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1.
The Comprehensive Nuclear-Test-Ban Treaty (CTBT) is supported by a network of certified laboratories that perform high-resolution gamma-spectrometry on global air filter samples for the identification of 85 radionuclides. At the UK CTBT Radionuclide Laboratory (GBL15), a novel cosmic veto gamma-spectrometer has been developed to improve the sensitivity of measurements for treaty compliance. The system consists of plastic scintillation plates operated in time-stamp mode to detect coincident cosmic-ray interactions within an HPGe gamma-spectrometer. This provides a mean background reduction of 75.2 % with MDA improvements of 45.6 %. The CTBT requirement for a 140Ba MDA is achievable after 1.5 days counting compared to 5–7 days using conventional systems. The system does not require dedicated coincidence electronics, and remains easily configurable with dual acquisition of unsuppressed and suppressed spectra. Performance has been significantly improved by complete processing of the cosmic-ray spectrum (0–25 MeV) combined with the Canberra Lynx? multi-channel analyser. The improved sensitivity has been demonstrated for a CTBT air filter sample collected after the Fukushima incident.  相似文献   

2.
The verification regime of the comprehensive test ban treaty (CTBT) is based on a network of three different waveform technologies together with global monitoring of aerosols and noble gas in order to detect, locate and identify a nuclear weapon explosion down to 1 kt TNT equivalent. In case of a low intensity underground or underwater nuclear explosion, it appears that only radioactive gases, especially the noble gas which are difficult to contain, will allow identification of weak yield nuclear tests. Four radioactive xenon isotopes, 131mXe, 133mXe, 133Xe and 135Xe, are sufficiently produced in fission reactions and exhibit suitable half-lives and radiation emissions to be detected in atmosphere at low level far away from the release site. Four different monitoring CTBT systems, ARIX, ARSA, SAUNA, and SPALAX? have been developed in order to sample and to measure them with high sensitivity. The latest developed by the French Atomic Energy Commission (CEA) is likely to be drastically improved in detection sensitivity (especially for the metastable isotopes) through a higher sampling rate, when equipped with a new conversion electron (CE)/X-ray coincidence spectrometer. This new spectrometer is based on two combined detectors, both exhibiting very low radioactive background: a well-type NaI(Tl) detector for photon detection surrounding a gas cell equipped with two large passivated implanted planar silicon chips for electron detection. It is characterized by a low electron energy threshold and a much better energy resolution for the CE than those usually measured with the existing CTBT equipments. Furthermore, the compact geometry of the spectrometer provides high efficiency for X-ray and for CE associated to the decay modes of the four relevant radioxenons. The paper focus on the design of this new spectrometer and presents spectroscopic performances of a prototype based on recent results achieved from both radioactive xenon standards and air sample measurements. Major improvements in detection sensitivity have been reached and quantified, especially for metastable radioactive isotopes 131mXe and 133mXe with a gain in minimum detectable activity (about 2 × 10?3 Bq) relative to current CTBT SPALAX? system (air sampling frequency normalized to 8 h) of about 70 and 30 respectively.  相似文献   

3.
The Comprehensive Nuclear-Test-Ban Treaty (CTBT) is supported by a global network of monitoring stations that perform high-resolution gamma-spectrometry on air filter samples for the identification of radionuclides indicative of nuclear weapons tests and reactor incidents. These daily measurements have created an invaluable resource for understanding variations in natural background radioactivity, including the contribution of 7Be. Statistical analysis has been performed on 7Be data collected by CTBT stations hosted by the United Kingdom including at British Indian Ocean Territory (RN66), St Helena (RN67) and Tristan da Cunha (RN68) during 2005–2013. The results have been found to follow a lognormal distribution which implies that the 7Be activity is the multiplicative product of many small independent factors, such as meteorology, elevation, local station conditions, sample acquisition and analysis. This has the potential to identify discrepant measurements not attributable to the intrinsic variability of the distribution and indicative of station malfunction. Variations in 7Be activity have been considered on monthly, weekly and daily timescales and characterised using the geometric mean in accordance with the properties of the lognormal probability density function. Seasonal variations have been identified, with summer maxima and winter minima that are attributable to changes in mixing within the stratosphere and troposphere. Such fluctuations have been examined using the Fast Fourier Transform which may indicate variations associated with the 27 day solar cycle.  相似文献   

4.
In order to reduce interferences from high activities of 24Na, 56Mn, 82Br, and 38Cl as well as to improve detection limits, precision, and accuracy of measuring iodine levels in biological materials, foods and diets in particular, an epithermal instrumental neutron activation analysis (EINAA) method in conjunction with anti-coincidence (EINAA-AC) gamma-ray spectrometry was employed. The Compton scattering background in the region of the 442.9-keV photopeak of 128I was significantly suppressed by anti-coincidence counting. In order to validate the EINAA-AC method as well as to evaluate its broad applicability to diverse types of biological material, 17 NIST and IAEA reference materials containing very low to high levels of iodine as well as interfering elements were analyzed by the EINAA-AC method. The samples were irradiated in the cadmium-lined pneumatic site at a neutron flux of 2 × 1011 cm?2 s?1 of the Dalhousie University SLOWPOKE-2 Reactor (DUSR) facility for 10 or 20 min followed by 1-min decay and 30-min counting. The detection limit for iodine by EINAA-AC was improved by a factor of 2–5 compared to EINAA depending on the sample matrix and other factors, and a limit of 3–5 μg kg?1 was achieved for low-salt foods. We found the RSD to be about ±5 % above 200, increasing to ±10 % at 20, and then to greater than ±30 % at about 5 μg kg?1 iodine levels.  相似文献   

5.
The selenium levels of Argentinean infant formulae and baby food were measured using the 162-keV gamma-ray of 77mSe (t ½ = 17.4 s) by a pseudo-cyclic instrumental neutron activation analysis (PC-INAA) method in conjunction with Compton suppression spectrometry (CSS). For comparison purposes, 5 selected infant formulae were also analyzed for selenium by a radiochemical neutron activation analysis (RNAA) method. The selenium levels for three samples agreed between ±2.8 and 6.5 % while the other two differed by 12 and 17 % which could perhaps be attributed to sample inhomogeneity. The selenium content of cow milk-based infant formulae varied from 42–146 μg kg?1 compared to 52–63 μg kg?1 for soy-based milk formulae. In the case of baby foods, the selenium levels varied from 34 to 74 μg kg?1. The detection limits for selenium by PC-INAA–CSS for all the samples analyzed in this work were between 8.5 and 65 μg kg?1 depending on the major elements present in the samples, while it was 20 μg kg?1 for the RNAA method. The expanded uncertainty (κ = 2) of the PC-INAA–CSS method was 7.0 % at the end of cycle #4 for a sample containing 73.7 μg kg?1 selenium compared to the RNAA value of 24.2 % for a sample of 67.0 μg kg?1 selenium content.  相似文献   

6.
A simple technique for pulse shape discrimination in HPGe-detectors of the so-called BEGe type, based on just one parameter obtained from one signal read out, is presented here. This technique allows discriminating between pulses generated when the deposited energy is located within a small region of about 1 mm3 from the pulses generated when the energy is deposited at different locations several mm or cm apart. Two possible applications using this technique are: (i) experiments that look for neutrinoless double β decay in 76Ge, such as GERDA; (ii) γ spectrometry measurements where the Compton continuum can be reduced and the efficiency for cascading γ-rays can remain high. With this active background reduction technique a Compton suppression factor of about 3 was obtained. The detector response may be influenced by the detector size. The detector used for this study had a diameter of 6 cm, a thickness of 2.6 cm and a relative efficiency of 19%. The results obtained with this detector were consistent with the results obtained by Budjá? et al. [J Instrum 4:10, 2009] with a 50% relative efficiency BEGe detector.  相似文献   

7.
Nuclear material accountancy is of continuous concern for the regulatory, safeguards, and verification communities. In particular, spent nuclear fuel reprocessing facilities pose one of the most difficult accountancy challenges: monitoring highly radioactive, fluid sample streams in near real-time. The Multi-Isotope Process monitor will allow for near-real-time indication of process alterations using passive gamma-ray detection coupled with multivariate analysis techniques to guard against potential material diversion or to enhance domestic process monitoring. The Compton continuum from the dominant 661.7 keV 137Cs fission product peak obscures lower energy lines which could be used for spectral and multivariate analysis. Compton suppression may be able to mitigate the challenges posed by the high continuum caused by scattering. A Monte Carlo simulation using the Geant4 toolkit is being developed to predict the expected suppressed spectrum from spent fuel samples to estimate the reduction in the Compton continuum. Despite the lack of timing information between decay events in the particle management of Geant4, encouraging results were recorded utilizing only the information within individual decays without accounting for accidental coincidences. The model has been validated with single and cascade decay emitters in two steps: as an unsuppressed system and with suppression activated. Results of the Geant4 model validation will be presented.  相似文献   

8.
Beibei Zhou  Jian Pan 《Chromatographia》2009,70(5-6):739-745
Cichoric acid is a water-soluble phenolic acid in Echinacea purpurea and has a high medicinal value. A rapid and novel argentation complex liquid chromatography method has been developed and validated for determination of cichoric acid in E. purpurea extract. The determination of cichoric acid was carried out on a Restek Pinnacle 11 C18 column (250 mm × 4.6 mm, 5 μm), using acetonitrile-deionized water (38:62, v/v, with 6 mmol L?1 AgNO3 and 0.8% acetic acid) as the mobile phase at a flow rate of 1.0 mL min?1 within 10 min. The wavelength was set at 326 nm. It improved the effect of determination by adding AgNO3 in the mobile phase while cichoric acid coordinated with Ag+. The mechanism of coordination between cichoric acid and Ag+ has been studied by Fourier transform infrared spectroscopy, electrospray ionization mass spectrometry. The mechanism which improved the effect of determination of cichoric acid is analyzed and applied in the rapid determination of salvianolic acid B (Sal B) in Danshen extract solution which has been stored for half a year. The possible structures of the complex and complex ratio are all provided in this article. The experiments have facilitated the study of cichoric acid–Ag+ and Sal B–Ag+ complex and provide a theoretical basis for industrialized extraction of cichoric acid and Sal B in the future.  相似文献   

9.
《Analytical letters》2012,45(10):1746-1757
Bifunctional combination of carbon nanotubes and ionophore is introduced for anodic stripping analysis of lead (Pb2+). Carbon nanotubes are employed to improve the detection sensitivity due to their excellent electrical conductivity and strong adsorption ability. An ionophore is utilized for its excellent selectivity toward Pb2+. The proposed carbon nanotubes/ionophore modified electrode shows improved sensitivity and selectivity for Pb2+. Low detection limit (1 nM), wide linear range (5 nM–8 µM) and excellent selectivity over other metal ions (Cd2+, Cu2+, and Hg2+) was obtained. The practical application has been carried out for determination of Pb2+ in real water samples.  相似文献   

10.
A reliable and sensitive method for determination of MCPA in soil by derivatization through p-toluenesulfonic acid and 1,3-dichloro-2-propanol followed by gas chromatographic detection under ECD mode has been established. After treatment with hydrochloric acid, the soil samples were directly extracted without any clean-up with dichloromethane by vortexing. After derivatization and liquid–liquid extraction, the product was subjected to GC analysis. Under optimized conditions, recovery of MCPA reached 87–91%; intra- and inter-day precision values were recorded in the range 3.4–6.4% and 7.4–8.7%, respectively. Excellent linear relationship was observed within 0.1–10 μg mL?1 (0.005–0.5 mg kg?1) with linear correlation coefficient (R) of 0.9997. The LOD and LOQ were 0.001 and 0.0026 mg kg?1, respectively, and the overall sensitivity for detection was found to be in the same range as with the conventional GC-MS technique.  相似文献   

11.
A liquid chromatographic method for analysis of pazufloxacin mesilate in human plasma and urine has been developed and validated for selectivity, sensitivity, accuracy, precision, and stability in pharmacokinetic analysis. The sensitivity of the method was 0.02 μg mL?1 in plasma and 0.5 μg mL?1 in urine, with overall intra-day and inter-day precision (RSD < 10%) and accuracy (90–120%) acceptable for clinical pharmacokinetic analysis. Recovery from plasma and urine was 80–110% for both pazufloxacin mesilate and enoxacin, the internal standard. Pazufloxacin was stable in both plasma and urine, with no significant degradation under four different conditions. The method was successfully used in a preliminary study of the bioavailability of pazufloxacin mesilate in healthy human volunteers after intravenous administration of 300 and 500 mg.  相似文献   

12.
A very sensitive, selective and simple flow injection time-based method was developed for on-line preconcentration and determination of thorium(IV) at micro g L–1 levels in environmental samples. The system operation was based on thorium(IV) ion retention at pH 4.0 in the minicolumn at a flow rate of 15.2 mL min–1. The trapped complex was then eluted with 3.6 mol L–1 HCl at a flow rate of 4.9 mL min–1. The amount of thorium(IV) in the eluate was measured spectrophotometrically at 651 nm using arsenazo-III solution (0.05 % in 3.6 mol L–1 HCl stabilized with 1 % triton X-100, 4.9 mL min–1) as colorimetric reagent. All chemical, and flow injection variables were optimized for the quantitative preconcentration of metal and a study of interference level of various ions was also carried out. The system offered low backpressure and improved sensitivity and selectivity. At a preconcentration time of 60 s and a sample frequency of 40 h–1, the enhancement factor was 97, the detection limit was 0.25 μg L–1, and the precision expressed as relative standard deviation was 1.08 % (at 50 μg L–1), whereas for 300 s of the preconcentration time and a sample frequency of 10 h–1, the enhancement factor of 357, the detection limit (3σ) of 0.069 μg L–1 and the precision of 1.32 % (at 10 μg L–1) was reported. The accuracy of the developed method was sufficient and evaluated by the analysis of certified reference material IAEA-SL-1 (Lake Sediment) and spiked water samples.  相似文献   

13.
Photoinitiators (PIs) are components of UV-cured inks widely used in printing of food packaging. These substances can migrate into food and may be a hazard to human health. High-performance liquid chromatography with diode-array detection (HPLC–DAD) has been used for analysis of PIs and amine synergists in food packaging. Analysis was performed with a Kromasil C18 column (250 mm?×?3.2 mm i.d., 5 μm particle size) with a binary mobile phase gradient prepared from acetonitrile and Milli-Q water. The flow rate was 0.5 mL min?1. The method enables separation of fourteen PIs and amine synergists in a single run. The method was validated for linearity, repeatability, and limits of detection and quantification. Excellent sensitivity (LODs?≤?1.56 μg dm2) and appropriate repeatability (RSD (n?=?10) <0.9 %) were achieved. Different types of food packaging material including plastic films, cardboard, and cans were analyzed and PIs were detected in 47 % of the samples tested (n?=?17). Positive samples were confirmed by use of LC–MS–MS in positive electrospray ionization (ESI) mode.  相似文献   

14.
A fiber optic aided spectrophotometric technique has been developed for the determination of free acidity in nuclear fuel reprocessing streams. In this method, nitric acid forms yellow colour complex with chrome azurol s. The system obeys Lambert–Beer’s law at 542 nm in the range of acidity 4–14 M. The molar absorption coefficient (ε) and Sandell’s sensitivity (S) of complex are 5.23 × 103 L.mol?1.cm?1 and 1.91 × 10?4 µg/cm2 respectively. Relative standard deviation is less than 1 % and correlation coefficient is 0.999. Results of the present method are in good agreement with those obtained by the standard procedure.  相似文献   

15.
Li  Wei  Zhang  Ming  Wang  Zi  Wang  Ying Ping  Zheng  Yi-nan  Zhang  Jing 《Chromatographia》2011,74(11):777-782

Platycosides, main pharmacological effective compounds, are known to have several biological activities, including anti-obesity, anti-cancer and anti-diabetes. Although enzymatic preparation of platycosides was considered as effective method to obtain them, few analytical methods have been reported on process control. In the present study, we developed an application of reversed-phase high-performance liquid chromatography (RP-HPLC) method for simultaneous determination of six platycosides during the process of enzymatic preparation of deapio-platycodin D (dPD) and platycodin D (PD). The method employed a Hypersil ODS2 analytical column (250 × 4.6 mm I.D., 5 μm) coupled with UV detector at 210 nm with flow rate of 1.0 mg mL−1. A step gradient of acetonitrile–water (v/v) was applied, leading to a sample analysis of 60 min. The method was validated in terms of linearity, sensitivity, precision and accuracy. The correlation coefficients (R 2) for calibration curves of platycosides were in the range of 0.9995–1.0 when the linearity range was from 0.85 to 10.2 mg mL−1. The proposed RP-HPLC method was successfully applied to the analysis of enzymatic preparation study and the recoveries of platycosides were in the range of 96.22–102.56% with RSD <3.3%. The method could be of use for rapid and routine evaluation of the quantity of platycosides during the enzymatic preparation process.

  相似文献   

16.
Tiantai No. 1, as a hospital Chinese materia medica preparation, has been used in the treatment of mild cognitive impairment and Alzheimer disease for nearly 20 years. It is composed of six herbal medicines: Panax Ginseng, Coptidis Rhizoma, Evodiae Fructus, Cistanches Herba, Curcuma Longa Rhizoma and Borneol. So far, lots of studies have been carried out on the pharmacodynamics but few on quality evaluation and pharmacokinetic study of Tiantai No. 1. A novel method of ultrahigh performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) developed to determine the concentrations of 21 bioactive components, including Ginsenoside Rg1, Rb1, Rd, Berberine, Epiberberine, Jatrorrhizine, Palmatine, Columbamine, Coptisine, Evodiamine, Dehydroevodiamine, Rutaecarpine, Limonin, Hyperin, Curcumin, Demethoxycurcumin, Bisdemethoxycurcumin, Geniposidic acid, Echinacoside, Isoacteoside and Verbascoside in Tiantai No. 1 and rat plasma is essential for further research. The separation by UHPLC was performed on an Agilent Zorbax Eclipse Plus C18 column (4.6 mm × 150 mm, 3.5 μm) at a flow rate of 0.4 mL min?1 using acetonitrile and 0.1%(v/v) formic acid aqueous solution as mobile phase. Mass spectrometric detection was performed on multiple reaction monitoring (MRM) in either positive or negative ionization mode. The established method was validated and showed good linearity (r2 > 0.9994), sensitivity (LLOQ among 1.000–2.200 ng mL?1), precision (RSD value among 0.81–12.51%), stability (RSD value less than 4.59%) and repeatability (RSD value less than 4.07%). The mean recoveries ranged from 93.12 to 100.25% with SD value less than 4.97%. Moreover, this proposed method was successfully utilized for simultaneous determination of 21 bioactive components in Tiantai No. 1 and rat plasma samples. Results showed that this proposed method was beneficial for quality standard improvement and further pharmacokinetic research of Tiantai No. 1.  相似文献   

17.
Uranium samples of various enrichments have been passively counted on the University of Texas detector gamma–gamma coincidence system. By observing gamma rays emitted from 235U and its daughters compared to gamma rays emitted by 238U daughters and comparing the data to standards of known enrichments, a technique has been developed to take a uranium sample of unknown enrichment and passively count it to determine its uranium isotopic concentration. Because the gamma rays from 235U are generally in the low-energy regime, there is a strong susceptibility to background interferences, especially from the Compton background produced from higher energy gamma rays. Other interferences, such as those from the decay series of uranium also exist for 235U gamma rays. In this light, we have collected data using list-mode to produce two-dimensional gamma–gamma coincidence spectra, which allows us to gate the low-energy gamma rays from 235U with gamma rays that are in coincidence. In doing this, much of the low energy interferences are reduced, and one can analyze the 235U gamma rays with high precision. Because of the high density of uranium, self-shielding has significant effects especially in the low-energy regime. To correct for this attenuation the detector system has been modeled by MCNP and self-shielding factors have been calculated across the energy spectrum. A big advantage to this method is the capability of performing this analysis with small (<1 g) samples in a non-destructive and relatively inexpensive manner. If necessary, this analysis can be performed within 24 h if an urgent nuclear forensics scenario arises.  相似文献   

18.
《Analytical letters》2012,45(5):856-867
A novel flow injection system incorporating a micro-column packed with carbon nanotubes (CNTs) as an adsorbent has been applied to the on-line preconcentration of trace silver with detection by flame atomic absorption spectrometry. Silver is first chelated by dithizone (H2Dz), then retained on the CNTs surface and afterward quantitatively eluted by methanol. Influencing parameters, including the concentration of reaction reagent, enrichment variables, and elution variables were investigated. The adsorption mechanisms of Ag-H2Dz chelate retained onto the CNTs surface have also been studied. By loading 6.9 mL sample solution, a linear calibration graph is obtained within the range of 3–120 µg L?1 with R of 0.9996, and a detection limit (3σ) of 0.8 µg L?1 is achieved, along with a precision of 1.6% R.S.D. at the 30 µg L?1 level (n = 7). The dynamic sorption capacity of CNTs for silver is 122 mg g?1. The procedure is demonstrated by measurement of spike recovery in a series of water samples, giving rise to spike recoveries in the range of 96.8–99.7%.  相似文献   

19.
In this study, we demonstrated a highly sensitive electrochemical sensor for the determination of glucose in alkaline aqueous solution by using nickel oxide single-walled carbon nanotube hybrid nanobelts (NiO–SWCNTs) modified glassy carbon electrode (GCE). The hybrid nanobelts were prepared by the deposition of SWCNTs onto the Ni(SO4)0.3(OH)1.4 nanobelt surface, followed by heat treatment at different temperatures ranging from 400 °C to 600 °C. The NiO–SWCNTs hybrid nanobelts modified electrode prepared at 500 °C displays enhanced electrocatalytic activity towards glucose oxidation, revealing a synergistic effect between the NiO and the deposited SWCNTs. The as-fabricated nonenzymatic glucose sensor exhibits excellent glucose sensitivity (2,980 μA cm?2 mM?1), lower detection limit (0.056 μM, signal/noise [S/N] ratio?=?3), and wider linear range (0.5–1,300 μM). Moreover, the sensor has been successfully used for the assay of glucose in serum samples with good recovery, ranging from 96.4 % to 102.4 %.  相似文献   

20.
Studies on lipase production and characterization were carried out with a bacterial strain Staphylococcus arlettae JPBW-1 isolated from rock salt mine, Darang, HP, India. Higher lipase activity has been obtained using 10 % inoculum with 5 % of soybean oil as carbon source utilizing a pH 8.0 in 3 h at 35 °C and 100 rpm through submerged fermentation. Partially purified S. arlettae lipase has been found to be active over a broad range of temperature (30–90 °C), pH (7.0–12.0) and NaCl concentration (0–20 %). It has shown extreme stability with solvents such as benzene, xylene, n-hexane, methanol, ethanol and toluene up to 30 % (v/v). The lipase activity has been found to be inhibited by metal ions of K+, Co2+ and Fe 2+ and stimulated by Mn2+, Ca2+ and Hg2+. Lipase activity has been diminished with denaturants, but enhanced effect has been observed with surfactants, such as Tween 80, Tween 40 and chelator EDTA. The K m and V max values were found to be 7.05 mM and 2.67 mmol/min, respectively. Thus, the lipase from S. arlettae may have considerable potential for industrial application from the perspectives of its tolerance towards industrial extreme conditions of pH, temperature, salt and solvent.  相似文献   

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