JPH0620997Y2 - Elemental analyzer for samples using crucible - Google Patents

Description

[Detailed Description of the Invention] <Industrial field of application> The present invention puts a sample of metal or the like in a crucible, directly energizes the crucible to melt the sample, and analyzes the gas generated at that time. The present invention relates to a device for analyzing elements contained in a sample.

<Prior Art> A conventional elemental analyzer for a sample using a crucible is configured as shown in FIG. 6, for example. That is, in the figure,
Reference numerals 71 and 72 denote an upper electrode and a lower electrode, respectively. The crucible 73 is sandwiched between the electrodes 71 and 72, and a voltage from a power source 74 is applied to the crucible 73.
A sample holder 75 is installed above the crucible 73, and the holder 75 is rotatably supported in an inserter block 76. Further, the thrower block 76 is provided with an openable / closable shutter 77 so that the inside of the thrower block 76 and the periphery of the crucible 73 are filled with an inert carrier gas (for example, He). Reference numeral 78 is an O-ring as a sealing material.

By the way, in this kind of analysis, the crucible 73 is degassed prior to the analysis work. Conventionally, the flux F was put in the crucible 73 from the start of degassing, and this was heated with high power and for a long time. Therefore, for example, in the case of a flux having a low melting point and a low boiling point such as Sn, the flakes are violently scattered during heating and melting, and in the fluxes of Ni, Fe, Pt, etc., the flux is analyzed by permeating into the crucible 73 or scattering. At times, it may not be able to fully function as a bathing agent, and as a result, gas extraction may not be performed smoothly and effectively, which may seriously affect the analysis.

Further, in the conventional apparatus configured as described above, the shutter 77 is opened, a fixed amount of the sample S is put into the sample holder 75, the shutter 77 is closed, and after degassing the crucible 73, the sample holder 75 is rotated. Then, the sample S is dropped into the crucible 73.
If it is a special material such as a powder or granular material, the sample S may be caught in the sample holder 75 or fall out of the sample holder 75, so that the entire amount of the sample S is surely dropped and stored in the crucible 73. However, there is a possibility that this may not be possible, and there is a risk that an error will occur in the analysis effect and that the analysis will be seriously affected.

<Problems to be solved by the invention> The present invention has been made in consideration of the above-mentioned matters, and the flask can be put into the crucible even during the degassing, and the sample and the flask can be securely stored. It is an object of the present invention to provide an elemental analysis device that can be put into a crucible.

<Means for Solving the Problems> In order to achieve the above object, in the present invention, a charging machine block is provided above the upper electrode, and a pair of charging means for charging a sample or a flux is provided in the charging machine block. An upper vertical hole, a pair of intermediate horizontal holes, and a lower bifurcated hole communicating with a descending hole provided in the upper electrode are provided to make them communicate with each other, and a shutter for opening and closing the upper vertical hole is provided. A guide shaft fixed to each of the guide shafts and a cylindrical shutter that covers the guide shafts are provided, and a holding hole is formed in the guide shaft at a position to communicate with the bifurcated hole. An upper elongated hole and a lower opening that always open the upper side of the holding hole are opened on the outer peripheral wall of the cylindrical shutter, and the holding is held only when the lower opening is aligned with the holding hole by sliding the cylindrical shutter. The lower side of the hole is open The sample or flux in the holding hole that is released is supplied to the crucible placed on the lower electrode.

<Embodiment> An embodiment of the present invention will be described below with reference to the drawings.

1 to 4 show the elemental analysis apparatus for samples according to the present invention, particularly the vicinity of a charging device for charging the flux F and the sample S in the crucible.

10 is an upper electrode fixed by the extraction furnace body 1, 20
Is a lower electrode driven up and down by the cylinder 2. The upper electrode 10 has an electrode surface 11 that contacts the opening edge of the crucible C, and the lower electrode 20 has an electrode surface 21 that contacts the bottom of the crucible C.
The crucible C is sandwiched between 1 and 21, and the crucible C is directly energized to generate a Jewil heat, the sample S contained in the crucible C is melted in the presence of the flux F, and the generated gas is made inert. It is configured to be carried on carrier gas and sent to an analyzer (not shown). Reference numeral 12 is a downhole provided in the upper electrode 10.

Reference numeral 30 denotes an inserter block provided on the upper electrode 10 and includes a pair of intermediate lateral plates that extend horizontally from the front side (X side in FIG. 2) to the rear side (also Y side) of the upper electrode 10. Holes 31 and 32, and a pair of upper vertical holes 33U and 3 that intersect with the intermediate lateral holes 31 and 32 facing downward (V side in FIG. 2) from the upper surface side (U side in FIG. 2), respectively.
4U and a lower bifurcated hole 35 that extends further downward and joins to form a substantially Y shape are provided. The lower bifurcated hole 35 communicates with the lower hole of the upper electrode 10. Then, these vertical holes 33U, 34U, the lower bifurcated hole 35, the descending hole 12
Is a hole through which the flux F and sample S dropped by loaders 40F and 40S described later pass, and also has a function as the above-mentioned carrier gas flow passage.

Reference numerals 40F and 40S denote loaders that are fitted and mounted in the lateral holes 31 and 32, and temporarily hold a flux F and a sample S that are loaded from a loading portion described later, and further, the vertical holes 33U and 34.
The flux F and the sample S are introduced into the crucible C through the U, the lower bifurcated hole 35 and the descending hole 12. Since both loaders 40F and 40S are composed of the same parts and have the same configuration, only the loader 40S on the sample side will be described for convenience.

Reference numeral 41 denotes a guide shaft fixedly provided in the lateral hole 32 and having a flange 41a at the front end and a male screw portion 41 at the rear end.
b, a cut portion 41c is formed. A holding hole 41d is pierced through the shaft intermediate portion in the diametrical direction. 42
Is a cylindrical shutter fitted so as to be slidable with respect to the guide shaft 41, a spring receiver 42a is provided at the front end thereof, and a connecting rod 43 is connected to the rear end thereof via a support pin 44. . Then, the outer peripheral wall 4 of the cylindrical shutter 42
An upper elongated hole 42b and a lower opening 42c, which always open the upper side of the holding hole 41d, are provided at positions different by 180 ° from 2 '. 45 is interposed between the step portion 41e of the guide shaft 41 and the spring receiver 42a of the cylindrical shutter 42,
A spring for biasing the cylindrical shutter 42 in the Y direction, 46 is a retaining ring that is screwed to the male screw portion 41b of the guide shaft 41 to prevent the cylindrical shutter 42 from slipping in the Y direction, and 47 is an O
It's a ring.

The loader 40S configured as described above is fitted and mounted in the lateral hole 32 of the loading machine block 30, and is fixed to the loading machine block 30 by the set screw 48. The upper side of the holding hole 41d of the guide shaft 41 is always in communication with the upper vertical hole 34U through the upper long hole 42b of the cylindrical shutter 42, but the lower side of the holding hole 41d is the peripheral wall of the cylindrical shutter 42. The tubular shutter 42 is closed by X.
Lower opening 42c only when slid a predetermined distance in the direction
Holding hole 41d, upper elongated hole 42b and lower opening 42c so as to communicate with one opening 34D of the bifurcated hole 35 through
Is positioned. Further, the support pin 44 is guided and held by the notch portion 41c of the guide shaft 41, and is configured to prevent the rotation of the cylindrical shutter 42.

Reference numerals 50F and 50S denote cylinders for horizontally sliding the cylindrical shutters 42 of the loaders 40F and 40S independently of each other. The cylinders 50F and 50S are provided on the rear surface side of the loading machine block 30, and the rods 51F and 51S are loaders 40F and 40S. Are connected to the connecting rods 43 of FIG.

Reference numeral 60 denotes a loading section provided above the loading machine block 30 for loading the flux F and the sample S into the loaders 40F and 40S.
And is configured as follows, for example.
Reference numeral 61 denotes a base plate fixed by the engaging portions 36 and 37 formed on the upper surface of the throwing machine block 30, which is made of a resin material such as fluorine resin having a smooth surface. A convex plane 61a and a concave plane 61b are formed on the upper surface of the base plate 61 so as to be adjacent to each other, and an inclined portion 61a 'is formed at an end of the convex plane 61a.
Are formed. Further, the concave plane 61b has an opening 6 communicating with the upper vertical holes 33U and 34U of the throwing machine block 30.
1b 'and 61b' are opened, and the respective openings 61
O-ring grooves 61 ″ and 61 ″ are provided around b ′ and 61b ′. 62 and 62 as a sealing material are O-rings.

Reference numeral 63 is a plate-shaped shutter that slides on the uneven surface of the base plate 61 to open and close the openings 61b 'and 61b'. The base plate 61 is provided on the lower surface of the plate-shaped shutter 63.
A concave flat surface 63a and a convex flat surface 63b having substantially the same shape as that of the uneven surface are formed. The concave plane 63a has openings 61b ', 61 formed in the concave plane 61b of the base plate 61.
Openings 63a 'and 63a' are opened corresponding to b '. Reference numeral 63c is a connecting portion to which the rod 71 of the cylinder 70 is connected. For example, a recessed portion 63c 'is formed so as to fit the end portion of the rod 71.

Reference numeral 64 denotes a pressing member. On the flat surface portion 64a thereof, loading cylinders 64b and 64c equipped with the flux F and the loading openings 64b 'and 64c' for the sample S are erected, and further vertically on both sides of the flat surface portion 64a. Skirts 64d, 64d extending to the bottom are formed. The skirt portions 64d, 64d regulate the side portions of the base plate 61 and the plate-shaped shutter 63 described above.

Reference numeral 65 is a holding plate, and the insertion tube 64 is provided on the flat surface portion 65a.
B and 64c are provided with holes 65b and 65c, respectively, and locking tools 65 having hooks on both sides are provided.
d and 65d are provided, and the locking members 65d and 65d are a pair of guides 6 that are erected on the upper surface of the loading machine block 30.
It is configured to engage with the stopper plates 66a, 67a provided on the reference numerals 6, 67. The guides 66 and 67 prevent lateral displacement of the plate-shaped shutter 63. 68 is a spring interposed between the pressing plate 65 and the pressing member 64, and the pressing member 64 is pressed against the upper surface portion 63d of the plate-shaped shutter 63 by the downward pressing force of the springs 68, 68. It slides integrally with the plate-shaped shutter 63. Incidentally, 69 is an upper vertical hole 33U, 34 of the loading machine block 30.
It is an O-ring as a sealing material fitted into the O-ring grooves 38 and 39 formed on the upper inlet peripheral surface of the U.

Next, regarding the operation of the apparatus configured as described above,
It will be described with reference to FIGS. 6 and 6.

1) In the initial state, the lower openings 42c, 42c of the cylindrical shutters 42, 42 of the loaders 40F, 40S, respectively.
Since both of them are not in communication with the openings 33D, 34D of the bifurcated hole 35, the cylindrical shutters 42, 42 are closed. On the other hand, the plate-shaped shutter 63 also has an opening 63.
a 'and 63a' are openings 61b 'and 61 in the base plate 61.
Since it is not in communication with b ', it is in a closed state (see Fig. 5 (A)).

2) Next, when the cylinder 70 operates and the plate-shaped shutter 63 slides in the X direction in FIG.
The a ', 63a' and the 61b ', 61b' are in communication with each other, and the plate-shaped shutter 63 is in the open state. As a result, the input cylinders 64b, 64c-openings 63a ', 63a'-opening 61
b ', 61b'-upper vertical hole 33U, 34U-holding hole 41
d and 41d are in a communication state. Of course, at this time, the lower parts of the cylindrical shutters 42, 42 are in a closed state (Fig. 5 (B), second).
See figure).

As described above, when the plate-shaped shutter 63 slides,
Since the uneven surface is formed on the lower surface of the shutter 63 and the upper surface of the base plate 61, the O-ring groove 6 of the base plate 61 is formed.
The O-rings 62, 62 for sealing provided in 1b ″, 61b ″ are not rubbed against the lower surface of the plate-like shutter 63, and the lateral displacement and the protrusion phenomenon are eliminated.

3) When the plate-shaped shutter 63 is in the open state, the flux F and the sample S are fed from the charging ports 64b 'and 64c', respectively.
Then, the flux F and the sample S are temporarily held in the loaders 40F and 40S because the lower sides of the holding holes 41d and 41d of the guide shaft 41 are closed (see FIG. 5B. )reference).

4) Next, the lower electrode 20 is lowered by the cylinder 2, the crucible C for analysis is placed on the electrode surface 21 of the lower electrode 20, and the cylinder 2 is raised to separate the upper electrode 10 and the lower electrode 20. Both electrodes 10 and 20 are closed so that the crucible C is held between them.

Then, a control switch (not shown) is turned on to energize the crucible C. In this case, the electric power used for heating the crucible C is larger than that during the analysis, and the crucible C is energized for a long time. In this way, the primary degassing is performed, but the temperature is approximately 2500 to 3000 ° C.

On the other hand, at the same time when the upper electrode 10 and the lower electrode 20 are completely closed, the cylinder 70 is returned to slide the plate-like shutter 63 in the Y direction to bring it into the closed state again. Even during this slide, the lower surface of the plate-like shutter 63 is O
Of course, the rings 62, 62 are not rubbed. In this way, the plate-shaped shutter 63 is closed, and the upper vertical holes 33U and 34U are completely sealed from the atmosphere.
By sending carrier gas into the loader 40F, 4
The flux F in 0S and the sample S are purged by the carrier gas.

5) When the primary gas is completed, the cylinder 50F is operated, the cylindrical shutter 42 of the loader 40F is slid in the X direction by a predetermined distance, and the lower opening 42c thereof is located below the holding hole 41d of the guide shaft 41 and the forked hole. When the cylindrical shutter 42 is opened so as to coincide with the mouth 33D of 35, the holding hole 41d communicates with the opening of the crucible C through the descending hole 12 of the upper electrode 10. As a result, the flux F held in the holding hole 41d drops into the fully heated crucible C (see FIG. 5 (C)). Then, after the flux F is put into the crucible C, secondary degassing continues, but the power is supplied at a lower power and for a shorter time than during the primary degassing, and the predetermined degassing is completed. To do. The temperature of this secondary degassing is relatively lower than the temperature of the primary degassing, eg about 2000-2500 ° C.

It should be noted that after the introduction of the flux F, the cylindrical shutter 42 returns to the closed state again.

6) Next, when the crucible C is heated again for sample analysis, the cylinder 50S is operated this time, and the cylindrical shutter 42 of the loader 40S is opened as in the case of the above-mentioned introduction of the flux, and the sample S is crucible C. Fall inside (Fig. 5
(See (D)). Then, it is heated together with the flux F already stored in the crucible C (about 2000 to 2500).
(° C) Melts to generate gas. This generated gas is carried on a carrier gas and sent to an analyzer (not shown) for predetermined gas analysis.

In the above-mentioned embodiment, the sample S may be made of metal or other material such as ceramics. Further, as the carrier gas, an inert gas such as helium is used.

Further, when the flux F having a relatively small blank amount and a constant value is used, the analysis may be performed without degassing the flux F, but in such a case, the crucible is used. It is also possible to put the flux F and the sample S into the crucible C at the same time by operating the cylinders 50F and 50S at the same time after heating only C to carry out a predetermined degassing, and the operator is free to do so. It can be thrown in at the time of.

<Effect of the Invention> As described above in detail, in the present invention, the thrower block is provided above the upper electrode, and the thrower block is provided with
A pair of upper vertical holes for introducing sample and flux,
A pair of intermediate lateral holes and a lower bifurcated hole communicating with a descending hole provided in the upper electrode are provided to communicate with each other, and a shutter for opening and closing the upper vertical hole is provided, and is fixed in each of the lateral holes. A guide shaft and a cylindrical shutter that covers the guide shaft are provided, and a holding hole is formed in the guide shaft at a position to communicate with the bifurcated hole.
An upper elongated hole and a lower opening that always open the upper side of the holding hole are opened in the outer peripheral wall of the cylindrical shutter, and only when the lower opening is aligned with the holding hole by sliding the cylindrical shutter, Since the lower side of the holding hole is opened, the flux and the sample in the holding hole sealed by the shutter that opens and closes the upper vertical hole can be temporarily held by the cylindrical shutter, and the pair of Since the cylindrical shutter can be opened and closed independently, the flux and the sample can be put into the crucible at any time. Therefore, the flux can be heated by a simple control so as not to impair the original function of the flux, whereby the gas can be extracted smoothly and effectively.

Further, since the upper long hole of the cylindrical shutter always communicates with the upper vertical hole, even if the sample and the flux protrude from the holding hole and protrude into the upper vertical hole, this protruding portion is cylindrical. There is no worry of disturbing the shutter slide.

Also, since the cylindrical shutter is slid to open the lower side of the holding hole, all the samples and the flux temporarily held in the holding hole fall downward,
Since it is all housed in the crucible, there is no inconvenience such as spilling of the sample to the outside or catching on the way like the conventional device of this kind, and it is possible to always supply a predetermined amount of sample etc. into the crucible. it can. As a result, accurate analysis can be easily performed.

[Brief description of drawings]

1 to 3 show the main structure of an elemental analysis device according to the present invention. FIG. 1 is a sectional front view, FIG. 2 is a sectional side view, and FIG. 3 is a partially sectional plan view. FIG. 4 is an exploded perspective view showing the main configuration of the charging device, FIG. 5 is an operation explanatory view,
FIG. 6 is a block diagram showing a conventional device. 10 ... Upper electrode, 12 ... Descent hole, 30 ... Inserting machine block, 41 ... Guide shaft, 41d ... Holding hole, 42 ...
... Cylindrical shutter, 42b ... Upper long hole, 42c ... Lower opening

Claims (1)

[Scope of utility model registration request] 1. A feeder block is provided above the upper electrode,
In this feeder block, a pair of upper vertical holes for feeding a sample or flux, a pair of intermediate horizontal holes, and a lower bifurcated hole communicating with a descending hole provided in the upper electrode are provided to communicate these. A shutter for opening and closing the upper vertical hole, a guide shaft fixed in each of the lateral holes, and a cylindrical shutter for covering the guide shaft, and the guide shaft having the forked portion. A holding hole is formed at a position where it should communicate with the hole, and on the other hand, an upper long hole and a lower opening which always open the upper side of the holding hole are formed on the outer peripheral wall of the cylindrical shutter, and the cylindrical shutter is slid. Then, only when the lower opening is aligned with the holding hole, the lower side of the holding hole is opened, and the sample or flux in the holding hole is supplied into the crucible placed on the lower electrode. Characterized by Ruru elemental analyzer in a sample using a jar.