Method of preparing standard aerosol samples

FIELD: chemistry.

SUBSTANCE: method of preparing standard aerosol samples based on a mixture of fine powder containing defined elements is characterised by that a dispersed mixture of mineral, synthetic and biological materials is used, wherein grain size analysis is used to detect presence of said types of simulating materials and content thereof in a real atmospheric suspension in said region as applied to a specific season is determined.

EFFECT: providing maximum similarity of simulated atmospheric suspensions for different regions and conditions.

11 dwg

 

The invention relates to analytical chemistry and experimental medicine, in particular to methods and means of production samples, simulating composition of atmospheric aerosols, and can be used to study their influence on immunoallergic status of living organisms.

A known method of preparation of standard samples of aerosols in the form of thin organic films, which are obtained by adding to the solution of methylcellulose standard solution containing trace elements, the mixture is then poured onto the cleaned glass plate positioned horizontally, dried in air at room temperature and the polymer film stamp samples of a given size (see Billiet J., Pams R., Hoste J. Multielement thin film standards for XRF analysis // X-ray Spectrom. - 1980. - Vol.9, No. 4. - P.206-211).

The disadvantage of this method is inadequate samples real samples of aerosols collected on the filter, on the physico-chemical properties due to the addition of the designated elements in the solution of methylcellulose in the form of soluble compounds. While atmospheric aerosols and industrial emissions into the atmosphere mainly consists of fine particles comprising water-insoluble metal compounds (silicates, oxides, carbonates and others).

The closest in technical essence and DOS is haemosu result to the invention is a method for preparing standard samples of aerosols on the basis of a mixture of finely dispersed powder, contains trace elements (see EN No. 2239170, G01N 1/28, 2002). Then, the mixture powder containing trace elements, mixed with powder of dry methyl cellulose and fill with distilled water, heated to a temperature of 70-80°C, thoroughly mixed and incubated at room temperature, stirring every 30 min for 2 hours. The mixture is slowly poured onto the cleaned glass plate positioned horizontally. The dried polymer film is removed from the glass and out of the punched samples of a given size.

The disadvantage of this approach is a rejection of approximately 5% of instances, with instability on the chemical composition of the remaining individual instances of the standard samples is characterized by a coefficient of variation equal to 4-7% depending on the element being defined. The difference of the contents of the designated elements in the individual instances of the standard samples reduces the accuracy of control of the chemical composition of atmospheric aerosols, which is loaded on the filter, using a variety of spectral and chemical methods of analysis. Also the disadvantage of this method is the length (about 3 hours) and intensity (all operations are performed manually process a homogeneous mixture of polymer solution and defined components. However, a significant disadvantage is the inability to use the output samples, simulating composition of atmospheric aerosols in the study of their impact on living organisms in the experiment, including immunoallergic status of living organisms.

The objective of the proposed method is the possibility of using samples, simulating composition of atmospheric aerosols in the study of their impact on living organisms in the experiment.

The technical result obtained by the solution of the problem, expressed in the possibility of using samples, simulating composition of atmospheric aerosols in the study of their impact on living organisms in the experiment. This permits the maximum similarity of the simulated atmospheric suspensions for different regions and conditions.

To solve this problem the method of preparation of standard samples of aerosols from a mixture of fine powder containing trace elements, characterized in that use dispersed mixture of mineral, synthetic and biological materials, such as mineral component use powdered zeolite tuff in two size fractions up to 1 μm and from 1 to 100 μm, as a synthetic component use plastic crushed to fractions of tens of microns, as a biological component using crushed to fractions not more than 100 μm mixture of leaves and grass, and/or animal hair and/or feathers of birds, representatives of the biosphere in the region, and previously using granulometric analysis, reveal the presence of these types of modeling materials and determine their content in real atmospheric composition of sediments in this region in relation to a particular season.

Comparative analysis of the characteristics of the claimed solution with the characteristics of the prototype and analogues demonstrates compliance of the claimed solution to the criterion "novelty".

Signs of a distinctive part of the formula of the invention provide a solution to complex functional tasks.

Signs "... use of a dispersed mixture of mineral, synthetic and biological materials" provide the maximum line models of real aerosol composition of atmospheric pollution.

Signs "... as a mineral component use powdered zeolite tuff" provide good availability of this material as a raw material component, and take into account the fact that the zeolite - rock weathering crust, constantly in contact with living organisms, because of their widespread prevalence (one of the most widely represented aluminosilicates, occupying sixth place in the world reserves).

Signs indicating that the zeolites must be represented "the two size fractions - up to 1 μm and from 1 to 100 μm, enable you to consider the real granulometric composition of mineral suspensions, which is important due to the different mechanism of action on the human body mentioned fractions (larger particles taking into account the density of the material does not pass beyond the nasopharynx and smaller because of its volatility are not deposited in the upper respiratory tract): according to Npostin (Bulletin of the DEPARTMENT of EARTH SCIENCES RAS - ELECTRONIC SCIENTIFIC INFORMATION JOURNAL No. 1(22) 2004, article "MINERAL WORLD AND HUMAN HEALTH) every person passes through their respiratory system daily about 12 m3air, i.e. about 15 kg Only in the earth's atmosphere weighed about 20 million tonnes of mineral substances. In the industrial areas of their concentration in the hundreds and even thousands of times higher; so that people see not pure the air, and the air-mineral mixture, aerosol with a particle size of from 0.001 to 1000 μm. Every breath is drawing to a million of mineral particles.

In the process of evolution, living organisms have developed a very effective cleaning mechanism of inhaled air: coarse particles (>5 μm) are deposited in the channels of the nasopharynx, up to 90% of small particles retained in the upper respiratory tract and bronchi, from which they are removed together with mucus by expectoration. As our research shows, the penetrating ability of the powder is shaped materials in the respiratory tract depends not only on the size of particles, but from the mode of respiration; deep vigorous breaths (increased intensity of respiration) the size of particle that can penetrate the upper respiratory tract, lying in the upper part of the claimed range (from 5-6 to 10 μm); in normal breathing the size of particle that can penetrate the upper respiratory tract, lies in the middle part of the claimed range (from 2-3 to 5-6 μm); at low intensity breathing the size of particle that can penetrate the upper respiratory tract, lying in the lower part of the claimed range (from 1-2 to 3-4 μm).

Signs indicating that "as a synthetic component use plastic crushed to fractions tens of microns", take into consideration achievable range of particle sizes of the synthetic component with the shredding of plastic in the manufacture of a component in the process of implementation of the method), and recorded in real samples of the aerosol.

Signs indicating that "as a biological component used crushed up the fractions less than 100 microns mixture of leaves and grass, and/or animal hair and/or feathers of birds, representatives of the biosphere of this region, provide the ability to accurately bindings of properties of the components of the standard samples of aerosols to the real conditions of the region.

Signs indicating that "previously, using granola etnicheskogo analysis, identify the presence of these types of modeling materials and determine their content in real atmospheric composition of sediments in this region, provide the ability to accurately bindings concentrations of the components of the standard samples of aerosols and their financial structure to the same parameters of real aerosols collected in the region.

The signs that reveal the presence of these types of modeling materials and determine their content in real atmospheric composition of sediments in the region "in relation to a specific season, allow to take into account seasonal changes in these parameters of real aerosols.

The claimed invention is illustrated in the drawings, where figure 1-8 shows samples of mineral mist: figure 1 - sample of snow collected on the shkot Peninsula (Increase x16); figure 2 - sample of snow collected in the area of the First river (magnification X10); figure 3 - sample of snow collected in the area Pushkin street (increase x8); figure 4 - sample of snow collected in the region of the Second river (increase K); figure 5 - sample of snow collected in the area Sadgorod (increase x8); figure 6 - from a sample of snow collected in the district Amar (increase x8): 7 - from a sample of snow collected in the district Zmeyka (increase K); Fig - from a sample of snow, assembled the CSOs in the Quiet Bay area (increase K); figure 9, a and b shows the electron micrograph of the rubber particles from the sample collected in the area of the Second river (increase) h and b) x 106); figure 10 shows the electron micrograph of the particles of plastic (a) and vitreous fibers from a sample collected near the Pushkinskaya (increase a) x111 and b) h); figure 11 shows electron micrographs of the particles of fragments of marine organic matter from the sample collected near the sea, in the samples area Sadgorod (a) and Egersheld (b).

The basis of the claimed invention based on the following considerations.

Suspended in the atmosphere particles have a significant impact on air quality and climate. The composition and air pollution are among the leading risk factors for health, for example, atmospheric pollution, reducing the immune resistance of the organism is accompanied by the growth of infectious and allergic respiratory diseases.

Evaluation of the atmospheric transport of substances and the total mass of sediment produced by different authors differ in tens and hundreds of times, due to imperfections of the used methodologies and disabilities instrumentation used (see Glazov NF Selected works in two volumes. So 1. Geochemical fluxes in the biosphere. - M.: Association of scientific, KMK, 2006. 535 C.2).

In this regard, the measured characteristics (material composition, the size and content) of natural atmospheric suspensions by the example of the port city of Vladivostok. Samples (precipitation in the form of snow) were collected during the winter season 2010-2011 during the snowfall. The sampling points were located in eight districts of Vladivostok: the shkot Peninsula (area street Krygina); Pushkinskaya street (near funicular); First river (near Komsomolskaya street); Second river (near the intersection of Russian, Bagration); Sadgorod (shore); Emar (shore); Zmeyka (district Kosmodemyanskaya street) and the silent Bay (green zone at a distance of 500 m from CHPP-2). In order to eliminate the secondary pollution by anthropogenic aerosols, selected, only the top layer (5-10 cm) of fresh snow. The snow was placed in sterile containers with a volume of 1 L. After a couple of hours, when the snow in containers completely dwindle to nothing, after tilting of each sample was scored 40 ml of liquid and analyzed on a laser particle analyzer Analysette 22 NanoTech (Fritsch). This enabled during one measurement to identify the distribution of particle sizes, and to determine their shape. Physical analysis of sediment produced by a light microscope Zeiss Discovery VI 2 (Germany) and electron microscope (Zeiss Ultra Plus with energy dispersive spectrometer (Germany). The coated samples for electron microscopy were made of gold.

In a typical sample taken is m on the shkot Peninsula (shore) (figure 1), revealed quartz, feldspar, quartz-feldspar intergrowths of quartz with malachite films, kaolinite, difficultly determined particles of rocks, silica-iron oxide particles, glassy particles, anthropogenic particles of unknown origin, plagioclase, particles of concrete, slag spectrum, vegetative detritus, rubber particles.

In the area of the First river (industrial area with the presence of TPP-1) (figure 2) revealed particles of carbon black, quartz, feldspar, bitumen, glass, rubber. Soot layer covers all other particles, but the predominant number are natural mineral particles.

In the sample taken at the Pushkin street (industrial area) (figure 3), were identified quartz, feldspar, synthetic fibers, carbon black (slag), the iron oxide film (organic and inorganic).

In the sample taken in the region of the Second river (the region with a high motor load) (figure 4), were identified quartz, rubber particles, feldspar, synthetic fibers, soot, slag particles, unidentified organics.

In the sample taken in the area Sadgorod (shore) (figure 5), were identified quartz, feldspar, slag, sludge, plant detritus, unidentified organics (animal hair and fragments of plants or algae), synthetic particles, particles of coal. Many particles are aggregated.

In the mod is Sze, taken in the district Amar (shore) (6), were identified quartz, feldspar, plagioclase, epidote, metal oxides, particles of coal and asphalt plant detritus.

In the sample taken in the area of Zmeyka (shore) (Fig.7)were quartz, feldspar, plagioclase, chalcedony, epidote, technogenic particles of unknown origin.

In the sample taken in the Quiet Bay area (industrial area near the CHPP-2) (Fig), were identified soot, slag, quartz, feldspar, plagioclase, changes.

In all areas, Vladivostok there is a marked correlation between the environmental characteristics of areas (e.g., increased motor load or the proximity of the sea) and the composition of the sediment (particles of rubber and fragments of organic matter, respectively). Thus, in the region of the Second stream with increased automotive press were rubber particles (figure 9, a, b); near Pushkinskaya there are many man-made particles, including plastic (figure 10,a) and glass (figure 10,b) fibres; near the sea, in the samples area Sadgorod (11,a) and Egersheld (11,b) there were found fragments of marine organic matter.

All observed particles atmospheric suspensions can be divided into three groups: natural inorganic (particles of minerals), man-made (synthetic particles, slag, soot and other) and natural organic matter (pollen, a fragment of the insects and plants, the fur of animals and others), which correlates with the observations of other researchers (see Ivanov V.V. Material composition of the insoluble particles in snow cover in southern Sakhalin (data from electron microscopy and IR spectroscopy) / V.V. Ivanov, N.A. Kazakov, G. Kolesov, etc. // Abstracts of International Symposium "Physics, chemistry and mechanics of snow". Yuzhno - Sakhalinsk, 2011. Pp.33-37; Svinarov VG's Research, modeling and prediction of air pollution in the city: author. dis. Dr. geogr. Sciences. - Vladivostok, 1997. 44 C.; Centrosema SV air Pollution and health status of the population of industrial cities. - St. Petersburg: Publishing house of Asterion, 2004. 246 S.; Khristoforova NICHOLAS Ecological problems of the region: far East Primorye. - Khabarovsk publishing house, 2005. 304 S.; Shevchenko V.P. Distribution and composition of the insoluble particles in the snow of the Arctic / Wepsiec, Apocynin, Rstin etc. // Problems of the Arctic and Antarctic. 2007. No. 75. P.106-118).

We can conclude that in the modern city (on the example of Vladivostok), despite the fairly large number of anthropogenic sources of atmospheric suspensions (TPP-1, TPP-2, 38 large boiler, incinerator and about 350 thousand vehicles), the share of anthropogenic particles is not dominant and is not more than 10-15%. This fact can explain the characteristic, Vladivostok strong the mi winter monsoon winds of the North-West points of the compass (mainland), strong partition of the territory, and relatively shallow snow cover.

Thus the structure of standard samples of aerosols was adopted as a mixture of mineral, synthetic and biological materials.

The claimed method is implemented as follows.

As the mineral component of the suspension, you must use powdered zeolite tuff in two size fractions:

the first, the second micro (1-100 μm) (its manufacture is provided by grinding sterilized (for example, by irradiation with ultraviolet light) hanging crushed to 4-10 mm zeolite in an ultrasonic disintegrator, for example, Bandelin SONOPULS HD 2070 (the working frequency of 22 kHz, the maximum power 400 W)), is subjected to grinding to obtain the fraction with a particle size of less than 100 microns;

second - nano (up to 1 µm) (its manufacture is provided by grinding in variablearea mill, for example, pulverisette 4, hanging the micro-size particles of the zeolite prepared in the first stage).

Synthetic component - shredded plastic (first crushed on a metal grater (up to granule size less than 1 mm), and then in a planetary mill (up to tens of microns)). Further grinding because of the plastic properties of the material impossible. The composition of the material for the manufacture of this component is determined by the real part of the atmospheres of the second suspension, defined in the region, which is modeled aerosol, using one or two, maximum three types of plastics that are identified in real aerosols in this region.

The biological component is a powdered in an ultrasonic disintegrator mixture leaves the ground of trees, algae, animal hair (cats, dogs). The composition of the material for the manufacture of this component is determined by the composition of the real atmospheric suspended sediment, specific to the region, which is modeled aerosol, using one or two, those kinds of materials, which share at least 15-20% in the composition of the sample of real aerosol in this region.

The thus prepared monocomponent in a known manner are mixed in proportions corresponding to their share in the structure of the real atmospheric suspended sediment, specific to the region or season using granulometric analysis.

The thus prepared material is used in a known manner, for example, implement the classical scheme of the study the impact of substance real atmospheric suspensions on living organisms (laboratory animals) in the experiment, using the claimed substance as adequate and repeatable experimental models of sediment. While animals perform inhalation exposure to known way, for example, the use of cells with dimensions exceeding the size of the animal, provided with a cover made of airtight material such as polyethylene. When this aerosol is injected into the cavity of the cell, filling its internal volume, which causes the animal to inhale it. As a means of formation of aerosol use ultrasonic nebulizer, for example ultrasonic portable nebulizer UE-0,25 "ARSA" (which loads a given sample of sprayed material), an exhaust channel which is reported with the cavity cells. The experimental animal is placed in a cage, and then form in the amount of cells the cloud aerosol. The amount of sprayed material and the length of stay of the animal in the cage is the rate of getting different groups of experimental animals doses from 100 to 1000 mg/kg (1 times a day up to 40 min). A group of control animals not exposed to the drug.

After experienced the events specified in the experiment produces the instantaneous slaughter of animals by decapitate and collect material for research. Next, in a known manner, in accordance with the purposes of the experiment, produce dissection laboratory animals, take samples of the biological material and carry out their analysis using appropriate laboratory tools. For example, to produce the color is and the preparation of slides for light microscopy for optical morphometrics or photography or other manipulation.

The method of preparation of standard samples of aerosols from a mixture of fine powder containing trace elements, characterized in that the obtained dispersion a mixture of mineral, biological and synthetic materials, by mixing them in proportions corresponding to their share in the structure of the real atmospheric mixture, the mineral material use powdered zeolite tuff in two size fractions up to 1 μm and from 1 to 100 μm, as the use of biological material crushed to fractions of not more than 100 μm mixture of leaves and grass, and/or animal hair and/or feathers of birds, representatives the biosphere of this region, and as a synthetic plastic material used crushed to fractions of tens of microns, then form an aerosol using an ultrasonic nebulizer, and previously using granulometric analysis reveals the presence of a named mineral, biological and synthetic materials and determine their content in real atmospheric composition of sediments in this region in relation to a particular season.



 

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