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1.
Summary Barium-137m radioisotope generator of the chromatographic column elution mode based on loading 1.5 g 6-tungstocerate(IV) gel matrix with ~54 kBq of fission-produced 137Cs is described. The elution performance of the generated 137mBa radionuclide was investigated as a function of chemical composition of the eluent, flow rate, elution frequency, and age of the generator system. At comparable conditions, 137mBa eluates with 0.9% NaCl-0.1M HCl eluent had higher elution yields and radionuclidic purity than with 0.1M NH4Cl-0.1M HCl eluent. The generator has been repeatedly eluted for 311 days by passing 4810 ml of the saline eluent (10 ml × 481 elution operations) at a flow rate of 3.0 ml/min. Barium-137m eluates of high and reproducible elution yields, chemical and radionuclidic purities of (≥ 99.99%) were obtained.  相似文献   

2.
The extraction of Nd(III) using binary mixtures of Cyanex 272 (HA), Cyanex 921/Cyanex 923 (B) in kerosene from nitric acid medium has been investigated. The effect of aqueous phase acidity, extractant concentration, nitrate ion concentration and diluents on the extraction of Nd(III) has been studied. On the basis of slope analysis results, extracted species are proposed as Nd(NO3)A2·3HA and Nd(NO3)2·A·3HA·B using Cyanex 272 and its mixture with Cyanex 921/Cyanex 923, respectively. With the mixture of 0.1 M Cyanex 272 and 0.1 M Cyanex 923 in kerosene, the extraction of 0.001 M Nd(III) from 0.001 M HNO3 solution was found to be 83.3 % whereas it was 73.3 % when 0.1 M Cyanex 921 used as synergist under same experimental conditions. The stripping data of Nd(III) from the loaded organic phase containing 0.1 M Cyanex 272 and 0.1 M Cyanex 921/Cyanex 923 with different acids indicated sulphuric acid to be the best stripping agent.  相似文献   

3.
An electrochemistry-based gravimetric method of analysis for the determination of thiosulfate concentrations in aqueous solutions and its application in chemical education are introduced. Nine standard aqueous thiosulfate solutions with triplicate concentrations of 0.02 M, 0.03 M, and 0.04 M were prepared in 1.0 M hydrochloric acid. The elemental sulfur produced in each sample was recovered by filtration, and the mass of the recovered elemental sulfur and the electrochemically determined equilibrium constant of the reaction at 25°C (Keq = 3.5) were used to determine the concentration of thiosulfate in each standard solution. The method % Error is 4.9 ± 3.0, which means that the average method % Error is less than 5.0.  相似文献   

4.
Kokot  Zenon J.  Matysiak  Jan 《Chromatographia》2009,69(11):1401-1405

The aim of the study was to develop an LC method for honeybee venom analysis, using cytochrome c as an internal standard. The SynChropack C8 6.5 μm, 4.6 × 100 mm column was applied. The bee venom was separated by linear gradient 5–80% B at 30 min (eluent A—0.1% TFA in water, eluent B—0.1% TFA in acetonitrile:water (80:20)). The flow rate of mobile phase was maintained at 1 mL min−1, injection volume: 40 μL, separation temperature: 25 °C. The analysis was monitored at 220 nm. Several honeybee venom constituents were separated and the content of four of them (apamine, mast cell degranulating peptide, phospholipase A2 and melittin) were determined. By applying this methodology differences in chemical composition of honeybee venom were evaluated. In order to confirm the data obtained, the following steps and parameters were taken into account for the validation of the method: selectivity, precision (injection repeatability, analysis repeatability), accuracy (recovery), linearity and operating range, limit of detection and limit of quantitation. All steps of validation proved that the developed analytical procedure was suitable for its intended purpose (standardization). Due to its simplicity, the developed method can be easily automated and incorporated into routine operations both in the bee venom identification, quality control and assay tests.

  相似文献   

5.
The aim of the study was to develop an LC method for honeybee venom analysis, using cytochrome c as an internal standard. The SynChropack C8 6.5 μm, 4.6 × 100 mm column was applied. The bee venom was separated by linear gradient 5–80% B at 30 min (eluent A—0.1% TFA in water, eluent B—0.1% TFA in acetonitrile:water (80:20)). The flow rate of mobile phase was maintained at 1 mL min?1, injection volume: 40 μL, separation temperature: 25 °C. The analysis was monitored at 220 nm. Several honeybee venom constituents were separated and the content of four of them (apamine, mast cell degranulating peptide, phospholipase A2 and melittin) were determined. By applying this methodology differences in chemical composition of honeybee venom were evaluated. In order to confirm the data obtained, the following steps and parameters were taken into account for the validation of the method: selectivity, precision (injection repeatability, analysis repeatability), accuracy (recovery), linearity and operating range, limit of detection and limit of quantitation. All steps of validation proved that the developed analytical procedure was suitable for its intended purpose (standardization). Due to its simplicity, the developed method can be easily automated and incorporated into routine operations both in the bee venom identification, quality control and assay tests.  相似文献   

6.
The effect of physicochemical parameters such as pH, salinity (e.g. [NaCl]) and competitive cation (e.g. Ca2+ and Fe3+) concentration on the separation recovery of plutonium and uranium from aqueous solutions by cation exchange has been investigated. The investigation was performed to evaluate the applicability of cation exchange as separation and pre-concentration method prior to the radiometric analysis of uranium and plutonium isotopes in natural water samples. Application of the method to test solutions of constant radionuclide concentration and variable composition (0.1, 0.5 and 1 M NaCl; 0.1 and 0.5 M Ca(NO3)2; 0.1 and 1 mM FeCl3; 10) has generally shown that: (1) the optimum pH is 4.5 for uranium and plutonium, (2) increasing salinity results in slightly lower for uranium and significantly higher chemical recovery plutonium and (3) the presence of Ca(II) cations doesn’t significantly affect the chemical recovery of both radionuclides. Contrary, the presence of Fe(III) cations ([Fe(III)] > 0.1 mM) results in significantly lower chemical recovery for both radionuclides (<50%). The later is attributed to the formation of Fe(III) colloids, which present increased chemical affinity for uranium and plutonium and hence compete with the radionuclide binding by the resin. Nevertheless, the results indicate that the method could be successfully applied to a wide range of natural waters.  相似文献   

7.
This work investigates the use of HPLC-SEC to characterise dissolved organic matter (DOM) of complex wastewater effluents. A silica-based column, sodium acetate eluent and multiple detections were employed: UV-254 absorbance for humictype, and tryptophan-like (Ex/Em = 270/355) and tyrosine-like (Ex/Em = 270/310) fluorescence for protein type compounds. Effects of eluent pH, eluent ionic strength and injection volume on separation efficiency were tested. Humic-type and protein-type fractions were clearly differentiated and eluted within and out of calibration range. Eluent ionic strength had the greatest influence on global resolution; the lowest eluent concentration of 0.01 M produced the best separation for all wastewater effluents tested at any detection. UV-254 absorbance was higher at neutral and basic eluent pH while tryptophan-like fluorescence depended on the sample composition rather than on the eluent pH or ionic strength. Tyrosine-like fluorescence decreased significantly with the increase of eluent ionic strength. Accurate molecular weight measurements could not be done, the separation being influenced by secondary interactions, but could be approximated using separate calibrations with sodium salts of polystyrene-sulfonates and protein standards. The results show that this method is suitable for determining DOM in wastewater at low eluent concentrations (up to 0.03 M), at neutral or slightly basic pH.  相似文献   

8.
《Analytical letters》2012,45(14):2417-2430
Diethyldithiocarbamate and 2-mercaptoethanol modifiers were compared for the preconcentration of mercury species in water by C18 solid phase extraction (SPE). The recovery values of mercury species were determined by high performance liquid chromatography–atomic fluorescence spectrometry. The eluent type, pH, chloride ion concentration, humic acid concentration, and storage time were evaluated to compare the preconcentration efficiency. L-cysteine was employed to elute the mercury compounds. Less eluent was needed for 2-mercaptoethanol modified SPE than for diethyldithiocarbamate modified SPE at an L-cysteine concentration of 0.12%. Diethyldithiocarbamate modified SPE could be used over a wider pH range and higher humic acid concentrations, whereas 2-mercaptoethanol modified SPE was less affected by the chloride concentration. Both modified SPE systems stored mercury species for 5 days, but diethyldithiocarbamate modified SPE could be stored longer. Diethyldithiocarbamate SPE provided limits of detections of 3.5, 2.5, and 4 ng · L?1 and average recoveries of 90.78 ± 3.37%, 96.79 ± 5.12%, and 84.88 ± 5.37% for mercury(II), methylmercury, and ethylmercury, respectively. The relative standard deviation was less 6.5%. For 2-mercaptoethanol modified SPE, the limits of detection were 1.4, 1, and 1.6 ng · L?1 and the recoveries were of 87.66 ± 8.45%, 86.70 ± 2.61%, and 91.31 ± 6.98% for mercury(II), methylmercury, and ethylmercury, respectively, with a relative standard deviation below 9.7%. Water should be characterized for its physical and chemical characteristics before mercury preconcentration to choose the most suitable method.  相似文献   

9.
An investigation was carried out into the fast determination of five homologue imidazolium cations in ionic liquids by ion chromatography using a cation-exchange column and direct conductivity detection. Ethylenediamine, complex organic acid (citric acid, oxalic acid and tartaric acid) and organic modifiers (acetonitrile) were used as mobile phase. The influences of the eluent types, eluent concentration, eluent pH and column temperature on separation of the cations were discussed. Simultaneous separation and determination of the five homologue imidazolium cations in ionic liquids were achieved under an optimum condition. The optimized mobile phase was consisted of 0.25 mmol L?1 ethylenediamine + 0.5 mmol L?1 citric acid + 3% acetonitrile (v/v) (pH 4.1), set at a flow rate of 1.0 mL min?1. The column temperature was 40 °C and detection limits were obtained in the range of 1.1–45.6 mg L?1. The relative standard deviations of the chromatographic peak areas for the cations were <3.0% (n = 5). This method was successfully applied to separate imidazolium cations in ionic liquids produced by organic synthesis. The recoveries of spiked components were 92.5–101.9%.  相似文献   

10.
A simple and sensitive method is presented for solid phase extraction (SPE) and preconcentration of trace quantities of beryllium using octadecyl silica gel modifed with aurin tricarboxylic acid (aluminon). Beryllium is then determined by flame atomic absorption spectroscopy. Parameters affecting SPE such as pH, sample solution and eluent flow rate, type, concentration and volume of eluent, interfering ions and breakthrough volume, were investigated. Under optimal conditions, the beryllium ions were retained on the sorbent at pH 6–6.7, while 3.0 mL of 0.05 mol L?1 HNO3 is sufficient to elute the ions. The limit of detection (LOD) based on 3σ was 0.8 µg L?1 for 250 mL sample solution and 5 mL 0.05 mol L?1 HNO3 as eluent. The LOD can reach 0.1 µg L?1 for 1 L sample solution and 3 mL of 0.05 mol L?1 HNO3. The accuracy and precision (RSD %) of the method is >90% and <10%, respectively. The method was applied to the determination of beryllium in aqueous samples.  相似文献   

11.
Two commonly used chemical pretreatment processes, sulphuric acid, and sodium hydroxide, were tested to provide comparative performance data. A connection between solid to liquid ratio (S/L) and sugars released was observed with an increase in S/L ratio between 0.02 and 0.2. Enzymatic digestibility of 1 M of NaOH-pretreated corncobs were released 210.7 mg ml?1 of sugars. Further, compared with different concentrations of acid pretreatments at 0.05, 0.1, 0.15, 0.2, 0.25, 0.3, and 0.5 M concentrations, sodium hydroxide pretreatment of corncob substantially increased accessibility and digestibility of cellulose. Another additional observation made was whole-cell and crude enzymatic hydrolysis of different concentrations of acid and NaOH (0.05, 0.1, 0.25 M)-treated materials released lower amount of sugars compared with the sugars released (310.9 mg ml?1) with whole-cell hydrolysis of 1 M of NaOH-treated corncobs. NaOH-pretreated corncobs contained higher content of sugars and which is more suitable for production of reducing sugars.  相似文献   

12.
A new solid-phase extraction method utilising polyacrylonitrile activated carbon fibres (PAN-ACFs) as adsorbent was developed for the preconcentration of trace metal ions prior to their determination by inductively coupled plasma optical emission spectrometry (ICP-OES). The PAN-ACFs oxidised with nitric acid were characterised by FT-IR, XRD, SEM and BET analysis. Then the resulting PAN-ACFs were used as solid-phase adsorbent for simultaneously determination of trace Al(III), Be(II), Bi(III), Cr(III), Cu(II), Fe(III) and Pb(II) ions in aqueous solutions. The influences of the analytical parameters on the recoveries of the studied ions were investigated. The optimum experimental conditions of the proposed method were pH: 6.0; eluent concentration and volume: 3.0 mL of 1.5 mol L?1 nitric acid; flow rates of sample and eluent solution: 1.5 mL min?1. The preconcentration factors were found to be 67 for Al(III), Bi(III); 83 for Cr(III), Cu(II), Fe(III) and 50 for Be(II), Pb(II). The precision of this method was in range of 1.5%~3.5% and the detection limit of this metal ions was between 0.06~1.50 μg L?1. The developed method was validated by the analysis of a certified reference sample and successfully applied to the determination of trace metal ions in water samples with satisfactory results.  相似文献   

13.
A highly sensitive sensor based on Ni nanoparticles/poly (1,2-diaminoanthraquinone) modified electrode was fabricated at glassy carbon (GC) electrode (Ni/PDAAQ@GC ME) using cyclic voltammetry technique. The incorporation of nickel (II) ions nanoparticles (Ni NPs) followed by anodic polarization process was achieved. Surface morphologies of both PDAAQ@GC ME and Ni/PDAAQ@GC MEs were studied by scanning electron microscope. Ni/PDAAQ@GC ME was tested for simultaneous determination of ascorbic acid (AA), dopamine (DA) and uric acid (UA) by square wave voltammetry technique. The ME showed excellent electrocatalytic activity toward electrooxidation of these biomolecules in their single, binary and ternary systems in alkaline 0.1 M NaOH solutions. Experiment revealed that the low detection limits (LOD) for AA, DA and UA were 0.11, 0.072 and 1.2 µM in single system, respectively, and 0.069, 0.29 and 0.12 µM in ternary system, respectively.  相似文献   

14.
《Analytical letters》2012,45(3):589-602
Abstract

The UV‐VIS spectrophotometric methods for the determination of Os(VIII) (as OsO4) and Os(IV) (as OsCl6 2? complex) in their mixtures were developed. Quercetin (Q), a flavonoid compound, was used as a chromogenic reagent. Both direct and derivative spectrophotometry can be employed for the determination of Os(VIII). The calculation of the first‐derivative spectrum of the examined mixture and the use of the signal at 285.1 nm allows reaching a better detection limit (0.01 µg mL?1 Os) as compared with direct spectrophotometry (0.1 µg mL?1 Os). Relative standard deviations of the results are in the range of 0.87%–4.65% and 0.45%–1.15% for direct and derivative mode, respectively. Selective redox reaction of OsO4 with Q under the conditions used (0.05 M HCl, 1×10?4 M Q, 15 min heating at 70°C) makes the basis of its determination in mixtures with the OsCl6 2? complex. Quercetin does not react with the OsCl6 2? complex. The signals of the OsCl6 2? complex can be isolated from the examined mixtures by the calculation of the third‐order derivative spectra and the use of the values at 340.0 nm. The effectiveness of the reduction of OsO4 in chloride solutions has been studied by the developed method.  相似文献   

15.
In this study, a rapid, sensitive, and fully automated on-line solid phase extraction (SPE)?Cliquid chromatography (LC)?Cmass spectrometry (MS) method for the analysis of explosive residues in water, was systematically investigated. First, separation of explosive residues was achieved by reverse-phase chromatography using an XDB-C18 column in 30 min with an eluent containing 0.1% acetic acid, 5 mM ammonium acetate, and methanol. Secondly, atmospheric pressures chemical ionization (APCI) and electrospray ionization (ESI) interfaced with the MS detector were used to examine the explosive residues, indicating that APCI?CMS was more suitable than ESI?CMS for the detection of explosives. Thirdly, the conditions for on-line SPE, including solvent pH and sample injected volume, were optimized. The calibration curves obtained for all explosives studied were linear in the concentration range 0.5?C50 ??g L?1. The detection limits of this method ranged from 0.05 to 0.5 ??g L?1 when 4000 ??L of sample was on-line pre-concentrated on C18 enrichment column. The recoveries from lake waters spiked with explosive standard solution ranged from 90.5 to 108.0%. The proposed method is simple, fast, and could be applied successfully to the analysis of explosive residues in contaminated water without any further pretreatment.  相似文献   

16.
《Analytical letters》2012,45(3):442-452
A procedure for the determination of trace levels of Cd, Co, Cr, Fe, Mn, Ni, and Pb by flame atomic absorption spectrometry using a column preconcentration system is described in which the metals were adsorbed on pulverized banana peel, an economically and environmentally acceptable sorbent. In the optimization procedure, five variables (sample pH, mass of biosorbent, type of eluent, sample flow rate, and volume) were optimized and the capacity of the biosorbent was established. Under the optimized conditions, the detection limits of the method were 2.4, 27.0, 49.4, 31.1, 6.7, 29.6, and 46.2 µg L?1 for Cd, Co, Cr, Fe, Mn, Ni, and Pb, respectively. The precision, expressed as relative standard deviation, was less than 4% based on twelve measurements. The recoveries were 81.1% (Cd), 91.4% (Co), 87.2% (Cr), 90.1% (Fe), 88.0% (Mn), 94.1% (Ni), and 93.2% (Pb) under the optimum conditions (pH; 9, sample flow rate; 3 mL min?1, mass of biosorbent; 200 mg; eluent; 1 mol L?1 nitric acid, preconcentration factor; 10). The sorption capacity of pulverized banana peel was 15.12, 28.85, 32.70, 30.44, 30.94, 28.97, and 8.21 µmol per gram of adsorbent for Cd, Co, Cr, Fe, Mn, Ni, and Pb, respectively.  相似文献   

17.
This study aims at investigating physical–chemical properties of a water-soluble heteropolysaccharide from Plnatago asiatica L. leaves, and its immunomodulatory effects on macrophages RAW264.7 cells. Hot water-extracted crude polysaccharide from the plant leaves (PLLCP) was fractionated into four fractions by DEAE Sepharose Fast Flow eluted with 0.1–0.5 M NaCl solutions. The most abundant fraction (0.3 M NaCl elution), designated PLLP-2, was identified as a heteropolysaccharide with an average molecular weight (Mw) of 3.54 × 104 and composed mainly of Gal (34.4%), GalA (36.5%), Ara (10.1%) and Rha (8.4%). PLLP-2 was an acidic polysaccharide exhibiting inflaky curly aggregation with smooth surface. PLLCP and its main subfraction PLLP-2 displayed immunomodulatory activities by stimulating the production of pro-inflammatory cytokines, including TNF-α and IL-1β in macrophage RAW264.7 cells. These results indicate that the main polysaccharide fraction purified from P. asiatica L. leaves is probably pectin, and have potential immunomodulatory function.  相似文献   

18.
The unsymmetrical diglycolamides (DGAs) such as N,N-dihexyl-N′,N′-dioctyl-3-oxapentane-1,5-diamide (DHDODGA), N,N-didecyl-N′,N′-dioctyl-3-oxapentane-1,5-diamide (D2DODGA), N,N-didodecyl-N′,N′-dioctyl-3-oxapentane-1,5-diamide (D3DODGA), were synthesized, and characterized by IR, NMR, and mass spectroscopic techniques. The extraction behaviour of Am(III), Eu(III), and Sr(II) by the solutions of these unsymmetrical DGAs in n-dodecane was studied as a function of concentration of nitric acid and DGA. The distribution ratio of Am(III) and Eu(III) increased with increase in the concentration of nitric acid; whereas, the distribution ratio of Sr(II) reached a maximum at 4 M nitric acid followed by decrease at higher acidities. The extraction of Am(III) and Eu(III) in 0.1 M DGA/n-dodecane decreased in the order DHDODGA > D2DODGA > D3DODGA. However, the order changed upon lowering the concentration of DGA. The third-phase formation behaviour of nitric acid and neodymium(III) in 0.1 M DGA/n-dodecane was studied as a function of concentration of nitric acid. The limiting organic concentration of nitric acid and neodymium increased with increase in the chain length of alkyl group attached to amidic nitrogen. Near stoichiometric amount of neodymium(III) was loaded in 0.1 M D3DODGA/n-dodecane without the formation of third-phase from 3 to 4 M nitric acid medium. The study revealed that the unsymmetrical diglycolamides D2DODGA and D3DODGA are superior candidates for partitioning the minor actinides from high-level liquid waste.  相似文献   

19.
A separation procedure of Ni has been described for the quantification of 59Ni and 63Ni in radioactive wastes discharged from nuclear power plants and various research activities related to the nuclear fuel cycle. For a rapid separation of the Ni-nuclides in sixteen sample solutions in 0.2 M NH4-oxalate, a separation system composed of a peristaltic pump with sixteen channels and the same number of Ni–Resin columns was constructed. After sorption of the Ni-nuclides by sequentially passing 100 mL of the sample solution in 0.2 M NH4-oxalate, 130 mL of 0.1 M NH4-oxalate solution and 10 mL of deionized water as a wash into the columns, these were purely recovered by passing 10 mL of 9 M HCl into the Ni–Resin columns stacked in series on the anion exchange resin columns. The separation of the Ni-nuclides in sixteen sample solutions can be achieved within 7 h. The chemical yield of the proposed procedure is 92.3 ± 0.8 % (n = 5) and the gravimetric recovery in the preparation stage of the Ni-nuclide sources is also acceptable, 88.5 ± 1.3 % (n = 5).  相似文献   

20.
《Analytical letters》2012,45(13):2049-2060
An analytical procedure has been evolved for the determination of seven guanidino compounds; guanidine (G), methylguanidine (MG), guanidinoacetic acid (GAA), guanidinopropionic acid (GPA), guanidinobutyric acid (GBA), arginine (Arg), and guanidinosuccinic acid (GSA) by micellar electrokinetic capillary chromatography (MEKC) within 6 min using benzoin as derivatizing reagent. Sodium dodecyl sulfate (SDS) was used as the micellar medium in a sodium tetraborate (0.1 M) buffer at pH 8.5. Uncoated fused silica capillary was used with an effective length of 39 cm and 75 μm id. Applied voltage was 25 kV and photo diode array detection was set at 228 nm. Linear calibrations obtained from 0.057 to 14.11 μmol/L and limits of detection (LOD) were within 0.019–0.03 μmol/L. The derivatization and separation was repeatable with relative standard deviation (RSD) within 1.9–3.8%. Serum of healthy volunteers and uremic patients was analyzed and amounts found in uremic patients were G 1.98–3.03, MG 1.21–1.79, GAA 3.67–6.09, GPA 1.17–1.37, GBA 1.29–1.46, Arg 9.49–19.17, and GSA 6.83–10.91 μmol/L with RSD (n = 4) within 1.3–4.5%. The amount of guanidino compounds was higher in uremic patients than in healthy volunteers.  相似文献   

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