JP2811225B2 - Solution swelling measurement system for polymer - Google Patents

Description

Description: TECHNICAL FIELD The present invention relates to a solution swelling property measurement of a polymer substance for measuring a swelling property of a substance which causes a swelling phenomenon in various liquids, in particular, an inorganic / organic polymer substance. Related to the device.

[Conventional technology]

In general, it is important to evaluate the characteristics of a solid substance that causes swelling due to contact with various solutions in order to understand the mechanism of the penetration of foreign molecules from the outside into the solid substance. The conventional device for measuring the swelling properties of polymer materials is to take the powdered sample in a cylindrical test tube, add the solution to it, leave it for several weeks, and measure the maximum swelling volume reached by the fixed material. Then, a method of obtaining an equilibrium swelling ratio (= Q) from comparison with the original volume has been performed. That is, the equilibrium swelling ratio Q satisfies the following equation.

Q = (apparent maximum swelling volume) / (original volume) [Problems to be Solved by the Invention] By the way, in the above-mentioned conventional apparatus for measuring the swelling properties of a polymer material, the specific gravity is larger than that of a solid sample. The solution cannot be used because the sample floats, and the maximum swelling volume is generally determined by visual measurement of the increase (height) in the test tube. Is difficult to measure, and the measurement accuracy of the solution swelling characteristics of the polymer substance is extremely low. Another major problem is that it is extremely difficult to continuously measure the time-dependent change in the swelling volume with a conventional apparatus for measuring the swelling properties of a polymer substance.

[Means for solving the problem]

An object of the present invention is to solve the above-mentioned problem. The swelling characteristics of substances (inorganic and organic polymer substances) that cause swelling in various liquids are equilibrium swelling ratios (= Q).
It is another object of the present invention to provide an apparatus for measuring a solution swelling property of a polymer substance which simply and accurately measures a swelling rate.

The present invention provides a fixed partition disposed at an upper portion of a sample chamber and permeable to a solution but not a solid polymer sample, the solution disposed at a lower portion of the sample chamber and transmitting a volume change due to swelling, A liquid medium for transmission having a higher specific gravity than the polymer solid sample and not mixed with the solution; and a capillary measuring unit communicating with the liquid medium for transmission,
The powdered polymer solid sample is filled in a flat plate shape between the fixed partition and the transfer liquid medium in the sample chamber, and the sample chamber is evacuated to vacuum. The change in the swelling volume of the solid polymer sample initiated by the contact between the solution introduced into the sample chamber and the solid polymer sample using the pressure difference is transmitted to the liquid medium for transmission. Guiding the change in swelling volume of the liquid medium for transmission to a capillary so as to expand the change in swelling volume of the solid polymer sample as a change in the length of the liquid column having a small bottom area; The present invention relates to an apparatus for measuring a solution swelling property of a polymer substance, comprising measuring a change in a column as the change in swelling volume of the polymer solid sample.

Since the apparatus for measuring the solution swelling characteristics of a polymer substance is constructed as described above, the sample portion to be measured is divided into a partition placed above the sample chamber through which only the solution passes and a sample and solution mixed below the sample chamber. The structure is such that it is sandwiched and fixed between a liquid medium having a large specific gravity and a liquid medium disposed below the sample chamber and communicates with the capillary. This solves the problem of the specific gravity difference between the liquid solution and the measurement sample and the problem of the colored solution. In addition, the change in volume of the measurement sample is transmitted as a change in the movement of the lower liquid medium, and the change in the movement of the liquid medium is further led to the capillary to amplify and expand as the change in the movement of the liquid medium in the liquid column of small bottom area. The change in the volume of the sample can be measured, the measurement accuracy of the change in the volume of the sample is significantly improved, and the change over time in the swelling volume of the sample can be easily measured.

〔Example〕

Hereinafter, an embodiment of a device for measuring a solution swelling property of a polymer substance according to the present invention will be described with reference to the drawings.

FIG. 1 is an explanatory view showing one embodiment of an apparatus for measuring a solution swelling property of a polymer substance according to the present invention.

The apparatus for measuring the solution swelling properties of a polymer substance is composed of a sample chamber s,
A glass filter partition b of a fixed partition which is disposed at the upper part of the sample chamber s and allows the solution to pass therethrough but does not allow the polymer solid sample to pass therethrough, a three-way cock a provided at the upper part of the sample chamber s, and a lower part of the sample chamber s The three-way cock c provided, the mercury Hg of the liquid medium for transmission filled in the lower part of the sample chamber s, and the solid polymer sample filled between the mercury Hg and the glass filter partition b in the sample chamber s Of the measurement sample j. The three-way cock a is connected to a solution reservoir i through a pipe m and to a vacuum pump k through a pipe n. The three-way cock c is connected to a mercury reservoir e through a pipe o and a capillary q constituting a capillary measuring section d through a pipe p.

Regarding the capillary measuring section d of the capillary q connected to the pipe p,
The point f at the end of the mercury column in the capillary q before measurement of the swelling volume change of the measurement sample j is at a height balanced with the weight of the measurement sample j and the solution, and the point h in the capillary q is from point f to point h. When the volume of the mercury column in the capillary q and the measurement sample j show the same swollen volume, the mercury level g in the sample chamber s
Are arranged so as to have an inclination in accordance with the position where is lowered. As a result, the principle of siphon acts between the mercury surface g and the point f at the end of the mercury column, and the pressure applied to the measurement sample j can be kept constant during the swelling of the measurement sample j.

First, a measurement sample j, which has been crushed and the particle size is made as uniform as possible, is charged onto mercury Hg below the glass filter partition b in the sample chamber s, and the three-way cock c is operated to move the sample chamber s from the capillary measuring section d. After shutting off, the sample chamber s is communicated with the mercury reservoir e, and after filling the sample chamber s with mercury Hg from the mercury reservoir e, the three-way cock a is operated to communicate the sample chamber s with the vacuum pump k. By the operation of k, the inside of the sample chamber s is evacuated through the three-way cock a.

On the other hand, the solution r is put into the solution reservoir i connected to the three-way cock a, and the three-way cock a is operated again to introduce the solution r through the three-way cock a into the sample chamber s which has been vacuum degassed. At the same time as introducing the solution r into the sample chamber s, the three-way cock c
Is operated to communicate the mercury Hg in the sample chamber s to the capillary measuring section d through the three-way cock c, and the change of the mercury column appearing in the capillary q is measured.

Since the apparatus for measuring a solution swelling property of a polymer substance according to the present invention is configured as described above, the measurement sample j is sealed between the partition wall b and the liquid medium mercury Hg, and the sample chamber s is evacuated to vacuum. Since the method of introducing the solution r at atmospheric pressure is adopted, the contact conditions between the measurement sample j and the solution r are standardized, the measurement of the swelling characteristics with extremely good reproducibility becomes possible, and the capillary measurement is performed. By adjusting the set position of the section d and its inclination, the pressure in the sample chamber s can be easily controlled, and further, the change in swelling volume in the sample chamber s is guided to the capillary q, and by expanding it, The temporal change of the swelling volume can be tracked with high measurement accuracy.

The liquid medium for swelling volume transfer used in the apparatus for measuring the swelling characteristics of a polymer substance according to the present invention has a specific gravity larger than that of the measurement sample j and the solution r and does not mix with them, for example, mercury Hg. Is used, but various low melting point alloys may be used for the measurement under the condition where the measurement temperature is high.

The capillary measuring section d in the apparatus for measuring the solution swelling characteristics of a polymer substance includes a liquid connected to the capillary q, in particular,
In the case of a conductive medium such as mercury Hg, a change in volume is converted into a change in length and the measurement can be performed easily, so that automatic optical or electrical measurement using a laser or the like is facilitated.

Since the apparatus for measuring the swelling characteristics of a polymer substance is configured as described above, the swelling characteristics of a polymer substance (polymer solid sample) which swells upon contact with the solution r can be measured with high precision. In addition, although the measurement can be carried out easily, the operation mechanism of the present invention is that
And the swelling phenomenon of the measurement material enclosed in the volume change transmission medium (mercury Hg) arranged at the lower part is guided to the capillary q through the medium and amplified and measured as the length of the liquid column with the small bottom area. Is considered to be significantly improved and the measurement over time is possible.

〔The invention's effect〕

As described above, the apparatus for measuring solution swelling properties of a polymer substance according to the present invention can be used in a solution having a specific gravity greater than that of a measurement sample, which is difficult to measure with a conventional apparatus, or in a solution that is significantly colored. Of the swelling characteristics of high molecular substances can be measured with high accuracy over time.
It can be used to evaluate the properties of polymer materials.

[Brief description of the drawings]

FIG. 1 is an explanatory view showing one embodiment of an apparatus for measuring a solution swelling property of a polymer substance according to the present invention. a ... three-way cock, b ... glass filter partition, c ... three-way cock, d ... capillary measuring part, e ... mercury reservoir, f, h ... capillary, g ... mercury surface, i ... solution reservoir , j …… measurement sample, k …… vacuum pump, m, n, o, p …… pipe line, q …… capillary, r …… solution, s…
... sample room.

Claims (1)

(57) [Claims] A fixed partition disposed above the sample chamber and permeable to the solution but not permeable to the solid polymer sample, and disposed below the sample chamber and transmitting the volume change due to swelling; A liquid medium for transmission having a higher specific gravity than the solid polymer sample and not mixed with the solution; and a capillary measuring unit communicating with the liquid medium for transmission, the powdered solid polymer sample is placed in the sample chamber. The space between the fixed partition and the liquid medium for transmission is filled in a flat plate shape, and the sample chamber is evacuated to a vacuum, and introduced into the sample chamber by utilizing a pressure difference between the sample chamber and the atmospheric pressure. The change in swelling volume of the solid polymer sample initiated by the contact between the solution and the solid polymer sample is transmitted to the liquid medium for transmission, and the change in swelling volume of the liquid medium for transmission is transmitted to the capillary tube. Leading Expanding more the swelling volume change of the polymer solids sample as a change in the length of the small footprint liquid column,
An apparatus for measuring a solution swelling property of a polymer substance, comprising measuring the change in the enlarged liquid column of the small bottom area as the change in swelling volume of the polymer solid sample.