A rapid method for spectrophotometric determination of phosphine residues in wheat has been developed. Phosphine-fumigated wheat kernels were added with 10% sulfuric acid in a gas-tight flask, and phosphine was releas...
详细信息
A rapid method for spectrophotometric determination of phosphine residues in wheat has been developed. Phosphine-fumigated wheat kernels were added with 10% sulfuric acid in a gas-tight flask, and phosphine was released into the headspace by microwave irradiation. Phosphine was spectrophotometrically determined after reaction with silver nitrate. A good linearity of the calibration curve was obtained with wheat spiked at levels ranging from 0.035 to 0.230 mu g/g with correlation coefficient (r) of 0.9965 and a detection limit of 0.026 mu g/g. The total time of analysis was 10 min. Headspace analysis was also performed by micro-gas chromatography (GC) with a thermal conductivity detector (micro-GC-TCD). Results obtained with the spectrophotometric and micro-GC-TCD methods showed good correlations with those obtained with the most widely used GC with nitrogen-phosphorus detector with r values of 0.9940 and 0.9946, respectively.
A rapid method for the determination of polonium-210 in urban matrices has been developed that can be used following a radiological event. Samples such as concrete, soil and granite are fused with sodium hydroxide to ...
详细信息
A rapid method for the determination of polonium-210 in urban matrices has been developed that can be used following a radiological event. Samples such as concrete, soil and granite are fused with sodium hydroxide to minimize polonium volatility during sample digestion and to achieve complete sample dissolution. Complete dissolution of samples is important to ensure method ruggedness. Polonium is concentrated and separated from the sample matrix using an iron hydroxide precipitation and extraction chromatography and subsequently measured by alpha spectrometry following microprecipitation with bismuth phosphate. The chromatographic separation removes alpha emitting interferences and matrix constituents which can adversely impact the measurement via alpha spectrometry.
The rapid measurement of plutonium isotopes in steel samples is very important in the event of a radiological emergency as well as for the characterization of nuclear decommissioning samples. A new method for the dete...
详细信息
The rapid measurement of plutonium isotopes in steel samples is very important in the event of a radiological emergency as well as for the characterization of nuclear decommissioning samples. A new method for the determination of plutonium isotopes in steel samples has been developed at the Savannah River Environmental Laboratory. The new method employs a rugged acid digestion method that includes hydrofluoric acid, followed by a single preconcentration step to rapidly preconcentrate the plutonium isotopes and remove most of the dissolved steel sample matrix. A fusion option improves ruggedness when soil or concrete is present and can be implemented after the steel dissolution. The Pu isotopes are separated using an extraction chromatographic resin and measured by alpha spectrometry. The method can also be adapted for measurement by inductively-coupled plasma mass spectrometry. This approach has a sample preparation time of 6-8 h for steel samples.
This study describes a new and rapid procedure for radiostrontium determination in milk samples based on the use of plastic scintillation resins (PS resins). The proposed method reduces the time of analysis by at leas...
详细信息
This study describes a new and rapid procedure for radiostrontium determination in milk samples based on the use of plastic scintillation resins (PS resins). The proposed method reduces the time of analysis by at least 2 h by combining separation and measurement preparation into a single step and optimizing the pre-treatment steps. The method is robust and reproducible, with good total recoveries (65% on average) and a relative bias for total radiostrontium activity (Sr-89 + Sr-90) below 7%. The minimum detectable activity for 100 mL of milk sample measured for 60 min is about 0.34 Bq L-1. The proposed method can quantify radiostrontium content in 5 h, which makes it suitable for use in emergency situations.
A new method for the determination of actinides and radiostrontium in limestone and marble samples has been developed that utilizes a rapid sodium hydroxide fusion to digest the sample. Following rapid pre-concentrati...
详细信息
A new method for the determination of actinides and radiostrontium in limestone and marble samples has been developed that utilizes a rapid sodium hydroxide fusion to digest the sample. Following rapid pre-concentration steps to remove sample matrix interferences, the actinides and Sr-89/90 are separated using extraction chromatographic resins and measured radiometrically. The advantages of sodium hydroxide fusion versus other fusion techniques will be discussed. This approach has a sample preparation time for limestone and marble samples of < 4 h.
The rapid measurement of Sr-89/90 in steel samples is important in the event of a radiological emergency as well as for the characterization of routine nuclear decommissioning samples. A new method for the determinati...
详细信息
The rapid measurement of Sr-89/90 in steel samples is important in the event of a radiological emergency as well as for the characterization of routine nuclear decommissioning samples. A new method for the determination of radiostrontium in 1-2 g steel samples has been developed at the Savannah River Environmental Laboratory. The new method employs a rugged acid digestion that includes hydrofluoric acid, followed by a single preconcentration step to rapidly collect the radiostrontium and remove nearly all of the high iron content. A fusion step can be implemented after the steel dissolution when soil, concrete, or highly refractory particles are present. The Sr-89 + Sr-90 and/or Y-90 are separated using extraction chromatographic resins and measured radiometrically, either by gas flow proportional counting or liquid scintillation counting. Several approaches for the measurement of Sr-89 + Sr-90, Sr-90, and discrimination between Sr-89 and Sr-90 are discussed. This approach has a sample preparation time of 6-8 h for steel samples.
Liquid chromatography in its classical forms has been used for many years in determining chemical group composition; however, as the determinations are time-consuming and unwieldy, liquid chromatography has been found...
详细信息
Liquid chromatography in its classical forms has been used for many years in determining chemical group composition; however, as the determinations are time-consuming and unwieldy, liquid chromatography has been found useful only in research work. There is an undoubted need for basic improvements in the equipment used for liquid-adsorption chromatography of petroleum products, as well as improvements in efficiency of the process of chromatographic separation into groups. The main obstacle to automation of the separation of heavy petroleum products is in the elution process and in the method of group identification. With the aim of solving these problems, the authors have developed a rapid method for the determination of group composition of heavy petroleum products. The liquid chromatograph technique described consists of three sections: an analytical section that effects chromatographic separation of the mixture sample into groups; a detector section, including an eluate transporter, a system for removal of the solvent, an oxidation cell, and a katharometer; and a section for registration of the detector signal. The report is presented under headings: elution method; adsorbent (silica gel pretreated with hydrogen peroxide); method of identification (chromatogram analysis). Recommendations for practical uses are included.
Adsorption chromatography, the method currently used to determine asphalt composition, is extremely time-consuming and hence is used only for research purposes. For rapid analysis, the authors have utilized the indivi...
详细信息
Adsorption chromatography, the method currently used to determine asphalt composition, is extremely time-consuming and hence is used only for research purposes. For rapid analysis, the authors have utilized the individual luminescence characteristics of light, medium, and heavy aromatic hydrocarbons, resins, and asphaltenes. The spectral characteristics of the aromatic hydrocarbons present in asphalt were investigated in solutions of benzene, isooctane, and pentane, and also in mixtures of the solvents used for analysis of structural-group composition in the method of the Bashkir Scientific-Research Institute for Petroleum Processing. In reported experiments, the absorption spectra were taken in spectrophotometers, the fluorescence spectra in a spectrofluorimeter. Also, in certain cases, further determinations were run in a unit built up on the basis of two quartz monochromators. The absorption spectra of the asphalt fractions, all taken at the same concentration (1. 5 multiplied by (times) 10** minus **3 g/liter) and the same lightpath length (1 cm), indicate that the above-indicated groups of hydrocarbons differ in terms of the position of the absorption maximum and in the optical density.
The radiation resistance of lubricating oils can be achieved either by selecting suitable oil base stocks or by the use of special additives known as antirads. At present, the selection of antirads and oil base stocks...
详细信息
The radiation resistance of lubricating oils can be achieved either by selecting suitable oil base stocks or by the use of special additives known as antirads. At present, the selection of antirads and oil base stocks to obtain radiation-resistant oils is largely empirical. This paper reports results of an investigation of the radiolysis of the oils I-12A, I-20A, and MGE-10A. The samples were irradiated in specially designed aluminum holders with numbered cells in an MRKh- gamma -25 unit with a **6**0Co source and an irradiation chamber with a volume of 1 liter, at a dose rate of 3 kGy/h and a temperature of 30 degree C. The maximum number of simultaneously irradiated samples in the investigation of gas evolution and viscosity was 100, in the investigation of refractive index 30. Measuring results are tabulated and evaluated by means of mathematical equations.
A new method that rapidly pre-concentrates and measures Ra-226 from hydraulic fracturing wastewater samples was developed in the Savannah River Environmental Laboratory. The method improves the quality of Ra-226 measu...
详细信息
A new method that rapidly pre-concentrates and measures Ra-226 from hydraulic fracturing wastewater samples was developed in the Savannah River Environmental Laboratory. The method improves the quality of Ra-226 measurements using gamma spectrometry by providing up to 100 x pre-concentration of Ra-226 from this difficult sample matrix, which contains very high levels of calcium, barium, strontium, magnesium and sodium. The high chemical yield, typically 80-90 %, facilitates a low detection limit, important for lower level samples, and indicates method ruggedness. Ba-133 tracer is used to determine chemical yield and correct for geometry-related counting issues. The Ra-226 sample preparation takes < 2 h.
暂无评论