RU2522207C2 - Device for determination of oil products quality - Google Patents

Abstract

FIELD: oil and gas industry.

SUBSTANCE: invention is related to the field of analysis of physical properties of liquids. A device contains a container for sampling with a scale with a piston and rod placed in it, software and hardware to measure time and temperature, a tube for liquid intake during sampling in order to determine the relative viscosity, a thermistor which can be installed at the tube during determination of microcone penetration, demulsifying ability and index of the liquid heating dynamics, a cone that can be installed instead of the piston on the rod by means of a threaded connection for determination of microcone penetration, a plug or a cover which can be installed into the container nipple instead of the tube for determination of microcone penetration and demulsifying ability, and a support for the container installation.

EFFECT: simplification and acceleration of the analysis as well as increase in its information content and reliability.

5 cl, 4 tbl, 10 dwg

Description

The invention relates to the field of analysis of the physical properties of liquids. The invention allows to determine various indicators of fluid quality, including conditional viscosity, micropenetration, demulsifying ability and indicators of the dynamics of heating and cooling of the liquid. It can be used for express analysis of fuel and lubricants in machines; for research purposes; for qualification tests in any areas. The device is a 20 ml capacity with a piston and tube. The selection of the product can be made from any containers and tanks, including from the crankcase of the engine or gearbox, the fuel tank of the car.

EFFECT: reduction of time for analysis, reduction of the number of preparatory operations, reduction of environmental pollution, increase in the number of determined quality indicators.

The invention can be used in oil refining, petrochemical, chemical, food, medical, pharmacological and other industries, in which it is required to control the quality of low and high viscosity liquids, including liquid and semi-liquid lubricants, pastes, suspensions, etc.

A known method for determining the viscosity of oil bitumen (GOST 6258-85. Petroleum products. The method for determining the viscosity). The essence of the method consists in measuring the time during which a certain amount of oil flows through a calibrated hole of a VU type viscometer according to GOST 1532-81 at a given temperature, and comparing this time with the time when the same amount of water expires from a given viscometer at 20 ° C. The disadvantage of this method is the high temperature of heating the oil product (100 ° C) and the need for preliminary tests with water.

Also known is a method for determining the conditional viscosity of petroleum bitumen (GOST 11503-74. Petroleum bitumen. Method for determining the conditional viscosity). The essence of the method is to measure the time during which a certain amount of bitumen flows through a calibrated bore of the apparatus cylinder at a given temperature. The disadvantage of this method is the need to heat to a high temperature when determining the viscosity of highly viscous liquids.

A known method for determining penetration (GOST 5346-78. Lubricants plastic. Methods for determining penetration by a penetrometer with a cone). The essence of the method is to determine the immersion depth of a standard cone in the test lubricant for 5 s at 25 ° C with a total load of 150 g, expressed as an integer of tenths of a millimeter on the penetrometer scale. The disadvantage of this method is the need for preliminary sampling and sample preparation operations.

A known method of determining micropenetration according to TU 0254-010-86136683-2009 for gear lubricants "STP". The essence of the method is to determine the immersion depth of a cone with a plunger (total weight 9.38 g) in 5 s, expressed as an integer of tenths of a millimeter on the penetrometer scale. The disadvantage of this method is the need for preliminary sampling and sample preparation operations, as well as the need for special equipment.

A known method for determining the demulsifying properties of liquids (ASTM D1401-10. The standard method for determining the rate of separation of water from petroleum oils and synthetic fluids). The essence of the method is that 40 ml of the product is heated to 54 ° C (or 82 ° C), 40 ml of water are added and stirred for 5 minutes at a speed of 1500 rpm, after which the ratio of the volumes of the pure product is recorded at certain intervals emulsions and pure water.

The prototype in terms of technical nature and the achieved result is a method and device for determining the performance and quality of lubricants (RF Patent No. 2392607, G01N 11/02, 06/20/2010). The essence of the invention lies in the fact that with the help of a diagnostic device, the performance of a lubricant is determined by a generalized indicator obtained on the basis of viscosity, density, electric capacity, corrosion activity, and the content of wear particles. The disadvantage of the prototype is the inability to determine micropenetration and demulsifying ability of the liquid.

The purpose of the invention is the simplification of the operations for determining the conditional viscosity, micropenetration and demulsifying ability of a liquid, reducing the test time, creating the possibility of determining the conditional viscosity of oil products in the field at any temperature, creating the possibility of determining the dynamics of the heating fluid.

The device (see figure 1, 2) consists of:

- capacity 1;

- rod with piston 2;

- springs 3;

- tubes 4;

- hardware and software complex 5;

- thermistor 6;

- covers 7;

- coasters 8;

- cone 9.

The measurement is as follows:

1) Determination of conditional viscosity at the location of the oil product (figure 1).

Compress the spring 3 completely, lowering the rod 2, then immerse the end of the tube 4 in the analyzed liquid and release the spring. Due to the vacuum created, the liquid begins to flow through the tube 4 into the container 1. After filling 20 cm ³ , the temperature T and the filling time t are displayed on the display of the hardware-software complex 5. The filling time of 20 cm ³ is an indicator of the nominal viscosity of the oil at the test temperature: WU _T = t. The diameter of the tube 4 is selected depending on the viscosity of the product and the required accuracy for determining the viscosity. For example, for a relatively low-viscosity SAE 5W-40 oil, it is advisable to use a tube with an inner diameter of 1.5 mm, for STP-3 grease - 2 mm, for high-viscosity grease OSp-L - 3 mm. For ease of sampling, a holder can be used to install the device on barrels and other containers, including a plate with a hole and a screw (Fig. 4), or a pendant mount with tape and hook mounted on the hood lid, in case of sampling from the crankcase car (figure 5). Using rarefaction instead of gravity makes it possible to determine the viscosity of even highly viscous products at low temperatures. To translate the viscosity values obtained on the device into standard units for the analyte, a graph of the viscosity-temperature dependence and the conversion coefficient should be used. The conversion factor is the ratio of the viscosity of the product in standard units of measurement to the relative viscosity obtained using the device (at the same temperature). The graph of the viscosity-temperature dependence is built once for a specific product (conduct several measurements at different temperatures), an example of the graph is shown in Fig.6.

2) Determination of micropenetration (figure 2).

After sampling using rod 2, squeeze the liquid to a level of 7 ... 12 cm ³ , remove the tube 4 with a thermistor 6 and the hardware-software complex 5 and install the cover 7 on the nozzle of the container 1. Install the container on the stand 8, remove the rod from the container, cool sample to the required temperature (if necessary). Install the cone 9 instead of the rubber seal on the stem 2 (by screwing a threaded rod extending from the base of the cone into the hole on the stem). The weight of the stem with the cone should be 9.38 ± 0.025 g. Then the measuring cone 9 is lowered so that its tip touches the surface of the test product. The position of the base of the cone 9 relative to the scale on the tank 1 determines the initial position of the cone. The cone is released, under the influence of gravity it is introduced into the test product. The scale determines the final position of the cone. The difference in values before and after immersion of the micropenetrometer is an indicator of micropenetration for this product.

3) Determination of demulsifying ability (figure 3).

After sampling, using rod 2, squeeze the liquid to a level of 10 cm ³ , remove the tube 4 with a thermistor 6 and the hardware and software complex 5, draw 10 cm ^{3 of} water using the rod and tightly install the lid 7 on the nozzle of the container 1. Mix at room temperature shaking for 5 minutes. Set the capacity on the stand 8 and start the stopwatch. Every 5 minutes for an hour, the volumes of pure oil, pure water and emulsion are recorded.

4) Determination of the dynamics of the heating fluid. The determination of the indicator of the dynamics of heating consists in measuring the time during which the liquid heats up to a certain temperature. The end of the tube 4 with a thermistor 6 is immersed in the analyzed liquid, then the liquid is heated. On the display of the firmware 5 control the time and temperature. The time and temperature are periodically recorded (for example, every 5 ° C), a curve is constructed from the results obtained (examples of heating curves are shown in Fig. 8). The time of temperature change in a certain range is an indicator of the dynamics of heating the liquid. The determination of the dynamics of heating can be carried out, for example, for oil in the crankcase with the aim of establishing the presence of impurities (water, soot, etc.). In this case, the engine warm-up time, for example, from 30 to 90 ° C, as well as the shape of the heating curve, will be different for pure oil and oil mixed with water. To simplify the comparison of measurement results, the determination of the heating dynamics should be carried out under the same conditions. Similarly, you can determine the dynamics of fluid cooling dynamics.

Also, the device can be equipped with a probe, including a plastic tube, magnet and wire, to determine the content of magnetized wear products (Fig.9). The dipstick eliminates the influence of corrosion particles that may be present in the oil probe channel when determining the content of magnetized wear products in oil filled in ICE. For analysis using a wire, set the magnet in position I, lower the dipstick along the channel for the oil dipstick, after the probe has left the channel, but has not yet reached the oil, the magnet is transferred to position II. As a result of this, products scraped from the channel walls will remain behind the limiter. Then the end of the dipstick is immersed in oil for a certain time, after which the magnet is returned to position I and the dipstick is removed. The content of magnetizable wear particles in the oil is characterized by the number of particles on the magnet. Particles collected in the oil probe channel will be on the outside of the plastic tube.

To eliminate the risk of the rod leaving the tank and reduce the error in measuring the nominal viscosity (due to the stabilization of the created vacuum), a clamp consisting of two parts — a plate and a wire — can be used (Fig. 10). The retainer plate is a circle with a cutout for the stem leg and is installed between the container and the spring. One end of the retainer wire is fixed to the end of the rod, the other remains free. Before compressing the spring, the retainer wire is bent to position I, so that when the spring is compressed, it passes into the gap between the rod and the retainer plate. After this, the spring is compressed, the end of the tube is lowered into the test fluid, and the rod is released. The spring will unclench, the rod will return to its original position, under the action of the elastic force, the retainer wire will take position II (if the spring elastic force is not enough to return the rod to its original position, the rod is pulled manually). The retainer plate prevents the rod from exiting the tank under the action of the spring, the retainer wire fixes the rod in the extreme position, which allows to achieve a constant volume and, therefore, created in the vacuum tank.

Enumeration of figures. Figure 1 presents the appearance of the device when determining the conditional viscosity. Figure 2 shows the process of determining micropenetration using a special cone. Figure 3 shows the process of determining the demulsifying ability of a liquid. Figure 4 shows the holder for installing the device on barrels and other containers. Figure 5 shows the tape for hanging the device to the bonnet when sampling from the crankcase. Figure 6 shows a graph of the conditional viscosity of the lubricant STP-3 on temperature. Figure 7 shows a graph of the temperature dependence of the conditional viscosity of gear lubricant OSP. On Fig depicted graphs of the temperature dependence of various samples of oil Nissan SAE 5W-40 from the heating time. Figure 9 shows the probe for determining the content of magnetized wear products. Figure 10 shows the latch to stabilize the vacuum created in the tank.

Examples of tests of petroleum products of the proposed device.

1. Determination of the conditional viscosity of the gearbox lubricant STP-3.

Using the above procedure, the viscosity of STP-3 grease was determined at different temperatures (tube length - 150 mm, inner diameter - 2 mm).

Table 1. The results of the measurement of the conditional viscosity of the lubricant STP-3. Temperature ° C The time of filling the capacity of the device 0 1006 10 678 25 238 40 64 one hundred 3

According to the measurement results, a graph was constructed (Fig. 6).

The conditional viscosity found in accordance with GOST 6258-85 at 100 ° C is 3 conditional degrees.

The conversion factor in arbitrary degrees for lubrication STP-3: 3/3 = 1.

2. Determination of the conditional viscosity of the gear lubricant OSp-L.

Using the above procedure, the viscosity of the OSp-L lubricant was determined at different temperatures (tube length - 150 mm, internal diameter - 3 mm).

Table 2. The results of the measurement of the conditional viscosity of the lubricant OSp-L. Temperature ° C Device filling time, s 0 2409 10 995 25 327 one hundred 6

According to the measurement results, a graph was constructed (Fig. 7).

The conditional viscosity found in accordance with GOST 6258-85 at 100 ° C is 13 arbitrary degrees.

The conversion factor to arbitrary degrees for OSp-L lubricant: 13/6 = 2.17.

3. Determination of micropenetration of gear lubricant STP-3.

Using the device, 10 ml of grease were selected, cooled to 0 ° C, the cone on the rod was lowered until it touched the grease surface. The base of the cone is at 13.3. Then they released the stem with the cone. The base of the cone dropped to 10.6. The micropenetration was 13.3-10.6 = 2.7 units, taking into account the distance between the divisions (3.5 mm) this corresponds to 2.7 * 3.5 = 9.45 mm = 94.5 mm / 10.

The micropenetration was measured at 0 ° C according to GOST 5346-78, method B, a value of 95 mm / 10 was obtained. The results of micropenetration measurements using the device coincide with the results of measurements in accordance with GOST 5346-78.

In accordance with the STP-3 grease standard, its micropenetration should lie within 80 ... 100 mm / 10, therefore, the analyzed grease complies with the standard.

4. Determination of demulsifying ability of compressor oil KP-8S.

Using the device, 10 ml of KP-8S oil and water were taken, mixed for 5 minutes, then set to stand at room temperature (25 ° C). Every 5 minutes, the volume of oil, water and emulsion was measured. The demulsifying ability was also determined in a standard manner (according to ASTM D1401-10) at 54 ° C. The results are shown in table 3.

Table 3. The results of measuring the demulsifying ability of oil KP-8C. Time min The proposed method ASTM D1401-10 Oil volume ml Water volume, ml The volume of the emulsion, ml Oil volume ml Water volume, ml The volume of the emulsion, ml 0 0 5 fifteen 0 twenty 60 5 3 7 10 19 33 28 10 5.5 8 6.5 34 39 7 fifteen 7 8.5 4,5 40 40 0 twenty 8 9 3 - - - 25 9 9.5 1,5 - - - thirty 9.5 9.5 one - - - 35 10 10 0 - - -

Both in the proposed method for measuring demulsifying ability, and in the case of ASTM D1401-10, the emulsion separation pattern is the same, only volumes (proportions remain the same) and time (due to temperature differences) differ.

5. The definition of the dynamics of heating oil Nissan SAE 5W-40.

We carried out the determination of the heating dynamics indicator for pure Nissan SAE 5W-40 oil and its mixtures with the main pollutants: water, gasoline, antifreeze and soot.

Samples weighing 60 g were heated to 150 ° C and the heating time was recorded with an interval of 5 ° C (table 4).

Table 4. The results of the measurement of the dynamics of heating oil Nissan SAE 5W-40. Temperature ° C Clean 3% water 3% antifreeze 10% gasoline 5% carbon black 35 0 0 0 0 0 40 36 33 32 39 31 45 88 72 65 94 80 fifty 122 108 113 132 127 55 156 153 147 162 154 60 184 185 175 189 187 65 215 223 200 214 224 70 242 255 223 237 259 75 260 290 250 268 294 80 279 323 283 288 325 85 304 356 311 317 350 90 332 383 345 341 379 95 355 408 370 362 408 one hundred 377 433 388 380 436 105 400 463 415 406 461 110 420 491 436 431 489 115 443 519 455 451 515 120 467 551 476 475 540 125 491 576 503 495 566 130 514 601 530 520 591 135 536 633 554 541 614 140 561 673 580 564 639 145 584 699 608 592 662 150 609 736 639 617 688

According to the results of the experiment, graphs were constructed (Fig. 8). It can be seen from the graphs that the indicator of the dynamics of oil heating is most affected by water - oil with the addition of 3% water heats up longer than other samples (due to the greater heat capacity of the water and the cost of water evaporation). Also, soot has a significant effect on the heating time. A slight increase in heating time is observed when coolant is added to the oil. The addition of a large amount of gasoline (10%) had practically no effect on the heating time of the oil.

Thus, an increase in the heating time of the oil (compared to pure) indicates the presence of impurities (water, soot, antifreeze) in it.

Claims (5)

1. A device for determining the quality of petroleum products, containing a container with a scale for sampling with a rod with a piston placed in it, a hardware-software complex (5) for measuring time and temperature, a tube for passing liquid into the container when sampling to determine the viscosity a thermistor that can be installed on the tube to determine micropenetration, demulsifying ability, and the rate of heating of the liquid; a cone that can be installed instead of the piston on the rod using a thread when determining ropenetratsii, plug or lid which may be mounted on the container instead of the tube fitting in determining mikropenetratsii and demulsibility, and a stand for mounting the container. 2. The device according to claim 1, characterized in that it is additionally equipped with a holder that includes a plate with a hole and a screw. 3. The device according to claim 1, characterized in that it is additionally equipped with a pendant mount, which includes a tape and a hook. 4. The device according to claim 1, characterized in that it is additionally equipped with a probe - detector of wear particles, including a plastic tube, magnet and wire. 5. The device according to claim 1, characterized in that it is additionally equipped with a latch that includes a plate and a wire.

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