CN106390520B - The separation method of Various Groups In Crude Oil analysis chromatographic column and Various Groups In Crude Oil - Google Patents
The separation method of Various Groups In Crude Oil analysis chromatographic column and Various Groups In Crude Oil Download PDFInfo
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- CN106390520B CN106390520B CN201611022748.7A CN201611022748A CN106390520B CN 106390520 B CN106390520 B CN 106390520B CN 201611022748 A CN201611022748 A CN 201611022748A CN 106390520 B CN106390520 B CN 106390520B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/22—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the construction of the column
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/20—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the sorbent material
- B01D15/206—Packing or coating
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Abstract
The present invention proposes the separation method of a kind of Various Groups In Crude Oil analysis chromatographic column and Various Groups In Crude Oil, it is related to Various Groups In Crude Oil analysis experimental field, the chromatographic column includes the upper funnel of sequence setting from top to bottom, alumina column and chromatographic silica gel post, between upper funnel and alumina column, it is removedly tightly connected between alumina column and chromatographic silica gel post, upper funnel, alumina column and chromatographic silica gel post all have cavity up and down, upper funnel is hollow back taper stage body, alumina column and chromatographic silica gel post are hollow column, the internal diameter of chromatographic silica gel post is greater than the internal diameter of alumina column.The chromatographic column above-mentioned can use different inner diameters for different fillers, so that the aluminium oxide and chromatographic silica gel as adsorbent have different cross-sectional area and height, ensure that aluminium oxide and chromatographic silica gel can reach optimal separating effect.
Description
Technical field
The present invention relates to Various Groups In Crude Oils to analyze experimental field, in particular to Various Groups In Crude Oil analysis chromatographic column and crude oil
The separation method of Group Component.
Background technique
Various Groups In Crude Oil is analyzed at present, it mainly " can in 2008 rock of SY/T5119-according to existing separation standard
Molten organic matter and Various Groups In Crude Oil analysis " in chromatographic column method carry out concrete operations.
Using column chromatography pair in standard " soluble organic and Various Groups In Crude Oil analysis in 2008 rock of SY/T5119-"
Crude oil carries out Group component separation, is divided into four kinds of saturated hydrocarbons, aromatic hydrocarbon, resin and asphalt Group Components.It is filled first using n-hexane
Divide dissolution water removal removal of impurities crude oil, then manually the short neck funnel of filling absorbent cotton is filtered and collects filtrate；Wherein, asphalitine
Because being separated insoluble in n-hexane, asphalitine is obtained with chloroform absorbent cotton later；And the filtrate collected then uses layer
Analysis column separate and then obtains saturated hydrocarbons, aromatic hydrocarbon and colloid.
Process using chromatography post separation saturated hydrocarbons, aromatic hydrocarbon and colloid is as follows: being 400mm~500mm, internal diameter in length
It is sequentially filled 2g aluminium oxide in the long neck funnel of 7mm~10mm and chromatographic column is made in 3g chromatographic silica gel；Chromatographic column is added in filtrate,
Saturated hydrocarbons is eluted with n-hexane again, elutes aromatic hydrocarbon with methylene chloride and n-hexane mixed solvent (volume ratio 2:1), is used
The sequence of chloroform elutes colloid after first dehydrated alcohol；The weighing bottle for undertaking above-mentioned four kinds of Group Components is finally respectively dried, counts
It calculates of poor quality and then obtains Group Component.
In application chromatography post separation saturated hydrocarbons, aromatic hydrocarbon and during colloid, filling alumina needed for chromatographic column and
The weighing of chromatographic silica gel is more time-consuming；Meanwhile aluminium oxide and chromatographic silica gel are led because directly contacting in filled chromatographic column
The crude petroleum materials of contact surface are caused to be not easy to be leached out, and the aluminium oxide of joint and chromatographic silica gel are difficult after the completion of experiment
It is collected separately and is recycled.
In addition, in above-mentioned separation method, to the aluminium oxide and chromatographic silica gel used as adsorbent its to crude oil race
The adsorption capacity of different component is different, and the speed and required time when eluent flows through aluminium oxide and chromatographic silica gel are also
Different, the elution power for eluting aluminium oxide and chromatographic silica gel Crude Oil Group Component is also different, if to reach optimal point
From effect, quality, granular size and the volume profiles (cross-sectional area and height) of required aluminium oxide and chromatographic silica gel are also answered
This is different.But currently, the quality and granular size that are only capable of to aluminium oxide and chromatographic silica gel carry out preferred, the prior art
In, aluminium oxide and chromatographic silica gel are sequentially filled in long neck funnel and form chromatographic column, and cross-sectional area having the same, this is transversal
Area cannot make aluminium oxide have optimal separating effect, and chromatographic silica gel can not be made to reach optimal separating effect；Meanwhile
In the prior art, it is longer to be sequentially filled chromatographic column its length formed in long neck funnel for aluminium oxide and chromatographic silica gel, saturated hydrocarbons,
Aromatic hydrocarbon and colloid separation process time-consuming are also longer.
It can thus be seen that there are many defects for the separation method of above-mentioned Various Groups In Crude Oil, therefore, it is necessary to above-mentioned original
The separation method of oily Group Component and experimental tool used are further improved.
Summary of the invention
The object of the present invention is to provide a kind of Various Groups In Crude Oil analysis chromatographic columns, can use for different fillers different
Internal diameter so that as adsorbent aluminium oxide and chromatographic silica gel have different cross-sectional area and height, ensure that aluminium oxide and
Chromatographic silica gel can reach optimal separating effect.
It is another object of the present invention to propose a kind of separation method of Various Groups In Crude Oil, the oxygen as adsorbent is enabled to
Changing aluminium and chromatographic silica gel has different cross-sectional area and height, ensure that aluminium oxide and chromatographic silica gel can reach optimal point
From effect.
In order to achieve the above objectives, the present invention proposes a kind of Various Groups In Crude Oil analysis chromatographic column, wherein the chromatographic column packet
Include upper funnel, alumina column and the chromatographic silica gel post of sequence setting from top to bottom, the upper funnel and the alumina column
Between, be removedly tightly connected between the alumina column and the chromatographic silica gel post, the upper funnel, the oxidation
Aluminium column and the chromatographic silica gel post all have cavity up and down, and the upper funnel is hollow back taper stage body, the oxygen
Change aluminium column and the chromatographic silica gel post is hollow column, the internal diameter of the chromatographic silica gel post is greater than the alumina column
Internal diameter.
Various Groups In Crude Oil analysis chromatographic column as described above, wherein the bottom end of the alumina column is downwardly extending
There is first connecting portion, the top of the chromatographic silica gel post, which upwardly extends, is sequentially formed with wide diameter portion and second connecting portion, and described
One interconnecting piece and the second connecting portion are hollow cylindrical body, and the first connecting portion outer wall is equipped with external screw thread, described
Second connecting portion inner wall is equipped with internal screw thread, the external screw thread and internal screw thread intermeshing, the inner wall of the wide diameter portion
Internal diameter for the conical surface of flaring from top to bottom, its bottom end of wide diameter portion is identical as the internal diameter of the chromatographic silica gel post.
Various Groups In Crude Oil analysis chromatographic column as described above, wherein the bottom end of the upper funnel is downwardly extending
Some third interconnecting pieces, the top of the alumina column, which upwardly extends, is sequentially formed with the first reducing diameter part and the 4th interconnecting piece, institute
Stating third interconnecting piece and the 4th interconnecting piece is hollow cylindrical body, and the third interconnecting piece outer wall is equipped with external screw thread,
The 4th interconnecting piece inner wall is equipped with internal screw thread, the external screw thread and internal screw thread intermeshing, first reducing diameter part
Inner wall be the from top to bottom tapered conical surface, the internal diameter phase of the diameter and the alumina column of its bottom end of first reducing diameter part
Together.
Various Groups In Crude Oil analysis chromatographic column as described above, wherein the bottom end of the chromatographic silica gel post extend downwardly according to
It is secondary to be formed with the second reducing diameter part and thin footpath outlet portion, the inner wall of second reducing diameter part be for the conical surface tapered from top to bottom,
The top internal diameter of second reducing diameter part is identical as the internal diameter of the chromatographic silica gel post, and the inner wall of the thin footpath outlet portion is column
Face.
Various Groups In Crude Oil analysis chromatographic column as described above, wherein the internal diameter of the alumina column is 6mm.
Various Groups In Crude Oil analysis chromatographic column as described above, wherein the internal diameter of the chromatographic silica gel post is 16mm.
Various Groups In Crude Oil analysis chromatographic column as described above, wherein the bottom end of the alumina column is provided with first
Filter, first filter are equipped with multiple first filter hole, and the aperture of first filter hole is 0.053mm；In the layer
The bottom end for analysing silicagel column is equipped with the second filter, and second filter is equipped with multiple second filter hole, second filter hole
Aperture is 0.09mm.Various Groups In Crude Oil analysis chromatographic column as described above, wherein the externally threaded surface and the interior spiral shell
The surface of line is frosting.
Various Groups In Crude Oil analysis chromatographic column as described above, wherein on the alumina column and the chromatographic silica gel post
It is equipped with graduation mark.
The present invention also proposes a kind of separation method of Various Groups In Crude Oil, wherein the separation method uses as described above
Various Groups In Crude Oil analysis chromatographic column, the separation method include:
Step A weighs crude oil, and the crude oil is completely dissolved to form suspension with n-hexane；
Step B is filtered to obtain filtrate using the funnel for having clogged absorbent cotton to the suspension；
Step C obtains asphalitine using the filtered absorbent cotton is completed in step B described in chloroform；
Step D fills aluminium oxide into the alumina column of the chromatographic column, to the chromatography silicon of the chromatographic column
Chromatographic silica gel is filled in glue, and the be linked in sequence upper funnel, alumina column and chromatographic silica gel post, assemble the chromatographic column；
Step E takes filtrate obtained in step B, is added into the upper funnel of the chromatographic column, successively utilizes
N-hexane, methylene chloride and n-hexane mixed solvent, dehydrated alcohol and chloroform elute the chromatographic column, realize saturation
The separation of hydrocarbon, aromatic hydrocarbon and colloid；
Step F removes the alumina column and the chromatographic silica gel post, carries out to the aluminium oxide and the chromatographic silica gel
Recycling.
Compared with prior art, the invention has the characteristics that and advantage:
The Various Groups In Crude Oil analysis proposed by the present invention separation method of chromatographic column and Various Groups In Crude Oil, using can dismantle
The alumina column and chromatographic silica gel post of connection, and for the aluminium oxide density characteristic different with chromatographic silica gel, alumina column and
Chromatographic silica gel post uses different internal diameters, different internal diameters is used for different fillers, so that the aluminium oxide as adsorbent
There is different cross-sectional area and height with chromatographic silica gel, ensure that aluminium oxide and chromatographic silica gel can reach optimal separation effect
Fruit.
The Various Groups In Crude Oil analysis proposed by the present invention separation method of chromatographic column and Various Groups In Crude Oil, using can dismantle
The alumina column and chromatographic silica gel post of connection are separately filled with aluminium oxide and chromatography silicon in alumina column and chromatographic silica gel post
Glue ensure that aluminium oxide and chromatographic silica gel are in the state being separated from each other always, avoid the direct of aluminium oxide and chromatographic silica gel
Contact also avoids the crude petroleum materials residual at aluminium oxide and chromatographic silica gel contact surface, not only improves separating effect, but also make
Aluminium oxide and chromatographic silica gel can be recycled individually and be recycled again, be conducive to environmental protection again while reducing cost.
Detailed description of the invention
Attached drawing described here is only used for task of explanation, and is not intended to limit model disclosed by the invention in any way
It encloses.In addition, shape and proportional sizes of each component in figure etc. are only schematical, it is used to help the understanding of the present invention, and
It is not the specific shape and proportional sizes for limiting each component of the present invention.Those skilled in the art under the teachings of the present invention, can
Implement the present invention to select various possible shapes and proportional sizes as the case may be.
Fig. 1 is the structural schematic diagram that chromatographic column is used in Various Groups In Crude Oil of the present invention analysis；
Fig. 2 is the assembling schematic diagram that chromatographic column is used in Various Groups In Crude Oil of the present invention analysis.
Description of symbols:
100 chromatographic columns；1 upper funnel；
2 alumina columns；3 chromatographic silica gel posts；
4 first connecting portions；5 wide diameter portions；
6 second connecting portions；7 third interconnecting pieces；
8 first reducing diameter parts；9 the 4th interconnecting pieces；
10 second reducing diameter parts；11 thin footpath outlet portions；
12 first filters；13 second filters；
21 aluminium oxide recommend graduation mark；22 aluminium oxide recommend graduation mark；
23 subsidiary scale marks；31 chromatographic silica gels recommend graduation mark；
32 chromatographic silica gels recommend graduation mark；33 subsidiary scale marks.
Specific embodiment
With reference to the drawings and the description of the specific embodiments of the present invention, details of the invention can clearly be understood.But
It is the specific embodiment of invention described herein, purpose for explaining only the invention, and cannot understand in any way
At being limitation of the present invention.Under the teachings of the present invention, technical staff is contemplated that based on any possible change of the invention
Shape, these are regarded as belonging to the scope of the present invention.
Various Groups In Crude Oil analysis chromatographic column and Various Groups In Crude Oil separation method proposed by the present invention are for existing separation
The concrete operations of chromatographic column method in standard " in 2008 rock of SY/T5119-soluble organic and Various Groups In Crude Oil analysis " and mention
Out.Now in conjunction with standard " soluble organic and Various Groups In Crude Oil analysis in 2008 rock of SY/T5119-" to proposed by the present invention
The separation method of Various Groups In Crude Oil analysis chromatographic column and Various Groups In Crude Oil is described further.
Please refer to Fig. 1, Fig. 2, wherein Fig. 1 is the structural schematic diagram that chromatographic column is used in Various Groups In Crude Oil of the present invention analysis；Fig. 2
For the assembling schematic diagram of Various Groups In Crude Oil analysis chromatographic column of the present invention.As shown in Figure 1 and Figure 2, crude oil race proposed by the present invention group
Divide analysis upper funnel 1, alumina column 2 and the chromatographic silica gel post 3 that chromatographic column 100 includes that from top to bottom sequence is tightly connected,
Wherein, it is removedly connected between upper funnel 1 and alumina column 2, between alumina column 2 and chromatographic silica gel post 3, top leakage
Bucket 1, alumina column 2 and chromatographic silica gel post 3 all have cavity up and down, and upper funnel 1 is hollow back taper stage body, oxidation
Aluminium column 2 and chromatographic silica gel post 3 are hollow column, and the internal diameter of chromatographic silica gel post 3 is greater than the internal diameter of alumina column 2.
Various Groups In Crude Oil analysis chromatographic column 100 proposed by the present invention, using the alumina column 2 and layer of energy dismantling connection
Silicagel column 3, and the density characteristic different with chromatographic silica gel for aluminium oxide are analysed, alumina column 2 and chromatographic silica gel post 3 use
Different internal diameters, the above-mentioned structure that different inner diameters are used for different fillers, so that aluminium oxide and chromatography silicon as adsorbent
Glue is provided with different cross-sectional area and height, ensure that aluminium oxide and chromatographic silica gel can reach optimal separating effect.
Various Groups In Crude Oil analysis chromatographic column 100 proposed by the present invention, using the alumina column 2 and layer of energy dismantling connection
Analyse silicagel column 3, be separately filled with aluminium oxide and chromatographic silica gel in alumina column 2 and chromatographic silica gel post 3, ensure that aluminium oxide and
Chromatographic silica gel is in the state being separated from each other always, avoids the direct contact of aluminium oxide and chromatographic silica gel, also avoids oxygen
Change the crude petroleum materials residual at aluminium and chromatographic silica gel contact surface, both improves separating effect；Meanwhile and making aluminium oxide and chromatography
Silica gel can be recycled individually and be recycled again, be conducive to environmental protection again while reducing cost.
In an optional example of the invention, as shown in Figure 1 and Figure 2, the bottom end of alumina column 2 is downwardly extending the
One interconnecting piece 4, the top of chromatographic silica gel post 3, which upwardly extends, is formed with wide diameter portion 5 and second connecting portion 6, first connecting portion 4 and
Two interconnecting pieces 6 are hollow cylindrical body, and 4 outer wall of first connecting portion is equipped with external screw thread, and 6 inner wall of second connecting portion is equipped with interior
Screw thread, external screw thread and internal screw thread intermeshing, the inner wall of wide diameter portion 5 are the conical surface of flaring from top to bottom, its bottom end of wide diameter portion 5
Internal diameter it is identical as the internal diameter of chromatographic silica gel post 3.Relative to traditional chromatographic column, wide diameter portion 5 and chromatographic silica gel post 3 are increased and are cut
Area and reduce length, the sectional area increased is more suitable for the granular size of chromatographic silica gel, improve chromatographic silica gel point
From effect, and reduced length also further reduces time of the rinse solvent by chromatographic silica gel, when finally having saved separation
Between.
In an optional example of the invention, as shown in Figure 1 and Figure 2, the bottom end of upper funnel 1 has been downwardly extending
Third interconnecting piece 7, the top of alumina column 2, which upwardly extends, is sequentially formed with the first reducing diameter part 8 and the 4th interconnecting piece 9,
Three interconnecting pieces 7 and the 4th interconnecting piece 9 are hollow cylindrical body, and 7 outer wall of third interconnecting piece is equipped with external screw thread, the 4th interconnecting piece
9 inner walls are equipped with internal screw thread, external screw thread and internal screw thread intermeshing, and the inner wall of the first reducing diameter part 8 is tapered from top to bottom
The diameter of the conical surface, 8 its bottom end of the first reducing diameter part is identical as the internal diameter of alumina column 2.
In an optional example of the invention, as shown in Figure 1 and Figure 2, the bottom end of chromatographic silica gel post 3 is extended downwardly successively
It is formed with the second reducing diameter part 10 and thin footpath outlet portion 11, the inner wall of the second reducing diameter part 10 is the conical surface tapered from top to bottom, the
The top internal diameter of two reducing diameter parts 10 is identical as the internal diameter of chromatographic silica gel post 3, and the inner wall of thin footpath outlet portion 11 is cylinder.Thin footpath goes out
Oral area 11 has certain length, can be achieved to block the liquid of outlet in the case where chromatography process low discharge, reduces air shadow
It rings.
In the identical situation of flow undergauge and it is expanding will lead to flow field change, cause to shake, reinforce flushing effect, reduce object
Matter residual, error are smaller；And transiens undergauge and arteriopathy expanding design further reduce circular bead surface type undergauge and expanding
The Group Component substance residual that may cause.
In an optional example of the invention, as shown in Figure 1 and Figure 2, the internal diameter of alumina column 2 is 6mm.With it is traditional
Chromatographic column (internal diameter is 7mm~10mm) is compared, and is reduced the cross-sectional area of aluminium oxide, is increased the length of aluminium oxide, laboratory
Test result shows that separating effect is best when the cross-sectional area of aluminium oxide is 6mm.
In an optional example of the invention, as shown in Figure 1 and Figure 2, the internal diameter of chromatographic silica gel post 3 is 16mm, with tradition
Chromatographic column (internal diameter be 7mm~10mm) compare, when the cross-sectional area of chromatographic silica gel is 16mm, separating effect is best.Together
When, due to increasing the internal diameter of chromatographic silica gel post 3, in the case where the mass conservation of required chromatographic silica gel, reduce chromatography silicon
The height of glue also just correspondingly reduces the height of entire chromatographic column, has saved disengaging time.
In an optional example of the invention, as shown in Figure 1 and Figure 2, the bottom end of alumina column 2 is provided with the first filter
First 12, it is equipped with the second filter 13 in the bottom end of chromatographic silica gel post 3, the first filter 12 is equipped with multiple first filter hole, the second filter
First 13 are equipped with multiple second filter hole, and the first filter 12 and the second filter 13 are that (term is called sand to glass sand filter again
Core filter plate), it is allowed to not fall and can guarantee that rinse solvent can pass through to carry filler.The lateral wall of filter 12 with
The inner wall of alumina column 2 or the inner wall plane-plane contact of lower chamber body 122 are simultaneously sealedly and fixedly connected；The lateral wall and chromatography of filter 13
The inner wall of silicagel column 3 or the inner wall plane-plane contact of lower chamber body 122 are simultaneously sealedly and fixedly connected.Specifically, according to aluminium oxide and layer
The difference of the particle diameter of silica gel is analysed, the aperture of the first filter hole is 0.053mm；The aperture of second filter hole is 0.09mm.
In an optional example of the invention, the externally threaded surface of 100 its threaded connection place of chromatographic column and internal screw thread
Surface be frosting, further ensure between upper funnel 1 and alumina column 2, alumina column 2 and chromatographic silica gel post 3
Between sealed connection sealing effect.
In an optional example of the invention, as shown in Figure 1 and Figure 2, it is all provided on alumina column 2 and chromatographic silica gel post 3
There is graduation mark.Wherein, according in application standard " soluble organic and Various Groups In Crude Oil are analyzed in 2008 rock of SY/T5119-"
Regulation, the usage amount of aluminium oxide is 2g, and the particle diameter of aluminium oxide is 100 mesh~200 mesh, marks two on alumina column 2
Aluminium oxide recommends graduation mark 21,22, respectively corresponds the aluminium oxide of two kinds of partial sizes (two kinds of partial sizes are respectively 100 mesh and 200 mesh),
Meanwhile finely tuning for convenience, there are also subsidiary scale marks 23 around aluminium oxide recommendation graduation mark 21,22, according to practical feelings
Condition adjusts packing volume；According in application standard " soluble organic and Various Groups In Crude Oil analysis in 2008 rock of SY/T5119-"
Regulation, the usage amount of chromatographic silica gel is 3g, and the particle diameter of chromatographic silica gel is 80 mesh~100 mesh, in 3 subscript of chromatographic silica gel post
Out two chromatographic silica gels recommend graduation mark 31,32, respectively correspond the layer of two kinds of partial sizes (two kinds of partial sizes are respectively 80 mesh and 100 mesh)
Silica gel is analysed, meanwhile, it finely tunes for convenience, there are also subsidiary scale marks 33 around chromatographic silica gel recommendation graduation mark 31,32 with root
Packing volume is adjusted according to actual conditions.In this way, the step of filling aluminium oxide and when chromatographic silica gel, weighing can be saved, according to
The granular size of used aluminium oxide and chromatographic silica gel, determines its corresponding graduation mark, when filling, aluminium oxide and chromatography silicon
Glue reaches corresponding graduation mark, simple and convenient, saves the time.
The invention also provides a kind of Various Groups In Crude Oil separation methods, are analyzed and are used using Various Groups In Crude Oil proposed by the present invention
Chromatographic column 100, specifically, the separation method includes:
Step A weighs crude oil, and crude oil is completely dissolved to form suspension with n-hexane；
Step B is filtered suspension to obtain filtrate using the funnel for having clogged absorbent cotton；
Step C obtains asphalitine using filtered absorbent cotton is completed in chloroform step B；
Step D fills the aluminium oxide of specified amount into the alumina column 2 of chromatographic column 100, to the chromatography silicon of chromatographic column 100
The chromatographic silica gel of specified amount, and the upper funnel 1 that is linked in sequence, alumina column 2 and chromatographic silica gel post 3, assembled layers are filled in rubber column gel column 3
Analyse column 100；Specifically, the quality for filling aluminium oxide into alumina column 2 is 2g, the diameter of alumina particle is 100 mesh~200
Mesh；Fill chromatographic silica gel into chromatographic silica gel post 3, the quality of chromatographic silica gel is 3g, the particle diameter of chromatographic silica gel be 80 mesh~
100 mesh.
Step E takes filtrate obtained in step B, is added into the upper funnel 1 of chromatographic column 100, successively using just oneself
Alkane, methylene chloride and n-hexane mixed solvent, dehydrated alcohol and chloroform elute the chromatographic column, realize saturated hydrocarbons, virtue
The separation of fragrant hydrocarbon and colloid；Specifically, saturated hydrocarbons is eluted with n-hexane, with methylene chloride and n-hexane mixed solvent (volume
Than eluting aromatic hydrocarbon for 2:1), colloid is eluted with the sequence of chloroform after first dehydrated alcohol.Concrete operations about this step
It is required that please referring to the regulation in " soluble organic and Various Groups In Crude Oil analysis in 2008 rock of SY/T5119-".
Step F removes alumina column 2 and chromatographic silica gel post 3, recycles to aluminium oxide and chromatographic silica gel.It can distinguish
Liquid scrub is added into alumina column 2 and chromatographic silica gel post 3 by the upper end of alumina column 2 and the upper end of chromatographic silica gel post 3
The mode poured out again, can also be passed through liquid from the lower end of the lower end of alumina column 2 and chromatographic silica gel post 3 respectively distinguishes liquid
By the first filter 12 and the second filter 13 again from the mode that chromatographic column filler is taken out of to the other end.
Various Groups In Crude Oil separation method proposed by the present invention can also include step G, respectively to four kinds of separating obtained groups
(four kinds of components are respectively asphalitine, saturated hydrocarbons, aromatic hydrocarbon and colloid) is divided to be dried and weighed, calculating is of poor quality to obtain race's group
Point.
For explaining in detail for the respective embodiments described above, purpose, which is only that, explains the present invention, in order to be able to
More fully understand the present invention, still, these descriptions cannot with any explanation at being limitation of the present invention, in particular,
Each feature described in different embodiments can also mutual any combination, so that other embodiments are formed, in addition to having
Opposite description is specified, these features should be understood to can be applied in any one embodiment, and be not limited merely to
Described embodiment.
Claims (10)
1. a kind of Various Groups In Crude Oil analysis chromatographic column, which is characterized in that the chromatographic column includes sequence setting from top to bottom
Upper funnel, alumina column and chromatographic silica gel post, between the upper funnel and the alumina column, the alumina column and institute
It states and is removedly tightly connected between chromatographic silica gel post, the upper funnel, the alumina column and the chromatographic silica gel post
Cavity up and down is all had, the upper funnel is hollow back taper stage body, the alumina column and the chromatographic silica gel
Column is hollow column, and the internal diameter of the chromatographic silica gel post is greater than the internal diameter of the alumina column.
2. Various Groups In Crude Oil as described in claim 1 analysis chromatographic column, which is characterized in that the bottom end of the alumina column to
Lower extension is formed with first connecting portion, and the top of the chromatographic silica gel post, which upwardly extends, is sequentially formed with wide diameter portion and the second connection
Portion, the first connecting portion and the second connecting portion are hollow cylindrical body, and the first connecting portion outer wall is equipped with outer
Screw thread, the second connecting portion inner wall are equipped with internal screw thread, the external screw thread and internal screw thread intermeshing, the wide diameter portion
Inner wall be from top to bottom flaring the conical surface, the internal diameter and the internal diameter phase of the chromatographic silica gel post of its bottom end of wide diameter portion
Together.
3. Various Groups In Crude Oil as described in claim 1 analysis chromatographic column, which is characterized in that the bottom end of the upper funnel to
Lower extension is formed with third interconnecting piece, and the top of the alumina column, which upwardly extends, is sequentially formed with the first reducing diameter part and the 4th company
Socket part, the third interconnecting piece and the 4th interconnecting piece are hollow cylindrical body, and the third interconnecting piece outer wall is equipped with
External screw thread, the 4th interconnecting piece inner wall are equipped with internal screw thread, and the external screw thread and the internal screw thread are intermeshed, and described first
The inner wall of reducing diameter part is the conical surface tapered from top to bottom, diameter and the alumina column of its bottom end of first reducing diameter part
Internal diameter is identical.
4. Various Groups In Crude Oil analysis chromatographic column as described in claim 1, which is characterized in that the bottom end of the chromatographic silica gel post
It extends downwardly and is sequentially formed with the second reducing diameter part and thin footpath outlet portion, the inner wall of second reducing diameter part is tapered from top to bottom
The conical surface, the top internal diameter of second reducing diameter part is identical as the internal diameter of the chromatographic silica gel post, the thin footpath outlet portion it is interior
Wall surface is cylinder.
5. the Various Groups In Crude Oil analysis chromatographic column as described in any one of Claims 1-4, which is characterized in that the oxygen
The internal diameter for changing aluminium column is 6mm.
6. the Various Groups In Crude Oil analysis chromatographic column as described in any one of Claims 1-4, which is characterized in that the layer
The internal diameter for analysing silicagel column is 16mm.
7. the Various Groups In Crude Oil analysis chromatographic column as described in any one of Claims 1-4, which is characterized in that described
The bottom end of alumina column is provided with the first filter, and first filter is equipped with multiple first filter hole, first filter hole
Aperture be 0.053mm；It is equipped with the second filter in the bottom end of the chromatographic silica gel post, second filter is equipped with multiple second
Filter hole, the aperture of second filter hole are 0.09mm.
8. Various Groups In Crude Oil analysis chromatographic column as claimed in claim 2 or claim 3, which is characterized in that the externally threaded surface
Surface with the internal screw thread is frosting.
9. Various Groups In Crude Oil analysis chromatographic column as described in claim 1, which is characterized in that the alumina column and the layer
Graduation mark is equipped on analysis silicagel column.
10. a kind of separation method of Various Groups In Crude Oil, which is characterized in that the separation method is used as appointed in claim 1 to 9
The analysis chromatographic column of Various Groups In Crude Oil described in meaning one, the separation method include:
Step A weighs crude oil, and the crude oil is completely dissolved to form suspension with n-hexane；
Step B is filtered to obtain filtrate using the funnel for having clogged absorbent cotton to the suspension；
Step C obtains asphalitine using the filtered absorbent cotton is completed in step B described in chloroform；
Step D fills aluminium oxide into the alumina column of the chromatographic column, into the chromatographic silica gel of the chromatographic column
Chromatographic silica gel, and the be linked in sequence upper funnel, alumina column and chromatographic silica gel post are filled, the chromatographic column is assembled；
Step E takes filtrate obtained in step B, is added into the upper funnel of the chromatographic column, successively using just oneself
Alkane, methylene chloride and n-hexane mixed solvent, dehydrated alcohol and chloroform elute the chromatographic column, realize saturated hydrocarbons, virtue
The separation of fragrant hydrocarbon and colloid；
Step F removes the alumina column and the chromatographic silica gel post, returns to the aluminium oxide and the chromatographic silica gel
It receives.
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| CN110687233B (en) * | 2019-08-30 | 2021-02-19 | 中国地质大学（武汉） | Organic matter group component analysis device with monitoring and early warning functions |
| CN111363587B (en) * | 2020-03-26 | 2021-04-27 | 中国石油大学(北京) | Method for separating thioether compounds in petroleum oil products |
| CN114425183B (en) * | 2020-09-24 | 2024-02-23 | 中国石油化工股份有限公司 | Separation method of chromatographic column and crude oil group component and application |
| CN113713428B (en) * | 2021-06-30 | 2022-10-04 | 上海海路生物技术有限公司 | Chromatographic column extension device, system and method for packing column by using same |
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