JPS62218868A - Infinitesimal heat-quantity measuring apparatus - Google Patents

Abstract

PURPOSE:To eliminate possible loss of a specimen purity, even if it is kept under operation continuously, by cleaning a suction needle every time when it is used directly after suction of a specimen and cleaning also a stirring rod simultaneously. CONSTITUTION:A specimen suction needle 10 and a stirring rod 13 are transported above cleaning cups 15, 16 and next, an air pump 48 is driven to feed air into an air admitting cylinder 11. Simultaneously, the needle 10 and the rod 13 are lowered into the cups 15, 16 and at this moment, each pipe and electromagnetic valves 58, 66, 69 are switched to a flow path shown with solid thick lines and cleaning water is allowed to flow into the needle 10 through pipe 57, 3-way electromagnetic valve 58, pipe 60, valve proper 41 of 4-way valve apparatus, pipes 50, 51. And, at the same time, a flow path from the cleaning cup 15 to an exhaust liquid storage tank 47 is also formed and a flow path is formed in such a way that the cleaned liquid drawn from the cup 15 is allowed to flow into the exhaust liquid storage tank 47 through pipe 65, electromagnetic valve 66, pipe 70, electromagnetic valve 69, and pipe 71. Next, by switching the pipe from the electromagnetic valves 58, 69, the stirring rod 13 can be cleaned approximately in the same way.

Description

DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a microcalorimetry device, and more particularly, the present invention relates to a microcalorimetry device, and more specifically, a microcalorimetry device that is characterized by cleaning a sample suction needle and a sample stirring rod after operation. 0 Related to calorimetry device “Prior art” The sample inhalation process using a microcalorimetry device consists of inhalation of the sample →
- Inhalation of a fixed amount of air → Inhalation of solvent → - Inhalation of a fixed amount of air → Inhalation of sample. Therefore, as shown in FIG.
The flow rate is in the order of air C1 solvent d and air C1 sample b'. Moreover, at the same time as the sample is inhaled by the sample inhalation needle, the next sample is also stirred by the sample stirring rod.

Although the sample is inhaled according to such a sample inhalation process, in the conventional process, the sample inhalation needle is not cleaned at all immediately after the sample inhalation. That is, when the sample inhalation needle inhales the sample in the sample bottle set on the turntable, it rises once, is moved from the sample bottle to the solvent tank, and descends to inhale the solvent. Note that a certain amount of air is sucked in when moving from the sample bottle to the solvent tank. Then, when the solvent is inhaled, it rises again and is moved onto the sample bottle.
The next sample is inhaled, and the sample inhalation needle is not cleaned at all during this process. Therefore, the steps proceed one after another while the previous sample remains attached to the sample suction needle, albeit in a small amount.

As a result, the previous sample is successively mixed into the solvent in the solvent tank. Therefore, when the sample suction needle enters the next sample after inhaling the solvent, a small amount of the previous sample will be mixed into the subsequent sample. However, since the amount of sample to be tested is extremely small, if a small amount of the previous sample is mixed in, the purity will be greatly affected, making it impossible to perform accurate measurements.

Furthermore, the stirring rod used to stir the next sample is not cleaned at all, which is also one of the causes of loss of purity.

For these reasons, conventional devices were unable to perform accurate measurements.

"Problems to be Solved by the Invention" The present invention has been made in view of the above points, and includes cleaning the single sample suction needle immediately after inhaling the sample and cleaning the stirring bar at the same time. The present invention aims to provide a microcalorific value measurement device that enables accurate measurement.

"Means for Solving the Problems" The gist of the present invention is that a sample suction needle connects a sample in a sample bottle held on an intermittently rotating turntable and a solvent tank disposed outside the turntable. In a microcalorimetry device that alternately inhales the solvent in the sample, while stirring the next sample with a stirring rod when the sample is inhaled by the sample inhale needle, there is a passage connecting the pipe from the sample inhale needle and a solvent tank or washing water. A fixed body with a passage connecting the pipe from the water tank, a passage sliding in close contact with the fixed body and connecting the pipe to the detector, and a passage connecting the pipe from the wash water tank. A pipe from a sample suction needle that reciprocates horizontally in the diametrical direction of the turntable and goes up and down, a pipe from a solvent tank or a wash water tank, and a pipe to a detector are connected to each passage of the valve device consisting of a movable body provided. A pipe provided with a pump in the middle and a pipe provided with a pump in the middle from the washing water tank are connected respectively, and the movable body is shifted to appropriately switch the communication state of each passage, and on the other hand, A cleaning tip for the sample suction needle and a stirring rod is provided on the outside of the turntable, and an overflow port and a water inlet are provided on the side wall of the cleaning tip, and a drain port is provided at the bottom. A microcalorific value characterized in that a pipe from a storage tank is connected, and a pipe from the washing water tank is connected to the water inlet, and a pump is used to suck the washing water inside the washing tip into the waste liquid storage tank. Located in the measuring device.

Hereinafter, a more detailed explanation will be given based on the illustrated embodiment.

In the following explanation, an example will be given in which two samples are inhaled at the same time, but it is of course possible to inhale one sample at a time.

Fig. 1 is a front view of the entire device, Fig. 2 is a side view of the same, Fig. 3 is a plan view of the turntable with some parts omitted, and Fig. 4 is taken along I-I in Fig. 3. A line cross-sectional view, FIG. 5 is a vertical cross-sectional view with a portion of the elevating device such as a sample suction nail omitted,
6 is a partially omitted plan view, FIG. 7 is a vertical sectional view of the four-way valve device, FIG. 8 is a plan view of the same, FIG. 9 is a diagrammatic explanatory diagram of the entire device, and FIG. 10 to 15 are action explanatory diagrams.

In the figure, 1 is a housing and 2 is a turntable.

Further, the turntable 2 is provided with a large number of sample bottle holding holes 3, 3, . . . arranged in two rows in the circumferential direction.

4 is a sample bottle into which the sample is placed. 5 is a motor for driving the turntable 20 rotations. Reference numeral 6 denotes an annular water tank provided below the turntable 2 in the direction of rotation of the sample bottle 4, and contains cooling water (not shown) for cooling the sample bottle. 7 is the water tank 6
The cooling water injection dust 8 is the drain outlet of the water tank 6, and 9 is the drain outlet of the water tank 6.
This is the overflow pipe. 10.10 is a sample suction needle, which corresponds to the arrangement of the sample bottles 4, 4 in two rows.
I have it as a book. Further, each of the sample suction needles 10.10 has an air outlet slightly larger than the sample suction needle 10, which surrounds the sample suction needle 10.10 and has an air outlet near the tip of the sample suction needle 10. It is equipped with an air introduction tube 11 having a diameter. The sample suction needle 10 and the air introduction cylinder 11 are integrated with a holder 12, and the base of the sample suction needle 10 is connected to a connection port 1 of the holder 12 to a pipe leading to a four-way valve device described later.
2a, and the base of the air introduction tube 11 are connected to a connection port 12b of the holder 12 to a pipe leading to an air pump, which will be described later. 13.13 is a stirring rod for stirring the sample in the sample bottles 4, 4, and the sample suction needle 10.10
Similarly, there are two. Moreover, the stirring rod 13.13 is
The sample suction needle 10.10 is used to stir the sample before inhaling the sample with the sample suction needle 10.10.
0.10 along the rotational direction of the turntable 2 by one sample bottle. Also, the stirring rod 1
3 and 13 are rotated by air motors 14 and 14, respectively. The air motor 14 has blades 14 around the circumference of a rotating shaft 14a to which a stirring rod 13 is fixed to the lower end.
Several blades b are fixed and rotated by blowing wind onto the blades i4b and x4b. Incidentally, FIG. 9 shows one in which a normal electric motor 14' is used in place of the air motor 14. Then, the stirring rod 13
, 13 and the sample suction needle 10.10 are attached to a slide plate in a lifting device such as a sample suction nail described later.

15 and 16 are cleaning tips, and the sample suction needle 10.
10 and stirring rods 13 and 13, respectively. The cleaning tips 15 and 16 have overflow ports 15a, 16a and water inlets 15b, 1 at the top of the side wall, respectively.
61) and a drain port 15C2160 is provided in a part. Furthermore, in the embodiment illustrated in FIG.
The cleaning tip 15 for the sample suction needle 10 has an inner diameter slightly larger than the outer diameter of the air introduction tube 11, including the upper opening portion. These cleaning tips 15 and 16 are arranged on the outside of the turntable 2 at approximately the same height as the sample bottle 4. In the illustrated embodiment, the sample suction nail is attached to a fixed support base in an elevating device such as a sample suction nail described later.

Reference numeral 17 denotes a device for lifting and lowering a sample suction nail, etc., to which a support frame 18, a motor 19 fixed perpendicularly to the support frame 18, and a screw 31121a screwed to a screw shaft 20 connected to a rotating shaft 19a of the motor 19 are fixed. a horizontal elevating support 21, a guide rod 22 of the elevating support 21, and a slide plate 23 slidably disposed in the diametrical direction of the turntable 2 above the elevating support 21; , a motor 26 fixed on the lifting support base 21 having a rack 24 provided on the slide plate 23 and a pinion 25 that meshes with the rack fixed to a rotating shaft for sliding the slide plate 23, and the slide plate 23. A switch actuator 27, 28 fixed to the switch actuator 23, a limit switch 29, 30 that opens and closes upon contact with the switch actuator 27, 28, and the support frame 18.
It also includes a fixed support base 31 fixed in parallel with the elevating support base 21. Note that 32 and 32' are sliding frames of the slide plate 23 fixed to the upper surface of the elevating support table 21.

33 is a four-way valve device. The four-way valve device 33 is connected to the base 3
- 4, a motor 35 fixed to the base 34 and capable of changing the rotational direction, fixed to the rotating shaft 35a of the motor 35, with a cross head 37 attached to the upper surface and a stepped portion 36 on the peripheral surface
It consists of a circular cam plate 36 provided with a circular cam plate 36, a switching operation section 40 consisting of limit switches 38 and 39 that are opened and closed by the stepped section 36a, and a valve body section 41. Also,
The valve main body portion 41 is composed of a fixed body 42 fixed to a support 34a extending laterally from the upper surface of the base 34, and a rotating body 43 whose upper and lower surfaces of the fixed body 42 are in sliding contact. The fixed body 42 also has four passages 42a, 42b, 420, 42d communicating from the lower surface side to the upper surface side.
is provided. Further, the rotating body 43 is integrated with the fixed body 42 by loosely inserting a support shaft 44 rising from the center of the fixed body 42 into a through hole in the center thereof, and connects the bottom surface of the rotating body 43 with the top surface of the fixed body 42 using a disc spring 45. The sliding contact surface is in close contact. Moreover, the rotating body 43 has seven rack parts 4 around it.
3', and the flange portion 43' is provided with a notched groove 43' into which the cross head 37 is slidably fitted. Furthermore, the rotating body 43 includes a passage 42a provided in the fixed body 42.

42b, 42c, and 42d, and four passages 43a, 43b, which communicate from the upper side to the lower side.
43c and 43d are provided.

46 is a water tank containing cleaning water, and 47 is a waste liquid storage tank. 48 is an air pump, and 49 is a pipe connected to the air pump 48 at one end and to the connecting port 12b of the two boulders 12, 12 at the other end. 50 has one end connected to the connection port 12 of one of the two holders 12.
one end side is connected to a, and the other end side is connected to the valve body portion 41.
This is a pipe connected to the passage 42a of the fixed body 420 in .

A pipe 51 has one end connected to the connection port 12a of the other holder 12 of the two holders, and the other end connected to the passage 420 of the fixed body 42 in the valve body 41. It is. 52 is a pipe having one end connected to the rotating body 430 passage 43b in the valve body 41 and the other end connected to the sample mixer 52a;
A pump 53 is disposed in the middle. A pipe 54 has one end connected to the passage 43a of the rotating body 430 in the valve body 41, and the other end connected to the same sample mixer 52a to which the pipe 52 is connected, and a pump 55 is connected in the middle. has been set up. In addition, these pipes 52
．． 54 is connected to the sample mixer 52a and then unified and connected to the detector 52b. A pipe 56 has one end connected to the passages 42b and 42d of the fixed body 42 in the valve body 41, and the other end connected to a solvent tank 56a containing a solvent. A pipe 57 has one end connected to a water tank 46 containing cleaning water and the other end connected to a three-way solenoid valve 58, and a pump 59 is disposed in the middle. A pipe 60 has one end connected to the three-way solenoid valve 58 and the other end connected to the passages 43a and 43Cj of the fixed body 43 in the valve body 41. A pipe 61 has one end connected to the three-way solenoid valve 58 and the other end connected to the three-way solenoid valve 62. 63 is the three-way solenoid valve 62
This is a pipe whose one end is connected to the water inlets 15t) and 15b of the two cleaning tips 15 and 15 at the other end. A pipe 64 has one end connected to the three-way solenoid valve 62 and the other end connected to the water inlets 16b, 16b of the two cleaning cups 16, 16. 65 has one end connected to the drain port 15 of the two cleaning tips 15.15.
0.150, and the other end is connected to the three-way solenoid valve 66. 67 has one end connected to the three-way solenoid valve 66, and the other end connected to the two cleaning tips 16.
These are pipes connected to the drain ports 16Cj and 160 at ゜16.

68 has one end connected to the 30,000 solenoid valve 69, and the other end connected to the overflow ports 15a, 15a, 16a, 16a of the four cleaning tips 15, 15, 1616.
This is a pipe connected to. A pipe 70 has one end connected to the three-way solenoid valve 66 and the other end connected to the three-way solenoid valve 69. 71 has one end connected to the three-way solenoid valve 69, and the other end connected to the waste liquid storage tank 47 through a nine-way valve. 72 has one end connected to the waste liquid storage tank 47
It is a nokuib connected to the vacuum pump 73 in the middle.
has been set up.

"For work" Next, the operation of the present invention having the above configuration will be explained.

At the start, the sample suction needle 10.10 is positioned above the cleaning tip 15.15, and each tube, solenoid valve, and valve body of the four-way valve device are placed in the flow path during cleaning. It is set. The operation starts when the turntable rotates 20 times, and when the turntable 2 starts rotating, the sample suction needle 10.10 and the stirring rods 13, 13 move onto the turntable 2, and at the same time, the stirring rods 13, 13 rotate and Air is supplied to the air introduction cylinder 11 by operating the air pump 4B. At this time, the valve body 41 of the four-way valve device is switched, and the sample inhaled by the sample suction needle 10.
A flow path is formed such that the liquid flows through the detector (not shown). At the same time, pump 5 for about 1 to 9 seconds.
3.55 causes air to be sucked in from each of the sample suction needles 10.10, so that the air that is between the sample that has already been sucked in and the sample that will be sucked in later is sucked in. Once this is completed, the sample suction needle 10.10 and the stirring bar 13.1
3 descends and enters the sample bottle 4. As a result, the sample in the sample bottles 4, 4 is sucked up from the sample suction needle 10.10, and the valve body 4 of the pipe 50, 51.
The liquid is sucked up into the pipes 52 and 54 through the passages 42a, 43b, 420, and 43d. Note that the sample suction time is appropriately set depending on the flow rate. In addition, while the sample is being sucked by the sample suction needle 10.10, air is released from the lower end of the air introduction tube 11.11 to prevent the sample from settling. Next, the sample suction needles 10, 10, which are stirring the sample to be aspirated, rise to suck air for several seconds. still,
This air suction time is appropriately set according to the time it takes for air to pass from the needle tip to the valve body 41 of the 40,000 valve device. Next, the valve body 41 of the four-way valve device is switched, and in this case, the valve body 41 is switched to the fixed body 4.
The passage 42b of No. 2 and the passage 43b of the rotating body 430 are in communication with each other, and the passage 42d of the fixed body 42 and the passage 43d of the rotating body 43 are in communication with each other. In this state, the pump 53
55 is activated for a predetermined period of time to draw solvent into pipes 52,54. The suction time by the pumps 53 and 55 is also set appropriately depending on the flow rate. Next, the valve main body 41 of the four-way valve device is switched, and the flow path is again switched to the above-mentioned flow path during sample intake, and a predetermined amount of air is sucked from the sample intake needle 10.10. Next, sample suction needle IQ, 10 and stirring bar 1
3.13 cleaning is performed.

First, the sample suction needle 10.10 and the stirring rod 13.13 are in the starting position, that is, the cleaning tip 15, 15, 16° 16
Move up. The air pump 48 is then activated to send air into the air introduction tube 11.11. At the same time, the sample suction needle 10.10 and the stirring rod 13.13 are cleaned by the cleaning tip 15.
, 15, 16, 16.

At this time, each pipe and solenoid valve are switched to form the flow path shown by the thick line in FIG. That is, the cleaning water is supplied to the pipe 57.
3-way solenoid valve 58, valve body 4 of the vibro 0.4-way valve device
1. A flow path is formed so that the sample flows through the pipe 50.51 to the sample suction needle 10.10.The valve body 41 is
At this time, the passage 42a of the fixed body 420 and the passage 43a of the rotary body 430 are in communication with each other, and the passage 42c of the fixed body 42 and the passage 430 of the rotary body 43 are in communication with each other. Also,
On the other hand, at the same time, a flow path from the cleaning tip 15.15 to the waste liquid storage tank 47 is also formed. That is, cleaning tip 15.
The washed waste liquid sucked from 15 is transferred to vibro 5 and solenoid valve 6.
6. A flow path is formed so that the waste liquid flows into the waste liquid storage tank 47 via the pipe 70, the electromagnetic valve 69, and the pipe 71.

With this setting, when the pump 59 is activated and sucks the wash water from the water tank 46 and sends it to the sample suction needle 10.10, the inside of the sample suction needle 10.10 is completely cleaned by the wash water. Ru. Further, the washing water flowing down from the tips of the sample suction needles io, io is sucked out from drain ports 150° 150 provided at the bottoms of the washing tips 15, 15, and flows into the waste liquid storage tank 47.

Note that suction of this waste liquid is performed by operating the vacuum pump 73.

After the internal cleaning of the sample suction needle 10.10 is performed as described above, the external cleaning of the sample suction needle 10.10 is then performed.

First, the pipes and solenoid valves are switched to form the flow path shown by the bold line in FIG. That is, the cleaning water flows through the pipe 57.
3-way solenoid valve 58, Vibro 1. 3-way solenoid valve 62, Vibro 3 and then cleaning tip 15° 150 water inlet 15b,
15k). Also, at the same time, the cleaning water overflows into the overflow ports 15a of the cleaning cups 15, 15.

A flow path is also formed that flows from the vibro 8, through the three-way solenoid valve 69 and the pipe 71, to the waste liquid storage tank 15a. With the settings set in this way, the pump 59 operates and sucks the cleaning water from the water tank 46 to the cleaning tip 15.15.
send to. By filling the cleaning tip 15.15 with cleaning water in this way, the sample suction needle 10,
10 is for cleaning the outside. The overflowing cleaning water is discharged from the overflow ports 15a, 15a through the vibro 8, three-way solenoid valve 69, and pipe 71 to the waste liquid storage tank 47. In addition, this is vacuum pump 7
This is done by the operation of 3.

Once the sample suction needle 10.10 has been externally cleaned in this manner, the stirring rods 13, 13 are then cleaned.

In this case, each pipe and solenoid valve are switched to form the flow path shown by the bold line in FIG. That is, the cleaning water flows through the pipe 57, the 3-way solenoid valve 58, the vibro 1.3-way solenoid valve 62,
Water inlet 16k of cleaning tip 16°16 via Vibro 4
), 16b. Note that the flow path from the overflow ports 16a, 16a to the waste liquid storage tank 47 has already been formed when washing water is injected into the washing tip 15.

In this state, the pump 59 is operated to suck cleaning water from the water tank 46 and send it to the cleaning tip 16, 16, thereby cleaning the stirring rods 13, 13.

As described above, the sample suction needle 10.10 and the stirring bar 13.
Once step 13 is done, each wash step 15.15
, 16, 16. This is done first from the cleaning tip 15.15.

In this case, as shown by the bold line in FIG.
, the flow path is switched so that the waste liquid flows into the waste liquid storage tank 47 via the pipe 71. Then, the vacuum pump 73 is operated to suck out the cleaning water in the cleaning cup 15°15.

Next, the cleaning water from the cleaning tips 16.16 is drained, but in this case, as shown by the thick line in FIG. The flow path is switched so that the waste liquid flows into the waste liquid storage tank 47 via the solenoid valve 66, the pipe 70, the three-way solenoid valve 69, and the pipe 71. And vacuum pump 73
is operated to suck out the washing water in the washing kelp 16°16.

After the shiso cleaning is performed in this way, the sample suction needle 1
0.10, the stirring rods 13 and 13 rise and return to the initial set state. Further, when the sample suction needle 10.10 and the stirring rod 13.13 are raised, the flow paths of the pipe and the electromagnetic valve are switched, as shown by the thick line in FIG. 15. That is, the water droplets sucked in from the overflow ports 15a, 15a, 16a, 16a of the cleaning tips 15, 15, 16.
A flow path is formed so that the waste liquid flows into the waste liquid storage tank 47 through d.

Then, a vacuum pump 72 is used to suck it.

As a result, water droplets adhering to the outer periphery of the air introduction tube 11.11 outside the sample suction needle 10.10 are sucked off by suction from the overflow ports 15a, 15a. Furthermore, since the outer diameter of the air introduction tubes ii and ii and the inner diameter of the opening of the cleaning tips 15a and 15a are almost the same, water droplets adhering to the outer periphery of the air introduction tubes 11 and 11 are almost completely absorbed. It is.

One process is completed by the above steps.

In addition, in the above explanation, when two samples are inhaled at the same time, 4
Although this has been explained using an example, it is of course possible to inhale the sample one by one.
6a and the wash water tank 46 are installed separately, but if the wash water also serves as a solvent, the pipe 56 of the solvent tank 56a may be connected to the wash water tank 46.

Next, the operating mode of each device will be explained.

- First, the turntable 2 will be explained. The turntable 2 is intermittently rotated by a motor 5. Next, the sample suction needle and stirring bar will be explained. The sample suction needle 10.10 and the stirring rods 13, 13 are moved up and down in the following manner. First, to explain the elevation, this elevation is performed by the operation of the motor 19 in the lifting/lowering device 17 for the sample suction nail, etc.
This is done by rotating a. That is, the state shown in FIG. 5 is a state in which the rotary shaft 19a rotates, the screw shaft 20 rotates, and the elevating support base 21 is raised, and in this state, the elevating support base 21 is raised. In order to
3 is also rising.

When descending, the opposite is true, and the motor 19
By rotating the 0-rotation shaft 19a in the opposite direction, the lifting support base 21 is lowered, and thereby the sample suction needles 10, 1
0, the stirring rod 13.13 is also lowered. Also, to explain the movement in the horizontal direction, the motor 26 operates to rotate the pinion 25, and the rack 2 that meshes with the motor 26 operates to rotate the pinion 25.
4 to move the slide plate 23 in the horizontal direction.

Next, to explain the four-way valve device, the motor 35 operates to reciprocate the circular cam plate 36 within a certain range.
This rotation causes the crosshead 37 and the flange portion 43 to
The rotary body 43 of the valve body 410 is rotated through the notched groove 43'. By this rotation, the passages provided in the fixed body 42 and the rotary body 43 are appropriately communicated with each other.

"Effects of the Invention" The present invention has the above-mentioned structure and operation, and is designed to completely clean the single-use sample inhalation needle from the inside and outside immediately after inhaling the sample, and also to clean the stirring rod at the same time as the trench. Because of this, there is no risk of losing the purity of the sample even if the operation is continued, and therefore accurate measurements can be made.

Moreover, since all cleaning is done automatically, there is no time loss, and there are many practical benefits.

[Brief explanation of drawings]

Fig. 1 is a front view of the entire device, Fig. 2 is a side view of the same, Fig. 3 is a partially omitted plan view of the turntable, Fig. 4 is a sectional view taken along line I-X in Fig. 3, Fig. 5 is a partially omitted vertical sectional view of the elevating device such as a sample suction nail, etc., Fig. 6 is a partially omitted plan view of the same, and Fig. 7 is a vertical sectional view of the four-way valve device. , FIG. 8 is a plan view of the same, FIG. 9 is a diagrammatic illustration of the entire device, FIGS. 10 to 15 are action illustrations, and FIG.
The figure is a partially enlarged sectional view of the pipe that sucked the sample and solvent. 1... Housing 2...
・・Turntef λ4・・・・Sample bottle
10... Sample suction needle 11... Air introduction cylinder 12... Holder) 3...
・Stirring rod ts, ia...Cleaning cup 15a, 16a... Overflow port 15b 16b... Water filler port 150
, 160...Drain port 17...Elevating and lowering moving device such as sample suction nail 19...Motor
20... Screw shaft 21... Lifting support base
23...Slide plate 24...Rack 25...Pinion 26...
...Motor 29, 30...Limit switch: (1...
...Fixed support stand 33...Four-way valve device 34...Base 35...Motor 36.
...Circular cam plate 37...Crosshead 38.39...Limit switch 40
......Switching operation part 41...Valve body part 42...Fixed body 42a, 42b, 42c, 42d=---
・Passage 43...Rotating bodies 43a, 43b, 43C, 4311...-
Passage 43'...Flange part 43'...
...Notch groove 44 ... Support shaft 4
5...Disc spring 46...Aquarium
47... Waste liquid storage tank 48... Air pump 49.50.51, 52, 54, 56, 57. [0,6
1,63,64°65,67,68,70.71
, 72...Pipe 53 55 59...
・Pump 5B, 62.66...3-way solenoid valve 73...
··Vacuum pump.

Claims (2)

[Claims] (1) The sample suction needle alternately sucks in the sample in the sample bottle held on the turntable that rotates intermittently and the solvent in the solvent tank placed outside the turntable. In a microcalorimetry device that stirs the next sample with a stirring rod, a fixed body is provided with a passage connecting a pipe from a sample suction needle and a passage connecting a pipe from a solvent tank or a washing water tank. , a turn is attached to each passage of the valve device, which is a movable body that slides in close contact with the fixed body and has a passage connecting the pipe to the detector and a passage connecting the pipe from the wash water tank. A pipe from a sample suction needle that moves back and forth horizontally in the diametrical direction of the table and rises and falls;
Connect a pipe from the solvent tank or the wash water tank, a pipe with a pump halfway to the detector, and a pipe with a pump halfway from the wash water tank, and shift the movable body. The communication state of each passage is changed as appropriate,
On the other hand, a cleaning cup for the sample suction needle and a stirring rod is provided outside the turntable, and an overflow port and a water inlet are provided on the side wall of the cleaning cup, and a drain port is provided at the bottom of the cleaning cup. A pipe from the waste liquid storage tank was connected to the mouth, and a pipe from the wash water tank was connected to the water inlet, and a pump was used to suck the wash water in the wash cup into the waste liquid storage tank. Features of microcalorie measuring device. (2) The sample suction needle alternately sucks in the sample in the sample bottle held on the turntable that rotates intermittently and the solvent in the solvent tank placed outside the turntable; In a microcalorimetry device that stirs the next sample with a stirring rod, a fixed body is provided with a passage connecting a pipe from a sample suction needle and a passage connecting a pipe from a solvent tank or a washing water tank. , a turn is attached to each passage of the valve device, which is a movable body that slides in close contact with the fixed body and has a passage connecting the pipe to the detector and a passage connecting the pipe from the wash water tank. A pipe from a sample suction needle that moves back and forth horizontally in the diametrical direction of the table and rises and falls;
Connect a pipe from the solvent tank or the wash water tank, a pipe with a pump halfway to the detector, and a pipe with a pump halfway from the wash water tank, and shift the movable body. The communication state of each passage is changed as appropriate,
On the other hand, a cleaning cup for the sample suction needle and a stirring rod is provided outside the turntable, and an overflow port and a water inlet are provided on the side wall of the cleaning cup, and a drain port is provided at the bottom. A pipe from the waste liquid storage tank is connected, and a pipe from the washing water tank is connected to the water inlet, and a pump is used to draw the washing water in the washing cup into the waste liquid storage tank, and the sample is then sucked. A plurality of needles are provided, and the number of pipes to the detector corresponds to the number of sample suction needles, and after the plurality of pipes are connected to a single sample mixer, a single pipe is connected from the sample mixer to the detector. 1. A microcalorimetry device characterized in that a sample is sent out using a microcalorimetry device.