SU1187039A1 - Method of determining dispersibility of multicomponents substance (its versions) - Google Patents

Abstract

1. A method for determining the scattering ability of a multicomponent substance, consisting in irradiating samples of an analyte and a substance with a known chemical composition (standard of comparison) with primary characteristic X-rays or gamma rays with energies that do not coincide with the excitation potentials and energies of the characteristic X-rays of any of the major elements of the analyte, and such that between the energies coherently and incoherently scattered by the sample of the primary radiation is not none of the energies of the edges of the absorption of the main elements of the analyte, and the measurement of the intensities coherently and incoherently scattered at the same angle of the primary radiation, characterized in that, in order to expand the possibilities of the method, the intensity of coherently and incoherently scattered breakdown is additionally measured for the other two angles of primary radiation, calculate for each of the scattering angles the value of the ratio of the relative intensities of coherently and incoherently scattered radiation, and chenie scattering ability paddle analyte exists is determined by calculation using the latter. 2. A method for determining the scattering ability of a multicomponent substance, consisting in the irradiation of samples of an analyte and a substance with a known chemical composition (standard of comparison), primary characteristic X-ray or gamma radiation with energy that does not coincide with the excitation potentials and characteristic rent energies; gene radiation of one of the main elements of the analyte, and such that between the energies of coherently and incoherently scattered by the breakdown of the primary radiation did not get any of the energies of the absorption edges of the main elements of the analyte, and measuring the intensity of incoherently scattered at one the same angle of primary radiation, characterized in that, in order to expand

Description

The capabilities of the method additionally measure the incoherently scattered intensity of the breakdown on three other angles, then using one of them as a reference signal for the equation, calculate the ratios of relative intensities, and the value of the scattering ability of the analyte is determined by calculation using the latter.

3. The method for determining the scattering ability of a multicomponent substance consists in irradiating samples of an analyte and a substance with a known chemical composition (standard of comparison) by the primary characteristic x-ray or gamma radiation with an energy that does not coincide with the excitation potentials and energies of the characteristic x-ray radiation of one of the main elements of the analyzed

87039

substances, and such that between the energies coherently and incoherently scattered by the breakdown of the primary radiation, none of the energies of the absorption edges of the main elements of the analyte fell, and the measurement of the intensities coherently and incoherently scattered through the same angle of the primary radiation, differing in that, in order to expand the capabilities of the method, the intensities of coherently and incoherently scattered by the breakdown of the primary radiation of two other energies that satisfy the above listed conditions are additionally measured , Rasschitgeayut for each radiation power ratio of the relative intensities of coherently and incoherently scattered radiation, and the value of scattering ability of the analyte is determined by calculation using the latter.

The invention relates to X-ray spectral (XRD) and nuclear-physical (YFMA) methods for analyzing the composition of a substance and can be used in analyzing materials of complex chemical composition (powders, solutions, alloys). The purpose of the invention is to expand the capabilities of x-ray spectral analysis. The invention is applicable to the study of materials containing elements with atomic numbers from 6 to 92 (and known methods only from 6 to 30), is implemented on any crystal diffraction spectrometer, quantometer, diffractometer (variants 1 and 2), as well as on any X-ray spectrometer, including on X-ray radiometric spectrometric devices (option 3). The proposed method for determining the scattering ability of a multicomponent substance -t-r- is applicable to a 1 analysis of powdered, liquid and solid substances. Photon energy E; characteristic components of primary x-ray radiation or gamma radiation in all variants of the method are selected from tabular data in accordance with the qualitative composition of the materials studied, the spectral characteristics of x-ray tubes and radioisotope sources that do not coincide with the excitation potentials and energies of the characteristic x-ray radiation and also so that the energy of the absorption edge of the latter does not fall within the energy intervals between the coherent lines None of the primary characteristic or gamma radiations used is coherently and incoherently scattered by the sample. The choice of scattering angles b- (option 1) is arbitrary within the limits of O - 180 ° and due to the technical capabilities of the spectrometer used. In addition, angles 9 are selected from the intervals O - or 90 - 180 ° (option 2). The reference standard is used to reduce the measurement error due to the instability of the instrument. The method (variants 1 and 2) can be implemented using an X-ray spectrometer, as well as a multichannel quantometer with different angles of selection of secondary radiation through channels or an X-ray / diffractometer. In addition, the method (option 3) can be implemented using any X-ray spectrometer, but it is preferable to use an instrument equipped with an X-ray tube with several interchangeable anodes, or an analyzer with replaceable radioisotope x-ray or gamma radiation sources. Example, Experimental n - conducted with the use of artificial preparations and fluorspar ores and products of their processing; the preparations include elements with an atomic number m z 8-82 Artificial preparations consisting of the initial components SiOj, ZnO, Se, ZrOg, PbO, simulate no scattering ability of fluorspar ores and their intermediate processing. The experiment was carried out using two instruments: a semi-automatic spectrometer on which the CMo-Au- and C-anodes tubes were installed, as well as a modernized short-wave spectrometer with variable geometry of the X-ray optical system and the BHV-8 tube (Pd). For the determination of option 1, the indicated spectrometer is used with a voltage of U 40 kV, current i 30 ta. The powdered sample of the preparation is poured into a spectrometric cuvette and irradiated with the primary radiation of the RT. The background intensity is recorded at the place of the lines of coherently and incoherently scattered PdKjjj radiation at the maxima of their distributions at the following scattering angles: 9, 60 °, 02 90 °, 0 120 °. The choice of angles 9 is determined by the technical capabilities of the spectrometer used. The most preferred are 0; . A similar operation is performed with the standard of comparison. The processing of the obtained analysis results is carried out according to the scheme. First, the relative intensities I f, (b;) and 1 (9;) of the background, measured in place of the coherently and incoherently scattered primary characteristic radiation lines, are calculated, t ().) Fl (9) "1 - rj, (9; ); (c;) and -TG, (9;)) Then for each of the scattering angles, the ratio Im C b is found; ) I J. (9,), and the value of the values calculated from d S2 dsz equations. K, kg 1f (9,), kg 1 (92) j d + dA - dkv к-N + d, il (Qz) (1) 1, ---- 1Г (9з) dmd j,, к 1ф (9,) W 1ф (9g). about-m | / 15.4 9,) I (QZ) nk 1f (0}) "- d ir (in, - g, kg nk, nk where dg, d;, do, d - are coefficients not depending on the composition of materials and defined in the calibration process, equations (1) and (2) using calibration agents and values for various and 0 using table values dmd / d P for elements. Definition -v-, r- for option 2 also using the specified short-wave spectrometer. The test sample is placed in a spectrometric cuvette, irradiated with RT radiation, and the background intensity Nm (9,) is recorded in place of the incoherent line. The entrained scattered radiation at the maximum distribution with scattering Q A5, 60, 75 and 90 °. A similar operation is carried out with the standard of comparison. Then, using the measured N (0,), the relative intensities Nc®;) and I (b;) ) and find ipc i the ratio l (9;) (Gg). For the reference angle Qn take 9 90 °. Sign

value reading; make some money a 41

from the equation

 nineteen

Gb7) 1 1F (00

(3)

+ d 3)

kg

HK

dm (j

dm b

for tf dsi

, 2 emissions for option 3 are carried out using a semi-automatic spectrometer with a fixed angle of 0 120 °. The mode of operation of the device: voltage U 50 kV, current i ZOta, FiNE impeller (distance between the plates 1 160 μm) (In the spectrometer, in turn, set PT with Mo-, Ag- and Ge-anodes, Tubes are chosen in such a way that so that the energies E of the characteristic radiation of their anode do not coincide with the excitation potentials or characteristic lines of fluorescent radiation of any of the basic elements of the sample, and the energy of the absorption edges of the latter does not fall between the line energies of the coherently and incoherently scattered sample Spectrometric cuvettes with analyzed sample and external standard are installed in the spectrometer, alternately irradiated with PT radiation with Mo, Ag and Ge anodes, and the intensities are recorded.) and k1 (E) of MoK radiation in the. distribution peaks.

Processing the results of the experiment are carried out according to the scheme of option 1, and dmcj

determine from ur equation

 .HG.GFSE ,,),

, kg; g I p (E)

rj-f

The values of the coefficients are determined by

using calibration samples

containing items included

in the composition of the analyte.

For these samples, it is calculated by

 drnd: Tabular 1-data values

d 52

drnd

for line MoK, then samples

dS2

R

they are irradiated with X-ray tubes with CMO, Ag and Ge anodes, registers the intensities in place of the lines of coherently and incoherently scattered primary radiation at 9,120 ° and make up the required number of equations

about

regarding the coefficients d dj, d.j, which is solved by the least squares method. So for equation (4) the values are obtained;

d 0.3988; d 0,2899; d

 0.5078 and d-0.0299,

As shown by experimental studies, all variants of the method. possess accuracy not inferior

accuracy of the known method, applicable to the study of substances containing elements with atomic numbers from 6 to 92, The method can be implemented with a wide class of X-ray equipment.

Claims (3)

1. A method for determining the scattering power of a multicomponent substance, which consists in irradiating samples of the analyte and a substance with a known chemical composition (comparison standard) with primary characteristic x-ray or gamma radiation with an energy that does not coincide with the excitation potentials and energies of the characteristic x-ray radiation of none of the main elements analyte, and such that the primary radiation did not fall between the energies of the coherently and incoherently scattered breakdown of the primary radiation not one of the edge energies of the absorption of the main elements of the analyte, and the measurement of intensities of the primary radiation coherently and incoherently scattered by the same angle, characterized in that, in order to expand the capabilities of the method, they additionally measure the intensity of the coherently and incoherently scattered breakdown into two other angle of primary radiation, calculate for each of the scattering angles the values of the ratio of the relative intensities of the coherent and incoherently scattered radiation, and the value of the scattered vayuschey ability of the analyte is determined by calculation using the latest. 2. A method for determining the scattering power of a multicomponent substance, which consists in irradiating samples of an analyte and a substance with a known chemical composition (standard of comparison) with primary characteristic x-ray or gamma radiation with an energy that does not coincide with the excitation potentials and energies of characteristic x-ray radiation, none of the main elements of the analyte, and such that the primary radiation does not fall between the energies of the coherently and incoherently scattered breakdown of the primary radiation not one of the energies of the absorption edges of the main elements of the analyte was measured, and the intensity of the primary radiation incoherently scattered by the same angle was measured, characterized in that, in order to expand the capabilities of the method, the intensities of the incoherently scattered breakdown were additionally measured at three other angles, then using one of them as a reference comparison signal, the ratios of relative intensities are calculated, and the scattering value of the analyte is determined by I eat with the latter. 3. A method for determining the scattering power of a multicomponent substance, which consists in irradiating samples of an analyte and a substance with a known chemical composition (standard of comparison) with primary characteristic x-ray or gamma radiation with an energy that does not coincide with the excitation potentials and energies of the characteristic x-ray radiation of none of the main elements analyte _(substance such that between the energies of coherently and incoherently scattered primary radiation sample without falling and not one of the energies of the absorption edges of the main elements of the analyte, and the measurement of intensities of the coherently and incoherently scattered by the same angle of primary radiation, characterized in that, in order to expand the capabilities of the method, they additionally measure the intensities of the coherently and incoherently scattered breakdown of the primary radiation of two other energies satisfying the listed conditions, the ratios of relative intensities are calculated for the emission of each energy, the ratios of the relative intensities are coherently and incoherently scattered th radiation, and the value of the scattering ability of the analyte is determined by calculation using the latest.