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1.
During this work selective separation of uranium from rock phosphate and columbite mineral was done before its quantitative estimation by using Inductively Coupled Plasma Optical Emission Spectrometery (ICP-OES). Uranium from the rock phosphate and columubite was extracted by sodium peroxide fusion followed by leaching in 2 M HNO3. To avoid spectral interference in the estimation of uranium by ICP-OES, the selective separation of uranium from the leachate was carried out by using two different extractants, 30% Tributyl Phophates (TBP) in CCl4 and a equi-volume mixture of Di(2-ethylhexyl) phosphoric acid (D2EHPA) & TBP in petrofin. Uranium was stripped from the organic phase by using 1 M ammonium carbonate solution. Determination of uranium by ICP-OES was done after dissolving the residue left after evaporation of ammonium carbonate solution in 4% HNO3. The concentration of the uranium observed in the rock phosphates samples was 40–200 μg g−1 whereas in columbite samples the concentration range was 100–600 μg g−1. Uranium concentration evaluated by ICP-OES was complimented by gamma & alpha spectrometry. Concentration of uranium evaluated by gamma spectrometry in case of rock phosphate and coulmbite was in close agreement with the uranium content obtained by ICP-OES. Uranium determination by alpha spectrometry showed only minor deviation (1–2%) from the results obtained by ICP-OES in case of rock phosphates whereas in case of coulmbites results are off by 20–30%.  相似文献   

2.
A multisyringe flow injection analysis method for the determination of uranium in water samples was developed. The methodology was based on the complexation reaction of uranium with arsenazo (III) at pH 2.0. Uranium concentrations were spectrophotometrically detected at 649 nm using a light emitting diode. Under the optimized conditions, a linear dynamic range from 0.1 to 4.0 μg mL−1, a 3σ detection limit of 0.04 μg mL−1, and a 10σ quantification limit of 0.10 μg mL−1 were obtained. The reproducibility (%) at 0.5, 2.5, and 4.0 μg mL−1 was 2.5, 0.9, and 0.6%, respectively (n = 10). The interference effect of some ions was tested. The proposed method was successfully applied to the determination of uranium in water samples.  相似文献   

3.
During this work the determination of uranium in the range of μg·L−1 to tens of μg·L−1 was done by alpha-spectrometry after electroplating the aliquots of water sample using (NH4)2SO4 as an electrolyte. In general, the determination of uranium by alpha-spectrometry needs its separation from other transuranics specially thorium. The process described here does not involve any sample digestion and radiochemical separation of uranium from other transuranics. In this method an aliquot (1 to 3 mL) of the sample was dried and dissolve in (NH4)2SO4 and thereafter the sample was electroplated on a stainless steel (SS) planchet by using an electrochemical cell of special design. The proposed techniques have a distinct advantage over the determination of uranium by adsorptive stripping voltammetry (AdSV) in which uranium-chloranilic (2,5-dichloro-3,6-dihydroxy-1,4-benzoquinone) acid complex was used for concentrating the uranium from the solution. Since in the case of AdSv, the determination of uranium was not possible for samples having dissolved organic carbon (DOC) more than 15 mg·L−1 and Cl concentration is in the range of 40,000 μ·g−1. In the case of spike experiments with 232U the recovery was observed in the range of 90–95% in aqueous medium having higher concentration of Cl and DOC as indicated above.  相似文献   

4.
For safety assessments of geological repositories of nuclear waste, understanding of uranium (U) fate in estuarine areas is important because U chemical behavior in the areas is expected to be complex. Environmental transfer parameters such as sediment–water distribution coefficients (K d) and concentration ratios (CRs) for marine organisms are useful in mathematical models for the assessment. However, due to its low concentration in estuarine water, K d and CF data for U are scarce. Thus we studied a rapid method for separation and concentration of U from estuarine water samples using NOBIAS-CHELATE PA1 resin columns followed by inductively coupled plasma mass spectrometry (ICP-MS) for U measurement. Chemical recovery was about 100% at pH of 5.7 ± 0.1 from the water samples and alkali and alkaline earth metals were removed. The method was used to measure U concentrations in estuarine water samples collected at eight Japanese estuarine areas; they ranged from 0.1 to 3.8 μg L−1. We also measured U concentrations in sediment and marine organism samples by ICP-MS after acid digestion. Using these values, we observed K d (range: 39–284 L kg−1) and CRs (0.86–52 L kg−1 for macroalgae, 0.087–15 L kg−1 for crustaceans, and 0.52–93 L kg−1 for molluscs).  相似文献   

5.
A simple, sensitive and efficient spectrophotometric method is proposed for rapid determination of uranium using arsenazo-III in perchloric acid. The reaction between arsenazo-III and U(VI) was instantaneous in 3 mol L−1 HClO4. N-cetyl-N,N,N-trimethylammonium bromide was used for increasing the sensitivity and selectivity of the complex. The absorbance remains stable for over 48 h in the presence of surfactant. The method allows the determination of uranium in the range of 1–20 μg g−1 with a molar absorptivity of 3.9 × 105 dm3 mol−1 cm−1 at 681 nm. Sandell’s sensitivity of the complex was calculated to be 6.4 ng cm−2 at λmax 681 nm. A significant enhancement was achieved in the sensitivity of the proposed method whereas, Relative Standard Deviation was reduced from 4.5 to 1.7% in the presence of surfactant. Among various diverse ions studied, fluoride, cyanide, citrate, sulfate and phosphate interfere beyond the tolerance limit. Among cations only Cr3+ and Co2+ decreased the normal absorbance. The validity of the reported method was tested by determining uranium in the environmental water samples and Standard Reference Material. The results agreed closely with the reported values. The proposed method is new, easy in operation and better in sensitivity than many of the existing methods.  相似文献   

6.
Currently, there is an increasing demand for the production of biodiesel and, consequently, there will be an increasing need to treat wastewaters resulting from the production process of this biofuel. The main objective of this work was, therefore, to investigate the effect of applied volumetric organic load (AVOL) on the efficiency, stability, and methane production of an anaerobic sequencing batch biofilm reactor applied to the treatment of effluent from biodiesel production. As inert support, polyurethane foam cubes were used in the reactor and mixing was accomplished by recirculating the liquid phase. Increase in AVOL resulted in a drop in organic matter removal efficiency and increase in total volatile acids in the effluent. AVOLs of 1.5, 3.0, 4.5 and 6.0 g COD L−1 day−1 resulted in removal efficiencies of 92%, 81%, 67%, and 50%, for effluent filtered samples, and 91%, 80%, 63%, and 47%, for non-filtered samples, respectively, whereas total volatile acids concentrations in the effluent amounted to 42, 145, 386 and 729 mg HAc L−1, respectively. Moreover, on increasing AVOL from 1.5 to 4.5 g COD L−1 day−1 methane production increased from 29.5 to 55.5 N mL CH4 g COD−1. However, this production dropped to 36.0 N mL CH4 g COD−1 when AVOL was increased to 6.0 g COD L−1 day−1, likely due to the higher concentration of volatile acids in the reactor. Despite the higher concentration of volatile acids at the highest AVOL, alkalinity supplementation to the influent, in the form of sodium bicarbonate, at a ratio of 0.5–1.3 g NaHCO3 g CODfed−1, was sufficient to maintain the pH near neutral and guarantee process stability during reactor operation.  相似文献   

7.
An ion exchange method has been developed for the separation of uranium from trace level metallic impurities prior to their determination by inductively coupled plasma optical emission spectrometry (ICP-OES) in uranium materials. Selective separation of uranium from trace level metallic impurities consisting Cr, Co, Cu, Fe, Mn, Cd, Gd, Dy, Ni, and Ca was achieved on anion exchange resin Dowex 1 × 8 in sulphate medium. The resin (100–200 mesh, in chloride form) was packed in a small Teflon column (7.8 cm × 0.8 cm I.D.) and brought into sulphate form by passing 0.2 N ammonium sulphate solution. Optimum experimental conditions including pH and concentration of sulphate in the liquid phase were investigated for the effective uptake of uranium by the column. Uranium was selectively retained on the column as anionic complex with sulphate, while impurities were passed through the column. Post column solution was collected and analyzed by ICP-OES for the determination of metallic impurities. Up to 2,500 μg/mL of uranium was retained with >99% efficiency after passing 25 mL sample through the column at pH 3. Percentage recoveries obtained for most of the metallic impurities were >95% with relative standard deviations <5%. The method established was applied for the determination of gadolinium in urania–gadolinia (UO2–Gd2O3) ceramic nuclear fuel and excellent results were achieved. Solvent extraction method using tributylphosphate (TBP) as extractant was also applied for the separation of uranium in urania–gadolinia nuclear fuel samples prior to the determination of gadolinium by ICP-OES. The results obtained with the present method were found very comparable with those of the solvent extraction method.  相似文献   

8.
New data are presented on 238U concentrations in surface and ground waters sampled at selected uranium mining sites in Kazakhstan and Kyrgyzstan and in water supplies of settlements located in the vicinity of these sites. Radiochemical neutron activation analysis (RNAA) was used for 238U determination in all cases. In addition, for data accuracy assessments purposes, a sub-set of these samples was analysed by high-resolution alpha spectrometry, following standard radiochemical separation and purification. Our data show that drinking waters sampled at various settlements located close to the uranium mining sites are characterised by relatively low uranium concentrations (1.9–35.9 μg L−1) compared to surface waters sampled within the same sites. The latter show high concentrations of total uranium, reflecting the influence from the radioactive waste generated as a result of uranium ore production.  相似文献   

9.
A novel method was developed for the determination of captan, folpet, and captafol in apples by dispersive liquid–liquid microextraction (DLLME) coupled with gas chromatography–electron capture detection (GC–ECD). Some experimental parameters that influence the extraction efficiency, such as the type and volume of the disperser solvents and extraction solvents, extraction time, and addition of salt, were studied and optimized to obtain the best extraction results. Under the optimum conditions, high enrichment factors for the compounds were achieved ranging from 824 to 912. The recoveries of fungicides in apples at spiking levels of 20.0 μg kg−1 and 70.0 μg kg−1 were 93.0–109.5% and 95.4–107.7%, respectively. The relative standard deviations (RSDs) for the apple samples at 30.0 μg kg−1 of each fungicide were in the range from 3.8 to 4.9%. The limits of detection were between 3.0 and 8.0 μg kg−1. The linearity of the method ranged from 10 to 100 μg kg−1 for the three fungicides, with correlation coefficients (r 2) varying from 0.9982 to 0.9997. The obtained results show that the DLLME combined with GC–ECD can satisfy the requirements for the determination of fungicides in apple samples. Figure Dispersive liquid–liquid microextraction (DLLME) coupled with gas chromatography–electron capture detection (GC–ECD) allows satisfactory determination of fungicides in apple samples  相似文献   

10.
Olive cake as low-cost abundantly available sorbent has been characterized by N2 at 77 K adsorption, porosity analysis, elemental analysis and IR spectra and has been used for preconcentrating of uranium(VI) and thorium(IV) ions prior to their determination spectrophotometrically. The optimum pH values for quantitative sorption of U(VI) and Th(IV) are 4–7 and 3–7, respectively. The enrichment factor for the preconcentration of U(VI) and Th(IV) were found to be 125 and 75 in the given order. The sorption capacity of olive cake is in the range of 2,260–15,000 μg g−1 for Th(IV) and in the range of 1,090–17,000 μg g−1 for U(VI) at pH 3–7. The sorbent exhibits good reusability and the uptake and stripping of the studied ions were fairly rapid. The elution of U(VI) and Th(IV) was performed with 0.3–1 M HCl/1–2 M HNO3 and 0.3–0.8 M HCl/1 M HNO3, respectively. The precision of the method was 1.8 RSD% for U(VI) and 2.5 RSD% for Th(IV) in a concentration of 1.00 μg mL−1 for 10 replicate analysis. The influence of some electrolytes and cations as interferents was discussed. Separation of U(VI) and Th(IV) from other metal ions in synthetic solution was achieved.  相似文献   

11.
A fully automated method has been developed for analysis of eighteen antibacterial compounds, including penicillins, cephalosporins and sulfonamides, in animal feed with limits of quantification in the range 0.25–5.79 μg kg−1. The method is based on pressurized liquid extraction of 3 g homogenized feed with water and online clean-up of 500 μL of the extract with C18HD cartridges. The purified sample was directly analysed by liquid chromatography–electrospray tandem mass spectrometry (SPE–LC–ESI-MS–MS). Chromatographic separation was achieved within 10 min by use of a C12 Phenomenex Hydro-RP reversed-phase analytical column and a mobile phase gradient (water + 0.1% formic acid–methanol + 0.1% formic acid). The method was validated, revealing capability for detection of concentrations as low as 0.09 μg kg−1, decision limits (CCα) and detection capabilities (CCβ) in the range 10–174 μg kg−1 and 22–182 μg kg−1, respectively, and inter-day precision ranging from 0.7 to 8.3%. Recovery, with internal standard correction, was in the range 93–134% for all analytes. The method was then applied to analysis of fifteen feed samples, nine of which contained at least one antimicrobial at concentrations between 0.006 and 1.526 mg kg−1. The performance data and results from the method were compared with those from a previous method developed by our group, using offline SPE, by analyzing the same set of samples by both methods. The online SPE approach resulted in slightly improved sensitivity, with LODs of 0.09–2.12 μg kg−1 compared with 0.12–3.94 μg kg−1 by the offline approach. In general, better recovery was achieved by use of online purification (for 72% of the analytes) and the correlation between the two methods was good. The main advantages of the new online method are rapid and automated sample pre-treatment, and reduction of sample manipulation, enabling high-throughput analysis and highly accurate results. Because of all these characteristics, the proposed method is applicable and could be deemed necessary within the field of food control and safety.  相似文献   

12.
A rapid, sensitive and environmentally friendly method for the analysis of 14 anilines in water samples by dispersive liquid–liquid microextraction based on solidification of floating organic drop (DLLME-SFO) prior to gas chromatography–mass spectrometry (GC-MS) was developed and optimized. In the proposed method, cyclohexane was used as the extraction solvent as its toxicity was much lower than that of the solvent usually used in dispersive liquid–liquid microextraction (DLLME). In the optimized conditions, the method exhibited good analytical performance. Based on a signal-to-noise ratio of 3, limits of detection for anilines were in the range of 0.07 to 0.29 μg L−1, and the linear range was 0.5–200 μg L−1 with regression coefficients (r 2) higher than 0.9977. It was efficient for qualitative and quantitative analysis of anilines in water samples. The relative standard deviations varied from 2.9 to 8.6 % depending on different compounds indicating good precision. Tap water and river water were selected for evaluating the application to real water samples. The relative recoveries of anilines for the two real samples spiked with 10 μg L−1 anilines were in the scope of 78.2–114.6 % and 77.3–115.6 %, respectively.  相似文献   

13.
The World Health Organization states that envenomation is responsible for a high number of deaths per year, especially in equatorial areas. The only effective specific treatment is the use of hyperimmune serum (antivenom). In Brazil, Crioula breed horses are used for antivenom production, with great importance in the maintenance of public health programs. A strict biochemical and metabolic control is required to attain specificity in antiserum. Inorganic elements represent only a small fraction of whole blood. Nonetheless, they play important roles in mammalian metabolism, being responsible for controlling enzymatic reactions, respiratory and cardiac functions and ageing. In this work, whole blood samples from Crioula breed horses were analyzed by EDXRF technique. The reference interval values were determined for the elements Na (1955–2013 μg g−1), Mg (51–75 μg g−1), P (523–555 μg g−1), S (1628–1730 μg g−1), Cl (2388–2574 μg g−1), K (1649–1852 μg g−1), Ca (202–213 μg g−1), Cu (4.1–4.5 μg g−1) and Zn (2.4–2.8 μg g−1) and a comparative study with NAA results was outlined. The samples were obtained from Instituto Butantan. Both techniques showed to be appropriate for whole blood sample analyses and offer a new perspective in Veterinary Medicine.  相似文献   

14.
A new chemiluminescence (CL) method combined with flow injection technique is described for the determination of Cr(III) and total Cr. It is found that a strong CL signal is generated from the reaction of Cr(III), lucigenin and KIO4 in alkaline condition. The determination of total Cr is performed by pre-reduction of Cr(VI) to Cr(III) by using H2SO3. The CL intensity is linearly related to the concentration of Cr in the range 4.0 × 10−10–1.0 × 10−6 g mL−1. The detection limit (3s b) is 1 × 10−10 g mL−1 Cr and the relative standard deviation is 1.9% (5.0 × 10−8 g mL−1 of Cr(III) solution, n = 11). The method was applied to the determination of Cr(III) and total Cr in water samples and compared satisfactorily with the official method.  相似文献   

15.
A sensitive and effective method for simultaneous determination of triazolopyrimidine sulfonamide herbicide residues in soil, water, and wheat was developed using ultra-performance liquid chromatography coupled with tandem mass spectrometry. The four herbicides (pyroxsulam, flumetsulam, metosulam, and diclosulam) were cleaned up with an off-line C18 SPE cartridge and detected by tandem mass spectrometry using an electrospray ionization source in positive mode (ESI+). The determination of the target compounds was achieved in <2.0 min. The limits of detection were below 1 μg kg−1, while the limits of quantification did not exceed 3 μg kg−1 in different matrices. Quantitation was determined from calibration curves of standards containing 0.05–100 μg L−1 with r 2 > 0.997. Recovery studies were conducted at three spiked levels (0.2, 1, and 5 μg kg−1 for water; 5, 10, and 100 μg kg−1 for soil and wheat). The overall average recoveries for this method in water, soil, wheat plants, and seeds at three levels ranged from 75.4% to 106.0%, with relative standard deviations in the range of 2.1–12.5% (n = 5) for all analytes.  相似文献   

16.
On the basis of flow injection analysis technology, a simple, accurate, and sensitive method has been developed for the determination of volatile phenols in environmental water samples by using CdTe/ZnSe nanocrystals as a fluorescent probe. The influences of coexisting metal ions and volatile phenol substitutes were also investigated. The method developed for analysis of volatile phenols displayed very good linearity in the range from 1.0 × 10−8 to 4.0 × 10−7 g L−1, with a correlation coefficient greater than 0.995 and a detection limit down to 2.7 × 10−9 g L−1 (signal-to-noise ratio 3). The proposed method was successfully applied to determine the content of volatile phenols in environmental water samples, and the quantitative recoveries were 93.4–106.1%. A possible reaction mechanism for the quenching of fluorescence is discussed using UV–vis absorption spectra, fluorescence spectra, and time-resolved luminescence spectra of volatile phenols obtained by titrating a CdTe/ZnSe nanocrystal aqueous solution and zeta potential data.  相似文献   

17.
This paper reports silica gel loaded with p-tert-butylcalix[8]arene as a new solid phase extractor for determination of trace level of uranium. Effective extraction conditions were optimized in column methods prior to determination by spectrophotometry using arsenazo(III). The results showed that U(VI) ions can be sorbed at pH 6 in a mini-column and quantitative recovery of U(VI) (>95–98%) was achieved by stripping 0.4 mol L−1 HCl. The sorption capacity of the functionalized sorbent is 0.072 mmol uranium(VI) g−1 modified silica gel. The relative standard deviation and detection limit were 1.2% (n = 10) for 1 μg uranium(VI) mL−1 solution and 0.038 μg L−1, respectively. The method was employed to the preconcentration of U(VI) ions from spiked ground water samples.  相似文献   

18.
A sensitive and non chromatographic analytical procedure for the separation of inorganic selenium species in natural water has been performed. A combination of APDC coprecipitation and determination by an absolute thin layer Energy dispersive X-ray fluorescence spectrometry method was used. The influence of various analytical parameters such as element concentration, oxidation states and pH on the recoveries of Se (IV) was examined. The presence of organic matter and bicarbonate anions, typical components in Cuban groundwater samples, was also tested. Negligible matrix effects were observed. At pH 4 a 100% recovery was found for Se (IV). The coprecipitation recovery of the oxidized selenium species (Se (VI)) was null for the selected concentration range (5–100 μg L−1). When the Se (VI) was reduced by heating the solution with 4 mol L−1 HCl, quantitative recovery was also obtained. The determination of total selenium was conducted by the application of the oxidation–reduction process and the analytical procedure for Se (IV). Se (VI) content was calculated as the difference between total selenium and Se (IV). The detection limit was 0.13 μg L−1. The relative standard deviation was lower than 3.5% for 5 μg L−1 of Se (IV). The trueness of the method was verified by using standardized hydride generation-atomic absorption spectrometry technique. The results obtained using the EDXRF technique were in good agreement with the ones determined by HG-AAS. The proposed method was applied to the determination of Se (IV) in surface water and groundwater samples.  相似文献   

19.
Fluoridized iron phosphate (F-FePO) is prepared via a hydrothermal protocol and characterized by means of 57Fe M?ssbauer spectra, Fourier transform infrared, and surface charge analysis. For the first time, F-FePO is used as an adsorbent for the adsorption of proteins, which exhibits favorable selectivity toward cytochrome c (cyt-c) in the presence of acidic and neutral proteins under controlled experimental conditions. At pH 10.5, an adsorption efficiency of 100% is achieved for 60 mg L−1 cyt-c in 1.0 mL of sample solution using 6.0 mg F-FePO. The adsorption behavior is consistent with the Langmuir adsorption model, corresponding to a theoretical adsorption capacity of 37.59 μg mg−1. The retained cyt-c on F-FePO could be readily collected by 0.1 mol L−1 Na2CO3–NaHCO3 buffer (pH 10.5), deriving a recovery of 100%. Circular dichroism spectra indicate no conformational change for cyt-c after the adsorption and desorption processes, demonstrating the favorable biocompatibility of the fluoridized iron phosphate. F-FePO is employed for the selective isolation of cyt-c from a spiked human whole blood, achieving satisfactory results by assay with SDS-polyacrylamide gel electrophoresis and native polyacrylamide gel electrophoresis.  相似文献   

20.
A fast and simple multisyringe flow injection analysis (MSFIA) method for routine determination of thorium in water samples was developed. The methodology was based on the complexation reaction of thorium with arsenazo (III) at pH 2.0. Thorium concentrations were spectrophotometrically detected at 665 nm. Under optimal conditions, Beer’s law was obeyed over the range from 0.2 to 4.5 μg mL−1 thorium, a 3σ detection limit of 0.05 μg mL−1, and a 10σ quantification limit of 0.2 μg mL−1 were obtained. The relative standard deviations (RSD, %) at 0.5, 2.5 and 4.5 μg mL−1 was 2.8, 1.5 and 0.8%, respectively (n = 10). It was found that most of the common metal ions and anions did not interfere with the thorium determination. The proposed method was successfully applied to its analysis in various water samples.  相似文献   

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