JPS6364735B2 - - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an apparatus for producing a sample solution for simultaneous multi-element quantitative analysis of powder analysis samples such as slag and iron ore.

Traditionally, most of the manufacturing methods for analytical sample solutions, such as slag and iron ore, have been carried out manually, resulting in significant delays in the feedback of analytical results and requiring skilled labor. Therefore, full automation was required.

As an improved method of such conventional methods, a required amount of a powder analysis sample such as iron ore and a melting agent such as sodium borate, lithium borate, etc. are loaded into a melting crucible, such as a platinum crucible, heated and melted, and then cooled and solidified. Next, the sample is melted by adding an acid and heating, or the melting crucible is housed in a heat-resistant container and the sample is heated and melted, and then an acid is added and the solidified sample in the crucible is heated and melted while blowing a high-temperature fluid into the heat-resistant and acid-resistant container. Proposed. However, even with this improved method, the analysis sample solution obtained in the steps up to this point does not immediately become a multi-element simultaneous quantitative analysis sample solution, and the following operation is required. That is, the operation of cleaning the heat-resistant acid-resistant container and the melting crucible in order to completely recover the solution after heating and acid dissolution, and the liquefaction of a certain amount of the analysis sample using a volumetric flask or the like so that the concentration of the analysis sample solution is constant. There is a dilution operation, and this process has to be carried out manually, which is insufficiently continuous and still requires skilled labor and time.

The present invention aims to advantageously solve these problems, and its gist is to provide a container for accommodating a sample and an acid solvent, and a lid removably provided directly above the container. The lid part includes a reflux condenser containing a corrugated pipe in cooling water, an acid solvent metering injection device having an opening/closing pot for controlling the amount of acid solvent injected and maintaining airtightness, and a solution This is an apparatus for producing a sample solution for simultaneous quantitative analysis of multiple elements, characterized by having a gas blowing pipe provided for stirring the liquid, and an in-container cleaning device consisting of a water supply pipe and a nozzle for washing water.

According to the above configuration, the melting crucible that has been heated, melted and cooled is housed in an acid dissolution tank equipped with a reflux condenser, and after adding an acid solution to a predetermined concentration of the analysis sample solution, the evaporated water is transferred to the acid dissolution tank. Since an analysis sample solution with a constant concentration can be obtained by heating acid dissolving while cooling under reflux, conventional heating melting - cooling solidification - acid addition -
By improving the process of acid dissolution and concentration adjustment (manual),
During the acid dissolution step, a step of preparing a solution of the analysis sample at a certain concentration is simultaneously performed, and the resulting sample can be immediately used for analysis.

Further, in the present invention, since a container cleaning means and a gas blowing pipe are provided, the container can be washed and dried immediately after producing a sample solution for analysis, and placed on a conveying device such as a turntable for circulation use. By incorporating the device of the present invention into a series of analysis sample solution manufacturing systems, all subsequent steps can be performed continuously without manual operations by simply loading an analysis sample into a container. can be carried out quickly and reliably, and can advantageously be automated.

Hereinafter, the present invention will be explained in detail with reference to the drawings along with its operation.

FIG. 1 is a process schematic diagram of an automatic continuous solution production method for simultaneous quantitative analysis of multiple elements on analysis samples such as slag and iron ore, showing an example in which the apparatus of the present invention is incorporated. An example of manufacturing a sample solution for analysis will be explained based on this figure in accordance with the operating order. Samples to be analyzed and a melting agent are placed in the melting crucibles _{A1 to Ao shown} in FIG. Next, the first melting crucible A 1 on the melting crucible set table C is transported by the driving device D to a position corresponding to the lifting device E, and then the melting crucible A ₁ is transferred to the _position corresponding to the lifting device E.
Lift it up from below and place it between the conveyor F and the first
The melting crucible is transported to a position corresponding to the induction heating device _G shown in FIG. After the contents have been heated and melted, the crucible A ₁ is conveyed to and delivered to the conveying device F while being naturally cooled by the elevating device G ₁ . On the other hand, only the reflux condenser section _H1 of the acid dissolving tank H equipped with the reflux condenser shown in FIG.
As shown in Figure c, the acid dissolving tank H _{2 is}
The melting crucible A 1 is tilted at 90 degrees and placed horizontally, and the melting crucible A ₁ is rotatably supported after the heating, melting and cooling.
While inserting the melting crucible A ₁ into the acid dissolving tank H 2 using the transport device F, tilt the melting crucible A ₁ by 180°, and open the lid B ₁ of the melting crucible.
melting crucible A ₁ after dropping it on the side of acid dissolving tank H ₂
With the melting crucible A1 returned vertically so that the open side faces upward, press the upper edge of the melting crucible _A1 against the melting crucible fixing jig K at the bottom of the acid dissolving tank _H2 .
While A ₁ is tilted, the open side of the crucible is placed in the acid dissolution tank H ₂
It is stored horizontally so that it faces the opening side.
Next, the conveying device F was moved out, and the acid dissolving tank _H2 containing the rubbish was made vertical with the opening side facing upward using the tilting device J, and then it was temporarily moved using the lifting device I. The reflux condenser section _H1 is lowered, and the acid dissolving tank _H2 containing the melting crucible _A1 is made into a pair, and as shown in FIG. After the injection, the pot is opened and a certain amount of acid solution is added into the acid dissolving tank H equipped with a reflux condenser, and the pot is closed. Then, gas is blown into the melting crucible _A1 by the gas blowing device N. A uniform analysis sample solution with a constant concentration can always be obtained by heating the solution while cooling and refluxing the evaporated water in an acid dissolution tank H equipped with a reflux condenser. Next, using the lifting device I, only the reflux condenser section _H1 is removed and moved upward to a predetermined position. Next, as shown in FIG. 1e, a funnel P ₁ to _{P o} into which a filter paper has been inserted in advance and a receiver Q ₁ to Q _o such as an Erlenmeyer flask are combined into an analytical sample solution receiver P ₁ Q ₁ - After the analytical sample solution receiver P ₁ Q ₁ is conveyed to a predetermined position by a drive device S, an analytical sample solution receiver setting table, for example, a turntable R, on which P _o Q _o is set, is then moved to another conveying device T. Acid dissolution tank
After transporting the analytical sample receivers P ₁ and Q ₁ to a predetermined position near H ₂ , the acid dissolution tank H ₂ is tilted using the tilting device J [Fig. After injecting an amount (appropriate amount) of approximately 10 to 100 ml that does not require precision into the funnel _{P1 ,} the transport device T returns the analytical sample solution receiver _P1Q1 to the analytical sample solution receiver set table. Next _, as _shown in _FIG . Return the acid dissolving tank H ₂ to the vertical position and lower the reflux condenser section H ₁ using the lifting device I shown in d above to return the acid dissolving tank H ₂ to the vertical position as shown in Fig. 1g.
Acid dissolving tank H is equipped with a reflux condenser using a washing water supply device V and a gas blowing device N.
After cleaning the acid dissolving tank equipped with a reflux condenser by spouting cleaning water from the nozzle in the upper part of the interior and proceeding with gas blowing, the reflux condenser part _H1 is raised by the lifting device I, and the reflux condenser part H1 is raised by the lifting device I, and the reflux condenser part H1 is raised by the lifting device I. As in the case, the acid dissolving tank H ₂ is tilted by the tilting device J to discharge the cleaning liquid into the drainage tank U, and then the acid dissolving tank H ₂ is returned to the vertical position and dried as shown in FIG. 1h. Melting crucible for more work
The entire process is repeated sequentially for A ₂ to A _o .
Manual operation of this device involves placing the melting crucibles A ₁ to _{A o} and the analysis sample solution receivers P ₁ Q ₁ to _{P o} Q _o on the setting table C.
, and all other continuously repeated steps are automatically carried out by the control device.

The apparatus of the present invention incorporated in the above process and the method of dissolving a sample using the apparatus will be explained in more detail with reference to the side cross-sectional view of FIG.

After heating _, melting, and cooling, place the melting crucible A ₁ in the predetermined position of the melting crucible fixing jig K with the opening side of the melting crucible A ₁ in the same direction as the opening side of the acid dissolving tank H 2 , and then install the reflux condenser section H ₁ . In Fig. 2 of the acid dissolving tank H equipped with a pair of reflux condensers closely connected by the acid dissolving tank H ₂ and packing H ₃ , an accurate amount of acid solution is injected into the upper part of the acid addition pipe M ₁ and the acid solution is dissolved. Enter tank _H2 and immerse the crucible. Next, gas is blown into the upper part of the fluid injection pipe N ₁ and gas is ejected from the fluid injection nozzle N ₂ located in the crucible at the bottom of the fluid injection pipe N ₁ and heated by the heater H ₄ while bubbling, and melts inside the crucible. Quickly dissolves the analyzed sample to create a uniform analysis sample solution. On the other hand, the evaporated moisture in the acid dissolution tank _H2 is guided from the cooling water injection port _H5 to the reflux cooling pipe _H6 in the cooling water flowing into the reflux condenser section _H1 , where it condenses. Reverse _H6 acid dissolving tank
The acid solution is refluxed into H ₂ and the acid dissolution is completed while maintaining the amount of the added acid solution, making it possible to always obtain a uniform analysis sample solution with a constant concentration. The sample can be directly analyzed at a constant concentration during the acid dissolution process without any manual operations such as cleaning the acid dissolution container and crucible for recovery and dilution operation to make the sample into a solution with a constant concentration using a volumetric flask. A sample solution is automatically produced.

Then, as described in FIGS. 1c and f above,
After transferring a portion of the constant concentration analysis sample solution that does not require the precision required for multi-element simultaneous quantitative analysis to the analysis sample solution receiver, the remaining analysis sample solution, melting crucible A ₁ , and lid B ₁ are discharged, as shown in Figure 2. Reflux condenser section H ₁ as
After pairing with the acid dissolving tank H ₂ , the cleaning water is sent from the cleaning injection pipe V ₁ , flows through the double pipe outer pipe of the gas blowing pipe, and is jetted out from the cleaning water nozzle V ₂ , and the acid dissolution is carried out using a reflux condenser. Clean the inside of tank H.

Thereafter, melting is automatically repeated in the same procedure for melting crucibles A ₂ to A _o .

As is clear from the above description, according to the present invention,
It can provide a sample solution that can be used immediately as a solution for simultaneous multi-element quantitative analysis of powder samples such as slag and iron ore, and the cleaning of the dissolution container after use can be automated, eliminating the need for manual operations after acid dissolution. It can be obtained continuously, quickly and reliably without any complication, and it is possible to save the labor of skilled workers.

[Brief explanation of drawings]

FIG. 1 is a diagram showing an example in which the apparatus of the present invention is incorporated, and FIG. 2 is a side cross-sectional explanatory diagram showing an example of an acid dissolving tank equipped with a reflux condenser. A ₁ to A _o ... Melting crucible, B ₁ to B _o ... Melting crucible lid, C... Melting crucible setting table, D... Drive device, E... Lifting device, F... Conveying device, G...
Induction heating device, G ₁ ... Lifting device, H ... Melting tank equipped with a reflux condenser, H ₁ ... Reflux condenser section, H ₂
...Acid dissolution tank, _H3 ...Packkin, _H4 ...Heating heater, _H5 ...Cooling water inlet, _H6 ...Recirculation cooling pipe, I...Elevating device, J...Tilt device, K... ...Melting crucible fixing jig, L...Acid addition device, M...Acid addition tank, _M1 ...Acid addition tube, N...Gas blowing device,
N ₁ ...Fluid injection pipe, N ₂ ...Fluid injection nozzle, P ₁
~P _o ...Funnel, _Q1 ~Q _o ...Receptor, R...Analysis sample solution receiver set stand, S...Driver, T...
...transport device, U...drainage tank, V...cleaning water supply device, _V1 ...cleaning water injection pipe, _V2 ...cleaning water discharge nozzle.

Claims (1)

[Claims] 1 Consists of a container for accommodating the sample and acid solvent, and a lid portion removably installed directly above the container; the lid portion includes a reflux condenser containing a corrugated tube in cooling water, and a container for storing the acid solvent. A container cleaning system consisting of an acid solvent quantitative injection device with an opening/closing mechanism to control the injection amount and maintain airtightness, a gas blowing pipe installed to stir the solution, and a cleaning water supply pipe and nozzle. 1. An apparatus for producing a sample solution for simultaneous quantitative analysis of multiple elements, characterized by comprising: