Method of manufacture of standard samples of atmospheric aerosols, which is loaded on the filter

 

(57) Abstract:

The invention relates to analytical chemistry, in particular, to methods for producing synthetic standard samples, simulating composition of atmospheric aerosols, which is loaded on the filter, and can be used in quantitative chemical analysis of atmospheric aerosols to determine the calibration characteristics and validation of the analysis results. In the method of manufacturing a synthetic standard samples of atmospheric aerosols, which is loaded on the filter, prepare methylcellulose film containing the designated elements. Then stamp foil individual instances. Selected in predetermined ratios sample fine powder containing trace elements, and dry methyl cellulose mixed to a solid color by color mixture and fill it with distilled water, heated to a temperature of 70-80C. Mix thoroughly and incubated at room temperature, stirring every 30 minutes for 2 hours Method can improve the accuracy of the analysis of atmospheric aerosols through the convergence of physical and chemical characteristics of the samples and comparison of real aerosol samples loaded on ski standard samples, simulating composition of atmospheric aerosols, which is loaded on the filter, and can be used in quantitative chemical analysis (KHA) composition of atmospheric aerosols to determine the calibration characteristics and validation of the analysis results.

One of the main difficulties in a non-destructive analysis of aerosols is the definition of calibration characteristics methods KHA due to the lack of close physical-chemical properties of standard samples of composition of the aerosol. Use as a specimen of the real aerosol samples analyzed by other methods, it is impossible due to their destruction in the process of analysis and complexity of parallel sampling of the same physico-chemical properties. The latter is caused by the uneven distribution of the designated components in the certified facility. Usually analysis techniques aerosols are calibrated using synthetic samples, simulating aerosols, which is loaded on the filter [1].

A known method of manufacturing a specimen by applying solutions containing trace elements, the filter of the same type that is used for sampling of atmospheric aerosols [2]. Fake is because atmospheric aerosols and industrial emissions into the atmosphere, mostly, are finely dispersed particles.

Known method of preparing the specimen by spraying of metals on organic thin films [3]. The disadvantage of this method is the inadequacy of the samples real samples of aerosols collected on the filter, because the elements are applied on the film in an atomic state and is located on its surface, whereas the aerosol particles are distributed throughout the volume of the suction filter and presents various chemical compounds.

The closest in technical essence and the achieved result to the invention is a method for preparing standard samples in the form of methylcellulose films containing a known amount of the designated items, which is that in the solution of methylcellulose add standard solution containing trace elements [4]. The resulting mixture is then poured onto the cleaned glass plate positioned horizontally, and dried in air at room temperature. From the obtained polymer film stamp samples of a given size. The disadvantage of this method is inadequate samples real samples of aerosols is the methyl cellulose in the form of soluble compounds. While atmospheric aerosols and industrial emissions into the atmosphere, mostly, are finely dispersed particles comprising water-insoluble metal compounds (silicates, oxides, carbonates and others). The difference in physico-chemical properties of the samples comparison and real samples of aerosols, which is loaded on the filter, reduces the accuracy of the results of the analysis of atmospheric aerosols.

Improving the accuracy of the results of the analysis of atmospheric aerosols through the convergence of physical and chemical characteristics of the samples of comparison and real samples of aerosols, which is loaded on the filter is achieved in the proposed method, the fact that selected in predetermined ratios sample fine powder containing trace elements, and dry methyl cellulose mixed to a solid color by color mixture and fill it with distilled water, heated to a temperature of 70-80C, thoroughly mixed and incubated at room temperature, stirring every 30 minutes for 2 hours Then the mixture is stirred and slowly poured onto the cleaned glass plate positioned horizontally. After drying the polymer film is removed from the glass and out of the punched samples of a given size.

Primeo in the prototype solution of methylcellulose has not given positive results due to aggregation therein fine particles of the powder material, contains trace elements, and, consequently, its uneven distribution over the volume of the solution. As a result, even after rejection of about 40% of the copies of the film samples, the relative standard deviation (Sse) characterizing the instability of the composition of the obtained instances, is 0.12.

Example 2 (in the prototype). Obtain standard samples of atmospheric aerosols by introducing a fine powder containing the designated elements in the polymer solution used in the prototype, in the form of water or acetone suspension has not led to positive results due to aggregation of the powder particles and the dependence of the quality of the film samples from the chemical composition of the powder mixture. After the rejection of about 20% of the samples the value of Ssecharacterizing the error of making quality copies, is 0.08.

Example 3. A portion of the powder state standard sample of fly ash coals (GSO, SW-1) mass of 10 g of milled for 3 h in an agate mortar with the addition of ethanol. To obtain a film sample of dry methyl cellulose mass of 1.1 g of the powder material by mass of 0.1 g was placed in a glass beaker and peremishliany water volume of 50 ml, heated to a temperature of 70-80 ° C, stirred for 20 min and leave for 2 hours, stirring every 30 minutes for the swelling of the polymer. Then the mixture is again stirred and slowly, over 2 minutes, and pour it on the precleaned using surfactants glass plate positioned horizontally. Dry film is easily separated from the glass. Foil stamped samples of a given size. The number of defective copies does not exceed 5%. After their rejection of the instability of the chemical composition of individual instances of the standard samples are characterized by a relative standard deviation constituting 0,04-0,07 depending on the element being defined.

Similar physico-chemical characteristics of standard samples of aerosols, which is loaded on the filter based on GSO soil.

The developed method allows to prepare synthetic standard samples of atmospheric aerosols, which is loaded on the filter, characterized by wide variations in the chemical composition and mass (20-500 mg/cm2) powder particles, which gives the opportunity to apply them in KHA composition of urban and industrial aerosols.

Sources of information

1. Smagulov. lab. - 1993. - T. 59, No. 4. - S. 20-28.

2. Russo I. C., Gutten D. R. Aerosol penetration in bulk filter samples of coastal maritime aerosols.// Atmospheric Enviroment. - 1989. - Vol.23, No. 6. - P. 1337-1347.

3. Maguar Century, Vonmant J. Kombinierte Anwenung der Atmabsorption on onder Routgen fluorescenz beider Bestimmung Von Blei in atmospharis Chem. Technol// Z. Anal. Chem. - 1976. - Vol.280, No. 2. - P. 115-120.

4. Billiet J., Pams R., Hoste J. Multielement thin film standards for XRF analysis.// X-ray Spectrom. - 1980. - Vol.9, No. 4. - P. 206-211.

A method of manufacturing a synthetic standard samples of atmospheric aerosols, which is loaded on the filter, including the preparation of methylcellulose films containing trace elements, and the stamping of her individual instances, wherein the selected predetermined correlation sample fine powder containing trace elements, and dry methyl cellulose mixed to a solid color by color mixture and fill it with distilled water, heated to 70-80C, thoroughly mixed and incubated at room temperature, stirring every 30 minutes for 2 hours

 

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