CN106770856B - A kind of chromatography column for being used to analyze hydrogen isotope mixed gas - Google Patents
A kind of chromatography column for being used to analyze hydrogen isotope mixed gas Download PDFInfo
- Publication number
- CN106770856B CN106770856B CN201710045036.5A CN201710045036A CN106770856B CN 106770856 B CN106770856 B CN 106770856B CN 201710045036 A CN201710045036 A CN 201710045036A CN 106770856 B CN106770856 B CN 106770856B
- Authority
- CN
- China
- Prior art keywords
- transition metal
- al2o3
- hydrogen isotope
- mixed gas
- chromatography column
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- 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
- G01N30/6052—Construction of the column body
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The invention discloses a kind of for analyzing the chromatography column of hydrogen isotope mixed gas, which is pipe profile, and pipe profile is metal tube, and the inside diameter ranges of metal tube are 0.8 mm ~ 1.2mm；It is carried in chromatographic column filled with transition metal modified active alundum (Al2O3), transition metal in the form of chloride or oxide on active alundum (Al2O3), transition metal element 3dnThe transition metal of middle n=5 ~ 10.The chromatography column of the present invention solves the poor separating degree brought using conventional packed column, the division of positive parahydrogen and caused by liquid nitrogen liquid fluctuating the problems such as shift of retention time.The chromatography column for being used to analyze hydrogen isotope mixed gas of the present invention, can be by H2、D2、T2, HD, HT, DT it is completely isolated, have many advantages, such as that separating degree is high, reproducible, cheap, preparation process is simple, can realize quantitative analysis hydrogen isotope.
Description
Technical field
The invention belongs to chromatographic technology fields, and in particular to a kind of fill color for being used to analyze hydrogen isotope mixed gas
Compose column.
Background technology
Hydrogen isotope protium (H), deuterium (D), tritium (T) be combined with each other can form same core hydrogen H2、D2、T2With heteronuclear hydrogen HD, HT, DT.
In same core hydrogen, since nuclear spin states are different, and it there are just (ortho-), secondary (para-) hydrogen isotope.Therefore, contain
The mixed gas of three kinds of hydrogen isotopes not only only has H2、D2、T2, also have HD, HT, DT and H2、D2、T2Positive Zhong Chengfen, be
One complicated micro-molecular gas mixture carries out it quantitative analysis with comparable difficulty.Gas chromatography analysis hydrogen is same
Position element have it is easy to operate, the advantages of having a wide range of application.Traditional alundum (Al2O3) packed column is difficult to six kinds of hydrogen isotopes point
Son efficiently separates, and the division of just (ortho-), secondary (para-) hydrogen isotope can cause the overlapping at part peak so that ingredient
It is difficult to quantitative.Although just secondary separation can be eliminated using modified alundum (Al2O3) packed column, due to existing packed column
Column length it is shorter（Less than 1m）Or column internal diameter is larger（About 2.6mm）When, six components still have the separating effect between the peak of part
The separating degree that baseline separation is not achieved is more than 1.5 requirement, and then influences quantitative analysis.Separation can be improved using capillary column
Degree, but have the deficiencies of expensive, preparation process is complicated part.Using longer（Column length 2m ~ 6m）Micro-packed column（Column internal diameter
1.0mm ~1.2mm）Separating degree between component can be effectively promoted, and it is cheap, and preparation process is simple.However, existing market
On do not fully meet requirement analysis hydrogen isotope mixed gas micro-packed column, there is an urgent need for carry out relevant development work.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of packing chromatography for being used to analyze hydrogen isotope mixed gas
Column.
The chromatography column for being used to analyze hydrogen isotope mixed gas of the present invention, its main feature is that：The chromatographic column is
Pipe profile, pipe profile are metal tube, and the inside diameter ranges of metal tube are 0.8 mm ~ 1.2mm；Transition metal is filled in chromatographic column
Modified active alundum (Al2O3), transition metal are carried in the form of chloride or oxide on active alundum (Al2O3), transition
Metallic element is 3dnThe transition metal of middle n=5 ~ 10；
The metal tube is one kind in stainless steel tube, copper pipe or aluminum pipe.
The pipe range of the chromatographic column is 2m ~ 6m, and the both ends of chromatographic column are not filled by transition metal modified active three oxidation two
Aluminium.
The molar ratio of transition metal and active alundum (Al2O3) is in the transition metal modified active alundum (Al2O3)
1：1~1：10.
The chromatography column for being used to analyze hydrogen isotope mixed gas of the present invention is solved to be brought using conventional packed column
Separating degree is poor, caused by the division of positive parahydrogen and liquid nitrogen liquid fluctuating the problems such as shift of retention time.The present invention's is used to divide
The chromatography column of liberation of hydrogen isotope mixed gas, can be by H2、D2、T2, HD, HT, DT it is completely isolated, have separating degree it is high,
The advantages that reproducible, cheap, preparation process is simple, can realize quantitative analysis hydrogen isotope.
Specific embodiment
The present invention is illustrated with reference to embodiment.
The chromatography column for being used to analyze hydrogen isotope mixed gas of the present invention, its main feature is that：The chromatographic column is
Pipe profile, pipe profile are metal tube, and the inside diameter ranges of metal tube are 0.8 mm ~ 1.2mm；Transition metal is filled in chromatographic column
Modified active alundum (Al2O3), transition metal are carried in the form of chloride or oxide on active alundum (Al2O3), transition
Metallic element is 3dnThe transition metal of middle n=5 ~ 10；
The metal tube is one kind in stainless steel tube, copper pipe or aluminum pipe.
The pipe range of the chromatographic column is 2m ~ 6m, and the both ends of chromatographic column are not filled by transition metal modified active three oxidation two
Aluminium.
The molar ratio of transition metal and active alundum (Al2O3) is in the transition metal modified active alundum (Al2O3)
1：1~1：10.
Embodiment 1
Use the stainless steel tube of 2.0 meters of inner surface cleanings（Internal diameter 1.2mm）, manganese is filled inside it（3d54s2）It is modified to live
Property alundum (Al2O3), the molar ratio range of manganese and active alundum (Al2O3) is 1：5.2.Make carrier gas with neon, carrier gas flux is
5ml/min measures H under liquid nitrogen temperature2/HD、HD/D2Separating degree be respectively：1.6、2.4.In test process is repeated several times,
Each component retention time repeatability is good, and uncertainty is less than 2%.All measurements of six kinds of hydrogen isotope gaseous mixtures, to safety condition
It is required that it is high, so chromatographic column test experiments are generally just for H2/D2System, only H2, HD and D2Three kinds of molecules, wherein H2/ HD is
Separated a pair of of ingredient is most difficult to, 1.5 separating degree has reached baseline separation, met requirement of the accurate quantitative analysis to separating degree.Root
Know according to document, if H2/ HD can be completely separable, also can be completely separable between remaining component, and simply the separation of HD/HT is slightly poor.It should
In embodiment, stainless steel tube both ends are respectively kept with the blank of 10cm and 8cm, i.e., without filling alundum (Al2O3)；It is being repeated several times
In test process, if liquid nitrogen liquid level not less than being filled with alundum (Al2O3) part, when liquid fluctuating will not cause the chromatographic peak to retain
Between significant change.
Embodiment 2
The present embodiment and the embodiment of embodiment 1 are essentially identical, and the main distinction is, use 6.0 meters of inner surface cleanings
Stainless steel tube（Internal diameter 1.0mm）, cobalt is filled inside it（3d74s2）Modified active alundum (Al2O3), cobalt and active three oxygen
The molar ratio range for changing two aluminium is 1：5.2.Make carrier gas with neon, carrier gas flux 10ml/min measures H under liquid nitrogen temperature2/HD、
HD/D2Separating degree be respectively：2.8、4.9.Stainless steel tube both ends are respectively kept with the blank of 12cm and 10cm.It is surveyed being repeated several times
During examination, each component retention time repeatability is good, and uncertainty is less than 2%.
Embodiment 3
The present embodiment and the embodiment of embodiment 1 are essentially identical, and the main distinction is, use 3.2 meters of inner surface cleanings
Copper pipe（Internal diameter 1.1mm）, copper is filled inside it（3d104s1）Modified active alundum (Al2O3), three oxidation two of copper and activity
The molar ratio range of aluminium is 1：10.Make carrier gas with neon, carrier gas flux 10ml/min measures H under liquid nitrogen temperature2/HD、HD/D2's
Separating degree is respectively：1.8、2.7.Stainless steel tube both ends are respectively kept with the blank of 11cm and 9cm.Test process is being repeated several times
In, each component retention time repeatability is good, and uncertainty is less than 2%.
Embodiment 4
The present embodiment and the embodiment of embodiment 1 are essentially identical, and the main distinction is, use 2.8 meters of inner surface cleanings
Aluminum pipe（Internal diameter 1.0mm）, nickel is filled inside it（3d84s2）Modified active alundum (Al2O3), three oxidation two of nickel and activity
The molar ratio range of aluminium is 1：1.Make carrier gas with neon, carrier gas flux 10ml/min measures H under liquid nitrogen temperature2/HD、HD/D2's
Separating degree is respectively：1.7、2.6.Stainless steel tube both ends are respectively kept with the blank of 8cm and 9cm.In test process is repeated several times,
Each component retention time repeatability is good, and uncertainty is less than 2%.
The present invention is not limited to above-mentioned specific embodiment, person of ordinary skill in the field from above-mentioned design,
Without performing creative labour, made a variety of conversion are within the scope of the present invention.
Claims (4)
1. a kind of chromatography column for being used to analyze hydrogen isotope mixed gas, it is characterised in that：The chromatographic column is cast
Material, pipe profile are metal tube, and the inside diameter ranges of metal tube are 0.8 mm ~ 1.2mm；Filled with transition metal modified in chromatographic column
Active alundum (Al2O3), transition metal are carried in the form of chloride or oxide on active alundum (Al2O3), transition metal
Element is 3dnThe transition metal of middle n=5 ~ 10.
2. the chromatography column according to claim 1 for being used to analyze hydrogen isotope mixed gas, it is characterised in that：It is described
Metal tube be one kind in stainless steel tube, copper pipe or aluminum pipe.
3. the chromatography column according to claim 1 for being used to analyze hydrogen isotope mixed gas, it is characterised in that：It is described
Chromatographic column pipe range for 2m ~ 6m, the both ends of chromatographic column are not filled by transition metal modified active alundum (Al2O3).
4. the chromatography column according to claim 1 for being used to analyze hydrogen isotope mixed gas, it is characterised in that：It is described
Transition metal modified active alundum (Al2O3) in the molar ratio of transition metal and active alundum (Al2O3) be 1：1~1：10.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710045036.5A CN106770856B (en) | 2017-01-22 | 2017-01-22 | A kind of chromatography column for being used to analyze hydrogen isotope mixed gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710045036.5A CN106770856B (en) | 2017-01-22 | 2017-01-22 | A kind of chromatography column for being used to analyze hydrogen isotope mixed gas |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106770856A CN106770856A (en) | 2017-05-31 |
| CN106770856B true CN106770856B (en) | 2018-05-22 |
Family
ID=58943791
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710045036.5A Expired - Fee Related CN106770856B (en) | 2017-01-22 | 2017-01-22 | A kind of chromatography column for being used to analyze hydrogen isotope mixed gas |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106770856B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107261845A (en) * | 2017-08-25 | 2017-10-20 | 中国工程物理研究院核物理与化学研究所 | A kind of separation method of hydrogen isotope mixed gas |
| CN112834636B (en) * | 2020-12-29 | 2022-03-11 | 中国原子能科学研究院 | Analysis device and analysis method for metastable components of ortho-para hydrogen |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101199936A (en) * | 2007-11-06 | 2008-06-18 | 兰州大学 | Isophthalic acid and m-toluic acid catalyst preparation and method thereof |
| CN101327440A (en) * | 2008-06-27 | 2008-12-24 | 安徽理工大学 | Composite catalyst for producing hydrogen by methane steam reforming technology |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100285593A1 (en) * | 2007-11-26 | 2010-11-11 | Waters Technologies Corporation | Internal standards and methods for use in quantitatively measuring analytes in a sample |
| RS52615B (en) * | 2008-05-15 | 2013-04-30 | Ivan SMAJLOVIĆ | Apparatus for determination of isotopic composition of non-exchangeable hydrogen and deuterium atoms in ethanol samples and procedure for determination authenticity and geographical origin of products |
-
2017
- 2017-01-22 CN CN201710045036.5A patent/CN106770856B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101199936A (en) * | 2007-11-06 | 2008-06-18 | 兰州大学 | Isophthalic acid and m-toluic acid catalyst preparation and method thereof |
| CN101327440A (en) * | 2008-06-27 | 2008-12-24 | 安徽理工大学 | Composite catalyst for producing hydrogen by methane steam reforming technology |
Non-Patent Citations (1)
| Title |
|---|
| 氢同位素在线分析用MnCl2\γ-Al2O3色谱填料的制备与性能;王晓英等;《分析化学（FENXI HUAXUE）研究报告》;20111031;第39卷(第10期);第1595-1596页第2节 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106770856A (en) | 2017-05-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106770856B (en) | A kind of chromatography column for being used to analyze hydrogen isotope mixed gas | |
| Brown et al. | Nucleosynthetic constraints on the mass of the heaviest supernovae | |
| CN105259291A (en) | Analysis method of fission gas | |
| CN105388225B (en) | UDPC analyzing detecting method in a kind of pharmaceutical preparation containing C14H25N4NaO11P2 | |
| Fujinaga | Electrolytic chromatography and coulometric detection with the column electrode | |
| CN106680407A (en) | Capillary chromatographic column for analyzing hydrogen isotope mixed gas | |
| CN105203655B (en) | The assay method of content astaxanthin in a kind of antarctic krill oil | |
| CN112946125B (en) | Apparatus and method for analyzing hydrogen fluoride in fluorine gas | |
| CN204389453U (en) | Nitrogen oxygen isotope measuring device of trace nitrate sample | |
| CN107261845A (en) | A kind of separation method of hydrogen isotope mixed gas | |
| Jones | Transfer reaction experiments with radioactive beams: from halos to the r-process | |
| CN104422729B (en) | A kind of method based on film Inlet Mass Spectrometry instrument analysis dissolved nitrogen isotopic content | |
| CN104914194B (en) | A method of with Determination of menthol in gas chromatograph detection Dementholized mint oil dripping pill | |
| CN108362783A (en) | A kind of detection method of 5 ingredients fingerprint of ginseng saponin F | |
| Jaison et al. | Direct determination of lanthanides in simulated irradiated thoria fuels using reversed-phase high-performance liquid chromatography | |
| Conde et al. | Behavior of the Pb–Li alloy impurities by ICP-MS | |
| Post et al. | Pharmacokinetics of N-desmethyldiazepam in healthy volunteers after single daily doses of dipotassium chlorazepate | |
| Acharya et al. | Analysis of SMELS and reference materials for validation of the k0-based internal monostandard NAA method using in-situ detection efficiency | |
| CN209640298U (en) | A kind of sulfur hexafluoride gas mixture mixing ratio chromatographic detection apparatus | |
| CN201622266U (en) | Double-transformation column methanator | |
| Herdzik et al. | Separation of gallium and indium isotopes by cation and anion exchange chromatography | |
| Junbo et al. | Quantitative analysis of oxygen, nitrogen, hydrogen and hydrogen deuteride in high-purity deuterium by gas chromatography | |
| CN106442797A (en) | Method for detecting fatty acid in food | |
| Stanciu et al. | Chemically modified glasses for analysis of hydrogen isotopes by gas-chromatography | |
| Barrado et al. | Towards the development of technical specifications for the production of lithium–lead alloys for the ITER HCLL TMB |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20180522 Termination date: 20190122 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |