JPS59212735A - Sampling apparatus of process analyzer - Google Patents

Abstract

PURPOSE:To sample a highly viscous liquid sample in high precision without causing any leakage by stopping a flow path temporarily in fluidizing state while passing the liquid sample continuously through a cylinder and compressing the fluid of a fixed volume by a piston. CONSTITUTION:The highly viscous liquid is allowed to flow continuously into a measuring cylinder 7 by a pump 6 in a sampling apparatus. The cylinder 7 is provided with an inlet shutting valve 8 and an outlet shutting valve 9, and the flow can be stopped temporarily under the fluidizing state while the liquid sample is passed therethrough continuously. Next, the piston 11 coupled to an air cylinder 10 for the piston is inserted into one end of the cylinder 7. The highly viscous liquid sample can be sampled with high accuracy without causing any leakage by compressing the fluid of a fixed volume.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a sampling device for a process analyzer that targets highly viscous liquids.

Traditionally, sample collection devices for process analyzers include a slide method, a measuring tube method, and a valve switching method. This has the disadvantage that sample accuracy deteriorates due to adhesion to the surface of the sample. Especially in the slide method, the sample adheres to the slide surface,
The slide may not move smoothly.Also, the liquid sample may seep out from the slide surface, causing leakage, which reduces sample measurement accuracy.

The present invention overcomes the drawbacks of the more conventional methods,
The object of the present invention is to provide an extrusion method using a piston, which is structured so that highly viscous liquid samples can be collected with high precision.

The sample collection device for a process analyzer according to the present invention adopts the extrusion method using the piston y, and while the liquid sample is continuously passed through the cylinder, the flow path is temporarily stopped in a flowing state, and the piston is pushed from one side of the cylinder. It has a structure that compresses a fixed volume of fluid and simultaneously opens the other valve of the cylinder to introduce a fixed amount of liquid into the process analyzer. Samples that adhere to the process analyzer introduction line are cleaned with a solvent or pressurized gas. It is characterized in that it can be introduced into a process analyzer.

According to this device, it is possible to quantitatively collect a highly viscous liquid sample at high temperature or room temperature.

The present invention will be explained below based on the drawings.

FIG. 1 is a sectional view showing a sliding type device as an example of a conventional sample collecting device.

In the figure, the liquid sample is continuously flowed into the sample tube l to avoid air bubbles. In this state, sample tube 1' inside cylinder 2
Slide the cylinder 2 in the direction of the arrow so that it aligns with the cleaning tube 3. After this, the cleaning tube 8 is purged with a cleaning gas or solvent, and a certain amount of the liquid sample in the sample tube 1' in the cylinder 2 located at the location of the cleaning tube 8 is introduced into the process analysis NtK (not shown in the figure). .

A set of blocks 4 sandwich the cylinder 2, and have a structure such that the cylinder 2 is slid by a spring 5, and the entire contact area between the cylinder 2 and the block Φ is evenly tightened.

However, with this slide method, a highly viscous liquid sample may adhere to the slide surface, interfering with smooth operation, and sample accuracy may deteriorate due to leakage from the slide surface.

FIG. 2 is a schematic cross-sectional view showing a sample collecting device according to an embodiment of the present invention.

High viscosity liquid is continuously pumped into the metering cylinder 7 by the pump 6.
flow inside. The metering cylinder is equipped with an inlet shut valve 8 and an outlet shut valve 9. While passing high viscosity liquid,
The inlet shut valve 8 and the outlet shut valve 9 are actuated simultaneously, or the inlet shut valve 8 is actuated slightly earlier so as not to build up pressure in the metering cylinder 7 to temporarily stop the flow of liquid. Next, the piston air cylinder 10 is activated, and the piston 11 connected to this cylinder 10 is inserted into one end of the measuring cylinder 7. At the same time, the shut valve air cylinder 12 is activated, and the shut valve 1 connected to this cylinder 12 closes the other end of the metering cylinder 7.
6 is opened, and the sample in the measuring cylinder 7 is transferred to the receiving cylinder 1.
When the outflow is finished, the shutoff valve 16 is closed again. Here, the intermediate stop valve 15 is activated by detection by the limiter 14, and the piston 11 is stopped at a certain distance. That is, by determining the position of the limiter 14, the piston 11
It becomes possible to extrude an arbitrary fixed volume of sample.

The liquid that has entered the liquid receiving cylinder 18 flows out by gravity into the measurement tank of the process meter located below, which is not shown in the figure.However, in order to sufficiently remove the liquid that has adhered to the inner wall, pressurized gas or the process meter is used. If there are no problems in terms of the measurement principle, a suitable solvent in which the liquid sample is dissolved is fed into the liquid receiving cylinder 18 via the valve 17. If the highly viscous liquid is at high temperature,
The seal 18 of the shut valve 16 is made of a heat-resistant material.

If the sample solidifies at ambient temperature, a heater is attached to the measuring cylinder 7 and the liquid receiving cylinder 18 along with the sample piping, and the temperature controller 19 is used to heat the sample to a constant temperature.

Next, an example will be shown in which the device of the present invention is applied to highly viscous liquids such as tar and pitch.

First, tar having a viscosity of 220 centipoise (50'C) was collected using a collection device while being heated to 50°C, and then benzene was used as a cleaning solvent.

The amount collected was actually measured as the benzene insoluble amount by filtration using J Engineering S Standard A5C. The amount to be collected was set at 2.5 me, and the amount of benzene used at one time was 100 m6. As a result of 10 consecutive measurements, the average benzene insoluble content was 0.219.
σ (repetition accuracy) is 0.00679, c, v at 6 g
, (coefficient of variation) was 8.0% sampling accuracy.

In addition, for pitch with a viscosity of 105 centipoise (160°C), toluene was used as the solvent, and the sampling accuracy was determined in the same manner as in the above example, and the average toluene insoluble content was 1.135.
,! 9 and σ is 0.015,! 9, c, v, is 1.8%
Met.

Furthermore, as a result of measuring the sampling accuracy using the same pitch as a sample without using a cleaning solvent, the average amount of sampling was 2.54. O
，! ;I, sampling accuracy is σ sail 0819, c, vo is 3.2
It was 0%.

As is clear from the above results, the sample collecting device according to the present invention can collect a highly viscous liquid sample with a C, V, sampling accuracy within 5%.

Further, a sample having a viscosity of up to 500 centipoise can be used.

As described above, according to the present invention, a highly viscous liquid sample can be collected with high precision without leaking.

[Brief explanation of the drawing]

Fig. 1 is a sectional view showing a sliding type device as a conventional sample device, and Fig. 2 is a sample collecting device according to an embodiment of the present invention. It is a schematic diagram without showing the construction. ]...Sample tube 2...Cylinder 3...
Cleaning pipe 4...Block 5...Spring 6...Pump 7...Measuring cylinder
8...Input Ronyat valve 9...Output Rochasoto valve 1
0...Air cylinder 11...Piston 12...Shut valve air cylinder 13...Liquid receiving cylinder 14...Limiter】5
... Middle 174] Stop valve 16 ... Shut valve 17 ... Valve 18 ... Barrage 19 ... Temperature controller. Figure 1 Figure 2

Claims (1)

[Scope of Claims] L: A cylinder through which a highly viscous sample passes continuously; A device for temporarily stopping a flow path while the sample in the cylinder is flowing; When the flow path is stopped, one of the cylinders a piston that compresses a volume of fluid and at the same time opens a valve located on the other side of the cylinder that introduces a volume of sample into the process analyzer; A sample collection device for a process analyzer that consists of a device that cleans the adhered sample and introduces it into the process analyzer.