Equipment for rapidly measuring sulfite in qualified solution for electrolytic manganese

Abstract

The utility model discloses equipment for rapidly measuring sulfite in qualified liquid for electrolytic manganese, which comprises a flask and an alcohol lamp, the alcohol lamp is used for heating the flask, the top of the flask is connected with a fluid delivery pipe and a constant-pressure funnel, one side of the flask is communicated with a condenser pipe, and the other side of the flask is communicated with the constant-pressure funnel. The output end of the condensation pipe is provided with a submerged pipe and a liquid level pipe through a flow dividing conveying pipe. According to the equipment for rapidly determining the sulfite in the qualified liquid for the electrolytic manganese, the difficulty is reduced by rapidly determining the sulfite in the qualified liquid for the electrolytic manganese, the operation is simple, the required reagent is non-toxic and harmless, the equipment is completely suitable for industrial detection, and the rapid determination of the sulfite in the qualified liquid for the electrolytic manganese can be better and more rapidly realized; and the process index of sulfite in the qualified liquid for electrolytic manganese is effectively monitored.

Description

Technical Field

[0001] The utility model belongs to the technical field of chemical detection, and in particular relates to a method for rapidly and accurately determining sulfite in a qualified solution for electrolytic manganese. Background Art

[0002] With the development of new energy in my country, manganese as a raw material of positive material requires higher purity. In the process of electrolytic manganese production, its additives have also changed accordingly, from the original selenium dioxide as an antioxidant to the current sulfur dioxide additive or sulfite compound additive, making the detection of sulfite index in the qualified solution for electrolytic manganese very critical. At present, the sulfite detection methods are mainly chromatography, spectrophotometry, electrochemical method, weight method, etc. The above methods have great deviations in the determination of trace sulfite due to the interference of elements such as manganese and sulfate. In the reference industrial boiler water quality sulfite determination method (GB / T1576-2008), the sulfite detection reagent iodine reacts with the reducing salts in the qualified solution, making the measurement result higher; in the reference food sulfite determination method (GB / T5009.34-1996), the reagents used, high mercuric chloride, formaldehyde, and lead acetate, are highly toxic and harmful substances.

[0003] In order to solve the above problems, it is necessary to study the method of sulfite determination, reduce the difficulty of determination and improve the safety of the test, and this patent is specially proposed. Utility Model Content

[0004] The utility model aims to provide a method for quickly determining sulfite in a qualified solution for electrolytic manganese, so as to solve the problems raised in the above-mentioned background technology.

[0005] In order to achieve the above purpose, the utility model provides the following technical solutions:

[0006] The invention discloses a rapid determination device for sulfite in qualified solution for electrolytic manganese, comprising a flask and an alcohol lamp, wherein the alcohol lamp heats the flask, the top of the flask is connected with a fluid delivery pipe and a constant pressure funnel, one side of the flask is connected with a condenser, and the output end of the condenser is respectively provided with a submerged pipe and a liquid surface pipe through a shunt delivery pipe.

[0007] As a further solution of the utility model: the flask is a two-mouth flat-bottom distillation flask, which has an opening a and a steam opening b respectively, and the fluid delivery pipe and the constant pressure funnel are extended into the flask through the opening a.

[0008] As a further solution of the utility model: the constant pressure funnel comprises a bottle body, a conduit, a constant pressure tube and two valve bodies;

[0009] The top of the bottle body is connected with the flask through a conduit, the conduit is communicated with the top of the bottle body through a constant pressure tube, and the output end of the bottle body and the constant pressure tube are both equipped with a valve body.

[0010] As a further solution of the utility model: the condenser tube includes a heat exchange tube and a medium tube, the two ends of the heat exchange tube are respectively connected to the steam port b and the diversion conveying pipe, and the medium tube is installed on the outside of the heat exchange tube.

[0011] As a further solution of the utility model: the heat exchange tube and the shunt delivery tube are detachably connected by a rubber tube sleeve, the shunt delivery tube is a glass tee tube, the condenser tube is arranged to be inclined downward, the top of the shunt delivery tube has a pipe opening which is the input end and is connected to the heat exchange tube, and the bottom of the shunt delivery tube has two pipe openings which are the output ends and are respectively connected to the underwater tube and the liquid surface tube.

[0012] As a further solution of the utility model: the submerged tube and the liquid surface tube are located in the vessel, the output end of the submerged tube extends to a position close to the bottom wall of the vessel, and the output end of the liquid surface tube is located close to the rubber stopper of the vessel.

[0013] As a further solution of the utility model: valves are arranged on the submerged pipe, the liquid surface pipe and the fluid delivery pipe.

[0014] Compared with the prior art, the beneficial effects of the utility model are:

[0015] The device for rapid determination of sulfite in qualified solution for electrolytic manganese comprises the following steps: placing qualified solution for electrolytic manganese in two flat-bottomed distillation flasks, adding pure water to the qualified solution through a fluid delivery pipe, installing a condensation device, inserting a submerged pipe of the condensation pipe into an oxidizing absorbent of a vessel, adding an acidulant into the flask through a constant pressure funnel, boiling and distilling for 10 minutes, switching a liquid level pipe, leaving the liquid level, further distilling for 2 minutes, washing a part immersed in the oxidizing absorbent device with a small amount of pure water, adding a quantitative acidic reducing agent into the absorption liquid, heating to 60-65°C, titrating with the oxidizing absorbent, and calculating the total amount of sulfite according to the titration volume. The device for rapid determination of sulfite in qualified solution for electrolytic manganese reduces the difficulty, is simple to operate, requires non-toxic and harmless reagents, is fully applicable to industrial detection, can better and faster realize rapid determination of sulfite in qualified solution for electrolytic manganese, and effectively monitors the process index of sulfite in qualified solution for electrolytic manganese. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 The flowchart of the rapid determination method of sulfite in qualified solution for electrolytic manganese is as follows;

[0017] Figure 2 This is a schematic diagram of a rapid determination device for sulfite in a qualified solution for electrolytic manganese;

[0018] Figure 3 Rapid determination equipment and method for sulfite in qualified solution for electrolytic manganese 2- Standard solution determination data table;

[0019] Figure 4 The data sheet of qualified solution for electrolytic manganese, which includes the rapid determination equipment and method for sulfite in qualified solution for electrolytic manganese;

[0020] Figure 5 This is a data sheet for the rapid determination of sulfite in qualified solution for electrolytic manganese and its determination method, and a spiked recovery experiment determination data sheet for qualified solution for electrolytic manganese.

[0021] In the figure: 1. flask; 2. fluid delivery pipe; 3. medium pipe; 4. heat exchange tube; 5. bottle body; 6. constant pressure tube; 7. catheter; 8. valve body; 9. rubber tube sleeve; 10. diversion delivery pipe; 11. container; 12. submerged pipe; 13. liquid surface pipe; 14. alcohol lamp; 15. valve. DETAILED DESCRIPTION

[0022] See also Figure 1 In the embodiment of the utility model, the rapid determination device of sulfite in the qualified solution for electrolytic manganese comprises a flask 1 and an alcohol lamp 14. The alcohol lamp 14 heats the flask 1. The top of the flask 1 is connected to a fluid delivery tube 2 and a constant pressure funnel. One side of the flask 1 is connected to a condenser. The output end of the condenser is respectively provided with a submerged tube 12 and a liquid surface tube 13 through a shunt delivery tube 10. The qualified solution for electrolytic manganese is put into the flask 1. A relative proportion of pure water is added through the fluid delivery tube 2, the solution is shaken, and the solution is boiled and distilled under the heating of the alcohol lamp 14. A condensation device is installed. The lower end of the condenser is inserted into the oxidizing absorbent. The submerged tube 12 is located below the liquid surface, and the liquid surface tube 13 is located above the liquid surface.

[0023] In a preferred embodiment, the flask 1 is a two-mouth flat-bottom distillation flask, which has an opening a and a steam opening b, respectively. The fluid delivery pipe 2 and the constant pressure funnel both extend into the flask 1 through the opening a. The constant pressure funnel includes a bottle body 5, a conduit 7, a constant pressure tube 6 and two valve bodies 8.

[0024] The top of the bottle body 5 is connected to the flask 1 through a conduit 7, and the conduit 7 is connected to the top of the bottle body 5 through a constant pressure tube 6. The output end of the bottle body 5 and the constant pressure tube 6 are both equipped with a valve body 8. The output end of the bottle body 5 extends downward into the conduit 7. The acidifier is stored in the bottle body 5 to prevent the acidifier from entering the constant pressure tube 6. The acidifier is added to the flask 1 through the constant pressure funnel.

[0025] In a preferred embodiment, the condenser includes a heat exchange tube 4 and a medium tube 3, the two ends of the heat exchange tube 4 are respectively connected to the steam port b and the shunt delivery tube 10, the medium tube 3 is installed on the outside of the heat exchange tube 4, the heat exchange tube 4 and the shunt delivery tube 10 are connected by a rubber tube sleeve 9, and two pipes for adding and discharging the medium are provided on the medium tube 3, and the two pipes can be sealed by a cover, and the medium is stored inside the medium tube 3, and the cold medium is stored in this application to condense the substance in the heat exchange tube 4;

[0026] The submerged tube 12 and the liquid surface tube 13 are located in the vessel 11, and the output end of the submerged tube 12 extends to near the bottom wall of the vessel 11, and the output end of the liquid surface tube 13 is located near the rubber stopper of the vessel 11. The submerged tube 12, the liquid surface tube 13 and the fluid delivery tube 2 are all provided with valves 15, and the submerged tube 12 and the liquid surface tube 13 are switched by opening and closing the valve 15. The constant pressure funnel adds 50 ml of acidifier into the distillation flask, and boils and distills for 10 minutes. During this process, the valve 15 of the submerged tube 12 is opened, and the valve 15 of the liquid surface tube 13 is closed. After boiling and distilling for 10 minutes, the valve 15 of the submerged tube 12 is closed, and the valve 15 of the liquid surface tube 13 is opened, and the distillation continues.

[0027] A method for rapidly determining sulfite in a qualified solution for electrolytic manganese, comprising the following steps:

[0028] S1: Take qualified solution for electrolytic manganese and place it in two flat-bottomed distillation flasks;

[0029] S2: adding pure water to the qualified solution;

[0030] S3: Install the condensing device, and insert the lower end of the condensing tube into the oxidation absorbent;

[0031] S4: adding an acidulant into the distillation flask through a constant pressure funnel;

[0032] S5: After boiling and distilling for 10 minutes, the lower end of the condenser is separated from the liquid surface, and distilled for another 2 minutes, and the part immersed in the oxidation absorbent device is rinsed with a small amount of pure water;

[0033] S6: Add a quantitative acidic reducing agent to the absorption liquid and heat it to 60-65°C;

[0034] S7: Titrate with an oxidizing absorbent and calculate the total amount of sulfite based on the titration volume.

[0035] In a preferred embodiment, the ratio of the qualified electrolytic manganese solution, the acidifier, the oxidizing absorbent and the acidic reducing agent is 1:1:2:2.

[0036] In a preferred embodiment, the oxidation absorbent is a KMnO4=0.0020 mol / L standard solution.

[0037] In a preferred embodiment, the acidifying agent is a sulfuric acid solution.

[0038] In a preferred embodiment, the acidic reducing agent is a mixture of sulfuric acid and sodium oxalate.

[0039] In a preferred embodiment, the acidulant is a 20% sulfuric acid solution (volume concentration).

[0040] In a preferred embodiment, the acidic reducing agent solution is 10% sulfuric acid (volume concentration), Na2C2O4=0.005mol / L standard solution.

[0041] For the utility model of the rapid determination method of sulfite in qualified solution for electrolytic manganese, a method of comparative verification by adding standard and recovering is adopted, and the specific steps are as follows:

[0042] Standard sample experiment: Take 50ml of SO3 2- 6 portions of 200mg / L sodium sulfite standard solution are placed in 500ml flat-bottomed two-necked flasks, 200ml of pure water is added, shaken, and a condenser is installed. The lower end of the condenser is inserted into the oxidizing absorbent. The oxidizing absorbent is 100ml of KMnO4=0.0020mol / L standard solution. 50ml of acidifier is added to the distillation flask through a constant pressure funnel. After boiling and distilling for 10min, the liquid level tube (13) is switched to make the lower end of the condenser leave the liquid surface. Distill for another 2min, rinse the part immersed in the oxidizing absorbent device with a small amount of pure water, add 100ml of acidic reducing agent Na2C2O4=0.005mol / L standard solution to the absorption liquid, heat to 60-65℃, and titrate with the oxidizing absorbent (KMnO4=0.0020mol / L standard solution) until light pink is the end point. Record the volume and calculate the total amount of sulfite. The calculation formula is ρSO3 2- =5×C KMnO4 ×V KMnO4 / 2〕×M / V 样 ×1000 (M is SO3 2- Molecular weight), the measurement results are as follows Figure 3 As shown, this method has good accuracy and precision, SO3 2- The detection standard deviation RSD was 0.66% and the relative error was -0.10%.

[0043] Qualified liquid sample experiment for electrolytic manganese: Take 10 portions of 50ml qualified liquid respectively, place them in 500ml flat-bottomed two-necked flasks, add 200ml pure water, shake well, install condensation device, insert the lower end of the condenser into the oxidizing absorbent, the oxidizing absorbent is 100ml KMnO4=0.0020mol / L standard solution, add 50ml acidifier into the distillation flask through the constant pressure funnel, boil and distill for 10min, switch the liquid level tube (13) to make the lower end of the condenser leave the liquid surface, distill for another 2min, rinse the part immersed in the oxidizing absorbent device with a small amount of pure water, add 100ml acidic reducing agent Na2C2O4=0.005mol / L standard solution into the absorption liquid, heat to 60-65℃, and titrate with oxidizing absorbent (KMnO4=0.0020mol / L standard solution) until light pink is the end point, record the volume, calculate the total amount of sulfite, and calculate the formula ρSO3 2- =5×C KMnO4 ×V KMnO4 / 2〕×M / V 样 ×1000 (M is SO3 2- Molecular weight), the measurement results are as follows Figure 4 As shown, the relative standard deviation of the determination of sulfite in the qualified solution for electrolytic manganese is 0.81%. This method has good stability in determining sulfite in the qualified solution for electrolytic manganese.

[0044] Electrolytic manganese qualified solution spike recovery experiment: Take 10 portions of 50ml electrolytic manganese qualified solution and place them in 500ml flat-bottomed two-necked flasks, then add 50ml, SO3 2- The content is 200mg / L sodium sulfite.

[0045] Add 150mL of pure water to the standard solution, shake well, install the condenser, insert the lower end of the condenser into the oxidizing absorbent, the oxidizing absorbent is 100mlKMnO4=0.0020mol / L standard solution, add 50ml of acidifier to the distillation flask through a constant pressure funnel, boil and distill for 10 minutes, switch the liquid level tube (13) to make the lower end of the condenser leave the liquid surface, distill for another 2 minutes, rinse the part immersed in the oxidizing absorbent device with a small amount of pure water, add 100ml of acidic reducing agent Na2C2O4=0.005mol / L standard solution to the absorption liquid, heat to 60-65℃, and titrate with the oxidizing absorbent (KMnO4=0.0020mol / L standard solution) to a light pink end point, record the volume, and calculate the total amount of sulfite. The calculation formula is ρSO3 2- =〔5×C KMnO4 ×V KMnO4 / 2〕×M / V 样 ×1000 (M is SO3 2- Molecular weight), the measurement results are as follows Figure 5As shown, the recovery rate of spiked qualified solution for electrolytic manganese is between 98.85% and 100.81%, indicating that this method has good accuracy and is accurate and reliable for the detection of sulfite in qualified solution for electrolytic manganese.

[0046] The utility model reduces the difficulty of rapid determination of sulfite in qualified solution for electrolytic manganese, is simple to operate, requires non-toxic and harmless reagents, is fully applicable to industrial detection, can better and faster realize rapid determination of sulfite in qualified solution for electrolytic manganese, and effectively monitors the process indicators of sulfite in qualified solution for electrolytic manganese.

[0047] It should be noted that the above embodiments all belong to the same utility model concept, and the description of each embodiment has its own focus. For matters that are not described in detail in some embodiments, reference can be made to the description in other embodiments.

[0048] The above-mentioned embodiments only express the implementation methods of the utility model, and the descriptions thereof are relatively specific and detailed, but they cannot be understood as limiting the scope of the utility model patent. It should be pointed out that for ordinary technicians in this field, several modifications and improvements can be made without departing from the concept of the utility model, and these all belong to the protection scope of the utility model. Therefore, the protection scope of the utility model patent shall be based on the attached claims.

Claims

1. A device for rapidly determining sulfite in a qualified solution for electrolytic manganese, comprising a flask (1) and an alcohol lamp (14), wherein the alcohol lamp (14) heats the flask (1), and is characterized in that: The top of the flask (1) is connected to a fluid delivery tube (2) and a constant pressure funnel, and one side of the flask (1) is connected to a condenser. The output end of the condenser is respectively equipped with a liquid submersible tube (12) and a liquid surface tube (13) via a split flow delivery tube (10).

2. The rapid determination device for sulfite in qualified solution for electrolytic manganese according to claim 1, characterized in that: The flask (1) is a two-mouth flat-bottom distillation flask, which has an opening a and a steam opening b. The fluid delivery pipe (2) and the constant pressure funnel both extend into the flask (1) through the opening a.

3. The rapid determination device for sulfite in qualified solution for electrolytic manganese according to claim 1 or 2, characterized in that: The constant pressure funnel comprises a bottle body (5), a conduit (7), a constant pressure tube (6) and two valve bodies (8); The top of the bottle body (5) is connected to the flask (1) via a conduit (7), the conduit (7) is connected to the top of the bottle body (5) via a constant pressure tube (6), and the output end of the bottle body (5) and the constant pressure tube (6) are both equipped with a valve body (8).

4. The rapid determination device for sulfite in qualified solution for electrolytic manganese according to claim 2, characterized in that: The condenser tube comprises a heat exchange tube (4) and a medium tube (3); both ends of the heat exchange tube (4) are respectively connected to a steam port b and a flow diversion pipe (10); and the medium tube (3) is installed on the outside of the heat exchange tube (4).

5. The rapid determination device for sulfite in qualified solution for electrolytic manganese according to claim 4, characterized in that: The heat exchange tube (4) and the shunt delivery tube (10) are detachably connected via a rubber tube sleeve (9); the shunt delivery tube (10) is a glass three-way tube; the condenser tube is arranged to be inclined downward; the top of the shunt delivery tube (10) has a pipe opening which is an input end and is connected to the heat exchange tube (4); the bottom of the shunt delivery tube (10) has two pipe openings which are output ends and are respectively connected to the submerged tube (12) and the liquid surface tube (13).

6. The rapid determination device for sulfite in qualified solution for electrolytic manganese according to claim 2, characterized in that: The submerged tube (12) and the liquid surface tube (13) are located in the vessel (11); the output end of the submerged tube (12) extends to a position close to the bottom wall of the vessel (11); and the output end of the liquid surface tube (13) is located close to the rubber stopper of the vessel (11).

7. The rapid determination device for sulfite in qualified solution for electrolytic manganese according to claim 6, characterized in that: The submerged pipe (12), the liquid surface pipe (13) and the fluid delivery pipe (2) are all provided with valves (15).

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