. The experimental results showed that the mediated oxidation peak current of isoniazid is linearly dependent on the concentration of isoniazid in the ranges of 8.0 × 10-6 – 1.18 × 10-3 M and 2.90 × 10-5 M – 1.67× 10-3 M with differential pulse voltammetry (DPV and amperometry methods, respectively. The detection limits (S/N = 3 were found to be 6.0 μM and 16.4 μM by DPV and amperometry methods, respectively. This developed method was applied to the determination of isoniazid in tablet samples with satisfactory results.

  1. Determination of uric acid in the presence of ascorbic acid with hexacyanoferrate lanthanum film modified electrode

    International Nuclear Information System (INIS)

    Wang Guangfeng; Meng Jian; Liu Hongying; Jiao Shoufeng; Zhang Wei; Chen Daolei; Fang Bin

    2008-01-01

    A glassy carbon electrode modified with LaHCF was constructed and was characterized by cyclic voltammetry (CV) and electrochemical impedance spectrum (EIS). The resulting LaHCF modified glassy carbon electrode had a good catalytic character on uric acid (UA) and was used to detect uric acid and ascorbic acid (AA) simultaneously. This modified electrode exhibits potent and persistent electron-mediating behavior followed by well-separated oxidation peaks towards UA and AA with activation overpotential. For UA and AA in mixture, one can well separate from the other with a potential large enough to allow the determination of one in presence of the other. The DPV peak currents obtained increased linearly on the UA in the range of 2.0 x 10 -7 to 1.0 x 10 -4 mol/L with the detection limit (signal-to-noise ratio was 3) for UA 1.0 x 10 -7 mol/L. The proposed method showed excellent selectivity and stability, and the determination of UA and AA simultaneously in urine was satisfactory

  2. Determination of Mercury (II Ion on Aryl Amide-Type Podand-Modified Glassy Carbon Electrode

    Directory of Open Access Journals (Sweden)

    Sevgi Güney

    2011-01-01

    Full Text Available A new voltammetric sensor based on an aryl amide type podand, 1,8-bis(o-amidophenoxy-3,6-dioxaoctane, (AAP modified glassy carbon electrode, was described for the determination of trace level of mercury (II ion by cyclic voltammetry (CV and differential pulse voltammetry (DPV. A well-defined anodic peak corresponding to the oxidation of mercury on proposed electrode was obtained at 0.2 V versus Ag/AgCl reference electrode. The effect of experimental parameters on differential voltammetric peak currents was investigated in acetate buffer solution of pH 7.0 containing 1 × 10−1 mol L−1 NaCl. Mercury (II ion was preconcentrated at the modified electrode by forming complex with AAP under proper conditions and then reduced on the surface of the electrode. Interferences of Cu2+, Pb2+, Fe3+, Cd2+, and Zn2+ ions were also studied at two different concentration ratios with respect to mercury (II ions. The modified electrode was applied to the determination of mercury (II ions in seawater sample.

  3. Electrochemical Determination of Uric Acid at CdTe Quantum Dot Modified Glassy Carbon Electrodes.

    Science.gov (United States)

    Pan, Deng; Rong, Shengzhong; Zhang, Guangteng; Zhang, Yannan; Zhou, Qiang; Liu, Fenghai; Li, Miaojing; Chang, Dong; Pan, Hongzhi

    2015-01-01

    Cyclic voltammetry and differential pulse voltammetry were used to investigate the electrochemical behavior of uric acid (UA) at a CdTe quantum dot (QD) modified the glassy carbon electrode (GCE). CdTe QDs, as new semiconductor nanocrystals, can greatly improve the peak current of UA. The anodic peak current of UA was linear with its concentration between 1.0×10(-6) and 4.0×10(-4) M in 0.1 M pH 5.0 phosphate buffer solution. The LOD for UA at the CdTe electrode (1.0×10(-7) M) was superior to that of the GCE. In addition, we also determined the effects of scan rate, pH, and interferences of UA for the voltammetric behavior and detection. The results indicated that modified electrode possessed excellent reproducibility and stability. Finally, a new and efficient electrochemical sensor for detecting UA was developed.

  4. Modified gold electrodes based on thiocytosine/guanine-gold nanoparticles for uric and ascorbic acid determination

    International Nuclear Information System (INIS)

    Vulcu, Adriana; Grosan, Camelia; Muresan, Liana Maria; Pruneanu, Stela; Olenic, Liliana

    2013-01-01

    The present paper describes the preparation of new modified surfaces for electrodes based on guanine/thiocytosine and gold nanoparticles. The gold nanoparticles were analyzed by UV–vis spectroscopy and transmission electron microscopy (TEM) and it was found that they have diameters between 30 and 40 nm. The layers were characterized by specular reflectance infrared spectroscopy (FTIR-RAS) and by atomic force microscopy (AFM). The thickness of layers was found to be approximately 30 nm for TC layers and 300 nm for GU layers. Every layer was characterized as electrochemical sensor (by cyclic voltammetry) both for uric acid and ascorbic acid determinations, separately and in their mixture. The modified sensors have good calibration functions with good sensitivity (between 1.145 and 1.406 mA cm −2 /decade), reproducibility ( t hiocytosine (Au T C) and gold g uanine (Au G U) layers

  5. Determination of nitrite ion at schiff's base derivative of chitosan modified glassy carbon electrode

    International Nuclear Information System (INIS)

    Xu Zhongliang; Zhang Jianmei; Liu Shujuan; Peng Daofeng

    2007-01-01

    Chitosan react with salicyclaldehyde by schiff's base reaction in water, a polymer product S-CTS can be prepared. Glassy carbon electrode was modified with S-CTS by drop-coating method. Then, its electrocatalysis effect on the reduction of nitrite by the films of S-CTS was investigated. Experimental results showed that S-CTS modified electrode could reduce the oxidation overpotential of nitrite in pH4.5 B-R buffer solution, the peak current of reduction was proportional to the concentration of nitrite and a good linear relation from 0.20 to 81 mg/kg (r=0.9899) with a detection limit of 2.8 x 10 -7 mol/L was obtained. The methods have been applied to determining nitrite in some samples, satisfactory results were obtained. (authors)

  6. Electrochemical Determination of Glycoalkaloids Using a Carbon Nanotubes-Phenylboronic Acid Modified Glassy Carbon Electrode

    Directory of Open Access Journals (Sweden)

    Huiying Wang

    2013-11-01

    Full Text Available A versatile strategy for electrochemical determination of glycoalkaloids (GAs was developed by using a carbon nanotubes-phenylboronic acid (CNTs-PBA modified glassy carbon electrode. PBA reacts with α-solanine and α-chaconine to form a cyclic ester, which could be utilized to detect GAs. This method allowed GA detection from 1 μM to 28 μM and the detection limit was 0.3 μM. Affinity interaction of GAs and immobilized PBA caused an essential change of the peak current. The CNT-PBA modified electrodes were sensitive for detection of GAs, and the peak current values were in quite good agreement with those measured by the sensors.

  7. Norepinephrine-modified glassy carbon electrode for the simultaneous determination of ascorbic acid and uric acid

    International Nuclear Information System (INIS)

    Zare, H.R.; Memarzadeh, F.; Ardakani, M. Mazloum; Namazian, M.; Golabi, S.M.

    2005-01-01

    The oxidation of norepinephrine (NE) on a preactivated glassy carbon electrode leads to the formation of a deposited layer of about 4.2 x 10 -10 mol cm -2 at the surface of the electrode. The electron transfer rate constant, k s , and charge transfer coefficient, α, for electron transfer between the electrode and immobilized NE film were calculated as 44 s -1 and 0.46, respectively. The NE-modified glassy carbon electrode exhibited good electrocatalytic properties towards ascorbic acid (AA) oxidation in phosphate buffer (pH 7.0) with an overpotential of about 475 mV lower than that of the bare electrode. The electrocatalytic response was evaluated by cyclic voltammetry, chronoamperometry, amperometry and rotating disk voltammetry. The overall number of electrons involved in the catalytic oxidation of AA and the number of electrons involved in the rate-determining step are 2 and 1, respectively. The rate constant for the catalytic oxidation of AA was evaluated by RDE voltammetry and an average value of k h was found to be 8.42 x 10 3 M -1 s -1 . Amperometric determination of AA in stirred solution exhibits a linear range of 2.0-1300.0 μM (correlation coefficient 0.9999) and a detection limit of 0.076 μM. The precision of amperometry was found to be 1.9% for replicate determination of a 49.0 μM solution of AA (n = 6). In differential pulse voltammetric measurements, the NE-modified glassy carbon electrode can separate the AA and uric acid (UA) signals. Ascorbic acid oxidizes at more negative potential than UA. Also, the simultaneous determination of UA and AA is achieved at the NE-modified electrode

  8. Determination of ascorbic acid in pharmaceutical preparation and fruit juice using modified carbon paste electrode

    Directory of Open Access Journals (Sweden)

    Simona Žabčíková

    2016-06-01

    Full Text Available Acrobic acid is key substance in the human metabolism and the rapid and accurate determination in food is of a great interest. Ascorbic acid is an electroactive compound, however poorly responded on the bare carbon paste electrodes. In this paper, brilliant cresyl blue and multi-walled carbon nanotubes were used for the modification of carbon paste electrode. Brilliant cresyl blue acts as a mediator improving the transition of electrons, whereas multiwalled carbon nanotubes increased the surface of the electrode. Both brilliant cresyl blue and multiwalled carbon nanotubes were added directly to the composite material. The electrochemical behavior of modified electode was determined in electrolyte at various pH, and the effect of the scan rate was also performed. It was shown that the electrochemical process on the surface of the modified carbon paste electrode was diffusion-controlled. The resulted modified carbon paste electrode showed a good electrocatalytic activity towards the oxidation of ascorbic acid at a reduced overpotential of +100 mV descreasing the risk of interferences. A linear response of the ascorbic acid oxidation current measured by the amperometry in the range of 0.1 - 350 µmol.L-1 was obtained applying the sensor for the standard solution. The limit of detection and limit of quantification was found to be 0.05 and 0.15 µmol.L-1, respectively. The novel method was applied for the determination of ascorbic acid in pharmaceutical vitamin preparation and fruit juice, and the results were in good agreement with the standard HPLC method. The presented modification of carbon paste electrode is suitable for the fast, sensitive and very accurate determination of ascorbic acid in fruit juices and pharmaceutical preparation.

  9. O-Anisidine as Indicator in Titrimetric Determination of Ascorbic Acid and Isonicotinic Acid Hydrazide in Pharmaceutical Formulations

    OpenAIRE

    B.S.A.Andrews; B.Sreenivas Rao; Som Shankar Dubey; B.Venkata Kiran

    2010-01-01

    Inspite of the beautiful red coloured oxidized product of O-anisidine, the studies on its application in analytical techniques are scanty. So, authors have taken up the investigation on the utility of O-anisidine as a new Analytical reagent in the bromatometric-Indicator reaction. The detailed reaction on the potassium bromate and OAnisidine has enabled the authors to utilize O-Anisidine in titration of Ascorbic Acid and Isonicitonic Acid Hydrazide. Suitable conditions has been established wi...

  10. Preconcentration and Determination of Antimony in Drinking Water Bottled by Modified Nano-Alumina

    Directory of Open Access Journals (Sweden)

    M Mohammad Zakizade

    2016-01-01

    Full Text Available Abstract Introduction: Antimony trioxide (Sb2O3 has been utilized as a catalyst in polyethylene terephtalate (PET production, and the studies conducted on the bottled water has demonstrated that antimony can be leached from PET bottles into drinking water. Methods: In this study, a simple method was applied in order to determine the trace amount of antimony in bottled drinking water based on preconcentration /solid phase extraction. The nano alumina modified with Schiff base ligand was used in regard with Sb preconcentration. The experiments were performed in a continuous system and HCI was used as eluent of Sb ion. Several chemical and flow variables were optimized for a quantitative preconcentration and determination of Sb ion. The atomic absorption spectroscopy was used to determine Sb ion concentration. In order to study the keeping conditions on the leaching of Sb ion from PET plastic, drinking water bottles were kept in different conditions(room temperature, sunny light and -18˚C. Results: The calibration graph was linear in the range of 0.5 to 15.0 ppm Sb with detection limit of 0.055 ppm. The flow rate of sample was optimized in range of 1.0-9.0 mLmin-1 and Sb ion can be quantitatively eluted at 90 Vsample: Veluent retio. Conclusion: The study results revealed that the modified nano alumina is an effective sorbent in regard with absorbing Sb ion from water and HCI 1M can be used as an appropriate eluent. Maximum leaching of Sb ion is observed when the bottled drinking water was exposed to the sun light. Keywords: Antimony; Bottled drinking water; Modified alumina; Preconcentration

  11. Electrochemical Determination of Caffeine Content in Ethiopian Coffee Samples Using Lignin Modified Glassy Carbon Electrode

    Directory of Open Access Journals (Sweden)

    Meareg Amare

    2017-01-01

    Full Text Available Lignin film was deposited at the surface of glassy carbon electrode potentiostatically. In contrast to the unmodified glassy carbon electrode, an oxidative peak with an improved current and overpotential for caffeine at modified electrode showed catalytic activity of the modifier towards oxidation of caffeine. Linear dependence of peak current on caffeine concentration in the range 6×10-6 to 100×10-6 mol L−1 with determination coefficient and method detection limit (LoD = 3 s/slope of 0.99925 and 8.37×10-7 mol L−1, respectively, supplemented by recovery results of 93.79–102.17% validated the developed method. An attempt was made to determine the caffeine content of aqueous coffee extracts of Ethiopian coffees grown in four coffee cultivating localities (Wonbera, Wolega, Finoteselam, and Zegie and hence to evaluate the correlation between users preference and caffeine content. In agreement with reported works, caffeine contents (w/w% of 0.164 in Wonbera coffee; 0.134 in Wolega coffee; 0.097 in Finoteselam coffee; and 0.089 in Zegie coffee were detected confirming the applicability of the developed method for determination of caffeine in a complex matrix environment. The result indicated that users’ highest preference for Wonbera and least preference for Zegie cultivated coffees are in agreement with the caffeine content.

  12. Electrochemical Determination of Caffeine Content in Ethiopian Coffee Samples Using Lignin Modified Glassy Carbon Electrode.

    Science.gov (United States)

    Amare, Meareg; Aklog, Senait

    2017-01-01

    Lignin film was deposited at the surface of glassy carbon electrode potentiostatically. In contrast to the unmodified glassy carbon electrode, an oxidative peak with an improved current and overpotential for caffeine at modified electrode showed catalytic activity of the modifier towards oxidation of caffeine. Linear dependence of peak current on caffeine concentration in the range 6 × 10 -6 to 100 × 10 -6  mol L -1 with determination coefficient and method detection limit (LoD = 3 s/slope) of 0.99925 and 8.37 × 10 -7  mol L -1 , respectively, supplemented by recovery results of 93.79-102.17% validated the developed method. An attempt was made to determine the caffeine content of aqueous coffee extracts of Ethiopian coffees grown in four coffee cultivating localities (Wonbera, Wolega, Finoteselam, and Zegie) and hence to evaluate the correlation between users preference and caffeine content. In agreement with reported works, caffeine contents (w/w%) of 0.164 in Wonbera coffee; 0.134 in Wolega coffee; 0.097 in Finoteselam coffee; and 0.089 in Zegie coffee were detected confirming the applicability of the developed method for determination of caffeine in a complex matrix environment. The result indicated that users' highest preference for Wonbera and least preference for Zegie cultivated coffees are in agreement with the caffeine content.

  13. Study and Electrochemical Determination of Tyrosine at Graphene Nanosheets Composite Film Modified Glassy Carbon Electrode

    Directory of Open Access Journals (Sweden)

    M. Behpour

    2013-06-01

    Full Text Available A graphene nanosheets (GNS film coated glassy carbon electrode (GCE was fabricated for sensitive determination of tyrosine (Tyr. The GNS-based sensor was characterized by scanning electron microscope and electrochemical impedance spectroscopy. The voltammetric techniques were employed to study electro-oxidation of Tyr. The results revealed that the modified electrode showed an electrocatalytic activity toward the anodic oxidation of Tyr by a marked enhancement in the current intensity and the shift in the oxidation potential to lower values (50 mV in comparison with the bare GCE. Some kinetic parameters such as the electron transfer coefficient (α were also determined for the Tyr oxidation. The detection limit  for Tyr was found to be 2.0×10-8 M (n=9, and the peak current increases linearly with the Tyr concentration within the molar concentration ranges of 5.0 ×10-6 to 1.2 ×10-4 M. The modified electrode shows good sensitivity, selectivity and stability. The prepared electrode was applied for the determination of Tyr in real sample.

  14. Adsorptive Stripping Determination of Trace Nickel Using Bismuth Modified Mesoporous Carbon Composite Electrode

    Science.gov (United States)

    Ouyang, Ruizhuo; Feng, Kai; Su, Yongfu; Zong, Tianyu; Zhou, Xia; Lei, Tian; Jia, Pengpeng; Cao, Penghui; Zhao, Yuefeng; Guo, Ning; Chang, Haizhou; Miao, Yuqing; Zhou, Shuang

    Novel bismuth nanoparticle-modified mesoporous carbon (MPC) was successfully prepared on a glassy carbon electrode (Bi@MPC/GCE) for the adsorptive stripping voltammetric determination of nickel by complexing with dimethylglyoxime (DMG). The presence of MPC obviously improved the properties of Bi particles like the electron transfer ability, particle size and hydrophicility, important parameters to achieve preferable analytical performances of Bi@MPC/GCE toward Ni(II). The best electrochemical behaviors of Bi@MPC/GCE was obtained for the stripping determination of Ni(II), compared with electrodes individually modified with Bi and MPC. The synergic effect between metallic Bi and ordered MPC (forming a 3D array like Bi microelectrodes) made major contribution to such improved electrochemical properties of Bi@MPC/GCE for Ni(II) sensing. The good linear analytical curve was achieved in a Ni(II) concentration range from 0.1μM to 5.0μM with a correlation coefficient of 0.9995. The detection limit and sensitivity were calculated to be 1.2nM (S/N=3) and 1410μAmM-1cm-2, respectively. The new method was successfully applied to Ni(II) determination in soybean samples with recoveries higher than 99% and proved to be a simple, efficient alternative for Ni(II) monitoring in real samples.

  15. Determinants and modifiers of bleeding phenotypes in haemophilia-A: General and tropical perspectives

    Directory of Open Access Journals (Sweden)

    Umma A. Ibrahim

    2018-07-01

    Full Text Available Haemophilia-A is an X-linked recessive bleeding disorder characterized by deficiency of FVIII. Although severity of haemophilia is largely determined by the extent to which different mutations abolish FVIII production, the overall phenotypic variations among haemophiliacs is determined by a combination of several other factors, which range from general to tropical factors on the one hand, and from genetic to immunologic and infective factors on the other hand. Determinants and modifiers of haemophilic bleeding phenotypes are important predictors of prognosis. However, tropical determinants of haemophilic bleeding phenotypes are virtually ignored because majority of haemophilia research originated from developed non-tropical countries. The aim of this paper is to present a balanced review of the haemophilic bleeding phenotypes from general and tropical perspectives. Hence, we present a concisely updated comprehensive review of the pathophysiologic and clinical significance of general vis-à-vis tropical determinants and modifiers of haemophilic bleeding phenotypes from genetic, immunologic and infective perspectives. Understanding of general phenotypic determinants such as FVIII gene mutations, immunological (inhibitors and infective (e.g. hepatitis and HIV complications, classical thrombophilias (e.g. FV-Leiden and non-classical thrombophilias (e.g. non-O blood groups will throw more light into the mechanisms by which some tropical prothrombotic gene mutations (such as sickle β-globin gene and certain chronic tropical pro-haemorrhagic parasitic infections (such as urinary and gastrointestinal helminthiasis may modify frequency, intensity and pattern of bleeding among haemophiliacs in the tropics. The clinical significance of iron deficiency within the context of helminthiasis and haemophilia is also reviewed. More research is needed to determine the precise effect of non-classical thrombophilias such as sickling disorders and ABO blood groups

  16. Determination of specific capacitance of modified candlenut shell based carbon as electrode material for supercapacitor

    Science.gov (United States)

    Zakir, M.; Budi, P.; Raya, I.; Karim, A.; Wulandari, R.; Sobrido, A. B. J.

    2018-03-01

    Surface modification of candlenut shell carbon (CSC) using three chemicals: nitric acid (HNO3), hydrogen peroxide (H2O2), and sulfuric acid (H2SO4) has been carried out. Activation of CSC was performed using H3PO4 solution with different ratio between CSC and activator. Carbon surface area was determined by methylene blue adsorption method. Surface characterization was performed using FTIR spectroscopy and Boehm titration method. Specific capacitance of electrode prepared from CSAC (candlenuts shell activated carbon) materials was quantified by Cyclic Voltammetry (CV) measurement. The surface area before and after activation are 105,127 m2/g, 112,488 m2/g, 124,190 m2/g, and 135,167 m2/g, respectively. Surface modification of CSAC showed the improvement in the chemical functionality of CSAC surface. Analyses using FTIR spectroscopy and Boehm titration showed that modifications with HNO3, H2SO4 and H2O2 on the surface of the CSAC increased the number of oxygen functional groups. As a consequence, the specific capacitance of CSAC modified with 65% HNO3 attained the highest value (127 μF/g). There is an incredible increase by a factor of 298% from electrode which was constructed with un-modified CSAC material. This increase correlates to the largest number of oxygen functional groups of CSAC modified with nitric acid (HNO3).

  17. Simultaneous determination of phenylethanoid glycosides and aglycones by capillary zone electrophoresis with running buffer modifier.

    Science.gov (United States)

    Dong, Shuqing; Gao, Ruibin; Yang, Yan; Guo, Mei; Ni, Jingman; Zhao, Liang

    2014-03-15

    Although the separation efficiency of capillary electrophoresis (CE) is much higher than that of other chromatographic methods, it is sometimes difficult to adequately separate the complex ingredients in biological samples. This article describes how one effective and simple way to develop the separation efficiency in CE is to add some modifiers to the running buffer. The suitable running buffer modifier β-cyclodextrin (β-CD) was explored to fast and completely separate four phenylethanoid glycosides and aglycones (homovanillyl alcohol, hydroxytyrosol, 3,4-dimethoxycinnamic acid, and caffeic acid) in Lamiophlomis rotata (Lr) and Cistanche by capillary zone electrophoresis with ultraviolet (UV) detection. It was found that when β-CD was used as running buffer modifier, a baseline separation of the four analytes could be accomplished in less than 20 min and the detection limits were as low as 10(-3) mg L(-1). Other factors affecting the CE separation, such as working potential, pH value and ionic strength of running buffer, separation voltage, and sample injection time, were investigated extensively. Under the optimal conditions, a successful practical application on the determination of Lr and Cistanche samples confirmed the validity and practicability of this method. Copyright © 2014 Elsevier Inc. All rights reserved.

  18. Simultaneous determination of flavonoids in chrysanthemum by capillary zone electrophoresis with running buffer modifiers.

    Science.gov (United States)

    Zhang, Shan; Dong, Shuqing; Chi, Langzhu; He, Pingang; Wang, Qingjiang; Fang, Yuzhi

    2008-08-15

    Despite the separation efficiency of capillary electrophoresis (CE) is much higher than other chromatographic methods, it is sometimes difficult to perfectly separate the complex ingredients in biological samples. One possible and simple way to develop the separation effect in CE is to add some modifiers in the running buffer. In this paper, the suitable running buffer modifiers were explored to simultaneously separate and detect six typical flavonoids (apigenin, luteolin, kaempferol, quercetin, (+)-catechin and (-)-epicatechin) which are the main active ingredients in chrysanthemum by capillary zone electrophoresis with amperometric detection (CZE-AD). It was found that when beta-cyclodextrin (beta-CD) and the mixture of methanol and ethanol were used as running buffer modifiers, a baseline separation of the six analytes could be accomplished in less than 20 min and the detection limits were as low as 10(-7) or 10(-8)gm l(-1). Other factors affecting the CZE separation, such as working potential, pH value and ionic strength of running buffer, separation voltage and sample injection time were extensively investigated. Under the optimum conditions, a successful practical application on the determination of chrysanthemum samples confirmed the validity and practicability of this method.

  19. Salicylate-spectrophotometric determination of inorganic monochloramine

    International Nuclear Information System (INIS)

    Tao Hui; Chen Zhonglin; Li Xing; Yang Yanling; Li Guibai

    2008-01-01

    On the basis of classical Berthelot reaction, a simple salicylate-spectrophotometric method was developed for quantitative determination of inorganic monochloramine in water samples. With the catalysis of disodium pentacyanonitrosylferrate(III), inorganic monochloramine reacts with salicylate in equimolar to produce indophenol compound which has an intense absorption at 703 nm. Parameters that influence method performance, such as pH, dosage of salicylate and nitroprussiate and reaction time, were modified to enhance the method performance. By using this method, inorganic monochloramine can be distinguished from organic chloramines and other inorganic chlorine species, such as free chlorine, dichloramine, and trichloramine. The molar absorptivities of the final products formed by these compounds are below ±3% of inorganic monochloramine, because of the α-N in them have only one exchangeable hydrogen atom, and cannot react with salicylate to produce the indophenol compound. The upper concentrations of typical ions that do not interfere with the inorganic monochloramine determination are also tested to be much higher than that mostly encountered in actual water treatment. Case study demonstrates that the results obtained from this method are lower than DPD-titrimetric method because the organic chloramines formed by chlorination of organic nitrogenous compounds give no response in the newly established method. And the result measured by salicylate-spectrophotometric method is coincident with theoretical calculation

  20. Electrochemically modified sulfisoxazole nanofilm on glassy carbon for determination of cadmium(II) in water samples

    International Nuclear Information System (INIS)

    Gupta, Vinod Kumar; Yola, Mehmet Lütfi; Atar, Necip; Solak, Ali Osman; Uzun, Lokman; Üstündağ, Zafer

    2013-01-01

    Highlights: • Sulfisoxazole was grafted onto glassy carbon electrode. • The electrode was characterized by spectroscopic and electrochemical methods. • It has been used for the determination of Cd(II) ions in real samples in very low concentrations. -- Abstract: Sulfisoxazole (SO) was grafted to glassy carbon electrode (GCE) via the electrochemical oxidation of SO in acetonitrile solution containing 0.1 M tetrabutylammoniumtetra-fluoroborate (TBATFB). The prepared electrode was characterized by using cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), reflection–absorption infrared spectroscopy (RAIRS) and X-ray photoelectron spectroscopy (XPS). The ellipsometric thickness of SO nanofilm at the glassy carbon surface was obtained as 14.48 ± 0.11 nm. The stability of the SO modified GCE was studied. The SO modified GCE was also utilized for the determination of Cd(II) ions in water samples in the presence of Pb(II) and Fe(II) by adsorptive stripping voltammetry. The linearity range and the detection limit of Cd(II) ions were 1.0 × 10 −10 to 5.0 × 10 −8 M and 3.3 × 10 −11 M (S/N = 3), respectively

  1. Modifiable Determinants of Obesity in Native Hawaiian and Pacific Islander Youth.

    Science.gov (United States)

    Braden, Katherine W; Nigg, Claudio R

    2016-06-01

    In the United States, obesity continues to be a major public health concern. Obesity disproportionately affects Native Hawaiian and Other Pacific Islanders (NHOPI) who demonstrate alarming rates of obesity and its related chronic conditions. However, little is known about the causes of obesity for this group. Given the modest effects of individual-level obesity treatments, identifying the most impactful determinants that can be modified to prevent or reduce obesity in NHOPI youth is critical to the development of interventions that best meet the needs of this population. A systematic review was conducted in PubMed, with additional expert-recommended articles identified through the Hawai'i Initiative for Childhood Obesity Research and Education (HICORE) research database, to evaluate the current body of research on modifiable determinants or correlates of obesity in NHOPI youth. Of an initial pool of 471 articles, 60 articles were read in full and 14 articles were selected for inclusion in the qualitative synthesis. Utilizing an ecological framework to identify gaps in the literature and suggest areas for future research, findings from this review indicate that early life and contextual factors-namely, infant-feeding mode, geographic location, and education-appear to play an important role in obesity in NHOPI youth. However, more research is needed, particularly pre-birth cohort studies evaluating the effects of prenatal and early life risk factors, studies on the sociocultural influences on obesity-related psychosocial factors and health behaviors, as well as the influence of environmental and policy-level variables.

  2. Electrochemical sensor based on magnetic molecularly imprinted nanoparticles modified magnetic electrode for determination of Hb.

    Science.gov (United States)

    Sun, Binghua; Ni, Xinjiong; Cao, Yuhua; Cao, Guangqun

    2017-05-15

    A fast and selective electrochemical sensor for determination of hemoglobin (Hb) was developed based on magnetic molecularly imprinted nanoparticles modified on the magnetic glassy carbon electrode. The nanoparticles Fe 3 O 4 @SiO 2 with a magnetic core and a molecularly imprinted shell had regular structures and good monodispersity. Hb could be determined directly by electrochemical oxidization with the modified electrode. A magnetic field increased electrochemical response to Hb by two times. Imprinting Hb on the surface of Fe 3 O 4 @SiO 2 shortened the response time within 7min. Under optimum conditions, the imprinting factor toward the non-imprinted sensor was 2.8, and the separation factor of Hb to horseradish peroxidase was 2.6. The oxidation peak current had a linear relationship with Hb concentration ranged from 0.005mg/ml to 0.1mg/ml with a detection limit (S/N =3) of 0.0010mg/ml. The sensors were successfully applied to analysis of Hb in whole blood samples with recoveries between 95.7% and 105%. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. Pre-concentration and determination of tartrazine dye from aqueous solutions using modified cellulose nanosponges.

    Science.gov (United States)

    Shiralipour, Roohollah; Larki, Arash

    2017-01-01

    In this study, a new absorbent based on cellulose nanosponges modified with methyltrioctylammonium chloride (aliquat 336) was prepared and used for pre-concentration, removal and determination of tartrazine dye, using UV-vis spectrophotometry. This adsorbent was fully characterized using various instrumental techniques such as SEM, FTIR and XRD spectra. The pre-concentration and removal procedures were studied in column and batch modes, respectively. The effects of parameters such as pH of the aqueous medium, methyltrioctylammounium chloride dose, adsorbent amount, desorbing conditions and interfering ions on the adsorption of tartrazine were investigated and optimized. The fitting experimental data with conventional isotherm models revealed that the adsorption followed the Brunauer-Emmett-Teller (BET) model and the maximum adsorption capacity for tartrazine was 180mg/g with modified nanosponges. Under the optimized conditions, the calibration curve was linear over the range of 2-300ng/mL and the limit of detection was 0.15ng/mL. The relative standard deviation (RSD) for 20 and 100ng/mL of tartrazine were 3.1% and 1.5%, respectively. The proposed method was applied for pre-concentration and determination of tartrazine dye in different water samples. Copyright © 2016 Elsevier Inc. All rights reserved.

  4. Electrochemical determination of 4-nitrophenol at polycarbazole/N-doped graphene modified glassy carbon electrode

    International Nuclear Information System (INIS)

    Zhang, Yuehua; Wu, Lihua; Lei, Wu; Xia, Xifeng; Xia, Mingzhu; Hao, Qingli

    2014-01-01

    Graphical abstract: - Highlights: • Polycarbazole/N-doping graphene (PCZ/N-GE) composite was fabricated. • The PCZ/N-GE composite shows good electrocatalytic activity to 4-nitrophenol. • PCZ/N-GE modified electrode was used for determination of 4-nitrophenol. • The proposed sensor exhibits good sensitivity, stability and reproducibility. - Abstract: Polycarbazole (PCZ)/nitrogen-doped graphene (N-GE) composite was prepared by electropolymerization of carbazole on the N-GE modified glass carbon electrode (N-GE/GCE) for fabricating a novel electrochemical sensor for 4-nitrophenol (4-NP). The PCZ/N-GE shows high conductivity and well-distributed nanostructure. The redox behavior of 4-NP at a PCZ/N-GE/GCE was investigated in acetate buffer solution by cyclic voltammetry (CV), compared with the bare GCE, reduced graphene oxide (RGO), N-GE and PCZ modified GCEs. The results indicate that all modified electrodes show the enhanced reduction peak currents. However, the PCZ/N-GE/GCE exhibits the highest peak current and most positive reduction potential of 4-NP, which reflects the PCZ/N-GE composite has the best electrocatalytic activity towards 4-NP. The enhanced electrochemical performance of PCZ/N-GE and the electrocatalytic activity to 4-NP are contributed to the synergic effect of PCZ and N-GE with highly conductivity and large surface area, which can greatly facilitate the electron-transfer processes between the electrolyte and electrode. An electrochemical sensor for 4-NP was developed based on the PCZ/N-GE modified electrode under the optimized conditions. The reduction peak current was linear with the concentration of 4-NP in the range of 8 × 10 -7 ∼2 × 10 -5 M. The low detection limit of the sensor was estimated to be 0.062 μM (S/N = 3). The sensor based on PCZ/N-GE/GCE was also applied to the detection of 4-NP in real water samples

  5. New titrimetric method for oxygen to metal ratio in uranium oxide powders

    International Nuclear Information System (INIS)

    Ray, Vinod Kumar; Brahmananda Reddy, G.; Balaji Rao, Y.; Subba Rao, Y.

    2015-01-01

    O/U ratio is of high importance to both U 3 O 8 and UO 2 powders for different reasons. In UO 2 powder it is a guiding parameter for sintering process where as for U 3 O 8 , it indicates efficiency of ammonium di-uranate (ADU) to U 3 O 8 conversion process. In the present method for O/U determination, UO 2 and U 3 O 8 powders are dissolved in 4.5 M sulphuric acid and little HF by heating on hot plate. Subsequently, optimized quantity of phosphoric acid is added on cooling, for getting sharp end point. The resultant solution is titrated with standard potassium dichromate using barium diphenylamine sulphonate (BDS) as an indicator. The expanded uncertainties calculated for UO 2 and U 3 O 8 powders are ±0.004 and ±0.006 O/U ratio units respectively at 95 % confidence level. (author)

  6. Electrochemical Determination of Food Preservative Nitrite with Gold Nanoparticles/p-Aminothiophenol-Modified Gold Electrode.

    Science.gov (United States)

    Üzer, Ayşem; Sağlam, Şener; Can, Ziya; Erçağ, Erol; Apak, Reşat

    2016-08-02

    Due to the negative impact of nitrate and nitrite on human health, their presence exceeding acceptable levels is not desired in foodstuffs. Thus, nitrite determination at low concentrations is a major challenge in electroanalytical chemistry, which can be achieved by fast, cheap, and safe electrochemical sensors. In this work, the working electrode (Au) was functionalized with p-aminothiophenol (p-ATP) and modified with gold nanoparticles (Au-NPs) to manufacture the final (Au/p-ATP-Aunano) electrode in a two-step procedure. In the first step, p-ATP was electropolymerized on the electrode surface to obtain a polyaminothiophenol (PATP) coating. In the second step, Au/p-ATP-Aunano working electrode was prepared by coating the surface with the use of HAuCl₄ solution and cyclic voltammetry. Determination of aqueous nitrite samples was performed with the proposed electrode (Au/p-ATP-Aunano) using square wave voltammetry (SWV) in pH 4 buffer medium. Characteristic peak potential of nitrite samples was 0.76 V, and linear calibration curves of current intensity versus concentration was linear in the range of 0.5-50 mg·L(-1) nitrite with a limit of detection (LOD) of 0.12 mg·L(-1). Alternatively, nitrite in sausage samples could be colorimetrically determined with high sensitivity by means of p-ATP‒modified gold nanoparticles (AuNPs) and naphthylethylene diamine as coupling agents for azo-dye formation due to enhanced charge-transfer interactions with the AuNPs surface. The slopes of the calibration lines in pure NO₂(-) solution and in sausage sample solution, to which different concentrations of NO₂(-) standards were added, were not significantly different from each other, confirming the robustness and interference tolerance of the method. The proposed voltammetric sensing method was validated against the colorimetric nanosensing method in sausage samples.

  7. Sex determination based on amelogenin DNA by modified electrode with gold nanoparticle.

    Science.gov (United States)

    Mazloum-Ardakani, Mohammad; Rajabzadeh, Nooshin; Benvidi, Ali; Heidari, Mohammad Mehdi

    2013-12-15

    We have developed a simple and renewable electrochemical biosensor based on carbon paste electrode (CPE) for the detection of DNA synthesis and hybridization. CPE was modified with gold nanoparticles (AuNPs), which are helpful for immobilization of thiolated bioreceptors. AuNPs were characterized by scanning electron microscopy (SEM). Self-assembled monolayers (SAMs) of thiolated single-stranded DNA (SH-ssDNA) of the amelogenin gene was formed on CPE. The immobilization of the probe and its hybridization with the target DNA was optimized using different experimental conditions. The modified electrode was characterized by electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). The electrochemical response of ssDNA hybridization and DNA synthesis was measured using differential pulse voltammetry (DPV) with methylene blue (MB) as an electroactive indicator. The new biosensor can distinguish between complementary and non-complementary strands of amelogenin ssDNA. Genomic DNA was extracted from blood and was detected based on changes in the MB reduction signal. These results demonstrated that the new biosensor could be used for sex determination. The proposed biosensor in this study could be used for detection and discrimination of polymerase chain reaction (PCR) products of amelogenin DNA. Copyright © 2013 Elsevier Inc. All rights reserved.

  8. Determining fracture energy parameters of concrete from the modified compact tension test

    Directory of Open Access Journals (Sweden)

    A. Fernández-Canteli

    2014-10-01

    Full Text Available The modified compact tension (MCT test, though not yet recognized as a valid test for determining fracture energy of concrete, is believed to represent a plausible and suitable alternative versus other well established procedures, such as the wedge-splitting test (WST and the three point (3PB or four point bending (4PB tests, due to its simplicity and low cost. The aim of the paper is twofold: Firstly, to demonstrate the necessary correspondence between the experimental MCT test setup and finite element simulations and secondly, to initiate the way of establishing the desirable conversion between the fracture energy parameter values resulting from the MCT test and the standard conventional procedures. MCT tests are carried out and compared with the numerical results from 2-D and 3-D finite element calculations using the commercial codes ABAQUS and ATENA, the latter being specifically developed for applications on concrete structures and elements. In this way, the usability of the modified compact tension test for practical purposes is confirmed.

  9. Prussian blue-modified nanoporous gold film electrode for amperometric determination of hydrogen peroxide.

    Science.gov (United States)

    Ghaderi, Seyran; Mehrgardi, Masoud Ayatollahi

    2014-08-01

    In this manuscript, the electrocatalytic reduction of hydrogen peroxides on Prussian blue (PB) modified nanoporous gold film (NPGF) electrode is described. The PB/NPGF is prepared by simple anodizing of a smooth gold film followed by PB film electrodeposition method. The morphology of the PB/NPGF electrode is characterized using scanning electron microscopy (SEM). The effect of solution pH and the scan rates on the voltammetric responses of hydrogen peroxide have also been examined. The amperometric determination of H2O2 shows two linear dynamic responses over the concentration range of 1μM-10μM and 10μM-100μM with a detection limit of 3.6×10(-7)M. Furthermore, this electrode demonstrated good stability, repeatability and selectivity remarkably. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. Manganese dioxide-modified carbon paste electrode for voltammetric determination of riboflavin

    International Nuclear Information System (INIS)

    Mehmeti, Eda; Kalcher, Kur; Stanković, Dalibor M.; Chaiyo, Sudkate; Švorc, Ľubomir

    2016-01-01

    A carbon paste electrode bulk was modified with MnO 2 and investigated for use as an electrochemical sensor for riboflavin (vitamin B 2 ) using differential pulse voltammetry (DPV). Riboflavin displays a well expressed oxidation peak at −0.15 V (versus Ag/AgCl) in solutions with a pH value of 2. Effects of pH value, pulse amplitude and pulse time were optimized by employing DPV. The signals obtained are linearly related to the concentrations of riboflavin in the range from 0.02 to 9 μM. Other features include a 15 nM detection limit, and good reproducibility (±3 %) and repeatability (±2 %). Interferences by common compounds were tested, and the method was successfully applied to the determination of riboflavin in pharmaceutical formulations where is gave recoveries in the range from 95 to 97 %. (author)

  11. Voltammetric determination of carbidopa and folic acid using a modified carbon nanotubes paste electrode

    Directory of Open Access Journals (Sweden)

    Keshtkar Nasrin

    2015-01-01

    Full Text Available A novel electrochemical sensor for the selective and sensitive detection of carbidopa in presence of large excess of folic acid at physiological pH was developed by the bulk modification of carbon paste electrode (CPE with carbon nanotubes (CNTs and vinylferrocene. Large peak separation, good sensitivity and stability allow this modified electrode to analyze carbidopa individually and simultaneously along with folic acid. Applying square wave voltammetry (SWV, a linear dynamic range of 1.0×10-6- 7.0×10-4 M with detection limit of 2.0×10-7 M was obtained for carbidopa. Finally, the proposed method was applied to the determination of carbidopa and folic acid in urine sample.

  12. Determination of glutamine and glutamic acid in mammalian cell cultures using tetrathiafulvalene modified enzyme electrodes.

    Science.gov (United States)

    Mulchandani, A; Bassi, A S

    1996-01-01

    Tetrathiafulvalene (TTF) mediated amperometric enzyme electrodes have been developed for the monitoring of L-glutamine and L-glutamic acid in growing mammalian cell cultures. The detection of glutamine was accomplished by a coupled enzyme system comprised of glutaminase plus glutamate oxidase, while the detection of glutamic acid was carried out by a single enzyme, glutamate oxidase. The appropriate enzyme(s) were immoblized on the Triton-X treated surface of tetrathiafulvalene modified carbon paste electrodes by adsorption, in conjunction with entrapment by an electrochemically deposited copolymer film of 1,3-phenylenediamine and resorcinol. Operating conditions for the glutamine enzyme electrode were optimized with respect to the amount of enzymes immoblized, pH, temperature and mobile phase flow rate for operation in a flow injection (FIA) system. When applied to glutamine and glutamic acid measurements in mammalian cell culture in FIA, the results obtained with enzyme electrodes were in excellent agreement with those determined by enzymatic analysis.

  13. 3-Mercaptopropyltrimethoxysilane Modified Diatomite: Preparation and Application for Voltammetric Determination of Lead (II and Cadmium (II

    Directory of Open Access Journals (Sweden)

    Dinh Quang Khieu

    2017-01-01

    Full Text Available In this study, functionalized diatomite was prepared by grafting of 3-mercaptopropyltrimethoxysilane (MPTMS to diatomite (MPTMS-diatomite. The diatomite with thermal treatment from 100 to 700°C was functionalized by MPTMS under dry and humid conditions. The obtained MPTMS-diatomite was characterized by X-ray diffraction (XRD, thermal gravity-differential scanning calorimeter (TG-DSC, and Fourier transformation infrared (FT-IR. The results showed that an increase in treatment temperature seems to reduce the loading of MPTMS onto diatomite. The humidity of diatomite was favorable for the grafting of functional groups on the surface. The possible mechanisms of MPTMS loading to diatomite (MPTMS-diatomite were also proposed. The performance of a carbon paste electrode (CPE modified with MPTMS-diatomite in the simultaneous determination of Cd(II and Pb(II ions was addressed.

  14. Fabrication and characterisation of high performance polypyrrole modified microarray sensor for ascorbic acid determination

    Energy Technology Data Exchange (ETDEWEB)

    Samseya, J. [Alagappa University, Karaikudi, Tamil Nadu (India); Srinivasan, R., E-mail: sivarunjan@gmail.com [Central Electro Chemical Research Insititute, Karaikudi, Tamil Nadu (India); Chang, Yu-Tsern; Tsao, Cheng-Wen [Department of Cosmetic Applications, Taoyuan Innovation Institute of Technology, Taiwan (China); Vasantha, V.S. [Madurai Kamaraj University, Madurai, Tamil Nadu (India)

    2013-09-02

    Graphical abstract: -- Highlights: •Gold microelectrode array (Au/MEA) with electrode of 12 μm diameter was fabricated by photolithography technique. •Subsequently, polypyrrole (Ppy) modified gold microarrays sensor (Ppy/Au/MEA) was prepared. •Ppy/Au/MEA used for ascorbic acid determination in the presence of different neurotransmitters. •The micro array exhibited wide linear range, very high sensitivity and very low LOD than the earlier reports. •It was used successfully to test ascorbic acid in different types real samples. -- Abstract: In this study, gold microelectrode array (Au/MEA) with electrode of 12 μm diameter was fabricated by photolithography technique. Subsequently, polypyrrole (Ppy) modified gold microarrays sensor (Ppy/Au/MEA) was prepared by cyclic voltammetry technique. The deposition potential range and number of cycles were optimised in order to get optimum thickness of Ppy film. Scanning Electron Microscope and Atomic Force Microscope investigations reveal that Ppy coating formed at 3 cycles is porous with thickness of 1.5 μm which exhibiting high catalytic current for ascorbic acid (AA) in square wave technique (SWV). In contrast to earlier sensors designs, these Ppy/Au/MEA sensors exhibits lower detection limit (LOD) of 10 nm towards AA at physiological conditions. It also exhibits enhanced sensitivity (2.5 mA cm{sup −2} mM{sup −1}) and long range of linear detection limit from 10 nm to 2.8 mM. In the same way, polypyrrole modified macro Au (Ppy/Au/MA) biosensor was also fabricated and its electro catalytic property towards AA was compared with that of Ppy/Au/MEA. The Ppy/Au/MA exhibits sensitivity of only 0.27 mA cm{sup −2} mM{sup −1}, LOD of 5 μM and linear range of 10 μM to 2.2 mM. Hence, our investigations indicate that the Ppy/Au/MEA could serve as highly sensitive sensor for AA than any of the earlier designs. So, the Ppy/Au/MEA electrode was utilised for determination AA in a wide variety of real samples.

  15. Fabrication and characterisation of high performance polypyrrole modified microarray sensor for ascorbic acid determination

    International Nuclear Information System (INIS)

    Samseya, J.; Srinivasan, R.; Chang, Yu-Tsern; Tsao, Cheng-Wen; Vasantha, V.S.

    2013-01-01

    Graphical abstract: -- Highlights: •Gold microelectrode array (Au/MEA) with electrode of 12 μm diameter was fabricated by photolithography technique. •Subsequently, polypyrrole (Ppy) modified gold microarrays sensor (Ppy/Au/MEA) was prepared. •Ppy/Au/MEA used for ascorbic acid determination in the presence of different neurotransmitters. •The micro array exhibited wide linear range, very high sensitivity and very low LOD than the earlier reports. •It was used successfully to test ascorbic acid in different types real samples. -- Abstract: In this study, gold microelectrode array (Au/MEA) with electrode of 12 μm diameter was fabricated by photolithography technique. Subsequently, polypyrrole (Ppy) modified gold microarrays sensor (Ppy/Au/MEA) was prepared by cyclic voltammetry technique. The deposition potential range and number of cycles were optimised in order to get optimum thickness of Ppy film. Scanning Electron Microscope and Atomic Force Microscope investigations reveal that Ppy coating formed at 3 cycles is porous with thickness of 1.5 μm which exhibiting high catalytic current for ascorbic acid (AA) in square wave technique (SWV). In contrast to earlier sensors designs, these Ppy/Au/MEA sensors exhibits lower detection limit (LOD) of 10 nm towards AA at physiological conditions. It also exhibits enhanced sensitivity (2.5 mA cm −2 mM −1 ) and long range of linear detection limit from 10 nm to 2.8 mM. In the same way, polypyrrole modified macro Au (Ppy/Au/MA) biosensor was also fabricated and its electro catalytic property towards AA was compared with that of Ppy/Au/MEA. The Ppy/Au/MA exhibits sensitivity of only 0.27 mA cm −2 mM −1 , LOD of 5 μM and linear range of 10 μM to 2.2 mM. Hence, our investigations indicate that the Ppy/Au/MEA could serve as highly sensitive sensor for AA than any of the earlier designs. So, the Ppy/Au/MEA electrode was utilised for determination AA in a wide variety of real samples

  16. VALIDITY OF THE MODIFIED CONCONI TEST FOR DETERMINING VENTILATORY THRESHOLD DURING ON-WATER ROWING

    Directory of Open Access Journals (Sweden)

    Jorge Villamil Cabo

    2011-12-01

    Full Text Available The objectives of this study were to design a field test based on the Conconi protocol to determine the ventilatory threshold of rowers and to test its reliability and validity. A group of sixteen oarsmen completed a modified Conconi test for on-water rowing. The reliability of the detection of the heart rate threshold was evaluated using heart rate breaking point in the Conconi test and retest. Heart rate threshold was detected in 88.8% of cases in the test-retest. The validity of the modified Conconi test was evaluated by comparing the heart rate threshold data acquired with that obtained in a ventilatory threshold test (VT2. No significant differences were found for the values of different intensity parameters i.e. heart rate (HR, oxygen consumption (VO2, stroke rate (SR and speed (S between the heart rate threshold and the ventilatory threshold, (170.9 ± 6.8 vs. 169.3 ± 6.4 beats·min-1; 42.0 ± 8.6 vs. 43.5 ± 8.3 ml·kg-1·min-1; 25.8 ± 3.3 vs. 27.0 ± 3.2 strokes·min-1 and 14.4 ± 0.8 vs. 14.6 ± 0.8 km·h-1. The differences in averages obtained in the Conconi test-retest were small with a low standard error of the mean. The reliability data between the Conconi test-retest showed low coefficients of variations (CV and high intraclass correlation coefficients (ICC. The total errors for the Conconi test-retest are low for the measured variables (1.31 HR, 0.87 VO2, 0.65 SR, and 0.1 S. The Bland- Altman's method for analysis validity showed a strong concordance according to the analyzed variables. We conclude that the modified Conconi test for on-water rowing is a valid and reliable method for the determination of the second ventilatory threshold (VT2.

  17. Anodic stripping voltammetric determination of silver ion at a carbon paste electrode modified with carbon nanotubes

    International Nuclear Information System (INIS)

    Tashkhourian, J.; Javadi, S.; Ana, F.N.

    2011-01-01

    A carbon paste electrode (CPE) was modified with multi-wall carbon nanotubes and successfully applied to the determination of silver ion by differential pulse anodic stripping voltammetry. Compared to a conventional CPE, a remarkably improved peak current response and sensitivity is observed. The analytical procedure consisted of an open circuit accumulation step for 2 min in -0.4 V, this followed by an anodic potential scan between +0.2 and + 0.6 V to obtain the voltammetric peak. The oxidation peak current is proportional to the concentration of silver ion in the range from 1.0 x 10 -8 to 1.0 x 10 -5 mol L -1 , with a detection limit of 1.8 x 10 -9 mol L -1 after an accumulation time of 120 s. The relative standard deviation for 7 successive determinations of Ag(I) at 0.1 μM concentration is 1.99%. The procedure was validated by determining Ag(I) in natural waters. (author)

  18. The MacDonald and savage titrimetric procedure for plutonium scaled-down to the milligram level: Automated procedure for routine analysis of safeguards samples containing 2 to 5 mg plutonium

    International Nuclear Information System (INIS)

    Ronesch, K.; Jammet, G.; Berger, J.; Doubek, N.; Bagliano, G.; Deron, S.

    1992-08-01

    A selective titrimetric procedure directly applicable to both input and product solutions from fast reactor fuel reprocessing was set up by MacDonald and Savage and scaled down to 3 mg of plutonium in sample aliquots at the request of the Safeguards Analytical Laboratory (SAL) of the International Atomic Energy Agency (IAEA), which needed to replace its silver (II) oxide titration procedure by a more selective electrochemical method. Although the procedure is very selective the following species still interfere: Vanadates (almost quantitatively), Neptunium (one electron exchange per mole); Nitrites, Fluorosilicates and Iodates present in mg amount yield slight biases. This paper describes the fully automatized procedure presently applied in SAL for the routine determination of 2 to 5 mg plutonium dissolved in nitric acid solution. The method allows the unattended analysis of 20 aliquots within a five hour period. The equipment including the reagent distribution system, the sample changer and the control units are introduced and the principle design of the software is shortly described. Safety requirements have been addressed and are also reviewed in the report. Results obtained on standard reference materials, international intercomparison samples and actual safeguards samples routinely analyzed with the proposed procedure are presented and compared with results achieved with the semiautomatic mode to demonstrate the performance. International requirements to reduce the amount of radioactive materials in waste will certainly lead to a further reduction of the amount of plutonium in one aliquot. Some future perspective to titrate 1 mg samples are presented in the discussion. 12 refs, 10 figs, 8 tabs

  19. Simultaneous determination of dopamine, uric acid and nitrite using carboxylated graphene oxide/lanthanum modified electrode

    International Nuclear Information System (INIS)

    Ye, Fengying; Feng, Chenqi; Jiang, Jibo; Han, Sheng

    2015-01-01

    Highlights: • The carboxylated graphene oxide/lanthanum-modified glassy carbon electrode (GO-COOLa/GCE) was successfully utilized for the simultaneous detection and quantification of DA, UA and NO 2 − . • Combining the benefits of carboxylated graphene oxide and lanthanum, the modified sensor displayed large peak separations, long linear ranges and low detection limits for simultaneously detecting DA, UA and NO 2 − . • The GO-COOLa/GCE electrode showed well stability, good repeatability, rapid response, and high catalytic performance toward the oxidations of DA, UA and NO 2 − . - Abstract: A bare glassy carbon electrode (GCE) was reformed by carboxylated graphene oxide/lanthanum, and the modified electrode, called GO-COOLa/GCE, was fabricated for simultaneously detecting dopamine (DA), uric acid (UA) and nitrite (NO 2 − ) by cyclic voltammetry (CV), differential pulse voltammetry (DPV) and amperometry. Several factors which affected the electrocatalytic activity of the GO-COOLa/GCE electrode, such as the effect of pH, scan rate and concentration were studied. Due to the combination of carboxylated graphene oxide and lanthanum ions, the GO-COOLa/GCE sensor showed rapid response, excellent selectivity and high catalytic performance toward the electrooxidation of DA, UA and NO 2 − . In optimized conditions, two linear response ranges for determining DA were obtained over ranges of 0.01-1.96×10 2 μM and 1.96×10 2 -1.23×10 3 μM with detection limit of 0.018 μM (S/N = 3). And the responses of the GO-COOLa/GCE electrode for UA and NO 2 − were linear in the region of 1-1.53×10 3 μM and 1-2.75×10 3 μM with detection limits of 0.058 μM and 0.070 μM, respectively. Furthermore, this reformed electrode was successfully used to the detection of DA, UA and NO 2 − in real urine and serum samples, showing its promising application in the electroanalysis of real samples.

  20. State infant mortality: an ecologic study to determine modifiable risks and adjusted infant mortality rates.

    Science.gov (United States)

    Paul, David A; Mackley, Amy; Locke, Robert G; Stefano, John L; Kroelinger, Charlan

    2009-05-01

    To determine factors contributing to state infant mortality rates (IMR) and develop an adjusted IMR in the United States for 2001 and 2002. Ecologic study of factors contributing to state IMR. State IMR for 2001 and 2002 were obtained from the United States linked death and birth certificate data from the National Center for Health Statistics. Factors investigated using multivariable linear regression included state racial demographics, ethnicity, state population, median income, education, teen birth rate, proportion of obesity, smoking during pregnancy, diabetes, hypertension, cesarean delivery, prenatal care, health insurance, self-report of mental illness, and number of in-vitro fertilization procedures. Final risk adjusted IMR's were standardized and states were compared with the United States adjusted rates. Models for IMR in individual states in 2001 (r2 = 0.66, P < 0.01) and 2002 (r2 = 0.81, P < 0.01) were tested. African-American race, teen birth rate, and smoking during pregnancy remained independently associated with state infant mortality rates for 2001 and 2002. Ninety five percent confidence intervals (CI) were calculated around the regression lines to model the expected IMR. After adjustment, some states maintained a consistent IMR; for instance, Vermont and New Hampshire remained low, while Delaware and Louisiana remained high. However, other states such as Mississippi, which have traditionally high infant mortality rates, remained within the expected 95% CI for IMR after adjustment indicating confounding affected the initial unadjusted rates. Non-modifiable demographic variables, including the percentage of non-Hispanic African-American and Hispanic populations of the state are major factors contributing to individual variation in state IMR. Race and ethnicity may confound or modify the IMR in states that shifted inside or outside the 95% CI following adjustment. Other factors including smoking during pregnancy and teen birth rate, which are

  1. Cathodic stripping voltammetric determination of arsenic in sugarcane brandy at a modified carbon nanotube paste electrode.

    Science.gov (United States)

    Teixeira, Meryene C; Tavares, Elisângela de F L; Saczk, Adelir A; Okumura, Leonardo L; Cardoso, Maria das Graças; Magriotis, Zuy M; de Oliveira, Marcelo F

    2014-07-01

    We have developed an eletroanalytical method that employs Cu(2+) solutions to determine arsenic in sugarcane brandy using an electrode consisting of carbon paste modified with carbon nanotubes (CNTPE) and polymeric resins. We used linear sweep (LSV) and differential-pulse (DPV) voltammetry with cathodic stripping for CNTPE containing mineral oil or silicone as binder. The analytical curves were linear from 30 to 110μgL(-1) and from 10 to 110μgL(-1) for LSV and DPV, respectively. The limits of detection (L.O.D.) and quantification (L.O.Q.) of CNTPE were 10.3 and 34.5μgL(-1) for mineral oil and 3.4 and 11.2μgL(-1) for silicone. We applied this method to determine arsenic in five commercial sugarcane brandy samples. The results agreed well with those obtained by hydride generation combined with atomic absorption spectrometry (HG AAS). Copyright © 2014 Elsevier Ltd. All rights reserved.

  2. Electrochemical behavior of labetalol at an ionic liquid modified carbon paste electrode and its electrochemical determination

    Directory of Open Access Journals (Sweden)

    Zhang Yan-Mei

    2013-01-01

    Full Text Available Electrochemical behavior of labetalol (LBT at carbon paste electrode (CPE and an ionic liquid1-benzyl-3-methylimidazolehexafluorophosphate([BnMIM]PF6modified carbon paste electrode([BnMIM]PF6/CPEin Britton-Robinson buffer solution (pH 2.0 was investigated by cyclic voltammetry (CV and square wave voltammetric (SWV. The experimental results showed that LBT at both the bare CPE and [BnMIM]PF6/CPEshowed an irreversible oxidation process, but at [BnMIM]PF6/CPE its oxidation peak current increased greatly and the oxidation peak potential shifted negatively. The electrode reaction process is a diffusion-controlled process involving one electron transferring accompanied by a participation of one proton at [BnMIM]PF6/CPE. At the same time, the electrochemical kinetic parameters were determined. Under the optimized electrochemical experimental conditions, the oxidation peak currents were proportional to LBT concentration in the range of 7.0 x 10-6-1.0 x 10-4 mol L-1 with the limit of detection(LOD, S/N=3 of 4.810 x 10-8 mol L-1and the limit of quantification(LOQ, S/N=10 of 1.60 x 10-7 mol L-1, respectively. The proposed method was successfully applied in the determination of LBT content in commercial tablet samples.

  3. Electrochemical determination of copper ions in spirit drinks using carbon paste electrode modified with biochar.

    Science.gov (United States)

    Oliveira, Paulo Roberto; Lamy-Mendes, Alyne C; Rezende, Edivaltrys Inayve Pissinati; Mangrich, Antonio Sálvio; Marcolino, Luiz Humberto; Bergamini, Márcio F

    2015-03-15

    This work describes for first time the use of biochar as electrode modifier in combination with differential pulse adsorptive stripping voltammetric (DPAdSV) techniques for preconcentration and determination of copper (II) ions in spirit drinks samples (Cachaça, Vodka, Gin and Tequila). Using the best set of the experimental conditions a linear response for copper ions in the concentration range of 1.5 × 10(-6) to 3.1 × 10(-5) mol L(-1) with a Limit of Detection (LOD) of 4.0 × 10(-7) mol L(-1). The repeatability of the proposed sensor using the same electrode surface was measured as 3.6% and 6.6% using different electrodes. The effect of foreign species on the voltammetric response was also evaluated. Determination of copper ions content in different samples of spirit drinks samples was also realized adopting inductively coupled plasma optical emission spectroscopy (ICP-OES) and the results achieved are in agreement at a 95% of confidence level. Copyright © 2014 Elsevier Ltd. All rights reserved.

  4. A modified FOX-1 method for Micro-determination of hydrogen peroxide in honey samples.

    Science.gov (United States)

    Li, Dan; Wang, Meng; Cheng, Ni; Xue, Xiaofeng; Wu, Liming; Cao, Wei

    2017-12-15

    Hydrogen peroxide (H 2 O 2 ) is a major antibacterial activity-associated biomarker in honey. Measurement of endogenous H 2 O 2 in honey is of great value in prediction of the H 2 O 2 -depended antibacterial activity and characterization or selection of honey samples for their use as an antibacterial agent or natural food preservative. Considering current methods for H 2 O 2 determination are either time-consuming or complicated with their high-cost, a study was conducted to modify and validate the spectrophotometry-based ferrous oxidation-xylenol orange (FOX-1) method for micro-determination of H 2 O 2 in honey samples. The result suggested that the proposed FOX-1 method is fast, sensitive, precise and repeatable. The method was successfully applied for the analysis of a total of 35 honey samples from 5 floral origins and 33 geographical origins. The proposed method is low-cost and easy-to-run, and it can be considered by researchers and industry for routine analysis. Copyright © 2017 Elsevier Ltd. All rights reserved.

  5. Ultrasensitive Determination of Piroxicam at Diflunisal-Derived Gold Nanoparticle-Modified Glassy Carbon Electrode

    Science.gov (United States)

    Shaikh, Tayyaba; uddin, SiraJ; Talpur, Farah N.; Khaskeli, Abdul R.; Agheem, Muhammad H.; Shah, Muhammad R.; Sherazi, Tufail H.; Siddiqui, Samia

    2017-10-01

    We present a simple and green approach for synthesis of gold nanoparticles (AuNps) using analgesic drug diflunisal (DF) as capping and stabilizing agent in aqueous solution. Characterization of the synthesized diflunisal-derived gold nanoparticles (DF-AuNps) was performed by ultraviolet-visible (UV-Vis) spectroscopy, revealing the surface plasmon absorption band at 520 nm under optimized experimental conditions. Fourier-transform infrared (FTIR) spectroscopy established the effective interaction of the capping agent with the AuNps. Topographical features of the synthesized DF-AuNps were assessed by atomic force microscopy (AFM), revealing average particle height of 29 nm to 32 nm. X-ray diffractometry was used to study the crystalline nature, revealing that the synthesized DF-AuNps possessed excellent crystalline properties. The synthesized DF-AuNps were employed to modify the surface of glassy carbon electrode (GCE) for selective determination of piroxicam (PX) using differential pulse voltammetry technique. The fabricated Nafion/DF-AuNps/GCE sensor exhibited high sensitivity compared with bare GCE. The current response of the fabricated sensor was found to be linear in the PX concentration range of 0.5 μM to 50 μM, with limit of detection (LOD) and limit of quantification (LOQ) of 50 nM and 150 nM, respectively. The proposed sensor was successfully utilized for sensitive and rapid determination of PX in human serum, urine, and pharmaceutical samples.

  6. A modified differential scanning calorimetry for determination of cell volumetric change during the freezing process.

    Science.gov (United States)

    Luo, Dawei; Han, Xu; He, Liqun; Cui, Xiangdong; Cheng, Shuxia; Lu, Caicheng; Liu, Jianghan; Gao, Dayong

    2002-01-01

    A modified analytical and experimental method using differential scanning calorimeter (DSC) was developed to determine the cell volume change during the freezing process. Two cell types were used in the study: human platelets and erythrocytes (red blood cells). Isotonic cell suspensions with different cytocrits were prepared and used in the DSC experiments. Low cooling rates were used to avoid intracellular ice formation. Cell suspensions were cooled from room temperature to -40 degrees C. Latent heat release from the freezing of cell suspensions was shown to be a linear function of cytocrit. From slope and intercept of the linear function, cell volume change was determined based on a developed theoretical model. From experimental data and theoretical analyses, it was revealed that (a) the final volume of a human platelet at -40 degrees C was 33.7% of its isotonic volume, and 15.2% of the original (at isotonic condition) intracellular water remained unfrozen inside platelets, and (b) the final volume of human erythrocyte at -40 degrees C was 50.0% of its isotonic volume, and 30.3% of the original intracellular water was kept inside cells as residual unfrozen water.

  7. Adherence to the oral contraceptive pill: a cross-sectional survey of modifiable behavioural determinants

    Directory of Open Access Journals (Sweden)

    Molloy Gerard J

    2012-10-01

    Full Text Available Abstract Background Poor adherence to the oral contraceptive pill (OCP is reported as one of the main causes of unintended pregnancy in women that rely on this form of contraception. This study aims to estimate the associations between a range of well-established modifiable psychological factors and adherence to OCP. Method A cross-sectional survey of 130 female University students currently using OCP (Mean age: 20.46 SD: 3.01, range 17–36 was conducted. An OCP specific Medication Adherence Report Scale was used to assess non-adherence. Psychological predictor measures included necessity and concern beliefs about OCP, intentions, perceived behavioural control (pbc, anticipated regret and action and coping planning. Multiple linear regression was used to analyse the data. Results Fifty-two per cent of participants reported missing their OCP once or more per month and 14% twice or more per month. In bivariate analysis intentions (r = −0.25, perceived behavioural control (r= −0.66, anticipated regret (r=0.20, concerns about OCP (r =0.31, and action (r= −0.25 and coping (r= −0.28 planning were all significantly associated with adherence to OCP in the predicted direction. In a multivariate model almost half (48% of the variation in OCP adherence could be explained. The strongest and only statistically significant predictors in this model were perceived behavioural control (β=−0.62, p Conclusion The present data point to a number of key modifiable psychological determinants of OCP use. Future work will establish whether changing these variables results in better adherence to the OCP.

  8. Alizarin red S functionalized mesoporous silica modified glassy carbon electrode for electrochemical determination of anthracene

    International Nuclear Information System (INIS)

    Liu, Shan; Wei, Maochao; Zheng, Xiangli; Xu, Shuai; Xia, Fangquan; Zhou, Changli

    2015-01-01

    Highlights: • Alizarin red S-SBA15 composite was prepared and characterized. • A novel sensing platform was constructed for anthracene determination. • The proposed sensor exhibited high sensitivity and low detection limit for detecting anthracene. • This method can be applied to the practical detection of anthracene in waste water. - Abstract: In the paper, a novel and sensitive electrochemical sensor based on modification of electroactive alizarin red S functionalized mesoporous silica material SBA15 onto glassy carbon electrode (ARS-SBA15/GCE) was developed. Alizarin red S, called electrochemical probe that can selectively recognize polycyclic aromatic hydrocarbons (PAHs), as tools for the detection of tricyclic aromatic hydrocarbon anthracene. The morphology and interface property of ARS modified SBA15 (ARS-SBA15) were examined by transmission electron microscopy (TEM) and fourier transform infrared spectroscopy (FTIR). Taking advantage of the π-π stacking force between alizarin red S and anthracene, the ARS-SBA15/GCE sensor could detect anthracene quantitatively in a wide range of 1.0 pM–10.0 nM and a low detection limit of 0.5 pM (S/N = 3). Other PAHs, such as naphthalene, phenanthrene, pyrene, and benzo[a]pyrene show little interference on the detection. Consequently, a simple and sensitive electrochemical method was proposed for the determination of anthracene, which can be used to determine anthracene in waste water samples. The electrochemical method provides a general tool that complements the commonly used spectroscopic methods and immune method for the detection of PAHs

  9. Electrocatalytic Determination of Isoniazid by a Glassy Carbon Electrode Modified with Poly (Eriochrome Black T)

    OpenAIRE

    Karim Asadpour-Zeynali; Venus Baghalabadi

    2017-01-01

    In this work poly eriochrome black T (EBT) was electrochemically synthesized on the glassy carbon electrode as electrode modifier. On the modified electrode, voltammetric behavior of isoniazid (INH) was investigated. The poly (EBT)-modified glassy carbon electrode has excellent electrocatalytic ability for the electrooxidation of isoniazid. This fact was appeared as a reduced overpotential of INH oxidation in a wide operational pH range from 2 to 13. It has been found that the catalytic peak ...

  10. Direct determination of cadmium in Orujo spirit samples by electrothermal atomic absorption spectrometry: Comparative study of different chemical modifiers

    Energy Technology Data Exchange (ETDEWEB)

    Vilar Farinas, M. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Barciela Garcia, J. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Garcia Martin, S. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Pena Crecente, R. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Herrero Latorre, C. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain)]. E-mail: cherrero@lugo.usc.es

    2007-05-22

    In this work, several analytical methods are proposed for cadmium determination in Orujo spirit samples using electrothermal atomic absorption spectrometry (ETAAS). Permanent chemical modifiers thermally coated on the platforms inserted in pyrolytic graphite tubes (such as W, Ir, Ru, W-Ir and W-Ru) were comparatively studied in relation to common chemical modifier mixtures [Pd-Mg(NO{sub 3}){sub 2} and (NH{sub 4})H{sub 2}PO{sub 4}-Mg(NO{sub 3}){sub 2}] for cadmium stabilization. Different ETAAS Cd determination methods based on the indicated modifiers have been developed. In each case, pyrolysis and atomization temperatures, atomization shapes, characteristic masses and detection limits as well as other analytical characteristics have been determined. All the assayed modifiers (permanent and conventional) were capable of achieving the appropriate stabilization of the analyte, with the exception of Ru and W-Ru. Moreover, for all developed methods, recoveries (99-102%) and precision (R.S.D. lower than 10%) were acceptable. Taking into account the analytical performance (best detection limit LOD = 0.01 {mu}g L{sup -1}), the ETAAS method based on the use of W as a permanent modifier was selected for further direct Cd determinations in Orujo samples from Galicia (NW Spain). The chosen method was applied in the determination of the Cd content in 38 representative Galician samples. The cadmium concentrations ranged

  11. Direct determination of cadmium in Orujo spirit samples by electrothermal atomic absorption spectrometry: Comparative study of different chemical modifiers

    International Nuclear Information System (INIS)

    Vilar Farinas, M.; Barciela Garcia, J.; Garcia Martin, S.; Pena Crecente, R.; Herrero Latorre, C.

    2007-01-01

    In this work, several analytical methods are proposed for cadmium determination in Orujo spirit samples using electrothermal atomic absorption spectrometry (ETAAS). Permanent chemical modifiers thermally coated on the platforms inserted in pyrolytic graphite tubes (such as W, Ir, Ru, W-Ir and W-Ru) were comparatively studied in relation to common chemical modifier mixtures [Pd-Mg(NO 3 ) 2 and (NH 4 )H 2 PO 4 -Mg(NO 3 ) 2 ] for cadmium stabilization. Different ETAAS Cd determination methods based on the indicated modifiers have been developed. In each case, pyrolysis and atomization temperatures, atomization shapes, characteristic masses and detection limits as well as other analytical characteristics have been determined. All the assayed modifiers (permanent and conventional) were capable of achieving the appropriate stabilization of the analyte, with the exception of Ru and W-Ru. Moreover, for all developed methods, recoveries (99-102%) and precision (R.S.D. lower than 10%) were acceptable. Taking into account the analytical performance (best detection limit LOD = 0.01 μg L -1 ), the ETAAS method based on the use of W as a permanent modifier was selected for further direct Cd determinations in Orujo samples from Galicia (NW Spain). The chosen method was applied in the determination of the Cd content in 38 representative Galician samples. The cadmium concentrations ranged -1

  12. Coulometric determination of dissolved hydrogen with a multielectrolytic modified carbon felt electrode-based sensor.

    Science.gov (United States)

    Matsuura, Hiroaki; Yamawaki, Yosuke; Sasaki, Kosuke; Uchiyama, Shunichi

    2013-06-01

    A multielectrolytic modified carbon electrode (MEMCE) was fabricated by the electrolytic-oxidation/reduction processes. First, the functional groups containing nitrogen atoms such as amino group were introduced by the electrode oxidation of carbon felt electrode in an ammonium carbamate aqueous solution, and next, this electrode was electroreduced in sulfuric acid. The redox waves between hydrogen ion and hydrogen molecule at highly positive potential range appeared in the cyclic voltammogram obtained by MEMCE. A coulometric cell using MEMCE with a catalytic activity of electrooxidation of hydrogen molecule was constructed and was used for the measurement of dissolved hydrogen. The typical current vs. time curve was obtained by the repetitive measurement of the dissolved hydrogen. These curves indicated that the measurement of dissolved hydrogen was finished completely in a very short time (ca. 10 sec). A linear relationship was obtained between the electrical charge needed for the electrooxidation process of hydrogen molecule and dissolved hydrogen concentration. This indicates that the developed coulometric method can be used for the determination of the dissolved hydrogen concentration.

  13. Determination of polyphenol content and colour index in wines through PEDOT-modified electrodes.

    Science.gov (United States)

    Pigani, Laura; Rioli, Cristina; Foca, Giorgia; Ulrici, Alessandro; Seeber, Renato; Terzi, Fabio; Zanardi, Chiara

    2016-10-01

    Poly(3,4-ethylenedioxythiophene)-modified electrodes have been used for the estimation of the polyphenolic content and of the colour index of different samples of wines. Synthetic wine solutions, prepared with different amount of oenocyanins, have been analysed spectrophotometrically and electrochemically in order to find a correlation between the total polyphenolic content or colour index and the current peak. The regression curves obtained have been used as external calibration lines for the analysis of several commercial wines, ranging from white to dark red wines. In this way, a rapid estimation of the total polyphenolic content and of the colour index may be accomplished from a single voltammetric measurement. Furthermore, principal component analysis has also been used to evaluate the effect of total polyphenolic content and colour index on the whole voltammetric signals within a selected potential range, both for the synthetic solutions and for the commercial products. Graphical abstract Electrochemical sensors for the rapid determination of colour index and polyphenol content in wines.

  14. Nonenzymatic amperometric determination of glucose by CuO nanocubes-graphene nanocomposite modified electrode.

    Science.gov (United States)

    Luo, Liqiang; Zhu, Limei; Wang, Zhenxin

    2012-12-01

    Here, we report a nonenzymatic amperometric glucose sensor based on copper oxide (CuO) nanocubes-graphene nanocomposite modified glassy carbon electrode (CuO-G-GCE). In this case, the graphene sheets were cast on the GCE directly. CuO nanocubes were obtained by oxidizing electrochemically deposited Cu on the graphene. The morphology of CuO-G nanocomposite was characterized by scanning electron microscopy. The CuO-G-GCE-based sensor exhibited excellent electrocatalytic activity and high stability for glucose oxidation. Under optimized conditions, the linearity between the current response and the glucose concentration was obtained in the range of 2μM to 4mM with a detection limit of 0.7μM (S/N=3), and a high sensitivity of 1360μAmM(-1)cm(-2). The proposed electrode showed a fast response time (less than 5s) and a good reproducibility. The as-made sensor was applied to determine the glucose levels in clinic human serum samples with satisfactory results. In addition, the effects of common interfering species, including ascorbic acid, uric acid, dopamine and other carbohydrates, on the amperometric response of the sensor were investigated and discussed in detail. Copyright © 2012 Elsevier B.V. All rights reserved.

  15. Determination of baroreflex sensitivity during the modified Oxford maneuver by trigonometric regressive spectral analysis.

    Directory of Open Access Journals (Sweden)

    Julia Gasch

    Full Text Available BACKGROUND: Differences in spontaneous and drug-induced baroreflex sensitivity (BRS have been attributed to its different operating ranges. The current study attempted to compare BRS estimates during cardiovascular steady-state and pharmacologically stimulation using an innovative algorithm for dynamic determination of baroreflex gain. METHODOLOGY/PRINCIPAL FINDINGS: Forty-five volunteers underwent the modified Oxford maneuver in supine and 60° tilted position with blood pressure and heart rate being continuously recorded. Drug-induced BRS-estimates were calculated from data obtained by bolus injections of nitroprusside and phenylephrine. Spontaneous indices were derived from data obtained during rest (stationary and under pharmacological stimulation (non-stationary using the algorithm of trigonometric regressive spectral analysis (TRS. Spontaneous and drug-induced BRS values were significantly correlated and display directionally similar changes under different situations. Using the Bland-Altman method, systematic differences between spontaneous and drug-induced estimates were found and revealed that the discrepancy can be as large as the gain itself. Fixed bias was not evident with ordinary least products regression. The correlation and agreement between the estimates increased significantly when BRS was calculated by TRS in non-stationary mode during the drug injection period. TRS-BRS significantly increased during phenylephrine and decreased under nitroprusside. CONCLUSIONS/SIGNIFICANCE: The TRS analysis provides a reliable, non-invasive assessment of human BRS not only under static steady state conditions, but also during pharmacological perturbation of the cardiovascular system.

  16. A bimetallic nanocomposite modified genosensor for recognition and determination of thalassemia gene.

    Science.gov (United States)

    Hamidi-Asl, Ezat; Raoof, Jahan Bakhsh; Naghizadeh, Nahid; Akhavan-Niaki, Haleh; Ojani, Reza; Banihashemi, Ali

    2016-10-01

    The main roles of DNA in the cells are to maintain and properly express genetic information. It is important to have analytical methods capable of fast and sensitive detection of DNA damage. DNA hybridization sensors are well suited for diagnostics and other purposes, including determination of bacteria and viruses. Beta thalassemias (βth) are due to mutations in the β-globin gene. In this study, an electrochemical biosensor which detects the sequences related to the β-globin gene issued from real samples amplified by polymerase chain reaction (PCR) is described for the first time. The biosensor relies on the immobilization of 20-mer single stranded oligonucleotide (probe) related to βth sequence on the carbon paste electrode (CPE) modified by 15% silver (Ag) and platinum (Pt) nanoparticles to prepare the bimetallic nanocomposite electrode and hybridization of this oligonucleotide with its complementary sequence (target). The extent of hybridization between the probe and target sequences was shown by using linear sweep voltammetry (LSV) with methylene blue (MB) as hybridization indicator. The selectivity of sensor was investigated using PCR samples containing non-complementary oligonucleotides. The detection limit of biosensor was calculated about 470.0pg/μL. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. Voltammetric Determination of Codeine on Glassy Carbon Electrode Modified with Nafion/MWCNTs

    Directory of Open Access Journals (Sweden)

    Robert Piech

    2015-01-01

    Full Text Available A glassy carbon electrode modified with a Nafion/MWCNTs composite is shown to enable the determination of codeine using differential pulse voltammetry in phosphate buffer of pH 3.0. At a preconcentration time of 15 s, the calibration graph is linear in the 0.5 µM (0.15 mg·L−1 to 15 µM (4.5 mg·L−1 concentration range with a correlation coefficient of 0.998. The detection limit at a preconcentration time of 120 s is as low as 4.5 μg·L−1. The repeatability of the method at a 0.6 μg·L−1 concentration level, expressed as the RSD, is 3.7% (for n=5. The method was successfully applied and validated by analyzing codeine in drug, human plasma, and urine samples.

  18. Carbon nanotubes paste sensor modified with bismuth film for determination of metallic ions in ethanol fuel

    Directory of Open Access Journals (Sweden)

    Felipe Augusto Gorla

    2015-05-01

    Full Text Available In the present study an anodic stripping voltammetric method using a bismuth film modified carbon nanotubes paste electrode for simultaneous determination of metals Zn2+, Cd2+and Pb2+in ethanol fuel is described. The metallic ions were preconcentrated on the bismuth film in the time and deposition potential of 500 s and -1.2 V and the stripping step was carried out by square wave voltammetry (frequency of 15 Hz, pulse amplitude of 25 mV and potential step of 5 mV. Acetate buffer at 0.1 mol L-1concentration and pH 4.5 was used as support electrolyte. The method showed linearity including the analytical blank up to 48.39 ?g L-1 for the metals and the obtained limits of detection were 3.36, 0.32 and 0.47 ?g L-1for Zn2+, Cd2+and Pb2+, respectively. The proposed method was applied in ethanol fuel samples.

  19. Molecular imprinted polypyrrole modified glassy carbon electrode for the determination of tobramycin

    International Nuclear Information System (INIS)

    Gupta, Vinod Kumar; Yola, Mehmet Lütfi; Özaltın, Nuran; Atar, Necip; Üstündağ, Zafer; Uzun, Lokman

    2013-01-01

    Graphical abstract: Atomic force microscopic images of (A) bare GCE and (B) TOB imprinted PPy/GCE surface. - Highlights: • Glassy carbon electrode based on molecularly imprinted polypyrrole was prepared. • The developed surfaces were characterized by AFM, FTIR, EIS and CV. • The developed nanosensor was applied to egg and milk samples. - Abstract: Over the past two decades, molecular imprinted polymers have attracted a broad interest from scientists in sensor development. In the preparation of molecular imprinted polymers the desired molecule (template) induces the creation of specific recognition sites in the polymer. In this study, the glassy carbon electrode (GCE) based on molecularly imprinted polypyrrole (PPy) was fabricated for the determination of tobramycin (TOB). The developed electrode was prepared by incorporation of a template molecule (TOB) during the electropolymerization of pyrrole on GCE in aqueous solution using cyclic voltammetry (CV) method. The performance of the imprinted and non-imprinted electrodes was evaluated by square wave voltammetry (SWV). The effect of pH, monomer and template concentrations, electropolymerization cycles on the performance of the imprinted and non-imprinted electrodes was investigated and optimized. The non-modified and TOB-imprinted surfaces were characterized by using atomic force microscopy (AFM), Fourier transform infrared spectroscopy (FTIR), electrochemical impedance spectroscopy (EIS) and CV. The linearity range of TOB was 5.0 × 10 −10 –1.0 × 10 −8 M with the detection limit of 1.4 × 10 −10 M. The developed nanosensor was applied successfully for the determination of TOB in egg and milk

  20. Environmental enrichment imparts disease-modifying and transgenerational effects on genetically-determined epilepsy and anxiety.

    Science.gov (United States)

    Dezsi, Gabi; Ozturk, Ezgi; Salzberg, Michael R; Morris, Margaret; O'Brien, Terence J; Jones, Nigel C

    2016-09-01

    The absence epilepsies are presumed to be caused by genetic factors, but the influence of environmental exposures on epilepsy development and severity, and whether this influence is transmitted to subsequent generations, is not well known. We assessed the effects of environmental enrichment on epilepsy and anxiety outcomes in multiple generations of GAERS - a genetic rat model of absence epilepsy that manifests comorbid elevated anxiety-like behaviour. GAERS were exposed to environmental enrichment or standard housing beginning either prior to, or after epilepsy onset, and underwent EEG recordings and anxiety testing. Then, we exposed male GAERS to early enrichment or standard housing and generated F1 progeny, which also underwent EEG recordings. Hippocampal CRH mRNA expression and DNA methylation were assessed using RT-PCR and pyrosequencing, respectively. Early environmental enrichment delayed the onset of epilepsy in GAERS, and resulted in fewer seizures in adulthood, compared with standard housed GAERS. Enrichment also reduced the frequency of seizures when initiated in adulthood. Anxiety levels were reduced by enrichment, and these anti-epileptogenic and anxiolytic effects were heritable into the next generation. We also found reduced expression of CRH mRNA in GAERS exposed to enrichment, but this was not due to changes in DNA methylation. Environmental enrichment produces disease-modifying effects on genetically determined absence epilepsy and anxiety, and these beneficial effects are transferable to the subsequent generation. Reduced CRH expression was associated with these phenotypic improvements. Environmental stimulation holds promise as a naturalistic therapy for genetically determined epilepsy which may benefit subsequent generations. Copyright © 2016 Elsevier Inc. All rights reserved.

  1. Determination of cyanide in wastewaters using modified glassy carbon electrode with immobilized silver hexacyanoferrate nanoparticles on multiwall carbon nanotube

    International Nuclear Information System (INIS)

    Noroozifar, Meissam; Khorasani-Motlagh, Mozhgan; Taheri, Aboozar

    2011-01-01

    Research highlights: → GC electrode modified with silver hexacyanoferrate nanoparticles (SHFNPs) immobilized on MWCNT. → Modified electrode use for determination of Cyanide in waste water. → The detection limit of the sensor is 8.3 nM. → The linear range is from 40.0 nM to 150.0 μM. - Abstract: The sensitive determination of cyanide in wastewaters using modified GC electrode with silver hexacyanoferrate nanoparticles (SHFNPs) immobilized on multiwall carbon nanotube (MWCNT) was reported. The immobilization of SHFNPs on MWCNT was confirmed by transmission electron microscopy (TEM). The TEM image showed that the SHFNPs retained the spherical morphology after immobilized on MWCNT. The size of SHFNPs was examined around 27 nm. The GC/MWCNT-SHFNPs was used for the determination of cyanide in borax buffer (BB) solution (pH 8.0). Using square wave voltammetry, the current response of cyanide increases linearly while increasing its concentration from 40.0 nM to 150.0 μM and a detection limit was found to be 8.3 nM (S/N = 3). The present modified electrode was also successfully used for the determination of 5.0 μM cyanide in the presence of common contaminants at levels presenting in industrial wastewaters. The practical application of the present modified electrode was demonstrated by measuring the concentration of cyanide in industrial wastewater samples. Moreover, the studied sensor exhibited high sensitivity, good reproducibility and long-term stability.

  2. Modified APHA closed-tube reflux colorimetric method for TOC determination in water and wastewater.

    Science.gov (United States)

    Salihu, Simon Olonkwoh; Bakar, Nor Kartini Abu

    2018-05-30

    The analysis of total organic carbon (TOC) by the American Public Health Association (APHA) closed-tube reflux colorimetric method requires potassium dichromate (K 2 Cr 2 O 7 ), silver sulfate (AgSO 4 ), and mercury (HgSO 4 ) sulfate in addition to large volumes of both reagents and samples. The method relies on the release of oxygen from dichromate on heating which is consumed by carbon associated with organic compounds. The method risks environmental pollution by discharging large amounts of chromium (VI) and silver and mercury sulfates. The present method used potassium monochromate (K 2 CrO 4 ) to generate the K 2 Cr 2 O 7 on demand in the first phase. In addition, miniaturizing the procedure to semi microanalysis decreased the consumption of reagents and samples. In the second phase, mercury sulfate was eliminated as part of the digestion mixture through the introduction of sodium bismuthate (NaBiO 3 ) for the removal of chlorides from the sample. The modified method, the potassium monochromate closed-tube colorimetry with sodium bismuthate chloride removal (KMCC-Bi), generates the potassium dichromate on demand and eliminates mercury sulfate. The semi microanalysis procedure leads to a 60% reduction in sample volume and ≈ 33.33 and 60% reduction in monochromate and silver sulfate consumption respectively. The LOD and LOQ were 10.17 and 33.90 mg L -1 for APHA, and 4.95 and 16.95 mg L -1 for KMCC-Bi. Recovery was between 83 to 98% APHA and 92 to 104% KMCC-Bi, while the RSD (%) ranged between 0.8 to 5.0% APHA and 0.00 to 0.62% KMCC-Bi. The method was applied for the UV-Vis spectrometry determination of COD in water and wastewater. Statistics was done by MINITAB 17 or MS Excel 2016. ᅟ Graphical abstract.

  3. Electrocatalytic oxidation of deferiprone and its determination on a carbon nanotube-modified glassy carbon electrode

    Energy Technology Data Exchange (ETDEWEB)

    Yadegari, H. [Department of Chemistry, Faculty of Science, K.N. Toosi University of Technology, P.O. Box 16315-1618, Tehran (Iran, Islamic Republic of); Jabbari, A. [Department of Chemistry, Faculty of Science, K.N. Toosi University of Technology, P.O. Box 16315-1618, Tehran (Iran, Islamic Republic of)], E-mail: jabbari@kntu.ac.ir; Heli, H.; Moosavi-Movahedi, A.A. [Institute of Biochemistry and Biophysics, University of Tehran, Tehran (Iran, Islamic Republic of); Karimian, K. [Arasto Pharmaceutical Chemicals Inc., Tehran (Iran, Islamic Republic of); Khodadadi, A. [Department of Chemical Engineering, Faculty of Engineering, University of Tehran, Tehran (Iran, Islamic Republic of)

    2008-02-15

    The electrochemical behavior of the anti-thalassemia and anti-HIV replication drug, deferiprone, was investigated on a carbon nanotube-modified glassy carbon (GC-CNT) electrode in phosphate buffer solution, pH 7.40 (PBS). During oxidation of deferiprone, two irreversible anodic peaks, with E{sub 1}{sup 0}=452 and E{sub 2}{sup 0}=906mV, appeared, using GC-CNT. Cyclic voltammetric study indicated that the oxidation process is irreversible and diffusion controlled. The number of exchanged electrons in the electro-oxidation process was obtained, and the data indicated that deferiprone is oxidized via two two-electron steps. The results revealed that carbon nanotube (CNT) promotes the rate of oxidation by increasing the peak current, so that deferiprone is oxidized at lower potentials, which thermodynamically is more favorable. This result was confirmed by impedance measurements. The diffusion coefficient, electron-transfer coefficient and heterogeneous electron-transfer rate constant of deferiprone were found to be 1.49 x 10{sup -6} cm{sup 2} s{sup -1}, 0.44, and 3.83 x 10{sup -3} cm s{sup -1}, respectively. A sensitive, simple and time-saving differential-pulse voltammetric procedure was developed for the analysis of deferiprone. Using the proposed method, deferiprone can be determined with a detection limit of 5.25 x 10{sup -7} M. The applicability of the method to direct assays of spiked human serum and urine fluids is described.

  4. ELECTROCHEMICAL DETERMINATION OF HYDROGEN SULFIDE AT CARBON NANOTUBE MODIFIED ELECTRODES. (R830900)

    Science.gov (United States)

    Carbon nanotube (CNT) modified glassy carbon electrodes exhibiting a strong and stable electrocatalytic response towards sulfide are described. A substantial (400 mV) decrease in the overvoltage of the sulfide oxidation reaction (compared to ordinary carbon electrodes) is...

  5. Parent-child mediated learning interactions as determinants of cognitive modifiability: recent research and future directions.

    Science.gov (United States)

    Tzuriel, D

    1999-05-01

    The main objectives of this article are to describe the effects of mediated learning experience (MLE) strategies in mother-child interactions on the child's cognitive modifiability, the effects of distal factors (e.g., socioeconomic status, mother's intelligence, child's personality) on MLE interactions, and the effects of situational variables on MLE processes. Methodological aspects of measurement of MLE interactions and of cognitive modifiability, using a dynamic assessment approach, are discussed. Studies with infants showed that the quality of mother-infant MLE interactions predict later cognitive functioning and that MLE patterns and children's cognitive performance change as a result of intervention programs. Studies with preschool and school-aged children showed that MLE interactions predict cognitive modifiability and that distal factors predict MLE interactions but not the child's cognitive modifiability. The child's cognitive modifiability was predicted by MLE interactions in a structured but not in a free-play situation. Mediation for transcendence (e.g., teaching rules and generalizations) appeared to be the strongest predictor of children's cognitive modifiability. Discussion of future research includes the consideration of a holistic transactional approach, which refers to MLE processes, personality, and motivational-affective factors, the cultural context of mediation, perception of the whole family as a mediational unit, and the "mediational normative scripts."

  6. Highly sensitive determination of hydroxylamine using fused gold nanoparticles immobilized on sol-gel film modified gold electrode

    Energy Technology Data Exchange (ETDEWEB)

    Kannan, P. [Department of Chemistry, Gandhigram Rural University, Gandhigram 624302, Dindigul, Tamilnadu (India); John, S. Abraham, E-mail: abrajohn@yahoo.co.in [Department of Chemistry, Gandhigram Rural University, Gandhigram 624302, Dindigul, Tamilnadu (India)

    2010-03-24

    We are reporting the highly sensitive determination of hydroxylamine (HA) using 2-mercapto-4-methyl-5-thiazoleacetic acid (TAA) capped fused spherical gold nanoparticles (AuNPs) modified Au electrode. The fused TAA-AuNPs were immobilized on (3-mercaptopropyl)-trimethoxysilane (MPTS) sol-gel film, which was pre-assembled on Au electrode. The immobilization of fused TAA-AuNPs on MPTS sol-gel film was confirmed by UV-vis absorption spectroscopy and atomic force microscopy (AFM). The AFM image showed that the AuNPs retained the fused spherical morphology after immobilized on sol-gel film. The fused TAA-AuNPs on MPTS modified Au electrode were used for the determination of HA in phosphate buffer (PB) solution (pH = 7.2). When compared to bare Au electrode, the fused AuNPs modified electrode not only shifted the oxidation potential of HA towards less positive potential but also enhanced its oxidation peak current. Further, the oxidation of HA was highly stable at fused AuNPs modified electrode. Using amperometric method, determination of 17.5 nM HA was achieved for the first time. Further, the current response of HA increases linearly while increasing its concentration from 17.5 nM to 22 mM and a detection limit was found to be 0.39 nM (S/N = 3). The present modified electrode was also successfully used for the determination of 17.5 nM HA in the presence of 200-fold excess of common interferents such as urea, NO{sub 2}{sup -}, NH{sub 4}{sup +}, oxalate, Mn{sup 2+}, Na{sup +}, K{sup +}, Mg{sup 2+}, Ca{sup 2+}, Ba{sup 2+} and Cu{sup 2+}. The practical application of the present modified electrode was demonstrated by measuring the concentration of HA in ground water samples.

  7. Application of methane as a gaseous modifier for the determination of silicon using electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Heinrich, Hans-Joachim, E-mail: hans-joachim.heinrich@bam.de; Kipphardt, Heinrich

    2012-04-15

    For determination of silicon in aqueous solutions by electrothermal atomic absorption spectrometry methane/argon mixtures as a gaseous modifier were applied during the pyrolysis step to improve the analytical performance. The beneficial effects observed on thermal stabilization, signal enhancement and shape of absorbance signals were attributed to the thermal decomposition products of methane, which were hydrogen and carbon black (soot). Using a 5% CH{sub 4} mixture with argon, the optimized pyrolysis and atomization temperatures were 1350 Degree-Sign C and 2450 Degree-Sign C, respectively. A flushing step following the pyrolysis was mandatory to avoid background absorption and accelerated deposition of pyrolytic graphite. Characteristic masses of 50 and 30 pg were obtained for standard transversely heated graphite atomizer (THGA) tubes and end-capped THGA tubes, respectively, which were lower than with other previously applied modifiers. A limit of detection of 0.2 {mu}g L{sup -1} (3 s, n = 10) has been obtained. In addition, this gaseous modifier did not contribute to contamination which often was significant when a liquid modifier solution was co-injected. The proposed method has been applied to the determination of silicon in ultrapure water, nitric and hydrochloric acids. - Highlights: Black-Right-Pointing-Pointer CH{sub 4}/Ar gas mixtures act as new modifier in the determination of Si using ET AAS. Black-Right-Pointing-Pointer CH{sub 4} improved thermal stabilization, atomization efficiency and signal shape of Si. Black-Right-Pointing-Pointer Optimum performance by addition of 5% CH{sub 4} during pyrolysis at 1350 Degree-Sign C. Black-Right-Pointing-Pointer Gaseous modifier does not contribute to blank values. Black-Right-Pointing-Pointer Optimized method suitable for determination of Si in ultrapure reagents.

  8. Comparison of renal dynamic imaging and modified MDRD equation in determining the stage of chronic kidney disease patients

    International Nuclear Information System (INIS)

    Xie Peng; Liu Xiaomei; Huang Jianmin; Zhang Fang; Pan Liping; Wu Weijie; Gao Jianqing

    2013-01-01

    Objective: To compare the accuracy of 99 Tc m -diethylene triamine pentaacetic acid ( 99 Tc m -DTPA) renal dynamic imaging and modified modification of diet in renal disease trail (MDRD) equation in determining the stage of the chronic kidney disease (CKD) patients in clinical practice. Methods: A total of 169 patients were enrolled whose glomerular filtration rate (GFR) were determined simultaneously by 3 methods: dual plasma sample clearance method, renal dynamic imaging and modified MDRD equation. The dual plasma sample clearance method was employed as the reference method. The accuracy of the other methods in determining the stage of CKD patients was compared and the comparison was repeated based on the different stages. Results: The accuracy of renal dynamic imaging and modified MDRD equation was 56.80% and 68.64%, respectively (P=0.019<0.05). And only in the stage of uremia, the difference of the above-mentioned two method reached statistical significance (P=0.012<0.05), while in other stages they showed similar performance (P=0.180, 0.424, 0.629 and 0.754, all P>0.05). Conclusion: Modified MDRD equation showed better performance than renal dynamic imaging or as good as the second one in determining the stage of CKD patients and the former one should be the first choice in clinical practice because of its simplicity and economy. (authors)

  9. A binderless, covalently bulk modified electrochemical sensor: Application to simultaneous determination of lead and cadmium at trace level

    Energy Technology Data Exchange (ETDEWEB)

    Gunigollahalli Kempegowda, Raghu [Department of Studies in Chemistry, Bangalore University, Central College Campus, Bangalore 560001 (India); Malingappa, Pandurangappa, E-mail: mprangachem@gmail.com [Department of Studies in Chemistry, Bangalore University, Central College Campus, Bangalore 560001 (India)

    2012-05-30

    Highlights: Black-Right-Pointing-Pointer Proposed sensor is a new type of binderless covalent bulk modified electrode. Black-Right-Pointing-Pointer Surface can be easily renewed by simple mechanical polishing using emery sheets. Black-Right-Pointing-Pointer Free from modifier leaching during electrochemical measurements. Black-Right-Pointing-Pointer Provides long term storage stability with good reproducibility. Black-Right-Pointing-Pointer Nanomolar level detection limit achieved with selectivity. - Abstract: A new type of covalent binderless bulk modified electrode has been fabricated and used in the simultaneous determination of lead and cadmium ions at nanomolar level. The modification of graphitic carbon with 4-amino salicylic acid was carried out under microwave irradiation through the amide bond formation. The electrochemical behavior of the fabricated electrode has been carried out to decipher the interacting ability of the functional moieties present on the modifier molecules toward the simultaneous determination of Pb{sup 2+} and Cd{sup 2+} ions using cyclic and differential pulse anodic stripping voltammetry. The possible mode of interaction of functional groups with metal ions is proposed based on the pKa values of the modifier functionalities present on the surface of graphitic carbon particles. The analytical utility of the proposed sensor has been validated by measuring the lead and cadmium content from pretreated waste water samples of lead acid batteries.

  10. Development of a poly(alizarin red S)/ionic liquid film modified electrode for voltammetric determination of catechol

    International Nuclear Information System (INIS)

    Zhang, Qing; Pan, Dawei; Zhang, Haiyun; Han, Haitao; Kang, Qi

    2014-01-01

    Highlights: • This study is the first to conduct electroploymerization of ARS in RTILs. • BMIMBF 4 was successfully mixed in polymeric ARS film. • PARS/BMIMBF 4 film was tighter, smoother and better electrochemical property. • PARS/BMIMBF 4 /GCE showed superior performance for catechol determination. - Abstract: A novel modified electrode for voltammetric catechol determination was fabricated by electroploymerization of alizarin red S (ARS) onto a glassy carbon electrode (GCE) in one kind of room-temperature ionic liquid (1-butyl-3-methylimidazolium tetrafluoroborate, BMIMBF 4 ). The polymeric ARS/ionic liquid (PARS/BMIMBF 4 ) film modified electrode was characterized by using scanning electron microscope (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR) and electrochemical methods. The EDX, XPS and FTIR results indicated that PARS/BMIMBF 4 film was successfully obtained. Compared with the GCE modified by electroploymerization of ARS in aqueous solution, the GCE modified by electroploymerization of ARS in BMIMBF 4 showed smoother and more compact morphology for coating and better electroanalytical properties. Given the combined electrochemical activity of PARS and excellent conductivity of BMIMBF 4 , the PARS/BMIMBF 4 /GCE has been successfully used for catechol determination by differential pulse voltammetry (DPV) with a linear range of 0.10 to 500 μM. The sensitivity and detection limit are 42 nA/μM and 0.026 μM, respectively. The PARS/BMIMBF 4 modified electrode was successfully applied to the determination of catechol in real water samples and may serve as a simple but high-performance sensor for the determination of some environmental pollutants

  11. DETERMINING LIGHTFASTNESS PROPERTIES OF VEGETABLE TANNINS AND CHEMICAL PROPERTIES OF THE LEATHERS TANNED WITH MODIFIED MIMOSA AND QUEBRACHO

    Directory of Open Access Journals (Sweden)

    OMUR Sukru

    2016-05-01

    Full Text Available The vegetable tannins are the oldest tanning agents used in leather industry. They give their natural character and colour to the leathers which they are applied to, but they have the disadvantage of colour change when they are exposed to light for prolonged times. In this study light fastness properties of leathers tanned with mimosa, quebracho, valonea and chestnut tannins were measured. Lightfastness properties of mimosa and quebracho tannins were found lower. Then these tannins were modified with sulphitation, novalac synthesis and sulphomethylation processes. Lightfastness and determination of volatile matter, determination of matter soluble in dichloromethane, determination of sulphated total ash and sulphated water-insoluble ash, determination of water soluble matter, water soluble inorganic matter and water soluble organic matter, determination of nitrogen content and hide substance, calculation of degree of tannage determination of formaldehyde content analyses were performed to the leathers tanned with modified mimosa and quebracho tannins. From comparison of results, it was understood that sulpmethylation process can be used for production of leathers with higher lightfastness and without major change on chemical properties. When chemical properties of leathers tanned with modified quebracho and mimosa are considered: volatile matter, sulphated total ash and sulphated water- insoluble ash, water soluble matter, water soluble inorganic matter and water soluble organic matter, hide substance and formaldehyde contents were found compatible with standard mimosa and quebracho. However degree of tannage and matter soluble in dichloromethane values were found lower, which means some enhancements in modification or fatliquoring process should be considered.

  12. Nanostructured Modified Electrode for Electrocatalytic Determination of Epinephrine in the Presence of Acetaminophen

    Directory of Open Access Journals (Sweden)

    M. Mazloum-Ardakani

    2011-04-01

    Full Text Available In this paper, a nanostructured modified electrode was fabricated by incorporating of 2,2′-[1,9-nonanediylbis(nitriloethylidyne]-bis-hydroquinone (NNH as a newly synthesized modifier and TiO2 nanoparticles to the carbon paste (MTCPE and then was used for the electroanalysis of epinephrine (EP. The electrochemical studies were carried out by using cyclic voltammetry, chronoamperometry and differential pulse voltammetry (DPV techniques. It has been found that the oxidation of EP at the surface of this electrode occurs at a potential about 235 mV less positive than that of an unmodified carbon paste electrode. A dynamic range of 1.0–2000.0 μM, with a detection limit of 0.37 μM for EP, was obtained using DPV. Also, this modified electrode exhibits well separated oxidation peaks for EP and acetaminophen (AC using DPV.

  13. Amperometric Sensor Used for Determination of Thiocyanate with a Silver Nanoparticles Modified Electrode

    OpenAIRE

    Wang, Guang-Feng; Li, Mao-Guo; Gao, Ying-Chun; Fang, Bin

    2004-01-01

    Abstract: A novel electrode modified with silver nanoparticles was fabricated. It is found that the reducibility of silver nanoparticles is higher than for bulk silver by comparing a silver nanoparticles modified electrode with a silver micro-disk electrode. When SCN- was added, a new oxidation peak occurred and the anodic peak current of silver nanoparticles decreased. The new anodic peak current is proportional to the thiocyanate concentration in the range of 5.0×10-7~4.0×10-4 mol/L i...

  14. Ionic Liquid Crystals Modifier for Selective Determination of Terazosin Antihypertensive Drug in Presence of Common Interference Compounds

    Directory of Open Access Journals (Sweden)

    Nada F. Atta

    2017-01-01

    Full Text Available Electrochemical sensor was fabricated based on carbon paste electrode modified with an ionic liquid crystal ILC (2-chloro-1,3-dimethyl-imidazolidinium hexafluorophosphate in presence of sodium dodecyl sulfate for the selective electrochemical determination of Terazosin (TZ in presence of common interference compounds. The electrode performance was compared in presence of other ionic liquids ILs (1-Butyl-4-methyl pyridinium tetrafluoroborate and (1-n-Hexyl-3-methyl imidazolium tetrafluoroborate. Ultrasensitive determination of Terazosin HCl at the ILC modified electrode in the linear dynamic ranges of 0.002 to 0.09 μmol·L−1 and 0.2 to 30 μmol·L−1 with correlation coefficients 0.996 and 0.995 and LODs 1.69 × 10−11 mol·L−1 and 6.43 × 10−9 mol·L−1, respectively, were obtained. Selective determination of TZ in presence of uric acid and ascorbic acid and simultaneous determination of binary mixtures of TZ/dopamine, TZ/paracetamol and TZ/Morphine were also determined successfully using the modified sensor.

  15. Determining fracture energy parameters of concrete from the modified compact tension test

    Czech Academy of Sciences Publication Activity Database

    Canteli, A.; Castañón, L.; Nieto, B.; Lozano, M.; Holušová, Táňa; Seitl, Stanislav

    2014-01-01

    Roč. 30, OCT (2014), s. 383-393 ISSN 1971-8993 R&D Projects: GA MŠk(CZ) EE2.3.20.0214 Grant - others:interní podpora AV ČR(CZ) M100411204 Institutional support: RVO:68081723 Keywords : Concrete fracture energy * Modified compact tension test * Concrete * Numerical simulation Subject RIV: JL - Materials Fatigue, Friction Mechanics

  16. Grade determination of crumb rubber-modified performance graded asphalt binder.

    Science.gov (United States)

    2013-08-01

    Due to particulates common in crumb rubber-modified asphalt binders, conventional PG grading using the Dynamic : Shear Rheometer (DSR) with a gap height of 1.0 mm may not be valid and in accordance with current specifications. : Asphalt binder testin...

  17. Improvement of Amperometric Sensor Used for Determination of Nitrate with Polypyrrole Nanowires Modified Electrode

    Directory of Open Access Journals (Sweden)

    Shi-chang Wang

    2005-12-01

    Full Text Available Polypyrrole(PPy nanowire modified electrodes were developed by template-freeelectrochemical method based on graphite electrode. The modified electrode wascharacterized by their amperometric response towards nitrate ions. Before reduction ofnitrate ions, electrochemical solid-phase extraction (EC-SPE of nitrate in/on modifiedelectrodes was conducted. It is found that the unusual nanowired structure of polypyrrolelayer (instead of well known cauliflower structure allows us to increase the effectivesurface area of the electrode and subsequently the sensitivity. And the effects ofelectrochemical preparation parameters of PPy nanowire modified electrodes on theircorresponding characters were evaluated. The experimental results show that theelectrochemical preparation parameters of the modified electrodes such as scan rate,polymerization potential, temperature of polymerization solution and polymerization timehave significantly effects on the morphology of PPy nanowires and subsequently effectivesurface area of the electrode and electroreduction current density of nitrate. Thedetermination sensitivity may be varied according to the modification parameters. Under acertain polymerization conditions, the corresponding sensitivity reaches 336.28 mA/M cm2 and the detection limit is 1.52×10-6 M. The proposed method was successfully applied in thedetection of nitrate in the real samples.

  18. Rapid determination of iron oxide content in magnetically modified particulate materials

    Czech Academy of Sciences Publication Activity Database

    Šafařík, Ivo; Nýdlová, L.; Pospíšková, K.; Baldíková, E.; Maděrová, Z.; Šafaříková, Miroslava

    2016-01-01

    Roč. 26, June (2016), s. 114-117 ISSN 1674-2001 Institutional support: RVO:60077344 Keywords : magnetic iron oxide s * magnetic permeability meter * magnetically modified materials Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 2.621, year: 2016

  19. Utilization of organic reagents in the volumetric determination of micro-quantities of iodine

    International Nuclear Information System (INIS)

    Gantchev, N.; Kireva, A.

    1975-01-01

    A method has been developed for the titrimetric determination of micro-quantities of iodine by means of the organic reagents: Chrompyrazol I and Methylene blue. The recommended method is based on the combination of the extraction and volumetric methods and permits the titration of as little as 1 μg of I-/ml. The determination is not impaired by the ions: Br-, Cl-, NO 3 - and SO 4 2 -. (author)

  20. Determination of Thallium(I by Hybrid Mesoporous Silica (SBA-15 Modified Electrode

    Directory of Open Access Journals (Sweden)

    Geeta Rani

    2016-01-01

    Full Text Available Chemically modified mesoporous silica material (SBA-15 was used for the construction of Tl(I selective carbon paste electrode. The best response was found with the electrode containing 10% modifier as electrode material. The electrode has a lower detection limit of 6.0 × 10−9 M in a working concentration range of 1.0 × 10−8–1.0 × 10−1 M. The selectivity coefficient calculated by match potential method (MPM shows the high selectivity of electrode towards Tl(I over other tested ions. The electrode was successfully applied as an indicator electrode for the titration of 0.01 M TlNO3 solution with standards EDTA solution and for sequential titration of mixture of different anions.

  1. Modified Delphi study to determine optimal data elements for inclusion in an emergency management database system

    Directory of Open Access Journals (Sweden)

    A. Jabar

    2012-03-01

    Conclusion: The use of a modified Expert Delphi study achieved consensus in aspects of hospital institutional capacity that can be translated into practical recommendations for implementation by the local emergency management database system. Additionally, areas of non-consensus have been identified where further work is required. This purpose of this study is to contribute to and aid in the development of this new system.

  2. Voltammetric determination of Os(VI)-modified oligo-saccharides at nanomolar level

    Czech Academy of Sciences Publication Activity Database

    Trefulka, Mojmír; Paleček, Emil

    2012-01-01

    Roč. 88, DEC (2012), s. 8-14 ISSN 1567-5394 R&D Projects: GA ČR(CZ) GPP301/10/P548; GA ČR(CZ) GAP301/11/2055; GA MŠk(CZ) ME09038 Institutional research plan: CEZ:AV0Z50040702 Keywords : electroactive labels * mercury electrodes * Os(VI)-modified oligosaccharides Subject RIV: BO - Biophysics Impact factor: 3.947, year: 2012

  3. Piezoelectric sensor for sensitive determination of metal ions based on the phosphate-modified dendrimer

    Science.gov (United States)

    Wang, S. H.; Shen, C. Y.; Lin, Y. M.; Du, J. C.

    2016-08-01

    Heavy metal ions arising from human activities are retained strongly in water; therefore public water supplies must be monitored regularly to ensure the timely detection of potential problems. A phosphate-modified dendrimer film was investigated on a quartz crystal microbalance (QCM) for sensing metal ions in water at room temperature in this study. The chemical structures and sensing properties were characterized by Fourier transform infrared spectroscopy and QCM measurement, respectively. This phosphate-modified dendrimer sensor can directly detect metal ions in aqueous solutions. This novel sensor was evaluated for its capacity to sense various metal ions. The sensor exhibited a higher sensitivity level and shorter response time to copper(II) ions than other sensors. The linear detection range of the prepared QCM based on the phosphate-modified dendrimer was 0.0001 ∼ 1 μM Cu(II) ions (R2 = 0.98). The detection properties, including sensitivity, response time, selectivity, reusability, maximum adsorption capacity, and adsorption equilibrium constants, were also investigated.

  4. Copper separation using modified active carbon before the polarographic determination of Pb, Cd, Ni, Zn and Fe in wastes

    International Nuclear Information System (INIS)

    Rubel, S.; Lada, Z.M.; Golimowski, J.

    1977-01-01

    The investigations on the selective separation of Pb 2+ , Cd 2+ , Ni 2+ , Zn 2+ and Fe 3+ ions from the excess of copper were carried out. For this purpose active carbon modified by Na-diethyldithiocarbamate was used. The manner of DDTK-Na deposition on active carbon has been elaborated. The influence of pH was investigated and it was found that at pH 1(HNO 3 ) copper ions are quantitavely bound on modified carbon whereas other ions (Pb 2+ , Cd 2+ , Ni 2+ , Zn 2+ and Fe 3+ ) remain in the solution and can be determined polarographically. The elaborated method was applied to the determination of mentioned ions in the samples of wastes containing even 100-fold excess of copper. The concentration of copper can not exceed 100 mg/dm 3 . (author)

  5. Determination of lead in water by electrothermal atomic absorption spectrometry with a nickel(II)-ammonium tartrate modifier

    International Nuclear Information System (INIS)

    Sekerka, I.; Lechner, J.F.

    1991-01-01

    A method is described for the determination of low concentrations of lead in water samples. Atomic absorption spectrometry is used with a tungsten ribbon furnace and Zeeman background correction. Interferences are eliminated by the addition of ammonium tartrate and nickel(II) nitrate to the samples to act as a matrix modifier and adjust the pH. The results show the superior performance of this modifier over other types used conventionally. The detection limit is 1 μg l -1 relative standard deviation of -1 can be obtained. The instrumentation is simple and the method is efficient for the determination of lead in various water samples. 25 refs.; 7 figs.; 6 tabs

  6. Highly sensitive interference-free electrochemical determination of pyridoxine at graphene modified electrode: Importance in Parkinson and Asthma treatments.

    Science.gov (United States)

    Raj, M Amal; Gowthaman, N S K; John, S Abraham

    2016-07-15

    To reduce the side effects in the medication of Parkinson and Asthma, pyridoxine (PY) is administered along with l-3,4-dihydroxyphenyl alanine (l-dopa) and theophylline (TP), respectively. However, excessive dosage of PY leads to nervous disorder. Thus, a sensitive and selective electrochemical method was developed for the determination of PY in the presence of major interferences including TP, l-dopa, ascorbic acid (AA) and riboflavin (RB) using electrochemically reduced graphene oxide (ERGO) film modified glassy carbon electrode (GCE) in this paper. The ERGO fabrication process involves the nucleophilic substitution of graphene oxide at basic pH on amine terminal of 1,6-hexadiamine which was pre-assembled on GCE followed by electrochemical reduction. The electrocatalytic activity of the ERGO modified electrode was examined towards the oxidation of PY. It greatly enhanced the oxidation current of PY in contrast to bare and GO modified GCEs due to facile electron transfer besides π-π interaction between ERGO film and PY. Since TP and l-dopa drugs antagonize the drug action of PY, ERGO modified GCE was also used for the simultaneous determination of PY and l-dopa and PY and TP. Further, the selective determination of PY in the presence of other water soluble vitamins such as ascorbic acid and riboflavin was also demonstrated. Using amperometry, detection of 100nM PY was achieved and the detection limit was found to be 5.6×10(-8)M (S/N=3). The practical application of the present method was demonstrated by determining the concentration of PY in human blood serum and commercial drugs. Copyright © 2016 Elsevier Inc. All rights reserved.

  7. Determination of Rhodium(III) Ions by Flame Atomic Absorption Spectrometry after Preconcentration with Modified Magnetic Activated Carbon

    OpenAIRE

    Maryam Fayazi; Masoud Ghanei-Motlagh; Mohammad Ali Taher; Raziyeh Fayazi

    2016-01-01

    A new method for analysis of trace amount of Rh(III) ions by magnetic activated carbon modified with 2,3,5,6-tetra(2-pyridyl)pyrazine (MAC/TPPZ) as the magnetic sorbent has been proposed. The proposed adsorbent was found to be advantageous over conventional solid phase extraction (SPE) in terms of operational simplicity and low time-consuming. The experimental parameters affecting the extraction/preconcentration and determination of the analyte were systematically examined. In order to invest...

  8. Electrocatalytical oxidation and sensitive determination of acetaminophen on glassy carbon electrode modified with graphene–chitosan composite

    International Nuclear Information System (INIS)

    Zheng, Meixia; Gao, Feng; Wang, Qingxiang; Cai, Xili; Jiang, Shulian; Huang, Lizhang; Gao, Fei

    2013-01-01

    The electrochemical behaviors of acetaminophen (ACOP) on a graphene–chitosan (GR–CS) nanocomposite modified glassy carbon electrode (GCE) were investigated by cyclic voltammetry (CV), chronocoulometry (CC) and differential pulse voltammetry (DPV). Electrochemical characterization showed that the GR–CS nanocomposite had excellent electrocatalytic activity and surface area effect. As compared with bare GCE, the redox signal of ACOP on GR–CS/GCE was greatly enhanced. The values of electron transfer rate constant (k s ), diffusion coefficient (D) and the surface adsorption amount (Γ ⁎ ) of ACOP on GR–CS/GCE were determined to be 0.25 s −1 , 3.61 × 10 −5 cm 2 s −1 and 1.09 × 10 −9 mol cm −2 , respectively. Additionally, a 2e − /2H + electrochemical reaction mechanism of ACOP was deduced based on the acidity experiment. Under the optimized conditions, the ACOP could be quantified in the range from 1.0 × 10 −6 to 1.0 × 10 −4 M with a low detection limit of 3.0 × 10 −7 M based on 3S/N. The interference and recovery experiments further showed that the proposed method is acceptable for the determination of ACOP in real pharmaceutical preparations. Highlights: ► A chitosan–graphene nanocomposite modified glassy carbon electrode was prepared. ► The modified electrode was electrochemically characterized by CV and EIS. ► Electro-oxidation of acetaminophen was examined on the modified electrode. ► Sensing analysis of the modified electrode toward acetaminophen was studied

  9. A modified time-of-flight method for precise determination of high speed ratios in molecular beams

    Energy Technology Data Exchange (ETDEWEB)

    Salvador Palau, A.; Eder, S. D., E-mail: sabrina.eder@uib.no; Kaltenbacher, T.; Samelin, B.; Holst, B. [Department of Physics and Technology, University of Bergen, Allégaten 55, 5007 Bergen (Norway); Bracco, G. [Department of Physics and Technology, University of Bergen, Allégaten 55, 5007 Bergen (Norway); CNR-IMEM, Department of Physics, University of Genova, V. Dodecaneso 33, 16146 Genova (Italy)

    2016-02-15

    Time-of-flight (TOF) is a standard experimental technique for determining, among others, the speed ratio S (velocity spread) of a molecular beam. The speed ratio is a measure for the monochromaticity of the beam and an accurate determination of S is crucial for various applications, for example, for characterising chromatic aberrations in focussing experiments related to helium microscopy or for precise measurements of surface phonons and surface structures in molecular beam scattering experiments. For both of these applications, it is desirable to have as high a speed ratio as possible. Molecular beam TOF measurements are typically performed by chopping the beam using a rotating chopper with one or more slit openings. The TOF spectra are evaluated using a standard deconvolution method. However, for higher speed ratios, this method is very sensitive to errors related to the determination of the slit width and the beam diameter. The exact sensitivity depends on the beam diameter, the number of slits, the chopper radius, and the chopper rotation frequency. We present a modified method suitable for the evaluation of TOF measurements of high speed ratio beams. The modified method is based on a systematic variation of the chopper convolution parameters so that a set of independent measurements that can be fitted with an appropriate function are obtained. We show that with this modified method, it is possible to reduce the error by typically one order of magnitude compared to the standard method.

  10. Determination of mechanical properties of PVC foam using a modified Arcan fixture

    DEFF Research Database (Denmark)

    Taher, Siavash Talebi; Thomsen, Ole Thybo; M Dulieu-Barton, Janice

    2012-01-01

    of the fixture and misalignment of the fixture and loading machine are discussed. Thermoelastic stress analysis (TSA) is used to directly examine and validate the uniformity and symmetry of the stress fields obtained for both tensile and shear specimens. To account for the inhomogeneity of the strain field...... conducted using conventional test tensile and shear test fixtures.......The design and development of a modified Arcan fixture (MAF) is described. The purpose of the fixture is to characterize polymer foam materials with respect to their tensile, compressive, shear and bidirectional mechanical properties. The MAF enables the application of pure compression or high...

  11. Determination of Periodic Solution for Tapered Beams with Modified Iteration Perturbation Method

    Directory of Open Access Journals (Sweden)

    Mohammad Mehdi Mashinchi Joubari

    2015-01-01

    Full Text Available In this paper, we implemented the Modified Iteration Perturbation Method (MIPM for approximating the periodic behavior of a tapered beam. This problem is formulated as a nonlinear ordinary differential equation with linear and nonlinear terms. The solution is quickly convergent and does not need to complicated calculations. Comparing the results of the MIPM with the exact solution shows that this method is effective and convenient. Also, it is predicated that MIPM can be potentially used in the analysis of strongly nonlinear oscillation problems accurately.

  12. Fabrication a new modified electrochemical sensor based on Au–Pd bimetallic nanoparticle decorated graphene for citalopram determination

    Energy Technology Data Exchange (ETDEWEB)

    Daneshvar, Leili [Department of Chemistry, Faculty of Sciences, Ferdowsi University of Mashhad, Mashhad (Iran, Islamic Republic of); Rounaghi, Gholam Hossein, E-mail: ghrounaghi@yahoo.com [Department of Chemistry, Faculty of Sciences, Ferdowsi University of Mashhad, Mashhad (Iran, Islamic Republic of); Es' haghi, Zarrin [Department of Chemistry, Faculty of Sciences, Payame Noor University, Mashhad (Iran, Islamic Republic of); Chamsaz, Mahmoud; Tarahomi, Somayeh [Department of Chemistry, Faculty of Sciences, Ferdowsi University of Mashhad, Mashhad (Iran, Islamic Republic of)

    2016-12-01

    This paper proposes a simple approach for sensing of citalopram (CTL) using gold–palladium bimetallic nanoparticles (Au–PdNPs) decorated graphene modified gold electrode. Au–PdNPs were deposited at the surface of a graphene modified gold electrode with simple electrodeposition method. The morphology and the electrochemical properties of the modified electrode were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), atomic force microscopy (AFM), energy dispersion spectroscopy (EDS), electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV) and square wave voltammetry (SWV). The novel sensor exhibited an excellent catalytic activity towards the oxidation of CTL. The oxidation peak current of CTL, was linear in the range of 0.5–50 μM with a detection limit 0.049 μM with respect to concentration of citalopram. The proposed sensor was successfully applied for determination of CTL tablet and human plasma samples with satisfactory results. - Highlights: • A novel sensor based on Au-PdNPs deposited graphene modified gold electrode was fabricated. • The morphology and the electrochemical properties of the sensor were characterized by several methods. • The fabricated sensor was employed for the detection of antidepressant drug CTL with satisfactory results.

  13. Electrothermal atomic absorption spectrometric determination of copper in nickel-base alloys with various chemical modifiers*1

    Science.gov (United States)

    Tsai, Suh-Jen Jane; Shiue, Chia-Chann; Chang, Shiow-Ing

    1997-07-01

    The analytical characteristics of copper in nickel-base alloys have been investigated with electrothermal atomic absorption spectrometry. Deuterium background correction was employed. The effects of various chemical modifiers on the analysis of copper were investigated. Organic modifiers which included 2-(5-bromo-2-pyridylazo)-5-(diethylamino-phenol) (Br-PADAP), ammonium citrate, 1-(2-pyridylazo)-naphthol, 4-(2-pyridylazo)resorcinol, ethylenediaminetetraacetic acid and Triton X-100 were studied. Inorganic modifiers palladium nitrate, magnesium nitrate, aluminum chloride, ammonium dihydrogen phosphate, hydrogen peroxide and potassium nitrate were also applied in this work. In addition, zirconium hydroxide and ammonium hydroxide precipitation methods have also been studied. Interference effects were effectively reduced with Br-PADAP modifier. Aqueous standards were used to construct the calibration curves. The detection limit was 1.9 pg. Standard reference materials of nickel-base alloys were used to evaluate the accuracy of the proposed method. The copper contents determined with the proposed method agreed closely with the certified values of the reference materials. The recoveries were within the range 90-100% with relative standard deviation of less than 10%. Good precision was obtained.

  14. Determination of kojic acid based on the interface enhancement effects of carbon nanotube/alizarin red S modified electrode.

    Science.gov (United States)

    Liu, Jieshu; Zhou, Dazhai; Liu, Xiaopeng; Wu, Kangbing; Wan, Chidan

    2009-04-01

    Based on non-covalent interactions such as pi-pi stacking, van der Waals interactions and strong adsorption, alizarin red S (ARS) interacts with multi-walled carbon nanotubes (MWNT), improving the solubility of MWNT in water and resulting in a stable MWNT/ARS solution. By successive cyclic sweeps between 0.0 and 2.2V in the MWNT/ARS solution, a MWNT/ARS composite film was fabricated on an electrode surface. The electrochemical behaviors of kojic acid at the bare electrode, the ARS film-modified electrode and the MWNT/ARS film-modified electrode were investigated. It was found that the oxidation signal of kojic acid significantly increased at the MWNT/ARS film-modified electrode, which was attributed to the unique properties of MWNT such as large surface area, strong adsorptive ability and subtle electronic character. The effects of pH and cyclic number of electropolymerization were examined. A rapid, sensitive and simple electrochemical method was then developed for the determination of kojic acid. This method exhibits good linearity over the range from 4.0 x 10(-7) to 6.0 x 10(-5)mol L(-1), and the limit of detection is as low as 1.0 x 10(-7)mol L(-1). In order to validate feasibility, the MWNT/ARS film-modified electrode was used for quantitative analysis of kojic acid in food samples.

  15. The influence of pyrolysis and matrix modifiers on determination of Cr and Pb in sediment samples by GFAAS

    Directory of Open Access Journals (Sweden)

    Risfidian Mohadi

    2016-04-01

    Full Text Available Abstract: The Influence of pyrolysis and matrix modifiers on determination of Cr and Pb in sediment samples using graphite furnace atomic absorption spectrometry has been investigated. The sediment samples including three certified reference materials (CRMs are reported. Analyses were performed using microwave assisted dissolution. The matrix modifiers Mg(NO32, Pd+Mg(NO32 and NH4H2PO4were shown to be optimazed. The recovery for Cr and Pb in CRMs in the case of sample dissolution was found to be between 81 to 91% for Cr and 94 to 98% for Pb of the certified values, respectively. Keywords: Sediment, Pyrolysis, Matrix modifiers, Cr, Pb Abstrak (Indonesia: Pengaruh pirolisis dan matriks pengubah pada penentuan Cr dan Pb dalam sampel sedimen menggunakan tungku grafit spektroskopi serapan atom telah diteliti. Sampel sedimen termasuk tiga bahan referensi bersertifikat (CRMs dilaporkan dianalisis dengan menggunakan bantuan microwave ekstraktor. Matriks pengubah Mg(NO32, Pd+Mg(NO32 dan NH4H2PO4 telah digunakan dan menghasilkan nilai temu balik untuk Cr dan Pb dalam CRMs ditemukan antara 81-91% untuk Cr dan 94-98 % untuk Pb dari nilai sertifikat masing-masing. Katakunci: Sedimen, Pirolisis, Matrix modifiers, Cr, Pb

  16. Sensitive and selective determination of Cu2+ at D-penicillamine functionalized nano-cellulose modified pencil graphite electrode

    Science.gov (United States)

    Taheri, M.; Ahour, F.; Keshipour, S.

    2018-06-01

    A novel electrochemical sensor based on D-penicillamine anchored nano-cellulose (DPA-NC) modified pencil graphite electrode was fabricated and used for highly selective and sensitive determination of copper (II) ions in the picomolar concentration by square wave adsorptive stripping voltammetric (SWV) method. The modified electrode showed better and increased SWV response compared to the bare and NC modified electrodes which may be related to the porous structure of modifier along with formation of complex between Cu2+ ions and nitrogen or oxygen containing groups in DPA-NC. Optimization of various experimental parameters influence the performance of the sensor, were investigated. Under optimized condition, DPA-NC modified electrode was used for the analysis of Cu2+ in the concentration range from 0.2 to 50 pM, and a lower detection limit of 0.048 pM with good stability, repeatability, and selectivity. Finally, the practical applicability of DPA-NC-PGE was confirmed via measuring trace amount of Cu (II) in tap and river water samples.

  17. Voltammetric Determination of Guanine on the Electrode Modified by Gold Deposit and Nafion Film

    Directory of Open Access Journals (Sweden)

    L.G. Shaidarova

    2016-09-01

    Full Text Available Electrodeposited gold and Nafion-gold composite on the surface of glassy carbon electrodes (GCE have shown electrocatalytic activity during guanine oxidation. In comparison with the unmodified electrode, decreasing of the oxidation potential by 100 mV and increasing of the current of organic compound oxidation have been observed. When the Nafion (NF film is applied to the surface of the glassy carbon electrode with electrodeposited gold, a five-fold increase of guanine oxidation current has been achieved compared to its oxidation on the modified electrode without the NF film. Conditions have been found for electrodeposition of gold on the surface of the glassy carbon electrode, including that one covered with the NF film, as well as for registration of the maximum catalytic current on these electrodes. Linear dependence of the electrocatalytic response of the modified electrode from the guanine concentration has been observed in the range from 5·10–6 to 5·10–3 mol·L–1 (for Au GCE and from 5·10–7 to 5·10–3 mol·L–1 (for NF-Au GCE.

  18. Differential pulse voltammetric determination of nanomolar concentrations of antiviral drug acyclovir at polymer film modified glassy carbon electrode

    Energy Technology Data Exchange (ETDEWEB)

    Dorraji, Parisa S.; Jalali, Fahimeh, E-mail: fjalali@razi.ac.ir

    2016-04-01

    An electrochemical sensor for the sensitive detection of acyclovir was developed by the electropolymerization of Eriochrome black T at a pretreated glassy carbon electrode. The surface morphology of the modified electrode was characterized by field emission scanning electron microscopy. Under the optimized conditions, a significant electrochemical improvement was observed toward the electrooxidation of acyclovir on the modified electrode surface relative to the unmodified electrode. The detection limit of 12 nM and two linear calibration ranges of 0.03–0.3 μM and 0.3–1.5 μM were obtained for acyclovir determination using a differential pulse voltammetric method in acetate buffer (0.1 M, pH 4.0). Real sample studies were carried out in human blood serum and pharmaceutical formulations, which offered good recovery (98–102%). The electrode showed excellent reproducibility, selectivity and antifouling effects. - Graphical abstract: Eriochrome black T (EBT) was electropolymerized at the surface of a pretreated glassy carbon electrode. The modified electrode enhanced the oxidation current of acyclovir, significantly. The sensor was used in the determination of acyclovir in human blood serum samples and pharmaceutical dosages. - Highlights: • Construction of a voltammetric sensor for acyclovir is described. • Eriochrome black T was electropolymerized at the electrode surface. • The sensor improved the sensitivity of the electrode for monitoring acyclovir. • The recoveries and standard deviations were acceptable in spiked human blood serum. • The proposed sensor had good lifetime to be used in biological matrices.

  19. Simultaneous DPV determination of morphine and codeine using dsDNA modified screen printed electrode strips coupled with electromembrane extraction

    Directory of Open Access Journals (Sweden)

    Rouhollah Feizbakhsh

    2016-01-01

    Full Text Available In this work a sensitive electrochemical sensor for simultaneous determination of morphine and codeine constructed by application of disposable screen printed carbon electrode strips (SPCE modified by double strand (ds calf thymus DNA. According to the results of the modified SPCE strips and experimented parameters, we observed a considerable shift between potentials of morphine and codeine current peaks. Related to these observed shifts, we studied on the effect of the concentration of modifier and pH value on the anodic oxidation pattern of morphine and codeine in the case of optimize the method to get better signals with maximum potential distance. Also to boosting the LODs of this electroanalytical method coupled with an electro-membrane preconcentration (EME step. The calibration curve which was plotted by the variation of differential pulse voltammetry (DPV currents as a function of different morphine and codeine concentration were linear within the range of 0.7– 40 µM and 2.3- 40 µM for morphine and codeine respectively. Also the limits of detection were 0.07 µM and 0.23 µM, respectively. Finally, the proposed method was able to determine morphine and codeine simultaneously and effectively in urinary real samples

  20. Differential pulse voltammetric determination of nanomolar concentrations of antiviral drug acyclovir at polymer film modified glassy carbon electrode

    International Nuclear Information System (INIS)

    Dorraji, Parisa S.; Jalali, Fahimeh

    2016-01-01

    An electrochemical sensor for the sensitive detection of acyclovir was developed by the electropolymerization of Eriochrome black T at a pretreated glassy carbon electrode. The surface morphology of the modified electrode was characterized by field emission scanning electron microscopy. Under the optimized conditions, a significant electrochemical improvement was observed toward the electrooxidation of acyclovir on the modified electrode surface relative to the unmodified electrode. The detection limit of 12 nM and two linear calibration ranges of 0.03–0.3 μM and 0.3–1.5 μM were obtained for acyclovir determination using a differential pulse voltammetric method in acetate buffer (0.1 M, pH 4.0). Real sample studies were carried out in human blood serum and pharmaceutical formulations, which offered good recovery (98–102%). The electrode showed excellent reproducibility, selectivity and antifouling effects. - Graphical abstract: Eriochrome black T (EBT) was electropolymerized at the surface of a pretreated glassy carbon electrode. The modified electrode enhanced the oxidation current of acyclovir, significantly. The sensor was used in the determination of acyclovir in human blood serum samples and pharmaceutical dosages. - Highlights: • Construction of a voltammetric sensor for acyclovir is described. • Eriochrome black T was electropolymerized at the electrode surface. • The sensor improved the sensitivity of the electrode for monitoring acyclovir. • The recoveries and standard deviations were acceptable in spiked human blood serum. • The proposed sensor had good lifetime to be used in biological matrices.

  1. Electrochemistry and determination of epinephrine using a mesoporous Al-incorporated SiO{sub 2} modified electrode

    Energy Technology Data Exchange (ETDEWEB)

    Zeng, Yanhong; Yang, Jinquan; Wu, Kangbing [Department of Chemistry, Huazhong University of Science and Technology, Wuhan 430074 (China)

    2008-05-30

    The potential application of Al-incorporated mesoporous SiO{sub 2} (denoted as Al-MCM-41) in electrochemistry as a novel electrode material was investigated. The peak currents of K{sub 3}[Fe(CN){sub 6}] remarkably increase and the peak potential separation obviously decreases at the mesoporous Al-MCM-41 modified carbon paste electrode (CPE). These phenomena suggest that the mesoporous Al-MCM-41 modified CPE possesses larger electrode area and electron transfer rate constant. Furthermore, the electrochemical behavior of epinephrine (EP) was investigated in different supporting electrolytes such as 0.01 mol L{sup -1} HClO{sub 4} and pH 7.0 phosphate buffer. It is found that the mesoporous Al-MCM-41 modified CPE exhibits catalytic ability to the oxidation of EP due to remarkable peak current enhancement and negative shift of peak potential. The electrochemical oxidation mechanism was also discussed. Finally, a novel electrochemical method was proposed for the determination of EP, which used to determine EP in urine samples. (author)

  2. Electrochemistry and determination of epinephrine using a mesoporous Al-incorporated SiO{sub 2} modified electrode

    Energy Technology Data Exchange (ETDEWEB)

    Zeng Yanhong; Yang Jinquan [Department of Chemistry, Huazhong University of Science and Technology, Wuhan 430074 (China); Wu Kangbing [Department of Chemistry, Huazhong University of Science and Technology, Wuhan 430074 (China)], E-mail: kbwu@mail.hust.edu.cn

    2008-05-30

    The potential application of Al-incorporated mesoporous SiO{sub 2} (denoted as Al-MCM-41) in electrochemistry as a novel electrode material was investigated. The peak currents of K{sub 3}[Fe(CN){sub 6}] remarkably increase and the peak potential separation obviously decreases at the mesoporous Al-MCM-41 modified carbon paste electrode (CPE). These phenomena suggest that the mesoporous Al-MCM-41 modified CPE possesses larger electrode area and electron transfer rate constant. Furthermore, the electrochemical behavior of epinephrine (EP) was investigated in different supporting electrolytes such as 0.01 mol L{sup -1} HClO{sub 4} and pH 7.0 phosphate buffer. It is found that the mesoporous Al-MCM-41 modified CPE exhibits catalytic ability to the oxidation of EP due to remarkable peak current enhancement and negative shift of peak potential. The electrochemical oxidation mechanism was also discussed. Finally, a novel electrochemical method was proposed for the determination of EP, which used to determine EP in urine samples.

  3. Glucose oxidase-modified carbon-felt-reactor coupled with peroxidase-modified carbon-felt-detector for amperometric flow determination of glucose

    International Nuclear Information System (INIS)

    Wang Yue; Hasebe, Yasushi

    2012-01-01

    Glucose oxidase (GOx) and horseradish peroxidase (HRP) were covalently immobilized on a porous carbon-felt (CF) by using cyanuric chloride (CC) as a linking reagent. The resulting GOx-modified-CF (GOx-ccCF) was used as column-type enzyme reactor and placed on upstream of the HRP-ccCF-based H 2 O 2 flow-detector to fabricate amperometric flow-biosensor for glucose. Sensor setting conditions and the operational conditions were optimized, and the analytical performance characteristics of the resulting flow-biosensor were evaluated. The chemical modification of the GOx via CC was found to be effective to obtain larger catalytic activity as compared with the physical adsorption. Under the optimized conditions (i.e., volume ratio of the GOx-ccCF-reactor to the HRP-ccCF-detector is 1.0; applied potential is − 0.12 V vs. Ag/AgCl; carrier pH is 6.5; and carrier flow rate is 4.3 ml/min), highly selective and quite reproducible peak current responses toward glucose were obtained: the RSD for 30 consecutive injections of 3 mM glucose was 1.04%, and no serious interferences were observed for fructose, ethanol, uric acid, urea and tartaric acid for the amperometric measurements of glucose. The magnitude of the cathodic peak currents for glucose was linear up to 5 mM (sensitivity, 6.38 ± 0.32 μA/μM) with the limit detection of 9.4 μM (S/N = 3, noise level, 20 nA). The present GOx-ccCF-reactor and HRP-ccCF-detector-coupled flow-glucose biosensor was utilized for the determination of glucose in beverages and liquors, and the analytical results by the sensor were in fairly good agreement with those by the conventional spectrophotometry. - Highlights: ► Glucose oxidase (GOx) and peroxidase (HRP) were modified on carbon-felt. ► GOx-CF reactor and HRP-CF detector-coupled flow glucose biosensor was developed. ► This flow biosensor enabled the determination of glucose in beverages and liquors.

  4. Glucose oxidase-modified carbon-felt-reactor coupled with peroxidase-modified carbon-felt-detector for amperometric flow determination of glucose

    Energy Technology Data Exchange (ETDEWEB)

    Wang Yue [School of Chemical Engineering, University of Science and Technology LiaoNing, 185 Qianshan Middle Road, High-tech Zone, Anshan, LiaoNing, 114501 (China); Hasebe, Yasushi, E-mail: hasebe@sit.ac.jp [Department of Life Science and Green Chemistry, Faculty of Engineering, Saitama Institute of Technology, 1690, Fusaiji, Fukaya, Saitama 369-0293 (Japan)

    2012-04-01

    Glucose oxidase (GOx) and horseradish peroxidase (HRP) were covalently immobilized on a porous carbon-felt (CF) by using cyanuric chloride (CC) as a linking reagent. The resulting GOx-modified-CF (GOx-ccCF) was used as column-type enzyme reactor and placed on upstream of the HRP-ccCF-based H{sub 2}O{sub 2} flow-detector to fabricate amperometric flow-biosensor for glucose. Sensor setting conditions and the operational conditions were optimized, and the analytical performance characteristics of the resulting flow-biosensor were evaluated. The chemical modification of the GOx via CC was found to be effective to obtain larger catalytic activity as compared with the physical adsorption. Under the optimized conditions (i.e., volume ratio of the GOx-ccCF-reactor to the HRP-ccCF-detector is 1.0; applied potential is - 0.12 V vs. Ag/AgCl; carrier pH is 6.5; and carrier flow rate is 4.3 ml/min), highly selective and quite reproducible peak current responses toward glucose were obtained: the RSD for 30 consecutive injections of 3 mM glucose was 1.04%, and no serious interferences were observed for fructose, ethanol, uric acid, urea and tartaric acid for the amperometric measurements of glucose. The magnitude of the cathodic peak currents for glucose was linear up to 5 mM (sensitivity, 6.38 {+-} 0.32 {mu}A/{mu}M) with the limit detection of 9.4 {mu}M (S/N = 3, noise level, 20 nA). The present GOx-ccCF-reactor and HRP-ccCF-detector-coupled flow-glucose biosensor was utilized for the determination of glucose in beverages and liquors, and the analytical results by the sensor were in fairly good agreement with those by the conventional spectrophotometry. - Highlights: Black-Right-Pointing-Pointer Glucose oxidase (GOx) and peroxidase (HRP) were modified on carbon-felt. Black-Right-Pointing-Pointer GOx-CF reactor and HRP-CF detector-coupled flow glucose biosensor was developed. Black-Right-Pointing-Pointer This flow biosensor enabled the determination of glucose in beverages and

  5. Rapid determination of nitrophenol isomers in polluted water based on multi-walled carbon nanotubes modified screen-printed electrode

    Directory of Open Access Journals (Sweden)

    Essy Kouadio Fodjo

    2014-07-01

    Full Text Available A sensitive screen-printed electrode modified with multi-walled carbon nanotubes (MWCNTs/SPE was applied to determine simultaneously m-nitrophenol, o-nitrophenol and p-nitrophenol. The electrochemical response showed that o-nitrophenol, m-nitrophenol and p-nitrophenol were entirely separated at the MWCNTs/SPE interface. Under the optimized conditions, it was found that the detection limits were 8.1×10-8 , 5.5×10-7 and 2.0×10-7 M and the linear calibration ranges were 1.0×10-6 ~1.9×10-5 M, 2.5×10-6 ~2.1×10-5 M and 2.0×10-6 ~2.0×10-5 M for m-nitrophenol, o-nitrophenol and p-nitrophenol respectively, proving that the electrode presented here could be easily used to determine nitrophenol isomers simultaneously with high sensitivity within pH range from 4.8 to 8.0. The applications in water samples showed that no interferences appeared with deviations below 5% to the determination of nitrophenol isomers with 1000 fold excess, indicating a good response of this method for nitrophenol isomers detection. This disposable modified SPE combining with a portable electrochemical device were performed for wastewater samples on-field rapid determination.

  6. A Modified Rule of Thumb for Evaluating Scale Reproducibilities Determined by Electronic Computers

    Science.gov (United States)

    Hofmann, Richard J.

    1978-01-01

    The Goodenough technique for determining scale error is compared to the Guttman technique and demonstrated to be more conservative than the Guttman technique. Implications with regard to Guttman's evaluative rule of thumb for evaluating a reproducibility are noted. (Author)

  7. Determination of beryllium in water using silica gel chemically modified with aminophosphonic acid

    International Nuclear Information System (INIS)

    Zajtseva, G.N.; Strelko, V.V.

    2001-01-01

    Considered are methods of Be determination based on Be isolation from the solutions using aminophosphonic acid covalently bound on silica gel surface (APA-SiO 2 ) and subsequent photometric or atomic-absorption determination of Be in eluate ( the limit of Be determination is 0.00005 mg/l or 0.00008 mg/l, respectively). APA-SiO 2 high efficiency and a possibility of beryllium ions extraction from diluted solutions by means of sorbent small weighed portions is shown. High efficiency of the sorbent both for concentration and waters purification from beryllium is shown. Methods are tested in analysis of waste water. To assess the accuracy of the proposed methods, parallel determination of beryllium in tests by means of the additions method was carried out. The given data testify to a sufficient accuracy and reproducibility of the proposed methods [ru

  8. Determining the Walker exponent and developing a modified Smith-Watson-Topper parameter model

    Energy Technology Data Exchange (ETDEWEB)

    Lv, Zhiqiang; Huang, Hong Zhong; Wang, Hai Kun; Gao, Huiying; Zuo, Fang Jun [University of Electronic Science and Technology of China, Chengdu (China)

    2016-03-15

    Mean stress effects significantly influence the fatigue life of components. In general, tensile mean stresses are known to reduce the fatigue life of components, whereas compressive mean stresses are known to increase it. To date, various methods that account for mean stress effects have been studied. In this research, considering the high accuracy of mean stress correction and the difficulty in obtaining the material parameter of the Walker method, a practical method is proposed to describe the material parameter of this method. The test data of various materials are then used to verify the proposed practical method. Furthermore, by applying the Walker material parameter and the Smith-Watson-Topper (SWT) parameter, a modified strain-life model is developed to consider sensitivity to mean stress of materials. In addition, three sets of experimental fatigue data from super alloy GH4133, aluminum alloy 7075-T651, and carbon steel are used to estimate the accuracy of the proposed model. A comparison is also made between the SWT parameter method and the proposed strainlife model. The proposed strain-life model provides more accurate life prediction results than the SWT parameter method.

  9. Dose determination in radiotherapy for photon beams modified by static intensity modulators

    International Nuclear Information System (INIS)

    Castellanos Lopez, M.E.

    1998-01-01

    The static intensity modulators, used in radiotherapy, modify the spectral composition of the beam and lead to specific problems of the dose calculation. The aim of this work was to establish a three dimensional calculation, global and accurate, adapted to the primary-diffused separation algorithm and valid for any static modulator type. A theoretical study, experimentally verified, allowed the evaluation of the primary fluence, resulting from metallic sheets placed between photons beams of 6 to 23 MV nominal energy. It has been showed that the diffused, coming from the modulators, could be neglected for weak thickness and for the relative dose variation. In return it leads to significant variations of many % on the absolute dose and must be take into account for the bigger thicknesses. Corrective methods for the primary fluence have been proposed. From the energy spectra of the beam, the metallic modulator influence has been studied on the primary and diffused components of the dose and improvements of the calculation method have been proposed. These improvements are based on the modulator representation as a transmission matrix and on semi-empirical corrective factors. (A.L.B.)

  10. Molecular responses of genetically modified maize to abiotic stresses as determined through proteomic and metabolomic analyses.

    Directory of Open Access Journals (Sweden)

    Rafael Fonseca Benevenuto

    Full Text Available Some genetically modified (GM plants have transgenes that confer tolerance to abiotic stressors. Meanwhile, other transgenes may interact with abiotic stressors, causing pleiotropic effects that will affect the plant physiology. Thus, physiological alteration might have an impact on the product safety. However, routine risk assessment (RA analyses do not evaluate the response of GM plants exposed to different environmental conditions. Therefore, we here present a proteome profile of herbicide-tolerant maize, including the levels of phytohormones and related compounds, compared to its near-isogenic non-GM variety under drought and herbicide stresses. Twenty differentially abundant proteins were detected between GM and non-GM hybrids under different water deficiency conditions and herbicide sprays. Pathway enrichment analysis showed that most of these proteins are assigned to energetic/carbohydrate metabolic processes. Among phytohormones and related compounds, different levels of ABA, CA, JA, MeJA and SA were detected in the maize varieties and stress conditions analysed. In pathway and proteome analyses, environment was found to be the major source of variation followed by the genetic transformation factor. Nonetheless, differences were detected in the levels of JA, MeJA and CA and in the abundance of 11 proteins when comparing the GM plant and its non-GM near-isogenic variety under the same environmental conditions. Thus, these findings do support molecular studies in GM plants Risk Assessment analyses.

  11. Modified emission-transmission method for determining trace elements in solid samples using the XRF techniques

    International Nuclear Information System (INIS)

    Poblete, V.; Alvarez, M.; Hermosilla, M.

    2000-01-01

    This is a study of an analysis of trace elements in medium thick solid samples, by the modified transmission emission method, using the energy dispersion X-ray fluorescence technique (EDXRF). The effects of absorption and reinforcement are the main disadvantages of the EDXRF technique for the quantitative analysis of bigger elements and trace elements in solid samples. The implementation of this method and its application to a variety of samples was carried out using an infinitely thick multi-element white sample that calculates the correction factors by absorbing all the analytes in the sample. The discontinuities in the masic absorption coefficients versus energies association for each element, with medium thick and homogenous samples, are analyzed and corrected. A thorough analysis of the different theoretical and test variables are proven by using real samples, including certified material with known concentration. The simplicity of the calculation method and the results obtained show the method's major precision, with possibilities for the non-destructive routine analysis of different solid samples, using the EDXRF technique (author)

  12. Determination of Diclofenac on a Dysprosium Nanowire- Modified Carbon Paste Electrode Accomplished in a Flow Injection System by Advanced Filtering

    Directory of Open Access Journals (Sweden)

    Ali Akbar Moosavi-Movahedi

    2009-09-01

    Full Text Available A new detection technique called Fast Fourier Transform Square-Wave Voltammetry (FFT SWV is based on measurements of electrode admittance as a function of potential. The response of the detector (microelectrode, which is generated by a redox processes, is fast, which makes the method suitable for most applications involving flowing electrolytes. The carbon paste electrode was modified by nanostructures to improve sensitivity. Synthesized dysprosium nanowires provide a more effective nanotube-like surface [1-4] so they are good candidates for use as a modifier for electrochemical reactions. The redox properties of diclofenac were used for its determination in human serum and urine samples. The support electrolyte that provided a more defined and intense peak current for diclofenac determination was a 0.05 mol L−1 acetate buffer pH = 4.0. The drug presented an irreversible oxidation peak at 850 mV vs. Ag/AgCl on a modified nanowire carbon paste electrode which produced high current and reduced the oxidation potential by about 100 mV. Furthermore, the signal-to-noise ratio was significantly increased by application of a discrete Fast Fourier Transform (FFT method, background subtraction and two-dimensional integration of the electrode response over a selected potential range and time window. To obtain the much sensivity the effective parameters such as frequency, amplitude and pH was optimized. As a result, CDL of 2.0 × 10−9 M and an LOQ of 5.0 × 10−9 M were found for the determination for diclofenac. A good recovery was obtained for assay spiked urine samples and a good quantification of diclofenac was achieved in a commercial formulation.

  13. Voltammetric determination of polyphenolic content in pomegranate juice using a poly(gallic acid/multiwalled carbon nanotube modified electrode

    Directory of Open Access Journals (Sweden)

    Refat Abdel-Hamid

    2016-07-01

    Full Text Available A simple and sensitive poly(gallic acid/multiwalled carbon nanotube modified glassy carbon electrode (PGA/MWCNT/GCE electrochemical sensor was prepared for direct determination of the total phenolic content (TPC as gallic acid equivalent. The GCE working electrode was electrochemically modified and characterized using scanning electron microscope (SEM, cyclic voltammetry (CV, chronoamperometry and chronocoulometry. It was found that gallic acid (GA exhibits a superior electrochemical response on the PGA/MWCNT/GCE sensor in comparison with bare GCE. The results reveal that a PGA/MWCNT/GCE sensor can remarkably enhance the electro-oxidation signal of GA as well as shift the peak potentials towards less positive potential values. The dependence of peak current on accumulation potential, accumulation time and pH were investigated by square-wave voltammetry (SWV to optimize the experimental conditions for the determination of GA. Using the optimized conditions, the sensor responded linearly to a GA concentration throughout the range of 4.97 × 10−6 to 3.38 × 10−5 M with a detection limit of 3.22 × 10−6 M (S/N = 3. The fabricated sensor shows good selectivity, stability, repeatability and (101% recovery. The sensor was successfully utilized for the determination of total phenolic content in fresh pomegranate juice without interference of ascorbic acid, fructose, potassium nitrate and barbituric acid. The obtained data were compared with the standard Folin–Ciocalteu spectrophotometric results.

  14. Simultaneous determination of hydroquinone and catechol based on glassy carbon electrode modified with gold-graphene nanocomposite

    International Nuclear Information System (INIS)

    Ma, X.; Liu, Z.; Qiu, C.; Chen, T.; Ma, H.

    2013-01-01

    We have synthesized a virtually monodisperse gold-graphene (Au-G) nanocomposite by a single-step chemical reduction method in aqueous dimethylformamide solution. The nanoparticles are homogenously distributed over graphene nanosheets. A glassy carbon electrode was modified with this nanocomposite and displayed high electrocatalytic activity and extraordinary electronic transport properties due to its large surface area. It enabled the simultaneous determination of hydroquinone (HQ) and catechol (CC) in acetate buffer solution of pH 4.5. Two pairs of well-defined, quasi-reversible redox peaks are obtained, one for HQ and its oxidized form, with a 43 mV separation of peak potentials (ΔEp), the other for CC and its oxidized form, with a ΔEp of 39 mV. Due to the large separation of oxidation peak potentials (102 mV), the concentrations of HQ and CC can be easily determined simultaneously. The oxidation peak currents for both HQ and CC increase linearly with the respective concentrations in the 1.0 μM to 0.1 mM concentration range, with the detection limits of 0.2 and 0. 15 μM (S/N = 3), respectively. The modified electrode was successfully applied to the simultaneous determination of HQ and CC in spiked tap water, demonstrating that the Au-G nanocomposite may act as a high-performance sensing material in the selective detection of some environmental pollutants. (author)

  15. Electrochemical determination of serotonin in urine samples based on metal oxide nanoparticles/MWCNT on modified glassy carbon electrode

    Directory of Open Access Journals (Sweden)

    Omolola E. Fayemi

    2017-04-01

    Full Text Available The electrochemical response of serotonin on the modified electrode based on multiwalled-carbon-nanotube (MWCNT doped respectively with nickel, zinc and iron oxide nanoparticles coating on glassy carbon electrode (GCE at physiological pH 7 was determined using cyclic voltammetry (CV and square wave voltammetry (SWV. The modified GCE/MWCNT-metal oxide electrodes exhibited excellent electrocatalytic activity towards the detection of serotonin at large peak current and lower oxidation potentials compared to other electrodes investigated. The dynamic range for the serotonin determination was between 5.98 × 10−3 μM to 62.8 μM with detection limits 118, 129 and 166 nM for GCE/MWCNT-NiO, GCE/MWCNT-ZnO and GCE/MWCNT-Fe3O4 sensors respectively. GCE-MWCNT-NiO was the best electrode in terms of serotonin current response, electrode stability, resistance to fouling and limit of detection towards the analyte. The developed sensors were found to be electrochemically stable, reusable, economically effective due to their extremely low operational cost, and have demonstrated good limit of detection, sensitivity and selectivity towards serotonin determination in urine samples. Keywords: Metal oxides nanoparticles, Multiwalled carbon nanotubes, Glassy carbon electrode, Serotonin, Cyclic voltammetry, Square wave voltammetry

  16. Chloroplatinum(II) complex-modified MWCNTs paste electrode for electrochemical determination of mercury in skin lightening cosmetics

    International Nuclear Information System (INIS)

    Isa, Illyas Md; Saidin, Mohamad Idris; Ahmad, Mustaffa; Hashim, Norhayati; Bakar, Suriani Abu; Ali, Noorshida Mohd; Si, Suyanta M.

    2017-01-01

    The chemically modified multiwalled carbon nanotubes (MWCNTs) paste electrode with chloroplatinum(II) complex for the determination of mercury is presented. The chloroplatinum(II) complex was characterized by nuclear magnetic resonance spectroscopy (NMR), Fourier transforms infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), energy-dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), scanning electron microscope (SEM), and transmission electron microscope (TEM). The capability of the electron transfer rate on the surface of modified electrode evaluated is by electrochemical impedance spectroscopy (EIS). The square wave stripping voltammetry (SWSV) technique was employed to investigate the performance of chloroplatinum(II) complex-MWCNTs paste electrode for determination of mercury. Several operational parameters such as the composition ratios of the electrode, type of supporting electrolyte, pH of the solution, and the SWSV parameters were thoroughly investigated. Under optimal conditions, the linear range obtained was from 5.0 μM to 0.1 mM with limit detection of 3.7 μM. The interference from other heavy metals such as Ca 2+ , Mg 2+ , Ni 2+ , Zn 2+ , Cd 2+ , Co 2+ , Ba 2+ , Mn 2+ , and Ce 3+ did not influence the electrochemical response. The chloroplatinum(II) complex-MWCNTs paste electrode was successfully applied to determine mercury in skin lightening cosmetics with a good recovery (98.9%–101.1%).

  17. Nickel and strontium nitrates as modifiers for the determination of selenium in wine by Zeeman electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Cvetkovic, J. [Inst. of Agriculture, Skopje (Yugoslavia); Stafilov, T. [Inst. of Chemistry, Faculty of Science Sts. Cyril and Methodius Univ., Skopje (Yugoslavia); Mihajlovic, D. [RZ Tehnicka Kontrola, Skopje (Yugoslavia)

    2001-08-01

    A mixed matrix modifier of nickel and strontium nitrates was used as a chemical modifier for the determination of selenium in wines by Zeeman electrothermal atomic absorption spectrometry. Wine samples were heated on a boiling water bath with small amounts of nitric acid and hydrogen peroxide. For complete elimination of interference, especially from sulfates and phosphates, selenium is complexed with ammonium pyrolidinedithiocarbamate (APDTC), extracted into methyl isobutyl ketone (MIBK), and measured by ETAAS. The graphite furnace temperature program was optimized for both aqueous and organic solutions. Pyrolysis temperatures of 1300 C and 800 C were chosen for aqueous and organic solutions, respectively; 2700 C and 2100 C were used as optimum atomization temperatures for aqueous and organic solutions, respectively. The optimum modifier mass established is markedly lower than those presented in the literature. The platform atomization ensures pretreatment stabilization up to 1100 C and 1600 C, respectively, for organic and aqueous selenium solutions. The procedure was verified by the method of standard addition. The investigated wine samples originated from the different regions of the Republic of Macedonia. The selenium concentration varied from not detectable to 0.93 {mu}g L{sup -1}. (orig.)

  18. Electrochemical determination of bisphenol A at ordered mesoporous carbon modified nano-carbon ionic liquid paste electrode.

    Science.gov (United States)

    Li, Yonghong; Zhai, Xiurong; Liu, Xinsheng; Wang, Ling; Liu, Herong; Wang, Haibo

    2016-02-01

    A simple bisphenol A (BPA) sensor was successfully fabricated based on ordered mesoporous carbon CMK-3 modified nano-carbon ionic liquid paste electrode (CMK-3/nano-CILPE). The nanostructure of CMK-3 and the surface morphologies of modified electrodes were characterized by transmission electron microscopy (TEM) and scanning electron microscopy (SEM). Electrochemical properties of the fabricated electrodes were investigated by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The fabricated sensor displayed excellent electroactivity towards bisphenol A using linear sweep voltammetry (LSV). Experimental conditions influencing the analytical performance of the modified electrode were optimized. Under optimal conditions, the oxidation peak current was proportional to BPA concentration in the range from 0.2 μM to 150 μM with a detection limit of 0.05 μM (S/N=3). This method was successfully used for determination of BPA leached from drinking bottle and plastic bag with good recoveries. Copyright © 2015 Elsevier B.V. All rights reserved.

  19. A ω-mercaptoundecylphosphonic acid chemically modified gold electrode for uranium determination in waters in presence of organic matter.

    Science.gov (United States)

    Merli, Daniele; Protti, Stefano; Labò, Matteo; Pesavento, Maria; Profumo, Antonella

    2016-05-01

    A chemically modified electrode (CME) on a gold surface assembled with a ω-phosphonic acid terminated thiol was investigated for its capability to complex uranyl ions. The electrode, characterized by electrochemical techniques, demonstrated to be effective for the determination of uranyl at sub-μgL(-1) level by differential pulse adsorptive stripping voltammetry (DPAdSV) in environmental waters, also in presence of humic matter and other potential chelating agents. The accuracy of the measurements was investigated employing as model probes ligands of different complexing capability (humic acids and EDTA). Copyright © 2016 Elsevier B.V. All rights reserved.

  20. Endogenous phenolics and starch modifying enzymes as determinants of sorghum for food use in Burkina Faso

    NARCIS (Netherlands)

    Dicko, M.H.

    2005-01-01

    The objective of this thesis is to screen for biochemical determinants in sorghum varieties cultivated in Burkina Faso to identify the best sorghum varieties to be used as source of bioactive components or for specific local foods, e.g. "tô", thin porridges for infants, granulated foods "couscous",

  1. Altering the sex determination pathway in Drosophila fat body modifies sex-specific stress responses.

    Science.gov (United States)

    Argue, Kathryn J; Neckameyer, Wendi S

    2014-07-01

    The stress response in Drosophila melanogaster reveals sex differences in behavior, similar to what has been observed in mammals. However, unlike mammals, the sex determination pathway in Drosophila is well established, making this an ideal system to identify factors involved in the modulation of sex-specific responses to stress. In this study, we show that the Drosophila fat body, which has been shown to be important for energy homeostasis and sex determination, is a dynamic tissue that is altered in response to stress in a sex and time-dependent manner. We manipulated the sex determination pathway in the fat body via targeted expression of transformer and transformer-2 and analyzed these animals for changes in their response to stress. In the majority of cases, manipulation of transformer or transformer-2 was able to change the physiological output in response to starvation and oxidative stress to that of the opposite sex. Our data also uncover the possibility of additional downstream targets for transformer and transformer-2 that are separate from the sex determination pathway and can influence behavioral and physiological responses. Copyright © 2014 the American Physiological Society.

  2. Determination of Food Oxalates Using Silica–Titania Xerogel Modified with Eriochrome Cyanine R

    Directory of Open Access Journals (Sweden)

    Maria A. Morosanova

    2018-03-01

    Full Text Available The interaction of silica–titania xerogel with triphenylmethane dyes (pyrocatechol violet, chrome azurol S, eriochrome cyanine R has been investigated to create a new sensor material for solid phase spectrophotometric determination of food oxalates. The complex forming reaction between xerogel incorporated titanium(IV and triphenylmethane dyes has been studied; half-reaction periods, complex composition, equilibrium constants, and xerogel sorption capacity have been calculated for each dye. Eriochrome cyanine R (ECR is characterized by the shortest half-reaction period, the smallest equilibrium constant, and the greatest capacity; it has been chosen for the sensor material construction because titanium(IV-ECR complex is formed faster and can be destroyed easier than other studied complexes. The interaction of this sensor material with oxalates has been described: the presence of oxalates causes sensor material discoloration and the absorbance is used as analytical signal. The analytical range is 35–900 mg/L (LOD 10.5 mg/L, n = 7. High concentrations of interfering inorganic anions, organic acids, and sucrose did not affect oxalate determination. Proposed solid phase spectrophotometric procedure has been successfully applied for the determination of oxalates in food samples (sorrel, spinach, parsley, ginger, and black pepper and the results are in good agreement with HPLC oxalate determination.

  3. Copy number ratios determined by two digital polymerase chain reaction systems in genetically modified grains

    Science.gov (United States)

    Pérez Urquiza, M.; Acatzi Silva, A. I.

    2014-02-01

    Three certified reference materials produced from powdered seeds to measure the copy number ratio sequences of p35S/hmgA in maize containing MON 810 event, p35S/Le1 in soybeans containing GTS 40-3-2 event and DREB1A/acc1 in wheat were produced according to the ISO Guides 34 and 35. In this paper, we report digital polymerase chain reaction (dPCR) protocols, performance parameters and results of copy number ratio content of genetically modified organisms (GMOs) in these materials using two new dPCR systems to detect and quantify molecular deoxyribonucleic acid: the BioMark® (Fluidigm) and the OpenArray® (Life Technologies) systems. These technologies were implemented at the National Institute of Metrology in Mexico (CENAM) and in the Reference Center for GMO Detection from the Ministry of Agriculture (CNRDOGM), respectively. The main advantage of this technique against the more-used quantitative polymerase chain reaction (qPCR) is that it generates an absolute number of target molecules in the sample, without reference to standards or an endogenous control, which is very useful when not much information is available for new developments or there are no standard reference materials in the market as in the wheat case presented, or when it was not possible to test the purity of seeds as in the maize case presented here. Both systems reported enhanced productivity, increased reliability and reduced instrument footprint. In this paper, the performance parameters and uncertainty of measurement obtained with both systems are presented and compared.

  4. What determines the acceptability of genetically modified food that can improve human nutrition?

    Science.gov (United States)

    Purchase, Iain F H

    2005-09-01

    It has been predicted that by 2025 there will be an annual shortfall of cereals for feeding the human population of 68.5 million tones. One possible solution is the use of genetically modified (GM) crops, which are already grown extensively (59 million ha of GM crops were planted in 2002) in the USA, South America, Africa and China. Nevertheless, there is considerable disagreement about the advisability of using such crops, particularly in Europe. Obviously, the safety of the food derived from the GM crops is a primary consideration. Safety assessment relies on establishing that the food is substantially equivalent to its non-GM counterpart and specific testing for allergenicity of proteins and toxicity of metabolites and the whole food. There appears to be international agreement on the principles of safety assessment. Safety to the environment is equally important, but will not be covered in this presentation. The public's perception of the risk of new technology is critical to its acceptance. Perception of risk, in turn, depends on the credibility of the source of the information and trust in the regulatory process. In many countries, the public appears to have lost its trust in the scientists and government dealing with GM food, making the acceptability of GM crops uncertain. Of equal importance are the socio-economic factors that impinge on the viability of GM produce. These include intellectual property protection, trade liberalization (through subsidy and tariff barriers in developed countries) and the intensity of bio safety regulations. The socio-economic interests of developed and developing countries may diverge and may even be contradictory in any one country. Acceptance of GM crops will thus depend on detailed issues surrounding particular crops and economies.

  5. What determines the acceptability of genetically modified food that can improve human nutrition?

    International Nuclear Information System (INIS)

    Purchase, Iain F.H.

    2005-01-01

    It has been predicted that by 2025 there will be an annual shortfall of cereals for feeding the human population of 68.5 million tonnes. One possible solution is the use of genetically modified (GM) crops, which are already grown extensively (59 million ha of GM crops were planted in 2002) in the USA, South America, Africa and China. Nevertheless, there is considerable disagreement about the advisability of using such crops, particularly in Europe. Obviously, the safety of the food derived from the GM crops is a primary consideration. Safety assessment relies on establishing that the food is substantially equivalent to its non-GM counterpart and specific testing for allergenicity of proteins and toxicity of metabolites and the whole food. There appears to be international agreement on the principles of safety assessment. Safety to the environment is equally important, but will not be covered in this presentation. The public's perception of the risk of new technology is critical to its acceptance. Perception of risk, in turn, depends on the credibility of the source of the information and trust in the regulatory process. In many countries, the public appears to have lost its trust in the scientists and government dealing with GM food, making the acceptability of GM crops uncertain. Of equal importance are the socio-economic factors that impinge on the viability of GM produce. These include intellectual property protection, trade liberalisation (through subsidy and tariff barriers in developed countries) and the intensity of bio safety regulations. The socio-economic interests of developed and developing countries may diverge and may even be contradictory in any one country. Acceptance of GM crops will thus depend on detailed issues surrounding particular crops and economies

  6. What determines the acceptability of genetically modified food that can improve human nutrition?

    Energy Technology Data Exchange (ETDEWEB)

    Purchase, Iain F.H. [University of Manchester, Oxford Road, Manchester M13 9PT (United Kingdom)

    2005-09-01

    It has been predicted that by 2025 there will be an annual shortfall of cereals for feeding the human population of 68.5 million tonnes. One possible solution is the use of genetically modified (GM) crops, which are already grown extensively (59 million ha of GM crops were planted in 2002) in the USA, South America, Africa and China. Nevertheless, there is considerable disagreement about the advisability of using such crops, particularly in Europe. Obviously, the safety of the food derived from the GM crops is a primary consideration. Safety assessment relies on establishing that the food is substantially equivalent to its non-GM counterpart and specific testing for allergenicity of proteins and toxicity of metabolites and the whole food. There appears to be international agreement on the principles of safety assessment. Safety to the environment is equally important, but will not be covered in this presentation. The public's perception of the risk of new technology is critical to its acceptance. Perception of risk, in turn, depends on the credibility of the source of the information and trust in the regulatory process. In many countries, the public appears to have lost its trust in the scientists and government dealing with GM food, making the acceptability of GM crops uncertain. Of equal importance are the socio-economic factors that impinge on the viability of GM produce. These include intellectual property protection, trade liberalisation (through subsidy and tariff barriers in developed countries) and the intensity of bio safety regulations. The socio-economic interests of developed and developing countries may diverge and may even be contradictory in any one country. Acceptance of GM crops will thus depend on detailed issues surrounding particular crops and economies.

  7. Glassy carbon electrodes modified with multiwalled carbon nanotubes for the determination of ascorbic acid by square-wave voltammetry

    Directory of Open Access Journals (Sweden)

    Sushil Kumar

    2012-05-01

    Full Text Available Multiwalled carbon nanotubes were used to modify the surface of a glassy carbon electrode to enhance its electroactivity. Nafion served to immobilise the carbon nanotubes on the electrode surface. The modified electrode was used to develop an analytical method for the analysis of ascorbic acid (AA by square-wave voltammetry (SWV. The oxidation of ascorbic acid at the modified glassy carbon electrode showed a peak potential at 315 mV, about 80 mV lower than that observed at the bare (unmodified electrode. The peak current was about threefold higher than the response at the bare electrode. Replicate measurements of peak currents showed good precision (3% rsd. Peak currents increased with increasing ascorbic acid concentration (dynamic range = 0.0047–5.0 mmol/L and displayed good linearity (R2 = 0.994. The limit of detection was 1.4 μmol/L AA, while the limit of quantitation was 4.7 μmol/L AA. The modified electrode was applied to the determination of the amount of ascorbic acid in four brands of commercial orange-juice products. The measured content agreed well (96–104% with the product label claim for all brands tested. Recovery tests on spiked samples of orange juice showed good recovery (99–104%. The reliability of the SWV method was validated by conducting parallel experiments based on high-performance liquid chromatography (HPLC with absorbance detection. The observed mean AA contents of the commercial orange juice samples obtained by the two methods were compared statistically and were found to have no significant difference (P = 0.05.

  8. Nanomolar determination of 4-nitrophenol based on a poly(methylene blue)-modified glassy carbon electrode.

    Science.gov (United States)

    Giribabu, Krishnamoorthy; Suresh, Ranganathan; Manigandan, Ramadoss; Munusamy, Settu; Kumar, Sivakumar Praveen; Muthamizh, Selvamani; Narayanan, Vengidusamy

    2013-10-07

    A poly(methylene blue)-modified glassy carbon electrode (PMB/GCE) was fabricated by electropolymerisation of methylene blue on a GCE and further utilized to investigate the electrochemical determination of 4-nitrophenol (4-NP) by cyclic voltammetry (CV), differential pulse voltammetry and chronocoulometry. The morphology of the PMB on GCE was examined using a scanning electron microscope (SEM). An oxidation peak of 4-NP at the PMB modified electrode was observed at 0.28 V, and in the case of bare GCE, no oxidation peak was observed, which indicates that PMB/GCE exhibits a remarkable effect on the electrochemical determination of 4-NP. Due to this remarkable effect of PMB/GCE, a sensitive and simple electrochemical method was proposed for the determination of 4-NP. The effect of the scan rate and pH was investigated to determine the optimum conditions at which the PMB/GCE exhibits a higher sensitivity with a lower detection limit. Moreover, kinetic parameters such as the electron transfer number, proton transfer number and standard heterogeneous rate constant were calculated. Under optimum conditions, the oxidation current of 4-NP is proportional to its concentration in the range of 15-250 nM with a correlation coefficient of 0.9963. The detection limit was found to be 90 nM (S/N = 3). The proposed method based on PMB/GCE is simple, easy and cost effective. To further confirm its possible application, the proposed method was successfully used for the determination of 4-NP in real water samples with recoveries ranging from 97% to 101.6%. The interference due to sodium, potassium, calcium, magnesium, copper, zinc, iron, sulphate, carbonate, chloride, nitrate and phosphate was found to be almost negligible.

  9. Modified method for zirconium or hafnium gravimetric determination with glycolic acid derivatives

    International Nuclear Information System (INIS)

    Barbieri, R.S.; Rocha, J.C.; Terra, V.R.; Marques Neto, A.

    1989-01-01

    The conditions for gravimetric determination of zirconium or hafnium by glicolic acid derivatives were studied by thermogravimetric analysis. The method utilized shown that after precipitation, washing and drying of precipitates at 150 0 C, the resulting solid was weighed in the form of [M{RCH(OH)COO} 4 ] (M = Zr,Hf;R = C 6 H 5 , β-C 10 H 7 ,p-BrC 6 H 4 ). (author) [pt

  10. Determining the optimum conditions for modified diesel fuel combustion considering its emission, properties and engine performance

    International Nuclear Information System (INIS)

    Fayyazbakhsh, Ahmad; Pirouzfar, Vahid

    2016-01-01

    Highlights: • Gas emissions, fuel properties and performance engine modeling. • Optimization of new modified fuel prepared from n-Butanol and Nano particles. • Model accuracy analysis. - Abstract: This essay scrutinizes an experimental study conducted to appraise the influence of using n-Butanol with diesel fuel in 5% and 10% (volume) n-Butanol, 1% nitro methane (NM), injection timing and two Nano-particles (alumina and a type of silica powder) on the engine performance (brake specific fuel consumption and engine power), fuel properties (Cetane number and flash point) and exhaust emissions (soot, NO_x and CO) of an engine with 4-cylinder (with a system of common rail fuel injection), intercooling, cooled exhaust gas recirculation (EGR), and turbocharged. The tests are conducted by varying the engine load (25 and 75 nm) and changing engine speed (1500 and 2200 rpm). Normal Butanol presents better brake specific fuel consumption (BSFC) but this blend doesn’t reflect better engine power. All the percentages of n-Butanol in the fuel make Cetane number decrease but adding 1% of nitro methane makes Cetane number increase. For all the n-Butanol, the percentage flash makes the fuel decrease in comparison to pure diesel fuel. The current experimental study demonstrates that adding the n-Butanol and nitro methane to diesel fuel direct into diminishing soot emission. In contrast, this blend raises NO_x and CO emissions. Furthermore, this research indicates that the increase of engine speed dwindle air pollutants and enhances BSFC. It also remarks that power gets increased at low engine speed. However, power gets reducedat high speed. This article represents that the increasing of engine load leads to increasing all of air pollutant, increasing of power and decreasing of brake specific fuel consumption. Both the Cetane number and flash point are independent from engine speed and engine load. The present paper shows that the effect of silica with high percentage of n

  11. An amperometric bienzymatic cholesterol biosensor based on functionalized graphene modified electrode and its electrocatalytic activity towards total cholesterol determination.

    Science.gov (United States)

    Manjunatha, Revanasiddappa; Shivappa Suresh, Gurukar; Melo, Jose Savio; D'Souza, Stanislaus F; Venkatesha, Thimmappa Venkatarangaiah

    2012-09-15

    Cholesterol oxidase (ChOx) and cholesterol esterase (ChEt) have been covalently immobilized onto functionalized graphene (FG) modified graphite electrode. Enzymes modified electrodes were characterized using cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). FG accelerates the electron transfer from electrode surface to the immobilized ChOx, achieving the direct electrochemistry of ChOx. A well defined redox peak was observed, corresponding to the direct electron transfer of the FAD/FADH(2) of ChOx. The electron transfer coefficient (α) and electron transfer rate constant (K(s)) were calculated and their values are found to be 0.31 and 0.78 s(-1), respectively. For the free cholesterol determination, ChOx-FG/Gr electrode exhibits a sensitive response from 50 to 350 μM (R=-0.9972) with a detection limit of 5 μM. For total cholesterol determination, co-immobilization of ChEt and ChOx on modified electrode, i.e. (ChEt/ChOx)-FG/Gr electrode showed linear range from 50 to 300 μM (R=-0.9982) with a detection limit of 15 μM. Some common interferents like glucose, ascorbic acid and uric acid did not cause any interference, due to the use of a low operating potential. The FG/Gr electrode exhibits good electrocatalytic activity towards hydrogen peroxide (H(2)O(2)). A wide linear response to H(2)O(2) ranging from 0.5 to 7 mM (R=-0.9967) with a sensitivity of 443.25 μA mM(-1) cm(-2) has been obtained. Copyright © 2012 Elsevier B.V. All rights reserved.

  12. Determination of hydroxide in the presence of aluminate using a modified potentiometric titration

    International Nuclear Information System (INIS)

    Hanson, T.J.

    1975-11-01

    A procedure for the determination of hydroxide concentration in the presence of aluminate and other interfering ions was developed using the method of standard additions (or more specifically in this case, standard subtractions). The procedure called for titration with a strong acid which was added in equal increments at regular time intervals. The potential was recorded after each addition of acid. The data was plotted on Gran's Plot Paper, which is based on work done originally by Gran, or it was entered into a computer to determine the equivalence volume of the titrant. When used on many different samples in different matrices, the method gave results that were approximately 100 +- 1 percent of the calculated value. This was shown to be true even in systems containing aluminate [Al(OH) 4 - ], phosphate (PO 4 3- ), sulfate (SO 4 2- ), nitrate (NO 3 - ), nitrite (NO 2 - ), carbonate (CO 3 2- ), and other ions. The effect of these ions was shown to be negligible if the initial OH - concentration was at least 10 -3 M and barium chloride (BaCl 2 ) was added to complex the PO 4 3- and CO 3 2- ions. These ions were checked at levels of up to 3 M for Al(OH) 4 - and NO 3 - , 2 M for NO 2 - , and 1 M for SO 4 2- , PO 4 3- , and CO 3 2- . The method is applicable to radioactive as well as nonradioactive samples and any heat involved with a radioactive sample is insufficient to cause an error in the determination. On the basis of the work performed it was shown that the method was general enough to be run on a routine basis

  13. Application of modified Martinez-Silva algorithm in determination of net cover

    Science.gov (United States)

    Stefanowicz, Łukasz; Grobelna, Iwona

    2016-12-01

    In the article we present the idea of modifications of Martinez-Silva algorithm, which allows for determination of place invariants (p-invariants) of Petri net. Their generation time is important in the parallel decomposition of discrete systems described by Petri nets. Decomposition process is essential from the point of view of discrete system design, as it allows for separation of smaller sequential parts. The proposed modifications of Martinez-Silva method concern the net cover by p-invariants and are focused on two important issues: cyclic reduction of invariant matrix and cyclic checking of net cover.

  14. Voltammetric Determination of Lead (II) and Cadmium (II) Using a Bismuth Film Electrode Modified with Mesoporous Silica Nanoparticles

    International Nuclear Information System (INIS)

    Yang, Die; Wang, Liang; Chen, Zuliang; Megharaj, Mallavarapu; Naidu, Ravi

    2014-01-01

    A new chemically modified glassy carbon electrode based on bismuth film coated mesoporous silica nanoparticles was developed and evaluated for reliable quantification of trace Pb 2+ and Cd 2+ by anodic stripping square wave voltammetry in natural water samples. Compared with conventional bismuth film electrodes or bismuth nanoparticles modified electrodes, this electrode exhibited significantly improved sensitivity and stability for Pb 2+ and Cd 2+ detection. The key experimental parameters related to the fabrication of the electrode and the voltammetric measurements were optimized on the basis of the stripping signals, where the peak currents increased linearly with the metal concentrations in a range of 2-150 μg L −1 with a detect limit of 0.2 μg L −1 for Pb 2+ , and 0.6 μg L −1 for Cd 2+ for 120s deposition. Good reproducibility was achieved on both single and equally prepared electrodes. In addition, scanning electron microscopy reveals that fibril-like bismuth structures were formed on silica nanoparticles, which could be responsible for the improved voltammetric performance due to the enhanced surface area. Finally, the developed electrode was applied to determine Pb 2+ and Cd 2+ in water samples, indicating that this electrode was sensitive, reliable and effective for the simultaneous determination of Pb 2+ and Cd 2+

  15. Multi-walled Carbon Nanotubes/Graphite Nanosheets Modified Glassy Carbon Electrode for the Simultaneous Determination of Acetaminophen and Dopamine.

    Science.gov (United States)

    Zhang, Susu; He, Ping; Zhang, Guangli; Lei, Wen; He, Huichao

    2015-01-01

    Graphite nanosheets prepared by thermal expansion and successive sonication were utilized for the construction of a multi-walled carbon nanotubes/graphite nanosheets based amperometric sensing platform to simultaneously determine acetaminophen and dopamine in the presence of ascorbic acid in physiological conditions. The synergistic effect of multi-walled carbon nanotubes and graphite nanosheets catalyzed the electrooxidation of acetaminophen and dopamine, leading to a remarkable potential difference up to 200 mV. The as-prepared modified electrode exhibited linear responses to acetaminophen and dopamine in the concentration ranges of 2.0 × 10(-6) - 2.4 × 10(-4) M (R = 0.999) and 2.0 × 10(-6) - 2.0 × 10(-4) M (R = 0.998), respectively. The detection limits were down to 2.3 × 10(-7) M for acetaminophen and 3.5 × 10(-7) M for dopamine (S/N = 3). Based on the simple preparation and prominent electrochemical properties, the obtained multi-walled carbon nanotubes/graphite nanosheets modified electrode would be a good candidate for the determination of acetaminophen and dopamine without the interference of ascorbic acid.

  16. Voltammetric determination of In3+ based on the bifunctionality of a multi-walled carbon nanotubes-nafion modified electrode.

    Science.gov (United States)

    Li, Junhua; Zhang, Fuxing; Wang, Jianqiu; Xu, Zhifeng; Zeng, Rongying

    2009-05-01

    Due to the strong cation-exchange ability of Nafion and the excellent properties of multi-walled carbon nanotubes (MWCNTs), a highly sensitive and mercury-free method of determining trace levels of In(3+) has been established based on the bifunctionality of a MWCNTs/Nafion modified glassy carbon electrode (GCE). The MWCNTs/Nafion modified GCE detects In(3+) in a 0.01 M HAc-NaAc buffer solution at pH 5.0 using anodic stripping voltammetry (ASV). The experimental results suggest that a sensitive anodic stripping peak appears at -0.58 V on anodic stripping voltammograms, which can be used as an analytical signal for the determination of In(3+). A good linear relationship between the stripping peak currents and the In(3+) concentration is obtained, covering the concentration range from 5.0 x 10(-10) to 2.0 x 10(-7) M, with a correlation coefficient of 0.999; the detection limit is 1.0 x 10(-11) M. This proposed method has been applied to detect In(3+) as a new way.

  17. Determination of fenitrothion in water using a voltammetric sensor based on a polymer-modified glassy carbon electrode.

    Science.gov (United States)

    Amare, Meareg; Abicho, Samuel; Admassie, Shimelis

    2014-01-01

    A glassy carbon electrode (GCE) modified with poly(4-amino-3-hydroxynaphthalene sulfonic acid) (poly-AHNSA) was used for the selective and sensitive determination of fenitrothion (FT) organophosphorus pesticide in water. The electrochemical behavior of FT at the bare GCE and the poly-AHNSA/GCE were compared using cyclic voltammetry. Enhanced peak current response and shift to a lower potential at the polymer-modified electrode indicated the electrocatalytic activity of the polymer film towards FT. Under optimized solution and method parameters, the adsorptive stripping square wave voltammetric reductive peak current of FT was linear to FT concentration in the range of 0.001 to 6.6 x 10(-6) M, and the LOD obtained (3delta/m) was 7.95 x 10(-10) M. Recoveries in the range 96-98% of spiked FT in tap water and reproducible results with RSD of 2.6% (n = 5) were obtained, indicating the potential applicability of the method for the determination of trace levels of FT in environmental samples.

  18. GC electrode modified with carbon nanotubes and NiO for the simultaneous determination of bisphenol A, hydroquinone and catechol

    International Nuclear Information System (INIS)

    Goulart, Lorena Athie; Mascaro, Lucia Helena

    2016-01-01

    This work reports the electrochemical determination of bisphenol A (BPA), hydroquinone (HQ) and catechol (CC) using glassy carbon electrode (GCE) modified with multi-walled carbon nanotubes (MWCNT) and nickel oxide nanoparticles (NiO). MWCNT were functionalized with sulfonitric solution (3H 2 SO 4 :1HNO 3 ) and dispersed in dimethylformamide for the MWCNT/GCE manufacturing. The MWCNT/GCE was modified with NiO using cyclic potential in pH 4 maintained by an acetate buffer solution containing 0.008 mol L −1 of nickel nitrate. The concentration of the nickel solution and the number of cycles in the electrodeposition were studied. Morphological characterization of NiO/MWCNT/GCE was carried out by scanning electron microscopy and the presence of NiO was observed. The electrochemical behavior was evaluated by cyclic voltammetry and electrochemical impedance spectroscopy using BPA solution and the results were compared with those of GCE. The NiO/MWCNT/GCE presented the lowest charge transfer resistance. The electrochemical detection of BPA, HQ and CC was developed using differential pulse voltammetry. The analytical curves showed an excellent linear response and the detection limits for the simultaneous determination of BPA, HQ and CC were 2.8 × 10 −8 mol L −1 , 2.70 × 10 −8 mol L −1 and 5.9 × 10 −8 mol L −1 , respectively.

  19. Determination of melamine in food contact materials using an electrode modified with gold nanoparticles and reduced graphene oxide

    International Nuclear Information System (INIS)

    Chen, Ningning; Zhang, Cuiling; Zhao, Kai; Xian, Yuezhong; Cheng, Yuxiao; Li, Chen

    2015-01-01

    We describe an electrochemical sensor for melamine based on a glassy carbon electrode (GCE) modified with reduced graphene oxide that was decorated with gold nanoparticles (AuNP/rGO). The AuNPs/rGO nanocomposite was synthesized by co-reduction of Au(III) and graphene oxide and characterized by transmission electron microscopy, Raman spectroscopy, X-ray diffraction and X-ray photoelectron spectroscopy. The response of the modified GCE to melamine was investigated by using hexacyanoferrate as an electrochemical reporter. It is found that the electrochemical response to hexacyanoferrate is increasingly suppressed by increasing concentration of melamine. This is attributed to competitive adsorption of melamine at the AuNP/rGO composite through the interaction between the amino groups of melamine and the AuNPs. The presence of rGO, in turn, provides a platform for a more uniform distribution of the AuNPs and enhances the electron transfer rate of the redox reaction. The findings were used to develop a sensitive method for the determination of melamine. Under optimized conditions, the redox peak current of hexacyanoferrate at a working voltage of 171 mV (vs. SCE) is linearly related to the concentration of melamine in 5.0 to 50 nM range. The method was successfully applied to the determination of melamine in food contact materials. (author)

  20. Voltammetric Determination of Anti-Hypertensive Drug Hydrochlorothiazide Using Screen-Printed Electrodes Modified with L-Glutamic Acid

    Directory of Open Access Journals (Sweden)

    Camilo González-Vargas

    2017-09-01

    Full Text Available This work deals with the development of screen-printed carbon electrodes modified with L-glutamic acid via two different approaches: electropolymerization (SPCE/PGA and aryl diazonium electrochemical grafting (SPCE/EGA. SPCE/PGA and SPCE/EGA were analytically compared in the determination of hydrochlorothiazide (HCTZ by differential pulse voltammetry. Both electrochemical characterization and analytical performance indicate that SPCE/EGA is a much better sensor for HCTZ. The detection and quantification limits were at the level of μmol L−1 with a very good linearity in the studied concentration range. In addition, the proposed SPCE/EGA was successfully applied for the determination of HCTZ in an anti-hypertensive drug with high reproducibility and good trueness.

  1. Reexamination of a novel determination of density, temperature, and symmetry energy based on a modified Fisher model

    Science.gov (United States)

    Liu, X.; Zheng, H.; Lin, W.; Huang, M.; Yang, Y. Y.; Wang, J. S.; Wada, R.; Bonasera, A.; Natowitz, J. B.

    2018-01-01

    In this article, a mistake in the formulation of the modified Fisher model (MFM) derived in the pioneering works of the Purdue group is addressed and corrected by reversing the sign of the mixing entropy term in the original formulation. The errors in the results of the previous MFM-related studies, such as isotopic yield distribution, isobaric yield ratios, isoscaling, m scaling, self-consistent determination of density, symmetry energy, and temperature, and density and temperature determination related to the intermediate mass fragment (IMF) freezeout, are quantitatively analyzed. It is found that the errors originating from the mistake in sign of the mixing entropy term are generally small and even have no effect in some cases.

  2. Facile synthesized SnO2 decorated functionalized graphene modified electrode for sensitive determination of daidzein.

    Science.gov (United States)

    Fu, Yamin; Wang, Lu; Duan, Yinghao; Zou, Lina; Ye, Baoxian

    2017-06-01

    A one-step and facile method using SnCl 2 ·H 2 O as reducing agent to reduce graphene oxide (GO) was performed in the aid of poly(diallyldimethylammonium chloride) solution (PDDA). SnCl 2 ·H 2 O is not only a reducing agent for graphene oxide (GO), but also a precursor of SnO 2 . SnO 2 -PDDA-GR composite was characterized by various surface, structural and electrochemical analysis techniques, such as transmission electron microscopy (TEM), UV spectrum (UV-vis), Infrared Spectrum (IR), X-ray diffraction (XRD), Cyclic voltammograms (CV) and electrochemical impedance (EIS). The SnO 2 -PDDA-GR composite was used to constructed electrochemical sensor (SnO 2 -PDDA-GR/GCE) for the determination of daidzein. Under the optimized experimental condition, it was found that the response of peak current is linear to the concentration of daidzein in the ranges of 2.0×10 -8 -1.0×10 -6 molL -1 , and the detection limit was estimated to be 6.7×10 -9 mol L -1 (S/N=3). Furthermore, this sensor was successfully applied for the determination of daidzein in traditional Chinese medicine (pueraria lobata) and Daidzein tablets. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. A Modified Fluorimetric Method for Determination of Hydrogen Peroxide Using Homovanillic Acid Oxidation Principle

    Directory of Open Access Journals (Sweden)

    Biswaranjan Paital

    2014-01-01

    Full Text Available Hydrogen peroxide (H2O2 level in biological samples is used as an important index in various studies. Quantification of H2O2 level in tissue fractions in presence of H2O2 metabolizing enzymes may always provide an incorrect result. A modification is proposed for the spectrofluorimetric determination of H2O2 in homovanillic acid (HVA oxidation method. The modification was included to precipitate biological samples with cold trichloroacetic acid (TCA, 5% w/v followed by its neutralization with K2HPO4 before the fluorimetric estimation of H2O2 is performed. TCA was used to precipitate the protein portions contained in the tissue fractions. After employing the above modification, it was observed that H2O2 content in tissue samples was ≥2 fold higher than the content observed in unmodified method. Minimum 2 h incubation of samples in reaction mixture was required for completion of the reaction. The stability of the HVA dimer as reaction product was found to be >12 h. The method was validated by using known concentrations of H2O2 and catalase enzyme that quenches H2O2 as substrate. This method can be used efficiently to determine more accurate tissue H2O2 level without using internal standard and multiple samples can be processed at a time with additional low cost reagents such as TCA and K2HPO4.

  4. Electrooxidation of Indomethacin at Multiwalled Carbon Nanotubes-Modified GCE and Its Determination in Pharmaceutical Dosage Form and Human Biological Fluids

    OpenAIRE

    Sataraddi, Sanjeevaraddi R.; Patil, Shreekant M.; Bagoji, Atmanand M.; Pattar, Vijay P.; Nandibewoor, Sharanappa T.

    2014-01-01

    A simple, rapid, selective, and sensitive electrochemical method for the direct determination of indomethacin was developed. The electrochemical behavior of indomethacin was carried at multiwalled carbon nanotube- (MWCNTs-) modified glassy carbon electrode (GCE). The cyclic voltammetric results indicated that MWCNT-modified glassy carbon electrode remarkably enhanced electrocatalytic activity towards the oxidation of indomethacin in slightly acidic solutions. It led to a considerable improvem...

  5. Voltammetric Determination of Flunixin on Molecularly Imprinted Polypyrrole Modified Glassy Carbon Electrode

    Directory of Open Access Journals (Sweden)

    Abd-Elgawad Radi

    2016-01-01

    Full Text Available A novel electrochemical sensing approach, based on electropolymerization of a molecularly imprinted polypyrrole (MIPpy film onto a glassy carbon electrode (GCE surface, was developed for the detection of flunixin (FXN. The sensing conditions and the performance of the constructed sensor were assessed by cyclic, differential pulse and (DPV square wave voltammetry (SWV. The sensor exhibited high sensitivity, with linear responses in the range of 5.0 to 50.0 µM with detection limits of 1.5 and 1.0 µM for DPV and SWV, respectively. In addition, the sensor showed high selectivity towards FXN in comparison to other interferents. The sensor was successfully utilized for the direct determination of FXN in buffalo raw milk samples.

  6. Repercussions of modified procedural roles on determining the facts in criminal proceedings

    Directory of Open Access Journals (Sweden)

    Ilić Ivan

    2014-01-01

    Full Text Available The main characteristic of the new Code of Criminal Procedure, 2011, which is based on adversial principle, is changed position of the main subjects. The public prosecutor gets more active role. It is head of the pre-investigative procedure and the investigation. At trial, the role of the parties emphasized, while the role of the court passivated. The Court adjudicate and manage the process, while in the presentation of evidence, for the proper and complete determination of the facts, his role significantly diminished. The court is not obliged ex officio to determine the truth, and the principle of truth is omitted from the basic principles of criminal procedure. Evidentiary initiative is, largely, up to the parties, while the court granted subsidiary role. Basis of the work is the thesis that the Code of Criminal Procedure from 2011, based on the truth principle, which is also the goal of the procedure. In fact, while working on the development of the legal text, and after of the adoption, to the beginning of its application in full range, in professional community there were lots of papers, which cast doubt on the principle of truth existence, in the currently valid procedural law of Serbia. Although this principle is not actually explicitly stipulated in the text of the new CPC, the author proves his existence by analyzing of certain provisions of the law, which has significantly altered the position of the main criminal procedural subjects, in terms establishing the facts in criminal proceedings. The author argues that the truth about a criminal matter remains the highest goal of the procedure, despite the fact that the concept of criminal proceedings is set on the adversial model od criminal proceedings.

  7. A modified assay method for determining serotonin uptake in human platelets

    International Nuclear Information System (INIS)

    Arora, R.C.; Meltzer, H.Y.

    1981-01-01

    Effects of various experimental conditions on serotonin (5-HT) uptake in human platelets were examined. The experimental design allowed the evaluation of the effect of diffusion and other non-saturable processes on the affinity and maximum activity of the membrane pump for 5-HT uptake. Total 5-HT uptake was determined by incubating platelet-rich plasma (PRP) with increasing concentrations of serotonin at 37 0 C for 4 min. The passive uptake was measured by the addition of various 5-HT concentrations to PRP in buffer at 37 0 C, followed by immediate transfer to an ice-cold water bath. The difference between the total and passive uptake was linear for 6 min. The affinity (Ksub(m)) for active platelet serotonin uptake was 0.45 +- 0.09 μmol/l and maximal rate of uptake (V) was 10.7 +- 2.1 pmol/10 7 platelets/min. The described method provides a convenient and reliable measure of active 5-HT uptake suitable for clinical investigation. The effect of passive diffusion on kinetic parameters is discussed. (Auth.)

  8. Determination of dopamine in presence of ascorbic acid and uric acid using poly (Spands Reagent) modified carbon paste electrode

    Energy Technology Data Exchange (ETDEWEB)

    Veera Manohara Reddy, Y.; Prabhakara Rao, V.; Vijaya Bhaskar Reddy, A.; Lavanya, M.; Venu, M.; Lavanya, M.; Madhavi, G., E-mail: gmchem01@gmail.com

    2015-12-01

    In this paper, we have fabricated a modified carbon paste electrode (CPE) by electropolymerisation of spands reagent (SR) onto surface of CPE using cyclic voltammetry (CV). The developed electrode was abbreviated as poly(SR)/CPE and the surface morphology of the modified electrode was studied by using scanning electron microscopy (SEM). The developed electrode showed higher electrocatalytic properties towards the detection of dopamine (DA) in 0.1 M phosphate buffer solution (PBS) at pH 7.0. The effect of pH, scan rate, accumulation time and concentration of dopamine was studied at poly(SR)/CPE. The poly(SR)/CPE was successfully used as a sensor for the selective determination of DA in presence of ascorbic acid (AA) and uric acid (UA) without any interference. The poly(SR)/CPE showed a good detection limit of 0.7 μM over the linear dynamic range of 1.6 μM to 16 μM, which is extremely lower than the reported methods. The prepared poly(SR)/CPE exhibited good stability, high sensitivity, better reproducibility, low detection limit towards the determination of DA. The developed method was also applied for the determination of DA in real samples. - Highlights: • Electropolymerization of spands reagent was fabricated by cyclic voltammetry • The Poly (spands reagent) electrode shows excellent electrocatalytic activity for the detection of dopamine. • The detection limit for dopamine was found to be 0.7 μM. • The proposed method can be applied for DA in injection and human blood serum samples.

  9. Preconcentration of gold ions from water samples by modified organo-nanoclay sorbent prior to flame atomic absorption spectrometry determination

    Energy Technology Data Exchange (ETDEWEB)

    Afzali, Daryoush, E-mail: daryoush_afzali@yahoo.com [Nanochemistry Department, Research Institute of Environmental Sciences, International Center for Science, High Technology and Environmental Sciences, Kerman (Iran, Islamic Republic of); Mostafavi, Ali [Chemistry Department, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Mirzaei, Mohammad [Nanochemistry Department, Research Institute of Environmental Sciences, International Center for Science, High Technology and Environmental Sciences, Kerman (Iran, Islamic Republic of); Chemistry Department, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of)

    2010-09-15

    In this work, the applicability of modified organo nanoclay as a new and easy prepared solid sorbent for the preconcentration of trace amounts of Au(III) ion from water samples is studied. The organo nanoclay was modified with 5-(4'-dimethylamino benzyliden)-rhodanine and used as a sorbent for separation of Au(III) ions. The sorption of gold ions was quantitative in the pH range of 2.0-6.0. Quantitative desorption occurred with 6.0 mL of 1.0 mol L{sup -1} Na{sub 2}S{sub 2}O{sub 3}. The amount of eluted Au(III) was measured using flame atomic absorption spectrometry. In the initial solution the linear dynamic range was in the range of 0.45 ng mL{sup -1} to 10.0 {mu}g mL{sup -1}, the detection limit was 0.1 ng mL{sup -1} and the preconcentration factor was 105. Also, the relative standard deviation was {+-}2.3% (n = 8 and C = 2.0 {mu}g mL{sup -1}) and the maximum capacity of the sorbent was 3.9 mg of Au(III) per gram of modified organo nanoclay. The influences of the experimental parameters including sample pH, eluent volume and eluent type, sample volume, and interference of some ions on the recoveries of the gold ion were investigated. The proposed method was applied for preconcentration and determination of gold in different samples.

  10. Direct determination of lead in human urine and serum samples by electrothermal atomic absorption spectrometry and permanent modifiers

    International Nuclear Information System (INIS)

    Andrada, Daniel; Pinto, Frederico G.; Magalhaes, Cristina Goncalves; Nunes, Berta R.; Silva, Jose Bento Borba da; Franco, Milton B.

    2006-01-01

    The object of the present study was the development of alternative methods for the direct determination of lead in undigested samples of human urine and serum by electrothermal atomic absorption spectrometry (ETAAS). Thus, some substances have been investigated to act as chemical modifiers. Volumes of 20 μL of diluted samples, 1 + 1, v/v for urine and 1 + 4, v/v for serum, with HNO 3 1% v/v and 0.02% v/v of cetyl trimethyl ammonium chloride (CTAC) were prepared directly in the autosampler cups and placed into the graphite furnace. For modifiers in solutions 10 μL were used. Pyrolysis and atomization temperature curves were used in all optimizations in the matrixes diluted as exposed. For urine with permanent iridium (500 μg), the best pyrolysis and atomization temperatures were 900 and 1600 deg C, respectively, with a characteristic mass of 12 pg (recommended of 10 pg), with symmetrical absorption pulses and corrected background. Spiked urine samples presented recoveries between 86 and 112% for Ir permanent. The analysis results of certified urine samples are in agreement with certified values (95% of confidence) for two levels of the metal. For serum, good results were obtained with the mixture of Zr+Rh or Ir+Rh as permanent modifiers, with characteristic masses of 9.8 and 8.1 pg, respectively. Recoveries from spiked serum samples varied between 98.6 and 100.1% (Ir+Rh) and between 93.9 and 105.2% (Zr+Rh). In both recovery studies, the relative standard deviation (n=3) was lower than 7%. Calibration for both samples were made with aqueous calibration curves and presented r 2 higher than 0.99. The limits of detection were 0.7 μg L -1 for serum samples, with Zr+Rh permanent, and 1.0 μg L -1 for urine with iridium permanent. (author)

  11. Direct determination of lead in human urine and serum samples by electrothermal atomic absorption spectrometry and permanent modifiers

    Directory of Open Access Journals (Sweden)

    Andrada Daniel

    2006-01-01

    Full Text Available The object of the present study was the development of alternative methods for the direct determination of lead in undigested samples of human urine and serum by electrothermal atomic absorption spectrometry (ET AAS. Thus, some substances have been investigated to act as chemical modifiers. Volumes of 20 µL of diluted samples, 1 + 1, v/v for urine and 1 + 4, v/v for serum, with HNO3 1% v/v and 0.02% v/v of cetil trimethyl ammonium chloride (CTAC were prepared directly in the autosampler cups and placed into the graphite furnace. For modifiers in solutions 10 µL were used. Pyrolysis and atomization temperature curves were used in all optimizations in the matrixes diluted as exposed. For urine with permanent iridium (500 µg, the best pyrolysis and atomization temperatures were 900 and 1600 ºC, respectively, with a characteristic mass of 12 pg (recommended of 10 pg, with symmetrical absorption pulses and corrected background. Spiked urine samples presented recoveries between 86 and 112% for Ir permanent. The analysis results of certified urine samples are in agreement with certified values (95% of confidence for two levels of the metal. For serum, good results were obtained with the mixture of Zr+Rh or Ir+Rh as permanent modifiers, with characteristic masses of 9.8 and 8.1 pg, respectively. Recoveries from spiked serum samples varied between 98.6 and 100.1% (Ir+Rh and between 93.9 and 105.2% (Zr+Rh. In both recovery studies, the relative standard deviation (n=3 was lower than 7%. Calibration for both samples were made with aqueous calibration curves and presented r² higher than 0.99. The limits of detection were 0.7 µg L-1 for serum samples, with Zr+Rh permanent, and 1.0 µg L-1 for urine with iridium permanent.

  12. Experience in usage of T-108 titrimetric laboratory unit for precision analysis of uranium-containing materials

    International Nuclear Information System (INIS)

    Ryzhinskij, M.V.; Bronzov, P.A.

    1989-01-01

    Possibilities of the T-108 device of potentiometric titration for precise determination of uranium in various uranium-containing materials are studied, the results being presented. Principle flowsheet of the device and the sequence of analytic procedure of uranium potentiometric titration are considered. U 3 O 8 , UO 2 and UF 4 were used as materials to be analyzed, state standard samples of K 2 Cr 2 O 7 -SSS 2215-81 and U 3 O 8 SSS 2396-83P- as standard samples. It is shown that relative standard deviation during titration using the T-108 device is mainly determined by the error of determination of the final titration point potention and it must not exceed 0.002 for uranium titration considered. The conclusion is made that the variant of potentiometric titration of uranium with the use of the T-108 device is not inferior in its accuracy to gravimetry and surpasses it in productivity and possibility of automation. 4 refs.; 2 figs.; 2 tabs

  13. Surface modification of amine-functionalised graphite for preparation of cobalt hexacyanoferrate (CoHCF)-modified electrode: an amperometric sensor for determination of butylated hydroxyanisole (BHA).

    Science.gov (United States)

    Prabakar, S J Richard; Narayanan, S Sriman

    2006-12-01

    A cobalt hexacyanoferrate (CoHCF)-modified graphite paraffin wax composite electrode was prepared by a new approach. An amine-functionalised graphite powder was used for the fabrication of the electrode. A functionalised graphite paraffin wax composite electrode was prepared and the surface of the electrode was modified with a thin film of CoHCF. Various parameters that influence the electrochemical behaviour of the modified electrode were studied by varying the background electrolytes, scan rates and pH. The modified electrode showed good electrocatalytic activity towards the oxidation of butylated hydroxyanisole (BHA) under optimal conditions and showed a linear response over the range from 7.9 x 10(-7) to 1.9 x 10(-4) M of BHA with a correlation coefficient of 0.9988. The limit of detection was 1.9 x 10(-7) M. Electrocatalytic oxidation of BHA was effective at the modified electrode at a significantly reduced potential and at a broader pH range. The utility of the modified electrode as an amperometric sensor for the determination of BHA in flow systems was evaluated by carrying out hydrodynamic and chronoamperometric experiments. The modified electrode showed very good stability and a longer shelf life. The modified electrode was applied for the determination of BHA in spiked samples of chewing gum and edible sunflower oil. The advantage of this method is the ease of electrode fabrication, good stability, longer shelf life, low cost and its diverse application for BHA determination.

  14. Electrochemical Determination of Chlorpyrifos on a Nano-TiO₂Cellulose Acetate Composite Modified Glassy Carbon Electrode.

    Science.gov (United States)

    Kumaravel, Ammasai; Chandrasekaran, Maruthai

    2015-07-15

    A rapid and simple method of determination of chlorpyrifos is important in environmental monitoring and quality control. Electrochemical methods for the determination of pesticides are fast, sensitive, reproducible, and cost-effective. The key factor in electrochemical methods is the choice of suitable electrode materials. The electrode materials should have good stability, reproducibility, more sensitivity, and easy method of preparation. Mercury-based electrodes have been widely used for the determination of chlorpyrifos. From an environmental point of view mercury cannot be used. In this study a biocompatible nano-TiO2/cellulose acetate modified glassy carbon electrode was prepared by a simple method and used for the electrochemical sensing of chlorpyrifos in aqueous methanolic solution. Electroanalytical techniques such as cyclic voltammetry, differential pulse voltammetry, and amperometry were used in this work. This electrode showed very good stability, reproducibility, and sensitivity. A well-defined peak was obtained for the reduction of chlorpyrifos in cyclic voltammetry and differential pulse voltammetry. A smooth noise-free current response was obtained in amperometric analysis. The peak current obtained was proportional to the concentration of chlorpyrifos and was used to determine the unknown concentration of chlorpyrifos in the samples. Analytical parameters such as LOD, LOQ, and linear range were estimated. Analysis of real samples was also carried out. The results were validated through HPLC. This composite electrode can be used as an alternative to mercury electrodes reported in the literature.

  15. Adsorptive stripping voltammetric determination of nitroimidazole derivative on multiwalled carbon nanotube modified electrodes: influence of size and functionalization of nanotubes

    Energy Technology Data Exchange (ETDEWEB)

    Jara-Ulloa, Paola; Canete-Rosales, Paulina; Nunez-Vergara, Luis J; Squella, Juan A., E-mail: asquella@ciq.uchile.c [University of Chile, Santiago (Chile). Chemical and Pharmaceutical Sciences Faculty. Bioelectrochemistry Lab.

    2011-07-01

    1-Methyl-4-nitro-2-bromine methylimidazole (4-NimMeBr), was electrochemically reduced on mercury, glassy carbon and multiwalled carbon nanotubes (MWCNT) modified electrodes. 4-NimMeBr was adsorbed on the MWCNT modified electrode thus permitting the implementation of an adsorptive stripping voltammetric (ASV) method. We have used 4-NimMeBr as a prototype electroactive nitro compound to study the effect of both the size of the nanotubes and its functionalization by oxidation. The oxidized MWCNT forms better dispersions than the non-oxidized, producing electrode surface with higher density of MWCNT as was determined by electrochemical mapping using scanning electrochemical microscopy (SECM). Under the optimized conditions, the peak current was proportional to the concentration of 4-NimMeBr in the range of 10{sup -6} mol L{sup -1} to 10{sup -4} mol L{sup -1} with detection and quantification limits of 4.41 x 10{sup -6} mol L{sup -1} and 6.21 x 10{sup -6} mol L{sup -1}, respectively. The sensibility of bare electrode was 0.01 {mu}A per mmol L{sup -1}, which was lower than the value of 5.34 and 6.97 mA per mmol L{sup -1} obtained using short and large oxidized MWCNT, respectively. (author)

  16. Cathodic stripping voltammetric determination of chromium in coastal waters on cubic Nano-titanium carbide loaded gold nanoparticles modified electrode

    Directory of Open Access Journals (Sweden)

    Haitao eHan

    2015-09-01

    Full Text Available The novel cubical nano-titanium carbide loaded gold nanoparticles modified electrode for selective and sensitive detection of trace chromium (Cr in coastal water was established based on a simple approach. Nano-titanium carbide is used as the typical cubical nanomaterial with wonderful catalytic activity towards the reduction of Cr(VI. Gold nanoparticles with excellent physical and chemical properties can facilitate electron transfer and enhance the catalytic activity of the modified electrode. Taking advantage of the synergistic effects of nano-titanium carbide and gold nanoparticles, the excellent cathodic signal responses for the stripping determination of Cr(VI can be obtained. The detection limit of this method is calculated as 2.08 μg L-1 with the linear calibration curve ranged from 5.2 to 1040 μg L-1. This analytical method can be used to detect Cr(VI effectively without using any complexing agent. The fabricated electrode was successfully applied for the detection of chromium in coastal waters collected from the estuary giving Cr concentrations between 12.48 and 22.88 μg L-1 with the recovery between 96% and 105%.

  17. Determination of the most favorable experimental conditions for obtaining asphalt emulsions modified with discarded polymers in the reconstruction of pavements

    International Nuclear Information System (INIS)

    Coward Ugalde, Hector Arturo

    2014-01-01

    The most favorable experimental conditions are determined for the production of asphalt emulsions modified with tire scrap rubber, petroleum material and recycled asphalt in the reconstruction of flexible pavements in a slow breaking process. Asphalt emulsions are made with 65% V/V of fluidized asphalt at different conditions of operation and composition of soap solution. The equipment of a centrifugal pump and a colloidal mill are used. Two different compositions are employed to make soap solutions. The best conditions to prepare the asphalt emulsions in the pilot plant have been: a stirring speed of 2100 rpm in the centrifugal pump and a speed of 3300 rpm of the colloidal mill. Asphaltic grouts made with asphalt emulsion modified to 1% m/m of rubber have shown the best coverage in the stripping test, evidencing little asphalt release, high adhesion of the asphalt on the aggregate and good stability. Asphalt emulsions with rubber are recommended with a granulometry that passes the No. 200 mesh for rubber and use the indicated equipment to carry out the process of asphalt modification to obtain better results in the performance of asphalt emulsion [es

  18. Electrochemical behavior of folic acid at calixarene based chemically modified electrodes and its determination by adsorptive stripping voltammetry

    International Nuclear Information System (INIS)

    Vaze, Vishwanath D.; Srivastava, Ashwini K.

    2007-01-01

    Voltammetric behavior of folic acid at plain carbon paste electrode and electrode modified with calixarenes has been studied. Two peaks for irreversible oxidation were observed. Out of the three calixarenes chosen for modification of the electrodes, p-tert-butyl-calix[6]arene modified electrode (CME-6) was found to have better sensitivity for folic acid. Chronocoulometric and differential pulse voltammetric studies reveal that folic acid can assemble at CME-6 to form a monolayer whose electron transfer rate is 0.00273 s -1 with 2-electron/2-proton transfer for the peak at +0.71 V against SCE. An adsorption equilibrium constant of 5 x 10 3 l/mol for maximum surface coverage of 2.89 x 10 -10 mol/cm 2 was obtained. The current is found to be rectilinear with concentration by differential pulse voltammetry. However, linearity in the lower range of concentration 8.79 x 10 -12 M to 1.93 x 10 -9 M with correlation coefficient of 0.9920 was achieved by adsorptive stripping voltammetry. The limit of detection obtained was found to be 1.24 x 10 -12 M. This method was used for the determination of folic acid in a variety of samples, viz. serum, asparagus, spinach, oranges and multivitamin preparations

  19. Modified Dispersive Liquid-Liquid Micro Extraction Using Green Solvent for Determination of Polycyclic Aromatic Hydrocarbons (PAHs) in Vegetable Samples

    International Nuclear Information System (INIS)

    Kin, C.M.; Shing, W.L.

    2016-01-01

    According to International Agency for Research on Cancer (IARC), most of Polycyclic Aromatic Hydrocarbons (PAHs) known as genotoxic human carcinogen and mutagenic. PAHs represent as poorly degradable pollutants that exist in soils, sediments, surface water and atmosphere. A simple, rapid and sensitive extraction method termed modified Dispersive Liquid-Liquid Micro extraction (DLLME) using green solvent was developed to determine PAHs in vegetable samples namely radish, cabbage and cucumber prior to Gas Chromatography Flame Ionization Detection (GC-FID). The extraction method is based on replacing chlorinated organic extraction solvent in the conventional DLLME with low toxic solvent, 1-bromo-3-methylbutane without using dispersive solvent. Several experimental factors such as type and volume of extraction solvents, extraction time, confirmation of 12 PAHs by GC-MS, recovery percentages on vegetable samples and the comparative analysis with conventional DLLME were carried out. Both DLLME were successfully extracted 12 types of PAHs. In modified DLLME, the recoveries of the analytes obtained were in a range of 72.72 - 88.07 % with RSD value below 7.5 % which is comparable to the conventional DLLME. The use of microliter of low toxic extraction solvent without addition of dispersive solvent caused the method is economic and environmental friendly which is fulfill the current requirement, green chemistry based analytical method. (author)

  20. Electrochemical behavior of folic acid at calixarene based chemically modified electrodes and its determination by adsorptive stripping voltammetry

    Energy Technology Data Exchange (ETDEWEB)

    Vaze, Vishwanath D. [Department of Chemistry, University of Mumbai, Vidyanagari, Santacruz (East), Mumbai 400098 (India); Srivastava, Ashwini K. [Department of Chemistry, University of Mumbai, Vidyanagari, Santacruz (East), Mumbai 400098 (India)], E-mail: aksrivastava@chem.mu.ac.in

    2007-12-31

    Voltammetric behavior of folic acid at plain carbon paste electrode and electrode modified with calixarenes has been studied. Two peaks for irreversible oxidation were observed. Out of the three calixarenes chosen for modification of the electrodes, p-tert-butyl-calix[6]arene modified electrode (CME-6) was found to have better sensitivity for folic acid. Chronocoulometric and differential pulse voltammetric studies reveal that folic acid can assemble at CME-6 to form a monolayer whose electron transfer rate is 0.00273 s{sup -1} with 2-electron/2-proton transfer for the peak at +0.71 V against SCE. An adsorption equilibrium constant of 5 x 10{sup 3} l/mol for maximum surface coverage of 2.89 x 10{sup -10} mol/cm{sup 2} was obtained. The current is found to be rectilinear with concentration by differential pulse voltammetry. However, linearity in the lower range of concentration 8.79 x 10{sup -12} M to 1.93 x 10{sup -9} M with correlation coefficient of 0.9920 was achieved by adsorptive stripping voltammetry. The limit of detection obtained was found to be 1.24 x 10{sup -12} M. This method was used for the determination of folic acid in a variety of samples, viz. serum, asparagus, spinach, oranges and multivitamin preparations.

  1. Comparation of fundamental analytical methods for quantitative determination of copper(IIion

    Directory of Open Access Journals (Sweden)

    Ačanski Marijana M.

    2008-01-01

    Full Text Available Copper is a ductile metal with excellent electrical conductivity, and finds extensive use as an electrical conductor, heat conductor, as a building material, and as a component of various alloys. In this work accuracy of methods for quantitative determination (gravimetric and titrimetric methods of analysis of copper(II ion was studied. Gravimetric methods do not require a calibration or standardization step (as all other analytical procedures except coulometry do because the results are calculated directly from the experimental data and molar masses. Thus, when only one or two samples are to be analyzed, a gravimetric procedure may be the method of choice because it involves less time and effort than a procedure that requires preparation of standards and calibration. In this work in gravimetric analysis the concentration of copper(II ion is established through the measurement of a mass of CuSCN and CuO. Titrimetric methods is a process in which a standard reagent is added to a solution of an analyze until the reaction between the analyze and reagent is judged to be complete. In this work in titrimetric analysis the concentration of copper(II ion is established through the measurement of a volume of different standard reagents: Km, Na2S2O3 and AgNO3. Results were discussed individually and mutually with the aspect of exactility, reproductivity and rapidity. Relative error was calculated for all methods.

  2. Preparation of alanine and tyrosine functionalized graphene oxide nanoflakes and their modified carbon paste electrodes for the determination of dopamine

    International Nuclear Information System (INIS)

    Kumar, Mohan; Swamy, B.E. Kumara; Asif, M.H. Mohammed; Viswanath, C.C.

    2017-01-01

    Highlights: • The prepared graphene oxide was functionalized by alanine and tyrosine. • The prepared materials were used for sensor for dopamine. • The functionalized graphene oxide modified carbon paste electrodes shows good sensitivity, stability and repeatability. - Abstract: Herein, established the synthesis of graphene oxide (GO) by Hummers Method with addition of KMnO_4 followed by thermal heating at 80 °C. The obtained GO was further functionalized by alanine and tyrosine. The prepared GO, alanine functionalized GO nanoflakes (AGONF) and tyrosine functionalized GO nanoflakes (TGONF) were characterized by spectroscopic technique using energy-dispersive spectroscopy (EDS), quantitatively by scanning electron microscopy (SEM) and structural studies along with interlayer distance verified through X-ray diffraction technique. Afterwards, the prepared AGONF and TGONF were used as the modifier for the carbon paste electrode (CPE). The electrochemical behavior of the AGONF and TGONF modified carbon paste electrodes (MCPEs) towards dopamine (DA) in phosphate buffer solution (PBS) were examined by cyclic voltammetric (CV) technique and the obtained consequences showed good electrocatalytic activity of MCPEs by increasing the redox peak current with a lower potential difference compared to the bare CPE (BCPE). The AGONF and TGONF MCPEs were further used for the optimization studies. From the pH studies, it was found that the equal number of proton and electron transfer reaction involved in both the modified electrodes. The scan rate studies demonstrate the adsorption controlled electrode process at AGONF MCPE and diffusion controlled at TGONF MCPE. The oxidation peak current increased linearly with two concentration interval of DA at a range of 2–7 μM and 10–30 μM in presence of PBS (pH 7.4) at MCPEs and the limit of detection (LOD) were found to be 0.84 μM and 0.96 μM for first interval DA concentration range (2–7 μM) at AGONF and TGONF MCPE. The

  3. Determination of arsenic and cadmium in shellfish samples by graphite furnace atomic absorption spectrometry using matrix modifier

    International Nuclear Information System (INIS)

    Cortez Diaz, Mirella del Carmen

    2002-01-01

    Heavy metals are a big source of environmental contamination and are also highly toxic to humans. Since shellfish are bio-accumulators of these metals, proper techniques for quantifying them should be available. This work aims to develop an analytical method for the quantitative determination of heavy metals in biological materials (shellfish), specifically arsenic and cadmium at the trace level, using graphite furnace atomic absorption spectrometry, for which nickel and phosphate solutions were used to modify the modifiers. Prior to the analysis, the sample was diluted with nitric acid in a DAB II pressure digestion system order to destroy the organic matter. The instrument conditions were initially set (wavelength, slit, integration peaks, graphite tube, etc.), then the work range was defined for each element and the most appropriate operational parameters were studied, such as: temperature, ramp times, hold times and internal gas flow, in the different stage of the electrothermal treatment (drying, calcination, atomization) for the furnace program. Once the above mentioned conditions were set and since this was a biological sample, a matrix chemical modifier had to be used, in order to make the elements that accompany the element being studied more volatile. In this way the chemical and spectral interferences decrease together with the high background absorption of the matrix. Therefore, different matrix modifiers were studied for the definition of each analyte. The method validation was done using Certified Oyster Tissue Reference Material N o 1566a from the National Institute of Standards and Technology applying different tests in order to eliminate outliers. Repeatability, uncertainty, sensitivity, lineal range, working range, detection limit and quantification limit were evaluated for each element, and the results were compared with the values for the certified material. The Fisher and Student tests were the statistical tools used. The experimental values

  4. Preparation of alanine and tyrosine functionalized graphene oxide nanoflakes and their modified carbon paste electrodes for the determination of dopamine

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, Mohan [Department of P.G. Studies and Research in Industrial Chemistry, Kuvempu University, Shankaraghatta, 577 451, Shimoga, Karnataka (India); Swamy, B.E. Kumara, E-mail: kumaraswamy21@yahoo.com [Department of P.G. Studies and Research in Industrial Chemistry, Kuvempu University, Shankaraghatta, 577 451, Shimoga, Karnataka (India); Asif, M.H. Mohammed [Nanoscience and Technology, Kuvempu University, Shankaraghatta, 577451, Shimoga, Karnataka (India); Viswanath, C.C. [Department of P.G. Studies and Research in Industrial Chemistry, Kuvempu University, Shankaraghatta, 577 451, Shimoga, Karnataka (India)

    2017-03-31

    Highlights: • The prepared graphene oxide was functionalized by alanine and tyrosine. • The prepared materials were used for sensor for dopamine. • The functionalized graphene oxide modified carbon paste electrodes shows good sensitivity, stability and repeatability. - Abstract: Herein, established the synthesis of graphene oxide (GO) by Hummers Method with addition of KMnO{sub 4} followed by thermal heating at 80 °C. The obtained GO was further functionalized by alanine and tyrosine. The prepared GO, alanine functionalized GO nanoflakes (AGONF) and tyrosine functionalized GO nanoflakes (TGONF) were characterized by spectroscopic technique using energy-dispersive spectroscopy (EDS), quantitatively by scanning electron microscopy (SEM) and structural studies along with interlayer distance verified through X-ray diffraction technique. Afterwards, the prepared AGONF and TGONF were used as the modifier for the carbon paste electrode (CPE). The electrochemical behavior of the AGONF and TGONF modified carbon paste electrodes (MCPEs) towards dopamine (DA) in phosphate buffer solution (PBS) were examined by cyclic voltammetric (CV) technique and the obtained consequences showed good electrocatalytic activity of MCPEs by increasing the redox peak current with a lower potential difference compared to the bare CPE (BCPE). The AGONF and TGONF MCPEs were further used for the optimization studies. From the pH studies, it was found that the equal number of proton and electron transfer reaction involved in both the modified electrodes. The scan rate studies demonstrate the adsorption controlled electrode process at AGONF MCPE and diffusion controlled at TGONF MCPE. The oxidation peak current increased linearly with two concentration interval of DA at a range of 2–7 μM and 10–30 μM in presence of PBS (pH 7.4) at MCPEs and the limit of detection (LOD) were found to be 0.84 μM and 0.96 μM for first interval DA concentration range (2–7 μM) at AGONF and TGONF MCPE

  5. Determination of Patulin Using Amperometric Tyrosinase Biosensors Based on Electrodes Modified with Carbon Nanotubes and Gold Nanoparticles

    Directory of Open Access Journals (Sweden)

    R.M. Varlamova

    2016-06-01

    Full Text Available New amperometric biosensors based on platinum screen printed electrodes modified with multi-walled carbon nanotubes, gold nanoparticles, and immobilized enzyme – tyrosinase have been developed for determination of patulin in the concentrations of 1·10–6 – 8·10–12 mol/L with an error of no more than 0.063. The best conditions for obtaining gold nanoparticles have been chosen. The conditions for immobilization of multi-walled carbon nanotubes and gold nanoparticles on the surface of the planar electrode have been revealed. The conditions for functioning of the proposed biosensors have been identified. The results have been used to control the content of patulin in food products within and lower than the maximum allowable levels.

  6. Determination of zinc and cadmium with characterized Electrodes of carbon and polyurethane modified by a bismuth film

    Directory of Open Access Journals (Sweden)

    Jossy Karla Brasil Bernardelli

    2011-09-01

    Full Text Available This study aims to use electrodes modified with bismuth films for the determination of zinc and cadmium. The film was electrodeposited ex situ on a composite carbon electrode with polyurethane and 2% metallic bismuth (2BiE and on a carbon bar electrode (CBE. The electrodes were characterized by scanning electron microscopy and energy dispersive spectroscopy. Through differential pulse anodic stripping voltammetry, the electrodes 2BiE and CBE containing bismuth films showed a limit of detection (LOD of 5.56 × 10-5 and 3.07 × 10-5 g.L-1 for cadmium and 1.24 × 10-4 and 1.53 × 10-4 g.L-1 for zinc, respectively. The presence of a bismuth film increased the sensitivity of both electrodes.

  7. Determination of total and electrolabile copper in agricultural soil by using disposable modified-carbon screen-printed electrodes.

    Science.gov (United States)

    Faucher, Stéphane; Cugnet, Cyril; Authier, Laurent; Lespes, Gaëtane

    2014-02-01

    The objective of the study is to evaluate modified-carbon screen-printed working electrodes (SPE) combined with square wave anodic stripping voltammetry (SWASV) to determine electrolabile and total copper in soils with the perspective to assess the environmental hazard resulting from copper anthropogenic contamination. The voltammetric method was investigated using a mineralized certified reference soil such that it can be assumed that the copper was totally under electrolabile form in the solution of mineralized soil. In optimal conditions, a copper recovery of 97% and a relative standard deviation (RSD) of 9% were found. The limits of detection and quantification for copper were 0.4 and 1.3 μg L(-1), respectively. Finally, the method was applied on soil leachates, which allowed evaluating the cupric transfer from the soil to the leachates and quantifying the electrolabile copper part in leachates.

  8. ELECTROCHEMICAL DETERMINATION OF ETHANOL, 2- PROPANOL AND 1-BUTANOL ON GLASSY CARBON ELECTRODE MODIFIED WITH NICKEL OXIDE FILM

    Directory of Open Access Journals (Sweden)

    A. Benchettara

    2014-12-01

    Full Text Available In this work, we present the modification of a glassy carbon electrode with nickel oxide film which is performed in two successive steps. In the first one, the electrochemical deposition of metallic nickel on the glassy carbon electrode (GCE is achieved in 0.1M boric acid; in the second step, the metallic deposit is anodically oxidized in 0.1M NaOH. These two operations were carried out in a three electrode cell with a filiform platinum auxiliary electrode, a SCE as potential reference and a working microelectrode of modified glassy carbon with nickel oxides. This electrode is characterized by several electrochemical techniques and is used for the catalytic determination of ethanol, 2-propanol and 1-butanol in 0.1 M NaOH. The proposed chemical mechanism shows that NiO2 acts as a mediator.

  9. Determination of quercetin using a photo-electrochemical sensor modified with titanium dioxide and a platinum(II)-porphyrin complex

    International Nuclear Information System (INIS)

    Tian, Li; Wang, Binbin; Chen, Ruizhan; Gao, Ye; Chen, Yanling; Li, Tianjiao

    2015-01-01

    A glassy carbon electrode (GCE) was modified with a film containing titanium dioxide and a Pt(II)-porphyrin complex, and its response to quercetin was investigated employing cyclic voltammetry and chronoamperometry. The oxidation current caused by quercetin is largely enhanced under UV illumination. The effects of pH value, mass of TiO 2 in the film, UV illumination time and applied potential were studied. Under optimized conditions, the peak current at a typically applied voltage of +0.4 V depends linearly on the concentration of quercetin in the 0.002 to 50 mg L −1 range. The detection limit (at an SNR of 3) is 0.8 μg L −1 . The method was successfully applied to the determination of quercetin in (spiked) samples of tea and apple juice. (author)

  10. Sulfite oxidase biosensors based on tetrathiafulvalene modified screen-printed carbon electrodes for sulfite determination in wine.

    Science.gov (United States)

    Molinero-Abad, Begoña; Alonso-Lomillo, M Asunción; Domínguez-Renedo, Olga; Arcos-Martínez, M Julia

    2014-02-17

    Screen-printed carbon electrodes have been modified with tetrathiafulvalene and sulfite oxidase enzyme for the sensitive and selective detection of sulfite. Amperometric experimental conditions were optimized taking into account the importance of quantifying sulfite in wine samples and the inherent complexity of these samples, particularly red wine. The biosensor responds to sulfite giving a cathodic current (at +200 mV vs screen-printed Ag/AgCl electrode and pH 6) in a wide concentration range, with a capability of detection of 6 μM (α=β=0.05) at 60°C. The method has been applied to the determination of sulfite in white and red samples, with averages recoveries of 101.5% to 101.8%, respectively. Copyright © 2014 Elsevier B.V. All rights reserved.

  11. ELECTROCHEMICAL DETERMINATION OF ETHANOL, 2- PROPANOL AND 1-BUTANOL ON GLASSY CARBON ELECTRODE MODIFIED WITH NICKEL OXIDE FILM

    Directory of Open Access Journals (Sweden)

    A. Benchettara

    2015-07-01

    Full Text Available In this work, we present the modification of a glassy carbon electrode with nickel oxide film which is performed in two successive steps. In the first one, the electrochemical deposition of metallic nickel on the glassy carbon electrode (GCE is achieved in 0.1M boric acid; in the second step, the metallic deposit is anodically oxidized in 0.1M NaOH. These two operations were carried out in a three electrode cell with a filiform platinum auxiliary electrode, a SCE as potential reference and a working microelectrode of modified glassy carbon with nickel oxides. This electrode is characterized by several electrochemical techniques and is used for the catalytic determination of ethanol, 2-propanol and 1-butanol in 0.1 M NaOH. The proposed chemical mechanism shows that NiO2 acts as a mediator.

  12. Preincubation of Penicillium commune conidia under modified atmosphere conditions: Influence on growth potential as determined by an impedimetric method

    DEFF Research Database (Denmark)

    Haasum, Iben; Nielsen, Per Væggemose

    1996-01-01

    The combined effect of preincubation time, relative humidity (r.h.), headspace carbon dioxide (CO2) and oxygen (O2) on subsequent growth potential of conidia from Penicillium commune was studied using Response Surface Modelling (RSM). Native conidia were preincubated under modified atmosphere...... conditions in sealed vials for 14, 35 and 56 d. Lag time and growth rates were determined using impedance microbiology on a Bactometer. Conidia survived and some swelling was observed during all experimental preincubation conditions. Regression analysis of the subsequent growth responses showed that relative...... humidity in the vials was the most significant factor affecting lag time of the conidia after preincubation for 14 and 35 d. Storage for 35 d extended lag times by 15 h when the level of r.h. was increased from 41% to 80%. After prolonged storage (56 d) r.h and CO2 levels elicited a significant effect...

  13. Graphite electrodes modified by 8-hydroxyquinolines and its application for the determination of copper in trace levels

    Directory of Open Access Journals (Sweden)

    Sousa Eliane R. de

    2006-01-01

    Full Text Available Surface modification by 8-hydroxyquinoline-5-sulfonic acid (8-HQS or 8-hydroxyquinoline (8-HQ on a graphite electrode through irreversible adsorption is reported in this paper. Cyclic voltammetry was used to characterize the surface behavior. The modified surface exhibited an affinity to chelating Cu(II in the solution, forming a Cu(II complex, which was employed for Cu(II trace analysis. Of the metals Zn, Ni, Pb, Co, and Cd, none presented interference until excess concentration of 10 times. Significant interference could be observed from Co(II, Cd(II and Fe(II for an excess concentration of 100 times on the analyte. A differential pulse voltammetry, combined with a preconcentrating-stripping process and a standard addition method was used for the analysis. A detection limit for trace copper determination in water, such as 5.110-9 mol L-1, was obtained.

  14. Electrochemical Behavior and Determination of Chlorogenic Acid Based on Multi-Walled Carbon Nanotubes Modified Screen-Printed Electrode

    Directory of Open Access Journals (Sweden)

    Xiaoyan Ma

    2016-10-01

    Full Text Available In this paper, the multi-walled carbon nanotubes modified screen-printed electrode (MWCNTs/SPE was prepared and the MWCNTs/SPE was employed for the electrochemical determination of the antioxidant substance chlorogenic acids (CGAs. A pair of well-defined redox peaks of CGA was observed at the MWCNTs/SPE in 0.10 mol/L acetic acid-sodium acetate buffer (pH 6.2 and the electrode process was adsorption-controlled. Cyclic voltammetry (CV and differential pulse voltammetry (DPV methods for the determination of CGA were proposed based on the MWCNTs/SPE. Under the optimal conditions, the proposed method exhibited linear ranges from 0.17 to 15.8 µg/mL, and the linear regression equation was Ipa (µA = 4.1993 C (×10−5 mol/L + 1.1039 (r = 0.9976 and the detection limit for CGA could reach 0.12 µg/mL. The recovery of matrine was 94.74%–106.65% (RSD = 2.92% in coffee beans. The proposed method is quick, sensitive, reliable, and can be used for the determination of CGA.

  15. Simultaneous determination of naphthol isomers at poly(3-methylthiophene)-nano-Au modified electrode with the enhancement of surfactant

    Energy Technology Data Exchange (ETDEWEB)

    Li, Linlin [School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100 (China); Shandong Institute for Product Quality Inspection, Jinan 250100 (China); Liu, Enli; Wang, Xiaolin; Chen, Jia [School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100 (China); Zhang, Xiaoli, E-mail: zhangxl@sdu.edu.cn [School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100 (China)

    2015-08-01

    A polymer film incorporated gold nanoparticle modified electrode was fabricated. The fabricated process involved eletrodeposition of gold nanoparticles and electropolymerization of the 3-methylthiophene (abbreviated 3MT) onto the glassy carbon electrode (GCE). The resulting electrode (P3MT-nano-Au/GCE) was characterized by scanning electron microscopy (SEM), and a simultaneous determination of naphthol isomers at P3MT-nano-Au/GCE was studied using semi-derivative voltammetry. Because of the synergistic effect of gold nanoparticles and poly(3MT), the sensitivity and distinguishability in the simultaneous determination of naphthol isomers were greatly increased. Besides, a further increase in the detecting sensitivity of naphthol isomers could be obtained in the presence of surfactant, cetyl trimethyl ammonium bromide (CTAB). Also, the role of different kinds of surfactants was texted and the action mechanism was discussed in detail. Under the optimal conditions, the linear calibration ranges of the determination of naphthols were 7.0 × 10{sup −7} to 1.5 × 10{sup −4} mol/L for 1-naphthol and 1.0 × 10{sup −6} to 1.5 × 10{sup −4} mol/L for 2-naphthol with detection limits of 1.0 × 10{sup −7} and 3.0 × 10{sup −7} mol/L (S/N = 3), respectively. - Highlights: • Nano-Au-polymer film was fabricated by eletrodeposition and electropolymerization. • Naphthol isomers were detected simultaneously. • Surfactant improved the sensitivity and selectivity.

  16. Determination of arsenic and cadmium in shellfish samples by graphite furnace atomic absorption spectrometry using matrix modifier

    International Nuclear Information System (INIS)

    Villalobos Aranda, Juan; Cortez Diaz, Mirella

    2003-01-01

    Serious problems of environmental contamination due to the activity of the man exist at the present time. Where the greater impact is the produced one by heavy metals that go to the sea. Where the shellfish can collect some of them, the highly toxic ones, since these are bioaccumulation of these metals. Therefore one becomes necessary to count with the reliable analytical procedures to determine these elements. The purpose of this work is to present the determination of arsenic and cadmium in shellfish, by spectroscopy of atomic absorption with graphite furnace. For each determined element, solutions of nickel and phosphate like matrix modifiers were used respectively The validation was made using a Reference Certified Material, Oyster ' Tissue 156 (National Institute of Standards and Technology). The sample previously was digested in triplicate by two consecutive days, with nitric acid in a pressure digestion system DAB 11. For each element it was evaluated: limit of detection and quantification, sensitivity, repeatability, linear, slope rank and uncertainty. In addition, the obtained results were compared with the certified values of the certified material of reference using like statistical tools the tests of Student and Fisher. In both tests the calculated values were smaller to the shown ones in table, for degrees of freedom with 95% of confidence. Thus it was verified that it does not exist significant differences between the precision and the average values of the results obtained with respect to the values of the certified material. In addition, the obtained parameters are appropriate for the determination of these trace elements in this type of environmental sample (author)

  17. Utility of solid phase spectrophotometry for the modified determination of trace amounts of cadmium in food samples.

    Science.gov (United States)

    Amin, Alaa S; Gouda, Ayman A

    2012-05-01

    A modified selective, highly sensitive and accurate procedure for the determination of trace amounts of cadmium which reacts with 1-(2-benzothiazolylazo)-2-hydroxy-3-naphthoic acid (BTAHNA) to give a deep violet complex with high molar absorptivity (7.05×10(6)Lmol(-1) cm(-1), 3.92×10(7)Lmol(-1)cm(-1), 1.78×10(8)Lmol(-1)cm(-1), and 4.10×10(8)Lmol(-1)cm(-1)), fixed on a Dowex 1-X8 type anion-exchange resin for 10mL, 100mL, 500mL, and 1000mL, respectively. Calibration is linear over the range 0.2-3.5μgL(-1) with RSD of ⩽1.14% (n=10). The detection and quantification limits were calculated. Increasing the sample volume can enhance the sensitivity. The method has been successfully applied for the determination of Cd(II) in food samples, water samples and some salts samples without interfering effect of various cations and anions. Copyright © 2011 Elsevier Ltd. All rights reserved.

  18. A New Sensor Based on Graphite Screen Printed Electrode Modified With Cu-Nanocomplex for Determination of Paracetamol

    Directory of Open Access Journals (Sweden)

    Hadi Beitollai

    2017-01-01

    Full Text Available Paracetamol is a non-steroidal anti-inflammatory drug used as an antipyretic agent for the alternative to aspirin. Conversely, the overdoses of paracetamol can cause hepatic toxicity and kidney damage. Hence, the determination of paracetamol receives much more attention in biological samples and also in pharmaceutical formulations. Here, we report a rapid and sensitive detection of the paracetamol based on screen-printed modified electrode (SPE with Cu nanocomplex (Cu in pH=7.0. The paracetamol is not stable in strong acidic and strong alkaline media, and is hydrolyzed and hydroxylated. However, it is stable in intermediate pHs due to the dimerization of paracetamol. The kinetics of the paracetamol oxidation was briefly studied and documented in the schemes. In addition, the characterization of Cu nanocomplex was probed by Fourier transform infrared spectroscopy (FT-IR, X-ray diffraction (XRD, scanning electron microscopy (SEM, and energy dispersive X-ray spectroscopy (EDX. Moreover, the voltammetry determined the paracetamol with the linear concentration ranging from 10.0 to 1000.0 μM and the lower detection limit of 1.0 μM. This method was also successfully used to detect the concentration of paracetamol in pharmaceutical formulations and urine samples.

  19. Preparation of polypyrrole/ferrocyanide films modified carbon paste electrode and its application on the electrocatalytic determination of ascorbic acid

    Energy Technology Data Exchange (ETDEWEB)

    Raoof, Jahan-Bakhsh; Ojani, Reza; Rashid-Nadimi, Sahar

    2004-01-15

    Functionalized polypyrrole film were prepared by incorporation of (Fe(CN){sub 6}){sup 4-} as doping anion, during the electropolymerization of pyrrole onto a carbon paste electrode (CPE) in aqueous solution by using potentiostatic method. The electrochemical behavior of the (Fe(CN){sub 6}){sup 3-}/(Fe(CN){sub 6}){sup 4-} redox couple in polypyrrole was studied by cyclic voltammetry and double step potential chronoamperometry methods. In this study, an obvious surface redox reaction was observed and dependence of this reaction on the solution pH was illustrated. The electrocatalytic ability of polypyrrole/ferrocyanide films modified carbon paste electrode (Ppy/FCNMCPEs) was demonstrated by oxidation of ascorbic acid. It has been found that under optimum condition (pH 7.00), the oxidation of ascorbic acid at the surface of such electrode occurs at a potential about 540 mV less positive than unmodified carbon paste electrode. The kinetic parameters such as electron transfer coefficient, {alpha} and catalytic reaction rate constant, k{sub h}', were also determined by using various electrochemical approaches. The catalytic oxidation peak current showed a linear dependent on the ascorbic acid concentration and a linear calibration curve was obtained in the range of 4.5x10{sup -4} to 9.62x10{sup -3} M of ascorbic acid with a correlation coefficient of 0.9999. The detection limit (2{sigma}) was determined as 5.82x10{sup -5} M.

  20. A glassy carbon electrode modified with cerium phosphate nanotubes for the simultaneous determination of hydroquinone, catechol and resorcinol.

    Science.gov (United States)

    Li, Zhen; Yue, Yuhua; Hao, Yanjun; Feng, Shun; Zhou, Xianli

    2018-03-12

    A nafion film containing cerium phosphate nanotubes was pasted onto a glassy carbon electrode (GCE) to obtain a sensor for hydroquinone (HQ). The morphologies and components of the coating were characterized by transmission electron microscopy, scanning electron microscopy and energy-dispersive spectroscopy. Cyclic voltammetry and differential pulse voltammetry (DPV) showed the specific surface of the electrode to be significantly increased and the electron transfer rate to be accelerated. The modified GCE was applied to the determination of hydroquinone (HQ) via DPV. The oxidation current increases linearly in the 0.23 μM to 16 mM HQ concentration range which is as wide as five orders of magnitude. The limit of detection is 0.12 μM (based on a signal-to-noise ratio of 3), and the sensitivity is 1.41 μA·μM -1  cm -2 . The method was further applied to the simultaneous determination of HQ, catechol and resorcinol. The potentials for the three species are well separated (20, 134, and 572 mV vs SCE). Average recoveries from (spiked) real water samples are between 95.2 and 107.0%, with relative standard deviations of 0.9~2.7% (for n = 3) at three spiking levels. The method was validated by independent assays using HPLC. Graphical abstract ᅟ.

  1. Highly sensitive sorption-luminescence determination of trace europium with preconcentration on silica chemically modified with iminodiacetic acid

    International Nuclear Information System (INIS)

    Voronina, R.D.; Zorov, N.B.

    2007-01-01

    Features of a sorption-luminescence method for the determination of trace europium were studied. The method includes the preliminary sorption of europium at pH 7.1 from solutions with silica chemically modified with iminodiacetic acid, the subsequent treatment of the sorbent with 2-thenoyltrifluoroacetone at pH 8.0, and the measurement of the intensity of luminescence of the surface three-component europium complex at 613 nm. The effect of moisture as the quencher of luminescence of the surface europium complex was studied, and techniques for its removal were proposed. Sorption in the static mode provides the detection limit of europium of 7 x 10 -5 g/ml. The calibration plot is linear in the range of two orders of magnitude of europium concentration in solutions. The relative standard deviation in the determination of 1.5 x 10 -2 μg/ml europium is 5%. In the dynamic mode of sorption from 1000 ml of an analyzed solution with the use of sorption-desorption, the detection limit of europium of 8 x 10 -7 μg/ml was attained [ru

  2. Electrochemical Preparation of a Molecularly Imprinted Polypyrrole-modified Pencil Graphite Electrode for Determination of Ascorbic Acid

    Directory of Open Access Journals (Sweden)

    Yücel Sahin

    2008-09-01

    Full Text Available A molecularly imprinted polymer (MIP polypyrrole (PPy-based film was fabricated for the determination of ascorbic acid. The film was prepared by incorporation of a template molecule (ascorbic acid during the electropolymerization of pyrrole onto a pencil graphite electrode (PGE in aqueous solution using a cyclic voltammetry method. The performance of the imprinted and non-imprinted (NIP films was evaluated by differential pulse voltammetry (DPV. The effect of pH, monomer and template concentrations, electropolymerization cycles and interferents on the performance of the MIP electrode was investigated and optimized. The molecularly imprinted film exhibited a high selectivity and sensitivity toward ascorbic acid. The DPV peak current showed a linear dependence on the ascorbic acid concentration and a linear calibration curve was obtained in the range of 0.25 to 7.0 mM of ascorbic acid with a correlation coefficient of 0.9946. The detection limit (3σ was determined as 7.4x10-5 M (S/N=3. The molecularly-imprinted polypyrrole-modified pencil graphite electrode showed a stable and reproducible response, without any influence of interferents commonly existing in pharmaceutical samples. The proposed method is simple and quick. The PPy electrodes have a low response time, good mechanical stability and are disposable simple to construct.

  3. Thallium (III) determination in the Baltic seawater samples by ICP MS after preconcentration on SGX C18 modified with DDTC.

    Science.gov (United States)

    Krasnodębska-Ostręga, Beata; Sadowska, Monika; Piotrowska, Katarzyna; Wojda, Marta

    2013-08-15

    The main difficulty of speciation analysis of thallium lies in extremely low concentrations of Tl(III) in comparison to Tl(I), which is the dominating form of thallium in environmental samples. In this study, a sensitive method is presented for separation of trace amounts of Tl(III) from Tl(I) and preconcentration of Tl(III) using octadecyl silica gel modified with diethyldithiocarbamate (DDTC). Under optimal conditions, only Tl(III) is retained on the sorbent, and then eluted with 96% ethanol. After chemical decomposition of Tl(III)-DDTC complex, thallium is determined by inductively coupled plasma mass spectrometry. High performance liquid chromatography with ICP MS detection was used to control the correctness of the obtained results. Parameters affecting solid phase extraction (SPE) such as pH, type, concentration and volume of eluent, breakthrough volume, and the impact of sample salinity (chlorides) and other interfering ions (Cd(II), Zn(II), Pb(II), Cu(II), Sn(II)) were investigated. The limit of detection (LOD), evaluated for 2 mL of sample solution, was 0.10 ng for Tl(I) and 0.43 ng for Tl(III). The method was applied to the determination of Tl(I) and Tl(III) in the Baltic seawater samples enriched in both thallium species. Copyright © 2013 Elsevier B.V. All rights reserved.

  4. Highly sensitive and selective determination of methylergometrine maleate using carbon nanofibers/silver nanoparticles composite modified carbon paste electrode.

    Science.gov (United States)

    Kalambate, Pramod K; Rawool, Chaitali R; Karna, Shashi P; Srivastava, Ashwini K

    2016-12-01

    A highly sensitive and selective voltammetric method for determination of Methylergometrine maleate (MM) in pharmaceutical formulations, urine and blood serum samples has been developed based on enhanced electrochemical response of MM at carbon nanofibers and silver nanoparticles modified carbon paste electrode (CNF-AgNP-CPE). The electrode material was characterized by various techniques viz., X-ray diffraction, scanning electron microscopy and energy dispersive X-ray spectroscopy. The electrocatalytic response of MM at CNF-AgNP-CPE was studied by cyclic voltammetry (CV), differential pulse voltammetry (DPV) and electrochemical impedance spectroscopy (EIS). Under optimized conditions, the proposed sensor exhibits excellent electrochemical response towards MM. The DPV study shows greatly enhanced electrochemical signal for MM at CNF-AgNP-CPE lending high sensitivity to the proposed sensor for MM detection. The peak (Ip) current for MM is found to be rectilinear in the range 4.0×10(-8)-2.0×10(-5)M with a detection limit of 7.1×10(-9)M using DPV. The feasibility of the proposed sensor in analytical applications was investigated by conducting experiments on commercial pharmaceutical formulations, human urine and blood serum samples, which yielded satisfactory recoveries of MM. The proposed electrochemical sensor offers high sensitivity, selectivity, reproducibility and practical utility. We recommend it as an authentic and productive electrochemical sensor for successful determination of MM. Copyright © 2016. Published by Elsevier B.V.

  5. Electrochemical Determination of Brilliant Blue and Tartrazine Based on an Ionic Liquid-Modified Expanded Graphite Paste Electrode.

    Science.gov (United States)

    Wang, Wenchang; Chen, Ye; Zhang, Jing; Wang, Xue; Chen, Zhidong

    2015-01-01

    A sensitive electrochemical method was developed for the simultaneous determination of Brilliant Blue (BB) and tartrazine (Tz) using an ionic liquid-modified expanded graphite paste electrode (IL-EGPE). The IL-EGPE was prepared by mixing ionic liquid-expanded graphite composite (IL-EG) with solid paraffin. Compared with the EGPE, the IL-EGPE remarkably enhanced the electrocatalytic oxidation signals of BB and Tz. Under optimal experimental conditions, the designed IL-EGPE exhibited wide linear responses to BB and Tz ranging from 5.0×10(-9) to 4.0×10(-6) M and 1.0×10(-8) to 1.0×10(-6) M, respectively. The detection limits for BB and Tz were 2.0×10(-9) M (1.6 ng/mL) and 3.3×10(-9) M (1.8 ng/mL) at an S/N of 3, respectively. This electrode showed good reproducibility, stability, and reusability. The proposed method was successfully applied in the simultaneous determination of BB and Tz in a soft drink with satisfactory results.

  6. Determination of temperature variation during the individual steps of the production of hospital diets of modified consistency.

    Science.gov (United States)

    Monteiro, T H; De Souza Santos, R; Cremonezi Japur, C; Neves Campanelli Marçal Vieira, M

    2011-01-01

    Many disease outbreaks of food origin are caused by foods prepared in Food Service and Nutrition Units of hospitals, affecting hospitalized patients who, in most cases, are immunocompromised and therefore at a higher risk of severe worsening of their clinical status. The aim of this study was to determine the variations in temperature and the time-temperature factor of hospital diets. The time and temperature for the preparation of 4 diets of modified consistency were determined on 5 nonconsecutive days in a hospital Diet and Nutrition Unit at the end of preparation and during the maintenance period, portioning and distribution at 3 sites, i.e., the first, the middle and the last to receive the diets. All foods reached an adequate temperature at the end of cooking, but temperature varied significantly from the maintenance period to the final distribution, characterizing critical periods for microorganism proliferation. During holding, temperatures that presented a risk were reached by 16.7% of the meats and 59% of the salads of the general diet, by 16.7% of the garnishes in the bland diet and by 20% of the meats and garnishes in the viscous diet. The same occurred at the end of distribution for 100% of the hot samples and of the salads and for 61% of the desserts. None of the preparations remained at risk temperature for a time exceeding that established by law. The exposure to inadequate temperature did not last long enough to pose risks to the patient.

  7. Poly(alizarin red)/Graphene modified glassy carbon electrode for simultaneous determination of purine and pyrimidine

    Energy Technology Data Exchange (ETDEWEB)

    Ba Xi; Luo Liqiang [Department of Chemistry, Shanghai University, Shanghai 200444 (China); Ding Yaping, E-mail: wdingyp@sina.com [Department of Chemistry, Shanghai University, Shanghai 200444 (China); Zhang Zhen [Department of Chemistry, Shanghai University, Shanghai 200444 (China); Chu Yuliang [Instrumental Analysis and Research Center, Shanghai University, Shanghai 200444 (China); Wang Bijun; Ouyang Xiaoqian [Department of Chemistry, Shanghai University, Shanghai 200444 (China)

    2012-11-08

    Graphical abstract: DPVs of PAR/Graphene/GCE (a) and the bare GCE (c) in 0.1 M PBS containing 50.0 {mu}M G, 50.0 {mu}M A, 100.0 {mu}M T and 100.0 {mu}M C, (b) PAR/Graphene/GCE in 0.1 M PBS. Highlights: Black-Right-Pointing-Pointer The sensor exhibited well-separated peaks and low detection limit. Black-Right-Pointing-Pointer The sensor possesses high sensitivity and wide linear range. Black-Right-Pointing-Pointer The sensor was used for simultaneous detection of G, A, T and C successfully. Black-Right-Pointing-Pointer The sensor was applied in a fish sperm DNA sample with satisfactory results. Black-Right-Pointing-Pointer The proposed sensor has good stability and reproducibility. - Abstract: In this work, a poly(alizarin red)/Graphene composite film modified glassy carbon electrode (PAR/Graphene/GCE) was prepared for simultaneous determination of four DNA bases (guanine, adenine, thymine and cytosine) without any pretreatment. The morphology and interface property of PAR/Graphene films were examined by scanning electron microscopy and electrochemical impedance spectroscopy. The PAR/Graphene/GCE exhibited excellent electrocatalytic activity toward purine (guanine and adenine) and pyrimidine (thymine and cytosine) in 0.1 M phosphate buffer solution (pH 7.4). Under optimum conditions, differential pulse voltammetry was used to detect the oxidation of purine and pyrimidine. The results showed that PAR/Graphene/GCE exhibited well-separated peaks, low detection limit, high sensitivity and wide linear range for simultaneous detection of purine and pyrimidine. The proposed sensor also has good stability and reproducibility. Furthermore, the modified electrode was applied for the detection of DNA bases in a fish sperm DNA sample with satisfactory results.

  8. Poly(alizarin red)/Graphene modified glassy carbon electrode for simultaneous determination of purine and pyrimidine

    International Nuclear Information System (INIS)

    Ba Xi; Luo Liqiang; Ding Yaping; Zhang Zhen; Chu Yuliang; Wang Bijun; Ouyang Xiaoqian

    2012-01-01

    Graphical abstract: DPVs of PAR/Graphene/GCE (a) and the bare GCE (c) in 0.1 M PBS containing 50.0 μM G, 50.0 μM A, 100.0 μM T and 100.0 μM C, (b) PAR/Graphene/GCE in 0.1 M PBS. Highlights: ► The sensor exhibited well-separated peaks and low detection limit. ► The sensor possesses high sensitivity and wide linear range. ► The sensor was used for simultaneous detection of G, A, T and C successfully. ► The sensor was applied in a fish sperm DNA sample with satisfactory results. ► The proposed sensor has good stability and reproducibility. - Abstract: In this work, a poly(alizarin red)/Graphene composite film modified glassy carbon electrode (PAR/Graphene/GCE) was prepared for simultaneous determination of four DNA bases (guanine, adenine, thymine and cytosine) without any pretreatment. The morphology and interface property of PAR/Graphene films were examined by scanning electron microscopy and electrochemical impedance spectroscopy. The PAR/Graphene/GCE exhibited excellent electrocatalytic activity toward purine (guanine and adenine) and pyrimidine (thymine and cytosine) in 0.1 M phosphate buffer solution (pH 7.4). Under optimum conditions, differential pulse voltammetry was used to detect the oxidation of purine and pyrimidine. The results showed that PAR/Graphene/GCE exhibited well-separated peaks, low detection limit, high sensitivity and wide linear range for simultaneous detection of purine and pyrimidine. The proposed sensor also has good stability and reproducibility. Furthermore, the modified electrode was applied for the detection of DNA bases in a fish sperm DNA sample with satisfactory results.

  9. Determination of 222Rn in water samples from wells and springs in Tokyo by a modified integral counting method

    International Nuclear Information System (INIS)

    Homma, Y.; Murase, Y.; Handa, K.; Murakami, I.

    1997-01-01

    222 Rn in 2L-water samples was extracted with 30 mL toluene, and 21 mL of the toluene solution was transferred into a liquid scintillation vial, in which PPO - 2,5-diphenyloxazole was placed in advance. The total activity of 222 Rn in the water sample was calculated based on the Ostwald's coefficient of solubilities of 222 Rn in toluene and water at the temperature of the sample water and the volume of water and toluene. About 40% of 222 Rn dissolved in 2L-water sample can be collected. After allowing to stand for 3.5 h, the equilibrium mixture of 222 Rn and its daughters was measured with an Aloka liquid scintillation spectrometer using a modified integral counting method which extrapolates the integral counting curve not to the zero pulse-height, but to the zero detection threshold, an average energy required to produce a measurable pulse, of the liquid scintillation spectrometer. The general method which agitates water sample (usually about 10 mL) with a liquid scintillation cocktail is practical when the activity of 222 Rn is high. By adding 10 mL of water sample, however, it is possible also to add variable amounts of quencher. In some cases water sample is preserved with nitric acid. The slope of the integral counting rate curve increases as quench level of the sample increases. Therefore, it is clear that the modified integral counting method gives more accurate 222 Rn concentrations for water samples of strong quench than the conventional integral counting method. 222 Rn sample of 0.2 Bq/L can be determined within an overall uncertainty of 3.1%

  10. Glassy carbon electrodes modified with a film of nanodiamond-graphite/chitosan: Application to the highly sensitive electrochemical determination of Azathioprine

    International Nuclear Information System (INIS)

    Shahrokhian, Saeed; Ghalkhani, Masoumeh

    2010-01-01

    A novel modified glassy carbon electrode with a film of nanodiamond-graphite/chitosan is constructed and used for the sensitive voltammetric determination of azathioprine (Aza). The surface morphology and thickness of the film modifier are characterized using atomic force microscopy. The electrochemical response characteristics of the electrode toward Aza are investigated by means of cyclic voltammetry. The modified electrode showed an efficient catalytic role for the electrochemical reduction of Aza, leading to a remarkable decrease in reduction overpotential and enhancement of the kinetics of the electrode reaction with a significant increase of peak current. The effects of experimental variables, such as the deposited amount of modifier suspension, the pH of the supporting electrolyte, the accumulation potential and time were investigated. Under optimal conditions, the modified electrode showed a wide linear response to the concentration of Aza in the range of 0.2-100 μM with a detection limit of 65 nM. The prepared modified electrode showed several advantages: simple preparation method, high stability and uniformity in the composite film, high sensitivity, excellent catalytic activity in physiological conditions and good reproducibility. The modified electrode can be successfully applied to the accurate determination of trace amounts of Aza in pharmaceutical and clinical preparations.

  11. Glassy carbon electrodes modified with a film of nanodiamond-graphite/chitosan: Application to the highly sensitive electrochemical determination of Azathioprine

    Energy Technology Data Exchange (ETDEWEB)

    Shahrokhian, Saeed, E-mail: shahrokhian@sharif.ed [Department of Chemistry, Sharif University of Technology, Tehran 11155-9516 (Iran, Islamic Republic of); Institute for Nanoscience and Technology, Sharif University of Technology, Tehran (Iran, Islamic Republic of); Ghalkhani, Masoumeh [Department of Chemistry, Sharif University of Technology, Tehran 11155-9516 (Iran, Islamic Republic of)

    2010-04-15

    A novel modified glassy carbon electrode with a film of nanodiamond-graphite/chitosan is constructed and used for the sensitive voltammetric determination of azathioprine (Aza). The surface morphology and thickness of the film modifier are characterized using atomic force microscopy. The electrochemical response characteristics of the electrode toward Aza are investigated by means of cyclic voltammetry. The modified electrode showed an efficient catalytic role for the electrochemical reduction of Aza, leading to a remarkable decrease in reduction overpotential and enhancement of the kinetics of the electrode reaction with a significant increase of peak current. The effects of experimental variables, such as the deposited amount of modifier suspension, the pH of the supporting electrolyte, the accumulation potential and time were investigated. Under optimal conditions, the modified electrode showed a wide linear response to the concentration of Aza in the range of 0.2-100 muM with a detection limit of 65 nM. The prepared modified electrode showed several advantages: simple preparation method, high stability and uniformity in the composite film, high sensitivity, excellent catalytic activity in physiological conditions and good reproducibility. The modified electrode can be successfully applied to the accurate determination of trace amounts of Aza in pharmaceutical and clinical preparations.

  12. MWCNT-cysteamine-Nafion modified gold electrode based on myoglobin for determination of hydrogen peroxide and nitrite.

    Science.gov (United States)

    Canbay, Erhan; Şahin, Berika; Kıran, Müge; Akyilmaz, Erol

    2015-02-01

    In this work, a novel amperometric biosensor of hydrogen peroxide (H2O2) was developed based on the immobilization of myoglobin (Mb) on the surface of the multi-walled carbon nanotube (MWCNT) -Nafion-cysteamine (CA) modified gold electrode (Au) and its electrocatalytic activity was used for the determination of nitrite (NO2(-)). In the optimization studies, the best MWCNT and myoglobin amount were investigated. It was discovered at the experiments for the optimization of the working conditions that the buffer at this study as 50.0mM, pH7.0 phosphate buffer (PBS) and working temperature as 30°C for the H2O2 biosensor. It was determined at the characterization studies on the biosensor that linear results are obtained between the ranges of 0.1μM to 70.0μM for H2O2 concentration and 1-250μM for NO2(-). The reproducibility of the biosensor was determined both H2O2 and nitrite. From the experiments, average value, standard deviation (SD) and coefficients of variation (CV%) were calculated to be 10.02±0.43μM, and 4.29% for 10.0μM H2O2 (n=6) and 52.0±2.1μM, and 3.89% for 50.0μM nitrite (n=8), respectively. At the same time the sample was analyzed for NO2(-) in drinking and mineral waters. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Rapid determination of free fatty acid content in waste deodorizer distillates using single bounce-attenuated total reflectance-FTIR spectroscopy.

    Science.gov (United States)

    Naz, Saba; Sherazi, Sayed Tufail Hussain; Talpur, Farah N; Mahesar, Sarfaraz A; Kara, Huseyin

    2012-01-01

    A simple, rapid, economical, and environmentally friendly analytical method was developed for the quantitative assessment of free fatty acids (FFAs) present in deodorizer distillates and crude oils by single bounce-attenuated total reflectance-FTIR spectroscopy. Partial least squares was applied for the calibration model based on the peak region of the carbonyl group (C=O) from 1726 to 1664 cm(-1) associated with the FFAs. The proposed method totally avoided the use of organic solvents or costly standards and could be applied easily in the oil processing industry. The accuracy of the method was checked by comparison to a conventional standard American Oil Chemists' Society (AOCS) titrimetric procedure, which provided good correlation (R = 0.99980), with an SD of +/- 0.05%. Therefore, the proposed method could be used as an alternate to the AOCS titrimetric method for the quantitative determination of FFAs especially in deodorizer distillates.

  14. Sensitive Adsorptive Voltammetric Method for Determination of Bisphenol A by Gold Nanoparticle/Polyvinylpyrrolidone-Modified Pencil Graphite Electrode

    Directory of Open Access Journals (Sweden)

    Yesim Tugce Yaman

    2016-05-01

    Full Text Available A novel electrochemical sensor gold nanoparticle (AuNP/polyvinylpyrrolidone (PVP modified pencil graphite electrode (PGE was developed for the ultrasensitive determination of Bisphenol A (BPA. The gold nanoparticles were electrodeposited by constant potential electrolysis and PVP was attached by passive adsorption onto the electrode surface. The electrode surfaces were characterized by electrochemical impedance spectroscopy (EIS and scanning electron microscopy (SEM. The parameters that affected the experimental conditions were researched and optimized. The AuNP/PVP/PGE sensor provided high sensitivity and selectivity for BPA recognition by using square wave adsorptive stripping voltammetry (SWAdSV. Under optimized conditions, the detection limit was found to be 1.0 nM. This new sensor system offered the advantages of simple fabrication which aided the expeditious replication, low cost, fast response, high sensitivity and low background current for BPA. This new sensor system was successfully tested for the detection of the amount of BPA in bottled drinking water with high reliability.

  15. Magnetic nanoparticles modified with polyfuran for the extraction of polycyclic aromatic hydrocarbons prior to their determination by gas chromatography

    International Nuclear Information System (INIS)

    Amiri, Amirhassan; Baghayeri, Mehdi; Kashmari, Milad

    2016-01-01

    We describe magnetite nanoparticles modified with polyfuran (PFu/Fe 3 O 4 ) and their use as adsorbents for the solid-phase extraction of the polycyclic aromatic hydrocarbons (PAHs) naphthalene, fluorene and anthracene from water and urine samples. The PFu/Fe 3 O 4 nanocomposite was characterized by Fourier transform infrared spectroscopy, scanning electron microscopy and vibrating sample magnetometry (VSM). The adsorbent was magnetically separated from the sample, extracted with dichloromethane, and the extracts were submitted to gas chromatographic analysis with flame ionization detection. The amount of adsorbent, adsorption and desorption time, salt addition and desorption solvent were optimized. The method displays detection limits (at an S/N ratio of 3) in the range from 5 to 20 pg mL −1 , and the limits of quantification (at an S/N ratio of 10) are between 20 and 50 pg mL −1 . Relative standard deviations (RSDs) for intra- and inter-day precision are 4.1–5.6, and 5.3–6.5 %, respectively. The feasibility of the method was demonstrated by extracting and determining PAHs in (spiked) real water and urine samples. (author)

  16. The use of phospholipid modified column for the determination of lipophilic properties in high performance liquid chromatography.

    Science.gov (United States)

    Godard, Tal; Grushka, Eli

    2011-03-04

    A new chromatographic stationary phase obtained by coating a reversed phase amide column with phosphatidylcholine based liposomes solution to yield a phospholipid modified column (PLM). The modification is achieved by the dynamic coating method which recycles the coating solution through the column in a closed loop for a period of 24 h. The chromatographic properties of the new column have changed significantly as compared to the original amide column due to the phospholipid coating. A good correlation was observed between n-octanol/water logP values and the logarithm of the retention factor obtained on the PLM column for a large number of solutes. In addition the PLM column was characterized using the linear solvation energy relationship (LSER). The values of the LSER system constants for the PLM column were calculated and were found to be very close to those of the n-octanol/water extraction system thus suggesting that the PLM column can be used for the estimation of n-octanol/water partition coefficient and serve as a possible alternative to the shake-flask method for lipophilicity determination. In addition, the results suggest that the PLM column can provide an alternative to other phospholipid-based column such as the IAM and the DPC columns. Copyright © 2011 Elsevier B.V. All rights reserved.

  17. A modified two-point titration method for the determination of volatile fatty acids in anaerobic systems.

    Science.gov (United States)

    Mu, Zhe-Xuan; He, Chuan-Shu; Jiang, Jian-Kai; Zhang, Jie; Yang, Hou-Yun; Mu, Yang

    2018-04-10

    The volatile fatty acids (VFA) concentration plays important roles in the rapid start-up and stable operation of anaerobic reactors. It's essential to develop a simple and accurate method to monitor the VFA concentration in the anaerobic systems. In present work, a modified two-point titration method was developed to determine the VFA concentration. The results show that VFA concentration in standard solutions estimated by the titration method coincided well with that measured by gas chromatograph, where all relative errors were lower than 5.5%. Compared with the phosphate, ammonium and sulfide subsystems, the effect of bicarbonate on the accuracy of the developed method was relatively significant. When the bicarbonate concentration varied from 0 to 8 mmol/L, the relative errors increased from 1.2% to 30% for VFA concentration at 1 mmol/L, but were within 2.0% for that at 5 mmol/L. In addition, the VFA composition affected the accuracy of the titration method to some extent. This developed titration method was further proved to be effective with practical effluents from a lab-scale anaerobic reactor under organic shock loadings and an unstable full-scale anaerobic reactor. Copyright © 2018 Elsevier Ltd. All rights reserved.

  18. An Easily Fabricated Electrochemical Sensor Based on a Graphene-Modified Glassy Carbon Electrode for Determination of Octopamine and Tyramine

    Science.gov (United States)

    Zhang, Yang; Zhang, Meiqin; Wei, Qianhui; Gao, Yongjie; Guo, Lijuan; Al-Ghanim, Khalid A.; Mahboob, Shahid; Zhang, Xueji

    2016-01-01

    A simple electrochemical sensor has been developed for highly sensitive detection of octopamine and tyramine by electrodepositing reduced graphene oxide (ERGO) nanosheets onto the surface of a glassy carbon electrode (GCE). The electrocatalytic oxidation of octopamine and tyramine is individually investigated at the surface of the ERGO modified glassy carbon electrode (ERGO/GCE) by using cyclic voltammetry (CV) and differential pulse voltammetry (DPV). Several essential factors including the deposition cycle of reduced graphene oxide nanosheets and the pH of the running buffer were investigated in order to determine the optimum conditions. Furthermore, the sensor was applied to the quantification of octopamine and tyramine by DPV in the concentration ranges from 0.5 to 40 μM and 0.1 to 25 μM, respectively. In addition, the limits of detection of octopamine and tyramine were calculated to be 0.1 μM and 0.03 μM (S/N = 3), respectively. The sensor showed good reproducibility, selectivity and stability. Finally, the sensor successfully detected octopamine and tyramine in commercially available beer with satisfactory recovery ranges which were 98.5%–104.7% and 102.2%–103.1%, respectively. These results indicate the ERGO/GCE based sensor is suitable for the detection of octopamine and tyramine. PMID:27089341

  19. Determination of Rhodium(III Ions by Flame Atomic Absorption Spectrometry after Preconcentration with Modified Magnetic Activated Carbon

    Directory of Open Access Journals (Sweden)

    Maryam Fayazi

    2016-06-01

    Full Text Available A new method for analysis of trace amount of Rh(III ions by magnetic activated carbon modified with 2,3,5,6-tetra(2-pyridylpyrazine (MAC/TPPZ as the magnetic sorbent has been proposed. The proposed adsorbent was found to be advantageous over conventional solid phase extraction (SPE in terms of operational simplicity and low time-consuming. The experimental parameters affecting the extraction/preconcentration and determination of the analyte were systematically examined. In order to investigate the selectivity of this magnetic sorbent, the effect of a variety of ions on preconcentration and recovery of Rh(III ions were also investigated. Under optimum conditions, the calibration graph was linear for the concentration range of 0.8-650 µg l-1. The limit of detection (LOD, 3Sb/m and the relative standard deviation (RSD, n = 8, c = 50 µg l-1 were 0.1 µg l-1 and 3.6%, respectively. The maximum sorption capacity of the adsorbent for rhodium was found to be 21.6 mg g-1. The presented procedure was applied to monitoring rhodium in water and synthetic samples.

  20. The use of tristimulus colorimetry for the determination of hydrogen cyanide in air by a modified König method

    Directory of Open Access Journals (Sweden)

    VLADIMÍR PITSCHMANN

    2010-06-01

    Full Text Available A simple visual and tristimulus colorimetric method (three-dimensional system CIE-L*a*b* for the determination of trace amounts of hydrogen cyanide in air has been developed. The method is based on the suction of hydrogen cyanide through a chlorinating cartridge where cyanogen chloride is formed, which is further driven to an indicator disc made of a modified cotton fabric. This indicator disc is placed into an adapter. Prior to analysis, the disc is saturated with a chromogenic reagent, a solution of 5,5-dimethyl-1,3-cyclohexanedione (dimedone and 4-benzylpyridine in ethanol. In the presence of hydrogen cyanide (cyanogen chloride, a pink coloration emerges on the indicator disc, the intensity of which is evaluated either visually or by use of a tristimulus colorimeter. The detection limit is 0.1 mg m-3. The method is mainly suitable for mobile field analyses. It was applied for the CHP-5 chemical agent detector introduced into the equipment of the Czech Army corps.

  1. Amperometric immunosensor based on multiwalled carbon nanotubes/Prussian blue/nanogold-modified electrode for determination of α-fetoprotein.

    Science.gov (United States)

    Jiang, Wen; Yuan, Ruo; Chai, Ya-Qin; Yin, Bing

    2010-12-01

    In this article, a conspicuously simple and highly sensitive amperometric immunosensor based on the sequential electrodeposition of Prussian blue (PB) and gold nanoparticles (GNPs) on multiwalled carbon nanotube (MWCNT)-modified glassy carbon electrode (GCE) surface is proposed for the detection of α-fetoprotein (AFP). By comparison with PB, the MWCNT/PB composite film had been proven to show much better electrochemical stability and a larger response current. The electrodeposited GNP film can be used not only to immobilize biomolecules but also to avoid the leakage of PB and to prevent shedding of MWCNT/PB composite film from the electrode surface. The performance and factors influencing the performance of the immunosensor were investigated. Under optimal experimental conditions, the proposed immunosensor for AFP was observed with an ultralow limit of detection (LOD) equal to 3 pg/ml (at 3δ), and the linear working range spanned the concentrations of AFP from 0.01 to 300 ng/ml. Moreover, the immunosensor, as well as a commercially available kit, was examined for use in the determination of AFP in real human serum specimens. More significant, the assay mentioned here is simpler than the traditional enzyme-linked immunosorbent assay (ELISA), and an excellent correlation of levels of AFP measured was obtained, indicating that the developed immunoassay could be a promising alternative approach for detection of AFP and other tumor markers in the clinical diagnosis. Copyright © 2010 Elsevier Inc. All rights reserved.

  2. H-M bearing capacity of a modified suction caisson determined by using load-/displacement-controlled methods

    Science.gov (United States)

    Zhang, Yu-kun; Gao, Yu-feng; Li, Da-yong; Mahfouz, Ali H.

    2016-12-01

    This paper presents a series of monotonically combined lateral loading tests to investigate the bearing capacity of the MSCs (modified suction caissons) in the saturated marine fine sand. The lateral loads were applied under load- and displacement-controlled methods at the loading eccentricity ratios of 1.5, 2.0 and 2.5. Results show that, in the displacement-controlled test, the deflection-softening behavior of load-deflection curves for MSCs was observed, and the softening degree of the load-deflection response increased with the increasing external skirt length or the decreasing loading eccentricity. It was also found that the rotation center of the MSC at failure determined by the load-controlled method is slightly lower than that by the displacement-controlled method. The calculated MSC capacity based on the rotation center position in serviceability limit state is relatively conservative, compared with the calculated capacity based on the rotation center position in the ultimate limit state. In the limit state, the passive earth pressures opposite the loading direction under load- and displacement-controlled methods decrease by 46% and 74% corresponding to peak values, respectively; however, the passive earth pressures in the loading direction at failure only decrease by approximately 3% and 7%, compared with their peak values.

  3. Simultaneous electrochemical determination of dopamine and paracetamol on multiwalled carbon nanotubes/graphene oxide nanocomposite-modified glassy carbon electrode.

    Science.gov (United States)

    Cheemalapati, Srikanth; Palanisamy, Selvakumar; Mani, Veerappan; Chen, Shen-Ming

    2013-12-15

    In the present study, multiwalled carbon nanotubes (MWCNT)/graphene oxide (GO) nanocomposite was prepared by homogenous dispersion of MWCNT and GO and used for the simultaneous voltammetric determination of dopamine (DA) and paracetamol (PA). The TEM results confirmed that MWCNT walls were wrapped well with GO sheets. The MWCNT/GO nanocomposite showed superior electrocatalytic activity towards the oxidation of DA and PA, when compared with either pristine MWCNT or GO. The major reason for the efficient simultaneous detection of DA and PA at nanocomposite was the synergistic effect between MWCNT and GO. The electrochemical oxidation of DA and PA was investigated by cyclic voltammetry, differential pulse voltammetry and amperometry. The nanocomposite modified electrode showed electrocatalytic oxidation of DA and PA in the linear response range from 0.2 to 400 µmol L(-1) and 0.5 to 400 µmol L(-1) with the detection limit of 22 nmol L(-1) and 47 nmol L(-1) respectively. The proposed sensor displayed good selectivity, sensitivity, stability with appreciable consistency and precision. © 2013 Elsevier B.V. All rights reserved.

  4. Prevalence and Modifiable Determinants of Non-Adherence in Adult Kidney Transplant Recipients in a German Sample.

    Science.gov (United States)

    Reber, Sandra; Morawa, Eva; Stößel, Lisa; Jank, Sabine; Vitinius, Frank; Eckardt, Kai-Uwe; Erim, Yesim

    2016-09-01

    The aim of this cross-sectional study was to investigate the prevalence and the modifiable determinants of non-adherence in adult kidney transplant patients in follow-up care. In 74 patients at least six months post-transplant, self-reported adherence (Basel Assessment of Adherence to ImmunosuppressiveMedications Scale, BAASIS©), subjective experience and attitudes after transplantation (Medication Experience Scale for Immunosuppressants, MESI), and depression and anxiety (Hospital Anxiety and Depression Scale,HADSD) were assessed. Non-adherence to any of the four BAASIS© items was 24.3%. For the sub-dimensions: dose taking, drug holidays, timing deviation more than two hours from prescribed time, and dose reduction, the non-adherence levelswere 9.5%, 0%,17.6% and 2.7%, respectively. Marital status, negative beliefs towards immunosuppressants, and prominent anxiety and depression were associated with non-adherence. Screening for adherence and its indicators is of substantial importance in communication with renal transplant recipients. After detecting non-adherence, supportive interventions can be offered to the patients.

  5. Electroanalytical Determination of Gemifloxacin Mesylate in Bulk, Tablets and Human Urine Using Gold Nanoparticles Modified Carbon Paste Electrode

    Directory of Open Access Journals (Sweden)

    Ali Attia

    2014-12-01

    Full Text Available A simple, precise, inexpensive and sensitive voltammetric method has been developed for the determination of gemifloxacin mesylate (GEM in the presence of tween 80 in the bulk, farmaceutical dosage forms and human urine at gold nanoparticles modified carbon paste electrode (GNCPE. The electrochemical behavior of GEM has been investigated by using cyclic voltammetry (CV and differential pulse voltammetry (DPV techniques. The electrochemical oxidation of GEM was an irreversible process which exhibited adsorption-diffusion controlled process behavior in Britton-Robinson (BR buffer over the entire pH range of values from 2 to 9. The adsorptive stripping response was evaluated as a function of some variables such as pH, type of surfactant, scan rate and accumulation time. The anodic peak current varied linearly over the range from 8.0 × 10-7 to 2.8 × 10-5 M. The limits of detection and quantification were 7.32 × 10-8 M and 2.44 × 10-7 M, respectively. The relative standard deviations and the percentage recoveries were found in the following ranges: 0.58-1.35% and 99.37-101.76%, respectively.

  6. Correlation of experimental rCBF determinations in goats with flow measurements from a Doppler-modified carotid artery shunt

    International Nuclear Information System (INIS)

    Loftus, C.M.; Silvidi, J.A.; Becker, J.A.; Miller, B.V.; Bernstein, D.D.

    1989-01-01

    A carotid artery shunt system has been developed that continuously monitors blood flow rates by embedding a Doppler crystal in the shunt wall. The crystal ranges through a liquid lens that enables it to be placed without violation of the shunt lumen. Because the crystal is at a fixed angle (45 degrees) to the axis of blood flow and the diameter of the lumen remains constant, a linear relationship exists between flow rates and the Doppler velocity signal. This shunt system was previously tested in vitro using a pulsatile pump and was found to be accurate to within 4.7% of the actual flow rate. In the present study, animal (goat) experiments were performed consisting of simultaneous carotid shunt flow and bilateral rCBF measurements by the radiolabeled microsphere technique to determine in vivo the accuracy of this Doppler modified shunt and to ascertain the ability of shunt flow to increase in the face of acute contralateral carotid occlusion. Data from five animals show that in vivo shunt flow can be recorded to within 13% of control rCBF and that shunt flow increases nearly 50% under conditions of distal demand (contralateral carotid occlusion). This device may prove useful in laboratory studies of carotid shunt dynamics and in clinical practice to quickly detect correctable shunt flow abnormalities

  7. Evaluation and determination of soil remediation schemes using a modified AHP model and its application in a contaminated coking plant.

    Science.gov (United States)

    Li, Xingang; Li, Jia; Sui, Hong; He, Lin; Cao, Xingtao; Li, Yonghong

    2018-07-05

    Soil remediation has been considered as one of the most difficult pollution treatment tasks due to its high complexity in contaminants, geological conditions, usage, urgency, etc. The diversity in remediation technologies further makes quick selection of suitable remediation schemes much tougher even the site investigation has been done. Herein, a sustainable decision support hierarchical model has been developed to select, evaluate and determine preferred soil remediation schemes comprehensively based on modified analytic hierarchy process (MAHP). This MAHP method combines competence model and the Grubbs criteria with the conventional AHP. It not only considers the competence differences among experts in group decision, but also adjusts the big deviation caused by different experts' preference through sample analysis. This conversion allows the final remediation decision more reasonable. In this model, different evaluation criteria, including economic effect, environmental effect and technological effect, are employed to evaluate the integrated performance of remediation schemes followed by a strict computation using above MAHP. To confirm the feasibility of this developed model, it has been tested by a benzene workshop contaminated site in Beijing coking plant. Beyond soil remediation, this MAHP model would also be applied in other fields referring to multi-criteria group decision making. Copyright © 2018 Elsevier B.V. All rights reserved.

  8. Electrochemical Sensor Based on Rh(III) Ion-Imprinted Polymer as a New Modifying Agent for Rhodium Determination.

    Science.gov (United States)

    Bai, Huiping; Xiong, Caiyun; Wang, Chunqiong; Liu, Peng; Dong, Su; Cao, Qiue

    2018-05-01

    A rhodium (III) ion carbon paste electrode (CPE) based on an ion imprinted polymer (IIP) as a new modifying agent has been prepared and studied. Rh(III) ion imprinted polymer was synthesized by copolymerization of acrylamide-Rh(III) complex and ethylene glycol dimethacrylate according to the precipitation polymerization. Acrylamide acted as both functional monomer and complexing agent to create selective coordination sites in a cross-linked polymer. The ion imprinted carbon paste electrode (IIP-CPE) was prepared by mixing rhodium IIP-nanoparticles and graphite powder in n-eicosane as an adhesive and then embedding them in a Teflon tube. Amperometric i-t curve method was applied as the determination technique. Several parameters, including the functional monomer, molar ratio of template, monomer and cross-linking agent, the amounts of IIP, the applied potential, the buffer solution and pH have been studied. According to the results, IIP-CPE showed a considerably higher response in comparison with the electrode embedded with non-imprinted polymer (NIP), indicating the formation of suitable recognition sites in the IIP structure during the polymerization stage. The introduced electrode showed a linear range of 1.00×10-8~3.0×10-5 mol·L-1 and detection limit of 6.0 nmol L-1 (S/N = 3). The IIP-CPE was successfully applied for the trace rhodium determination in catalyst and plant samples with RSD of less than 3.3% (n = 5) and recoveries in the range of 95.5~102.5%.

  9. Highly selective direct determination of chlorate ions by using a newly developed potentiometric electrode based on modified smectite.

    Science.gov (United States)

    Topcu, Cihan

    2016-12-01

    A novel polyvinyl chloride membrane chlorate (ClO 3 - ) selective electrode based on modified smectite was developed for the direct determination of chlorate ions and the potentiometric performance characteristics of its were examined. The best selectivity and sensitivity for chlorate ions were obtained for the electrode membrane containing ionophore/polyvinylchloride/o-nitrophenyloctylether in composition of 12/28/60 (w/w%). The proposed electrode showed a Nernstian response toward chlorate ions at pH=7 in the concentration range of 1×10 -7 -1×10 -1 M and the limit of detection was calculated as 9×10 -8 M from the constructed response plot. The linear slope of the electrode was -61±1mVdecade -1 for chlorate activity in the mentioned linear working range. The selectivity coefficients were calculated according to both the matched potential method and the separate solution method. The calculated selectivity coefficients showed that the electrode performed excellent selectivity for chlorate ions. The potentiometric response of electrode toward chlorate ions was found to be highly reproducible. The electrode potential was stable between pH=4-10 and it had a dynamic response time of <5s. The potentiometric behavior of the electrode in partial non-aqueous medium was also investigated and the obtained results (up to 5% (v/v) alcohol) were satisfactory. The proposed electrode was used during 15 weeks without any significant change in its potential response. Additionally, the electrode was very useful in water analysis studies such as dam water, river water, tap water, and swimming pool water where the direct determination of chlorate ions was required. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Highly sensitive and selective determination of methylergometrine maleate using carbon nanofibers/silver nanoparticles composite modified carbon paste electrode

    International Nuclear Information System (INIS)

    Kalambate, Pramod K.; Rawool, Chaitali R.; Karna, Shashi P.; Srivastava, Ashwini K.

    2016-01-01

    A highly sensitive and selective voltammetric method for determination of Methylergometrine maleate (MM) in pharmaceutical formulations, urine and blood serum samples has been developed based on enhanced electrochemical response of MM at carbon nanofibers and silver nanoparticles modified carbon paste electrode (CNF-AgNP-CPE). The electrode material was characterized by various techniques viz., X-ray diffraction, scanning electron microscopy and energy dispersive X-ray spectroscopy. The electrocatalytic response of MM at CNF-AgNP-CPE was studied by cyclic voltammetry (CV), differential pulse voltammetry (DPV) and electrochemical impedance spectroscopy (EIS). Under optimized conditions, the proposed sensor exhibits excellent electrochemical response towards MM. The DPV study shows greatly enhanced electrochemical signal for MM at CNF-AgNP-CPE lending high sensitivity to the proposed sensor for MM detection. The peak (I p ) current for MM is found to be rectilinear in the range 4.0 × 10 −8 –2.0 × 10 −5 M with a detection limit of 7.1 × 10 −9 M using DPV. The feasibility of the proposed sensor in analytical applications was investigated by conducting experiments on commercial pharmaceutical formulations, human urine and blood serum samples, which yielded satisfactory recoveries of MM. The proposed electrochemical sensor offers high sensitivity, selectivity, reproducibility and practical utility. We recommend it as an authentic and productive electrochemical sensor for successful determination of MM. - Highlights: • Voltammetric sensor for methylergometrine maleate using carbon nanofibers and silver nanoparticle - carbon paste electrode • Wide working range, good reproducibility, fast response and high stability were the main advantages of the proposed sensor • Analysis of methylergometrine maleate in pharmaceutical formulations, urine and blood serum samples • Lowest limit of detection obtained for methylergometrine maleate

  11. A comparison of methods to determine tannin acyl hydrolase activity

    Directory of Open Access Journals (Sweden)

    Cristóbal Aguilar

    1999-01-01

    Full Text Available Six methods to determine the activity of tannase produced by Aspergillus niger Aa-20 on polyurethane foam by solid state fermentation, which included two titrimetric techniques, three spectrophotometric methods and one HPLC assay were tested and compared. All methods assayed enabled the measurement of extracellular tannase activity. However, only five were useful to evaluate intracellular tannase activity. Studies on the effect of pH on tannase extraction demonstrated that tannase activity was considerably under-estimated when its extraction was carried out at pH values below 5.5 and above 6.0. Results showed that the HPLC technique and the modified Bajpai and Patil methods presented several advantages in comparison to the other methods tested.Seis métodos para determinar a atividade de tannase produzida por Aspergillus niger O Aa-20 em espuma de polyuretano por fermentação em estado sólido foram estudados. Duas técnicas titulométricas , três métodos spectrofotométricos e um método por HPLC foram testados e comparados. Todos os métodos testados permitiram determinar a atividade da tannase produzida extracelularmente. Entretanto, somente cinco se mostraram úteis para avaliar a atividade da tannase produzida intracelularmente. Os estudos do efeito do pH na extração de tannase demonstraram que a atividade de tannase era consideravelmente subestimada quando sua extração foi executada em valores de pH inferiores a 5.5 e superior a pH 6.0. Os resultados demostraram que a técnica de HPLC o método Bajpai and Patil modificado apresentam várias vantagens em comparação aos outros métodos testados.

  12. Square wave voltammetry at carbon paste electrode modified with surfactant for alpha tocopheryl acetate determination in cosmetics

    Directory of Open Access Journals (Sweden)

    Simona Žabčíková

    2018-03-01

    Full Text Available Normal 0 false false false CS X-NONE X-NONE The aim of this study was describe electrochemical properties of a carbon paste electrode (CPE bulk modified with 30% (w/w surfactant sodium dodecyl sulphate (CPE/SDS and demonstrates its application in the determination of α‑tocopheryl acetate (α‑TAc, known as vitamin E acetate, in selected cosmetic products, especially body creams. In addition to anionic SDS, cationic hexadecylpyridinium chloride monohydrate (CPC was also tested as possible modifier. It was found that selection of surfactant type and its content significantly affect an electrical conductivity and mechanical stability of these heterogeneous electroanalytical sensors in pure organic solvents. Under this study, it was found that CPC is a totally inappropriate mediator due to very high backgroundcurrent. Together with other lipophilic vitamins characterized by antioxidant activity (dominantly retionoids, this completely synthetic substance is widely used as significant cosmetic additive due its preservative properties. Monitoring of its content in cosmetic products is usually performed by high‑performance liquid chromatography (HPLC with UV detection. This standard analytical protocol is always burdened with the complex and time‑consuming preparation of the sample before analysis. For that reason, robust and simple electroanalytical method based on anodic oxidation of the α‑TAc at CPE/SDS by square wave voltammetry (SWV performed in pure organic electrolyte (99.8% acetonitrile containing 0.1 mol·L‑1 LiClO4 was developed. Moreover, simple dissolution of sample in supporting electrolyte using ultrasonic bath and subsequent filtering through a stacked filter included all the necessary procedures for sample preparation. The linear range from 0.1 to 1.2 mmol·L‑1and limit of detection 37 µmol·L‑1 were found at pulse amplitude 10 mV and frequency 10 Hz as optimum. In analysis of selected cosmetics, the developed

  13. Electrochemically pretreated zeolite-modified carbon-paste electrodes for determination of linuron in an agricultural formulation and water

    International Nuclear Information System (INIS)

    Siara, L.R.; Lima, F. de; Cardoso, C.A.L.; Arruda, G.J.

    2015-01-01

    Highlights: • Cyclic voltammetry, square-wave voltammetry, electrochemical impedance spectroscopic, and scanning electron microscopy were employed. • Kinetic parameters (n, α, k s , and Γ) were calculated. • High sensitivity was observed in the linear concentration range. • Excellent recovery rates were achieved for tap water samples. • The method proved applicable to the determination of linuron in the presence of potential organic and inorganic interferents, none of which affected the results. - Abstract: A simple and inexpensive, yet highly sensitive electrochemical method for quantifying linuron in tap and distilled water and in agricultural formulations was developed using electrochemically pretreated zeolite-modified carbon-paste electrodes (ZMCPEs). Compared with untreated ZMCPEs, the electrochemically pretreated electrodes showed significantly enhanced peak currents for linuron oxidation. Scanning electron microscopy and energy-dispersive x-ray spectroscopy were used to examine the structure of the zeolite-modified and unmodified carbon-paste electrodes (CPEs). ZMCPEs were electrochemically characterized using cyclic voltammetry, chronocoulometry, square-wave voltammetry, and electrochemical impedance spectroscopy. A mechanism for linuron oxidation on ZMCPE surfaces was proposed. The electrochemical variables taken into account were electrode area, number of transferred electrons, electron transfer coefficient, electrode reaction standard rate constant, surface coverage, and capacitance of the electric double layer. Zeolite was found to have a strong influence on these variables. The electrochemical procedure applied to linuron was developed using electrochemically pretreated ZMCPEs under optimal conditions. Linuron oxidation currents exhibited linear concentration in the 87.36 to 625.72 nmol L −1 range, with a limit of detection of 22.57 nmol L −1 . The proposed electrochemical method was employed to quantify linuron in tap and distilled

  14. Differential pulse voltammetric determination of methyl parathion based on multiwalled carbon nanotubes-poly(acrylamide) nanocomposite film modified electrode

    Energy Technology Data Exchange (ETDEWEB)

    Zeng, Yanbo [Department of Chemistry and Shanghai Key Laboratory of Green Chemistry and Chemical Process, East China Normal University, 3663 Zhongshan Road(N), Shanghai, 200062 (China); College of Biological, Chemical Sciences and Engineering, Jiaxing University, Jiaxing 314001 (China); Yu, Dajun; Yu, Yanyan [Department of Chemistry and Shanghai Key Laboratory of Green Chemistry and Chemical Process, East China Normal University, 3663 Zhongshan Road(N), Shanghai, 200062 (China); Zhou, Tianshu [Department of Environmental Science, East China Normal University, 3663 Zhongshan Road(N), Shanghai, 200062 (China); Shi, Guoyue, E-mail: gyshi@chem.ecnu.edu.cn [Department of Chemistry and Shanghai Key Laboratory of Green Chemistry and Chemical Process, East China Normal University, 3663 Zhongshan Road(N), Shanghai, 200062 (China)

    2012-05-30

    Highlights: Black-Right-Pointing-Pointer A sensitive electrochemical sensor for detecting methyl parathion in environmental samples. Black-Right-Pointing-Pointer The preparation, characterization and application of this novel MWCNTs-PAAM nanocomposite. Black-Right-Pointing-Pointer The MWCNTs-PAAM/GCE exhibited a high adsorption and strong affinity toward methyl parathion. Black-Right-Pointing-Pointer Wide linear range and low detection limit of the proposed method for detecting methyl parathion. - Abstract: A sensitive electrochemical differential pulse voltammetry method was developed for detecting methyl parathion based on multiwalled carbon nanotubes-poly(acrylamide) (MWCNTs-PAAM) nanocomposite film modified glassy carbon electrode. The novel MWCNTs-PAAM nanocomposite, containing high content of amide groups, was synthesized by PAAM polymerizing at the vinyl group functionalized MWCNTs surface using free radical polymerization. The MWCNTs-PAAM nanocomposite was characterized by Fourier transform infrared spectroscopy, thermal gravimetric analysis and scanning electron microscopy. Electrochemical behavior and interference studies of MWCNTs-PAAM/GCE for methyl parathion were investigated. The experimental results demonstrated that the MWCNTs-PAAM/GCE exhibited a high adsorption and strong affinity toward methyl parathion compared with some metal ions and nitroaromatic compounds, which exist in environmental samples. The adsorbed amount of methyl parathion on the MWCNTs-PAAM/GCE approached the equilibrium value upon 5 min adsorption time. A linear calibration curve for methyl parathion was obtained in the concentration range from 5.0 Multiplication-Sign 10{sup -9} to 1.0 Multiplication-Sign 10{sup -5} mol L{sup -1}, with a detection limit of 2.0 Multiplication-Sign 10{sup -9} mol L{sup -1}. The MWCNTs-PAAM/GCE was proved to be a suitable sensing tool for the fast, sensitive and selective determination of methyl parathion in environmental water samples.

  15. Validation of three new methods for determination of metal emissions using a modified Environmental Protection Agency Method 301

    Energy Technology Data Exchange (ETDEWEB)

    Catherine A. Yanca; Douglas C. Barth; Krag A. Petterson; Michael P. Nakanishi; John A. Cooper; Bruce E. Johnsen; Richard H. Lambert; Daniel G. Bivins [Cooper Environmental Services, LLC, Portland, OR (United States)

    2006-12-15

    Three new methods applicable to the determination of hazardous metal concentrations in stationary source emissions were developed and evaluated for use in U.S. Environmental Protection Agency (EPA) compliance applications. Two of the three independent methods, a continuous emissions monitor-based method (Xact) and an X-ray-based filter method (XFM), are used to measure metal emissions. The third method involves a quantitative aerosol generator (QAG), which produces a reference aerosol used to evaluate the measurement methods. A modification of EPA Method 301 was used to validate the three methods for As, Cd, Cr, Pb, and Hg, representing three hazardous waste combustor Maximum Achievable Control Technology (MACT) metal categories (low volatile, semivolatile, and volatile). The measurement methods were evaluated at a hazardous waste combustor (HWC) by comparing measured with reference aerosol concentrations. The QAG, Xact, and XFM met the modified Method 301 validation criteria. All three of the methods demonstrated precisions and accuracies on the order of 5%. The measurement methods should be applicable to emissions from a wide range of sources, and the reference aerosol generator should be applicable to additional analytes. EPA recently approved an alternative monitoring petition for an HWC at Eli Lilly's Tippecanoe site in Lafayette, IN, in which the Xact is used for demonstrating compliance with the HWC MACT metal emissions (low volatile, semivolatile, and volatile). The QAG reference aerosol generator was approved as a method for providing a quantitative reference aerosol, which is required for certification and continuing quality assurance of the Xact. 30 refs., 5 figs., 11 tabs.

  16. Highly sensitive electrochemical determination of 1-naphthol based on high-index facet SnO2 modified electrode

    International Nuclear Information System (INIS)

    Huang Xiaofeng; Zhao Guohua; Liu Meichuan; Li Fengting; Qiao Junlian; Zhao Sichen

    2012-01-01

    Highlights: ► It is the first time to employ high-index faceted SnO 2 in electrochemical analysis. ► High-index faceted SnO 2 has excellent electrochemical activity toward 1-naphthol. ► Highly sensitive determination of 1-naphthol is realized on high-index faceted SnO 2 . ► The detection limit of 1-naphthol is as low as 5 nM on high-index faceted SnO 2 . ► Electro-oxidation kinetics for 1-napthol on the novel electrode is discussed. - Abstract: SnO 2 nanooctahedron with {2 2 1} high-index facet (HIF) was synthesized by a simple hydrothermal method, and was firstly employed to sensitive electrochemical sensing of a typical organic pollutant, 1-naphthol (1-NAP). The constructed HIF SnO 2 modified glassy carbon electrode (HIF SnO 2 /GCE) possessed advantages of large effective electrode area, high electron transfer rate, and low charge transfer resistance. These improved electrochemical properties allowed the high electrocatalytic performance, high effective active sites and high adsorption capacity of 1-NAP on HIF SnO 2 /GCE. Cyclic voltammetry (CV) results showed that the electrochemical oxidation of 1-NAP obeyed a two-electron transfer process and the electrode reaction was under diffusion control on HIF SnO 2 /GCE. By adopting differential pulse voltammetry (DPV), electrochemical detection of 1-NAP was conducted on HIF SnO 2 /GCE with a limit of detection as low as 5 nM, which was relatively low compared to the literatures. The electrode also illustrated good stability in comparison with those reported value. Satisfactory results were obtained with average recoveries in the range of 99.7–103.6% in the real water sample detection. A promising device for the electrochemical detection of 1-NAP with high sensitivity has therefore been provided.

  17. Differential pulse voltammetric determination of methyl parathion based on multiwalled carbon nanotubes–poly(acrylamide) nanocomposite film modified electrode

    International Nuclear Information System (INIS)

    Zeng, Yanbo; Yu, Dajun; Yu, Yanyan; Zhou, Tianshu; Shi, Guoyue

    2012-01-01

    Highlights: ► A sensitive electrochemical sensor for detecting methyl parathion in environmental samples. ► The preparation, characterization and application of this novel MWCNTs–PAAM nanocomposite. ► The MWCNTs–PAAM/GCE exhibited a high adsorption and strong affinity toward methyl parathion. ► Wide linear range and low detection limit of the proposed method for detecting methyl parathion. - Abstract: A sensitive electrochemical differential pulse voltammetry method was developed for detecting methyl parathion based on multiwalled carbon nanotubes–poly(acrylamide) (MWCNTs–PAAM) nanocomposite film modified glassy carbon electrode. The novel MWCNTs–PAAM nanocomposite, containing high content of amide groups, was synthesized by PAAM polymerizing at the vinyl group functionalized MWCNTs surface using free radical polymerization. The MWCNTs–PAAM nanocomposite was characterized by Fourier transform infrared spectroscopy, thermal gravimetric analysis and scanning electron microscopy. Electrochemical behavior and interference studies of MWCNTs–PAAM/GCE for methyl parathion were investigated. The experimental results demonstrated that the MWCNTs–PAAM/GCE exhibited a high adsorption and strong affinity toward methyl parathion compared with some metal ions and nitroaromatic compounds, which exist in environmental samples. The adsorbed amount of methyl parathion on the MWCNTs–PAAM/GCE approached the equilibrium value upon 5 min adsorption time. A linear calibration curve for methyl parathion was obtained in the concentration range from 5.0 × 10 −9 to 1.0 × 10 −5 mol L −1 , with a detection limit of 2.0 × 10 −9 mol L −1 . The MWCNTs–PAAM/GCE was proved to be a suitable sensing tool for the fast, sensitive and selective determination of methyl parathion in environmental water samples.

  18. Electrochemical behaviors and simultaneous determination of guanine and adenine based on graphene–ionic liquid–chitosan composite film modified glassy carbon electrode

    International Nuclear Information System (INIS)

    Niu Xiuli; Yang Wu; Ren Jie; Guo Hao; Long Shijia; Chen Jiaojiao; Gao Jinzhang

    2012-01-01

    Highlights: ► This work developed a novel electrochemical biosensors for guanine and adenine detection simultaneously. ► A disposable electrode based on graphene sheets, ionic liquid and chitosan was proposed. ► The presented method was also applied to simultaneous determination of guanine and adenine in denatured DNA samples with satisfying results. ► Easy fabrication, high sensitivity, excellent reproducibility and long-term stability. - Abstract: A graphene sheets (GS), ionic liquid (IL) and chitosan (CS) modified electrode was fabricated and the modified electrode displayed excellent electrochemical catalytic activities toward guanine and adenine. The transfer electron number (n) and the charge transfer coefficient (α) were calculated with the result as n = 2, α = 0.58 for guanine, and n = 2, α = 0.51 for adenine, which indicated the electrochemical oxidation of guanine and adenine on GS/IL/CS modified electrode was a two-electron and two-proton process. The oxidation overpotentials of guanine and adenine were decreased significantly compared with those obtained at the bare glassy carbon electrode and multi-walled carbon nanotubes modified electrode. The modified electrode exhibited good analytical performance and was successfully applied for individual and simultaneous determination of guanine and adenine. Low detection limits of 0.75 μM for guanine and 0.45 μM for adenine were obtained, with the linear calibration curves over the concentration range 2.5–150 μM and 1.5–350 μM, respectively. At the same time, the proposed method was successfully applied for the determination of guanine and adenine in denatured DNA samples with satisfying results. Moreover, the GS/IL/CS modified electrode exhibited good sensitivity, long-term stability and reproducibility for the determination of guanine and adenine.

  19. Gold nanoparticle/multi-walled carbon nanotube modified glassy carbon electrode as a sensitive voltammetric sensor for the determination of diclofenac sodium

    International Nuclear Information System (INIS)

    Afkhami, Abbas; Bahiraei, Atousa; Madrakian, Tayyebeh

    2016-01-01

    A simple and highly sensitive sensor for the determination of diclofenac sodium based on gold nanoparticle/multi-walled carbon nanotube modified glassy carbon electrode is reported. Scanning electron microscopy along with energy dispersive X-ray spectroscopy, electrochemical impedance spectroscopy, cyclic voltammetry and square wave voltammetry was used to characterize the nanostructure and performance of the sensor and the results were compared with those obtained at the multi-walled carbon nanotube modified glassy carbon electrode and bare glassy carbon electrode. Under the optimized experimental conditions diclofenac sodium gave linear response over the range of 0.03–200 μmol L −1 . The lower detection limits were found to be 0.02 μmol L −1 . The effect of common interferences on the current response of DS was investigated. The practical application of the modified electrode was demonstrated by measuring the concentration of diclofenac sodium in urine and pharmaceutical samples. This revealed that the gold nanoparticle/multiwalled carbon nanotube modified glassy carbon electrode shows excellent analytical performance for the determination of diclofenac sodium in terms of a very low detection limit, high sensitivity, very good accuracy, repeatability and reproducibility. - Highlights: • GCE was modified with multiwalled carbon nanotube and gold nanoparticles. • AuNP/MWCNT/GCE was used for the determination of diclofenac sodium. • Modified electrode was characterized by SEM, EDS and EIS. • The proposed method showed excellent analytical figures of merit. • This sensor was used for the determination of diclofenac sodium in real samples.

  20. Gold nanoparticle/multi-walled carbon nanotube modified glassy carbon electrode as a sensitive voltammetric sensor for the determination of diclofenac sodium

    Energy Technology Data Exchange (ETDEWEB)

    Afkhami, Abbas, E-mail: afkhami@basu.ac.ir; Bahiraei, Atousa; Madrakian, Tayyebeh

    2016-02-01

    A simple and highly sensitive sensor for the determination of diclofenac sodium based on gold nanoparticle/multi-walled carbon nanotube modified glassy carbon electrode is reported. Scanning electron microscopy along with energy dispersive X-ray spectroscopy, electrochemical impedance spectroscopy, cyclic voltammetry and square wave voltammetry was used to characterize the nanostructure and performance of the sensor and the results were compared with those obtained at the multi-walled carbon nanotube modified glassy carbon electrode and bare glassy carbon electrode. Under the optimized experimental conditions diclofenac sodium gave linear response over the range of 0.03–200 μmol L{sup −1}. The lower detection limits were found to be 0.02 μmol L{sup −1}. The effect of common interferences on the current response of DS was investigated. The practical application of the modified electrode was demonstrated by measuring the concentration of diclofenac sodium in urine and pharmaceutical samples. This revealed that the gold nanoparticle/multiwalled carbon nanotube modified glassy carbon electrode shows excellent analytical performance for the determination of diclofenac sodium in terms of a very low detection limit, high sensitivity, very good accuracy, repeatability and reproducibility. - Highlights: • GCE was modified with multiwalled carbon nanotube and gold nanoparticles. • AuNP/MWCNT/GCE was used for the determination of diclofenac sodium. • Modified electrode was characterized by SEM, EDS and EIS. • The proposed method showed excellent analytical figures of merit. • This sensor was used for the determination of diclofenac sodium in real samples.

  1. Investigation of chemical modifiers for sulfur determination in diesel fuel samples by high-resolution continuum source graphite furnace molecular absorption spectrometry using direct analysis

    Energy Technology Data Exchange (ETDEWEB)

    Huber, Charles S. [Instituto Federal Sul-rio-grandense, Câmpus Pelotas, Pelotas, RS (Brazil); Universidade Federal do Rio Grande do Sul, Instituto de Química, Porto Alegre, RS (Brazil); Vale, Maria Goreti R. [Universidade Federal do Rio Grande do Sul, Instituto de Química, Porto Alegre, RS (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Welz, Bernhard [Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Universidade Federal de Santa Catarina, Departamento de Química, Florianópolis, SC (Brazil); Andrade, Jailson B. [Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Dessuy, Morgana B., E-mail: mbdessuy@ufrgs.br [Universidade Federal do Rio Grande do Sul, Instituto de Química, Porto Alegre, RS (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq, INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil)

    2015-06-01

    High-resolution continuum source graphite furnace molecular absorption spectrometry has been applied for sulfur determination in diesel fuel. The sharp rotational lines of the carbon monosulfide molecule (formed during the vaporization step) were used to measure the absorbance. The analytical line at 258.056 nm was monitored using the sum of three pixels. Different chemical modifiers were investigated and the mixture of palladium and magnesium was used as chemical modifier in combination with iridium as permanent modifier. L-Cysteine was chosen as sulfur standard and the calibration was done against aqueous standard solutions. The proposed method was applied for the analyses of four diesel samples: two S10 samples and two S500 samples. The trueness of the method was checked with a certified reference material (CRM) of sulfur in diesel fuel (NIST 2724b). Accurate results, for samples and CRM, were achieved after a dilution with propan-1-ol. The following figures of merit were obtained: characteristic mass of 17 ± 3 ng, limit of detection and limit of quantification of 1.4 mg kg{sup −1} and 4.7 mg kg{sup −1}, respectively. - Highlights: • Ir, Ru and Zr were investigated as permanent modifiers. • Ca, Mg, Pd and Pd/Mg were investigated as modifiers in solution. • Indirect determination of sulfur monitoring the molecular absorbance of the CS • Direct analysis of diesel samples using a dilution in propan-1-ol.

  2. Gravimetric determination of uranium in SALE samples

    International Nuclear Information System (INIS)

    Anon.

    1981-01-01

    As a participant in the Safeguards Analytical Laboratory Evaluation (SALE) program, the Analytical Chemistry Laboratory at General Atomic routinely assays uranium dioxide and uranyl nitrate SALE samples for uranium content. Gravimetric methods are relatively easy and inexpensive to apply when the samples for uranium content. Gravimetric methods are relatively easy and inexpensive to apply when the samples are free from substantial amounts of metallic impurities. Clearly the gravimetric procedure alone is not specific for uranium and must be enhanced by the use of impurity corrections. Emission spectrography is used routinely as the technique of choice for making such corrections. In cases where it is essential to assay specifically for uranium, the modified Davies-Gray titration using a weighed titrant method is applied. In this paper some essential features of these gravimetric and titrimetric procedures are discussed

  3. Electrochemiluminescent determination of methamphetamine based on tris(2,2'-bipyridine)ruthenium(II) ion-association in organically modified silicate films

    International Nuclear Information System (INIS)

    Yi Changqing; Tao Yin; Wang Bo; Chen Xi

    2005-01-01

    Tetramethoxysilane (TMOS) and dimethyldimethoxysilane (DiMe-DiMOS) were used as co-precursor to immobilize poly(p-styrenesulfonate) (PSS), then tris(2,2'-bipyridine)ruthenium(II) (Ru(bpy) 3 2+ ) was successfully immobilized on a glass carbon electrode via ion-association. The immobilized Ru(bpy) 3 2+ shows good electrochemical and photochemical activities. Electrochemical and electrochemiluminescence (ECL) characterizations of the organically modified silicates (ORMOSILs) modified film electrodes were made by means of cyclic voltammetry and chronocoulometry. The ORMOSIL films were investigated by atomic force microscopy, scanning electrochemical microscope, tunnelling electrochemical microscope, X-ray photoelectron spectroscopy (XPS), UV-vis spectroscopy and fluorescence spectroscopy. XPS in-depth profiles revealed a homogeneous distribution of Ru(bpy) 3 2+ inside the silica thin layers. The modified electrode was used for the ECL determination of methamphetamine (METH) and showed high sensitivity. Detection limit was 2.0 x 10 -7 mol l -1 for METH (S/N = 3) with a linear range from 5.0 x 10 -7 to 1.0 x 10 -3 mol l -1 (R = 0.986). The relative standard deviation (n = 6) was 1.1% for the determination of 1.0 x 10 -5 mol l -1 METH. Furthermore, the Ru(bpy) 3 2+ immobilized modified electrode was applied in the ECL determination of methamphetamine (METH) in scout cases

  4. Electrochemiluminescent determination of methamphetamine based on tris(2,2'-bipyridine)ruthenium(II) ion-association in organically modified silicate films

    Energy Technology Data Exchange (ETDEWEB)

    Yi Changqing [Key Laboratory of Analytical Sciences of Ministry of Education, Department of Chemistry, Xiamen University, Xiamen 361005 (China); Tao Yin [Key Laboratory of Analytical Sciences of Ministry of Education, Department of Chemistry, Xiamen University, Xiamen 361005 (China); Wang Bo [Institute of Criminal Science and Technology of Xiamen, Xiamen 361005 (China); Chen Xi [Key Laboratory of Analytical Sciences of Ministry of Education, Department of Chemistry, Xiamen University, Xiamen 361005 (China)]. E-mail: xichen@xmu.edu.cn

    2005-06-13

    Tetramethoxysilane (TMOS) and dimethyldimethoxysilane (DiMe-DiMOS) were used as co-precursor to immobilize poly(p-styrenesulfonate) (PSS), then tris(2,2'-bipyridine)ruthenium(II) (Ru(bpy){sub 3} {sup 2+}) was successfully immobilized on a glass carbon electrode via ion-association. The immobilized Ru(bpy){sub 3} {sup 2+} shows good electrochemical and photochemical activities. Electrochemical and electrochemiluminescence (ECL) characterizations of the organically modified silicates (ORMOSILs) modified film electrodes were made by means of cyclic voltammetry and chronocoulometry. The ORMOSIL films were investigated by atomic force microscopy, scanning electrochemical microscope, tunnelling electrochemical microscope, X-ray photoelectron spectroscopy (XPS), UV-vis spectroscopy and fluorescence spectroscopy. XPS in-depth profiles revealed a homogeneous distribution of Ru(bpy){sub 3} {sup 2+} inside the silica thin layers. The modified electrode was used for the ECL determination of methamphetamine (METH) and showed high sensitivity. Detection limit was 2.0 x 10{sup -7} mol l{sup -1} for METH (S/N = 3) with a linear range from 5.0 x 10{sup -7} to 1.0 x 10{sup -3} mol l{sup -1} (R = 0.986). The relative standard deviation (n = 6) was 1.1% for the determination of 1.0 x 10{sup -5} mol l{sup -1} METH. Furthermore, the Ru(bpy){sub 3} {sup 2+} immobilized modified electrode was applied in the ECL determination of methamphetamine (METH) in scout cases.

  5. Direct determination of Cd and Pb in human urine by GFAAS with deuterium-lamp background correction using different chemical modifiers

    International Nuclear Information System (INIS)

    Husakova, L.; Baoinova, M.; Sramkova, J.; Cernohorsky, T.

    2007-01-01

    Several authors have contributed to the elaboration of methodology for direct determination of Cd and Pb in urine by graphite furnace atomic absorption spectrometry (GFAAS). In the proposed approaches, Zeeman background correction systems were predominantly used, without paying much attention to the selection of an appropriate chemical modifier. However, systematic studies on eleven recommended and less commonly used modifiers have resulted in optimization of atomization conditions, so that accurate analysis also with the use of D 2 -lamp background correction became possible. This was confirmed by comparative measurements using both background correction systems. For determination of Cd in urine, NH 4 F has been selected resulting in the lowest limit of detection (LOD): 0.07 μg L -1 . NH 4 F promotes efficient atomization at low temperatures and suppresses chloride interference effect. Pd + Sr (nitrate) has been selected as the most adequate modifier for determination of Pb. Its presence raised the maximum tolerable pyrolysis temperature up to 1200 o C, which resulted in the maximum reduction of the background signal and the lowest LOD of 1.5 mg L -1 for Pb (10 μL aliquots of dispensed urine). Applying the above modifiers to the analysis of standards and samples, direct aqueous calibration for accurate analysis of diluted and acidified urine samples became possible. Accuracy of the analysis was verified by the use of commercially available quality control reference materials. (authors)

  6. Nanomolar simultaneous determination of levodopa and serotonin at a novel carbon ionic liquid electrode modified with Co(OH)2 nanoparticles and multi-walled carbon nanotubes

    International Nuclear Information System (INIS)

    Babaei, Ali; Taheri, Ali Reza; Aminikhah, Majid

    2013-01-01

    Highlights: ► A novel modified carbon ionic liquid electrode is fabricated as Nafion/Co(OH) 2 –MWCNTs/CILE. ► The modified electrode was used as the new sensor for nanomolar simultaneous determinations of L-dopa and serotonin. ► The electrode was impermeable to uric acid and ascorbic acid and other anionic species as electroactive coexistent compounds. ► Several techniques as cyclic voltammetry, differential pulse voltammetry and chronoamperometry were used for investigations. ► The proposed sensor showed a wide linear range, low detection limit, high stability and good reproducibility. -- Abstract: A novel modified carbon ionic liquid electrode is prepared as an electrochemical sensor for simultaneous determination of levodopa (L-dopa) and serotonin (5-HT). The experimental results suggest that a carbon ionic liquid electrode modified with multi-walled carbon nanotubes and cobalt hydroxide nanoparticles, and coated with Nafion (Nafion/Co(OH) 2 –MWCNTs/CILE), accelerates the electron transfer reactions of L-dopa and 5-HT. In addition it shows no significant interferences of uric acid and ascorbic acid as electroactive coexistent compounds with L-dopa and 5-HT in biological systems. The fabricated sensor revealed some advantages such as convenient preparation, good stability and high sensitivity toward 5-HT and L-dopa determination. The DPV data showed that the obtained anodic peak currents were linearly dependent on the L-dopa and 5-HT concentrations in the range of 0.25–225 and 0.05–75 μmol L −1 , respectively. The applicability of the modified electrode was demonstrated by simultaneous determination of 5-HT and L-dopa in human serum

  7. Development of a Novel Cu(II Complex Modified Electrode and a Portable Electrochemical Analyzer for the Determination of Dissolved Oxygen (DO in Water

    Directory of Open Access Journals (Sweden)

    Salvatore Gianluca Leonardi

    2016-04-01

    Full Text Available The development of an electrochemical dissolved oxygen (DO sensor based on a novel Cu(II complex-modified screen printed carbon electrode is reported. The voltammetric behavior of the modified electrode was investigated at different scan rates and oxygen concentrations in PBS (pH = 7. An increase of cathodic current (at about −0.4 vs. Ag/AgCl with the addition of oxygen was observed. The modified Cu(II complex electrode was demonstrated for the determination of DO in water using chronoamperometry. A small size and low power consumption home-made portable electrochemical analyzer based on custom electronics for sensor interfacing and operating in voltammetry and amperometry modes has been also designed and fabricated. Its performances in the monitoring of DO in water were compared with a commercial one.

  8. Distribution of phosphorus and hydroxypropyl groups within granules of modified sweet potato starches as determined after chemical peeling

    NARCIS (Netherlands)

    Zhao, J.; Schols, H.A.; Chen Zenghong,; Jin, Z.; Buwalda, P.; Gruppen, H.

    2015-01-01

    The distributions of phosphorus and hydroxypropyl groups within granules of cross-linked and hydroxypropylated sweet potato starches were investigated. Chemical surface peeling of starch granules was performed after sieving of native and modified starches into large-size (diameter = 20 µm) and

  9. Critical biological parameters modulate affinity as a determinant of function in T-cell receptor gene-modified T-cells.

    Science.gov (United States)

    Spear, Timothy T; Wang, Yuan; Foley, Kendra C; Murray, David C; Scurti, Gina M; Simms, Patricia E; Garrett-Mayer, Elizabeth; Hellman, Lance M; Baker, Brian M; Nishimura, Michael I

    2017-11-01

    T-cell receptor (TCR)-pMHC affinity has been generally accepted to be the most important factor dictating antigen recognition in gene-modified T-cells. As such, there is great interest in optimizing TCR-based immunotherapies by enhancing TCR affinity to augment the therapeutic benefit of TCR gene-modified T-cells in cancer patients. However, recent clinical trials using affinity-enhanced TCRs in adoptive cell transfer (ACT) have observed unintended and serious adverse events, including death, attributed to unpredicted off-tumor or off-target cross-reactivity. It is critical to re-evaluate the importance of other biophysical, structural, or cellular factors that drive the reactivity of TCR gene-modified T-cells. Using a model for altered antigen recognition, we determined how TCR-pMHC affinity influenced the reactivity of hepatitis C virus (HCV) TCR gene-modified T-cells against a panel of naturally occurring HCV peptides and HCV-expressing tumor targets. The impact of other factors, such as TCR-pMHC stabilization and signaling contributions by the CD8 co-receptor, as well as antigen and TCR density were also evaluated. We found that changes in TCR-pMHC affinity did not always predict or dictate IFNγ release or degranulation by TCR gene-modified T-cells, suggesting that less emphasis might need to be placed on TCR-pMHC affinity as a means of predicting or augmenting the therapeutic potential of TCR gene-modified T-cells used in ACT. A more complete understanding of antigen recognition by gene-modified T-cells and a more rational approach to improve the design and implementation of novel TCR-based immunotherapies is necessary to enhance efficacy and maximize safety in patients.

  10. Simultaneous determination of mycophenolate mofetil and its active metabolite, mycophenolic acid, by differential pulse voltammetry using multi-walled carbon nanotubes modified glassy carbon electrode

    Energy Technology Data Exchange (ETDEWEB)

    Madrakian, Tayyebeh, E-mail: madrakian@basu.ac.ir; Soleimani, Mohammad; Afkhami, Abbas

    2014-09-01

    A highly sensitive electrochemical sensor for the simultaneous determination of mycophenolate mofetil (MPM) and mycophenolic acid (MPA) was fabricated by multi-walled carbon nanotubes modified glassy carbon electrode (MWCNTs/GCE). The electrochemical behavior of these two drugs was studied at the modified electrode using cyclic voltammetry and adsorptive differential pulse voltammetry. MPM and MPA were oxidized at the GCE during an irreversible process. DPV analysis showed two oxidation peaks at 0.87 V and 1.1 V vs. Ag/AgCl for MPM and an oxidation peak at 0.87 V vs. Ag/AgCl for MPA in phosphate buffer solution of pH 5.0. The MWCNTs/GCE displayed excellent electrochemical activities toward oxidation of MPM and MPA relative to the bare GCE. The experimental design algorithm was used for optimization of DPV parameters. The electrode represents linear responses in the range 5.0 × 10{sup −6} to 1.6 × 10{sup −4} mol L{sup −1} and 2.5 × 10{sup −6} mol L{sup −1} to 6.0 × 10{sup −5} mol L{sup −1} for MPM and MPA, respectively. The detection limit was found to be 9.0 × 10{sup −7} mol L{sup −1} and 4.0 × 10{sup −7} mol L{sup −1} for MPM and MPA, respectively. The modified electrode showed a good sensitivity and stability. It was successfully applied to the simultaneous determination of MPM and MPA in plasma and urine samples. - Highlights: • A new modified electrochemical sensor was constructed and used. • Multiwalled carbon nanotubes were used as the modifiers. • MPM and MPA were measured simultaneously at the low levels. • The sensor was used to the determination of MPA and MPM in real samples.

  11. Cost-effective flow injection amperometric system with metal nanoparticle loaded carbon nanotube modified screen printed carbon electrode for sensitive determination of hydrogen peroxide.

    Science.gov (United States)

    Reanpang, Preeyaporn; Themsirimongkon, Suwaphid; Saipanya, Surin; Chailapakul, Orawon; Jakmunee, Jaroon

    2015-11-01

    Various metal nanoparticles (NPs) decorated on carbon nanotube (CNT) was modified on the home-made screen printed carbon electrode (SPCE) in order to enhances sensitivity of hydrogen peroxide (H2O2) determination. The simple casting method was used for the electrode modification. The monometallic and bimetallic NPs modified electrodes were investigated for their electrochemical properties for H2O2 reduction. The Pd-CNT/SPCE is appropriated to measure the H2O2 reduction at a potential of -0.3 V, then this modified electrode was incorporated with a home-made flow through cell and applied in a simple flow injection amperometry (FI-Amp). Some parameters influencing the resulted modified electrode and the FI-Amp system were studied. The proposed detection system was able to detect H2O2 in the range of 0.1-1.0 mM, with detection limit of 20 µM. Relative standard deviation for 100 replicated injections of 0.6 mM H2O2 was 2.3%. The reproducibility of 6 electrodes preparing in 3 different lots was 8.2%. It was demonstrated for determination of H2O2 in disinfectant, hair colorant and milk samples. Recoveries in the range of 90-109% were observed. The developed system provided high stability, good repeatability, high sample throughput and low reagent consumption. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. A new sensor based on glassy carbon electrode modified with nanocomposite for simultaneous determination of acetaminophen, ascorbic acid and uric acid

    Directory of Open Access Journals (Sweden)

    Mohammad Afrasiabi

    2016-09-01

    Full Text Available A chemically-modified electrode has been constructed based on a single walled carbon nanotube/chitosan/room temperature ionic liquid nanocomposite modified glassy carbon electrode (SWCNTs–CHIT–RTIL/GCE. It was demonstrated that this sensor could be used for simultaneous determination of acetaminophen (ACT, uric acid (URI and ascorbic acid (ASC. The measurements were carried out by application of differential pulse voltammetry (DPV, cyclic voltammetry (CV and chronoamperometry (CA methods. Electrochemical studies suggested that the RTIL and SWCNTs provided a synergistic augmentation that can increase current responses by improvement of electron transfers of these compounds on the electrode surface. The presence of the CHIT in the modified electrode can enhance the repeatability of the sensor by its antifouling effect. The modified electrode showed electrochemical responses with high sensitivity for ACT, URI and ASC determination, which makes it a suitable sensor for simultaneous sub-μmol L−1 detection of ACT, URI and ASC in aqueous solutions. The analytical performance of this sensor has been evaluated for detection of ACT, URI and ASC in human serum and urine with satisfactory results.

  13. Gold nanoparticle/multi-walled carbon nanotube modified glassy carbon electrode as a sensitive voltammetric sensor for the determination of diclofenac sodium.

    Science.gov (United States)

    Afkhami, Abbas; Bahiraei, Atousa; Madrakian, Tayyebeh

    2016-02-01

    A simple and highly sensitive sensor for the determination of diclofenac sodium based on gold nanoparticle/multi-walled carbon nanotube modified glassy carbon electrode is reported. Scanning electron microscopy along with energy dispersive X-ray spectroscopy, electrochemical impedance spectroscopy, cyclic voltammetry and square wave voltammetry was used to characterize the nanostructure and performance of the sensor and the results were compared with those obtained at the multi-walled carbon nanotube modified glassy carbon electrode and bare glassy carbon electrode. Under the optimized experimental conditions diclofenac sodium gave linear response over the range of 0.03-200μmolL(-1). The lower detection limits were found to be 0.02μmolL(-1). The effect of common interferences on the current response of DS was investigated. The practical application of the modified electrode was demonstrated by measuring the concentration of diclofenac sodium in urine and pharmaceutical samples. This revealed that the gold nanoparticle/multiwalled carbon nanotube modified glassy carbon electrode shows excellent analytical performance for the determination of diclofenac sodium in terms of a very low detection limit, high sensitivity, very good accuracy, repeatability and reproducibility. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. Determination of Oxygen - to - Uranium Ratio in Hyperstoichio - Metric Uranium Dioxide. RCN Report

    International Nuclear Information System (INIS)

    Tolk, A.; Lingerak, W.A.

    1970-09-01

    For the determination of the O/U ratio in hyperstoichiometric uranium dioxide we prefer the following chemical procedure. The sample is dissolved in concentrated phosphoric acid without change in valence of the uranium. Then the amount of U (VI) present in the solution is titrated with a Fe (II) - standard solution in phosphoric acid. The titrimetric end-point is detected following the ''dead-stop-end-point'' procedure. When special precautions are made the O/U value can be determined with an accuracy and precision of + 0.0001 0/U units when 500 mg sample aliquots are used. (author)

  15. Differential pulse voltammetric determination of salbutamol sulfate in syrup pharmaceutical formulation using poly(4-amino-3-hydroxynaphthalene sulfonic acid modified glassy carbon electrode

    Directory of Open Access Journals (Sweden)

    Meareg Amare

    2017-10-01

    Full Text Available A new method for determination of salbutamol sulfate has been developed using poly(4-amino-3-hydroxynaphthalene sulfonic acid/GCE. Cyclic voltammetric investigation of the electrochemical behavior of salbutamol sulfate at the polymer modified glassy carbon unveiled electrocatalytic activity of the modifier towards irreversible oxidation of salbutamol sulfate. Dependence of peak current predominantly on scan rate than on square root of scan rate, and peak potential shift with pH demonstrated that oxidation of salbutamol sulfate at the polymer modified electrode follows adsorption reaction kinetics with proton participation.Under optimized solution and differential pulse voltammetric parameters, the oxidative peak current showed linear dependence on salbutamol sulfate concentration in the range 0.2 to 8 μM with method detection limit (3s/m and determination coefficient (R2 of 6.8 × 10−8 M and 0.99786, respectively. Low method detection limit, relatively wide linear range, and recovery results of spiked standard salbutamol sulfate in syrup samples in the range 96.7–98.9% validated the method for determination of salbutamol sulfate in pharmaceutical formulations.Differential pulse voltammetric analysis of salbutamol sulfate syrup formulation for its salbutamol sulfate content revealed 98.8 to 99.3% of the labeled value confirming the applicability of the developed method for determination of salbutamol sulfate in real samples. Keywords: Electrochemistry, Analytical chemistry

  16. A simple and efficient electrochemical sensor for folic acid determination in human blood plasma based on gold nanoparticles–modified carbon paste electrode

    International Nuclear Information System (INIS)

    Arvand, Majid; Dehsaraei, Mohammad

    2013-01-01

    Folic acid (FA) is a water soluble vitamin that exists in many natural species. The lack of FA causes some deficiencies in human body, so finding a simple and sensitive method for determining the FA is important. A new chemically modified electrode was fabricated for determination of FA in human blood plasma using gold nanoparticles (AuNPs) and carbon paste electrode (CPE). Gold nanoparticles–modified carbon paste electrode (AuNPs/CPE) was characterized by transmission electron microscopy (TEM) and scanning electron microscopy (SEM). The experimental parameters such as pH, scan rate (ν) and amount of modifier were studied by cyclic voltammetry and the optimized values were chosen. The electrochemical parameters such as diffusion coefficient of FA (D FA ), electrode surface area (A) and electron transfer coefficient (α) were calculated. Square wave voltammetry as an accurate technique was used for quantitative calculations. A good linear relation was observed between anodic peak current (i pa ) and FA concentration (C FA ) in the range of 6 × 10 −8 to 8 × 10 −5 mol L −1 , and the detection limit (LOD) achieved 2.7 × 10 −8 mol L −1 , that is comparable with recently studies. This paper demonstrated a novel, simple, selective and rapid sensor for determining the FA in the biological samples. - Highlights: • We examine a AuNPs/CPE for direct electrooxidation behavior and determination of FA. • Characterization of the electrode showed an obvious increase in surface area and porosity after modification. • The modified electrode showed good ability to distinguish the electrochemical response of FA. • The results were attributed to the specific characteristics of AuNPs present in the AuNPs/CPE. • This paper demonstrated a simple and rapid sensor for determination of FA in plasma

  17. Determination of Copper in Different Ethanolic Matrices Using a Chloropropyl Silica Gel Modified with a Nanostructured Cubic Octa(3-aminopropyloctasilsesquioxane

    Directory of Open Access Journals (Sweden)

    Devaney Ribeiro Do Carmo

    2013-01-01

    Full Text Available The chloropropyl silica gel was modified with octa(3-aminopropyloctasilsesquioxane and characterized by Fourier transform infrared (FTIR spectroscopy, nuclear magnetic resonance (NMR, spectroscopies, and surface and area porosity. The specific sorption capacity of metallic ions (Cu2+ and Ni2+ increases in the following solvent order: water < ethanol 42% < ethanol < ketone. The high values of the constant (K in the order of 103 L mol−1 suggested the high adsorbent capacity of the modified silica (SGAPC for Cu2+ and Ni2+. SGAPC was applied to a separation column and shows recoveries of around 100% of copper in samples of sugar cane spirit, vodka, ginger brandy, and ethanol fuel.

  18. Determination of local constitutive properties of titanium alloy matrix in boron-modified titanium alloys using spherical indentation

    International Nuclear Information System (INIS)

    Sreeranganathan, A.; Gokhale, A.; Tamirisakandala, S.

    2008-01-01

    The constitutive properties of the titanium alloy matrix in boron-modified titanium alloys are different from those of the corresponding unreinforced alloy due to the microstructural changes resulting from the addition of boron. Experimental and finite-element analyses of spherical indentation with a large penetration depth to indenter radius ratio are used to compute the local constitutive properties of the matrix alloy. The results are compared with that of the corresponding alloy without boron, processed in the same manner

  19. Combining the modified Skyrme-like model and the local density approximation to determine the symmetry energy of nuclear matter

    Science.gov (United States)

    Liu, Jian; Ren, Zhongzhou; Xu, Chang

    2018-07-01

    Combining the modified Skyrme-like model and the local density approximation model, the slope parameter L of symmetry energy is extracted from the properties of finite nuclei with an improved iterative method. The calculations of the iterative method are performed within the framework of the spherical symmetry. By choosing 200 neutron rich nuclei on 25 isotopic chains as candidates, the slope parameter is constrained to be 50 MeV nuclear matter can be obtained together.

  20. Selective determination of four arsenic species in rice and water samples by modified graphite electrode-based electrolytic hydride generation coupled with atomic fluorescence spectrometry.

    Science.gov (United States)

    Yang, Xin-An; Lu, Xiao-Ping; Liu, Lin; Chi, Miao-Bin; Hu, Hui-Hui; Zhang, Wang-Bing

    2016-10-01

    This work describes a novel non-chromatographic approach for the accurate and selective determining As species by modified graphite electrode-based electrolytic hydride generation (EHG) for sample introduction coupled with atomic fluorescence spectrometry (AFS) detection. Two kinds of sulfydryl-containing modifiers, l-cysteine (Cys) and glutathione (GSH), are used to modify cathode. The EHG performance of As has been changed greatly at the modified cathode, which has never been reported. Arsenite [As(III)] on the GSH modified graphite electrode (GSH/GE)-based EHG can be selectively and quantitatively converted to AsH3 at applied current of 0.4A. As(III) and arsenate [As(V)] on the Cys modified graphite electrode (Cys/GE) EHG can be selectively and efficiently converted to arsine at applied current of 0.6A, whereas monomethylarsonic acid (MMA) and dimethylarsinic acid (DMA) do not form any or only less volatile hydrides under this condition. By changing the analytical conditions, we also have achieved the analysis of total As (tAs) and DMA. Under the optimal condition, the detection limits (3s) of As(III), iAs and tAs in aqueous solutions are 0.25μgL(-1), 0.22μgL(-1) and 0.10μgL(-1), respectively. The accuracy of the method is verified through the analysis of standard reference materials (SRM 1568a). Copyright © 2016 Elsevier B.V. All rights reserved.

  1. Activated carbon-modified knotted reactor coupled to electrothermal atomic absorption spectrometry for sensitive determination of arsenic species in medicinal herbs and tea infusions

    Energy Technology Data Exchange (ETDEWEB)

    Grijalba, Alexander Castro; Martinis, Estefanía M. [Laboratory of Analytical Chemistry for Research and Development (QUIANID), Facultad de Ciencias Exactas y Naturales, Universidad Nacional de Cuyo, Padre J. Contreras 1300, (5500) Mendoza (Argentina); Consejo Nacional de Investigaciones Científicas y Técnicas (CONICET), Buenos Aires (Argentina); Lascalea, Gustavo E. [Consejo Nacional de Investigaciones Científicas y Técnicas (CONICET), Buenos Aires (Argentina); Wuilloud, Rodolfo G., E-mail: rwuilloud@mendoza-conicet.gob.ar [Laboratory of Analytical Chemistry for Research and Development (QUIANID), Facultad de Ciencias Exactas y Naturales, Universidad Nacional de Cuyo, Padre J. Contreras 1300, (5500) Mendoza (Argentina); Consejo Nacional de Investigaciones Científicas y Técnicas (CONICET), Buenos Aires (Argentina)

    2015-01-01

    A flow injection system based on a modified polytetrafluoroethylene (PTFE) knotted reactor (KR) was developed for arsenite [As(III)] and arsenate [As(V)] species preconcentration and determination by electrothermal atomic absorption spectrometry (ETAAS). Activated carbon (AC) was immobilized on the inner walls of a PTFE KR by a thermal treatment. A significant increase in analyte retention was obtained with the AC-modified KR (100%) as compared to the regular PTFE KR (25%). The preconcentration method involved the on-line formation of As(III)-ammonium pyrrolidinedithiocarbamate (As-APDC) complex, followed by its adsorption onto the inner walls of the AC-modified KR. After analyte retention, the complex was eluted with acetone directly into the graphite furnace of ETAAS. The parameters affecting the flow injection system were evaluated with a full central composite face centered design with three center points. Under optimum conditions, a preconcentration factor of 200 was obtained with 10 ml of sample. The detection limit was 4 ng L{sup −1} and the relative standard deviation (RSD) for six replicate measurements at 0.2 μg L{sup −1} of As were 4.3% and 4.7% for As(III) and As(V), respectively. The developed methodology was highly selective towards As(III), while As(V), monomethylarsonic acid [MMA(V)] and dimethylarsinic [DMA(V)] were not retained in the AC-modified KR. The proposed method was successfully applied for As speciation analysis in infusions originated from medicinal herbs and tea. - Highlights: • We report an efficient method for As speciation. • We have modified a knotted reactor with activated carbon for high sorption capacity. • We provide a simple procedure for surface modification of a PTFE knotted reactor. • We have selectively separated inorganic As species from complex matrix samples. • We have implemented a modified KR in a flow injection system coupled to ETAAS.

  2. Activated carbon-modified knotted reactor coupled to electrothermal atomic absorption spectrometry for sensitive determination of arsenic species in medicinal herbs and tea infusions

    International Nuclear Information System (INIS)

    Grijalba, Alexander Castro; Martinis, Estefanía M.; Lascalea, Gustavo E.; Wuilloud, Rodolfo G.

    2015-01-01

    A flow injection system based on a modified polytetrafluoroethylene (PTFE) knotted reactor (KR) was developed for arsenite [As(III)] and arsenate [As(V)] species preconcentration and determination by electrothermal atomic absorption spectrometry (ETAAS). Activated carbon (AC) was immobilized on the inner walls of a PTFE KR by a thermal treatment. A significant increase in analyte retention was obtained with the AC-modified KR (100%) as compared to the regular PTFE KR (25%). The preconcentration method involved the on-line formation of As(III)-ammonium pyrrolidinedithiocarbamate (As-APDC) complex, followed by its adsorption onto the inner walls of the AC-modified KR. After analyte retention, the complex was eluted with acetone directly into the graphite furnace of ETAAS. The parameters affecting the flow injection system were evaluated with a full central composite face centered design with three center points. Under optimum conditions, a preconcentration factor of 200 was obtained with 10 ml of sample. The detection limit was 4 ng L −1 and the relative standard deviation (RSD) for six replicate measurements at 0.2 μg L −1 of As were 4.3% and 4.7% for As(III) and As(V), respectively. The developed methodology was highly selective towards As(III), while As(V), monomethylarsonic acid [MMA(V)] and dimethylarsinic [DMA(V)] were not retained in the AC-modified KR. The proposed method was successfully applied for As speciation analysis in infusions originated from medicinal herbs and tea. - Highlights: • We report an efficient method for As speciation. • We have modified a knotted reactor with activated carbon for high sorption capacity. • We provide a simple procedure for surface modification of a PTFE knotted reactor. • We have selectively separated inorganic As species from complex matrix samples. • We have implemented a modified KR in a flow injection system coupled to ETAAS

  3. Determination of the quadrupole moment of the fission-isomeric state in 238U by a modified charge-plunger method

    International Nuclear Information System (INIS)

    Pedersen, J.; Goerlach, U.; Habs, D.; Just, M.; Metag, V.; Mosler, E.; Schukraft, J.; Singer, P.; Specht, H.J.; Ulfert, G.

    1978-01-01

    A modified version of the charge plunger method has been developed which, by utilizing electrostatic fields, renders possible the separation of low- and high-charge recoil ions over short flight distances. With this technique the quadrupole moment of the 200 ns fission isomer in 238 U has been determined to be (29 +- 3) b. The corresponding deformation of c/a = (1.8 +- 0.1) provides another quantitative proof for shape isomerism in the actinide region. (orig.) [de

  4. Influence of citric acid as chemical modifier for lead determination in dietary calcium supplement samples by graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Cezar Paz de Mattos, Julio; Medeiros Nunes, Adriane; Figueiredo Martins, Ayrton; Luiz Dressler, Valderi; Marlon de Moraes Flores, Erico

    2005-01-01

    Citric acid was used as a chemical modifier for Pb determination by graphite furnace atomic absorption spectrometry in dietary supplement samples (calcium carbonate, dolomite and oyster shell samples) and its efficiency was compared to the use of palladium. Pyrolysis and atomization curves were established without use of chemical modifier, with the addition of 20, 100 and 200 μg of citric acid, and with 3 μg of palladium. The citric acid modifier made possible the interference-free Pb determination in the presence of high concentrations of Ca and Mg nitrates. Acid sample digestion involving closed vessels (microwave-assisted and conventional heating) and acid attack using polypropylene vessels at room temperature were compared. All digestion procedures presented similar results for calcium carbonate and dolomite samples. However, for oyster shell samples accurate results were obtained only with the use of closed vessel systems. Analyte addition and matrix-matched standards were used for calibration. The characteristic mass for Pb using citric acid and palladium were 16 and 25 pg, respectively. The relative standard deviation (RSD) was always less than 5% when citric acid was used. The relative and absolute limits of detection were 0.02 μg g -1 and 8 pg with citric acid and 0.1 μg g -1 and 44 pg with the Pd modifier, respectively (n = 10, 3σ). The recovery of Pb in spiked calcium supplement samples (10 μg l -1 ) was between 98% and 105%. With the use of 100 μg of citric acid as chemical modifier, problems such as high background absorption and high RSD values were minimized in comparison to the addition of 3 μg of palladium

  5. Reliability and validity of a modified MEDFICTS dietary fat screener in South African schoolchildren are determined by use and outcome measures.

    Science.gov (United States)

    Wenhold, Friedeburg Anna Maria; MacIntyre, Una Elizabeth; Rheeder, Paul

    2014-06-01

    In South Africa, noncommunicable diseases and obesity are increasing and also affect children. No validated assessment tools for fat intake are available. To determine test-retest reliability and relative validity of a pictorial modified meats, eggs, dairy, fried foods, fats in baked goods, convenience foods, table fats, and snacks (MEDFICTS) dietary fat screener. We determined test-retest reliability and diagnostic accuracy with the modified MEDFICTS as the index test and a 3-day weighed food record and parental completion of the screener as primary and secondary reference methods, respectively. Grade-six learners (aged 12 years, 4 months) in an urban, middle-class school (n=93) and their parents (n=72). Portion size, frequency of intake, final score, and classification of fat intake of the modified MEDFICTS, and percent energy from fat, saturated fatty acids, and cholesterol of the food record. For categorical data agreement was based on kappa statistics, McNemar's test for symmetry, and diagnostic performance parameters. Continuous data were analyzed with correlations, mean differences, the Bland-Altman method, and receiver operating characteristics. The classification of fat intake by the modified MEDFICTS was test-retest reliable. Final scores of the group did not differ between administrations (P=0.86). The correlation of final scores between administrations was significant for girls only (r=0.58; P=0.01). Reliability of portion size and frequency of intake scores depended on the food category. For girls the screener final score was significantly (P90%), but chance corrected agreement between the classifications was poor. Parents did not agree with their children. Test-retest reliability and relative validity of a modified MEDFICTS dietary fat screener in South African schoolchildren depended on the use and outcome measures applied. Copyright © 2014 Academy of Nutrition and Dietetics. Published by Elsevier Inc. All rights reserved.

  6. Simultaneous determination of paracetamol and ascorbic acid using tetraoctylammonium bromide capped gold nanoparticles immobilized on 1,6-hexanedithiol modified Au electrode

    International Nuclear Information System (INIS)

    Nair, Santhosh S.; John, S. Abraham; Sagara, Takamasa

    2009-01-01

    Tetraoctylammonium bromide stabilized gold nanoparticles (TOAB-AuNPs) attached to 1,6-hexanedithiol (HDT) modified Au electrode was used for the simultaneous determination of paracetamol (PA) and ascorbic acid (AA) at physiological pH. The attachment of TOAB-AuNPs on HDT modified Au surface was confirmed by attenuated total reflectance (ATR)-FT-IR spectroscopy and atomic force microscope (AFM). The ATR-FT-IR spectrum of TOAB-AuNPs attached to the HDT monolayer showed a characteristic stretching modes corresponding to -CH 2 and -CH 3 of TOAB, confirming the immobilization of AuNPs with surface-protecting TOAB ions on the surface of the AuNPs after being attached to HDT modified Au electrode. AFM image showed that the immobilized AuNPs were spherical in shape and densely packed to a film of ca. 7 nm thickness. Interestingly, TOAB-AuNPs modified electrode shifted the oxidation potential of PA towards less positive potential by 70 mV and enhanced its oxidation current twice when compared to bare Au electrode. In addition, the AuNPs modified electrode separated the oxidation potentials of AA and PA by 210 mV, whereas bare Au electrode failed to resolve them. The amperometry current of PA was increased linearly from 1.50 x 10 -7 to 1.34 x 10 -5 M with a correlation coefficient of 0.9981 and the lowest detection limit was found to be 2.6 nM (S/N = 3). The present method was successfully used to determine the concentration of PA in human blood plasma and commercial drugs.

  7. Simultaneous determination of paracetamol and ascorbic acid using tetraoctylammonium bromide capped gold nanoparticles immobilized on 1,6-hexanedithiol modified Au electrode

    Energy Technology Data Exchange (ETDEWEB)

    Nair, Santhosh S. [Department of Chemistry, Gandhigram Rural University, Gandhigram 624302, Dindigul (India); John, S. Abraham [Department of Chemistry, Gandhigram Rural University, Gandhigram 624302, Dindigul (India)], E-mail: abrajohn@yahoo.co.in; Sagara, Takamasa [Department of Chemistry, Gandhigram Rural University, Gandhigram 624302, Dindigul (India)], E-mail: sagara@nagasaki-u.ac.jp

    2009-11-30

    Tetraoctylammonium bromide stabilized gold nanoparticles (TOAB-AuNPs) attached to 1,6-hexanedithiol (HDT) modified Au electrode was used for the simultaneous determination of paracetamol (PA) and ascorbic acid (AA) at physiological pH. The attachment of TOAB-AuNPs on HDT modified Au surface was confirmed by attenuated total reflectance (ATR)-FT-IR spectroscopy and atomic force microscope (AFM). The ATR-FT-IR spectrum of TOAB-AuNPs attached to the HDT monolayer showed a characteristic stretching modes corresponding to -CH{sub 2} and -CH{sub 3} of TOAB, confirming the immobilization of AuNPs with surface-protecting TOAB ions on the surface of the AuNPs after being attached to HDT modified Au electrode. AFM image showed that the immobilized AuNPs were spherical in shape and densely packed to a film of ca. 7 nm thickness. Interestingly, TOAB-AuNPs modified electrode shifted the oxidation potential of PA towards less positive potential by 70 mV and enhanced its oxidation current twice when compared to bare Au electrode. In addition, the AuNPs modified electrode separated the oxidation potentials of AA and PA by 210 mV, whereas bare Au electrode failed to resolve them. The amperometry current of PA was increased linearly from 1.50 x 10{sup -7} to 1.34 x 10{sup -5} M with a correlation coefficient of 0.9981 and the lowest detection limit was found to be 2.6 nM (S/N = 3). The present method was successfully used to determine the concentration of PA in human blood plasma and commercial drugs.

  8. Electrochemical behavior and voltammetric determination of acetaminophen based on glassy carbon electrodes modified with poly(4-aminobenzoic acid)/electrochemically reduced graphene oxide composite films

    International Nuclear Information System (INIS)

    Zhu, Wencai; Huang, Hui; Gao, Xiaochun; Ma, Houyi

    2014-01-01

    Poly(4-aminobenzoic acid)/electrochemically reduced graphene oxide composite film modified glassy carbon electrodes (4-ABA/ERGO/GCEs) were fabricated by a two-step electrochemical method. The electrochemical behavior of acetaminophen at the modified electrode was investigated by means of cyclic voltammetry. The results indicated that 4-ABA/ERGO composite films possessed excellent electrocatalytic activity towards the oxidation of acetaminophen. The electrochemical reaction of acetaminophen at 4-ABA/ERGO/GCE is proved to be a surface-controlled process involving the same number of protons and electrons. The voltammetric determination of acetaminophen performed with the 4-ABA/ERGO modified electrode presents a good linearity in the range of 0.1–65 μM with a low detection limit of 0.01 μM (S/N = 3). In the case of using the 4-ABA/ERGO/GCE, acetaminophen and dopamine can be simultaneously determined without mutual interference. Furthermore, the 4-ABA/ERGO/GCE has good reproducibility and stability, and can be used to determine acetaminophen in tablets. - Highlights: • The 4-ABA/ERGO/GCE was fabricated by a two-step electrochemical method. • Electrochemical behavior of acetaminophen at the 4-ABA/ERGO/GCE was investigated. • The electrochemical sensor exhibited a low detection limit and good selectivity. • This sensor was applied to the detection of acetaminophen in commercial tablets

  9. Electrochemical behavior and voltammetric determination of acetaminophen based on glassy carbon electrodes modified with poly(4-aminobenzoic acid)/electrochemically reduced graphene oxide composite films

    Energy Technology Data Exchange (ETDEWEB)

    Zhu, Wencai [Key Laboratory for Colloid and Interface Chemistry of State Education Ministry, School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100 (China); School of Chemistry and Chemical Engineering, Qilu Normal University, Jinan 250013 (China); Huang, Hui; Gao, Xiaochun [Key Laboratory for Colloid and Interface Chemistry of State Education Ministry, School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100 (China); Ma, Houyi, E-mail: hyma@sdu.edu.cn [Key Laboratory for Colloid and Interface Chemistry of State Education Ministry, School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100 (China)

    2014-12-01

    Poly(4-aminobenzoic acid)/electrochemically reduced graphene oxide composite film modified glassy carbon electrodes (4-ABA/ERGO/GCEs) were fabricated by a two-step electrochemical method. The electrochemical behavior of acetaminophen at the modified electrode was investigated by means of cyclic voltammetry. The results indicated that 4-ABA/ERGO composite films possessed excellent electrocatalytic activity towards the oxidation of acetaminophen. The electrochemical reaction of acetaminophen at 4-ABA/ERGO/GCE is proved to be a surface-controlled process involving the same number of protons and electrons. The voltammetric determination of acetaminophen performed with the 4-ABA/ERGO modified electrode presents a good linearity in the range of 0.1–65 μM with a low detection limit of 0.01 μM (S/N = 3). In the case of using the 4-ABA/ERGO/GCE, acetaminophen and dopamine can be simultaneously determined without mutual interference. Furthermore, the 4-ABA/ERGO/GCE has good reproducibility and stability, and can be used to determine acetaminophen in tablets. - Highlights: • The 4-ABA/ERGO/GCE was fabricated by a two-step electrochemical method. • Electrochemical behavior of acetaminophen at the 4-ABA/ERGO/GCE was investigated. • The electrochemical sensor exhibited a low detection limit and good selectivity. • This sensor was applied to the detection of acetaminophen in commercial tablets.

  10. Electrochemical behavior and voltammetric determination of acetaminophen based on glassy carbon electrodes modified with poly(4-aminobenzoic acid)/electrochemically reduced graphene oxide composite films.

    Science.gov (United States)

    Zhu, Wencai; Huang, Hui; Gao, Xiaochun; Ma, Houyi

    2014-12-01

    Poly(4-aminobenzoic acid)/electrochemically reduced graphene oxide composite film modified glassy carbon electrodes (4-ABA/ERGO/GCEs) were fabricated by a two-step electrochemical method. The electrochemical behavior of acetaminophen at the modified electrode was investigated by means of cyclic voltammetry. The results indicated that 4-ABA/ERGO composite films possessed excellent electrocatalytic activity towards the oxidation of acetaminophen. The electrochemical reaction of acetaminophen at 4-ABA/ERGO/GCE is proved to be a surface-controlled process involving the same number of protons and electrons. The voltammetric determination of acetaminophen performed with the 4-ABA/ERGO modified electrode presents a good linearity in the range of 0.1-65 μM with a low detection limit of 0.01 μM (S/N=3). In the case of using the 4-ABA/ERGO/GCE, acetaminophen and dopamine can be simultaneously determined without mutual interference. Furthermore, the 4-ABA/ERGO/GCE has good reproducibility and stability, and can be used to determine acetaminophen in tablets. Copyright © 2014 Elsevier B.V. All rights reserved.

  11. Highly sensitive and simultaneous electrochemical determination of 2-aminophenol and 4-aminophenol based on poly(l-arginine)-β-cyclodextrin/carbon nanotubes@graphene nanoribbons modified electrode.

    Science.gov (United States)

    Yi, Yinhui; Zhu, Gangbing; Wu, Xiangyang; Wang, Kun

    2016-03-15

    Owing to the similar characteristics and physiochemical property of 2-aminophenol (2-AP) and 4-aminophenol (4-AP), the highly sensitive simultaneous electrochemical determination of 2- and 4-AP is a great challenge. In this paper, by electropolymerizing β-cyclodextrin (β-CD) and l-arginine (l-Arg) on the surface of carbon nanotubes@graphene nanoribbons (CNTs@GNRs) core-shell heterostructure, a P-β-CD-l-Arg/CNTs@GNRs nanohybrid modified electrode was prepared successfully, and it could exhibit the synergetic effects of β-CD (high host-guest recognition and enrichment ability), l-Arg (excellent electrocatalytic activity) and CNTs@GNRs (prominent electrochemical properties and large surface area), the P-β-CD-l-Arg/CNTs@GNRs modified electrode was used in the electrochemical determination of 2- and 4-AP, the results demonstrated that the highly sensitive and simultaneous determination of 2- and 4-AP is successfully achieved and the modified electrode has a linear response range of 25.0-1300.0 nM for both 2- and 4-AP, and the detection limits of 2- and 4-AP obtained in this work are 6.2 and 3.5 nM, respectively. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. Fabrication of gallium hexacyanoferrate modified carbon ionic liquid paste electrode for sensitive determination of hydrogen peroxide and glucose

    International Nuclear Information System (INIS)

    Haghighi, Behzad; Khosravi, Mehdi; Barati, Ali

    2014-01-01

    Gallium hexacyanoferrate (GaHCFe) and graphite powder were homogeneously dispersed into n-dodecylpyridinium hexafluorophosphate and paraffin to fabricate GaHCFe modified carbon ionic liquid paste electrode (CILPE). Mixture experimental design was employed to optimize the fabrication of GaHCFe modified CILPE (GaHCFe-CILPE). A pair of well-defined redox peaks due to the redox reaction of GaHCFe through one-electron process was observed for the fabricated electrode. The fabricated GaHCFe-CILPE exhibited good electrocatalytic activity towards reduction and oxidation of H 2 O 2 . The observed sensitivities for the electrocatalytic oxidation and reduction of H 2 O 2 at the operating potentials of + 0.8 and − 0.2 V were about 13.8 and 18.3 mA M −1 , respectively. The detection limit (S/N = 3) for H 2 O 2 was about 1 μM. Additionally, glucose oxidase (GOx) was immobilized on GaHCFe-CILPE using two methodology, entrapment into Nafion matrix and cross-linking with glutaraldehyde and bovine serum albumin, in order to fabricate glucose biosensor. Linear dynamic rage, sensitivity and detection limit for glucose obtained by the biosensor fabricated using cross-linking methodology were 0.1–6 mM, 0.87 mA M −1 and 30 μM, respectively and better than those obtained (0.2–6 mM, 0.12 mA M −1 and 50 μM) for the biosensor fabricated using entrapment methodology. - Highlights: • Gallium hexacyanoferrate modified carbon ionic liquid paste electrode was fabricated. • Mixture experimental design was used to optimize electrode fabrication. • Response trace plot was used to show the effect of electrode materials on response. • The sensor exhibited electrocatalytic activity towards H 2 O 2 reduction and oxidation. • Glucose biosensor was fabricated by immobilization of glucose oxidase on sensor

  13. Modified solution calorimetry approach for determination of vaporization and sublimation enthalpies of branched-chain aliphatic and alkyl aromatic compounds at T = 298.15 K

    International Nuclear Information System (INIS)

    Varfolomeev, Mikhail A.; Novikov, Vladimir B.; Nagrimanov, Ruslan N.; Solomonov, Boris N.

    2015-01-01

    Highlights: • Solution enthalpies of 18 branching-chain alkyl aromatic and aliphatic compounds in cyclohexane were measured. • Group contributions to the enthalpy of solvation due to branching and substitution in carbon chain were evaluated. • Modified solution calorimetry based approach for determination of vaporization/sublimation enthalpies was proposed. • This approach provides vaporization/sublimation enthalpies directly at T = 298.15 K. • Vaporization/sublimation enthalpies of 35 branched-chain alkyl aromatic and aliphatic compounds were determined. - Abstract: The enthalpies of solution, solvation and vaporization/sublimation are interrelated values combined in the simplest thermodynamic circle. Hence, experimental determination of vaporization/sublimation enthalpy can be substituted by experimentally simpler determination of solution enthalpy when solvation enthalpy is known. Previously it was found that solvation enthalpies of a wide range of unbranched aliphatic and aromatic solutes in saturated hydrocarbons are in good linear correlation with their molar refraction values. This allows to estimate the vaporization/sublimation enthalpy of any unbranched organic compound from its solution enthalpy in saturated hydrocarbon and molar refraction. In the present work this approach was modified for determination of vaporization/sublimation enthalpy of branched-chain alkyl aromatic and aliphatic compounds. Group contributions to the enthalpy of solvation due to the branching of carbon chain were evaluated. Enthalpies of solution at infinite dilution of 18 branched-chain aliphatic and alkyl aromatic compounds were measured at T = 298.15 K. Vaporization/sublimation enthalpies for 35 branched aliphatic and alkyl aromatic compounds were determined by using modified solution calorimetry approach. These values are in good agreement with available literature data on vaporization/sublimation enthalpies obtained by conventional methods.

  14. The modified CKD-EPI equation may be not more accurate than CKD-EPI equation in determining glomerular filtration rate in Chinese patients with chronic kidney disease.

    Science.gov (United States)

    Xie, Peng; Huang, Jian-Min; Li, Ying; Liu, Huai-Jun; Qu, Yan

    2017-06-01

    To investigate the application of the new modified Chronic Kidney Disease Epidemiology Collaboration (mCKD-EPI) equation developed by Liu for the measurement of glomerular filtration rate (GFR) in Chinese patients with chronic kidney disease (CKD) and to evaluate whether this modified form is more accurate than the original one in clinical practice. GFR was determined simultaneously by 3 methods: (a) 99m Tc-diethylene triamine pentaacetic acid ( 99m Tc-DTPA) dual plasma sample clearance method (mGFR), which was used as the reference standard; (b) CKD-EPI equation (eGFRckdepi); (c) modified CKD-EPI equation (eGFRmodified). Concordance correlation and Passing-Bablok regression were used to compare the validity of eGFRckdepi and eGFRmodified. Bias, precision and accuracy were compared to identify which equation showed the better performance in determining GFR. A total of 170 patients were enrolled. Both eGFRckdepi and eGFRmodified correlated well with mGFR (concordance correlation coefficient 0.90 and 0.74, respectively) and the Passing-Bablok regression equation of eGFRckdepi and eGFRmodified against mGFR was mGFR = 0.37 + 1.04 eGFRckdepi and -49.25 + 1.74 eGFRmodified, respectively. In terms of bias, precision and 30 % accuracy, eGFRmodified showed a worse performance compared to eGFRckdepi, in the whole cohort. The new modified CKD-EPI equation cannot replace the original CKD-EPI equation in determining GFR in Chinese patients with CKD.

  15. A modified HPLC method improves the simultaneous determination of plasma kynurenine and tryptophan concentrations in patients following maintenance hemodialysis

    Science.gov (United States)

    XIAO, CHENGGEN; CHEN, YUANHAN; LIANG, XINLING; XIE, ZHEN; ZHANG, MIN; LI, RUIZHAO; LI, ZHILIAN; FU, XIA; YU, XIYONG; SHI, WEI

    2014-01-01

    The ratio between plasma kynurenine (Kyn) and tryptophan (Trp) serves as a marker of indoleamine 2,3-dioxygenase, a critical immunomodulatory molecule. Simultaneous detection of the two markers may be performed using high-pressure liquid chromatography (HPLC). However, for uremic patients, the conventional detection method may be affected by a range of accumulated toxins. The current study aimed to establish a method for the simultaneous measurement of Kyn and Trp in patients following maintenance hemodialysis via HPLC-ultraviolet detection. The procedure involved the use of a SinoChrom ODS-BP C18 column (4.6×150 mm; inner diameter, 4.5 μm) and a mobile phase of 15 mmol/l sodium acetate acetic acid solution (containing 5% acetonitrile, pH 4.8). The modified method was verified using plasma samples from 10 healthy controls and 91 maintenance hemodialysis patients. The results demonstrated that the modified method was successful in simultaneously detecting the concentrations of Trp and Kyn in the healthy controls and maintenance hemodialysis patients. The method is simple, fast, accurate and suitable for clinical and research purposes in maintenance hemodialysis patients. PMID:24669249

  16. Determination of Arsenic in Soil Alkali by Graphite Furnace Atomic Absorption Spectrophotometery Using Modified Corn Silk Fiber as Adsorbent

    International Nuclear Information System (INIS)

    Zhou, X.; Ju, S.; Liu, M.; Zhao, Y.

    2015-01-01

    A safe, rapid, simple and environmentally friendly method based modified corn silk fiber (MC), chemical modified with succinic anhydride (C/sub 4/H/sub 4/O/sub 3/), was developed for the extraction and preconcentration of As(III) in food additives soil alkali sample prior to graphite furnace atomic absorption spectrometry (GFAAS) analysis. The structure and properties of VC (unmodified corn silk fiber) and MC were analyzed and discussed by means of FTIR, SEM and TG, and the effect of adsorbent amount, pH, soil alkali solution concentration, adsorption time and adsorption temperature were carefully optimized. Under the optimum conditions, the relative standard deviations (RSD, n=6) were 1.27-3.05%, the calibration graph was linear in the range of 0-100 meu g/ L and the limits of detection (LOD) was 0.13 meu g/L. The surface of MC became loose and porous which increased the adsorption area. Comparing with VC, carboxy groups were measured in MC and the increase of negative electron group in fiber molecular made its coordination combining ability with As(III) enhanced; In comparison with the removal arsenic rate of VC, MC's significantly increased by 2.86 fold. The recovery rate of soil alkali, treated by VC and MC, reached to 96.85% and 94.32%, and it did not affected the function of soil alkali. (author)

  17. A Stabilized Finite Element Method for Modified Poisson-Nernst-Planck Equations to Determine Ion Flow Through a Nanopore

    Science.gov (United States)

    Chaudhry, Jehanzeb Hameed; Comer, Jeffrey; Aksimentiev, Aleksei; Olson, Luke N.

    2013-01-01

    The conventional Poisson-Nernst-Planck equations do not account for the finite size of ions explicitly. This leads to solutions featuring unrealistically high ionic concentrations in the regions subject to external potentials, in particular, near highly charged surfaces. A modified form of the Poisson-Nernst-Planck equations accounts for steric effects and results in solutions with finite ion concentrations. Here, we evaluate numerical methods for solving the modified Poisson-Nernst-Planck equations by modeling electric field-driven transport of ions through a nanopore. We describe a novel, robust finite element solver that combines the applications of the Newton's method to the nonlinear Galerkin form of the equations, augmented with stabilization terms to appropriately handle the drift-diffusion processes. To make direct comparison with particle-based simulations possible, our method is specifically designed to produce solutions under periodic boundary conditions and to conserve the number of ions in the solution domain. We test our finite element solver on a set of challenging numerical experiments that include calculations of the ion distribution in a volume confined between two charged plates, calculations of the ionic current though a nanopore subject to an external electric field, and modeling the effect of a DNA molecule on the ion concentration and nanopore current. PMID:24363784

  18. Functionalized-graphene modified graphite electrode for the selective determination of dopamine in presence of uric acid and ascorbic acid.

    Science.gov (United States)

    Mallesha, Malledevaru; Manjunatha, Revanasiddappa; Nethravathi, C; Suresh, Gurukar Shivappa; Rajamathi, Michael; Melo, Jose Savio; Venkatesha, Thimmappa Venkatarangaiah

    2011-06-01

    Graphene is chemically synthesized by solvothermal reduction of colloidal dispersions of graphite oxide. Graphite electrode is modified with functionalized-graphene for electrochemical applications. Electrochemical characterization of functionalized-graphene modified graphite electrode (FGGE) is carried out by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The behavior of FGGE towards ascorbic acid (AA), dopamine (DA) and uric acid (UA) has been investigated by CV, differential pulse voltammetry (DPV) and chronoamperommetry (CA). The FGGE showed excellent catalytic activity towards electrochemical oxidation of AA, DA and UA compared to that of the bare graphite electrode. The electrochemical oxidation signals of AA, DA and UA are well separated into three distinct peaks with peak potential separation of 193mv, 172mv and 264mV between AA-DA, DA-UA and AA-UA respectively in CV studies and the corresponding peak potential separations in DPV mode are 204mv, 141mv and 345mv. The FGGE is successfully used for the simultaneous detection of AA, DA and UA in their ternary mixture and DA in serum and pharmaceutical samples. The excellent electrocatalytic behavior of FGGE may lead to new applications in electrochemical analysis. Copyright © 2011 Elsevier B.V. All rights reserved.

  19. tRNA modifying enzymes, NSUN2 and METTL1, determine sensitivity to 5-fluorouracil in HeLa cells.

    Directory of Open Access Journals (Sweden)

    Mayumi Okamoto

    2014-09-01

    Full Text Available Nonessential tRNA modifications by methyltransferases are evolutionarily conserved and have been reported to stabilize mature tRNA molecules and prevent rapid tRNA decay (RTD. The tRNA modifying enzymes, NSUN2 and METTL1, are mammalian orthologs of yeast Trm4 and Trm8, which are required for protecting tRNA against RTD. A simultaneous overexpression of NSUN2 and METTL1 is widely observed among human cancers suggesting that targeting of both proteins provides a novel powerful strategy for cancer chemotherapy. Here, we show that combined knockdown of NSUN2 and METTL1 in HeLa cells drastically potentiate sensitivity of cells to 5-fluorouracil (5-FU whereas heat stress of cells revealed no effects. Since NSUN2 and METTL1 are phosphorylated by Aurora-B and Akt, respectively, and their tRNA modifying activities are suppressed by phosphorylation, overexpression of constitutively dephosphorylated forms of both methyltransferases is able to suppress 5-FU sensitivity. Thus, NSUN2 and METTL1 are implicated in 5-FU sensitivity in HeLa cells. Interfering with methylation of tRNAs might provide a promising rationale to improve 5-FU chemotherapy of cancer.

  20. Investigation of chemical modifiers for the determination of lead in fertilizers and limestone using graphite furnace atomic absorption spectrometry with Zeeman-effect background correction and slurry sampling

    Energy Technology Data Exchange (ETDEWEB)

    Borges, Aline R. [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq–INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Becker, Emilene M.; Dessuy, Morgana B. [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Vale, Maria Goreti R., E-mail: mgrvale@ufrgs.br [Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre, RS (Brazil); Instituto Nacional de Ciência e Tecnologia do CNPq–INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Welz, Bernhard [Instituto Nacional de Ciência e Tecnologia do CNPq–INCT de Energia e Ambiente, Universidade Federal da Bahia, Salvador, BA (Brazil); Departamento de Química, Universidade Federal de Santa Catarina, 88040-900 Florianópolis, SC (Brazil)

    2014-02-01

    In this work, chemical modifiers in solution (Pd/Mg, NH{sub 4}H{sub 2}PO{sub 4} and NH{sub 4}NO{sub 3}/Pd) were compared with permanent modifiers (Ir and Ru) for the determination of lead in fertilizer and limestone samples using slurry sampling and graphite furnace atomic absorption spectrometry with Zeeman-effect background correction. The analytical line at 283.3 nm was used due to some spectral interference observed at 217.0 nm. The NH{sub 4}H{sub 2}PO{sub 4} was abandoned due to severe spectral interference even at the 283.3-nm line. For Pd/Mg and NH{sub 4}NO{sub 3}/Pd the optimum pyrolysis and atomization temperatures were 900 °C and 1900 °C, respectively. For Ru and Ir, the integrated absorbance signal was stable up to pyrolysis temperatures of 700 °C and 900 °C, respectively, and up to atomization temperature of 1700 °C. The limit of detection (LOD) was 17 ng g{sup −1} using Pd/Mg and 29 ng g{sup −1} using NH{sub 4}NO{sub 3}/Pd. Among the permanent modifiers investigated, the LOD was 22 ng g{sup −1} Pb for Ir and 10 ng g{sup −1} Pb for Ru. The accuracy of the method was evaluated using the certified reference material NIST SRM 695. Although Ru provided lower LOD, which can be attributed to a lower blank signal, only the modifiers in solution showed concordant values of Pb concentration for the NIST SRM 695 and the most of analyzed samples. Moreover, the Pd/Mg modifier provided the highest sensitivity and for this reason it is more suitable for the determination of Pb in fertilizers samples in slurry; besides this it presented a better signal-to-noise ratio than NH{sub 4}NO{sub 3}/Pd. - Highlights: • Lead has been determined in fertilizers using slurry sampling GF AAS. • The mixture of palladium and magnesium nitrates was found to be the ideal chemical modifier. • Calibration could be carried out against aqueous standard solutions. • The proposed method is much faster than the EPA method, which includes sample digestion.

  1. Fabrication of gallium hexacyanoferrate modified carbon ionic liquid paste electrode for sensitive determination of hydrogen peroxide and glucose

    Energy Technology Data Exchange (ETDEWEB)

    Haghighi, Behzad, E-mail: haghighi@iasbs.ac.ir; Khosravi, Mehdi; Barati, Ali

    2014-07-01

    Gallium hexacyanoferrate (GaHCFe) and graphite powder were homogeneously dispersed into n-dodecylpyridinium hexafluorophosphate and paraffin to fabricate GaHCFe modified carbon ionic liquid paste electrode (CILPE). Mixture experimental design was employed to optimize the fabrication of GaHCFe modified CILPE (GaHCFe-CILPE). A pair of well-defined redox peaks due to the redox reaction of GaHCFe through one-electron process was observed for the fabricated electrode. The fabricated GaHCFe-CILPE exhibited good electrocatalytic activity towards reduction and oxidation of H{sub 2}O{sub 2}. The observed sensitivities for the electrocatalytic oxidation and reduction of H{sub 2}O{sub 2} at the operating potentials of + 0.8 and − 0.2 V were about 13.8 and 18.3 mA M{sup −1}, respectively. The detection limit (S/N = 3) for H{sub 2}O{sub 2} was about 1 μM. Additionally, glucose oxidase (GOx) was immobilized on GaHCFe-CILPE using two methodology, entrapment into Nafion matrix and cross-linking with glutaraldehyde and bovine serum albumin, in order to fabricate glucose biosensor. Linear dynamic rage, sensitivity and detection limit for glucose obtained by the biosensor fabricated using cross-linking methodology were 0.1–6 mM, 0.87 mA M{sup −1} and 30 μM, respectively and better than those obtained (0.2–6 mM, 0.12 mA M{sup −1} and 50 μM) for the biosensor fabricated using entrapment methodology. - Highlights: • Gallium hexacyanoferrate modified carbon ionic liquid paste electrode was fabricated. • Mixture experimental design was used to optimize electrode fabrication. • Response trace plot was used to show the effect of electrode materials on response. • The sensor exhibited electrocatalytic activity towards H{sub 2}O{sub 2} reduction and oxidation. • Glucose biosensor was fabricated by immobilization of glucose oxidase on sensor.

  2. Piezoelectric Sensor for Determination of Genetically Modified Soybean Roundup Readyâ in Samples not Amplified by PCR

    Directory of Open Access Journals (Sweden)

    Hanna Radecka

    2007-08-01

    Full Text Available The chemically modified piezoelectrodes were utilized to develop relativelycheap and easy to use biosensor for determination of genetically modified Roundup Readysoybean (RR soybean. The biosensor relies on the immobilization onto goldpiezoelectrodes of the 21-mer single stranded oligonucleotide (probes related to5-enolpyruvylshikimate-3-phosphate synthase (EPSPS gene, which is an active componentof an insert integrated into RR soybean genome. The hybridization reaction between theprobe and the target complementary sequence in solution was monitored. The system wasoptimized using synthetic oligonucleotides, which were applied for EPSPS gene detectionin DNA samples extracted from animal feed containing 30% RR soybean amplified by thePCR and nonamplified by PCR. The detection limit for genomic DNA was in the range of4.7·105 numbers of genom copies contained EPSPS gene in the QCM cell. The propertiessuch as sensitivity and selectivity of piezoelectric senor presented here indicated that it could be applied for the direct determination of genetically modified RR soybean in the samples non-amplified by PCR.

  3. Structure of a complex of uridine phosphorylase from Yersinia pseudotuberculosis with the modified bacteriostatic antibacterial drug determined by X-ray crystallography and computer analysis

    Energy Technology Data Exchange (ETDEWEB)

    Balaev, V. V.; Lashkov, A. A., E-mail: alashkov83@gmail.com; Gabdoulkhakov, A. G.; Seregina, T. A.; Dontsova, M. V.; Mikhailov, A. M. [Russian Academy of Sciences, Shubnikov Institute of Crystallography (Russian Federation)

    2015-03-15

    Pseudotuberculosis and bubonic plague are acute infectious diseases caused by the bacteria Yersinia pseudotuberculosis and Yersinia pestis. These diseases are treated, in particular, with trimethoprim and its modified analogues. However, uridine phosphorylases (pyrimidine nucleoside phosphorylases) that are present in bacterial cells neutralize the action of trimethoprim and its modified analogues on the cells. In order to reveal the character of the interaction of the drug with bacterial uridine phosphorylase, the atomic structure of the unligated molecule of uridine-specific pyrimidine nucleoside phosphorylase from Yersinia pseudotuberculosis (YptUPh) was determined by X-ray diffraction at 1.7 Å resolution with high reliability (R{sub work} = 16.2, R{sub free} = 19.4%; r.m.s.d. of bond lengths and bond angles are 0.006 Å and 1.005°, respectively; DPI = 0.107 Å). The atoms of the amino acid residues of the functionally important secondary-structure elements—the loop L9 and the helix H8—of the enzyme YptUPh were located. The three-dimensional structure of the complex of YptUPh with modified trimethoprim—referred to as 53I—was determined by the computer simulation. It was shown that 53I is a pseudosubstrate of uridine phosphorylases, and its pyrimidine-2,4-diamine group is located in the phosphate-binding site of the enzyme YptUPh.

  4. Tantalum electrodes modified with well-aligned carbon nanotube-Au nanoparticles: application to the highly sensitive electrochemical determination of cefazolin.

    Science.gov (United States)

    Fayazfar, Haniyeh; Afshar, Abdollah; Dolati, Abolghasem

    2014-07-01

    Carbon nanotube/nanoparticle hybrid materials have been proven to exhibit high electrocatalytic activity suggesting broad potential applications in the field of electroanalysis. For the first time, modification of Ta electrode with aligned multi-walled carbon nanotubes/Au nanoparticles introduced for the sensitive determination of the antibiotic drug, cefazolin (CFZ). The electrochemical response characteristics of the modified electrode toward CFZ were investigated by means of cyclic and linear sweep voltammetry. The modified electrode showed an efficient catalytic activity for the reduction of CFZ, leading to a remarkable decrease in reduction overpotential and a significant increase of peak current. Under optimum conditions, the highly sensitive modified electrode showed a wide linear range from 50 pM to 50 μM with a sufficiently low detection limit of 1 ± 0.01 pM (S/N = 3). The results indicated that the prepared electrode presents suitable characteristics in terms of sensitivity (458.2 ± 2.6 μAcm(-2)/μM), accuracy, repeatability (RSD of 1.8 %), reproducibility (RSD of 2.9 %), stability (14 days), and good catalytic activity in physiological conditions. The method was successfully applied for accurate determination of trace amounts of CFZ in pharmaceutical and clinical preparations without the necessity for samples pretreatment or any time-consuming extraction or evaporation steps prior to the analysis.

  5. Structure of a complex of uridine phosphorylase from Yersinia pseudotuberculosis with the modified bacteriostatic antibacterial drug determined by X-ray crystallography and computer analysis

    International Nuclear Information System (INIS)

    Balaev, V. V.; Lashkov, A. A.; Gabdoulkhakov, A. G.; Seregina, T. A.; Dontsova, M. V.; Mikhailov, A. M.

    2015-01-01

    Pseudotuberculosis and bubonic plague are acute infectious diseases caused by the bacteria Yersinia pseudotuberculosis and Yersinia pestis. These diseases are treated, in particular, with trimethoprim and its modified analogues. However, uridine phosphorylases (pyrimidine nucleoside phosphorylases) that are present in bacterial cells neutralize the action of trimethoprim and its modified analogues on the cells. In order to reveal the character of the interaction of the drug with bacterial uridine phosphorylase, the atomic structure of the unligated molecule of uridine-specific pyrimidine nucleoside phosphorylase from Yersinia pseudotuberculosis (YptUPh) was determined by X-ray diffraction at 1.7 Å resolution with high reliability (R work = 16.2, R free = 19.4%; r.m.s.d. of bond lengths and bond angles are 0.006 Å and 1.005°, respectively; DPI = 0.107 Å). The atoms of the amino acid residues of the functionally important secondary-structure elements—the loop L9 and the helix H8—of the enzyme YptUPh were located. The three-dimensional structure of the complex of YptUPh with modified trimethoprim—referred to as 53I—was determined by the computer simulation. It was shown that 53I is a pseudosubstrate of uridine phosphorylases, and its pyrimidine-2,4-diamine group is located in the phosphate-binding site of the enzyme YptUPh

  6. Structure of a complex of uridine phosphorylase from Yersinia pseudotuberculosis with the modified bacteriostatic antibacterial drug determined by X-ray crystallography and computer analysis

    Science.gov (United States)

    Balaev, V. V.; Lashkov, A. A.; Gabdoulkhakov, A. G.; Seregina, T. A.; Dontsova, M. V.; Mikhailov, A. M.

    2015-03-01

    Pseudotuberculosis and bubonic plague are acute infectious diseases caused by the bacteria Yersinia pseudotuberculosis and Yersinia pestis. These diseases are treated, in particular, with trimethoprim and its modified analogues. However, uridine phosphorylases (pyrimidine nucleoside phosphorylases) that are present in bacterial cells neutralize the action of trimethoprim and its modified analogues on the cells. In order to reveal the character of the interaction of the drug with bacterial uridine phosphorylase, the atomic structure of the unligated molecule of uridine-specific pyrimidine nucleoside phosphorylase from Yersinia pseudotuberculosis ( YptUPh) was determined by X-ray diffraction at 1.7 Å resolution with high reliability ( R work = 16.2, R free = 19.4%; r.m.s.d. of bond lengths and bond angles are 0.006 Å and 1.005°, respectively; DPI = 0.107 Å). The atoms of the amino acid residues of the functionally important secondary-structure elements—the loop L9 and the helix H8—of the enzyme YptUPh were located. The three-dimensional structure of the complex of YptUPh with modified trimethoprim—referred to as 53I—was determined by the computer simulation. It was shown that 53I is a pseudosubstrate of uridine phosphorylases, and its pyrimidine-2,4-diamine group is located in the phosphate-binding site of the enzyme YptUPh.

  7. Selective Determination of Serotonin on Poly(3,4-ethylenedioxy pyrrole)-single-walled Carbon Nanotube-Modified Glassy Carbon Electrodes

    International Nuclear Information System (INIS)

    Kim, Seul Ki; Bae, Si Ra; Ahmed, Mohammad Shamsuddin; You, Jung Min; Jeon, Seung Won

    2011-01-01

    An electrochemically-modified electrode [P(EDOP-SWNTs)/GCE] was prepared by electropolymerization of 3,4-ethylenedioxy pyrrole (EDOP) single-walled carbon nanotubes (SWNTs) on the surface of a glassy carbon electrode (GCE) and characterized by SEM, CV, and DPV. This modified electrode was employed as an electrochemical biosensor for the selective determination of serotonin concentrations at pH 7.4 and exhibited a typical enhanced effect on the current response of serotonin with a lower oxidation overpotential. The linear response was in the range of 1.0 x 10"-"7 to 1.0 x 10"-"5 M, with a correlation coefficient of 0.998 on the anodic current. The lower detection limit was calculated as 5.0 nM. Due to the relatively low currents and difference of potentials in the electrochemical responses of uric acid (UA), ascorbic acid (AA), and dopamine (DA), the modified electrode was a useful and effective sensing device for the selective and sensitive serotonin determination in the presence of UA, AA, and DA

  8. Selective Determination of Serotonin on Poly(3,4-ethylenedioxy pyrrole)-single-walled Carbon Nanotube-Modified Glassy Carbon Electrodes

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Seul Ki; Bae, Si Ra; Ahmed, Mohammad Shamsuddin; You, Jung Min; Jeon, Seung Won [Chonnam National University, Gwangju (Korea, Republic of)

    2011-04-15

    An electrochemically-modified electrode [P(EDOP-SWNTs)/GCE] was prepared by electropolymerization of 3,4-ethylenedioxy pyrrole (EDOP) single-walled carbon nanotubes (SWNTs) on the surface of a glassy carbon electrode (GCE) and characterized by SEM, CV, and DPV. This modified electrode was employed as an electrochemical biosensor for the selective determination of serotonin concentrations at pH 7.4 and exhibited a typical enhanced effect on the current response of serotonin with a lower oxidation overpotential. The linear response was in the range of 1.0 x 10{sup -7} to 1.0 x 10{sup -5} M, with a correlation coefficient of 0.998 on the anodic current. The lower detection limit was calculated as 5.0 nM. Due to the relatively low currents and difference of potentials in the electrochemical responses of uric acid (UA), ascorbic acid (AA), and dopamine (DA), the modified electrode was a useful and effective sensing device for the selective and sensitive serotonin determination in the presence of UA, AA, and DA.

  9. Dithizone-modified graphene oxide nano-sheet as a sorbent for pre-concentration and determination of cadmium and lead ions in food.

    Science.gov (United States)

    Moghadam Zadeh, Hamid Reza; Ahmadvand, Parvaneh; Behbahani, Ali; Amini, Mostafa M; Sayar, Omid

    2015-01-01

    Graphene oxide nano-sheet was modified with dithizone as a novel sorbent for selective pre-concentration and determination of Cd(II) and Pb(II) in food. The sorbent was characterised by various analytical methods and the effective parameters for Cd(II) and Pb(II) adsorption were optimised during this work. The high adsorption capacity and selectivity of this sorbent makes the method capable of fast determinations of the Cd(II) and Pb(II) content in complicated matrices even at μg l(-1) levels using commonly available instrumentation. The precision of this method was < 1.9% from 10 duplicate determinations and its accuracy verified using standard reference materials. Finally, this method was applied to the determination of Cd(II) and Pb(II) ions in common food samples and satisfactory results were obtained.

  10. Analytical determination of size-dependent natural frequencies of fully clamped rectangular microplates based on the modified couple stress theory

    Energy Technology Data Exchange (ETDEWEB)

    Askari, Amir R.; Tahani, Masoud [Ferdowsi University of Mashhad, Mashhad (Iran, Islamic Republic of)

    2015-05-15

    This paper presents an analytical and size-dependent model for vibrational analysis of fully clamped rectangular microplates. Modified couple stress theory (MCST) and the Kirchhoff plate model are considered, and Hamilton's principle is employed to derive the size dependent equation of motion that accounts for the effect of residual stresses. The natural frequencies of the microplate are extracted analytically by extended Kantorovich method. The present findings are validated with the available results in the literature, and an excellent agreement is observed between them. In addition, a parametric study is conducted to demonstrate the significant effects of couple stress components on the natural frequencies of fully clamped microplates. The ratio of MCST natural frequencies to those obtained with classical theory depends only on the Poisson's ratio of the plate and is independent of the aspect ratio of the plate for cases with no residual stresses.

  11. Analytical determination of size-dependent natural frequencies of fully clamped rectangular microplates based on the modified couple stress theory

    International Nuclear Information System (INIS)

    Askari, Amir R.; Tahani, Masoud

    2015-01-01

    This paper presents an analytical and size-dependent model for vibrational analysis of fully clamped rectangular microplates. Modified couple stress theory (MCST) and the Kirchhoff plate model are considered, and Hamilton's principle is employed to derive the size dependent equation of motion that accounts for the effect of residual stresses. The natural frequencies of the microplate are extracted analytically by extended Kantorovich method. The present findings are validated with the available results in the literature, and an excellent agreement is observed between them. In addition, a parametric study is conducted to demonstrate the significant effects of couple stress components on the natural frequencies of fully clamped microplates. The ratio of MCST natural frequencies to those obtained with classical theory depends only on the Poisson's ratio of the plate and is independent of the aspect ratio of the plate for cases with no residual stresses.

  12. Determinants of consumer attitudes and purchase intentions with regard to genetically modified foods: Results of a cross-national survey

    DEFF Research Database (Denmark)

    Bredahl, Lone

    2000-01-01

    purchasing the products, which were, in turn, significantly influenced by overall attitudes towards genetic modification in food production through their effects on beliefs that consumer hold about the quality and trustworthiness of the products. 6. The results clearly verify that consumer acceptance...... the results of a survey which was carried out in Denmark, Germany, Italy and the United Kingdom to investigate the formation of consumer attitudes towards genetic modification in food production and of purchase decisions with regard to genetically modified yoghurt and beer. Altogether, 2031 consumers were...... towards nature and attitude towards technology. These general attitudes were found to influence attitudes towards genetic modification through their impact on perceived risks and benefits of the technology. In Denmark, Germany and the United Kingdom, perceived risks of applying genetic modification...

  13. Reverse engineering of modified genes by Bayesian network analysis defines molecular determinants critical to the development of glioblastoma.

    Directory of Open Access Journals (Sweden)

    Brian W Kunkle

    Full Text Available In this study we have identified key genes that are critical in development of astrocytic tumors. Meta-analysis of microarray studies which compared normal tissue to astrocytoma revealed a set of 646 differentially expressed genes in the majority of astrocytoma. Reverse engineering of these 646 genes using Bayesian network analysis produced a gene network for each grade of astrocytoma (Grade I-IV, and 'key genes' within each grade were identified. Genes found to be most influential to development of the highest grade of astrocytoma, Glioblastoma multiforme were: COL4A1, EGFR, BTF3, MPP2, RAB31, CDK4, CD99, ANXA2, TOP2A, and SERBP1. All of these genes were up-regulated, except MPP2 (down regulated. These 10 genes were able to predict tumor status with 96-100% confidence when using logistic regression, cross validation, and the support vector machine analysis. Markov genes interact with NFkβ, ERK, MAPK, VEGF, growth hormone and collagen to produce a network whose top biological functions are cancer, neurological disease, and cellular movement. Three of the 10 genes - EGFR, COL4A1, and CDK4, in particular, seemed to be potential 'hubs of activity'. Modified expression of these 10 Markov Blanket genes increases lifetime risk of developing glioblastoma compared to the normal population. The glioblastoma risk estimates were dramatically increased with joint effects of 4 or more than 4 Markov Blanket genes. Joint interaction effects of 4, 5, 6, 7, 8, 9 or 10 Markov Blanket genes produced 9, 13, 20.9, 26.7, 52.8, 53.2, 78.1 or 85.9%, respectively, increase in lifetime risk of developing glioblastoma compared to normal population. In summary, it appears that modified expression of several 'key genes' may be required for the development of glioblastoma. Further studies are needed to validate these 'key genes' as useful tools for early detection and novel therapeutic options for these tumors.

  14. From Bolam-Bolitho to Modified-Montgomery - A Paradigm Shift in the Legal Standard of Determining Medical Negligence in Singapore.

    Science.gov (United States)

    Neo, Han Yee

    2017-09-01

    In a recent landmark litigation, the Singapore Court of Appeal introduced a new legal standard for determining medical negligence with regards to information disclosure - the Modified-Montgomery test. This new test fundamentally shifts the legal position concerning the standard of care expected of a doctor when he dispenses medical advice. Previously, a doctor is expected to disclose what a "reasonable physician" would tell his patient. Now, a doctor must disclose "all material risks" that a "reasonable patient" would want to know under his unique circumstances. Patient-centred communication is no longer an aspirational ideal but has become a legal mandate. Manpower, administrative, logistic and medical educational reforms should start now, so as to support the average physician transit from the era of the Bolam-Bolitho, to that of the Modified-Montgomery.

  15. Electrocatalytic determination of L-ascorbic acid by modified glassy carbon with Ni(Me2(CH3CO)2[14]tetraenoN4) complex.

    Science.gov (United States)

    Khorasani-Motlagh, Mozhgan; Noroozifar, Meissam

    2003-12-01

    A novel modified glassy carbon electrode containing Ni(Me2(CH3CO)2[14]tetraenoN4) complex was used as an electrocatalytic sensor for the determination of L-ascorbic acid in pH = 6.6. The peak potential shifted to negative by 205 mV compared with that for a bare electrode in cyclic voltammograms. The calibration curve was linear up to 6.2 x 10(-3) M with a detection limit 3.1 x 10(-7) M and an RSD% better than 2.47%. This newly modified electrode was applied to commercial pharmaceutical tablets, injections and foods. The obtained results were identical to those obtained by the classical 2,6-dichlorophenolindophenol method.

  16. Amperometric determination of 6-mercaptopurine on functionalized multi-wall carbon nanotubes modified electrode by liquid chromatography coupled with microdialysis and its application to pharmacokinetics in rabbit.

    Science.gov (United States)

    Cao, Xu-Ni; Lin, Li; Zhou, Yu-Yan; Shi, Guo-Yue; Zhang, Wen; Yamamoto, Katsunobu; Jin, Li-Tong

    2003-07-27

    In this paper, multi-wall carbon nanotubes functionalized with carboxylic groups modified electrode (MWNT-COOH CME) was fabricated. This chemically modified electrode (CME) can be used as the working electrode in the liquid chromatography for the determination of 6-mercaptopurine (6-MP). The results indicate that the CME exhibits efficiently electrocatalytic oxidation for 6-MP with relatively high sensitivity, stability and long-life. The peak currents of 6-MP are linear to its concentrations ranging from 4.0 x 10(-7) to 1.0 x 10(-4) mol l(-1) with the calculated detection limit (S/N=3) of 2.0 x 10(-7) mol l(-1). Coupled with microdialysis, the method has been successfully applied to the pharmacokinetic study of 6-MP in rabbit blood. This method provides a fast, sensible and simple technique for the pharmacokinetic study of 6-MP in vivo.

  17. Very sensitive electrochemical determination of diuron on glassy carbon electrode modified with reduced graphene oxide-gold nanoparticle-Nafion composite film.

    Science.gov (United States)

    Zarei, K; Khodadadi, A

    2017-10-01

    In this work, a very sensitive electrochemical sensor based on glassy carbon electrode (GCE) modified with reduced graphene oxide-gold nanoparticles/Nafion (rGO-AuNPs/Nafion) composite film was applied to determine diuron. Synthesized GO was characterized using X-ray diffraction (XRD) and UV-visible spectroscopy. The surface morphology of the rGO-AuNPs/Nafion film was also characterized using scanning electron microscopy and electrochemical impedance spectroscopy. Cyclic voltammetry (CV) and adsorptive differential pulse voltammetry (AdDPV) were applied to investigate the electrochemical response of the diuron on the modified electrode. The electrode showed a linear response at 1.0×10 -9 -1.0×10 -7 M and a detection limit of 0.3nM under the optimized conditions. The effect of some other species on the determination of diuron was investigated and the sensor showed good selectivity for determination of diuron. The constructed sensor was applied to determine diuron in enriched samples of orange juice, mineral and tap water which statistical t-test showed accuracy of method. Also the sensor was applied to obtain diuron content in the tea sample. The reliability of the proposed sensor was confirmed after comparing the results with those obtained using high performance liquid chromatography (HPLC) as a comparative method. Copyright © 2017 Elsevier Inc. All rights reserved.

  18. Modified carbon nanotubes as a sorbent for solid-phase extraction of gold, and its determination by graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Moghaddam, Firouzeh Hassani; Behzadi, Mansoureh; Naghizadeh, Matin; Taher, Mohammad Ali

    2015-01-01

    A simple, sensitive and accurate method was developed for solid-phase extraction and preconcentration of trace levels of gold in various samples. It is based on the adsorption of gold on modified oxidized multi-walled carbon nanotubes prior to its determination by graphite furnace atomic absorption spectrometry. The type and volume of eluent solution, sample pH value, flow rates of sample and eluent, sorption capacity and breakthrough volume were optimized. Under these conditions, the method showed linearity in the range of 0.2–6.0 ng L −1 with coefficients of determination of >0.99 in the sample. The relative standard deviation for seven replicate determinations of gold (at a level of 0.6 ng L −1 ) is ±3.8 %, the detection limit is 31 pg L −1 (in the initial solution and at an S/N ratio of 3; for n = 8), and the enrichment factor is 200. The sorption capacity of the modified MWCNTs for gold(III) is 4.15 mg g −1 . The procedure was successfully applied to the determination of gold in (spiked) water samples, human hair, human urine and standard reference material with recoveries ranging from 97.0 to 104.2 %. (author)

  19. A novel disposable electrochemical sensor for determination of carbamazepine based on Fe doped SnO{sub 2} nanoparticles modified screen-printed carbon electrode

    Energy Technology Data Exchange (ETDEWEB)

    Lavanya, N. [Department of Biosensors and Bioelectronics, Alagappa University, Karaikudi 630003, TN (India); Department of Electronic Engineering, Chemistry and Materials Engineering, University of Messina, Messina 98166 (Italy); Sekar, C., E-mail: Sekar2025@gmail.com [Department of Biosensors and Bioelectronics, Alagappa University, Karaikudi 630003, TN (India); Ficarra, S.; Tellone, E. [Department of Chemical Sciences, University of Messina, Messina 98166 (Italy); Bonavita, A.; Leonardi, S.G.; Neri, G. [Department of Electronic Engineering, Chemistry and Materials Engineering, University of Messina, Messina 98166 (Italy)

    2016-05-01

    An effective strategy to fabricate a novel disposable screen printing carbon electrode modified by iron doped tin dioxide nanoparticles for carbamazepine (CBZ) detection has been developed. Fe–SnO{sub 2} (Fe = 0 to 5 wt.%) NPs were synthesized by a simple microwave irradiation method and assessed for their structural and morphological changes due to Fe doping into SnO{sub 2} matrix by X-ray diffraction and scanning and transmission electron microscopy. The electrochemical behaviour of carbamazepine at the Fe–SnO{sub 2} modified screen printed carbon electrode (SPCE) was investigated by cyclic voltammetry and square wave voltammetry. Electron transfer coefficient α (0.63) and electron transfer rate constant k{sub s} (0.69 s{sup −1}) values of the 5 wt.% Fe–SnO{sub 2} modified SPCE indicate that the diffusion controlled process takes place on the electrode surface. The fabricated sensor displayed a good electrooxidation response towards the detection of CBZ at a lower oxidation potential of 0.8 V in phosphate buffer solution at pH 7.0. Under the optimal conditions, the sensor showed fast and sensitive current response to CBZ over a wide linear range of 0.5–100 μM with a low detection limit of 92 nM. Furthermore, the practical application of the modified electrode has been investigated by the determination of CBZ in pharmaceutical products using standard addition method. - Highlights: • A novel mediator-free disposable screen printed carbon electrode has been fabricated based on Fe- SnO{sub 2} nanoparticles for determination of carbamazepine • The Fe-SnO{sub 2}/SPCE showed wide linear range (0.5–100 μM), low detection limit (92 nM), high sensitivity, good stability and reproducibility. • The carbamazepine sensor was successfully applied to the analysis of pharmaceutical products with satisfactory recoveries.

  20. Voltammetric determination of ultratrace levels of cerium(III) using a carbon paste electrode modified with nano-sized cerium-imprinted polymer and multiwalled carbon nanotubes

    International Nuclear Information System (INIS)

    Alizadeh, Taher; Ganjali, Mohammad Reza; Akhoundian, Maede; Norouzi, Parviz

    2016-01-01

    A carbon paste electrode was modified with a Ce(III)-imprinted polymer (Ce-IP) and used for voltammetric determination of Ce(III) ions in real water samples. Precipitation polymerization was used for synthesis of the nano-sized Ce-IP from vinylpyridine and methacrylic acid (acting as the complexing ligands and functional monomers), divinylbenzene (cross-linker) and AIBN as the radical starter. The Ce-IP was characterized by scanning electron microscopy and zeta potentials. A carbon paste electrode (CPE) was then impregnated with the Ce-IP and used for the extraction and subsequent determination of Ce(III). Oxidative square wave voltammetry showed the electrode to give a significantly better response than an electrode modified with the non-imprinted polymer. The addition of multiwalled carbon nanotubes to the Ce-IP-modified electrode further improves the signal, thereby increasing the sensitivity of the method. The effects of electrode composition, extraction pH value, volume and time were optimized. The electrode, if operated at a voltage of 1.05 V (vs. Ag/AgCl), displays a linear response to Ce(III) in the 1.0 μM to 25 pM concentration range, and the detection limit is 10 pM (at an S/N ratio of 3). The relative standard deviation of 5 separate determinations is 3.1 %. The method was successfully applied to the determination of Ce(III) in the spiked samples of drinking water and sea water. (author)

  1. Electrocatalytic simultaneous determination of ascorbic acid, uric acid and L–Cysteine in real samples using quercetin silver nanoparticles–graphene nanosheets modified glassy carbon electrode

    Energy Technology Data Exchange (ETDEWEB)

    Zare, Hamid R., E-mail: hrzare@yazd.ac.ir; Jahangiri-Dehaghani, Fahime; Shekari, Zahra; Benvidi, Ali

    2016-07-01

    Highlights: • Quercetin AgNPs graphene nanosheets modified GCE (Q–AgNPs–GNs–GCE) was prepared as a new sensor. • Q–AgNPs–GNs–GCE shows a high catalytic activity for L–Cysteine (L–Cys) oxidation. • In DPV, the calibration plots were linear within two ranges of 0.9–12.4 μM and 12.4–538.5 μM of L–Cys. • The proposed modified electrode is used for the simultaneous determinations of AA, UA and L–Cys. • Q–AgNPs–GNs–GCE was satisfactorily used for the determination of AA, UA and L–Cys in real samples. - Abstract: By immobilizing of quercetin at the surface of a glassy carbon electrode modified with silver nanoparticles and graphene nanosheets (Q–AgNPs–GNs–GCE) a new sensor has been fabricated. The cyclic voltammogram of Q–AgNPs–GNs–GCE shows a stable redox couple with surface confined characteristics. Q–AgNPs–GNs–GCE demonstrated a high catalytic activity for L–Cysteine (L–Cys) oxidation. Results indicated that L–Cys peak potential at Q–AgNPs–GNs–GCE shifted to less positive values compared to GNs–GCE or AgNPs–GCE. Also, the kinetic parameters such as the electron transfer coefficient,, and the heterogeneous electron transfer rate constant, k′, for the oxidation of L–Cys at the Q–AgNPs–GNs–GCE surface were estimated. In differential pulse voltammetric determination, the detection limit of L–Cys was obtained 0.28 μM, and the calibration plots were linear within two ranges of 0.9–12.4 μM and 12.4–538.5 μM of L–Cys. Also, the proposed modified electrode is used for the simultaneous determinations of ascorbic acid (AA), uric acid (UA), and L–Cys. Finally, this study has demonstrated the practical analytical utility of the sensor for determination of AA in vitamin C tablet, L–Cys in a milk sample and UA in a human urine sample.

  2. Electrocatalytic simultaneous determination of ascorbic acid, uric acid and L–Cysteine in real samples using quercetin silver nanoparticles–graphene nanosheets modified glassy carbon electrode

    International Nuclear Information System (INIS)

    Zare, Hamid R.; Jahangiri-Dehaghani, Fahime; Shekari, Zahra; Benvidi, Ali

    2016-01-01

    Highlights: • Quercetin AgNPs graphene nanosheets modified GCE (Q–AgNPs–GNs–GCE) was prepared as a new sensor. • Q–AgNPs–GNs–GCE shows a high catalytic activity for L–Cysteine (L–Cys) oxidation. • In DPV, the calibration plots were linear within two ranges of 0.9–12.4 μM and 12.4–538.5 μM of L–Cys. • The proposed modified electrode is used for the simultaneous determinations of AA, UA and L–Cys. • Q–AgNPs–GNs–GCE was satisfactorily used for the determination of AA, UA and L–Cys in real samples. - Abstract: By immobilizing of quercetin at the surface of a glassy carbon electrode modified with silver nanoparticles and graphene nanosheets (Q–AgNPs–GNs–GCE) a new sensor has been fabricated. The cyclic voltammogram of Q–AgNPs–GNs–GCE shows a stable redox couple with surface confined characteristics. Q–AgNPs–GNs–GCE demonstrated a high catalytic activity for L–Cysteine (L–Cys) oxidation. Results indicated that L–Cys peak potential at Q–AgNPs–GNs–GCE shifted to less positive values compared to GNs–GCE or AgNPs–GCE. Also, the kinetic parameters such as the electron transfer coefficient,, and the heterogeneous electron transfer rate constant, k′, for the oxidation of L–Cys at the Q–AgNPs–GNs–GCE surface were estimated. In differential pulse voltammetric determination, the detection limit of L–Cys was obtained 0.28 μM, and the calibration plots were linear within two ranges of 0.9–12.4 μM and 12.4–538.5 μM of L–Cys. Also, the proposed modified electrode is used for the simultaneous determinations of ascorbic acid (AA), uric acid (UA), and L–Cys. Finally, this study has demonstrated the practical analytical utility of the sensor for determination of AA in vitamin C tablet, L–Cys in a milk sample and UA in a human urine sample.

  3. Reverse Engineering of Modified Genes by Bayesian Network Analysis Defines Molecular Determinants Critical to the Development of Glioblastoma

    Science.gov (United States)

    Kunkle, Brian W.; Yoo, Changwon; Roy, Deodutta

    2013-01-01

    In this study we have identified key genes that are critical in development of astrocytic tumors. Meta-analysis of microarray studies which compared normal tissue to astrocytoma revealed a set of 646 differentially expressed genes in the majority of astrocytoma. Reverse engineering of these 646 genes using Bayesian network analysis produced a gene network for each grade of astrocytoma (Grade I–IV), and ‘key genes’ within each grade were identified. Genes found to be most influential to development of the highest grade of astrocytoma, Glioblastoma multiforme were: COL4A1, EGFR, BTF3, MPP2, RAB31, CDK4, CD99, ANXA2, TOP2A, and SERBP1. All of these genes were up-regulated, except MPP2 (down regulated). These 10 genes were able to predict tumor status with 96–100% confidence when using logistic regression, cross validation, and the support vector machine analysis. Markov genes interact with NFkβ, ERK, MAPK, VEGF, growth hormone and collagen to produce a network whose top biological functions are cancer, neurological disease, and cellular movement. Three of the 10 genes - EGFR, COL4A1, and CDK4, in particular, seemed to be potential ‘hubs of activity’. Modified expression of these 10 Markov Blanket genes increases lifetime risk of developing glioblastoma compared to the normal population. The glioblastoma risk estimates were dramatically increased with joint effects of 4 or more than 4 Markov Blanket genes. Joint interaction effects of 4, 5, 6, 7, 8, 9 or 10 Markov Blanket genes produced 9, 13, 20.9, 26.7, 52.8, 53.2, 78.1 or 85.9%, respectively, increase in lifetime risk of developing glioblastoma compared to normal population. In summary, it appears that modified expression of several ‘key genes’ may be required for the development of glioblastoma. Further studies are needed to validate these ‘key genes’ as useful tools for early detection and novel therapeutic options for these tumors. PMID:23737970

  4. Distal biceps brachii tendon repair: a systematic review of patient outcome determination using modified Coleman methodology score criteria.

    Science.gov (United States)

    Nyland, John; Causey, Brandon; Wera, Jeff; Krupp, Ryan; Tate, David; Gupta, Amit

    2017-07-01

    This systematic literature review evaluated the methodological research design quality of studies that evaluated patient outcomes following distal biceps brachii tendon repair and developed evidence-based recommendations for future patient clinical outcomes research. Following the preferred reporting items for systematic reviews and meta-analyses criteria, and using "biceps brachii", "tendon", "repair" and "outcome assessment" search terms, the CINAHL, Academic Search Premier and MEDLINE databases were searched from January 1960-October 2015. The modified Coleman methodology score (MCMS) served as the primary outcome measure. Descriptive statistical analysis was performed for composite and component MCMS and for patient outcome assessment methodology use frequency. A total of 93 studies were evaluated. Overall MCMS was low (57.1 ± 14). Only 12 (12.9 %) had prospective cohort or randomized controlled trial designs. There was a moderate relationship between publication year and MCMS (r = 0.53, P research study methodological scores improved on average since 2008, generally low MCMS scores, retrospective designs, lack of eccentric elbow flexor or supinator strength testing, and poorly described surgical and rehabilitation descriptions remain commonplace. These findings decrease clinical study validity and generalizability. III.

  5. Flanking sequence determination and event-specific detection of genetically modified wheat B73-6-1.

    Science.gov (United States)

    Xu, Junyi; Cao, Jijuan; Cao, Dongmei; Zhao, Tongtong; Huang, Xin; Zhang, Piqiao; Luan, Fengxia

    2013-05-01

    In order to establish a specific identification method for genetically modified (GM) wheat, exogenous insert DNA and flanking sequence between exogenous fragment and recombinant chromosome of GM wheat B73-6-1 were successfully acquired by means of conventional polymerase chain reaction (PCR) and thermal asymmetric interlaced (TAIL)-PCR strategies. Newly acquired exogenous fragment covered the full-length sequence of transformed genes such as transformed plasmid and corresponding functional genes including marker uidA, herbicide-resistant bar, ubiquitin promoter, and high-molecular-weight gluten subunit. The flanking sequence between insert DNA revealed high similarity with Triticum turgidum A gene (GenBank: AY494981.1). A specific PCR detection method for GM wheat B73-6-1 was established on the basis of primers designed according to the flanking sequence. This specific PCR method was validated by GM wheat, GM corn, GM soybean, GM rice, and non-GM wheat. The specifically amplified target band was observed only in GM wheat B73-6-1. This method is of high specificity, high reproducibility, rapid identification, and excellent accuracy for the identification of GM wheat B73-6-1.

  6. Voltammetric determination of bisphenol A in food package by a glassy carbon electrode modified with carboxylated multi-walled carbon nanotubes

    International Nuclear Information System (INIS)

    Li, J.; Kuang, D.; Feng, Y.; Zhang, F.; Liu, M.

    2011-01-01

    A highly sensitive and mercury-free method for determination of bisphenol A (BPA) was established using a glassy carbon electrode that was modified with carboxylated multi-walled carbon nanotubes. A sensitive oxidation peak is found at 550 mV in linear sweep voltammograms at pH 7. Based on this finding, trace levels of bisphenol A can be determined over a concentration range that is linear from 10 nM to 104 nM, the correlation coefficient being 0.9983, and the detection limit (S/N = 3) being 5.0 nM. The method was successfully applied to the determination of BPA in food package. (author)

  7. Determination of multiple pesticides in fruits and vegetables using a modified quick, easy, cheap, effective, rugged and safe method with magnetic nanoparticles and gas chromatography tandem mass spectrometry.

    Science.gov (United States)

    Li, Yan-Fei; Qiao, Lu-Qin; Li, Fang-Wei; Ding, Yi; Yang, Zi-Jun; Wang, Ming-Lin

    2014-09-26

    Based on a modified quick, easy, cheap, effective, rugged and safe (QuEChERS) sample preparation method with Fe3O4 magnetic nanoparticles (MNPs) as the adsorbing material and gas chromatography-tandem mass spectrometry (GC-MS/MS) determination in multiple reaction monitoring (MRM) mode, we established a new method for the determination of multiple pesticides in vegetables and fruits. It was determined that bare MNPs have excellent function as adsorbent when purified, and it is better to be separated from the extract. The amount of MNPs influenced the clean-up performance and recoveries. To achieve the optimum performance of modified QuEChERS towards the target analytes, several parameters including the amount of the adsorbents and purification time were investigated. Under the optimum conditions, recoveries were evaluated in four representative matrices (tomato, cucumber, orange and apple) with the spiked concentrations of 10 μg kg(-1), 50 μg kg(-1)and 200 μg kg(-1) in all cases. The results showed that the recovery of 101 pesticides ranged between 71.5 and 111.7%, and the relative standard deviation was less than 10.5%. The optimum clean-up system improved the purification efficiency and simultaneously obtained satisfactory recoveries of multiple pesticides, including planar-ring pesticides. In short, the modified QuEChERS method in addition to MNPs used for removing impurities improved the speed of sample pre-treatment and exhibited an enhanced performance and purifying effect. Copyright © 2014 Elsevier B.V. All rights reserved.

  8. An aptasensor for voltammetric and impedimetric determination of cocaine based on a glassy carbon electrode modified with platinum nanoparticles and using rutin as a redox probe

    International Nuclear Information System (INIS)

    Roushani, Mahmoud; Shahdost-fard, Faezeh

    2016-01-01

    We describe a method for the determination of cocaine that is based on a glassy carbon electrode modified with a nanocomposite consisting of multiwalled carbon nanotubes, an ionic liquid, and chitosan. The electrode was made cocaine-responsive by immobilizing a cocaine-specific aptamer and platinum nanoparticles (PtNPs) on the modified electrode. The use of PtNPs resulted in the acceleration of the electron transfer kinetics of the reduction of the redox probe rutin and enhances sensitivity. The sensor, best operated at a working voltage of 260 mV vs. Ag/AgCl, has a linear response to cocaine in the 1 nM to 11 μM concentration range, and the detection limit is 100 pM (at an S/N ratio of 3). We think this strategy to represent a promising platform for the sensitive and selective determination of cocaine. The sensor is adequately stable and was successfully applied to the determination of cocaine in spiked serum. (author)

  9. An electrochemical sensor for rizatriptan benzoate determination using Fe3O4 nanoparticle/multiwall carbon nanotube-modified glassy carbon electrode in real samples.

    Science.gov (United States)

    Madrakian, Tayyebeh; Maleki, Somayeh; Heidari, Mozhgan; Afkhami, Abbas

    2016-06-01

    In this paper a sensitive and selective electrochemical sensor for determination of rizatriptan benzoate (RZB) was proposed. A glassy carbon electrode was modified with nanocomposite of multiwalled carbon nanotubes (MWCNTs) and Fe3O4 nanoparticles (Fe3O4/MWCNTs/GCE). The results obtained clearly show that the combination of MWCNTs and Fe3O4 nanoparticles definitely improves the sensitivity of modified electrode to RZB determination. The morphology and electroanalytical performance of the fabricated sensor were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS), square wave voltammetry (SWV) and cyclic voltammetry (CV). Also, the effect of experimental and instrumental parameters on the sensor response was evaluated. The square wave voltammetric response of the electrode to RZB was linear in the range 0.5-100.0 μmol L(-1) with a detection limit of 0.09 μmol L(-1) under the optimum conditions. The investigated method showed good stability, reproducibility and repeatability. The proposed sensor was successfully applied for real life samples of blood serum and RZB determination in pharmaceutical. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Electrocatalytic simultaneous determination of ascorbic acid, uric acid and L-Cysteine in real samples using quercetin silver nanoparticles-graphene nanosheets modified glassy carbon electrode

    Science.gov (United States)

    Zare, Hamid R.; Jahangiri-Dehaghani, Fahime; Shekari, Zahra; Benvidi, Ali

    2016-07-01

    By immobilizing of quercetin at the surface of a glassy carbon electrode modified with silver nanoparticles and graphene nanosheets (Q-AgNPs-GNs-GCE) a new sensor has been fabricated. The cyclic voltammogram of Q-AgNPs-GNs-GCE shows a stable redox couple with surface confined characteristics. Q-AgNPs-GNs-GCE demonstrated a high catalytic activity for L-Cysteine (L-Cys) oxidation. Results indicated that L-Cys peak potential at Q-AgNPs-GNs-GCE shifted to less positive values compared to GNs-GCE or AgNPs-GCE. Also, the kinetic parameters such as the electron transfer coefficient,, and the heterogeneous electron transfer rate constant, k‧, for the oxidation of L-Cys at the Q-AgNPs-GNs-GCE surface were estimated. In differential pulse voltammetric determination, the detection limit of L-Cys was obtained 0.28 μM, and the calibration plots were linear within two ranges of 0.9-12.4 μM and 12.4-538.5 μM of L-Cys. Also, the proposed modified electrode is used for the simultaneous determinations of ascorbic acid (AA), uric acid (UA), and L-Cys. Finally, this study has demonstrated the practical analytical utility of the sensor for determination of AA in vitamin C tablet, L-Cys in a milk sample and UA in a human urine sample.

  11. Simultaneous determination of Cd(II) and Pb(II) by differential pulse anodic stripping voltammetry based on graphite nanofibers-Nafion composite modified bismuth film electrode.

    Science.gov (United States)

    Li, Dongyue; Jia, Jianbo; Wang, Jianguo

    2010-12-15

    A bismuth-film modified graphite nanofibers-Nafion glassy carbon electrode (BiF/GNFs-NA/GCE) was constructed for the simultaneous determination of trace Cd(II) and Pb(II). The electrochemical properties and applications of the modified electrode were studied. Operational parameters such as deposition potential, deposition time, and bismuth ion concentration were optimized for the purpose of determination of trace metal ions in 0.10 M acetate buffer solution (pH 4.5). Under optimal conditions, based on three times the standard deviation of the baseline, the limits of detection were 0.09 μg L(-1) for Cd(II) and 0.02 μg L(-1) for Pb(II) with a 10 min preconcentration. In addition, the BiF/GNFs-NA/GCE displayed good reproducibility and selectivity, making it suitable for the simultaneous determination of Cd(II) and Pb(II) in real sample such as river water and human blood samples. Copyright © 2010 Elsevier B.V. All rights reserved.

  12. Simultaneous determination of caffeine and paracetamol by square wave voltammetry at poly(4-amino-3-hydroxynaphthalene sulfonic acid)-modified glassy carbon electrode.

    Science.gov (United States)

    Tefera, Molla; Geto, Alemnew; Tessema, Merid; Admassie, Shimelis

    2016-11-01

    Poly(4-amino-3-hydroxynaphthalene sulfonic acid)-modified glassy carbon electrode (poly(AHNSA)/GCE) was prepared for simultaneous determination of caffeine and paracetamol using square-wave voltammetry. The method was used to study the effects of pH and scan rate on the voltammetric response of caffeine and paracetamol. Linear calibration curves in the range of 10-125μM were obtained for both caffeine and paracetamol in acetate buffer solution of pH 4.5 with a correlation coefficient of 0.9989 and 0.9986, respectively. The calculated detection limits (S/N=3) were 0.79μM for caffeine and 0.45μM for paracetamol. The effects of some interfering substances in the determination of caffeine and paracetamol were also studied and their interferences were found to be negligible which proved the selectivity of the modified electrode. The method was successfully applied for the quantitative determination of caffeine and paracetamol in Coca-Cola, Pepsi-Cola and tea samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

  13. Penicillamine-modified sensor for the voltammetric determination of Cd(II) and Pb(II) ions in natural samples.

    Science.gov (United States)

    Pérez-Ràfols, Clara; Serrano, Núria; Díaz-Cruz, José Manuel; Ariño, Cristina; Esteban, Miquel

    2015-11-01

    A new penicillamine-GCE was developed based on the immobilization of d-penicillamine on aryl diazonium salt monolayers anchored to the glassy carbon electrode (GCE) surface and it was applied for the first time to the simultaneous determination of Cd(II) and Pb(II) ions by stripping voltammetric techniques. The detection and quantification limits at levels of µg L(-1) suggest that the penicillamine-GCE could be fully suitable for the determination of the considered ions in natural samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. Solid Phase Extraction of Trace Copper in Aqueous Samples Using C18 Membrane Disks Modified by Benzildithiosemicarbazone Prior to Flame Atomic Absorption Spectrometric (FAAS Determination

    Directory of Open Access Journals (Sweden)

    M. Mohammadhosseini

    2013-08-01

    Full Text Available A highly convenient, selective and sensitive procedure for pre-concentration, separation and determination of sub-ppm levels of Cu2+ in aqueous samples based on modification of octadecyl silica bonded phase membrane (OSBPM disks is described using benzildithiosemicarbazone  (BDSC as a powerful modifier. It was revealed that each loaded OSBPM disk with 6.0 mg of BDSC serves as excellent bead for trapping, enrichment and isolation of trace copper. The analyte was trapped during introduction the aqueous solutions through the surface of each modified membrane, quantitatively, while other interfering ions passed through the disk to drain. The adsorbed Cu2+ ions were then stripped by appropriate eluting agents followed by monitoring of the eluates by FAAS. The effects of sample pH, amount of the modifier, stripping agent types and sample flow-rates were also investigated. The described method permitted a pre-concentration factor of about 200. The detection limit of the procedure was predicted to be about 0.013 ng L-1. The method was successfully employed for recovery and quantification of trace copper in different water samples. 

  15. Highly selective determination of dopamine in the presence of ascorbic acid and serotonin at glassy carbon electrodes modified with carbon nanotubes dispersed in polyethylenimine.

    Science.gov (United States)

    Rodríguez, Marcela C; Rubianes, María D; Rivas, Gustavo A

    2008-11-01

    We report the highly selective and sensitive voltammetric dopamine quantification in the presence of ascorbic acid and serotonin by using glassy carbon electrodes modified with a dispersion of multi-wall carbon nanotubes (MWCNT) in polyethylenimine, PEI (GCE/MWCNT-PEI). The electrocatalytic activity of the MWCNT deposited on the glassy carbon electrode has allowed an important decrease in the overvoltages for the oxidation of ascorbic acid and dopamine, making possible a clear definition of dopamine, serotonin and ascorbic acid oxidation processes. The sensitivities for dopamine in the presence and absence of 1.0 mM ascorbic acid and serotonin were (2.18 +/- 0.03) x 10(5) microAM(-1) (r = 0.9998); and (2.10 +/- 0.07) x 10(5) miroAM(-1) (r=0.9985), respectively, demonstrating the excellent performance of the GCE/MWCNT-PEI. The detection limit for dopamine in the mixture was 9.2 x 10(-7) M. The R. S. D. for the determination of 50 microM dopamine using four different electrodes was 3.9% when modified with the same MWCNT/PEI dispersion, and 4.6% when using four different dispersions. The modified electrode has been successfully applied for recovery assays of dopamine in human blood serum. Therefore, the new sensor represents an interesting and promising alternative for the electrochemical quantification of neurotransmitters and other analytes of clinical interest.

  16. Determination of the major tautomeric form of the covalently modified adenine in the (+)-CC-1065-DNA adduct by 1H and 15N NMR studies

    International Nuclear Information System (INIS)

    Lin, Chin Hsiung; Hurley, L.H.

    1990-01-01

    (+)-CC-1065 is an extremely potent antitumor antibiotic produced by Streptomyces zelensis. The potent cytotoxic effects of the drug are thought to be due to the formation of a covalent adduct with DNA through N3 of adenine. Although the covalent linkage sites between (+)-CC-1065 and DNA have been determined, the tautomeric form of the covalently modified adenine in the (+)-CC-1065-DNA duplex adduct was not defined. The [6- 15 N]deoxyadenosine-labeled 12-mer duplex adduct was then studied by 1 H and 15 N NMR. One-dimensional NOE difference and two-dimensional NOESY 1 H NMR experiments on the nonisotopically labeled 12-mer duplex adduct demonstrate that the 6-amino protons of the covalently modified adenine exhibit two signals at 9.19 and 9.08 ppm. Proton NMR experiments on the [6- 15 N]deoxyadenosine-labeled 12-mer duplex adduct show that the two resonance signals for adenine H6 observed on the nonisotopically labeled duplex adduct were split into doublets by the 15 N nucleus with coupling constants of 91.3 Hz for non-hydrogen-bonded and 86.8 Hz for hydrogen-bonded amino protons. The authors conclude that the covalently modified adenine N6 of the (+)-CC-1065-12-mer duplex adduct is predominantly in the doubly protonated form, in which calculations predict that the C6-N6 bond is shortened and the positive charge is delocalized over the entire adenine molecule

  17. Voltammetric Study of the Copper Pentacyanonitrosylferrate Adsorbed on the Silica Modified with a Poly(propyleneimine Hexadecylamine Dendrimer for Determination of Nitrite

    Directory of Open Access Journals (Sweden)

    D. R. do Carmo

    2012-01-01

    Full Text Available Poly(propyleneimine hexadecylamine dendrimer (DAB-Am-16 was anchored on the surface of 3-chloropropylsilyl silica gel and subsequently interacted with copper nitroprusside. The composite was characterized by infrared (FTIR, energy dispersive X-ray (EDX, and cyclic voltammetry. The above techniques confirmed the successful anchoring of the dendrimer on the silica gel modified surface and its interaction with copper nitroprusside. The cyclic voltammogram of CuNPSD was found to exhibit two redox couples with (Eθ′1 = 0.30 V and (Eθ′2 = 0.78 V versus Ag/AgCl (KCl=1.0 mol L−1; =20 mV s−1 attributed to the redox processes Cu(I/Cu(II and Fe(II(CN5NO/Fe(III(CN5NO, respectively. The CuNPSD-modified graphite paste electrode was found to show a linear response of 5.0×10−4 to 9.0×10−3 mol L−1 for nitrite determination with a detection limit (DL of 3.8×10−4 mol L−1 and an amperometric sensitivity of 25.0 mA/mol L−1. The CuNPSD-modified graphite paste electrode was found to show a good electrochemical stability and an excellent response to the electrocatalytic oxidation of sodium nitrite.

  18. Anchor of Ni2+ on the Agmatine Sulfate-Modified Electrodes for the Determination of H2O2 in Food

    Science.gov (United States)

    Yan, Yuhua; Zhang, Zhonghui; Xiao, Mingshu; Zhou, Hualan

    2017-07-01

    A method was developed to conveniently and rapidly determine hydrogen peroxide (H2O2) in food. The glassy carbon electrode (GCE) modified with agmatine sulfate (AS) easily anchoring nickel ion was attached to AS with polyamine structure. As a result, more Ni2+ was obtained and transformed to Ni(OH)2/NiOOH on the AS-GCE, which caused the electrode to own much better electrocatalytic performance on H2O2. Based on these, the content of H2O2 in thin sheet of bean curd sample was detected with standard addition method, by which good results were obtained.

  19. Electrochemical oxidation of adenosine-5 Prime -triphosphate on a chitosan-graphene composite modified carbon ionic liquid electrode and its determination

    Energy Technology Data Exchange (ETDEWEB)

    Sun Wei, E-mail: swyy26@hotmail.com [College of Chemistry and Chemical Engineering, Hainan Normal University, Haikou, 571158 (China); College of Chemistry and Molecular Engineering, Qingdao University of Science and Technology, Qingdao 266042 (China); Liu Jun; Wang Xiuzhen; Li Tongtong; Li Guangjiu; Wu Jie [College of Chemistry and Molecular Engineering, Qingdao University of Science and Technology, Qingdao 266042 (China); Zhang Liqi [State Key Laboratory of Coal Combustion, Huazhong University of Science and Technology, Wuhan 430074 (China)

    2012-10-01

    In this paper a new electrochemical method was proposed for the determination of adenosine-5 Prime -triphosphate (ATP) based on a chitosan (CTS) and graphene (GR) composite film modified carbon ionic liquid electrode (CTS-GR/CILE). CILE was fabricated by using ionic liquid 1-butyl-3-methylimidazolium dihydrogen phosphate ([BMIM]H{sub 2}PO{sub 4}) as the binder, which was further modified by GR and CTS composite. The modified electrode exhibited an excellent electrocatalytic activity toward the oxidation of ATP with the increase of the oxidation peak current and the decrease of the oxidation peak potential. The electrochemical parameters of ATP on CTS-GR/CILE were calculated with the electron transfer coefficient ({alpha}) as 0.329, the electron transfer number (n) as 2.15, the apparent heterogeneous electron transfer rate constant (ks) as 3.705 Multiplication-Sign 10{sup -5} s{sup -1} and the surface coverage ({Gamma}{sub T}) as 9.33 Multiplication-Sign 10{sup -10} mol cm{sup -2}. Under the optimal conditions the oxidation peak current was proportional to ATP concentration in the range from 1.0 Multiplication-Sign 10{sup -6} to 1.0 Multiplication-Sign 10{sup -3} M with the detection limit of 0.311 {mu}M (S/N = 3). The proposed electrode showed excellent reproducibility, stability, anti-interference ability and further successfully applied to the ATP injection sample detection. - Highlights: Black-Right-Pointing-Pointer Ionic liquid [BMIM]H{sub 2}PO{sub 4} based carbon ionic liquid electrode (CILE) was prepared. Black-Right-Pointing-Pointer Graphene modified CILE was fabricated for the sensitive electrochemical detection of ATP. Black-Right-Pointing-Pointer Good electrocatalytic ability to the ATP oxidation was achieved. Black-Right-Pointing-Pointer Detection of 5 Prime -ATP in commercial injection samples with satisfactory results.

  20. Voltammetric Determination of Ivabradine Hydrochloride Using Multiwalled Carbon Nanotubes Modified Electrode in Presence of Sodium Dodecyl Sulfate

    Directory of Open Access Journals (Sweden)

    Ali Kamal Attia

    2017-04-01

    Full Text Available Purpose: A new sensitive sensor was fabricated for the determination of ivabradine hydrochloride (IH based on modification with multiwalled carbon nanotubes using sodium dodecyl sulfate as micellar medium to increase the sensitivity. Methods: The electrochemical behavior of IH was studied in Britton-Robinson buffer (pH: 2.0-11.0 using cyclic and differential pulse voltammetry. Results: The voltammetric response was linear over the range of 3.984 x 10-6-3.475 x 10-5 mol L-1. The limits of detection and quantification were found to be 5.160 x 10-7 and 1.720 x 10-6 mol L-1, respectively. Conclusion: This method is suitable for determination of IH in tablets and plasma.

  1. Voltammetric Determination of Ivabradine Hydrochloride Using Multiwalled Carbon Nanotubes Modified Electrode in Presence of Sodium Dodecyl Sulfate.

    Science.gov (United States)

    Attia, Ali Kamal; Abo-Talib, Nisreen Farouk; Tammam, Marwa Hosny

    2017-04-01

    Purpose: A new sensitive sensor was fabricated for the determination of ivabradine hydrochloride (IH) based on modification with multiwalled carbon nanotubes using sodium dodecyl sulfate as micellar medium to increase the sensitivity. Methods: The electrochemical behavior of IH was studied in Britton-Robinson buffer (pH: 2.0-11.0) using cyclic and differential pulse voltammetry. Results: The voltammetric response was linear over the range of 3.984 x 10 -6 -3.475 x 10 -5 mol L -1 . The limits of detection and quantification were found to be 5.160 x 10 -7 and 1.720 x 10-6 mol L -1 , respectively. Conclusion: This method is suitable for determination of IH in tablets and plasma.

  2. Direct and precise determination of environmental radionuclides in solid materials using a modified Marinelli beaker and a HPGe detector

    International Nuclear Information System (INIS)

    Seo, B.K.; Lee, D.W.; Lee, K.Y.; Yoon, Y.Y.

    2001-01-01

    A simple but precise detection method was studied for the determination of natural radionuclides using a conventional HPGe detector. A new aluminium beaker instead of a plastic Marinelli beaker was constructed and examined to reach radioactive equilibrium conditions between radon and its daughter elements without the escape of gaseous radon. Using this beaker fifteen natural radionuclides from three natural decay series could be determined by direct γ-ray measurement and sixteen radionuclides could be determined indirectly after radioactive equilibrium had been reached. Analytical results from ground water were compared with those from conventional α spectroscopy and the results agreed well within 12% difference. Nitrogen gas purge was used to replace the surrounding air of the detector to obtain a stable background and reducing the interference of radon daughter nuclides in the atmosphere. The use of nitrogen purging and the aluminium Marinelli beaker results in an approximately tenfold increase of sensitivity and a decrease of the detection limit of 226 Ra to about 0.74 Bq kg -1 in soil samples. (orig.)

  3. Direct and precise determination of environmental radionuclides in solid materials using a modified Marinelli beaker and a HPGe detector.

    Science.gov (United States)

    Seo, B K; Lee, K Y; Yoon, Y Y; Lee, D W

    2001-06-01

    A simple but precise detection method was studied for the determination of natural radionuclides using a conventional HPGe detector. A new aluminium beaker instead of a plastic Marinelli beaker was constructed and examined to reach radioactive equilibrium conditions between radon and its daughter elements without the escape of gaseous radon. Using this beaker fifteen natural radionuclides from three natural decay series could be determined by direct gamma-ray measurement and sixteen radionuclides could be determined indirectly after radioactive equilibrium had been reached. Analytical results from ground water were compared with those from conventional alpha spectroscopy and the results agreed well within 12% difference. Nitrogen gas purge was used to replace the surrounding air of the detector to obtain a stable background and reducing the interference of radon daughter nuclides in the atmosphere. The use of nitrogen purging and the aluminium Marinelli beaker results in an approximately tenfold increase of sensitivity and a decrease of the detection limit of 226Ra to about 0.74 Bq kg(-1) in soil samples.

  4. Determination of the ionic transport numbers of lanthanum gallate materials by impedance spectroscopy and modified EMF method

    Directory of Open Access Journals (Sweden)

    Peña-Martínez, J.

    2008-06-01

    Full Text Available A combination of impedance spectroscopy and a modified electromotive force method (emf were used to evaluate the ionic transport numbers and the overall conductivity of several doped lanthanum gallate materials, i.e. La0.9Sr0.1Ga1-xMgxO3-δ (x=0.05-0.30, La0.9A0.1Ga0.8Mg0.2O3-δ (A=Sr, Ba and Ca and La0.9Sr0.1Ga0.8Mg0.2-yCoyO3-δ (y=0.015 and 0.045. La0.9Sr0.1Ga0.8Mg0.2O2.85 (LSGM sample showed the maximum ionic transport number in the temperature range 900-1173 K, around 0.99 in both O2/air and H2/air gradients.

    La conductividad total y los números de transporte iónico de las composiciones, basadas en el galato de lantano, La0,9Sr0,1Ga1-xMgxO3-δ (x=0,05-0,30, La0,9A0,1Ga0,8Mg0,2O3-δ (A=Sr, Ba, Ca y La0,9Sr0,1Ga0,8Mg0,2-yCoyO3-δ (y=0.015; 0,045 fueron estudiadas mediante una combinación de técnicas de espectroscopia de impedancia compleja y fuerza electromotriz (fem. La composición La0,9Sr0,1Ga0,8Mg0,2O2,85 (LSGM presenta el mayor número de transporte iónico, concretamente 0,99 en el rango de temperaturas 900-1173 K, tanto en gradiente de O2/aire como de H2/aire.

  5. Use of cyclic voltammetry and electrochemical impedance spectroscopy for determination of active surface area of modified carbon-based electrodes

    International Nuclear Information System (INIS)

    Souza, Leticia Lopes de

    2011-01-01

    Carbon-based electrodes as well the ion exchange electrodes among others have been applied mainly in the treatment of industrial effluents and radioactive wastes. Carbon is also used in fuel cells as substrate for the electrocatalysts, having high surface area which surpasses its geometric area. The knowledge of the total active area is important for the determination of operating conditions of an electrochemical cell with respect to the currents to be applied (current density). In this study it was used two techniques to determine the electrochemical active surface area of glassy carbon, electrodes and ion exchange electrodes: cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The experiments were carried out with KNO 3 0.1 mol.L -1 solutions in a three-electrode electrochemical cell: carbon-based working electrode, platinum auxiliary electrode and Ag/AgCl reference electrode. The glassy carbon and porous carbon electrodes with geometric areas of 3.14 x 10 -2 and 2.83 X 10 -1 cm 2 , respectively, were used. The ion exchange electrode was prepared by mixing graphite, carbon, ion exchange resin and a binder, and this mixture was applied in three layers on carbon felt, using a geometric area of 1.0 cm 2 during the experiments. The capacitance (Cd) of the materials was determined by EIS using Bode diagrams. The value of 172 μF.cm -2 found for the glassy carbon is consistent with the literature data (∼ 200 μF.cm'- 2 ). By VC, varying the scan rate from 0.2 to 2.0 mV.s-1, the capacitance CdS (S = active surface area) in the region of the electric double layer (EDL) of each material was determined. By EIS, the values of C d , 3.0 x 10 -5 μF.cm'- 2 and 11 x 10 3 μF.cm-2, were found for the porous carbon and ion exchange electrodes, respectively, which allowed the determination of active surface areas as 3.73 x 106 cm 2 and 4.72 cm 2 . To sum up, the combined use of EIS and CV techniques is a valuable tool for the calculation of active surface

  6. Cellulose membrane modified with polypyrrole as an extraction device for the determination of emerging contaminants in river water with GC-MS.

    Science.gov (United States)

    de Noronha, Bárbara Viero; Bergamini, Márcio Fernando; Marcolino Junior, Luiz Humberto; da Silva, Bruno José Gonçalves

    2018-05-21

    In this study, a simple, efficient, and reusable device based on cellulose membranes modified with polypyrrole was developed to extract 14 emerging contaminants from aqueous matrices. For chemical polymerization, a low-cost cellulose membrane was immersed in 0.1 mol L -1 pyrrole and 0.5 mol L -1 ammonium persulfate for 40 min in an ice/water bath. The cellulose membranes modified with polypyrrole were accommodated in a polycarbonate holder suitable for solid-phase extraction disks. Solid-phase extraction parameters that affect extraction efficiency, such as sample volume, pH, flow-rate, and desorption were optimized. Subsequently, determination of target compounds was performed by gas chromatography with mass spectrometry. The linear range for analytes ranged from 0.05 to 500 μg L -1 , with coefficients of determination above 0.990. The limits of quantification varied between 0.05 and 10 μg L -1 , with relative standard deviations lower than 17%. The performance of the proposed cellulose membranes modified with polypyrrole device for real samples was evaluated after extraction of emerging contaminants from a river water sample from the city of Curitiba-Brazil. Bisphenol A (6.39 μg L -1 ), caffeine (17.83 μg L -1 ), and paracetamol (19.28 μg L -1 ) were found in these samples. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

  7. 3,5-Diamino-1,2,4-triazole@electrochemically reduced graphene oxide film modified electrode for the electrochemical determination of 4-nitrophenol

    International Nuclear Information System (INIS)

    Kumar, Deivasigamani Ranjith; Kesavan, Srinivasan; Baynosa, Marjorie Lara; Shim, Jae-Jin

    2017-01-01

    Highlights: •Triazole film was formed on electrochemically reduced graphene oxide. •pDAT@ERGO/GC was utilized for the electrochemical determination of 4-nitrophenol. •pDAT@ERGO/GC electrode offered wide concentration and nanomolar detection limit. •The fabricated electrode was employed in water sample analyses. -- Abstract: In this study, an eco-friendly benign method for the modification of electrochemically reduced graphene oxide (ERGO) on glassy carbon (GC) surface and electrochemical polymerized 3,5-diamino-1,2,4-triazole (DAT) film composite (pDAT@ERGO/GC) electrode was developed. The surface morphologies of the pDAT@ERGO/GC modified electrode were analyzed by field emission scanning electron microscopy (FESEM). FESEM images indicated that the ERGO supported pDAT has an almost homogeneous morphology structure with a size of 70 to 80 nm. It is due to the water oxidation reaction occurred while pDAT@ERGO/GC fabrication peak at +1.4 V leads to O 2 evolution and oxygen functional group functionalization on ERGO, which confirmed by X-ray photoelectron spectroscopy (XPS). In contrast, the bare GC modified with pDAT showed randomly arranged irregular bulky morphology structure compared to those of pDAT@ERGO/GC. Electrochemical reduction of graphene oxide was confirmed by Raman spectroscopy, XPS, and electrochemical impedance spectroscopy (EIS). The pDAT@ERGO/GC modified electrode was used for the electrochemical determination of 4-nitrophenol (4-NP). The 4-NP oxidation peak was observed at +0.25 V, and the differential pulse voltammetry demonstrated wide concentration range (5–1500 μM), high sensitivity (0.7113 μA μM −1 ), and low limit of detection (37 nM). Moreover, the pDAT@ERGO/GC electrode was applied to real water sample analysis by standard addition method, where in good recoveries (97.8% to 102.4%) were obtained.

  8. Anodic stripping voltammetric determination of traces of Pb(II) and Cd(II) using a glassy carbon electrode modified with bismuth nanoparticles

    International Nuclear Information System (INIS)

    Yang, Die; Wang, Liang; Chen, Zuliang; Megharaj, Mallavarapu; Naidu, Ravi

    2014-01-01

    We report on a glassy carbon electrode modified with bismuth nanoparticles (NanoBiE) for the simultaneous determination Pb 2+ and Cd 2+ by anodic stripping voltammetry. Operational parameters such as bismuth nanoparticles labelling amount, deposition potential, deposition time and stripping parameters were optimized with respect to the determination of Pb 2+ and Cd 2+ in 0.1 M acetate buffer solution (pH 4.5). The NanoBiE gives well-defined, reproducible and sharp stripping peaks. The peak current response increases linearly with the metal concentration in a range of 5.0–60.0 μg L −1 , with a detection limit of 0.8 and 0.4 μg L −1 for Pb 2+ and Cd 2+ , respectively. The morphology and composition of the modified electrode before and after voltammetric measurements were analysed by scanning electron microscopy and energy dispersive X-ray analysis. The NanoBiE was successfully applied to analysis of Pb 2+ and Cd 2+ in real water samples and the method was validated by ICP-MS technique, suggesting that the electrode can be considered as an interesting alternative to the bismuth film electrode for possible use in electrochemical studies and electro analysis. (author)

  9. Determination of As, Cd, and Pb in Tap Water and Bottled Water Samples by Using Optimized GFAAS System with Pd-Mg and Ni as Matrix Modifiers

    Directory of Open Access Journals (Sweden)

    Sezgin Bakırdere

    2013-01-01

    Full Text Available Arsenic, lead, and cadmium were determined in tap and bottled water samples consumed in the west part of Turkey at trace levels. Graphite furnace atomic absorption spectrometry (GFAAS was used in all detections. All of the system parameters for each element were optimized to increase sensitivity. Pd-Mg mixture was selected as the best matrix modifier for As, while the highest signals were obtained for Pb and Cd in the case of Ni used as matrix modifier. Detection limits for As, Cd, and Pb were found to be 2.0, 0.036, and 0.25 ng/mL, respectively. 78 tap water and 17 different brands of bottled water samples were analyzed for their As, Cd, and Pb contents under the optimized conditions. In all water samples, concentration of cadmium was found to be lower than detection limits. Lead concentration in the samples analyzed varied between N.D. and 12.66 ± 0.68 ng/mL. The highest concentration of arsenic was determined as 11.54 ± 2.79 ng/mL. Accuracy of the methods was verified by using a certified reference material, namely, Trace Element in Water, 1643e. Results found for As, Cd, and Pb in reference materials were in satisfactory agreement with the certified values.

  10. Sensitive electrochemical determination of trace cadmium on a stannum film/poly(p-aminobenzene sulfonic acid)/electrochemically reduced graphene composite modified electrode

    International Nuclear Information System (INIS)

    Wang, Zhiqiang; Wang, Hui; Zhang, Zhihao; Yang, Xiaojing; Liu, Gang

    2014-01-01

    In this study, a novel stannum film/poly(p-aminobenzene sulfonic acid)/graphene composite modified glassy carbon electrode (GCE) was prepared by using electrodeposition of exfoliated graphene oxide, electropolymerization of p-aminobenzene sulfonic acid (p-ABSA) and in situ plating stannum fim methods, successively. This sensor was further used for sensitive determination of trace cadmium ions by square wave anodic stripping voltammetry (SWASV). The morphologies and electrochemistry properties of the modified electrode were characterized by scanning electron microscopy, Raman spectroscopy, cyclic voltammetry, electrochemical impedance spectroscopy and linear sweep voltammetry. It was found that the formed graphene layer on the top of GCE could remarkably facilitate the electron transfer and enlarge the specific surface area of the electrode. While the poly(p-ABSA) film could effectively increase the adhesion and stability of graphene layer, enhance ion-exchange capacity and prevent the macromolecule in real samples absorbing on the surface of electrode. By combining co-deposits ability with heavy metals of stannum film, the obtained electrode exhibited a good stripping performance for the analysis of Cd(II). Under the optimum conditions, a linear response was observed in the range from 1.0 to 70.0 μgL −1 with a detection limit of 0.05 μgL −1 (S/N = 3). The sensor was further applied to the determination of cadmium ions in real water samples with satisfactory results

  11. A simple and sensitive methodology for voltammetric determination of valproic acid in human blood plasma samples using 3-aminopropyletriethoxy silane coated magnetic nanoparticles modified pencil graphite electrode.

    Science.gov (United States)

    Zabardasti, Abedin; Afrouzi, Hossein; Talemi, Rasoul Pourtaghavi

    2017-07-01

    In this work, we have prepared a nano-material modified pencil graphite electrode for the sensing of valproic acid (VA) by immobilization 3-aminopropyletriethoxy silane coated magnetic nanoparticles (APTES-MNPs) on the pencil graphite surface (PGE). Electrochemical studies indicated that the APTES-MNPs efficiently increased the electron transfer kinetics between VA and the electrode and the free NH 2 groups of the APTES on the outer surface of magnetic nanoparticles can interact with carboxyl groups of VA. Based on this, we have proposed a sensitive, rapid and convenient electrochemical method for VA determination. Under the optimized conditions, the reduction peak current of VA is found to be proportional to its concentration in the range of 1.0 (±0.2) to 100.0 (±0.3) ppm with a detection limit of 0.4 (±0.1) ppm. The whole sensor fabrication process was characterized by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) methods with using [Fe(CN) 6 ] 3-/4- as an electrochemical redox indicator. The prepared modified electrode showed several advantages such as high sensitivity, selectivity, ease of preparation and good repeatability, reproducibility and stability. The proposed method was applied to determination of valproic acid in blood plasma samples and the obtained results were satisfactory accurate. Copyright © 2017. Published by Elsevier B.V.

  12. Electrochemical sensor for the determination of thiourea using a glassy carbon electrode modified with a self-assembled monolayer of an oxadiazole derivative and with silver nanoparticles

    International Nuclear Information System (INIS)

    Moghadam, Masoud Rohani; Akbarzadeh, Sanaz; Nasirizadeh, Navid

    2016-01-01

    This article reports on an electrochemical sensor for thiourea. It is based on a glassy carbon electrode (GCE) modified with a self-assembled monolayer of an oxadiazole derivative and with silver nanoparticles. The modified GCE demonstrated highly catalytic activity in terms of thiourea oxidation. The peak potential is shifted to negative values compared to a GCE coated with silver nanoparticles only. The electrode was characterized by linear sweep voltametry, cyclic voltammetry and chronoamperometry, and thiourea was determined by differential pulse voltammetry in aqueous buffer of pH 7.0 resulting in two linear response ranges of 0.001 − 69.4 and 69.4 − 833.3 μM and the limit of detection of 0.1 nM. The method was applied to the determination of thiourea in copper refinery electrolyte, orange juice and tap water samples. The recoveries ranged from 96.9 to 108.0 %. (author)

  13. Voltammetric determination of total dissolved iron in coastal waters using a glassy carbon electrode modified with reduced graphene oxide, Methylene Blue and gold nanoparticles

    International Nuclear Information System (INIS)

    Lin, Mingyue; Zhang, Haiyun; Han, Haitao; Pan, Dawei; Su, Zhencui

    2015-01-01

    A nanocomposite, prepared from reduced graphene oxide (rGO), Methylene Blue (MB) and gold nanoparticles (AuNPs), was used to modify a glassy carbon electrode for the determination of total dissolved iron by differential pulse voltammetry. The use of rGO warrants a larger electrode surface and the presence of more active sites, while electron transfer is accelerated by incorporating AuNPs. MB acts as an electron mediator, as an anchor for the AuNPs (which were grown in situ), and also prevents the aggregation of rGO. The modified electrode displayed a remarkably improved sensitivity and selectivity for Fe(III). The kinetics of the electrode reaction is adsorption-controlled, and the reversible process involves one proton and one electron. The response to Fe(III) is linear in the 0.3 to 100 μM concentration range, and the detection limit is 15 nM. Possible interferences by other ions were studied. The electrode was successfully applied to the determination of total dissolved iron in real coastal waters. (author)

  14. Synthesis and characterization of manganese diselenide nanoparticles (MnSeNPs): Determination of capsaicin by using MnSeNP-modified glassy carbon electrode.

    Science.gov (United States)

    Sukanya, Ramaraj; Sakthivel, Mani; Chen, Shen-Ming; Chen, Tse-Wei; Al-Hemaid, Fahad M A; Ajmal Ali, M; Elshikh, Mohamed Soliman

    2018-06-02

    A new type of manganese diselenide nanoparticles (MnSeNPs) was synthesized by using a hydrothermal method. Their surface morphology, crystallinity and elemental distribution were characterized by using transmission electron microscopy, X-ray diffraction, energy dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy which scrutinize the formation of the NPs. The NPs were coated on a glassy carbon electrode (GCE), and electrochemical impedance spectroscopy, cyclic voltammetry and differential pulse voltammetry were applied to study the electroanalytical properties towards the oxidation of the food additive capsaicin. The modified GCE displays lower charge transfer resistance (R ct  = 29.52 Ω), a larger active surface area (0.089 cm 2 /g, and more efficient electrochemical oxidation of capsaicin compared to a MnS 2 /GCE and a bare GCE. The oxidation peak potential is 0.43 V (vs. Ag/AgCl) which is lower than that of previously reported GCEs. The sensor has a detection limit as low as 0.05 μM and an electrochemical sensitivity of 2.41 μA μM -1  cm -2 . The method was applied to the determination of capsaicin in pepper samples. Graphical abstract Electrochemical determination of capsaicin in pepper extract by using MnSeNPs modified electrode.

  15. Simultaneous voltammetric determination of 2-nitrophenol and 4-nitrophenol based on an acetylene black paste electrode modified with a graphene-chitosan composite

    International Nuclear Information System (INIS)

    Deng, Peihong; Xu, Zhifeng; Li, Junhua

    2014-01-01

    We describe a simple and sensitive voltammetric method for the simultaneous determination of 2-nitrophenol and 4-nitrophenol. It is based on the use of an acetylene black paste electrode modified with a graphene-chitosan composite film (denoted as Gr-Chit/ABPE). The reduction peak currents of 2-nitrophenol (at −252 mV) and of 4-nitrophenol (at −340 mV) in pH 1.0 solution increase significantly at the Gr-Chit/ABPE in comparison to a bare ABPE. Factors affecting sensitivity were optimized and a linear relationship is found between peak current and the concentrations of 2-nitrophenol (in the 0.4 μM to 80 μM range) and for 4-nitrophenol (in the 0.1 μM to 80 μM range). The detection limits (at an SNR of 3 and after a 30-s accumulation time) are 200 nM for 2-nitrophenol and 80 nM for 4-nitrophenol, respectively. The modified electrode was successfully applied to the direct and parallel determination of 2-nitrophenol and 4-nitrophenol in spiked water samples. (author)

  16. Modified Au nanoparticles-imprinted sol-gel, multiwall carbon nanotubes pencil graphite electrode used as a sensor for ranitidine determination.

    Science.gov (United States)

    Rezaei, B; Lotfi-Forushani, H; Ensafi, A A

    2014-04-01

    A new, simple, and disposable molecularly imprinted electrochemical sensor for the determination of ranitidine was developed on pencil graphite electrode (PGE) via cyclic voltammetry (CV). The PGEs were coated with MWCNTs containing the carboxylic functional group (f-MWCNTs), imprinted with sol-gel and Au nanoparticle (AuNPs) layers (AuNP/MIP-sol-gel/f-MWCNT/PGE), respectively, to enhance the electrode's electrical transmission and sensitivity. The thin film of molecularly imprinted sol-gel polymers with specific binding sites for ranitidine was cast on modified PGE by electrochemical deposition. The AuNP/MIP-sol-gel/f-MWCNT/PGE thus developed was characterized by electrochemical impedance spectroscopy (EIS) and CV. The interaction between the imprinted sensor and the target molecule was also observed on the electrode by measuring the current response of 5.0mMK3[Fe(CN)6] solution as an electrochemical probe. The pick currents of ranitidine increased linearly with concentration in the ranges of 0.05 to 2.0μM, with a detection limit of (S/N=3) 0.02μM. Finally, the modified electrode was successfully employed to determine ranitidine in human urine samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. Evaluation of an ODS column modified with zwitterionic/nonionic mixed surfactants and its application to direct injection determination of inorganic anions.

    Science.gov (United States)

    Hasegawa, Takuya; Umemura, Tomonari; Koide, Akira; Chiba, Koichi; Ueki, Yuji; Tsunoda, Kin-ichi; Haraguchi, Hiroki

    2005-08-01

    An octadecylsilica (ODS) column modified with zwitterionic/nonionic mixed surfactants was evaluated for the direct injection determination of inorganic anions in biological fluids by ion chromatography. A zwitterionic surfactant (sulfobetaine-type) and a nonionic surfactant (polyoxyethylene-type) were used for a stationary-phase modification. When aqueous electrolyte solutions with concentrations of sub-mM to several mM were used as a mobile phase, the zwitterionic surfactant coated on the ODS surface exhibited unique separation selectivity for ionic species, while the nonionic surfactant coated on the ODS might have formed a hydrophilic network over the ODS surface and restricted matrix proteins from adsorbing on the stationary phase. Consequently, the mixed surfactant-modified column system allowed an efficient ion chromatographic separation of inorganic anions as well as a size-exclusive removal of column-fouling proteins. This separation system was applied to the direct injection determination of UV-absorbing anions in human saliva. The detection limits for nitrite, nitrate, iodide and thiocyanate were 3.1, 2.7, 4.5 and 25 microM, respectively, with UV detection at 210 nm (injection volume; 20 microl), and their relative standard deviations for 5 replicate measurements of saliva samples spiked with 100 microM each of those anions were 1.4, 0.9, 2.2 and 5.5%, respectively.

  18. Investigation of chemical modifiers for the direct determination of arsenic in fish oil using high-resolution continuum source graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Pereira, Éderson R; de Almeida, Tarcísio S; Borges, Daniel L G; Carasek, Eduardo; Welz, Bernhard; Feldmann, Jörg; Campo Menoyo, Javier Del

    2016-04-01

    High-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS) has been applied for the development of a method for the determination of total As in fish oil samples using direct analysis. The method does not use any sample pretreatment, besides dilution with 1-propanole, in order to decrease the oil viscosity. The stability and sensitivity of As were evaluated using ruthenium and iridium as permanent chemical modifiers and palladium added in solution over the sample. The best results were obtained with ruthenium as the permanent modifier and palladium in solution added to samples and standard solutions. Under these conditions, aqueous standard solutions could be used for calibration for the fish oil samples diluted with 1-propanole. The pyrolysis and atomization temperatures were 1400 °C and 2300 °C, respectively, and the limit of detection and characteristic mass were 30 pg and 43 pg, respectively. Accuracy and precision of the method have been evaluated using microwave-assisted acid digestion of the samples with subsequent determination by HR-CS GF AAS and ICP-MS; the results were in agreement (95% confidence level) with those of the proposed method. Copyright © 2015 Elsevier B.V. All rights reserved.

  19. Determination of picomolar silver concentrations by differential pulse anodic stripping voltammetry at a carbon paste electrode modified with phenylthiourea-functionalized high ordered nanoporous silica gel

    International Nuclear Information System (INIS)

    Javanbakht, Mehran; Divsar, Faten; Badiei, Alireza; Fatollahi, Fatemeh; Khaniani, Yeganeh; Ganjali, Mohammad Reza; Norouzi, Parviz; Chaloosi, Marzieh; Ziarani, Ghodsi Mohammadi

    2009-01-01

    This study introduces the design of an anodic stripping voltammetric (ASV) method for the silver ion determination at a carbon paste electrode (CPE), chemically modified with phenylthiourea-nanoporous silica gel (Tu-SBA-15-CPE). The electroanalytical pro includes two steps: preconcentration of metal ions at an electrode surface, followed by quantification of the accumulated species by differential pulse anodic stripping voltammetric methods. Factors affecting the performance of the anodic stripping were investigated, including the modifier quantity in the paste, the electrolyte concentrations, the solution pH and the accumulation potential or time. The most sensitive and reliable electrode contained 10% Tu-SBA-15 and 90% carbon paste. The accumulation potential and time were set at, -200 mV and 300 s, respectively, and the scan rate at 50 mV s -1 in the scan range of -200 to 700 mV. The resulting electrode demonstrated a linear response over range of silver ion concentration of 8.0-80 pmol/L with detection limit (S/N = 3) of 5 pmol/L. The prepared electrodes were used for the silver determination in sea and tap water samples and very good recovery results were obtained. The accuracy was assessed through recovery experiments and independent analysis by graphite furnace atomic absorption spectrometry.

  20. Determination of picomolar silver concentrations by differential pulse anodic stripping voltammetry at a carbon paste electrode modified with phenylthiourea-functionalized high ordered nanoporous silica gel

    Energy Technology Data Exchange (ETDEWEB)

    Javanbakht, Mehran [Department of Chemistry, Amirkabir University of Technology, Tehran (Iran, Islamic Republic of); Nano Science and Technology Research Center, Amirkabir University of Technology, Tehran (Iran, Islamic Republic of)], E-mail: mehranjavanbakht@gmail.com; Divsar, Faten [Department of Chemistry, University of Tarbiat Moallem, Tehran (Iran, Islamic Republic of); Badiei, Alireza [School of Chemistry, University College of Science, University of Tehran, Tehran (Iran, Islamic Republic of); Fatollahi, Fatemeh [Department of Chemistry, Amirkabir University of Technology, Tehran (Iran, Islamic Republic of); Khaniani, Yeganeh [School of Chemistry, University College of Science, University of Tehran, Tehran (Iran, Islamic Republic of); Ganjali, Mohammad Reza; Norouzi, Parviz [Center of Excellence in Electrochemistry, Faculty of Chemistry, University of Tehran, Tehran (Iran, Islamic Republic of); Chaloosi, Marzieh [Department of Chemistry, University of Tarbiat Moallem, Tehran (Iran, Islamic Republic of); Ziarani, Ghodsi Mohammadi [Department of Chemistry, University of Alzahra, Tehran (Iran, Islamic Republic of)

    2009-09-30

    This study introduces the design of an anodic stripping voltammetric (ASV) method for the silver ion determination at a carbon paste electrode (CPE), chemically modified with phenylthiourea-nanoporous silica gel (Tu-SBA-15-CPE). The electroanalytical pro includes two steps: preconcentration of metal ions at an electrode surface, followed by quantification of the accumulated species by differential pulse anodic stripping voltammetric methods. Factors affecting the performance of the anodic stripping were investigated, including the modifier quantity in the paste, the electrolyte concentrations, the solution pH and the accumulation potential or time. The most sensitive and reliable electrode contained 10% Tu-SBA-15 and 90% carbon paste. The accumulation potential and time were set at, -200 mV and 300 s, respectively, and the scan rate at 50 mV s{sup -1} in the scan range of -200 to 700 mV. The resulting electrode demonstrated a linear response over range of silver ion concentration of 8.0-80 pmol/L with detection limit (S/N = 3) of 5 pmol/L. The prepared electrodes were used for the silver determination in sea and tap water samples and very good recovery results were obtained. The accuracy was assessed through recovery experiments and independent analysis by graphite furnace atomic absorption spectrometry.

  1. Organic palladium and palladium-magnesium chemical modifiers in direct determination of lead in fractions from distillation of crude oil by electrothermal atomic absorption analysis

    Science.gov (United States)

    Kowalewska, Zofia; Bulska, Ewa; Hulanicki, Adam

    1999-05-01

    Platinum reforming catalysts are easily poisoned by increased levels of lead, therefore a sensitive atomic absorption spectrometric procedure for lead determination in fractions from crude oil distillation was developed. Lead was present in organic form in the samples analysed therefore the behaviour of various lead compounds (Pb-alkylarylsulphonate, Pb-4-cyclohexanobutyrate, tetraethyllead, Pb in fuel oil) was studied. The best procedure for the determination of lead in different petroleum products, including those containing asphaltenes includes a pretreatment with iodine and methyltrioctylammonium chloride, followed by the use of an organic Pd-Mg modifier. Under these conditions an effective matrix removal is possible at a pyrolysis temperature up to approximately 1100°C and the behaviour of lead present in different forms is unified. The characteristic mass is 11-12 pg Pb, corresponding to a detection limit of 0.25 ng g -1 for 20 μl sample solution. This can be lowered by multiple injection.

  2. Electrochemical fabrication of a novel ZnO/cysteic acid nanocomposite modified electrode and its application to simultaneous determination of sunset yellow and tartrazine.

    Science.gov (United States)

    Dorraji, Parisa S; Jalali, Fahimeh

    2017-07-15

    A new nanocomposite (ZnO/Cysteic acid) was deposited on glassy carbon electrode by cyclic voltammetry. Uniform deposition of the nanocomposite was observed by scanning electron microscopy. The electron transfer characteristics of two food additives, sunset yellow and tartrazine, were greatly improved on the modified electrode. The prepared electrode was used in the sensitive simultaneous determination of sunset yellow and tartrazine by differential pulse voltammetry. Linear calibration curves were obtained in the concentration ranges of 0.1-3.0, and 0.07-1.86μM, and detection limits of 0.03 and 0.01μM for sunset yellow and tartrazine, respectively. The proposed method was evaluated by determination of the dyes in processed soft drinks with satisfactory results (recovery>95% and RSD%<5%). Copyright © 2017 Elsevier Ltd. All rights reserved.

  3. Polyaniline Langmuir-Blodgett film modified glassy carbon electrode as a voltammetric sensor for determination of Ag+ ions

    International Nuclear Information System (INIS)

    Liu Qiongyan; Wang Fei; Qiao Yonghui; Zhang Shusheng; Ye Baoxian

    2010-01-01

    A highly sensitive electrochemical sensor made of a glassy carbon electrode (GCE) coated with a Langmuir-Blodgett film (LB) containing polyaniline (PAn) doped with p-toluenesulfonic acid (PTSA) (LB/PAn-PTSA/GCE) has been used for the detection of trace concentrations of Ag + . UV-vis absorption spectra indicated that the PAn was doped by PTSA. The surface morphology of the PAn LB film was characterized by atomic force microscopy (AFM). The electrochemical properties of this LB/PAn-PTSA/GCE were studied using electrochemical impedance spectroscopy (EIS) and cyclic voltammetry. The LB/PAn-PTSA/GCE was used as a voltammetric sensor for determination of trace Ag + at pH 5.0 using linear scanning stripping voltammetry. Under the optimal experimental conditions, the stripping current was proportional to the Ag + concentration over the range from 6.0 x 10 -10 mol L -1 to 1.0 x 10 -6 mol L -1 , with a detection limit of 4.0 x 10 -10 mol L -1 . The high sensitivity, selectivity, and stability of this LB/PAn-PTSA/GCE also demonstrated its practical utility for simple, rapid and economical determination of Ag + in water samples.

  4. Screen-printed electrodes modified with carbon nanotubes or graphene for simultaneous determination of melatonin and serotonin

    International Nuclear Information System (INIS)

    Gomez, Federico José Vicente; Martín, Aída; Escarpa, Alberto; Silva, María Fernanda

    2015-01-01

    Single-walled carbon nanotubes (SWCNT), multi-walled carbon nanotubes (MWCNT) and graphene have been tested as carbon allotropes for the modification of carbon screen-printed electrodes (CSPEs) to simultaneously determine melatonin (MT) and serotonin (5-HT). Two groups of CSPEs, both 4 mm in diameter, were explored: The first includes commercial SWCNT, MWCNT and graphene, the second includes SWCNT, MWCNT, graphene oxide nanoribbons and reduced nanoribbons that were drop casted on the electrodes. The carbon nanomaterials enhanced the electroactive area in the following order: CSPE determination of 5-HT and MT at the working potentials of +50 mV and +390 mV (vs. Ag), respectively. The use of carbon nanomaterials, in particular of graphene oxide nanoribbons on CSPEs, represents an excellent and disposable tool for sensing the two target molecules in even small sample volumes. Figures of merit for MT and 5-HT include (a) detection limit of 1.1 and 0.4 μM for MT and 5-HT, respectively; (b) an inter-electrode reproducibility with RSD ≤ 8 %; (c) 120 s response time, and (d) recoveries (in case of spiked samples) ranging from 94 to 103 % (with an RSD < 1 %). (author)

  5. A Modified LC/MS/MS Method with Enhanced Sensitivity for the Determination of Scopolamine in Human Plasma

    Science.gov (United States)

    Wang, Zuwei; Vaksman, Zalman; Putcha, Lakshmi

    2008-01-01

    Intranasal scopolamine is a choice drug for the treatment of motion sickness during space flight because of its quick onset of action, short half-life and favorable sideeffects profile. The dose administered usually ranges between 0.1 and 0.4 mg. Such small doses make it difficult to detect concentrations of scopolamine in biological fluids using existing sensitive LC/MS/MS method, especially when the biological sample volumes are limited. To measure scopolamine in human plasma to facilitate pharmacokinetic evaluation of the drug, we developed a sensitive LC/MS/MS method using 96 well micro elution plates for solid phase extraction (SPE) of scopolamine in human plasma. Human plasma (100-250 micro L) were loaded onto Waters Oasis HLB 96 well micro elution plate and eluted with 50 L of organic solvent without evaporation and reconstitution. HPLC separation of the eluted sample was performed using an Agilent Zorbax SB-CN column (50 x 2.1 mm) at a flow rate of 0.2 mL/min for 3 minutes. The mobile phase for separation was 80:20 (v/v) methanol: ammonium acetate (30 mM) in water. Concentrations of scopolamine were determined using a Micromass Quattro Micro(TM) mass spectrometer with electrospray ionization (ESI). ESI mass spectra were acquired in positive ion mode with multiple reaction monitoring for the determination of scopolamine m/z = 304.2 right arrow 138.1 and internal standard hyoscyamine m/z = 290.2 right arrow 124.1. The method is rapid, reproducible, specific and has the following parameters: scopolamine and the IS are eluted at about 1.1 and 1.7 min respectively. The linear range is 25-10000 pg/mL for scopolamine in human plasma with correlation coefficients greater than 0.99 and CV less than 0.5%. The intra-day and inter-day CVs are less than 15% for quality control samples with concentrations of 75,300, and 750 pg/mL of scopolamine in human plasma. SPE using 96 well micro elution plates allows rapid sample preparation and enhanced sensitivity for the LC

  6. A modified fluorimetric host cell reactivation assay to determine the repair capacity of primary keratinocytes, melanocytes and fibroblasts

    Directory of Open Access Journals (Sweden)

    Gebhard Daniel

    2010-06-01

    Full Text Available Abstract Background The Host Cell Reactivation Assay (HCRA is widely used to identify circumstances and substances affecting the repair capacity of cells, however, it is restricted by the transfection procedure used and the sensitivity of the detection method. Primary skin cells are particularly difficult to transfect, and therefore sensitive methods are needed to detect any variations due to the cell-type or inter-individual differences or changes induced by diverse substances. A sensitive and repeatable method to detect the repair capacity of skin cells would be useful in two different aspects: On the one hand, to identify substances influencing the repair capacity in a positive manner (these substances could be promising ingredients for cosmetic products and on the other hand, to exclude the negative effects of substances on the repair capacity (this could serve as one step further towards replacing or at least reducing animal testing. Results In this paper, we present a rapid and sensitive assay to determine the repair capacity of primary keratinocytes, melanocytes and fibroblasts based on two wave-length Green Fluorescent Protein (GFP and DsRed reporter technology in order to test different substances and their potential to influence the DNA repair capacity. For the detection of plasmid restoration, we used FACS technology, which, in comparison to luminometer technology, is highly sensitive and allows single cell based analysis. The usefulness of this assay and studying the repair capacity is demonstrated by the evidence that DNA repair is repressed by Cyclosporin A in fibroblasts. Conclusions The methodology described in this paper determines the DNA repair capacity in different types of human skin cells. The described transfection protocol is suitable for the transfection of melanocytes, keratinocytes and fibroblasts, reaching efficacies suitable for the detection of the restored plasmids by FACS technology. Therefore the repair capacity

  7. SU-G-201-10: Experimental Determination of Modified TG-43 Dosimetry Parameters for the Xoft Axxent® Electronic Brachytherapy Source

    Energy Technology Data Exchange (ETDEWEB)

    Simiele, S; Palmer, B; DeWerd, L [Department of Medical Physics, School of Medicine and Public Health, University of Wisconsin-Madison, Madison, WI (United States)

    2016-06-15

    Purpose: The establishment of an air kerma rate standard at NIST for the Xoft Axxent{sup ®} electronic brachytherapy source (Axxent{sup ®} source) motivated the establishment of a modified TG-43 dosimetry formalism. This work measures the modified dosimetry parameters for the Axxent{sup ®} source in the absence of a treatment applicator for implementation in Xoft’s treatment planning system. Methods: The dose-rate conversion coefficient (DRCC), radial dose function (RDF) values, and polar anisotropy (PA) were measured using TLD-100 microcubes with NIST-calibrated sources. The DRCC and RDF measurements were performed in liquid water using an annulus of Virtual Water™ designed to align the TLDs at the height of the anode at fixed radii from the source. The PA was measured at several distances from the source in a PMMA phantom. MCNP-determined absorbed dose energy dependence correction factors were used to convert from dose to TLD to dose to liquid water for the DRCC, RDF, and PA measurements. The intrinsic energy dependence correction factor from the work of Pike was used. The AKR was determined using a NIST-calibrated HDR1000 Plus well-type ionization chamber. Results: The DRCC was determined to be 8.6 (cGy/hr)/(µGy/min). The radial dose values were determined to be 1.00 (1cm), 0.60 (2cm), 0.42 (3cm), and 0.32 (4cm), with agreement ranging from (5.7% to 10.9%) from the work of Hiatt et al. 2015 and agreement from (2.8% to 6.8%) with internal MCNP simulations. Conclusion: This work presents a complete dataset of modified TG-43 dosimetry parameters for the Axxent{sup ®} source in the absence of an applicator. Prior to this study a DRCC had not been measured for the Axxent{sup ®} source. This data will be used for calculating dose distributions for patients receiving treatment with the Axxent{sup ®} source in Xoft’s breast balloon and vaginal applicators, and for intraoperative radiotherapy. Sources and partial funding for this work were provided by Xoft

  8. SU-G-201-10: Experimental Determination of Modified TG-43 Dosimetry Parameters for the Xoft Axxent® Electronic Brachytherapy Source

    International Nuclear Information System (INIS)

    Simiele, S; Palmer, B; DeWerd, L

    2016-01-01

    Purpose: The establishment of an air kerma rate standard at NIST for the Xoft Axxent"® electronic brachytherapy source (Axxent"® source) motivated the establishment of a modified TG-43 dosimetry formalism. This work measures the modified dosimetry parameters for the Axxent"® source in the absence of a treatment applicator for implementation in Xoft’s treatment planning system. Methods: The dose-rate conversion coefficient (DRCC), radial dose function (RDF) values, and polar anisotropy (PA) were measured using TLD-100 microcubes with NIST-calibrated sources. The DRCC and RDF measurements were performed in liquid water using an annulus of Virtual Water™ designed to align the TLDs at the height of the anode at fixed radii from the source. The PA was measured at several distances from the source in a PMMA phantom. MCNP-determined absorbed dose energy dependence correction factors were used to convert from dose to TLD to dose to liquid water for the DRCC, RDF, and PA measurements. The intrinsic energy dependence correction factor from the work of Pike was used. The AKR was determined using a NIST-calibrated HDR1000 Plus well-type ionization chamber. Results: The DRCC was determined to be 8.6 (cGy/hr)/(µGy/min). The radial dose values were determined to be 1.00 (1cm), 0.60 (2cm), 0.42 (3cm), and 0.32 (4cm), with agreement ranging from (5.7% to 10.9%) from the work of Hiatt et al. 2015 and agreement from (2.8% to 6.8%) with internal MCNP simulations. Conclusion: This work presents a complete dataset of modified TG-43 dosimetry parameters for the Axxent"® source in the absence of an applicator. Prior to this study a DRCC had not been measured for the Axxent"® source. This data will be used for calculating dose distributions for patients receiving treatment with the Axxent"® source in Xoft’s breast balloon and vaginal applicators, and for intraoperative radiotherapy. Sources and partial funding for this work were provided by Xoft Inc. (a subsidiary of i

  9. Multiwall carbon nanotubes chemically modified carbon paste electrodes for determination of gentamicin sulfate in pharmaceutical preparations and biological fluids

    Energy Technology Data Exchange (ETDEWEB)

    Khalil, M.M., E-mail: magdy_mmagdy@yahoo.com; Abed El-aziz, G.M., E-mail: Gamal_abedelaziz@yahoo.com

    2016-02-01

    This article focused on the construction and characteristics of novel and sensitive gentamicin carbon paste electrodes which are based on the incorporation of multiwall carbon nanotubes (MWCNTs) which improve the characteristics of the electrodes. The electrodes were constructed based on gentamicin-phosphotungstate (GNS-PTA) called CPE{sub 1}, gentamicin-phosphomolybdate (GNS-PMA) called CPE{sub 2}, GNS-PTA + MWMCNTs called MWCPE{sub 1}, and GNS-PMA + MWMCNTs called MWCPE{sub 2}. The constructed electrodes, at optimum paste composition, exhibited good Nernstian response for determination of gentamicin sulfate (GNS) over a linear concentration range from 2.5 × 10{sup −6} to 1 × 10{sup −2}, 3.0 × 10{sup −6} to 1 × 10{sup −2}, 4.9 × 10{sup −7} to 1 × 10{sup −2} and 5.0 × 10{sup −7} to 1 × 10{sup −2} mol L{sup −1}, with lower detection limit 1 × 10{sup −6}, 1 × 10{sup −6}, 1.9 × 10{sup −7} and 2.2 × 10{sup −7} mol L{sup −1}, and with slope values of 29.0 ± 0.4, 29.2 ± 0.7, 31.2 ± 0.5 and 31.0 ± 0.6 mV/decade for CPE{sub 1}, CPE{sub 2}, MWCPE{sub 1} and MWCPE{sub 2}, respectively. The response of electrodes is not affected by pH in the range 3–8 for CPE{sub 1} and CPE{sub 2} and in the range 2.5–8.5 for MWCPE{sub 1} and MWCPE{sub 2}. The results showed fast dynamic response time (about 8–5 s) and long lifetime (more than 2 months) for all electrodes. The sensors showed high selectivity for gentamicin sulfate (GNS) with respect to a large number of interfering species. The constructed electrodes were successfully applied for determination of GNS in pure form, its pharmaceutical preparations and biological fluids using standard addition and potentiometric titration methods with high accuracy and precision. - Graphical abstract: The incorporation of MWCNTs in paste composition improves the characteristics of the MWCPE electrodes which show better responses in terms of sensitivity, Nernstian slope, linear range, faster

  10. Multiwall carbon nanotubes chemically modified carbon paste electrodes for determination of gentamicin sulfate in pharmaceutical preparations and biological fluids.

    Science.gov (United States)

    Khalil, M M; Abed El-Aziz, G M

    2016-02-01

    This article focused on the construction and characteristics of novel and sensitive gentamicin carbon paste electrodes which are based on the incorporation of multiwall carbon nanotubes (MWCNTs) which improve the characteristics of the electrodes. The electrodes were constructed based on gentamicin-phosphotungstate (GNS-PTA) called CPE1, gentamicin-phosphomolybdate (GNS-PMA) called CPE2, GNS-PTA+ MWMCNTs called MWCPE1, and GNS-PMA+ MWMCNTs called MWCPE2. The constructed electrodes, at optimum paste composition, exhibited good Nernstian response for determination of gentamicin sulfate (GNS) over a linear concentration range from 2.5×10(-6) to 1×10(-2), 3.0×10(-6) to 1×10(-2), 4.9×10(-7) to 1×10(-2) and 5.0×10(-7) to 1×10(-2)molL(-1), with lower detection limit 1×10(-6), 1×10(-6), 1.9×10(-7) and 2.2×10(-7)molL(-1), and with slope values of 29.0±0.4, 29.2±0.7, 31.2±0.5 and 31.0±0.6mV/decade for CPE1, CPE2, MWCPE1 and MWCPE2, respectively. The response of electrodes is not affected by pH in the range 3-8 for CPE1 and CPE2 and in the range 2.5-8.5 for MWCPE1 and MWCPE2. The results showed fast dynamic response time (about 8-5s) and long lifetime (more than 2months) for all electrodes. The sensors showed high selectivity for gentamicin sulfate (GNS) with respect to a large number of interfering species. The constructed electrodes were successfully applied for determination of GNS in pure form, its pharmaceutical preparations and biological fluids using standard addition and potentiometric titration methods with high accuracy and precision. Published by Elsevier B.V.

  11. Determinants of the Acceptance of Sustainable Production Strategies among Dairy Farmers: Development and Testing of a Modified Technology Acceptance Model

    Directory of Open Access Journals (Sweden)

    Simona Naspetti

    2017-10-01

    Full Text Available An extended version of the Technology Acceptance Model (TAM was applied by means of Structural Equation Modelling to testing various hypotheses on attitudes and intentions of dairy farmers towards three novel sustainable production strategies, as well as the influence of organic practices and collaborative behaviours, such as information sharing with supply-chain partners. Data on the acceptance of three sustainable production strategies, namely ‘Agro-forestry’, ‘Alternative protein source’, and ‘Prolonged maternal feeding’ were collected by a survey of dairy farmers in six European Union (EU countries (Austria, Belgium, Denmark, Finland, Italy, United Kingdom. We found that perceived usefulness is the key determinant of acceptance, while the intention to adopt a sustainable production strategy may derive from the influence of opinions (and behaviours of relevant others (e.g., leading dairy farmers, family members, advisors showing the role of interactions among farmers and other stakeholders in the adoption of innovations. Finally, the perceived usefulness of all of the investigated strategies is higher for organic farmers, while collaborative patterns reduce the impact of subjective norm on usefulness and overall acceptance. Our findings should encourage policy makers to consider the important role of supply chain management practices, including collaboration, to enhance the sustainability of dairy farming systems.

  12. MIPs-graphene nanoplatelets-MWCNTs modified glassy carbon electrode for the determination of cardiac troponin I.

    Science.gov (United States)

    Ma, Ya; Shen, Xiao-Lei; Wang, Hai-Shui; Tao, Jia; Huang, Jian-Zhi; Zeng, Qiang; Wang, Li-Shi

    2017-03-01

    An electrochemical sensor with high selectivity in addition to sensitivity was developed for the determination of cardiac troponin I (cTnI), based on the modification of cTnI imprinted polymer film on a glassy carbon electrode (GCE). The sensor was fabricated by layer-by-layer assembled graphene nanoplatelets (GS), multiwalled carbon nanotubes (MWCNTs), chitosan (CS), glutaraldehyde (GA) composites, which can increase the electronic transfer rate and the active surface area to capture a larger number of antigenic proteins. MWCNTs/GS based imprinted polymers (MIPs/MWCNTs/GS) were synthesized by means of methacrylic acid (MAA) as the monomer, ethylene glycol dimethacrylate (EGDMA) as the cross linker α,α'-azobisisobutyronitrile (AIBN) as the initiator and cTnI as the template. In comparison with conventional methods, the proposed electrochemical sensor is highly sensitive for cTnI, providing a better linear response range from 0.005 to 60 ng cm -3 and a lower limit of detection (LOD) of 0.0008 ng cm -3 under optimal experimental conditions. In addition, the electrochemical sensor exhibited good specificity, acceptable reproducibility and stability. Moreover, satisfactory results were obtained in real human serum samples, indicating that the developed method has the potential to find application in clinical detection of cTnI as an alternative approach. Copyright © 2016 Elsevier Inc. All rights reserved.

  13. Electrochemical Behaviour of Tinidazole at 1,4-Benzoquinone Modified Carbon Paste Electrode and Its Direct Determination in Pharmaceutical Tablets and Urine by Differential Pulse Voltammetry

    Directory of Open Access Journals (Sweden)

    Yosef Nikodimos

    2017-01-01

    Full Text Available A simple and highly sensitive electrochemical method based on a 1,4-benzoquinone modified carbon paste electrode (1,4-BQMCPE was described for the determination of tinidazole (TDZ. In Britton Robinson buffer solution, TDZ yields well-defined irreversible reduction peak at −0.344 V on a 1,4-BQMCPE. Compared with that on a bare CPE, the reduction peak of TDZ increased significantly on the modified CPE and the effects of different parameters on the voltammetric responses were also investigated. Differential pulse voltammetric method was proposed and optimized for TDZ determination and its reductive peak current response at 1,4-BQMCPE was found to show linear dependence on the concentration of TDZ in the range of 1.0 × 10−6 to 5.0 × 10−4 M with a linear regression equation, correlation coefficient, limit of detection (LOD, and limit of quantification (LOQ of IPC (μA = 0.19958 + 0.02657C (μM, 0.99486, 1.10 × 10−7 M, and 3.77 × 10−7, respectively. Excellent recovery results for spiked TDZ in pharmaceutical tablet samples ranging within 97.44–97.51% and in urine ranging within 95.37–96.91% were observed. The selectivity of the method for TDZ was further studied in the presence of selected potential interferents and confirmed the potential applicability of the developed method for the determination of TDZ.

  14. Rapid determination of 9 aromatic amines in mainstream cigarette smoke by modified dispersive liquid liquid microextraction and ultraperformance convergence chromatography tandem mass spectrometry.

    Science.gov (United States)

    Deng, Huimin; Yang, Fei; Li, Zhonghao; Bian, Zhaoyang; Fan, Ziyan; Wang, Ying; Liu, Shanshan; Tang, Gangling

    2017-07-21

    Aromatic amines in mainstream cigarette smoke have long been monitored due to their carcinogenic toxicity. In this work, a reliable and rapid method was developed for the simultaneous determination of 9 aromatic amines in mainstream cigarette smoke by modified dispersive liquid liquid microextraction (DLLME) and ultraperformance convergence chromatography tandem mass spectrometry (UPC 2 -MS/MS). Briefly, the particulate phase of the cigarette smoke was captured by a Cambridge filter pad, and diluted hydrogen chloride aqueous solution is employed to extract the aromatic amines under mechanical shaking. After alkalization with sodium hydroxide solution, small amount of toluene was introduced to further extract and enrich aromatic amines by modified DLLME under vortexing. After centrifugation, toluene phase was purified by a universal QuEChERS cleanup kit and was finally analyzed by UPC 2 -MS/MS. Attributing to the superior performance of UPC 2 -MS/MS, this novel approach allowed the separation and determination of 9 aromatic amines within 5.0min with satisfactory resolution and sensitivity. The proposed method was finally validated using Kentucky reference cigarette 3R4F, and emission levels of targeted aromatic amines determined were comparable to previously reported methods At three different spiked levels, the recoveries of most analytes were ranged from 74.01% to 120.50% with relative standard deviation (RSD) less than 12%, except that the recovery of p-toluidine at low spiked level and 3-aminobiphenyl at medium spiked level was 62.77% and 69.37% respectively. Thus, this work provides a novel alternative method for the simultaneous analysis of 9 aromatic amines in mainstream cigarette smoke. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. Optimization of modified carbon paste electrode with multiwalled carbon nanotube/ionic liquid/cauliflower-like gold nanostructures for simultaneous determination of ascorbic acid, dopamine and uric acid

    International Nuclear Information System (INIS)

    Afraz, Ahmadreza; Rafati, Amir Abbas; Najafi, Mojgan

    2014-01-01

    We describe the modification of a carbon paste electrode (CPE) with multiwalled carbon nanotubes (MWCNTs) and an ionic liquid (IL). Electrochemical studies by using a D-optimal mixture design in Design-Expert software revealed an optimized composition of 60% graphite, 14.2% paraffin, 10.8% MWCNT and 15% IL. The optimal modified CPE shows good electrochemical properties that are well matched with model prediction parameters. In the next step, the optimized CPE was modified with gold nanostructures by applying a double-pulse electrochemical technique. The resulting electrode was characterized by scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray diffraction, and electrochemical impedance spectroscopy. It gives three sharp and well-separated oxidation peaks for ascorbic acid (AA), dopamine (DA), and uric acid (UA). The sensor enables simultaneous determination of AA, DA and UA with linear responses from 0.3 to 285, 0.08 to 200, and 0.1 to 450 μM, respectively, and with 120, 30 and 30 nM detection limits (at an S/N of 3). The method was successfully applied to the determination of AA, DA, and UA in spiked samples of human serum and urine. - Highlights: • New method for simultaneous determination of AA, DA and UA was developed. • MWCNT/ionic liquid/cauliflower-like Au nanostructure was used for CPE modification. • Optimization of electrode composition was done by Design-Expert software. • The pH effect, peak separation mechanism and real samples was thoroughly studied

  16. Optimization of modified carbon paste electrode with multiwalled carbon nanotube/ionic liquid/cauliflower-like gold nanostructures for simultaneous determination of ascorbic acid, dopamine and uric acid

    Energy Technology Data Exchange (ETDEWEB)

    Afraz, Ahmadreza [Department of Physical Chemistry, Faculty of Chemistry, Bu-Ali Sina University, P.O. Box 65174, Hamedan (Iran, Islamic Republic of); Rafati, Amir Abbas, E-mail: aa_rafati@basu.ac.ir [Department of Physical Chemistry, Faculty of Chemistry, Bu-Ali Sina University, P.O. Box 65174, Hamedan (Iran, Islamic Republic of); Najafi, Mojgan [Department of Materials Engineering, Hamedan University of Technology (HUT), 65169 Hamedan (Iran, Islamic Republic of)

    2014-11-01

    We describe the modification of a carbon paste electrode (CPE) with multiwalled carbon nanotubes (MWCNTs) and an ionic liquid (IL). Electrochemical studies by using a D-optimal mixture design in Design-Expert software revealed an optimized composition of 60% graphite, 14.2% paraffin, 10.8% MWCNT and 15% IL. The optimal modified CPE shows good electrochemical properties that are well matched with model prediction parameters. In the next step, the optimized CPE was modified with gold nanostructures by applying a double-pulse electrochemical technique. The resulting electrode was characterized by scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray diffraction, and electrochemical impedance spectroscopy. It gives three sharp and well-separated oxidation peaks for ascorbic acid (AA), dopamine (DA), and uric acid (UA). The sensor enables simultaneous determination of AA, DA and UA with linear responses from 0.3 to 285, 0.08 to 200, and 0.1 to 450 μM, respectively, and with 120, 30 and 30 nM detection limits (at an S/N of 3). The method was successfully applied to the determination of AA, DA, and UA in spiked samples of human serum and urine. - Highlights: • New method for simultaneous determination of AA, DA and UA was developed. • MWCNT/ionic liquid/cauliflower-like Au nanostructure was used for CPE modification. • Optimization of electrode composition was done by Design-Expert software. • The pH effect, peak separation mechanism and real samples was thoroughly studied.

  17. The Cu-MOF-199/single-walled carbon nanotubes modified electrode for simultaneous determination of hydroquinone and catechol with extended linear ranges and lower detection limits

    International Nuclear Information System (INIS)

    Zhou, Jian; Li, Xi; Yang, Linlin; Yan, Songlin; Wang, Mengmeng; Cheng, Dan; Chen, Qi; Dong, Yulin; Liu, Peng; Cai, Weiquan; Zhang, Chaocan

    2015-01-01

    A novel electrochemical sensor based on Cu-MOF-199 [Cu-MOF-199 = Cu 3 (BTC) 2 (BTC = 1,3,5-benzenetricarboxylicacid)] and SWCNTs (single-walled carbon nanotubes) was fabricated for the simultaneous determination of hydroquinone (HQ) and catechol (CT). The modification procedure was carried out through casting SWCNTs on the bare glassy carbon electrode (GCE) and followed by the electrodeposition of Cu-MOF-199 on the SWCNTs modified electrode. Cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and scanning electron microscopy (SEM) were performed to characterize the electrochemical performance and surface characteristics of the as-prepared sensor. The composite electrode exhibited an excellent electrocatalytic activity with increased electrochemical signals towards the oxidation of HQ and CT, owing to the synergistic effect of SWCNTs and Cu-MOF-199. Under the optimized condition, the linear response range were from 0.1 to 1453 μmol L −1 (R HQ  = 0.9999) for HQ and 0.1–1150 μmol L −1 (R CT  = 0.9990) for CT. The detection limits for HQ and CT were as low as 0.08 and 0.1 μmol L −1 , respectively. Moreover, the modified electrode presented the good reproducibility and the excellent anti-interference performance. The analytical performance of the developed sensor for the simultaneous detection of HQ and CT had been evaluated in practical samples with satisfying results. - Highlights: • Cu-MOF-199/SWCNTs/GCE was facilely fabricated by the electrodeposition on SWCNTs/GCE. • An electrochemical sensor for detecting HQ and CT was constructed based on this modified electrode. • The proposed electrochemical sensor showed an extended linear range and lower detection limits. • The proposed electrochemical sensor had an excellent stability and reproducibility.

  18. Removal of acidic interferences in multi-pesticides residue analysis of fruits using modified magnetic nanoparticles prior to determination via ultra-HPLC-MS/MS

    International Nuclear Information System (INIS)

    Qi, Peipei; Wang, Zhiwei; Yang, Guiling; Wang, Xinquan; Shang, Chunqing; Xu, Hao; Wang, Xiangyun; Zhang, Hu; Wang, Qiang

    2015-01-01

    The authors describe magnetite (Fe 3 O 4 ) nanoparticles modified with 3-(N,N-diethylamino) propyltrimethoxysilane (Fe 3 O 4 -PSA NPs) for use as a sorbent for dispersive solid phase extraction of pesticide residues. The Fe 3 O 4 -PSA NPs were prepared by silanizing Fe 3 O 4 NPs and modifying them with 3-(N,N-diethylamino) propyltrimethoxysilane. Field-emission scanning electron microscopy, FTIR and zeta potential measurements were employed to characterize the modified NPs. They were then used as an adsorbent to remove acidic interferences (such as malic acid and succinic acid), which are major interferences in LC-MS/MS analysis in causing ion suppression in the MS spectra of pesticides. In addition, graphitized carbon black (GCB) was used as an adsorbent to eliminate interferences by pigments. The use of Fe 3 O 4 -PSA NPs can replace time-consuming centrifugation as used in the so-called QuEChERS (quick, easy, cheap, effective, rugged and safe) method. This improvement is particularly significant in high-throughput analysis. Following the optimization of the quantities of Fe 3 O 4 -PSA NPs and GCB, the method was applied to the determination of 56 pesticides in (spiked) fruits (apple, kiwi, orange and pear) by ultra-HPLC-MS/MS. The analytical ranges typically extend from 1 to 200 ng∙mL −1 , and recoveries range from 60.2 to 130 % at different concentrations of all four kinds of fruits. The LOQs for the pesticides are 10 ng∙kg −1 , which makes the method a viable tool for pesticide monitoring in fruits. (author)

  19. Clinical diagnostic value of determination of serum lschemia modified albumin, homocysteine and high-sensitivity C-reactive protein levels in patients with acute coronary syndrome

    International Nuclear Information System (INIS)

    Lu Weiqun; Jiang Donglin; Lu Weigu

    2009-01-01

    Objective: To study the clinical diagnostic value of determination of serum ischemia modified albumin (IMA), homocysteine (Hcy) and high-sensitivity C-reactive protein (hs-CRP) levels in patients with acute coronary syndrome (ACS). Methods: Serum IMA (with albumin-cobalt binding assay), Hcy (with ELISA) and hs-CRP (with RIA) levels were determined in 73 patients with ACS within 3 hours after onset of chest pain and 40 controls. Results: The sensitivity of IMA was 87.67%, the specificity was 100%. The area under curve of ROC was 0.985 (95% confidence interval 0.969 ∼ 1.001). All the figures were higher than those of Hcy and hs-CRP. Combined determination of IMA, Hcy and hs-CRP, would increass the sensitivity to 97.26%. Conclusion: IMA is one of the earliest sensitive indicators for clinical diagnosis of early myocardial ischemia in patients with ACS. Combined determination of IMA, Hcy and hs-CRP would be even more sensitive. (authors)

  20. Mixed ion-exchanger chemically modified carbon paste ion-selective electrodes for determination of triprolidine hydrochloride

    Directory of Open Access Journals (Sweden)

    Yousry M. Issa

    2010-01-01

    Full Text Available Triprolidine hydrochloride (TpCl ion-selective carbon paste electrodes were constructed using Tp-TPB/Tp-CoN and Tp-TPB/Tp-PTA as ion-exchangers. The two electrodes revealed Nernstian responses with slopes of 58.4 and 58.1 mV decade−1 at 25 °C in the ranges 6 × 10−6–1 × 10−2 and 2 × 10−5–1 × 10−2 M for Tp-TPB/Tp-CoN and Tp-TPB/Tp-PTA, respectively. The potentials of these electrodes were independent of pH in the ranges of 2.5–7.0 and 4.5–7.0, and detection limits were 6 × 10−6 and 1 × 10−5 M for Tp-TPB/Tp-CoN and Tp-TPB/Tp-PTA, respectively. The electrodes showed a very good selectivity for TpCl with respect to a large number of inorganic cations and compounds. The standard addition, potentiometric titration methods and FIA were applied to the determination of TpCl in pure solutions and pharmaceutical preparations. The results obtained were in close agreement with those found by the official method. The mean recovery values were 100.91% and 97.92% with low coefficient of variation values of 0.94%, and 0.56% in pure solutions, 99.82% and 98.53% with coefficient of variation values of 2.20%, and 0.73% for Actifed tablet and Actifed syrup, respectively, using the Tp-TPB/Tp-CoN electrode, and 98.85%, and 99.18% with coefficient of variation values of 0.48% and 0.85% for Actifed tablet and Actifed syrup, respectively, using the Tp-TPB/Tp-PTA electrode.

  1. Graphite furnace atomic absorption spectrometric determination of Ni and Pb in diesel and gasoline samples stabilized as microemulsion using conventional and permanent modifiers

    International Nuclear Information System (INIS)

    Matos Reyes, Mariela N.; Campos, Reinaldo C.

    2005-01-01

    A procedure for the graphite furnace atomic absorption spectrometric determination of Ni and Pb in diesel and gasoline samples was developed. Sample stabilization was necessary because of evident analyte losses that occurred immediately after sampling. Excellent long-term sample stabilization was observed by mixing different organic solvents with propan-1-ol and 50% vol/vol HNO 3 at a 3.3:6.5:1 volume ratio. For Pb, efficient thermal stabilization was obtained using aqueous Pd-Mg modifier as well as for Ir as permanent modifier. The drying temperature and ramp rate influenced the sensitivity obtained for Ni, and had to be carefully optimized. Taking this into account, the same sensitivity was attained in all investigated organic media stabilized as microemulsion. Thus, calibration with microemulsions prepared with a single organic solvent was possible, using aqueous or organic stock solutions. Commercial gasoline and diesel samples were directly analyzed after stabilization as microemulsion and by comparative UOP procedures. n-Hexane microemulsions were used for calibration, and good agreement was obtained between the results using the proposed and comparative procedures. Typical coefficients of variation (n = 6) ranged from 1% to 4%, and from 1% to 3% for Ni and Pb, respectively. Detection limits (k = 3) in the original gasoline or diesel samples, derived from 10 blank measurements, were 4.5 and 3.6 μg l -1 for Ni and Pb, respectively, comfortably below the values found in the analyzed samples

  2. Determination of residual nonsteroidal anti-inflammatory drugs in aqueous sample using magnetic nanoparticles modified with cetyltrimethylammonium bromide by high performance liquid chromatography.

    Science.gov (United States)

    Khoeini Sharifabadi, Malihe; Saber-Tehrani, Mohammad; Waqif Husain, Syed; Mehdinia, Ali; Aberoomand-Azar, Parviz

    2014-01-01

    A simple and sensitive solid-phase extraction method for separation and preconcentration of trace amount of four nonsteroidal anti-inflammatory drugs (naproxen, indomethacin, diclofenac, and ibuprofen) using Fe3O4 magnetic nanoparticles modified with cetyltrimethylammonium bromide has been developed. For this purpose, the surface of MNPs was modified with cetyltrimethylammonium bromide (CTAB) as a cationic surfactant. Effects of different parameters influencing the extraction efficiency of drugs including the pH, amount of salt, shaking time, eluent type, the volume of solvent, amount of adsorbent, sample volume, and the time of desorption were investigated and optimized. Methanol has been used as desorption solvent and the extracts were analysed on a reversed-phase octadecyl silica column using 0.02 M phosphate-buffer (pH = 6.02) acetonitrile (65 : 35 v/v) as the mobile phase and the effluents were measured at 202 nm with ultraviolet detector. The relative standard deviation (RSD%) of the method was investigated at three concentrations (25, 50, and 200 ng/mL) and was in the range of 3.98-9.83% (n = 6) for 50 ng/mL. The calibration curves obtained for studied drugs show reasonable linearity (R (2) > 0.99) and the limit of detection (LODs) ranged between 2 and 7 ng/mL. Finally, the proposed method has been effectively employed in extraction and determination of the drugs in biological and environmental samples.

  3. Study of the Analytical Conditions for the Determination of Cadmium in Coal Fly Ashes by GFAAS with evaluation of several matrix modifiers

    International Nuclear Information System (INIS)

    Rucandio, M.I.; Petit, M.D.

    1998-01-01

    A new method for the determination of cadmium in coal fly ash samples by Graphite Furnace Atomic Absorption Spectrometry (GFAAS) has been developed. Analytical conditions and different instrumental parameters have been optimized. In a first step, several types of matrix modifiers have been tested and a mixture of 2% NH 4 H 2 PO 4 with 0.4%Mg(NO 3 ) 2 in 0.5N HNO 3 has been selected, since it provides the highest sensitivity. In a second step, an optimization of several conditions, using the selected modifier, has been carried out, such as ashing and atomization temperatures, heating rate, etc. The influence of the use of a L' vov platform on the analytical and background signals has been studied, showing a significative decrease on the background signal, being the net absorbance similar to those obtained in absence of the platform. Using the optimal conditions, the direct method with standard samples provides cadmium concentration consistent with those obtained using the standard addition method. (Author) 18 refs

  4. Electrochemical immunosensor for the determination of insulin-like growth factor-1 using electrodes modified with carbon nanotubes-poly(pyrrole propionic acid) hybrids.

    Science.gov (United States)

    Serafín, V; Agüí, L; Yáñez-Sedeño, P; Pingarrón, J M

    2014-02-15

    An amperometric immunosensor for the determination of the hormone insulin-like growth factor 1 (IGF1) is reported for the first time in this work. As electrochemical transducer, a multiwalled carbon nanotubes-modified glassy carbon electrode on which poly(pyrrole propionic acid) was electropolymerized was prepared. This approach provided a high content of surface confined carboxyl groups suitable for direct covalent binding of anti-IGF1 monoclonal antibody. A sandwich-type immunoassay using a polyclonal antibody labeled with peroxidase, hydrogen peroxide as the enzyme substrate and catechol as redox mediator was employed to monitor the affinity reaction. All the variables involved in the preparation of the modified electrode were optimized and the electrodes were characterized by electrochemical impedance spectroscopy and cyclic voltammetry. Moreover, the different experimental variables affecting the amperometric response of the immunosensor were also optimized. The calibration graph for IGF1 showed a range of linearity extending from 0.5 to 1000 pg/mL, with a detection limit, 0.25 pg/mL, more than 100 times lower than the lowest values reported for the ELISA immunoassays available for IGF1 (30 pg/mL, approximately). Excellent reproducibility for the measurements carried out with different immunosensors and selectivity against other hormones were also evidenced. A commercial human serum spiked with IGF1 at different levels between 0.01 and 10.0 ng/mL was analyzed with good results. © 2013 Elsevier B.V. All rights reserved.

  5. Multiplexed determination of human growth hormone and prolactin at a label free electrochemical immunosensor using dual carbon nanotube-screen printed electrodes modified with gold and PEDOT nanoparticles.

    Science.gov (United States)

    Serafín, V; Martínez-García, G; Agüí, L; Yáñez-Sedeño, P; Pingarrón, J M

    2014-09-21

    A label-free dual electrochemical immunosensor was constructed for the multiplexed determination of human growth (hGH) and prolactin (PRL) hormones. The immunosensor used an electrochemical platform composed of carbon nanotube-screen printed carbon electrodes (CNT/SPCEs) modified with poly(ethylene-dioxythiophene) (PEDOT) and gold nanoparticles, on which the corresponding hGH and PRL antibodies were immobilized. The affinity reactions were monitored by measuring the decrease in the differential pulse voltammetric oxidation response of the redox probe dopamine. The experimental variables involved in the preparation of both AuNP/PEDOT/CNT/SPC modified electrodes and the dual immunosensor were optimized. The immunosensor exhibited an improved analytical performance for hGH and PRL with respect to other electrochemical immunosensor designs, showing wide ranges of linearity and low detection limits of 4.4 and 0.22 pg mL(-1), respectively. An excellent selectivity against other hormones and in the presence of ascorbic and uric acids was found. The usefulness of the dual immunosensor for the simultaneous analysis of hGH and PRL was demonstrated by analyzing human serum and saliva samples spiked with the hormones at different concentration levels.

  6. Dual-opposite multi-walled carbon nanotube modified carbon fiber microelectrode for microfluidic chip-capillary electrophoresis determination of methyl parathion metabolites in human urine.

    Science.gov (United States)

    Du, Fuying; Fung, Ying-Sing

    2018-03-03

    Methyl parathion (MP) is a highly toxic organophosphate and its exposure may lead to substantial adverse effects to human health. The existence of 4-nitrophenol (4-NP) in the form of free phenol, glucuronide (4-NP-G) or as a sulfate ester (4-NP-S) can be used as biomarkers to assess the duration and extent of MP exposure. In this work, a MC-CE device incorporating post-CE amperometric detection using multi-walled carbon nanotubes (MWNTs) modified carbon fiber microelectrode (CFME) was fabricated and assessed for simultaneous determination of 4-NP, 4-NP-G, and 4-NP-S in human urine. The detection sensitivity and stability was greatly enhanced by the modification of MWNTs. The capability of the MC-CE device with dual MWNTs modified CFME for detecting impurity was assessed and reliability established by high recoveries from 95 to 97% for spiked MP biomarkers. The method developed is shown to provide a simple, sensitive, and reliable means for monitoring 4-NP, 4-NP-G, and 4-NP-S in human urine. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Voltammetric determination of nitric oxide using a glassy carbon electrode modified with a nanohybrid consisting of myoglobin, gold nanorods, and reduced graphene oxide

    International Nuclear Information System (INIS)

    Marlinda, Ab Rahman; Jayabal, Subramaniam; Yusoff, Norazriena; Huang, Nay Ming; Pandikumar, Alagarsamy; Suriani, Abu Bakar

    2016-01-01

    Myoglobin-modified gold nanorods incorporating reduced graphene oxide (rGO) were fabricated and deposited on a glassy carbon electrode (GCE) to obtain a sensor for nitric oxide (NO). The Mb-AuNR/rGO nanohybrid showed a transverse localized surface plasmon resonance (LSPR) band with a peak at 508 nm, and a longitudinal LSPR band at 724 nm. The AuNRs have an average length of 38 ± 3 nm and a width of 11 ± 1 nm. The GCE modified with the nanohybrid is shown to be a viable sensor for the determination of NO by linear sweep voltammetry. Its electrocatalytic response toward the oxidation of NO is distinctly enhanced compared to other electrodes. The sensor, best operated at a working voltage of 0.85 V (vs. SCE), showed two linear response ranges (from 10 to 100 μM, and from 100 to 1000 μM), with a detection limit of 5.5 μM. Furthermore, it exhibits excellent selectivity for NO over common interferents such as NaNO 3 , and also over electroactive species such as ascorbate, dopamine, glucose, and uric acid. These properties make it a promising tool for the detection of NO in situations such as capillary and pulmonary hypertension and embolism, and during vasodilation. (author)

  8. High-performance liquid chromatography using reversed-phase stationary phases dynamically modified with organophosphorus compound for the separation and determination of lanthanoid elements

    International Nuclear Information System (INIS)

    Tsuyoshi, Akira; Akiba, Kenichi

    2000-01-01

    An acidic organophosphorus compound, 2-ethylhexylphosphonic acid mono-2-ethlhexyl ester (EHPA), has been applied to reversed-phase high-performance liquid chromatography (RP-HPLC). The reversed-phase stationary phase was dynamically modified with EHPA by flowing the mobile phase of an acetone-water mixture containing the extracting regent. The retention of lanthanoid elements was widely varied by changing the conditions of the mobile phase, i.e., the pH, the EHPA concentration and the acetone content. The selectivity of EHPA is well reflected to the chromatographic systems, and a precise separation of lanthanoid elements was achieved with sufficient resolution. The determination of Sm was examined in the presence of a large amount of Nd. A linear calibration graph was obtained for Sm at the level of 10 -7 mol dm -3 , in the presence of 1x10 -4 mol dm -3 of Nd. (author)

  9. A modified energy transfer model for determination of upconversion emission of β-NaYF{sub 4}:Yb,Er: Role of self-quenching effect

    Energy Technology Data Exchange (ETDEWEB)

    Zhu, Hongyuan [The Key Laboratory of Biomedical Information Engineering, Ministry of Education, School of Life Science and Technology, Xi' an Jiaotong University, Xi’an 710049 (China); Bioinspired Engineering and Biomechanics Center (BEBC), Xi’an Jiaotong University, Xi’an 710049 (China); Lin, Min, E-mail: minlin@mail.xjtu.edu.cn [The Key Laboratory of Biomedical Information Engineering, Ministry of Education, School of Life Science and Technology, Xi' an Jiaotong University, Xi’an 710049 (China); Bioinspired Engineering and Biomechanics Center (BEBC), Xi’an Jiaotong University, Xi’an 710049 (China); Jin, Guorui [The Key Laboratory of Biomedical Information Engineering, Ministry of Education, School of Life Science and Technology, Xi' an Jiaotong University, Xi’an 710049 (China); Bioinspired Engineering and Biomechanics Center (BEBC), Xi’an Jiaotong University, Xi’an 710049 (China); Lu, Tian Jian [Bioinspired Engineering and Biomechanics Center (BEBC), Xi’an Jiaotong University, Xi’an 710049 (China); Xu, Feng [The Key Laboratory of Biomedical Information Engineering, Ministry of Education, School of Life Science and Technology, Xi' an Jiaotong University, Xi’an 710049 (China); Bioinspired Engineering and Biomechanics Center (BEBC), Xi’an Jiaotong University, Xi’an 710049 (China)

    2017-05-15

    A modified energy transfer model by incorporating self-quenching effect is introduced to determine upconversion emission of β-NaYF{sub 4}:Yb,Er. The simulation results agree well with existing experimental results, demonstrating the critical role of self-quenching effect in upconversion emission. Our results confirm that a 4.4-fold increase of green upconversion and 86-fold increase in the intensity of red upconversion emission could be realized by suppressing self-quenching. In addition, the optimal doping concentrations for integral emission intensity are found to be independent of excitation power, while the green to red ratio is found to rely significantly on excitation power. Our model offers mechanistic insight into upconversion emission processes and provides inspirations in improving upconversion emission efficiency through optimization of energy transfer pathways in different types of matrix sub-lattice.

  10. A glassy carbon electrode modified with a nickel(II) norcorrole complex and carbon nanotubes for simultaneous or individual determination of ascorbic acid, dopamine, and uric acid

    International Nuclear Information System (INIS)

    Deng, Keqin; Li, Xiaofang; Huang, Haowen

    2016-01-01

    The authors report on the synthesis of a hybrid material consisting of the porphyrinoid metal complex nickel(II) norcorrole that was noncovalently bound to carbon nanotubes (CNT-NiNC). The hybrid was characterized by UV–vis, FTIR spectroscopy, and thermogravimetric analysis. The CNT-NiNC hybrid possesses high catalytic activity and selectivity toward the oxidation of ascorbic acid, dopamine, and uric acid. It was used to modify a glassy carbon electrode which then is shown to enable simultaneous or individual determination of ascorbic acid (AA), dopamine (DA), and uric acid (UA) at pH 6.5 and typical working potentials of −70, 200 and 380 mV (vs. SCE). The detection limits (at an SNR of 3) are 2.0 μM for AA, 0.1 μM for DA, and 0.4 μM for UA. (author)

  11. Determination of two-liquid mixture composition by assessing its dielectric parameters 2. modified measuring system for monitoring the dehydration process of bioethanol production

    Directory of Open Access Journals (Sweden)

    Vilitis O.

    2014-02-01

    Full Text Available In Part 2 of the work we describe a modified measuring system for precise monitoring of the dehydration process of bioethanol production. This is based on the earlier proposed system for measuring the concentration of solutions and two-liquid mixtures using devices with capacitive sensors (1-300pF, which provides a stable measuring resolution of ± 0.005 pF at measuring the capacitance of a sensor. In this part of our work we determine additional requirements that are to be imposed on the measuring system at monitoring the ethanol dehydration process and control of bioethanol production. The most important parameters of the developed measuring system are identified. An exemplary calculation is given for the thermocompensated calibration of measuring devices. The results of tests have shown a good performance of the developed measuring system.

  12. Determination of vanadium(V) by direct automatic potentiometric titration with EDTA using a chemically modified electrode as a potentiometric sensor.

    Science.gov (United States)

    Quintar, S E; Santagata, J P; Cortinez, V A

    2005-10-15

    A chemically modified electrode (CME) was prepared and studied as a potentiometric sensor for the end-point detection in the automatic titration of vanadium(V) with EDTA. The CME was constructed with a paste prepared by mixing spectral-grade graphite powder, Nujol oil and N-2-naphthoyl-N-p-tolylhydroxamic acid (NTHA). Buffer systems, pH effects and the concentration range were studied. Interference ions were separated by applying a liquid-liquid extraction procedure. The CME did not require any special conditioning before using. The electrode was constructed with very inexpensive materials and was easily made. It could be continuously used, at least two months without removing the paste. Automatic potentiometric titration curves were obtained for V(V) within 5 x 10(-5) to 2 x 10(-3)M with acceptable accuracy and precision. The developed method was applied to V(V) determination in alloys for hip prosthesis.

  13. Simultaneous determination of 2,4,6-trichlorophenol and pentachlorophenol based on poly(Rhodamine B)/graphene oxide/multiwalled carbon nanotubes composite film modified electrode

    International Nuclear Information System (INIS)

    Zhu, Xiaolin; Zhang, Kexin; Lu, Nan; Yuan, Xing

    2016-01-01

    Graphical abstract: A poly(Rhodamine B)/graphene oxide/multiwalled carbon nanotubes composite film modified glassy carbon electrode (PRhB/GO/MWCNTs/GCE) was developed for the simultaneous determination of 2,4,6-trichlorophenol (2,4,6-TCP) and pentachlorophenol (PCP) without any pretreatment. - Highlights: • A poly(RhB)/graphene oxide/multiwalled carbon nanotubes composite was synthesized. • The composite film was characterized by SEM, XRD, EIS and Raman spectroscopy. • The simultaneous electrochemical determination of 2,4,6-TCP and PCP was realized. • The electrode showed high sensitivity, excellent reproducibility and good stability. • The electrode was used to determine 2,4,6-TCP and PCP in practical water samples. - Abstract: In the present study, a poly(Rhodamine B)/graphene oxide/multiwalled carbon nanotubes nanocomposite modified glass carbon electrode (PRhB/GO/MWCNTs/GCE) was developed for the simultaneous determination of 2,4,6-trichlorophenol (2,4,6-TCP) and pentachlorophenol (PCP). The PRhB/GO/MWCNTs film was extensively characterized by emission scanning electron microscopy (SEM), X-ray diffraction (XRD), Raman spectroscopy and electrochemical impedance spectroscopy (EIS). The electrochemical behaviors of 2,4,6-TCP and PCP were investigated by cyclic voltammetry, linear sweep voltammetry and differential pulse voltammetry. Due to the synergistic effect, the PRhB/GO/MWCNTs/GCE significantly facilitated the simultaneous electro-oxidation of 2,4,6-TCP and PCP with peak potential difference of 160 mV and enhanced oxidation currents. Under optimum conditions, the oxidation current of 2,4,6-TCP was linear to its concentration in the ranges of 4.0 × 10"−"9 to 1.0 × 10"−"7 M and 1.0 × 10"−"7 to 1.0 × 10"−"4 M with the detection limit (S/N = 3) of 8.0 × 10"−"1"0 M. And the linear concentration ranges for PCP were 2.0 × 10"−"9 to 1.0 × 10"−"7 M and 1.0 × 10"−"7 to 9.0 × 10"−"5 M with the detection limit of 5.0 × 10"−"1"0 M

  14. Simultaneous determination of 2,4,6-trichlorophenol and pentachlorophenol based on poly(Rhodamine B)/graphene oxide/multiwalled carbon nanotubes composite film modified electrode

    Energy Technology Data Exchange (ETDEWEB)

    Zhu, Xiaolin; Zhang, Kexin; Lu, Nan; Yuan, Xing, E-mail: yuanx@nenu.edu.cn

    2016-01-15

    Graphical abstract: A poly(Rhodamine B)/graphene oxide/multiwalled carbon nanotubes composite film modified glassy carbon electrode (PRhB/GO/MWCNTs/GCE) was developed for the simultaneous determination of 2,4,6-trichlorophenol (2,4,6-TCP) and pentachlorophenol (PCP) without any pretreatment. - Highlights: • A poly(RhB)/graphene oxide/multiwalled carbon nanotubes composite was synthesized. • The composite film was characterized by SEM, XRD, EIS and Raman spectroscopy. • The simultaneous electrochemical determination of 2,4,6-TCP and PCP was realized. • The electrode showed high sensitivity, excellent reproducibility and good stability. • The electrode was used to determine 2,4,6-TCP and PCP in practical water samples. - Abstract: In the present study, a poly(Rhodamine B)/graphene oxide/multiwalled carbon nanotubes nanocomposite modified glass carbon electrode (PRhB/GO/MWCNTs/GCE) was developed for the simultaneous determination of 2,4,6-trichlorophenol (2,4,6-TCP) and pentachlorophenol (PCP). The PRhB/GO/MWCNTs film was extensively characterized by emission scanning electron microscopy (SEM), X-ray diffraction (XRD), Raman spectroscopy and electrochemical impedance spectroscopy (EIS). The electrochemical behaviors of 2,4,6-TCP and PCP were investigated by cyclic voltammetry, linear sweep voltammetry and differential pulse voltammetry. Due to the synergistic effect, the PRhB/GO/MWCNTs/GCE significantly facilitated the simultaneous electro-oxidation of 2,4,6-TCP and PCP with peak potential difference of 160 mV and enhanced oxidation currents. Under optimum conditions, the oxidation current of 2,4,6-TCP was linear to its concentration in the ranges of 4.0 × 10{sup −9} to 1.0 × 10{sup −7} M and 1.0 × 10{sup −7} to 1.0 × 10{sup −4} M with the detection limit (S/N = 3) of 8.0 × 10{sup −10} M. And the linear concentration ranges for PCP were 2.0 × 10{sup −9} to 1.0 × 10{sup −7} M and 1.0 × 10{sup −7} to 9.0 × 10{sup −5} M with the

  15. A screen-printed carbon electrode modified with gold nanoparticles, poly(3,4-ethylenedioxythiophene), poly(styrene sulfonate) and a molecular imprint for voltammetric determination of nitrofurantoin.

    Science.gov (United States)

    Dechtrirat, Decha; Yingyuad, Peerada; Prajongtat, Pongthep; Chuenchom, Laemthong; Sriprachuabwong, Chakrit; Tuantranont, Adisorn; Tang, I-Ming

    2018-04-23

    A molecularly imprinted polymer (MIP) and a nanocomposite prepared from gold nanoparticles (AuNP) and poly(3,4-ethylenedioxythiophene)/poly(styrene sulfonate) (PEDOT:PSS) were deposited on a screen-printed carbon electrode (SPCE). The nanocomposite was prepared by one-pot simultaneous in-situ formation of AuNPs and PEDOT:PSS and was then inkjet-coated onto the SPCE. The MIP film was subsequently placed on the modified SPCE by co-electrodeposition of o-phenylenediamine and resorcinol in the presence of the antibiotic nitrofurantoin (NFT). Using differential pulse voltammetry (DPV), response at the potential of ~ 0.1 V (vs. Ag/AgCl) is linear in 1 nM to 1000 nM NFT concentration range, with a remarkably low detection limit (at S/N = 3) of 0.1 nM. This is two orders of magnitude lower than that of the control MIP sensor without the nanocomposite interlayer, thus showing the beneficial effect of AuNP-PEDOT:PSS. The electrode is highly reproducible (relative standard deviation 3.1% for n = 6) and selective over structurally related molecules. It can be re-used for at least ten times and was found to be stable for at least 45 days. It was successfully applied to the determination of NFT in (spiked) feed matrices and gave good recoveries. Graphical abstract Schematic representation of a voltammetric sensor for the determination of nitrofurantoin. The sensor is based on a screen-printed carbon electrode (SPCE) modified with an inkjet-printed gold nanoparticles-poly(3,4-ethylenedioxythiophene):poly(styrene sulfonate) nanocomposite and a molecularly imprinted polymer.

  16. An ultrasensitive and selective electrochemical sensor for determination of estrone 3-sulfate sodium salt based on molecularly imprinted polymer modified carbon paste electrode.

    Science.gov (United States)

    Song, Han; Wang, Yuli; Zhang, Lu; Tian, Liping; Luo, Jun; Zhao, Na; Han, Yajie; Zhao, Feilang; Ying, Xue; Li, Yingchun

    2017-11-01

    A highly sensitive and selective electrochemical sensor based on carbon paste electrode (CPE) modified with molecularly imprinted polymers (MIPs) has been developed for the determination of estrone 3-sulfate sodium salt (ESS). MIPs were prepared in polar medium via bulk polymerization and characterized by scanning electron microscopy and infrared spectroscopy. Cyclic voltammetry was performed to the study preparation process and binding behavior of the MIP-modified CPE (MIP/CPE) toward ESS. The conditions for preparing MIPs and MIP/CPE as well as ESS detection were optimized. Under the optimal experimental conditions, the detection linear range for ESS is 4 × 10 -12 to 6 × 10 -9  M with a limit of detection of 1.18 × 10 -12  M (S/N = 3). In addition, the sensor exhibits high binding affinity toward ESS over its structural analogues with excellent repeatability and stability. The fabricated MIP/CPE was then successfully employed to detect ESS in pregnant mare urine (PMU) without any pretreatment, and the average recoveries were from 99.6 to 104.9% with relative standard deviation less than 3.0%. High-performance liquid chromatography was adopted as a reference to validate the established approach in detecting ESS and their results showed good agreement. The as-prepared sensor has high potential to be a decent tool for on-site determination of ESS in PMU in a fast and convenient manner. Graphical Abstract ᅟ.

  17. Square-wave voltammetric determination of rutin in pharmaceutical formulations using a carbon composite electrode modified with copper (II phosphate immobilized in polyester resin

    Directory of Open Access Journals (Sweden)

    Kellen Heloizy Garcia Freitas

    2012-12-01

    Full Text Available A carbon composite electrode modified with copper (II phosphate immobilized in a polyester resin (Cu3(PO42-Poly for the determination of rutin in pharmaceutical samples by square-wave voltammetry is described herein. The modified electrode allows the determination of rutin at a potential (0.20 V vs. Ag/AgCl (3.0 mol L-1 KCl lower than that observed at an unmodified electrode. The peak current was found to be linear to the rutin concentration in the range from 9.9 × 10-8 to 2.5 × 10-6 mol L-1, with a detection limit of 1.2×10-8 mol L-1. The response of the electrode was stable, with no variation in baseline levels within several hours of continuous operation. The surface morphology of the modified electrode was characterized by scanning electron microscopy (SEM and energy dispersive X-ray (EDX system. The results obtained are precise and accurate. In addition, these results are in agreement with those obtained by the chromatographic method at a 95% confidence level.Descreve-se um eletrodo de carbono modificado com fosfato de cobre (II imobilizado em uma resina de poliéster (Cu3(PO42-Poly para a determinação de rutina em amostras farmacêuticas por voltametria de onda quadrada. O eletrodo modificado permite a determinação de rutina em potencial (0.20 V vs Ag / AgCl (3,0 mol L-1 KCl menor que o observado em um eletrodo não modificado. Verificou-se que a corrente de pico foi linear com a concentração de rutina na faixa de 9,9 × 10-8 a 2,5 × 10-6 mol L-1, com um limite de detecção de 1,2 × 10-8 mol L¹. A resposta do eletrodo foi estável, sem variação significativa dentro de várias horas de operação contínua. A morfologia da superfície do eletrodo modificado foi caracterizada por microscopia eletrônica de varredura (MEV e pelo sistema de energia dispersiva de raios-X (EDX. Os resultados obtidos foram precisos e exatos. Ademais, estes resultados estão de acordo com aqueles obtidos pelo método cromatográfico a um nível de

  18. Gold-copper bimetallic nanoparticles supported on nano P zeolite modified carbon paste electrode as an efficient electrocatalyst and sensitive sensor for determination of hydrazine.

    Science.gov (United States)

    Amiripour, Fatemeh; Azizi, Seyed Naser; Ghasemi, Shahram

    2018-06-01

    In this report, a facile, efficient and low cost electrochemical sensor based on bimetallic Au-Cu nanoparticles supported on P nanozeolite modified carbon paste electrode (Au-Cu/NPZ/CPE) was constructed and its efficiency for determination of hydrazine in trace level was studied. For this purpose, agro waste material, stem sweep ash (SSA) was employed as the starting material (silica source) for the synthesis of nano P zeolite (NPZ). After characterization of the synthesized NPZ by analytical instruments (scanning electronic microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectroscopy), construction of Au-Cu/NPZ/CPE was performed by three steps procedure involving preparation of nano P zeolite modified carbon paste electrode (NPZ/CPE), introducing Cu +2 ions into nano zeolite structure by ion exchange and electrochemical reduction of Cu +2 ions upon applying constant potential. This procedure is followed by partial replacement of Cu by Au due to galvanic replacement reaction (GRR). The electrochemical properties of hydrazine at the surface of Au-Cu/NPZ/CPE was evaluated using cyclic voltammetry (CV), amperometry, and chronoamperometry methods in 0.1 M phosphate buffer solution (PBS). It was found that the prepared sensor has higher electrocatalytic activity at a relatively lower potential compared to other modified electrodes including Au/NPZ/CPE, Cu/NPZ/CPE, Au-Cu/CPE and etc. Moreover, the proposed electrochemical sensor presented the favorable analytical properties for determination of hydrazine such as low detection limit (0.04 µM), rapid response time (3 s), wide linear range (0.01-150 mM), and high sensitivity (99.53 µA mM -1 ) that are related to the synergic effect of bimetallic of Au-Cu, porous structure and enough surface area of NPZ. In addition, capability of Au-Cu/NPZ/CPE sensor was successfully tested in real samples with good accuracy and precision. Copyright

  19. Electrocatalytic Oxidation of Venlafaxine at a Multiwall Carbon Nanotubes-Ionic Liquid Gel Modified Glassy Carbon Electrode and Its Electrochemical Determination

    Directory of Open Access Journals (Sweden)

    Ling Ding

    2015-03-01

    Full Text Available The electrocatalytic oxidation of venlafaxine (VEN was investigated at a glassy carbon electrode (GCE, the modified electrode by a gel containing multiwall carbon nanotubes (MWCNTs and a room-temperature ionic liquid (RTIL, 1-butyl-3-methylimidazolium hexafluorophate (BMIMPF6 in 0.10 mol L−1 phosphate buffer solution (PBS, pH 6.8. It was found that an irreversible anodic oxidation peak of VEN with the peak potential (Epa as 0.780 V appeared at MWCNTs-RTIL/GCE. The electrode reaction process was a diffusion-controlled one and the electrochemical oxidation involved two electrons transferring and two protons participation. Furthermore, the charge-transfer coefficient (α, and the electrode reaction rate constant (kf of VEN were found to be 0.91 and 3.04×10−2 s−1, respectively. Under the optimized conditions, the electrocatalytic oxidation peak currents were linearly dependent on the concentration of VEN in the concentration range from 2.0×10−6 mol L−1 ~ 2.0×10−3 mol L−1 with the limit of detection (S / N = 3 as 1.69×10−6 mol L−1. The proposed method has been successfully applied in the electrochemical quantitative determination of VEN content in commercial venlafaxine hydrochloride capsules and the determination results could meet the requirement of the quantitative determination.

  20. Determination of Silver(I by Differential Pulse Voltammetry Using a Glassy Carbon Electrode Modified with Synthesized N-(2-Aminoethyl-4,4'-Bipyridine

    Directory of Open Access Journals (Sweden)

    Gabriel Lucian Radu

    2010-12-01

    Full Text Available A new modified glassy carbon electrode (GCE based on a synthesized N-(2-aminoethyl-4,4'-bipyridine (ABP was developed for the determination of Ag(I by differential pulse voltammetry (DPV. ABP was covalently immobilized on GC electrodes surface using 4-nitrobenzendiazonium (4-NBD and glutaraldehyde (GA. The Ag(I ions were preconcentrated by chemical interaction with bipyridine under a negative potential (−0.6 V; then the reduced ions were oxidized by differential pulse voltammetry and a peak was observed at 0.34 V. The calibration curve was linear in the concentration range from 0.05 μM to 1 μM Ag(I with a detection limit of 0.025 μM and RSD = 3.6%, for 0.4 μM Ag(I. The presence of several common ions in more than 125-fold excess had no effect on the determination of Ag(I. The developed sensor was applied to the determination of Ag(I in water samples using a standard addition method.

  1. Evaluation of a carbon paste electrode modified with Strontium substituted bismuth and titanium oxide nanoparticles in the toxic metal chromium (VI determination potentiometric method

    Directory of Open Access Journals (Sweden)

    Atefeh Badri

    2016-09-01

    Full Text Available Strontium substituted bismuth and titanium oxide nanoparticles with aurivillius morphology synthesized by chemical co-precipitation method and were characterized using XRD. The nanopartcles were used in the composition of the carbon paste to improve conductivity and transduction of chemical signal to electrical signal. A procedure for the determination of chromium is described based on pre-concentration of the dichromate anion at a carbon paste electrode modified. A novel potentiometric Cr6+carbon paste electrode incorporating Strontium substituted bismuth and titanium oxide nanoparticles (SSBTO. Ina acetate buffer solution of pH 5, the sensor displays a rapid and linear response for Cr6+ over the concentration range 1.0×10-5 to 1.0×10-1mol L-1 M with an anionic slope of 54.8± 0.2 mV decade ’ and a detection limit of the order of0.002 /µg ml ‘. The sensor is used for determination of Cr6+ by direct monitoring of Cr6+.The average recoveries of Cr6+at concentration levels of 0.5~40 pg/ml ’is 98.3. The electrode has a short response time (<6s and can be used for at least twenty days without any considerable divergence in potentials and the working pH range was 4.5-6.5. The proposed electrode was successfully used as an indicator for potentiometric determination of Cr6+in water sample.

  2. Electrochemical behavior and voltammetric determination of vanillin based on an acetylene black paste electrode modified with graphene-polyvinylpyrrolidone composite film.

    Science.gov (United States)

    Deng, Peihong; Xu, Zhifeng; Zeng, Rongying; Ding, Chunxia

    2015-08-01

    The graphene-polyvinylpyrrolidone composite film modified acetylene black paste electrode (GR-PVP/ABPE) was fabricated and used to determine vanillin. In 0.1M H3PO4 solution, the oxidation peak current of vanillin increased significantly at GR-PVP/ABPE compared with bare ABPE, PVP/ABPE and GR/ABPE. The oxidation mechanism was discussed. The experimental conditions that exert influence on the voltammetric determination of vanillin, such as supporting electrolytes, pH values, accumulation potential and accumulation time, were optimized. Besides, the interference, repeatability, reproducibility and stability measurements were also evaluated. Under the optimal experimental conditions, the oxidation peak current was proportional to vanillin concentration in the range of 0.02-2.0 μM, 2.0-40 μM and 40-100 μM. The detection limit was 10nM. This sensor was used successfully for vanillin determination in various food samples. Copyright © 2015 Elsevier Ltd. All rights reserved.

  3. An electrochemical sensor for warfarin determination based on covalent immobilization of quantum dots onto carboxylated multiwalled carbon nanotubes and chitosan composite film modified electrode

    International Nuclear Information System (INIS)

    Gholivand, Mohammad Bagher; Mohammadi-Behzad, Leila

    2015-01-01

    A method is described for the construction of a novel electrochemical warfarin sensor based on covalent immobilization of CdS-quantum dots (CdS-QDs) onto carboxylated multiwalled carbon nanotubes/chitosan (CS) composite film on the surface of a glassy carbon electrode. The CdS-QDs/CS/MWCNTs were characterized by field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), Fourier transform infra-red (FTIR) spectroscopy, XRD analysis and electrochemical impedance spectroscopy (EIS). The sensor showed optimum anodic stripping response within 90 s at an accumulation potential of 0.75 V. The modified electrode was used to detect the concentration of warfarin with a wide linear range of 0.05–80 μM and a detection limit (S/N = 3) of 8.5 nM. The proposed sensor has good storage stability, repeatability and reproducibility and was successfully applied for the determination of warfarin in real samples such as urine, serum and milk. - Highlights: • A new sensitive sensor for warfarin determination was developed. • The sensor was constructed based on covalent immobilization of CdS-QDs on the chitosan/MWCNTs/GCE. • The parameters affecting the stripping analysis of warfarin were optimized. • The proposed sensor is used for trace determination of warfarin in urine, serum and milk

  4. Sensitive determination of glucose in Dulbecco's modified Eagle medium by high-performance liquid chromatography with 1-phenyl-3-methyl-5-pyrazolone derivatization: application to gluconeogenesis studies.

    Science.gov (United States)

    Ling, Zhaoli; Xu, Ping; Zhong, Zeyu; Wang, Fan; Shu, Nan; Zhang, Ji; Tang, Xiange; Liu, Li; Liu, Xiaodong

    2016-04-01

    A new pre-column derivative high-performance liquid chromatography (HPLC) method for determination of d-glucose with 3-O-methyl-d-glucose (3-OMG) as the internal standard was developed and validated in order to study the gluconeogenesis in HepG2 cells. Samples were derivatized with 1-phenyl-3-methy-5-pyrazolone at 70°C for 50 min. Glucose and 3-OMG were extracted by liquid-liquid extraction and separated on a YMC-Triart C18 column, with a gradient mobile phase composed of acetonitrile and 20 mm ammonium acetate solution containing 0.09% tri-ethylamine at a flow rate of 1.0 mL/min. The eluate were detected using a UV detector at 250 nm. The assay was linear over the range 0.39-25 μm (R(2) = 0.9997, n = 5) and the lower limit of quantitation was 0.39 μm (0.070 mg/mL). Intra- and inter-day precision and accuracy were gluconeogenesis in Dulbecco's modified Eagle medium (DMEM) cultured HepG2 cells. Glucose concentration was determined to be about 1-2.5 μm in this gluconeogenesis assay. In conclusion, this method has been shown to determine small amounts of glucose in DMEM successfully, with lower limit of quantitation and better sensitivity when compared with common commercial glucose assay kits. Copyright © 2015 John Wiley & Sons, Ltd.

  5. Mercury-free simultaneous determination of cadmium and lead at a glassy carbon electrode modified with multi-wall carbon nanotubes

    International Nuclear Information System (INIS)

    Wu Kangbing; Hu Shengshui; Fei Junjie; Bai Wen

    2003-01-01

    A multi-wall carbon nanotube (MWNT) modified glassy carbon electrode (GCE) was described for the simultaneous determination of trace levels of cadmium and lead by anodic stripping voltammetry (ASV). In pH 4.5 NaAc-HAc buffer containing 0.02 mol/l KI, Cd 2+ and Pb 2+ first adsorb onto the surface of a MWNT film coated GCE and then reduce at -1.20 V. During the positive potential sweep, reduced cadmium and lead were oxidized, and two well-defined stripping peaks appeared at -0.88 and -0.62 V. Compared with a bare GCE, a MWNT film coated GCE greatly improves the sensitivity of determining cadmium and lead. Low concentration of I - significantly enhances the stripping peak currents since it induces Cd 2+ and Pb 2+ to adsorb at the electrode surface. The striping peak currents change linearly with the concentration of Cd 2+ from 2.5x10 -8 to 1x10 -5 mol/l and with that of Pb 2+ from 2x10 -8 to 1x10 -5 mol/l. The lowest detectable concentrations of Cd 2+ and Pb 2+ are estimated to be 6x10 -9 and 4x10 -9 mol/l, respectively. The high sensitivity, selectivity, and stability of this MWNT film coated electrode demonstrated its practical application for a simple, rapid and economical determination of trace levels of Cd 2+ and Pb 2+ in water samples

  6. Determination of subnanomolar levels of mercury (II) by using a graphite paste electrode modified with MWCNTs and Hg(II)-imprinted polymer nanoparticles.

    Science.gov (United States)

    Alizadeh, Taher; Hamidi, Negin; Ganjali, Mohamad Reza; Rafiei, Faride

    2017-12-05

    Mercury ion-imprinted polymer nanoparticles (Hg-IP-NPs) were synthesized via precipitation polymerization by using itaconic acid as a functional monomer. A carbon paste electrode was impregnated with the synthesized Hg-IP-NPs and MWCNTs to obtain a highly sensitive and selective electrode for determination of Hg(II). Mercury ion is first accumulated on the electrode surface via an open circuit procedure. After reduction of Hg(II) ions to its metallic form at a negative pre-potential, square wave anodic stripping voltammetry was applied to generate the electrochemical signal. The high affinity of the Hg-IP-NPs for Hg(II) was substantiated by comparing of the signals of electrodes with imprinted and non-imprinted polymer. The beneficial effect of MWCNTs on the voltammetric signal is also demonstrated. Under the optimized conditions and at a typical working potential of +0.05 V (vs. Ag/AgCl), the electrode has a linear response in the 0.1-20 nmol L -1 Hg(II) concentration range and a 29 pM detection limit. The electrochemical sensitivity is as high as 1441 A·M -1 ·cm -2 which is among the best values known. The electrode was applied to the determination of Hg(II) in water samples. Graphical abstract Schematic representation of the sensor electrode modified with mercury-imprinted polymer nanoparticles, and the recognition and voltammetric determination steps.

  7. A glassy carbon electrode modified with an amphiphilic, electroactive and photosensitive polymer and with multi-walled carbon nanotubes for simultaneous determination of dopamine and paracetamole

    International Nuclear Information System (INIS)

    Liu, Ren; Zeng, Xuebiao; Liu, Jingcheng; Luo, Jing; Zheng, Yuanyi; Liu, Xiaoya

    2016-01-01

    The article describes an electrochemical sensor for simultaneous determination of dopamine (DA) and paracetamole (PAT). It is based on the use of an electroactive polymer (referred to as BPVCM) to functionalize multi-walled carbon nanotubes. BPVCM is a branched amphiphilic photo-sensitive and electroactive polymer that was obtained by copolymerization of a vinyl benzyl carbazole, maleic acid anhydride, 4-vinyl benzylthiol and a vinylbenzyl oxycoumarin. BPVCM efficiently disperses MWCNT in aqueous solution. The electropolymerization of the carbazole moieties of the BPVCM enhances the current response. It also facilitates electron transfer in the MWCNT-BPVCM hybrid as evidenced by cyclic voltammetry and electrochemical impedance spectroscopy. A glassy carbon electrode modified with the nanocomposite displays outstanding electrocatalytic activity towards DA and PAT. DA can be determined, best at a working voltage of 0.2 V (vs. SCE), in the 5 to 1000 μM concentration range with a 2.3 μM detection limit. PAT can be determined in parallel, at a working voltage of 0.39 V (vs. SCE), in the same concentration range with a 3.5 μM detection limit. This analytical range of this method is wider than that of most alternative methods. (author)

  8. Application of l-cystine modified zeolite for preconcentration and determination of ultra-trace levels of cadmium by flame atomic absorption spectrometry.

    Science.gov (United States)

    Rezvani, Seyyed Ahmad; Soleymanpour, Ahmad

    2016-03-04

    A very convenient, sensitive and precise solid phase extraction (SPE) system was developed for enrichment and determination of ultra-trace of cadmium ion in water and plant samples. This method was based on the retention of cadmium(II) ions by l-cystine adsorbed in Y-zeolite and carry out in a packed mini-column. The retained cadmium ions then were eluted and determined by flame atomic absorption spectrometry. The scanning electron microscopy (SEM), powder X-ray diffraction (XRD) and Fourier Transform Infrared (FT-IR) spectroscopy techniques were applied for the characterization of cystine modified zeolite (CMZ). Some experimental conditions affecting the analytical performance such as pH, eluent type, concentration of sample, eluent flow rate and also the presence of interfering ions were investigated. The calibration graph was linear within the range of 0.1-7.5ngmL(-1) and limit of detection was obtained 0.04ngmL(-1) with the preconcentration factor of 400. The relative standard deviation (RSD) was obtained 1.4%, indicating the excellent reproducibility of this method. The proposed method was successfully applied for the extraction and determination of cadmium(II) ion in black tea, cigarette's tobacco and also various water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  9. An electrochemical sensor for warfarin determination based on covalent immobilization of quantum dots onto carboxylated multiwalled carbon nanotubes and chitosan composite film modified electrode

    Energy Technology Data Exchange (ETDEWEB)

    Gholivand, Mohammad Bagher, E-mail: mbgholivand2013@gmail.com; Mohammadi-Behzad, Leila

    2015-12-01

    A method is described for the construction of a novel electrochemical warfarin sensor based on covalent immobilization of CdS-quantum dots (CdS-QDs) onto carboxylated multiwalled carbon nanotubes/chitosan (CS) composite film on the surface of a glassy carbon electrode. The CdS-QDs/CS/MWCNTs were characterized by field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), Fourier transform infra-red (FTIR) spectroscopy, XRD analysis and electrochemical impedance spectroscopy (EIS). The sensor showed optimum anodic stripping response within 90 s at an accumulation potential of 0.75 V. The modified electrode was used to detect the concentration of warfarin with a wide linear range of 0.05–80 μM and a detection limit (S/N = 3) of 8.5 nM. The proposed sensor has good storage stability, repeatability and reproducibility and was successfully applied for the determination of warfarin in real samples such as urine, serum and milk. - Highlights: • A new sensitive sensor for warfarin determination was developed. • The sensor was constructed based on covalent immobilization of CdS-QDs on the chitosan/MWCNTs/GCE. • The parameters affecting the stripping analysis of warfarin were optimized. • The proposed sensor is used for trace determination of warfarin in urine, serum and milk.

  10. Method development for the determination of arsenic by sequential injection/anodic stripping voltammetry using long-lasting gold-modified screen-printed carbon electrode.

    Science.gov (United States)

    Punrat, Eakkasit; Chuanuwatanakul, Suchada; Kaneta, Takashi; Motomizu, Shoji; Chailapakul, Orawon

    2013-11-15

    An automated method has been developed for determining the concentration of inorganic arsenic. The technique uses sequential injection/anodic stripping voltammetry with a long-lasting gold-modified screen-printed carbon electrode. The long-lasting gold electrode was electrochemically deposited onto a screen-printed carbon electrode at a potential of -0.5 V vs. Ag/AgCl in a supporting electrolyte solution of 1M hydrochloric acid. Under optimal conditions and the applied potentials, the electrode demonstrated that it can be used for a long time without a renewal process. The linear range for the determination of arsenic(III) was 1-100 μg L(-1), and the limit of detection (LOD) in standard solutions was as low as 0.03 μg L(-1) for a deposition time of 120 s and sample volume of 1 mL. This method was used to determine the concentration of arsenic(III) in water samples with satisfactory results. The LOD in real samples was found to be 0.5 μg L(-1). In addition, speciation between arsenic(III) and arsenic(V) has been achieved with the proposed method using deposition potentials of -0.5 V and -1.5 V for the determination of the arsenic(III) concentration and the total arsenic concentration, respectively; the results were acceptable. The proposed method is an automated system that offers a less expensive alternative for determining trace amounts of inorganic arsenic. © 2013 Elsevier B.V. All rights reserved.

  11. Modified cyanobacteria

    Science.gov (United States)

    Vermaas, Willem F J.

    2014-06-17

    Disclosed is a modified photoautotrophic bacterium comprising genes of interest that are modified in terms of their expression and/or coding region sequence, wherein modification of the genes of interest increases production of a desired product in the bacterium relative to the amount of the desired product production in a photoautotrophic bacterium that is not modified with respect to the genes of interest.

  12. A novel magnetic ionic liquid modified carbon nanotube for the simultaneous determination of aryloxyphenoxy-propionate herbicides and their metabolites in water

    Energy Technology Data Exchange (ETDEWEB)

    Luo, Mai; Liu, Donghui; Zhao, Lu; Han, Jiajun; Liang, Yiran; Wang, Peng; Zhou, Zhiqiang, E-mail: zqzhou@cau.edu.cn

    2014-12-10

    Highlights: • A new kind of ionic liquid modified carbon nanotube has been synthesized and applied for simultaneous analysis of AOPPs and their metabolites. • The potential pollutants, such as metabolites of AOPPs, have been analyzed. • The mechanism of absorption has been discussed. • Varieties of experiment factors were optimized and selected. • This method has been successfully applied in the analysis of real water samples. - Abstract: A reliable, sensitive, rapid and environmentally friendly analysis procedure for the simultaneous determination of the analytes with a wide range of polarity in the environmental water was developed by coupling dispersive magnetic solid-phase extraction (d-MSPE) with high-performance liquid chromatography (HPLC)–diode array detector (DAD) and ultra-high pressure liquid chromatography (UHPLC)-triple quadrupole mass spectrometer (MS/MS), in this work. Magnetic ionic liquid modified multi-walled carbon nanotubes (m-IL-MWCNTs) were prepared by spontaneous assembly of magnetic nanoparticles and imidazolium-modified carbon nanotubes, and used as the sorbent of d-MSPE to simultaneously extract aryloxyphenoxy-propionate herbicides (AOPPs) and their polar acid metabolites due to the excellent π–π electron donor–acceptor interactions and anion exchange ability. The factors, including the amount of sorbent, pH of the sample solution, extraction time and the volume of elution solvent were investigated. Under the optimized conditions, the proposed d-MSPE coupling to HPLC–DAD system had a satisfactory performance, the limits of detection (LODs, defined as the signal to noise ratio of 3) and the limits of quantification (LOQs, defined as the signal to noise ratio of 10) for analytes in Milli-Q water were in the range of 2.8–14.3 and 9.8–43.2 μg L{sup −1} respectively. Calibration curves were linear (r{sup 2} > 0.998) over the concentration range from 0.02 to 1 mg L{sup −1}. The recoveries of the eight analytes ranged

  13. Separation, preconcentration and determination of silver ion from water samples using silica gel modified with 2,4,6-trimorpholino-1,3,5-triazin

    International Nuclear Information System (INIS)

    Madrakian, Tayyebeh; Afkhami, Abbas; Zolfigol, Mohammad Ali; Solgi, Mohammad

    2006-01-01

    A new modified silica gel using 2,4,6-trimorpholino-1,3,5-triazin was used for separation, preconcentration and determination of silver ion in natural water by atomic absorption spectrometry (AAS). This new bonded silica gel was used as an effective sorbent for the solid-phase extraction (SPE) of silver ion from aqueous solutions. Experimental conditions for effective adsorption of trace levels of silver ion were optimized with respect to different experimental parameters in column process. Common coexisting ions did not interfere with the separation and determination of silver at pH 3.5 so that silver ion completely adsorbed on the column. The preconcentration factor is 130 (1 mL elution volume for a 130 mL sample volume). The relative standard deviation (R.S.D.) under optimum conditions is 3.03% (n = 5). The accuracy of the method was estimated by using spring and tap water samples that were spiked with different amounts of silver ion. The adsorption isotherm of silver ion was obtained. The capacity of the sorbent at optimum conditions has been found to be 384 μg of silver per gram of sorbent

  14. Modified surface based on magnetic nanocomposite of dithiooxamide/Fe{sub 3}O{sub 4} as a sorbent for preconcentration and determination of trace amounts of copper

    Energy Technology Data Exchange (ETDEWEB)

    Mirabi, Ali, E-mail: mirabi2012@yahoo.com [Department of Chemistry, Qaemshahr Branch, Islamic Azad University, Qaemshahr (Iran, Islamic Republic of); Shokuhi Rad, Ali, E-mail: a.shokuhi@gmail.com [Department of Chemical Engineering, Qaemshahr Branch, Islamic Azad University, Qaemshahr (Iran, Islamic Republic of); Khodadad, Hadiseh [Department of Chemistry, Qaemshahr Branch, Islamic Azad University, Qaemshahr (Iran, Islamic Republic of)

    2015-09-01

    Magnetic nanocomposites surface (MNCS) which has anionic surfactant sodium dodecyl sulfate (SDS) coating and has undergone dithiooxamide treatment as the sorbent could be an easy and useful method to extract and make a pre-concentrated in detecting the copper ions before they are determined via the flame atomic absorption spectrometry (FAAS). The influences of the experimental parameters such as the pH of the sample, the type and concentration of the eluent, dithiooxamide concentration and volume, amount of sorbent and the interactions of ions with respect to the copper ion detection have been studied. The calibration graph was linear in the range of 2–600 ng ml{sup −1} with detection limit of 0.2 ng ml{sup −1}. Relative standard deviation (RSD) for 6 replicate measurements was 1.8%. This method of detection has been applied to the determination of Cu ions at levels in real samples such as wheat flour, tomatoes, potatoes, red beans, oat, tap water, river water and sea water with satisfactory results. - Highlights: • Fe{sub 3}O{sub 4} nano-magnetic improved by SDS/dithiooxamide. • It can be used in both the pre-concentration function and detecting of Cu ions. • This modified surface shows high adsorptive characteristics. • This procedure is relatively simple, fast and imposes less test analysis expenses.

  15. Determination of Uranium in Aqueous and Organic Medium From Product and Waste Processes by Potentiometric Titration Using Modified Davies Gray Method

    International Nuclear Information System (INIS)

    Putro, K.P; Suripto, A

    1998-01-01

    Determination of uranium in aqueous and organic solution generated from nuclear fuels production and liquid radioactive waste at Fuel Element Production Installation for Research Reactor, by modified Davies-Gray method using phosphoric acid as medium and vanadium as catalyst has been carried out. The performed at different concentration of phosphoric acid, vanadium and the effect of impurities, as Al, Fe, Si, Cl and F in sample are measurement. Determination of uranium in organic solvent are the sample volume, agitation time and the optimum concentration of uranium to measurement. It was observed that, the optimum conditions for uranium analysis were : 5 -400 mg uranium in 3.2 M phosphoric acid medium containing 220 mg/l vanadium as catalyst. The impurities of Al ≤ 40.5 μg/ml, Fe ≤ 67.6 μg/ml, Si ≤ 20.3 μg/ml, Cl ≤ 135.1 μg/ml and F 13.5 μg/ml have not effect, but the concentration of F ≥ 40.5 μg/ml have effect in analysis result. The uranium content detectable in organic medium has been found between 0.01 to 0.10 g/l and the reproducibility range between 0.09 to 0.15 as well as the sample volume should be in the range of 5 and 10 ml by the agitation time for 4 minute

  16. Modified surface based on magnetic nanocomposite of dithiooxamide/Fe3O4 as a sorbent for preconcentration and determination of trace amounts of copper

    International Nuclear Information System (INIS)

    Mirabi, Ali; Shokuhi Rad, Ali; Khodadad, Hadiseh

    2015-01-01

    Magnetic nanocomposites surface (MNCS) which has anionic surfactant sodium dodecyl sulfate (SDS) coating and has undergone dithiooxamide treatment as the sorbent could be an easy and useful method to extract and make a pre-concentrated in detecting the copper ions before they are determined via the flame atomic absorption spectrometry (FAAS). The influences of the experimental parameters such as the pH of the sample, the type and concentration of the eluent, dithiooxamide concentration and volume, amount of sorbent and the interactions of ions with respect to the copper ion detection have been studied. The calibration graph was linear in the range of 2–600 ng ml −1 with detection limit of 0.2 ng ml −1 . Relative standard deviation (RSD) for 6 replicate measurements was 1.8%. This method of detection has been applied to the determination of Cu ions at levels in real samples such as wheat flour, tomatoes, potatoes, red beans, oat, tap water, river water and sea water with satisfactory results. - Highlights: • Fe 3 O 4 nano-magnetic improved by SDS/dithiooxamide. • It can be used in both the pre-concentration function and detecting of Cu ions. • This modified surface shows high adsorptive characteristics. • This procedure is relatively simple, fast and imposes less test analysis expenses

  17. A Fast Strategy for Determination of Vitamin B9 in Food and Pharmaceutical Samples Using an Ionic Liquid-Modified Nanostructure Voltammetric Sensor

    Directory of Open Access Journals (Sweden)

    Fatemeh Khaleghi

    2016-05-01

    Full Text Available Vitamin B9 or folic acid is an important food supplement with wide clinical applications. Due to its importance and its side effects in pregnant women, fast determination of this vitamin is very important. In this study we present a new fast and sensitive voltammetric sensor for the analysis of trace levels of vitamin B9 using a carbon paste electrode (CPE modified with 1,3-dipropylimidazolium bromide (1,3-DIBr as a binder and ZnO/CNTs nanocomposite as a mediator. The electro-oxidation signal of vitamin B9 at the surface of the 1,3-DIBr/ZnO/CNTs/CPE electrode appeared at 800 mV, which was about 95 mV less positive compared to the corresponding unmodified CPE. The oxidation current of vitamin B9 by square wave voltammetry (SWV increased linearly with its concentration in the range of 0.08–650 μM. The detection limit for vitamin B9 was 0.05 μM. Finally, the utility of the new 1,3-DIBr/ZnO/CNTs/CPE electrode was tested in the determination of vitamin B9 in food and pharmaceutical samples.

  18. Sodium dodecyl sulfate coated γ-alumina support modified by a new Schiff base for solid phase extraction and flame-AAS determination of lead and copper ions

    Directory of Open Access Journals (Sweden)

    Ardeshir Shokrollahi

    2013-01-01

    Full Text Available A simple and fast approach for solid phase extraction is herein described, and used to determine trace amounts of Pb2+ and Cu2+ metal ions. The solid phase support is sodium dodecyl sulfate (SDS-coated γ-alumina modified with bis(2-hydroxy acetophenone-1,6-hexanediimine (BHAH ligand. The adsorbed ions were stripped from the solid phase by 6 mL of 4 M nitric acid as eluent. The eluting solution was analyzed by flame atomic absorption spectrometry (FAAS. The sorption recovery of metal ions was investigated with regard to the effects of pH, amount of ligand, γ-alumina and surfactant and the amount and type of eluent. Complexation of BHAH with Pb2+ or Cu2+ ions was examined via spectrophotometry using the HypSpec program. The detection limit for Cu2+ was 7.9 µg L-1 with a relative standard deviation of 1.67%, while that for Pb2+ was 6.4 µg L-1 with a relative standard deviation of 1.64%. A preconcentration factor of 100 was achieved for these ions. The method was successfully applied to determine analyte concentrations in samples of liver, parsley, cabbage, and water.

  19. Voltammetric determination of sudan ii in food samples at graphene modified glassy carbon electrode based on the enhancement effect of sodium dodecyl sulfate

    International Nuclear Information System (INIS)

    Ma, X.; Chen, M.; Chao, M.

    2013-01-01

    Summary: Herein, a novel electrochemical method was de veloped for the determination of Sudan II based on the electrochemical catalytic activity of graphene modified glassy carbon electrode (GME) and the enhancement effect of sodium dodecyl sulfate (SDS). In a pH 6.0 phosphate buffer solution, Sudan II exhibited a pair of well-defined quasi reversible redox peaks at the GME in the presence of 5.0x10/sup -5/ mol L/sup 1/ SDS. The oxidation peak current of Sudan II was linearly proportional to its concentration in a range from 4.0x10/sup -8/ to 4.0x10/sup -6/ mol L/sup 1/, with a linear regression equation of ipa (A) = 3.35 c + 5.96 x 10/sup -6/, r = 0.9988 and a detection limit of 8.0x10/sup -9/ mol L/sup 1/. The recoveries from the standards fortified blank samples were in the range of 94.7% to 97.5% with RSD lower than 4.0%. The novel method has been successfully used to determine Sudan II in food products with satisfactory results. (author)

  20. Determination of Zinc, Cadmium, Lead, Copper and Silver Using a Carbon Paste Electrode and a Screen Printed Electrode Modified with Chromium(III Oxide

    Directory of Open Access Journals (Sweden)

    Zuzana Koudelkova

    2017-08-01

    Full Text Available In this study, the preparation and electrochemical application of a chromium(III oxide modified carbon paste electrode (Cr-CPE and a screen printed electrode (SPE, made from the same material and optimized for the simple, cheap and sensitive simultaneous determination of zinc, cadmium, lead, copper and the detection of silver ions, is described. The limits of detection and quantification were 25 and 80 µg·L−1 for Zn(II, 3 and 10 µg·L−1 for Cd(II, 3 and 10 µg·L−1 for Pb(II, 3 and 10 µg·L−1 for Cu(II, and 3 and 10 µg·L−1 for Ag(I, respectively. Furthermore, this promising modification was transferred to the screen-printed electrode. The limits of detection for the simultaneous determination of zinc, cadmium, copper and lead on the screen printed electrodes were found to be 350 µg·L−1 for Zn(II, 25 µg·L−1 for Cd(II, 3 µg·L−1 for Pb(II and 3 µg·L−1 for Cu(II. Practical usability for the simultaneous detection of these heavy metal ions by the Cr-CPE was also demonstrated in the analyses of wastewaters.

  1. Development of an alcohol dehydrogenase biosensor for ethanol determination with toluidine blue O covalently attached to a cellulose acetate modified electrode.

    Science.gov (United States)

    Alpat, Senol; Telefoncu, Azmi

    2010-01-01

    In this work, a novel voltammetric ethanol biosensor was constructed using alcohol dehydrogenase (ADH). Firstly, alcohol dehydrogenase was immobilized on the surface of a glassy carbon electrode modified by cellulose acetate (CA) bonded to toluidine blue O (TBO). Secondly, the surface was covered by a glutaraldehyde/bovine serum albumin (BSA) cross-linking procedure to provide a new voltammetric sensor for the ethanol determination. In order to fabricate the biosensor, a new electrode matrix containing insoluble Toluidine Blue O (TBO) was obtained from the process, and enzyme/coenzyme was combined on the biosensor surface. The influence of various experimental conditions was examined for the characterization of the optimum analytical performance. The developed biosensor exhibited sensitive and selective determination of ethanol and showed a linear response between 1 × 10(-5) M and 4 × 10(-4) M ethanol. A detection limit calculated as three times the signal-to-noise ratio was 5.0 × 10(-6) M. At the end of the 20(th) day, the biosensor still retained 50% of its initial activity.

  2. Development of an Alcohol Dehydrogenase Biosensor for Ethanol Determination with Toluidine Blue O Covalently Attached to a Cellulose Acetate Modified Electrode

    Directory of Open Access Journals (Sweden)

    Azmi Telefoncu

    2010-01-01

    Full Text Available In this work, a novel voltammetric ethanol biosensor was constructed using alcohol dehydrogenase (ADH. Firstly, alcohol dehydrogenase was immobilized on the surface of a glassy carbon electrode modified by cellulose acetate (CA bonded to toluidine blue O (TBO. Secondly, the surface was covered by a glutaraldehyde/bovine serum albumin (BSA cross-linking procedure to provide a new voltammetric sensor for the ethanol determination. In order to fabricate the biosensor, a new electrode matrix containing insoluble Toluidine Blue O (TBO was obtained from the process, and enzyme/coenzyme was combined on the biosensor surface. The influence of various experimental conditions was examined for the characterization of the optimum analytical performance. The developed biosensor exhibited sensitive and selective determination of ethanol and showed a linear response between 1 × 10−5 M and 4 × 10−4 M ethanol. A detection limit calculated as three times the signal-to-noise ratio was 5.0 × 10−6 M. At the end of the 20th day, the biosensor still retained 50% of its initial activity.

  3. Determination of Zinc, Cadmium, Lead, Copper and Silver Using a Carbon Paste Electrode and a Screen Printed Electrode Modified with Chromium(III) Oxide.

    Science.gov (United States)

    Koudelkova, Zuzana; Syrovy, Tomas; Ambrozova, Pavlina; Moravec, Zdenek; Kubac, Lubomir; Hynek, David; Richtera, Lukas; Adam, Vojtech

    2017-08-09

    In this study, the preparation and electrochemical application of a chromium(III) oxide modified carbon paste electrode (Cr-CPE) and a screen printed electrode (SPE), made from the same material and optimized for the simple, cheap and sensitive simultaneous determination of zinc, cadmium, lead, copper and the detection of silver ions, is described. The limits of detection and quantification were 25 and 80 µg·L -1 for Zn(II), 3 and 10 µg·L -1 for Cd(II), 3 and 10 µg·L -1 for Pb(II), 3 and 10 µg·L -1 for Cu(II), and 3 and 10 µg·L -1 for Ag(I), respectively. Furthermore, this promising modification was transferred to the screen-printed electrode. The limits of detection for the simultaneous determination of zinc, cadmium, copper and lead on the screen printed electrodes were found to be 350 µg·L -1 for Zn(II), 25 µg·L -1 for Cd(II), 3 µg·L -1 for Pb(II) and 3 µg·L -1 for Cu(II). Practical usability for the simultaneous detection of these heavy metal ions by the Cr-CPE was also demonstrated in the analyses of wastewaters.

  4. Determination of dopamine using a glassy carbon electrode modified with a graphene and carbon nanotube hybrid decorated with molybdenum disulfide flowers

    International Nuclear Information System (INIS)

    Mani, Veerappan; Govindasamy, Mani; Chen, Shen-Ming; Karthik, Raj; Huang, Sheng-Tung

    2016-01-01

    We describe a hybrid material that consists of molybdenum sulfide flowers placed on graphene nanosheets and multiwalled carbon nanotubes (GNS-CNTs/MoS_2). It was deposited on a glassy carbon electrode (GCE) which then is well suited for sensitive and selective determination of dopamine. The GNS-CNTs/MoS_2 nanocomposite was prepared by a hydrothermal method and characterized by scanning electron and transmission emission microscopies, energy-dispersive X-ray spectroscopy, cyclic voltammetry, differential pulse voltammetry and electrochemical impedance spectroscopy. Electrochemical studies show the composite to possess excellent electrochemical properties such as a large electrochemically active surface, high capacitance current, a wide potential window, high conductivity and large porosity. The electrode displays excellent electrocatalytic ability to oxidize dopamine. The modified GCE, best operated at a working potential as low as 0.15 V (vs. Ag/AgCl), responds linearly to dopamine in the 100 nM to 100 μM concentration range. The detection limit is 50 nM, and the sensitivity is 10.81 (± 0.26) μA⋅μM"−"1⋅cm"−"2. The sensor has good selectivity, appreciable stability, repeatability and reproducibility. It was applied to the determination of dopamine in (spiked) biological and pharmaceutical samples. (author)

  5. Determination of Residual Nonsteroidal Anti-Inflammatory Drugs in Aqueous Sample Using Magnetic Nanoparticles Modified with Cetyltrimethylammonium Bromide by High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Malihe Khoeini Sharifabadi

    2014-01-01

    Full Text Available A simple and sensitive solid-phase extraction method for separation and preconcentration of trace amount of four nonsteroidal anti-inflammatory drugs (naproxen, indomethacin, diclofenac, and ibuprofen using Fe3O4 magnetic nanoparticles modified with cetyltrimethylammonium bromide has been developed. For this purpose, the surface of MNPs was modified with cetyltrimethylammonium bromide (CTAB as a cationic surfactant. Effects of different parameters influencing the extraction efficiency of drugs including the pH, amount of salt, shaking time, eluent type, the volume of solvent, amount of adsorbent, sample volume, and the time of desorption were investigated and optimized. Methanol has been used as desorption solvent and the extracts were analysed on a reversed-phase octadecyl silica column using 0.02 M phosphate-buffer (pH = 6.02 acetonitrile (65 : 35 v/v as the mobile phase and the effluents were measured at 202 nm with ultraviolet detector. The relative standard deviation (RSD% of the method was investigated at three concentrations (25, 50, and 200 ng/mL and was in the range of 3.98–9.83% (n=6 for 50 ng/mL. The calibration curves obtained for studied drugs show reasonable linearity (R2>0.99 and the limit of detection (LODs ranged between 2 and 7 ng/mL. Finally, the proposed method has been effectively employed in extraction and determination of the drugs in biological and environmental samples.

  6. MgO nanobelt-modified graphene-tantalum wire electrode for the simultaneous determination of ascorbic acid, dopamine and uric acid

    International Nuclear Information System (INIS)

    Zhao, Liwei; Li, Hongji; Gao, Sumei; Li, Mingji; Xu, Sheng; Li, Cuiping; Guo, Wenlong; Qu, Changqing; Yang, Baohe

    2015-01-01

    Graphical abstract: Display Omitted -- Highlights: •Graphene and MgO nanobelts are deposited on tantalum wires to form biosensors. •Ascorbic acid, dopamine and uric acid are determined with the biosensors. •The biosensors show high electrocatalytic activity for oxidation of these species. •The biosensors show high selectivity and good sensitivity. -- ABSTRACT: A promising electrochemical biosensor for simultaneous detection of ascorbic acid (AA), dopamine (DA) and uric acid (UA) was fabricated by electrochemical deposition of MgO nanobelts on a graphene-modified tantalum wire (denoted as MgO/Gr/Ta) electrode. The MgO nanobelts and graphene were verified by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Electrochemical performances of the electrodes were characterized by electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The CV results show that AA, DA and UA could be detected simultaneously using MgO/Gr/Ta electrode with peak-to-peak separation of 300 mV, 147 mV and 447 mV for AA-DA, DA-UA and AA-UA, respectively. In the threefold co-existence system, the linear calibration plots for AA, DA and UA were obtained over the concentration range of 5.0–350 μM, 0.1–7 μM and 1–70 μM with detection limits of 0.03 μM, 0.15 μM and 0.12 μM, respectively. The modified electrode shows excellent selectivity, good sensitivity and good stability, making it attractive as a sensor for simultaneous detection of AA, DA and UA in biological fluids

  7. Challenges and opportunities in establishing scientific and regulatory standards for determining therapeutic equivalence of modified-release products: Workshop summary report.

    Science.gov (United States)

    Chen, Mei-Ling; Shah, Vinod P; Ganes, Derek; Midha, Kamal K; Caro, James; Nambiar, Prabu; Rocci, Mario L; Thombre, Avinash G; Abrahamsson, Bertil; Conner, Dale; Davit, Barbara; Fackler, Paul; Farrell, Colm; Gupta, Suneel; Katz, Russell; Mehta, Mehul; Preskorn, Sheldon H; Sanderink, Gerard; Stavchansky, Salomon; Temple, Robert; Wang, Yaning; Winkle, Helen; Yu, Lawrence

    2010-09-01

    Modified-release (MR) products are complex dosage forms designed to release drug in a controlled manner to achieve the desired efficacy and safety profiles. Inappropriate control of drug release from such products may result in reduced efficacy or increased toxicity. This paper is a summary report of the American Association of Pharmaceutical Scientists, International Pharmaceutical Federation, and Product Quality Research Institute workshop titled "Challenges and Opportunities in Establishing Scientific and Regulatory Standards for Assuring Therapeutic Equivalence of Modified Release Products", held October 1-2, 2009, in Baltimore, Maryland. The workshop provided an opportunity for pharmaceutical scientists from academia, industry, and regulatory agencies to discuss current regulatory expectations and industry practices for evaluating the pharmaceutical equivalence and bioequivalence of oral MR products. In the case of conventional monophasic MR formulations, the current regulatory approaches and criteria for bioequivalence evaluation were considered adequate for the assessment of therapeutic equivalence and inter-changeability of drug products. Additional measures may occasionally be needed to determine the bioequivalence of multiphasic MR products. The metric of partial AUC proposed by the US Food and Drug Administration received broad support as an additional measure for evaluating bioequivalence of multiphasic MR products designed to have a rapid onset of drug action followed by sustained response. The cutoff for partial AUCs may be based on the pharmacokinetic/pharmacodynamic or pharmacokinetic/ response characteristics of the products under examination. If the new metric is highly variable, the bioequivalence limits may be set based on the known within-subject variability for the reference product. The current regulatory approaches and criteria for bioequivalence evaluation were considered adequate for the assessment of therapeutic equivalence and

  8. Extraction of Flavonoids from the Flowers of Abelmoschus manihot (L. Medic by Modified Supercritical CO2 Extraction and Determination of Antioxidant and Anti-Adipogenic Activity

    Directory of Open Access Journals (Sweden)

    Jingjing Li

    2016-06-01

    Full Text Available Abelmoschus manihot (L. Medic has been used for many years in Chinese traditional medicine. In this study, supercritical CO2 plus a modifier was utilized to extract flavonoids from the flowers of Abelmoschus manihot (L. Medic. The effects of temperature (40 °C–60 °C, pressure (10–30 MPa and different concentrations of ethanol as modifier (60%–90%, ethanol:water, v/v on major flavonol content and the antioxidant activity of the extracts were studied by response surface methodology (RSM using a Box-Behnken design. The flavonol content was calculated as the sum of the concentrations of seven major flavonoids, namely rutin, hyperin, isoquercetin, hibifolin, myricetin, quercetin-3′-O-glucoside and quercetin, which were simultaneously determined by a HPLC method. The antioxidant activity was evaluated by a 2,2-diphenyl-1-picrylhydarzyl (DPPH free radical-scavenging assay. The results showed that three factors and their interactions could be well fitted to second-order polynomial models (p < 0.05. At the optimal extraction conditions for flavonol content (20 MPa, 52 °C, and 85% ethanol content, the yield of flavonoids was 41.96 mg/g and the IC50 value was 0.288 mg/mL, respectively, suggesting the extract has high antioxidant activity. Furthermore, the anti-adipogenic activity of the extract on the 3T3-L1 cell line was investigated. The results indicated that it can downregulate PPARγ and C/EBPα expression at mRNA. In summary, in this study, we have established a cost-effective method for the extraction of flavonoids from the flowers of Abelmoschus manihot (L. Medic using supercritical fluid extraction and the extracts exhibited potent antioxidant and anti-adipogenic effects, suggesting a possible therapeutic approach for the prevention and treatment of obesity.

  9. Mercury-free simultaneous determination of cadmium and lead at a glassy carbon electrode modified with multi-wall carbon nanotubes

    Energy Technology Data Exchange (ETDEWEB)

    Wu Kangbing; Hu Shengshui; Fei Junjie; Bai Wen

    2003-08-18

    A multi-wall carbon nanotube (MWNT) modified glassy carbon electrode (GCE) was described for the simultaneous determination of trace levels of cadmium and lead by anodic stripping voltammetry (ASV). In pH 4.5 NaAc-HAc buffer containing 0.02 mol/l KI, Cd{sup 2+} and Pb{sup 2+} first adsorb onto the surface of a MWNT film coated GCE and then reduce at -1.20 V. During the positive potential sweep, reduced cadmium and lead were oxidized, and two well-defined stripping peaks appeared at -0.88 and -0.62 V. Compared with a bare GCE, a MWNT film coated GCE greatly improves the sensitivity of determining cadmium and lead. Low concentration of I{sup -} significantly enhances the stripping peak currents since it induces Cd{sup 2+} and Pb{sup 2+} to adsorb at the electrode surface. The striping peak currents change linearly with the concentration of Cd{sup 2+} from 2.5x10{sup -8} to 1x10{sup -5} mol/l and with that of Pb{sup 2+} from 2x10{sup -8} to 1x10{sup -5} mol/l. The lowest detectable concentrations of Cd{sup 2+} and Pb{sup 2+} are estimated to be 6x10{sup -9} and 4x10{sup -9} mol/l, respectively. The high sensitivity, selectivity, and stability of this MWNT film coated electrode demonstrated its practical application for a simple, rapid and economical determination of trace levels of Cd{sup 2+} and Pb{sup 2+} in water samples.

  10. Electrothermal vaporization inductively coupled plasma mass spectrometry for the determination of trace amount of lanthanides and yttrium in soil with polytetrafluroethylene emulsion as a chemical modifier

    International Nuclear Information System (INIS)

    He Man; Hu, Bin; Jiang Zucheng

    2005-01-01

    A method of electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) for the determination of trace lanthanides and yttrium in soil samples with a polytetrafluorethylene (PTFE) emulsion as chemical modifier to promote the vaporization of the analytes from the graphite furnace was developed in this paper. The analytical characteristics, spectral interference and matrix effect of the analytical method were evaluated and critically compared with those of pneumatic nebulization inductively coupled plasma mass spectrometry (PN-ICP-MS). Under the optimized operation conditions, the relative detection limits of lanthanides (La-Lu) and yttrium for ETV-ICP-MS and PN-ICP-MS were 0.4-20 ng l -1 and 1.0-21 ng l -1 , respectively, the absolute detection limits for ETV-ICP-MS were 4-200 fg, which were improved by 1-2 orders of magnitude compared with PN-ICP-MS. While the analytical precision of ETV-ICP-MS is worse than that of PN-ICP-MS, with the R.S.D.s (%) of 4.1-10% for the former and 2.9-7.8% for the latter. Regarding to the matrix effect, both conventional method and stepwise dilution method were employed to observe the effect of matrix and the very similar results were obtained. It was found that the highest tolerance concentration of the matrix is 1000 mg l -1 and 800 mg l -1 for ETV-ICP-MS and PN-ICP-MS, respectively. To assess the accuracy, the proposed method was applied to the determination of trace lanthanides and yttrium in three different soil standard reference materials and one soil sample, and the determined values are in good agreement with the certified values or reference values

  11. Simultaneous Determination of Copper, Lead, and Cadmium Ions at a Mo6S9-xIx Nanowires Modified Glassy Carbon Electrode Using Differential Pulse Anodic Stripping Voltammetry

    International Nuclear Information System (INIS)

    Lin, Hong; Li, Meixian; Mihailovič, Dragan

    2015-01-01

    Highlights: • An electrochemical sensor based on Mo 6 S 9-x I x nanowires was constructed. • Mo 6 S 9-x I x nanowires can amplify electrochemical responses of heavy metal ions. • Mo 6 S 9-x I x nanowires can promote electron transfer. • Mo 6 S 9-x I x nanowires can accumulate metal ions due to large surface area. • The preparation of the sensor is simple, short-time and it does not require a special apparatus. -- ABSTRACT: A novel electrochemical sensor based on a new kind of nanomaterials Mo 6 S 9-x I x nanowires modified glassy carbon electrode (GCE) was constructed for simultaneous determination of cadmium(II), lead(II) and copper(II) using differential pulse anodic stripping voltammetry (DPASV). Various experimental parameters such as the modified amount, pH, deposition time and deposition potential were optimized. Under the optimal conditions, the stripping peak currents increase linearly with increasing concentrations of Cd(II), Pb(II) and Cu(II) ions in the ranges of 0.5∼150 μg · L −1 , 1.5∼450 μg · L −1 and 0.8~240 μg · μg·L −1 , 1.5∼450 μg·L −1 and 0.8∼240 μg·L −1 , respectively. And the limits of detection (S/N = 3) are estimated to be 0.10 μg · L −1 for Cd (II), 0.45 μg·L −1 for Pb(II) and 0.20 μg·L −1 for Cu(II), which are two orders of magnitude lower than those obtained at the unmodified electrodes. Most importantly, the sensor has been successfully applied to the determination of trace metal ions in the tap water samples. This developed electrochemical sensor exhibits high sensitivity, good stability and reproducibility

  12. Electrochemical sensors for the simultaneous determination of zinc, cadmium and lead using a Nafion/ionic liq