RU2679232C1 - Device for collecting films of oil and oil products from water surface - Google Patents

Abstract

FIELD: sampling.

SUBSTANCE: invention relates to the field of analytical research of films from oil and oil products, in particular to methods of sampling for subsequent analyzes and surface concentration control. Device for sampling oil and oil products from the water surface contains a sampler made in the form of a hollow cylinder of inert material, on the outer surface of which there are risks for measuring the volume of the sample being taken, and a cover of inert material, which can be installed on the end of the cylinder from the side of sampling from the surface of the water. Cylinder of the sampler has a wide L₁ and narrow L₂ sections. Lengths of the wide and narrow sections are chosen from the setting L₁≤3.5–5.5 L₂, diameters from setting D₁≥2.5–4.5 D₂. Device further comprises a cover that can be installed on the second end of the cylinder of the sample catcher. Risks for measuring the volume of the sample taken are performed on the surface of a narrow section of the cylinder.

EFFECT: invention allows to precisely and rapidly determine the qualitative and quantitative content of oil and oil products on the water surface due to the concentration of organic matter in the process of sampling and expansion of the research objects and improves the analytical characteristics of the method.

1 cl, 10 dwg

Description

The invention relates to the field of analytical studies of films of oil and oil products, in particular, to methods for sampling for subsequent analyzes and control of surface concentration.

A known sampler for evaluating the thickness of a layer of oil above water, containing a thin-walled, transparent vertical casing of a material that is not wetted by oil and oil products. A case without a bottom has a constant internal sectional area and a sharp edge in the lower part; in the upper part, the body is conically narrowed and connected to a flexible outlet, to which two valves are connected: side - for air passage and central - for liquid passage, to the central a calibrated pipette is attached to the crane, which in turn is connected to a double-acting pump. A calibrated pipette is configured to pre-place a fixed volume of oil solvent and then feed the solvent into the oil using a pump. The body of the sampler exceeds a calibrated pipette in terms of internal cross-section [RF Patent No. 2534791, cl. G01N 1/10, G01F 23/04, publ. 12/10/2014].

A disadvantage of the known sampler is an insufficient amount of sample taken, due to the execution of the body of the sampler from non-wettable material, which does not allow for slow drainage of the sample and, as a consequence, the deposition of oil film on the surface of the sampler in sufficient quantity.

A known sampler for determining the thickness of the oil layer above water, containing a thin-walled vertical body with a handle in the upper part and a tapered valve seat in the lower part, a ball for overlapping the saddle, suspended on a fishing line from the handle with two positions of the ball relative to the saddle, and at the lower mounting point fishing line to the handle of the ball freely lies on the saddle and overlaps it, and at the top point of attachment, the ball is raised above the saddle. Before the sampler is lowered into the test liquid, the conical saddle is closed with a ball, the body is filled with water with a density exceeding the density of the test water under a layer of oil [RF Patent No. 2452933, cl. G01N 1/10. G01F 23/04, publ. 10.12.2014].

A disadvantage of the known sampler is the low accuracy of the analysis of the selected sample. The low accuracy of the analysis is due to the fact that the design of the device does not provide for the deposition of film on the surface of the sampler. A sampler is used to determine the thickness of the oil layer above water. Moreover, the thickness of the oil layer is determined visually by a measuring ruler. And since since this thickness is insignificant (practically this is a film), then the measurement accuracy will be very low.

The closest technical solution to the proposed one is a device for the selection of films of oil and oil products from the surface of the water, containing a sampler of inert material, made in the form of a hollow cylinder with a developed inner surface, which on the one hand can be closed with a stopper of inert material, and on the other hand made with a tip in which a precision valve is installed; on the outer surface of the sampler, risks are taken for measuring the volume of the sample taken. The hollow cylinder is made with a ratio of the diameter of the inner section to the height of 1: 3-1: 10. The sampler can be made of quartz, glass or ceramic materials. [RF patent No. 2604843, cl. G01N 1/10, publ. 12/10/2016].

The disadvantages of the device include the inability to concentrate organic matter during the sampling process, the inability to take very thin films from the surface of the water, the difficulty of sampling for analysis make it difficult to use it in the field.

The technical problem to be solved in the present invention is the exact rapid determination of the qualitative and quantitative content of oil and oil products on the surface of the water due to the concentration of organic matter in the sampling process and the expansion of research objects (thin films).

The specified technical problem is solved due to the fact that in the device for collecting films of oil and oil products from the water surface containing a sampler made in the form of a hollow cylinder of inert material, on the outer surface of which risks for measuring the volume of the sample taken, and two covers of inert material. One of them can be installed on the end of the cylinder from the sampling side from the surface of the water, and the other on the second end of the cylinder of the sampler. The sampler cylinder has two sections: wide L ₁ and narrow L ₂ , while the lengths of the wide and narrow sections are selected from the condition L ₁ ≤3.5-5.5L ₂ , and the diameters from the condition D ₁ ≥2.5-4.5D ₂ , and the risks for measuring the volume of the sample taken are performed on the surface of a narrow section of the cylinder.

The essence of the invention is illustrated by drawings: FIG. 1 - a device for selecting films of oil and oil products from the surface of the water;

FIG. 2 - annealing of the device before selecting the film; FIG. 3-position of the device before selecting the film; figure 4 - the beginning of the sampling; FIG. 5 - end of sampling;

FIG. 6 - raising the sample and measuring the height of the layer of oil and oil products; FIG. 7 - removal of water from the sampler and deposition of a film of oil and oil products on the inner surface of the narrow part of the sampler; FIG. 8 - dissolution of a film of oil and oil products deposited on the inner surface of a narrow section of the sampler to perform analysis by standard methods of analytical chemistry;

FIG. 9 - removal of a film of oil and oil products from the outer surface

sampler for analysis by express method;

FIG. 10 - determination of the content of organic substances in the film of oil and oil products by the express method.

A device for selecting films of oil and oil products from a water surface is shown in FIG. 1 and contains a sampler made in the form of a hollow cylinder of inert material. The cylinder of the sampler has wide 1 (length L ₁ ) and narrow 2 (length L ₂ ) sections, while the lengths of the wide and narrow sections are selected from the condition L ₁ ≤3.5-5.5L ₂ , and the diameters from the condition D ₁ ≥2 5-4.5D ₂ .

On the outer surface of narrow section 2, risks 3 are fulfilled for measuring the volume of the sample taken. At the ends of the cylinder of the sampler, covers 4 and 5 are made of inert material.

A device for the selection of films of oil and oil products from the surface of the water works as follows.

Before sampling the films, annealing (see Fig. 2) is carried out in the furnace 6 of a narrow section 2 of the sampler. Next, the sampler is cooled to ambient temperature.

For sampling, the sampler has a wide section 1 above the liquid 7 with a film in the tank 8 (Fig. 3).

Then the sampler is quickly lowered vertically down into the water with a film of oil and oil products 9 on the surface (Fig. 4). The immersion process must be carried out quickly so that the film does not have time to wet the inner surface of the sampler. At the same time, the film of oil and oil products located on the area S ₁ defined by the wide section 1 of the sampler begins to concentrate on the smaller area S _{2 of the} narrow section 2 of the sampler.

The immersion depth is controlled by external risks 3 applied on the outside of the narrow portion 2 of the sampler. When immersing the sampler, ensure that the liquid level in the inner narrow portion 2 of the sampler is in its upper third (Fig. 5).

The order of subsequent actions is determined by the solution of a specific task. If it is necessary to determine the thickness of the film of oil and oil products 9 on the surface of the water, then after immersion the sampler is slowly removed from the liquid until the layer of oil and oil products 10 in the sampler is higher than the level of the liquid with the film 9 in the test reservoir (Fig. 6). Then, using Fig. 3, the thickness of the Н ₂ layer of oil and oil products is measured in a narrow section 2 of the sampler. From the elementary equation for the equality of the volume of the film 9 in a wide area of the sampler and the layer of oil and oil products in a narrow area 2, determine the thickness of the film 9 in the studied reservoir:

H ₁ × S ₁ = H _{2 ×} S ₂ ,

Whence H ₁ = H _{2 ×} S ₂ / S ₁ ,

where H ₁ is the desired film thickness in a wide area of the sampler, which is equal to the film thickness in the studied reservoir;

N ₂ - the thickness of the layer of oil and oil products in a narrow section of the sampler (measured by risk);

S ₁ is the cross-sectional area of a wide portion of the sampler (calculated by the known diameter D ₁ );

S ₂ is the cross-sectional area of a narrow portion of the sampler (calculated by the known diameter D ₂ ).

If the problem of qualitative and quantitative determination of the content of oil and oil products on the surface of the water is solved, then after the completion of the collection of samples (Fig. 5), the sampler is slowly removed from the liquid (Fig. 7). In this case, the liquid inside the sampler begins to slowly be removed from its volume. This leads to the fact that the phase boundary inside the narrow section 2 of the sampler begins to slowly decrease. The rate of decrease in the interface is selected visually depending on the thickness of the layer of oil and oil products, i.e. when raising the sampler, oil and oil products should wet the inner surface of the narrow section. If the wetting is stopped, then it is necessary to reduce the lifting speed. The smaller the thickness of the layer of oil and oil products, the lower should be the speed of extraction of the sampler.

Further, there are two approaches for analyzing a film transferred onto the inner surface of a sampler.

The first approach is based on the washing off of organic matter from the inner surface of a narrow section 2 of the sampler.

After wetting the narrow section 2, the sampler is quickly removed from the water, the narrow section is closed with a lid 5. The sampler is turned so that the wide section is at the top, and the volume of solvent 12 is poured through it to remove the film 11 from the surface of the sampler 12. Then, the wide part is closed with the cover 4. and the sampler is shaken (Fig. 8). In this case, organic substances from the inner surface of the sampler pass into the solution. The volume of solvent used is determined by the internal volume of the narrow section 2 of the sampler and is significantly smaller compared to the prototype. The use of a smaller volume leads to an increase in the concentration of organic matter in the solvent. This improves the analytical characteristics of the proposed method and reduces the costs of further disposal of the solvent and allows to reduce its environmental impact.

Analysis of the solvent for the content of organic substances in it can be performed by standard methods of analytical chemistry, IR spectrometry, chromatography, chromatography and mass spectrometry, as well as oxythermography.

The second approach to the analysis of the film transferred to the inner surface of the sampler is based on the express method.

The method does not require any chemicals and therefore is environmentally friendly. When applying this method, it is necessary to first remove organic substances from the outside of the sampler that settle to the outer surface when the sampler is removed from water with a surface film of oil and oil products. To do this, a narrow section of the sampler with a cover 5 at the end is lowered into the water and shaking, incubated for several minutes (Fig. 9). This removes the film from the outside of the narrow portion 2 of the sampler. In the prototype method, this operation is not performed, as a result of which the organic substances remaining on the outer surface distort the values in the quantitative analysis. Next, remove the sampler from the liquid and remove the cover 5 from a narrow section 2.

The analysis of the film deposited on the inner surface of the narrow section 2 of the sampler is carried out by introducing a narrow section 2 into a high-temperature tubular reactor 13 heated to 1000 ° C, through which air coming from the open end of the reactor is pumped using a flow rate 17 (Fig. 10). At the end of the reactor there is a catalyst 15. The catalyst is located in the high temperature zone of the reactor. Using the temperature sensor 14, the temperature of the catalyst is monitored. At the outlet of the reactor behind the catalyst is an oxygen sensor 16, which continuously monitors the oxygen content in the stream of air leaving the reactor. When a narrow section 2 of a sampler with a film of organic matter located on the inner surface is introduced into a high-temperature reactor, the oxidation of organic substances by atmospheric oxygen occurs. The fullness of oxidation is achieved by the high temperature of the reactor and the use of a catalyst 15, on which the oxidation of organic matter molecules takes off from the inner surface during the heating of the sampler and does not have time to oxidize in it. This leads to a natural improvement in the accuracy of the analysis compared to the prototype.

Using the oxygen sensor 16, a decrease in the oxygen content in the air, i.e. the amount of oxygen that was used to oxidize the organic substances that make up the film. This value, called chemical oxygen demand (COD), is widely used to determine the total organic matter in water.

The invention allows to determine with increased accuracy the thickness of the film of oil and oil products on the surface of the water, creates the opportunity for accurate qualitative and quantitative determination of the content of oil and oil products on the surface of the water, allows to quantify the content of organic substances in the film by the express method by concentrating the sample during sampling from thin film into the layer of oil and oil products with visually observed thickness, expand the objects of study (thin films).

Claims (1)

A device for selecting films of oil and oil products from the surface of the water, containing a sampler made in the form of a hollow cylinder of inert material, on the outer surface of which risks are taken to measure the volume of the sample taken, and a cover of inert material, which can be installed on the cylinder end sampling from the surface of the water, characterized in that the cylinder of the sampler has a wide L ₁ and narrow L ₂ sections, while the lengths of the wide and narrow sections are selected from the condition L ₁ ≤3.5-5.5 L ₂ , and the diameters from the condition of D ₁ ≥ 2.5–4.5 D ₂ , the device additionally contains a cover that can be installed on the second end of the cylinder of the sampler, and the risks for measuring the volume of the sample taken are performed on the surface of a narrow section of the cylinder.

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