Separation activation analysis

Catalytic activity tests have been performed in a quartz microreactor (I.D.=0.8 cm) filled with 0.45 g of fine catalyst powders (dp=0 1 micron). The reactor has been fed with lean fiiel/air mixtures (1.3% of CO, 1.3% of H2 and 1% of CH4 in air resp ively) and has been operated at atmospheric pressure and with GHSV= 54000 Ncc/gcath The inlet and outlet gas compositions were determined by on-line Gas Chromatography. A 4 m column (I D. =5mm) filled with Porapak QS was used to separate CH4, CO2 and H2O with He as carrier gas. Two molecular sieves (5 A) columns (I D.=5 mm) 3m length, with He and Ar as carrier gases, were used for the separation and analysis of CO, N2, O2, CH4, and H2, N2, O2 respectively... 

Filtration of the catalytic mixture using pore membrane filters or filter aids allows the distinction between soluble and insoluble catalysts. Further catalytic activity analysis from the solution and insoluble residue can give information about the state of the real catalyst. In turn, centrifugation can be appropriated to separate metal NPs from the catalytic solutions, due to their high molecular weight and density, and thus to be separated from molecular species. 

Pietra, R., Fortaner, S., and Sabbioni, E. (1993). Use of Chelex 100 resin in preconcentration and radiochemical separation neutron activation analysis applied to environmental toxicology and biomedical research. /. Trace Microprobe Tech. 11, 235-250. 

Yusov et al. [67] separated arsenic (III) and arsenic (V) in seawater using a chloroform solution of ammonium pyrrolidine diethyldthiocarbamate. The separated fractions were then analysed by neutron activation analysis. 

Differentiation of inorganic and organic mercury can be achieved in a number of different ways, many of which depend upon the reduction and vapourisation of the inorganic mercury, followed by reduction [84] or oxidation [85,86] of the organic mercury compounds, and a final measurement by atomic absorption or mass spectrometry. Similar methods of separation of the inorganic and organic components are used in the pretreatment of samples where the final analysis for mercury is to be made by neutron activation analysis [87,88]. 

Trace amounts of Tc are also determined in filter paper and vegetable samples by neutron activation analysis The procedure consists of the following major steps separation of technetium from the sample, thermal neutron irradiation of the Tc fraction to produce °°Tc, post-irradiation separation and purification of °°Tc from other activated nuclides, and counting of the 16 s Tc in a low-background P counter. The estimated detection limits for Tc in this procedure are 5 x 10 g in filter paper and 9 x 10 g in vegetable samples. 

A method has been developed for the determination of technetium-99 in mixed fission products by neutron activation analysis Tc is separated from most fission products by a cyclohexanone extraction from carbonate solution, the stripping into water by addition of CCI4 to the cylohexanone phase, and the adsorption on an anion exchange column. Induced Tc radioactivity is determined using X-ray spectrometry to measure the 540 and 591 keV lines. The sensitivity of the analysis under these conditions is approximately 5 ng. The method has been successfully applied to reactor fuel solutions. 

Metolachlor is applied as a mixture of eight different stereoisomers, only four of which have herbicidal activity (10). This implies that the other four isomers are applied as contaminants, with no additional benefit to crop production. Whether the chirality of metolachlor influences its degradation rate is unknown. This lack of information is mainly due to the difficulty of separation and analysis of its isomers. Because the stereochemistry of compounds plays an important role in their biological activity and degradation pathways, it is valuable to investigate the influence of stereochemistry on the rate of metolachlor degradation in soil. 

In the first step, we were able to separate this penta derivative by preparative H.P.L.C. and we subsequently treated it with an excess of propyleneimine in order to reach the required hexasubstituted compound. Under such conditions, we succeeded in preparing a N3P3(MeAz)g real sample (free of chlorine, as demonstrated by neutron activation analysis) identified by mass spectrometry (Fig. 32) and by P nmr (Fig. 33) (6 = — 36 ppm with 85 % HjPO as standard, to be compared with 8(N3P3Azg) = --37 ppm). The refractive index of this sample, n = 1.4825, appeared to be significantly far from Ratz s value. 

Protactinium is separated by solvent extraction and anion exchange processes by using sulfate solutions. After chemical separation, the protactinium salts are ignited to a pentoxide, Pa205, which may be converted into an arsenazo(III) complex. The absorbance of the solution is measured at 630 nm with a spectrophotometer. Protactinium-231 is an alpha emitter and also forms photons at 300 KeV, which can be measured by various radioactive counters and spectrophotometric techniques. Protactinium also can be measured by neutron activation analysis. 

With analytical methods such as x-ray fluorescence (XRF), proton-induced x-ray emission (PIXE), and instrumental neutron activation analysis (INAA), many metals can be simultaneously analyzed without destroying the sample matrix. Of these, XRF and PEXE have good sensitivity and are frequently used to analyze nickel in environmental samples containing low levels of nickel such as rain, snow, and air (Hansson et al. 1988 Landsberger et al. 1983 Schroeder et al. 1987 Wiersema et al. 1984). The Texas Air Control Board, which uses XRF in its network of air monitors, reported a mean minimum detectable value of 6 ng nickel/m (Wiersema et al. 1984). A detection limit of 30 ng/L was obtained using PIXE with a nonselective preconcentration step (Hansson et al. 1988). In these techniques, the sample (e.g., air particulates collected on a filter) is irradiated with a source of x-ray photons or protons. The excited atoms emit their own characteristic energy spectrum, which is detected with an x-ray detector and multichannel analyzer. INAA and neutron activation analysis (NAA) with prior nickel separation and concentration have poor sensitivity and are rarely used (Schroeder et al. 1987 Stoeppler 1984). 

Selenium can also be separated from the bulk of the coal samples by the combustion technique described by H. L. Rook (7), which was originally used in a neutron activation analysis. The equipment was... 

Trace Elements in Coal by Neutron Activation Analysis with Radiochemical Separations... 

Procedures for the determination of 11 elements in coal—Sb, As, Br, Cd, Cs, Ga, Hg, Rb, Se, U, and Zn—by neutron activation analysis with radiochemical separation are summarized. Separation techniques include direct combustion, distillation, precipitation, ion exchange, and solvent extraction. The evaluation of the radiochemical neutron activation analysis for the determination of mercury in coal used by the Bureau of Mines in its mercury round-robin program is discussed. Neutron activation analysis has played an important role in recent programs to evaluate and test analysis methods and to develop standards for trace elements in coal carried out by the National Bureau of Standards and the Environmental Protection Agency. 

The post-bombardment processing of the activated sample may follow either a nondestructive assay of the radioactivity in the sample (gamma-ray scintillation spectrometry is used most often for this) or a chemical processing of the sample prior to the radioactivity assay. Techniques involving either precipitation, electrodeposition. solvent extraction, and ion exchange or some combination of these form the basts of the radio-chemical separation techniques used in activation analysis. 

The detection limits in ICP-MS are certainly equal to those achieved by activation analysis. In addition, ICP-MS apparatus is frequently connected to ordinary chemical separation apparatus, such as liquid chromatography (LC), thus allowing a sensitive determination of both the amount and chemical species present for both metals and nonmetals. 

For the following analyses, indicate whether radiochemical neutron activation analysis would be preferred to instrumental neutron activation analysis. If radiochemistry is indicated, briefly sketch the separation procedures to be used (a) the determination of ppm levels of Mo in flathead minnows, (b) the determination of the trace-element content of agricultural field-burning particulate matter, (c) the use of stable activable tracers to determine flow patterns in an ocean estuary, and (d) the determination of Dy in pine needles. 

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