CN213780007U - Hydroxypropoxyl content measuring device - Google Patents
Hydroxypropoxyl content measuring device Download PDFInfo
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- CN213780007U CN213780007U CN202022913292.1U CN202022913292U CN213780007U CN 213780007 U CN213780007 U CN 213780007U CN 202022913292 U CN202022913292 U CN 202022913292U CN 213780007 U CN213780007 U CN 213780007U
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Abstract
The utility model discloses a hydroxypropoxyl content measuring device, which belongs to the technical field of detection and analysis devices and comprises a distillation flask, a distillation head, a liquid adding funnel, an air duct and a condenser, wherein the side part of the distillation head is provided with a first connecting pipe and a second connecting pipe; the first connecting pipe is connected with the lower port of the liquid feeding funnel, the second connecting pipe is connected with the upper pipe port of the condenser, and the second connecting pipe is formed by integrally connecting an upper inclined section and a lower inclined section. The utility model discloses a hydroxypropoxyl assay device, liquid level in the convenient control distillation flask is the same with the oil level in the oil bath pot, guarantees that the distillation process is stable, takes out volatile acetic acid through the nitrogen gas constancy, and the speed of evaporating of easy control distillate collects the abundant condensation of acetic acid in the distillate, and the acetic acid of avoiding generating comes too late cooling and volatilizees, and whole reaction distillation time is short, and the testing result is accurate.
Description
Technical Field
The utility model relates to a hydroxypropoxyl assay device belongs to detection and analysis instrument technical field.
Background
Hydroxypropyl cellulose, hydroxypropyl methyl cellulose and the like are common pharmaceutical excipients, for example, the hydroxypropyl methyl cellulose has excellent cold water solubility, strong sensitivity resistance, metabolic inertia and the like, can be used as a film coating material, can also be used as a binder and a disintegrating agent, and can also be used as a material for promoting dissolution, slowly releasing and controlling release of a solid preparation. The content of the hydroxypropoxyl group in the hydroxypropyl cellulose and the hydroxypropyl methyl cellulose can affect the performance of the product, for example, the content and the ratio of the hydroxypropoxyl group and the methoxyl group in the hydroxypropyl methyl cellulose can affect the water retention energy, the water solubility, the surface activity and the gel temperature of the product. Therefore, the accurate measurement of the hydroxypropoxyl content in the production process to monitor the product quality is a very important link.
At present, a pharmacopeia designation device is mainly adopted when the hydroxypropoxyl content is measured by a volumetric method, a steam generating pipe for generating steam in the pharmacopeia designation device needs to be added with water once before the reaction, and water cannot be added again in the reaction process. With the progress of the reaction, the water level in the steam generating pipe is lowered due to continuous generation of steam, the generated amount of the steam is unstable due to the difference between the water level in the steam generating pipe and the oil level in the oil bath pan, the carrying amount of the nitrogen to the detected object is unstable, and the accuracy of the detection result is affected. Moreover, the distillation flask and the reaction flask in the pharmacopeia designation device are respectively arranged separately as a unit, and can be operated after being assembled, so that not only is the whole installation and the fixation inconvenient, but also the joint of the assembled interface may influence the air tightness of the device, and the accuracy of the detection result is influenced.
The above description is included in the technical recognition scope of the inventors, and does not necessarily constitute the prior art.
SUMMERY OF THE UTILITY MODEL
The utility model discloses a solve the problem that prior art exists, provide a hydroxypropoxyl assay device, improved the gas tightness of device, the speed of evaporating of easy control distillate collects the abundant condensation of acetic acid in the distillate, and the testing result is accurate.
The utility model discloses an adopt following technical scheme to realize above-mentioned purpose:
a hydroxypropoxyl content measuring device comprises a distillation flask, a distillation head, a liquid adding funnel, an air guide pipe and a condenser, wherein the distillation head is provided with an upper connecting port and a lower connecting port;
the first connecting pipe is hermetically connected with the lower port of the liquid feeding funnel, the second connecting pipe is hermetically connected with the upper pipe port of the condenser, and the second connecting pipe is formed by integrally connecting an upper inclined section and a lower inclined section;
the condenser comprises an inner pipe and an outer pipe sleeved on the inner pipe, the upper end of the inner pipe is bent towards the upper oblique direction and connected with a second connecting pipe, and the outer pipe is provided with a water inlet and a water outlet.
Optionally, an included angle of 120-140 ° is formed between the upper inclined section and the lower inclined section of the second connecting pipe.
Optionally, the bending angle of the upper end of the inner tube towards the oblique upper side is equal to the included angle between the lower oblique section of the second connecting tube and the axis of the distillation head.
Optionally, the first connecting pipe of the distillation head is formed by integrally connecting a horizontal section and an upward-bent vertical section.
Optionally, the hydroxypropoxyl content measuring device further comprises a collecting bottle, and the inner pipe of the condenser extends into the collecting bottle.
Optionally, the liquid feeding funnel is the cylindric funnel that takes the scale, the lower port of liquid feeding funnel is provided with the piston valve.
Optionally, the hydroxypropoxyl content measuring device further comprises an oil bath pot, and the distillation bottle is placed in the oil bath pot for heating.
Optionally, the oil bath pot is a normal-pressure constant-temperature oil bath pot.
Optionally, the lower connecting port of the distillation head and the bottle mouth of the distillation flask, the gas guide tube and the upper connecting port of the distillation head, the first connecting tube of the distillation head and the lower port of the liquid adding funnel, and the second connecting tube of the distillation head and the inner tube of the condenser are hermetically connected through ground connectors.
Benefits of the present application include, but are not limited to:
the utility model provides a hydroxypropoxyl assay device integrates steam generation process and reaction process, has reduced the tie point between the instrument, has improved the gas tightness of device. The distillation flask is used for containing a hydroxypropyl cellulose sample, a chromium trioxide solution and organic-free water added in batches, the generated volatile acetic acid is conveyed by nitrogen through the condenser, and the distillate is collected into the collection flask after condensation. In the test process, after a certain amount of distillate is collected in the collecting bottle, corresponding amount of water without organic matters is added into the distilling bottle through the liquid adding funnel, the liquid level in the distilling bottle is conveniently controlled to be the same as the oil level in the oil bath pot, the stability of the distilling process is ensured, volatile acetic acid is constantly brought out through nitrogen, the distilling speed of the distillate is easily controlled, the acetic acid in the distillate is fully condensed and collected, the generated acetic acid is prevented from volatilizing due to insufficient cooling, the whole reaction distillation time is short, and the measuring result is accurate.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application. In the drawings:
fig. 1 is a schematic structural diagram of a hydroxypropoxyl content measuring device provided by the utility model;
in the figure, 1, a distillation flask; 2. a distillation head; 21. a first connecting pipe; 211. a horizontal segment; 212. a vertical section; 22. a second connecting pipe; 221. an upper inclined section; 222. a downward inclined section; 3. a liquid adding funnel; 4. an air duct; 5. a condenser; 51. an inner tube; 52. an outer tube; 521. a water inlet; 522. a water outlet; 6. a collection bottle; 7. and (6) oil bath of the pan.
Detailed Description
In order to clearly illustrate the technical features of the present invention, the present invention is explained in detail by the following embodiments in combination with the accompanying drawings.
It should be noted that in the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, the present invention may be practiced in other ways than those described herein. Accordingly, the scope of the present invention is not limited by the specific embodiments disclosed below.
As shown in figure 1, the utility model discloses a hydroxypropoxyl assay device, including retort 1, distillation head 2, liquid feeding funnel 3, air duct 4 and condenser 5. Specifically, the distillation head 2 is provided with an upper connecting port and a lower connecting port, a first connecting pipe 21 and a second connecting pipe 22 are arranged on the side branch of the distillation head 2, the lower connecting port of the distillation head 2 is hermetically connected with the bottle mouth of the distillation flask 1, the air guide pipe 4 extends into the upper connecting port of the distillation head 2 and extends to the lower part of the distillation flask 1, and the air guide pipe 4 is hermetically connected with the upper connecting port of the distillation head 2; both the first connecting pipe 21 and the second connecting pipe 22 are integrally formed with the distillation head.
The first connecting pipe 21 is hermetically connected with the lower port of the liquid feeding funnel 3, the second connecting pipe 22 is hermetically connected with the upper pipe port of the condenser 5, and the second connecting pipe 22 is formed by integrally connecting an upper inclined section 221 and a lower inclined section 222;
the condenser 5 comprises an inner pipe 51 and an outer pipe 52 sleeved on the inner pipe 51, the upper end of the inner pipe 51 is bent obliquely upwards to be connected with the second connecting pipe 22, a water inlet 521 and a water outlet 522 are arranged on the outer pipe 52, and the water inlet 521 and the water outlet 522 are used for introducing cold water to cool down the gaseous acetic acid.
Further, the hydroxypropoxyl content measuring device further comprises a collecting bottle 6, and the inner pipe 51 of the condenser 5 extends into the collecting bottle 6.
Different from traditional survey device, integrate steam generation process and reaction process in this application, retort 1 is used for holding hydroxypropyl cellulose sample and chromium trioxide solution, and hydroxyl in the hydroxypropyl cellulose is oxidized by chromic acid, at first generates ketone, then further oxidation generates volatile acetic acid, and nitrogen gas transports the volatile acetic acid that generates through condenser 5 along with vapor, and the distillate is collected in collecting bottle 6 after condenser 5 condenses. Through the arrangement, connecting points among instruments are reduced, and the air tightness of the device is improved.
In the test process, after a certain amount of distillate is collected in the collecting bottle 6, a corresponding amount of water without organic matters is added into the distillation bottle 1 through the liquid adding funnel 3, the liquid level in the distillation bottle 1 is ensured to be the same as the oil level in the oil bath pot, the generated steam is ensured to be stable, and the volatile acetic acid is constantly brought out through nitrogen.
In order to facilitate the control of the liquid reflux and the connection of the distillation head 2 to the condenser 5, ensuring the gas tightness of the apparatus, in the preferred embodiment, the angle between the upper inclined section 221 and the lower inclined section 222 of the second connection pipe 22 is 120 ° to 140 °. The upper end of the inner tube 51 is bent obliquely upward at an angle equal to the angle between the lower oblique section 222 of the second connecting tube 22 and the axis of the distillation head 2.
Further, the first connecting pipe 21 of the distillation head 2 is formed by integrally connecting a horizontal section 211 and an upward bent vertical section 212, the upper end of the vertical section is hermetically connected with the lower port of the liquid adding funnel 3, so that the distillation head 2 and the liquid adding funnel 3 are conveniently connected, the butt joint is firm and tight, and the air tightness is ensured.
Preferably, the liquid feeding funnel 3 is the cylindric funnel that takes the scale, and the lower port of liquid feeding funnel 3 is provided with the piston valve, conveniently controls the addition of no organic matter water.
The hydroxypropoxyl content measuring device also comprises an oil bath pot 7, the distillation flask 1 is placed in the oil bath pot 7 for heating, and the oil bath pot 7 is a normal-pressure constant-temperature oil bath pot.
In one embodiment, the lower connection port of the distillation head 2 and the mouth of the distillation flask 1, the gas guide tube 4 and the upper connection port of the distillation head 2, the first connection tube 21 of the distillation head 2 and the lower port of the filling funnel 3, and the second connection tube 22 of the distillation head 2 and the inner tube 51 of the condenser 5 are hermetically connected through ground joints.
The following detailed steps for testing the hydroxypropoxyl content measuring device provided by the utility model are adopted.
The reagents used were:
potassium iodide: analyzing and purifying;
sodium bicarbonate: analyzing and purifying;
phenolphthalein indicator: 1% ethanol solution;
starch indicator: 0.5% aqueous solution;
pure nitrogen gas: first-grade products;
sulfuric acid: (1+16.5) an aqueous solution;
potassium permanganate: c (1/5 KMnO)4) 0.1mol/L KMnO prepared according to GB/T601 ═ 0.02mol/L4Standard solution, then diluting to 0.02 mol/L;
no organic water: 10ml of dilute sulfuric acid (1+16.5) are added to 100ml of water and heated to boiling, and 0.1ml of 0.02mol/L KMnO is added4Boiling the standard solution for 10min, and keeping pink;
chromium trioxide: 30% aqueous solution (60 g of chromium trioxide is weighed out and dissolved in 140ml of organic-free water);
sodium hydroxide: (NaOH) 0.02mol/L, preparation of C (Na) according to GB/T6012S2O3) The solution was diluted to 0.02mol/L with distilled water when used.
The test steps are as follows:
(1) weighing about 0.05g (accurate to 0.0002g) of hydroxypropyl cellulose sample dried at 105 ℃, putting the hydroxypropyl cellulose sample into a distillation flask 1, and adding 10ml of 30% chromium trioxide solution into the distillation flask 1;
(2) immersing the distillation flask 1 into an oil bath pan, and fixing the distillation flask 1 through a fixing frame to ensure that the liquid level in the distillation flask 1 is consistent with the liquid level of the oil bath;
(3) the liquid adding funnel 3 is hermetically connected with the first connecting pipe 21, the second connecting pipe 22 is hermetically connected with the inner pipe 51 of the condenser 5, the gas guide pipe 4 is connected with the distillation head 2, and each instrument is fixed through a fixing frame;
(4) starting a power supply of the oil bath pot to heat the liquid in the distillation bottle 1, introducing nitrogen into the distillation bottle 1 through the gas guide pipe 4, controlling the speed of the nitrogen to be 1-2 bubbles/second, heating the oil bath pot to 110 ℃ at 100-;
(5) heating the oil bath kettle continuously, heating and distilling at the temperature of 148-152 ℃, oxidizing hydroxyl in the hydroxypropyl cellulose by chromic acid to generate ketone, further oxidizing to generate volatile acetic acid, conveying the generated volatile acetic acid into a collecting bottle 6 by nitrogen through a condenser 5, slowly adding 5ml of organic-free water into a distilling bottle 1 through a liquid adding funnel 3 when the volume of distillate in the collecting bottle 6 reaches 5ml, continuing distilling until the volume of distillate increases 5ml, slowly adding 5ml of organic-free water, repeating the operation until the volume of distillate reaches 55ml, stopping distilling and removing the oil bath;
(6) washing the inner wall of a condenser 5 by using distilled water, combining the washing water and the distillate, placing the mixture in a 500ml iodometric flask, adding 2 drops of 1% phenolphthalein indicator, determining the mixture to be red by using 0.02mol/L sodium hydroxide solution, boiling for 5min, cooling, then titrating by using 0.02mol/L sodium hydroxide solution to keep the reddish color unchanged for 10s, and recording the total milliliters of sodium hydroxide consumed before and after the titration;
(7) adding 0.5g of sodium bicarbonate and 10ml of dilute sulfuric acid into an iodine measuring flask, standing until no bubbles are generated, adding 1g of potassium iodide, shaking, standing in the dark for 5min, adding 3-4 drops of 0.5% starch indicator, titrating with 0.02mol/L sodium thiosulfate until the blue color disappears, recording the number of milliliters of consumed sodium thiosulfate, and carrying out a blank test by the same method.
The content of the hydroxypropoxyl is calculated according to a formula:
V1: sample testing consumes volume, ml, of standard solution of sodium hydroxide;
c1: concentration of sodium hydroxide standard solution;
k: correction coefficients for blank tests;
V2: sample testing consumes the volume of sodium thiosulfate standard solution;
m: sample mass;
0.075: a coefficient;
and (3) calculating the correction coefficient of the blank test according to a formula:
b: the blank test consumes the volume of the sodium hydroxide solution, ml;
a: the blank consumes the volume of the sodium thiosulfate solution, ml;
c: concentration of sodium hydroxide standard solution, mol/L.
In the description of the present invention, it is to be understood that the terms "center", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "axial", "radial", "circumferential", and the like, indicate orientations and positional relationships based on those shown in the drawings, and are used only for convenience of description and simplicity of description, and do not indicate or imply that the device or element so referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be construed as limiting the present invention.
In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," and "fixed" are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integrally formed; the connection can be mechanical connection, electrical connection or communication; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meaning of the above terms in the present invention can be understood according to specific situations by those skilled in the art.
The above-mentioned specific embodiments can not be regarded as the restriction to the protection scope of the present invention, to the technical personnel in this technical field, it is right that any replacement improvement or transformation that the embodiment of the present invention made all fall within the protection scope of the utility model.
The parts of the present invention not described in detail are the known techniques of those skilled in the art.
Claims (9)
1. A hydroxypropoxyl content measuring device is characterized by comprising a distillation flask, a distillation head, a liquid adding funnel, an air guide pipe and a condenser, wherein the distillation head is provided with an upper connecting port and a lower connecting port;
the first connecting pipe is hermetically connected with the lower port of the liquid feeding funnel, the second connecting pipe is hermetically connected with the upper pipe port of the condenser, and the second connecting pipe is formed by integrally connecting an upper inclined section and a lower inclined section;
the condenser comprises an inner pipe and an outer pipe sleeved on the inner pipe, the upper end of the inner pipe is bent towards the upper oblique direction and connected with a second connecting pipe, and the outer pipe is provided with a water inlet and a water outlet.
2. The hydroxypropoxyl content measuring device as defined in claim 1, wherein an included angle of 120-140 degrees is formed between the upper inclined section and the lower inclined section of the second connecting pipe.
3. The hydroxypropoxyl content measuring device as defined in claim 1, wherein the upper end of the inner tube is bent obliquely upward at an angle equal to an angle between a lower oblique section of the second connecting tube and an axis of the distillation head.
4. The hydroxypropoxyl content measuring device as defined in claim 1, wherein the first connecting pipe of the distillation head is formed by integrally connecting a horizontal section and an upwardly bent vertical section, and the upper end of the vertical section is hermetically connected to the lower port of the charging funnel.
5. The hydroxypropoxyl content measuring device according to claim 1, further comprising a collection bottle, wherein the inner pipe of the condenser extends into the collection bottle.
6. The hydroxypropoxyl content measuring device as defined in claim 1, wherein the filling funnel is a cylindrical funnel with scales, and a piston valve is provided at the lower port of the filling funnel.
7. The hydroxypropoxy group content measurement apparatus as set forth in claim 1, further comprising an oil bath, wherein the retort is heated while being placed in the oil bath.
8. The hydroxypropoxy group content measurement apparatus as set forth in claim 7, wherein the oil bath is a constant-pressure and constant-temperature oil bath.
9. The hydroxypropoxyl content measuring device as defined in claim 1, wherein the lower connecting port of the distillation head and the mouth of the distillation flask, the gas-guide tube and the upper connecting port of the distillation head, the first connecting tube of the distillation head and the lower port of the liquid-adding funnel, and the second connecting tube of the distillation head and the inner tube of the condenser are hermetically connected by ground joints.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202022913292.1U CN213780007U (en) | 2020-12-07 | 2020-12-07 | Hydroxypropoxyl content measuring device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202022913292.1U CN213780007U (en) | 2020-12-07 | 2020-12-07 | Hydroxypropoxyl content measuring device |
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| CN213780007U true CN213780007U (en) | 2021-07-23 |
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| CN202022913292.1U Active CN213780007U (en) | 2020-12-07 | 2020-12-07 | Hydroxypropoxyl content measuring device |
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