CS266708B1 - A method for determining the content of all sulfur in a titanium-containing coal - Google Patents

Abstract

The method of eliminating the disturbing influence of changes in the titanium content on the determination of the total sulfur content in coal by the method of spectral radionuclide X-ray fluorescence analysis is addressed. The method of determining the total sulfur content in coal containing titanium depends on the fact that the coal sample is successively irradiated with the radionuclide 238Pu and 55Fe, the spectra of the characteristic radiation of the coal sample are measured, then the K(alpha) of titanium is distinguished from other peaks by the method of overlapping factors and the total sulfur content is correlatedly evaluated. The method is intended for operating conditions of mining plants.

Description

The present invention relates to a method for determining the total sulfur content of titanium-containing coal by spectral radionuclide X-ray fluorescence analysis using a proportional detector and solves the problem of increasing the accuracy of the determination of sulfur when the titanium content fluctuates.

The method of determination of all sulfur in coal by spectral radionuclide X-ray fluorescence analysis, eg according to MS. author's certificate No. 262 318, which in the result of the analysis takes into account the effect of fluctuations in the content of calcium, iron and ash in the measured sample of coal.

By comparing the results of classical chemical analysis and X-ray fluorescence analysis in determining the content of all sulfur in different samples of coal, it was found that the accuracy of the results is affected by a hitherto unweighed effect. The inventors have found that the interference is caused by fluctuations in the titanium content of the coal.

The methods used so far by X-ray fluorescence analysis and their modifications did not consider the interfering effect of titanium in coal on the determination of all sulfur. This interfering effect of titanium impurities in the coal is a matrix phenomenon when applying radionuclide X-ray fluorescence analysis (similar to calcium, iron and ash contents) and causes a significant reduction in the accuracy of the results in determining the total sulfur content of coal by the method.

The essence of the invention, which reduces the said negative effects of the titanium content, is that the coal sample is gradually irradiated with the radionuclide ^ ^^ Pu and ^ Fe, the characteristic radiation spectra of the coal sample are measured, the titanium sulfur is correlated.

Using this method, the peaks of calcium and titanium in the spectrum that otherwise coincide when using a proportional detector are distinguished. At the same time, the whole process of determining the area of the sought peaks not only of titanium, but also of calcium and iron will be specified. The use of correction factors is simple and can be adjusted as a microcomputer program that can be built directly into a portable spectrometric radionuclide X-ray fluorescence analyzer. The overlapping factor method is a computational procedure that allows peak areas to be calculated even if they overlap. Fig. 1 shows the characteristic radiation spectra of two coal samples after treatment according to the method of the invention, Fig. 2 shows the spectrum of the coal sample originally obtained.

The results of the present invention can be further assessed from Table 1, which shows a comparison of the process used so far with the process according to the invention for 20 coal samples. All sulfur contents are given in%, the prior art using sulfur, calcium, iron and Pu emitter backscatter peaks, the process of the present invention utilizing sulfur, calcium, iron 238 and titanium peaks and the Pu emitter backscatter peak. For both procedures, the results of the determination of the total sulfur contents by classical chemical analysis according to CSN are given below. ;

A comparison of the values given in the table shows that when using the current procedure the error of determination is S 1 = 0.297, when using the method according to the invention only S 2 = 0.174.

The determination of the total sulfur content of the coal according to the invention is intended for operating conditions.

CS 266 708 Bl 3

Table

Sample number Current method Contents S _x . (%) total The method according to the invention ^{with a content} VESKO. ^(%) according to RFA according to chemical analysis according to RFA according to chemical analysis 1 1,258 th most common 1.03 0.66 1.03 2 1,196 th most common 1.37 1.62 1.37 3 2,256 th most common 2.86 2.86 2.86 4 1,065 th most common 1.18 1.32 1.18 5 1,340 th most common 1.07 0.93 1.07 6 1,911 th most common 2.13 2.37 2.13 7 1,487 th most common 2.18 1.96 2.18 8 2,150 th most common 2.87 2.98 2.87 9 1,667 th most common 1.32 0.97 1.32 10 1,820 th most common 2.08 2.19 2.08 11 1,891 th most common 1.84 . 1.97 1.84 12 2,771 th most common 2.24 2.19 2.24 13 2,019 th most common 2.57 2.17 2.57 14 2,104 th most common 1.71 1.56 1.71 15 1,345 th most common 1.23 1.21 1.23. 16 1,660 th most common 1.43 1.56 1.43 17 1,287 th most common 1.27 1.59 1.27 18 3,466 th most common 3.35 3.61 3.35 19 1,789 th most common 1.83 1.91 1.83 20 2,132 th most common 2.39 2.56 2.39

OBJECT OF THE INVENTION

Claims (1)

OBJECT OF THE INVENTION Method for the determination of the total sulfur content of coal containing titanium by the method of spectral radionuclide X-ray fluorescence analysis using a proportional detector, marked 238 55 by sequentially irradiating the coal sample with the radionuclide Pu and Fe, measure the characteristic radiation spectra of the coal sample, distinguish K _and titanium from the other peaks by the method of overlapping coefficients, and evaluate the total sulfur content by correlation.