Distillation equipment for measuring free ammonia and fixed ammonia

Abstract

The utility model discloses distillation equipment for measuring free ammonia and fixed ammonia, and relates to the field of distillation measurement. Distillation equipment for measuring free ammonia and fixed ammonia comprises a water bath electric pot, a distillation flask, a communicating pipe, a condensation pipe, a conical flask and an iron stand, the distillation flask and the condensation pipe are installed on a supporting rod on the iron stand through fixing clamps, and the distillation flask is located in the water bath electric pot; in the whole measuring process of free ammonia and fixed ammonia, through the arrangement of the sealing heat preservation cover, the rapid diffusion of water vapor generated by heated water can be effectively inhibited, and heat is more intensively acted on the distillation flask, so that the heat loss is reduced, the temperature rise of liquid in the distillation flask is quicker, and the boiling is quicker, thereby accelerating the distillation speed; compared with a non-sealed heat preservation device, the single distillation time can be greatly shortened, the overall detection efficiency can be remarkably improved when free ammonia and fixed ammonia are measured, and an experimenter can complete detection of multiple samples within shorter time.

Description

Technical Field

[0001] This utility model belongs to the field of distillation determination technology, specifically, it relates to distillation equipment for determining free ammonia and fixed ammonia. Background Technology

[0002] In numerous tests such as water quality testing, environmental monitoring, and chemical production, accurate determination of the content of free ammonia and fixed ammonia is of paramount importance. Free ammonia exists in water in the form of ammonia molecules, has strong volatility and an irritating odor, and is highly toxic to aquatic organisms. Fixed ammonia exists in the form of ammonium ions, is relatively stable, but excessive content can lead to eutrophication of water bodies. Therefore, accurate determination of free ammonia and fixed ammonia helps to assess water quality, ensure ecological and environmental safety, and control industrial production processes.

[0003] Currently, distillation is a commonly used and effective method for determining free and fixed ammonia. Traditional distillation equipment typically consists of a water bath, a distillation flask, a connecting tube, a condenser, an Erlenmeyer flask, and an iron stand. However, during the distillation process, the steam generated by the water bath easily diffuses into the surrounding environment, resulting in a significant loss of heat. This not only slows down the heating of the liquid in the distillation flask, prolonging the distillation time and reducing detection efficiency, but also wastes energy and increases detection costs. Furthermore, the unstable heat loss may cause temperature fluctuations during distillation, which in turn affects the quality and stability of the distillate, ultimately impacting the accuracy of the measurement results. Therefore, this invention is proposed. Utility Model Content

[0004] The technical problem to be solved by this utility model is to overcome the shortcomings of the prior art and provide a distillation apparatus for determining free ammonia and fixed ammonia that can overcome or at least partially solve the above problems.

[0005] To solve the above-mentioned technical problems, the basic concept of the technical solution adopted by this utility model is as follows: a distillation apparatus for determining free ammonia and fixed ammonia, including a water bath, a distillation flask, a connecting tube, a condenser, a conical flask, and an iron stand. The distillation flask and the condenser are both mounted on the support rods on the iron stand by fixing clamps. The distillation flask is located in the water bath, and the conical flask is located below the condenser. The two ends of the connecting tube are located at the opening ends of the distillation flask and the condenser, respectively. The heat exchange tube in the condenser passes downward through the condenser and extends into the conical flask. The connecting tube and the distillation flask, the condenser, and the heat exchange tube and the conical flask are all sealed by sealing plugs. The apparatus also includes a sealing and heat-insulating cover, which is threadedly connected to the opening of the water bath. The sealing and heat-insulating cover has an opening for use with the distillation flask and a pressure relief port with a pressure relief valve installed inside.

[0006] To facilitate the insulation of steam and prevent premature condensation into water, an insulating sleeve is further fitted onto the connecting pipe. The insulating sleeve has an air inlet and an air outlet at both ends, and the air inlet of the insulating sleeve is connected to the pressure relief port of the sealing insulation cover through a gas transmission pipe.

[0007] To facilitate the recycling and reuse of water resources, a condenser shell is fixedly fitted onto the condenser tube. The air outlet of the insulation sleeve is connected to the air inlet of the condenser shell through an exhaust pipe. A receiving box is placed on the iron frame. A drain pipe is fixedly connected to the drain outlet of the condenser shell, and the outlet of the drain pipe extends downward into the receiving box.

[0008] To prevent rapid leakage of steam from the water bath electric cooker, the threaded connection between the sealing heat insulation cover and the water bath electric cooker is further sealed by a sealing gasket, and a sealing ring is fixedly connected to the opening of the sealing heat insulation cover to seal between the sealing heat insulation cover and the distillation flask.

[0009] To further improve the service life and sealing effect of the gasket and sealing ring, both the gasket and sealing ring are made of high-temperature resistant rubber.

[0010] To further improve the seal between the sealing insulation cover and the distillation flask, the sealing ring is further described as an air bladder ring, which is filled with a volatile liquid.

[0011] To facilitate easier and safer rotation of the sealing and heat-insulating cover, a ring handle is further fixedly connected to the outer side of the sealing and heat-insulating cover via a connecting rod.

[0012] After adopting the above technical solution, the present invention has the following beneficial effects compared with the prior art: In the entire process of determining free ammonia and fixed ammonia, the present invention can effectively suppress the rapid diffusion of water vapor generated by the heated water through the setting of the sealed heat insulation cover, so that the heat is more concentrated on the distillation flask, thereby reducing heat loss, and the liquid in the distillation flask heats up faster and boils more rapidly, thereby accelerating the distillation speed. Compared with no sealed heat insulation device, it can significantly shorten the single distillation time. When determining free ammonia and fixed ammonia, it can significantly improve the overall detection efficiency, enabling the experimenter to complete the detection of multiple samples in a shorter time.

[0013] The specific embodiments of this utility model will be described in further detail below with reference to the accompanying drawings. Attached Figure Description

[0014] In the attached diagram:

[0015] Figure 1 This is a schematic diagram of the structure of this utility model;

[0016] Figure 2 This utility model Figure 1 A schematic diagram of the structure of part A;

[0017] Figure 3 This is a top view of the sealing and heat-insulating cover, sealing ring, and annular handle in this utility model.

[0018] In the diagram: 1. Water bath electric cooker; 101. Sealed insulation cover; 102. Sealing gasket; 103. Ring handle; 104. Sealing ring; 105. Gas supply pipe; 2. Distillation flask; 3. Connecting pipe; 301. Insulation sleeve; 302. Exhaust pipe; 303. Condenser shell; 304. Drain pipe; 4. Condenser tube; 401. Heat exchange tube; 402. Conical flask; 5. Iron stand; 501. Support rod; 502. Fixing clamp; 503. Receiving box; 6. Sealing plug. Detailed Implementation

[0019] To make the objectives, technical solutions, and advantages of the embodiments of this utility model clearer, the technical solutions in the embodiments will be clearly and completely described below with reference to the accompanying drawings. The following embodiments are used to illustrate this utility model, but are not intended to limit the scope of this utility model.

[0020] Example 1:

[0021] Reference Figures 1-3 The distillation apparatus for determining free and fixed ammonia includes a water bath 1, a distillation flask 2, a connecting pipe 3, a condenser 4, a conical flask 402, and an iron stand 5. The distillation flask 2 and the condenser 4 are both mounted on a support rod 501 on the iron stand 5 via a fixing clamp 502. The distillation flask 2 is located in the water bath 1, and the conical flask 402 is located below the condenser 4. The two ends of the connecting pipe 3 are located at the opening ends of the distillation flask 2 and the condenser 4, respectively. The heat exchange tube 401 in the condenser 4 passes downward through the condenser 4 and extends into the conical flask 402. The connecting pipe 3 is sealed with the distillation flask 2 and the condenser 4, and the heat exchange tube 401 is sealed with the conical flask 402 via a sealing plug 6. The apparatus also includes a sealing and heat-insulating cover 101, which is threadedly connected to the opening of the water bath 1. The sealing and heat-insulating cover 101 has an opening for use with the distillation flask 2 and a pressure relief port with a pressure relief valve installed inside.

[0022] When accurate quantitative analysis of free and fixed ammonia in water is required, first place a 500ml conical flask 402 below the condenser 4, add 50ml of a sulfuric acid standard solution with a concentration of C((1 / 2H2SO4) = 0.100mol / L), and add 3-4 drops of bromocresol green-methyl red mixed indicator. Accurately measure 50ml of the sample using a 50ml pipette and add it to the distillation flask 2 located in the water bath 1. Then add 300-40 ml of [unspecified substance] to the distillation flask 2. 0ml of water. At this time, the sealing and heat preservation cover 101 is threadedly connected to the opening of the water bath electric cooker 1. Its opening matches the distillation flask 2, covering the distillation flask 2 and sealing the water bath electric cooker 1. Due to the sealing effect of the sealing and heat preservation cover 101, the water vapor generated by the heated water is suppressed from diffusion. Only when the internal steam pressure is greater than the threshold of the pressure relief valve will the excess steam be discharged, thereby making the heat more concentrated on the distillation flask 2, enhancing the heating effect on the liquid inside the distillation flask 2, and improving the distillation efficiency.

[0023] When distilling and determining free ammonia, the temperature-controlled electric furnace is turned on to heat the water bath 1, causing the liquid in the distillation flask 2 to boil and distill. The vapor generated in the distillation flask 2 enters the condenser 4 through the connecting pipe 3, where it liquefies upon cooling in the heat exchange tube 401 of the condenser 4. The liquefied distillate flows down the heat exchange tube 401 into the conical flask 402 below, with the distillation rate controlled at 3-4 ml / min. Distillation is stopped when approximately 200 ml of distillate has been obtained. At this point, the sulfuric acid standard solution in the conical flask 402 absorbs the distilled free ammonia. The remaining sulfuric acid is then back-titrated with a sodium hydroxide standard solution of C(NaOH) = 0.100 mol / L. The titration endpoint is reached when the solution color changes from red to grayish-purple, according to the formula... Calculate the free ammonia content, where C1 is the concentration of sulfuric acid standard solution, C2 is the concentration of sodium hydroxide standard solution, V1 is the volume of sulfuric acid standard solution used, V2 is the volume of sodium hydroxide standard solution used, and V is the sampling volume.

[0024] When determining and distilling fixed ammonia, replace the flask with another 500ml Erlenmeyer flask (402), add 50ml of the above-mentioned sulfuric acid standard solution, and add 3-4 drops of methyl red indicator. Add excess NaOH solution to the residue after distillation of free ammonia to promote the conversion of fixed ammonia (existing as ammonium ions) into free ammonia. Restart the heating device and continue distillation. The sealing and heat preservation cover 101 continues to play its sealing role and improve distillation efficiency. Stop distillation when the distillate is about 200ml. Wash the inner wall of the cooler with pure water and add the washing liquid to the conical flask 402.

[0025] Finally, the sulfuric acid standard solution that has absorbed freshly distilled free ammonia (derived from the conversion of the original fixed ammonia) is titrated with sodium hydroxide standard solution. The endpoint is reached when the solution color changes from red to yellow, using the same formula as for calculating free ammonia. Calculate the fixed ammonia content.

[0026] Throughout the determination of free and fixed ammonia, the sealing and heat preservation cover 101 effectively inhibits the rapid diffusion of water vapor generated by the heated water, allowing the heat to be more concentrated on the distillation flask 2, thereby reducing heat loss. The liquid in the distillation flask 2 heats up faster and boils more rapidly, thus accelerating the distillation speed. Compared with the absence of a sealing and heat preservation device, it can significantly shorten the single distillation time. When determining free and fixed ammonia, it can significantly improve the overall detection efficiency, enabling the experimenter to complete the detection of multiple samples in a shorter time.

[0027] A stable and efficient distillation process is key to accurately determining the content of free and fixed ammonia. The sealed heat insulation cover 101 ensures stable distillation conditions and avoids fluctuations in the distillation process due to heat loss. Stable distillation results in a more uniform rate and composition of distillate, which reduces sources of error in titration calculations. For example, in the determination of free ammonia, a stable distillate ensures that the sulfuric acid standard solution absorbs free ammonia more fully and stably, leading to more accurate results in the subsequent sodium hydroxide back titration. Ultimately, the calculated content of free and fixed ammonia is closer to the true value.

[0028] The sealed heat insulation cover 101 is equipped with a pressure relief port and a pressure relief valve. During the distillation process, if excessive steam is generated due to heating, causing the pressure inside the device to become too high, the pressure relief valve will automatically open to release the pressure, preventing safety accidents such as device explosion caused by excessive pressure. This creates a safer operating environment for the experimenters, avoids personal injury and property loss caused by equipment failure, and ensures the smooth progress of the experiment.

[0029] Example 2:

[0030] Reference Figures 1-3The distillation apparatus used for determining free and fixed ammonia is basically the same as in Example 1, but with a further improvement: a heat-insulating sleeve 301 is fitted onto the connecting pipe 3. The heat-insulating sleeve 301 has an inlet and an outlet at both ends, respectively. The inlet of the heat-insulating sleeve 301 is connected to the pressure relief port of the sealed heat-insulating cover 101 via a gas supply pipe 105. The heat-insulating sleeve 301 effectively reduces the heat loss of the steam in the connecting pipe 3. During distillation, steam enters the condenser 4 from the distillation flask 2 through the connecting pipe 3. If the connecting pipe 3 is not insulated, the steam heat... The steam is easily dissipated into the surrounding environment, causing the steam temperature to drop and some steam to condense prematurely, affecting the distillation efficiency. However, the insulation sleeve 301 can maintain the steam temperature, allowing more steam to smoothly enter the condenser 4 and ensuring that the distillation process is carried out efficiently. At the same time, the steam discharged from the pressure relief port of the sealed insulation cover 101 is introduced into the air inlet of the insulation sleeve 301 through the gas delivery pipe 105, realizing the reuse of waste heat. This steam heat, which might have been directly discharged, can be used to maintain the steam temperature in the connecting pipe 3, further improving the energy utilization rate and reducing the overall energy consumption.

[0031] A condenser shell 303 is fixedly fitted onto the condenser tube 4. The outlet of the insulation sleeve 301 and the inlet of the condenser shell 303 are connected through an exhaust pipe 302. A receiving box 503 is placed on the iron stand 5. A drain pipe 304 is fixedly connected to the drain outlet of the condenser shell 303. The outlet of the drain pipe 304 extends downward into the receiving box 503. The condenser shell 303 is fixedly fitted onto the condenser tube 4, and the outlet of the insulation sleeve 301 and the inlet of the condenser shell 303 are connected through an exhaust pipe 302. This allows the steam discharged from the insulation sleeve 301 to enter the condenser shell 303, thereby condensing the discharged steam on the condenser tube 4. The condensed water can be transported to the receiving box 503 through the drain pipe 304 for collection, which facilitates the reuse of water resources and saves testing costs.

[0032] Example 3:

[0033] Reference Figures 1-3The distillation apparatus for determining free and fixed ammonia is basically the same as in Example 2, but with a further improvement: the threaded connection between the sealing heat insulation cover 101 and the water bath electric cooker 1 is sealed by a sealing gasket 102, and a sealing ring 104 is fixedly connected to the opening of the sealing heat insulation cover 101 to seal between the sealing heat insulation cover 101 and the distillation flask 2. The sealing gasket 102 is used to seal the threaded connection between the heat insulation cover 101 and the water bath electric cooker 1, and the sealing ring 104 seals the opening between the heat insulation cover 101 and the distillation flask 2. The double sealing design greatly enhances the sealing performance of the entire distillation system and effectively prevents the leakage of water vapor in the water bath electric cooker 1. During the distillation process, reducing water vapor leakage means that more heat can be concentrated on the liquid in the distillation flask 2, causing it to reach the boiling state faster and maintain a stable distillation rate. For example, when determining free ammonia, efficient distillation allows the free ammonia in the sample to be distilled out more quickly and completely, thereby improving the distillation efficiency and shortening the detection time.

[0034] Both the sealing gasket 102 and the sealing ring 104 are made of high-temperature resistant rubber, such as silicone rubber, fluororubber, or ethylene propylene rubber. During the distillation process, the water bath 1 will continuously heat, generating a large amount of heat. The sealing gasket 102 and the sealing ring 104 are in a high-temperature environment. The high-temperature resistant rubber can withstand this high temperature and will not deform, melt, or age due to the temperature rise, effectively ensuring the sealing performance and service life. At high temperatures, it can still fit tightly against the sealing parts and maintain a good sealing effect. This ensures that water vapor will not leak from the threaded connection between the sealing insulation cover 101 and the water bath 1, or from the opening between the sealing insulation cover 101 and the distillation flask 2, so that the heat is concentrated on the liquid inside the distillation flask 2, ensuring distillation efficiency and ensuring that free ammonia and fixed ammonia can be fully distilled out, thereby ensuring the accuracy of the measurement results.

[0035] The sealing ring 104 is an air bladder ring filled with a volatile liquid. The gas generated by the volatile liquid evaporating when heated fills the air bladder ring, making it more tightly connected to the opening of the distillation flask 2 and the sealing insulation cover 101. Compared with ordinary sealing rings 104, the air bladder ring can distribute pressure more evenly on the sealing surface under gas pressure, effectively filling tiny pores and preventing vapor leakage. During the determination of free ammonia and fixed ammonia, it can prevent ammonia vapor from escaping, ensuring that all generated ammonia can be accurately collected and measured, thus improving the accuracy of the measurement results.

[0036] For volatile liquids, liquids with low boiling points such as ethanol, acetone, and diethyl ether can be used.

[0037] Example 4:

[0038] Reference Figures 1-3The distillation equipment used for determining free ammonia and fixed ammonia is basically the same as in Example 3, except that: a ring handle 103 is fixedly connected to the outside of the sealed heat insulation cover 101 via a connecting rod.

[0039] The design of the ring handle 103 provides the operator with a stable and easy-to-grip part. When it is necessary to rotate the sealing and heat insulation cover 101, the operator can easily hold the ring handle 103 and apply force to rotate the sealing and heat insulation cover 101. Compared with opening by directly contacting the surface of the sealing and heat insulation cover 101, the ring handle 103 provides a larger force application area and better grip stability, making the opening and closing operation more effortless and convenient, and effectively improving the operating efficiency.

[0040] During the distillation process, the sealed heat insulation cover 101 will heat up by absorbing heat from the water bath electric kettle 1, and the surface temperature will be high. The ring handle 103 is fixedly connected to the sealed heat insulation cover 101 through the connecting rod, which keeps the handle at a certain distance from the surface of the sealed heat insulation cover 101. When the operator holds the ring handle 103, his / her hand is away from the high temperature area, avoiding direct contact with the sealed heat insulation cover 101, thereby effectively reducing the risk of burns and ensuring the personal safety of the operator.

[0041] The above description is only a preferred embodiment of the present utility model and is not intended to limit the present utility model in any way. Although the present utility model has been disclosed above with reference to a preferred embodiment, it is not intended to limit the present utility model.

Claims

1. A distillation apparatus for determining free ammonia and fixed ammonia, comprising a water bath (1), a distillation flask (2), a connecting tube (3), a condenser (4), a conical flask (402), and an iron stand (5), wherein the distillation flask (2) and the condenser (4) are mounted on a support rod (501) on the iron stand (5) by means of a fixing clamp (502), the distillation flask (2) is located in the water bath (1), the conical flask (402) is located below the condenser (4), the two ends of the connecting tube (3) are respectively located at the open ends of the distillation flask (2) and the condenser (4), the heat exchange tube (401) in the condenser (4) extends downward through the condenser (4) and into the conical flask (402), and the connecting tube (3) is sealed with a sealing plug (6) to the distillation flask (2), the condenser (4), and the heat exchange tube (401) and the conical flask (402), characterized in that, Also includes: A sealing heat insulation cover (101) is threadedly connected to the pot opening of the water bath electric pot (1). The sealing heat insulation cover (101) has an opening for use with a distillation flask (2). The sealing heat insulation cover (101) has a pressure relief port, and a pressure relief valve is installed in the pressure relief port.

2. The distillation apparatus for determining free ammonia and fixed ammonia according to claim 1, characterized in that, The connecting pipe (3) is fitted with a heat-insulating sleeve (301). The heat-insulating sleeve (301) has an air inlet and an air outlet at both ends. The air inlet of the heat-insulating sleeve (301) is connected to the pressure relief port of the sealing heat-insulating cover (101) through a gas transmission pipe (105).

3. The distillation apparatus for determining free ammonia and fixed ammonia according to claim 2, characterized in that, A condenser shell (303) is fixedly sleeved on the condenser tube (4). The air outlet of the insulation sleeve (301) is connected to the air inlet of the condenser shell (303) through an exhaust pipe (302). A receiving box (503) is placed on the iron frame (5). A drain pipe (304) is fixedly connected to the drain outlet of the condenser shell (303). The outlet of the drain pipe (304) extends downward into the receiving box (503).

4. The distillation apparatus for determining free ammonia and fixed ammonia according to claim 1, characterized in that, The threaded connection between the sealing heat insulation cover (101) and the water bath electric cooker (1) is sealed by a sealing gasket (102), and a sealing ring (104) is fixedly connected to the opening of the sealing heat insulation cover (101) to seal between the sealing heat insulation cover (101) and the distillation flask (2).

5. The distillation apparatus for determining free ammonia and fixed ammonia according to claim 4, characterized in that, Both the sealing gasket (102) and the sealing ring (104) are made of high-temperature resistant rubber.

6. The distillation apparatus for determining free ammonia and fixed ammonia according to claim 5, characterized in that, The sealing ring (104) is an airbag ring, and the airbag ring is filled with a volatile liquid.

7. The distillation apparatus for determining free ammonia and fixed ammonia according to claim 1, characterized in that, The outer side of the sealing and heat-insulating cover (101) is fixedly connected to a ring handle (103) via a connecting rod.

Images