JPH0455739A - Apparatus for measuring swelling characteristic of solution of macromolecular substance - Google Patents

Abstract

PURPOSE:To make it possible to perform highly accurate measurement by transferring the change in volume of the part of a sample to be measured to a medium at a lower part, further guiding the change into a capillary tube, amplifying and expanding the change as the change in liquid column having the small bottom area, and measuring the change. CONSTITUTION:This apparatus comprises the upper part of a chamber for a sample to be measured and the lower part. The upper part has a three-way cock (a) which is linked to a vacuum pump and a solution well (i) and a glass filter partitioning wall (b). The lower part has a capillary-tube measuring part (d) wherein mercury is used as a transfer solution and which is communicated to a three-way cock (c) and a mercury well (e). At first, the sample to be measured which is prepared by grinding so as to make the particle diameters equal as much as possible is picked up and placed on the mercury in the sample chamber. The mercury well (e) and the cock (c) are operated, and the chamber is filled with the sample. Thereafter, the sample chamber is shut off from the measuring part. The inside of the sample chamber is evacuated with a vacuum pump through the cock (a). Meanwhile, solution to be measured is inputted into the solution well (i) which is connected to (a). The cock (a) is operated again, and the solution is introduced into the evacuated sample chamber. The cock (c) is operated at the same time of the introduction. The mercury in the sample chamber is communicated into the capillary-tube measuring part, and the change in mercury column which appears in the capillary tube is measured.

Description

[Detailed Description of the Invention] [Industrial Application Field] This invention provides a substance that causes a swelling phenomenon in various liquids,
In particular, the f, wettability characteristics of inorganic/organic polymeric substances, that is, the t-equilibrium swelling rate (Q-value) defined by the quadratic equation, and the swelling rate can be easily calculated using H
The present invention relates to a device for accurately measuring

Q - Apparent maximum swelling volume Volume of 7 elements [Prior art] In general, the evaluation of the characteristics of solid substances that cause swelling phenomena upon contact with various solutions is useful for understanding the mechanism of penetration of foreign molecules into the solid substance from the outside. Conventionally, a powdered measurement sample was placed in a cylindrical test tube, a solution was added to it, and after leaving it for several weeks, the maximum PM volume reached by the solid substance was measured, and the original From the comparison with the volume of
A method of determining Q-IM is performed using the following formula.

[Problems to be solved by the invention] By the way, in this conventional method, a solution with a higher specific gravity than the solid sample cannot be used because the sample will float, and the maximum swelling volume generally increases due to the increase in sample II tube. Another major drawback of the conventional method is that it is difficult to measure in a solution where the supernatant liquid is darkly colored, and therefore the measurement accuracy is extremely low. The problem is that it is extremely difficult to continuously measure changes in swelling volume over time.

In order to solve the problem described in 1.2, the present invention has a partition wall that allows only the solution to pass through the measurement sample portion in the upper part, and a partition wall that allows the passage of the LK material and the solution in the lower part. A method is adopted in which the liquid medium is sandwiched and fixed with a liquid medium that does not mix and has a high specific gravity, and the medium placed below this medium is communicated with the capillary tube. This solves the problem of the difference in specific gravity between the solution and the sample to be measured (4) and the colored solution. Moreover, the measurement accuracy is significantly improved because the fM constant: The volume change of the In addition, it becomes possible to easily measure changes in swelling volume over time.

[Embodiments] Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings.

FIG. 1 shows an embodiment of a melt-liquid swelling characteristic measuring device, and shows a three-way cock 14 connected to a vacuum pump and a solution reservoir 1. and an upper part of a measurement sample chamber having a glass filter partition;
It consists of a capillary measuring part d, which uses mercury as a transmission solution, and which are communicated via a three-way cock c2, and a lower part having a mercury reservoir e. In particular, the arrangement of the capillary measurement section is such that one point at the end of the mercury column before the start of measurement is balanced with the pattern of the measurement sample and the FD liquid, and the point h is located in the capillary from point 1 to point h. The slope is made to match the volume of the mercury column and the position where the mercury surface g in the sample chamber falls when the measurement sample shows the same swelling volume. As a result, the two-siphon principle acts on both ends g and r, making it possible to always keep the pressure applied to the measurement sample J during swelling constant. First of all,
After pulverizing the measurement sample and making the particle size as uniform as possible into the mercury tank in the sample chamber and filling it by operating the mercury reservoir and C,
Place the sample chamber close to the measurement section and evacuate the inside of the test t1 chamber using a vacuum pump through a. On the other hand, the gi connected to a
Pour the measurement solution into m, i, and operate a again to introduce the solution into the sample chamber, which has been evacuated under vacuum. Simultaneously with the introduction, C is operated to communicate the mercury in the sample chamber to the capillary measurement section, and changes in the mercury column appearing in the capillary are measured.

As mentioned above, one feature of the present invention is that the measurement sample portion is sealed with a partition wall and a liquid medium, and after vacuum degassing, a measurement solution at atmospheric pressure is introduced into it. By standardizing the contact conditions with the sample chamber and making it possible to measure the swelling characteristics with extremely good reproducibility, by adjusting the setting position of the capillary measurement section and its inclination, the pressure in the sample chamber can be adjusted to the side of the sample chamber. In addition, by guiding the swelling volume change in the two sample chambers to the capillary tube and enlarging it, it is possible to track the temporal change in the swelling volume with high measurement accuracy.

The liquid medium for swelling volume transfer used in the above invention is as follows:
A material whose specific gravity is higher than that of the sample and solution and which does not mix with them is used, for example, mercury, but various low melting point alloys may be used for measurements under high measurement temperature conditions.

In the case of a liquid passed through a capillary tube, especially a conductive medium such as mercury, the measurement section C' of the present invention converts the change in volume into a change in the length of the liquid and easily determines 71+11. Therefore, automatic electrical or optical measurement using a laser or the like becomes easy.

[Made by Kawa] The above-mentioned method is used to measure the swelling properties of fused sleeves.

The swelling properties of polymeric substances that cause swelling in solutions can be measured with high precision and easily.2 The mechanism of action of this invention is to use a partition wall that allows only the solution to pass through and a volume change placed at the bottom. The swelling phenomenon of the measurement material sealed in the transmission medium is guided through the medium to the capillary tube and amplified and measured as the length of the small bottom liquid column, so the yI degree is significantly improved and measurement over time is possible. It is thought that it will become.

1. Effects of the invention] As stated above, this invention enables the conventional method to achieve the following:
71111It is now possible to measure the swelling properties of polymeric substances over time and with high accuracy in solutions that have a specific gravity greater than that of the measurement sample or in solutions that are significantly colored, which has been difficult to determine. It is believed that this method will be able to demonstrate its power in evaluating the characteristics of polymeric substances.

[Brief explanation of the drawing]

Figure 1 shows an example of a device for determining the fa liquid f moisture characteristic α1.
'. a...Three-way cock, b...Glass filter C...
・Three-way hook, f, h...capillary tube, ・mercury reservoir, j・
・・Measurement sample

Claims (1)

[Claims] It has a fixed partition at the top that allows the solution to pass through but does not pass through the solid polymer sample, and has a specific gravity greater than the solution and the polymer material that is mixed with the solution to transmit volume changes due to swelling to the bottom. a sample chamber with a liquid medium that does not contain
This is a solution swelling characteristic measuring device equipped with a capillary measuring section communicating with the medium, and starts by contacting the measurement sample with the solution introduced into the sample chamber using the pressure difference from atmospheric pressure after vacuum degassing. The solution swelling characteristics of polymeric substances are characterized by transmitting the change in swelling volume to the lower liquid medium for transmission, and further guiding it into a capillary tube to expand and measure it as a change in a small bottom area liquid column. measuring device.