CN107389834B - Visual low pressure isotope separation chromatographic column - Google Patents
Visual low pressure isotope separation chromatographic column Download PDFInfo
- Publication number
- CN107389834B CN107389834B CN201710564662.5A CN201710564662A CN107389834B CN 107389834 B CN107389834 B CN 107389834B CN 201710564662 A CN201710564662 A CN 201710564662A CN 107389834 B CN107389834 B CN 107389834B
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- column
- cavity
- sealing ring
- column head
- tube
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/60—Construction of the column
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/065—Preparation using different phases to separate parts of sample
Abstract
The invention provides a visual low-pressure isotope separation chromatographic column which comprises a column head, a sieve plate and a sealing ring, wherein the column head comprises a column head upper part, the inner wall of the column head upper part is provided with a first cavity and a second cavity, the second cavity is communicated with the first cavity, the sieve plate is arranged in the second cavity close to the first cavity, the sealing ring is embedded in the periphery of the sieve plate, the sealing ring is tightly contacted and pressed with the inner wall of the second cavity, the column head is sleeved with a sealing ring, the sealing ring is attached to the column head, the column head is inserted into the second cavity in the column head upper part, the outer side of the sealing ring is inserted into the second cavity along with the column head, the sealing ring is extruded to be tightly contacted and pressed with the inner wall of the second cavity under the action of elastic force, the column head is contacted with the sieve plate and is tightly attached to the sealing ring, and the column head is fixedly connected to the column head upper part. The invention has good acid-base tolerance and transparency.
Description
Technical Field
The invention relates to the technical field of isotope analysis instruments, in particular to a visual low-pressure isotope separation chromatographic column.
Background
At present, the liquid chromatography exchange column is mainly made of stainless steel and PEEK (polyetheretherketone), has a simple structure, and is widely applied to a gas-liquid phase analysis laboratory. Experiments show that the chromatographic exchange column made of stainless steel material has poor tolerance to strong acid, so that the chromatographic exchange column cannot be widely used for chromatographic separation by taking acid as a mobile phase, and the chromatographic exchange column made of PEEK material has certain tolerance to strong acid, but has poor tolerance to nitric acid and hydrofluoric acid which are commonly used in an isotope analysis process, so that chromatographic separation by taking strong acid as eluent is involved in a liquid chromatographic analysis process, and a chromatographic exchange column with good adaptability is not available at present.
The Fluorinated Ethylene Propylene (FEP) is a copolymer of tetrafluoroethylene and hexafluoropropylene, has chemical stability similar to that of polytetrafluoroethylene, has excellent chemical stability, is not corroded when being contacted with other chemicals except for reaction with fluorine element, molten alkali metal, chlorine trifluoride and the like at high temperature, is widely applied to high-purity analysis, particularly to isotope analysis in the geochemistry field, has the characteristics of acid and alkali resistance and low background, is widely used by laboratories in the global isotope analysis field, and is mainly used for storing high-purity reagents at present. For example, vessels made of FEP material are suitable for ultra trace analysis experiments, as is well known from the american Nalgene corporation. Currently no ion exchange chromatography column made of FEP is available that can be suitable for low pressure liquid chromatography.
In addition, the conventional ion exchange column made of stainless steel and PEEK has the following disadvantages: the condition that the elution of the stationary phase (ion exchange resin) and the mobile phase changes in the ion chromatography process is difficult to observe, especially for the low-pressure chromatography process, because the stationary phase (ion exchange resin and the like) with larger porosity is adopted, whether bubbles are generated in the chromatography process and the conditions of the drying of the stationary phase and the like caused by poor pressure control can seriously influence the separation and purification effect of the isotope chromatography, the traditional ion exchange column made of stainless steel and PEEK can not observe the phenomenon, in addition, because the processing difficulty of the inner wall of the PEEK tube is larger, the smoothness of the PEEK tube is far lower than that of the inner wall of the FEP tube, and the tube wall effect of the PEEK tube in the chromatography process is also obviously larger than that of the FEP tube. The low-pressure chromatographic column made of glass in the current market can dissolve out potassium, sodium and other ions in the glass for strong acid substances involved in the isotope analysis process, cannot meet the needs of isotope trace analysis, and meanwhile, a joint and a sieve plate made of plastic are integrated, so that the joint and the sieve plate are not easy to clean, and the low-pressure chromatographic column is not suitable for an international general chromatographic manual joint.
Disclosure of Invention
In view of the above, the present invention provides a visible low-pressure isotope separation chromatographic column having good acid-base resistance and transparency characteristics.
The invention provides a visual low-pressure isotope separation chromatographic column which comprises a column head, a sieve plate and a sealing ring, wherein the column head comprises a column head upper part, the inner wall of the column head upper part is provided with a first cavity and a second cavity, the second cavity is communicated with the first cavity, the sieve plate is arranged in the second cavity close to the first cavity, the sealing ring is embedded in the periphery of the sieve plate and tightly contacted and pressed with the inner wall of the second cavity, the column pipe is sleeved with a sealing ring, the sealing ring is attached to the column head, the column pipe is inserted into the second cavity in the column head upper part, the outer side of the sealing ring is inserted into the second cavity along with the column pipe, the sealing ring is extruded and tightly contacted and pressed with the inner wall of the second cavity under the action of elastic force, the column pipe is contacted with the sieve plate and tightly attached to the sealing ring, so that the column pipe is fixedly connected to the column head upper part, and the column pipe is made of a material with good acid resistance, alkali resistance and flexibility and transparency.
The column head further comprises a lower part of the column head, a third cavity is formed in the inner wall of the lower part of the column head, the column tube is inserted into the third cavity, the lower part of the column head can slide along the column tube, a second internal thread is arranged in the third cavity, a first external thread is arranged outside the second cavity, the second internal thread is matched and connected with the first external thread so as to connect the upper part of the column head with the lower part of the column head, and when the second internal thread is matched and connected with the first external thread, the sealing ring is extruded to realize tight contact and compression of the sealing ring and the inner wall of the second cavity.
Furthermore, the chromatographic column further comprises a joint matched with the column head, a second external thread is arranged at the lower end of the joint, a first internal thread is arranged in the first cavity at the upper part of the column head, the second external thread is matched and connected with the first internal thread so as to connect the joint with the upper part of the column head, a through hole is formed in the joint, the lower end of the joint is connected with a butt joint, and the joint and the butt joint are both made of polytetrafluoroethylene materials.
Further, the sealing ring comprises an upper bottom surface and a lower bottom surface, the diameter of the upper bottom surface is smaller than that of the lower bottom surface, the diameter of the upper bottom surface is consistent with the inner diameter of the column tube, the diameter of the lower bottom surface is consistent with the outer diameter of the column tube, and the sealing ring is in a circular truncated cone shape.
Further, the inner diameter of the sealing ring is consistent with the inner diameter of the column tube, and the diameter of the second cavity is larger than the outer diameter of the column tube.
Furthermore, the upper part of the column head and the lower part of the column head are both provided with a clamping groove position, and the upper part of the column head and the lower part of the column head can rotate by rotating the clamping groove positions through a wrench, so that the upper part of the column head and the lower part of the column head can be tightly connected.
Furthermore, the column cap, the sieve plate, the sealing ring and the sealing ring are all made of polytetrafluoroethylene materials.
Further, the column tube is made of a fluorinated ethylene propylene material.
Furthermore, column heads are mounted at two ends of the column tube, and the two column heads have the same structure.
Furthermore, the inside packing of column tube has the resin, and the sample adds the back through the injector, along the through-hole flows in the butt joint, then flows out to the second cavity along the inner wall of butt joint, and the sample flows in the column tube and carries out the separation process after the sieve screen in the second cavity.
The technical scheme provided by the invention has the beneficial effects that:
1. the visible low-pressure isotope separation chromatographic column provided by the invention has good tolerance to acid and alkali, and has wider application prospect in the field of low-pressure chromatographic separation compared with the traditional ion exchange column;
2. the column tube has good transparent characteristic, can realize the observation of the change of the stationary phase in the ion chromatography process at any time, and improves the reliability of judging the separation and purification effect of the low-pressure isotope chromatography;
3. the invention does not need to process threads on the column tube, thereby reducing the processing technique, and the length of the column tube can be adjusted according to the requirement, thereby being convenient for use;
4. the column head and the sieve plate of the visual low-pressure isotope separation chromatographic column provided by the invention are of a separation structure, are convenient to install and clean, and are suitable for international universal chromatographic hand-tightening joints.
Drawings
Fig. 1 is a schematic structural view of a visible low-pressure isotope separation chromatographic column according to the present invention.
Fig. 2 is a front view of a visible low pressure isotope separation chromatically layered column of the present invention.
Fig. 3 is a schematic structural diagram of a column head of a visible low-pressure isotope separation chromatically-layered column according to the present invention.
Fig. 4 is a schematic structural diagram of a column tube of a visible low-pressure isotope separation chromatographic column of the present invention.
Fig. 5 is a schematic structural diagram of a seal ring of a visible low-pressure isotope separation chromatographic column according to the present invention.
Fig. 6 is a schematic structural diagram of a joint of a visible low-pressure isotope separation chromatographic column according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be further described with reference to the accompanying drawings.
Referring to fig. 1, 2 and 3, an embodiment of the present invention provides a visible low-pressure isotope separation chromatographic column, including a column tube 1, a column head 2, a screen plate 3, a sealing ring 4 and a joint 5 matched with the column head, where the column head 2 includes a column head upper part 21 and a column head lower part 22 in a matching connection, the joint 5 is connected with the column head upper part 21, the column head lower part 22 can slide along the column tube 1, the inner wall of the column head upper part 21 is provided with a first cavity 211 and a second cavity 213, the second cavity 213 is communicated with the first cavity 211, the first cavity 211 is provided with a first internal thread 212, the joint 5 is inserted into the first cavity 211, the second cavity 213 is provided with a first external thread 214 on the outside, the screen plate 3 is placed in the second cavity 213 near the first cavity 211, the peripheral sealing ring 4 of the screen plate 3 is embedded, the sealing ring 4 is tightly contacted and pressed with the inner wall of the second cavity 213, the inner wall of the column head lower part 22 is provided with a third cavity 221, the second internal thread 222 is arranged in the third cavity 221, the second internal thread 222 is matched and connected with the first cavity 214, and the column head 22, and two column head 2 is provided with the same structure.
The inner diameter of the sealing ring 4 is the same as the inner diameter of the column tube 1, and the diameter of the second cavity 213 is larger than the outer diameter of the column tube 1.
Referring to fig. 4 and 5, the column tube 1 is a hollow structure, the upper end and the lower end of the column tube 1 are both sleeved with the sealing ring 6 in a truncated cone shape, the sealing ring 6 is attached to the column tube 1, the column tube 1 is inserted into the third cavity 221, then the column tube 1 is inserted into the second cavity 213 of the column head upper portion 21, the outer side of the sealing ring 6 is inserted into the second cavity 213 along with the column tube 1, the column head lower portion 22 is rotated to connect the second internal thread 222 with the first external thread 214, when the second internal thread 222 is connected with the first external thread 214 in a matching manner, the sealing ring 6 is squeezed to enable the sealing ring 6 to be tightly contacted and pressed with the inner wall of the second cavity 213 under the effect of elastic force, the upper end and the lower end of the column tube 1 are respectively contacted with the screen plate 3 and tightly attached to the sealing ring 4, so that the column tube 1 is fixedly connected to the column head upper portion 21, the sealing performance of the chromatographic column is effectively ensured, and the dead volume is reduced.
The sealing ring 6 comprises an upper bottom surface 61 and a lower bottom surface 62, the diameter of the upper bottom surface 61 is smaller than that of the lower bottom surface 62, the diameter of the upper bottom surface 61 is consistent with the inner diameter of the column tube 1, the diameter of the lower bottom surface 62 is consistent with the outer diameter of the column tube 1, and the diameter of the lower bottom surface 62 is larger than that of the upper bottom surface 61, so that the sealing ring 6 is effectively guaranteed to be tightly contacted and pressed with the inner wall of the second cavity 213; in one embodiment, the included angle between the lower bottom surface 62 and the side surface of the sealing ring 6 is 30 degrees, so that the sealing ring 6 can be tightly attached to the column tube 1, and the sealing ring 6 can generate large elastic force when being extruded, thereby effectively reducing the dead volume of the color layer column.
The column tube 1 is uniformly filled with resin, and the resin forms a stationary phase of the visible low-pressure isotope separation chromatographic column.
Referring to fig. 6, the lower end of the joint 5 is provided with a second external thread 51, the second external thread 51 is connected with the first internal thread 212 in a matching manner, a through hole 52 is formed in the joint 5, the lower end of the joint 5 is connected with a butt joint 7 in the shape of a hollow circular ring, a sample is added by a sample adding device, flows into the butt joint 7 along the through hole 52, flows out to the second cavity 213 along the inner wall of the butt joint 7, and flows into the column tube 1 for a separation process after being screened by the screen plate 3 in the second cavity 213.
The column tube 1 is made of a material which is acid-resistant, alkali-resistant, flexible and transparent, the column tube 1 is cylindrical, in an embodiment, the column tube 1 is made of Fluorinated Ethylene Propylene (FEP) material, and the FEP has good resistance to strong acid.
In one embodiment, the inner diameter of vial 1 is 3mm and the outer diameter of vial 1 is 6mm.
The column cap 2, the sieve plate 3, the sealing ring 4, the sealing ring 6, the joint 5 and the butt joint 7 are all made of polytetrafluoroethylene materials.
The column head upper part 21 and the column head lower part 22 are both provided with the clamping groove positions 8, the clamping groove positions 8 are rotated by a wrench to enable the column head upper part 21 and the column head lower part 22 to rotate, and the tight connection of the column head upper part 21 and the column head lower part 22 can be ensured.
The visible low-pressure isotope separation chromatographic column provided by the invention has good tolerance to acid and alkali, and has wider application prospect in the field of low-pressure chromatographic separation compared with the traditional ion exchange column; the column tube 1 has good transparent characteristic, can realize the observation of the change of the stationary phase in the ion chromatography process at any time, and improves the reliability of judging the separation and purification effect of the low-pressure isotope chromatography; according to the invention, threads do not need to be machined on the column tube 1, so that the machining process is reduced, and the length of the column tube 1 can be adjusted as required, so that the column tube is convenient to use; the column head 2 and the sieve plate 3 of the visual low-pressure isotope separation chromatographic column provided by the invention are of a separation structure, are convenient to install and clean, and are suitable for international universal chromatographic hand-tightening joints.
In this document, the terms front, back, upper, lower and the like in the drawings are used for the sake of clarity and convenience only for the components are located in the drawings and the positions of the components relative to each other. It is to be understood that the use of the directional terms should not be taken to limit the scope of the claims.
The embodiments and features of the embodiments described herein above may be combined with each other without conflict.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (5)
1. The visible low-pressure isotope separation chromatographic column is characterized by comprising a column tube, a column cap, a sieve plate and a sealing ring, wherein the column cap comprises a column cap upper part, the inner wall of the column cap upper part is provided with a first cavity and a second cavity, the second cavity is communicated with the first cavity, the sieve plate is arranged in the second cavity close to the first cavity, the sealing ring is embedded in the periphery of the sieve plate, the sealing ring is tightly contacted and pressed with the inner wall of the second cavity, a sealing ring is sleeved on the column tube and is attached to the column tube, the column tube is inserted into the second cavity in the column cap upper part, the outer side of the sealing ring is inserted into the second cavity along with the column tube, the sealing ring is extruded to be tightly contacted and pressed with the inner wall of the second cavity under the action of elastic force, the column tube is contacted with the sieve plate and is tightly attached to the sealing ring, so that the column tube is fixedly connected to the column cap upper part, and the column tube is made of fluorinated ethylene propylene; the column heads are arranged at two ends of the column tube, and the two column heads have the same structure;
the column head further comprises a column head lower part, a third cavity is formed in the inner wall of the column head lower part, the column tube is inserted into the third cavity, the column head lower part can slide along the column tube, a second internal thread is arranged in the third cavity, a first external thread is arranged outside the second cavity, the second internal thread is matched and connected with the first external thread so as to connect the column head upper part with the column head lower part, and when the second internal thread is matched and connected with the first external thread, the sealing ring is extruded to realize that the sealing ring is tightly contacted and compressed with the inner wall of the second cavity;
the column cap is characterized by further comprising a joint matched with the column cap, a second external thread is arranged at the lower end of the joint, a first internal thread is arranged in a first cavity in the upper portion of the column cap, the second external thread is matched and connected with the first internal thread so as to connect the joint with the upper portion of the column cap, a through hole is formed in the joint, the lower end of the joint is connected with an abutting joint, and the joint and the abutting joint are both made of polytetrafluoroethylene materials;
the sealing ring comprises an upper bottom surface and a lower bottom surface, the diameter of the upper bottom surface is smaller than that of the lower bottom surface, the diameter of the upper bottom surface is consistent with the inner diameter of the column tube, the diameter of the lower bottom surface is consistent with the outer diameter of the column tube, and the sealing ring is in a circular truncated cone shape;
after the sample is added through the sample injector, the sample flows into the butt joint through the through hole, flows out of the inner wall of the butt joint to the second cavity, and flows into the column tube for separation after the sieve plate in the second cavity is sieved.
2. A visual low pressure isotope separation chromatically layered column in accordance with claim 1 wherein an inner diameter of said seal ring corresponds to an inner diameter of said column tube and a diameter of said second cavity is greater than an outer diameter of said column tube.
3. The visible low-pressure isotope separation chromatically-layered column of claim 1, wherein a locking groove is formed in each of the upper column head portion and the lower column head portion, and the locking groove is rotated by a wrench to rotate the upper column head portion and the lower column head portion, so that the upper column head portion and the lower column head portion can be tightly connected.
4. A visual low pressure isotope separation chromatically layered column according to claim 1, wherein said column head, said sieve plate, said seal ring, and said seal ring are all constructed of polytetrafluoroethylene material.
5. The visible low-pressure isotope separation chromatographic column in accordance with claim 1, wherein the interior of said column tube is filled with resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710564662.5A CN107389834B (en) | 2017-07-12 | 2017-07-12 | Visual low pressure isotope separation chromatographic column |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710564662.5A CN107389834B (en) | 2017-07-12 | 2017-07-12 | Visual low pressure isotope separation chromatographic column |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107389834A CN107389834A (en) | 2017-11-24 |
| CN107389834B true CN107389834B (en) | 2022-11-01 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710564662.5A Active CN107389834B (en) | 2017-07-12 | 2017-07-12 | Visual low pressure isotope separation chromatographic column |
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| CN (1) | CN107389834B (en) |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CH465271A (en) * | 1963-10-02 | 1968-11-15 | Ceskoslovenska Akademie Ved | Column closure for column chromatograph |
| US3954291A (en) * | 1973-01-13 | 1976-05-04 | Bobensweewerk Perkin-Elmer & Co. Gmbh | Reusable sealed coupling for glass tubes |
| DE4014605A1 (en) * | 1990-05-07 | 1991-11-14 | Kronwald Separationstechnik Gm | MULTI-PIECE CHROMATOGRAPHIC COLUMN CONNECTION |
| WO2009147001A1 (en) * | 2008-05-22 | 2009-12-10 | Proxeon Biosystems A/S | Pre-assembled separation columns |
| US9707558B2 (en) * | 2009-12-22 | 2017-07-18 | Waters Technologies Corporation | Fluidic coupler assembly with conical ferrule |
| JP2015513105A (en) * | 2012-04-14 | 2015-04-30 | メルク パテント ゲゼルシャフト ミット ベシュレンクテル ハフツングＭｅｒｃｋ Ｐａｔｅｎｔ Ｇｅｓｅｌｌｓｃｈａｆｔ ｍｉｔ ｂｅｓｃｈｒａｅｎｋｔｅｒ Ｈａｆｔｕｎｇ | Holder for monolithic adsorbent |
| JP6760299B2 (en) * | 2015-10-02 | 2020-09-23 | 三菱瓦斯化学株式会社 | High-purity carboxylic acid ester and its manufacturing method |
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2017
- 2017-07-12 CN CN201710564662.5A patent/CN107389834B/en active Active
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