JPH041555A - Measuring instrument for liquid penetration speed to power and granular material - Google Patents

Abstract

PURPOSE:To improve measuring accuracy by stopping driving when a relative position between a pipe for sample powder fluid packing and a penetration liquid container is set at a preset position. CONSTITUTION:The pipe 1 provided with a bottom part through which liquid can be penetrated freely is suspended under a weigher 2, and a container 5 is placed on a board 4 on which a driving device 3 for elevation is mounted, and the container 5 is brought near the pipe 1 by elevation, and the liquid L in the container 5 is penetrated from the bottom part of the pipe 1 to sample powder fluid S, and the change of the weight of the pipe 1 according to penetration to the powder fluid S is measured. It is decided whether or not the relative position is set at a preset relative position where the powder fluid S is brought into contact with fluid L by the computing element B of a computer C, and the device 3 is stopped by a controller A. In such a way, the measuring accuracy can be improved.

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention provides a pipe for filling a sample powder or granule having a bottom portion through which liquid can freely flow, in order to measure the permeation rate of liquid into the powder or granule;
A driving device is provided for vertically approaching a container containing a liquid to be permeated into the sample powder in the pipe from the bottom, and after the sample powder in the pipe is brought into contact with the liquid in the container, An apparatus including a controller that automatically operates the drive device to stop the approach of the pipe and the container, and a measuring device that measures a change in the weight of the pipe as liquid permeates into the sample powder in the pipe. Regarding.

[Conventional technology]

Conventionally, when a measurement is started, a timer is activated, and the pipe and container are brought close together for the time set by the timer, and the sample powder in the pipe is transferred to the liquid in the container through the liquid-flowable bottom of the pipe. It was configured to make contact.

[Problem to be solved by the invention]

However, measurement errors were large, making it difficult to achieve highly accurate measurements with excellent reproducibility.

An object of the present invention is to investigate the cause of large measurement errors and to enable highly accurate measurements to be easily and reliably performed.

[Means to solve the problem]

The characteristic configuration of the present invention is that in the apparatus for measuring the rate of liquid penetration into powder and granule specified in the above [Industrial Application Field] section, when bringing the sample powder and granule in the pipe into contact with the liquid in the container, A position determining means is provided for determining whether the relative positions of the pipe and the container have reached a set relative position where the sample powder and granule come into contact with the liquid, and the pipe and the container are adjusted based on a stop instruction from the position determining means. The present invention is based on the provision of an output means for stopping the drive device when the relative position of the drive device reaches a set relative position, and its effects are as follows.

[For production]

In the past, when we investigated the cause of the large measurement error, we found that the initial level difference between the pipe and the container was not constant, and the timer setting time was adjusted according to the initial level difference, but in reality, It was found that there was considerable variation in the depth at which sample powder and granular material was immersed in the liquid in the container, and that measurement errors were large due to the influence of liquid pressure due to the variation in immersion depth.

Therefore, the position determination means determines whether the relative position of the pipe and the container has reached the set relative position, and when it is confirmed that the set position has been reached, the output means automatically stops the drive device. By configuring the sample powder to be immersed in the liquid at a constant depth regardless of the initial level difference between the pipe and container, high-precision measurements with small errors and good reproducibility can be easily and reliably performed. Now you can.

[Effects of the invention] As a result, the measurement accuracy and operability are further improved.
It is now possible to provide an extremely high-performance device for measuring the rate of liquid penetration into powder and granular materials.

As described in claim 2, the pipe and the container are caused to approach each other intermittently by the intermittent movement execution means and the intermittent movement instruction means,
When the drive device is stopped, the weight measured by the scale is read by the measured value storage means to eliminate measurement errors due to the dynamic inertia of the pipe or the container, and the measured value storage means reads and stores a plurality of measured weights, The measured weight is read and stored by the measured value storage means until the deviation determination means confirms that the deviation of the plurality of measured weights is within the set range, and when the deviation falls within the set range, the stable measured weight is When the measured weight to be stored is determined by the memorized value determining means based on the determined value and the determined measured weight stored in the determined value memorizing means is free from errors caused by shaking of the pipe or liquid, the immersion depth of the sample powder or granule in the liquid is determined. This makes it possible to more precisely stabilize the temperature and improve measurement accuracy even more effectively.

〔Example〕

Next, examples will be shown.

As shown in Figure 1, a pipe (1) with a bottom made of filter paper or the like through which liquid can freely flow is suspended from a measuring instrument (2) such as an electronic balance, and a lifting drive device (3) such as a linear helical motor is suspended. ) The container (5) is placed on a stand (4) attached to a table (4), and the container (5) is raised by the drive device (3) to approach the pipe (1), and the sample powder filled in the pipe (1) is removed. The liquid (L) in the container (5) is infiltrated into (S) from the bottom of the pipe (1), and the weight change of the pipe (1) as the liquid (L) permeates into the sample powder (S) is measured using a measuring instrument. It is configured to measure in (2).

A computer (C) that automatically operates the drive device (3) and processes information from the measuring instrument (2) is provided, and an input device (6) for the computer (C) and information obtained by the computer (C) are provided. A display (7) displays the measured results.
) is provided.

The computer (C) consists of a controller (A) that automatically operates the drive device (3) and a calculator (B) that calculates various data based on changes in weight measured by the weighing device (2). .

As shown in FIG. 2, the controller (A) is provided with the following means (a) to h).

(a) Based on the measurement start instruction from the input device (6),
intermittent movement execution means (8) for intermittently operating the drive device (3);
) for instructing the pipe (1) to be immersed in the liquid (L), that is, to raise the container (5).

Incidentally, the intermittent movement execution means (8) operates the drive device (3) for a minute period of about 0.2 seconds each time, for example.

(b) Measured value storage means (11) for reading and storing a plurality of weights measured by the scale (2) when the drive device (3) is stopped based on information from the intermittent movement execution means (8).

(C) Deviation determining means (12) for determining whether the deviations of the plurality of measured weights are within a set range based on information from the measured value storage means (11).

In other words, the program is programmed to determine whether or not all of the set number of recently read measured weights, for example three or more, are within a set range of deviations from the average value.

(d) When the deviation falls within the set range based on the information from the deviation determining means (12), the stored value determining means (13) determines the measured weight to be stored based on the information from the measured value storing means (11). ).

That is, the program is such that, for example, an appropriate value such as the average value, the measured weight closest to the average value, or the latest measured weight is determined as the measured weight to be stored.

(e) Determined value storage means (14) for storing the determined measured weight from the stored value determination means (13).

(g) intermittent movement instruction means () which instructs the intermittent movement execution means (8) to carry out the next intermittent movement, that is, to raise the container (5), when the deviation falls within the set range based on the information from the deviation determination means (12); 15).

(g) Storage value change state determination means (16) for determining whether the determined measured weight has increased based on the information from the determined value storage means (14).

(h) Stop position determining means (18) for transmitting a stop instruction for the drive device (3) to the output means (17) when the determined measured weight increases based on information from the storage value change state determining means (16).

As shown in FIG. 3, the computing unit (B) is provided with the means described in (a) to (d) below.

(a) S calculation means (19) for calculating the cross-sectional area S of the sample powder layer based on ρ51 ws, H from the input device (6) using the following formula % formula %.

In addition, ρ5 is the sample powder (S) filled in the pipe (1).
), W5 is the weight of the sample powder (S), and H is the filling height of the sample powder (S).

(b) ρ5 from input device (6). ε calculation means (20) for calculating the porosity ε of the sample powder layer based on Ws+H using the following formula (% formula %);

(c) Drive device (3) based on information from output means (17)
) is stopped, the measurement timer (21) starts.
.

(d) Correlation storage means (22) for storing the correlation between the measured weight W1 from the scale (2) and the measurement time t from the measurement timer (21) as shown in FIG.

(e) When the set measurement time has elapsed based on the information from the measurement timer (21), W, - is stored in the correlation storage means (22).
Based on the information from dW, /d as shown in Fig.
Analyze and store the correlation between t and 1/W1 dW, /d t
-1/W, correlation storage means (23).

(to) dW, /dt-1/W, correlation storage means (23
), as shown in FIG. 5, α and β determination means (24) for determining the slope α and the y-slice β.

(g) Based on the information from the α and β determination means (24), the permeated liquid weight W at the time when liquid (L) permeation into the sample powder (S) reaches equilibrium is calculated using the following formula: Wω calculating means (25) for calculating.

(H) ρ1 from the input device (6). η, g, s calculation means (
ε, α, β from S18 calculation means (20) from 19)
r calculation means (26) for calculating the average capillary radius r of the sample powder layer according to the following formula based on β from the determination means (24);

In addition, ρ is the density of the liquid (L) in the container (5), η is the viscosity of the liquid (Sh), and g is the gravitational acceleration.

(i) rt, g, S calculation means (1) from input device (6)
9), ε from the ε calculation means (20), WooSr from the Woo calculation means (25), r from the calculation means (26), the sample powder (S) as shown in FIG. ) and the liquid (L), the contact angle θ and the adhesion tension TLcos
θ calculating means (27) for calculating θ using the following formula.

Note that T is the surface tension of the liquid (L), which was actually measured in advance by the ring method.

Next, measurement using the above device will be explained with reference to FIG.

(1) Using the input device (6), ρSI WS, H, ρ[
,η.

When γt and g are input, means (19), (20>
S and ε are calculated.

[2] When the input device (6) instructs to start measurement, the container (5) is intermittently raised. Then, each time the container (5) is stopped, a plurality of measured weights are read, a deviation is determined, and it is determined whether or not the measurement is stable.

(3) When the measurement becomes stable, the measured weight to be stored is determined and stored. Further, it is determined whether the determined measured weight has increased.

(4) As a result, during the time period when the sample powder (S) in the pipe (1) is away from the liquid (L), the determined measurement weight does not increase, so the intermittent rise of the container (5) continues. Ru.

(5) Measurement determined by the surface tension of the liquid (L) when the sample powder (S) approaches the liquid (L) and the liquid (L) adheres to the sample powder (S) due to surface tension. If the weight suddenly increases, the lifting of the container (5) is stopped and
A measurement timer (21) is started.

(6) The means (22) stores the correlation between W and t, and when the set measurement time elapses, W, as shown in FIG.
- A correlation diagram is created on the display (7).

(7) dW as shown in Figure 5 based on the correlation diagram of W, -
, /dt and 1/W are stored by means (23), and a correlation diagram of dW, /d t -1/W is displayed on a display (7).
Created with.

(8) Based on dW, /dt-1/W, and the correlation diagram, α and β are determined by the means (24) as shown in FIG.

(9) ρ1. r is calculated by means (26) based on ηtgl ε+S+β.

(10) 7+, g, e, S, W",
θ based on r.

γ+CO3θ is calculated by means (27).

αυ ρS+WS+ H, ρ+, 77 + 7 +,
g + WoO+ e + r Tγ+CO5θ, θ is shown on the display (7).

[Another example]

The following another embodiment will be described.

When bringing the sample powder (S) in the pipe (1) into contact with the liquid (L) in the container (5), the pipe (1) may be lowered by the drive device (3). 1)
The relative position of the container (5) and the sample powder (S) and the liquid (
Various position determining means can be used to determine whether or not L) has reached the set relative position where it makes contact. For example, the relative positional relationship between the pipe (1) and the container (5) may be detected using a non-contact sensor such as an optical sensor, and the output means (17) may be used to stop the drive device (3) based on the information from the sensor. It may be configured as follows.

The data to be displayed on the display (7) may include at least one of Wl-, a correlation diagram, dW, /dt-1/W, a correlation diagram, γ+CO3θ, and θ.

Incidentally, although reference numerals are written in the claims section for convenient comparison with the drawings, the present invention is not limited to the structure shown in the accompanying drawings.

[Brief explanation of drawings]

1 to 7 show embodiments of the present invention, FIG. 1 is a conceptual diagram of the device, FIG. 2 is a block diagram of the controller, FIG. 3 is a block diagram of the arithmetic unit, and FIG. 4 is a W , - is a correlation diagram, FIG. 5 is a dW, /d t -1/W1 correlation diagram, FIG. 6 is an explanatory diagram of the contact angle θ, and FIG. 7 is a flowchart for explaining the operation. (1) Pipe, (2) Measuring device, (3) Drive device, (5) Container, (8) ...Intermittent movement execution means, (11).
. . . Measured value storage means, (12) . . . Deviation judgment means, (13) . . . Memory value determination means, (1
4)... Determined value storage means, (15)...
・Intermittent movement instruction means, (16)...Memorized value change state determination means, (17)...Output means, (18)
)... Stop position determining means, (L)...
Liquid, (S)... Sample granular material.

Claims (1)

[Claims] 1. A pipe for filling sample powder or granular material having a bottom portion through which liquid can freely flow (
1) and a container (5) for storing a liquid (L) to be infiltrated into the sample powder (S) in the pipe (1) from the bottom thereof in a vertical direction. After bringing the sample powder (S) in the pipe (1) into contact with the liquid (L) in the container (5), the pipe (1) and container (5)
A controller is provided to automatically operate the drive device (3) to stop the approach of the sample powder (1) in the pipe (1).
A device equipped with a measuring device (2) for measuring a change in the weight of the pipe (1) as liquid (L) permeates into the pipe (S), the device comprising: The container (5
) When bringing the liquid (L) into contact with the liquid (L) in the pipe (
The relative position of 1) and the container (5) is such that the sample powder (S)
A position determining means is provided for determining whether or not a set relative position is reached at which the pipe (1) and the liquid (L) come into contact with each other, and the relative positions of the pipe (1) and the container (5) are determined based on a stop instruction from the position determining means. output means (for stopping the drive device (3) when the set relative position is reached;
17) A device for measuring the rate of liquid penetration into a powder or granular material. 2. An intermittent movement execution means (8) for intermittently operating the drive device (3) is provided, and the following items (a) to (a) are provided to form the position determination means.
(a) Based on the information from the intermittent movement execution means (8), when the drive device (3) is stopped, a plurality of weights measured by the weighing device (2) are read and stored; measurement value storage means (
11), (b) deviation determining means (12) for determining whether the deviations of the plurality of measured weights are within a set range based on the information from the measured value storage means (11); (c) the deviation; When the deviation falls within the set range based on the information from the determination means (12), the measured value storage means (11)
(d) storage value determining means (13) for determining the measured weight to be stored based on information from;
) determined value storage means (14) for storing determined measuring means from
), (e) When the deviation falls within the set range based on the information from the deviation determination means (12), the intermittent movement execution means (8)
an intermittent movement instructing means (15) for instructing the next intermittent movement; determining means (16); (g) stop position determining means (18) for transmitting a stop instruction to the output means (17) when the determined measured weight increases based on information from the stored value change state determining means (16); ) The device for measuring the rate of liquid penetration into powder or granular material according to claim 1.