JPH0620133Y2 - Pour point and cloud point measuring equipment - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial application] The present invention relates to an apparatus for measuring the pour point of crude oil and petroleum products and the cloud point of petroleum products.

[Prior Art] The pour point and cloud point are measured as quality control items for crude oil and petroleum products. According to JIS K-2269, "The pour point is when the sample is cooled without stirring by the specified method,
The lowest temperature at which a sample flows. The cloud point is defined as the temperature at which paraffin and other precipitates start to separate when the sample is cooled by a specified method without stirring.

Regarding the device that automatically measures the cloud point, the light emitting part and the light receiving part are installed with the sample in between, and the cloud point is found by detecting that the transmitted light that has passed through the sample changes with the crystallization of the sample. The device is considered. The apparatus is disclosed in Japanese Patent Application No. 63-276220 previously filed by the applicants of the present application as an apparatus for measuring a precipitation point, and this apparatus can be directly used for an apparatus for measuring a cloud point.

[Problems to be Solved] On the other hand, as for a device for automatically measuring a pour point, a differential pressure type, a rotary type or a tilt type pour point measuring device is currently on the market. However, since the pour point has to detect a subtle crystal change of the sample beyond the cloud point, the conventional pour point measuring devices have complicated structures and are difficult to maintain.

The present invention has been made in view of the above problems. For the purpose of provision.

[Means for Solving the Problems] In order to achieve the above object, the pour point and cloud point measuring device of the present invention communicates with a cloud point measuring chamber that stores a fixed amount of sample and the cloud point measuring chamber. A pour point detection tube that can move in the vertical direction, a means for adjusting the temperature in the cloud point measurement chamber, a cloud point measurement temperature sensor that measures the sample temperature in the cloud point measurement chamber, and the pour point detection tube A temperature sensor for pour point measurement for measuring the temperature of the sample in the pour point detection tube that has risen with the ascending movement, and a transmitted light amount detector in which a light emitting part and a light receiving part are arranged with the cloud point measuring chamber sandwiched therebetween. is there.

[Embodiment] An embodiment of the present invention will be described below with reference to the drawings.

FIG. 1 is a sectional configuration diagram of a pour point and cloud point measuring device according to the present embodiment.

In the drawing, 10 is a measuring cell, 20 is a temperature controller,
Reference numeral 30 is a pour point detection tube, and 40 is a transmitted light amount detector.

The measurement cell 10 includes a cloud point measuring chamber 11 that stores a small amount (2 to 3 ml) of a sample (hydrocarbon oil), an injection path 12, a delivery port 13, and an injection path 12 that are connected to the cloud point measuring room 11. An injector 14 is provided to inject the sample into the cloud point measuring chamber 11 via the injector. For this measuring cell 10, it is preferable to use aluminum or the like, which has good thermal conductivity and is resistant to corrosion. Further, in the cloud point measuring chamber 11, a cloud point measuring temperature sensor 15 for measuring the cloud point of the sample is inserted. As the cloud point measuring temperature sensor 15, for example, a platinum side heating element is used.

The temperature controller 20 has an electronic temperature controller 21 and a cool jacket 22. Of these, the electronic temperature controller 21 is formed by a Peltier effect element in which a p-type semiconductor and an n-type semiconductor are joined with a metal, and is arranged on both sides of the measurement cell. The thermoelectric phenomenon of the element is used. By changing the direction of the current flowing through the Peltier effect element by a controller (not shown), heat is generated and absorbed, and the sample is heated and cooled.
On the other hand, the cool jackets 22 are also arranged on both sides of the measuring cell 10, and the coolant is circulated and supplied to the cool jacket 22 from a coolant tank (not shown).

The temperature control device 20 performs comparatively strong cooling by flowing a refrigerant through the cool jacket 22, and the electronic temperature controller 21 performs delicate temperature control of the sample at low temperature.

The pour point detection pipe 30 is formed in a stepped cylindrical shape with both ends open, and the pour point detection part 3 having a large diameter above the step part 31.
It is 2. In addition, on the peripheral wall of the pour point detector 32,
A branch pipe 33 that is inclined downward toward the tip is formed.
The lower end of the pour point detection tube 30 communicates with the cloud point measurement chamber 11 in the measurement cell 10 via the flexible tube 34.

The pour point detection tube 30 is vertically movable and is supported by the support base 3
5 and is driven in the vertical direction by the vertical movement drive member 36. The vertical drive member 36 of this embodiment utilizes the repulsive force of the electromagnet, and the electromagnetic coil 3 is mounted on the support base 35.
6a is provided, and a permanent magnet 36b is attached to the step 31 of the pour point detection tube 30. In this way, when the repulsive force of the electromagnet is used, the vertical movement can be performed at a slow speed.

A temperature sensor 37 for measuring the pour point of the sample is provided in the hollow portion of the pour point detection tube 30 at a certain height above the connecting portion of the branch tube 33 (a height smaller than the amount of rise of the same tube 30). .
As the pour point measuring temperature sensor 37, for example, a thermocouple is used.

The transmitted light amount detector 40 has optical fibers 41 and 42 arranged at positions facing each other with the cloud point measuring chamber 11 interposed therebetween, and a light source 43 is provided at an input end of one optical fiber 41 and the other optical fiber 42. The light receiving element 44 is provided at the output end of the. When the light source 43 and the light receiving element 44 are provided at positions apart from the measurement cell 10 via the optical fibers 41 and 42 in this way, the light source 43 and the light receiving element 44 are not adversely affected by the temperature of the measurement cell 10.

Next, the procedure for measuring the pour point and cloud point using the apparatus of the above-described embodiment will be described with reference to FIGS. 2 to 4. 2 to 4 are sectional views for illustrating the measurement procedure.

Cloud point measurement chamber 11 from injector 14 via injection path 12
Input about 5 ml of the sample (see Fig. 2).

A part of the injected sample is stored in the cloud point measuring chamber 11, and the other part is stored through the flexible tube 34 in the pour point detecting tube 30.
All the samples that flow into the inside through the lower end opening and exceed the branch pipe 33 are discharged through the branch pipe 33. Therefore, a fixed amount of sample is stored in the cloud point measuring chamber 11 and the pour point detecting tube 30. Here, since the branch pipe 33 is provided on the peripheral wall of the pour point detector 32 and is an inclined pipe, the excess sample can be quickly discharged.

While the sample in the cloud point measuring chamber 11 is being cooled by the temperature control device 20, light is incident on the sample from the light source 43 and the amount of transmitted light is detected by the light receiving element 44 (see FIG. 3).

As the cooling progresses, the amount of transmitted light gradually decreases when crystals start to form in the sample. Since the temperature at the point where the crystals start to occur is the cloud point, the sample temperature at that point is measured by the cloud point measuring temperature sensor 15.

Further, the temperature controller 20 cools the sample in the cloud point measuring chamber 11, and the temperature sensor 1 for cloud point measurement is used.
The indicated value of 5 is confirmed, and the vertical driving member 36 is operated to raise the pour point detection tube 30 every time the sample temperature decreases by a certain unit (see FIG. 4).

When the sample has fluidity, the liquid surface on the injection path 12 side and the liquid surface on the pour point detection tube 30 side try to maintain equilibrium.
Only the pour point detection tube 30 rises and the liquid level of the sample maintains the same height. Therefore, the pour point measuring temperature sensor 37
Since the sample does not come into contact with, the indicated value of the temperature sensor 37 does not change.

On the other hand, when the sample reaches the pour point and loses fluidity, the sample rises together with the pour point detection tube 30. As a result, the sample comes into contact with the temperature sensor 37 for measuring the pour point, and the indicated value of the temperature sensor 37 changes. Therefore, if the temperature when the indicated value changes is measured, that temperature becomes the pour point.

The present invention is not limited to the above-described embodiment, and various modifications can be made within the scope of the invention.

For example, the vertical driving member of the pour point detection tube is not limited to the electromagnet, and a known means such as a hydraulic cylinder or an air cylinder may be used. Further, the temperature adjusting means, the cloud point detecting sensor and the pour point detecting sensor may use modes and means other than those in the above embodiment.

[Effects of the Invention] As described above, according to the pour point and cloud point measuring device of the present invention, the pour point of crude oil and petroleum products and the cloud point of petroleum products can be automatically calculated with a simple structure and easy operation. There is an effect that it can be measured as desired.

[Brief description of drawings]

FIG. 1 is a sectional configuration diagram of a pour point and cloud point measuring device according to an embodiment of the present invention, and FIGS. 2, 3, and 4 are sectional views illustrating measuring means using the same device. . 10: Measurement cell, 11: Cloud point measuring chamber 15: Temperature sensor for cloud point measurement 20: Temperature control device, 30: Pour point detection pipe 32: Pour point detection part, 33: Branch pipe 36: Vertical drive member 37: Flow Temperature sensor for point measurement 40: Transmitted light amount detector

Claims (1)

[Scope of utility model registration request] 1. A cloud point measuring chamber for storing a fixed amount of sample,
A pour point detection tube which is in communication with the cloud point measuring chamber and is movable in the vertical direction, a means for adjusting the temperature in the cloud point measuring chamber, and a cloud point measuring unit for measuring the sample temperature in the cloud point measuring chamber. A temperature sensor, a temperature sensor for pour point measurement that measures the temperature of the sample in the pour point detection tube that has risen with the upward movement of the pour point detection tube, and a light emitting unit and a light receiving unit across the cloud point measurement chamber. A device for measuring a pour point and a cloud point, comprising: a transmitted light amount detector arranged.