JPH05340902A - Method and equipment for detecting pour point of fluid - Google Patents

Abstract

PURPOSE:To detect the pour point of a petroleum product surely and safely by a method wherein the presence or absence of a flow of a fluid is detected by a flow detecting sensor by tilting a cell at each cooling temperature while cooling down the fluid in stages from an ordinary temperature to a coagulation point. CONSTITUTION:While a sample 2 of which the pour point is to be detected is held in a cell 3, the cell 3 is provided with a flow detecting sensor 6 which detects a flow of the sample at the time when the cell 3 is tilted. While the sample 2 is cooled down in stages from a normal temperature to a coagulation point, the presence or absence of the flow of the sample 2 is detected by the sensor 5 by tilting the cell 3 at each cooling temperature. When the sample 2 is cooled down to the coagulation point and coagulates and it is detected by the sensor 5 that it does not flow, a cooling temperature T in the stage just before the detection is made the pour point. Accordingly, the pour point of the sample 2 can be detected surely and stably.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a fluid pour point detecting method and apparatus for reliably and stably detecting the pour point of a fluid such as petroleum products.

[0002]

2. Description of the Related Art As a method for measuring the pour point of a petroleum product, there is the petroleum product pour point test method (JISK2269).

This is a method in which the temperature of the petroleum product contained in the cell is lowered stepwise from room temperature to the freezing point, the cell is tilted at each temperature step, and the flow state is visually observed and determined.

[0004]

However, with this method, it is not easy to reliably and stably detect the pour point.

Therefore, an object of the present invention is to solve the above-mentioned problems and to provide a pour point detecting method for a petroleum product and an apparatus therefor for surely and stably detecting the pour point of a petroleum product.

[0006]

In order to achieve the above object, the present invention stores a fluid whose pour point is to be detected in a cell and detects the fluid flow when the cell is tilted. A flow detection sensor is installed to cool the fluid stepwise from room temperature to the freezing point, and the cell is tilted at each cooling temperature to detect the presence or absence of fluid flow with the flow detection sensor.The fluid is cooled to the freezing point and solidifies. When the non-flow is detected by the flow detection sensor, the cooling temperature in the preceding stage is used as the pour point.

The present invention also includes a cell for containing a fluid whose pour point is to be measured, a cooling means for gradually cooling the fluid by a predetermined temperature, an inclining means for inclining the cell at each cooling temperature, and a cell. And a flow detection sensor for detecting the presence or absence of fluid flow.

[0008]

According to the above construction, when detecting the presence or absence of flow of the fluid by gradually cooling the fluid by a predetermined temperature and tilting the cell at each temperature stage, the presence or absence of the flow is detected by the flow detection sensor. By doing so, the temperature at which the fluidity is no longer exhibited, that is, the freezing point is obtained stably, reliably and easily, and when the freezing point is obtained, the temperature in the previous stage of the freezing point is used as the pour point to automatically determine the pour point. Therefore, it can be detected reliably and stably.

[0009]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment of the present invention will be described in detail below with reference to the accompanying drawings.

FIG. 2 is a conceptual diagram showing an embodiment of a pour point detecting device to which the method for detecting a pour point of a fluid according to the present invention is applied.

In FIG. 1, a pour point detecting device 1 comprises a cell 3 containing a fluid (hereinafter referred to as sample) 2 whose pour point is to be measured.
A thermo module 4 as a cooling means for cooling the sample 2 step by step at a predetermined temperature, an inclining means (not shown) for inclining the cell 3 at each cooling temperature, and a sample 2 provided above the cell 3. Flow sensor 5 for detecting the presence or absence of flow
A thermocouple 6 for detecting the temperature of the sample 2 is arranged in the cell 3, is provided outside the cell 3, and is connected to a temperature controller 7 that controls the temperature of the sample 2. There is.

The flow detecting sensor 5 has an upper end swingably supported by a fulcrum 9 of a supporting member 8 provided above the cell 3, and a lower end penetrating into the sample 2 and a pendulum member 10. The eddy current (or eddy current) from the displacement oscillator 11 (or eddy current) is provided between the cell 3 and the thermo module 4 and the displacement oscillator (SUS) 11 which is provided below the sample so as not to contact the sample 2. (Displacement detector 12) for detecting the displacement d ₁ between the displacement transmitter 11 and the magnetic field). still,
Displacement detection sensor 1 including displacement transmitter 11 and displacement detector 12
3 is used, and for example, an eddy current displacement pickup is used in this embodiment.

The present application detects the change (displacement difference) of the displacement d ₁ obtained by the displacement detection sensor 13 as the presence or absence of the flow of the sample 2, and the pendulum member 10 and the displacement detection sensor 13 detect the flow detection sensor. Make up 5.

Since the cell 3 does not affect the eddy current of the displacement detecting sensor 13, it is preferably made of a porcelain material.

At the lower end of the pendulum member 10, the cross-sectional area of the contact portion with the sample 2 is made as small as possible in order to reduce the change of the surface state of the sample 2 due to the temperature.

The inclining means inclines the cell 3 together with the thermo module 4 at a constant angle during the pour point detecting operation. The inclining means can incline up to the angle necessary for ejecting the sample 2 when ejecting the sample 2.
However, this does not apply to the case of discharging by means of a pump, for example.

Next, the operation of the embodiment will be described.

FIG. 1 is a flow chart for explaining the concept of the fluid pour point detecting method of the present invention, and FIG. 3 is FIG.
It is a figure which shows the inclined state of the pour point detection apparatus shown in FIG.

In FIG. 1, an operator first places a sample 2 in a horizontal stationary cell 3, a thermocouple 6 and a pendulum member 1.
A certain amount is injected so that the lower end of 0 contacts (S-1).

The temperature controller 7 cools the cell 3 into which the sample 2 is injected to a temperature T near the upper side of the pour point by operating the thermo module (FIG. 2) 4 (S).
-2).

The temperature controller 7 detects that the temperature of the sample 2 is T
When it is detected by the thermocouple (FIG. 2) 7 that the temperature has reached 0 ° C., the thermomodule 4 is operated to lower the temperature T by a predetermined temperature ΔT ° C., for example, 2.5 ° C. (S-3).

When the temperature of the sample 2 drops to (T-ΔT) ° C, the cell 3 is gently tilted to a certain angle by the tilting means (S-4).

Displacement detection sensor 13 in the tilted cell 3
Detects the displacement of the pendulum member 10. Sample 2 at this time
If the liquid crystal has fluidity, the displacement decreases from d ₁ to d ₂ , so this displacement difference (d ₁ −d ₂ ) is detected (S-5).

In step (S-6), the displacement difference (d
_{If 1-} d ₂ ) is not 0, that is, if the sample 2 is fluid, the tilting means returns the cell 3 to the horizontal step (S).
-3), and from step (S-3) to step (S-
Repeat until 7). Thereby, the sample 2 is cooled stepwise from room temperature to the freezing point.

In step (S-6), the displacement difference (d
_{When 1-} d ₂ ) is 0, that is, when the sample 2 becomes non-fluid, the tilting means returns the cell 3 to the horizontal position and stands still for a certain time, for example, 5 seconds (S-8), and the operator It is confirmed whether the displacement difference (d ₁ -d ₂ ) is 0 (S-9). When the displacement difference (d ₁ -d ₂ ) is 0, the temperature T-ΔT of the sample 2 at this time is set as the freezing point. A temperature T higher than the freezing point by a predetermined temperature ΔT is set as a pour point (S-10). If the displacement difference (d ₁ -d ₂ ) is not 0 in step (S-9), the displacement detection sensor may be out of order. In such a case, processing such as suspension of the pour point detection operation is performed.

After detecting the pour point, the operator controls the temperature controller 7 to raise the temperature of the sample 2 and activates the inclining means to incline the cell 3 to eject the sample 2 from the cell 3 (S -11), the detection of the pour point of the sample 2 is completed.
In this embodiment, the temperature of the sample 2 is cooled from room temperature to the vicinity of the pour point and then cooled by a predetermined temperature. However, the temperature may be cooled by a predetermined temperature from room temperature.

Here, the constitution for detecting the freezing point first is that when the sample is cooled stepwise by a predetermined temperature and the cell is tilted at each cooling temperature to detect the flow of the petroleum product. This is because by detecting the presence or absence of this flow with a flow detection sensor, the temperature at which the sample shows no flow, that is, the freezing point can be obtained stably, reliably and easily. This is because the pour point that is difficult to detect by eye can be automatically and reliably and stably detected by setting the temperature of P to the pour point.

In the above, according to this embodiment, the cell 3
The sample 2 whose pour point is to be detected is housed therein, and a flow detection sensor for detecting the flow of the sample 2 when the cell 3 is tilted is provided in the cell 3, and the sample 2 is gradually heated from room temperature to the freezing point. While cooling, the cell 3 is inclined at each cooling temperature and the flow detection sensor 5 detects the flow of the sample 2, and the sample 2 is cooled to the freezing point and solidified, and the flow detection sensor 5
When the non-flow is detected in, the cooling temperature T of the previous stage is used as the pour point, so that the pour point of the sample 2 can be detected reliably and stably.

In this embodiment, the operator injects and evacuates the sample, operates the tilting means, etc., but from step (S-1) to step (S-11), for example, a microcomputer or a sensor is used. It may be formed so as to be automated.

Further, in the present embodiment, the displacement detecting sensor is formed by the displacement transmitter and the displacement detector, but the present invention is not limited to this, and it is possible to detect the displacement between the pendulum member and the cell. If so, a sensor using ultrasonic waves, light, capacitance, or the like may be used.

Further, in the present embodiment, the thermocouple is used for detecting the temperature of the sample, but other temperature sensors such as a thermistor and a posistor may be used instead of the thermocouple.

[0032]

In summary, according to the present invention, the following excellent effects are exhibited.

(1) Since the eddy current displacement pickup that operates stably even in a low temperature region is used, the pour point of a petroleum product can be detected reliably and stably.

[Brief description of drawings]

FIG. 1 is a flow chart for explaining the concept of a fluid pour point detection method of the present invention.

FIG. 2 is a conceptual diagram showing an embodiment of a pour point detecting device to which the fluid pour point detecting method of the present invention is applied.

3 is a diagram showing a tilted state of the pour point detecting device shown in FIG.

[Explanation of symbols]

 1 Pour point detection device 2 Sample 3 Cell 4 Thermo module 5 Flow detection sensor 6 Thermocouple 7 Temperature controller 8 Support member 9 Support point 10 Pendulum member 11 Displacement transmitter 12 Displacement detector 13 Displacement detection sensor

Claims (3)

[Claims] 1. A cell is provided with a fluid for detecting a pour point, and a flow detection sensor is provided in the cell for detecting the flow of the fluid when the cell is tilted. Cooling to the freezing point stepwise and tilting the cell at each cooling temperature to detect the presence or absence of flow of the fluid with a flow detection sensor, the fluid is cooled to the freezing point and solidifies, and the flow detection sensor does not flow When is detected,
A pour point detection method for a fluid, characterized in that the cooling temperature in the preceding stage is used as the pour point. 2. A cell containing a fluid whose pour point is to be measured, cooling means for gradually cooling the fluid at a predetermined temperature, tilting means for inclining the cell at each cooling temperature, and the cell. A fluid pour point detection device, comprising: a flow detection sensor that is provided and detects whether or not the fluid is flowing. 3. The flow detection sensor has an upper end swingably supported above the cell, and a lower end detects a pendulum-shaped member that has penetrated into the fluid, and a displacement of the pendulum-shaped member due to the swing. The fluid pour point detection device according to claim 2, comprising a displacement detection sensor.