CN2226768Y - Aluminium trioxide filling capillary chromatographic column - Google Patents

Aluminium trioxide filling capillary chromatographic column Download PDF

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Publication number
CN2226768Y
CN2226768Y CN 94211913 CN94211913U CN2226768Y CN 2226768 Y CN2226768 Y CN 2226768Y CN 94211913 CN94211913 CN 94211913 CN 94211913 U CN94211913 U CN 94211913U CN 2226768 Y CN2226768 Y CN 2226768Y
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CN
China
Prior art keywords
capillary
column
chromatographic column
glass
aluminium trioxide
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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
Application number
CN 94211913
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Chinese (zh)
Inventor
赵让海
许岳兴
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sinopec Yangzi Petrochemical Co Ltd
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Sinopec Yangzi Petrochemical Co Ltd
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Priority to CN 94211913 priority Critical patent/CN2226768Y/en
Application granted granted Critical
Publication of CN2226768Y publication Critical patent/CN2226768Y/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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  • Treatment Of Liquids With Adsorbents In General (AREA)

Abstract

The utility model provides an aluminium trioxide filling capillary chromatographic column. A thick-wall glass tube can be filled by the fine particle of aluminium trioxide; can be pulled to a molding by adding glass softening point. Because the processing method of the filler aluminium trioxide adopts sylvite infiltration and section heating activation, the short chromatographic column can be used for achieving high separating power to the low carbon hydrocarbon. The utility model has the advantages of good stability and long service life; in addition, the both ends of the capillary column of filling glass are connected with a flexible quartz capillary respectively, which enhances the operability of the glass capillary column.

Description

A kind of capillary chromatographic column filled with aluminum trioxide
The utility model relates to a kind of capillary chromatographic column filled with aluminum trioxide, belongs to the chromatographic resolution field in the analytical chemistry field.
Gas chromatograph is the key instrument during lighter hydrocarbons are analyzed, and chromatographic column is to play the critical component of centrifugation in this instrument.The technology of preparing of chromatographic column is related to the quality of column performance and separating power thereof.The column type of the general chromatographic column of using has 1. packed column in the analysis of lower carbon number hydrocarbons, 2. 3. porous layer open tubular column of packed capillary column (comprising little post of filling out), and the material of use has tubing such as metal, quartz, glass, nylon.
Packed column: in early days to the analysis of lower carbon number hydrocarbons what is called " distribution type " packed column [P.K.Kuchal.etal that is coated with the stain stationary phase commonly used, Chromatographia 8641 (1975) blue fossil oil rubber petroleum gas workshop " petrochemical technology " 3.4.6 (1973)], the advantage of these posts is that column capacity is big, to chromatographic sampling system, detection system and operating personnel require lower, are Industry Control analysis column types commonly used.The shortcoming of this class post is a poor permeability, and the column length of use is restricted, and generally is no more than 10m, and the separating power of post is lower, can not analyze the material composition assorted than the summer, and needs to press before the higher post and lower column temperature (room temperature or 0 ℃ ice-water bath).If room temperature changes, the degree of separation of each component of sample can change, and it is relatively poor to analyze data repeatability.
Al 2O 3Wall is coated with open tubular column: its advantage is the good penetrability of post, can make very longly (tens meters to rice up to a hundred).Total number of effective plate of post is very high, and separating power is also stronger.But this class post is attached to the Al on the tube wall 2O 3Coating comes off easily, the poor repeatability (cost raising) of system post.And the column capacity of open tubular column is low, and the dead volume of instrument air-channel system is had relatively high expectations, and operation easier is also big.
Packed capillary column: performance Jie gives packed column and wall is coated with between the post, imitates height than the post of packed column, and the capacity that is coated with post than wall is big, and the system column method is simple, good reproducibility, and the post cost is low.The domestic people of having develops a kind of packed capillary column (Yang Haiying " chromatogram " 3 (1987) 71) that inner core arranged has higher permeability and gratifying post to imitate, but this post is still longer analysis time, in addition owing to contain inner core in the middle of the pillar, therefore, this post and instrument to be connected versatility poor.
The purpose of this utility model is to overcome the shortcoming that wall is coated with post and conventional filled capillary pipe, proposes a kind of short but can analyze C quickly and efficiently 1-C 7The novel packed capillary column of lower carbon number hydrocarbons.
The purpose of this utility model is achieved in that
1. choose about long 1m, external diameter 6-7mm, the heavy wall glass tube of internal diameter 2-3mm cleans inwall, drying successively with washing lotion, distilled water;
2. take by weighing 30gAl 2O 3(chromatography usefulness, 180-200 order) soaks half an hour with the KCl solution of 30ml 1.5mol, after the filtration, activates 4h down at 380-420 ℃; 490-520 ℃ activates 5h down, relays in exsiccator;
3. after cooling, in the 1. described glass tube of packing into, on the kapillary drawing machine with 1: 100 drawing than being drawn into the filling glass capillary column that internal diameter is 0.45-0.5mm;
4. get its Len req (1-6m is long), 5mmAl is removed at the post two ends 2O 3Particle, the glass fiber a little (accounting for the 2mm pipe range) that the silanization of packing into is handled respectively inserts one section then greater than the long flexible quartz capillary of 50mm, with resistant to elevated temperatures silicone rubber seal junction.
The Al of moulding 2O 3Capillary chromatographic column filled structure as shown in Figure 1, among the figure: the 1st, glass is capillary chromatographic column filled; The 2nd, Al 2O 3Particle; The 3rd, glass fiber; The 4th, silicon rubber; The 5th, flexible quartz capillary.
The utility model is because to Al 2O 3Adopt soluble potassium salt to soak into and the segmentation methods of heating treatment, and be connected with flexible quartz ampoule, make its adsorbability just right, therefore produced following effect lower carbon number hydrocarbons at the glass column two ends:
1. strengthened separating power, used short post, in the short time, can make C such as oil gas unsaturated hydrocarbon 1-C 7Hydrocarbon is well separated, and uses column temperature higher (exceeding room temperature more than 30 ℃), is convenient to control.
2. on any one gas chromatograph that has a capillary system, all can use, because the two ends of post have flexible quartz ampoule, increase the elasticity of glass capillary column to a certain extent simultaneously, be convenient to install dismounting.
3. column capacity is big, and method for making is simple, good reproducibility, and cost is low.
The concrete structure of utility model is provided by following embodiment and accompanying drawing thereof.
Fig. 1 is Al of the present utility model 2O 3Capillary chromatographic column filled structural drawing.
Describe details and working condition in detail below in conjunction with Fig. 1 according to the concrete device that the utility model proposes.
Al 2O 3The preparation of filling glass capillary column (1):
1. choose long 1m, outer path length 6-7mm, the heavy wall glass tube of internal diameter 2-3mm cleans inwall, drying successively with washing lotion, distilled water.
2. take by weighing 30gAl 2O 3(2) (chromatography usefulness, 180-200 order) soaks half an hour with the KCL solution of 30ml 1.5N, after the filtration, activates 4h down at 380-420 ℃; 490-520 ℃ activates 5h down, relays in exsiccator;
3. after cooling, in the 1. described glass tube of packing into, on the day GDM-IB type drawing machine produced of island proper Tianjin company with 1: 100 drawing than being drawn into the filling glass capillary column (1) that internal diameter is 0.45-0.5mm;
4. get its Len req (1-6m is long), 5mmAl is removed at the post two ends 2O 3Particle (2), the glass fiber (3) a little (accounting for the 2mm pipe range) of packing into and handling through silanization, it is long respectively to insert a segment length 20-30cm then, and the flexible quartz capillary (5) of internal diameter 0.32mm is with resistant to elevated temperatures silicon rubber (4) place that is tightly connected.

Claims (3)

1. AL 2O 3Capillary chromatographic column filled, by AL 2O 3Fine grained is filled the heavy wall glass capillary, draws moulding through high-temperature fusion, and it is characterized in that: the two ends of kapillary 1 connect flexible quartz capillary 5 respectively.
2. the AL that asks according to claim 1 2O 3Capillary chromatographic column filled, it is characterized in that: the glass fiber of handling through silanization that accounts for the 2mm pipe range 3 also is housed at the two ends of post.
3. AL according to claim 2 2O 3Capillary chromatographic column filled, it is characterized in that: the length of flexible quartz capillary 5 is 20-30cm, with resistant to elevated temperatures silicon rubber 4 place that is tightly connected.
CN 94211913 1994-05-12 1994-05-12 Aluminium trioxide filling capillary chromatographic column Expired - Fee Related CN2226768Y (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 94211913 CN2226768Y (en) 1994-05-12 1994-05-12 Aluminium trioxide filling capillary chromatographic column

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 94211913 CN2226768Y (en) 1994-05-12 1994-05-12 Aluminium trioxide filling capillary chromatographic column

Publications (1)

Publication Number Publication Date
CN2226768Y true CN2226768Y (en) 1996-05-08

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Family Applications (1)

Application Number Title Priority Date Filing Date
CN 94211913 Expired - Fee Related CN2226768Y (en) 1994-05-12 1994-05-12 Aluminium trioxide filling capillary chromatographic column

Country Status (1)

Country Link
CN (1) CN2226768Y (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101949909A (en) * 2010-08-19 2011-01-19 中国科学院兰州地质研究所 Connector for connecting capillary column with ceramic tube in individual hydrocarbon test system

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101949909A (en) * 2010-08-19 2011-01-19 中国科学院兰州地质研究所 Connector for connecting capillary column with ceramic tube in individual hydrocarbon test system

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