Method to examine samples of non-consolidated porous media

FIELD: measurement equipment.

SUBSTANCE: sample is previously frozen, a frozen sample under conditions of negative temperature is put in contact with a frozen solution of a radio-opaque agent, upon completion of sample saturation, computer X-ray microtomography of the sample is carried out under negative temperatures, and by means of analysis of the produced computer tomographic image they detect spatial distribution and concentration of ice and/or gas hydrate inclusions of open and closed porosity, distribution of pores by size, specific surface in the sample.

EFFECT: higher accuracy of assessment of characteristics of non-consolidated porous media.

10 cl, 1 dwg

 

The invention relates to the field of research samples of unconsolidated porous media and can be used to explore an open or closed porosity, distribution of pore size, specific surface area, spatial distribution and concentration of ice and/or gas hydrate inclusions in the pore space of the sample, determine the size of the inclusions, etc.

Most of the methods of investigation of properties of porous structures, in particular the petrophysical properties of rocks, designed for consolidated materials (Vamjobine, Boundaryscan, Daugavpils, Petrophysics (physics of rocks), M: "Oil and gas state oil and gas University. University, 2004. - 368 S. ISBN 5-7246-0295-4; Beep NS, Bogdanovich, N., Martynov, V.G. Determination of physical properties Neftegazgeodeziya breeds, M.: OOO "Nedra-Center", 2007. - 592 S. ISBN 978-5-8365-0298-0). To study weakly cemented rocks requires special equipment and modification of the known methods, so that during the measurements was kept the structure of the pore space and sample volume (US Pat. 4587857, the Method for mounting poorly consolidated core samples). It is often necessary impregnation of the samples with a special solution, which, freezing, cement pore space, however, may be in breach of the original structure and properties change (US Pat. 3941191, Mehod of consolidating unconsolidated or insufficiently consolidated formations). Known and research methods, providing preliminary low-temperature freezing samples of unconsolidated porous media (see, for example, O.Torsaeter, The effect of freezing of slightly consolidated cores, SPE Formation Evaluation, 1987, v.2, N3, p.357-360). Further studies of macro-and microfabrics of organic skeleton frozen samples of unconsolidated porous media subjected to vacuum sublimation. However, it lost the information about the pore fluids, in addition, freeze-dried samples of unconsolidated media can warp and crack, leading to inaccuracies characteristics of the pore space.

For identification of organic and mineral skeleton of the pore space and frozen pore fluids (ice formations, gas hydrates), a method of improving the contrast that allows you to estimate characteristics of a porous material and evaluation of the spatial distribution and concentration of ice and/or gas hydrates in the pore space by analyzing x-ray images.

In accordance with the claimed method research designs unconsolidated sediment sample pre-frozen, in conditions of negative temperatures are put in contact with the frozen solution radiopaque agent, at the end of the feast upon the Deposit of a sample carried out x-ray computer microtomography imaging of the sample at low temperatures and determine petrophysical characteristics and spatial distribution, the concentration of ice and/or gas hydrate inclusions by computer analysis of the obtained tomographic image.

As a radiopaque agent used is a water-soluble compound, which includes a chemical element that has a high degree of attenuation of x-rays.

As a chemical element that has the ability to attenuate x-ray radiation, use an element with a large atomic weight, and a water-soluble compound is a salt or oxide.

As element with a large atomic weight can be used heavy metal from the group of Pb, Ba, Sr, Ra, etc.

Contact of the sample with a frozen solution of radiopaque agent is carried out at a temperature below the phase transition temperature of the ice-water, that is, melting of ice in the sample, preferably from -7°C to -10°C.

Pre-analyzed sample permafrost and frozen solution x-ray contrast agent can be maintained at a temperature of -7°C to -10°C to stabilize the temperature of the sample.

Computerized x-ray microtomography imaging of the sample is carried out in the condition of negative temperature, in order to avoid melting of the ice/hydrate in the pore space, preferably at a temperature of -7°C to -10°C.

The invention is illustrated by figure 1, where is shown a portion of an image of a 2-d slice of the 3-dimensional digital models reconsolidating river sand, cemented by ice. The image obtained through the experiment by x-ray microtomography carried out at a temperature of -10°C. This image obtained with the use of radiopaque agent.

The method is based on x-ray microtomography is the reconstruction of the spatial distribution of the linear attenuation coefficient (LCO) x-ray radiation in a thin layer on the sample by means of computer processing of the projection of x-rays in various directions along the investigated layer.

The value of LCO each material depends on the chemical composition, the density of matter and radiation:

µ=µmρ,

µmmass attenuation coefficient under the influence of x-ray radiation (cm2/g), ρ is the density (g/cm3).

The claimed invention is based on the effect of ion diffusion of water-soluble compounds of the elements with the ability to attenuate x-ray radiation (for example, salts of heavy metals), solid phase ice/hydrate in the pore space of rocks at low temperatures, which provides improved contrast when conducting x-ray microtomography at low (negative) temperature of ice/hydrate.

Suitable radiopaque agents are water-soluble compounds, the content is the following elements with high atomic number, for example, salts of heavy metals (Pb, Ba, Sr, Ra, and etc). As heavy metal chosen soluble salt in accordance with the table of solubility of inorganic substances in water. Such salts can be: Pb(NO3)2, BaCl2and other

In the example implementation of the invention to enhance x-ray contrast ice/hydrate in the pore space of the rock was used frozen 1% solution of Pb(NO3)2as a source of lead ions for diffusion in the solid phase of ice/hydrate at low temperatures.

Saturation of ice salt of the metal leads, for example, the temperature of the phase transition of ice-water, which in turn can lead to melting of the sample at temperatures below 0°C (the phase transition of ice-water for distilled water at normal pressure). On the other hand, when the temperature decreases, the speed of difusiy ions in the sample slows down, which leads to an increase in contact time for saturation of the sample ions. In General, the temperature during contact of the sample with frozen solution should be less than the phase transition temperature of the ice-water or hydrate/water in the sample.

Sample unconsolidated porous medium and prepared with 1% solution of Pb(NO3)2frozen at -15°C to -20°C, then frozen solution and frozen fo the EC is transferred into the cooling chamber with a temperature of about -7°C, where they are maintained until temperature stabilization. After that, the sample set on the frozen solution, i.e. they perform their direct contact. The sample in contact with the frozen solution is maintained at isothermal conditions (constant temperature of about -7°C) for 7 days. During this period of diffusion saturation of the sample frozen rock heavy metal ions. After saturation of the contact of the sample with frozen solution should be cleaned and the sample is ready for scanning in the x-ray tomograph at low temperatures.

Survey the sample using a low-temperature attachment (Cooling stage, http://www.skyscan.be/products/stages.htm) on x-ray micro. The sample was scanned at a temperature of about -10°C to avoid melting of the ice.

The result of scanning is a 3-dimensional digital model of the core, the analysis of which allows to determine the petrophysical characteristics of the unconsolidated rocks, and distribution of ice/hydrate in the pore space, etc.

1. The method of examination of samples of unconsolidated porous media, in accordance with which the sample is pre-frozen, the frozen sample in conditions of negative temperatures are put in contact with the frozen solution radiopaque agent, okoncane the saturation of the sample hold x-ray computer microtomography imaging of the sample at low temperatures and by analyzing the obtained CT images to determine the spatial distribution of and the concentration of ice and/or gas hydrate inclusions, open and closed porosity, pore size, specific surface area in the sample.

2. The method according to claim 1, in which the contrast agent used is a water-soluble compound, which includes a chemical element with high x-ray attenuation.

3. The method according to claim 2, in which the chemical element that has a high degree of attenuation of x-rays, use an element with a large atomic weight, and a water-soluble compound is a salt or oxide.

4. The method according to claim 3, in which the element with a large atomic weight use of heavy metal from the group of Pb, Ba, Sr, Ra, etc.

5. The method according to claim 1, in which the contact of the frozen sample unconsolidated porous media with frozen solution radiopaque agent is carried out at a temperature below the melting ice/hydrate in the pore space of the sample.

6. The method according to claim 5, in which the contact of the frozen sample unconsolidated porous media with frozen solution radiopaque agent is carried out at a temperature from -7°C to -10°C.

7. The method according to claim 1, in which a sample of unconsolidated porous media frozen and the frozen solution roentgenocontrast what about the agent previously maintained at a temperature below the melting ice/hydrate in the pore space of the sample to stabilize the temperature.

8. The method according to claim 7, in which a sample of unconsolidated porous media frozen, and the frozen solution radiopaque agent is pre-incubated at temperatures ranging from -7°C to -10°C.

9. The method according to claim 1, in which x-ray computer microtomography imaging of the sample is carried out at a temperature below the melting ice/hydrate in the pore space of the sample.

10. The method according to claim 9, in accordance with which the x-ray computer microtomography imaging of the sample is carried out at temperatures ranging from -7°C to -10°C.



 

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1 ex

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