CN219186929U - Condensation reflux unit and sodium alginate content measuring device - Google Patents
Condensation reflux unit and sodium alginate content measuring device Download PDFInfo
- Publication number
- CN219186929U CN219186929U CN202222020266.5U CN202222020266U CN219186929U CN 219186929 U CN219186929 U CN 219186929U CN 202222020266 U CN202222020266 U CN 202222020266U CN 219186929 U CN219186929 U CN 219186929U
- Authority
- CN
- China
- Prior art keywords
- liquid adding
- flask
- sodium alginate
- content measuring
- measuring device
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The utility model belongs to the field of chemical reaction instrument devices, and particularly relates to a condensation reflux device and a sodium alginate content measuring device. In order to solve the defect that the existing sodium alginate content measuring device is inconvenient when hydrochloric acid is added, the utility model provides a condensation reflux device and a sodium alginate content measuring device. The condensing reflux device provided by the utility model is provided with a liquid adding device, the liquid adding device comprises a liquid adding port from top to bottom, a liquid adding port branch pipe is connected below the liquid adding port, and a switch is arranged on the liquid adding port branch pipe. The sodium alginate content measuring device provided by the utility model comprises a flask, a condensation reflux device, a gas washing device, an absorption device and a heating device. The condensing reflux device provided by the utility model adds the concentrated hydrochloric acid into the flask through the liquid adding opening, so that the operation of adding the hydrochloric acid into the flask is convenient, the flask can keep good air tightness all the time, and the concentrated hydrochloric acid is prevented from corroding the rubber tube filled with nitrogen.
Description
Technical Field
The utility model belongs to the field of chemical reaction instrument devices, and particularly relates to a condensation reflux device and a sodium alginate content measuring device.
Background
Sodium alginate is a common food or pharmaceutical additive. The method for detecting sodium alginate in food or pharmaceutical products is generally an alginate assay method as described in U.S. pharmacopoeia USP43-NF38, code 311. The principle of the measuring method is as follows: in a closed heating system, the alginate and the concentrated hydrochloric acid undergo decarboxylation reaction to generate carbon dioxide, the carbon dioxide is taken out of the system by taking nitrogen as carrier gas, the carbon dioxide is absorbed by excessive sodium hydroxide, and the content of sodium alginate in the sample can be calculated by testing the amount of the residual sodium hydroxide by a titration method.
The instrument is shown in figure 1, A is a capillary metering valve, B is N 2 Flowmeter, D is 250ml round bottom flask with branch pipe, C is branch pipe mouth, and N 2 The pipe connection, E is heating jacket, F is snakelike condensation back flow, G is U-shaped pipe, fills up 2 sections 20 mesh zinc powder, and the centre and both sides use 3 inch glass cotton plugs, H is adapter, I is polyethylene plug, J is the absorption bottle. The interface size of the absorption bottle is 45/50, and the rest of the interfaces of the device are 24/40.
The measuring method comprises the following operation steps:
1. precisely weighing 250mg sample into flask D, adding 50ml of 0.1mol/L hydrochloric acid, adding several zeolite particles, connecting to reflux device F, coating vacuum silicone grease on the joint, sealing, and connecting branch pipe orifice C to N 2 On the tube, the flow rate of the cooling water of the reflux device F was adjusted to 2L/min.
2. The preheating step need only be performed in the presence of inorganic carbonates in the sample.
The preheating operation steps are as follows: regulation of N 2 The flow rate is 90-100 ml/min, the sample in the flask D is heated to be boiled, kept for 2min, and the heating is closed, and the temperature is reduced for 10min. If the sample does not contain carbonate, no preheating step is required.
3. The absorption device J was connected, 46ml of concentrated hydrochloric acid was added to the flask D, and N was adjusted 2 The flow speed is 90-100 ml/min, the system is balanced for 5min, and N is reduced 2 The flow rate is 60-65 ml/min, 10 drops of N-butanol, 25ml of 0.25mol/L sodium hydroxide titration solution and 50ml of distilled water are sequentially added into an absorption device, a flask D is heated until a reaction system boils, the boiling reflux is maintained for 2h, the heating is stopped, and the N is increased 2 The flow rate is 90-100 ml/min, and the cooling is carried out for 10min. Washing the absorber 3 times with distilled water, and washing with N 2 The liquid was pressed into the absorption bottle together. The absorbent bottle was removed and 10mL10% BaCl was immediately added 2 The solution was mixed by shaking to give a barium carbonate precipitate, 3 drops of phenolphthalein indicator were added, and the remaining sodium hydroxide was titrated with 0.1mol/L hydrochloric acid.
Blank experiments were performed (no sample was added, the rest of the procedure was as above).
The existing sodium alginate content measuring device comprises a flask, a pipe orifice of the flask is connected with a condensation reflux device, a branch pipe orifice of the flask is connected with a rubber pipe serving as a nitrogen inlet, when concentrated hydrochloric acid is added into the flask, the rubber pipe which is filled with nitrogen into the flask needs to be pulled out, the concentrated hydrochloric acid is added into the flask through the pipe orifice, at this time, the interior of the flask is communicated with the outside atmosphere, the air tightness of the flask is reduced, and when the rubber pipe is reinserted into the pipe orifice, the concentrated hydrochloric acid corrodes the rubber pipe, and the operation of adding hydrochloric acid into the flask is inconvenient.
Disclosure of Invention
In order to solve the defect that the existing sodium alginate content measuring device is inconvenient when hydrochloric acid is added, the utility model provides a condensation reflux device and a sodium alginate content measuring device. The condensing reflux device provided by the utility model is provided with the liquid adding opening, and concentrated hydrochloric acid is added into the flask through the liquid adding opening, so that the operation of adding the hydrochloric acid into the flask is convenient, the flask can keep good air tightness all the time, and the corrosion of the concentrated hydrochloric acid to the rubber tube filled with nitrogen is avoided.
In order to solve the technical problems, the utility model adopts the following technical scheme.
The utility model provides a condensation reflux device which is provided with a liquid adding device.
Further, the liquid adding device comprises a liquid adding port 11 from top to bottom, a liquid adding port branch pipe 13 is connected below the liquid adding port, and a switch 12 is arranged on the liquid adding port branch pipe. As shown in fig. 2.
The condensing reflux device enables the sodium alginate content measuring device to realize the channel separation of nitrogen gas feeding, reflux heating and hydrochloric acid liquid feeding, and is convenient to operate.
Further, the switch is arranged below the liquid filling opening.
Further, the switch is a piston switch.
Further, the liquid adding opening is cup-shaped.
Further, the condensing reflux device comprises a cooling jacket 101 and a reflux pipe 102, the reflux pipe is arranged in the cooling jacket, and an opening below the liquid adding port branch pipe is arranged in the reflux pipe of the condensing reflux device.
When the concentrated hydrochloric acid is added, the piston switch can be turned on, the concentrated hydrochloric acid is poured into the liquid adding port of the liquid adding device, enters the return pipe through the branch pipe of the liquid adding port, and flows into the flask along the return pipe.
The utility model also provides a sodium alginate content measuring device, which comprises a flask, the condensing reflux device, the gas washing device and the absorption device; the lower end of the condensing reflux device is communicated with the flask, the upper end of the condensing reflux device is communicated with one end of the gas washing device, and the other end of the gas washing device is communicated with the absorption device.
Further, the flask is a two-neck flask and comprises a main pipe orifice and a branch pipe orifice, the lower end of the condensation reflux device is connected with the main pipe orifice, and the branch pipe orifice is used for introducing nitrogen.
Further, the cooling jacket of the condensing reflux device comprises a liquid inlet and a liquid outlet, and the cooling medium flows into the cooling jacket through the liquid inlet and flows out from the liquid outlet.
The cooling medium is typically a cooling liquid.
Further, the gas washing device comprises a gas washing sleeve, absorbent cotton is plugged at two ends of the gas washing sleeve, the gas washing sleeve is internally provided with a getter material, the getter material is divided into two sections, and the absorbent cotton is plugged between the two sections of getter material.
Further, the getter material is zinc particles. Further, the zinc particles had a particle diameter of 3mm.
Further, the measuring device further comprises a heating device for heating the flask.
Further, the heating device is a heating jacket. Further, the heating device is a numerical control temperature heating sleeve.
Further, the absorption device comprises an absorption tower, a sand core and a triangular flask; the upper opening of the absorption tower is communicated with the atmosphere, a sand core is arranged in the absorption tower, and the lower opening of the absorption tower is connected with a triangular flask; the other end of the gas washing device is communicated with the space below the sand core in the absorption tower. The triangular flask is used for receiving NaOH absorption liquid after the reaction is finished.
The other end of the gas washing device is communicated with the space in the absorption tower.
The absorption tower can ensure the air tightness of a reaction system, is easy to observe the gas flow and improves the absorption efficiency.
The device realizes the reaction under the reflux condition by introducing nitrogen, heating the flask and adding liquid into the flask through the liquid adding port branch pipe, thereby being convenient to operate.
Compared with the prior art, the sodium alginate content measuring device provided by the utility model has the advantages that the operation of adding concentrated hydrochloric acid is convenient, the air tightness of the flask is good, and the air tightness of the whole reaction system is good. In addition, the gas flow is easy to observe, and the absorption efficiency is improved.
Drawings
FIG. 1 shows a sodium alginate content measuring device in the prior art;
fig. 2 shows a sodium alginate content measuring device provided by the utility model.
Detailed Description
For a better understanding of the present utility model, its construction, and the functional features and advantages attained by the same, reference should be made to the accompanying drawings in which:
example 1
The utility model provides a sodium alginate content measuring device. As shown in fig. 2, the measuring device includes the following structure:
a is a connection N 2 A partial pressure gauge of the steel cylinder.
B is N 2 The measuring range of the capillary flowmeter is 0-100ml/min.
D is a 250ml round bottom flask with a branch pipe, a standard grinding mouth with a straight mouth size of 29/32, C is a branch pipe mouth, a standard grinding mouth with a size of 19/26, a bent pipe plug, a bent pipe and N 2 The pipe is connected and fixed, let in N 2 And directly plugging the grinding port to the branch pipe port.
4.E is a digital display temperature control heating jacket.
F is a custom-modified straight condensate return tube, with a 50ml inlet manifold 13 of the piston 12. The upper end of the return pipe is provided with a bent pipe plug, and the size of the bent pipe plug is 29/32 of a standard grinding port.
6.G is a modified straight air-washing pipe filled with 2 sections of zinc particles, and absorbent cotton plugs are used at the interfaces of the middle and two sides H.
The device realizes the reaction under the reflux condition by introducing nitrogen, heating the flask and adding liquid into the flask through the liquid adding port branch pipe, thereby being convenient to operate.
The zinc particles have the effect of absorbing the hydrogen chloride gas carried out in the generated carbon dioxide, the particle size of the zinc particles is about 3mm which is common in the laboratory, while the zinc particles described in the United states pharmacopoeia are 20 mesh (i.e. 0.85 mm), theoretically the smaller the particle size of the zinc particles, the larger the specific surface area, and the higher the efficiency of absorbing the hydrogen chloride gas. Zinc reacts with hydrogen chloride to generate zinc chloride and hydrogen, and the hydrogen rises in the absorption tower to enter the atmosphere. The application examines the measurement results of zinc particles with the particle diameters of 3mm and 20 meshes, the absorption efficiency of zinc particles with different particle diameters is satisfactory, the measurement results of the sample content are consistent, and the zinc particles with larger particle size can meet the test requirement. In practice, attention is paid to the compactness of zinc particle filling and the air tightness of the connecting grinding plug.
7.J is an absorption tower, the upper opening is communicated with the atmosphere, and the lower opening is connected with a 250ml triangular flask L for receiving absorption liquid after the reaction is finished. The size of the upper end vent and the lower end connecting port are standard grinding openings of 29/32. After the reaction starts, N is continuously introduced into the system 2 Adding absorption liquid from the upper port, and stopping introducing N after the reaction is finished, wherein the absorption liquid is added from the upper port, and the liquid is positioned above the G2 sand core K due to positive pressure of the system, and bubbles continuously emerge (a small amount of hydrogen is absorbed by sodium hydroxide, and most of carbon dioxide gas is introduced nitrogen gas) 2 The absorption liquid flows into the receiving bottle through a glass conduit M connected below the sand core K for the subsequent titration step. The absorption tower can ensure the air tightness of a reaction system, is easy to observe the gas flow and improves the absorption efficiency of carbon dioxide.
As shown in FIG. 2, the G2 sand core K is a part of the absorption tower in a transverse direction, only one layer of separation medium is arranged, the absorption liquid is above the sand core K under the positive pressure condition of the reaction system, and when the absorption liquid is communicated with the atmosphere, the absorption liquid flows into the triangular flask L under the action of gravity through the glass conduit M connected below the sand core K
The chemical reaction involved in the determination of sodium alginate content in a sample by using the sodium alginate content determination device provided by the utility model is as follows:
in the flask, sodium alginate reacts with concentrated hydrochloric acid to generate carbon dioxide gas;
sodium alginate + concentrated hydrochloric acid- > carbon dioxide;
in the absorption device, carbon dioxide gas reacts with NaOH in absorption liquid, and the reaction formula is as follows:
CO 2 +2NaOH＝Na 2 CO 3 +H 2 O；
generated Na 2 CO 3 With BaCl 2 The reaction generates barium carbonate sediment, and the reaction formula is as follows:
BaCl 2 +Na 2 CO 3 ＝BaCO 3 ↓+2NaCl；
finally, the NaOH remaining in the absorption was titrated with HCl, with the following equation:
HCl+NaOH＝NaCl+H 2 O。
the end point of acid-base titration is that the phenolphthalein indicator is changed from pink to colorless, hydrochloric acid is sodium hydroxide remained in the neutralization reaction, the end point of the reaction is reached, if hydrochloric acid is continuously added dropwise, the reaction is carried out with barium carbonate precipitation to generate carbon dioxide, the precipitation is dissolved, and the action of adding barium chloride is to convert the generated sodium carbonate into barium carbonate precipitation so as to prevent the reaction of hydrochloric acid and sodium carbonate and influence the judgment of the end point of the titration reaction.
The calculation method for measuring the sodium alginate content in the sample by using the sodium alginate content measuring device provided by the utility model comprises the following steps:
sodium alginate content (%) = 222.00/44.01 ×2200[ (a-B) -C ]/[ (1000W) (1-D) ]
Wherein:
a: the amount of 25ml of sodium hydroxide 0.25mol/L material used, mmol;
b: the amount of material consumed 0.1mol/L hydrochloric acid, mmol;
c: titration net value (according to United states pharmacopoeia, the amount of 0.1mol/L hydrochloric acid titration solution consumed in the blank test: theoretically should be 0, since the blank test is sodium hydroxide free; small value in practical experiments), mmol;
d: a weight loss on drying value (weight loss on drying value refers to percent weight loss) of the sample or standard;
w: sample or standard sample weighing amount, unit g;
222.00: the average molecular weight of sodium alginate;
44.01: molecular weight of carbon dioxide.
2200 is obtained by: CO 2 +2NaOH＝Na 2 CO 3 +H 2 In O, 2mol of sodium hydroxide are reacted with 1mol of carbon dioxide (i.e., 44 g), i.e., 1mol of sodium hydroxide corresponds to 22g of carbon dioxide, and the conversion percentage is multiplied by 100 to obtain 2200. And then carrying out mass conversion on the carbon dioxide and the sodium alginate, and calculating the coefficient 222.00/44.01 to obtain the content of the sodium alginate.
The foregoing description is only of the preferred embodiments of the present utility model, and is not intended to limit the scope of the present utility model. All equivalent changes and modifications made in accordance with the present utility model are intended to be covered by the scope of the appended claims.
Claims (7)
1. The condensing reflux device is characterized by being provided with a liquid adding device; the liquid adding device comprises a liquid adding port from top to bottom, a liquid adding port branch pipe is connected below the liquid adding port, and a switch is arranged on the liquid adding port branch pipe; the switch is arranged below the liquid adding port, the switch is a piston switch, and the liquid adding port is cup-shaped; the condensing reflux device comprises a cooling sleeve and a reflux pipe, the reflux pipe is arranged in the cooling sleeve, and an opening below the liquid adding port branch pipe is arranged in the reflux pipe of the condensing reflux device.
2. A sodium alginate content measuring device, which is characterized by comprising a flask, the condensation reflux device, the gas washing device and the absorption device according to claim 1; the lower end of the condensing reflux device is communicated with the flask, the upper end of the condensing reflux device is communicated with one end of the gas washing device, and the other end of the gas washing device is communicated with the absorption device.
3. The sodium alginate content measuring device according to claim 2, wherein the flask is a two-necked flask including a main pipe orifice and a branch pipe orifice, the lower end of the condensation reflux device is connected with the main pipe orifice, and the branch pipe orifice is used for introducing nitrogen.
4. A sodium alginate content measuring device according to claim 3, wherein the air washing device comprises an air washing sleeve, absorbent cotton is plugged at two ends of the air washing sleeve, a getter material is filled in the air washing sleeve, the getter material is divided into two sections, and absorbent cotton is plugged between the two sections of getter material.
5. The sodium alginate content measuring device according to claim 4, wherein the getter material is zinc particles, and the particle size of the zinc particles is 3mm.
6. The sodium alginate content measuring device according to claim 4 or 5, further comprising a heating device for heating the flask.
7. The sodium alginate content measuring device according to claim 6, wherein the absorption device comprises an absorption tower, a sand core and a triangular flask; the upper opening of the absorption tower is communicated with the atmosphere, a sand core is arranged in the absorption tower, and the lower opening of the absorption tower is connected with a triangular flask; the other end of the gas washing device is communicated with the space below the sand core in the absorption tower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202222020266.5U CN219186929U (en) | 2022-08-02 | 2022-08-02 | Condensation reflux unit and sodium alginate content measuring device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202222020266.5U CN219186929U (en) | 2022-08-02 | 2022-08-02 | Condensation reflux unit and sodium alginate content measuring device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN219186929U true CN219186929U (en) | 2023-06-16 |
Family
ID=86704391
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202222020266.5U Active CN219186929U (en) | 2022-08-02 | 2022-08-02 | Condensation reflux unit and sodium alginate content measuring device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN219186929U (en) |
-
2022
- 2022-08-02 CN CN202222020266.5U patent/CN219186929U/en active Active
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102590374B (en) | Test system for hydrogen production by hydrolyzing complex metal hydride in water vapour | |
| CN103091194A (en) | Carbon dioxide content determination apparatus | |
| CN201378135Y (en) | Liquid and on-line fluid density measuring device | |
| CN219186929U (en) | Condensation reflux unit and sodium alginate content measuring device | |
| CN205861640U (en) | A kind of vehicle-mounted natural gas sulfurated hydrogen detection equipment | |
| CN205484237U (en) | Active verifying attachment of raney's nickel | |
| CN207268734U (en) | Free chlorine detection device in a kind of hydrogen chloride | |
| CN101324460B (en) | Ultra-low temperature liquid-level meter | |
| CN207379777U (en) | The sampling system of air sampler | |
| CN205642511U (en) | Be used for categorised measuring device of vapor -liquid separation and liquid flow | |
| CN213068546U (en) | Condensed water collecting and reading device for steam quality test | |
| CN104764854B (en) | Apparatus for determining content of carbon in manganese carbon alloy, and method thereof | |
| CN106053290A (en) | Nuclear power plant vapor generator washing and sediment reaction device | |
| CN111189743A (en) | Experimental device for measuring content of carbonate in soil and operation method | |
| CN211799902U (en) | Sulfuric acid mist sampling device applied to waste gas | |
| CN205786180U (en) | A kind of nuclear power station steam generator rinses sediment reaction unit | |
| CN203824599U (en) | Device for measuring escape rate of non-condensable gas through expansion elastic bag | |
| CN207351972U (en) | A kind of arsenic reaction unit | |
| CN207335944U (en) | A kind of highly practical hydrogen pressure gauge | |
| CN206618732U (en) | The device of multi element analysis sample pre-treatments in petroleum coke | |
| CN211602792U (en) | Experimental device for survey soil carbonate content | |
| CN218157751U (en) | Device for measuring carbon dioxide in soil | |
| CN204904683U (en) | Measurement device for gas production speed | |
| CN220231493U (en) | Experimental device for heating strong ammonia water to prepare ammonia gas and prevent tail gas from suck-back | |
| CN202471541U (en) | Water-to-steam ratio measuring device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant |