Method for determining disappearance point of oil product crystals and apparatus for performing the same

FIELD: measuring technique.

SUBSTANCE: method comprises steps of introducing analyzed sample in measuring cell 4 placed into cryostat-provided chamber 1; turning on laser irradiator 6 and corresponding to it optical detector 7 for passing optical beam through analyzed sample; storing intensity values of light received by optical detector 7; gradually lowering temperature in chamber 1 and then again increasing it for registering curve showing change of intensity values of light received by detector 7 as temperature function. According to registered curve crystal disappearance point is determined.

EFFECT: enhanced accuracy and reliability of measurement results.

7 cl, 4 dwg

 

The technical field

The present invention relates to a method of determining a vanishing point of the crystals of petroleum products, including aviation fuel, in the temperature range from -5 to -120°C.

Prior art

The vanishing point of the crystals is defined as the temperature of disappearance of the last of the crystals in the pre-crystallized sample with a gradual increase in temperature.

There are various standards that define the conditions determining the vanishing point of the crystals; this point is of particular interest to specialists in the field of aviation, as it allows you to define the time during which the aircraft can remain at a given high altitude without the risk of driving fuel lines and filters.

In addition, the temperature of disappearance of the crystals allows you to know whether kerosene clean or contaminated with oil (diesel fuel).

Currently on sale are a variety of instruments to determine the vanishing point of the crystals in the samples of oil.

As an example, you can specify the devices firm ISL under the names FZP 5 Gs and FZP 5 G, which are fully automated devices operating on the basis of ASTM D 2386, IP 468 and ISO 3013.

The principle of operation of these devices is the Ohm, the light beam emitted by the diode is passed through the measuring cell containing the analyzed sample, which is placed in cryostation camera, equipped with a temperature sensor connected to the cooling system and temperature control, and measure the light power, adopted by the optical receiver, in line with the infrared emitter for measuring cell containing the analyzed samples.

When the test temperature christineromans camera gradually reduced until such time as the optical detector ceases to detect light, which means that the sample is fully crystallized, and then the temperature is again gradually increased, recording a curve showing the change of light power, adopted by the optical receiver, as a function of temperature.

When the sample disappear crystals on the curve see curve, corresponding to the vanishing point of the crystals, followed by a plot of a constant temperature.

The device has the advantage - it is compact and automatic allows you to get fully reproducible results regardless of the skill of the operator.

The drawback of the device is that its sensitivity in certain cases, it may be insufficient, in particular when we want to determine the point icesn the disappearance of crystals kerosene, contaminated with a small amount of oil.

Indeed, in the presence of oil, the vanishing point of the crystals in the sample of kerosene increases significantly. In the case of a sample containing several % of gasoil, the curve showing changes in the intensity of light received by the optical detector, as a function of temperature has a fairly distinct inflection to determine the vanishing point of the crystals and, consequently, the share of oil, in comparison with the vanishing point of the crystals of pure kerosene.

On the contrary, in the case of a small contamination of the oil curve is brief and no longer gives a clear inflection, so it is impossible to determine the vanishing point of the crystals.

Another device designed to determine the vanishing point of the crystals described in patent US 5088833.

The specified device operates according to the standard ASTM D 5972. To measure placed analyzed microabrasion product in the Cup, the inside of which is formed by a mirror, cooled by Peltier elements, and gradually cooling the sample to its crystallization, and then again gradually heated.

During the test, analyze the sample light beam of light, and the angle of incidence is chosen so that the light reflected by the mirror, did not reach the optical detector located above it.

When present in the sample crystal is, they scatter light randomly and part of this light will be accepted by the optical detector.

Therefore, the appearance and disappearance of the crystals can be detected by analyzing the signal received by the optical detector, which is zero in the absence of crystals increases with the appearance of crystals in the sample.

The sensitivity is sufficient to detect a very small quantity of oil in kerosene. However, the use of the device is uncomfortable, and the results largely depend on the skill of the operator.

A brief statement of the substance of the invention

The present invention is to provide a method for determining the point of disappearance of the crystals of petroleum products, including aviation fuel, is able to eliminate these drawbacks.

The problem is solved according to the invention by creating a method of determining the point of disappearance of the crystals of petroleum products, in which

set the laser emitter and the longitudinal optical receiver, on either side of the tubular measuring cell installed almost horizontally placed in cryostation camera, equipped with a temperature sensor connected to the cooling system and temperature control so that the optical beam from the laser izluchatelei on the longitudinal axis of the measuring cell and the longitudinal optical receiver

connect the temperature sensor, the cooling system and temperature control, as well as the longitudinal optical receiver with programmable means for determining and displaying,

directly behind the laser emitter set the aperture to the optical beam from the laser emitter was thin enough to completely eliminate the reflection from the walls of the measuring cell,

before the longitudinal optical receiver set the polarizer is adjusted so as not to miss the optical beam from the laser emitter,

enter the analyzed sample in the measuring cell,

include a laser emitter and the longitudinal optical receiver and transmit the optical beam through the analyzed sample, write light power, received the longitudinal optical receiver

gradually reduce the temperature christineromans camera up to the end temperature of crystallization of the analyzed sample (cloud point), and then gradually increase the temperature of this camera, record a curve showing the change of light intensity received the longitudinal optical receiver, as a function of the temperature curve detection, and

determine the vanishing point of the crystals on the specified curve.

Thus, this method is fundamentally different use of the polarized beam the data light to the longitudinal optical receiver did not receive light in the absence of crystals. On the contrary, when the appearance of crystals in the analyzed sample a certain amount of light detected by the receiver. Specialists are well aware that the crystals change the polarization direction of the light.

This method cannot work in the absence of full reflection from the walls of the measuring cell; therefore, if the state of the surface of the cell does not reflect light, it is necessary that the cross section of the beam passing through it, was sufficiently reduced aperture.

According to the invention, was able to establish that the diameter of the aperture should preferably be from 1 to 1.5 mm, since the diameter of 1 mm may face the risk of diffraction.

In addition, for optimum receiver sensitivity wavelength of the laser beam should be about 650 nanometers.

Preferably in the immediate vicinity of the measuring cell, in its front part, set side optical receiver for receiving the optical beam from the laser oscillator, and programmable means of payment and means of programmable display.

On the side of the optical receiver no light comes through in the absence of crystals, as the analyzed sample in this case are completely transparent, but p is the disposal of the scattered light with the appearance of crystals in the sample.

During the test recording is also a curve showing change of the light power received side optical receiver, as a function of temperature, or the curve of turbidity and using this curve, determine the temperature of the end of the crystallization of the analyzed sample, or point cloud, i.e. the temperature at which the direction of change of temperature should be changed to the opposite.

Therefore, the function side of the optical receiver is to manage the process.

More precisely, at the beginning of testing on both detector light is not received.

Upon cooling, the first crystals appear, which change the polarization of the light from the laser emitter, and a certain amount of light may also pass through the polarizer and to achieve the longitudinal optical receiver.

When the number of crystals within the analyzed sample becomes significant, it becomes cloudy, causing scattering of light, part of which comes to transverse optical receiver.

When the clouding becomes very strong, the light beam from the laser emitter can no longer reach the polarizer, and therefore, the power of light detected by the longitudinal optical receiver decreases.

The point cloud is achieved when the power of light detected by the lateral optical receiver, HC is incremented, while the power of the light detected by the longitudinal optical receiver decreases.

When reached the point of turbidity, gradually increase the temperature of the cryostat chamber to determine the value of the vanishing point of the crystals of the sample on the curve detection.

While increasing the power of the light detected by the optical receiver increases, starting from the moment when the sample becomes sufficiently transparent to the light beam from the laser emitter can reach the polarizer, and then decreases again, disappear when the last of the crystals.

The point from which the longitudinal optical receiver no longer detects light, matches the vanishing point of the crystals.

According to the second aspect of the present invention relates to a device for implementing this method.

According to the invention, the device is characterized in that it contains:

cryostation camera, equipped with a temperature sensor connected to the cooling system and temperature control,

the measuring tube is U-shaped, set in christineromans the camera, the Central part of the tube, almost horizontal, forms a measuring cell, and the side parts allow you to enter the analyzed sample in the cell and out of the cell

laser emitter and svyazannyis him longitudinal optical receiver, installed one on each side of the measuring cell along its longitudinal axis,

the diaphragm is installed directly behind the laser emitter,

a polarizer mounted in front of the longitudinal optical receiver

programmable means of calculation and display, connected to the temperature sensor, cooling system and temperature control, as well as with the longitudinal optical receiver.

The above structure of the device, the only operations that must be performed manually in order to perform testing, consist in the introduction of the analyzed sample in the measuring cell with a syringe and the inclusion of a laser emitter and its corresponding longitudinal optical receiver, and a cooling system and temperature control.

Then testing is carried out automatically under the control of the means of calculation and display, pre-programmed depending on the observed standard, which control the cooling system and temperature control depending on the information that they gave the temperature sensor, and install at the same time curve detection, depending on the information passed on to them the longitudinal optical receiver.

Preferably, the device comprises a lateral optical receiver mounted in nepo is rodstvennoi vicinity of the measuring cell at its front end and connected to the programmable means of calculation and display.

In accordance with this feature, programmable means for determining and displaying determine the curve of turbidity based on the information that is conveyed to them side by the optical receiver, and use this curve to automatically control the cooling system and temperature control and, therefore, temperature changes christineromans the camera.

According to the invention, the light is passed to the optical receiver through the optical fibers, preferably installed together with lenses for concentrating optical radiation.

Lenses may be formed of glass balls with a diameter of 5 to 8 mm, is placed on the optical axis.

As the fibers used in the fiber located in the focal plane of the lens.

The measuring tube is made in the form of a metallic element, in particular of aluminium, provided with Windows through which the detected optical beam.

It is important that these Windows are usually made of glass, had absolutely parallel to the surface.

According to the invention, the cooling system and temperature control can be performed in the form of a cooling unit, in particular, acting on the Stirling cycle, the cold piston which is fitted on the free end of the heat transfer system dry contact, working together with cryostation is authorized by the camera, in order to carry out cooling to the desired temperature.

Device for analysis of a sample of oil containing the installation of the cooling cycle Stirling, described in the document FR 2801381.

Application installation cooling cycle Stirling allows you to get the design of the device in a compact portable device.

Brief description of drawings

Characteristics of the method and device according to the invention will be described in more detail with reference to the attached drawings, on which:

Figure 1 depicts a diagram of an apparatus for determining the point of disappearance of the crystals of petroleum products, according to the invention;

2, 3, 4 diagrams obtained programmable means for determining and displaying respectively, for the sample of pure kerosene, sample weakly contaminated kerosene and sample heavily contaminated kerosene, according to the invention.

Description of the preferred embodiment variants of the invention

Device for determining the point of disappearance of the crystals oil contains cryostation the camera 1 (Fig 1), is equipped with a sensor 2 temperature and installation of cooling and temperature control, operating on the Stirling cycle (not shown).

In christineromans camera 1 is placed a metal measuring tube 3, U-shaped, horizontal centre is supplemented flax part 4 which represents the measuring cell, which is placed in the analyzed sample.

The side parts 5 and 5' of the measuring tube 3 are for input of the sample and its output.

The device also contains a laser diode 6, which is placed opposite longitudinal optical receiver 7, so that the emitted beam 8 of the laser radiation passed through the same line with the longitudinal axis of the measuring cell 4 and through the analyzed sample is introduced into the cell.

Before the longitudinal optical receiver 7 in the direction of propagation of the laser beam from the diode 6 has a polarizer 9.

The polarizer 9 is configured so that the longitudinal optical receiver 7 has not received the light, when the sample contained in the measuring cell 4, transparent and does not contain crystals.

Glass window 10, 10', having absolutely parallel to the surface, allow the laser beam 8 passing through the measuring cell 4 and reach the longitudinal optical receiver 7, ensuring the integrity of the cell.

Auxiliary polarizer 11, crossed with the polarizer 9 and mounted directly behind the laser diode 6, performs the function of attenuating the amplitude of the beam emitted by this diode.

Auxiliary polarizer 11 operates together with the diaphragm 12 that is installed directly behind him, so that the laser beam passing through the measuring cell 4 was to the rather thin, to completely eliminate the reflection on the walls of this cell.

The device also includes a lateral optical receiver mounted near the measuring cell 4 at its front.

Glass window 10', similar to the Windows 10 and 10', allows the beam, scattered in front of the measuring cell 4, walk to the side of the optical receiver 13.

Before reaching the receivers 7, 13 polarized light from the polarizer 9 and the scattered light coming from the window 10", focus on the light guides 15, 15' lenses 14, 14', respectively.

Install cooling, sensor 2 temperature and longitudinal optical receiver 7 and the lateral optical receiver 13 is connected to a programmable means of calculation and display (not shown)that control the process in accordance with the specified standard.

Programmable means for determining and displaying control the installation of cooling christineromans camera 1 depending on the information that was passed on from sensor 2 temperature and receivers 7, 13, and simultaneously determine the curve detection, showing changes in light intensity, adopted by the longitudinal optical receiver 7, and the curve of turbidity, showing changes in light intensity received side optical receiver 13.

Figure 3, 4, 5 presents three graphs corresponding to three different samples of ke is aspen, where the abscissa axis represents time expressed in minutes and the ordinate axis pending the strength of the light received by the receiver, expressed in relative scale from 0 to 100, and the temperature of the sample, expressed as °C, left scale right scale, respectively.

The dotted curves show the temperature change of the sample as a function of time (right scale).

The dashed lines correspond to the change of turbidity and show changes of light intensity in time, the received receiver side (left scale).

Solid lines correspond to detect and show the changes of light intensity with time, obtained by a longitudinal receiver (right scale).

The analysis of the three diagrams allows to determine the point cloud point, i.e. the temperature at which the direction of change of temperature in christineromans the camera should change to the opposite.

Solid curves allow us to determine the desired point of disappearance of the crystals.

In the case of pure kerosene without impurities (Figure 2) the appearance of the first crystals were observed after 7 minutes 30 seconds, or at a temperature of -59°C.

The point cloud was detected at temperatures very close to -60°C.

The vanishing point of the crystals was detected in 11 minutes, or at a temperature of -54°C.

In the case of kerosene with a low content of impurities (Figure 3) paaul is the first of crystals was observed after 6 minutes 30 seconds or at a temperature of -45°C, and the point of turbidity after 7 minutes 45 seconds, or at a temperature of -60°C.

The disappearance of turbidity in the sample, it was noted in 11 minutes 30 seconds, or at a temperature of -55°C, and the point of disappearance of the crystals in 13 minutes 30 seconds, or when the temperature -38,7°C.

"Leap"is marked on the curve of discovery about 12 minutes associated with physical phenomena inside the sample.

In the case of heavily contaminated kerosene (Figure 4), the vanishing point of the crystals was observed after 14 minutes 30 seconds, or when the temperature -27,5°C.

1. The method of determining the point of disappearance of the crystals of petroleum products, including aviation fuel, in the temperature range from -5 to -120°C, characterized in that

set the laser emitter (6) and longitudinal optical receiver (7) on either side almost horizontal tubular measuring cell (4), placed in cryostation chamber (1)equipped with a sensor (2) temperature, connected to the cooling system and temperature control so that the optical beam from the laser emitter (6) was in line with the longitudinal axis of the measuring cell (4) and longitudinal optical receiver (7), connect the sensor (2) temperature with cooling system and temperature control, and also connect the longitudinal optical receiver is (7) programmable means for determining and displaying,

set the aperture (12) directly behind the laser emitter (6)to the optical beam (8) from the laser emitter was thin enough to completely eliminate the reflection from the walls of the measuring cell (4),

set before the longitudinal optical receiver (7) polarizer (9)that is configured so as not to miss the right optical beam from the laser emitter (6),

set in the immediate vicinity of the measuring cell (4) at its front end side of the optical receiver (13) for receiving the optical beam (8) from the laser emitter (6) and connected to the programmable means for determining and displaying,

enter the analyzed sample in the measuring cell (4),

include a laser emitter (6), longitudinal optical receiver (7) and the lateral optical receiver (13) and transmit the optical beam through the analyzed sample,

gradually reduce the temperature kristalicheskie camera (1), write the curve representing the change of light power, received the longitudinal optical receiver (7), as a function of temperature representing the curve detection, and a curve showing the change of light intensity taken side optical receiver (13), as a function of temperature, which represents the curve of turbidity, and is determined by the curve of turbidity is the temperature of the end of the crystallization of the analyzed sample - the point cloud, from which again gradually increase the temperature of the chamber (1), and write the curve detection and curve opacity

determine the vanishing point of the crystals along the curve detection.

2. The device for implementing the method of determining the point of disappearance of the crystals of oil products according to claim 1, characterized in that it contains

tristatecheckbox chamber (1)equipped with a sensor (2) temperature, connected to a cooling system and temperature control,

the measuring tube (3) U-shaped, set in kristalicheskie chamber (1), the Central part of the tube, almost horizontal, forms a measuring cell (4)and side parts (5, 5') provide input for the analyzed sample in the cell, and the output of the cell

laser emitter (6) and the associated longitudinal optical receiver (7)installed on either side of the measuring cell (4) along its longitudinal axis,

the aperture (12), installed directly behind the laser emitter (6),

the polarizer (9), mounted in front of the longitudinal optical receiver (7),

programmable means of calculation and display, connected to the sensor (2) temperature, cooling system and temperature control, as well as with the longitudinal optical receiver (7),

Bo the OIC optical receiver (13), installed close to the measuring cell (4) at its front end connected to the programmable means of calculation and display.

3. The device according to claim 2, characterized in that it contains an intermediate fibers (15, 15') for transmitting light to an optical(s) receiver(s) (7, 13).

4. The device according to claim 3, characterized in that the light guides (15, 15') is merged with the lenses (14, 14') for concentrating optical beam (8).

5. The device according to claim 4, characterized in that the measuring tube (3) made in the form of a metallic element, in particular of aluminium, provided with Windows (10, 10', 10") for the passage of the detected optical beam (8).

6. Device according to any one of claim 2 to 5, characterized in that the cooling system and the temperature adjustment is made in the form of cooling unit operating on the Stirling cycle, the cold piston which is fitted on the free end of the heat transfer system dry contact operating in conjunction with kristalicheskie camera (1) for cooling to the desired temperature.

7. The device according to claim 6, characterized in that it is a compact and portable device.



 

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7 cl, 4 dwg

FIELD: oil industry.

SUBSTANCE: device comprises standard tank (1) transparent for visible and microwave radiation, microwave chamber (2) made of a rectangular hollow parallelepiped, source of microwave radiation (3), illuminator (4), TV camera (5), two solenoid-operated valves (6) and (7), weight pickup (8), measuring converter (9), electronic commutator (10), analogue-digital converter (11), interface (12), and computer (13). The walls of microwave chamber (2) are provided with holes (18)-(23) for introducing and recording the radiation from microwave source (3) and for filling and empting tank (1) with the crude oil. Standard tank (1) is formed by two straight hollow cylinders of different diameters. Illuminator (4) is made of a cylindrical luminescence arc-discharge lamp mounted inside the cylinder of smaller diameter so that the cylinder and standard tank are axially aligned. The cylinder is secured from outer side of bottom (17) and top (16) walls of microwave chamber (2). Solenoid-operated valves (6) and (7) are locked.

EFFECT: enhanced precision.

6 dwg

FIELD: creation of machine models, at output of which calculated data is received about properties of fluids contained in oil and gas bearing collector beds.

SUBSTANCE: method and device are used for transformation of data of pressure gradient, formation pressure and formation temperature, measured by logging device on cable, to evaluation data of PVT-properties of hydrocarbon fluid, which do not depend on presence of drill mud on hydrocarbon base, without necessary taking of physical fluid samples from the well for laboratory analysis on the surface.

EFFECT: increased statistical precision of PVT-properties of formation fluids.

5 cl, 9 dwg

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