CN211478183U - Thin-layer chromatography stick and adsorbent smearing device thereof - Google Patents

Thin-layer chromatography stick and adsorbent smearing device thereof Download PDF

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CN211478183U
CN211478183U CN201921857528.5U CN201921857528U CN211478183U CN 211478183 U CN211478183 U CN 211478183U CN 201921857528 U CN201921857528 U CN 201921857528U CN 211478183 U CN211478183 U CN 211478183U
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rectangular
layer chromatography
adsorbent
thin
stick
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孙建军
龚争辉
刘强民
李洁
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China Petroleum and Chemical Corp
Technology Inspection Center of Sinopec Shengli Oilfield Co
Shengli Oilfield Testing and Evaluation Research Co Ltd
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China Petroleum and Chemical Corp
Technology Inspection Center of Sinopec Shengli Oilfield Co
Shengli Oilfield Testing and Evaluation Research Co Ltd
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Abstract

The utility model provides a thin-layer chromatography stick belongs to the thin-layer chromatography field. The technical scheme is as follows: the thin-layer chromatography rod is characterized by comprising a 150mm long pipe body with the inner diameter of 0.53mm and the outer diameter of 0.69mm, and an adsorbent coating is arranged on the outer wall of the pipe body. The utility model has the advantages that: the thin-layer chromatography rod has the advantages of simple structure, light weight, material conservation and convenience in drying after the adsorbent is coated.

Description

Thin-layer chromatography stick and adsorbent smearing device thereof
Technical Field
The utility model relates to a chemistry field especially relates to a thin-layer chromatography stick and device is paintd to adsorbent thereof.
Background
Chromatography is the most effective method for analyzing and separating complex mixtures mastered by human beings so far. Thin-layer chromatography is the only effective method for quantitative analysis of group compositions of heavy oils and macromolecules. The rod-shaped thin layer chromatography is characterized in that a conventional plate thin layer is changed into a rod thin layer, namely, a monomer is coated on the surface of a cylinder according to a certain thickness to form a thin layer rod as a component separation tool, and the thin layer rod is combined with a hydrogen flame ionization detection technology commonly used in gas chromatography to realize automatic testing of a plurality of samples. At present, the method is mainly used in the aspects of petrochemical industry, petroleum geology, coal chemistry, fine chemical industry, medicine and health, environmental chemistry and the like.
At present, the chromatographic rod is made by self and is a commodity prefabricated rod. The commodity prefabricated rod is imported generally, the price is expensive, and the pertinence is poor. Self-control chromatographic rod generally adopts solid cylinder, and weight is heavier to drying rate is slower after carrying out the coating, influences the degree of consistency of coating like this, leads to the fact the error to later stage detection.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide a thin-layer chromatography stick and adsorbent of drying carry out after simple structure, light in weight, save the material, conveniently paint the adsorbent paint device.
The utility model discloses a realize through following technical scheme: the thin-layer chromatography rod is characterized by comprising a 150mm long pipe body with the inner diameter of 0.53mm and the outer diameter of 0.69mm, and an adsorbent coating is arranged on the outer wall of the pipe body.
The tube body is a quartz tube.
The thickness of the adsorbent coating is 0.05mm, and the length of the coating is 130 mm.
The sorbent coating may be operated according to the following steps:
(1) pouring the screened silica gel or alumina and the inorganic adhesive into a closed stirrer according to the proportion of 1:2.5, adding a certain amount of solvent, and uniformly stirring the mixture to form paste for later use;
(2) cleaning the quartz tube and drying the quartz tube at 120 ℃ for 30 min;
(3) pouring the prepared uniform slurry into a container gradually, starting ultrasonic waves for 10min, and discharging mixed gas;
(4) putting the cleaned quartz tube into a container, soaking for 5min, and taking out; the container may employ an adsorbent application device as described below.
(5) And introducing hot air flow into the quartz tube for 30min, and drying the solvent.
The inorganic adhesive is glass powder with the particle size of 5 mu m and the temperature of 900-1300 ℃, the solvent is acetone, and the acetone is 2 times of the total mass of the silica gel or the alumina and the inorganic adhesive. The silica gel can be 5 micron silica gel of German Merck, the surface of the prepared rod is porous and smooth, and the oil, wax and polar substances in the crude oil can be completely separated and the separation speed is high when the sample is actually separated.
The utility model provides a device is paintd to adsorbent for thin-layer chromatography stick includes the open rectangle box in sealed top in bottom, be provided with the adsorbent in the rectangle box, it has the supporting seat to peg graft above the rectangle box, open and the equipartition has a plurality of chromatography stick socket hole on the supporting seat, it has the bottom to open to peg graft above the supporting seat, the lid of upper portion seal, the intermediate position of lid is opened to have the connecting hole, the connecting hole passes through the pipeline and connects the heat source.
The support seat comprises a rectangular block, the chromatographic rod insertion hole is formed in the rectangular block, a rectangular frame I is externally connected to the upper portion of the rectangular block, a rectangular annular slot is formed in the rectangular frame I, the rectangular block is inserted in the rectangular box body, and the cover is inserted in the rectangular annular slot.
And a second rectangular frame matched with the rectangular block is externally connected to one side of the upper part of the rectangular box body.
The upper end face of the second rectangular frame is higher than the upper end face of the rectangular block.
The rectangular block is internally provided with a cavity.
Will the body is pegged graft in the chromatogram stick spliced eye, make the upper end of body be a little higher than with the rectangle piece, will the rectangle piece with the body all inserts in the rectangle box, after waiting for a certain time, take out the rectangle piece, will the rectangle piece is pegged graft on the rectangle frame two, and will the lid is pegged graft in the rectangle ring slot, then will the connecting hole is connected with the heat source, the heat source can be steam also can be the hot gas flow that 110 ℃ nitrogen source produced, and steam is through getting into inside the whole device, finally gets into the tubulose chromatogram stick, carries out rapid draing through the heat conductivity of tubulose chromatogram stick inner wall.
And a protective cover can be arranged outside the second rectangular frame for ensuring safety.
The utility model has the advantages that: the thin-layer chromatography rod has the advantages of simple structure, light weight, material conservation and convenience in drying after the adsorbent is coated.
Drawings
FIG. 1 is a schematic diagram of the structure of a chromatography rod.
Fig. 2 is a schematic view of the overall structure of the adsorbent applying apparatus.
Fig. 3 is a schematic structural diagram of a rectangular box body.
Fig. 4 is a schematic structural view of the support base.
Fig. 5 is a schematic view of the structure of the cover.
Wherein the reference numerals are: 1. a pipe body; 2. an adsorbent coating; 3. a rectangular box body; 4. a supporting seat; 5. a cover; 301. a second rectangular frame; 401. a rectangular block; 402. a first rectangular frame; 403. a chromatography rod jack; 404. a rectangular annular slot; 501. and connecting the holes.
Detailed Description
In order to clearly illustrate the technical features of the present solution, the present solution is explained below by way of specific embodiments.
The first embodiment is as follows:
referring to fig. 1, the utility model relates to a thin-layer chromatography stick, the internal diameter of chromatography stick is 0.53mm, and the external diameter is 0.69mm, is 150 mm's body 1 for long, is provided with adsorbent coating 2 on the outer wall of body 1.
The tube body 1 is a quartz tube.
The thickness of the adsorbent coating 2 was 0.05mm and the coating length was 130 mm.
Example two:
referring to fig. 1, the utility model relates to a thin-layer chromatography stick, the internal diameter of chromatography stick is 0.53mm, and the external diameter is 0.69mm, is 150 mm's body 1 for long, is provided with adsorbent coating 2 on the outer wall of body 1.
The tube body 1 is a quartz tube.
The thickness of the adsorbent coating 2 was 0.05mm and the coating length was 130 mm.
The sorbent coating 2 may be operated according to the following steps:
(1) pouring the screened silica gel or alumina and the inorganic adhesive into a closed stirrer according to the proportion of 1:2.5, adding a certain amount of solvent, and uniformly stirring the mixture to form paste for later use;
(2) cleaning the quartz tube and drying the quartz tube at 120 ℃ for 30 min;
(3) pouring the prepared uniform slurry into a container gradually, starting ultrasonic waves for 10min, and discharging mixed gas;
(4) putting the cleaned quartz tube into a container, soaking for 5min, and taking out; the container may employ an adsorbent application device as described below.
(5) And introducing hot air flow into the quartz tube for 30min, and drying the solvent.
The inorganic adhesive is glass powder with the particle size of 5 mu m and the temperature of 900-1300 ℃, the solvent is acetone, and the acetone is 2 times of the total mass of the silica gel or the alumina and the inorganic adhesive. The silica gel can be 5 micron silica gel of German Merck, the surface of the prepared rod is porous and smooth, and the oil, wax and polar substances in the crude oil can be completely separated and the separation speed is high when the sample is actually separated.
The utility model provides a device is paintd to adsorbent for thin-layer chromatography stick includes the open rectangle box 3 in bottom seal top, is provided with the adsorbent in the rectangle box 3, and it has supporting seat 4 to peg graft in 3 tops of rectangle box, opens on supporting seat 4 and the equipartition has a plurality of chromatography stick socket 403, and it has the bottom to open to peg graft in 4 tops of supporting seat, and upper portion is sealed covers 5, and the intermediate position of lid 5 opens to have connecting hole 501, and connecting hole 501 passes through the pipe connection heat source.
The supporting seat 4 comprises a rectangular block 401, the chromatographic rod insertion holes 403 are formed in the rectangular block 401, a rectangular frame 402 is externally connected to the upper portion of the rectangular block 401, a rectangular annular insertion groove 403 is formed in the rectangular frame 402, the rectangular block 401 is inserted into the rectangular box body 4, and the cover 5 is inserted into the rectangular annular insertion groove 403.
One side of the upper part of the rectangular box body 3 is externally connected with a rectangular frame II 301 matched with the rectangular block 401.
The upper end face of the second rectangular frame 301 is higher than the upper end face of the rectangular block 401.
A cavity is provided inside the rectangular block 401.
The tube body 1 is inserted into the chromatographic rod insertion hole 403, the upper end of the tube body 1 is slightly higher than the rectangular block 401, the rectangular block 401 and the tube body are inserted into the rectangular box body 3, after a certain time, the rectangular block 401 is taken out, the rectangular block 401 is inserted into the rectangular frame II 301, the cover 5 is inserted into the rectangular annular insertion groove 404, the connection hole 501 is connected with a heat source, the heat source can be steam or hot air generated by a 110 ℃ nitrogen source, the steam enters the whole device and finally enters the tube body, and rapid drying is performed through the heat conductivity of the inner wall of the tube body.
A protective cover can be arranged outside the second rectangular frame 301 for ensuring safety.
Example three:
in order to better illustrate the stability of the test method, the following examples are provided:
1. precision experiment of same sample by same operator
Taking 1 part of crude oil sample, preparing the test solution according to the test solution preparation method, adopting the chromatographic condition, carrying out continuous sample introduction for 5 times, wherein the relative retention time and the relative peak area RSD of 4 chromatographic peaks are respectively in the ranges of 0-0.5% and 0-0.4%, and the table 1 shows that the method has good precision.
TABLE 1 precision test
Figure DEST_PATH_GDA0002571119940000051
2. Reproducibility of different operators on the same sample
Taking 1 part of crude oil sample of the same batch number, preparing a test solution according to a test solution preparation method, and respectively measuring by different operators, wherein the relative retention time of 4 chromatographic peaks and the relative deviation of the relative peak area are both 0-2%. Table 2 shows that the method has good reproducibility and meets the measurement requirements.
TABLE 2 reproducibility test
Figure DEST_PATH_GDA0002571119940000052
The technical features that the utility model has not been described can be realized through or adopt prior art, and no longer give unnecessary details here, and of course, the above-mentioned explanation is not right the utility model discloses a restriction, the utility model discloses also not only be limited to the above-mentioned example, ordinary skilled person in this technical field is in the utility model discloses a change, modification, interpolation or replacement made in the essential scope also should belong to the utility model discloses a protection scope.

Claims (8)

1. The thin-layer chromatography rod is characterized by comprising a 150mm long pipe body with the inner diameter of 0.53mm and the outer diameter of 0.69mm, and an adsorbent coating is arranged on the outer wall of the pipe body.
2. The thin layer chromatography rod of claim 1, wherein the tube body is a quartz tube.
3. The thin layer chromatography rod of claim 1, wherein the adsorbent coating thickness is 0.05mm and the coating length is 130 mm.
4. An adsorbent coating device based on the thin layer chromatography stick of claim 1, which comprises a rectangular box body with a bottom seal and an open top, wherein an adsorbent is arranged in the rectangular box body, a supporting seat is inserted above the rectangular box body, a plurality of chromatographic stick insertion holes are formed in the supporting seat in an inserting manner and are uniformly distributed, a cover with an open bottom and a sealed upper portion is inserted above the supporting seat, a connecting hole is formed in the middle of the cover in an inserting manner, and the connecting hole is connected with a heat source through a pipeline.
5. The adsorbent coating device for the thin-layer chromatography stick as claimed in claim 4, wherein the supporting seat comprises a rectangular block, the chromatography stick insertion hole is arranged on the rectangular block, a rectangular frame I is externally connected to the upper portion of the rectangular block, a rectangular annular slot is arranged on the rectangular frame I, the rectangular block is inserted into the rectangular box body, and the cover is inserted into the rectangular annular slot.
6. The adsorbent coating device of the thin layer chromatography stick as claimed in claim 5, wherein a second rectangular frame matched with the rectangular block is externally connected to one side of the upper part of the rectangular box body.
7. The adsorbent application device of the thin layer chromatography stick of claim 6, wherein the upper end face of the second rectangular frame is higher than the upper end face of the rectangular block.
8. The adsorbent application device of the thin layer chromatography stick of claim 7, wherein the rectangular block is provided with a cavity inside.
CN201921857528.5U 2019-10-31 2019-10-31 Thin-layer chromatography stick and adsorbent smearing device thereof Active CN211478183U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112748212A (en) * 2019-10-31 2021-05-04 中国石油化工股份有限公司 Method for analyzing wax content in crude oil

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112748212A (en) * 2019-10-31 2021-05-04 中国石油化工股份有限公司 Method for analyzing wax content in crude oil

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