JPH0620126Y2 - Degasser for elemental analyzer - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial field of application] The present invention relates to a degassing device used in, for example, an inert gas melting type or oxygen gas combustion gas analysis type elemental analysis device.

[Conventional technology]

Conventionally, for performing elemental analysis of a metal sample, the surface of the metal sample is grinded or sanded to remove segregation or rust on the sample surface, and then the polished surface is treated with an acid or alkali solution. After that, it is washed with water and dried, or washed with an organic solvent and then dried, and this metal sample is put into an elemental analyzer for elemental analysis.

[Problems to be solved by the device]

However, if the drying and cleaning agent removal in the above pretreatment was insufficient, some water or organic matter remained on the surface of the metal sample, or the surface of the metal sample was activated during the drying process. Therefore, air or the like may be adsorbed on the surface of the sample.

There is room for improvement in that they are decomposed at the time of analysis and are measured as gas components such as H, O, N, and S, which gives an error to the measured values and it is difficult to obtain highly accurate measurement results. .

Therefore, it is conceivable to employ an apparatus that performs degassing in order to remove such gas components in advance. However, it goes without saying that it is desirable that the degassing device is formed compact in order to save space and has good operability.

The present invention has been made in view of the above situation,
It is an object of the present invention to provide a degassing apparatus for an elemental analyzer, which is compact and has good operability, in which the error factor is eliminated by performing the pretreatment more strictly, and the accuracy and reliability of sample measurement are improved.

[Means for Solving the Problems]

In order to achieve the above object, the present invention provides an airtight opening / closing lid for inserting a metal sample at the upper part, and a metal sample supply port at the lower part for allowing the metal sample to pass downward.
An airtight degasser provided with a metal sample loading tool having a receiving member capable of loading a metal sample and dropping the metal sample from the outside in the middle part. The main body is mounted on the upper part of the elemental analysis device and the metal sample inlet provided on the upper part of the elemental analysis device is made to correspond to the metal sample supply port, while the gas in the degasser main body is evacuated. And an inert gas or carrier gas supply line used in the elemental analysis device are connected to the degasser body, and both lines are provided with exhaust gas and gas supply to the degasser body. It is characterized in that a valve for performing the operation is provided.

[Action]

According to the above characteristic configuration, by placing the degasser main body, on which the metal sample is mounted on the receiving member and closed the airtight opening / closing lid, under vacuum evacuation, the surface of the metal sample and the surface layer that cause an error in measurement. The gas components attached to the parts and the water remaining on the surface of the metal sample are evacuated.

Then, after the above vacuum evacuation treatment, the inside of the degasser main body is replaced with an atmosphere of an inert gas or a carrier gas, and then the receiving member is slid to drop the degassed metal sample into the elemental analyzer. By doing so, the gas components and water that cause the measurement error are removed, and the sample surface is covered with an inert gas to protect the clean state, so that highly accurate and reliable analysis values can be obtained. .

In the above operation, without taking out the metal sample to the outside,
After degassing, it is sufficient to slide the receiving member and drop the metal sample, and the operability is extremely good.

〔Example〕

 Embodiments of the present invention will be described below with reference to the drawings.

FIG. 1 shows a degassing apparatus 1. FIG. 2 shows an elemental analysis facility. For example, the degassing apparatus 1 is connected to a metal sample supply port 3 of an elemental analysis apparatus 2 of an inert gas melting type or a combustion gas analysis type in an oxygen stream.

The degassing device 1 has an insertion port 5 for the metal sample a formed in the upper part of the degasser main body 4 and a supply port 6 for the metal sample a in the lower part, and is opened / closed by a driving means 7 such as an air cylinder. An airtight open / close lid 8 is attached to the metal sample insertion port 5, and the metal sample a inserted through the metal sample insertion port 5 is received, and the metal sample insertion port of the elemental analyzer 2 is supplied from the supply port 6. 3 is provided with a slidable metal sample introduction tool 9 and a heater H for heating the gas in the degasser main body 4.

An exhaust line 10 to which a compressor P is connected is connected to the degasser main body 4, and an inert gas supply line 11 to which an inert gas cylinder B is connected is joined to the exhaust line 10. And the exhaust line 10
On-off valves V ₁ and V ₂ are provided on the supply line 11 and the supply line 11, respectively.

The metal sample throwing tool 9 is provided with a receiving member 12 for the metal sample a inserted through the metal sample insertion port 5 slidably in an airtight state with respect to the degasser main body 4, and A driving means 13 such as a solenoid for slidingly operating 12 is communicatively connected to the receiving member 12.

Then, with the valves V ₁ and V ₂ of the both lines 10 and 11 closed, the airtight open / close lid 8 is opened and the metal sample a is placed on the receiving member 12 to set the airtightness. When the opening / closing lid 8 is closed, the limit switch LS detects that the airtight opening / closing lid 8 is closed, and degassing control is performed by the following program.

That is, based on the detection of blockage of the airtight open / close lid 8 by the limit switch LS, first, the heater H is controlled to generate heat so as to heat the atmosphere of the degasser main body 4 to about 100 to 300 ° C. The compressor P is driven when the temperature of the metal sample a is raised to a predetermined temperature.

Then, the valve V ₁ of the exhaust line 10 is opened for a predetermined time (for example, about 1 to 2 minutes), and the degasser main body 4 is opened.
Heating gas inside (main body air, gas components such as O ₂ , N ₂ , CO ₂ and SO ₂ adsorbed on the surface and surface layer of the metal sample a, and remaining on the surface of the metal sample a) Water) is evacuated.

Next, the valve V ₁ of the exhaust line 10 is opened, the valve V ₂ of the supply line 11 is opened, and the driving of the compressor P and the heat generation control for the heater H are stopped. The inside of the degasser main body 4 is replaced with an inert gas.

Then, when the predetermined gas replacement is completed, the receiving member 12 of the metal sample introducing tool 9 is slid, and the metal sample a of the receiving member 12 is introduced into the elemental analyzer 2 through the metal sample introducing port 3. To be done.

After that, the receiving member 12 is slid to the original posture, and the valve V _{2 of the} supply line 11 is closed.
This completes a series of pretreatments for the metal sample a.

In addition, after the gas in the degasser main body 4 is evacuated,
Although the pretreatment in the form of supplying the inert gas into the degasser main body 4 has been described, the inside of the degasser main body 4 is replaced with the carrier gas used in the elemental analysis device 2 instead of the above-mentioned inert gas. May be replaced.

Further, although the degassing and gas replacement for the degasser main body 4 are described as program control, this is merely an example, and it goes without saying that other automatic control or manual control can be arbitrarily selected. .

Further, when performing the above-described vacuum exhaust, it is considered that the atmosphere inside the degasser main body 4 is heated to enhance the exhaust efficiency, but this is an example of a preferable exhaust mode, and the heater H is omitted. Can be implemented.

[Effects of the Invention] As described above, according to the degasser for elemental analyzer of the present invention, the degasser main body connected to the elemental analyzer is placed under vacuum exhaust, which causes an error in measurement. It becomes possible to efficiently evacuate the gas components adhering to the sample surface and the surface layer portion and the residual water on the sample surface, and thus, after the above-mentioned vacuum evacuation treatment, the inside of the degasser main body is fed with an inert gas or After substituting the atmosphere of carrier gas, by dropping the metal sample after the degassing treatment into an elemental analyzer,
It was possible to perform elemental analysis with extremely high operability, high accuracy and high reliability without individual differences, and in turn, to improve the reliability of sample measurement. Since the degasser main body is mounted on the upper part of the elemental analysis device, the entire device can be made compact and space saving can be realized.

[Brief description of drawings]

FIG. 1 is a vertical sectional side view of a degassing apparatus, and FIG. 2 is a configuration diagram of elemental analysis equipment. 2 ... Elemental analysis device, 3 ... Metal sample inlet, 4 ... Degasser main body, 6 ... Metal sample inlet, 8 ... Airtight opening / closing lid, 9 ... Metal sample inlet, 10 ... Exhaust line, 11 ... Supply line, V ₁ , V ₂
…valve.

Claims (1)

[Scope of utility model registration request] 1. An airtight opening / closing lid for inserting a metal sample is provided on an upper part, a metal sample supply port for allowing a metal sample to pass downward is provided on a lower part, and a metal sample is mounted on an intermediate part. The degasser main body of the airtight structure is provided on the upper part of the elemental analyzer, which is provided with a metal sample input tool having a receiving member capable of sliding the metal sample from the outside and capable of dropping the metal sample. The metal sample inlet provided on the upper part of the elemental analyzer is made to correspond to the metal sample supply port, and an exhaust line for exhausting the gas in the degasser main body to vacuum, an inert gas or the above A carrier gas supply line used in an elemental analyzer is connected to the degasser body, and a valve for causing both lines to perform exhaust and gas supply to the degasser body. Vignetting degasser elemental analysis apparatus characterized by being.