SU1318899A1 - Method of manufacturing glass-metal reference electrode - Google Patents

Abstract

This invention relates to methods for making an electrochemical cell comparison electrode. The purpose of the invention is to increase the service life and stability of the electrode. The goal is achieved by using an electrode body, separating the capillary into upper and lower volumes, placing a portion of the metal in the upper volume and evacuating the body. The residual gases are then expelled from the lower to the upper volume, the metal is melted and introduced through the capillary under the pressure of the residual gases into the lower volume, which is then sealed. The proposed method allows to increase the service life and stability of the electrode. 00 00 () with

Description

JO

11318899

The invention relates to a method of making a reference electrode for an electrochemical cell used in the study of EMF of sodium glasses by the method of electromotive force, and can be used in the manufacture of reference electrodes containing byproduct-acid acid, the content of oxides of this element is permissible.

The purpose of the invention is to increase the stability and service life of the electrode.

In the proposed method, due to the displacement of residual gases (by slight heating) from the main working volume, the formation of an oxide film in it on the rapidly oxidizing element is excluded. In addition, under pressure of the displaced residual gases, the melt very quickly flows through the capillary into the main volume, leaving an oxide film on the walls of the capillary

The proposed method is carried out as follows.

The billet of the glass body of the electrode is divided into two volumes by the waist: the upper and lower capillaries have an internal diameter of 1-1.5 mm. A platinum rod is introduced into the lower volume and sealed onto a gas burner at the end of the preform until a vacuum-tight layer is obtained. Then, in a sealed box filled with argon, 1-2 g of metallic sodium are placed in the upper volume, the billet is sealed with a rubber stopper, removed from the box, evacuated to mm Hg. and otpaivat on peret zhke. On a gas burner, 40 ke is slightly warmed up the lower volume.

25

5 in

20 in in p

-m m to l 35.o t n

thirty

in order for residual gases contained in the lower volume to pass through the capillary to the upper volume. Heat the upper volume to melt the sodium in it. The molten sodium is entrained in gas particles passing through the capillary from more

The manufacture of the electrode according to the proposed method allows to improve the Y.

the currently heated upper volume to a colder lower volume. The quality of the electrode, namely: contrac- tion. In this case, only the number of failures of work to melt pure sodium passes through the capillary, and the sodium oxide film remains on the machines of the lower volume and near the entrance to the capillary. Then the capillary tube is powered on gas 55

electrodes due to the oxidation of sodium j stabilize the measurement results, the variation of the emf values is reduced due to the presence of an oxide film.

In addition, in the proposed method, the electrode manufacturing technology is simplified by reducing the number of operations (the billet is burned out and otpaivayu.

Example 1. For the investigation of sodium-containing chalcocheO melts.

0

Sight glass in the temperature range of 750-850 K is collected galvanic cell:

(+) Pt, Na / NaCl - KCl - CdClj / CSP. Pt (-).

B as the auxiliary electrode - the reference electrode is used sodium electrode, the body of which is made of Pyrex glass and

five

is an ion exchange membrane separating sodium from a liquid electrolyte.

The spread of emf values for glasses of the same compositions of parallel floats is 0.1%.

EXAMPLE 2 A distinctive feature of an electrode for examining sodium-containing glasses in solid state is that the top volume with the capillary is soldered to the side. The body of the electrode is made of laboratory glass No. 23. As a solid electrolyte, glass of the composition is used, mol.%: / - 22; snO - 5; SiO - 73.

Soldering of the solid electrolyte is carried out on a gas burner. A drop of molten solid electrolyte is placed on the tip of a preheated quartz rod and soldered into the flame of a gas burner into the electrode body billet until a quality layer is obtained. In order to avoid cracking of the layer, the preform 5 is burned in a weak flame of the burner for 5-7 minutes and placed in a preheated muffle furnace for final annealing during the cooling process with the furnace.

With the help of the cell (+) Pt, Na / NajO- SnOj - CGS. Pt (-). thermodynamic studies are carried out.

The spread of EMF values for glasses of the same compositions of parallel heats is 0.1%.

The manufacture of the electrode according to the proposed method allows to improve the Y.

0

five

0 electrode quality, namely: the number of work failures is reduced 5

electrode quality, namely: the number of work failures is reduced

electrodes due to the oxidation of sodium j stabilize the measurement results, the variation of the emf values is reduced due to the presence of an oxide film.

In addition, in the proposed method, the electrode fabrication technology is simplified by reducing the number of operations (blank

yes at the same time it serves as an electrode body and a sodium oxide cleaning system). The proposed method allows one to obtain multiple-use electrodes. There is no need to use an inert medium in the measurement process.

Claims (1)

Invention Formula A method of manufacturing a glass-metal comparison electrode comprising vacuum melting of a metal followed by the introduction of molten Editor A. Shandor Compiled by I. Rogal Tehred L. Oliynyk Proofreader V. But ha Order 2503/37 Circulation 776 Subscription VNIIPI USSR State Committee for Inventions and Discoveries 4/5, Moscow, Zh-35, Raushsk nab. 113035 Production and printing company, Uzhgorod, st. Project, 4 four Metal in the body of the electrode through the capillary, characterized in that, in order to increase the service life and stability of the electrode, the body of the electrode is divided into two volumes: upper and lower, placed in the upper volume of the metal, vacuum of the body displaces residual gases from the lower the bulk into the upper one, the metal portion is melted down and the molten metal is forced out of the upper bulk into the lower volume through the capillary, which is then sealed.