JPS58102145A - Sample holder for electrolytic analyzer - Google Patents

Abstract

PURPOSE:To positively hold the formed product without slipping it out of position until the completion of dissolution by a holder which includes a shield plate between a support holding a formed sample in contact with an anode rod and an agitating gas inlet pipe. CONSTITUTION:A sample holder comprises a sample support 7, a circular shield plate 8 positioned below the support 7 and having much larger size than it, and an agitating gas inlet pipe 9 adapted to jet out electrolytic solution agitating gas therefrom. The support 7 is selected to be smaller than the outer diameter of a conductive material part 12 at the center of a sample 6, so that both upper and lower surfaces of a sample part 11 are exposed. With such a construction, the formed sample 6 can be positively held on the support 7 until the sample part 11 is dissolved completely. The inlet pipe 9 serves to integrally support the support 7 and the shield plate 8 in a proper position.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a sample holder for an electrolytic analyzer.

For example, the electrolytic analyzer f can electrochemically analyze non-metallic inclusions in steel.
R] 4i! ! It's snow.

Generally, in addition to the iron matrix, nonmetallic inclusions such as chemical compounds, sulfides, subrides, nitrides, and intermetallic compounds are present in steel. Among these, nonmetallic inclusions *tl-
As an analytical method for accurate determination, it is known to conduct elemental analysis on the residue obtained by electrochemically dissolving the iron matrix, but other methods include performing elemental analysis on the residue obtained by electrochemically dissolving the iron matrix. A method of separating cedars according to their condition is also being considered. In particular, the latter is a technique that utilizes the differences in the electrochemical stability of each of the above compounds, and is formed by integrally molding the above residue with a conductive material and In this method, electrolysis is carried out using an apparatus such as that shown in FIG.

In the case of the above device, the molded powder sample is subjected to electrolysis as positive and negative by mixing the powder sample with a paint of a conductive substance and fixing it on a platinum plate.
! Alternatively, a powder sample is pressure-molded and brought into contact with a platinum wire, or wrapped in a platinum wire mesh, and this platinum wire = j
, Lead! One possible method is to connect with IK and turn on electricity.

By the way, the molded powder sample prepared in this way [When performing electrolysis by immersing it in a non-aqueous solvent-based electrolytic solution, the paint has priority over the non-aqueous solvent when using conductive substances of the IIi family. The powder sample cannot be kept in the form of an anode sample forever because it dissolves. In addition, if the sample was simply pressure-molded and brought into contact with a platinum wire or wrapped in a platinum mesh, the contact point between the sample and the platinum part would melt first, and the anode sample would fall apart. In the case of a friend sample extracted from other systems, the cementite contained in the residue decomposes, and at this time carbon is liberated and deposited on the sample surface, making it possible to maintain the sample tube at a constant potential at all times. First, constant potential electrolysis becomes impossible.

Therefore, the present invention addresses the problems of the US technology as described above.
When electrolyzing the powder sample with the molded T-FI1M, it can be held securely without falling off until the end of dissolution, and it is also suitable for sample holding to achieve efficient constant potential electrolysis. For the purpose of obtaining a, we propose the following summary structure. That is, the special feature of the structure of the present invention is that a molded sample having a disk-shaped conductive material in the center and a powder sample combined in a ring shape around it is used as an anode, and this is placed against the electrode surface in an electrolytic solution. The outer diameter of the conductive material part of the molded sample is to be installed in the electrolyte of the device for electrolysis, and the molded sample is held at a position where the upper surface of the molded sample just contacts the lower end of the anode rod. A small holding table, an upward blowing rotor, and a curved stirring gas introduction pipe, and a cutoff for isolating the sample from the upward flow of stirring gas located between and integrally formed with them. The sample holder of an electrolytic analyzer consists of a plate. The details of the configuration of the present invention will be explained below.

Figure 1 shows an electrolytic analyzer in good condition with the sample holder of the present invention inside. ◇The /ij electrolytic vessel shown in the figure contains a lithium chloride/methanol electrolyte containing IO-rich acetalacetone. , Attach a rosette to the top and configure the device bodyFi5
tt, it's there. Inside the container L, there is a cathode J using a ring-shaped platinum plate that runs along the vessel wall, and a calomel electrode (with a beak) that maintains a constant potential, with its lower end located approximately in the center surrounded by the cathode JK. (band-shaped) dream and platinum anode rod j are accommodated.

A molded sample 4 of a mixture of a conductive parasitic substance and a powder sample is held in a container l that is brought into contact with the lower end of the anode rod j. For this purpose, the present invention employs a sample holder having the following configuration. The sample holder preferably has an integrated structure made of plastic, and includes a sample holding stand 7, a circular shielding plate l located below the holding stand 7, which is much larger than the holding stand 7, and an electrolyte stirring gas injected therein. The stirring gas introduction pipe is composed of a J-shaped bent pipe whose tip outlet a opens upward.
The holding table 7 is placed at a predetermined interval of 1kl in front! Judgment &f
It is a wing-shaped protrusion on top of the anode rod, and at the same time, the anode rod is placed on top of it. The lower end of the sample 4 is energized so that it contacts the upper surface of the sample 4 to induce an energized state. For this purpose, the holding table 7 is attached to the molded sample 1 which will be described later.
The diameter is smaller than the outer diameter of the conductive material part located at the center of the sample part 11, so that the bottom +ii of the sample part 11 protrudes. With such a structure, the molded sample 1 is held on the holding table 7 at a height of Km until the entire melting process is completely completed. The role of the above-mentioned S-cut root 1 is to separate the sample 4 from the upward flow of stirring gas from the stirring gas outlet 1 located below it, and to prevent the residue adhering to the electrode surface from falling off from the electrode during electrolysis. This is also to make sure that you don't get caught. The stirring gas introduction pipe also integrally supports the holding table 7 and the blocking plate l,
The end on the introduction side is fixed to the holder 7111 through the holder 7, and the lower end of the holding table 7111 is used to aerially support the molded sample at the right position to bring it into contact with the upper surface. Figure 2 is a book showing a preferred example of molded sample 4. For example, prepare a sample // of carbon steel electrolytic residue t'Il! mixed with one body of copper, and divide it into diameter /jmmφ.
The molded body of copper powder is assembled concentrically around the outer periphery of the molded body of copper powder.
Pressurization! It molds a tablet (molding sample: t) with a diameter of 20 mtaφ by 1 m.
φ.

Prepare a platinum wire mesh/Jt with an inner diameter of 2.5 mm and embed it in the sample at the same time as pressure molding. The anode sample tube prepared in this manner is held in the center of the sample holder and energized.

The sample holding table 7 (diameter/Jmmφ) according to the present invention is as follows.

The above-mentioned molded sample 1 (electrolytic residue mixing part: outer diameter: Omm-.

Because the inner diameter is smaller than the inner diameter izntmφ), electrolysis is performed on molded sample 4.
Electrolysis proceeds not only from the top surface but also from the bottom surface, shortening the electrolysis time.

As the electrolysis progresses, copper ions become concentrated on the sample surface, so gas agitation is performed to gently diffuse the copper ions.
Prevents the electrolytic current value from decreasing due to the energizing voltage. Further, gas stirring has the effect of making the copper electrodeposited St uniform and smooth on the cathode, and prevents the steel from falling off from the cathode. In this case, the gas introduction pipe! To prevent the gas blown from the tip of the tube from hitting the sample and causing residue to fall off the anode, a circular glass plate is placed above the gas outlet to gently stir the sample. According to the present invention having the configuration,
It is suitable for efficient constant potential electrolysis of powder samples, and can reliably hold the sample until it is completely dissolved without falling off.

FIG. 7 is a sectional view of an electrolytic analysis and stomach including the holder of the present invention, and FIG. 2 is a sectional view of a molded sample.

l...container, λ...lid, 3...@pole, l...calomel electrode, j...molded sample, 7...holding stand, t...
・Shutoff class, ri... Stirring gas inlet pipe, ? a...Blowout port of stirring gas inlet pipe, io・°・packing, ti・
...Powder sample, lλ...Conductive material, /3...Platinum mesh.

Patent applicant: Kawasaki Steel Corporation

Claims (1)

[Claims] 1. Electrolysis of a device that uses a molded sample with a disk-shaped conductive material in the center and a powder sample combined in a ring shape around it as an anode, which is placed opposite the electrode surface in an electrolytic solution. The book is placed in a liquid, and includes a holding table having a diameter smaller than the outer diameter of the conductive material part of the molded sample and an upwardly facing holder for holding the molded sample in a position where its upper surface just contacts the lower end of the molded sample. A sample of an electrolytic analyzer consisting of a curved stirring gas inlet pipe having a blowout hole f: and a shielding plate located between the two and integrally formed therewith for isolating the sample from the upward flow of the stirring gas. retainer.