CN111380994A - Preparation method of chromatographic rod for rod-shaped thin-layer chromatography - Google Patents
Preparation method of chromatographic rod for rod-shaped thin-layer chromatography Download PDFInfo
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Abstract
The invention belongs to the field of rod-shaped thin-layer chromatography analysis equipment, and particularly relates to a preparation method of a chromatographic rod for rod-shaped thin-layer chromatography. The method comprises the following steps: (1) uniformly mixing microsphere porous silica gel, superfine glass powder, sodium polyacrylate, an organic solvent and an organic suspending agent to prepare a suspension; (2) uniformly coating the suspension on the surface of a quartz rod in a dipping and pulling mode; (3) naturally drying, and volatilizing the solvent at 80-120 ℃ to obtain a coated quartz rod; (4) heating the coated quartz rod to burn, and stopping when the temperature reaches the initial melting point of the superfine glass powder; (5) continuously introducing nitrogen, naturally cooling to room temperature, and putting the burnt quartz rod into secondary distilled water for cleaning; (6) and removing water to obtain the product. The chromatographic rod prepared by the method has high column efficiency, the surface coating is firmly attached, the chromatographic rod can be used at high temperature, the use temperature is as high as 850 ℃, the chromatographic rod can be recycled for many times, and the column efficiency is not obviously changed.
Description
Technical Field
The invention belongs to the field of rod-shaped thin-layer chromatography analysis equipment, and particularly relates to a preparation method of a chromatographic rod for rod-shaped thin-layer chromatography.
Background
The rod-shaped thin-layer chromatography is a rapid analysis device, can analyze various high-boiling-point organic matters, comprises crude oil and organic high-molecular polymers, adopts a core separation device which is a thin-layer chromatography rod, and adopts the following traditional preparation method: the silica gel is adhered to a glass rod by an adhesive, and the chromatographic rod is dried by hot air for use. The chromatographic rod prepared by the method has the advantages that silica gel and the adhesive are easy to fall off and can not be recycled for multiple times, and the adhesive is mainly modified starch and carboxymethyl cellulose, so that the chromatographic rod is carbonized and falls off after high temperature to cause permanent failure.
Chinese patent CN 201420380520.5 discloses a thin layer chromatography rod, which is prepared by mixing silica gel powder and adhesive into paste, mixing uniformly, supporting adsorbent, spraying on a glass rod by a special spraying machine, and drying by hot air. Because the glass rod is limited by the particularity of glass materials and the silica gel is coated on the surface of the glass rod by adopting a drying method, the silica gel still falls off, can be used only once and cannot be used at high temperature, and the use temperature is lower than 300 ℃.
Disclosure of Invention
The invention aims to provide a preparation method of a chromatographic rod for rod-shaped thin-layer chromatography, the chromatographic rod prepared by the method has high column efficiency and firm surface coating adhesion, can be used at high temperature, has the use temperature of up to 850 ℃, can be recycled for many times, and has no obvious change in column efficiency.
The technical scheme adopted by the invention is as follows:
the preparation method of the chromatographic rod for the rod-shaped thin-layer chromatography comprises the following steps:
(1) uniformly mixing microsphere porous silica gel, superfine glass powder, sodium polyacrylate, an organic solvent and an organic suspending agent to prepare a suspension;
(2) uniformly coating the suspension on the surface of a quartz rod in a dipping and pulling mode;
(3) naturally drying, and volatilizing the solvent at 80-120 ℃ to obtain a coated quartz rod;
(4) heating the coated quartz rod by a program, and stopping when the temperature reaches the initial melting point of the superfine glass powder;
(5) continuously introducing nitrogen or argon, naturally cooling to room temperature, and putting the burnt quartz rod into secondary distilled water for cleaning;
(6) and removing water to obtain the product.
Wherein:
the particle diameter of the microsphere porous silica gel is 3-40 mu m, and the pore diameter
Specific surface area>300m2(ii) in terms of/g. Preference is given toThe particle diameter of the microsphere porous silica gel is 4-5 mu m, d 504.5 mu m and the pore diameter
Specific surface area 450m2/g。
The particle size of the superfine glass powder is 3-40 μm, preferably 10 μm; the initial melting point is 700 ℃ and 900 ℃, preferably 870 ℃.
The relative molecular mass of the sodium polyacrylate is 200-800 ten thousand, preferably 500 ten thousand.
The organic solvent is one or more of benzene, acetone or toluene, and benzene is preferred. Water may also be used as a solvent, but the selectivity of the added suspending agent is poor.
The organic suspending agent is one or more of polymethacrylate, dibutyl phthalate or styrene, and dibutyl phthalate is preferred. The function of the suspension is to suspend the silica gel in the mixed solution for a long time.
The microsphere porous silica gel, the superfine glass powder, the sodium polyacrylate, the organic solvent and the organic suspending agent account for the following mass percent: 10-15% of microsphere porous silica gel, 30-40% of superfine glass powder, 15-20% of sodium polyacrylate, 10-35% of organic solvent and 10-15% of organic suspending agent. Preferably, the composite material comprises 15% of microsphere porous silica gel, 35% of superfine glass powder, 15% of sodium polyacrylate, 25% of an organic solvent and 10% of an organic suspending agent. The superfine glass powder also has better dispersibility in the sodium polyacrylate solution.
The temperature at which the suspension is prepared is between room temperature and 50 c, preferably a constant temperature of 35 c, which temperature influences the consistency of the suspension.
The dipping and pulling mode can adopt a finished product dipping and pulling device sold in the market and a dipping and pulling machine manufactured by self. Pulling rate range: 1-110mm/s, and 120-140mm of stroke, a coating with a thickness of 25-75 μm can be formed, and the pulling speed can be properly adjusted according to the viscosity degree of the suspension. Preferably, a dip-drawing machine is used, the drawing speed is 24mm/s, and a coating having a thickness of 33 to 37 μm can be formed.
The quartz rod is made of high-purity quartz, and the rod is a solid straight rod with the diameter of 0.3-2mm and the length of 100-150 mm. The diameter and length can be arbitrarily selected according to the actual sample analysis requirements, and preferably, the quartz rod has a diameter of 1mm and a length of 120 mm.
The quartz rod is subjected to sand blasting or frosting treatment before dipping and pulling, and an etching technology can be adopted to form a rough surface with consistent thickness on the surface of the quartz rod so as to increase the adhesiveness of the suspension, wherein the rough surface can be the whole surface of the quartz rod or a part of the surface for coating the suspension.
The natural drying is carried out, the solvent is volatilized at the temperature of 80-120 ℃, the important step of ensuring the uniform thickness of the suspension coated on the surface of the quartz rod and the important step of preparing the chromatographic rod are also carried out, the natural drying time is 1-2 hours, the preferable time is 2 hours, the temperature of the volatilized solvent is 100 ℃, and modes such as an infrared lamp, an oven and hot air convection can be adopted. The time for volatilizing the solvent is controlled to 10-30 minutes, preferably 30 minutes, and in practice, a dried surface coating layer can be obtained after volatilizing for 20 minutes.
The chromatographic rod is heated and burned by a program, any burning furnace capable of heating by a program can be adopted, such as a high-temperature resistance furnace, an atmosphere tube furnace and the like, and the maximum use temperature is 950-1200 ℃. In the temperature rise process, a small amount of residual organic solvent and organic suspending agent are gasified and flow out along with nitrogen or argon, and when the temperature reaches 300-400 ℃, sodium polyacrylate is completely decomposed, and an irregular primary porous structure is formed. The primary porous structure is an irregular loose porous structure left after the coating attached to the quartz rod is completely decomposed by the sodium polyacrylate. The primary porous structure is an important physical structure for preparing the chromatographic rod, is a functional porous structure, and can greatly improve the development speed by enabling the developing agent to climb along the primary porous structure in the development operation process.
The temperature programming ignition is as follows:
heating the mixture from room temperature to 180 ℃ at the speed of 40 ℃/min, and drying the residual organic solvent without keeping the temperature;
heating to 350 deg.C at a rate of 50 deg.C/min, maintaining for 10-20 min, and burning the suspending agent;
heating to 400-420 ℃ at the speed of 15 ℃/min, and keeping for 10-20 min to decompose the sodium polyacrylate;
heating to 800 deg.C at 50 deg.C/min, and maintaining for 5-10 min;
the temperature is raised to the initial melting point at the rate of 2 ℃/min. Wherein the initial melting point is: and observing through the window until the glass powder is softened and deformed.
The temperature reaches the initial melting point of the superfine glass powder, the temperature is an experimental temperature, a thermogravimetric analyzer (TGA) is used for analyzing the softening point temperature of the used glass powder, the softening point of the used glass powder is reduced by 1 ℃ each time by taking the temperature as a basis until the initial melting phenomenon occurs, and the temperature is defined as the initial melting point of the used glass powder. At the moment, the glass powder starts to be initially melted, the silica gel is bonded with the surface of the quartz rod by the initially melted glass powder, and a firm irregular secondary porous structure is formed, wherein the secondary porous structure is an irregular porous structure between the microsphere porous silica gel and the superfine glass powder. The secondary porous structure and the primary porous structure are important physical structures for preparing the chromatographic rod, are functional porous, and can ensure that a developing agent climbs along the primary porous structure in the developing operation process, thereby greatly improving the developing speed.
The cleaning specifically comprises the following steps: the salt attached to the surface of the chromatographic rod is washed for many times, and is sodium carbonate generated after sodium polyacrylate added in the process of preparing the chromatographic rod is decomposed, and water-soluble salt decomposed by other impurities. Deionized water can be used for repeated soaking and washing, and the removal of salt can be accelerated by properly increasing the soaking and washing temperature.
The water removal refers to the water attached to the chromatographic rod when the salt attached to the surface of the chromatographic rod is washed, and the microsphere porous silica gel is saturated in water adsorption, so that the silica gel loses activity and does not have a separation function, so that the water adsorbed by the microsphere porous silica gel needs to be desorbed, and the microsphere porous silica gel is recovered in activity after the water is desorbed by heating. In fact, this method can also be used for the activation of long shelf life chromatographic bars.
Compared with the prior art, the invention has the following beneficial effects:
the chromatographic rod prepared by the method has high column efficiency, firm surface coating adhesion, can be used at high temperature, has the use temperature of 850 ℃, can be recycled for multiple times, can be repeatedly used for 100 times, and has no obvious change in column efficiency.
Drawings
FIG. 1 is a schematic diagram of the structure of a chromatography rod of the present invention;
FIG. 2 is a schematic view of dip-pull;
FIG. 3 is an SEM photograph of a chromatography rod of the present invention;
FIG. 4 is a separation spectrum of example 1 of the present invention;
FIG. 5 is a separation spectrum of example 2 of the present invention;
FIG. 6 is a separation spectrum of comparative example 1 of the present invention;
FIG. 7 is a 10-time spectrum of the reuse of example 3 of the present invention;
FIG. 8 is a 20-time spectrum of the reuse of example 3 of the present invention;
FIG. 9 is a graph of 50 reuses of example 3 of the present invention;
FIG. 10 is a 100-time spectrum of the reuse of example 3 of the present invention;
FIG. 11 is a graph of the 110 reuse pattern of example 3 of the present invention;
FIG. 12 is an SEM photograph of example 4 of the present invention;
FIG. 13 is an SEM photograph of example 5 of the present invention;
FIG. 14 is an SEM photograph of example 6 of the present invention.
Detailed Description
The present invention will be further described with reference to the following detailed description, but is not limited thereto.
Example 1
The structure of the chromatographic rod for rod-shaped thin layer chromatography is shown in FIG. 1.
The chromatographic rod is prepared from the following raw materials in parts by mass: 15% of microsphere porous silica gel, 35% of superfine glass powder, 15% of sodium polyacrylate, 25% of organic solvent and 10% of organic suspending agent.
Wherein the content of the first and second substances,
the particle size of the microsphere porous silica gel is 4-5 μm, d 504.5 μm, and the pore diameter
Specific surface area 450m2/g。
The grain diameter of the superfine glass powder is 10 mu m; the initial melting point is 850 ℃.
The molecular weight of the sodium polyacrylate is 800 ten thousand.
The organic solvent is benzene.
The organic suspending agent is dibutyl phthalate.
The preparation method comprises the following steps:
(1) preparing microsphere porous silica gel, superfine glass powder, sodium polyacrylate, an organic solvent and an organic suspending agent into a uniform suspension at a constant temperature of 35 ℃;
(2) uniformly coating the suspension on the surface of a quartz rod by adopting a dip-coating mode, wherein the dip-coating mode is schematically shown in figure 2, the coating thickness is 33-37 mu m, and the coating speed is 24 mm/s; wherein the quartz rod is made of high-purity quartz, the diameter is 1mm, the length is 120mm, and sand blasting treatment is carried out before dipping and pulling so as to lead the surface of the quartz rod to present a rough surface with consistent thickness;
(3) naturally airing for 2 hours, and volatilizing the solvent at 100 ℃ for 30 minutes to obtain a coated quartz rod;
(4) putting the coated quartz rod into a corundum bracket, putting the corundum bracket into an inert atmosphere tube furnace, and carrying out high-temperature firing on the chromatographic rod by adopting temperature programming, wherein the temperature programming system is as follows: raising the temperature from room temperature to 180 ℃ at the speed of 40 ℃/min without maintaining; heating to 350 deg.C at a speed of 50 deg.C/min, and maintaining for 10 min; heating to 400 ℃ at the speed of 15 ℃/min, and keeping for 20 min; heating to 800 deg.C at 50 deg.C/min, and holding for 5 min; the temperature was raised to 850 ℃ at 2 ℃ per minute. Observing through a window until the glass powder is softened and deformed; the heating was stopped.
In the temperature rise process, a small amount of residual organic solvent and organic suspending agent are gasified and flow out along with nitrogen, and when the temperature reaches 300-400 ℃, the sodium polyacrylate is completely decomposed, and an irregular primary porous structure is formed. And continuously heating, and when the temperature reaches the initial melting point of the superfine glass powder, initially melting the glass powder, and bonding the silica gel with the surface of the quartz rod to form a firm irregular secondary porous structure.
(5) And continuously introducing nitrogen, naturally cooling to room temperature, putting the burnt quartz rod into secondary distilled water, and cleaning impurities such as salt and the like attached to the surface of the quartz rod for many times.
(6) The washed chromatographic bar was dehydrated at 100 ℃. At the moment, the glass powder is firmly bonded with the surface of the quartz rod, and meanwhile, a porous structure is formed between the partially melted glass powder and the microsphere porous silica gel, so that the microsphere porous silica gel is reliably and firmly bonded to the surface of the quartz rod.
The SEM photograph of the prepared chromatographic rod is shown in FIG. 3.
The chromatographic rod is adopted for testing, and the test samples are as follows: 0.53% n-hexadecane, 0.51% fluorene, 0.49% cetyl ether solution, scanning speed: 1.14 mm/s.
The test finds that: the separation effect of the hexadecanol, the fluorene and the hexadecane is good, the separation degree reaches 1.5, and a separation spectrogram is shown in an attached figure 4.
Example 2
The chromatographic rod is prepared from the following raw materials in parts by mass: 10% of microsphere porous silica gel, 40% of superfine glass powder, 15% of sodium polyacrylate, 25% of organic solvent and 10% of organic suspending agent.
Wherein the content of the first and second substances,
the particle size of the microsphere porous silica gel is 4-5 μm, d 504.5 μm, and the pore diameter
Specific surface area 450m2/g。
The grain diameter of the superfine glass powder is 10 mu m; the initial melting point was 870 ℃.
The molecular weight of the sodium polyacrylate is 500 ten thousand.
The organic solvent is benzene.
The organic suspending agent is dibutyl phthalate.
The preparation method comprises the following steps:
(1) preparing microsphere porous silica gel, superfine glass powder, sodium polyacrylate, an organic solvent and an organic suspending agent into a uniform suspension at a constant temperature of 35 ℃;
(2) uniformly coating the suspension on the surface of a quartz rod by adopting a dip-coating mode, wherein the coating thickness is 28-36 mu m, and the coating speed is 24 mm/s; wherein the quartz rod is made of high-purity quartz, the diameter is 1mm, the length is 120mm, and sand blasting treatment is carried out before dipping and pulling so as to lead the surface of the quartz rod to present a rough surface with consistent thickness;
(3) naturally airing for 2 hours, and volatilizing the solvent at 100 ℃ for 30 minutes to obtain a coated quartz rod;
(4) putting the coated quartz rod into a corundum bracket, putting the corundum bracket into an inert atmosphere tube furnace, and carrying out high-temperature firing on the chromatographic rod by adopting temperature programming, wherein the temperature programming system is as follows: raising the temperature from room temperature to 180 ℃ at the speed of 40 ℃/min without maintaining; heating to 350 deg.C at a speed of 50 deg.C/min, and maintaining for 20 min; heating to 420 ℃ at the speed of 15 ℃/min, and keeping for 10 min; heating to 800 deg.C at 50 deg.C/min, and holding for 10 min; the temperature was raised to 870 ℃ at 2 ℃ per minute. Observing through a window until the glass powder is softened and deformed; the heating was stopped. In the temperature rise process, a small amount of residual organic solvent and organic suspending agent are gasified and flow out along with nitrogen, and when the temperature reaches 300-400 ℃, the sodium polyacrylate is completely decomposed, and an irregular primary porous structure is formed. And continuously heating, and when the temperature reaches the initial melting point of the superfine glass powder, initially melting the glass powder, and bonding the silica gel with the surface of the quartz rod to form a firm irregular secondary porous structure.
(5) And continuously introducing nitrogen, naturally cooling to room temperature, putting the burnt quartz rod into secondary distilled water, and cleaning impurities such as salt and the like attached to the surface of the quartz rod for many times.
(6) The washed chromatographic bar was dehydrated at 100 ℃. At the moment, the glass powder is firmly bonded with the surface of the quartz rod, and meanwhile, a porous structure is formed between the partially melted glass powder and the microsphere porous silica gel, so that the microsphere porous silica gel is reliably and firmly bonded to the surface of the quartz rod.
The chromatographic rod is adopted for testing, and the test samples are as follows: 0.51% n-hexadecane, 0.52% fluorene, 0.56% cetyl ether solution, scanning speed: 1.14 mm/s.
Tests show that the separation effect of hexadecanol and fluorene is poor, but the hexadecanol and fluorene can still be separated into independent peaks to achieve the separation purpose, and the separation spectrum is shown in figure 5, which shows that 10% of silica gel is also feasible.
Comparative example 1
The chromatographic rod is prepared from the following raw materials in parts by mass: 9% of microsphere porous silica gel, 41% of superfine glass powder, 15% of sodium polyacrylate, 25% of organic solvent and 10% of organic suspending agent.
Wherein the content of the first and second substances,
the particle size of the microsphere porous silica gel is 4-5 μm, d 504.5 μm, and the pore diameter
Specific surface area 450m2/g。
The grain diameter of the superfine glass powder is 10 mu m; the initial melting point was 870 ℃.
The molecular weight of the sodium polyacrylate is 500 ten thousand.
The organic solvent is benzene.
The organic suspending agent is dibutyl phthalate.
The preparation method comprises the following steps:
(1) preparing microsphere porous silica gel, superfine glass powder, sodium polyacrylate, an organic solvent and an organic suspending agent into a uniform suspension at a constant temperature of 35 ℃;
(2) uniformly coating the suspension on the surface of a quartz rod by adopting a dip-coating mode, wherein the dip-coating mode is shown in figure 2, the coating thickness is 28-36 mu m, and the coating speed is 24 mm/s; wherein the quartz rod is made of high-purity quartz, the diameter is 1mm, the length is 120mm, and sand blasting treatment is carried out before dipping and pulling so as to lead the surface of the quartz rod to present a rough surface with consistent thickness;
(3) naturally airing for 2 hours, and volatilizing the solvent at 100 ℃ for 30 minutes to obtain a coated quartz rod;
(4) putting the coated quartz rod into a corundum bracket, putting the corundum bracket into an inert atmosphere tube furnace, and carrying out high-temperature firing on the chromatographic rod by adopting temperature programming, wherein the temperature programming system is as follows: raising the temperature from room temperature to 180 ℃ at the speed of 40 ℃/min without maintaining; heating to 350 deg.C at a speed of 50 deg.C/min, and maintaining for 20 min; heating to 420 ℃ at the speed of 15 ℃/min, and keeping for 10 min; heating to 800 deg.C at 50 deg.C/min, and holding for 10 min; the temperature was raised to 870 ℃ at 2 ℃ per minute. Observing through a window until the glass powder is softened and deformed; the heating was stopped.
In the temperature rise process, a small amount of residual organic solvent and organic suspending agent are gasified and flow out along with nitrogen, and when the temperature reaches 300-400 ℃, the sodium polyacrylate is completely decomposed, and an irregular primary porous structure is formed. And continuously heating, and when the temperature reaches the initial melting point of the superfine glass powder, initially melting the glass powder, and bonding the silica gel with the surface of the quartz rod to form a firm irregular secondary porous structure.
(5) And (3) continuously introducing nitrogen, naturally cooling to room temperature, putting the burnt quartz rod into secondary distilled water, and cleaning impurities such as salt and the like attached to the surface of the quartz rod for multiple times.
(6) The washed chromatographic bar was dehydrated at 100 ℃. At the moment, the glass powder is firmly bonded with the surface of the quartz rod, and meanwhile, a porous structure is formed between the partially melted glass powder and the microsphere porous silica gel, so that the microsphere porous silica gel is reliably and firmly bonded to the surface of the quartz rod.
The chromatographic rod is adopted for testing, and the test samples are as follows: 0.51% n-hexadecane, 0.52% fluorene, 0.56% cetyl ether solution, scanning speed: 1.14 mm/s.
Tests show that the hexadecanol, the fluorene and the n-hexadecane can not be separated and can not achieve the separation purpose, and a separation spectrogram is shown in an attached figure 6. Silica gel in a proportion of 10% or less is unusable. In fact, during the deployment process, a significant reduction in deployment speed was also observed. Associated with a reduction in secondary porosity.
Example 3
The chromatographic rod prepared in example 1 was subjected to a repeated use test for a plurality of times, and the test samples were: 0.53% n-hexadecane, 0.51% fluorene, 0.49% cetyl ether solution, scanning speed: 1.14 mm/s.
The pattern was repeated 10 times as shown in FIG. 7, and the appearance of the bar was visually unchanged.
The spectrogram is shown in figure 8 after repeated use for 20 times, the separation degree is unchanged, the visual appearance of a chromatographic bar is unchanged,
the chromatogram obtained after repeated use for 50 times is shown in FIG. 9, the separation degree is unchanged, and the visual appearance of the chromatographic bar is unchanged.
The chromatogram is shown in figure 10 after repeated use for 100 times, the separation degree is reduced compared with the separation degree in the first use, the separation degree still can reach 1.5, and the visual appearance of the chromatographic bar is yellowish brown. The coating is complete and has no coating falling off.
The chromatogram is shown in figure 11 after repeated use for 110 times, the separation degree is poor, the retention time of hexadecanol is advanced, fluorene and hexadecane cannot be separated, and the visual appearance of a chromatographic bar is dark yellow brown. The coating parts at the two ends fall off, the unfolding speed is lower than that of the first use, and the continuous use cannot be realized.
In fact, the column efficiency of the chromatographic rod gradually decreases with the increase of the number of uses. The reduction of column effect is mainly influenced by the shedding degree of the surface coating and the pollution condition. Through spectrogram observation, when the column effect is repeatedly used for less than 100 times, the separation requirement can be met. The column effect is mutated after more than 110 times, so that the separation cannot be realized. Even by solvent washing, or secondary burning, the chromatographic rod cannot be activated.
Example 4
15% of microsphere porous silica gel, 35% of superfine glass powder, 15% of sodium polyacrylate, 25% of organic solvent and 10% of organic suspending agent. The rods of example 1 were prepared under other conditions at a pull rate of 1mm/s, with a SEM scan coating thickness of 45-71 μm and a coating thickness variation of < 26 μm. The separation requirements were met by testing as in example 3. SEM is shown in figure 12.
Example 5
15% of microsphere porous silica gel, 35% of superfine glass powder, 15% of sodium polyacrylate, 25% of organic solvent and 10% of organic suspending agent. The rods of example 1 were prepared under other conditions at a pull rate of 110mm/s, and the coating thickness was 28 to 37 μm by SEM scanning. The difference in coating thickness was < 10 μm. The separation requirements were met by testing as in example 3. SEM is shown in figure 13.
Example 6
15% of microsphere porous silica gel, 35% of superfine glass powder, 15% of sodium polyacrylate, 25% of organic solvent and 10% of organic suspending agent. The rods were produced as in example 1 at a pull rate of 24mm/s, with a coating thickness of 33-37 μm by SEM scanning and a coating thickness difference of < 4 μm. The separation requirements were met by testing as in example 3. SEM is shown in FIG. 14.
Claims (10)
1. A method for preparing a chromatographic rod for rod-shaped thin-layer chromatography is characterized by comprising the following steps: the method comprises the following steps:
(1) uniformly mixing microsphere porous silica gel, superfine glass powder, sodium polyacrylate, an organic solvent and an organic suspending agent to prepare a suspension;
(2) uniformly coating the suspension on the surface of a quartz rod in a dipping and pulling mode;
(3) naturally drying, and volatilizing the solvent at 80-120 ℃ to obtain a coated quartz rod;
(4) heating the coated quartz rod by a program, and stopping when the temperature reaches the initial melting point of the superfine glass powder;
(5) continuously introducing nitrogen, naturally cooling to room temperature, and putting the burnt quartz rod into secondary distilled water for cleaning;
(6) and removing water to obtain the product.
2. The method for producing a chromatography rod for rod-like thin layer chromatography according to claim 1, characterized in that: the particle diameter of the microsphere porous silica gel is 3-40 mu m, and the pore diameter
Specific surface area>300m2/g。
3. The method for producing a chromatography rod for rod-like thin layer chromatography according to claim 1, characterized in that: the particle size of the superfine glass powder is 3-40 mu m, and the initial melting point is 700-900 ℃.
4. The method for producing a chromatography rod for rod-like thin layer chromatography according to claim 1, characterized in that: the relative molecular mass of the sodium polyacrylate is 200-800 ten thousand.
5. The method for producing a chromatography rod for rod-like thin layer chromatography according to claim 1, characterized in that: the organic solvent is one or more of benzene, acetone or toluene, and the organic suspending agent is one or more of polymethacrylate, dibutyl phthalate or styrene.
6. The method for producing a chromatography rod for rod-like thin layer chromatography according to claim 1, characterized in that: the microsphere porous silica gel, the superfine glass powder, the sodium polyacrylate, the organic solvent and the organic suspending agent account for the following mass percent: 10-15% of microsphere porous silica gel, 30-40% of superfine glass powder, 15-20% of sodium polyacrylate, 10-35% of organic solvent and 10-15% of organic suspending agent.
7. The method for producing a chromatography rod for rod-like thin layer chromatography according to claim 1, characterized in that: the temperature at which the suspension is prepared is from room temperature to 50 ℃.
8. The method for producing a chromatography rod for rod-like thin layer chromatography according to claim 1, characterized in that: the dipping and pulling speed is 1-110mm/s, the stroke is 120-140mm, and the thickness of the suspension coated on the surface of the quartz rod is 25-75 mu m.
9. The method for producing a chromatography rod for rod-like thin layer chromatography according to claim 1, characterized in that: the quartz rod is a solid straight rod with the diameter of 0.3-2mm and the length of 100-150mm, and is treated by sand blasting, sanding or etching technology before dipping and pulling.
10. The method for producing a chromatography rod for rod-like thin layer chromatography according to claim 1, characterized in that: the temperature programming ignition is as follows:
raising the temperature from room temperature to 180 ℃ at the speed of 40 ℃/min without maintaining;
heating to 350 deg.C at a rate of 50 deg.C/min, and maintaining for 10-20 min;
raising the temperature to 400-420 ℃ at the speed of 15 ℃/min, and keeping the temperature for 10-20 min;
heating to 800 deg.C at 50 deg.C/min, and maintaining for 5-10 min;
the temperature is raised to the initial melting point at the rate of 2 ℃/min.
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Citations (5)
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| GB1343976A (en) * | 1970-03-14 | 1974-01-16 | Shionogi & Co | Chromatographic plates |
| US3839205A (en) * | 1971-09-08 | 1974-10-01 | Shionogi & Co | Chromatographic element and method for producing the same |
| CN102557714A (en) * | 2012-01-09 | 2012-07-11 | 江南大学 | Hole channel amplification method of porous ceramic microballoon sphere |
| CN106994361A (en) * | 2017-06-02 | 2017-08-01 | 钦州学院 | A kind of alumina support and preparation method with macroporous structure |
| CN107913742A (en) * | 2016-10-10 | 2018-04-17 | 中国石油天然气股份有限公司 | A kind of alumina support containing macropore and preparation method thereof |
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2020
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Patent Citations (5)
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| GB1343976A (en) * | 1970-03-14 | 1974-01-16 | Shionogi & Co | Chromatographic plates |
| US3839205A (en) * | 1971-09-08 | 1974-10-01 | Shionogi & Co | Chromatographic element and method for producing the same |
| CN102557714A (en) * | 2012-01-09 | 2012-07-11 | 江南大学 | Hole channel amplification method of porous ceramic microballoon sphere |
| CN107913742A (en) * | 2016-10-10 | 2018-04-17 | 中国石油天然气股份有限公司 | A kind of alumina support containing macropore and preparation method thereof |
| CN106994361A (en) * | 2017-06-02 | 2017-08-01 | 钦州学院 | A kind of alumina support and preparation method with macroporous structure |
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| 吴凤锷: "色谱棒制备技术的研究", 《兰州大学学报(自然科学版)》 * |
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| CN111380994B (en) | 2023-02-28 |
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