SU1073660A1 - Lead capsule for determination of gas content in materials - Google Patents

Description

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The invention relates to gas analysis and can be used in analytical chemistry to determine the content of gases in refractory materials by the method of Borestanvity that has been melted and

The famous graphite capsule of a vertical vertical cylindrical body with a camera made in it, and a krylka with

 passing an electric current the camera heats up. unevenly, the ends of it, - the code of Sh. Oes in contact with current leads; have a lower temperature compared to the temperature in the center of the chamber. In this case, the temperature of the sample, depending on its position in the chamber, can vary significantly, both from experiment to range, and PI in the course of one process and one meter, - and about a to c the completeness of the emission depends significantly on the sample temperature, it is negative for the accuracy of the analysis, CKa3bi.Bae7fCH

Closest to the offer is. graphite tsapsul to determine content. gases B material ah f comprising a housing with a chamber that has been completed therein; Dvide and Krgliku, the inner part of the roof and has a conical:. 21 "In the capsule, the test image.,; - ng go to the tzer house of condition. ;; kki,; l1-: aet. Hip titeggyy TeiijioBoii contact with, hp ;; clear

; i i reci-jiiweH g open state: When

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y;: e. difference pls. and srazva €: ss.:: a .. to about tonyvsS) mi ej: atura: cyiuecTBeHHo nyugs

ra in the central part of the chamber: D. p.

reaching the required temperature

sample - all ka must be: sulu k

its ueHTpajTbH, / to part overheating.

vat prnodit.it to, cpolmite.l-Howy gazoB-delenkyu nz

ness to huvtsulsy; what is with: lower then :;

skill

znichnost of the analysis to the Capsule tru.tsosrok kagyult, tight and to;

Capacity in izgotoleniif TKK Amp,

Requires currents in dest e siaoa

Eletsov.Pno, and Maccj

electroforming,

The invention of the invention - PoB; e; e: -1ke, the exactness of the reference point is contained ;: gases 3 materials.laho

Lost Blenn. The goal is to (:; t; 1;) because in the traffital capsule ol determine the content of the hooks from the g. materials containing a housing with a sslslennoy kogleroy; in HanpasijSHKH, the zklind axes are: (an air casing,: c: then ... and Kyts are equal

n is between 1/3 and 1/20 of the body length,

A positive effect is achieved due to the fact that due to a shzkoy conductivity of the material of the bottom and the lid compared with the material of the body, the specific power released in them is higher. Behind. this account is an additional heating of the end parts of the capsule, which compensates for the heat loss in the cooled current leads and thereby helps to equalize the temperature along the height of the capsule. The lower thermal conductivity of the bottom material and the cover as compared to the mother of the housing helps to reduce heat from the ends of the capsule to the current leads and to equalize the temperature along the length of the capsule. .o reduce temperature drops in the radial direction. These effects make it possible to obtain a practically isothermal field in the chamber volume. The absence of chilled parts in the chamber contributes to a more complete emission of gases containing: from the test material, and, next, TC .jjHo. and the behavior. sensitivities and ACCURACY analysis,

Equal thickness 71n; 1shte and: -sry: iki is due to the fact that the electrical resistances must be equal in this case. The temperatures are also equal; and the covers, since the power and heat dissipation used in the Bodo-cooled current leads are the same. The indicated ratio of dyagda and krtyki thickness and length of the body is due to the fact that with a ratio of less than 1/20, the pyrographite produces heat and electric equipment correspondingly added: t: heating, insufficient heat supply, but to compensate for retraction

ia, in a water-cooled current lead ratio of greater than 1/3, the volume of pyrolytic raphite increases unobligibly, which is an additional source of gas evolution and, consequently, decreases in sensitivity to heat and energy. but,

The drawing shows a graphite capsule.

The capsule consists of a cylindrical body 1. the bottom 2 and the cover 3

The device works as follows.

When a 3, T current flows through the capsule, it is heated to a predetermined temperature. Due to the higher specific electrical resistance of the bottom material and the cover

(6000 Omtlm / m) compared with the material of the cylindrical body (10-30 Ohm-g.1m2 / m) and lower thermal conductivity (2 BT / M-JC for pyrographite and 80-200 for graphite) additional heat dissipation in the bottom and KpbniiKe allows you to compensate for heat loss in water-cooled current leads and to achieve equal temperature across the entire working volume of the capsule.

The proposed device is implemented and tested in a laboratory setup for measuring the oxygen content of carbon and graphite materials. The cylindrical body was made of G1PG-6 OSCh material, the bottom and the cover were made of pyrographite brand UPV-1. The outer diameter of the capsule is 7 mm, the internal diameter of the cylindrical body is 5 mm, and its length is 8 mm. The thicknesses of the bottom and the cover included in the chamber were made equal to 0.5 mm, and not included in the chamber varied within 0, 4-2, 7 mm. The amount of escaping gases was measured using a coulometer. Coke of CNPC brand was used as a test subject. The sample charge was 40 + 5 mg.

Ten measurements were made for each capsule variant.

The test results are presented in the table. In the table, the following designations are accepted: I variant camera is made according to the prototype / O option - the bottom and the ruler thicknesses that are not included in the package are 0.4 mm / IM and w the thicknesses are respectively 1.5 and 2.7 mm.

Claims (1)

GRAPHITE CAPSULE FOR DETERMINING THE GAS CONTENT IN MATERIALS, containing a body with a chamber made in it, a bottom and a cover, molded in that, in order to increase the accuracy of determination, the bottom and cover are made of pyrographite oriented with a crystallographic axis of ¹ . ¹ in the direction of the axis of the cylindrical body, and the thickness of the bottom and cover are equal to each other and range from 1/3 to 1/20 'of the length of the body. ί 10