CN107389834A - A kind of visual low pressure isotopic separation chromatograph post - Google Patents

A kind of visual low pressure isotopic separation chromatograph post Download PDF

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Publication number
CN107389834A
CN107389834A CN201710564662.5A CN201710564662A CN107389834A CN 107389834 A CN107389834 A CN 107389834A CN 201710564662 A CN201710564662 A CN 201710564662A CN 107389834 A CN107389834 A CN 107389834A
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CN
China
Prior art keywords
column
cavity
sealing ring
column cap
jecket
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Granted
Application number
CN201710564662.5A
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Chinese (zh)
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CN107389834B (en
Inventor
周炼
胡雅婷
王倩
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China University of Geosciences
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China University of Geosciences
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Priority to CN201710564662.5A priority Critical patent/CN107389834B/en
Publication of CN107389834A publication Critical patent/CN107389834A/en
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Publication of CN107389834B publication Critical patent/CN107389834B/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/60Construction of the column
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • G01N2030/065Preparation using different phases to separate parts of sample

Abstract

The present invention provides a kind of visual low pressure isotopic separation chromatograph post,Including column jecket,Column cap,Sieve plate and sealing ring,The column cap includes column cap top,The inwall on the column cap top is provided with the first cavity and the second cavity,Second cavity connects with the first cavity,In second cavity sieve plate is placed close to the position of the first cavity,Inlay sealing ring in the periphery of the sieve plate,The inwall of the sealing ring and the second cavity, which is in close contact, to be compressed,Sealing ring is arranged with the column jecket,The sealing ring is bonded with column jecket,In second cavity on the column jecket insertion column cap top,The outside of the sealing ring is inserted in the second cavity with column jecket,The sealing ring is extruded and is in close contact and compresses with the inwall of the second cavity in the presence of elastic force,The column jecket contacts with sieve plate,And it is brought into close contact with sealing ring,So as to which the column jecket is fixedly connected on column cap top.The present invention has good degrees and transparent characteristic.

Description

A kind of visual low pressure isotopic separation chromatograph post
Technical field
The present invention relates to isotope analysis Instrument technology field, more particularly to a kind of visual low pressure isotopic separation chromatograph Post.
Background technology
Liquid chromatogram exchange column is mainly by stainless steel and PEEK (polyetheretherketone, polyether-ether-ketone) material at present Material is made, its simple structure, and is widely used in liquid phase assay laboratory.It our experiments show that as made from stainless steel material Chromatogram exchange column is very poor to the tolerance of strong acid, therefore can not be widely used in the chromatography using acid as mobile phase, and by PEEK Although chromatogram exchange column has certain tolerance to strong acid made from material, for what is commonly used during isotope analysis The tolerance of nitric acid and hydrofluoric acid is also bad, therefore, during liquid-phase chromatographic analysis, is related to color of the strong acid as eluent Layer separation, has not yet to see the good chromatogram exchange column of adaptability.
Perfluoroethylene-propylene (FEP) is the copolymer of tetrafluoroethene and hexafluoropropene, its chemical-resistant stability and polytetrafluoro Ethene is similar, has excellent chemical-resistant stability, except with the fluorine element under high temperature, the alkali metal of melting and the hair such as chlorine trifluoride Raw reaction is outer, is not corroded when being contacted with other chemicals, is widely used in High Purity analysis, and particularly geochemistry is led Domain isotope analysis, FEP materials have the characteristics of acid and alkali-resistance, Low background, wide by global isotope analysis field laboratory General use, it is currently used primarily in the storage of high purity reagent.Such as the Nalgene companies of famous American are using made of FEP materials Vessel are adapted to ultra trace analysis experiment.Not yet occur made of FEP at present, go for low pressure liquid phase chromatography separation from Son exchanges chromatograph post.
In addition, traditional ion exchange column has the following disadvantages made of stainless steel and PEEK:It is difficult to observe by ion color Stationary phase (ion exchange resin) and the situation of mobile phase elution change in layer separation process, especially for low pressure chromatography During, due to using the larger stationary phase (ion exchange resin etc.) of porosity, whether produced during chromatograph bubble and The generation for situations such as stationary phase is dry caused by Stress control is bad, the effect of isotope chromatography purifying can be had a strong impact on, And traditional ion exchange column made of stainless steel and PEEK can not observe the generation of this phenomenon, PEEK is additionally, since The inwall processing difficulty of pipe is larger, and its finish is well below the inwall of FEP pipes, tube wall of the PEEK pipes during chromatography Effect is also significantly greater than FEP pipes.The low pressure chromatograph post made of glass that currently there are, in isotope analysis The acidic materials being related in journey, the dissolution containing potassium, sodium plasma in glass can be caused, it is impossible to meet isotope trace analysis Need, while the joint and sieve plate being made of plastics are an entirety, it is not easy to which butt joint and sieve plate are cleaned, and can not be fitted For the hand-tight joint of international chromatogram.
The content of the invention
In view of this, the invention provides a kind of same position of visual low pressure with good degrees and transparent characteristic Element separation chromatograph post.
The present invention provides a kind of visual low pressure isotopic separation chromatograph post, including column jecket, column cap, sieve plate and sealing ring, institute Stating column cap includes column cap top, and the inwall on the column cap top is provided with the first cavity and the second cavity, second cavity and One cavity is connected, and sieve plate is placed close to the position of the first cavity in second cavity, and sealing ring is inlayed in the periphery of the sieve plate, The inwall of the sealing ring and the second cavity, which is in close contact, to be compressed, and sealing ring, the sealing ring and post are arranged with the column jecket Pipe is bonded, and in second cavity on the column jecket insertion column cap top, the outside of the sealing ring is with column jecket the second cavity of insertion Interior, the sealing ring is extruded and is in close contact and compresses with the inwall of the second cavity in the presence of elastic force, the column jecket with Sieve plate contacts, and is brought into close contact with sealing ring, and so as to which the column jecket is fixedly connected on column cap top, the column jecket is by acidproof, resistance to Alkali, flexible material that is preferable, having the transparency are formed.
Further, the column cap also includes column cap bottom, and the inwall of the column cap bottom is provided with the 3rd cavity, by described in Column jecket is inserted in the 3rd cavity, and the column cap bottom can be slided along column jecket, and the second internal thread, institute are provided with the 3rd cavity The outside for stating the second cavity is provided with the first external screw thread, and second internal thread and the first external screw thread are connected so as to by column cap Portion is connected with column cap bottom, and sealing ring is extruded and realizes sealing ring when second internal thread and the first external screw thread are connected It is in close contact and compresses with the inwall of the second cavity.
Further, the chromatograph post also includes the joint matched with column cap, and the lower end of the joint is provided with the second outer spiral shell Line, first cavity on the column cap top is interior to be provided with the first internal thread, and second external screw thread is connected with the first screw-internal thread fit So as to which joint be connected with column cap top, through hole, the lower end connection butt joint of the joint, the joint are provided with the joint Formed with butt joint by polytetrafluoroethylmaterial material.
Further, the sealing ring includes upper bottom surface and bottom surface, and the diameter of the upper bottom surface is less than the straight of bottom surface Footpath, the diameter of the upper bottom surface is consistent with the internal diameter of column jecket, and the diameter of the bottom surface is consistent with the external diameter of column jecket, the sealing Circle is shaped as truncated cone-shaped.
Further, the internal diameter of the sealing ring and the internal diameter of column jecket are consistent, and the diameter of second cavity is more than column jecket External diameter.
Further, the column cap top and column cap bottom are equipped with slot, and rotating slot by spanner makes column cap Top and the rotation of column cap bottom, it can be ensured that the close connection of column cap top and column cap bottom.
Further, the column cap, sieve plate, sealing ring and sealing ring are formed by polytetrafluoroethylmaterial material.
Further, the column jecket is made up of perfluoroethylene-propylene material.
Further, the both ends of the column jecket are mounted on column cap, and the structure of two column caps is identical.
Further, the inside of the column jecket is filled with resin, and sample flows into after sample injector adds along the through hole Butt joint, the second cavity is flowed out to then along the inwall of butt joint, sample is flowed into after the sieve plate screening in the second cavity Separation process is carried out in column jecket.
The beneficial effect that technical scheme provided by the invention is brought is:
It is and traditional 1. visual low pressure isotopic separation chromatograph post provided by the invention has good tolerance to soda acid Ion exchange column is compared, and has wider array of application prospect in low pressure chromatography field;
2. the column jecket of the present invention has good transparent characteristic, can realize observe at any time it is solid during ion chromatography Determine the situation of phase change, improve the reliability for judging low pressure isotope chromatography purification effect;
3. the present invention need not process screw thread on column jecket, reduce processing technology, and the length of column jecket being capable of basis Need to adjust, convenient use;
4. the column cap and sieve plate of visual low pressure isotopic separation chromatograph post provided by the invention are isolating construction, it is easily installed And cleaning, suitable for the hand-tight joint of international chromatogram.
Brief description of the drawings
Fig. 1 is a kind of structural representation of visual low pressure isotopic separation chromatograph post of the present invention.
Fig. 2 is a kind of front view of visual low pressure isotopic separation chromatograph post of the present invention.
Fig. 3 is a kind of structural representation of the column cap of visual low pressure isotopic separation chromatograph post of the present invention.
Fig. 4 is a kind of structural representation of the column jecket of visual low pressure isotopic separation chromatograph post of the present invention.
Fig. 5 is a kind of structural representation of the sealing ring of visual low pressure isotopic separation chromatograph post of the present invention.
Fig. 6 is a kind of structural representation of the joint of visual low pressure isotopic separation chromatograph post of the present invention.
Embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with accompanying drawing to embodiment party of the present invention Formula is further described.
Fig. 1, Fig. 2 and Fig. 3 are refer to, the embodiment provides a kind of visual low pressure isotopic separation chromatograph post, Including column jecket 1, column cap 2, sieve plate 3, sealing ring 4 and the joint 5 matched with column cap, column cap 2 includes the column cap top being connected 21 and column cap bottom 22, joint 5 be connected with column cap top 21, column cap bottom 22 can be slided along column jecket 1, column cap top 21 it is interior Wall is provided with the first cavity 211 and the second cavity 213, and the second cavity 213 is connected with the first cavity 211, is provided with the first cavity 211 First internal thread 212, joint 5 are inserted in the first cavity 211, and the outside of the second cavity 213 is provided with the first external screw thread 214, and second Sieve plate 3 is placed close to the position of the first cavity 211 in cavity 213, sealing ring 4, sealing ring 4 and second are inlayed in the periphery of sieve plate 3 The inwall of cavity 213, which is in close contact, to be compressed, and the inwall of column cap bottom 22 is provided with the 3rd cavity 221, provided with the in the 3rd cavity 221 Two internal threads 222, the second internal thread 222 and the first external screw thread 214 are connected so as to by column cap top 21 and column cap bottom 22 Connect, in an embodiment, the both ends of column jecket 1 are mounted on column cap 2, and the structure of two column caps 2 is identical.
The internal diameter of sealing ring 4 is consistent with the internal diameter of column jecket 1, and the diameter of the second cavity 213 is more than the external diameter of column jecket 1.
With reference to figure 4 and Fig. 5, column jecket 1 is hollow structure, and its top and bottom is arranged with the sealing ring for being shaped as truncated cone-shaped 6, sealing ring 6 is bonded with column jecket 1, and column jecket 1 is inserted in the 3rd cavity 221, and column jecket 1 then is inserted into the second of column cap top 21 In cavity 213, the outside of sealing ring 6 is as in the second cavity 213 of insertion of column jecket 1, rotating column cap bottom 22 makes the second internal thread 222 are connected with the first external screw thread 214, and sealing ring 6 is extruded then when the second internal thread 222 and the first external screw thread 214 are connected Make sealing ring 6 be in close contact with the inwall of the second cavity 213 in the presence of elastic force to compress, the upper end of column jecket 1, lower end difference Contact with sieve plate 3, and be brought into close contact with sealing ring 4, so as to which column jecket 1 is fixedly connected on into column cap top 21, and is effectively ensured The sealing of chromatograph post, reduce dead volume.
Sealing ring 6 includes upper bottom surface 61 and bottom surface 62, and the diameter of upper bottom surface 61 is less than the diameter of bottom surface 62, upper bottom surface 61 diameter is consistent with the internal diameter of column jecket 1, and the diameter of bottom surface 62 is consistent with the external diameter of column jecket 1, and the diameter of bottom surface 62 is more than The close contact that the inwall of the cavity 213 of sealing ring 6 and second has been effectively ensured in the diameter of upper bottom surface 61 compresses;In one embodiment, Bottom surface 62 and the angle of the side of sealing ring 6 are 30 °, it is ensured that sealing ring 6 is brought into close contact with column jecket 1 and sealing ring 6 exists Larger elastic force can be produced when being squeezed, so as to effectively reduce the dead volume of chromatograph post.
Uniform potting resin in column jecket 1, resin constitute the stationary phase of visual low pressure isotopic separation chromatograph post.
With reference to figure 6, the lower end of joint 5 is provided with the second external screw thread 51, and the second external screw thread 51 and the first internal thread 212, which coordinate, to be connected Connect, through hole 52 is provided with joint 5, the lower end connection of joint 5 is shaped as the butt joint 7 of hollow ring, and sample adds through sample injector Afterwards, butt joint 7 is flowed into along through hole 52, flows out to the second cavity 213 then along the inwall of butt joint 7, sample is empty through second After sieve plate 3 in chamber 213 sieves, it is flowed into column jecket 1 and carries out separation process.
Column jecket 1 is made up of acidproof, alkaline-resisting, the flexible material for preferably, having the transparency, and column jecket 1 is shaped as cylinder, and one In embodiment, column jecket 1 is made up of perfluoroethylene-propylene (fluorinated ethylenepropylene, FEP) material, FEP pairs Strong acid has good tolerance.
In one embodiment, the internal diameter of column jecket 1 is 3mm, and the external diameter of column jecket 1 is 6mm.
Column cap 2, sieve plate 3, sealing ring 4, sealing ring 6, joint 5 and butt joint 7 are formed by polytetrafluoroethylmaterial material.
Column cap top 21 and column cap bottom 22 are equipped with slot 8, and rotating slot 8 by spanner makes the He of column cap top 21 Column cap bottom 22 rotates, it can be ensured that the close connection of column cap top 21 and column cap bottom 22.
Visual low pressure isotopic separation chromatograph post provided by the invention has good tolerance to soda acid, with it is traditional from Sub- exchange column is compared, and has wider array of application prospect in low pressure chromatography field;The column jecket 1 of the present invention has well transparent Characteristic, it can realize to observe at any time and fix the situation of phase change during ion chromatography, raising judges low pressure isotope color Layer isolates and purifies the reliability of effect;The present invention need not process screw thread on column jecket 1, reduce processing technology, and column jecket 1 Length can adjust as needed, convenient use;The He of column cap 2 of visual low pressure isotopic separation chromatograph post provided by the invention Sieve plate 3 is isolating construction, is easily installed and cleans, suitable for the hand-tight joint of international chromatogram.
Herein, the involved noun of locality such as forward and backward, upper and lower is to be located at parts in accompanying drawing in figure and zero The mutual position of part is intended merely to the clear of expression technology scheme and conveniently come what is defined.It should be appreciated that the noun of locality Use should not limit the claimed scope of the application.
In the case where not conflicting, the feature in embodiment and embodiment herein-above set forth can be combined with each other.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and Within principle, any modification, equivalent substitution and improvements made etc., it should be included in the scope of the protection.

Claims (10)

1. a kind of visual low pressure isotopic separation chromatograph post, it is characterised in that described including column jecket, column cap, sieve plate and sealing ring Column cap includes column cap top, and the inwall on the column cap top is provided with the first cavity and the second cavity, second cavity and first Cavity is connected, and sieve plate is placed close to the position of the first cavity in second cavity, and sealing ring is inlayed in the periphery of the sieve plate, institute The inwall for stating sealing ring and the second cavity is in close contact compression, and sealing ring, the sealing ring and column jecket are arranged with the column jecket Fitting, in second cavity on column jecket insertion column cap top, the outside of the sealing ring is inserted in the second cavity with column jecket, The sealing ring is extruded and is in close contact and compresses with the inwall of the second cavity in the presence of elastic force, the column jecket and sieve plate Contact, and be brought into close contact with sealing ring, so as to which the column jecket is fixedly connected on column cap top, the column jecket is by acidproof, alkaline-resisting, soft Property preferably, have the transparency material form.
2. visual low pressure isotopic separation chromatograph post as claimed in claim 1, it is characterised in that the column cap also includes column cap Bottom, the inwall of the column cap bottom are provided with the 3rd cavity, the column jecket are inserted in the 3rd cavity, the column cap bottom can edge Column jecket slip, is provided with the second internal thread in the 3rd cavity, the outside of second cavity is provided with the first external screw thread, described Second internal thread and the first external screw thread are connected so as to which column cap top be connected with column cap bottom, second internal thread and the Sealing ring is extruded and realizes the inwall of sealing ring and the second cavity and be in close contact compression when one external screw thread is connected.
3. low pressure isotopic separation chromatograph post as claimed in claim 1 visual, it is characterised in that the chromatograph post also include with The joint of column cap matching, the lower end of the joint are provided with the second external screw thread, first are provided with first cavity on the column cap top Internal thread, second external screw thread are connected with the first screw-internal thread fit so as to which joint be connected with column cap top, in the joint Provided with through hole, the lower end connection butt joint of the joint, the joint and butt joint are formed by polytetrafluoroethylmaterial material.
4. visual low pressure isotopic separation chromatograph post as claimed in claim 1, it is characterised in that the sealing ring includes upper bottom Face and bottom surface, the diameter of the upper bottom surface are less than the diameter of bottom surface, and the diameter of the upper bottom surface is consistent with the internal diameter of column jecket, The diameter of the bottom surface is consistent with the external diameter of column jecket, and the sealing ring is shaped as truncated cone-shaped.
5. low pressure isotopic separation chromatograph post as claimed in claim 1 visual, it is characterised in that the internal diameter of the sealing ring with The internal diameter of column jecket is consistent, and the diameter of second cavity is more than the external diameter of column jecket.
6. visual low pressure isotopic separation chromatograph post as claimed in claim 2, it is characterised in that the column cap top and column cap Bottom is equipped with slot, and rotating slot by spanner rotates column cap top and column cap bottom, it can be ensured that column cap top With the close connection of column cap bottom.
7. visual low pressure isotopic separation chromatograph post as claimed in claim 1, it is characterised in that the column cap, sieve plate, sealing Ring and sealing ring are formed by polytetrafluoroethylmaterial material.
8. visual low pressure isotopic separation chromatograph post as claimed in claim 1, it is characterised in that the column jecket is by perfluoroethylene Propylene material is formed.
9. visual low pressure isotopic separation chromatograph post as claimed in claim 1, it is characterised in that pacify at the both ends of the column jecket Equipped with column cap, and the structure of two column caps is identical.
10. visual low pressure isotopic separation chromatograph post as claimed in claim 3, it is characterised in that the inside of the column jecket is filled out Filled with resin, sample flows into butt joint after sample injector adds, along the through hole, is flowed out to then along the inwall of butt joint Second cavity, sample are flowed into column jecket after the sieve plate screening in the second cavity and carry out separation process.
CN201710564662.5A 2017-07-12 2017-07-12 Visual low pressure isotope separation chromatographic column Active CN107389834B (en)

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Application Number Priority Date Filing Date Title
CN201710564662.5A CN107389834B (en) 2017-07-12 2017-07-12 Visual low pressure isotope separation chromatographic column

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Application Number Priority Date Filing Date Title
CN201710564662.5A CN107389834B (en) 2017-07-12 2017-07-12 Visual low pressure isotope separation chromatographic column

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CN107389834A true CN107389834A (en) 2017-11-24
CN107389834B CN107389834B (en) 2022-11-01

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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US3954291A (en) * 1973-01-13 1976-05-04 Bobensweewerk Perkin-Elmer & Co. Gmbh Reusable sealed coupling for glass tubes
US5188730A (en) * 1990-05-07 1993-02-23 Kronwald Separationstechnik Gmbh Multipart chromatography column connection
US20110120926A1 (en) * 2008-05-22 2011-05-26 Proxeon Biosystems A/S Pre-assembled separation columns
US20130043672A1 (en) * 2009-12-22 2013-02-21 Waters Technologies Corporation Fluidic Coupler Assembly With Conical Ferrule
US20150068979A1 (en) * 2012-04-14 2015-03-12 Merck Patent Gmbh Holder for monolithic sorbents
WO2017057320A1 (en) * 2015-10-02 2017-04-06 三菱瓦斯化学株式会社 High-purity carboxylic acid ester and method for producing same

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3511377A (en) * 1963-10-02 1970-05-12 Ceskoslovenska Akademie Ved Closure of columns,particularly of chromatographic columns
US3954291A (en) * 1973-01-13 1976-05-04 Bobensweewerk Perkin-Elmer & Co. Gmbh Reusable sealed coupling for glass tubes
US5188730A (en) * 1990-05-07 1993-02-23 Kronwald Separationstechnik Gmbh Multipart chromatography column connection
US20110120926A1 (en) * 2008-05-22 2011-05-26 Proxeon Biosystems A/S Pre-assembled separation columns
US20130043672A1 (en) * 2009-12-22 2013-02-21 Waters Technologies Corporation Fluidic Coupler Assembly With Conical Ferrule
US20150068979A1 (en) * 2012-04-14 2015-03-12 Merck Patent Gmbh Holder for monolithic sorbents
WO2017057320A1 (en) * 2015-10-02 2017-04-06 三菱瓦斯化学株式会社 High-purity carboxylic acid ester and method for producing same

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Title
童铄云 等: "钙同位素分析测试技术进展", 《矿物岩石地球化学通报》 *

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