KR101794669B1 - Gas chromatographic column for separation of saturated and unsaturated hydrocarbon mixtures - Google Patents
Gas chromatographic column for separation of saturated and unsaturated hydrocarbon mixtures Download PDFInfo
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- KR101794669B1 KR101794669B1 KR1020150159250A KR20150159250A KR101794669B1 KR 101794669 B1 KR101794669 B1 KR 101794669B1 KR 1020150159250 A KR1020150159250 A KR 1020150159250A KR 20150159250 A KR20150159250 A KR 20150159250A KR 101794669 B1 KR101794669 B1 KR 101794669B1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- C—CHEMISTRY; METALLURGY
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- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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Abstract
The GC for the gas chromatography (GC) according to the present invention is a GC column using a spray-dried spherical γ-alumina having an average particle diameter of 100 to 200 μm as a filler, and separates C1 to C5 saturated and unsaturated hydrocarbons .
Description
The present invention relates to a GC column for separating saturated and unsaturated hydrocarbons, and more particularly, to a novel GC column having improved separation performance of C1 to C5 hydrocarbons and excellent durability by using spherical γ-alumina as a filler .
GC (Gas Chromatography or Gas Chromatography) is one of the most widely used and used instruments in analytical chemistry laboratories. The basic configuration may include a carrier gas, a sample injector, a column or a column, a detector, and the like. Among these components, the column can be roughly divided into a packed column and a capillary column. Among these columns, a solid support may be filled directly or a solid support may be coated with a liquid.
Generally, the solid support is composed of an inorganic material such as titania, alumina, silica, zirconia, etc., and a solid support using such an inorganic material is superior in heat resistance, chemical resistance, stain resistance and solvent resistance, It is known that it has the advantage of being excellent in thermal stability at high temperature and being usable at high temperature.
Such an inorganic material may be prepared in various physical forms such as a powder form, a dense particle form (ball type), and a granule type depending on the use thereof.
Particularly, in the case of the GC separation tube filler, a spherical phase is used, but the resolution may vary depending on the particle size and size distribution characteristics, and problems such as peak tailing may occur.
The present invention provides a new GC column with improved durability and separation performance using spherically agglomerated y-alumina as a filler in the separation and quantification of C1 to C5 saturated and unsaturated hydrocarbons.
According to an aspect of the present invention,
As a GC column with improved durability and separation performance, spherical agglomerated γ-alumina having an average particle size of 100 to 200 μm spray-dried was used as a filler to solve the above problems.
In addition, the GC column provides a column that separates C1 to C5 hydrocarbons very precisely without occurrence of peak tailing.
In the GC column according to an embodiment of the present invention, the column may satisfy the following
[Relation 1]
N ≥ 700
In the above
In the GC column according to an embodiment of the present invention, the filler and the column may have an average particle diameter of the filler: a column average inner diameter = 1: 10 to 40, but the present invention is not limited thereto.
In the GC column according to an embodiment of the present invention, the filler may satisfy the following
[Relation 2]
150 μm ≤ D 90 ≤ 180 μm
In the
In the GC column according to an embodiment of the present invention, the circularity of the filler may be 0.8 to 1, but is not limited thereto.
The GC column according to the present invention is excellent in durability, heat resistance, chemical resistance, stain resistance and solvent resistance, and further improves the separation performance of C1 to C5 saturated and unsaturated hydrocarbons by using a spherical γ-alumina filler.
Further, the controlled spherical γ-alumina filler according to the present invention improves the separation performance by the average particle diameter and the high circularity.
In addition, the present invention can be very usefully used in a packing column capable of separating / quantifying low-carbon hydrocarbons of liquefied natural gas (LNG) and liquefied petroleum gas (LPG), which have been difficult to analyze substantially in the meantime.
1 is a schematic diagram of a GC apparatus according to embodiments of the present invention and comparative examples.
2 is a schematic diagram of a GC column according to Examples 1 to 3 of the present invention.
3 is an XRD graph showing the crystal structure of the filler according to Examples 1 to 3 of the present invention.
4 is a SEM photograph showing the surface shape of the filler according to Example 1 of the present invention.
5 is a graph showing the separation performance of C1 to C5 saturated and unsaturated hydrocarbons according to Example 1 of the present invention.
Hereinafter, a GC column for separating C1 to C5 hydrocarbons according to the present invention will be described in detail. The following embodiments and drawings are provided by way of example so that those skilled in the art can fully understand the spirit of the present invention. In addition, unless otherwise defined in the technical and scientific terms used herein, unless otherwise defined, the meaning of what is commonly understood by one of ordinary skill in the art to which this invention belongs is as follows, A description of known functions and configurations that may unnecessarily obscure the gist of the present invention will be omitted. It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In the present specification, the singular form includes plural forms unless otherwise specified in the specification. It is noted that the terms "comprises" and / or "comprising" used in the specification are intended to be inclusive in a manner similar to the components, steps, operations, and / Or additions. The terms used herein are used only for the purpose of distinguishing one element from another. Hereinafter, the same member numbers are used for the same members in order to facilitate understanding. In the present specification, the term " connected "includes not only a direct connection but also a connection via another member in the middle.
In describing the present invention, the term "spherical" can be understood to mean not only purely symmetrical spheres but also shapes deviating therefrom, such as, for example, ellipses.
In describing the present invention, the term "alumina " refers to aluminum oxide and includes, for example, alumina, beta -alumina, gamma -alumina, delta-alumina, monohydrated a- Trihydrated? -Alumina, trihydrated? -Alumina, and the like.
In describing the present invention, the inventor of the present invention developed a GC column capable of using γ-alumina as a raw material as a spherical filler, and when using the same, develops components of a GC column in which the separation performance of C1 to C5 hydrocarbons is further maximized And discovered and filed applications.
That is, the GC column according to the present invention has a characteristic that the separation performance of C1 to C5 hydrocarbons can be maximized, and a GC column using a spherical γ-alumina having an average particle diameter of 100 to 200 μm as a spraying agent ) To separate C1 to C5 saturated and unsaturated hydrocarbons.
Specifically, the GC column may be a GC column for C1 to C5 saturated and unsaturated hydrocarbon separation.
Further, the GC column may satisfy the following relational expression (1), but the present invention is not limited thereto.
[Relation 1]
N ≥ 700
In the above
Further, the filler and the column (or the separation tube) according to the present invention may have a mutual size ratio. Specifically, the average inner diameter of the column with respect to the average particle diameter of the filler may be the average particle diameter of the filler: the column average inner diameter = 1: 10 to 1:40, preferably 1:13 to 1:35, more preferably 1 : 15 to 1:30, but the present invention is not limited to this category.
This is to accommodate the fixed-bed filler in the column with a proper distribution, and the C1 to C5 saturated and unsaturated hydrocarbons to be separated through the GC column having the above category can be further increased in speed difference for each component. This may be to improve separation performance according to the present invention.
Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
1 is a diagram illustrating a GC apparatus according to an embodiment of the present invention. 1, the
The
In a specific, non-limiting example, the average length of the
In addition, the
2, the
The filler 110 according to an embodiment of the present invention may be a secondary particle formed by mutually agglomerating primary particles containing gamma -alumina, but the present invention is not necessarily limited thereto.
The average particle diameter of the primary particles is not particularly limited, but preferably has an average particle diameter of 10 to 1,000 nm.
Referring to FIG. 3, it can be confirmed that the filler 110 according to the present invention is formed of gamma-type alumina. As shown in FIG. 3, it can be confirmed that the filler has a pure γ-alumina crystal structure.
Also, the average grain size of the gamma -alumina measured by the Scherrer formula may be 10 to 100 nm, and primary particles having the grain size of the above category uniformly aggregate to form secondary particles Able to know. This improves the durability of the filler according to the present invention and improves the performance of the separator.
Further, as shown in FIG. 3, the peak of the [311] crystal face at about 38 °, the peak of the [222] crystal face at about 39 °, the peak of the [400] crystal face at about 46 °, And the peaks of the [440] crystal face are respectively observed.
In addition, when the intensity of the peak of the [400] crystal face is I1 and the intensity of the peak of the [440] crystal face is I2, the peak intensity ratio I1 / I2 of the two peaks is 0.5 to 1 And more preferably 0.6 to 0.8, but the present invention is not limited to the category of the peak intensity ratio. As a result, the separation performance of C1 to C5 saturated and unsaturated hydrocarbons measured according to the present invention can be further increased.
In the method of measuring the XRD graph shown in FIG. 3, although not particularly limited, the wavelength of copper (Cu) Kα may be 0.154 nm, the acceleration voltage may be 40 kV, and the current may be 150 mA . An example of the measuring device of the XRD graph may be the
Referring to FIG. 4, the filler 110 according to the present invention can confirm the surface shape through an electron microscope (SEM). As shown in FIG. 4, it can be seen that the filler 110 has a spherical shape at a magnification of about 200 times, and that the average size of the filler is 100 to 200 μm. However, It does not.
Also, the spherical filler 110 can measure its roundness by circularity. That is, the circularity is a measurement value of how far the circular form deviates from an accurate circle, and may have a range of 0 to 1. The closer the circularity is to 1, the closer to the ideal circle.
According to one embodiment of the present invention, the circularity of the filler 110 may range from 0.8 to 1, preferably from 0.9 to 1, but is not limited thereto.
In detail, the method of measuring the circularity is not limited to a specific one, but the spherical fillers may be randomly sampled and measured using FPIA-3000.
In addition, when the circularity is 0.8 or more, the resolution R is increased and the peak tailing phenomenon disappears when the hydrocarbon separation performance is measured. Therefore, it is very suitable as a solid support and more precise analysis becomes possible.
In a manufacturing method aspect, the filler (110) comprises the steps of: a) mixing an alumina powder with a solution to produce an alumina slurry; b) spray drying the prepared slurry to produce a spherical dried material; And c) sieving the dried material to obtain a spherical filler.
In the step c), the spherical filler is preferably prepared in a ratio of the average particle diameter of the filler: the column average inner diameter = 1: 10 to 40, but is not limited thereto.
The solution may be any material capable of mixing alumina powder, and may be distilled water or an alcohol having 1 to 5 carbon atoms, but is not limited thereto.
Further, the method of mixing the alumina powder and the solution may be performed by a method known to a person skilled in the art, and it is needless to say that the detailed mixing method can be changed according to the content of the alumina powder, .
In the step b), the spray drying may be performed at 50 to 200 ° C, though not limited thereto.
That is, the filler produced by such a method may have a circularity of 0.8 to 1, and the separation performance of C1 to C5 saturated and unsaturated hydrocarbons is further improved in this range.
In addition, the filler prepared by the above method can have a uniform size distribution. That is, the spherical filler produced in the step c) may satisfy the following relational expression (2). When the filler according to the present invention satisfies the following
[Relation 2]
150 μm ≤ D 90 ≤ 180 μm
In the
In the measurement method of the
In one embodiment of the present invention, referring to FIG. 1, the
The inert gas may be injected under the conditions of 10 to 100 psi, but the present invention is not limited thereto.
In addition, the
In detail, the hydrocarbon according to the present invention may be vaporized by the
In a specific, non-limiting example, the flow rate of the hydrocarbon may be between 10 and 100 mL per minute, more preferably between 10 and 60 mL / min, and even more preferably between 20 and 40 mL / min.
In addition, the
In a GC column according to an embodiment of the present invention, a GC column for containing the above-mentioned filler and separating saturated and distributed hydrocarbons having 1 to 5 carbon atoms can satisfy the following relational expression (1).
[Relation 1]
N ≥ 700
In the above
The number N of the theoretical number N can be expressed by N = 5.55 (t R / W 1/2 ) 2 , where W 1/2 is a half time width of each component peak in terms of time.
In addition, the separation efficiency of the GC column of the present invention can be determined according to the value of the theoretical number of stages N. For example, when the theoretical number N exceeds 500, the separation efficiency is "excellent". When N is 300 to 500 Quot; good ", and when N is 200 to 300, it can be expressed or expressed as "bad ". In particular, when the theoretical number N is 1,000 or more, it can be expressed or expressed as " very excellent ", which is very good for achieving the object of the present invention, but is not limited thereto.
In a specific and non-limiting example, the theoretical number N may be from 700 to 5,000, more preferably from 1,000 to 2,000, but the present invention is not particularly limited to this category.
In other words, the hydrocarbons may be about 15 hydrocarbons, for example the hydrocarbons may be CH 4 , C 2 H 6 , C 2 H 4 , C 3 H 8 , C 3 H 6 , C 2 H 2 , iC 4 H 10 , nC 4 H 10 , ter-2 -C 4 H 8 , 1 -C 4 H 8 , iC 4 H 8 , cis-2 -C 4 H 8 , iC 5 H 12 , nC 5 H 12 , -C 4 H 6 , N 2 balance, and the like.
Referring to FIG. 5, there is shown a graph illustrating separation performance of hydrocarbons according to an embodiment of the present invention. As shown in FIG. 5, the C1 to C5 unsaturated hydrocarbons of the present invention are clearly separated from each other over time, and it can be confirmed that the phenomenon of Tag, tail drag, etc. does not appear.
When the present invention satisfies the above-described relationship (2), the GC column according to the present invention can satisfy the following relationship (3), but the present invention is not limited thereto.
[Relation 3]
R? 0.9
In the above formula (3), R is the resolution and is represented by R = 2 (t R2 -t R1 ) / (
In a specific, non-limiting example, the resolution R may be greater than or equal to 0.9, preferably greater than or equal to 1.0, and more preferably greater than or equal to 1.1, although the present invention is not limited to the above categories.
Further, in the present invention, the filler (100) may contain 98% or more of gamma -alumina. Preferably, the? -Alumina may be 99% or more, more preferably 99.9% or more.
The method of measuring the component or purity of the filler (100) is not particularly limited, but it is possible to investigate each element composition through ICP-OES (inductively coupled plasma-optical emission) analysis, and the present invention is not limited thereto.
Hereinafter, the present invention will be described in detail with reference to the following examples. However, the present invention is not limited to the following examples.
Example 1
100 g of? -alumina powder was mixed with 150 mL of distilled water and stirred for 2 hours at 40 rpm using a magnetic stirrer to prepare a? -alumina slurry.
The prepared slurry was maintained at a temperature of 150 ° C by using a spray drier to prepare a spherical filler (dried material).
The prepared filler was sieved and sieved to obtain a spherical filler having an average particle diameter of 150 μm and a particle size distribution of 100 to 200 μm. In addition, the circularity of the obtained filler was 0.95.
The content of the impurity in the filler was quantitatively measured using ICP-OES (Optima 5300 DV, Perkin-Elmer). As a result of the ICP-OES analysis, Al was 99.99%, and the sum of impurities other than Al (including Li and 4-period transition metal) was 0.005%.
Thereafter, the thus-obtained dried product was filled in a tube made of stainless steel having a length of 2 m and a diameter of 1/8 inch to prepare a filler separation tube (GC column).
The gas chromatography apparatus (GC apparatus) including the above-prepared GC column is similar to or identical to that shown in FIG. 1, and GC analysis for separating
Example 2
The granules prepared by using a spray drier were sieved and sieved to prepare fillers having an average particle diameter of 165 μm and a particle size distribution of 150 to 180 μm, The roundness of one filler was 0.98. The separation characteristics measured in Example 2 are listed in Table 2 and are the same composition as Example 1, but with respect to Example 1 a) increase in average particle size, b) uniformity of size distribution of the particles, and c) Due to the increase in the number of theoretical N, the trailing phenomenon did not appear.
Example 3
The granules prepared by using a spray dryer were sieved and sieved to prepare fillers having an average particle diameter of 130 μm and a particle size distribution of 120 to 150 μm, The circularity of the obtained filler was 0.90. The separation characteristics measured by Example 3 are listed in Table 2 and are the same composition as Example 1, but due to a) reduction in average particle size as compared to Example 1, and b) reduction in the roundness of the filler, N decreased slightly, but no trailing phenomenon occurred.
Comparative Example 1
except that? -alumina was used instead of? -alumina. The separation characteristics measured by Comparative Example 1 are listed in Table 2, and a) the change in the alumina crystal structure (using a-alumina) compared to Example 1 significantly reduced the theoretical number N in GC analysis, .
Comparative Example 2
A solid support of a ball type formed of a-alumina and having an average particle diameter of 2 mm was pulverized with a vibrator micro mill (Fritsch GmBH), sieved and sieved, (Circularity: 0.7) having a diameter of 150 μm and a size distribution of 100 to 200 μm. The separation characteristics measured by Comparative Example 2 are listed in Table 2 and the theoretical number N of the GC analysis greatly decreased due to a) change in alumina crystal structure and b) decrease in circularity compared to Example 1, Phenomenon.
Comparative Example 3
alumina, a filler having an average particle size of 90 占 퐉, a particle size distribution of 75 to 105 占 퐉, and a circularity of 0.95 was prepared. The separation characteristics measured by Comparative Example 3 are listed in Table 2, and because of the decrease in the average particle size compared to Example 1, the theoretical number N of the GC analysis decreased and a tailing phenomenon appeared.
In the separation performance of C1 to C5 saturated and unsaturated hydrocarbons according to Example 1 of the present invention, referring to FIG. 5, hydrocarbons separated according to Example 1 are CH 4 , C 2 H 6 , C 2 H 4 , C 3 H 8, C 3 H 6 , C 2
In Examples 1 to 3 and Comparative Examples 1 to 3, the theoretical number N of each theoretical number N was measured and calculated using the above-described
While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed embodiments, but, on the contrary, Those skilled in the art will recognize that many modifications and variations are possible in light of the above teachings.
Accordingly, the spirit of the present invention should not be construed as being limited to the embodiments described, and all of the equivalents or equivalents of the claims, as well as the following claims, belong to the scope of the present invention .
100, 101: GC column, 110: filler, 120: tube
200: carrier body
300:
400:
1000: GC device
Claims (5)
Wherein the filler satisfies the following relational expression (2), has a circularity of 0.9 to 1,
A gas chromatographic column for C1 to C5 hydrocarbon separation satisfying the following relational expression (1).
[Relation 1]
N ≥ 700
(In the relational expression 1, N is a theoretical number, T R represents the retention time of the peak corresponding to each of the saturated and unsaturated hydrocarbons and W represents the width of the peak corresponding to each of the saturated and unsaturated hydrocarbons in terms of time)
[Relation 2]
150 μm ≤ D 90 ≤ 180 μm
(In the formula 2, D 90 is a particle size corresponding to 90% in the particle size cumulative distribution of the filler)
Wherein the filler and the column are a gas chromatography column for C1 to C5 hydrocarbon separation for a filler having an average particle diameter: a column average inner diameter = 1: 10 to 40.
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KR102139431B1 (en) | 2019-04-02 | 2020-07-29 | 박웅기 | Gas Chromatography Column Cleaner |
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Non-Patent Citations (2)
Title |
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Bulletin of the Japan Petroleum Institute, Vol(2), 1960* |
http://www.chemnet.com/Global/OffertoSell/AluminiumOxideforColumn Chromatography4377919.html(2014.02)* |
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KR102139431B1 (en) | 2019-04-02 | 2020-07-29 | 박웅기 | Gas Chromatography Column Cleaner |
WO2020204592A1 (en) | 2019-04-02 | 2020-10-08 | 박웅기 | Gc column cleaner |
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