JPH059646Y2 - - Google Patents

Description

[Detailed description of the invention] Industrial application field The present invention relates to a bubble crusher for a gas analyzer, and more specifically, it is used when analyzing gas in glass bubbles. This invention relates to a bubble crusher for introducing gas into an analyzer.

BACKGROUND ART Gas generated when raw materials are heated and melted may remain in the form of microbubbles in glass products, and products in which such bubbles remain are considered to be defective. Therefore, in order to solve the above-mentioned problem of residual bubbles, the gas inside the bubbles is analyzed to know the composition and total amount, and the cause of the bubbles is inferred and countermeasures are taken.

In the above analysis, generally a piece of glass containing bubbles is extracted from a glass product as a sample piece, the sample piece is broken with a gas extraction device called a bubble crusher, and the gas inside the bubbles is extracted. This is done by introducing the gas into an analyzer, and examples of the analyzer include a gas chromatograph that introduces the gas inside the bubbles together with a carrier gas and analyzes the difference in movement speed of each gas component, and a gas chromatograph that introduces the gas inside the bubbles together with a carrier gas and analyzes the difference in movement speed of each gas component. A mass spectrometer or the like is used that performs analysis by introducing and ionizing the ions and electrically detecting the ions.

As the bubble crusher, for example, the 8th
1, 9, and 10 are currently in use.

In the device shown in FIG. 8, a sample table 2 is screwed onto the lower part of the main body 1 from below, and a pressing pin 3 having a conical tip is screwed onto the upper part of the main body 1.
With purge gas being supplied between the main body 1 and the side surface of the pressing pin 3, and carrier gas being supplied between the pressing pin 3 and the sample table 2, the pressing pin 3 is further screwed into the pressing pin. 3 and a saucer 2a having a conical recess fixed to the upper surface of the sample table 2, the sample piece S is crushed and the gas inside the bubbles is introduced into the analyzer [gas chromatograph] together with the carrier gas. It is something.

In the case shown in FIG. 9, the extracted sample piece S is placed on the sample table 5 so that the bubble b is located near the bottom surface, and the sample piece S is airtightly placed on the sample table 5 by a clamper 6. The needle 7 passing through the center of the sample table 5 pierces the bubble b from below, and the gas inside the bubble b is transferred to the analyzer from the gas inlet 9 along with the carrier gas supplied from the gas supply port 8. It is designed to flow towards a [gas chromatograph].

What is shown in FIG. 10 is an airtight container 12 constructed by screwing together an upper container body 10 and a lower container body 11.
The sample piece S is housed in the chamber, and the sample piece S is placed on the lower vessel body 11 side via the plunger 14, thin copper plate 15, and sealing cup 16 by means of the operating screw 13 disposed on the upper vessel body 10. By pressing toward the needle point 17, the sample piece S
The gas inside the bubble is introduced into the analyzer by vacuum suction through the gas outlet 18 provided in the lower vessel body 11.

Furthermore, although not shown, instead of the above-mentioned flat sample piece, a sample piece formed into a capillary shape by stretching glass bubbles is inserted into a flexible tube arranged in the carrier gas introduction path, and the above-mentioned Japanese Patent Application Laid-Open No. 1983-1997 introduced a method in which the gas inside the bubbles was introduced into an analysis device (gas chromatograph) by breaking the sample piece.
It is disclosed in Publication No. 41350.

Problems that the invention attempts to solve By the way, the above bubble crusher had the following problems.

First of all, all of the bubble crushers shown in FIGS. 8 to 10 above are operated manually by the operator, and the bursting of the bubble b in the sample piece S is due to the delicate touch of the human fingers. Detection is done by sensation or small sounds, and therefore, the work of crushing bubbles B using a bubble crusher requires a person to be present at all times, and requires skill.

In addition, when using a sample piece in which bubbles are stretched into a capillary shape, it is necessary to cut out the glass piece containing the bubbles and then stretch it into a capillary shape, which requires a large number of man-hours and requires a lot of skill. The problem is that it is necessary and not common.

Secondly, when the bubble b of the sample piece S is crushed by the bubble crusher, if the above-mentioned crushing sound and sensation are overlooked and the sample piece S is further pressurized, the sample piece S will be crushed into pieces. In this case, the gas in the bubbles is adsorbed on the newly formed fracture surface, and the degree of adsorption of gas on the glass surface is different for each gas component. There is a problem in that the amounts and compositions are analyzed differently than they actually are.

Means for Solving the Problems The present invention was devised in view of the above-mentioned problems, and it is possible to break a sample piece containing glass bubbles by pressing a needle in an airtight sample chamber. The bubble crusher extracts the gas from the sample chamber and introduces it into the gas analyzer via the pipe line, and the bubble crusher includes a needle holder in the center that holds a needle so as to be movable up and down in an airtight state, and the needle holder. a sample table located below, having a pedestal for the sample piece on its upper surface, and forming an airtight sample chamber between the needle holder and the lower surface of the needle holder by pressure contact with the needle holder; and the needle holder or the sample. a first lifting device for moving the table toward the sample table or the needle holder and pressing them together with a predetermined force; a second lifting device for inching and lowering the needle toward the sample piece in the sample chamber; After the sample table and the needle holder are brought into pressure contact by the vibration sensor which is disposed on the sample table and detects the sound when the sample piece breaks due to the pressure of the needle, and the first lifting device, the second lifting device This is a bubble crusher for a gas analyzer that includes a control device that operates the device until a signal from a vibration sensor is input.

Function The bubble crusher of the gas analyzer according to the present invention places a glass sample piece wrapped in bubbles on the sample table, and operates the first lifting device by the control device to bring the sample table and needle holder into pressure contact. When it is detected that an airtight sample chamber in which the sample piece is accommodated is formed by pressure contact between the sample table and the needle holder, the control device inches the needle toward the sample piece using a second lifting device. By lowering the needle and detecting the instantaneous sound when the sample piece is broken by the vibration sensor, the controller stops the lowering operation of the needle and drains the gas in the bubbles of the sample piece. The sample is introduced into the analyzer via the route.

Embodiment FIGS. 1 to 7 show an embodiment of a bubble crusher of a gas analyzer according to the present invention.
In this embodiment, the analyzer A to which the bubble crusher B is connected is a gas chromatograph into which a sample gas is introduced together with a carrier gas.

In the drawing, 20 is a frame of bubble crusher B, 30 is a sample table, 40 is a needle holder that fits with the sample table 30 to form a closed container, 50 is a needle supported by the needle holder 40, and 60 is a vibration sensor. , D ₁ is the lifting device for the sample table 30, D ₂ is the lifting device for the needle 50, C is the lifting device D ₁ ,
The control device of D ₂ is shown.

A support frame 21 for the needle holder 40 is horizontally fixed approximately at the center of the frame 20, and a pair of support arms parallel to each other are provided above and below the support frame 21, respectively. 22a, 22b, 23a, and 23b are horizontally fixed to the frame 20. Between each pair of support arms 22a, 22b, and 23a, 23b
Guide rods 24 and 25 are vertically installed and fixed on the inner side of the gap. A support block 26 for a needle holder 40 is disposed on the upper guide rod 24 so as to be slidable up and down along the central axis of the guide rod 24, and a support block 26 for a sample table 30 is disposed on the lower guide rod 25. A support block 27 is disposed along the central axis of the guide rod 25 so as to be vertically slidable.

The sample table 30 is connected to the support block 2.
No. 7 is inserted into the mounting hole 27a at the tip of the sample table 30 and fixed with a screw.
As shown in the figure, a substantially cylindrical recess 31 is formed. A recess 32 having a smaller diameter is formed in the bottom of the recess 31, and a sample holder 33 is disposed within the recess 32. The above sample holder 33
As shown in FIG. 3, this sample holder 33 has a substantially disk shape and has perpendicular V-shaped grooves 33a, 33a formed on its upper surface.The diameter of this sample holder 33 is smaller than that of the recess 32, and the thickness is , is set shorter than the depth of the recess 32. An O-ring O ₁ is disposed on the bottom surface of the recess 31 around the recess 32 in order to maintain airtightness with the needle holder 40 .

Furthermore, a vibration sensor 60 is attached to the lower surface of the sample table 30.

The needle holder 40 is fitted into the mounting hole 21a at the tip of the support frame 21 and fixed with screws, and is coaxial with the sample table 30.

The lower end of the needle holder 40 is formed to have a diameter slightly smaller than the diameter of the recess 31 of the sample table 30, and the center of the lower surface of the needle holder 40 has a recess 32 of the sample table 30 as well as a sample chamber 4.
A recess 41 constituting the recess 7 is formed, and the diameter of the recess 41 is the same as that of the recess 32 described above. Then, along the axis of the needle holder 40,
A through hole 42 having a smaller diameter than the recess 41 is bored, and a needle 50 is slidably inserted into this through hole 42. Further, the support frame 21 is provided on both sides of the upper part of the needle holder 40.
Purge gas conduits 43a and 43b are provided on both sides of the lower surface, and are provided on both sides of the lower surface. Conduits 44a and 44b are provided. Of the carrier gas pipes 44a and 44b, the downstream pipe 44b is connected to the gas chromatograph A via an electromagnetic switching valve (hereinafter simply referred to as a switching valve) V.
It is connected to the.

The needle 50 is inserted into the through hole 42 of the needle holder 40 with its base end fixed to the support block 26, and the tip of the needle 50 is formed into a substantially conical shape as shown in the figure. ing. A total of four annular grooves 51, two each, are formed on the tip side and the center of the needle 50, and each of the annular grooves 51 has an O.
A ring O ₂ is fitted to maintain airtightness between the through hole 42 and the through hole 42 .

The elevating device D ₁ for the sample table 30 is composed of a drive motor M ₁ , a lead screw 70 and a nut 71 .

In this embodiment, a torque motor is used as the drive motor _M1 , and this torque motor _M1 is attached to the lower end of the frame 20 via a bracket 28.

The lead screw 70 has a guide rod 25 on the front side between the support arms 23a and 23b.
It is rotatably supported parallel to the
This lead screw 70 is connected to the support block 27.
It is screwed together with a nut 71 disposed at. The lower end of a lead screw 70 protruding from the lower support arm 23b is connected via a joint 72 _to a motor shaft _m1 of a torque motor M1.

The lifting device D ₂ for the needle 50 also includes a drive motor M ₂ , a lead screw 73, and a nut 74, similar to the lifting device D ₁ .

In this embodiment, a step motor is used as the drive motor M ₂ in the lifting device D ₂ for the convenience of controlling the inching and lowering operation of the needle 50. This step motor M ₂ is connected to the upper end of the frame 20 via a bracket 29. installed.

As described above, the lead screw 73 is rotatably supported on the front side between the support arms 22a and 22b so as to be parallel to the guide rod 24.
is screwed into a nut 74 disposed on the support block 26. And the upper support arm 22a
The upper end of the lead screw 73 protruding from the shaft is connected to the motor shaft _m2 of the step motor M2 via _a joint 75.

The control device C controls the operations of the torque motor M ₁ , step motor M ₂ and switching valve V based on signals from an operation switch (not shown) of the bubble crusher B and the vibration sensor 60.

Reference numbers 81 to 84 in the figure each indicate proximity switches, 81 and 83 are proximity switches for setting the standby positions of the sample table 30 and the needle 50, and 82 and 84 are proximity switches for setting the standby positions of the sample table 30 and the needle 50, respectively. The proximity switches 81 to 84 are also connected to a control device C for setting the movement limit of the needle 10.

Now, the procedure for gas analysis of glass bubbles using bubble crusher B having the above configuration will be explained below. still,
In the initial state, the sample table 30 is at the lowest position, the needle 50 is at the highest position and in a standby state, and the purge gas conduits 43a, 43b are in a standby state.
It is also assumed that gas has not yet been supplied to the carrier gas pipes 44a and 44b, and that the switching valve V is open to the atmosphere. Furthermore, sample piece S
As shown in FIG. 4, the bubble b is sampled from the glass product so that it is located approximately in the center, and has a generally rectangular shape that can be accommodated in the recess 32 of the sample table 30. , a slit-like notch is cut out on both sides of the bubble b along the axis passing through the bubble b for convenience in breaking the sample piece S, and
It is designed so that the fracture surface when cracked is small.

First, the sample piece S is placed on the sample holder 33 housed in the recess 32 of the sample table 30, and the operation switch (not shown) is turned on to operate the torque motor _M1 . Then, the torque motor M ₁ rotates the lead screw 70 to rotate the sample table 30 together with the support block 27.
to rise. Recess 31 of the sample table 30
and the lower end of the needle holder 40 are fitted together, and when the bottom surface of the recess 31 and the lower end surface of the needle holder 40 come into contact, the torque motor _M1 is stopped by receiving a reaction force that balances the drive torque, and this torque motor
Upon stopping _M1 , the control device C stops supplying power to the torque motor _M1 . In this state, the sample table 30 is pressed against the needle holder 40 with a predetermined pressure as shown in _FIG . Since airtightness with the lower end surface is maintained, an airtight sample chamber 47 is formed by the recess 32 of the sample table 30 and the recess 41 of the needle holder 40.

Next, a carrier gas, e.g.
Supply He gas. That is, the purge gas conduit 43a is connected to the through hole 4 of the needle holder 40.
2 and the side surface of the needle 40 and then released into the atmosphere from the purge gas pipe 43b to prevent outside air from leaking into the sample chamber 47 due to the downward movement of the needle 50. , from the carrier gas pipe 44a to the sample chamber 4.
After He gas is introduced into the sample chamber 47, it is discharged into the atmosphere from the carrier gas conduit 44b, thereby replacing the residual air in the sample chamber 47 with the He gas.

After maintaining the above state for a predetermined time, the control device C controls the switching valve V so that the carrier gas flows from the pipe line 44b toward the gas tomatograph A.
At the same time, a high frequency pulse signal is sent to the step motor _M2 for a predetermined period of time.

Then, the step motor _M2 rotates at a predetermined amount at a high speed, rotates the lead screw 73, and quickly moves the needle 50 together with the support block 26 to a predetermined position and lowers it, and then moves to an inching operation. The step motor _M2 above is
The needle 50 rotates by a predetermined minute angle in response to a low frequency pulse signal from the control position C, and this intermittent rotation is transmitted as an intermittent fine downward movement of the needle 50 due to the screwing relationship between the lead screw 73 and the nut 74.

Then, the tip of the needle 50 is connected to the sample chamber 4.
When the sample piece S breaks along the slit groove as shown in Fig. 7, the bubble b bursts. The cracking sound at the moment when the vibration sensor 60
Based on the signal from the vibration sensor 60, the control device C controls the step motor _M2.
interrupts the transmission of pulse signals to.

Through the above series of operations, the gas in the bubble b is taken out into the sample chamber 47, and this gas is introduced into the gas chromatograph A from the pipe 44b through the switching valve V, together with the carrier gas, to determine the composition and the absolute value of each component. quantity is analyzed.

After this, the switching valve V is opened to the atmosphere by a signal from the control device C, and the pulse motor M ₂
A pulse signal of a predetermined high frequency is input to reverse the rotation, and the needle 50 is raised and returned to its original position, and the torque motor _M1 is reversed to lower and return the sample table 30 to its original position.
The proximity switch 83 determines whether the needle 50 and sample table 30 have returned to their original positions.
and 81, and the signals from the proximity switches 83 and 81 cause the control device C to:
The driving of the step motor _M2 and torque motor _M1 is interrupted.

After that, the broken sample piece S is taken out from the sample pedestal 33, a new sample piece S is placed on the sample pedestal 33, and the gas analysis is continued as described above.

In the above embodiment, a plurality of sample tables 30 are arranged in parallel on the support block 27, and
Each sample table 30 may be sequentially controlled and moved directly below the needle holder 40 on the support block 27 via a feeding mechanism, so that a plurality of sample pieces S may be subjected to gas analysis one after another.

Further, in the above embodiment, when a sample piece in which the bubble b is stretched into a capillary shape is used instead of the flat sample piece S, the V-shaped groove 33a formed in the sample holder 33 stabilizes the sample. Can be held in position.

Furthermore, although the bubble crusher of the above embodiment is compatible with a gas chromatograph, when it is compatible with a material spectrometer, the purge gas conduit 43
a and 43b are no longer necessary, and the carrier gas pipe 4
4a and 44b may be connected to a vacuum system.

Effects of the Device As explained above, according to the bubble crusher for gas analysis according to the present invention, once a sample piece containing glass bubbles is placed on the sample table, the controller automatically controls the The sample piece is housed in an airtight sample chamber formed by a sample table and a needle holder, and the sample piece can be broken by a needle.Moreover, the needle is used so that the sound at the moment the sample piece is broken is detected by a vibration sensor. As soon as a break is detected, the controller immediately stops the sample, which allows the sample to be broken without pulverizing it. This makes it possible to save labor and automate gas analysis, and to Adsorption is prevented and accurate analysis can be performed.

[Brief explanation of drawings]

1 to 7 show an embodiment of a bubble crusher for a gas analyzer according to the present invention, in which FIG. 1 is a front view, FIG. 2 is a side view including a partial cross section, Figure 3 is an enlarged perspective view of the sample holder;
The figure is an enlarged perspective view of a sample piece, and FIGS. 5 to 7 are enlarged longitudinal sectional side views of main parts for explaining the operation procedure. 8 to 10 are longitudinal sectional side views showing bubble crushers of conventional gas analyzers, respectively. S... Sample piece, b... Bubbles, A... Gas analyzer, B... Bubble crusher, C... Control device,
_D1 ...Sample table lifting device [first lifting device], _D2 ...Needle lifting device [second lifting device], 30...sample table, 33...sample holder,
40... Needle holder, 44b... Conduit, 47
...Sample chamber, 50...Needle, 60...Vibration sensor.

Claims (1)

[Claims for Utility Model Registration] A sample piece containing glass bubbles is broken by the pressure of a needle in an airtight sample chamber, and the gas within the bubbles is extracted from the sample chamber through a pipe line. The bubble crusher is introduced into a gas analyzer, and includes a needle holder that holds a needle in the center so that it can be raised and lowered in an airtight manner, and a holder that is located below the needle holder and that holds the sample piece on the top surface. a sample table having an airtight sample chamber formed between the needle holder and the lower surface of the needle holder by pressure contact with the needle holder; and the needle holder or the sample table;
a first elevating device for moving the needle toward the sample table or the needle holder and pressing them together with a predetermined force; a second elevating device for inching and lowering the needle toward the sample piece in the sample chamber; A vibration sensor is provided to detect the sound when the sample piece breaks due to the pressure of the needle, and after the sample table and the needle holder are brought into pressure contact by the first lifting device, the second lifting device is moved. 1. A bubble crusher for a gas analyzer, comprising a control device that operates until a signal from a vibration sensor is input.