JPS61189458A - Automatic analysis of sulfur content of coal or the like by using robot hand - Google Patents

Abstract

PURPOSE:To automate the entire stage so as to lessen manpower and to improve the accuracy of analysis by analyzing the combustion gas generated when a ceramic boat contg. a sample is inserted through a combustion pipe by a robot hand into an electric furnace by a prescribed method thereby determining the total sulfur content. CONSTITUTION:A sample is sampled, weighed and put into the ceramic boat by the robot hand. Such boat is inserted into the tubular electric furnace 5. A valve 7 is opened, after the prescribed heating treatment, to feed oxygen through an oxygen feed port 8 into the furnace 5 to burn the sample of cool or the like in the boat and to fix the sulfur in the combustion gas as a sulfuric acid by the aq. hydrogen peroxide soln. in an absorption tank 9. An NaOH standard soln. is fed from an NaOH standard soln. tank 13 to the tank 9 via an electrically driven buret 11 and the sulfuric acid is quantitatively determined by titration. The quantity of the NaOH standard soln. is detected by a metering pump 12 by which the total sulfur can be quantitatively determined. These analytical operations are controlled by an analysis control part 15 and an automatic titrator 14.

Description

DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for automatically analyzing sulfur in industrial analysis of coal by using a general-purpose robot hand.

[Conventional technology]

Conventionally, sulfur analysis in the industrial analysis of coal was conducted using JISM8.
812 and JISM 8813 - Sample approximately 1 g or o, s g of powdered coal or coke sample, place it in a porcelain boat aI as shown in Fig. 2, and store it in a porcelain tube K. The sample was then inserted into the annular electric furnace (2) by pushing it with the push rod (7), and the sample was heated to a high temperature in an oxygen stream to oxidize and gasify all the sulfur, which was then added to a hydrogen peroxide solution. After collecting the sulfur in an absorption bottle, the absorption bottle was removed and the sample was titrated with an IJ standard solution to measure the total sulfur content in the sample.

[Problem that the invention seeks to solve]

However, such conventional sulfur analysis methods are inefficient because all operations are performed manually.

However, the titration operation requires skill due to visual judgment and is therefore prone to individual errors.

[Means for solving problems]

Therefore, the inventors of the present invention conducted intensive studies to automate the industrial analysis of coal, and as a result, the inventors of the present invention found that all operations such as handling of the analysis container, sampling of the sample, insertion of the analysis container into the electric furnace, extraction, etc. It can now be performed by a general-purpose robot. As a means of improving this, we have developed a hand that uses a general-purpose robot with an operating range of at least five axes, and that can grip an analysis container and perform analysis operations on its final axis arm. The automatic sulfur analysis method of the present invention, which will be described below, was developed using a robot hand.

That is, the present invention follows the above-mentioned analysis method stipulated in JIS and automates only its operation.The gist of the present invention is to use a robot hand to insert a combustion tube into a porcelain boat containing a sample. The sample is inserted into an electric furnace through the ignition tube to burn it, and the combustion gas is flowed into a gas absorption tube filled with hydrogen peroxide solution to fix all the sulfur in the combustion gas as sulfuric acid, and then into the gas absorption tank. For titration, the sodium hydroxide standard solution is sent through the electric billet of the automatic titrator, and the end point of the titration is determined by the oxidation-reduction potentiometer installed in the gas absorption tank. This is an automatic sulfur analysis method for coal using a robot hand that calculates the total sulfur content from the sodium content.

All of these operations can be performed by computer control or electric servo, and everything from measurement to form creation is performed according to predetermined programming.

[Effect]

According to the automatic sulfur analysis method for coals of the present invention as explained above, the steps of sanfing a sample into a container, weighing it, inserting it into an electric furnace, fixing the combustion gas in an absorption tank, titrating, and determining the titration end point are performed. All operations such as determination and determination of the total amount of sulfur based on the amount of titrant liquid consumed until the end of the titration are performed automatically.

[Embodiments of the invention]

Next, one embodiment of the sulfur analysis method of the present invention will be explained with reference to the process diagram shown in FIG. (5) is an annular electric furnace, and (6
) is a sample insertion section, in which a sample is sampled in advance from a porcelain boat as shown in Fig. 2 by operation of a robot hand, a weighing device is placed thereon, and a push rod is pushed by a control operation based on a sequence program. A porcelain boat is inserted into the annular electric furnace (5). Next, heat treatment is performed in the annular electric furnace (5) at 1650° C. or higher for 8 minutes, which is specified as the conditions for sulfur analysis in the above-mentioned JIS method. At this time, by opening ff (7), oxygen introduced from the oxygen inlet (8) is transferred to the annular electric furnace (5).
), the coal sample in the porcelain boat is burned in an oxygen stream, and all the sulfur is fixed as sulfuric acid by the hydrogen peroxide solution that fills the gas absorption tank (9) with the combustion gas. In addition, the hydrogen peroxide solution can be poured into the hydrogen peroxide tank (by opening the valve (4).
2) into the gas absorption tank (9).

In this way, the sodium hydroxide standard solution for determining the amount of sulfuric acid fixed in the gas absorption tank by titration is transferred from the tank (1) to the gas absorption tank (9) via the electric billet (1).
). (2) is a metering pump installed in the electric billet α-rei. αQ is an oxidation-reduction potential meter, which is provided to determine the end point (neutralization) of the titration in the gas absorption tank (9). The titration ends when the electrometer α1 determines the end point.

The amount of the sodium hydroxide standard solution consumed by the end of the titration is known by the metering pump (2), and from this the total sulfur in the sample can be determined.

These series of analysis operations are controlled by an analysis control section (g) and an automatic titration device α◆.

Incidentally, after the analysis is completed, the waste liquid in the gas absorption tank (9) is flowed into the waste liquid tank α by opening the valve α→.
Alternatively, the valve (3) is opened and the cleaning liquid is poured in from the cleaning liquid tank (1) to clean the absorption tank (9) in preparation for the next analysis.

〔Effect of the invention〕

According to the sulfur analysis method of the present invention, the sulfur content determination of coal is automated from the insertion of the sample into the electric furnace to the calculation of the analysis value, which not only saves labor but also improves the accuracy of the analysis value (individual There was no difference).

[Brief explanation of drawings]

FIG. 1 is a process diagram of the method of the present invention, and FIG. 2 is a process diagram of the conventional method. In the figure, (1) is the cleaning liquid tank, (2) is the hydrogen peroxide tank, (3), (4) is the square, (5) is the annular electric furnace, (6) is the sample charging part, and (7) is the Oxygen valve, (8) is oxygen inlet, (
9) is a gas absorption tank, (7) is a redox potential meter, αυ is an electric billet, (6) is a metering pump, 2) is a sodium hydroxide tank, α4 is an automatic titrator, (to) is an analysis control unit, α
Q is the valve, (b) is the waste liquid tank, AS/FI porcelain boat,
(to) is the LiB back tube, kan is the push rod, (2) is the electric furnace, and ni) is the absorption bottle.

Claims (1)

[Claims] A porcelain boat containing a sample is inserted into an electric furnace via a combustion tube using a robot hand to combust the sample, and this combustion gas is flowed into a gas absorption tank filled with hydrogen peroxide solution to remove the The total sulfur is fixed as sulfuric acid, and a standard sodium hydroxide solution is sent into the gas absorption tank via the electric bead of the automatic titration device for titration, and the end point of the titration is determined by the redox electrometer installed in the gas absorption tank. An automatic sulfur analysis method for coal using a robot hand that calculates the total sulfur content from the amount of sodium hydroxide consumed by the end of titration.