Purifying device of dissolving reducing agent for measuring sulfur content

Abstract

The utility model relates to a solution purifying device, which belongs to the field of chemical industry, in particular to a purifying device for a dissolving reducing agent used for measuring sulfur content, and is characterized by comprising a flask, a condenser and a gas absorption tube which are sequentially connected in a sealing manner through a pipeline, different types of reducing agents for dissolving are arranged in the flask, a heating device is arranged below the flask, a flask opening is in sealed connection with an inlet of the condenser, and an outlet of the condenser is in sealed connection with the gas absorption pipe; an inert gas input pipeline is arranged on the side wall of the flask. According to the purification device of the high-efficiency dissolving reducing agent for measuring the trace sulfur content in the steel and iron substances, interferents in the solvent are fully removed after the treatment of the device, so that the efficiency is high, the measuring steps are simple, and the result is accurate and stable when the sulfur content of the steel and iron substances is subsequently measured.

Description

TECHNICAL FIELD

[0001] The utility model relates to a solution purification device belongs to chemical industry field, especially relates to the purification device of reducing agent used in the determination of trace sulfur in steel material. BACKGROUND

[0002] Sulfur in steel can seriously affect its performance. Sulfur can have a "hot brittle" effect on steel performance, that is, when hot deformation occurs, the workpiece cracks, so its harm is great. Sulfur can also reduce the mechanical properties of steel, especially significantly reduce the fatigue limit, plasticity and wear resistance, affecting the service life of steel parts. When the sulfur content is high, it will also cause welding difficulties and decrease in corrosion resistance and other adverse effects. However, adding an appropriate amount of sulfur to some special specifications of steel can improve the machinability, processability and magnetic properties. Generally, the sulfur content in steel is controlled at several ppm to several thousand ppm, or even lower, according to its use. Therefore, the sulfur content is a must-check index in steel composition analysis.

[0003] Currently, the main methods for determining sulfur content are infrared absorption spectroscopy, titration analysis, atomic emission spectroscopy, ion chromatography, electrochemical analysis method, and spectrophotometry. The titration analysis method has high accuracy in the determination of constant, but has large error in the determination of trace sulfur; the atomic emission spectroscopy method has many interferences that need to be eliminated in advance, and the ion chromatography and electrochemical analysis methods are limited by the sensitivity and blank value of the instrument. At the same time, due to the high cost of the instrument, these methods have certain limitations in the determination of trace sulfur. SUMMARY

[0004] The utility model provides a kind of solution purification device, and the purified solution is used as dissolved reducing agent to dissolve measured material and make sulfur compound escape in the form of hydrogen sulfide, and then subsequent determination is carried out.

[0005] Invention purpose: the determination of trace sulfur in steel requires that steel material be completely dissolved, and then all sulfur-containing substances are precipitated. The present purification device uses ordinary test equipment to purify the solvent, so as to dissolve the sample, precipitate the sulfur-containing substances and eliminate the blank interference.

[0006] Technical scheme: a purification device for dissolving reducing agent used in the determination of sulfur content, characterized in that the purification device comprises a flask, a condenser and a gas absorption tube connected in sequence by a pipeline; different types of dissolving reducing agent are placed in the flask, a heating device is arranged below the flask, the flask mouth is sealingly connected with the inlet of the condenser, and the outlet of the condenser is sealingly connected with the gas absorption tube; an inert gas input pipeline is arranged on the side wall of the flask.

[0007] Further, the side wall of the flask is also provided with a sealing port for adding or sucking the dissolving reducing agent, or inserting a temperature control device.

[0008] Further preferably, the sealing plug is provided.

[0009] Further, the horizontal section of the inert gas input pipeline penetrates from the sidewall of the flask, and the vertical section of the inert gas inlet extends into the reducing agent for dissolving in the flask.

[0010] Further, the outlet of the condenser extends into the absorption liquid of the gas absorption tube through a pipeline.

[0011] Further, the pipeline is a glass tube, a ceramic tube or a flexible tube.

[0012] Further, the inert gas input pipeline is a glass tube or a ceramic tube.

[0013] Further, the inert gas input pipeline is provided with a gas flow meter.

[0014] The utility model discloses a dissolving reducing agent for measuring the sulfur content of steel material, which comprises a flask, a condenser, a gas absorption tube and an inert gas input pipeline.

[0015] The purification device of the utility model can be equipped with different kinds of reducing agents according to different methods.

[0016] The utility model also comprises a piston and a connecting pipeline which are well known in the field.

[0017] The utility model has the advantages that the purification device for the dissolving reducing agent for measuring the sulfur content of steel material is provided. BRIEF DESCRIPTION OF DRAWINGS

[0018] Figure 1 Fig. 1 is a schematic view of the connection structure of the purification device for the dissolving reducing agent for measuring the sulfur content of steel material.

[0019] In the figure, 1 is a flask, 2 is a condenser, 3 is a gas absorption tube, 4 is an inert gas input pipeline, 5 is a sealing plug and 6 is a heater. DETAILED DESCRIPTION

[0020] The utility model will be combined with the drawings and examples to be described in detail. EXAMPLE

[0021] The purification device for the dissolving reducing agent for measuring the sulfur content of steel material is shown in Fig. 1. Figure 1, mainly including flask 1, condenser 2 and gas absorption tube 3 connected by pipeline in turn; flask 1 is internally provided with different types of dissolving reducing agent, and the lower portion of flask 1 is provided with a heater 6, the mouth of flask 1 is sealingly connected with the inlet of condenser 2, and the outlet of condenser 2 is sealingly connected with gas absorption tube 3; the side wall of flask 1 is provided with an inert gas input pipeline 4.

[0022] In the embodiment, the side wall of flask 1 is further provided with a sealing port for inserting a temperature control device, and the sealing port is provided with a sealing plug 5.

[0023] In the embodiment, the horizontal section of inert gas input pipeline 4 penetrates from the side wall of flask 1, the vertical section of inert gas inlet extends in the dissolving reducing agent in flask 1, and the inert gas input pipeline 4 is provided with a gas flow meter (not shown in the figure).

[0024] In the embodiment, the outlet of condenser 2 extends into the absorption liquid in gas absorption tube 3 through a pipeline.

[0025] The embodiment further includes a piston and a connecting pipeline which are well known in the art, and the pipeline can be a glass tube, a ceramic tube or a flexible tube.

[0026] The working process of the embodiment is as follows: firstly, a certain volume of dissolving reducing agent is loaded in the purification flask, and nitrogen gas or other inert gas is introduced to make the solvent uniform and to remove the excess air in the system. The condensate water of the condenser is opened, the purification flask is heated, and the temperature of the solvent is kept at a set temperature. During the heating process of the flask, the temperature can be accurately controlled through the inserted temperature control device. After the purification is completed, the heating is stopped, and after the solvent is cooled, the solvent is transferred to a sealed container.

[0027] Application Example 1: The process of reagent purification for measuring trace sulfur content in niobium-iron alloy sample. The device is shown in Figure 1 .

[0028] The working process is as follows: firstly, 200 mL of hydriodic acid (mass fraction about 57%) and 60 mL of hypophosphoric acid (mass fraction about 50%) are loaded in the purification flask, nitrogen gas is introduced at a flow rate of 100 mL / min for 10 min to make the solvent uniform and to remove the excess air in the system. The heating device is opened and heated to boiling. The nitrogen gas flow is kept to control the temperature at 115℃±2℃, and the temperature is kept at micro-boiling for about 120 min. After the purification is completed, the heating device is closed. Then the solution is cooled and stored in a brown bottle for use.

[0029] Application Example 2: The process of reagent purification for measuring trace sulfur content in medium carbon steel sample. The device is shown in Figure 1 .

[0030] Its working process is as follows: first in the purification flask is equipped with 250 mL hydroiodic acid (mass fraction of about 57%) and 30 mL hypophosphorous acid (mass fraction of about 50%), with a flow rate of 120 mL / min nitrogen flow, keep 10 min, make the solvent mix evenly and exclude the system of excess air. Open the heating device, heating to boiling. Keep the nitrogen flow, make the temperature control at 115℃±2℃, keep micro-boiling about 120 min, after the purification, close the heating device. Then the solution is cooled, and stored in brown bottle, for use.

[0031] Application example 3: this embodiment is a process for the determination of trace sulfur content in pure iron sample reagent purification. The device is shown in Figure 1 .

[0032] Its working process is as follows: first in the purification flask is equipped with 500 mL hydroiodic acid (mass fraction of about 47%), 60 g sodium hypophosphite and 120 mL glacial acetic acid, with a flow rate of 120 mL / min nitrogen flow, keep 10 min, make the solvent mix evenly and exclude the system of excess air. Open the heating device, heating to boiling. Keep the nitrogen flow, make the temperature control at 113℃±2℃, keep micro-boiling about 120 min. After the purification, close the heating device. Then the solution is cooled, and stored in brown bottle, for use.

[0033] Application example 4: this embodiment is a process for the determination of trace sulfur content in low carbon steel sample reagent purification. The device is shown in Figure 1 .

[0034] Its working process is as follows: first in the purification flask is equipped with 250 mL phosphoric acid (mass fraction of about 85%), heated to 25℃, after cooling, add 33 g tin dichloride, continue to pass into the nitrogen flow, the flow rate is 150 mL / min. Open the heating device, heating to boiling. Keep the nitrogen flow, make the temperature control at 280℃±2℃, keep micro-boiling about 30 min, after the purification, close the heating device. Then the solution is cooled, sealed storage, for use.

[0035] It should be understood that: the above embodiment of the present application to the idea of doing a text description, but these text description, only the simple text description of the design idea of the present application, and not to the design idea of the present application limit, any combination, increase or modification, fall within the scope of the present application.

Claims

1. A purification device for a dissolving reducing agent used for determining the sulfur content, characterized in that The purification device comprises a flask, a condenser and a gas absorption tube which are connected in sequence by pipelines; different kinds of dissolving reducing agents are arranged in the flask; a heating device is arranged below the flask; the mouth of the flask is connected with the inlet of the condenser; the outlet of the condenser is connected with the gas absorption tube; an inert gas input pipeline is arranged on the side wall of the flask.

2. The purification device of claim 1, wherein A sealed mouth for adding or sucking the dissolving reducing agent or inserting a temperature control device is arranged on the side wall of the flask.

3. The purification apparatus of claim 2, wherein The sealed mouth is provided with a plug.

4. The purification device of claim 1, wherein The horizontal section of the inert gas input pipeline penetrates from the side wall of the flask, and the vertical section of the inert gas inlet extends into the dissolving reducing agent in the flask.

5. The purification apparatus of claim 1, wherein The outlet of the condenser extends into the absorption liquid of the gas absorption tube through a pipeline.

6. The purification apparatus of claim 1 or 5, wherein The pipeline is a glass tube, a ceramic tube or a flexible tube.

7. The purification apparatus of claim 1 or 4, wherein The inert gas input pipeline is a glass tube or a ceramic tube.

8. The purification apparatus of claim 1 or 4, wherein The inert gas input pipeline is provided with a gas flow meter.

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