JPS6015158Y2 - sample preparation machine - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a sample preparation machine for converting substances into glassy disks and solutions for use in analysis by chemical-physical methods.

It is well known that chemical analysis values of most substances can be measured from the emission spectrum and absorption vector when excited by electrons, X-rays, high temperatures, or electric arcs.

The ideal physical state of the substance before analysis is a homogeneous glass or a homogeneous solution.

The inventor discovered the sample preparation method in 1956 (Que
Department of Mines
P, R @ No, 327t (1956); Nor
elco Reporter Vol.3. P
3 (1957)).

This method makes X-ray analysis more accurate and has been adopted by many laboratories around the world.

This method is called the 1-melt method, the borax bed method, or the borax bed method.

The proposed method involves placing a mixture of the sample and a flux, e.g. borax, in a crucible, heating it until it melts, and injecting this melt into a ring of a heating plate, after cooling, obtaining a glass-like button for analysis. .

Although analysis by that method can give excellent results, the preparation of buttons as described in the original publication is problematic and inconvenient.

This means that the operator must frequently stir the crucible, handling heated materials is dangerous, the high heat and strong visible radiation from the flame are cumbersome and cumbersome, the life of the crucible is short, and the surface of the button is The surface is not smooth and requires a trained operator.

Conventional chemical methods for transforming substances in solution are complex;
It's time consuming and boring.

For example, in the case of a sample containing silica, acid dissolution requires several hours and many operations.

The method for transforming a solid sample into a glassy material as described above was improved by Crowe and Contree and published in the ASTM Journal.
l ofTesting and Evaluation
n, p. 382, September 1973) A solution is made instead of a glassy substance.

A glassy substance obtained by melting a sample using lithium metaborate as a flux can be completely dissolved by injecting a heated molten glassy substance of dilute nitric acid solution and stirring the solution for several minutes.

The present inventor has also discovered another fluxing agent.

It is clear that similar results can be obtained using, for example, lithium tetraborate, and that other liquid solvents exist for dissolving glassy materials.

Although machines were invented for the purpose of preparing glass buttons, these machines did not overcome all of the above-mentioned difficulties and had their own limitations.

For example, buttons of different sizes cannot be used if the buttons need to be polished before analysis and significant modifications are not made to the machine.

The button production rate is slow, and the machines are heavy, complex, and difficult to handle.

The initial cost of the machine is high and the cost of replacing the crucible is also high.

Machines have been built to prepare solutions from molten glass, but these machines have the same drawbacks as machines designed to make glassy buttons.

At present, to the best of the inventor's knowledge, there is an apparatus for simultaneously melting several mixtures of solid substances and fluxes, and an apparatus for simultaneously rawhing several combinations of glassy buttons and solutions from the above-mentioned molten glass. There are no machines.

The invented machine described below is easy to assemble and operate;
It is easy, flexible and economical.

Also, this machine can automatically and quickly chemically process several samples at the same time, converting each sample into glass buttons and solutions respectively, converting some samples into glass buttons and converting other samples into solutions. .

The machine of the present invention has four main functions: melting, homogenizing, pouring and melting.

One of the purposes of this invention is to melt many samples at the same time.
The object of the present invention is to provide an effective homogenizing device, in which various heat sources, such as gas burners, are connected to a column supplying energy to this heat source, and the columns are connected via a rocking joint, by means of which the column and A heat source attached to the column is moved in an oscillating motion about a vertical axis, and the crucible containing its contents is held above the heat source and moved with the heat source.

As soon as the material begins to melt, the stirring action of the crucible causes intense convection of the liquid, thus reducing the melt homogenization time of the melt.

In the present invention, in order to provide a simple method of sample casting, in a new device for holding and moving the crucible and mold, a fork holds a flat-bottomed mold above the crucible, and a shaft of the fork that holds the mold is loosely attached. The above fork is held by another installed fork.

During casting, the mold is moved beneath the crucible and the crucible is rotated before reaching its final position, transferring the melt to the mold where solidification is occurring.

In the present invention, the same fork is used to hold the crucible, but with a fork provided for the mold, in order to provide a simple method of preparing a solution from heated glass that is compatible with the process of casting glassy discs. Do not set a mold on the

During casting, the crucible holder is moved from the burner to a beaker adjacent to the burner and containing a solution for melting the glass;
The machine was designed so that molten glassy material was injected.

In this way, a glass button and a solution can be obtained at the same time.

In the present invention, in order to provide a simple and quick method of melting glassy substances, we introduce an apparatus used to raw the homogeneous material in molten glass, stirring the solution and then stirring an insoluble metal disc that is placed in this solution. used for

The invention will now be explained in detail with reference to the drawings.

FIG. 1 is a sectional view of the machine showing only one burner.

The machine shown in Fig. 1 has a rocking joint that allows the columns 1 and 2 to be tilted in the longitudinal and lateral directions but prevents the column 2 from rotating around its axis; An assembly of several gas burners 1 mounted around the column 2 by means of pipes 3 supplying gas or air to the burners 1 together with 60; speed for rotating the platform 8 which maintains the drive mechanism for various mechanical operations; Variable motor 7; spring 9 to pull the column in the vertical position when the motor 7 is at rest and an air regulating valve 6 to minimize shocks when the column 2 is stopped.
2 (see FIG. 4); a cam 10 that pushes the column 2 into an inclined position when the platform 8 begins to rotate; a holder 11 for the crucible. holder 12 for the mold, holder 13 for the beaker; column for inverting the crucible 16 (Fig. 6-7.8) in order to transfer the molten glassy substance into the mold 17 or beaker 18 (Fig. 9); Gear mechanism 14, 1 provided at the upper end of 2
5; magnetic clutch assembly 19, 20 on the platform 8 for driving the gear assembly 14, 15 during casting; with electronics for controlling the operations that have to be carried out with fully adjustable operating conditions;

The individual operations of the machine according to the invention will be explained in detail with reference to FIGS. 1 to 9. FIG.

The rocking joint shown in FIGS. 1 and 5 consists of three concentric rings 4. 5. 6 and two mutually perpendicular rotation axes 2
4. From 25 (Fig. 5), the outer ring 4 is the frame 2 of the machine.
6, and the middle ring 5 rotates around the diameter of the outer ring 4 to the inside of the ring 4, tilting the column in the left-right direction.

The inner ring 6 is fixed to the column and rotates around the diameter of the middle ring 5 to the inside of the ring 5, tilting the column in the longitudinal direction.

At the beginning of the oscillating motion, move the assembly of burner 1 to cam 1.
tilt by the action of 0.

The lower end 23 (FIG. 4) of the column is movable, but the arm 21
It must remain at a certain distance from the center of rotation 27.

When the motor 7 is at rest, the spring 9 pulls on the ball bearing 28 at the lower end 23 of the column, so that the column remains on the short axis of the cam 10 and then becomes vertical.

When the motor 7 is turned on, the table 8 starts rotating.

The cam 10 also rotates about its axis due to friction between the O-ring 61 of the cam 10 and the non-rotating column 23.

When the cam 10 has made about half a revolution, its long axis faces the column and pushes the column into an inclined position.

The centrifugal force of the burner assembly then takes over and pushes the column 2, causing it to tilt progressively until the ring 29 around the bearing 28 hits the stop 22.

The spring 30 returns the cam to its original position by directing the short axis of the cam toward the column.

As long as the motor is ON, the lower end 23 of the column does not rotate on its axis but moves in a circular manner, since it cannot be moved by the rocking joint.

As a result, the movement of the crucible holder 11 is a circular motion in which it swings back and forth and from side to side and slightly moves up and down so as to completely and sufficiently stir the contents of the crucible 16.

During melting and stirring, the mold holding part 12 and the crucible holding part 11 are
in the position shown in the figure.

The mold 17 is in an inverted position with its holder 12 and the crucible 16 is in an upright position with its holder 11.

The pin 31 rests in a stop 32. At that location, the temperature of the mold is high enough for successful casting, yet significantly lower than the temperature of the crucible.

This arrangement is very convenient since high temperatures are desirable to speed up the melting and violently melt the poorly soluble substances in the crucible.

On the other hand, such high temperatures are undesirable in molds because the flat surface of the mold is deformed by the heat and requires polishing the manufactured glass buttons.

The casting operation is carried out as follows after the glass mixture has been melted and homogenized.

The motor stops and the spring 9 pulls the column 2 back into the vertical position.

Turn off the gas and the flame goes out.

A current then flows through the solenoid 33 and the resulting magnetic field pulls the clutch plate 19 upwardly against the square nut 20.

At the same time, the motor 7 moves and the table 8 rotates.

When the base 8 rotates slightly, the clutch plate 19
The rectangular hole 34 faces the stationary square nut 20 and engages around it.

When the table 8 continues to rotate, the nut 20 rotates.The drive shaft 35 with the shafts 64 and 65 of the waist extension rotates.The waist main gear 14 rotates, the small gear 15 rotates, and the shaft 36 of the mold holder 12 rotates. Rotate.

The rotation angle of the mold holder is 180 degrees. The rotation starts from the top of the crucible as shown in FIG. 6 and reaches the bottom of the crucible as shown in FIG.

Therefore, the rotation of the drive shaft 35 is stopped by the two stop parts 63 (1
The movement of pin 37 must be restricted between two stops (only one stop is shown in FIG. 1).

The crucible holder 11 (FIG. 6) is fixed to the counterweight 38 with a screw 39, but the crucible holder 11 and the counterweight 38
The respective connections are not fixed, and the shaft 36 of the mold holder is
move around.

During the melting operation, gravity is applied to the counterweights, but the crucible does not rotate because the pin 31 of each counterweight rests in a stop 32.

During casting, mold holder 12 rotates around its shaft 36 and when it reaches the position shown in FIG.
2 (FIG. 1) rotates the counterweight and crucible holder 11 at the same speed as the mold.

Just before the mold reaches the final casting position shown in FIG. 8, the counterweight 38 itself tilts to the opposite side of the vertical plane and then lies there.

Gravity causes the counterweight 38 to rotate faster than the mold.

The crucible rotates until the pin 31 hits the stop 41,
As shown in FIG. 8, the liquid glass is poured into a horizontal mold 17 directly below, and the mold is positioned at an inclined position convenient for pouring.

After a rest phase during which the glass disk solidifies and cools, the casting operation is carried out again with the motor rotation in the opposite direction and the resulting disk is removed from the mold.

Then, the crucible 16 and the mold 17 are returned from the position shown in FIG. 8 to the original position shown in FIG.

The glass disk separates from the mold and, depending on its size, falls on top or inside the crucible.

The glass disk is flat, shiny and transparent, free of bubbles and cracks, and is a perfect sample as far as X-ray fluorescence analysis is concerned.

To prepare the solution, operate the machine as described above.

The method is the same as that for making a glass disk, except for the following points (see Figure 9): a. The mold is not placed on the holder 12.

Instead, isolation sections 42 are placed between the plaids of each holding section.

b. Place the gear housing 43 and install the pin 44 in the groove 45.

In that position the gear housing is free to rotate about the vertical axis, but the position of the pin 44 inside the groove 45 limits rotation.

The crucible holder (FIG. 1) is above the burner 1 when the pin 44 is on the right side of the groove 45 as shown in FIGS. 9 and the top of FIG.

When the pin 44 moves to the left side of the groove 45, the crucible is filled with the solution 4.
The beaker 18 (FIG. 9) containing 7 is moved horizontally into position next to the burner 1.

The glass mixture is melted and stirred as described for making the glass disks.

Perform the operation.

During the operation, the pin 44 is on the right side of the groove 45.

During melting, the complex stirring motion of the machine is controlled by the gear housing 43.
It is designed to generate a slight force that rotates the crucible counterclockwise when viewed from above, ensuring that the crucible remains above the burner 1.

When pouring the glassy material into the beaker, mechanical operations similar to those described above for casting buttons are performed.

However, when the drive shaft 35 (FIG. 1) begins to rotate, the gear housing 43 first rotates because the rotation of the gear housing 43 is easier than the rotation of the gears 14 and 15.
rotates.

Gear housing 43 rotates until pin 44 reaches the left side of groove 45.

At this time, the crucible is on top of the beaker 18.

The rotation of the drive shaft 35 continues, and the 6th. 7. Tilt the crucible as shown in Figure 8.

The flowing molten glass passes between the isolation parts of the mold holding part 12 (FIG. 9) and falls into the solution 47 in the beaker 18.

This hot glass immediately turns into tiny, solid glass flakes.

Immediately after injection, start the stirring movement again.

The metal disk 48 in the beaker 18 moves and breaks into smaller pieces of glass, which melt even faster.

If the glass disk and the solution are to be made at the same time, the machine should be operated in the same way as for the solution described above, and the pin 44 should be in the groove 45.

The mold 17 is placed in the mold holder 12, where a glass button is made and the separator 42 (FIG. 9) is placed between the plaids of the mold holder where the solution is to be made.

Melting, stirring and casting are carried out in the same manner as for the solutions described above.

After casting, stirring and casting to dissolve the glass chips in the solution are carried out in the same manner as for the solution described above.

After casting, a rest period is required to allow the glass button to solidify before beginning agitation to dissolve the glass chips in the solution.

Automatic control is a desirable element of the machine in order to operate the machine in the best possible condition and make only glass buttons or only solution or glass buttons and solution at the same time.

A machine was assembled that included two electric gas valves, one electric air valve, a motor speed control that could vary the motor speed for each operating step, and a device that could reverse the motor rotation.

Use a timer to preset the time for each operating step.

The completed sequential stages are shown in Table 1 along with the control accessories.

The first stage heating/stirring provides for heating the glass mixture with a controllable low gas flow, with or without stirring, if such an operation as drying a wet sample is desired.

The second stage, melt/poach, is to ensure proper melting using adjustable high gas flow and vigorous agitation.

The third stage of melting is usually a continuation of melting without stirring;
Return the burner to the vertical position required for casting or pouring molten glass.

The fourth stage of heating is based on the discovery that it is sometimes better to lower the temperature of the molten glass before pouring it into solution.
This is a low-temperature heating step used only when preparing solutions.

The fifth stage of casting drives both the motor and solenoid as described above.

The sixth stage, waiting, is a rest stage to allow the glassy material in the mold to solidify.

The seventh stage of cooling is a rapid cooling of the glass button obtained by opening an air valve connected to the compressed air line and allowing air to pass through the burner and around the mold.

The final stage discharge was described above.

That is, the motor and solenoid are both driven simultaneously to move the mold back onto the crucible and separate the glass button from the mold.

The electronic circuitry for automatic control will not be described as many methods are known to those skilled in the art.

The machine described above has many parts, the operation of which will be obvious to those skilled in the art and therefore not described.

There are a few parts whose operation is less obvious.

That is, the collar 49 is used to rotate the column 2 up and down to position the crucible on the burner.

The spring 50 is used to constantly push up the drive shaft 35 in order to prevent the clutch plate 19 from slipping between the nut 20 and the ball bearing 28.

The O-ring 51 is used to prevent gas leakage.

The flat portion 52 (FIGS. 1 and 2) of the drive shaft 35 and the connecting shaft 36 always reliably transmit the rotation of the shaft 35 to the other shaft 65 while raising the gear housing 43 slightly when necessary.

The spring 53 prevents the mold holder 12 from rotating downward during stirring.

The tension of the spring 53 is caused by the rotation of the ring 54 and the screw 55.
Adjust by tightening.

The casting operation can be performed by manually rotating the knob 56 via the handle 57.

Safety pin 58 (FIG. 7) is designed to prevent the crucible and mold from accidentally falling from the holder during stirring.

The groove 46 at the top of the column 2 is convenient for use with the bottle 44 when it does not need to be removed from the heater, for example when only making glass buttons.

[Brief explanation of the drawing]

1 is a partial sectional view of the machine of the invention showing only one burner; FIG. 2 is a sectional view of the column of the machine taken along line A-A in FIG. 1; and FIG. Figure 4 is a plan view showing details of the drive mechanism;
Figure 5 is a plan view showing details of the rocking joint, Figure 6 is a perspective view of the holder that holds the crucible and mold in the melting position when making a glass button, and Figure 7 is the crucible in the intermediate position between melting and casting. FIG. 8 is a perspective view of the holding part that holds the mold, FIG. 8 is a perspective view of the holding part that holds the crucible mold in the position of casting into the mold,
The figure is a perspective view of an apparatus for making a solution. 1...Gas burner, 2...Column, 3
...Pipe, 4, 5.6 ... Swing joint, 7 ... Motor, 8 ... Stand, 9 ...
... Spring, 10 ... Cam, 11.1
2, 13... Holding part, 14, 15...
Gear, 16... Crucible, 17... Type,
18...Beaker 19...Clutch plate, 20...Clutch nut, 21...
・Arm, 22.32.41.63... Stop part, 2
3...lower end, 24.25...rotation axis, 26...frame, 27...rotation center, 2
8...Bearing, 29...Ring,
30,50.53...Spring, 31,37
, 40, 44...Pin, 33...Solenoid, 34...L 35--Drive shaft, 36...Shaft, 38- ...Balance weight, 39.55 ...Screw, 42 ...Isolation part, 43 ...Gear housing, 45.46.
...Groove, 47...Dissolution liquid, 48...
・・Metal disk, 49・kawa・・color 1.51.61
...O-ring, 52 ...Flat part, 5
4...Ring, 56...Knob, 57.
...handle, 58 ...safety bin, 59
...Hose, 60...Gap, 62...
... Air control valve, 64, 65 ... Shaft of extension part.

Claims (1)

[Claims for Utility Model Registration] 1. A foundation structure, a column movably attached to the foundation structure, a circular motion device within the foundation structure for performing circular motion at one end of the column, and a glass-like substance placed therein. at least one crucible and a device for holding said crucible at the other end of said column, a device for heating and melting the contents of said crucible, at least one mold suitable for receiving molten glass from said crucible; a bead force and a glass button in conjunction with the device for holding the solution and inverting the crucible to transfer the molten contents to the beaker or the mold after activation when the column stops moving; Sample preparation machine. 2. A utility model registration in which the foundation structure section includes a rocking joint that receives the pivot-shaped column and tilts the column in all directions, and the rocking joint prevents rotation of the column about the vertical axis. A sample preparation machine according to claim 1. 3. The circular motion device includes a motor connected to a pulley, a stand fixed to the pulley, an arm fixed to the stand to freely move one end of the column, and when the motor is stopped, the column in the direction of the center of the pulley. a spring that pulls one end of the
an eccentric cam installed on the platform and adjacent to the one end of the column so as to sequentially cause rotation about the axis of the column; and the platform with which the one end comes into contact when the one end of the column is tilted by centrifugal force. A sample preparation machine according to claim 1 of the utility model registration claim, comprising a stop section. 4. The mold is installed in a U-shaped holder at the end of a rectangular shaft defining a horizontal axis, and the crucible is installed at the end of a straight shaft adjacent to the horizontal axis and rotatable around it. The sample preparation machine according to claim 1, wherein the beaker is installed in a U-shaped holding part fixed next to the heating device. 5. A first gear of the dowel-shaped shaft, and a second gear supported by the column and engaged with the first gear, and the rotation of the second gear rotates the dowel-shaped shaft. The sample preparation machine according to claim 4, wherein the mold is rotated around the horizontal axis. 6. The sample preparation machine according to claim 4, which is provided with a device for injecting molten glass into a mold next to the heater or on top of the heater or next to the heater.