首页 | 本学科首页   官方微博 | 高级检索  
相似文献
 共查询到20条相似文献,搜索用时 609 毫秒
1.
Summary The effect of some surfactants and protective colloids on the absorbance of the iron(III)-phenylfluorone complex has been investigated. The binary complex formed at pH 9.0 show a molar absorptivity of 7.5×104 l · mol–1 · cm–1 at 530 nm. In the presence of 2% Triton X-100, at the same pH, the molar absorptivity of the sensitized complex was 1.19×105 l · mo–1 · cm–1 at 555 nm. Full colour development of the sensitized complex occurred within 25 min and Beer's law was followed up to 0.53 ppm of iron. The molar ratio and continuous variation methods indicated a 13 metal-ligand ratio for the sensitized complex. The effect of various amounts of different ions has been studied under the experimental conditions and some masking agents were recommended. The method has been applied to the determination of iron in copper and nickel metals and some non-ferrous alloys.
Spektralphotometrische Bestimmung von Eisen als Phenylfluoronkomplex sensibilisiert mit Triton X-100
  相似文献   

2.
The electrochemical reduction of fenofibrate at a hanging mercury drop electrode (HMDE) was investigated by cyclic voltammetry, square-wave voltammetry, and chronoamperometry. Different buffer solutions were used over a wide pH range (3.0–10.0). The best definition of the analytical signals was found in borate buffer (pH 9.0)–tetrabutylammonium iodide mixture containing 12.5% (v/v) methanol at –1.2 V (versus Ag/AgCl). According to cyclic voltammetric studies, the reduction was irreversible and diffusion controlled. The diffusion coefficient was 2.38×10–6 cm2 s–1 as determined by chronoamperometry. Under optimized conditions of square-wave voltammetry, a linear relationship was obtained between 0.146–4.96 g mL–1 of fenofibrate with a limit of detection of 0.025 g mL–1. Validation parameters such as sensitivity, accuracy, precision, and recovery were evaluated. The proposed method was applied to the determination of fenofibrate in pharmaceutical formulations. The results were compared with those obtained by a published high-performance liquid chromatography method. No difference was found statistically.  相似文献   

3.
A new, simple, highly sensitive spectrophotometric method for the determination of trace amounts of cerium(IV) is described. The method is based on the oxidation of leuco disulphine blue (LDSB) to its blue form of disulphine blue by Ce(IV) in a sulfuric acid medium (pH 1.3–3.0); the absorbance of the formed dye is measured in an acetate buffer medium (pH 3.0–4.8) at 635 nm. The color system obeys Beer's law in the concentration range from 0.5 to 5.5 g mL–1 cerium with a molar absorptivity of 1.75 × 104 L mol–1 cm–1 and a Sandell's sensitivity of 0.008 g cm–2. All variables were studied in order to optimize the reaction conditions. The developed method has been successfully applied to the determination of cerium in high purity rare-earth oxides, soil, natural water, plant tissue, human hair, and rock samples.  相似文献   

4.
Thin polyimide (PI) and polyethersulfone (PES) films are widely used as functional layers for microelectronic sensors. Ion implantation modifies the layer structure and morphology of these polymers and hence results in new mechanical and optical properties. However, ion-modified layers also show a change in sensitivity to moisture uptake under specific conditions. This is important for developing humidity sensors. Therefore, the water sorption ability of such modified polymer layers is studied by spectroscopic ellipsometry under definite relative humidity conditions (1–95%). Swelling data were obtained by fitting procedures based on changes of effective layer thickness and optical constants due to water uptake. Irradiation doses from 0.5 to 5×1015 B+ cm–2 at an energy of 180 keV were used for polymer modification. At irradiation doses from 0.5 to 0.7×1015 B+ cm–2, the maximum out-of-plane swelling is reached. At higher doses >2×1015 B+ cm–2, the swelling decreases and corresponds to values of the pure polymer layers. The wetting properties of the layer surfaces determined by contact angle measurements are important to explain this behavior.  相似文献   

5.
A novel PVC-based membrane sensor based on the Co(II)-salophen complex (CSC) is described. The electrode revealed a Nernstian response over a wide nitrite ion concentration range (1.0×10–6–1.0×10–1M). The detection limit of the sensor is 8.0×10–7M. The best performance was obtained with a membrane composition of 33% PVC, 61% ortho-nitrophenyloctyl ether, 3% cobalt(II)-salophen, and 3% hexadecyltrimethylammonium bromide. The potentiometric response of the sensor is independent of the pH of solution in the pH range 4.5–11.9. The electrode exhibits a very fast response time and good selectivity over a variety of common inorganic and organic anions, including fluoride, bromide, iodide, sulfite, nitrate, thiocyanate, thriiodide and perchlorate. The selectivity behavior of the proposed sensor shows substantial improvements compared to the previously reported electrodes for nitrite ion. The membrane sensor can be used for at least 2 months without any divergence in potential. The electrode was successfully applied to the monitoring of nitrite ion in water, sausage, flour, wheat, cheese and milk.  相似文献   

6.
Summary It has been established that 1-(2-phenyl-2-hydroxyiminoethyl)-1-quinolinium chloride, 1-(2-phenyl-2-hydroxyiminoethyl)-1-isoqui-nolinium chloride, 1-(2-phenyl-2-hydroxyiminoethyl)-1-(4-methyl)-quinolinium chloride and 1-(2-phenyl-2-hydroxyiminoethyl)-1-(6-methyl)quinolinium chloride react with palladium(II) chloride in the pH range 3.3–7.1 and form yellow water-soluble 11 complexes with maximum absorbance at 413 nm. The conditional stability constants of the complexes at the optimum pH of 6.5 are all about 104.7, and the molar absorptivities are in the range 2.2–2.6×103 l·l mole–1·cm–1 at pH 6.5 and 413 nm. Beer's law is obeyed up to 3–4×10–4 M oxime concentration, depending on the oxime determined.  相似文献   

7.
Summary Tetraphenylphosphoniumbromide (TPP), a lipophilic cation used for the determination of plasma membrane potential, was quantified by isotachophoresis. The optimized leading electrolyte consisted of 10 mmol/l KOH as leading ion, supplemented with 0.5% hydroxy-ethylcellulose. The pH was adjusted to 9.5 with methionine. The terminating ion was 10 mmol/l tris(hydroxymethyl)-aminomethane (pH 9.2, adjusted with methionine). Leading ion concentrations of 10, 1 and 0.5 mmol/l respectively, showed nearly the same detection limits (2×10–11 mol of TPP). This detection limit allowed the quantitative determination of TPP down to a concentration of 2 mol/l. Calibration curves in the range of 2×10–11 to 1.5×10–10 mol of TPP showed correlation coefficients greater than 0.95 (n=12; =0.01).  相似文献   

8.
A glassy carbon electrode (GCE) was modified with electropolymerized films of amidosulfonic acid in pH 7.0 phosphate buffer solution (PBS) by cyclic voltammetry (CV). The modified electrode showed an excellent electrocatalytical effect on the oxidation of dopamine (DA). In pH 7.0 PBS, the anodic peak current increased linearly with the concentration of DA in the range of 5.0×10–7 1.0×10–4moldm–3, with a correlation coefficient of 0.9932, and a detection limit (S/N=3) of 1.0× 10–7moldm–3. The relative standard deviation of 10 successive scans was 2.5% for 1.0×10–6moldm–3 DA. The interference of ascorbic acid (AA) with the determination of DA could be eliminated because of the very distinct attracting interaction between DA cations and the negatively poly(amidosulfonic acid) film in pH 7.0 PBS. The proposed method exhibited good recovery and reproducibility.  相似文献   

9.
Column preconcentration methods have been established for the spectrophotometric determination of trace nitrite with sulfanilic acid (SA) orp-aminoacetophenone (AAP) as the diazotizable aromatic amine andN, N-dimethylaniline (DMA) or 1-aminonaphthalene (AN) as the coupling agent, using differention-pairs co-precipitated with biphenyl. Nitrite ion reacts with SA in the pH range 2.0–3.0 and AAP in the pH range 1.7–3.0 in HCl medium to form water-soluble colourless diazonium cations. These cations are subsequently coupled with DMA in the pH range 3.7–6.1 for the SA-DMA system and AN in the pH range 1.7–2.3 for the AAP-AN system to be retained on microcrystalline biphenyl packed in a column. The solid mass is dissolved out from the column with 5 ml of DMF and the absorbance is measured by a spectrophotometer at 420 nm for the SA-DMA system and at 517 nm for the AAP-AN system. The calibration was linear over the concentration ranges 0.3–6.0 g of nitrite in 5 ml of DMF solution (i.e., 0.02–0.40 g/ml in the sample solution) for the SA-DMA system and 0.5–7.0 g of nitrite in 5 ml of DMF solution (i.e., 0.03–0.47 g/ml in the sample solution) for the AAP-AN system. The molar absorptivity and Sandell's sensitivity were respectively 2.63 × 104lmol–1cm–1 and 1.75 × 10–3 g cm–2 for SA-DMA and 3.28 × 104lmol–1 cm–1 and 1.40 × 10–3 g cm–2 for AAP-AN. The concentration factors were 4 and 16 for SA-DMA and AAP-AN, respectively. The detection limits were 0.0138 and 0.0175 g/ml NO2 for SA-DMA and AAP-AN, respectively. Seven replicate determinations of a solution containing 3.5 g of nitrite gave mean absorbances of 0.410 and 0.500 with relative standard deviations of 0.51 and 0.55% for SA-DMA and AAP-AN, respectively. Interference from various foreign ions has been studied and the methods have been applied to the determination of nitrite in environmental samples.  相似文献   

10.
Two diaza-crown ether compounds were synthesized and evaluated as Ag+-selective carriers in polyvinylchloride (PVC) membrane electrodes of solid-state type. The all-solid-state PVC membrane electrode based on N,N-Dibenzyl-dibenzo-diaza-18-crown-6 exhibited a super-Nernstian response (75±10mV per decade) over the concentration range of 1×10–1 to 7×10–6M of Ag+ ion and a detection limit of 3×10–6M, at a wide range of pH (pH 4–7). The response time of the electrode was fast (less than 10s), and it can be used for three months without any significant deviation in potential. The proposed all-solid-state PVC membrane electrodes revealed high selectivity toward Ag+ ion with respect to alkali, alkaline earth, heavy and transition metal ions. A flow-through cell of all-solid-state PVC membrane Ag+-selective electrode based on N,N-Dibenzyl-dibenzo-diaza-18-crown-6 has also been prepared and applied for flow-injection analysis of Ag+ ion in solution.  相似文献   

11.
Carbon nanotubes were modified on the surface of a glassy carbon electrode (GC) and initially applied in semi-derivative anode stripping voltammetry for the determination of 6-benzylaminopurine. The experiments demonstrated that the presence of the carbon nanotube greatly increased the current of the oxidation peak of benzylaminopurine. Cyclic voltammetry (CV) and semi-derivative voltammetry were used in a comparative investigation into the electrochemical oxidation of benzylaminopurine with the modified electrode. Studies on the effect of pH on the peak current and potential were carried out over the pH range of 9.013.0 with the NH3–NH4Cl buffer solution. A pH of 10.0 was chosen as the optimum pH. Other experimental parameters, such as film thickness, accumulation potential, temperature etc. were optimized. The anodic peak current was found to be linearly related to the concentration of benzylaminopurine over the range of 4.0×10–8 to 1.0×10–5mol·L–1 with a detection limit of 5.0×10–9mol·L–1 in an accumulation time of 5min. Interferences of some inorganic and organic species on the response have been studied.  相似文献   

12.
In this work, a multicommutated flow system incorporating a sol–gel optical sensor is proposed for direct spectrophotometric determination of Cu(II) in urine. The optical sensor was developed by physical entrapment of 4-(2-pyridylazo)resorcinol (PAR) in sol–gel thin films by means of a base-catalysed process. The immobilised PAR formed a red 2:1 complex with Cu(II) with maximum absorbance at 500 nm. Optical transduction was based on a dual-colour light-emitting diode (LED) (green/red) light source and a photodiode detector. The sensor had optimum response and good selectivity towards Cu(II) at pH 7.0 and its regeneration was accomplished with picolinic acid. Linear response was obtained for Cu(II) concentrations between 5.0 and 80.0 g L–1, with a detection limit of 3.0 g L–1 and sampling frequency of 14 samples h–1. Interference from foreign ions was studied at a 10:1 (w/w) ion:Cu(II) ratio. Results obtained from analysis of urine samples were in very good agreement with those obtained by inductively coupled plasma mass spectrometry (ICP–MS); there was no significant differences at a confidence level of 95%.  相似文献   

13.
The ultraviolet absorbance data from experiments conducted at constant pH and total iron concentration but variable B(OH)3 concentration were used to determined the stability constants of FeB(OH) 4 2+ and Fe[B(OH)4 2 + at 25°C and an ionic strength of 0.68. The estimates obtained were *1 = 1.0 ± 0.2 × 10–2 and *2 = 2 ± 1 × 10–5, respectively (uncertainties are two times the standard error of the estimates). A calculation of the extent of iron(III) borate formation in ocean water at pH 8.2 shows that iron(III) borates are not a significantly large component of iron(III) speciation in seawater.  相似文献   

14.
Procedures were developed for determining ionol by voltammetry and by coulometric titration with electrogenerated chlorine using the amperometric indication of the titration end point. Possible mechanisms of ionol oxidation with electrogenerated chlorine and its electrochemical oxidation at a glassy carbon and a gold electrode were discussed. Procedures were developed for determining ionol in mineral oil in analytical ranges from 1.0 × 10–4 to 1.0 × 10–2 M (RSD = 9%) and from 3.0 × 10–5 to 4.0 × 10–3 M (RSD = 9%) using a glassy carbon and a gold electrode, respectively. The detection limits for ionol at the glassy carbon and gold electrode were 2.8 × 10–4 and 1.0 × 10–5 M, respectively. The detection limit in coulometric titration was 20 g/mL.  相似文献   

15.
Adsorption of the cationic polymers poly(methacrylamidopropyltrimethyl ammonium chloride) (PMAPTAC) and poly(1,1-dimethylpiperidinium-3,5-diallylmethylene chloride) (PDMPDAMC) on human hair was studied by measurements of the amount of polymer adsorbed and by the streaming potential method. Results reflect the amphoteric nature of the keratin surface and show that the excess of anionic sites at pH values above 4 is the main driving force for the adsorption of cationic polyelectrolytes. Lowering the pH below 4 or addition of neutral salt (KCl) reduces the amount of adsorbed polymer. It was shown that the adsorption of cationic polymer in the concentration range 0.01 to 0.1 % and at neutral pH reverses the overall character of the surface from anionic to cationic. Keratin fibers modified in this manner do not exhibit amphoteric character and bear excess positive charge in the pH range 2–9.5. The value of the amount of the polymer adsorbed at saturation concentration (2 mg/g) as well as the lack of molecular weight effect in the range (5 · 104 – 106) on the amount of polymer adsorbed suggest that polymer chains adopt a rather extended conformation on the fiber surface. Some data concerning the formation of a complex between adsorbed cationic polymer and anionic detergents or polyelectrolytes are also presented.  相似文献   

16.
A reliable and reproducible method, capillary zone electrophoresis with amperometric detection (CZE–AD), has been developed for separation and quantification of levodopa methyl ester (LDME) and its biotransformation products levodopa (L-DOPA) and dopamine (DA) in rat serum. A carbon-disk electrode was used as working electrode. The optimum conditions for CZE detection were 50 mmol L–1 phosphate solution at pH 7.0 as running buffer, 17 kV as separation voltage, 1.0 V (vs Ag/AgCl, 3.0 mol L–1) as detection potential, and sample injection for 8 s at 17 kV. The linear ranges were from 2.4×10–2 to 2.2 g mL–1 for LDME, 2.9×10–1 to 49.5 g mL–1 for L-DOPA, and 1.4×10–2 to 1.5 g mL–1 for DA with correlation coefficients of 0.9997, 0.9994, and 0.9999, respectively. The detection limits for LDME, L-DOPA, and DA were 14.6, 98.0, and 9.7 ng mL–1, respectively. Recoveries were 80.3% for LDME, 93.5% for L-DOPA, and 86.5% for DA. This method was applied to serum samples after intravenous injection of LDME and L-DOPA to rats.  相似文献   

17.
Summary A new spectrophotometric method for the determination of iron (III) after adsorption of its red TTA complex onto microcrystalline naphthalene has been developed. Iron(III) reacts with 2-thenoyltri-fluoroacetone in pH range 2.4–5.2 to form a water-insoluble 13 red complex which is easily adsorbed onto microcrystalline naphthalene from its acetone solution. The naphthalene mixture is separated, dried and dissolved in 10 ml dioxane. The red organic phase has a plateau around 480–500 nm while the reagent has no absorbance beyond 420 nm. The system obeys Beer's law over 20–120g iron(III) in 10 ml of dioxane solution or 0.4–2.4 ppm aqueous. The molar absorptivity of the complex species is 3.9×103·l·mol–1·cm–1, while the sensitivity for Fe(III) extends to 1.43×10–2 g cm–2 for 0.001 absorbance. Samples containing 80g of iron gave a relative standard deviation of 1.23%. The effects of experimental variables such as pH, amount of reagents, shaking and digestion time, aqueous volume and diverse ions have been examined. The method has been applied to the determination of iron(III) in standard reference and environmental samples and results compared with other standard colorimetric procedures.
Spektrophotometrische Bestimmung von Eisen(III) nach Adsorption seines 2-Thenoyltrifluoraceton-Komplexes an mikrokristallines Naphthalin
Zusammenfassung Eine neue spektrophotometrische Methode zur Bestimmung von Eisen (III) nach Adsorption seines roten TTA-Komplexes an mikrokristallines Naphthalin wurde ausgearbeitet. Fe(III) reagiert mit 2-Thenoyltrifluoraceton bei pH 2,4-5,2 unter Bildung eines roten, wasser-unlöslichen 13-Komplexes, der sich aus seiner acetonischen Lösung leicht an mikrokristallines Naphthalin adsorbieren läßt. Das Naphthalin-Gemisch wird abgetrennt, getrocknet und in 10 ml Dioxan gelöst. Die rote organische Phase hat ein Adsorptions-Plateau bei 480–500 nm, während das Reagens jenseits 420 nm nicht adsorbiert. Das System entspricht dem Beerschen Gesetz von 20–120g Fe(III) in 10 ml Dioxan-Lösung bzw. 0,4–2,4 ppm in wäßriger Lösung. Die molare Extinktion der Komplexverbindung beträgt 3,9× 103l·mol–1·cm–1. Die Empfindlichkeit für Fe(III) entspricht 1,43×10–2 g cm–2 für 0,001 Absorptionseinheiten. Proben mit 80g Fe(III) zeigen eine rel. Standardabweichung von 1,23%. Die Wirkung variabler Versuchsbedingungen pH, Reagensmenge, Zeit, Volumen und diverse Fremdionen wurden geprüft. Das Verfahren wurde an Standardsubstanzen geprüft und seine Ergebnisse mit denen anderer kolorimetrischer Verfahren verglichen.
  相似文献   

18.
New macromolecular chelators have been synthesized, by loading 2,3-dihydroxypyridine (DHP) on cellulose via linkers -NH-CH2-CH2-NH-SO2-C6H4-N=N- and -SO2-C6H4-N=N-, and characterized by elemental analysis, TGA, IR, and CPMAS 13C NMR spectra. The cellulose with DHP anchored by the shorter linker had better sorption capacity (between 69.7 and 431.1 mol g–1) for Co(II), Ni(II), Cu(II), Zn(II), Cd(II), Pb(II), and Fe(III)) than the other (51.9–378.1 mol g–1); the former was therefore studied in detail as a solid extractant for these metal ions. The optimum pH ranges for quantitative sorption (recovery 97.6–99.8%) on this matrix were: 7.0–9.0, 6.0–9.0, 3.0–8.0, 6.0–8.0, 6.0–9.0, 6.0–7.0, and 2.0–6.0 respectively. Desorption was quantitative with 0.5 mol L–1 HCl and 0.5 mol L–1 HNO3 (for Pb). Simultaneous sorption (at pH 7.0) of all metal ions other than Fe(III) was possible if their total concentration did not exceed the sorption capacity (lowest value). The recovery of seven metal ions from their mixture at pH 6.0 was nearly quantitative when the concentration level of each metal ion was 0.2 g mL–1. The optimum flow rate of metal ion solutions for quantitative sorption of metal onto a column packed with DHP-modified cellulose was 2–7 mL min–1, whereas for desorption the optimum flow rate for the acid solution was 2–4 mL min–1. The time needed to reach 50% of the total loading capacity (t1/2) was <5 min for all the metal ions except Ni and Pb. The limit of detection (blank+3s) was from 0.70 to 4.75 g L–1 and the limit of quantification (blank+10s) was between 0.79 and 4.86 g L–1. The tolerance limits for NaCl, NaBr, NaI, NaNO3, Na2SO4, Na3PO4, humic acid, EDTA, Ca(II), and Mg(II) for sorption of all metal ions are reported. The column packed with DHP-anchored cellulose can be reused at least 20 times for enrichment of metal ions in water sample. It has been used to enrich all the metal ions in pharmaceutical and water samples before their determination by flame AAS. RSD for these determinations was between 1.1 and 6.9%.  相似文献   

19.
A reagent-free sorption photometric method for determining trace iron(III) in alkali-metal and ammonium thiocyanates was developed. The method consists in the adsorption of iron(III) thiocyanate complexes on polyurethane foams at pH 2–3 followed by the desorption of complexes with acetone and a measurement of the absorbance of solutions. The analytical range for iron was 0.5–20 g in a 0.2–2.5-g portion of salt. The determination limit and relative standard deviation were 2 × 10–5% and 20–30%, respectively (n= 3; P= 0.95). The specific feature of the determination is that an additional photometric reagent is not introduced in the solution of the salt to be analyzed, because thiocyanate, that is, the matrix component of the test sample, acts as such a reagent.  相似文献   

20.
Aspartic acid was covalently grafted on to a glassy carbon electrode (GCE) by amine cation radical formation in the electrooxidation of the amino-containing compound. X-ray photoelectron spectroscopic (XPS) measurement and cyclic voltammetric experiments proved the aspartic acid was immobilized as a monolayer on the GCE. Electron transfer to Fe(CN)64– in solution of different pH was studied by cyclic voltammetry. Changes in solution pH resulted in the variation of the charge state of the terminal group; surface pKa values were estimated on the basis of these results. Because of electrostatic interactions between the negatively charged groups on the electrode surface and dopamine (DA) and ascorbic acid (AA), the modified electrode was used for electrochemical differentiation between DA and AA. The peak current for DA at the modified electrode was greatly enhanced and that for AA was significantly reduced, which enabled determination of DA in the presence of AA. The differential pulse voltammetric (DPV) peak current was linearly dependent on DA concentration over the range 1.8×10–6–4.6×10–4 mol L–1 with slope (nA mol–1 L) and intercept (nA) of 47.6 and 49.2, respectively. The detection limit (3) was 1.2×10–6 mol L–1. The high selectivity and sensitivity for dopamine was attributed to charge discrimination and analyte accumulation. The modified electrode has been used for determination of DA in samples, in the presence of AA, with satisfactory results.  相似文献   

设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号