共查询到20条相似文献,搜索用时 46 毫秒
1.
A. N. Dubey G. R. Relan S. Vaidyanathan 《Journal of Radioanalytical and Nuclear Chemistry》1999,240(3):741-746
A derivative spectrophotometric method has been developed for the simultaneous determination of uranium and plutonium at trace
levels in various process streams in 3M HNO3 medium using Arsenazo III. The method was developed with the objective of measuring both uranium and plutonium in the same
aliquot in fairly high burn-up fuels. The first derivative absorbances of the uranium and plutonium Arsenazo III complexes
at 632 nm and 606.5 nm, respectively, were used for their quantification. Mixed aliquots of uranium (20–28 μg/ml) and plutonium
(0.5–1.5 μg/ml) with U/Pu ratio varying from 25 to 40 were analysed using this technique. A relative error of about 5% was
obtained for uranium and plutonium. The method is simple, fast and does not require separation of uranium and plutonium. The
effect of presence of many fission products, corrosion products and complexing anions on determination of uranium and plutonium
was also studied. 相似文献
2.
A rapid extractive photometric method using Aliquat-336 and xylenol organe for the determination of plutonium(IV) at μg levels
has been developed. Quantitative extraction is obtained from ∼4M aqueous HNO3 medium, affording estimation in the presence of several commonly occurring impurities, viz. iron, uranium, fission products
and cladding materials. Effects of acidity, reagent concentration and diverse ions on the estimation have also been invetigated.
Unlike the well-known absorptiometric method for determining plutonium(IV) employing Arsenazo III, the procedure presented
here tolerates manyfold excesses of uranium(VI) as well as chromium(III), iron(III) and zirconium(IV), which are some of the
major contaminants of plutonium during reprocessing. 相似文献
3.
F. Sus J. Krtil V. Bulovič E. Klosová Z. Maksimovič 《Journal of Radioanalytical and Nuclear Chemistry》1979,51(1):143-151
Determination of the isotopic composition and concentration of uranium, plutonium and neodymium by mass-spectrometric isotope
dilution is described. Isotopes233U,242Pu and150Nd were used as spikes. Isotopic composition was measured with a Varian-TH 5 mass spectrometer. Optimum amounts loaded onto
the filament were 2–5 μg U, ∼0.1 μg Pu and <0.1 μg Nd. The accuracy and reproducibility of the isotopic ratio and concentration
measurements were evaluated. 相似文献
4.
Y. Baba 《Journal of Radioanalytical and Nuclear Chemistry》1983,79(1):83-92
A combined solvent extraction—liquid scintillation method is suggested for the determination of plutonium. The quenching by
twenty four extracting reagents was examined systematically, and the organo phosphorus extractants such as tributylphosphate
(TBP), bis-(2-ethyhexyl) phosphoric acid (HDEHP), and tri-n-octylphosphineoxide (TOPO) were shown to be least quenching compared
with amines and beta-diketones. Using TOPO, plutonium from 1 ng to 2 μg was determined within 5% of standard deviation, and
the detection limit was 3·10−10 g of239Pu. The quenching by the different ions and the effects of the radioactive elements were also shown. 相似文献
5.
A highly sensitive and very simple spectrophotometric flow-injection analysis (FIA) method for the determination of iron(III)
at low concentration levels is presented. The method is based on the measurement of absorbance intensity of the red complex
at 410 nm formed by iron(III) and diphenylamine-4-sulfonic acid sodium salt (DPA-4-SA). It is a simple, highly sensitive,
fast, and low cost alternative method using the color developing reagent DPA-4-SA in acetate buffer at pH 5.50 and the flow-rate
of 1 mL min−1 with the sample throughput of 60 h−1. The method provided a linear determination range between 5 μg L−1 and 200 μg L−1 with the detection limit (3S) of 1 μg L−1 of iron(III) using the injection volume of 20 μL. FIA variables influencing the system performance were optimized. The amount
of iron(III) and total iron in river and seawater samples was successfully determined. Repeatability of the measurements was
satisfactory at the relative standard deviation of 3.5 % for 5 determinations of 10 μg L−1 iron(III). The accuracy of the method was evaluated using the standard addition method and checked by the analysis of the
certified material Std Zn/Al/Cu 43 XZ3F. 相似文献
6.
R. T. Chitnis S. G. Talnikar V. A. Thakur A. H. Paranjape 《Journal of Radioanalytical and Nuclear Chemistry》1979,49(1):63-70
The method for plutonium determination based on secondary controlled-potential coulometry, as described by SHULTS, is applied
for analysis in the range of 0.1–5 mg plutonium. The method involves the oxidation of plutonium to Pu(VI) with perchloric
acid followed by its reduction by an internally generated ferrous mediator. This is a two step procedure, involving the reduction
of Pu(VI) and Fe(III) to a mixture of Pu(III) and Fe(II), followed by the oxidation of Pu(III) and Fe(II) to Pu(IV) and Fe(III),
respectively. The net results is the reduction of Pu(VI) to Pu(IV), measured as the difference between the currents consumed
during the reduction and oxidation steps. The original method of SHULTS involves 10–25 mg plutonium for each determination.
Since the present method is intended for the analysis of smaller amounts of plutonium, the oxidation procedure described in
the original version had to be modified. The method is found to work satisfactorily with a precision better than 0.1% at 5
mg level and 1.2% for 0.1 mg plutonium. 相似文献
7.
The sorption of ions of zinc on carriers modified by 8-oxychinoline and its derivative is investigated. The optimum parameters
of sorption are revealed, based on which silochrome S-60 with immobilized 8-oxychinoline (pH 7.1, time of contact 30 min,
weight of sorbent 0.3 g, capacity of sorbent on the modifier 60 μmol/g) is chosen. A yellow-green fluorescence sorbate arises
on irradiation by ultra-violet light in a phase sorbent. The spectrum of fluorescence represents a wide unstructured strip
with a maximum at 505 nm. In the construction of a calibrated graph, Cu(II), Cd(II), Pb (II), Bi(III), and Fe(III) do not
prevent the determination of 5–50 μg of zinc; however, equal amounts of Al(III) (50–100 μg) do prevent it. The technique is
applied for the sorption-fluorimetric determination of zinc in river and waste water. The relative standard deviation does
not exceed 0.05 (n = 5). 相似文献
8.
Neelam Goyal Paru J. Purohit A. G. Page 《Fresenius' Journal of Analytical Chemistry》1998,361(5):429-432
Atomization processes for uranium in aqueous media and in the presence of a plutonium matrix have been studied and a chemical
mechanism is proposed. These studies have been utilized for the determination of uranium in plutonium by Electrothermal Atomization-
Atomic Absorption Spectrometry (ETA-AAS) within the constraints of its stable carbide forming tendency and complexity caused
by formation of plutonium suboxide at high temperatures. In spite of these limitations the analytical range obtained for determination
of uranium is 2.5–100 ng with a sample aliquot of 5 μL containing 5 mg/mL plutonium concentration. The precision of the method
is evaluated as 9% RSD.
Received: 9 September 1997 / Revised: 29 December 1997 / Accepted: 31 December 1997 相似文献
9.
E. Morosanova A. Velikorodny Y. Zolotov 《Fresenius' Journal of Analytical Chemistry》1998,361(3):305-308
Two approaches to immobilize complex-forming analytical reagents (PAN, PAR, Xylenol orange, Brombenzothiazo, Crystal violet,
Cadion, and Sulfochlorophenolazorhodanine) for the preparation of new sorbents and indicator powders are suggested: on-line
coating of reversed-phase silica gel by reagents or doping of porous sol-gel silica with reagents. The retention of Ag, Cd,
Cu(II), Co(II), Fe(III), Mn(II), Ni, Pb, and Zn on the sorbents developed was investigated. Quantitative sorption and desorption
conditions were optimized. Procedures for the determination of Cd, Cu(II), Fe(III), Pb, and Zn with flame atomic absorption,
spectrophotometric, and diffusion scattering spectrometric detection were elaborated. Detection limits for Cd, Cu(II), Fe(III),
Pb, and Zn were 3 μg/L, 6 μg/L, 5 μg/L, 40 μg/L, and 1 μg/L, respectively. The procedures were used for the analysis of various
real samples, e.g., natural and waste waters, and food.
Received: 17 July 1997 / Revised: 20 January 1998 / Accepted: 5 February 1998 相似文献
10.
A simple and rapid flow-injection spectrophotometric method for the determination of iron(III) and total iron is proposed.
The method is based on the reaction between iron(III) and O-acetylsalicylhydroxamic acid (AcSHA) in a 2 % methanol solution resulting in an intense violet complex with strong absorption
at 475 nm. Optimum conditions for the determination of iron(III) and the interfering ions were tested. The relative standard
deviation for the determination of 5 μg L−1 iron(III) was 0.85 % (n = 10), and the limit of detection (blank signal plus three times the standard deviation of the blank) was 0.5 μg L−1, both based on the injection volumes of 20 μL. The method was successfully applied in the determination of iron(III) and
total iron in water and ore samples. The method was verified by analysing a certified reference material Zn/Al/Cu 43XZ3F and
also by the AAS method. 相似文献
11.
N. K. Chaudhuri R. Sampathkumar R. H. Iyer 《Journal of Radioanalytical and Nuclear Chemistry》1976,33(1):53-65
Analysis of fissile materials in solution by fission track registration technique has been extended to plutonium in solution
of its alloys. In these estimations, the results agreed within 1–4% with the average of those obtained by other chemical and
instrumental methods like potentiometry, mass-spectrometry and X-ray fluorescence. Some special practical problems encountered
in the analysis of plutonium solutions are noted. Various factors affecting the results have been investigated and the necessary
precautions for reducing these errors have been indicated. The advantages of the method over some other conventional methods
have also been discussed. It is suggested that a source of about 10 μg of252Cf corresponding to a neutron flux of about 107 n·cm−2·sec−1 is ideal for these experiments. 相似文献
12.
V. G. Amelin N. S. Aleshin O. I. Abramenkova Yu. N. Nikolaev I. A. Lomonosov 《Journal of Analytical Chemistry》2011,66(8):709-713
A fluorimeter is developed, which provides sample pretreatment, preconcentration of analytes from natural waters on the surface
of indicator cellulose matrices, and the simultaneous measurement of their fluorescence. The device employs a L-711UVC ultraviolet
light diode and a Digital color sensor S9706 photodiode, which registers simultaneously in the red (615 nm), green (540 nm),
and blue (465 nm) spectrum regions. The opportunities of the application of this fluorimeter have been shown by an example
of determination of 1–100 μg/L Al(III) and 0.1–10 μg/L Be(II) and Ga(III). 相似文献
13.
Summary A reversed-phase ion-pair chromatographic (RPIPC) method withN,N,N′, N′-ethylenediaminetetrakis(methylenephosphonic acid) (EDTMP) as coordinating agent has been developed for simultaneous separation
and detection of Cu(II), Fe(III), and Pb(II) ions. Response is linearly dependent on amount of sample over the range 9.52–50.8
μg mL−1 for Cu(II), 8.31–41.8 μg mL−1 for Fe(III), and 37.3–51.8 μg mL−1 for Pb(II). The method has been applied successfully to an artificial mixed-ore sample. 相似文献
14.
L’. Jurica A. Manová J. Dzurov E. Beinrohr J. A. C. Broekaert 《Analytical and bioanalytical chemistry》2000,366(3):260-266
A simple and rapid procedure for the calibrationless determination of trace concentrations of As(III) and total As in contaminated
water samples is presented. Arsenic is preconcentrated as As(III) in a flow-through cell with a gold plated porous electrode
and is then stripped anodically by a constant current. The stripping chronopotentiogram is registered and evaluated. The As
concentration is calculated directly from the combined Faraday’s laws. The total As content was determined after converting
all As species to As(III) by microwave-assisted reduction with hydrazine hydrochloride in a closed vessel. The detection limit
was found to be 0.15 μg/L and the linear response range was 0.5 to 10 000 μg/L. Tap water, surface water, and waste water
samples were analyzed.
Received: 14 July 1999 / Revised: 21 September 1999 / Accepted: 24 September 1999 相似文献
15.
The feasibility of measuring plutonium and uranium concentrations in reprocessing plant solutions by tube-excited energy dispersive
XRF spectrometry is described. By using the K-series lines, materials compatible with a reprocessing plant can be used for
construction of the sample cell. Calibration data for Pu and U solutions in the range 1–10 g/l are given. Measurements are
presented which demonstrate that fission product activity at the 100 μCi/ml level and passive radiation from Pu isotopes and
their daughters present only a minor interference to the analyte signal. 相似文献
16.
This paper describes a novel method to determine methimazole by spectrophotometry using a potassium ferricyanide-Fe(III) reaction.
The study indicates that at pH 4.0 Fe(III) is reduced to Fe(II) by methimazole and in situ formed Fe(II) reacts with potassium
ferricyanide to give soluble Prussian Blue which is characterized by means of XRD analysis. The absorbance of Prussian Blue
is measured at the absorption maximum of 735 nm, and the amount of methimazole can be determined based on this absorbance.
Beer’s law is obeyed in the range of methimazole concentrations of 0.02–6.00 μg/mL. The equation of the linear regression
is A = −0.0058 + 0.49988c (μg/mL), with a correlation coefficient of 0.9998 and RSD of 0.80%. The detection limit (3σ/k) is 0.015 μg/mL, and the apparent
molar absorption coefficient of indirect determination of methimazole is 5.7 ± 104 L/mol cm. This method has been successfully applied to the determination of methimazole in pharmaceutical, serum and urine
samples, and average recoveries are in the range of 98.6–102.4%. Analytical results obtained with this novel method are satisfactory. 相似文献
17.
J. Starý J. Prášilová T. Bouda 《Journal of Radioanalytical and Nuclear Chemistry》1975,28(1-2):95-100
Very simple and rapid radiochemical procedures for the determination of traces of arsenic(III) (up to 0.1 μg) and antimony(III)
(up to 0.01 μg) have been developed. The method is based on the isotope exchange between labelled metal diethyldithiocarbamate
in carbon tetrachloride and an aqueous sample containing the metal to be determined. The selectivity of the method is rather
high; in the presence of thiourea most common metals do not interfere with the determination. 相似文献
18.
Rapid kinetic determination of silver (I), using in-cuvette mixing and computerized data acquisition 总被引:1,自引:0,他引:1
The determination of silver(I) based on its catalytic effect on the oxidation of indigo carmine with hexacyanoferrate(III)
is described. The reaction is monitored spectrophotometrically by means of a home-made rapid system with computer data acquisition.
The decrease in absorbance of indigo carmine at 612 nm, pH 6 and at a fixed concentration of hexacyanoferrate(III) and indigo
carmine is proportional to the concentration of Ag(I). The acquired data based on the initial rate and fixed time are processed.
Up to 100.0 μg/ml of silver are determined. The limit of detection and average relative standard deviation are 0.13 μg/ml
and 1.9%, respectively. The effect of foreign ions on the determination of silver is also discussed. The proposed method is
applied to the determination of Ag(I) in expired photographic film.
Received: 17 June 1996 / Revised: 26 July 1996 / Accepted: 2 August 1996 相似文献
19.
Summary Capillary GC of metal chelates of diethyl dithiocarbamate (DDTC) was examined on a methylsilicone DB-1 column, (25 meter,
0.2 mm. i.d) with a film thickness of 0.25 μm. Elution was carried out at the initial column temperature of 180°C and programmed
at 5°C min−1 to 260°C. Detection was by FID or ECD. Symmetrical peaks with base line separation were obtained with the metal chelates
of copper(II), nickel(II), cobalt(III), manganese(II) and chromium(III). The ECD gave better sensitivity than the FID with
a linear calibration range of 5–50 μg mL−1 and detection limits 2.0–6.0 μg mL−1, corresponding to 111–333 pg of metal ion reaching the detector. The method was applied to the determination of metal ions
in water and pharmaceutical preparations with a coefficient of variation (CV) within 4.0%. When compared with a standard flame
AAS method the results revealed no significant difference. 相似文献
20.
A continuous flow atomic absorption spectrometric system was used to develop an efficient on-line preconcentration-elution
procedure for the determination of iodide traces. Chromium (VI) is introduced into the flow system and is reduced to chromium
(III) in acid medium proportionally to the iodide present in the sample. The Cr(III) reduced by iodide is retained on a minicolumn
packed with a poly(aminophosphonic acid) chelating resin, while unreduced Cr(VI) is not retained. Reduced Cr(III) is preconcentrated
by passing the sample containing iodide through the system during 3 min, and is then eluted with 0.5 mol L–1 hydrochloric acid and determined by flame atomic absorption spectrometry (FAAS). The detection limit (3σ) obtained is 2.5
μg L–1. Other ions typically present in waters do not interfere. The proposed method allows the determination of iodide in the range
6–220 μg L–1 with a relative standard deviation of 2.7% at a rate of 17 samples h–1. The method has been applied to the determination of iodide in tap and sea waters.
Received: 16 September 1999 / Revised: 15 November 1999 / Accepted: 19 November 1999 相似文献